CN105576220A - Preparation method of porous carbon-coated lithium iron phosphate anode material - Google Patents
Preparation method of porous carbon-coated lithium iron phosphate anode material Download PDFInfo
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- CN105576220A CN105576220A CN201610161867.4A CN201610161867A CN105576220A CN 105576220 A CN105576220 A CN 105576220A CN 201610161867 A CN201610161867 A CN 201610161867A CN 105576220 A CN105576220 A CN 105576220A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a preparation method of a porous carbon-coated lithium iron phosphate anode material. The preparation method comprises the following steps: (1) mixing LiFePO4 with a carbon source to obtain a mixture A, and mixing the mixture A with volatile ammonium salt so as to obtain a mixture B; mixing deionized water with absolute ethanol to obtain a solution C; finally, mixing the mixture B with the solution C, so as to prepare slurry; (2) stirring the slurry obtained in the step (1), freezing the slurry at minus 50-minus 10 DEG C for 1-2 hours, drying and grinding at a vacuum state, and heating at 50-120 DEG C for 1-2 hours; and (3) sintering at 400-750 DEG C for 2-4 hours in the presence of nitrogen, and cooling to the room temperature, so as to obtain the porous carbon-coated LiFePO4/C. By forming holes by virtue of inorganic salt which can be directly decomposed in a gas phase, the preparation method has the special advantages that the process is simple, the cost is low, impurities are not introduced, and the like; and the preparation method is applicable to large-scale industrial production.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries preparation field, particularly relate to a kind of preparation method of cellular carbon-coated LiFePO 4 for lithium ion batteries positive electrode.
Background technology
LiFePO4 (LiFePO
4) advantage such as high and security performance is good with its raw material rich reserves, environmental friendliness, good stability, specific capacity, become the emphasis of anode material for lithium ion battery of future generation development.But conductivity is low and lithium ion diffusion coefficient is little, and make its rate charge-discharge performance and poor performance at low temperatures, this seriously restricts LiFePO
4extensive use.Therefore, how LiFePO is improved
4conductivity and Li
+diffusion coefficient is the important goal of this material improvement.
At present, carbon coating technology improves LiFePO
4the most practical and the most effective means of chemical property, coated modified carbon is for raising LiFePO
4the chemical property of material plays great function.At LiFePO
4particle surface coated with conductive carbon: can strengthen the conductivity between particle and particle on the one hand, reduces the polarization of battery; Electron tunnel can also be provided for material on the other hand, suppress crystal grain to increase, the effect of reducing agent can also be played simultaneously, avoid Fe
3+generation.So material with carbon-coated surface is unique a kind of raising LiFePO be applied in actual production
4conductivity and Li
+the method of ionic diffusion coefficient.
But, LiFePO
4surface coated carbon is inert matter, and carbon addition too much not only can affect tap density and the processing characteristics of material, reduces LiFePO to a certain extent simultaneously
4contact area with electrolyte, hinders Li
+motion.Therefore, carbon cladding process is improved for preparation LiFePO
4material has important production meaning.At present, do a lot of work improving in carbon cladding process.CN101714634A provides the coated LiFePO of a kind of carbon
4microwave preparation, CN102290567A discloses the coated LiFePO of a kind of polyacrylonitrile cracking carbon
4preparation method, CN102544508A discloses the coated LiFePO of a kind of carbon
4the preparation method of composite material, CN104617296A discloses one and has the coated LiFePO of mesoporous carbon
4the preparation method of positive electrode, CN102367170A discloses a kind of hud typed carbon-coated nano level LiFePO
4the preparation method of composite positive pole, CN104779395A discloses a kind of three-dimensional conductive network configuration LiFePO
4the preparation method of positive electrode.But the carbon-coating that existing carbon cladding process is formed is at raising LiFePO
4liFePO is hindered while positive electrode conductivity
4with fully contacting of electrolyte, be unfavorable for Li simultaneously
+motion.So, seek one and can improve electrolyte and LiFePO
4the carbon cladding process of abundant contact is particularly necessary.
