CN101955176A - Method for preparing anode material lithium vanadium phosphate of lithium ion battery by microwave sintering - Google Patents
Method for preparing anode material lithium vanadium phosphate of lithium ion battery by microwave sintering Download PDFInfo
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Abstract
The invention relates to a method for preparing an anode material for a Li3V2(PO4)3 lithium ion battery, belonging to the field of lithium ion battery materials. The method comprises the following steps: weighing a lithium source compound, V2O5 and phosphoric acid according to a molar ratio that Li to V to P is 3:1.8-2.0:2.8-3.0; mixing the V2O5 and the phosphoric acid, uniformly stirring, and standing for 2 to 4 hours to obtain mixture A of primary reaction; adding the lithium source compound into carbon source compound water solution to prepare mixture, adding the mixture into the mixture A, uniformly stirring to obtain a pasty precursor; and placing the pasty precursor into a microwave oven, heating to the temperature of between 700 and 800 DEG C at the heating rate of between 5 and 15 DEG C/min, and cooling to room temperature after 20 to 55min of heat treatment. The method has the advantages of rich production raw material sources, simple preparation process, easy control, low energy consumption, low cost, high product purity, stable quality and excellent electrochemical performance, and can be widely applied to industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of active substance of lithium ion battery anode, particularly relate to a kind of anode material for lithium-ion batteries Li
3V
2(PO
4)
3The preparation method.
Background technology
Lithium ion battery because of its output voltage height, specific energy height, have extended cycle life, and advantages such as self-discharge is little, safety, memory-less effect, become the emphasis of our times various countries in the development of new energy materials field, wherein positive electrode material is the key of lithium ion battery.The positive electrode current material mainly contains: cobalt acid lithium, lithium nickelate, lithium manganate etc., but domesticly only have cobalt acid lithium to form large-scale production.Because cobalt belongs to precious metal, resource-constrained, poisonous, its development is restricted, and there is potential safety hazard in cobalt acid lithium, so people are just striving to find the substitute of cobalt acid lithium.
As polyanion positive electrode, Li
3V
2(PO
4)
3Owing to have high stability, high power capacity and the high potential of general polyanion material, also be subjected in recent years people's close attention.Li
3V
2(PO
4)
3Belong to P2
1/ n space group, molecular weight are 407.6, Li
3V
2(PO
4)
3In V can have+2 ,+3 ,+4 and+5 4 kinds appraise at the current rate, have in theory 5 lithium ions can in material, take off embedding, theoretical capacity is up to 332 mAh/g.
Although vanadium has certain toxicity, discover that the v element of lower concentration is to the not influence of most animals and plants, vanadium still is the important composition element of a lot of medical medicines.At occurring in nature, vanadium content in the earth's crust is abundanter, and content is 0.02%, but its distribution in the nature disperses very much, can not form independent vanadium deposit, mainly is present in vanadium titano-magnetite and the bone coal.There is abundant navajoite resource in China, although resource does not have iron abundant, has the higher vanadium of content in iron steel smelting slag.Therefore from economy and environment angle, Li
3V
2(PO
4)
3The exploitation of cell positive material is significant.
At present, to anode material for lithium-ion batteries Li
3V
2(PO
4)
3Study on the industrialization just just begin known Li
3V
2(PO
4)
3Synthetic method mainly contains two kinds of high temperature solid-state method, sol-gal processes.The raw material that high temperature solid-state method adopts is lithium salts, vanadic salts and phosphoric acid salt nearly all, through pre-burning, adds carbon reduction again or the hydrogen reducing roasting forms.Not only operation is more loaded down with trivial details, and has the problem that purity is low and production cost is high of sintetics.The control of sol-gel method synthesis condition is harsh, is unsuitable for suitability for industrialized production.
