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CAS No. : | 554-13-2 | MDL No. : | MFCD00011084 |
Formula : | CLi2O3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | XGZVUEUWXADBQD-UHFFFAOYSA-L |
M.W : | 73.89 | Pubchem ID : | 11125 |
Synonyms : |
Li2CO3
|
Num. heavy atoms : | 6 |
Num. arom. heavy atoms : | 0 |
Fraction Csp3 : | 0.0 |
Num. rotatable bonds : | 0 |
Num. H-bond acceptors : | 3.0 |
Num. H-bond donors : | 0.0 |
Molar Refractivity : | 6.77 |
TPSA : | 63.19 Ų |
GI absorption : | Low |
BBB permeant : | No |
P-gp substrate : | No |
CYP1A2 inhibitor : | No |
CYP2C19 inhibitor : | No |
CYP2C9 inhibitor : | No |
CYP2D6 inhibitor : | No |
CYP3A4 inhibitor : | No |
Log Kp (skin permeation) : | -6.84 cm/s |
Log Po/w (iLOGP) : | 0.0 |
Log Po/w (XLOGP3) : | -0.13 |
Log Po/w (WLOGP) : | -2.45 |
Log Po/w (MLOGP) : | -1.6 |
Log Po/w (SILICOS-IT) : | -0.44 |
Consensus Log Po/w : | -0.92 |
Lipinski : | 0.0 |
Ghose : | None |
Veber : | 0.0 |
Egan : | 0.0 |
Muegge : | 2.0 |
Bioavailability Score : | 0.55 |
Log S (ESOL) : | -0.22 |
Solubility : | 44.9 mg/ml ; 0.608 mol/l |
Class : | Very soluble |
Log S (Ali) : | -0.74 |
Solubility : | 13.3 mg/ml ; 0.181 mol/l |
Class : | Very soluble |
Log S (SILICOS-IT) : | 1.49 |
Solubility : | 2280.0 mg/ml ; 30.8 mol/l |
Class : | Soluble |
PAINS : | 0.0 alert |
Brenk : | 0.0 alert |
Leadlikeness : | 1.0 |
Synthetic accessibility : | 1.76 |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P301+P312+P330-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H319-H351-H361 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In neat (no solvent, solid phase) Li2CO3, TiO2, ZnO mixed, milled in EtOH for 24 h, dried, calcined at 900°C for 4 h, ground, polyvinyl alcohol added, dried, ground, pressed at 100 MPa, sintered at 1000-1125°C for 4 h; monitored by XRD; | ||
With polyvinyl alcohol In neat (no solvent, solid phase) milled in alcohol for 4 h, dried, calcined at 900 °C for 4 h, mixed with polyvinyl alcohol, heated at 550 °C for 4 h, sintered at 1075 °C for 2 h; | ||
In neat (no solvent, solid phase) molar ratio of Li-, Ti-, and Zn-compounds 20:60:20, three-stage annealing (800°C/20 h, 1100°C/10 h, 1200°C/10 h), regrinding in acetone between stages, 3% addn. of Li-carbonate in 2nd and 3rd stages; |
In neat (no solvent, solid phase) mixt. Ln2CO3, TiO2, and ZnO was heated at 800-1170 K for 80-100 h with intermittent homogenization every 20-30 h; X-ray powder diffraction; | ||
In neat (no solvent, solid phase) ball milled in water for 6 h, calcined at 900 °C for 4 h, dried, sintered at 840-920 °C for 4 h; | ||
Stage #1: lithium carbonate; titanium(IV) oxide; zinc(II) oxide for 4h; Stage #2: In neat (no solvent, solid phase) at 900℃; for 4h; Calcination; Stage #3: With PVA In neat (no solvent, solid phase) at 550 - 1075℃; Milling; | Experimental procedure High-purity starting reagents of Li2CO3, ZnO, and TiO2 were mixed according to the stoichiometric formulation Li1.33xZn2-2xTi1+0.67xO4 (x=0.8, 0.9, 0.95). The mixed oxides were ball-milled for 4h in nylon jars with zirconia balls using alcohol as a medium. The wet mixtures were rapidly dried and calcined at 900°C for 4h and then ball-milled again for 4h. The resulting slurries were dried and reground with PVA as binder. The milled powders were pressed into 10mm-diameter disks at a uniaxial pressure of 200MPa. The samples were first heated at 550°C for 4h for debinding and then sintered at various temperatures in ambient atmosphere. | |
Stage #1: lithium carbonate; titanium(IV) oxide; zinc(II) oxide In ethanol for 2h; Sonication; Stage #2: at 80℃; Heating; Stage #3: at 800℃; for 5h; Calcination; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In melt by melting a stoich. mixt. of Li-contg. compd. and V2O5; | ||
byproducts: CO2; at 700°C, in O2 flow; | ||
With O2 In neat (no solvent, solid phase) V2O5 and slight excess of Li2CO3 mixed, pelletized, fired at 600°C for 24 h on O2 stream, then ground, mixed, pelletized again, then fired between 600-800°C for 24 h in O2 stream; |
In neat (no solvent) long heating at 400-450°C in air or slow cooling molten mixt.; detd. by X-ray diffraction, IR-spectroscopy and electron spin resonance; | ||
In neat (no solvent) (air); heating (800°C, 1 d); | ||
In neat (no solvent, solid phase) heating (air, 953 K, 48 h); | ||
In neat (no solvent, solid phase) stoich. mixt. heating in air at 700°C; | ||
Stage #1: vanadia; lithium carbonate In water for 1h; Stage #2: for 7h; Calcination; | ||
With nitric acid | ||
Stage #1: vanadia; lithium carbonate In neat (no solvent, solid phase) at 450℃; for 10h; Stage #2: In neat (no solvent, solid phase) at 680℃; for 48h; | ||
Stage #1: vanadia; lithium carbonate at 600℃; for 5h; Calcination; Stage #2: With air at 900℃; for 3h; | ||
Stage #1: vanadia; lithium carbonate With hexamethylenetetramine In water for 0.5h; Stage #2: In water at 120℃; for 24h; Autoclave; | Synthesis of Li3VO4-Ga2O3/NC All the chemicals were of analytical grade and purchased from Aladdin Chemical Reagent Company. Generally, 1mmol V2O5, 3mmol Li2CO3 and 5mmol hexamethylenetetramine were dissolved in 40ml deionized water and stirred at room temperature for 30min. Then, the above solution was transferred into a 50ml teflon-sealed autoclave and maintained at 120°C for 24h, obtaining Li3VO4 precursor solution. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In neat (no solvent) formation of Li2SnO3 at heating with Li2CO3;; | ||
In neat (no solvent, solid phase) powders were mixed, milled for 4 h, calcined at 1000°C for 4 h, then remilled; XRD; | ||
1000°C, 2 d; |
In neat (no solvent) formation of Li2SnO3 at heating with Li2CO3;; | ||
In neat (no solvent, solid phase) 950-1000°C; tempering with intervals;; | ||
In neat (no solvent, solid phase) Li2CO3 and SnO2 heated at 800°C fo 8 h; | ||
In neat (no solvent) sintered in air at 900°C for 20 h and at 1000°C for 40 h; X-ray diffraction; | ||
In neat (no solvent) byproducts: CO2; calcined at 700°C for 24 h; repeatedly reground and reheated: at1000°C for 16 h, at 1400°C for several h; XRD; | ||
heating (900-950°C, 24 h, Ar atmosphere); XRD; | ||
In neat (no solvent, solid phase) mixed with a molar ratio 1:1 with ethanol, ball-milled for 15 h, dried in ambient atmosphere, calcined at 800°C for 6 h, grinded, pressedinto pellets, sintered at 1000°C for 12 h in air; | ||
In neat (no solvent, solid phase) SnO2 and Li2CO3 were ground, pressed, and calcined for 2 h at 700°C, regrinded, pressed and heated for 2 h at 900°C in air; | ||
In neat (no solvent, solid phase) at 1000℃; for 8h; | ZnSnO3 was prepared using a precursor Li2SnO3 following a modified ion-exchange reaction proposed by Kovacheva [27]. First, Li2SnO3 was prepared by asolid state reaction with Li2CO3, by the following equation: SnO2sLi2CO3s-Li2SnO3sCO2g↑ 1 In this reaction, about 10% excess of Li2CO3 was used for volatility and the mixture was heated at 450 C fo r4-5 h and then at 1000 C for 8h. The product was washed with distilled water and ethanol to remove the excessive lithium component and driedat 70 C. Then as-prepared Li2SnO3 was mixed with KNO3 and ZnCl2 with a weight ratio of 1:8:6 and then put into a pyrextube, which was sealed under vacuum (o1 Torr) and heated at 300 C for 14 days to carry out by the following equation: Li2SnO3s ZnCl2l-ZnSnO3s 2LiCl2l: 2 The excess salts were removed by washing out with distilled water and 0.1 M HCl aqueous solution for several times. White product of ZnSnO3 was finally recovered by rinsing out the HCl solution with distilled water and ethanol followed by drying at 70 C. Particle sizes [25,28] are about 10 nm for SnO2, 50100 nm forZnO, 30100 nm for Zn2SnO4, and 200700 nm for ZnSnO3. | |
With air In neat (no solvent, solid phase) at 650 - 1100℃; for 15h; | 2.1 Experiment General procedure: All the raw materials are purchased from the Aladdin Chemical Reagent Company in Shanghai, China, such as, Li2CO3 (A.R. 99.5%), MnCO3 (A.R. 99.9%), and SnO2 (99.95%). A series of Li2Sn(1-x)O3:xMn4+ (x=0, 0.2, 0.4, 0.6, 0.8, and 1.0mol%) phosphors are synthesized by high temperature solid-state reaction method in air. The stoichiometric raw materials are well grounded in an agate mortar without further purification. The mixtures are placed in an alumina boat, heated to 650°C for 5h, and allowed to cool to room temperature in air. The obtained product is ground again in order to improve the homogeneity and reheated for 10hat 1100°C in air. All products are obtained after natural cooling to room temperature. | |
at 740℃; Inert atmosphere; | ||
at 1000℃; for 48h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In neat (no solvent, solid phase) stoich. mixt. progressive heating between 200 and 1000°C, according to H. Fakrane, A. Aatiq, M. Lamire, A. El Jazouli C. Delmas, Ann. Chim. Fr., in press; | ||
In neat (no solvent) mixt. were heated progressively at 200°C (24 h); 600°C (24h); 900°C (48 h) and 1000°C (48 h) in air; | ||
With poly-vinyl-alcohol In water mixt. of LiCO3, NH4H2PO4 and TiO2 in H2O blended with soln. of poly-vinyl-alcohol in H2O; stirred at 80°C untyl H2O evapd.; heat-treated at 900°C for 12 h under N2 flow in a tube furnace; detd. by XRD, SEM, TEM; |
In neat (no solvent, solid phase) byproducts: NH3, CO2, H2O; Starting materials grounded in the agate mortar was heated to 523 K and further heated at 623 K for 6h. After cooling to room temp. pellets wereformed and heated at 923 K for 6 h, calcinated at 1073 K for 36 h and s intered at 1223 K for 2 h.; XRD; | ||
With polyethylene glycol In further solvent(s) polyethylene glycol solvent; stirred at 80 °C, dried at 150 °C, sintered at 450 °C for 4 h, calcined at 850 °C underAr; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
grinding, heating in air (750°C, 30 h); high-resolution electron microscopy; | ||
With air In solid heating (650°C, 12 h), heating (850°C, 24 h); | ||
In solid reaction in air, initially at 600°C to decompose Li2CO3 and finally at 900°C for 16 h; |
In neat (no solvent) at 850°C; obtained as nanocrystals; | ||
With O2 In neat (no solvent, solid phase) stoich. amount of Li2CO3, Mn2O3 mixed, sintered at 750°C for 24 h; ground, mixed, pressed into pellet, annealed at 860°C for 100 h(O2); cooling;; elem. anal.;; | ||
With air In neat (no solvent, solid phase) a mixt. of Li2CO3 and Mn2O3 (molar ratio 1:2) was calcined at 650°C for 12 h, then heated at 850°C for further 24 h;; | ||
In neat (no solvent, solid phase) mixt. (Mn2O3:Li2CO3=2:1) heated (650°C for 12 h, 850°C, 24 h); atomic absorption spectroscopy, thermogravimetric and differential thermal anal.; | ||
In neat (no solvent, solid phase) solid-state reaction in air, calcinating at 650°C for 12 h, heating to 850°C for 24 h; | ||
In neat (no solvent, solid phase) 6 h at 650°C, 24 h at 850°C in air; | ||
With O2 In neat (no solvent, solid phase) stoich. mixt. ball milling (overnight, EtOH), calcination at 700°C for 10 h in air, annealing at 850°C for 24 h in O2, slow cooling to room temp.; DSC; | ||
In neat (no solvent, solid phase) heating (640°C, 5 h), heating (air, 800°C, 36 h); | ||
In neat (no solvent, solid phase) ball milling (ethanol, 2 h), ethanol evapn. (70°C), calcination (750°C, air), firing (O2, 850°C, 24 h), cooling; | ||
In neat (no solvent) mixt. heated in air from room temp. to 650°C over 3 h; hold at 650°C for 12 h; heated to 800°C over 3 h; hold at 800°C for 12 h; | ||
In neat (no solvent) firing (650°C, 12 h and 850°C, 24 h or 650°C, 48 h or 600°C, 48 h or 550°C, 48 h, resp.); | ||
In neat (no solvent) mixing, milling (ethanol), calcining air (700°C), firing in O2 (870°C, 24 h), slow cooling to room temp.; powder X-ray diffraction; | ||
In neat (no solvent, solid phase) prepd. by solid-state react.; mixt. heated at 820°C for 3 d in air, and cooled with rate of 0.5 °C/min; elem. anal. detd. by ICP after dissolving oxide with diluted sulfuric acid; detd. by powder XRD; | ||
In neat (no solvent, solid phase) stoich. mixt. ground, calcined at 750°C in air for 3 d, with three intermittent grindings, slow cooling to 300°C (0.5°/min); | ||
In neat (no solvent, solid phase) solid-state react.; mixt. fired at 800°C for 48 h; detd. by powder XRD; | ||
In neat (no solvent, solid phase) mixed, heated at 820°C for 3 d (air); cooled 0.5°C/min, elem. anal., XRD; | ||
In neat (no solvent, solid phase) (air) synthesized at 800°C for 48 h; (air) cooled slowly; | ||
In neat (no solvent, solid phase) Mn2O3, Li2CO3 were mixed, heated at 820°C for 72 h in air, quenched; | ||
In neat (no solvent, solid phase) mixt. heated at 830°C in ambient atm.; | ||
With air In neat (no solvent, solid phase) mixt. heating (850°C, air, 1 h); elem. anal.; | ||
In neat (no solvent, solid phase) stoich., mixed, heated at 750°C for 72 h (air); | ||
With air In neat (no solvent, solid phase) stoich.; heated at 820°C for 3 d in air, cooled (0.5°/min); | ||
With air In neat (no solvent, solid phase) stoich. mixt. fired at 800 °C for 48 h in air; detd. by XRD; | ||
With air In neat (no solvent, solid phase) firing Li2CO3, Mn2O3 at 800°C for 48 h in air; elem. anal.; | ||
In neat (no solvent, solid phase) grinding of Li2CO3 and Mn2O3; pelletizing; heating at 700°C for 12 h in air and cooling at rate of 1°C/min; | ||
With air at 800℃; for 24h; | ||
With oxygen In neat (no solvent, solid phase) at 800℃; for 15h; | Samples are synthesized by solid-state reactions. Adequate amounts of Li2CO3 and Mn2O3 are mixed in a mortar and heated at 800 °C for 15 h in an oxygen atmosphere. Obtained products ground and heated for several times. | |
at 750℃; for 12h; | ||
Stage #1: manganese(III) oxide; lithium carbonate In pentane for 0.5h; Milling; Stage #2: at 800℃; for 8h; | ||
at 800℃; for 24h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In solid at 1173 K for 24 h in air or at 973 K for 5 h and then at 1073 K for 10 h in air with intermediate grinding; elem. anal.; | ||
In solid mixt. of Li2CO3 and Co3O4 grinded and therefore was slowly burnt up to 900°C; elem. anal.; detn. by atomic absorption spectroscopy; | ||
In solid solid-state chem. react.; mixt. treated for 10 h at 900°C; detd. by XRD; |
In neat (no solvent) heating (air, 900°C, 3h); | ||
In neat (no solvent) heating a mixt. at 900°C in O2 atm.; | ||
In neat (no solvent) prepd. by the ceramic method from stoichiometric mixtures of Co3O4 and Li2CO3, heated at 1000°C for 2 days; | ||
In neat (no solvent) stoich. amts.; mixt. heated to 500°C, then to 800-1000°C for 48 h in O2; | ||
With air In solid byproducts: CO2; stoich. mixt. ball-milled in ethanol; dried (80°C); heated (520-600°C); quenched; DTA-TGA; XRD; | ||
In neat (no solvent, solid phase) mixt. Li2CO3 and Co3O4 was heated at 850°C for 24 h under O2 flow; | ||
In not given 900°C, in flowing oxygen; | ||
mixt. grinding, pelletizing, heating in air at 800°C for 20 h; | ||
In neat (no solvent) firing stoich. mixt. of Li2CO3 and Co3O4 in air at 900°C for 72 h; elem. anal., X-ray diffraction anal.; | ||
In neat (no solvent, solid phase) in air at 900°C for 24 h; | ||
In neat (no solvent, solid phase) by sintering a Co3O4 an Li2CO3 mixt. at 850°C for 25 h; slow cooling; XRD anal.; | ||
In neat (no solvent, solid phase) firing (500°C, 5 h), firing (850°C, 24 h), cooling (1°C/min); X-ray diffraction; | ||
In neat (no solvent, solid phase) stoich. mixt. ground, pelletized, and treated at 600°C for 12 h under O2 and twice at 900°C for 24 h with intermediate grinding; detd. by XRD; | ||
In neat (no solvent, solid phase) fired at 600°C in air for 24 h or at 400°C in air for 1 wkor at 800°C in air for 24 h; | ||
In neat (no solvent) solid-state reaction, at 900°C for 24 h; XRD; | ||
In neat (no solvent, solid phase) Co3O4 and Li2CO3 were sintered in air at 850°C for 25 h, slow cooled; | ||
With O2 In neat (no solvent, solid phase) Li2CO3 and Co3O4 heated at 900°C in the presence of oxygen; XRD; | ||
dry Li2CO3 mixed with dry Co3O4 (Li:Co=1.05:1) at 750°C for 20 h; XRD; | ||
In neat (no solvent, solid phase) (O2); heated at 600°C for 12 h, then heated at 900°C for 24 and 12 h; | ||
In neat (no solvent) firing (600°C, 10 h and 800°C, 48 h); | ||
In neat (no solvent, solid phase) traditional ceramique technique, 800°C; | ||
