CN102610818B - Preparing method of anode material for composite lithium ferric phosphate cell - Google Patents
Preparing method of anode material for composite lithium ferric phosphate cell Download PDFInfo
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- CN102610818B CN102610818B CN201210094652.7A CN201210094652A CN102610818B CN 102610818 B CN102610818 B CN 102610818B CN 201210094652 A CN201210094652 A CN 201210094652A CN 102610818 B CN102610818 B CN 102610818B
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 11
- 239000002131 composite material Substances 0.000 title claims abstract description 7
- 238000000034 method Methods 0.000 title abstract description 14
- 239000010405 anode material Substances 0.000 title abstract description 7
- 239000005955 Ferric phosphate Substances 0.000 title abstract 3
- 229940032958 ferric phosphate Drugs 0.000 title abstract 3
- 229910000399 iron(III) phosphate Inorganic materials 0.000 title abstract 3
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 239000011261 inert gas Substances 0.000 claims abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000000498 ball milling Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- YNQRWVCLAIUHHI-UHFFFAOYSA-L dilithium;oxalate Chemical compound [Li+].[Li+].[O-]C(=O)C([O-])=O YNQRWVCLAIUHHI-UHFFFAOYSA-L 0.000 claims abstract description 3
- 229940062993 ferrous oxalate Drugs 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims abstract description 3
- OWZIYWAUNZMLRT-UHFFFAOYSA-L iron(2+);oxalate Chemical compound [Fe+2].[O-]C(=O)C([O-])=O OWZIYWAUNZMLRT-UHFFFAOYSA-L 0.000 claims abstract description 3
- 238000002360 preparation method Methods 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229910010710 LiFePO Inorganic materials 0.000 claims description 5
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 5
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 5
- 230000002441 reversible effect Effects 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 229910052493 LiFePO4 Inorganic materials 0.000 abstract 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 abstract 1
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 abstract 1
- 235000019837 monoammonium phosphate Nutrition 0.000 abstract 1
- 229910052698 phosphorus Inorganic materials 0.000 abstract 1
- 239000011574 phosphorus Substances 0.000 abstract 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 18
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 17
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 11
- 239000000463 material Substances 0.000 description 9
- 239000000126 substance Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000000428 dust Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 229910012820 LiCoO Inorganic materials 0.000 description 2
- 229910014689 LiMnO Inorganic materials 0.000 description 2
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 230000004087 circulation Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910015645 LiMn Inorganic materials 0.000 description 1
- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 description 1
- 229910021314 NaFeO 2 Inorganic materials 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000005030 aluminium foil Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
-
- 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
Landscapes
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a preparing method of anode material for a composite lithium ferric phosphate cell. The preparing method is characterized in that: the anode material consists of 95wt% of LiFePO4 and 5wt% of SiC, wherein the grain diameter of the SiC is greater than 50mum; the preparing method comprises the following steps: (1) mixing lithium oxalate, ammonium dihydrogen phosphate and ferrous oxalate and ball-milling, wherein the mol ratio of lithium element to iron element to phosphorus element is 1 to 1 to 1, drying and then pre-heating at 400-500 DEG C for 3-5 hours under the protection of an inner gas; (2) adding a proper amount of SiC into mixture, wherein a weight ratio of the mixture to the SiC is 19 to 1; (3) heating the mixture obtained in the step (2) in a microwave oven, adjusting the power of microwave to be 500-800W and controlling time to be 10-30min; and (4) tabletting the product obtained after roasting, and roasting at a temperature of 300-500 DEG C for 10-15 hours under the protection of inert gases. The preparing method disclosed by the invention overcomes the shortages in the existing technology, including long synthesis period, high energy consumption and the like; and meanwhile, through the preparing method, the electrochemical performances such as reversible capacity, cycle performance and high-magnification performance of the lithium ferric phosphate in the anode material for a lithium ion cell are improved.
Description
Technical field
The present invention relates to a kind of cell positive material and preparation method thereof, relate in particular to a kind of preparation method of composite phosphate lithium iron battery positive electrode.
Background technology
Lithium ion battery is within 1991, to start commercial mechanism of new electrochemical power sources, have that energy density is high, operating voltage is high, load characteristic is good, charging rate is fast, have extended cycle life, the advantage such as safety non-pollution, be widely used at present portable electric appts, annual production increases very fast.
At present, the positive electrode that is mainly used in lithium ion battery is embedding lithium transition-metal oxide, research the earliest be to there is α-sodium ferrite (α-NaFeO
2) the cobalt acid lithium (LiCoO of type layer structure
2), lithium nickelate (LiNiO
2), LiMn2O4 (LiMnO
2) and there is the spinel lithium manganate (LiMn of spinel structure
2o
4) and their doped compound.The LiCoO of layer structure wherein
2the positive electrode of developing the earliest, although its stable performance, easily preparation, good reversibility, toxicity is larger and expensive, thereby application is restricted.LiNiO
2because it synthesizes difficulty and compares LiCoO
2worsely overcharge safety problem and limited its application.People expect stratiform LiMnO
2although there is very high embedding lithium capacity, its crystal structure in charge and discharge process easily subsides and to spinelle transformation of configuration, causes charge/discharge capacity to decline, and cyclicity is very poor, has restricted its practical application.
