CN107394158A - A kind of method that the compound lithium cell cathode material of silicon-carbon is prepared based on expanded graphite - Google Patents
A kind of method that the compound lithium cell cathode material of silicon-carbon is prepared based on expanded graphite Download PDFInfo
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- CN107394158A CN107394158A CN201710599847.XA CN201710599847A CN107394158A CN 107394158 A CN107394158 A CN 107394158A CN 201710599847 A CN201710599847 A CN 201710599847A CN 107394158 A CN107394158 A CN 107394158A
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Abstract
The invention discloses a kind of method that the compound lithium cell cathode material of silicon-carbon is prepared based on expanded graphite, potassium permanganate and concentrated sulfuric acid oxidation intercalation natural flake graphite are used in the present invention, the oxy radicals such as hydroxyl, epoxide group and carboxyl are introduced in graphite layers, increase graphite layers away from, afterwards under microwave field action, oxy radical thermal decomposition inside graphite, produces CO, CO2And H2The gases such as O, caused impulsive force causes graphite flake layer rapid expansion, graphite linings lamella is softened, further increase graphite layers away from, weaken interlayer Van der Waals force, increase stone ink Women piece interlayers distance, so as to lift the embedding lithium capacity of electrode material to a certain extent, " buffering matrix " as silicon electrode simultaneously, can accommodate expansion/contraction of the nano-silicon dioxide particle in charge and discharge process, improve the cyclical stability and high rate performance of electrode material.
Description
Technical field
The present invention relates to a kind of lithium cell cathode material field, and in particular to it is compound that one kind based on expanded graphite prepares silicon-carbon
The method of type lithium cell cathode material.
Background technology
Lithium battery has big operating voltage height, energy density, discharging voltage balance, circulation compared with other secondary cells
Long lifespan and advantages of environment protection, the fields such as portable type electronic product and electric tool are had been widely used for, and be expected to
As one of the main energy sources of following hybrid vehicle and pure power vehicle supply.Negative material is evaluation lithium battery integrated
One of key factor that can be good and bad.
So far, in negative material silicon theoretical capacity highest.It is generally acknowledged that at normal temperatures, silicium cathode and lithium alloyage
Caused rich lithium product is mainly Li3.75Si phases, capacity are up to 3572mAh/g, much larger than the theoretical capacity of graphite, but it is adjoint
Huge Volume Changes, its volumetric expansion is up to 270%, and the efflorescence of silicon causes electrode structure unstability and failed, and causes electrode knot
The avalanche of structure and active material are peeled off and electrode is lost electrical contact, and the capacity of electrode significantly declines therewith even to be lost completely
Effect.
In order to avoid the disadvantages mentioned above of silicon, in numerous schemes using " cushioning frame " come the method that compensating material expands by
Pay attention to.Graphite has lamellar structure, can slow down the structural remodeling process in charge and discharge process, so as to avoid negative material structure
Avalanche, be suitable as buffer matrix.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides one kind and prepares the compound cathode of lithium battery of silicon-carbon based on expanded graphite
The method of material.
