CN106848275A - A kind of preparation method of lithium ion battery negative material silica aerogel - Google Patents
A kind of preparation method of lithium ion battery negative material silica aerogel Download PDFInfo
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- CN106848275A CN106848275A CN201710138571.5A CN201710138571A CN106848275A CN 106848275 A CN106848275 A CN 106848275A CN 201710138571 A CN201710138571 A CN 201710138571A CN 106848275 A CN106848275 A CN 106848275A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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
Abstract
The present invention relates to a kind of preparation method of lithium ion battery negative material, lithium ion battery silica aerogel negative material involved in the present invention is to prepare nanometer titanium dioxide silica aerogel by traditional sol-gal process first, then aerosil is reduced to by nano-silicon by magnesium reduction process, lithium ion battery is applied to as negative material.Nano-silicon in lithium ion battery active material research with specific capacity very high due to having become focus, but silica-base material is during the deintercalation of lithium ion because the volumetric expansion of itself can cause caving in and atomizing for structure, cause active material cyclical stability reduction in charge and discharge process, capacity attenuation is very fast, the nano-silicon that this method is obtained, because the grain diameter for constituting structure is smaller, specific surface area is big, above-mentioned problem can be effectively prevented from, possesses good application prospect.
Description
Technical field
The invention belongs to electrochemical technology field, and in particular to a kind of lithium ion battery negative material nanometer silica aerogel
Preparation method.
Background technology
Aerosil is lightweight, porous, the amorphous solid nanostructure material being made up of ultrafine dust coalescence
Material, is typical nano material with special three-dimensional net structure, by hydrolyzing silica obtained in the method for waterglass
Aeroge, is not developed because preparation technology is complicated and product impurity.With sol-gel process extensive use and
The fast development and popularization of Supercritical Drying Technology, the drying process of aeroge have obtained qualitative leap, have overcome drying process
In solid powdering and structure collapses caused by surface tension is present, be greatly promoted aeroge to more refining
Direction is developed, and aeroge solia particle is more refined, and micropore is more evenly distributed, so that the density of aerogel material is lower, hole
Rate is higher, and intensity is significantly improved, and aeroge has preferable mechanical performance in addition, thus it is in high temperature resistant heat insulation material, sound
The aspect such as impedance lotus root condensation material, gas absorption and seperation film, effective catalyst and its carrier has extensive purposes.
Lithium ion battery negative material mainly has graphite, metal oxide, silica-base material etc., and nano-silicon has more negative than graphite
Pole material theoretical specific capacity higher, is the research emphasis of the negative material of current lithium ion battery.But in cyclic process
Silicon causes efflorescence effect due to stereomutation effect, and the problem for causing capacity attenuation too fast is the Main Bottleneck for limiting its application.
By the nanosizing of active material, the volumetric expansion during lithiumation can be effectively prevented from, because aerosil is
It is made up of ultra-fine grain, reduction treatment is carried out to it, obtained the porous structure material with nanostructured, with good electricity
Chemical property, can be as lithium ion battery negative material.
The content of the invention
The present invention is prepared for aerosil by sol-gel process, is then reduced by magnesium powder and obtains nano-silicon
, in the reduction process of silica, there is the defect of following several respects using traditional magnesium reduction process in aeroge:
1. severe reaction conditions;
2. course of reaction can generate Mg2Si impurity;
3. reduction reaction process yields are relatively low;
In order to solve above-mentioned problem, the present invention, will the Mg that produces of reduction process by two step reduction method2Si is by changing
Method is removed, and we employ the oxidation reaction of magnesium silicide and oxygen here, and magnesium silicide is converted into silicon and magnesia.It is this
Method not only successfully eliminates magnesium silicide, improves the purity of nanometer silica aerogel, and substantially increases the yield of reaction.
In order to solve the technical problem existing for above-mentioned reducing silica, the present invention is adopted the following technical scheme that.
1. high temperature is forged under an argon atmosphere sol-gel process to be prepared into the mixture of aerosil and magnesium powder
Burn, specific technical scheme is as follows:
Aerosil and magnesium powder are well mixed by certain mass ratio, first it is risen under argon gas protection in tube furnace
Warm speed is 20C/min, 6000C high-temperature calcinations, are slowly dropped to room temperature after some time.
2., by the said goods high-temperature calcination in air atmosphere, specific technical scheme is as follows:
(1) it is 5 product obtained above to be continued into heating rate in air atmosphere0C/min, 6000C high-temperature calcinations are some
Hour, obtain magnesia/nanometer Silica Aerogels;
(2) product for obtaining is reduced due to generation magnesia and the silica not being reduced sufficiently by magnesium powder, be after
Treatment can just obtain pure product, and the present invention takes liquid phase reactor to be removed, and specific step is as follows:
(3) removal of impurities of magnesia:The silica aerogel containing oxidation magnesium addition that will be obtained is placed in beaker, adds 1.5 mol/L
Hydrochloric acid, 24 h are wherein sufficiently stirred for by both mixed solutions in magnetic agitation, and the turbid solution that will be obtained is obtained by centrifugation
To the product for not containing magnesia, then it is vacuum dried and is obtained solid for future use.