Carborundum (SiC) has another name called diamond dust or fire sand, and its hardness is very large, has good heat conduction and electric conductivity, can be anti-oxidant during high temperature.
At present the synthetic method of lithium battery has the synthetic methods such as hydrothermal synthesis method, liquid-phase coprecipitation, sol-gel process, although can synthesize granularity compared with homogeneous, LiFePO that particle diameter is more tiny
4material powder, has shortened Li
+the evolving path, but not obvious to the improvement of material electric conductivity, and said method also exists the shortcomings such as or technique high to equipment requirement is more complicated, is difficult for carrying out industrialization production.
Adopt the method for simple doping carbon also commonplace, carbon black consumption is more, due to the density ratio LiFePO of carbon black
4much smaller, thereby can reduce significantly the real density of material, thereby also reduced volumetric specific energy and the volumetric specific power of material; And directly metal dust sedimentation easily occurs the technical process of doping metals powder method, there is a top-down concentration gradient in metal dust, makes metal dust at LiFePO
4skewness in material, thus the electrical property of material affected.
Summary of the invention
The invention provides a kind of preparation method of composite phosphate lithium iron battery positive electrode, for improving the chemical property of anode material for lithium-ion batteries LiFePO 4, mainly improve reversible capacity, cycle performance and high rate capability.
Composite phosphate lithium iron battery positive electrode of the present invention is by the LiFePO of 95wt%
4form with the SiC of 5wt%, wherein the particle diameter of SiC is greater than 50 μ m, according to following steps, carries out:
(1), by lithium oxalate, phosphoric acid dihydro amine and ferrous oxalate mixing and ball milling, the mol ratio of described lithium, iron and P elements is 1: 1: 1, dry after under inert gas shielding 400-500 ℃ of preheating 3-5 hour;
(2) in above-mentioned mixture, add appropriate SiC, the weight ratio of described mixture and SiC is 19:1;
(3) mixture step (2) being obtained is heating in microwave oven, and microwave power is adjusted to 500-800W, and the control time is 10-30 minute;
(4) by the product compressing tablet after microwave heating, under inert gas shielding, carry out roasting, sintering temperature is 300-500 ℃, roasting time is 10-15 hour.
In embodiment further, the particle diameter of described SiC is preferably 100 μ m; The preheat temperature of described step (1) is preferably 400 ℃; The preferably 4 hours warm-up time of described step (1); Described microwave power is preferably adjusted to 800W; It is 10 minutes that the time of described step (3) is preferably controlled; Described sintering temperature is preferably 400 ℃; Described roasting time is preferably 10 hours; Described inert gas is a kind of in nitrogen, argon gas or hydrogen-argon-mixed body.
Synthesis cycle length, energy that technical solution of the present invention has overcome prior art consume the shortcomings such as high, improve the chemical property of LiFePO 4 in anode material for lithium-ion batteries, as reversible capacity, cycle performance and high rate capability simultaneously.
In addition, due to the increase along with silicon-carbide particle size, its electric conductivity also increases.Preferred dimension of the present invention is greater than 50 μ m, is especially of a size of the SiC of 100 μ m as raw material, improves greatly the chemical property of anode material of lithium battery.
Accompanying drawing explanation
Fig. 1 is LiFePO
4/ SiC sample a(SiC is 50 μ m) and pure LiFePO
4specific discharge capacity comparison diagram under 0.1C current density;
Fig. 2 is LiFePO
4/ SiC sample b(SiC is 100 μ m) and the specific discharge capacity comparison diagram of sample a under 0.1C current density.
Embodiment
Below in conjunction with figure and specific embodiment the invention will be further described:
Abscissa in Fig. 1-2 is the number of times recycling, and ordinate is specific discharge capacity (mAh/g).The LiFePO preparing according to the method for embodiment 1-2
4/ SiC sample a, b, and by both and pure LiFePO
4compare: in Fig. 1, that square curve description is carbon encapsulated material LiFePO
4the chemical property of/SiC sample a, that circle point curve is described is pure LiFePO
4chemical property.The initial capacity of sample a is 135mAh/g, far away higher than pure LiFePO
4119mAh/g.After 40 circulations, the capacity of sample a still remains on 125mAh/g.In Fig. 2, that square curve description is carbon encapsulated material LiFePO
4the chemical property of/SiC sample b, what circle point curve was described is the chemical property of sample a.The initial capacity that can see sample b under 0.1C current density by Fig. 2, slightly far above sample a, is 145mAh/g, and after 40 circulations, the capacity of sample b still remains on 135 mAh/g.
