CN102627266A - Vanadium titanium lithium phosphate material for positive electrode of lithium ion battery - Google Patents

Vanadium titanium lithium phosphate material for positive electrode of lithium ion battery Download PDF

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CN102627266A
CN102627266A CN2012101181594A CN201210118159A CN102627266A CN 102627266 A CN102627266 A CN 102627266A CN 2012101181594 A CN2012101181594 A CN 2012101181594A CN 201210118159 A CN201210118159 A CN 201210118159A CN 102627266 A CN102627266 A CN 102627266A
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lithium
source
titanium
vanadium
ion battery
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王联
李湘
薛雯娟
杨锦
李�权
姜爱民
蒋显全
李雷霆
皮晓青
潘复生
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Chongqing Academy of Science and Technology
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a vanadium titanium lithium phosphate material for a positive electrode of a lithium ion battery. The chemical formula of the material is Li3V2-xTix(PO4)3, wherein x=0.1-0.5. The preparation method of the material comprises the steps of weighing a lithium source, a vanadium source, a titanium source and a phosphorus source, fully mixing the sources and adding a coordination agent, wherein the mass ratio of the lithium source to the vanadium source to the titanium source to phosphorus source to the coordination agent is 3.9:1.90-1.50:0.1-0.50:3.0:0.5-2.0, and deionized water is added and controlled in the stirring process till mixed materials gradually become light blue slurry; standing slurry liquid for 10-30 minutes, using ammonia water to adjust potential of hydrogen (pH) to be neutral, placing the slurry liquid into a vacuum drying chamber to be dried for 2-6 hours at the temperature of 70-90 DEG C; fetching out the materials, grinding the materials, placing the materials in a drying oven to be roasted for 2-5 hours at the temperature of 200-270 DEG C, then placing the materials in an inert atmosphere protecting furnace to be sintered at the sintering temperature of 600-670 DEG C for 100-240 minutes and naturally cooling the materials to be at the room temperature to obtain vanadium titanium lithium phosphate. The vanadium titanium lithium phosphate material for the positive electrode of the lithium ion battery has better electro-chemical performance than lithium vanadium phosphate, the preparation process is simple, the cost is low, the selectivity of synthetic reaction is high, and the stability of the batched electro-chemical performance is good.

Description

A kind of ion battery anode material vanadium lithium phosphate titanium lithium
Technical field
The invention belongs to a kind of positive electrode material of lithium ion battery, particularly a kind of novel ion battery anode material vanadium lithium phosphate titanium lithium.
Background technology
(its chemical formula is Li to the cathode material lithium vanadium phosphate of lithium ion battery that generally uses at present 3V 2(PO 4) 3, as follows) and have unique mesh architecture and removal lithium embedded ionic performance, its theoretical specific capacity, discharge platform, voltage, intrinsic conductivity and specific energy all are higher than LiFePO 4, thereby it has huge development prospect.Though Li 3V 2(PO 4) 3Have many advantages, but its unique reticulated structure makes electronic conductivity on the low side.The approach that improves its performance is to adopt carbon to coat particularly original position carbon coating technology, but this method is prone to cause the material tap density to reduce, and the processing that increases material is like (mixing and coating) difficulty.Industrial normal employing solid-phase sintering prepares phosphoric acid vanadium lithium at present.This method is difficult for accurately control stoichiometry; Select very sensitive to raw material and operational path; To the requirement of process control also very high and since raw materials mix even inadequately; Therefore must be synthetic at down long-time (>=6 hours) sintering of high temperature (>=850 ℃), this just very easily causes material granule to grow excessive and generation impurity mutually, causes the consistence difficult problem of material produce.And the liquid phase synthesizing method that adopt in the laboratory is very high to equipment requirements when large-scale production, and inferior vanadium ion is prone to oxidized and makes the pollution problem that batches of materials stability is wayward and produce waste gas and waste water, and above reason has caused current Li 3V 2(PO 4) 3Still rest on test manufacture or short run stage.
Summary of the invention
In order to solve the problems of the technologies described above, to the object of the present invention is to provide a kind of passing through to mix or replace, thereby make titanium partly replace the new type lithium ion battery positive pole material phosphoric acid vanadium titanium lithium of the vanadium ion raising chemical property in the phosphoric acid vanadium lithium.
