CN102157736A - Ferrous disulfide/carbon composite cathode material of primary lithium battery and preparation method and application thereof - Google Patents
Ferrous disulfide/carbon composite cathode material of primary lithium battery and preparation method and application thereof Download PDFInfo
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- CN102157736A CN102157736A CN2011100709029A CN201110070902A CN102157736A CN 102157736 A CN102157736 A CN 102157736A CN 2011100709029 A CN2011100709029 A CN 2011100709029A CN 201110070902 A CN201110070902 A CN 201110070902A CN 102157736 A CN102157736 A CN 102157736A
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Abstract
The invention discloses a ferrous disulfide/carbon composite cathode material of primary lithium battery, wherein the mass percentage of ferrous disulfide is 50-99.5 percent, and the mass percentage of carbon is 0.5-50 percent. The preparation method comprises the steps of: (1) mixing a carbon source material with dispersant in mass ratio of 1:(20-120) to obtain suspension; adding pyrite to the suspension, wherein the mass ratio of the pyrite to the carbon source is (90-99.5):(0.5-10), then mixing for 1-10h to obtain mixed paste; and (2), heating the mixed paste obtained from the step 1 to reach the temperature of 50-150 DEG C under the protection of an inert gas, keeping the temperature for 1-40h, then heating to reaching the temperature of 250-400 DEG C, keeping the temperature for 1-20h, then cooling to the room temperature, and obtaining granular ferrous disulfide/carbon composite cathode material of the primary lithium battery through ball-milling and sieving. The invention has the advantage that the battery prepared by the composite cathode material has higher large-current discharge performance and remarkably improved discharge plateau potential.
Description
Technical field
The present invention relates to a kind of primary cell electrode material, especially relate to a kind of disposable lithium-battery ferrous disulfide/carbon composite anode material and its production and application.
Background technology
Battery of lithium-iron disulphide be by ferrous disulfide as positive electrode, lithium metal is as negative material, the lithium battery that uses organic bath to form.Lithium-ferrous disulfide primary cell is the room temperature discharge battery, and its rated voltage is 1.5 V, and this is complementary with present employed general electrical appliance, can directly replace 1.5 traditional V aqueous solution batteries (as Zn/HgO, Zn/Ag
2O, Zn/MnO
2Battery etc.).Its positive electrode ferrous disulfide has very excellent characteristic, solubility is less in organic bath, and can keep its electrochemical reaction activity, single step of releasing electric theory specific capacity is up to 894 mAh/g, its negative pole lithium metal has lower standard electrode EMF (3.05 V), and its theoretical specific capacity value is also up to 3860 mA/g; Therefore battery of lithium-iron disulphide has high energy density, high-power characteristic and long storage time preferably, on compact electric apparatus such as digital camera, toy car, remote-control toy, shaver, medicine equipment, army's communication even more important using value is arranged all.In addition, ferrous disulfide is nontoxic environment-friendly material, its raw material pyrite aboundresources.
Anode material of lithium-iron disulphide battery is general direct to be made through removal of impurities and pulverizing by natural pyrite, and resulting ferrous disulfide material conductivity is not high, and effective ratio area is relatively low, and prepared battery discharge efficient is not high, and the heavy-current discharge characteristic is not good enough.
Summary of the invention
Technical problem to be solved by this invention provides a kind of heavy-current discharge characteristic disposable lithium-battery ferrous disulfide/carbon composite anode material and preparation method preferably, and the disposable lithium-battery positive pole and the disposable lithium-battery that provide positive electrode thus to make.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: disposable lithium-battery ferrous disulfide/carbon composite anode material, the mass percentage content that it is characterized in that ferrous disulfide in this ferrous disulfide/carbon composite anode material is 50～99.5%, and the mass percentage content of carbon is 0.5～50%.
The mass percentage content of described ferrous disulfide is 95～98%, and the mass percentage content of carbon is 2～5%.