In battery is made, according to usual way.As the polytetrafluoroethylene (PTFE) of 70% this positive electrode of weight ratio percentage, 20% acetylene black and 10% is dissolved in solvent absolute ethyl alcohol and forms slurry.Slurry is evenly coated on aluminium foil, and the thickness of coating is about 80 μ m, and it is 1cm that the electrode slice coating is cut into area
2work electrode, at 85 ℃, vacuumize 12h is standby.Test battery adopts conventional button cell, take metallic lithium foil as to electrode, and the EC-DMC of the LiPF6 of 1mol/L (volume ratio is 1: 1) solution is electrolyte, at drying room, is assembled.Charge-discharge test adopts current constant mode to carry out, and discharging and recharging cut-ff voltage is 2.0 ~ 4.5V.
Embodiment 1
By 0.7438gLi
2cO
3, 3.5966gFeC
2o
4.
2h
2o and 2.3234gNH
4h
2pO
4mixing and ball milling; after dry, put into the lower 400 ℃ of preheatings of tube furnace nitrogen protection 4 hours; to adding 0.35g SiC(particle diameter in the mixture after preheating, be 50 μ m); put into microwave oven and heat, regulate microwave power to 800W, control generated time is 10min; cooling; grind, by the product compressing tablet after roasting, then put into 400 ℃ of roastings of tube furnace nitrogen protection 10 hours.
Embodiment 2
By 0.7438gLi
2cO
3, 3.5966gFeC
2o
4.
2h
2o and 2.3234gNH
4h
2pO
4mixing and ball milling; after dry, put into the lower 400 ℃ of preheatings of tube furnace nitrogen protection 4 hours; to adding 0.35g SiC(particle diameter in the mixture after preheating, be 100 μ m); put into microwave oven and heat, regulate microwave power to 800W, control generated time is 10min; cooling; grind, by the product compressing tablet after roasting, then put into 400 ℃ of roastings of tube furnace nitrogen protection 10 hours.
Above specific embodiments of the invention be have been described in detail, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and alternative also all among category of the present invention.Therefore, equalization conversion and the modification done without departing from the spirit and scope of the invention, all should contain within the scope of the invention.
Claims (8)
1. a preparation method for composite phosphate lithium iron battery positive electrode, is characterized in that, by the LiFePO of 95wt%
4form with the SiC of 5wt%, wherein the particle diameter of SiC is 100 μ m, according to following steps, carries out:
(1), by lithium oxalate, phosphoric acid dihydro amine and ferrous oxalate mixing and ball milling, the mol ratio of described lithium, iron and P elements is 1: 1: 1, dry after under inert gas shielding 400-500 ℃ of preheating 3-5 hour;
(2) in above-mentioned mixture, add appropriate SiC, the weight ratio of described mixture and SiC is 19:1;
(3) mixture step (2) being obtained heats in microwave oven, and microwave power is adjusted to 500-800W, and the control time is 10-30 minute;
(4) by the product compressing tablet after microwave heating, under inert gas shielding, carry out roasting, sintering temperature is 300-500 ℃, roasting time is 10-15 hour.
2. preparation method according to claim 1, is characterized in that, the preheat temperature of described step (1) is 400 ℃.
3. preparation method according to claim 1, is characterized in that, be 4 hours the warm-up time of described step (1).
4. preparation method according to claim 1, is characterized in that, described microwave power is adjusted to 800W.
5. preparation method according to claim 1, is characterized in that, it is 10 minutes that the time of described step (3) is controlled.
6. preparation method according to claim 1, is characterized in that, described sintering temperature is 400 ℃.
7. preparation method according to claim 1, is characterized in that, described roasting time is 10 hours.
8. preparation method according to claim 1, is characterized in that, described inert gas is a kind of in nitrogen, argon gas or hydrogen-argon-mixed body.
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|---|---|---|---|
| CN201210094652.7A CN102610818B (en) | 2012-04-01 | 2012-04-01 | Preparing method of anode material for composite lithium ferric phosphate cell |
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|---|---|---|---|
| CN201210094652.7A CN102610818B (en) | 2012-04-01 | 2012-04-01 | Preparing method of anode material for composite lithium ferric phosphate cell |
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|---|---|---|---|---|
| CN1925195A (en) * | 2006-09-30 | 2007-03-07 | 天津大学 | Anode material for lithium ion battery and method for making same |
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| US7781100B2 (en) * | 2005-05-10 | 2010-08-24 | Advanced Lithium Electrochemistry Co., Ltd | Cathode material for manufacturing rechargeable battery |
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Effective date of registration: 20170914 Address after: No. 2 C-2 Du Ruan Zhen Long Xi industrial zone Pengjiang District Guangdong city Jiangmen province two 529075 Patentee after: Jiangmen Shun Ye Technology Industrial Co. Ltd. Address before: 312365 Zhejiang Province, Shaoxing city Shangyu District Songxia Town City Station International Plaza building 36 unit room 1-101 Patentee before: Zhejiang Hongsheng Technology Transfer Services Ltd. |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20141119 Termination date: 20180401 |