Summary of the invention
Order of the present invention is to improve the coated LiFePO of carbon
4technique, particularly provides a kind of cellular carbon coated LiFePO
4the preparation method of positive electrode.The method mixes volatile ammonium salt in the coated process of carbon with carbon source, be evenly coated on LiFePO
4surface, heats after freeze drying, utilizes the effumability of ammonium salt, at LiFePO
4, after sintering, there is porous surface shape LiFePO in particle surface " pore-creating "
4/ C.The carbon of porous surface is coated can provide more passage for lithium ion, improves high rate performance and the cryogenic property of positive electrode.
Technical scheme of the present invention is:
A preparation method for cellular carbon-coated LiFePO 4 for lithium ion batteries positive electrode, comprises the following steps:
Step one: by preparation LiFePO
4be mixed to get mixture A with carbon source, get mixture A and mix obtained mixture B with volatility ammonium salt; Separately deionized water and absolute ethyl alcohol are mixed to get solution C; Finally, mixture B is mixed with solution C, is mixed with slurry;
Wherein, mol ratio is carbon: iron=0.1:1 ~ 1:1; Quality is than mixture A: volatility ammonium salt=20:1 ~ 2:1; Volume ratio deionized water: absolute ethyl alcohol=10:1 ~ 1:1; Quality is than mixture B: solution C=1:1 ~ 1:2;
Step 2: the slurry first step obtained stirs 1h ~ 2h in a kettle., stir disposed slurry and put into freeze drier, 1h ~ 2h is freezed at-50 DEG C ~-10 DEG C, then dry 2h ~ 5h under vacuo, product will be obtained and pulverize frustillatum, then baking oven is put into, 50 DEG C ~ 120 DEG C heating 1h ~ 2h;
Step 3: sintering furnace put into by material step 2 finally obtained, nitrogen atmosphere 400 DEG C ~ 750 DEG C sintering 2h ~ 4h, is cooled to room temperature, obtains the LiFePO that cellular carbon is coated
4/ C.
Described carbon source be specially in glucose, sucrose, polyethylene glycol, starch and xylitol one or more.
Described volatility ammonium salt be specially in ammonium carbonate, ammonium oxalate and carbonic hydroammonium one or more.
Vacuum pressure in described step 2 is 1.3 ~ 13Pa.
Substantive distinguishing features of the present invention is: first carbon source is coated on LiFePO uniformly
4particle surface, first through freeze drying, in freezing dry process, due to moisture content and absolute ethyl alcohol distillation, LiFePO
4particle surface carbon source layer there will be certain hole.Then, in 50 DEG C ~ 120 DEG C baking ovens, ammonium salt decomposition becomes gas, to LiFePO
4particle surface carbon source layer carries out second time pore-creating.Through freeze drying and ammonium salt decomposition process, LiFePO
4there is a large amount of hole in particle surface carbon source layer.Finally by high temperature sintering, the carbonization of carbon source layer, obtains the LiFePO that cellular carbon is coated
4/ C.
Beneficial effect of the present invention is:
The present invention utilizes the ammonium salt heating such as ammonium carbonate, ammonium oxalate, carbonic hydroammonium easily to resolve into the feature of gas, and 50 DEG C ~ 120 DEG C heating ammonium salt decomposition become gas, at LiFePO
4particle surface forms carbon source (glucose, sucrose, polyethylene glycol, starch, the xylitol etc.) layer of one deck porous.Be coated with the LiFePO of porous carbon source
4particle is high temperature sintering in a nitrogen environment, porous carbon source carbonization under high temperature, is formed and has the coated LiFePO of cellular carbon-coating
4/ C.The coated LiFePO of cellular carbon prepared by the inventive method
4/ C positive electrode material, there is a large amount of hole in particle surface.The appearance major advantage of hole is: 1, these holes are Li
+embedding between both positive and negative polarity is embedding to be gone out to provide passage, reduces Li
+by the diffusional resistance that carbon-coating runs into, improve the diffusion rate of lithium ion; 2, the appearance of these holes, increases the specific area of material, makes LiFePO
4particle fully contacts with electrolyte, adds the diffusing capacity of lithium ion.Above 2 multiplying power discharging properties that greatly can improve positive electrode.Compared with positive electrode under normal temperature, the electrolyte under low-temperature condition activity itself reduces, Li
+movement rate in the electrolytic solution can significantly slow down, and adds LiFePO
4the self reason of material olivine structural, causes LiFePO
4the cryogenic property that material is poor.LiFePO
4the appearance in particle surface aperture, reduces ion diffuse resistance, to a certain extent, is conducive to Li under low temperature environment
+motion between both positive and negative polarity, thus the cryogenic property improving cell positive material.In embodiment two, the material of preparation reaches 119mAhg at-20 DEG C of low temperature environment 0.2C specific discharge capacities
-1, the cryogenic property preparing material compared with domestic market improves about 10%.
