CN102456876A - Lithium-ion battery graphitized mesoporous carbon/silicon composite anode materials and preparation method thereof - Google Patents
Lithium-ion battery graphitized mesoporous carbon/silicon composite anode materials and preparation method thereof Download PDFInfo
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Abstract
The invention discloses lithium-ion battery graphitized mesoporous carbon/silicon composite anode materials and a preparation method thereof. Mesoporous carbon materials with different degrees of graphitization are synthesized by using mesoporous silicon oxide as a hard template and combining transition metal (Fe, Ni, Co, etc) catalysis, and the mesoporous carbon materials are used as the carrier to deposit amorphous silicon on the mesoporous carbon pore walls through the chemical vapor deposition (CVD) technology to obtain the graphitized mesoporous carbon/silicon composite anode materials. The composite materials have stable performance; and when used as the anode materials of the lithium-ion battery, the composite materials have the advantages of large lithium storage capacity, long life, high safety and the like.
Description
Technical field
The present invention relates to a kind of silicon/carbon/graphite in lithium ion batteries mesoporous carbon/silicon composite cathode material and preparation method thereof, relate to electrochemistry and field of material synthesis technology.It is characterized in that the mesoporous carbon that adopts hard template method to combine transition metal (Ni, Fe, Co etc.) catalyzed graphitization to obtain is a carrier, utilize chemical gas-phase method deposit amorphous silicon on the mesoporous carbon hole wall to obtain.The characteristics of composite negative pole material of the present invention are: be used for lithium ion battery as negative material and have the lithium storage content height, advantage such as long and fail safe of life-span is good.
Background technology
Lithium ion battery is because advantages such as open circuit voltage is high, energy density is big, good cycle obtain increasingly extensive application.The negative material that commercialization is at present used is the graphite-like carbon negative pole material mostly; Has good cycle life; But its theoretical lithium storage content is less; Volume and capacity ratio does not have advantage especially, can not satisfy the demand of people to high energy density cells gradually, and the novel negative material of therefore developing height ratio capacity, high charge-discharge efficient, high cyclical stability has become the focus of current research.
Find the alloy type material that Si, Sn, Co, Al etc. and Li form in the negative material research; Its reversible lithium storage capacity will be higher than the graphite-like negative pole far away; And wherein silicon owing to have the highest theoretical lithium storage content (4200mAh/g), advantage such as the doff lithium current potential is low, cheap and become the focus of research.But there is very huge volumetric expansion (up to 300%) in the pure silicon material in height doff lithium process, causes material to reunite or powdered easily in cyclic process, and cycle efficieny is not high so can not satisfy the demand of practicability.For fear of the shortcoming of above-mentioned silicon, the researcher has taked multiple measure, and the method effect of wherein utilizing " buffering skeleton " to come compensative material to expand is the most obvious, and this method is mainly utilized the cooperative effect between each component of composite material, can reach the purpose of mutual supplement with each other's advantages.It is that nuclear, amorphous carbon are nucleocapsid composite lithium ion battery cathode material of shell and preparation method thereof with the nano-silicon that Chinese invention patent CN 101527357A discloses a kind of; This composite material can effectively be controlled the change in volume of silicon in charge and discharge process, have good cycle life.(Zheng Ying such as Zheng Ying; Yang Jun etc.; Chinese Journal of Inorganic Chemistry; 2007,23 (11): 1882-1886) processed porous silicon/graphite/carbon composite lithium ion battery cathode material through two steps such as step high-energy ball milling, acid etching and carbon coatings etc., Electrochemical results shows that this composite material wants ratio nano silicon/graphite/carbon composite material to have better cyclical stability; Charging capacity remains on 649.9mAh/g, almost not decay after wherein using 200 circulations of electrode of 10% LA132 binding agent.But see that from application point of view the first charge-discharge efficiency of this material remains further to be improved.
