CN102664261A - Method for preparing high-conductivity lithium ion battery cathode material - Google Patents
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- CN102664261A CN102664261A CN2012101513922A CN201210151392A CN102664261A CN 102664261 A CN102664261 A CN 102664261A CN 2012101513922 A CN2012101513922 A CN 2012101513922A CN 201210151392 A CN201210151392 A CN 201210151392A CN 102664261 A CN102664261 A CN 102664261A
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Abstract
The invention relates to a method for preparing a high-conductivity lithium ion battery cathode material and is characterized by comprising the following steps of dissolving soluble phosphate and ferric salt in deionized water in a molar ratio of Li to Fe of 1:1 and preparing a ferrous phosphate material coated with surface silver according to the silver mirror reaction principle of glucose. According to the method, glucose plays a role of a carbon source in the reaction process, and serves as an important raw material in the silver mirror reaction; and the ferrous phosphate material is relatively high in conductivity, rate performance and cycling stability.
Description
Technical field
The present invention relates to a kind of preparation method of high conductivity anode material for lithium-ion batteries, belong to the anode material for lithium-ion batteries technical field.
Background technology
The performance of lithium ion battery depends on used positive electrode to a great extent, and positive electrode selects whether appropriately directly to affect each item index of lithium ion battery.The tradition anode material for lithium-ion batteries mainly is the transition metal oxide material, mix valence state because transition metal oxide exists, so they all has more satisfactory electronic conductivity.At present, the more transition metal oxide positive electrode of research mainly comprises LiCoO
2, LiNiO
2, LiNi
1/3Co
1/3Mn
1/3O
2And LiMn
2O
4Etc. several kinds.
In recent years, one type of positive electrode with polyanion type structure has caused people's extensive concern.Wherein, LiFePO 4 (LiFePO
4) be the positive electrode that people know the earliest with polyanion type structure; Because of it has stable structure, higher specific capacity, cheap price and advantage such as environmentally friendly causes showing great attention to of people, be considered to present optimal power lithium-ion battery positive electrode.At LiFePO
4In the material structure, bigger phosphate anion has substituted the oxonium ion in the traditional metal oxide type positive electrode, has improved LiFePO on the one hand
4The structural stability of material, and then improved the cyclical stability of material.But, but increased the distance between the metallic iron ion on the one hand in addition, reduced LiFePO
4Electronic conductivity.
At present, to LiFePO
4The problem that conductivity is lower, mainly surface carbon coats the researcher and the preparation composite material solves through it is carried out.Patent CN102088079, CN102013478 etc. disclose a kind of preparation method of carbon cladded ferrous lithium phosphate; Though carbon coats the conductivity that can improve LiFePO 4 to a certain extent; But also reduced the tap density of this material simultaneously, and then had influence on its energy density; Patent CN101891179 and CN102034980 disclose and have a kind ofly prepared the method for lithium ferrous phosphate composite material with the metal simple-substance aluminium powder, but this procedure is comparatively complicated, and conductivity improves limited; Patent CN101339988 discloses a kind of preparation method who coats copper on the LiFePO 4 surface, but higher owing to anodal current potential, causes the easy oxidation of copper, is not suitable for business-like application.
Given this, this patent will utilize glucose silver mirror reaction principle through simple preparation technology, prepare silver-colored cladded ferrous lithium phosphate positive electrode.Patent searching does not also have discovery to prepare the related patent U.S. Patent No. of silver-colored cladded ferrous lithium phosphate material through the former lithium of silver mirror reaction.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of high conductivity anode material for lithium-ion batteries; It utilizes the silver mirror reaction principle of glucose; Prepare the ferrousphosphate lithium material with surface silver coating, glucose had both played the effect of carbon source in course of reaction, also was the important source material of silver mirror reaction simultaneously; Conductivity of electrolyte materials is higher, is very beneficial for improving the high rate performance and the cyclical stability of ferrousphosphate lithium material.