The present invention compared with CN104617296A, although be all that material with carbon element by having hole is to LiFePO
4carry out coated, but CN104617296A adopt calcium carbonate as filler, is finally dissolved removal with diluted acid.And the present invention adopts to have and the inorganic salts of direct gas-phase decomposition can carry out pore-creating, have technique simple, with low cost, the special benefits such as impurity can not be introduced, be suitable for large-scale industrial production.
Accompanying drawing explanation
Fig. 1 preparation flow schematic diagram of the present invention;
Cellular LiFePO prepared by Fig. 2 embodiment of the present invention one
4/ C normal temperature charging and discharging curve;
Cellular LiFePO prepared by Fig. 3 embodiment of the present invention one
4/ C scanning electron microscope (SEM) photograph;
Cellular LiFePO prepared by Fig. 4 embodiment of the present invention two
4/ C low temperature-20 DEG C of discharge curves;
Embodiment
Carry out clear, complete description by the technical scheme in the embodiment of the present invention below, obviously, described embodiment is a part of embodiment of the present invention, instead of whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under the prerequisite not making creative work, all belongs to the scope of protection of the invention.
The LiFePO that the present invention relates to
4for well known materials, commercially availablely can obtain, or draw with presoma sintering preparation prepared by coprecipitation.Following examples are the latter, but are not limited thereto.
Embodiment one
Take 136.2g absolute ethyl alcohol (Tianjin Sheng Ao chemical reagent Co., Ltd) to be dissolved in 136.2g deionization, pour reactor into; Take 157gLiFePO
4(1mol, 0.2um≤D
50≤ 1um), 19.4g glucose (0.098mol, because of containing a crystallization water, molecular weight is according to 198, the mole of corresponding carbon is 0.098*6=0.59mol, Tianjin the north sky medical chemistry chemical reagent work) mix with 88.2g ammonium carbonate (Tianjin Long Yu Chemical Co., Ltd.) after put into reactor, mixture fully stirs 1h.Vacuum freeze drier (Shanghai is than bright Instrument Ltd.) put into by slurry after stirring, freezes 1h at-10 DEG C, then dry 5h under vacuum 13Pa environment.The broken frustillatum of solid powder after dry is put into 100 DEG C of baking ovens, dry 1h, after oven dry under nitrogen protection atmosphere 750 DEG C sintering 2h.Be cooled to room temperature, cross 325 mesh sieves after grinding, obtain the coated LiFePO of cellular carbon
4/ C.In glove box (Lab2000 type, Etelux company), be prepared into button cell, tested 0.2C, 1C, 2C multiplying power discharging property of button cell by LAND tester (Wuhan Lan electricity electronics limited company).As shown in Figure 2, under recording target material normal temperature, 0.2C multiplying power discharging specific capacity reaches 158mAhg
-1, 1C multiplying power discharging specific capacity reaches 145mAhg
-1, 2C multiplying power discharging specific capacity reaches 140mAhg
-1.Fig. 3 is the target material electron-microscope scanning figure of preparation, can see that material surface forms comparatively multiple hole in figure.
The present invention mixes volatile ammonium salt by the coated process of carbon with carbon source, be evenly coated on LiFePO
4surface, heats after freeze drying, utilizes the effumability of ammonium salt, at LiFePO
4, after sintering, there is porous surface shape LiFePO in particle surface " pore-creating "
4/ C.The carbon of porous surface is coated can provide more passage for lithium ion, improves the high rate performance of positive electrode.