In neat (no solvent, solid phase) (air) synthesized at 900°C for 24 h; (air) cooled slowly; | ||
In neat (no solvent, solid phase) thoroughly mixed, finely ground; calcined at 900°C in O2 atm. forseveral h followed by furnace-cooling; procedure repeated three times; | ||
In neat (no solvent, solid phase) mixed for 2 h; preheated at 600°C for 6 h, thoroughly remixed again, fired at 900°C for 24 h; | ||
In melt mixt. melted in Ar atm. at 550°C for 6 h, cooled, ground, mixed, annealed at 800°C for 10 h, cooled, mixed, annealed for further 10 h; ICP anal.; | ||
With air In neat (no solvent) byproducts: CO2, CO; stoich. mixt. grinding (acetone, planetary mill, 2 h), mixt. heating at 5 or 10 or 20K/min in thermoanalyzer in static or dynamic air and dynamic N2/O2 (50 ml/min) or in separate furnace using same temp. programme upto 900°C; TG, DTG, DTA, XRD; | ||
In acetone mixed in acetone; dried overnight in explosion-resistant safely drying oven at 54°C; heated at 850°C for 5 h; elem. anal.; | ||
In neat (no solvent) sintering (850°C, 25 h), annealing in O2, He or vac. (750°C); | ||
In neat (no solvent, solid phase) mixed; reacted; ICP; | ||
In neat (no solvent, solid phase) mixt. sintered at 1000°C for 4 h; | ||
With air In neat (no solvent, solid phase) stoich. mixt. fired at 900 °C for 24 h in air; | ||
In neat (no solvent, solid phase) mixt. of Li2CO3 and Co3O4 heated at 800°C; | ||
In neat (no solvent, solid phase) at 600°C for 12 h and at 900°C for 24 h in air with intermediate grinding; | ||
In neat (no solvent, solid phase) stoich. mixt. heated (800°C); cooled to ambient temp.; | ||
In neat (no solvent, solid phase) Li2CO3 and Co3O4 heated at 600°C for 12 h, ground, sintered at 900°C for 12 h; | ||
In neat (no solvent, solid phase) mixt. fired at 1000°C for 3 h; XRD; | ||
In neat (no solvent, solid phase) mixt. heated at 850°C for 20 h in air; | ||
In neat (no solvent, solid phase) solid state react.; mixed in acetone; dried overnight at 54°C; then annealed at 850°C for 5 h, cooling ramp for 2 or 5 h, then annealed at 1010°C, quenched; annealed at 850°C for 4 h, thenat 1010°C, 5 h cooling ramp; | ||
In neat (no solvent, solid phase) heated in air for 1 d at 900.degree,C; | ||
In neat (no solvent, solid phase) mixt. heated at 600°C for 12 h in dry O2 flow, thn fired at 900°C for 15 d; | ||
In neat (no solvent, solid phase) mixed and ground; heated at 750°C for 3 h; | ||
In neat (no solvent, solid phase) byproducts: K2O; heating stoich. mixt. of cobalt oxide and Li2CO3 at 600°C for 12 h under oxygen flow, regrounging, heating at 900°C for 15 d; NMR; | ||
In neat (no solvent) stoich. mixt. of Li2CO3 and Co3O4 sintered; | ||
In neat (no solvent, solid phase) N2, stoich. mixt. calcined at 800 °C for 6 h and cooled; N2, mixt. ground, sintered at 850 °C for 10 h; detd. by XRD; | ||
In neat (no solvent, solid phase) stoich. amts. mixed; calcined (850°C, 20 h) in air; SEM; | ||
In neat (no solvent, solid phase) heated at 850 °C for 12 h in air; | ||
Stage #1: cobalt(II,III) oxide; lithium carbonate In neat (no solvent, solid phase) Milling; Stage #2: In neat (no solvent, solid phase) at 700℃; for 6h; | ||
at 80℃; | ||
With air at 850 - 950℃; for 12h; Calcination; | ||
With air at 950℃; for 16h; | Pristine LiCoO2 powder was prepared by mixing Co3O4 and Li2CO3 at a molar ratio of 1:1.04, and firing at 950 C for 16 h in air. | |
at 799.84℃; for 12h; Calcination; | 2. Experimental The pure powders of Li2CO3(Aldrich, ACS), and Co3O4(Aldrich,ACS) were weighed and mixed in an agate mortar in ratios cor-responding to stoichiometric LiCoO2and calcined in a platinumcrucible at 1073 K for 12 h. After the calcination the powderwas manually reground and homogenized. The powder was thenpressed into pellets under the pressure of 300 MPa. The pellets weresintered in air dynamic oxygen atmosphere at 1123 K for 100 h andslowly cooled down (3 K min-1) to ensure the formation of a phasefully saturated by oxygen. | |
Stage #1: cobalt(II,III) oxide; lithium carbonate In neat (no solvent, solid phase) at 750℃; for 8h; Calcination; Stage #2: In neat (no solvent, solid phase) at 1050℃; for 6h; | ||
Stage #1: cobalt(II,III) oxide; lithium carbonate at 650℃; for 5h; Stage #2: at 1000℃; for 10h; | ||
at 980℃; for 10h; | ||
With air In neat (no solvent, solid phase) at 900℃; for 12h; | ||
at 1000℃; for 10h; | General procedure: In our work, LiNixCo1-2xMnxO2 (x=0, 0.01 and 0.05) were synthesized by a Sol-gel-assisted high-temperature solid-phase method. Reagent-grade Co(CH3COO)2·4H2O, Ni(CH3COO)2·4H2O, and Mn(CH3COO)2·4H2O were dissolved in distilled water at the required stoichiometric ratio. The aqueous solution was stirred at 130°C continuously until a gel was formed. Followed by a drying under 80°C overnight and a uniformly grinding, the mixture was heated at 350°C for 5h under air atmosphere to form Ni-Mn co-doped Co3O4 precursor. The doped LiCoO2 were then synthesized by sintering the precursor with Li2CO3 at 1000°C for 10h in air. To avoid the loss of lithium in the composition at high temperature, 5% excess Li2CO3 was added during the calcination. For comparation, LiMnxCo1-xO2 and LiNixCo1-xO2 (x=0.05 and 0.1) were also synthesized in the same way without the addition of Ni or Mn. All the prepared samples were used directly without further processing. | |
at 1000℃; for 10h; | The LCO and TLCO materials were both prepared by a traditional solid-state reaction method that used Li2CO3 (99%), Co3O4 (99.7%), Al2O3 (99.9%), MgO (99%), and TiO2 (99.9%) as precursors. All raw materials used are industrialmaterials and pure tothe battery grade. An excess of 5 wt % Li2CO3 was added to compensate for the Li loss during synthesis. The precursors were first ground in an Agate mortar and then the obtained mixed powders were sintered at 1,000C for 10 h. Finally, the intermediate products were ground again in an Agate mortar and sintered for a second timeat 900C for 10 h. | |
Stage #1: cobalt(II,III) oxide; lithium carbonate at 1000℃; for 12h; Stage #2: at 900℃; for 6h; | ||
In neat (no solvent, solid phase) at 750℃; for 15h; | LiCoO2 by solid-state reaction According to the process sketched in Fig. 1, the LiCoO2 was resynthesized by two routes: solid-state reaction employing the Co3O4 residue as one of the reactants and the sol-gel technique having the Li+ and Co2+ ions in the filtered solution as the reactants. The resynthesis of LiCoO2 by the solid-state reaction (5) employed the recovered Co3O4 powder and commercial Li2CO3 as reactants in the Li:Co = 1.05:1 molar ratio, leading to the (Li2CO3)/(Co3O4) molar weight ratio equal to 0.483. After weighted, the reagent powders were mixed and homogenized in a ball mill. The thermally activated solid-state reaction was carried out in a muffle furnace at 750 °C for 15 h, in oxygen flow, under a heating and cooling rate of 10 °C min-1, according to, 2Co3O4 +3Li2CO3 + 1/2O2 → 6LiCoO2 + 3CO2 (5) | |
Stage #1: cobalt(II,III) oxide; lithium carbonate at 600℃; for 5h; Stage #2: With air at 1050℃; for 10h; Calcination; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In solid reaction in air, initially at 600°C to decompose Li2CO3 and finally at 900°C for 16 h; | ||
With air In neat (no solvent, solid phase) multiple mixt. heating (850°C, air); elem. anal.; | ||
In neat (no solvent, solid phase) mixt. heating (1073 K, 24 h); |
for 12h; Calcination; | ||
Stage #1: manganese oxide; lithium carbonate In neat (no solvent, solid phase) for 6h; Milling; Stage #2: With oxygen In neat (no solvent, solid phase) at 550℃; for 6h; Stage #3: With oxygen In neat (no solvent, solid phase) at 750 - 900℃; for 12h; | For preparing LiMn2O4, the mixture of as-prepared Mn3O4 and Li2CO3 (the mole ratio of Li/Mn = 1.05:2) was mixed with alcohol in the ball mill at a speed of 400 r/min for 6 h, then dried at 55 C for 8 h. Then the mixtures were annealed at 550 C for 6 h and sintering at 750, 800, 850, 900 C, respectively, for 12 h and then natural cooling to room temperature under oxygen atmosphere through the whole process [27-29]. Finally a black powder (LiMn2O4) was obtained. Pristine Mn3O4 and Li2CO3 come from industrial manufactures, which mean lower price and less purity than analytical reagent. | |
at 770℃; for 15h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In water mixing N2H6SO4 and Li2CO3 in 2:1 molar ratio in water;; | ||
In water molar ratio (N2H6)SO4/Li2CO3 2:1; recrystn. (water, 40°C); | ||
In water N2H6SO4 and Li2CO3 in 2:1 molar ratio in H2O; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In neat (no solvent, solid phase) powders were mixed, milled for 4 h, calcined at 1000°C for 4 h, then remilled; XRD; | ||
In neat (no solvent, solid phase) stoich. quantities TiO2, Li2CO3 mixed; mixt. pellttized; heated at 600°X for 24 h; cooling, ground, pelletized; heated at 750°C for 24 h; step repeated at 800°C for 48 h;; | ||
In neat (no solvent, solid phase) 950-1000°C; tempering with intervals;; |
annealing in air below 800°C; | ||
In neat (no solvent) heating (800°C, 9.5 h); X-ray anal., differential thermal anal., elem. anal.; | ||
byproducts: CO2; mixt. of Li2CO3 and TiO2 ground and pressed into pellets, fired in oxygen at 800°C for 8 h in an alumina boat lined with gold foil; X-ray anal.; | ||
In neat (no solvent) sintered in air at 900°C for 20 h and at 1000°C for 40 h; X-ray diffraction; | ||
In neat (no solvent) byproducts: CO2; mixed with acetone in agate mortar, dried, fired at 600 to 700°Cfor few hours, 900°C for 12-48 h, ground, fired at 900 to 1200°C for 24-72 h; X-ray powder diffraction; | ||
XRD; | ||
In neat (no solvent) equimol., fired at 700°C for 24 h; | ||
In neat (no solvent, solid phase) mixt. of Li2CO3 and TiO2 in alumina crucible heated at 1273 K in air for12 h; XRD; | ||
In neat (no solvent, solid phase) mixing for 4 h, mixt. was dried and calcined at 800°C for 2 h; XRD; | ||
In neat (no solvent, solid phase) at 820℃; for 4h; Milling; | General procedure: LT and LZT compounds were individually synthesized by conventional solidstate reaction method. Li2CO3 (99%), ZnO (99.9%), and TiO2 (P99%) were used as the starting materials. Stoichiometric quantities of starting materials according to the general formula Li2TiO3 and Li2Zn3Ti4O12 were ball-milled for 6 h using ZrO2 balls with ethanol. After drying at 80 C, the mixed powders were individually ground. The LT and LZT powders were calcined at 820 C for 4 h and 900 C for 8 h, respectively. | |
at 700℃; | ||
Stage #1: lithium carbonate; titanium(IV) oxide In neat (no solvent, solid phase) for 2h; Milling; Stage #2: In neat (no solvent, solid phase) at 900℃; for 24h; Calcination; Inert atmosphere; | 2.1. Material synthesis Li2TiO3 powders were synthesized by a solid-state reaction usingLi2CO3 and TiO2 as precursors. The starting materials were thoroughly mixed by milling in acetone for 2 h. The resulting precursorswere calcined for 24 h in 1 atm of Ar gas. The calcinationtemperatures were 600, 650, 700, 750, 800, 850, and 900 C, andthe heating rate up to each resultant temperature and cooling ratedown to 100 C were both 300 C/h. The powder specimens wereproduced by crushing heat-treated ingots and then packing theminto flat glass sample holders with a depth of 0.2 mm for X-raymeasurements in the Bragg-Brentano geometry. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In neat (no solvent) Fe, P and Li compds. in molar ratio of 1:1:0.5 mixed by ball milling in acetone for 12 h, resulting gel dried at 60°C in vac., reground, heated under N2 for 24 h at 700°C, according to Amine, K. et al.,Electrochem. Commun. 2005, 7, 669; | ||
stoich. mixt. of Li2CO3, FeC2O4, NH4H2PO4 ball milled in acetone; calcined at 350°C for 10 h; annealed at 600°C in Ar; detn. by XRD; | ||
In neat (no solvent, solid phase) stoich.; heated at 350°C for 5 h, treated at 650°C for 18 h in high purity Ar flow, air-cooled to room temp.; |
In neat (no solvent, solid phase) under Ar; milled in high energy AGO-2 planetary mill for 1-10 min, heated at 700°C for 1 h; | ||
With H2 In neat (no solvent) mixt. of Li2CO3, NH4(H2PO4) and Fe(C2O4)*2H2O heated at 350°C for10 h in Ar, calcined at 700°C in H2(5%)/N2 (10°C/min) for 1 h, cooled to room temp.; | ||
In neat (no solvent, solid phase) prepd. by solid-state react.; dispersed into acetone, thoroughly mixed, reground by ball-milling; after evapn. solvent, under N2 gas flow (800 cm**3/min), mixt. decompd. at 280°C for 3 h, reground, then heatedfor 24 h at 600°C; detd. by XRD; | ||
In neat (no solvent, solid phase) byproducts: H2O, NH3; Li-, Fe-contg. compds. and NH4H2PO4 were mixed by a ball milling for a 2h and initial heating to 300°C in an Ar (92%)+ H2 (8%) for 10 h to remove H2O and NH3; the compd. was ground, homogenized, and further h eated to 700°C for 24 h; cooling to room temp.; detd. by powder XRD; | ||
In neat (no solvent) stoich. amts. mixed; ground; pressed; taken in swagelok; fired (700°C, 10 h); XRD; | ||
In neat (no solvent, solid phase) Li2CO3, FeC2O4*2H2O and NH4H2PO4 were mixed, milled in acetone for 1 d, dried, ground, heated to 350°C for 10 h under Ar, reground, sintered at 700°C for 10 h under Ar; | ||
With nitric acid In water soln. of Li2CO3, FeC2O4*2H2O and NH4H2PO4 with nitric acid spray pyrolysed at 450°C; sintered at 800°C under continuous Ar flow; | ||
With poly(styrene-methyl methacrylate-acrylic acid) In nitric acid aq. HNO3; Sonication; reagents dissolved in aq. HNO3 (20% wt.) under N2 and added drop-wise totemplate of org. latex with stirring, mixt. dispersed by ultrasonic, de ssicated at 70°C, pretreatment at 400°C for 8 h, calcined at 600-800°C for 14 h in N2; XRD, SEM, elem. anal.; | ||
In neat (no solvent, solid phase) Fe(C2O4)*2H2O, NH4H2PO4, and Li2CO3 mixed in the molar ratio 1:1:0.5 andthen ball milled in acetone for 12 h; dried at 60°C in vacuum; r eground and heated in a nitrogen atmosphere at 700°C for 24 h; | ||
In neat (no solvent, solid phase) stoich. mixt. of Li2CO3, FeC2O4*2H2O, and NH4H2PO4 heated (600-800°C, 20 h); SEM; | ||
In neat (no solvent, solid phase) stoich.; thoroughly mixed by high-energy ball milling under Ar (zirconiaball-to-powder wt. ratio 10/3, 400 rpm, acetone), slurry dried, calcine d at 700°C for 20 h in tube furnace under flow N2 with heating/cooling rate of 5°C/min; | ||
In neat (no solvent, solid phase) mixt. grinded in agate mortar; pressed into pellets; heated at 350°C for 12 h; annealed at 650°C for 12 h under Ar flow with intermediate grinding; | ||
In neat (no solvent, solid phase) mech. activation followed by high-temp. calcination; stoich. amts. of salts dispersed in EtOH, ground for 4 h by ball milling (200 rpm) at room temp.; dried in oven at 80°C; calcined at 650°C for 12 h in flowing Ar, cooled to room temp.; | ||
In neat (no solvent, solid phase) weighed, mixed in ball milling pot; acetone added; ball milled with agate balls for 10 h; dried in vac. oven for 3 h; sintered in Ar for 6 h at 350°C, then at 650°C in Ar for 20 h; cooled; | ||
In neat (no solvent) at 350 - 700℃; for 38h; Inert atmosphere; | LiFePO4 samples were prepared by mixing stoichiometric amounts of ammonium dihydrogen phosphate (NH4H2PO4, AR), iron oxalate dehydrate (FeC2O4⋅2H2O, AR), and lithium carbonate (Li2CO3, AR) as initial raw materials. The above materials were dispersed into ethanol and then ball milled for 4 h. After evaporating ethanol, in a purified N2 atmosphere, the mixture was treated at 350 °C for 10 h, then was heated to 700 °C and held for 24 h. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In neat (no solvent, solid phase) solid-state react.; mixt. fired at 800°C for 48 h; | ||
In neat (no solvent, solid phase) (air) synthesized at 800°C for 48 h; (air) cooled slowly; | ||
With air In neat (no solvent, solid phase) stoich. mixt. fired at 800 °C for 48 h in air; detd. by XRD; |
With oxygen In neat (no solvent, solid phase) at 800℃; for 15h; | Samples are synthesized by solid-state reactions. Adequate amounts of Li2CO3, NiO, and Mn2O3 are mixed in a mortar and heated at 800 °C for 15 h in an oxygen atmosphere. Obtained products ground and heated for several times. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In neat (no solvent, solid phase) 750 °C; | ||