Technical scheme of the present invention is achieved in that a kind of preparation method of high conductivity anode material for lithium-ion batteries, it is characterized in that the preparation method, and concrete steps are following:
A) soluble phosphate, Fe salt are dissolved in the deionized water according to mol ratio Li:Fe=1:1, are mixed with A solution, the A solution concentration is 3 ~ 6mol/L;
B) liquor argenti nitratis ophthalmicus with 4 ~ 5% concentration splashes in the ammonia spirit of 15 ~ 35% concentration, forms silver ammino solution, is called B solution at this;
C) A solution is slowly splashed in the B solution, regulate pH value scope to 9 ~ 9.7, form C solution; The mol ratio of the silver in said Fe salt and the said liquor argenti nitratis ophthalmicus is Fe:Ag=(20 ~ 76): 1;
D) glucose solution with concentration 21.5 ~ 35% slowly splashes in the C solution, and the molar ratio range of the silver described in glucose and the step b) in the liquor argenti nitratis ophthalmicus is (1 ~ 1.5): 1, and then 80 ~ 90
oCarry out magnetic agitation under the temperature of C, until forming precursor;
E) precursor is put into the tube furnace that is connected with inert gas shielding and carry out the preliminary treatment sintering, the pretreatment temperature scope is 300 ~ 450
oC, pretreatment time is 3 ~ 4 hours, obtains the preliminary treatment powder;
F) above-mentioned preliminary treatment powder is carried out sintering once more in being connected with the tube furnace of inert gas shielding, control heating rate 10 ~ 15
oC/min, sintering temperature 700 ~ 800
oC, sintering time 6 ~ 10 hours, cooling method are with the stove cooling, can obtain silver-colored cladded ferrous lithium phosphate material;
Described phosphate is lithium dihydrogen phosphate;
Described Fe salt comprises ferric nitrate, ferric acetate and ferric oxalate;
Described inert gas comprises argon gas, nitrogen, or two kinds mist.
Good effect of the present invention is: utilize the silver mirror reaction principle of glucose, prepare the ferrousphosphate lithium material with surface silver coating, this material electric conductivity is higher, and silver exists with metallic forms, and is evenly distributed; Glucose had both played the effect of carbon source in course of reaction, also be the important source material of silver mirror reaction simultaneously; Adopt the synthetic LiFePO 4 good rate capability of this method, cycle performance excellence.
Description of drawings
Fig. 1 is the charging and discharging curve collection of illustrative plates of 3.3wt% silver cladded ferrous lithium phosphate material in the instance 1 of the present invention;
Fig. 2 is the cycle performance collection of illustrative plates of 1.3wt% silver cladded ferrous lithium phosphate material in the instance 2 of the present invention.
Fig. 3 is the XRD figure spectrum of 0.9wt% silver cladded ferrous lithium phosphate material in the instance 3 of the present invention.
Fig. 4 is the SEM collection of illustrative plates of 0.9wt% silver cladded ferrous lithium phosphate material in the instance 3 of the present invention.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is described further:
Embodiment 1
With lithium dihydrogen phosphate and ferric nitrate in molar ratio the ratio of Li:Fe=1:1 be dissolved in the proper amount of deionized water, be mixed with the solution that concentration is 3mol/L; With concentration be 5% liquor argenti nitratis ophthalmicus to splash into concentration be in 20% the ammonia spirit, form silver ammino solution; The ratio of above-mentioned 3 mol/L solution according to Fe:Ag=20:1 slowly splashed in the silver ammino solution, through ammoniacal liquor the pH value of solution is adjusted to 9.5 then; With concentration be 30% glucose solution slowly to splash into above-mentioned pH value be 9.5 solution, control glucose is 1:1 with the mol ratio of silver, then 80
oCarry out magnetic agitation under the C, form precursor; After precursor simply ground, put into the tube furnace that is connected with argon shield and carry out sintering, sintering temperature is 300
oC, sintering time is 4 hours, obtains the preliminary treatment powder; The preliminary treatment powder is carried out sintering again in being connected with the tube furnace of argon shield, sintering temperature is 700
oC (heating rate 10
oC/min), sintering time is 10 hours, adopts with the mode of stove cooling and lowers the temperature, and can obtain 3.3wt% silver cladded ferrous lithium phosphate material.Fig. 1 is that this material is interval at 2.7 ~ 4.2V, the charging and discharging curve of half-cell under the 2C multiplying power.The initial charge capacity of material is 119mAhg
-1, discharge capacity is 116mAhg
-1, efficiency for charge-discharge is higher, and high rate performance is better.