The present invention seeks to realize like this: a kind of ion battery anode material vanadium lithium phosphate titanium lithium, its chemical formula is Li 3V 2-xTi x(PO 4) 3, x=0.1-0.5 wherein; This preparation methods is:
(1) takes by weighing lithium source, vanadium source, titanium source and phosphorus source thorough mixing and grind back adding coordination agent; Wherein the amount of substance ratio of lithium source, vanadium source, titanium source, phosphorus source, coordination agent is 3.0: 1.90-1.50: 0.1-0.50: 3.0: 0.5-2.0, stir control simultaneously and add deionized water till mixture gradually becomes light blue mud;
(2) with this mud liquid leave standstill move into after using the ammoniacal liquor adjust pH as neutrality after 10-30 minute in the vacuum drying oven 70-90 ℃ dry 2-6 hour down;
(3) material in the step (2) is taken out; Putting into baking oven after the grinding toasted 2-5 hour down at 200-270 ℃; Insert then and carry out sintering in the inert atmosphere protection stove, sintering temperature 600-670 ℃, naturally cool to room temperature after sintering 100-240 minute and obtain phosphoric acid vanadium titanium lithium.
In technique scheme, mix the titanium source in the preparation process of phosphoric acid vanadium lithium, behind the raw materials mix sintering, make the titanium ion that mixes replace the part vanadium ion, synthesize phosphoric acid vanadium titanium lithium.Titanium ion can cause the material unit cell volume to increase after getting into material lattice, produces fractional distortion, but suitable distortion induced material activate quickly, thereby can improve its chemical property.
Preparing method of the present invention carries out the technological improvement of raw materials mix in the process of preparation presoma to using solid-phase coordination, adopts wet method coordination technology so that form crystal water in the raw mix.Crystal water plays an important role in reaction process: be chemical action on the one hand, the evaporable crystal water forms liquid bridge, the carrying out of impelling reaction at the interface; Be physical action on the other hand, crystal water overflows system during reaction, in lattice, produces defective, impels solid state reaction to carry out.Final effect can obtain more mixed uniformly presoma exactly.Reduce the activation energy of sintering building-up reactions; This preparation method process is simple, and is with low cost, and the selectivity of building-up reactions is high, batch stable electrochemical property property good.
In technique scheme, preferred said x=0.2-0.4.
In technique scheme: said lithium source is one or more the mixture in lithium oxalate, Lithium Acetate, lithium nitrate, Quilonum Retard, the Lithium Hydroxide MonoHydrate.
In technique scheme: said vanadium source is one or more the mixture in vanadium dioxide, Vanadium Pentoxide in FLAKES, the ammonium meta-vanadate.
In technique scheme: said titanium source is one or more the mixture in titanium oxide, titanium hydroxide, the butyl(tetra)titanate.
In technique scheme: said coordination agent is one or more the mixture in Hydrocerol A, oxalic acid, tartrate, the oxysuccinic acid.
In technique scheme: said phosphorus source is one or more the mixture in ammonium phosphate, primary ammonium phosphate, Secondary ammonium phosphate, Trilithium phosphate, the phosphoric acid.
Beneficial effect: ion battery anode material vanadium lithium phosphate titanium lithium of the present invention has better chemical property than phosphoric acid vanadium lithium, and the preparation process is simple, and is with low cost, and the selectivity of building-up reactions is high, batch stable electrochemical property property good.
Figure of description
Fig. 1 embodiment of the invention 3, embodiment 1 and embodiment 2 synthetic phosphoric acid vanadium titanium lithium Li 3V 1.8Ti 0.2(PO 4) 3, Li 3V 1.7Ti 0.3(PO 4) 3, Li 3V 1.6Ti 0.4(PO 4) 3X-ray diffraction (XRD) test pattern of the phosphoric acid vanadium lithium of the powder particle and (embodiment of the invention 6) preparation that uses the same method.