In neat (no solvent, solid phase) solid-state react.; mixt. fired at 800°C for 48 h; | ||
In neat (no solvent, solid phase) (air) synthesized at 800°C for 48 h; (air) cooled slowly; |
With oxygen In neat (no solvent, solid phase) at 800℃; for 15h; | Samples are synthesized by solid-state reactions. Adequate amounts of Li2CO3, NiO, and Mn2O3 are mixed in a mortar and heated at 800 °C for 15 h in an oxygen atmosphere. Obtained products ground and heated for several times. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With H2 mixing stoich. amounts Li2CO3, V2O5, NH4H2PO4; heated to 650°C insealed tube under stream of H2 for 8 h; as described by Saidi, M.Y.; Ba rker, J.; Huang, H.; Swoyer, J.L.; Adamson, G. Electrochem. Solid State Lett. 2002, 5, A149.; | ||
In acetone V2O5, NH4H2PO4 and Li2CO3 dispersed into acetone; ball milled for 7 h inplanetary mill; solvent evapd.; mixt. decompd. at 350°C for 10 h in air; reground, sintered for 12 h at 700-850°C under H2/Ar flo w; | ||
In acetone byproducts: Li3PO4; V2O5, NH4H2PO4 and Li2CO3 dispersed into acetone; ball milled for 7 h inplanetary mill; solvent evapd.; mixt. decompd. at 350°C for 10 h in air; reground, sintered for 12 h at temp. higher than 850°C u nder H2/Ar flow; |
With citric acid In water byproducts: C; stoich. amts. of V2O5, Li2CO3, NH4H2PO4 dissolved in H2O; satd. aq. soln. of citric acid added (stirring); heated (80°C, stirring); gel dried in air (300°C, 4 h) in Ar flow; ground; pressed; sintered (750°C, 4 h) in Ar flow; TG; TEM; | ||
With citric acid or glucose or PVDF or starch In neat (no solvent, solid phase) byproducts: C; Li2CO3, V2O5, NH4H2PO4, citric acid or glucose or poly(vinylidene difluoride) or starch (Li:V:P:C molar ratio 3:2:3:4.8) dispersed in acetone; ball-milled; dried (70°C); heated (350°C, 5 h) in N2; ground; fired (750°C, 16 h) in N2; SEM; | ||
With acetylene black; H2 In neat (no solvent, solid phase) stoich. mixt. of Li salt, V2O5 and NH4H2PO4 milled for 30 min, heated at350°C for 5 h under 70% Ar + 30% H2 atm., reground, pelletized, sintered at 80°C for 10 h under Ar+H2 atm.; detd. by TGA; | ||
With oxalic acid In neat (no solvent, solid phase) other Radiation; stoich. mixt. of oxalic acid and H2O reacted in H2O (70°C); NH4H2PO4+Li2CO3 (Li:V:P molar ratio 2.10-2.95:1.98-2.04:3) added (stirring, 4h); dried (70°C); heated in Ar (350°C, 4 h); heated by mi crowaves (650-900°C, 3-30 min); SEM; TEM; | ||
With citric acid byproducts: C; according to J. of Power Sources 201(2012)301; gel formed from Li2CO3, V2O5, NH4H2PO4 and citric acid; evapd. (80°C); ground (1 h); presintered (350°C, 4 h) in N2; pressed (15 MPa); heated (750°C, 8 h) in N2; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With carbon In neat (no solvent, solid phase) Li2CO3, NiO, Mn3O4 mixed with carbon; ignited at 800°C, heated to900°C for 3 h, cool to RT in air; | ||
Stage #1: manganese oxide; nickel(II) oxide; lithium carbonate for 1h; Milling; Stage #2: at 500 - 850℃; for 13h; Calcination; | ||
Stage #1: manganese oxide; nickel(II) oxide; lithium carbonate In neat (no solvent, solid phase) for 1h; Milling; Stage #2: In neat (no solvent, solid phase) at 500℃; for 5h; Calcination; Stage #3: In neat (no solvent, solid phase) at 850℃; for 8h; Calcination; | Stoichiometric amounts of NiO, Mn3O4, Li2CO3 (3% excess) and Y2O3 were ball milled for 1 h and then calcinated at 500°C for 5 h and 850°C for 8 h under air atmosphere. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Example 10 [0074] This example describes the preparation and testing of a catalyst of composition 100Fe/3K/1.2Li/2Ag/25SiO2. An iron precipitate was prepared by adding a 1.0 M ammonium carbonate solution to a 1.0 M Fe(NO3)3.9H2O solution at a constant pH of 6.0. The iron precipitate was thoroughly washed with deionized water by vacuum filtration. An aqueous solution comprising Li2CO3, KHCO3 and silicic acid was added to a slurry comprising the iron precipitate. The slurry was spray dried and calcined in air at 300 C. for 5 h. The spray-dried product was impregnated with an aqueous solution of AgNO3 in an amount sufficient to deliver the desired loading of silver via the technique of incipient wetness impregnation. The catalyst was dried for 16 h at 120 C. and calcined in air at 280 C. for 2 h. The testing results may be found in Table 1, wherein CO conversion is expressed as mol % of CO converted to products, C1 selectivity is expressed as wt % of methane relative to total hydrocarbons produced, C5+ productivity is the mass of hydrocarbons of at least 5 carbons atoms produced per hour per kilogram catalyst, alpha is derived from the Anderson-Schulz-Flory plot and CO2 selectivity is mol % CO2 relative to CO converted to all products. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In neat (no solvent, solid phase) according to: Sasaki, T.; Kooli, F.; Iida, M.; Michiue, Y.; Takenouchi, S.; Yajima, Y.; Izumi, F.; Chakoumakos, B. C.; Watanabe, M. Chem. Mater.1998, 10, 4123; | ||
Stage #1: lithium carbonate; potassium carbonate; titanium(IV) oxide for 2h; Milling; Green chemistry; Stage #2: at 600℃; for 20h; Calcination; Green chemistry; | Sample preparation A break-down approach by ball milling the pre-synthesized KTLO was conducted to decrease the particle size. For this, KLTO was synthesized according to the previous report [22] buy the solid-state reaction from K2CO3, Li2CO3 and TiO2 (at the molar ratio of 2.4:0.8:10.4). The starting materials were mixed manually with an agate mortar and a pestle for 2 h and the mixture was calcined in air at 800 °C for 20 h. After cooling to room temperature, the sample was mixed again with an agate mortar and a pestle for another 2 h and the mixture was heated again at 800 °C for 20 h. The product was designated as K0.8TLO(T), where T indicate the temperature for the solid-state reactions in the second step. K0.8TLO(800) was ball-milled using planetary ball mill (Planet M2-3, Gokin Planetaring, Japan), which has two mill pots (80 cm3 inner volume each). K0.8TLO(800) (1 g) and 5 g of zirconia balls with the diameter of 2 mm were added in 5 mL of isopropyl alcohol and the suspension was milled under the speed of 700 rpm (revolution) and 1750 rpm (rotation). After the drying at 80 °C, the product was calcined in air at 600 °C for 3 h. | |
at 899.84℃; for 20h; |
With molybdenum(VI) oxide at 1150℃; for 0.5h; | ||
at 900℃; for 20h; Calcination; | Synthesis General procedure: Lepidocrocite titanate K0.8Zn0.4Ti1.6O4 was synthesized [11] by the calcination of the stoichiometric mixture of K2CO3, ZnO, and TiO2 at 900 °C for 20h. Two other compositions, K0.8Mg0.4Ti1.6O4 and K0.8Li0.27Ti1.73O4, can be prepared similarly but replacing ZnO with MgO [11] and Li2CO3 [18,19], respectively. | |
Stage #1: lithium carbonate; potassium carbonate; titanium(IV) oxide at 600℃; for 0.5h; Calcination; Stage #2: for 20h; Heating; | ||
In neat (no solvent, solid phase) | ||
Heating; | ||
With air at 899.84℃; for 20h; Calcination; | ||
In neat (no solvent) at 1000℃; for 20h; Calcination; | 2.2 Synthesis The layered protonic titanate, H1.07Ti1.73O4·H2O (hereafter HTO), was prepared by the previous proton-exchange method with K0.8Ti1.73Li0.27O4 as a precursor [51]. K0.8Ti1.73Li0.27O4 was prepared by calcining a mixture of TiO2, K2CO3 and Li2CO3 in a stoichiometric ratio at 1000 °C for 20 h. The proton-exchange reaction was carried out in an aqueous of HCl (1 mol L-1, 100 mL/g of K0.8Ti1.73Li0.27O4) at room temperature for 3 day. The acid solution was replaced daily with a fresh one by decantation. After treatment, the sample was collected by filtration, washed with water, and air dried. The protonic product was exfoliated into its monolayer sheets by reacting with ethylamine in a molal ratio of C2H5NH2/H+ (the exchangeable protons in the protonic titanate) being 1:1. Briefly, 0.4 g of protonic titanate was immersed in 100 mL of 0.025 M ethylamine solution, and then kept shaking at room temperature for 24 h. | |
at 900℃; for 20h; Calcination; | 2.1. Synthesis General procedure: Lepidocrocite titanate K0.8Zn0.4Ti1.6O4 was prepared by calcination ofthe stoichiometric mixture containing K2CO3 (5.58 g, 40.4 mmol), ZnO(3.29 g, 40.4 mmol), and TiO2 (12.91 g, 161.6 mmol) at 900 °C for 20 h twice with intermediate grinding [17,18,20]. Other compositions(K0.8M0.4Ti1.6O4, M Co, Ni, Mg; K0.8Fe0.8Ti1.2O4; andK0.8Li0.27Ti1.73O4) can be similarly prepared but replacing ZnO by the respective metal oxide/carbonate (MO, Fe2O3, or Li2CO3 [21] respectively).The sodium titanate nanotubes (NaTNTs) were hydrothermally prepared using the method slightly modified from that of Sun and Li [22].An amount of 2 g of P25 TiO2 and 100 mL of 10 M NaOH was heated at160 °C for 48 h inside a Teflon-lined stainless-steel autoclave. The product was washed with an excess amount of deionized water prior to drying at 80 °C overnight, and calcination at 300 °C for 2 h. The as-made K0.8Zn0.4Ti1.6O4, or the 300 °C-calcined NaTNTs, were kept in a desiccator prior to the intercalation experiments. Potassium palmitate and potassium decanoate were prepared by reacting the corresponding acid with potassium hydroxide [17]. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In neat (no solvent) mixed; pre-heated (500°C, 5 h); calcined (820°C, 12 h) in air; | ||
In neat (no solvent, solid phase) calcined at 480 °C for 6 h, at 850-910 °C for 12 h; | ||
Stage #1: [Ni0.5Co0.2Mn0.3](OH)2; lithium carbonate In water at 120℃; for 12h; Milling; Stage #2: With oxygen at 900℃; for 15h; Calcination; | General procedure: Ni0.5Co0.2Mn0.3(OH)2 precursor was prepared by co-precipitation firstly and from Jinchuan Group Co., Ltd. China. The as-prepared Ni0.5Co0.2Mn0.3(OH)2 and Li2CO3 (99.9%) were mixed thoroughly by ball mill in molar ratio of Li: (Ni0.5Co0.2-Mn0.3) = 1.08:1 using deionized water as grinding aid. The milled mixture was dried at 120°C for 12 h, and calcined at 900°C for 15 h in atmosphere with oxygen concentration of 10 vol.%, 20 vol.%, 30 vol.% and 40 vol.%, then LiNi0.5Co0.2Mn0.3O2 samples were obtained and marked in N-L532, A-L532, O-L532, O2-L532, respectively. |
In ethanol at 80 - 850℃; | ||
Stage #1: [Ni0.5Co0.2Mn0.3](OH)2; lithium carbonate In neat (no solvent, solid phase) at 480℃; for 5h; Stage #2: In neat (no solvent, solid phase) at 880℃; for 12h; Calcination; | 2.1. Materials synthesis Spherical LiNi0.5Co0.2Mn0.3O2 layered materials are synthesized by solid-state reaction using Li2CO3 (99.9%, Kernel, Tianjin) and commercial transition-metal hydroxide precursors (Ni0.5Co0.2Mn0.3)(OH)2 as raw materials. The precursor is mixed thoroughly with excess Li2CO3 in a molar ratio of 2:1.05. The mixture is heated at 480 oC for 5 h then calcined at 880 oC for 12 h in air at a heating rate of 5 oC min-1. | |
In neat (no solvent, solid phase) at 480 - 880℃; for 17h; | 2.1. Materials synthesis Spherical LiNi0.5Co0.2Mn0.3O2 layered materials are synthesized by solid-state reaction using Li2CO3 (99.9%, Kernel, Tianjin) and commercial transition metal hydroxide precursors (Ni0.5Co0.2Mn0.3)(OH)2 as raw materials. The precursor is mixed thoroughly with excess Li2CO3 in a molar ratio of 2:1.05. The mixture isheated at 480 C for 5 h then calcined at 880 C for 12 h in air at aheating rate of 5 C min1. | |
Stage #1: [Ni0.5Co0.2Mn0.3](OH)2; lithium carbonate In neat (no solvent) at 500℃; for 4h; Calcination; Stage #2: With air In neat (no solvent) at 850℃; for 12h; Calcination; | Spherical precursor Ni0.5Co0.2Mn0.3(OH)2 was prepared by the co-precipitation method using sodium hydroxide and oxalic acid as precipitator and complex agent, respectively [29]. The dried precursor was mixed thoroughly with the excess Li2CO3 in molar ratio of 1:1.06. Finally, the mixture was first calcined at 500 C for 4 h, and then at 850 C for 12 h in air to obtain the spherical LiNi0.5Co0.2Mn0.3O2 powders. | |
Stage #1: [Ni0.5Co0.2Mn0.3](OH)2; lithium carbonate In neat (no solvent) at 500℃; for 5h; Stage #2: In neat (no solvent) at 870℃; for 12h; Calcination; | The pristine Li[Ni0.5Co0.2Mn0.3]O2 was prepared by calcining a stoichiometric mixture of [Ni0.5Co0.2Mn0.3](OH)2 precursor (supplied by Jingyuan New Materials Technology Co., Ltd., Chengdu)and Li2CO3 at 500 C for 5 h, then at 870 C for 12 h with a heating rate of 5 C min1. | |
Stage #1: [Ni0.5Co0.2Mn0.3](OH)2; lithium carbonate In neat (no solvent, solid phase) at 500℃; for 5h; Stage #2: With air In neat (no solvent, solid phase) at 900℃; for 12h; Calcination; | Experimental General procedure: Spherical precursor Ni0.5Co0.2Mn0.3(OH)2 particles were synthesized via the hydroxide co-precipitation method. A 2 M starting aqueous solution of NiSO4, MnSO4 and CoSO4 (the cationic molar ratio of Ni:Mn:Co = 5:3:2) was pumped into a stirred tank reactor under the protection of nitrogen atmosphere. A 4 M NaOH solution and NH3*H2O were also pumped into the reactor as the precipitant and chelating agent, respectively. The concentrations of ammonium in tank reactor was controlled at 0.34 mol/L. Solution was pumped in at a feeding rate of about 0.2 L h-1, and the stirring speed were controlled 800 r/min. The pH value was controlledat 11 carefully. The temperature was 50° C. The product was filtered out, washed three times, and then dried at 110° C for 12 h. Certain amounts of Li2CO3 and nickel-cobalt-manganese hydroxide precursor were mixed in a high speed universal disintegrator. The mixture of precursor hydroxide with Li2CO3 was first heatedat 500° C for 5 h and then calcined at 900° C for 12 h in air to obtain crystalline Li1+xNi0.5Co0.2Mn0.3O2. The technological composition for each metal in Li1+xNi0.5Co0.2Mn0.3O2 (x = 0, 0.02, 0.04, 0.06, 0.08) is the same as the stoichiometry determined by inductively coupled plasma (ICP) spectroscopy. | |
Stage #1: [Ni0.5Co0.2Mn0.3](OH)2; lithium carbonate In neat (no solvent) at 500℃; for 5h; Stage #2: In neat (no solvent) at 800℃; for 10h; | 2.1 Synthesis of pristine and coated material General procedure: The pristine LiNi0.5Co0.2Mn0.3O2 (NCM) material was synthesized via co-precipitation method as described in a previously paper [25]. In brief, Ni(NO3)2.6H2O (Aladdin Industrial Corporation, use Aladdin for short in the following part), Co(NO3)2.6H2O (Aladdin) and Mn(NO3)2 (50% aqueous solution) (Aladdin) were used as starting material and NaOH (Aladdin) as complexing agent. The obtained Ni0.5Co0.2Mn0.3(OH)2 precursor was mixed with Li2CO3 (Aladdin) and sintered at 500°C for 5h firstly and then at 800°C for 10h, respectively. The coated materials were prepared by the following procedure. For preparing the Al2O3-coated NCM (AO-NCM), 4.2g Al(NO3)3 (Aladdin) was dissolved in 80ml distilled water (DI water) firstly, then 300g NCM material was added to the reactor and the pH value of the solution was adjusted to 8 by adding NH3.H2O (Aladdin), then the whole turbid liquid was stirred for 1h. Then the whole mixture was dried and sintered at 400°C for 4h. For obtaining the AlPO4-coated NCM (AP-NCM) composite, 4.2g Al(NO3)3 and 1.28g NH4H2PO4 (Aladdin) were dissolved in 50ml DI water, respectively, then putting 300g NCM material to the Al(NO3)3 solution. The NH4H2PO4 solution was added to the turbid liquid slowly with vigorous stirring and the pH value of the solution was adjusted to 8 by adding NH3.H2O. The whole mixture was dried and sintered at 400°C for 4h. | |
Stage #1: [Ni0.5Co0.2Mn0.3](OH)2; lithium carbonate In neat (no solvent, solid phase) at 480℃; for 5h; Stage #2: at 880℃; for 12h; Calcination; | 2.1. Materials preparation Layer oxide cathode materials LiNi0.5Co0.2Mn0.3O2 are producedvia a solid-state process by using commercial-grade precursorNi0.5Co0.2Mn0.3(OH)2 (Haina, Hunan) and Li2CO3 (99.9%, Kernel,Tianjin) as raw materials. The Ni0.5Co0.2Mn0.3(OH)2 precursorpowders are mixed with Li2CO3, while a molar ratio of thetransition-metals and lithium is 1:1.05. Excessive Li2CO3 is used tocompensate for the loss of lithium evaporation during hightemperaturecalcination. The resulting mixtures are heated at480 C for 5h and subsequently calcined at 880 C for 12 h under airatmosphere, with a heating rate of 5 C min1. The sample islabeled as NCM. The LaNi0.5Co0.5O3 and La4NiLiO8 co-coatedLiNi0.5Co0.2Mn0.3O2, labeled as NCM-La 1% (abbreviated as 1 mol%La), NCM-La 3% (abbreviated as 3 mol% La), NCM-La 5% (5 mol% La),are prepared by the following steps: 1) The Ni0.5Co0.2Mn0.3(OH)2powders are mixed with Li2CO3 and C6H9O6LaxH2O (99.9%,Aladdin), and the molar ratio of Ni0.5Co0.2Mn0.3(OH)2/Li2CO3/C6H9O6LaxH2O is 2:1.05:(0.02, 0.06, 0.1), respectively. 2) Themixtures are calcined at the same conditions as the pristine sample. | |