Embodiment 2
With lithium dihydrogen phosphate and ferric acetate in molar ratio the ratio of Li:Fe=1:1 be dissolved in the proper amount of deionized water, be mixed with the solution that concentration is 3.5mol/L; With concentration be 4% liquor argenti nitratis ophthalmicus to splash into concentration be in 15% the ammonia spirit, form silver ammino solution; The ratio of above-mentioned 3.5 mol/L solution according to Fe:Ag=50:1 slowly splashed in the silver ammino solution, through ammoniacal liquor the pH value of solution is adjusted to 9 then; With concentration is that slowly to splash into above-mentioned pH value be that control glucose is 1.2:1 with the mol ratio of silver, then 85 in 9 the solution for 35% glucose solution
oCarry out magnetic agitation under the C, form precursor; After precursor ground, put into the tube furnace that is connected with argon shield and carry out sintering, sintering temperature is 350
oC, sintering time is 3 hours, obtains the preliminary treatment powder; The preliminary treatment powder is carried out sintering again in being connected with the tube furnace of nitrogen protection, sintering temperature is 800
oC (heating rate 15
oC/min), sintering time is 6 hours, adopts with the mode of stove cooling and lowers the temperature, and can obtain 1.3wt% silver cladded ferrous lithium phosphate material.Fig. 2 is that this material is interval at 2.7 ~ 4.2V, the cycle performance curve of half-cell under the 1C multiplying power.Can find out material first discharge capacity be 146mAhg
-1, 30 times circulation back capacity still can remain on 144mAhg
-1, capability retention 99%, cycle performance is better.
Embodiment 3
With lithium dihydrogen phosphate and ferric nitrate in molar ratio the ratio of Li:Fe=1:1 be dissolved in the deionized water, be mixed with the solution that concentration is 6mol/L; With concentration be 4.5% liquor argenti nitratis ophthalmicus to splash into concentration be in 35% the ammonia spirit, form silver ammino solution; The ratio of above-mentioned 4.5 mol/L solution according to Fe:Ag=76:1 splashed in the silver ammino solution, through ammoniacal liquor the pH value of solution is adjusted to 9.7 then; With concentration is that slowly to splash into above-mentioned pH value be that control glucose is 1.5:1 with the mol ratio of silver, then 90 in 9.7 the solution for 21.5% glucose solution
oStir under the C, form precursor; After precursor ground, put into the tube furnace that is connected with argon gas and nitrogen (volume ratio is 1:1) mist and carry out sintering, sintering temperature is 320
oC, sintering time is 4 hours, obtains the preliminary treatment powder; The preliminary treatment powder is carried out sintering in being connected with the tube furnace of argon shield, sintering temperature is 720
oC (heating rate 12
oC/min), sintering time is 7 hours, adopts with the mode of stove cooling and lowers the temperature, and can obtain 0.9wt% silver cladded ferrous lithium phosphate material.Fig. 3 is that material is 10 ~ 60
oXRD figure spectrum in the scope, as can be seen from the figure material is consistent with the XRD figure spectrum of pure phase ferrousphosphate lithium material, and the reason of not seeing metal A g diffraction maximum is because the content of metal A g is less.Fig. 4 is that this material is 5000 o'clock scanning electron microscope diagram spectrum in multiplication factor.