Embodiment two
Take 136.2g absolute ethyl alcohol (Tianjin Sheng Ao chemical reagent Co., Ltd) to be dissolved in 136.2g deionization, pour reactor into; Take 157gLiFePO
4(1mol, 0.2um≤D
50≤ 1um), 19.4g glucose (0.098mol, Tianjin the north sky medical chemistry chemical reagent work) puts into reactor after mixing with 88.2g carbonic hydroammonium (Tianjin Long Yu Chemical Co., Ltd.), mixture fully stirs 1h.Vacuum freeze drier (Shanghai is than bright Instrument Ltd.) put into by slurry after stirring, freezes 1h at-10 DEG C, then dry 5h under vacuum 13Pa environment.After dry, 100 DEG C of baking ovens put into by solid, dry 1h, the lower 750 DEG C of sintering 2h of nitrogen protection atmosphere.Be cooled to room temperature, cross 325 mesh sieves after grinding, obtain the coated LiFePO of cellular carbon
4/ C.Button cell is prepared in glove box (Lab2000 type, Etelux company produces).Electricity is full of by LAND tester (Wuhan Lan electricity electronics limited company) 0.2C, put into cryogenic box (Rong Xinli testing equipment Co., Ltd), shelve 10h for-20 DEG C, battery 0.2C and 0.5C multiplying power discharging specific capacity under new prestige cell tester (Xin Wei new energy technology Co., Ltd of Shenzhen) test for low temperature-20 DEG C of environment.As shown in Figure 4, record, at target material low temperature-20 DEG C, 0.2C multiplying power discharging specific capacity reaches 119mAhg
-1, 5C multiplying power discharging specific capacity reaches 90mAhg
-1.
Embodiment three
Take 24.7g absolute ethyl alcohol (Tianjin Sheng Ao chemical reagent Co., Ltd) to be dissolved in 247.6g deionization, pour reactor into; Take 157gLiFePO
4(1mol, 0.2um≤D
50≤ 1um), 19.4g glucose (0.098mol, Tianjin the north sky medical chemistry chemical reagent work) puts into reactor after mixing with 35.3g carbonic hydroammonium (Tianjin chemical reagent Co., Ltd of Jin Hui the Pacific-Asian), mixture fully stirs 1h.Vacuum freeze drier (Shanghai is than bright Instrument Ltd.) put into by slurry after stirring; 1h is freezed at-10 DEG C; then dry 5h under vacuum 13Pa environment, after dry, 100 DEG C, baking oven heating 1h put into by solid, the lower 750 DEG C of sintering 2h of nitrogen protection atmosphere.Be cooled to room temperature, cross 325 mesh sieves after grinding, obtain target product.
Embodiment four
Take 45.4g absolute ethyl alcohol (Tianjin Sheng Ao chemical reagent Co., Ltd) to be dissolved in 272.4g deionization, pour reactor into; Take 157gLiFePO
4(1mol, 0.2um≤D
50≤ 1um), 28.5g sucrose (0.083mol, Tianjin chemical reagent Co., Ltd of Jin Hui the Pacific-Asian) puts into reactor after mixing with 8.8g ammonium carbonate (Tianjin chemical reagent Co., Ltd of Jin Hui the Pacific-Asian), mixture fully stirs 1h.Vacuum freeze drier (Shanghai is than bright Instrument Ltd.) put into by slurry after stirring; 1h is freezed at-10 DEG C; then dry 5h under vacuum 13Pa environment, after dry, 100 DEG C, baking oven heating 1h put into by solid, the lower 750 DEG C of sintering 2h of nitrogen protection atmosphere.Be cooled to room temperature, cross 325 mesh sieves after grinding, obtain target product.
Unaccomplished matter of the present invention is known technology.
Claims (4)
1. a preparation method for cellular carbon-coated LiFePO 4 for lithium ion batteries positive electrode, is characterized by and comprise the following steps:
Step one: by preparation LiFePO
4be mixed to get mixture A with carbon source, get mixture A and mix obtained mixture B with volatility ammonium salt; Separately deionized water and absolute ethyl alcohol are mixed to get solution C; Finally, mixture B is mixed with solution C, is mixed with slurry;
Wherein, mol ratio is carbon: iron=0.1:1 ~ 1:1; Quality is than mixture A: volatility ammonium salt=20:1 ~ 2:1; Volume ratio deionized water: absolute ethyl alcohol=10:1 ~ 1:1; Quality is than mixture B: solution C=1:1 ~ 1:2;
Step 2: the slurry first step obtained stirs 1h ~ 2h in a kettle., stir disposed slurry and put into freeze drier, 1h ~ 2h is freezed at-50 DEG C ~-10 DEG C, then dry 2h ~ 5h under vacuo, product will be obtained and pulverize frustillatum, then baking oven is put into, 50 DEG C ~ 120 DEG C heating 1h ~ 2h;
Step 3: sintering furnace put into by material step 2 finally obtained, nitrogen atmosphere 400 DEG C ~ 750 DEG C sintering 2h ~ 4h, is cooled to room temperature, obtains the LiFePO that cellular carbon is coated
4/ C.