Summary of the invention
The object of the present invention is to provide a kind of silicon/carbon/graphite in lithium ion batteries mesoporous carbon/silicon composite cathode material and preparation method thereof.It is characterized in that the mesoporous carbon that adopts hard template method to combine transition metal (Ni, Fe, Co etc.) catalyzed graphitization to obtain is a carrier, and obtain through chemical gas-phase method deposit amorphous silicon on the mesoporous carbon hole wall.
The preparation method of silicon/carbon/graphite in lithium ion batteries mesoporous carbon/silicon composite cathode material provided by the invention; It is characterized in that containing in the prepared different graphitization degree degree mesoporous carbon material that obtains the transition metal (Ni, Fe or Mn) of 0.05-0.5wt%, the existence of these transition metal is played important effect to the deposition of follow-up amorphous elemental silicon.
Silicon/carbon/graphite in lithium ion batteries mesoporous carbon/silicon composite cathode material provided by the invention, order is carried out according to the following steps:
(1) the orderly mesopore silica template of the synthetic different structure of the method for reference literature: SBA-15 (Zhao D, Feng J, et al., the Science of two dimension six side p6m; 1998,279:548-552), KIT-6 (Kleitz F, Choi S H, the et al. of three-dimensional cubic structure Ia3d; Chem.Commun., 2003,2136-2137) with MSU-X (Takahashi R, the Sato S of three-dimensional vermicular texture; Et al., J.Phys.Chem.B, 2000,104:12184-12191.).
(2) the orderly mesopore silica template of above-mentioned preparation is impregnated in the ethanol water of 0.05mol/L transition metal (Ni, Fe, Co etc.) nitrate (the ethanol/water volume ratio is 1); And under 35-85 ℃ of condition, stirred dry 5-20 hour, the mol ratio that wherein makes Si and transition metal is 20-50.
(3) through liquid impregnation carbon source is impregnated into containing in Ni or the orderly mesopore silica of the Fe template duct that step (2) obtains; Make it under nitrogen or argon shield, be warming up to 700-1100 ℃ of pyrolysis catalytic graphitization 1-8 hour then, remove the mesoporous carbon material that silica can obtain containing transition metal (Ni, Fe or Co) and different graphitization degree degree with the NaOH etching at last.
(4) the mesoporous carbon material that contains transition metal and different graphitization degree degree that step (3) is obtained places in the tube furnace; After vacuumizing, argon purge is heated to 300-600 ℃; Treat the logical 1-3% silane-argon gas mist that contains behind the temperature stabilization; Flow control is deposited on the mesoporous carbon hole wall amorphous Si between 5-60ml/min, stops cooling after 2-60 minute and can obtain graphitization mesoporous carbon/silicon composite cathode material.
The mass ratio of carbon and silicon is 0.3-20 in silicon/carbon/graphite in lithium ion batteries mesoporous carbon/silicon composite cathode material provided by the invention.
Silicon/carbon/graphite in lithium ion batteries mesoporous carbon/silicon composite cathode material provided by the invention has the lithium storage content height, has extended cycle life and advantage such as security performance is good.
Embodiment
Embodiment 1
The SBA-15 that takes by weighing 3.0 gram two dimensions, six side p6m is impregnated into the Ni (NO of 28.5ml concentration 0.05mol/L
3)
2In the ethanol water, and under 35-85 ℃ of condition, stir 10 hours until the complete volatile dry of solvent.With above-mentioned Ni/SBA-15 be impregnated into contain 3.75 the gram sucrose; 0.42 in the solution of gram sulfuric acid and 15.0 gram water; Fully stir the back in 100 ℃ of dryings 6 hours, then 160 ℃ of heat treatments 6 hours, repeated impregnations is once but the amount of sucrose and sulfuric acid is original 50-60% again after the cooling.With compound 900 ℃ of carbonizations and catalyzed graphitization 6 hours under nitrogen atmosphere, silica is removed with the NaOH etching of 2mol/L then, can obtain the part graphitization and contain the orderly mesoporous carbon CMK-3 of Ni.