In neat (no solvent, solid phase) at 650 - 950℃; for 20h; Calcination; | Afterward, the as-prepared Ni0.5Co0.2Mn0.3(OH)2 was then mixedwith Li2CO3 (99.5%, Jiangxi Ganfeng Lithium Co., Ltd.) with a Li/TM ratio of 1.04, and nanosized SrCO3 (99.5%, Shanghai MacklinBiochemical Co., Ltd.) with weight percentage of 0%, 0.2%, 0.5% and1%, respectively. The mixtures were calcined at 650 °C for 8 h andthen 950 °C for 12 h with the heating rate of 3 °C min-1 under anoxygen atmosphere. After cooling, the calcined products were groundthen pass through a 400-mesh sieve to achieve the final productswhich were denoted as 0%Sr-MC, 0.2%Sr-MC, 0.5%Sr-MC, 1%Sr-MC, respectively. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In neat (no solvent, solid phase) at 850℃; for 10h; Calcination; | General procedure: Nickel-rich ternary compounds were synthesized by calcining the mixture of as-prepared precursor and Li2CO3 at 850°C for 10h in air. Excessive Li (0-20mol%) was added in order to compensate the loss of lithium during the calcination process. | |
With air In neat (no solvent, solid phase) at 750 - 930℃; for 20h; | 2.1 Preparations of the materials Commercially available spherical hydroxide precursor powder (Ni0.5Co0.2Mn0.3) (OH)2 was chosen as the raw material. The bare LiNi0.5Co0.2Mn0.3O2 was prepared by thoroughly mixing commercial-grade (Ni0.5Co0.2Mn0.3) (OH)2 with Li2CO3, and the xLi2MoO4-inlaid LiNi0.5Co0.2Mn0.3O2 (x=0.005, 0.01, 0.02, 0.05) materials were prepared by thoroughly mixing commercial (Ni0.5Co0.2Mn0.3) (OH)2 with Li2CO3 and certain amounts of MoO3. The obtained mixtures were sintered at 750°C for 8h and then at 930°C for 12h in air. | |
Stage #1: (Ni<SUB>0.5</SUB>Co<SUB>0.2</SUB>Mn<SUB>0.3</SUB>)(OH)<SUB>2</SUB>; lithium carbonate In neat (no solvent, solid phase) Milling; Stage #2: In neat (no solvent, solid phase) at 550 - 850℃; for 18h; Calcination; |
at 500 - 900℃; for 20h; | The Ni0.5Co0.2Mn0.3(OH)2 precursor was obtained from commercial supply. The bare LiNi0.5Co0.2Mn0.3O2 was synthesized as following. The precursor and Li2CO3 were mixed in a molar ratio of 1:1.05 and thoroughly ground, followed by annealing at 500°C for 5h and 900°C for 15h, sequentially. |
Yield | Reaction Conditions | Operation in experiment |
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80% | With 1,3-dimethyl-2-imidazolidinone; 5,5'-(1,4-phenylene)bis(1H-tetrazole); at 100℃; for 96h; | General procedure: Zn(NO3)2.6H2O (0.071 g, 0.24 mmol), 1,2,4,5-benzenetetracarboxylateacid (H4btec, 0.06 g, 0.24mmol), 5,5′-(1,4-phenylene)bis(1H-tetrazole) [6] (H2pbtz,0.05 g, 0.2 mmol), 2 mL N, N′-dimethylformamide (DMF), 1 mL 1,3-Dimethyl-2-imidazolidinone (DMI) in a 20 mL vial was heated at 100 C for 4 days, and then cooled to room temperature, colorless block crystals of 1 were obtained (0.104 g;yield: 90% based on H4btec). |
Yield | Reaction Conditions | Operation in experiment |
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With oxygen In ethanol at 900℃; | General procedure: LiMn1.5Ni0.5O4-xClx (x = 0, 0.05, and 0.1) was prepared by a wet process using MnO2, Li2CO3, NiO and LiCl as starting materials. First, the stoichiometric amount-of LiCl was dissolved in ethanol (this process was excluded during preparation of LiMn1.5Ni0.5O4) followed by addition of Li2CO3. Then, MnO2 and NiO were added to the ethanol solution in which LiCl and Li2CO3 were already dispersed. The solution was stirred for 10 h, and then dried for 6 h at 100 C for vaporizing the ethanol solvent. The obtained precursor mixture was pressed into a pellet and placed in the middle of a quartz bottle. The quartz bottle was located in a uniform heating zone of a tube furnace, and then heated for 12 h at 900 C in a flow of O2 gas. | |
Stage #1: nickel(II) oxide; manganese(IV) oxide; lithium carbonate for 1h; Milling; Green chemistry; Stage #2: at 600 - 850℃; for 18h; Calcination; Green chemistry; | ||
With air at 700 - 900℃; for 48h; Milling; |
Stage #1: nickel(II) oxide; manganese(IV) oxide; lithium carbonate for 12h; Milling; Stage #2: at 850℃; for 10h; Calcination; | ||
Stage #1: nickel(II) oxide; manganese(IV) oxide; lithium carbonate Milling; Stage #2: In neat (no solvent, solid phase) at 850℃; for 10h; Calcination; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With oxygen In ethanol at 900℃; | General procedure: LiMn1.5Ni0.5O4-xClx (x = 0, 0.05, and 0.1) was prepared by a wet process using MnO2, Li2CO3, NiO and LiCl as starting materials. First, the stoichiometric amount-of LiCl was dissolved in ethanol (this process was excluded during preparation of LiMn1.5Ni0.5O4) followed by addition of Li2CO3. Then, MnO2 and NiO were added to the ethanol solution in which LiCl and Li2CO3 were already dispersed. The solution was stirred for 10 h, and then dried for 6 h at 100 C for vaporizing the ethanol solvent. The obtained precursor mixture was pressed into a pellet and placed in the middle of a quartz bottle. The quartz bottle was located in a uniform heating zone of a tube furnace, and then heated for 12 h at 900 C in a flow of O2 gas. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With oxygen In ethanol at 900℃; | General procedure: LiMn1.5Ni0.5O4-xClx (x = 0, 0.05, and 0.1) was prepared by a wet process using MnO2, Li2CO3, NiO and LiCl as starting materials. First, the stoichiometric amount-of LiCl was dissolved in ethanol (this process was excluded during preparation of LiMn1.5Ni0.5O4) followed by addition of Li2CO3. Then, MnO2 and NiO were added to the ethanol solution in which LiCl and Li2CO3 were already dispersed. The solution was stirred for 10 h, and then dried for 6 h at 100 C for vaporizing the ethanol solvent. The obtained precursor mixture was pressed into a pellet and placed in the middle of a quartz bottle. The quartz bottle was located in a uniform heating zone of a tube furnace, and then heated for 12 h at 900 C in a flow of O2 gas. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
61.8% | In ethanol at 20℃; for 5h; |
Yield | Reaction Conditions | Operation in experiment |
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Stage #1: [Ni0.6Co0.2Mn0.2](OH)2; lithium carbonate In neat (no solvent, solid phase) for 3h; Milling; Stage #2: In neat (no solvent, solid phase) at 850℃; for 15h; Calcination; | The stoichiometric amounts of Ni0.6Co0.2Mn0.2(OH)2 precursor and 5wt.% excess Li2CO3 (molar ratio of Li/(Ni+Co+Mn)=1.05:1) were mixed thoroughly by ball milling for 3h, and then was calcined at 850°C for 15h in air to get the layered LiNi0.6Co0.2Mn0.2O2 powder. | |
Stage #1: [Ni0.6Co0.2Mn0.2](OH)2; lithium carbonate In ethanol Stage #2: at 500℃; for 4h; Stage #3: With oxygen at 850℃; for 15h; | The stoichiometric amounts of Ni0.6Co0.2Mn0.2(OH)2 precursor and excess Li2CO3 (molar ratio of (Ni+Co+Mn)/Li = 1:1.05) were mixed thoroughly in ethanol and dried overnight. The mixture microspheres was first heated at 500 C for 4 h, and then sintered at 850 C for 15 h under oxygen flowing, with heat rate of 3 C/min | |
With oxygen In neat (no solvent, solid phase) at 800℃; for 12h; Calcination; | The co-precipitated Ni0.6Co0.2Mn0.2(OH)2 was thoroughly mixed with an excess amount of Li2CO3 (Li/(Ni+Co+Mn)=1.05:1) and then calcinated at 800°C for 12h in flowing oxygen to obtain final LiNi0.6Co0.2Mn0.2O2. The Ni0.6Co0.2Mn0.2(OH)2 precursor with NH3/M of 0.6, 0.8 and 1.0 were denoted as P1, P2 and P3, and the corresponding final LiNi0.6Co0.2Mn0.2O2 products synthesized with precursors obtained at 32h were denoted as L1, L2 and L3. |
Stage #1: [Ni0.6Co0.2Mn0.2](OH)2; lithium carbonate In neat (no solvent) for 4h; Milling; Stage #2: In neat (no solvent) at 500℃; for 4h; Stage #3: In neat (no solvent) at 750℃; for 8h; Calcination; | 2.1 Material synthesis The raw materials of Li2CO3 and Ni0.6Co0.2Mn0.2(OH)2 were well mixed in a molar ratio of 0.525:1 using a planetary ball mill. After being milled for 4h at 180rpm, the precursor mixture was preheated at 500°C for 4h, and then calcined at 750°C for 8h in a tube furnace full of air. The NCM622 samples modified with various AlPO4 contents were prepared by calcining the mixture of the as-synthesized NCM622 and AlPO4 powders at 750°C for 8h in an argon atmosphere. As the modification contents of AlPO4 were 0, 0.1, 0.3, 0.6, 0.9wt%, the corresponding AlPO4-modified NCM622 samples were marked as P, Al1, Al3, Al6 and Al9, respectively. Besides, the sample Al3 and sample P after 50 cycles were named Al3 A and P A, respectively | |
With oxygen at 780 - 850℃; for 17h; | 2.1. Materials synthesis LiNi0.6Co0.2Mn0.2O2 was synthesized via co-precipitation method under an O2 atmosphere. The Ni0.6Co0.2Mn0.2(OH)2 precursorand Li2CO3 were mixed in a mortar with a molar ratio of1:1.04. The obtained compound was first sintered at 780 C for 5 h,and further sintered at 850 C for 12 h under an O2 atmosphere. ThecPAN-NCM composites were prepared via a wet-coating method.Polyacrylonitrile (PAN) was firstly dissolved in N, N-dimethylformamide(DMF). Then, LiNi0.6Co0.2Mn0.2O2 powders weredispersed into the above solution, and the mixture was stirredcontinuously at 50 C to vaporize the solvent and adsorb PAN on thesurface of NCM particles. When the solvent was almost completelyvolatilized, the rest of the dispersion was ultrasound dispersedevenly for 10 min and then heated under vacuum at 120 C for 8 hto completely vaporize the solvent. The resulting powder wasfinally heat-treated at 400 C for 30 min in the air. PAN was alsoheat-treated at 400 C for 30 min to synthesize cPAN, which wasused to analyze the structural characteristics of cPAN. The cPANcoatedNCM cathode material was finally obtained. Concentrationsof 1 wt%, 2 wt% and 4 wt% of cPAN-coated NCM were labeledas cPAN-NCM-1, cPAN-NCM-2, cPAN-NCM-4, respectively (Massloss during heat treatment is not considered). Scheme 1 shows aschematic for the preparation of cPAN-coated LiNi0.6Co0.2Mn0.2O2. | |
Stage #1: [Ni0.6Co0.2Mn0.2](OH)2; lithium carbonate at 1000℃; for 10h; Stage #2: at 900℃; for 2h; Calcination; | 2.1. Materials preparation Ni 0.6 Co 0.2 Mn 0.2 (OH) 2 precursor was synthesized via a coprecipitationroute. 2 mol L -1 NiSO 4 , CoSO 4 and MnSO 4 (molarratio, Ni:Co:Mn = 6:2:2) solution was pumped into a continuousstirred tank reactor (CSTR, capacity of 10 L). At thesame time, 10 mol L -1 NaOH (aq) as pH control agent and0.2 mol L -1 NH 3 •H 2 O (aq) as chelating agent were mixed uniformlywith the volume ratio of 7:3 as alkaline solution. The pH,temperature, and stirring speed in the CSTR were 11.4, 50 °C and550 rpm., respectively. After that, the aging process was furthermaintained for 24 h to ensure complete reaction. The whole reactionprocess in the CSTR was conducted under N 2 . The obtained(Ni 0.6 Co 0.2 Mn 0.2 )(OH) 2 precursor was filtered, washed andthen dried at 120 °C for 24 h in air. To prepare the micronsizedsingle-crystal LiNi 0.6 Co 0.2 Mn 0.2 O 2 (SC-NCM622), the obtainedNi 0.6 Co 0.2 Mn 0.2 (OH) 2 precursor was first mixed with the stoichiometricamount of Li 2 CO 3 (molar ratio, Li/(Ni + Co + Mn) = 0.45),and the mixtures were calcined at 10 0 0 °C for 10 h in a mufflefurnace to form large layered/spinel oxide single particles. Followingthis, the stoichiometric amount of Li 2 CO 3 (molar ratio,Li/(Ni + Co + Mn) = 0.55) was further mixed with the above oxidesand calcined at 900 °C for 12 h in a muffle furnace to finally formthe micron-sized single-crystal particles. Considering the volatilizationof lithium at high temperature, 10% excess lithium sourceswere added. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In neat (no solvent, solid phase) at 750℃; for 6h; | Preparation General procedure: All the samples were prepared by a solid state reaction method. The raw materials were K2CO3 (99.9%), SrCO3 (99%), H3BO3 (99.5%), NH4H2PO4 (98%), Dy2O3(99.99%), Na2CO3 (99.9%) and Li2CO3 (99.9%). The overall reaction of KSrBP2O8:Dy(3+) and KSrBP2O8:Dy(3+), M(+) may be respectively written as (1) and (2) exhibited below. (1/2)K2CO3 + (1-x)SrCO3 + H3BO3 + 2NH4H2PO4 + (x/2)Dy2O3 = KSr(1-x)BP2O8 : xDy(3+) (1) (1/2)K2CO3 + (1-x-y)SrCO3 + H3BO3 + 2NH4H2PO4 + (x/2)Dy2O3 + (y/2)M2CO3 = KSr(1-x)BP2O8 : xDy(3+); yM(+) (2) The starting materials were weighed according to the ratios of (1) and (2), then blended and milled thoroughly in an agate mortar. The mixture were put into analumina crucible and sintered in a muffle at 750 C for 6.5 h. Finally, the as synthesized samples were slowly cooled to room temperature. |
Yield | Reaction Conditions | Operation in experiment |
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Stage #1: niobium(V) oxide; lithium carbonate; sodium carbonate; potassium carbonate In neat (no solvent, solid phase) at 750℃; for 4h; Calcination; Stage #2: With PVA In neat (no solvent, solid phase) at 600 - 1080℃; for 3h; | 2 Experimental Sodium carbonate (Na2CO3, 99.8%), potassium carbonate (K2CO3, 99%), lithium carbonate (Li2CO3, 99.5%), and niobium oxide (Nb2O5, 99.95%) were used as raw materials. These powders were weighed to the composition of [Li0.06(Na0.52K0.48)0.94+x]NbO3 (x=0, 0.5, 1.0, 1.5, 2.0, and 2.5at.%) and then ball milled in ethanol for 4h with the stabilized ZrO2 ceramic balls. The ball-milled slurry was dried and then calcined at 750°C for 4h to synthesize a single phase. The calcined powders were then compacted into disks of 10mm in diameter and 1mm in thickness at 200MPa using 5wt.% PVA as a binder. The disks were heated at 600°C for 1h to remove the binder and then normally sintered at 1020-1080°C for 2h without any protection to suppress volatilization of sodium and potassium. Silver electrodes were fired on the top and bottom surfaces of the sintered samples. | |
Stage #1: niobium(V) oxide; lithium carbonate; sodium carbonate; potassium carbonate In neat (no solvent, solid phase) for 24h; Milling; Stage #2: In neat (no solvent, solid phase) at 750 - 850℃; for 5h; Calcination; | 2. Experimental procedure General procedure: Different Li concentration modified [Lix(K0.48Na0.52)1-x]NbO3 powders (x 2%, 4%, 6%), which were named as L2 (Li: 2%), L4(Li: 4%) and L6 (Li: 6%), were separately prepared by a conventional solid state reaction method. High purity powders of Na2CO3(99.5%), K2CO3 (99.9%), Li2CO3 (99%) and Nb2O5 (99.99%) were used as starting raw materials. The powders in the stoichiometric ratio were mixed in the alcohol using ball milling for 24 h. After ball milling, the raw materials were dried and calcinated at the temperature range of 750-850° C for 5 h according to Li concentration. |
Yield | Reaction Conditions | Operation in experiment |