Fig. 2 is the Li of the embodiment of the invention 1 preparation 3V 1.7Ti 0.3(PO 4) 3The exterior appearance of material granule, its median size are about 0.5 μ m (magnification is 6000);
Fig. 3 is the charge-discharge performance test pattern (between the 3.30-4.80V electrochemical window, test with the 100mA/g current density, X-coordinate is represented specific storage, and ordinate zou is the relative current potential of lithium) with the phosphoric acid vanadium lithium of the embodiment of the invention 6 preparations;
Fig. 4 is the Li of the embodiment of the invention 1 preparation 3V 1.7Ti 0.3(PO 4) 3Charge-discharge performance test pattern (between the 3.30-4.80V electrochemical window, test with the 100mA/g current density, X-coordinate is represented specific storage, and ordinate zou is the relative current potential of lithium);
Fig. 5 is Li 3V 1.8Ti 0.2(PO 4) 3, Li 3V 1.7Ti 0.3(PO 4) 3, Li 3V 1.6Ti 0.4(PO 4) 3Carry out the figure as a result of discharge test at the electrochemical window of 3.30-4.80V with the current density of 100mA/g, X-coordinate is represented specific storage, and ordinate zou is the relative current potential of lithium;
Fig. 6 is Li 3V 1.8Ti 0.2(PO 4) 3, Li 3V 1.7Ti 0.3(PO 4) 3, Li 3V 1.6Ti 0.4(PO 4) 3Li with embodiment 6 preparations 3V 2(PO 4) 3Carry out the figure as a result of cycle charge discharge electrical testing at the electrochemical window of 3.30-4.80V with the constant current density of 100mA/g, X-coordinate representes that circulation please charge and discharge number of times, and ordinate zou is a specific storage;
Fig. 7 is the Li of embodiment 6 preparations 3V 2(PO 4) 3Between the 3.00-4.30V electrochemical window, carry out the figure as a result (X-coordinate is represented the relative current potential of lithium, and ordinate zou is an electrode reaction current) that cyclic voltammetric is tested with the scanning speed of 0.2mV/s;
Fig. 8 is Li 3V 1.8Ti 0.2(PO 4) 3Between the 3.00-4.30V electrochemical window, carry out the figure as a result (X-coordinate is represented the relative current potential of lithium, and ordinate zou is an electrode reaction current) that cyclic voltammetric is tested with the scanning speed of 0.2mV/s;
Fig. 9 is Li 3V 1.7Ti 0.3(PO 4) 3Between the 3.00-4.30V electrochemical window, carry out the figure as a result (X-coordinate is represented the relative current potential of lithium, and ordinate zou is an electrode reaction current) that cyclic voltammetric is tested with the scanning speed of 0.2mV/s;
Figure 10 is Li 3V 1.6Ti 0.4(PO 4) 3Between the 3.00-4.30V electrochemical window, carry out the figure as a result (X-coordinate is represented the relative current potential of lithium, and ordinate zou is an electrode reaction current) that cyclic voltammetric is tested with the scanning speed of 0.2mV/s.
Embodiment
Specific embodiment one:
(1) with 198.73 gram (1.7mol) NH 4VO 3Mix with 126 gram (3mol) LiOH, fully stir the back and add 345 gram (3mol) NH 4H 2PO 4, 23.96 gram (0.3mol) titanium oxide (TiO 2), fully add 288.2 gram (1.5mol) Hydrocerol A (C behind the agitation grinding again 6H 8O 7), control adds deionized water and is stirred to mixture is light blue muddy.Left standstill 10 minutes.With ammoniacal liquor (NH 3H 2O) adjust pH be neutral back move in the vacuum drying oven in 80 ℃ dry 4 hours down.
(2) again in 250 ℃ of bakings 2.5 hours, after grinding, insert in the inert atmosphere protection stove 600 ℃ of following sintering 240 minutes, naturally cool to room temperature in the stove, obtain Li 3V 1.7Ti 0.3(PO 4) 3
Specific embodiment two:
(1) with 132.8 gram (1.6mol) VO 2With 110.8 gram (1.5mol) Li 2CO 3Mix, fully stir the back and add 46.35 gram (0.4mol) titanium hydroxide (Ti (OH) 4), 609.3 the gram (3mol) (NH 4) 3PO 4H 2O fully adds 300.1 gram (2mol) tartrate (C again behind the agitation grinding 4H 6O 6), control adds deionized water and is stirred to mixture is light blue muddy.Left standstill 20 minutes.With ammoniacal liquor (NH 3H 2O) adjust pH is that neutral back moves in the vacuum drying oven in 75 ℃ of dryings 6 hours.