The orderly mesoporous carbon CMK-3 that takes by weighing above-mentioned 2 gram part graphitizations and contain Ni is tiled in the quartz boat and places vacuum tube furnace;, 3-5 high-purity argon gas purging be heated to 500 ℃ after vacuumizing; Treat the logical 2% silane-argon gas mist that contains behind the temperature stabilization; Flow control is about 10ml/min; Amorphous Si stops heating and logical silane in deposition on the mesoporous carbon hole wall after 15 minutes, continue logical argon gas until cool to room temperature, can obtain part graphitization mesoporous carbon/silicon composite lithium ion battery cathode material.
Embodiment 2
The SBA-15 that takes by weighing 3.0 gram two dimensions, six side p6m is impregnated into the Fe (NO of 28.5ml concentration 0.05mol/L
3)
3In the ethanol water, and under 35-85 ℃ of condition, stir 10 hours until the complete volatile dry of solvent.With above-mentioned Fe/SBA-15 be impregnated into contain 3.75 the gram sucrose; 0.42 in the solution of gram sulfuric acid and 15.0 gram water; Fully stir the back in 100 ℃ of dryings 6 hours, then 160 ℃ of heat treatments 6 hours, repeated impregnations is once but the amount of sucrose and sulfuric acid is original 50-60% again after the cooling.With compound 950 ℃ of carbonizations and catalyzed graphitization 4 hours under nitrogen atmosphere, silica is removed with the NaOH etching of 2mol/L then, can obtain the part graphitization and contain the orderly mesoporous carbon CMK-3 of Fe.
The orderly mesoporous carbon CMK-3 that takes by weighing above-mentioned 2 gram part graphitizations and contain Fe is tiled in the quartz boat and places vacuum tube furnace;, 3-5 high-purity argon gas purging be heated to 500 ℃ after vacuumizing; Treat the logical 2% silane-argon gas mist that contains behind the temperature stabilization; Flow control is about 15ml/min; Amorphous Si stops heating and logical silane in deposition on the mesoporous carbon hole wall after 10 minutes, continue logical argon gas until cool to room temperature, can obtain part graphitization mesoporous carbon/silicon composite lithium ion battery cathode material.
Embodiment 3
The SBA-15 that takes by weighing 3.0 gram two dimensions, six side p6m is impregnated into the Co (NO of 28.5ml concentration 0.05mol/L
3)
2In the ethanol water, and under 35-85 ℃ of condition, stir 10 hours until the complete volatile dry of solvent.With above-mentioned Co/SBA-15 be impregnated into contain 3.75 the gram sucrose; 0.42 in the solution of gram sulfuric acid and 15.0 gram water; Fully stir the back in 100 ℃ of dryings 6 hours, then 160 ℃ of heat treatments 6 hours, repeated impregnations is once but the amount of sucrose and sulfuric acid is original 50-60% again after the cooling.With compound 900 ℃ of carbonizations and catalyzed graphitization 4 hours under nitrogen atmosphere, silica is removed with the NaOH etching of 2mol/L then, can obtain the part graphitization and contain the orderly mesoporous carbon CMK-3 of Co.
The orderly mesoporous carbon CMK-3 that takes by weighing above-mentioned 2 gram part graphitizations and contain Co is tiled in the quartz boat and places vacuum tube furnace;, 3-5 high-purity argon gas purging be heated to 500 ℃ after vacuumizing; Treat the logical 2% silane-argon gas mist that contains behind the temperature stabilization; Flow control is about 20ml/min; Amorphous Si stops heating and logical silane in deposition on the mesoporous carbon hole wall after 7 minutes, continue logical argon gas until cool to room temperature, can obtain part graphitization mesoporous carbon/silicon composite lithium ion battery cathode material.