Embodiment 4
With lithium dihydrogen phosphate and ferric oxalate in molar ratio the ratio of Li:Fe=1:1 be dissolved in the proper amount of deionized water, be mixed with the solution that concentration is 3mol/L; With concentration be 5% liquor argenti nitratis ophthalmicus to splash into concentration be in 20% the ammonia spirit, form silver ammino solution; The ratio of above-mentioned 3 mol/L solution according to Fe:Ag=20:1 slowly splashed in the silver ammino solution, through ammoniacal liquor the pH value of solution is adjusted to 9.5 then; With concentration be 30% glucose solution slowly to splash into above-mentioned pH value be 9.5 solution, control glucose is 1:1 with the mol ratio of silver, then 80
oCarry out magnetic agitation under the C, form precursor; After precursor simply ground, put into the tube furnace that is connected with argon shield and carry out sintering, sintering temperature is 300
oC, sintering time is 4 hours, obtains the preliminary treatment powder; The preliminary treatment powder is carried out sintering again in being connected with the tube furnace of argon shield, sintering temperature is 700
oC (heating rate 10
oC/min), sintering time is 10 hours, adopts with the mode of stove cooling and lowers the temperature, and can obtain 3.3wt% silver cladded ferrous lithium phosphate material.
Claims (4)
1. the preparation method of a high conductivity anode material for lithium-ion batteries is characterized in that the preparation method, and concrete steps are following:
A) soluble phosphate, Fe salt are dissolved in the deionized water according to mol ratio Li:Fe=1:1, are mixed with A solution, the A solution concentration is 3 ~ 6mol/L;
B) liquor argenti nitratis ophthalmicus with 4 ~ 5% concentration splashes in the ammonia spirit of 15 ~ 35% concentration, forms silver ammino solution, is called B solution at this;
C) A solution is slowly splashed in the B solution, regulate pH value scope to 9 ~ 9.7, form C solution; The mol ratio of the silver in said Fe salt and the said liquor argenti nitratis ophthalmicus is Fe:Ag=(20 ~ 76): 1;
D) glucose solution with concentration 21.5 ~ 35% slowly splashes in the C solution, and the molar ratio range of the silver described in glucose and the step b) in the liquor argenti nitratis ophthalmicus is (1 ~ 1.5): 1, and then 80 ~ 90
oCarry out magnetic agitation under the temperature of C, until forming precursor;
E) precursor is put into the tube furnace that is connected with inert gas shielding and carry out the preliminary treatment sintering, the pretreatment temperature scope is 300 ~ 450
oC, pretreatment time is 3 ~ 4 hours, obtains the preliminary treatment powder;
F) above-mentioned preliminary treatment powder is carried out sintering once more in being connected with the tube furnace of inert gas shielding, control heating rate 10 ~ 15
oC/min, sintering temperature 700 ~ 800
oC, sintering time 6 ~ 10 hours, cooling method are with the stove cooling, can obtain silver-colored cladded ferrous lithium phosphate material.
2. according to the preparation method of a kind of high conductivity anode material for lithium-ion batteries described in the claim 1, it is characterized in that described phosphate is lithium dihydrogen phosphate.
3. according to the preparation method of a kind of high conductivity anode material for lithium-ion batteries described in the claim 1, it is characterized in that described Fe salt comprises ferric nitrate, ferric acetate and ferric oxalate.