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Stage #1: niobium(V) oxide; lithium carbonate; sodium carbonate; potassium carbonate In neat (no solvent, solid phase) at 750℃; for 4h; Calcination; Stage #2: With PVA In neat (no solvent, solid phase) at 600 - 1080℃; for 3h; | 2 Experimental Sodium carbonate (Na2CO3, 99.8%), potassium carbonate (K2CO3, 99%), lithium carbonate (Li2CO3, 99.5%), and niobium oxide (Nb2O5, 99.95%) were used as raw materials. These powders were weighed to the composition of [Li0.06(Na0.52K0.48)0.94+x]NbO3 (x=0, 0.5, 1.0, 1.5, 2.0, and 2.5at.%) and then ball milled in ethanol for 4h with the stabilized ZrO2 ceramic balls. The ball-milled slurry was dried and then calcined at 750°C for 4h to synthesize a single phase. The calcined powders were then compacted into disks of 10mm in diameter and 1mm in thickness at 200MPa using 5wt.% PVA as a binder. The disks were heated at 600°C for 1h to remove the binder and then normally sintered at 1020-1080°C for 2h without any protection to suppress volatilization of sodium and potassium. Silver electrodes were fired on the top and bottom surfaces of the sintered samples. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Stage #1: niobium(V) oxide; lithium carbonate; sodium carbonate; potassium carbonate In neat (no solvent, solid phase) at 750℃; for 4h; Calcination; Stage #2: With PVA In neat (no solvent, solid phase) at 600 - 1080℃; for 3h; | 2 Experimental Sodium carbonate (Na2CO3, 99.8%), potassium carbonate (K2CO3, 99%), lithium carbonate (Li2CO3, 99.5%), and niobium oxide (Nb2O5, 99.95%) were used as raw materials. These powders were weighed to the composition of [Li0.06(Na0.52K0.48)0.94+x]NbO3 (x=0, 0.5, 1.0, 1.5, 2.0, and 2.5at.%) and then ball milled in ethanol for 4h with the stabilized ZrO2 ceramic balls. The ball-milled slurry was dried and then calcined at 750°C for 4h to synthesize a single phase. The calcined powders were then compacted into disks of 10mm in diameter and 1mm in thickness at 200MPa using 5wt.% PVA as a binder. The disks were heated at 600°C for 1h to remove the binder and then normally sintered at 1020-1080°C for 2h without any protection to suppress volatilization of sodium and potassium. Silver electrodes were fired on the top and bottom surfaces of the sintered samples. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Stage #1: niobium(V) oxide; lithium carbonate; sodium carbonate; potassium carbonate In neat (no solvent, solid phase) at 750℃; for 4h; Calcination; Stage #2: With PVA In neat (no solvent, solid phase) at 600 - 1080℃; for 3h; | 2 Experimental Sodium carbonate (Na2CO3, 99.8%), potassium carbonate (K2CO3, 99%), lithium carbonate (Li2CO3, 99.5%), and niobium oxide (Nb2O5, 99.95%) were used as raw materials. These powders were weighed to the composition of [Li0.06(Na0.52K0.48)0.94+x]NbO3 (x=0, 0.5, 1.0, 1.5, 2.0, and 2.5at.%) and then ball milled in ethanol for 4h with the stabilized ZrO2 ceramic balls. The ball-milled slurry was dried and then calcined at 750°C for 4h to synthesize a single phase. The calcined powders were then compacted into disks of 10mm in diameter and 1mm in thickness at 200MPa using 5wt.% PVA as a binder. The disks were heated at 600°C for 1h to remove the binder and then normally sintered at 1020-1080°C for 2h without any protection to suppress volatilization of sodium and potassium. Silver electrodes were fired on the top and bottom surfaces of the sintered samples. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Stage #1: niobium(V) oxide; lithium carbonate; sodium carbonate; potassium carbonate In neat (no solvent, solid phase) at 750℃; for 4h; Calcination; Stage #2: With PVA In neat (no solvent, solid phase) at 600 - 1080℃; for 3h; | 2 Experimental Sodium carbonate (Na2CO3, 99.8%), potassium carbonate (K2CO3, 99%), lithium carbonate (Li2CO3, 99.5%), and niobium oxide (Nb2O5, 99.95%) were used as raw materials. These powders were weighed to the composition of [Li0.06(Na0.52K0.48)0.94+x]NbO3 (x=0, 0.5, 1.0, 1.5, 2.0, and 2.5at.%) and then ball milled in ethanol for 4h with the stabilized ZrO2 ceramic balls. The ball-milled slurry was dried and then calcined at 750°C for 4h to synthesize a single phase. The calcined powders were then compacted into disks of 10mm in diameter and 1mm in thickness at 200MPa using 5wt.% PVA as a binder. The disks were heated at 600°C for 1h to remove the binder and then normally sintered at 1020-1080°C for 2h without any protection to suppress volatilization of sodium and potassium. Silver electrodes were fired on the top and bottom surfaces of the sintered samples. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Stage #1: niobium(V) oxide; lithium carbonate; sodium carbonate; potassium carbonate In neat (no solvent, solid phase) at 750℃; for 4h; Calcination; Stage #2: With PVA In neat (no solvent, solid phase) at 600 - 1080℃; for 3h; | 2 Experimental Sodium carbonate (Na2CO3, 99.8%), potassium carbonate (K2CO3, 99%), lithium carbonate (Li2CO3, 99.5%), and niobium oxide (Nb2O5, 99.95%) were used as raw materials. These powders were weighed to the composition of [Li0.06(Na0.52K0.48)0.94+x]NbO3 (x=0, 0.5, 1.0, 1.5, 2.0, and 2.5at.%) and then ball milled in ethanol for 4h with the stabilized ZrO2 ceramic balls. The ball-milled slurry was dried and then calcined at 750°C for 4h to synthesize a single phase. The calcined powders were then compacted into disks of 10mm in diameter and 1mm in thickness at 200MPa using 5wt.% PVA as a binder. The disks were heated at 600°C for 1h to remove the binder and then normally sintered at 1020-1080°C for 2h without any protection to suppress volatilization of sodium and potassium. Silver electrodes were fired on the top and bottom surfaces of the sintered samples. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Stage #1: titanium(IV) oxide; lithium carbonate With air at 450℃; for 6h; Calcination; Stage #2: With air at 850℃; for 20h; Calcination; | ||
Stage #1: titanium(IV) oxide; lithium carbonate In water for 4h; Milling; Stage #2: at 800℃; for 12h; Calcination; | ||
In neat (no solvent, solid phase) at 850℃; for 12h; Calcination; Inert atmosphere; | 2 Experimental The Ce-modified LTO was prepared via a conventional solid-state reaction method. 1.0548 g Li2CO3, 2.6360 g TiO2 (anatase) and 0.0868 g Ce(NO3)3·6H2O were blended with anhydrous ethanol as the milling medium and ball-milled at a speed of 300 rpm for 3 h to obtain a slurry. Excessive Li2CO3 was provided to compensate the loss of Li during the high-temperature synthesis. The resultant slurry was dried at 80 °C for 12 h in a vacuum to obtain the precursors. The precursors were then calcinated at 850 °C for 12 h in a flowing N2 atmosphere. To make a contrast, pristine LTO was prepared in the similar way, but treated in air without Ce(NO3)3·6H2O. The obtained samples were named LTO-Ce and LTO-0, respectively. |
With potassium chloride; sodium chloride In melt at 850℃; for 4h; | General procedure: In this study, Li4Ti5O12 powders were prepared by two different methods. The precursors of LTO powder samples were synthesized using Li2CO3 (analytically pure 99.9%), TiO2 (anatase, average particle size0.8μm, purity >99%, Panzhihua Tianlun Chemical Corporation, Panzhihua, China) (denoted as LTO-S), Li2CO3 (analytically pure 99.9%) and ultrafine titanium powder (average particle size1-2μm micron-sized, Pangang Group Research Institute Co. Ltd.) (denoted as LTO-Ti). Such precursors were mixed and grinded in a mortar with a pestle. The molar ration of TiO2 and Li2CO3 was 5:2, Ti: Li2CO3 was 6:2. The molar ratio of the eutectic mixture of NaCl-KCl was fixed at 1:1which was used as solvent. The mixed salts were mixed thoroughly and grinded in a mortar with a pestle and dried under vacuum at 120°C for 24h, to minimize the water content in the molten salt (NaCl-KCl). Then, precursor and solvent were mixed in alumina crucibles and transferred to a muffle furnace immediately. The mixed precursor powders were calcined at 850°C for 4h and then naturally cooled to room temperature. The heating rate was 10°Cmin-1 for all temperature settings. After sintering, a powder was immediately precipitated in the molten salt solution. After cooling and solidification, this solid mixture was immersed in deionized water, and all of the salt elements were dissolved. The precipitated powders were the metal oxide particles which are insoluble in water, so that all of the precipitates could be separated. The obtained particles were collected and vacuum treated again at 120°C for 24h to eliminate residual water on particle surfaces. | |
In neat (no solvent, solid phase) at 800℃; for 6h; Inert atmosphere; | The pristine Li4Ti5O12 sample was prepared by a solid-state reaction from 1.22 g Li2CO3 (AR, Shanghai Chemical Agents Co., Ltd.)and 2.415 g TiO2 (AR, Nanjing High Technology Nano Material Co.,Ltd.) as raw materials. The TiO2 and Li2CO3 were mixed in a mortar and pestle, which were heated for 6 h at 800 C under Ar atmosphere. The sample was simply named as LTO. | |
Stage #1: titanium(IV) oxide; lithium carbonate for 4h; Milling; Stage #2: In neat (no solvent, solid phase) at 850℃; for 10h; Calcination; Inert atmosphere; | General procedure: Size-tailored Ce-doped Li4Ti5O12 (STCLTO) was synthesized by solid-state reaction. TiO2 (99.8%, 10-25 nm, anatase, Aladdin Industrial Corporation), Li2CO3 (AR 99%, Aladdin Industrial Corporation), and CeN3O9*6H2O (AR 99.5%, Aladdin Industrial Corporation) were ball-milled with ethanol in a planetary ball-mill system at the speed of 300 rpm for 4 h, with molar ratio based on the formula Li4Ti4.95Ce0.05O12. Glucose (Sinopharm Chemical Reagent Co., Ltd) was used as the carbon source and mixed with the above components according to the weight ratio of TiO2: C6H12O6 3:1. The homogeneous slurry was obtained after the ball-milling step and dried at 80 °C for 12 h to get the precursor. The precursor was calcined at 850 °C for 10 h in a tube furnace under N2 atmosphere to produce the carbon coated Ce-doped Li4Ti5O12 (CLTO/C) sample. The CLTO/C sample was further treated in a muffle furnace at 500 °C for 4 h in air to remove the carbon coating and obtain STCLTO. Pristine Li4Ti5O12 (LTO) was synthesized based on the same procedure except that both CeN3O9*6H2O and glucose were not used during the ball-milling step. Similarly, Ce-doped Li4Ti5O12 (CLTO) was also synthesized based on the same procedure except that glucose was not used during the ball-milling step. | |
In neat (no solvent, solid phase) at 750℃; for 12h; | LTO and FLTO were synthesized by a step and two-step solid method, respectively. Due to lithium source can volatilizeat higher temperature, Li2CO3 and anatase TiO2 were mixed with the atomic ratio of 0.88 for Li:Ti with ethanol. Then it sinterized at 650, 700, 750, 800, 850, 900 °C for 12 h to obtain pure LTO. | |
Stage #1: titanium(IV) oxide; lithium carbonate In neat (no solvent, solid phase) for 6h; Milling; Stage #2: In neat (no solvent, solid phase) at 800℃; for 12h; Calcination; | 2.1. Synthesis of Li4Ti5-xYxO12 General procedure: Li4Ti5-xYxO12 were prepared by ball-milling pretreatment andhigh-temperature solid-state method. The specific steps were as follows: Li2CO3 (AR,97%), anatase-TiO2 (AR,99%) andY(NO3)36H2O (AR,99.5%) were used as lithium, titanium and yttrium source, respectively and mixed at stoichiometric ratio.Anhydrous ethanol was added into the mixture as solvent forhigh-speed ball milling for 6 h. After that, the homogeneousmixtures were put into oven at 60C for 12 h. The dried sampleswere placed in muffle furnace and calcined at 800 C for 12 hunder air condition. After cooled to room temperature, the Li4Ti5-xYxO12 samples were ground to powder. The obtained Li4Ti5-xYxO12 (x = 0, 0.10, 0.15, 0.20, 0.25) samples with differentdoping amounts (x) were named as Y0, Y10, Y15, Y20, Y25,respectively. |
Yield | Reaction Conditions | Operation in experiment |
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Stage #1: ammonium dihydrogen phosphate; vanadyl oxalate; lithium carbonate With cetyltrimethylammonim bromide In water at 60℃; Sonication; Stage #2: at 400℃; for 5h; Inert atmosphere; Stage #3: at 700℃; for 10h; Inert atmosphere; | Synthesis of Li3V2-(4/3)xTix(PO4)3/C General procedure: 0.01 mol monoclinic Li3V2-(4/3)xTix (PO4)3/C were obtained using an ultrasound-assisted sol-gel method to mix stoichiometric amounts of V2O5, H2C2O4, Li2CO3, NH4H2PO4, TiO2 and CTAB. TiO2 is dopant and CTAB is cationic surfactant. Moreover, 1.0 g Polyvinylidene Fluoride (PVDF) was also added in as carbon source. First, V2O5 and H2C2O4 in a molar ratio of 1:3 were dissolved in deionized water under magnetic stirring at 60°C. After about half an hour a clear blue VOC2O4 solution formed (V2O5+3H2C2O4→2VOC2O4+2CO2+3H2O). Second, Li2CO3 and NH4H2PO4 were added in this solution in turn. Both processes were with gas generating and a hydrophilic homogeneous colloid was formed. Third, the aqueous suspension of Cetyltrimethyl Ammonium Bromide (CTAB, 1 mmol), TiO2 and PVDF (1.0 g), which was obtained with the help of ultrasound, was added in the colloid. The mixture was magnetic stirred at 60°C until the water evaporates mostly. One thing to note here is that the TiO2 and PVDF is water insoluble, so we put them and CTAB together into the deionized water and then stirred and ultrasonic dispersed to obtain this aqueous suspension, at 60°C. Driven by Coulomb force, CTAB captured the anionic LVP colloid, which rearranged the charge density and formed composite micelles in the solution [27]. Finally, the green thick sol was dried at 80°C in vacuum oven and then heated at 400°C for 5 h and 700°C for 10 h under Argon flow to synthesize the final composites. |
Yield | Reaction Conditions | Operation in experiment |
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Stage #1: ammonium dihydrogen phosphate; vanadyl oxalate; lithium carbonate; titanium(IV) oxide With cetyltrimethylammonim bromide In water at 60℃; Sonication; Stage #2: at 400℃; for 5h; Inert atmosphere; Stage #3: at 700℃; for 10h; Inert atmosphere; | Synthesis of Li3V2-(4/3)xTix(PO4)3/C General procedure: 0.01 mol monoclinic Li3V2-(4/3)xTix (PO4)3/C were obtained using an ultrasound-assisted sol-gel method to mix stoichiometric amounts of V2O5, H2C2O4, Li2CO3, NH4H2PO4, TiO2 and CTAB. TiO2 is dopant and CTAB is cationic surfactant. Moreover, 1.0 g Polyvinylidene Fluoride (PVDF) was also added in as carbon source. First, V2O5 and H2C2O4 in a molar ratio of 1:3 were dissolved in deionized water under magnetic stirring at 60°C. After about half an hour a clear blue VOC2O4 solution formed (V2O5+3H2C2O4→2VOC2O4+2CO2+3H2O). Second, Li2CO3 and NH4H2PO4 were added in this solution in turn. Both processes were with gas generating and a hydrophilic homogeneous colloid was formed. Third, the aqueous suspension of Cetyltrimethyl Ammonium Bromide (CTAB, 1 mmol), TiO2 and PVDF (1.0 g), which was obtained with the help of ultrasound, was added in the colloid. The mixture was magnetic stirred at 60°C until the water evaporates mostly. One thing to note here is that the TiO2 and PVDF is water insoluble, so we put them and CTAB together into the deionized water and then stirred and ultrasonic dispersed to obtain this aqueous suspension, at 60°C. Driven by Coulomb force, CTAB captured the anionic LVP colloid, which rearranged the charge density and formed composite micelles in the solution [27]. Finally, the green thick sol was dried at 80°C in vacuum oven and then heated at 400°C for 5 h and 700°C for 10 h under Argon flow to synthesize the final composites. |
Yield | Reaction Conditions | Operation in experiment |
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Stage #1: ammonium dihydrogen phosphate; vanadyl oxalate; lithium carbonate; titanium(IV) oxide With cetyltrimethylammonim bromide In water at 60℃; Sonication; Stage #2: at 400℃; for 5h; Inert atmosphere; Stage #3: at 700℃; for 10h; Inert atmosphere; | Synthesis of Li3V2-(4/3)xTix(PO4)3/C General procedure: 0.01 mol monoclinic Li3V2-(4/3)xTix (PO4)3/C were obtained using an ultrasound-assisted sol-gel method to mix stoichiometric amounts of V2O5, H2C2O4, Li2CO3, NH4H2PO4, TiO2 and CTAB. TiO2 is dopant and CTAB is cationic surfactant. Moreover, 1.0 g Polyvinylidene Fluoride (PVDF) was also added in as carbon source. First, V2O5 and H2C2O4 in a molar ratio of 1:3 were dissolved in deionized water under magnetic stirring at 60°C. After about half an hour a clear blue VOC2O4 solution formed (V2O5+3H2C2O4→2VOC2O4+2CO2+3H2O). Second, Li2CO3 and NH4H2PO4 were added in this solution in turn. Both processes were with gas generating and a hydrophilic homogeneous colloid was formed. Third, the aqueous suspension of Cetyltrimethyl Ammonium Bromide (CTAB, 1 mmol), TiO2 and PVDF (1.0 g), which was obtained with the help of ultrasound, was added in the colloid. The mixture was magnetic stirred at 60°C until the water evaporates mostly. One thing to note here is that the TiO2 and PVDF is water insoluble, so we put them and CTAB together into the deionized water and then stirred and ultrasonic dispersed to obtain this aqueous suspension, at 60°C. Driven by Coulomb force, CTAB captured the anionic LVP colloid, which rearranged the charge density and formed composite micelles in the solution [27]. Finally, the green thick sol was dried at 80°C in vacuum oven and then heated at 400°C for 5 h and 700°C for 10 h under Argon flow to synthesize the final composites. |