The preparation method of disposable lithium-battery ferrous disulfide/carbon composite anode material has following steps:
(1) carbon source material and dispersant are the mixed of 1:15～120 by mass ratio after, obtain suspension-turbid liquid; Pyrite is joined in the suspension-turbid liquid, and wherein the mass ratio of pyrite and carbon source material is (90 ~ 99.5): (0.5 ~ 10), and stir and obtain mixing pastel after 1～10 hour;
(2) the mixing pastel that step (1) is obtained is heated to 50～150 ℃ under inert gas shielding, keeps after 1～40 hour; Be heated to 250～400 ℃ again, kept 1～20 hour, be cooled to room temperature then, obtain granular disposable lithium-battery ferrous disulfide/carbon composite anode material with sieving by ball milling.
The carbon source material that obtains in the step (1) is carried out ultrasonic dispersion with the suspension-turbid liquid that mixes of dispersant, and ultrasonic power is 300～800 watts, keeps 1～5 hour.
The pyrite average grain diameter is 10 ~ 30 microns, the mass percentage content of ferrous disulfide is not less than 95% in the pyrite, Fe element mass percentage content must not be lower than 43%, S element mass percentage content must not be lower than 49%, the water-soluble iron mass percentage content is not higher than 1.0%, the mass percentage content of sulfate ion is not higher than 1.0%, and pyrite and water are by mass ratio 1:(5～20) mix the back form mix suspension-turbid liquid supernatant liquor pH value between 4.0 ~ 8.0.
Dispersant is at least a of water, ethanol, methyl alcohol, acetone and N-methyl pyrrolidone.
Carbon source material is at least a in carbon black, acetylene black, active carbon, mesoporous carbon, carbon nano-tube, graphene film, glucose, sucrose, starch and the p-aminobenzoic acid.
The ball milling time in the step (2) is 1～10 hour, sieves and adopts 160～200 mesh sieves; Inert gas is for flowing atmosphere, and air velocity is 1～15 liter/minute, and inert gas is at least a in nitrogen and the argon gas.
The disposable lithium-battery positive pole comprises disposable lithium-battery ferrous disulfide/carbon composite anode material.
Disposable lithium-battery comprises the disposable lithium-battery positive pole.
Compared with prior art, the invention has the advantages that the use of ferrous disulfide/carbon composite can improve the electron conduction of positive electrode, increase the passage of electron transport, reduce the resistance of electron transport, help improving the efficient that transports of electronics, can effectively improve the discharging efficiency of positive electrode.Simultaneously, can increase the effective ratio area of positive electrode by heat treatment and carbon source material in the expansion of heat treatment process, the imbibition effect of material is improved significantly.Therefore, the discharging efficiency of positive electrode active materials is improved, and plants the preparation-obtained battery of composite material thus and has better heavy-current discharge characteristic, and the discharge platform current potential significantly improves.
Description of drawings
Fig. 1 a is FeS
2Stereoscan photograph displayed map (amplifying 3500 times);
Fig. 1 b is FeS
2/ MCNTs composite positive pole stereoscan photograph displayed map (amplifying 3500 times);
Fig. 2 is FeS
2With various FeS
2/ C composite positive pole X ray diffracting spectrum;
Fig. 3 is FeS
2And various FeS
2The battery 1000 mA continuous discharge curve ratio that/C composite positive pole is made are: a:FeS
2, b:FeS
2/ MCNTs, c:FeS
2/ AC, d:FeS
2/ CB, e:FeS
2/ GC.
Embodiment
Embodiment describes in further detail the present invention below in conjunction with accompanying drawing.
Embodiment one: disposable lithium-battery ferrous disulfide/carbon composite anode material, and the mass percentage content of ferrous disulfide is 55% in this ferrous disulfide/carbon composite anode material, the mass percentage content of carbon is 45%.
The preparation method of disposable lithium-battery ferrous disulfide/carbon composite anode material has following steps:
(1) carbon black (being abbreviated as CB) or acetylene black and water are the mixed of 1:20 by mass ratio after, obtain suspension-turbid liquid; The suspension-turbid liquid that obtains is carried out ultrasonic dispersion, and ultrasonic power is 800 watts, keeps 5 hours, pyrite is joined in the suspension-turbid liquid again, and wherein the mass ratio of pyrite and carbon black or acetylene black is 60:40, stirs and obtains mixing pastel after 8 hours; Carbon source material also can be the mixture of carbon black and acetylene black.