4. according to the preparation method of a kind of high conductivity anode material for lithium-ion batteries described in the claim 1, it is characterized in that described inert gas comprises argon gas, nitrogen, or two kinds mist.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103413942A (en) * | 2013-07-30 | 2013-11-27 | 中国第一汽车股份有限公司 | Preparation method for low-cost high-electrical conductivity lithium ion battery positive pole material |
| CN107093710A (en) * | 2017-03-31 | 2017-08-25 | 宁夏博尔特科技有限公司 | Two-coat lithium ion battery negative material and preparation method thereof and lithium ion battery |
| CN107359343A (en) * | 2017-07-28 | 2017-11-17 | 南京理工大学 | The preparation method of one species spiral shape silver nanochains conductor bridging modified phosphate iron lithium composite material |
| CN108270005A (en) * | 2018-01-19 | 2018-07-10 | 河北力滔电池材料有限公司 | Iron lithium phosphate compound anode pole piece and preparation method thereof |
| CN108390054A (en) * | 2018-03-07 | 2018-08-10 | 南京理工大学 | The preparation method of four-prism shape LiFePO4/silver/graphene oxide ternary composite electrode material |
| CN108539179A (en) * | 2018-04-28 | 2018-09-14 | 河南工业大学 | Phosphoric acid vanadium lithium combination electrode material and the preparation method and application thereof |
| CN112038629A (en) * | 2020-09-30 | 2020-12-04 | 合肥国轩高科动力能源有限公司 | Integrated high-rate lithium iron phosphate positive electrode material and preparation method and application thereof |
| CN113130891A (en) * | 2021-04-16 | 2021-07-16 | 中国工程物理研究院电子工程研究所 | Thermal battery composite cathode material and preparation method thereof |
| CN115775883A (en) * | 2023-02-13 | 2023-03-10 | 四川富临新能源科技有限公司 | Surface modification method of lithium iron phosphate anode material |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103413942A (en) * | 2013-07-30 | 2013-11-27 | 中国第一汽车股份有限公司 | Preparation method for low-cost high-electrical conductivity lithium ion battery positive pole material |
| CN107093710B (en) * | 2017-03-31 | 2019-10-08 | 宁夏博尔特科技有限公司 | Two-coat lithium ion battery negative material and preparation method thereof and lithium ion battery |
| CN107093710A (en) * | 2017-03-31 | 2017-08-25 | 宁夏博尔特科技有限公司 | Two-coat lithium ion battery negative material and preparation method thereof and lithium ion battery |
| CN107359343A (en) * | 2017-07-28 | 2017-11-17 | 南京理工大学 | The preparation method of one species spiral shape silver nanochains conductor bridging modified phosphate iron lithium composite material |
| CN107359343B (en) * | 2017-07-28 | 2020-06-19 | 南京理工大学 | Preparation method of spiral-like silver nanochain conductor bridged modified lithium iron phosphate composite material |
| CN108270005A (en) * | 2018-01-19 | 2018-07-10 | 河北力滔电池材料有限公司 | Iron lithium phosphate compound anode pole piece and preparation method thereof |
| CN108270005B (en) * | 2018-01-19 | 2020-06-09 | 河北力滔电池材料有限公司 | Lithium iron phosphate composite positive pole piece and preparation method thereof |
| CN108390054A (en) * | 2018-03-07 | 2018-08-10 | 南京理工大学 | The preparation method of four-prism shape LiFePO4/silver/graphene oxide ternary composite electrode material |
| CN108539179A (en) * | 2018-04-28 | 2018-09-14 | 河南工业大学 | Phosphoric acid vanadium lithium combination electrode material and the preparation method and application thereof |
| CN108539179B (en) * | 2018-04-28 | 2020-11-20 | 河南工业大学 | Lithium vanadium phosphate composite electrode material and preparation method and application thereof |
| CN112038629A (en) * | 2020-09-30 | 2020-12-04 | 合肥国轩高科动力能源有限公司 | Integrated high-rate lithium iron phosphate positive electrode material and preparation method and application thereof |
| CN112038629B (en) * | 2020-09-30 | 2022-07-05 | 合肥国轩高科动力能源有限公司 | Integrated high-rate lithium iron phosphate positive electrode material and preparation method and application thereof |
| CN113130891A (en) * | 2021-04-16 | 2021-07-16 | 中国工程物理研究院电子工程研究所 | Thermal battery composite cathode material and preparation method thereof |
| CN115775883A (en) * | 2023-02-13 | 2023-03-10 | 四川富临新能源科技有限公司 | Surface modification method of lithium iron phosphate anode material |
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