Yield | Reaction Conditions | Operation in experiment |
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Stage #1: ammonium dihydrogen phosphate; vanadyl oxalate; lithium carbonate; titanium(IV) oxide With cetyltrimethylammonim bromide In water at 60℃; Sonication; Stage #2: at 400℃; for 5h; Inert atmosphere; Stage #3: at 700℃; for 10h; Inert atmosphere; | Synthesis of Li3V2-(4/3)xTix(PO4)3/C General procedure: 0.01 mol monoclinic Li3V2-(4/3)xTix (PO4)3/C were obtained using an ultrasound-assisted sol-gel method to mix stoichiometric amounts of V2O5, H2C2O4, Li2CO3, NH4H2PO4, TiO2 and CTAB. TiO2 is dopant and CTAB is cationic surfactant. Moreover, 1.0 g Polyvinylidene Fluoride (PVDF) was also added in as carbon source. First, V2O5 and H2C2O4 in a molar ratio of 1:3 were dissolved in deionized water under magnetic stirring at 60°C. After about half an hour a clear blue VOC2O4 solution formed (V2O5+3H2C2O4→2VOC2O4+2CO2+3H2O). Second, Li2CO3 and NH4H2PO4 were added in this solution in turn. Both processes were with gas generating and a hydrophilic homogeneous colloid was formed. Third, the aqueous suspension of Cetyltrimethyl Ammonium Bromide (CTAB, 1 mmol), TiO2 and PVDF (1.0 g), which was obtained with the help of ultrasound, was added in the colloid. The mixture was magnetic stirred at 60°C until the water evaporates mostly. One thing to note here is that the TiO2 and PVDF is water insoluble, so we put them and CTAB together into the deionized water and then stirred and ultrasonic dispersed to obtain this aqueous suspension, at 60°C. Driven by Coulomb force, CTAB captured the anionic LVP colloid, which rearranged the charge density and formed composite micelles in the solution [27]. Finally, the green thick sol was dried at 80°C in vacuum oven and then heated at 400°C for 5 h and 700°C for 10 h under Argon flow to synthesize the final composites. |
Yield | Reaction Conditions | Operation in experiment |
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Stage #1: ammonium dihydrogen phosphate; vanadyl oxalate; lithium carbonate; titanium(IV) oxide With cetyltrimethylammonim bromide In water at 60℃; Sonication; Stage #2: at 400℃; for 5h; Inert atmosphere; Stage #3: at 700℃; for 10h; Inert atmosphere; | Synthesis of Li3V2-(4/3)xTix(PO4)3/C General procedure: 0.01 mol monoclinic Li3V2-(4/3)xTix (PO4)3/C were obtained using an ultrasound-assisted sol-gel method to mix stoichiometric amounts of V2O5, H2C2O4, Li2CO3, NH4H2PO4, TiO2 and CTAB. TiO2 is dopant and CTAB is cationic surfactant. Moreover, 1.0 g Polyvinylidene Fluoride (PVDF) was also added in as carbon source. First, V2O5 and H2C2O4 in a molar ratio of 1:3 were dissolved in deionized water under magnetic stirring at 60°C. After about half an hour a clear blue VOC2O4 solution formed (V2O5+3H2C2O4→2VOC2O4+2CO2+3H2O). Second, Li2CO3 and NH4H2PO4 were added in this solution in turn. Both processes were with gas generating and a hydrophilic homogeneous colloid was formed. Third, the aqueous suspension of Cetyltrimethyl Ammonium Bromide (CTAB, 1 mmol), TiO2 and PVDF (1.0 g), which was obtained with the help of ultrasound, was added in the colloid. The mixture was magnetic stirred at 60°C until the water evaporates mostly. One thing to note here is that the TiO2 and PVDF is water insoluble, so we put them and CTAB together into the deionized water and then stirred and ultrasonic dispersed to obtain this aqueous suspension, at 60°C. Driven by Coulomb force, CTAB captured the anionic LVP colloid, which rearranged the charge density and formed composite micelles in the solution [27]. Finally, the green thick sol was dried at 80°C in vacuum oven and then heated at 400°C for 5 h and 700°C for 10 h under Argon flow to synthesize the final composites. |
Yield | Reaction Conditions | Operation in experiment |
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Stage #1: chromium(III) oxide; ammonium dihydrogen phosphate; lithium carbonate In neat (no solvent, solid phase) at 299.84℃; for 11h; Stage #2: In neat (no solvent, solid phase) at 699.84℃; for 12h; | solid-state reaction LiCrP2O7 compound was prepared by conventional method based on solid-state reaction. Analytical grade reagents of Li2CO3,Cr2O3 and NH2H4PO4 were used as raw materials with appropriate mass according to the stoichiometric ratio and mixed in a mortar for 3 h. The powder mixture was progressively heated firstly to 573 K for 8 h to expel NH3, H2O and CO2 then the obtained sample was ground, pelletized and again heated at 973 K for 12 h. |
Yield | Reaction Conditions | Operation in experiment |
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In ethanol for 10h; Milling; Inert atmosphere; | The pure LiFePO4 was prepared by a solide state reaction method [14,15]. Stoichiometric FeC2O4*2H2O, NH4H2PO4, and Li2CO3 were scattered in ethanol and then ball milled for 10 h. After completely evaporating the ethanol, the precursor powder was heated at 350 C for 6 h and sintered at 700 C for 10 h under a nitrogen atmosphere. The pure LiFePO4 was collected after cooling to room temperature. | |
Stage #1: ammonium dihydrogen phosphate; iron(II) oxalate dihydrate; lithium carbonate In neat (no solvent, solid phase) for 10h; Inert atmosphere; Milling; Stage #2: In neat (no solvent, solid phase) at 350 - 650℃; for 26h; Calcination; Inert atmosphere; | General procedure: The LiFePO4 and Li0.99Zr0.0025Fe1-xCoxPO4 (x=0.005, 0.01, 0.015, 0.02) particles were synthesized using a conventional two-step heating solid-state reaction under argon atmosphere. The stoichiometric amount of Li2CO3 (A.R.), ZrO2 (A.R.), FeC2O4·2H2O (A.R.), CoC2O4·2H2O (A.R.), NH4H2PO4 (A.R.) were mixed in sufficient acetone media with polyethylene bottles for 10h. The weight ratio of agate ball to powders is 20:1, and a rotation speed is 400rpm. After ball milling, the slurry was dried in a vacuum drying oven at 60°C for 4h. Then the mixture was ground in an agate mortar. After this, the mixture was calcined in a tube furnace at 350°C for 6h under argon atmosphere and then cooled to room temperature. The calcined samples were remilled and dried in the same condition with the first milling. After remilling, the dried powders were calcined in a tube furnace at 650°C for 20h under argon atmosphere and then cooled to room temperature. | |
Stage #1: ammonium dihydrogen phosphate; iron(II) oxalate dihydrate; lithium carbonate In water at 20℃; for 7h; Stage #2: With zirconium(IV) oxide In water at 20℃; for 15h; Inert atmosphere; Milling; Stage #3: In water at 600℃; for 10h; Inert atmosphere; | 2. Experimental Pure LiFePO4 (LFP) and carbon-coated LiFePO4 (C-LFP) were synthesized by a modified mechanical activation method from the precursors (Li2CO3, FeC2O42H2O, and NH4H2PO4, 99% purity from Aldrich) in stoichiometric quantities. The orange peel precursor was immersed in 100mL of 7 % KOH solution at room temperature for 24 h and then dried at 80 °C for carbon coating on the surface LiFePO4, as shown in Fig. 1. The KOH was used as activating agent. Pure LiFePO4 was synthesized without orange peel powder. The precursors were firstly mixed with magnetic stirring in 60 wt% of triply distilled water at room temperature for 7 h followed by reduced pressure drying of the blend at 70 °C for 2 h using a rotary evaporator at 60 rpm to yield a solid powder. After the rotary evaporator, they had a high-energy ball milling in a hardened steel vial with zirconia balls at room temperature for 15 h under argon atmosphere. Finally, thermal treatment was performed on the pellets at 600 °C for 10 h under nitrogen atmosphere. |
Yield | Reaction Conditions | Operation in experiment |
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General procedure: KNLNTS ceramics with Fe2O3 doping (0-1.0 wt%) were fabricated by the solid state combustion method with glycine as the fuel. Reagent grade oxide, carbonate or nitrate powders of KHCO3 (%99.5), NaNO3 (%99.5), Li2CO3 (%99.5), Nb2O5 (%99.5), Ta2O5 (%99.5) and Sb2O3 (%99.5) were used as raw materials. The raw materials were mixed in stoichiometric ratio and ball milled in ethanol for 24 h. The suspensions were dried and then sieved to obtain fine powders. The powders were then mixed with glycine (C2H5NO2) ina ratio of 1:0.56 in an agate mortar and the mixed powders were calcined at 650 C for 2 h. The calcined powders were mixed with Fe2O3 (%99.5) at various compositions (0-1.0 wt%) and 3 wt% of polyvinyl alcohol (PVA) solution. Then, they were ball milled againfor 24 h. After that, the mixed solution was dried, then crushed and sieved. These powders were pressed into disks of 15 mm in diameter and 10 mm thick under a pressure of 80 MPa. Subsequently, the disks were sintered at 1130 C for 2 h. |
Yield | Reaction Conditions | Operation in experiment |
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Stage #1: nickel(II) oxide; manganese(III) oxide; lithium carbonate With air In neat (no solvent, solid phase) at 569.84℃; for 5h; Calcination; Stage #2: With air In neat (no solvent, solid phase) at 869.84℃; for 22h; | Experimental General procedure: Samples of nominal compositions of Li1.05Mn2O4-δ, Li1.05Mn1.5Ni0.5O4-δ, and Li1.05Mn1.0Ni0.5Ti0.5O4-δ were synthesized by a solid-state reaction technique using Li2CO3, Mn2O3, NiO, and TiO2 powders. A lithium-rich content should be prepared for the undertaking of effectively evaporating lithium oxide. The mixed powders were calcined in air at 843 K for 5 h, and then heated at 1143 K for 10 h. After grinding, the heated powders were pressed into pellets and finally sintered in air at 1143 K for 12 h. The cooling rate following the heating process was 100 K per hour. | |
Stage #1: nickel(II) oxide; manganese(III) oxide; lithium carbonate at 569.84℃; for 5h; Calcination; Stage #2: at 869.84℃; for 10h; Stage #3: at 869.84℃; for 12h; | 2. Experimental General procedure: Li1.05Mn2O4δ, Li1.05Mn2xNixO4δ (x 0.1, 0.2, 0.3, 0.4, 0.5), andLi1.05Mn2xTixO4δ (x 0.1, 0.2, 0.3) were prepared via a conventionalsolid-state reaction technique using Li2CO3, Mn2O3, NiO, and TiO2powders. A Li-rich solid was prepared to effectively evaporate Li2O. Themixed powders were pelletized and calcined in air at 843 K for 5 h andthen heated at 1143 K for 10 h. After the heated pellets were ground intopowders, they were pressed into pellets again and finally sintered in air at1143 K for 12 h. The contents of the samples after the second heattreatment were characterized using inductively coupled plasma withoptical emission spectroscopy (ICP-OES). The oxidation state of Mn wasdetermined by an iodometric titration method described in detail in Refs.[40,41]. | |
With air In neat (no solvent, solid phase) at 569.84 - 869.84℃; for 27h; Calcination; | General procedure: Li1.05Mn2O4δ, Ni-substituted samples Li1.05Mn2-xNixO4δ (x 0.1,0.2, 0.3, 0.4, and 0.5) and Ti-substituted samples Li1.05Mn2-xTixO4δ (x 0.1, 0.2, and 0.3) were synthesized by a conventional solid-state reactiontechnique from Li2CO3, Mn2O3, NiO, and TiO2 powders. A lithium-richcontent is prepared for effectively evaporating lithium oxide. Themixture was pelletized and calcined in air at 843 K for 5 h, and subsequentlyheated at 1143 K for 10 h. After the heated pellets were carefullyground into powders, the calcined powders were re-pelletized and sinteredin air at 1143 K for 12 h. The cooling rate following the heatingprocess was 100 K per hour. The lithium content was approximately 1.0after synthesis. The method of sample preparation is the same as that ofour previous work of Ref. [30]. An iodometric titration method wasemployed to characterize the oxidation state of Mn as described in ourprevious paper [30]. Ni substitution increased Mn oxidation state tonearly 4, whereas Ti substitution made Mn oxidation state less than 3.5. |
Yield | Reaction Conditions | Operation in experiment |
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General procedure: Li2MgTi3O8:Mn4+ samples were prepared by the Pechini-type solegel method, as follows. All the chemicals, namely, Li2CO3 (AR), Mn(CH3COO)2*4H2O (AR), Mg(CH3COO)2*4H2O (AR), TiO2 nanoparticles (99.999%, 28 nm) and citric acid were used as starting materials. A typical synthesis procedure for Li2MgTi3O8:0.5%Mn4+ phosphor is as follows: 0.953 g Li2CO3, 1.072 g Mn(CH3COO)2*4H2O, 0.018 g Mg(CH3COO)2*4H2O and 1.192 g TiO2 were weighed based on the chemical proportion, Li2MgTi3x(1-0.005)O8:0.005Mn4+, with the addition of 5 mol% excess of Li2CO3. Excess lithium was added to compensate for loss, which occurs at a high temperature. The molar ratio of citric acid to total metalions was 1:1. Li2CO3, Mn(CH3COO)2*4H2O, Mg(CH3COO)2*4H2O, and TiO2 were dissolved in deionized water under vigorous stirring. Simultaneously, a stoichiometric amounts of citric acid was added to the solution. At the end, the pH value of the mixed solution was adjusted to 7-8 by dropwise addition of NH3*H2O, and the transparent solution was heated to 100 C in a water bath to produce a brown transparent resin. The resin was further dried at 160 C in an oven for 10 h. Finally, the dried gel was annealed at different temperatures, namely, 600 C, 700 C, 800 C, 900 C and 1000 C. |
Yield | Reaction Conditions | Operation in experiment |
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46.4% | In water at 20℃; for 1461h; | Dimethylmalonic acid (0.365 g, 2.76 mmol) and Li2CO3 (0.204 g, 2.76 mmol) were dissolved in distilled water (15 mL) at 30-40 °C. Then VOSO4•3H2O (0.15 g, 0.69 mmol) in distilled water (10 mL) was added. After 20 min stirring, the resulting dark blue solution was left at room temperature. Slow evaporation of the solvent for two months gave blue crystals suitable for X-ray diffraction. The crystals were washed with cold (~3 °C) ethanol and dried in air. The yield of complex 1 was 0.109 g (46.4% based on the initial amount of VOSO4•3H2O). Found (%): C, 34.98; H, 3.76. C10H12Li2O9V. Calculated (%):C, 35.22; H, 3.55. IR, ν/cm-1: 2990.74 vw, 2940 vw, 2879.4 vw, 1583.27 vs, 1559.69 vs, 1459.06 w, 1411.06 vs, 1372.43 m, 1356.13 s, 1189.80 s, 1139.67 w, 1006.90 vs, 940.83 s, 789.73 w, 756.80 m, 613.16 s, 484.51 s, 467.51 s. |
Yield | Reaction Conditions | Operation in experiment |
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42.3% | at 20℃; for 2h; | Vanadyl sulfate trihydrate (0.15 g, 0.69 mmol), H2Me2mal (0.365 g, 2.76 mmol), and Li2CO3 (0.204 g, 2.76 mmol) were simultaneously added to ethanol (30 mL) and dissolved with stirring at 30-40 °C for 2 h. The reaction mixture was kept at room temperature for 2 h. The green solution was filtered to remove a white precipitate, concentrated in vacuo to a volume of 10-15 mL, and left at room temperature. The blue crystals that formed were separated from the mother liquor by decantation, washed with cold (~3 °C) ethanol, and dried in air. The yield of complex 2 was 0.06 g (42.3% based on the initial amount VOSO4•3H2O). Found (%):C, 35.43; H, 4.78. C12H20Li2O11V. Calculated (%): C, 35.58;H, 4.98. IR, ν/cm-1: 3648.2-3126.3 w. br, 2989.12 w, 2937.48 w, 2907.3 w, 2874.7 w, 1633.44 vs, 1585.18 vs, 1455.65 m, 1399.45 vs, 1368.58 s, 1350.56 vs, 1287.15 s, 1187.15 s, 1088.52 w, 1046.58 s, 1011.91 vs, 963.25 w, 932.67 s, 886.01 w, 789.54 s, 744.18 m, 724.13 s, 693.21 s, 605.72 s, 502.93 s. |
Yield | Reaction Conditions | Operation in experiment |