The present invention is achieved by the following technical solutions:
A kind of method that the compound lithium cell cathode material of silicon-carbon is prepared based on expanded graphite, its preparation technology are as follows:
(1)Coated Si O2Forerunner's dispersion liquid:
1., under magnetic stirring, into 90-120 parts by weight of ethanol, the mixing liquid of 5-9 parts deionized water and 6-12 part ammoniacal liquor
3-8 part TEOS are slowly added dropwise, stirs centrifuge washing, drying after 4-6 hours, obtains silica nanosphere, it is standby;
2., by 30-50 parts ethanol, 1-3 parts cetyl trimethylammonium bromide and 5-10 parts zinc acetate mix, strong agitation 40-
60 minutes, homogeneous solution is obtained, adds silica nanosphere afterwards, ultrasonic disperse is uniform, and generation cladding salt precursor body disperses
Liquid;
(2)Weigh 20-40 part crystalline flake graphites to be slowly added into 110-180 part concentrated sulfuric acids, be slowly added to 35- under agitation
55 parts of potassium permanganate, under 30-40 DEG C of bath temperature, intermittent stirring 1-2 hours, it is washed with deionized to neutrality, filtering, dries
It is dry, expansible graphite is produced, dried expansible graphite is placed in micro-wave oven expanded afterwards, Bulking Time 15-
25s, obtain expanded graphite;
(3)To step(1)Step is added in forerunner's dispersion liquid(2)Expanded graphite, it is placed in reaction bulb, vacuumizes 20- in advance
40 minutes, 5-10 minutes then are stood, then are repeated and vacuumize-stewing process 3-5 time, under pressure inducement, liquid injects
To the interlayer of expanded graphite;
(4)By step(3)The expanded graphite of injection forerunner's dispersion liquid is transferred in reactor, is heated in reducing atmosphere stove
900-1200 DEG C of sintering 10-20 minute, zinc oxide/graphene coated silica complex is obtained after being cooled to room temperature, then
To be soaked 8-25 minutes with hydrochloric acid solution, cleaning removes zinc oxide, after being washed repeatedly with absolute ethyl alcohol, deionized water, vacuum drying,
Obtain silica@graphene composite negative poles.
Wherein, step(2)Described in microwave expansion actual conditions be:Microwave power is 10kW, temperature 900-980
℃。
Wherein, step(4)Described in the concentration of hydrochloric acid solution be 10-30%.
Wherein, step(4)Described in vacuum drying temperature be 60-70 DEG C.
Compared with prior art, the present invention has advantages below:
(1)In the present invention using potassium permanganate and the concentrated sulfuric acid oxidation intercalation natural flake graphite, graphite layers introduce hydroxyl,
The oxy radical such as epoxide group and carboxyl, increase graphite layers away from, afterwards under microwave field action, oxy radical inside graphite
Thermal decomposition, produce CO, CO2And H2The gases such as O, caused impulsive force cause graphite flake layer rapid expansion, and graphite linings lamella is supportted
Open, further increase graphite layers away from, weaken interlayer Van der Waals force, increase stone ink Women piece interlayers distance, so as to one
Determine the embedding lithium capacity of lifting electrode material in degree, while as " the buffering matrix " of silicon electrode, nanometer titanium dioxide can be accommodated
Expansion/contraction of the silicon particle in charge and discharge process, improve the cyclical stability and high rate performance of electrode material.
(2)Zinc oxide ZnO nano crystalline substance reaches the effect of exfoliated graphite layer in expanded graphite interlayer growth in situ in the present invention
Fruit, after high temperature reduction, silica/zinc oxide is uniformly adhered in the space of graphene sheet layer, can effectively prevent stone
The stacking of black alkene, agglomeration traits, after soaked through hydrochloric acid and remove zinc oxide, composite inner forms abundant pore passage structure,
These pore passage structures can provide substantial amounts of passage for lithium ion, increase the embedded location of lithium ion, greatly improve it
Storage lithium performance as lithium cell cathode material.
Embodiment
A kind of method that the compound lithium cell cathode material of silicon-carbon is prepared based on expanded graphite, its preparation technology are as follows:
(1)Coated Si O2Forerunner's dispersion liquid:
1., under magnetic stirring, to 90 parts by weight of ethanol, 6 parts of deionized waters with being slowly added dropwise 7 in the mixing liquid of 6 parts of ammoniacal liquor
Part TEOS, centrifuge washing, drying, obtain silica nanosphere after stirring 5 hours, standby;
2., 40 parts of ethanol, 2 parts of cetyl trimethylammonium bromides and 8 parts of zinc acetates are mixed, strong agitation 50 minutes, obtain
Homogeneous solution, silica nanosphere is added afterwards, ultrasonic disperse is uniform, generation cladding salt precursor dispersion liquid;
(2)Weigh 30 parts of crystalline flake graphites to be slowly added into 120 parts of concentrated sulfuric acids, be slowly added to 45 parts of permanganic acid under agitation
Potassium, under 35 DEG C of bath temperatures, intermittent stirring 2 hours, it is washed with deionized to neutrality, filtering, drying, produces inflatable stone
Ink, dried expansible graphite is placed in micro-wave oven expanded afterwards, Bulking Time 25s, obtain expanded graphite;
(3)To step(1)Step is added in forerunner's dispersion liquid(2)Expanded graphite, it is placed in reaction bulb, vacuumizes 30 points in advance
Clock, 8 minutes then are stood, then be repeated and vacuumize-stewing process 4 times, under pressure inducement, liquid is injected into expanded graphite
Interlayer;
(4)By step(3)The expanded graphite of injection forerunner's dispersion liquid is transferred in reactor, is heated in reducing atmosphere stove
900 DEG C are sintered 15 minutes, and zinc oxide/graphene coated silica complex is obtained after being cooled to room temperature, then molten with hydrochloric acid
Liquid soaks 20 minutes, and cleaning removes zinc oxide, after being washed repeatedly with absolute ethyl alcohol, deionized water, vacuum drying, obtains titanium dioxide
Silicon@graphene composite negative poles.