(2) again in 230 ℃ of bakings 2.5 hours, after grinding, insert that 650 ℃ of sintering naturally cooled to room temperature after 200 minutes in the inert atmosphere protection stove, obtain Li 3V 1.6Ti 0.4(PO 4) 3
Specific embodiment three:
(1) with 163.7 gram (0.9mol) V 2O 5With 306.1 gram (3mol) CH 3COOLi2H 2O mixes and fully adds 68.06 gram (0.2mol) butyl(tetra)titanates, 396.2 gram (3mol) (NH after the stirring 4) 2HPO 4H 2O fully adds 90.1 gram (1mol) C again behind the agitation grinding 2H 2O 4, control adds deionized water and is stirred to mixture is light blue muddy.Left standstill 10 minutes.With ammoniacal liquor (NH 3H 2O) adjust pH is that neutral back moves in the vacuum drying oven in 70 ℃ of dryings 5 hours.
(2) again in 270 ℃ of bakings 2 hours, after grinding, insert that 600 ℃ of sintering naturally cooled to room temperature after 180 minutes in the inert atmosphere protection stove, obtain Li 3V 1.8Ti 0.2(PO 4) 3
Specific embodiment four:
(1) with 81.85 gram (0.45mol) V 2O 5, 82.98g (1mol) VO 2With 153.05 gram (1.5mol) CH 3COOLi2H 2O and 76.43g (0.75mol) lithium oxalate mixes and fully adds 7.98 gram (0.1mol) titanium oxide, 396.2 gram (3mol) (NH after the stirring 4) 2HPO 4H 2O fully adds 67 gram (0.5mol) oxysuccinic acid behind the agitation grinding, control adds deionized water and is stirred to mixture is light blue muddy.Left standstill 10 minutes.With ammoniacal liquor (NH 3H 2O) adjust pH is that neutral back moves in the vacuum drying oven in 70 ℃ of dryings 5 hours.
(2) again in 200 ℃ of bakings 5 hours, after grinding, insert that 670 ℃ of sintering naturally cooled to room temperature after 100 minutes in the inert atmosphere protection stove, obtain Li 3V 1.9Ti 0.1(PO 4) 3
Embodiment five
(1) with 136.41 gram (0.75mol) V 2O 5Mixes and fully stir the back with 206.85 gram (3mol) lithium nitrates and add 170.15 gram (0.5mol) butyl(tetra)titanates, 294 gram (3mol) phosphoric acid, fully add 90.1 behind the agitation grinding again and restrain (1mol) C 2H 2O 4, control adds deionized water and is stirred to mixture is light blue muddy.Left standstill 30 minutes.With ammoniacal liquor (NH 3H 2O) adjust pH is that neutral back moves in the vacuum drying oven in 70 ℃ of dryings 5 hours.
(2) again in 270 ℃ of bakings 2 hours, after grinding, insert that 600 ℃ of sintering naturally cooled to room temperature after 180 minutes in the inert atmosphere protection stove, obtain Li 3V 1.5Ti 0.5(PO 4) 3
Embodiment 6
(1) with 233.8 gram (2mol) NH 4VO 3Mix with 126 gram (3mol) LiOH, fully stir the back and add 345 gram (3mol) NH 4H 2PO 4, fully add 288.2 (1.5mol) gram Hydrocerol A (C behind the agitation grinding again 6H 8O 7), control adds deionized water and is stirred to mixture is light blue muddy.Left standstill 10 minutes.With ammoniacal liquor (NH 3H 2O) adjust pH be neutral back move in the vacuum drying oven in 80 ℃ dry 4 hours down.