By retrieval; the patent No. is a kind of anode material for lithium-ion batteries of the patent disclosure of CN200910113805.6 prepares lithium ion battery anode material vanadium lithium phosphate with the microwave rapid reaction a method; comprise that with mol ratio be after vanadium pentoxide powder, phosphoric acid salt, organic acid, lithium salts and the villiaumite of 0.95-1.1:1.9-2.1:0.95-1.1:1.9-2.1:1.9-2.1 mixes; under protection of inert gas in microwave reactor 450-750 ℃ of sintering 10-40min, be finished product LiVPO after the cooling
4F.The anode material for lithium-ion batteries that this method makes is LiVPO
4F, its reaction process, reaction mechanism and preparation phosphoric acid vanadium lithium are inequality.In addition, this method just be carried out sintering after mixing with related raw material is simple, preceding half section identical with solid phase method; This method is just in prepared in laboratory, and the product of preparation has only several grams, and in view of the singularity of microwave sintering, this method also can't be carried out industrialization production at present.
Summary of the invention
The technical problem to be solved in the present invention is: overcome anode material for lithium-ion batteries Li in the prior art
3V
2(PO
4)
3The cost height, the shortcoming of poor performance of preparation provide a kind of work simplification, cost is low, energy consumption is low anode material for lithium-ion batteries Li
3V
2(PO
4)
3The preparation method.
Technical scheme of the present invention:
A kind of anode material for lithium-ion batteries Li
3V
2(PO
4)
3The preparation method, may further comprise the steps,
(1) with Li source compound, V
2O
5, phosphoric acid is that the mol ratio of 3:1.8 ~ 2.0:2.8 ~ 3.0 is measured respectively by Li:V:P, then with V
2O
5, phosphoric acid mixes, and makes V
2O
5Be dissolved in the phosphoric acid, stir, leave standstill 2 ~ 4h, obtain the mixture A of initial reaction;
(2) weight with target product is benchmark, and water-soluble carbon-source cpd of metering 6～30% and 50～120% pure water add carbon-source cpd in the pure water, stir, and obtain the carbon-source cpd aqueous solution;
(3) described Li source compound is added in the described carbon-source cpd aqueous solution, stir, obtain mixture B;
(4) mixture A, B are mixed, stir, obtain the paste presoma; Leave standstill 2～4h;
(5) described paste presoma is placed non-metallic vessel, through industrial microwave oven heat treatment, prepare Li
3V
2(PO
4)
3
Described phosphoric acid is the industrial phosphoric acid of mass concentration 85%.
Described Li source compound is lithium hydroxide, Quilonum Retard or Lithium Acetate.
Described water-soluble carbon-source cpd is oxalic acid, citric acid, glucose, sucrose, lactose or maltose.
Described non-metallic vessel is carborundum crucible, plumbago crucible, glass pot or paper container.
The power of described industrial microwave oven is 5 ~ 25KW, and it is to utilize microwave to be warming up to 700 ~ 800 ℃ with the speed of 5 ~ 15 ℃ of per minutes that microwave thermal is handled, and keeps 25 ~ 55min in this temperature.
Beneficial effect of the present invention:
(1) raw material mixing in early stage of the present invention adopts liquid phase to mix (V
2O
5Be dissolved in phosphoric acid) method, can make its reaction reach the molecular level level, adding then lithium salts and pure water, that raw material is mixed is more abundant, makes more even that early stage, raw material mixed.
(2) the present invention directly is dissolved in water-soluble carbon-source cpd in the pure water, compares with traditional solid phase method, makes that carbon is easier to mix, and more helps synthesizing.
(3) the paste presoma that will form after the present invention will mix directly enters and carries out sintering in the industrial microwave oven, has omitted the technical process such as traditional ball milling, drying, work simplification, and technology controlling and process is simple, is conducive to the control of product quality.
(4) the present invention adopts the industrial microwave heating, and material self integral body is heated up simultaneously, and firing rate is fast, pollution-free, processed sample grain refinement, and even structure, simultaneously heating using microwave can accurately be controlled, and has shortened generated time, energy savings.Traditional sintering time need to be incubated about 10h, and microwave sintering time of the present invention not enough 1h only shortens generated time greatly.
(5) technology of the present invention is simple, need not to adopt gas shield in the production process, can react under normal pressure, and production cost is low, and the favorable reproducibility of different batches product is fit to large-scale industrial production.
(6) technology of the present invention can not produce various obnoxious flavoures in sintering process, and is pollution-free, is very beneficial for environmental protection.
(7) the present invention directly is dissolved in water-soluble carbon-source cpd in the pure water, and carbon is coated on the prepared positive electrode equably, is increasing substantially Li
3V
2(PO
4)
3In the time of electrical conductivity, but Effective Raise Li also
3V
2(PO
4)
3Charge/discharge capacity and cycle-index.