(2) the mixing pastel that step (1) is obtained is under 3 liters/minute the nitrogen or argon shield, to be heated to 90 ℃ in air velocity, keeps after 30 hours; Be heated to 250 ℃ again, kept 10 hours, be cooled to room temperature then, by ball milling and sieving, the ball milling time is 3 hours, sieves and adopts 170 mesh sieves, obtains granular disposable lithium-battery ferrous disulfide/carbon composite anode material.Inert gas also can be the mist of nitrogen and argon gas.
The pyrite average particle size particle size is 20 microns, the mass percentage content of ferrous disulfide is 95% in the pyrite, Fe element mass percentage content is 43%, S element mass percentage content is 49%, the water-soluble iron mass percentage content is 0.8%, and the mass percentage content of sulfate ion is 0.8%, after pyrite is water-soluble, pyrite mixes the back with water by mass ratio 1:8 and forms the mixing suspension-turbid liquid, and the supernatant liquor pH value of suspension-turbid liquid is 4.5 ± 0.2.
The disposable lithium-battery positive pole comprises disposable lithium-battery ferrous disulfide/carbon composite anode material.
Disposable lithium-battery comprises the disposable lithium-battery positive pole.
Embodiment two: disposable lithium-battery ferrous disulfide/carbon composite anode material, and the mass percentage content of ferrous disulfide is 80% in this ferrous disulfide/carbon composite anode material, the mass percentage content of carbon is 20%.
The preparation method of disposable lithium-battery ferrous disulfide/carbon composite anode material has following steps:
(1) active carbon (being abbreviated as AC) or mesoporous carbon and ethanol or methyl alcohol or acetone are the mixed of 1:40 by mass ratio after, obtain suspension-turbid liquid; The suspension-turbid liquid that obtains is carried out ultrasonic dispersion, and ultrasonic power is 600 watts, keeps 4 hours, and pyrite is joined in the suspension-turbid liquid, and wherein the mass ratio of pyrite and active carbon or mesoporous carbon is 85:15, stirs and obtains mixing pastel after 5 hours; The carbon black material can be the mixture of active carbon and mesoporous carbon, and dispersant also can be two or three mixed liquor in ethanol, methyl alcohol and the acetone.
(2) the mixing pastel that step (1) is obtained is under 8 liters/minute the nitrogen or argon shield, to be heated to 70 ℃ in air velocity, keeps after 20 hours; Be heated to 300 ℃ again, kept 5 hours, be cooled to room temperature then, by ball milling and sieving, the ball milling time is 5 hours, sieves and adopts 180 mesh sieves, obtains granular disposable lithium-battery ferrous disulfide/carbon composite anode material.Inert gas also can be the mist of nitrogen and argon gas.
The pyrite average particulate diameter is 25 microns, the mass percentage content of ferrous disulfide is 97% in the pyrite, Fe element mass percentage content is 44%, S element mass percentage content is 50%, the water-soluble iron mass percentage content is 0.5%, and the mass percentage content of sulfate ion is 0.5%, after pyrite is water-soluble, pyrite mixes the back with water by mass ratio 1:10 and forms the mixing suspension-turbid liquid, and the supernatant liquor pH value of mixing suspension-turbid liquid is 5.0 ± 0.2.
Embodiment three: disposable lithium-battery ferrous disulfide/carbon composite anode material, and the mass percentage content of ferrous disulfide is 98% in this ferrous disulfide/carbon composite anode material, the mass percentage content of carbon is 2%.
The preparation method of disposable lithium-battery ferrous disulfide/carbon composite anode material has following steps:
(1) carbon nanometer tube (being abbreviated as MCNTs) or graphene film or glucose (being abbreviated as GC) or sucrose or starch or p-aminobenzoic acid and N-methyl pyrrolidone are the mixed of 1:100 by mass ratio after, obtain suspension-turbid liquid; The suspension-turbid liquid that obtains is carried out ultrasonic dispersion, ultrasonic power is 700 watts, kept 3 hours, pyrite is joined in the suspension-turbid liquid, wherein pyrite and carbon nanometer tube or graphene film mass ratio are 98:2, the mass ratio of carbon is 97:3 in pyrite and glucose or sucrose or starch or the p-aminobenzoic acid, stirs and obtains mixing pastel after 8 hours; Carbon source material is two or more material that mixes of carbon nanometer tube, graphene film, glucose, sucrose, starch and p-aminobenzoic acid.