(2) again in 250 ℃ of bakings 2.5 hours, after grinding, insert in the inert atmosphere protection stove 600 ℃ of following sintering 240 minutes, naturally cool to room temperature in the stove, obtain Li 3V 2(PO 4) 3
Phosphoric acid vanadium titanium lithium and phosphoric acid vanadium lithium to method preparation of the present invention are done the performance comparison test, obtain following collection of illustrative plates:
Accompanying drawing 1 is the embodiment of the invention 3, embodiment 1 and embodiment 2 synthetic phosphoric acid vanadium titanium lithium Li 3V 1.8Ti 0.2(PO 4) 3, Li 3V 1.7Ti 0.3(PO 4) 3, Li 3V 1.6Ti 0.4(PO 4) 3X-ray diffraction (XRD) test pattern of the phosphoric acid vanadium lithium of the powder particle and (embodiment of the invention 6) preparation that uses the same method, the result shows: Li 3V 1.8Ti 0.2(PO 4) 3, Li 3V 1.7Ti 0.3(PO 4) 3, Li 3V 1.6Ti 0.4(PO 4) 3Crystalline structure be the monocline crystalline phase.Because the titanium that mixes forms sosoloid with phosphoric acid vanadium lithium, so and Li 3V 2(PO 4) 3The crystalline phase test result basic identical.
Accompanying drawing 2 is Li of the embodiment of the invention 1 preparation 3V 1.7Ti 0.3(PO 4) 3The exterior appearance of material granule, its median size are about 0.5 μ m.With Li 3V 2(PO 4) 3Exterior appearance and indifference.
Fig. 3 and Fig. 4 are respectively the embodiment of the invention 6 synthetic phosphoric acid vanadium lithium powder particles and use the same method the phosphoric acid vanadium titanium lithium Li of (embodiment of the invention 1) preparation 3V 1.7Ti 0.3(PO 4) 3Charge-discharge performance test pattern (electrochemical window at 3.30-4.80V is tested with the current density of 100mA/g, and X-coordinate is represented specific storage, and ordinate zou is the relative current potential of lithium)
Li 3V 1.7Ti 0.3(PO 4) 3Carry out constant current charge and discharge circulation its for the second time specific discharge capacity be higher than Li up to 173mAh/g 3V 2(PO 4) 3161.7mAh/g.
Fig. 5 is Li 3V 1.8Ti 0.2(PO 4) 3, Li 3V 1.7Ti 0.3(PO 4) 3, Li 3V 1.6Ti 0.4(PO 4) 3At the figure as a result that the electrochemical window of 3.30-4.80V is tested with the current density of 100mA/g, X-coordinate is represented specific storage, and ordinate zou is the relative current potential of lithium: three's the specific storage of constant-current discharge first is respectively 172mAh/g, 177mAh/g and 170mAh/g.
Fig. 6 is Li 3V 1.8Ti 0.2(PO 4) 3, Li 3V 1.7Ti 0.3(PO 4) 3, Li 3V 1.6Ti 0.4(PO 4) 3Li with embodiment 6 preparations 3V 2(PO 4) 3Carry out the figure as a result of cycle charge discharge electrical testing with the constant current density of 100mA/g at the electrochemical window of 3.30-4.80V; X-coordinate representes that circulation please charge and discharge number of times, and ordinate zou is a specific storage: put specific capacitance through the constant current of the above-mentioned sample in 30 week backs and be respectively 167mAh/g, 170mAh/g, 164mAh/g and 157mAh/g.
Fig. 7-10 is respectively the Li of embodiment 6 preparations 3V 2(PO 4) 3, Li 3V 1.8Ti 0.2(PO 4) 3, Li 3V 1.7Ti 0.3(PO 4) 3, Li 3V 1.6Ti 0.4(PO 4) 3The cyclic voltammetric test pattern (between the 3.00-4.30V electrochemical window with the 0.2mV/s rate test.X-coordinate is represented the relative current potential of lithium, and ordinate zou is an electrode reaction current):
From figure, can be observed: with Li 3V 2(PO 4) 3Relatively, Li 3V 1.8Ti 0.2(PO 4) 3, Li 3V 1.7Ti 0.3(PO 4) 3And Li 3V 1.6Ti 0.4(PO 4) 3Increase in the value of 3.60-3.57V electrochemical window place's redox peak point current with respect to 3.64-3.78V electrochemical window place.This shows Li 3V 1.8Ti 0.2(PO 4) 3, Li 3V 1.7Ti 0.3(PO 4) 3And Li 3V 1.6Ti 0.4(PO 4) 3Under this electrochemical window, has the Li of ratio 3V 2(PO 4) 3Higher electrochemical activity.