Wherein, step(2)Described in microwave expansion actual conditions be:Microwave power is 10kW, and temperature is 950 DEG C.
Wherein, step(4)Described in hydrochloric acid solution concentration be 20%.
Wherein, step(4)Described in vacuum drying temperature be 70 DEG C.
Claims (4)
- A kind of 1. method that the compound lithium cell cathode material of silicon-carbon is prepared based on expanded graphite, it is characterised in that it prepares work Skill is as follows:(1)Coated Si O2Forerunner's dispersion liquid:1., under magnetic stirring, into 90-120 parts by weight of ethanol, the mixing liquid of 5-9 parts deionized water and 6-12 part ammoniacal liquor 3-8 part TEOS are slowly added dropwise, stirs centrifuge washing, drying after 4-6 hours, obtains silica nanosphere, it is standby;2., by 30-50 parts ethanol, 1-3 parts cetyl trimethylammonium bromide and 5-10 parts zinc acetate mix, strong agitation 40- 60 minutes, homogeneous solution is obtained, adds silica nanosphere afterwards, ultrasonic disperse is uniform, and generation cladding salt precursor body disperses Liquid;(2)Weigh 20-40 part crystalline flake graphites to be slowly added into 110-180 part concentrated sulfuric acids, be slowly added to 35- under agitation 55 parts of potassium permanganate, under 30-40 DEG C of bath temperature, intermittent stirring 1-2 hours, it is washed with deionized to neutrality, filtering, dries It is dry, expansible graphite is produced, dried expansible graphite is placed in micro-wave oven expanded afterwards, Bulking Time 15- 25s, obtain expanded graphite;(3)To step(1)Step is added in forerunner's dispersion liquid(2)Expanded graphite, it is placed in reaction bulb, vacuumizes 20- in advance 40 minutes, 5-10 minutes then are stood, then are repeated and vacuumize-stewing process 3-5 time, under pressure inducement, liquid injects To the interlayer of expanded graphite;(4)By step(3)The expanded graphite of injection forerunner's dispersion liquid is transferred in reactor, is heated in reducing atmosphere stove 900-1200 DEG C of sintering 10-20 minute, zinc oxide/graphene coated silica complex is obtained after being cooled to room temperature, then To be soaked 8-25 minutes with hydrochloric acid solution, cleaning removes zinc oxide, after being washed repeatedly with absolute ethyl alcohol, deionized water, vacuum drying, Obtain silica@graphene composite negative poles.
- A kind of 2. side that the compound lithium cell cathode material of silicon-carbon is prepared based on expanded graphite according to claims 1 Method, it is characterised in that step(2)Described in microwave expansion actual conditions be:Microwave power is 10kW, temperature 900- 980℃。
- A kind of 3. side that the compound lithium cell cathode material of silicon-carbon is prepared based on expanded graphite according to claims 1 Method, it is characterised in that step(4)Described in the concentration of hydrochloric acid solution be 10-30%.