The Performance Detection of product: the Li that the carbon that the present invention is prepared coats
3V
2(PO
4)
3Sample and conductive agent (acetylene black), binding agent (Kynoar) in mass ratio 80:15:5 evenly mix, and mixture is dissolved in the 1-METHYLPYRROLIDONE, are modulated into paste, evenly are applied on the aluminium foil.Behind seasoning 8h, roll, put into temperature and be more than 80 ~ 100 ℃ the dry 12h of vacuum drying oven.Cut film,, put into the glove box that is full of Ar gas the Small diaphragm-piece weighing.In glove box, make counter electrode, put into polypropylene screen Cellgard2400 barrier film, splash into electrolytic solution then through the wetting mistake of electrolytic solution [1 mol/L LiPF6/ NSC 11801 (EC)+diethyl carbonate (DEC)+methylcarbonate (DMC)] with the lithium sheet; With the stainless steel gasket is collector, is assembled into the button Experimental cell and tests.
The CT2001A type cell tester that adopts Wuhan City blue electronics limited (LAND) company to produce is tested voltage range 3.0 ~ 4.8 V to the capacity and the cycle performance of battery.
Adopt the inventive method when carbon-source cpd is sucrose or glucose, to prepare positive electrode, with synthetic Li
3V
2(PO
4)
3Positive electrode is assembled into the button Experimental cell and tests, and at room temperature the constant current with 30 mA/g discharges and recharges under the condition, and recording maximum discharge capacity is 146.1 ~ 150.2mAh/g, and after 100 circulations, capacity is 113.6 ~ 118.2 mAh/g.
When carbon-source cpd is citric acid, with synthetic Li
3V
2(PO
4)
3Material is assembled into the button Experimental cell and tests, and at room temperature the constant current with 30 mA/g discharges and recharges under the condition, and recording maximum discharge capacity is 181.7 ~ 186.2mAh/g, and after 100 circulations, capacity is 143.6 ~ 148.2 mAh/g.
Test shows, when using citric acid, synthesizes Li
3V
2(PO
4)
3The small size of material granule can make the insertion of lithium path contraction, and the carbon that citric acid at high temperature decomposes generation is present in the material more, has increased the conductance of material, and two kinds of effects have improved the chemical property of material jointly.
Description of drawings:
The Li that Fig. 1 prepares when adopting carbon-source cpd for glucose for the present invention
3V
2(PO
4)
3Sem photograph.
The Li that Fig. 2 prepares when adopting carbon-source cpd for citric acid for the present invention
3V
2(PO
4)
3Sem photograph.
Can be found out the Li for preparing when adopting carbon-source cpd for glucose by Fig. 1, Fig. 2
3V
2(PO
4)
3Particle size not of uniform size, big greater than 10 microns, little of below 1 micron.With respect to glucose, adopt the Li of citric acid preparation
3V
2(PO
4)
3Material is spherical in shape, and granule size is even, and size is between 2～5 microns, and particle disperses, and this is conducive to taking off into going out with embedding of lithium ion.
Fig. 3 is the Li of the present invention's preparation
3V
2(PO
4)
3XRD figure.
The Li of this spectrogram and monocline
3V
2(PO
4)
3Spectrogram very identical.Strong and sharp-pointed diffraction maximum shows the product well-crystallized in the spectrogram; Not assorted peak exists in the spectrogram, illustrates that the present invention can synthesize the Li of pure phase
3V
2(PO
4)
3, residual RESEARCH OF PYROCARBON exists with unformed.
Embodiment:
In order to understand better the present invention, for example the present invention is specifically described below, percentages wherein all refers to mass percent concentration as not specifying.