In sum, the Li of the present invention's preparation 3V 2-xTi x(PO 4) 3The chemical property of (wherein x=0.1-0.5) is superior to phosphoric acid vanadium lithium, can realize a batch stable performance, low-cost preparation method.

Claims (7)

1. ion battery anode material vanadium lithium phosphate titanium lithium, its chemical formula does
Li 3V 2-xTi x(PO 4) 3, x=0.1-0.5 wherein; This preparation methods is:
(1) takes by weighing lithium source, vanadium source, titanium source and phosphorus source thorough mixing and grind back adding coordination agent; Wherein the amount of substance ratio of lithium source, vanadium source, titanium source, phosphorus source, coordination agent is 3.0: 1.90-1.50: 0.1-0.50: 3.0: 0.5-2.0, stir control simultaneously and add deionized water till mixture gradually becomes light blue mud;
(2) with this mud liquid leave standstill move into after using the ammoniacal liquor adjust pH as neutrality after 10-30 minute in the vacuum drying oven 70-90 ℃ dry 2-6 hour down;
(3) material in the step (2) is taken out; Putting into baking oven after the grinding toasted 2-5 hour down at 200-270 ℃; Insert then and carry out sintering in the inert atmosphere protection stove, sintering temperature 600-670 ℃, naturally cool to room temperature after sintering 100-240 minute and obtain phosphoric acid vanadium titanium lithium.
2. according to the said a kind of ion battery anode material vanadium lithium phosphate titanium lithium of claim 1.It is characterized in that: said x=0.2-0.4.
3. according to claim 1 or 2 said a kind of ion battery anode material vanadium lithium phosphate titanium lithiums.It is characterized in that: said lithium source is one or more the mixture in lithium oxalate, Lithium Acetate, lithium nitrate, Quilonum Retard, the Lithium Hydroxide MonoHydrate.
4. according to claim 1 or 2 said a kind of ion battery anode material vanadium lithium phosphate titanium lithiums.It is characterized in that: said vanadium source is one or more the mixture in vanadium dioxide, Vanadium Pentoxide in FLAKES, the ammonium meta-vanadate.
5. according to claim 1 or 2 said a kind of ion battery anode material vanadium lithium phosphate titanium lithiums.It is characterized in that: said titanium source is one or more the mixture in titanium oxide, titanium hydroxide, the butyl(tetra)titanate.
6. according to claim 1 or 2 said a kind of ion battery anode material vanadium lithium phosphate titanium lithiums.It is characterized in that: said coordination agent is one or more the mixture in Hydrocerol A, oxalic acid, tartrate, the oxysuccinic acid.
7. according to claim 1 or 2 said a kind of ion battery anode material vanadium lithium phosphate titanium lithiums.It is characterized in that: said phosphorus source is one or more the mixture in ammonium phosphate, primary ammonium phosphate, Secondary ammonium phosphate, Trilithium phosphate, the phosphoric acid.
CN2012101181594A 2012-04-20 2012-04-20 Vanadium titanium lithium phosphate material for positive electrode of lithium ion battery Pending CN102627266A (en)

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CN110858643A (en) * 2018-08-24 2020-03-03 湖南杉杉新能源有限公司 Fast ion conductor modified lithium ion battery cathode material and preparation method thereof
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CN116120050A (en) * 2023-02-15 2023-05-16 中国振华集团云科电子有限公司 Ultralow-temperature sintered LTCC ceramic material and preparation method thereof
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110858643A (en) * 2018-08-24 2020-03-03 湖南杉杉新能源有限公司 Fast ion conductor modified lithium ion battery cathode material and preparation method thereof
CN112390242A (en) * 2020-11-23 2021-02-23 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of titanium-doped lithium vanadium phosphate cathode material
WO2024032508A1 (en) * 2022-08-10 2024-02-15 比亚迪股份有限公司 Positive electrode active material, and preparation method therefor and use thereof
CN116120050A (en) * 2023-02-15 2023-05-16 中国振华集团云科电子有限公司 Ultralow-temperature sintered LTCC ceramic material and preparation method thereof
CN116120050B (en) * 2023-02-15 2023-12-19 中国振华集团云科电子有限公司 Ultralow-temperature sintered LTCC ceramic material and preparation method thereof

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Application publication date: 20120808