- A kind of 4. side that the compound lithium cell cathode material of silicon-carbon is prepared based on expanded graphite according to claims 1 Method, it is characterised in that step(4)Described in vacuum drying temperature be 60-70 DEG C.
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Cited By (11)
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CN108410066A (en) * | 2018-04-13 | 2018-08-17 | 西南交通大学 | A kind of SiO2The preparation method of nanometer particle-modified expansible graphite and polypropylene flame redardant |
CN108832087A (en) * | 2018-06-08 | 2018-11-16 | 湖南大学 | A kind of cell negative electrode material and preparation method thereof |
CN109841818A (en) * | 2019-03-05 | 2019-06-04 | 电子科技大学 | A kind of preparation method and applications of lithium secondary battery cathode material |
CN109920582A (en) * | 2019-01-28 | 2019-06-21 | 芜湖航天特种电缆厂股份有限公司 | Corrosion-resistant anti-mildew cable and preparation method thereof |
CN111933916A (en) * | 2020-10-12 | 2020-11-13 | 长沙矿冶研究院有限责任公司 | Negative electrode active material and preparation method thereof |
CN113036306A (en) * | 2021-02-20 | 2021-06-25 | 山东天瀚新能源科技有限公司 | Silicon-doped lithium supplement technical scheme and assembly method of lithium ion battery |
CN113511651A (en) * | 2021-09-09 | 2021-10-19 | 成都特隆美储能技术有限公司 | Preparation method of polypyrrole-modified micro-oxidation expanded graphite negative electrode material |
CN114464790A (en) * | 2022-01-25 | 2022-05-10 | 四川金汇能新材料股份有限公司 | Pre-lithiated silica composite material, preparation method and application |
CN115057466A (en) * | 2022-08-04 | 2022-09-16 | 安徽进化硅纳米材料科技有限公司 | Modified nano zinc oxide composite material and preparation method and application thereof |
CN115286347A (en) * | 2022-08-15 | 2022-11-04 | 威赫炘源纳米科技(苏州)有限公司 | Preparation method of nano aerogel heat insulation material |
CN115676819A (en) * | 2021-07-21 | 2023-02-03 | 比亚迪股份有限公司 | Graphite material preparation method, graphite material and power battery |
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CN108410066A (en) * | 2018-04-13 | 2018-08-17 | 西南交通大学 | A kind of SiO2The preparation method of nanometer particle-modified expansible graphite and polypropylene flame redardant |
CN108832087A (en) * | 2018-06-08 | 2018-11-16 | 湖南大学 | A kind of cell negative electrode material and preparation method thereof |
CN108832087B (en) * | 2018-06-08 | 2021-04-30 | 湖南大学 | Battery negative electrode material and preparation method thereof |
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CN109841818B (en) * | 2019-03-05 | 2021-12-03 | 电子科技大学 | Preparation method and application of negative electrode material of lithium secondary battery |
CN109841818A (en) * | 2019-03-05 | 2019-06-04 | 电子科技大学 | A kind of preparation method and applications of lithium secondary battery cathode material |
CN111933916A (en) * | 2020-10-12 | 2020-11-13 | 长沙矿冶研究院有限责任公司 | Negative electrode active material and preparation method thereof |
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CN115676819A (en) * | 2021-07-21 | 2023-02-03 | 比亚迪股份有限公司 | Graphite material preparation method, graphite material and power battery |
CN113511651A (en) * | 2021-09-09 | 2021-10-19 | 成都特隆美储能技术有限公司 | Preparation method of polypyrrole-modified micro-oxidation expanded graphite negative electrode material |
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CN114464790A (en) * | 2022-01-25 | 2022-05-10 | 四川金汇能新材料股份有限公司 | Pre-lithiated silica composite material, preparation method and application |
CN114464790B (en) * | 2022-01-25 | 2023-06-02 | 四川金汇能新材料股份有限公司 | Pre-lithiated silica composite material, preparation method and application |
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CN115057466B (en) * | 2022-08-04 | 2024-03-08 | 安徽进化硅纳米材料科技有限公司 | Modified nano zinc oxide composite material and preparation method and application thereof |
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