(2) the mixing pastel that step (1) is obtained is under 14 liters/minute the nitrogen or argon shield, to be heated to 130 ℃ in air velocity, keeps after 15 hours; Be heated to 400 ℃ again, kept 20 hours, be cooled to room temperature then, by ball milling and sieving, the ball milling time is 8 hours, sieves and adopts 190 mesh sieves, obtains granular disposable lithium-battery ferrous disulfide/carbon composite anode material.
The pyrite average particulate diameter is 28 microns, the mass percentage content of ferrous disulfide is 98% in the pyrite, Fe element mass percentage content is 45% in the pyrite, S element mass percentage content is 51%, the water-soluble iron mass percentage content is 0.2%, and the mass percentage content of sulfate ion is 0.2%, after pyrite is water-soluble, pyrite mixes the back with water by mass ratio 1:18 and forms the mixing suspension-turbid liquid, and the supernatant liquor pH value of mixing suspension-turbid liquid is 6.0 ± 0.2.
The ferrous disulfide material is natural pyrite, through removal of impurities and pulverization process, controls its particle mean size in 10 ~ 30 micrometer ranges before using, and the ferrous disulfide mass percentage content reaches more than 98 %, and the microscopic appearance of this ferrous disulfide material is seen Fig. 1 a, FeS
2/ MCNTs(FeS
2With the MCNTs mass ratio be 98:2) microscopic appearance such as Fig. 1 b of composite material, as can be seen, FeS
2Ferrous disulfide fully mixes with carbon nano-tube in the/MCNTs composite material, is covered in the ferrous disulfide particle surface to the better conductivity even carbon nanotube, and the conductivity of composite material will obtain bigger raising.
The X-ray diffracting spectrum of various ferrous disulfide/carbon composite anode materials and ferrous disulfide material is seen Fig. 2, significant change does not take place in various as seen from Figure 2 composite material X-ray diffractions peak position, illustrates that the crystal structure of composite material and pure ferrous disulfide are consistent substantially.The specific area of ferrous disulfide and various ferrous disulfide/carbon composite anode materials sees Table 1.The lithium/pyrite battery that the positive plate that the ferrous disulfide material is made is made, its cell discharge performance are seen Fig. 3 (a), and concrete discharge data sees Table 2.
The battery performance that various ferrous disulfide/carbon composite anode materials are made: cell discharge performance adopts room temperature (23 ° of C) 1000 mA continuous discharge modes to compare, above composite positive pole battery and pure ferrous disulfide positive electrode battery 1000 mA continuous discharge curves are seen Fig. 3, as can be seen FeS
2/ MCNTs, FeS
2/ AC, FeS
2/ CB, FeS
2/ GC composite material (FeS
2With the mass ratio of C element be 98:2) discharge platform to be higher than pure FeS
2The discharge platform of positive electrode active materials, preparation-obtained composite positive pole battery, 1.3 V current potentials above discharge times all more than 60 min, and pure FeS
2Positive electrode has only 0.5 min, and discharging to 0.9 V remains unchanged total time substantially, as shown in table 2.This shows that the composite material discharge platform is obviously promoted, high pressure section obviously promotes discharge time.
Table 1:
| Positive electrode active materials | FeS 2 | FeS 2/MCNTs | FeS 2/AC | FeS 2/CB | FeS 2/GC |
| Specific area (m 2/g） | 0.8360 | 1.292 | 33.197 | 1.657 | 0.9969 |
Table 2:
| Final voltage | FeS 2 | FeS 2/MCNTs | FeS 2/AC | FeS 2/CB | FeS 2/GC |
| 1.3 V | 0.5 min | 67 min | 73 min | 74 min | 63 min |
| 1.2 V | 110 min | 127 min | 131 min | 132 min | 127 min |
| 0.9 V | 165 min | 162 min | 170 min | 167 min | 161 min |
Claims (10)
1. disposable lithium-battery ferrous disulfide/carbon composite anode material, the mass percentage content that it is characterized in that ferrous disulfide in this ferrous disulfide/carbon composite anode material is 50～99.5%, the mass percentage content of carbon is 0.5～50%.