Embodiment one:Anode material for lithium-ion batteries Li
3V
2(PO
4)
3The preparation method
(1) with 7360 gram V
2O
5Mix with the phosphoric acid of 13800 grams 85%, stir, make V
2O
5Be dissolved in the phosphoric acid, leave standstill 4h, obtain vanadium oxonium ion and the V of initial reaction
2O
5, phosphoric acid mixture; The vanadium oxonium ion is VO
3+, VO
+Deng;
(2) 2400 gram sucrose are dissolved in the 8000mL pure water, stir, obtain aqueous sucrose solution;
(3) with 5100 gram LiOHH
2O joins in the above-mentioned aqueous sucrose solution, stirs, and obtains mixture;
(4) mixture of step (3) and the mixture of step (1) are mixed, stir, obtain the paste presoma, leave standstill 4h;
(5) described paste presoma is put into the carborundum crucible, the carborundum crucible is put into industrial microwave oven, be warmed up to 780 ℃ with the speed of 6 ℃ of per minutes, insulation 30min namely obtains positive electrode Li
3V
2(PO
4)
3
(LiOHH wherein
2O molecular weight 42, V
2O
5Molecular weight 182, the phosphoric acid molecules amount is 98, the mol ratio that can be calculated Li:V:P is 3:2:3).
This example can prepare about 16kg Li
3V
2(PO
4)
3, the amount that adds pure water is equivalent to Li
3V
2(PO
4)
350% of amount, the amount that adds sucrose is equivalent to Li
3V
2(PO
4)
315% of amount.
Embodiment two:Anode material for lithium-ion batteries Li
3V
2(PO
4)
3The preparation method
(1) with 7360 gram V
2O
5Mix with the phosphoric acid of 13800 grams 85%, stir, make V
2O
5Be dissolved in the phosphoric acid, leave standstill 2h, obtain vanadium oxonium ion and the V of initial reaction
2O
5, phosphoric acid mixture;
(2) 2000 gram glucose are dissolved in the 1100mL pure water, stir, obtain D/W;
(3) with 4600 gram Li
2CO
3Add in the D/W of step (2) preparation, stir, obtain mixture;
(4) mixture with step (3) joins in the mixture of step (1), stirs, and obtains the paste presoma, leaves standstill 2h;
(5) described paste presoma is put into the brown paper crucible, the brown paper crucible is put into industrial microwave oven, be warmed up to 720 ℃ with the speed of 8 ℃ of per minutes, insulation 20min obtains positive electrode Li
3V
2(PO
4)
3
This example can prepare about 16kg Li
3V
2(PO
4)
3, the amount that adds pure water is equivalent to Li
3V
2(PO
4)
369% of amount, the amount that adds sucrose is equivalent to Li
3V
2(PO
4)
312.5% of amount.
Embodiment three:Anode material for lithium-ion batteries Li
3V
2(PO
4)
3The preparation method
(1) with 7360 gram V
2O
5Mix with the phosphoric acid of 13800 grams 85%, stir, make V
2O
5Be dissolved in the phosphoric acid, leave standstill 3h, obtain vanadium oxonium ion and the V of initial reaction
2O
5, phosphoric acid mixture;
(2) 2000 gram citric acids are dissolved in the pure water of 17000mL, stir, obtain the lemon aqueous acid;
(3) 13000 gram Lithium Acetates are added in the aqueous citric acid solution of step (2), stir, obtain mixture;
(4) mixture of step (3) and the mixture of step (1) are mixed, stir, obtain the paste presoma; Leave standstill 3h;
(5) described paste presoma is put into the glass pot crucible, the glass pot crucible is put into industrial microwave oven, be warmed up to 750 ℃ with the speed of 10 ℃ of per minutes, insulation 25min obtains positive electrode Li
3V
2(PO
4)
3
This example can prepare about 16kg Li
3V
2(PO
4)
3, the amount that adds pure water is equivalent to Li
3V
2(PO
4)
3106.25% of amount.
Embodiment four:Anode material for lithium-ion batteries Li
3V
2(PO
4)
3The preparation method, basic identical with embodiment one, difference is:
Replace the carborundum crucible with graphite crucible, replace sucrose with glucose, add pure water 14000mL, the microwave thermal treatment temperature is 780 ℃, insulation 50min;
This example can prepare about 16kg Li
3V
2(PO
4)
3, the amount that adds pure water is equivalent to Li
3V
2(PO
4)
387.5% of amount.
Embodiment five:Anode material for lithium-ion batteries Li
3V
2(PO
4)
3The preparation method, basic identical with embodiment two, difference is:
Replace the brown paper crucible with glass pot, replace glucose with lactose or maltose; The microwave thermal treatment temperature is 800 ℃, insulation 25min.