2. the preparation method of cellular carbon-coated LiFePO 4 for lithium ion batteries positive electrode as claimed in claim 1, it is characterized by that described carbon source is specially in glucose, sucrose, polyethylene glycol, starch and xylitol one or more.
3. the preparation method of cellular carbon-coated LiFePO 4 for lithium ion batteries positive electrode as claimed in claim 1, it is characterized by that described volatility ammonium salt is specially in ammonium carbonate, ammonium oxalate and carbonic hydroammonium one or more.
4. the preparation method of cellular carbon-coated LiFePO 4 for lithium ion batteries positive electrode as claimed in claim 1, the vacuum pressure that it is characterized by described step 2 is 1.3 ~ 13Pa.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107180957A (en) * | 2017-05-27 | 2017-09-19 | 广东烛光新能源科技有限公司 | A kind of lithium titanate anode material and preparation method thereof |
| CN107316995A (en) * | 2017-05-27 | 2017-11-03 | 广东烛光新能源科技有限公司 | A kind of anode material for lithium-ion batteries and preparation method thereof |
| CN108428859A (en) * | 2018-04-03 | 2018-08-21 | 广西睿奕新能源股份有限公司 | A method of preparing lithium thionyl chloride cell cathode |
| CN108862230A (en) * | 2018-09-18 | 2018-11-23 | 天津先众新能源科技股份有限公司 | A kind of processing method of the ultra-fine powder material of LiFePO4 |
| CN109037609A (en) * | 2018-07-03 | 2018-12-18 | 江苏乐能电池股份有限公司 | A kind of porous triple composite positive pole and preparation method thereof |
| CN109019549A (en) * | 2018-08-09 | 2018-12-18 | 芜湖彰鸿工程技术有限公司 | A kind of porous lithium ionic cell positive pole material and its preparation method and application |
| CN110165178A (en) * | 2019-05-24 | 2019-08-23 | 东莞市安德丰电池有限公司 | A kind of anode material of lithium battery and preparation method thereof and the lithium battery comprising the positive electrode |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107180957A (en) * | 2017-05-27 | 2017-09-19 | 广东烛光新能源科技有限公司 | A kind of lithium titanate anode material and preparation method thereof |
| CN107316995A (en) * | 2017-05-27 | 2017-11-03 | 广东烛光新能源科技有限公司 | A kind of anode material for lithium-ion batteries and preparation method thereof |
| CN108428859A (en) * | 2018-04-03 | 2018-08-21 | 广西睿奕新能源股份有限公司 | A method of preparing lithium thionyl chloride cell cathode |
| CN109037609A (en) * | 2018-07-03 | 2018-12-18 | 江苏乐能电池股份有限公司 | A kind of porous triple composite positive pole and preparation method thereof |
| CN109019549A (en) * | 2018-08-09 | 2018-12-18 | 芜湖彰鸿工程技术有限公司 | A kind of porous lithium ionic cell positive pole material and its preparation method and application |
| CN108862230A (en) * | 2018-09-18 | 2018-11-23 | 天津先众新能源科技股份有限公司 | A kind of processing method of the ultra-fine powder material of LiFePO4 |
| CN108862230B (en) * | 2018-09-18 | 2021-10-08 | 天津先众新能源科技股份有限公司 | Treatment method of lithium iron phosphate superfine powder material |
| CN110165178A (en) * | 2019-05-24 | 2019-08-23 | 东莞市安德丰电池有限公司 | A kind of anode material of lithium battery and preparation method thereof and the lithium battery comprising the positive electrode |
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| Publication number | Publication date |
|---|---|
| CN105576220B (en) | 2018-03-30 |
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