2. disposable lithium-battery ferrous disulfide/carbon composite anode material according to claim 1, the mass percentage content that it is characterized in that described ferrous disulfide is 95～98%, the mass percentage content of carbon is 2～5%.
3. the preparation method of disposable lithium-battery ferrous disulfide/carbon composite anode material is characterized in that having following steps:
(1) carbon source material and dispersant are the mixed of 1:15～120 by mass ratio after, obtain suspension-turbid liquid; Pyrite is joined in the suspension-turbid liquid, and wherein the mass ratio of pyrite and carbon source material is (90 ~ 99.5): (0.5 ~ 10), and stir then after 1～10 hour and obtain mixing pastel;
(2) the mixing pastel that step (1) is obtained is heated to 50～150 ℃ under inert gas shielding, keeps after 1～40 hour; Be heated to 250～400 ℃ again, kept 1～20 hour, be cooled to room temperature then, obtain granular disposable lithium-battery ferrous disulfide/carbon composite anode material with sieving by ball milling.
4. the preparation method of disposable lithium-battery ferrous disulfide/carbon composite anode material according to claim 3, it is characterized in that the carbon source material that will obtain in the step (1) carries out ultrasonic dispersion with the suspension-turbid liquid that mixes of dispersant, ultrasonic power is 300～800 watts, keeps 1～5 hour.
5. the preparation method of disposable lithium-battery ferrous disulfide/carbon composite anode material according to claim 3, it is characterized in that the pyrite average grain diameter is 10 ~ 30 microns, the mass percentage content of ferrous disulfide is not less than 95% in the pyrite, Fe element mass percentage content must not be lower than 43%, S element mass percentage content must not be lower than 49%, the water-soluble iron mass percentage content is not higher than 1.0%, the mass percentage content of sulfate ion is not higher than 1.0%, and pyrite and water are by mass ratio 1:(5～20) mix the back form mix suspension-turbid liquid supernatant liquor pH value between 4.0 ~ 8.0.
6. the preparation method of disposable lithium-battery ferrous disulfide/carbon composite anode material according to claim 3 is characterized in that dispersant is at least a of water, ethanol, methyl alcohol, acetone and N-methyl pyrrolidone.
7. the preparation method of disposable lithium-battery ferrous disulfide/carbon composite anode material according to claim 3 is characterized in that carbon source material is at least a in carbon black, acetylene black, active carbon, mesoporous carbon, carbon nano-tube, graphene film, glucose, sucrose, starch and the p-aminobenzoic acid.
8. the preparation method of disposable lithium-battery ferrous disulfide/carbon composite anode material according to claim 3 is characterized in that the ball milling time in the step (2) is 1～10 hour, sieves and adopts 160～200 mesh sieves; Inert gas is for flowing atmosphere, and air velocity is 1～15 liter/minute, and inert gas is at least a in nitrogen and the argon gas.
9. the disposable lithium-battery positive pole is characterized in that comprising as the arbitrary described disposable lithium-battery ferrous disulfide/carbon composite anode material of claim 1～2.