Embodiment six:Anode material for lithium-ion batteries Li
3V
2(PO
4)
3The preparation method, basic identical with embodiment three, difference is: replace citric acid with oxalic acid.
Embodiment seven:Anode material for lithium-ion batteries Li
3V
2(PO
4)
3The preparation method
(1) with lithium acetate, V
2O
5, phosphoric acid is that the mol ratio of 3:1.8:2.8 is measured respectively by Li:V:P, with V
2O
5, phosphoric acid mixes, and stirs, and makes V
2O
5Be dissolved in the phosphoric acid, leave standstill 2h, obtain the mixture A of initial reaction; Used phosphoric acid is 85% industrial phosphoric acid;
(2) the standby target product Li of metrology
3V
2(PO
4)
3The citric acid of weight 10%, the pure water of the target product weight 50% of adding preparation stirs then, obtains aqueous citric acid solution;
(3) Lithium Acetate with metering adds in the aqueous citric acid solution, stirs, and obtains mixture B;
(4) mixture A, B are mixed, stir, obtain the paste presoma, leave standstill 2h;
(5) the paste presoma is put in the graphite crucible, through industrial microwave oven heat treatment, microwave power is 20KW, and microwave is warming up to 700 ℃ with the speed of 15 ℃ of per minutes, and keeps 45min in this temperature, prepares Li
3V
2(PO
4)
3
Embodiment eight:Anode material for lithium-ion batteries Li
3V
2(PO
4)
3The preparation method
(1) with lithium acetate, V
2O
5, phosphoric acid is that the mol ratio of 3:2.0:2.8 is measured respectively by Li:V:P, with V
2O
5, phosphoric acid mixes, and stirs, and makes V
2O
5Be dissolved in the phosphoric acid, leave standstill 3h, obtain the mixture A of initial reaction;
(2) with the target product be benchmark, the citric acid of metering 20% and 120% pure water add citric acid in the pure water, stir, and obtain aqueous citric acid solution;
(3) Lithium Acetate is added in the aqueous citric acid solution, stir, obtain mixture B;
(4) mixture A, B are mixed, stir, obtain the paste presoma, leave standstill 3h;
(5) the paste presoma is put in the graphite crucible, through industrial microwave oven heat treatment, microwave power is 10KW, and microwave is warming up to 750 ℃ with the speed of 10 ℃ of per minutes, and keeps 35min in this temperature, prepares Li
3V
2(PO
4)
3
Embodiment nine:Anode material for lithium-ion batteries Li
3V
2(PO
4)
3The preparation method
(1) with lithium hydroxide, V
2O
5, phosphoric acid is that the mol ratio of 3:1.9:2.9 is measured respectively by Li:V:P, with V
2O
5, phosphoric acid mixes, and stirs, and makes V
2O
5Be dissolved in the phosphoric acid, leave standstill 4h, obtain the mixture A of initial reaction;
(2) with the target product be benchmark, the oxalic acid of metering 20% and 60% pure water add oxalic acid in the pure water, stir, and obtain oxalic acid aqueous solution;
(3) Li source compound is added in the oxalic acid aqueous solution, stir, obtain mixture B;
(4) mixture A, B are mixed, stir, obtain the paste presoma, leave standstill 2.5h;
(5) described paste presoma is placed glass pot, through industrial microwave oven heat treatment, the power of industrial microwave oven is 25KW, and microwave is warming up to 740 ℃ with the speed of 15 ℃ of per minutes, and keeps 50min in this temperature, prepares Li
3V
2(PO
4)
3
Embodiment ten:Anode material for lithium-ion batteries Li
3V
2(PO
4)
3The preparation method
(1) with lithium carbonate, V
2O
5, phosphoric acid is that the mol ratio of 3:2.0:2.8 is measured respectively by Li:V:P, with V
2O
5, phosphoric acid mixes, and stirs, and makes V
2O
5Be dissolved in the phosphoric acid, leave standstill 3.5h, obtain the mixture A of initial reaction;
(2) with the target product be benchmark, the maltose of metering 25% and 100% pure water add maltose in the pure water, stir, and obtain maltose solution;
(3) Quilonum Retard is added in the maltose solution, stir, obtain mixture B;
(4) mixture A, B are mixed, stir, obtain the paste presoma; Leave standstill 4h;