Embodiment 4
The KIT-6 that takes by weighing 3.0 gram three-dimensional cubic structure Ia3d is impregnated into the Ni (NO of 28.5ml concentration 0.05mol/L
3)
2In the ethanol water, and under 35-85 ℃ of condition, stir 10 hours until the complete volatile dry of solvent.With above-mentioned Ni/SBA-15 be impregnated into contain 3.75 the gram sucrose; 0.42 in the solution of gram sulfuric acid and 15.0 gram water; Fully stir the back in 100 ℃ of dryings 6 hours, then 160 ℃ of heat treatments 6 hours, repeated impregnations is once but the amount of sucrose and sulfuric acid is original 50-60% again after the cooling.With compound 900 ℃ of carbonizations and catalyzed graphitization 4 hours under nitrogen atmosphere, silica is removed with the NaOH etching of 2mol/L then, can obtain the part graphitization and contain the orderly mesoporous carbon CMK-8 of Ni.
The orderly mesoporous carbon CMK-8 that takes by weighing above-mentioned 2 gram part graphitizations and contain Ni is tiled in the quartz boat and places vacuum tube furnace;, 3-5 high-purity argon gas purging be heated to 500 ℃ after vacuumizing; Treat the logical 1% silane-argon gas mist that contains behind the temperature stabilization; Flow control is about 15ml/min; Amorphous Si stops heating and logical silane in deposition on the mesoporous carbon hole wall after 10 minutes, continue logical argon gas until cool to room temperature, can obtain part graphitization mesoporous carbon/silicon composite lithium ion battery cathode material.
Embodiment 5
The SBA-15 that takes by weighing 3.0 gram two dimensions, six side p6m is impregnated into the Ni (NO of 28.5ml concentration 0.05mol/L
3)
2In the ethanol water, and under 35-85 ℃ of condition, stir 10 hours until the complete volatile dry of solvent.Get the 3.0g mesophase pitch and place ceramic crucible to be heated to 140 ℃, treat softening back stirring 0.5 hour.Add in this melt above-mentioned Ni/SBA-15 template and stirring, finally generate the complex solid powder of brown.With composite powder 900 ℃ of carbonizations and catalyzed graphitization 6 hours under nitrogen atmosphere, silica is removed with the NaOH etching of 2mol/L, can obtain high-graphitized and contains the orderly mesoporous carbon CMK-3 of Ni.
Taking by weighing the high-graphitized and orderly mesoporous carbon CMK-3 that contain Ni of above-mentioned 2 grams is tiled in the quartz boat and places vacuum tube furnace;, 3-5 high-purity argon gas purging be heated to 500 ℃ after vacuumizing; Treat the logical 1% silane-argon gas mist that contains behind the temperature stabilization; Flow control is about 10ml/min; Amorphous Si stops heating and logical silane in deposition on the mesoporous carbon hole wall after 10 minutes, continue logical argon gas until cool to room temperature, can obtain high-graphitized mesoporous carbon/silicon composite lithium ion battery cathode material.Embodiment 6
The SBA-15 that takes by weighing 3.0 gram two dimensions, six side p6m is impregnated into the Fe (NO of 28.5ml concentration 0.05mol/L
3)
3In the ethanol water, and under 35-85 ℃ of condition, stir 10 hours until the complete volatile dry of solvent.Get 4.5g soya-bean oil and be dissolved in the 20ml acetone and form homogeneous solution, above-mentioned Fe/SBA-15 template is added in the acetone soln of soya-bean oil, at room temperature stir and make its bone dry.With composite powder 900 ℃ of carbonizations and catalyzed graphitization 5 hours under nitrogen atmosphere, silica is removed with the NaOH etching of 2mol/L, can obtain high-graphitized and contains the orderly mesoporous carbon CMK-3 of Fe.
Taking by weighing the high-graphitized and orderly mesoporous carbon CMK-3 that contain Fe of above-mentioned 2 grams is tiled in the quartz boat and places vacuum tube furnace;, 3-5 high-purity argon gas purging be heated to 500 ℃ after vacuumizing; Treat the logical 1% silane-argon gas mist that contains behind the temperature stabilization; Flow control is about 15ml/min; Amorphous Si stops heating and logical silane in deposition on the mesoporous carbon hole wall after 15 minutes, continue logical argon gas until cool to room temperature, can obtain high-graphitized mesoporous carbon/silicon composite lithium ion battery cathode material.