10. disposable lithium-battery is characterized in that comprising disposable lithium-battery positive pole as claimed in claim 9.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103326002A (en) * | 2013-06-26 | 2013-09-25 | 冯林杰 | Preparation method of graphene and ferrous disulfide composite positive electrode material |
| CN103606677A (en) * | 2013-11-25 | 2014-02-26 | 山东神工海特电子科技有限公司 | Preparation method of iron disulfide/carbon composite positive electrode material of primary lithium battery and method for assembling button cell by using positive electrode material |
| CN106745323A (en) * | 2016-12-09 | 2017-05-31 | 太原理工大学 | A kind of preparation method of iron sulphur compound and its composite |
| CN107090586A (en) * | 2017-04-13 | 2017-08-25 | 上海应用技术大学 | A kind of FeS2RGO composites, preparation method and applications |
| CN107819127A (en) * | 2017-10-26 | 2018-03-20 | 中银（宁波）电池有限公司 | Anode material of lithium-iron disulfide battery with function of reducing open-circuit voltage and preparation method of anode material |
| CN109243846A (en) * | 2018-10-24 | 2019-01-18 | 昆明理工大学 | A kind of FeSx/ C/CNT hybrid supercapacitor electrode |
| CN111162261A (en) * | 2020-01-14 | 2020-05-15 | 广东工业大学 | Iron disulfide/graphene oxide/nitrogen-doped multi-walled carbon nanotube composite material and preparation method and application thereof |
| CN113224275A (en) * | 2021-04-20 | 2021-08-06 | 阳原县仁恒精细粘土有限责任公司 | Graphene/clay nano composite electrode material and preparation method thereof |
| US11145854B2 (en) | 2019-09-16 | 2021-10-12 | Zhongyin (Ningbo) Battery Co., Ltd. | Process for preparing cathode of lithium battery and lithium battery having the cathode |
| CN113517443A (en) * | 2021-06-19 | 2021-10-19 | 天目湖先进储能技术研究院有限公司 | Preparation method of polyacrylonitrile/iron disulfide composite positive electrode material for lithium secondary battery |
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| CN1843941A (en) * | 2006-05-12 | 2006-10-11 | 清华大学 | Method for preparing anode material of lithium-iron disulphide battery |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103326002A (en) * | 2013-06-26 | 2013-09-25 | 冯林杰 | Preparation method of graphene and ferrous disulfide composite positive electrode material |
| CN103326002B (en) * | 2013-06-26 | 2015-11-04 | 国网浙江嵊州市供电公司 | The preparation method of a kind of Graphene-ferrous disulfide composite positive pole |
| CN103606677A (en) * | 2013-11-25 | 2014-02-26 | 山东神工海特电子科技有限公司 | Preparation method of iron disulfide/carbon composite positive electrode material of primary lithium battery and method for assembling button cell by using positive electrode material |
| CN106745323B (en) * | 2016-12-09 | 2018-08-21 | 太原理工大学 | A kind of preparation method of iron sulphur compound and its composite material |
| CN106745323A (en) * | 2016-12-09 | 2017-05-31 | 太原理工大学 | A kind of preparation method of iron sulphur compound and its composite |
| CN107090586A (en) * | 2017-04-13 | 2017-08-25 | 上海应用技术大学 | A kind of FeS2RGO composites, preparation method and applications |
| CN107819127A (en) * | 2017-10-26 | 2018-03-20 | 中银（宁波）电池有限公司 | Anode material of lithium-iron disulfide battery with function of reducing open-circuit voltage and preparation method of anode material |
| CN109243846A (en) * | 2018-10-24 | 2019-01-18 | 昆明理工大学 | A kind of FeSx/ C/CNT hybrid supercapacitor electrode |
| US11145854B2 (en) | 2019-09-16 | 2021-10-12 | Zhongyin (Ningbo) Battery Co., Ltd. | Process for preparing cathode of lithium battery and lithium battery having the cathode |
| CN111162261A (en) * | 2020-01-14 | 2020-05-15 | 广东工业大学 | Iron disulfide/graphene oxide/nitrogen-doped multi-walled carbon nanotube composite material and preparation method and application thereof |
| CN113224275A (en) * | 2021-04-20 | 2021-08-06 | 阳原县仁恒精细粘土有限责任公司 | Graphene/clay nano composite electrode material and preparation method thereof |
| CN113224275B (en) * | 2021-04-20 | 2022-07-19 | 阳原县仁恒精细粘土有限责任公司 | Graphene/clay nano composite electrode material and preparation method thereof |
| CN113517443A (en) * | 2021-06-19 | 2021-10-19 | 天目湖先进储能技术研究院有限公司 | Preparation method of polyacrylonitrile/iron disulfide composite positive electrode material for lithium secondary battery |
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Application publication date: 20110817 |