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82.5% | at 20℃; for 336h; | Butylmalonic acid (0.221 g, 1.38 mmol) and Li2CO3 (0.102 g, 1.38 mmol) were dissolved in distilled water (10 mL) at 30-40 °C. Then VOSO4•3H2O (0.15 g, 0.69 mmol) in distilled water (10 mL) was added. After 20 min stirring, the resulting blue solution was left at room temperature. Slow evaporation of the solvent for two weeks produced blue crystals suitable for Xray diffraction. The crystals were washed with cold (~3 °C) ethanol and dried in air. The yield of complex 4 was 0.283 g (82.5% based on the initial amount of VOSO4•3H2O). Found (%): C, 33.61; H, 6.28. C14H31Li2O14.5V. Calculated (%): C, 33.89; H, 6.30. IR, ν/cm-1: 3676.2-3042.5 w. br, 2959.78 vw, 2934.83 vw, 2873.47 vw, 1574.36 vs, 1406.82 s, 1334.63 m, 1318.66 m, 1293.5 w, 1198.14 w, 1101.72 w, 985.40 s, 956.83 w, 907.87 vw, 866.28 vw, 806.54 w, 727.75 s, 631.22 s, 601.38 s. |
Yield | Reaction Conditions | Operation in experiment |
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In neat (no solvent, solid phase); at 350 - 700℃; for 11h;Calcination; Inert atmosphere; | The LiFe0.9Mg0.1PO4 sample was synthesized by using a solid-state reaction method. The starting materials of Li2CO3 (99.99%), FeC2O4*2H2O (99%), (CH3COO)2Mg4H2O (99.999%), and NH4H2PO4(99.999%) were mixed with the correct stoichiometric ratio. The mixture was calcined at 350 C for 3 h under Ar atmosphere and pelletized at 5000 N/cm2. The sample was reheated at 700 C for 8 h under Ar atmosphere. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With manganese(II)carbonate In neat (no solvent) at 1150℃; for 0.583333h; | 2.1.2. Synthesis process The well-mixed raw chemicals were melted at 1150°C for 35 min in a covered alumina crucible at ambient atmosphere. Then,the glass melt was rapidly quenched on a 370°C pre-heated copperplate, and annealed at 650°C for 120 min. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
75% | Stage #1: bis(chlorosulfonyl)amine; lithium carbonate With fluorine resin In N,N-dimethyl-formamide at 25℃; Inert atmosphere; Green chemistry; Stage #2: ammonium fluoride In N,N-dimethyl-formamide at 25 - 80℃; Green chemistry; | 3; 5; 7 Example 5Preparation of lithium bis (fluorosulfonyl) imide powder (lithium carbonate (Li 2 CO 3)When the powder is used as a lithiation reagent) In a 500 ml reactor made of fluorocarbon resin equipped with a stirrer, a condenser and a thermometer, 18.0 g of anhydrous lithium carbonate powder in dimethylformamide,100 g of bis (chlorosulfonyl) imide and 100 g of bis (chlorosulfonyl) imide were gradually added at room temperature (25 DEG C)At 60 rpm with a magnetic stirrer to obtain a lithium bis (chlorosulfonyl) imide compound through a lithiation reaction.Immediately thereafter, lithium bis (trimethylsilyl) bis(Chlorosulfonyl) imide compound was stirred at 80 rpm to remove the generated gas, and then the anhydrous ammonium fluoride obtained in Example 1Was added at room temperature (25 ) to prepare a second reactant.Subsequently, the second reactant was stirred at 60 rpmThe reaction was carried out by raising the temperature to 80 ° C to prepare a lithium bis (fluorosulfonyl) imide compound.After completion of the reaction, the lithium bis (fluorosulfonyl) imide compound was allowed to react at room temperature (25 DEG C)And the resulting salt was filtered through a filter paper to obtain a colorless transparent lyeTris (fluorosulfonyl)Dimethyl carbonate solution of imide was obtained(170.0 g, yield: 81%, purity: 99.6%).Concentration was carried out using an evaporator. The obtained dimethyl carbonate solution was added to the crude product in an amount of 5 wt%Or less at 40 DEG C or less and at a pressure of 3 Torr or less for 4 hours under reduced pressure to obtain a white concentrate.1.5 times by weight of 1,2-dichloroethane was slowly added to the obtained concentrate at 80 DEG C or lower, and the mixture was gradually cooled to room temperature (25 DEG C).The resulting crystals were filtered with a filter paper to obtain lithium bis(Fluorosulfonyl) imide (64.9 g, yield: 75%, purity: 99.7%). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With gallium(III) oxide In water at 219.84℃; for 168h; Autoclave; | 2.1. Synthesis and crystallization Analytical grade chemicals were used for all syntheses.NH4(H2AsO4)(H3AsO4) was grown by hydrothermal methods(T = 493 K, 7 d, Teflon-lined stainless steel autoclave) from amixture of In2O3 and H3AsO40.5H2O in an approximatevolume ratio of 1:10 and 10 drops of NH4(OH) (32%). Noadditional H2O was added. The reaction product was a solidmass of colourless intergrown crystals with less than 10 vol%of a yellow unidentified material. The NH4(H2AsO4)-(H3AsO4) crystals are stable in air.Cs(H2AsO4)(H3AsO4)2 formed as the secondary productfrom further reaction of hydrothermally grown CsAs3O8(Schwendtner & Kolitsch, 2007a). CsAs3O8 contains AsO6groups, is highly hygroscopic and, at room temperature,decomposes to a highly acidic liquid in which rounded prismaticglassy colourless crystals of Cs(H2AsO4)(H3AsO4)2grew within a few weeks.Li2(H2PO4)2 was also a secondary product of a hydrothermalrun (T = 493 K, 7 d, Teflon-lined stainless steelautoclave) from a mixture of Li2CO3, Ga2O3, phosphoric acidand distilled water. The initial and final pH values were bothabout 1. The hydrothermal synthesis yielded globular crystal aggregates of rounded hexagonal prisms of GaPO4. From theremaining acidic liquid of the synthesis, Li2(H2PO4)2 grew ascolourless crude block-shaped crystals by slow evaporation atroom temperature. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
at 79.84℃; | General procedure: Both title compounds have been prepared using the samemethod. A mixture of A2CO3 (A = Li or Na) andCr(NO3)3*9H2O in equal stoichiometric amounts (0.2 mmol)was added to a solution of <strong>[6153-56-6]<strong>[6153-56-6]oxalic acid</strong> dehydrate</strong> in deionizedwater (0.05 M, 20 ml) and the resulting solution stirred forseveral hours under reflux at 353 K. Pink prismatic singlecrystals of LiCr(C2O4)2(H2O)4, (I), were grown by slowevaporation at 313 K over a period of approximately twoweeks. Suitable single crystals were selected for X-raydiffraction analysis after washing the preparation with diethylether. In the case of NaCr(C2O4)2(H2O)4, (II), the crystalgrowth is more complex, and the purple solution was kept at313 K for evaporation for two weeks. A smectic-like state ofthe preparation was obtained, dissolved in water and subjectedto a new evaporation. This step was repeated severaltimes; however, the addition of a small amount of methanol isrequired to favour the growth of crystals and led to purpleprismatic single crystals which were washed with diethyl etherfor further analysis. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Stage #1: nickel(II) oxide; manganese(III) oxide; lithium carbonate at 569.84℃; for 5h; Calcination; Stage #2: at 869.84℃; for 10h; Stage #3: at 869.84℃; for 12h; | 2. Experimental General procedure: Li1.05Mn2O4δ, Li1.05Mn2xNixO4δ (x 0.1, 0.2, 0.3, 0.4, 0.5), andLi1.05Mn2xTixO4δ (x 0.1, 0.2, 0.3) were prepared via a conventionalsolid-state reaction technique using Li2CO3, Mn2O3, NiO, and TiO2powders. A Li-rich solid was prepared to effectively evaporate Li2O. Themixed powders were pelletized and calcined in air at 843 K for 5 h andthen heated at 1143 K for 10 h. After the heated pellets were ground intopowders, they were pressed into pellets again and finally sintered in air at1143 K for 12 h. The contents of the samples after the second heattreatment were characterized using inductively coupled plasma withoptical emission spectroscopy (ICP-OES). The oxidation state of Mn wasdetermined by an iodometric titration method described in detail in Refs.[40,41]. | |
With air In neat (no solvent, solid phase) at 569.84 - 869.84℃; for 27h; Calcination; | General procedure: Li1.05Mn2O4δ, Ni-substituted samples Li1.05Mn2-xNixO4δ (x 0.1,0.2, 0.3, 0.4, and 0.5) and Ti-substituted samples Li1.05Mn2-xTixO4δ (x 0.1, 0.2, and 0.3) were synthesized by a conventional solid-state reactiontechnique from Li2CO3, Mn2O3, NiO, and TiO2 powders. A lithium-richcontent is prepared for effectively evaporating lithium oxide. Themixture was pelletized and calcined in air at 843 K for 5 h, and subsequentlyheated at 1143 K for 10 h. After the heated pellets were carefullyground into powders, the calcined powders were re-pelletized and sinteredin air at 1143 K for 12 h. The cooling rate following the heatingprocess was 100 K per hour. The lithium content was approximately 1.0after synthesis. The method of sample preparation is the same as that ofour previous work of Ref. [30]. An iodometric titration method wasemployed to characterize the oxidation state of Mn as described in ourprevious paper [30]. Ni substitution increased Mn oxidation state tonearly 4, whereas Ti substitution made Mn oxidation state less than 3.5. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Stage #1: nickel(II) oxide; manganese(III) oxide; lithium carbonate at 569.84℃; for 5h; Calcination; Stage #2: at 869.84℃; for 10h; Stage #3: at 869.84℃; for 12h; | 2. Experimental General procedure: Li1.05Mn2O4δ, Li1.05Mn2xNixO4δ (x 0.1, 0.2, 0.3, 0.4, 0.5), andLi1.05Mn2xTixO4δ (x 0.1, 0.2, 0.3) were prepared via a conventionalsolid-state reaction technique using Li2CO3, Mn2O3, NiO, and TiO2powders. A Li-rich solid was prepared to effectively evaporate Li2O. Themixed powders were pelletized and calcined in air at 843 K for 5 h andthen heated at 1143 K for 10 h. After the heated pellets were ground intopowders, they were pressed into pellets again and finally sintered in air at1143 K for 12 h. The contents of the samples after the second heattreatment were characterized using inductively coupled plasma withoptical emission spectroscopy (ICP-OES). The oxidation state of Mn wasdetermined by an iodometric titration method described in detail in Refs.[40,41]. | |
With air In neat (no solvent, solid phase) at 569.84 - 869.84℃; for 27h; Calcination; | General procedure: Li1.05Mn2O4δ, Ni-substituted samples Li1.05Mn2-xNixO4δ (x 0.1,0.2, 0.3, 0.4, and 0.5) and Ti-substituted samples Li1.05Mn2-xTixO4δ (x 0.1, 0.2, and 0.3) were synthesized by a conventional solid-state reactiontechnique from Li2CO3, Mn2O3, NiO, and TiO2 powders. A lithium-richcontent is prepared for effectively evaporating lithium oxide. Themixture was pelletized and calcined in air at 843 K for 5 h, and subsequentlyheated at 1143 K for 10 h. After the heated pellets were carefullyground into powders, the calcined powders were re-pelletized and sinteredin air at 1143 K for 12 h. The cooling rate following the heatingprocess was 100 K per hour. The lithium content was approximately 1.0after synthesis. The method of sample preparation is the same as that ofour previous work of Ref. [30]. An iodometric titration method wasemployed to characterize the oxidation state of Mn as described in ourprevious paper [30]. Ni substitution increased Mn oxidation state tonearly 4, whereas Ti substitution made Mn oxidation state less than 3.5. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Stage #1: nickel(II) oxide; manganese(III) oxide; lithium carbonate at 569.84℃; for 5h; Calcination; Stage #2: at 869.84℃; for 10h; Stage #3: at 869.84℃; for 12h; | 2. Experimental General procedure: Li1.05Mn2O4δ, Li1.05Mn2xNixO4δ (x 0.1, 0.2, 0.3, 0.4, 0.5), andLi1.05Mn2xTixO4δ (x 0.1, 0.2, 0.3) were prepared via a conventionalsolid-state reaction technique using Li2CO3, Mn2O3, NiO, and TiO2powders. A Li-rich solid was prepared to effectively evaporate Li2O. Themixed powders were pelletized and calcined in air at 843 K for 5 h andthen heated at 1143 K for 10 h. After the heated pellets were ground intopowders, they were pressed into pellets again and finally sintered in air at1143 K for 12 h. The contents of the samples after the second heattreatment were characterized using inductively coupled plasma withoptical emission spectroscopy (ICP-OES). The oxidation state of Mn wasdetermined by an iodometric titration method described in detail in Refs.[40,41]. | |
With air In neat (no solvent, solid phase) at 569.84 - 869.84℃; for 27h; Calcination; | General procedure: Li1.05Mn2O4δ, Ni-substituted samples Li1.05Mn2-xNixO4δ (x 0.1,0.2, 0.3, 0.4, and 0.5) and Ti-substituted samples Li1.05Mn2-xTixO4δ (x 0.1, 0.2, and 0.3) were synthesized by a conventional solid-state reactiontechnique from Li2CO3, Mn2O3, NiO, and TiO2 powders. A lithium-richcontent is prepared for effectively evaporating lithium oxide. Themixture was pelletized and calcined in air at 843 K for 5 h, and subsequentlyheated at 1143 K for 10 h. After the heated pellets were carefullyground into powders, the calcined powders were re-pelletized and sinteredin air at 1143 K for 12 h. The cooling rate following the heatingprocess was 100 K per hour. The lithium content was approximately 1.0after synthesis. The method of sample preparation is the same as that ofour previous work of Ref. [30]. An iodometric titration method wasemployed to characterize the oxidation state of Mn as described in ourprevious paper [30]. Ni substitution increased Mn oxidation state tonearly 4, whereas Ti substitution made Mn oxidation state less than 3.5. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Stage #1: nickel(II) oxide; manganese(III) oxide; lithium carbonate at 569.84℃; for 5h; Calcination; Stage #2: at 869.84℃; for 10h; Stage #3: at 869.84℃; for 12h; | 2. Experimental General procedure: Li1.05Mn2O4δ, Li1.05Mn2xNixO4δ (x 0.1, 0.2, 0.3, 0.4, 0.5), andLi1.05Mn2xTixO4δ (x 0.1, 0.2, 0.3) were prepared via a conventionalsolid-state reaction technique using Li2CO3, Mn2O3, NiO, and TiO2powders. A Li-rich solid was prepared to effectively evaporate Li2O. Themixed powders were pelletized and calcined in air at 843 K for 5 h andthen heated at 1143 K for 10 h. After the heated pellets were ground intopowders, they were pressed into pellets again and finally sintered in air at1143 K for 12 h. The contents of the samples after the second heattreatment were characterized using inductively coupled plasma withoptical emission spectroscopy (ICP-OES). The oxidation state of Mn wasdetermined by an iodometric titration method described in detail in Refs.[40,41]. | |
With air In neat (no solvent, solid phase) at 569.84 - 869.84℃; for 27h; Calcination; | General procedure: Li1.05Mn2O4δ, Ni-substituted samples Li1.05Mn2-xNixO4δ (x 0.1,0.2, 0.3, 0.4, and 0.5) and Ti-substituted samples Li1.05Mn2-xTixO4δ (x 0.1, 0.2, and 0.3) were synthesized by a conventional solid-state reactiontechnique from Li2CO3, Mn2O3, NiO, and TiO2 powders. A lithium-richcontent is prepared for effectively evaporating lithium oxide. Themixture was pelletized and calcined in air at 843 K for 5 h, and subsequentlyheated at 1143 K for 10 h. After the heated pellets were carefullyground into powders, the calcined powders were re-pelletized and sinteredin air at 1143 K for 12 h. The cooling rate following the heatingprocess was 100 K per hour. The lithium content was approximately 1.0after synthesis. The method of sample preparation is the same as that ofour previous work of Ref. [30]. An iodometric titration method wasemployed to characterize the oxidation state of Mn as described in ourprevious paper [30]. Ni substitution increased Mn oxidation state tonearly 4, whereas Ti substitution made Mn oxidation state less than 3.5. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Stage #1: nickel(II) oxide; iron(III) oxide; lithium carbonate In neat (no solvent, solid phase) at 750 - 800℃; for 8h; Stage #2: With polyvinyl alcohol In neat (no solvent, solid phase) at 950℃; for 2h; | Compound Li0.3Ni0.4Fe2.3O4 (LNFO) was synthesised using the Solid-State reaction method. High purity Li2CO3(99.0%, HIMEDIA), NiO (99.0%, Alfa Aesar) and Fe2O3(98.0%, HIMEDIA) were taken as precursors. All these precursors were weighed and mixed in the appropriate stoichiometric ratio. The mixed powder was grounded for 3h in acetone medium. The grounded powder was pre-sintered at 750 and 800°C for 8h and obtained powder samples were termed as LNFO-1 and LNFO-2, respectively. The pre-sintered powders were grounded for 15min to get the homogeneous powder. These obtained homogeneous powders were pelletised into square pellets of dimensions 2cm×2cm using Polyvinyl alcohol (PVA) as binder. These obtained pellets were then sintered at 950°C for 2h. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