Result of the test
Graphitization mesoporous carbon/silicon composite lithium ion battery cathode material electrochemical property test that above-mentioned each embodiment is made; Test condition with lithium metal as to electrode; Being combined into button cell, is electrolyte with 1mol/LLiPF6/EC/DMC (volume ratio 1: 1), and barrier film is UBE3025; Voltage range during charge-discharge test is 0.005-3V, and current density is: 100mA/g.Each the embodiment data such as the following table 1 that record
The chemical property of the negative material that table 1. various embodiments of the present invention make
Visible from last table test data, the composite negative pole material that adopts the inventive method to make not only has high storage reason capacity, has good cyclical stability simultaneously concurrently.
Claims (7)
1. silicon/carbon/graphite in lithium ion batteries mesoporous carbon/silicon composite cathode material and preparation method thereof; It is characterized in that the mesoporous carbon that adopts hard template method to combine transition metal (Ni, Fe, Co etc.) catalyzed graphitization to obtain is a carrier, obtain through chemical gas-phase method deposit amorphous silicon on the mesoporous carbon hole wall.
2. the described composite negative pole material of claim 1 is characterized in that comprising the steps:
(1) the mesopore silica template of at first synthetic different structure: SBA-15, the KIT-6 of three-dimensional cubic structure Ia3d and the MSU-X of three-dimensional vermicular texture of two dimension six side p6m.
(2) the mesopore silica template of above-mentioned preparation is impregnated in the ethanol water of 0.05mol/L transition metal (Ni, Fe, Co etc.) nitrate (the ethanol/water volume ratio is 1); And under 35-85 ℃ of condition, stirred dry 5-20 hour, the mol ratio that wherein makes Si and transition metal is 20-100.
(3) carbon source being impregnated into step (2) obtains containing in the mesopore silica template duct of transition metal; It was warming up under nitrogen or argon shield 700-1100 ℃ of pyrolysis catalytic 1-8 hour, removes the mesoporous carbon material that silica can obtain containing transition metal (Ni, Fe or Co) and different graphitization degree degree with the NaOH etching at last.
(4) the mesoporous carbon material that contains transition metal and different graphitization degree degree that step (3) is obtained places in the tube furnace; After vacuumizing, argon purge is heated to 300-600 ℃; Treat the logical 1-3% silane-argon gas mist that contains behind the temperature stabilization; Amorphous Si is deposited on the mesoporous carbon hole wall, stops cooling behind the certain hour and can obtain graphitization mesoporous carbon/silicon composite cathode material.
3. the preparation method of the described graphitization mesoporous carbon/silicon composite cathode material of claim 1 is characterized in that carbon source used among the preparation method 2 (3) is one or more of sucrose, soya-bean oil, mesophase pitch or phenolic resins etc.
4. the preparation method of the described graphitization mesoporous carbon/silicon composite cathode material of claim 1 is characterized in that containing in the prepared different graphitization degree degree mesoporous carbon material transition metal Ni, Fe or the Mn of 0.05-0.5wt%.
5. the preparation method of the described graphitization mesoporous carbon/silicon composite cathode material of claim 1 is characterized in that transition metal Ni contained in the mesoporous carbon material, Fe, Mn etc. play important effect to the deposition of elemental silicon.
6. the described graphitization mesoporous carbon/silicon composite cathode material of claim 1 is characterized in that the mass ratio of carbon and silicon is 0.3-20 in this composite material.
7. the described graphitization mesoporous carbon/silicon composite cathode material of claim 1 is characterized in that this composite material is used to the application of lithium ion battery negative material.
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| CN114122352A (en) * | 2021-10-29 | 2022-03-01 | 西安交通大学 | Silicon-carbon negative electrode material for inducing silicon deposition by doping porous carbon and preparation method thereof |
| CN115986124A (en) * | 2023-03-15 | 2023-04-18 | 河北坤天新能源股份有限公司 | Silicon-carbon composite material for lithium ion battery and preparation method thereof |
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