(5) described paste presoma is placed paper container, through industrial microwave oven heat treatment, the power of industrial microwave oven is 10KW, and microwave is warming up to 720 ℃ with the speed of 12 ℃ of per minutes, and keeps 45min in this temperature, prepares Li
3V
2(PO
4)
3
Claims (6)
1. anode material for lithium-ion batteries Li
3V
2(PO
4)
3The preparation method, it is characterized in that: this method may further comprise the steps,
(1) with Li source compound, V
2O
5, phosphoric acid is that the mol ratio of 3:1.8 ~ 2.0:2.8 ~ 3.0 is measured respectively by Li:V:P, then with V
2O
5, phosphoric acid mixes, and makes V
2O
5Be dissolved in the phosphoric acid, stir, leave standstill 2 ~ 4h, obtain the mixture A of initial reaction;
(2) weight with target product is benchmark, and water-soluble carbon-source cpd of metering 6～30% and 50～120% pure water add carbon-source cpd in the pure water, stir, and obtain the carbon-source cpd aqueous solution;
(3) described Li source compound is added in the described carbon-source cpd aqueous solution, stir, obtain mixture B;
(4) mixture A, B are mixed, stir, obtain the paste presoma; Leave standstill 2～4h;
(5) described paste presoma is placed non-metallic vessel, through industrial microwave oven heat treatment, prepare Li
3V
2(PO
4)
3
2. preparation method according to claim 1 is characterized in that: described phosphoric acid is the industrial phosphoric acid of mass concentration 85%.
3. preparation method according to claim 1 is characterized in that: described Li source compound is lithium hydroxide, Quilonum Retard or Lithium Acetate.
4. preparation method according to claim 1 is characterized in that: described water-soluble carbon-source cpd is oxalic acid, citric acid, glucose, sucrose, lactose or maltose.
5. preparation method according to claim 1 is characterized in that: described non-metallic vessel is carborundum crucible, plumbago crucible, glass pot or paper container.
6. according to each described preparation method of claim 1-5, it is characterized in that: the power of described industrial microwave oven is 5 ~ 25KW, and it is to utilize microwave to be warming up to 700 ~ 800 ℃ with the speed of 5 ~ 15 ℃ of per minutes that microwave thermal is handled, and keeps 25 ~ 55min in this temperature.
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|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102290575A (en) * | 2011-07-21 | 2011-12-21 | 中国电子科技集团公司第十八研究所 | Lithium ion cell anode material and preparation method thereof |
| CN110504422A (en) * | 2019-07-29 | 2019-11-26 | 全球能源互联网研究院有限公司 | A kind of cell positive material and preparation method thereof |
| CN113991167A (en) * | 2021-10-26 | 2022-01-28 | 西安交通大学 | Halide solid electrolyte material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101262060A (en) * | 2008-04-15 | 2008-09-10 | 中南大学 | A method for making anode material Li3V2(PO4)3 of lithium ion battery |
| CN101794881A (en) * | 2010-03-22 | 2010-08-04 | 河南联合新能源有限公司 | Method for preparing anode material of lithium ion batteries by one-step microwave sintering |
-
2010
- 2010-10-20 CN CN 201010513033 patent/CN101955176A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101262060A (en) * | 2008-04-15 | 2008-09-10 | 中南大学 | A method for making anode material Li3V2(PO4)3 of lithium ion battery |
| CN101794881A (en) * | 2010-03-22 | 2010-08-04 | 河南联合新能源有限公司 | Method for preparing anode material of lithium ion batteries by one-step microwave sintering |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102290575A (en) * | 2011-07-21 | 2011-12-21 | 中国电子科技集团公司第十八研究所 | Lithium ion cell anode material and preparation method thereof |
| CN110504422A (en) * | 2019-07-29 | 2019-11-26 | 全球能源互联网研究院有限公司 | A kind of cell positive material and preparation method thereof |
| CN113991167A (en) * | 2021-10-26 | 2022-01-28 | 西安交通大学 | Halide solid electrolyte material and preparation method and application thereof |
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Application publication date: 20110126 |