at 65℃; for 12h;Inert atmosphere; Glovebox; | All chemicals were purchased from Jinniu Power Sources Co., Ltd. (Tianjin,China). LiPO2F2is prepared via the reaction of the LiPF6 with the Li2CO3 in dimethylcarbonate (DMC) solvent (Reaction 1). Firstly, 0.5 mol LiPF6was dissolved into 100mL DMC (LiPF6/DMC = 20.0 wt%) in a 250 mL Teflon reaction vessel at 0 insidea nitrogen-filled glove box. Next, a certain amount of Li2CO3 was slowly added intothe solution with continuous stirring. The reaction vessel was heated to differenttemperatures (25, 45, 65 ) for 12 h. It should be noted that there are bubblesgenerated during the reaction process.LiPF6 + 2Li2CO3 LiPO2F2 + 4LiF (s) + 2CO2 (g)Reaction 1After the reaction, the salt solution was collected via vacuum filtration to removethe insoluble LiF. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
General procedure: At the beginning, the stoichiometricamounts of Mg(CH3COO)2*4H2O, Ba(NO3)2, WO2, Eu2O3, and Li2CO3 were weighed and transferred into the milling cup. Lithium ions were applied as a charge compensator agent. Due to the probability of the sublimation of magnesium ions, extra 10% of Mg(CH3COO)2*4H2O was applied. The powders were ground using a planetary ball milling in anhydrous ethanol with 3 mm Si3N4 balls. To optimize the synthesis condition, a large number of factors were verified, e.g. milling speed and annealing temperature. The prepared powder was dried for 24 h in a laboratory dryer and preannealed at 600 C for 6 h in a muffle oven. The final annealing was conducted at various temperature values from 900 to 1300 C in the air atmosphere. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
General procedure: At the beginning, the stoichiometricamounts of Mg(CH3COO)2*4H2O, Ba(NO3)2, WO2, Eu2O3, and Li2CO3 were weighed and transferred into the milling cup. Lithium ions were applied as a charge compensator agent. Due to the probability of the sublimation of magnesium ions, extra 10% of Mg(CH3COO)2*4H2O was applied. The powders were ground using a planetary ball milling in anhydrous ethanol with 3 mm Si3N4 balls. To optimize the synthesis condition, a large number of factors were verified, e.g. milling speed and annealing temperature. The prepared powder was dried for 24 h in a laboratory dryer and preannealed at 600 C for 6 h in a muffle oven. The final annealing was conducted at various temperature values from 900 to 1300 C in the air atmosphere. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
General procedure: At the beginning, the stoichiometricamounts of Mg(CH3COO)2*4H2O, Ba(NO3)2, WO2, Eu2O3, and Li2CO3 were weighed and transferred into the milling cup. Lithium ions were applied as a charge compensator agent. Due to the probability of the sublimation of magnesium ions, extra 10% of Mg(CH3COO)2*4H2O was applied. The powders were ground using a planetary ball milling in anhydrous ethanol with 3 mm Si3N4 balls. To optimize the synthesis condition, a large number of factors were verified, e.g. milling speed and annealing temperature. The prepared powder was dried for 24 h in a laboratory dryer and preannealed at 600 C for 6 h in a muffle oven. The final annealing was conducted at various temperature values from 900 to 1300 C in the air atmosphere. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
General procedure: At the beginning, the stoichiometricamounts of Mg(CH3COO)2*4H2O, Ba(NO3)2, WO2, Eu2O3, and Li2CO3 were weighed and transferred into the milling cup. Lithium ions were applied as a charge compensator agent. Due to the probability of the sublimation of magnesium ions, extra 10% of Mg(CH3COO)2*4H2O was applied. The powders were ground using a planetary ball milling in anhydrous ethanol with 3 mm Si3N4 balls. To optimize the synthesis condition, a large number of factors were verified, e.g. milling speed and annealing temperature. The prepared powder was dried for 24 h in a laboratory dryer and preannealed at 600 C for 6 h in a muffle oven. The final annealing was conducted at various temperature values from 900 to 1300 C in the air atmosphere. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
General procedure: At the beginning, the stoichiometricamounts of Mg(CH3COO)2*4H2O, Ba(NO3)2, WO2, Eu2O3, and Li2CO3 were weighed and transferred into the milling cup. Lithium ions were applied as a charge compensator agent. Due to the probability of the sublimation of magnesium ions, extra 10% of Mg(CH3COO)2*4H2O was applied. The powders were ground using a planetary ball milling in anhydrous ethanol with 3 mm Si3N4 balls. To optimize the synthesis condition, a large number of factors were verified, e.g. milling speed and annealing temperature. The prepared powder was dried for 24 h in a laboratory dryer and preannealed at 600 C for 6 h in a muffle oven. The final annealing was conducted at various temperature values from 900 to 1300 C in the air atmosphere. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
General procedure: At the beginning, the stoichiometricamounts of Mg(CH3COO)2*4H2O, Ba(NO3)2, WO2, Eu2O3, and Li2CO3 were weighed and transferred into the milling cup. Lithium ions were applied as a charge compensator agent. Due to the probability of the sublimation of magnesium ions, extra 10% of Mg(CH3COO)2*4H2O was applied. The powders were ground using a planetary ball milling in anhydrous ethanol with 3 mm Si3N4 balls. To optimize the synthesis condition, a large number of factors were verified, e.g. milling speed and annealing temperature. The prepared powder was dried for 24 h in a laboratory dryer and preannealed at 600 C for 6 h in a muffle oven. The final annealing was conducted at various temperature values from 900 to 1300 C in the air atmosphere. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
General procedure: At the beginning, the stoichiometricamounts of Mg(CH3COO)2*4H2O, Ba(NO3)2, WO2, Eu2O3, and Li2CO3 were weighed and transferred into the milling cup. Lithium ions were applied as a charge compensator agent. Due to the probability of the sublimation of magnesium ions, extra 10% of Mg(CH3COO)2*4H2O was applied. The powders were ground using a planetary ball milling in anhydrous ethanol with 3 mm Si3N4 balls. To optimize the synthesis condition, a large number of factors were verified, e.g. milling speed and annealing temperature. The prepared powder was dried for 24 h in a laboratory dryer and preannealed at 600 C for 6 h in a muffle oven. The final annealing was conducted at various temperature values from 900 to 1300 C in the air atmosphere. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Stage #1: iron(III) oxide; lithium carbonate With oxygen In neat (no solvent, solid phase) Calcination; Stage #2: With oxygen In neat (no solvent, solid phase) at 700℃; for 24h; Sealed tube; | General procedure: Polycrystalline samples of LixFe5O8-y (x=0.91 and 1.02) were prepared by a conventional solid-state reaction technique. The excess Li (8% and 15% molar excess for x=0.91 and 1.02, respectively) was used for the synthesis to compensate the loss of highly volatile lithium which is expected to occur during the calcinations and sintering of powders at high temperature. Appropriate quantities of the starting compounds, Fe2O3 (Alfa Aesar Inc.) and Li2CO3 (LTS research labs Inc.) of 99.99% purity, were initially mixed thoroughly in an agate mortar and calcined in a tube furnace (under oxygen flow) using alumina crucibles. The mixed powders were kept in quartz tubes and evacuated up to 10-5Torr. The quartz tubes were sealed under O2 gas (P=5×10-1 Torr) and were subsequently kept in furnace and annealed at 700°C for 24h. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Stage #1: iron(III) oxide; lithium carbonate With oxygen In neat (no solvent, solid phase) Calcination; Stage #2: With oxygen In neat (no solvent, solid phase) at 700℃; for 24h; Sealed tube; | General procedure: Polycrystalline samples of LixFe5O8-y (x=0.91 and 1.02) were prepared by a conventional solid-state reaction technique. The excess Li (8% and 15% molar excess for x=0.91 and 1.02, respectively) was used for the synthesis to compensate the loss of highly volatile lithium which is expected to occur during the calcinations and sintering of powders at high temperature. Appropriate quantities of the starting compounds, Fe2O3 (Alfa Aesar Inc.) and Li2CO3 (LTS research labs Inc.) of 99.99% purity, were initially mixed thoroughly in an agate mortar and calcined in a tube furnace (under oxygen flow) using alumina crucibles. The mixed powders were kept in quartz tubes and evacuated up to 10-5Torr. The quartz tubes were sealed under O2 gas (P=5×10-1 Torr) and were subsequently kept in furnace and annealed at 700°C for 24h. |
Tags: 554-13-2 synthesis path| 554-13-2 SDS| 554-13-2 COA| 554-13-2 purity| 554-13-2 application| 554-13-2 NMR| 554-13-2 COA| 554-13-2 structure
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P372 | Explosion risk in case of fire. |
P373 | DO NOT fight fire when fire reaches explosives. |
P374 | Fight fire with normal precautions from a reasonable distance. |
P376 | Stop leak if safe to do so. Oxidising gases (section 2.4) 1 |
P377 | Leaking gas fire: Do not extinguish, unless leak can be stopped safely. |
P378 | |
P380 | Evacuate area. |
P381 | Eliminate all ignition sources if safe to do so. |
P390 | Absorb spillage to prevent material damage. |
P391 | Collect spillage. Hazardous to the aquatic environment |
P301 + P310 | IF SWALLOWED: Immediately call a POISON CENTER or doctor/physician. |
P301 + P312 | IF SWALLOWED: call a POISON CENTER or doctor/physician IF you feel unwell. |
P301 + P330 + P331 | IF SWALLOWED: Rinse mouth. Do NOT induce vomiting. |
P302 + P334 | IF ON SKIN: Immerse in cool water/wrap in wet bandages. |
P302 + P350 | IF ON SKIN: Gently wash with plenty of soap and water. |
P303 + P361 + P353 | IF ON SKIN (or hair): Remove/Take off Immediately all contaminated clothing. Rinse SKIN with water/shower. |
P304 + P312 | IF INHALED: Call a POISON CENTER or doctor/physician if you feel unwell. |
P304 + P340 | IF INHALED: Remove victim to fresh air and Keep at rest in a position comfortable for breathing. |
P304 + P341 | IF INHALED: If breathing is difficult, remove victim to fresh air and keep at rest in a position comfortable for breathing. |
P305 + P351 + P338 | IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. Continue rinsing. |
P306 + P360 | IF ON CLOTHING: Rinse Immediately contaminated CLOTHING and SKIN with plenty of water before removing clothes. |
P307 + P311 | IF exposed: call a POISON CENTER or doctor/physician. |
P308 + P313 | IF exposed or concerned: Get medical advice/attention. |
P309 + P311 | IF exposed or if you feel unwell: call a POISON CENTER or doctor/physician. |
P332 + P313 | IF SKIN irritation occurs: Get medical advice/attention. |
P333 + P313 | IF SKIN irritation or rash occurs: Get medical advice/attention. |
P335 + P334 | Brush off loose particles from skin. Immerse in cool water/wrap in wet bandages. |
P337 + P313 | IF eye irritation persists: Get medical advice/attention. |
P342 + P311 | IF experiencing respiratory symptoms: call a POISON CENTER or doctor/physician. |
P370 + P376 | In case of fire: Stop leak if safe to Do so. |
P370 + P378 | In case of fire: |
P370 + P380 | In case of fire: Evacuate area. |
P370 + P380 + P375 | In case of fire: Evacuate area. Fight fire remotely due to the risk of explosion. |
P371 + P380 + P375 | In case of major fire and large quantities: Evacuate area. Fight fire remotely due to the risk of explosion. |
Storage | |
Code | Phrase |
P401 | |
P402 | Store in a dry place. |
P403 | Store in a well-ventilated place. |
P404 | Store in a closed container. |
P405 | Store locked up. |
P406 | Store in corrosive resistant/ container with a resistant inner liner. |
P407 | Maintain air gap between stacks/pallets. |
P410 | Protect from sunlight. |
P411 | |
P412 | Do not expose to temperatures exceeding 50 oC/ 122 oF. |
P413 | |
P420 | Store away from other materials. |
P422 | |
P402 + P404 | Store in a dry place. Store in a closed container. |
P403 + P233 | Store in a well-ventilated place. Keep container tightly closed. |
P403 + P235 | Store in a well-ventilated place. Keep cool. |
P410 + P403 | Protect from sunlight. Store in a well-ventilated place. |
P410 + P412 | Protect from sunlight. Do not expose to temperatures exceeding 50 oC/122oF. |
P411 + P235 | Keep cool. |
Disposal | |
Code | Phrase |
P501 | Dispose of contents/container to ... |
P502 | Refer to manufacturer/supplier for information on recovery/recycling |
Physical hazards | |
Code | Phrase |
H200 | Unstable explosive |
H201 | Explosive; mass explosion hazard |
H202 | Explosive; severe projection hazard |
H203 | Explosive; fire, blast or projection hazard |
H204 | Fire or projection hazard |
H205 | May mass explode in fire |
H220 | Extremely flammable gas |
H221 | Flammable gas |
H222 | Extremely flammable aerosol |
H223 | Flammable aerosol |
H224 | Extremely flammable liquid and vapour |
H225 | Highly flammable liquid and vapour |
H226 | Flammable liquid and vapour |
H227 | Combustible liquid |
H228 | Flammable solid |
H229 | Pressurized container: may burst if heated |
H230 | May react explosively even in the absence of air |
H231 | May react explosively even in the absence of air at elevated pressure and/or temperature |
H240 | Heating may cause an explosion |
H241 | Heating may cause a fire or explosion |
H242 | Heating may cause a fire |
H250 | Catches fire spontaneously if exposed to air |
H251 | Self-heating; may catch fire |
H252 | Self-heating in large quantities; may catch fire |
H260 | In contact with water releases flammable gases which may ignite spontaneously |
H261 | In contact with water releases flammable gas |
H270 | May cause or intensify fire; oxidizer |
H271 | May cause fire or explosion; strong oxidizer |
H272 | May intensify fire; oxidizer |
H280 | Contains gas under pressure; may explode if heated |
H281 | Contains refrigerated gas; may cause cryogenic burns or injury |
H290 | May be corrosive to metals |
Health hazards | |
Code | Phrase |
H300 | Fatal if swallowed |
H301 | Toxic if swallowed |
H302 | Harmful if swallowed |
H303 | May be harmful if swallowed |
H304 | May be fatal if swallowed and enters airways |
H305 | May be harmful if swallowed and enters airways |
H310 | Fatal in contact with skin |
H311 | Toxic in contact with skin |
H312 | Harmful in contact with skin |
H313 | May be harmful in contact with skin |
H314 | Causes severe skin burns and eye damage |
H315 | Causes skin irritation |
H316 | Causes mild skin irritation |
H317 | May cause an allergic skin reaction |
H318 | Causes serious eye damage |
H319 | Causes serious eye irritation |
H320 | Causes eye irritation |
H330 | Fatal if inhaled |
H331 | Toxic if inhaled |
H332 | Harmful if inhaled |
H333 | May be harmful if inhaled |
H334 | May cause allergy or asthma symptoms or breathing difficulties if inhaled |
H335 | May cause respiratory irritation |
H336 | May cause drowsiness or dizziness |
H340 | May cause genetic defects |
H341 | Suspected of causing genetic defects |
H350 | May cause cancer |
H351 | Suspected of causing cancer |
H360 | May damage fertility or the unborn child |
H361 | Suspected of damaging fertility or the unborn child |
H361d | Suspected of damaging the unborn child |
H362 | May cause harm to breast-fed children |
H370 | Causes damage to organs |
H371 | May cause damage to organs |
H372 | Causes damage to organs through prolonged or repeated exposure |
H373 | May cause damage to organs through prolonged or repeated exposure |
Environmental hazards | |
Code | Phrase |
H400 | Very toxic to aquatic life |
H401 | Toxic to aquatic life |
H402 | Harmful to aquatic life |
H410 | Very toxic to aquatic life with long-lasting effects |
H411 | Toxic to aquatic life with long-lasting effects |
H412 | Harmful to aquatic life with long-lasting effects |
H413 | May cause long-lasting harmful effects to aquatic life |
H420 | Harms public health and the environment by destroying ozone in the upper atmosphere |
Sorry,this product has been discontinued.
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