(4) removal of impurities of silica:Solid obtained above is placed in beaker, 1.0 mol/L HF are added, incite somebody to action both
Mixed solution be wherein sufficiently stirred for 24 h in magnetic agitation, the turbid solution that will be obtained is by being centrifugally separating to obtain without titanium dioxide
The nanometer silica aerogel of silicon.
By above-mentioned experimental procedure, pure nano-silicon is finally given, compared to the reduction of general silica, this
Not only productivity ratio is higher for invention method used, and the purity of the product for obtaining is very high.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of lithium ion battery negative material nanometer silica aerogel.
Fig. 2 is cycle performance figure of the lithium ion battery negative material nanometer silica aerogel under 0.1 C current densities.
Fig. 3 is charge and discharge electrograph of the lithium ion battery negative material nanometer silica aerogel under 0.1 C current densities.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings, and following examples are explanation of the invention, this
Invention is not limited to following examples.
Embodiment 1:
Aerosil is prepared by sol-gel process first:With tetraethyl orthosilicate as raw material, by tetraethyl orthosilicate:Water:
The volume ratio of alcohol is 1:4.2:8, water and ethanol are added, the mixed solution of three is stirred into 12 h, it is then molten with 1mol/L oxalic acid
Liquid regulation PH is 3.2, and mixed solution static some days at room temperature are fully hydrolyzed the silester in mixed solution, constantly
Ammonia spirit is slowly added under stirring controls PH to obtain silica hydrosol for 7.2, and gained silica hydrosol is in room temperature
It is lower to stand to generation gel, by gel aging 3 days at room temperature, the aging gel for finishing is put into n-hexane and is soaked, every
Change n-hexane once within 12 hours, to extract the water in wet gel and ethanol, the n-hexane of the gel surface that will finally obtain is removed
Go, gel is dried using supercritical fluid drying technology, that is, obtain aerosil.
Aerosil reduction obtains nano-silicon:By aerosil:The mass ratio of magnesium powder is 1:2 accurate titles
The g of the aerosil 0.76 and g of magnesium powder 1.52 is taken, then both is well mixed, nitrogen protection in tube furnace by it
Lower 6000C high-temperature calcinations, heating rate is 20C/min, room temperature is slowly dropped to after 10 h of insulation, then in air atmosphere 6000The h of C high-temperature calcinations 5, heating rate is 50C/min, is slowly dropped to room temperature, obtains magnesia/nano silicon material.
The removal of impurities of magnesia:After being fully ground, weigh the nano-silicon containing oxidation magnesium addition and be placed in 50 mL beakers, plus
Enter the mL of 1.5 mol/L hydrochloric acid 25, both mixed solutions are sufficiently stirred for 24 h in magnetic stirring apparatus, the muddiness that will be obtained
Liquid passes through to be centrifugally separating to obtain the product for not containing magnesia.
The removal of impurities of silica:The nano-silicon for weighing the above-mentioned removing magnesia of 0.38g is placed in 50 mL beakers, adds 1.0
The mL of mol/L hydrofluoric acid 25,24 h are sufficiently stirred for by both mixed solutions in magnetic stirring apparatus, and the turbid solution that will be obtained leads to
Cross and be centrifugally separating to obtain the nano-silicon for not containing impurity, finally by the nano-silicon 70 in vacuum drying chamber0C dries 12 h and obtains
To product.
According to nano-silicon:Acetylene black:Kynoar=8:1:The ratio of 1 (mass ratio) accurately weighs nano-silicon, acetylene black
It is well mixed with Kynoar, appropriate 1-METHYLPYRROLIDONE is drawn, drip has the measuring cup of Kynoar in drop in advance
In, stirred in constant-temperature heating magnetic stirring apparatus, uniform sample will be ground and be added thereto, 24 h systems are stirred together
Into slurry.With copper sheet as collector, slurry is coated uniformly on Copper Foil, circular electrode pole piece is stamped into after vacuum drying, used
Assay balance claim pole piece and metal copper sheet quality, thus can calculate the quality of active material nano-silicon, be to electricity with lithium piece
Pole nano-silicon is negative pole, and the barrier film selection standard films of Celgard 2400, electrolyte selects 1 mol/L LiPF6/EMC+DC+EC
(Volume ratio is 1:1:1), from the button cell shell of 2016 types, its assembling process is in the hand of oxygen and water content less than 1 ppm
Carried out in casing, argon gas protection.The button cell that will be completed carries out constant current charge-discharge test, and charging/discharging voltage scope is
0.01-1.0 V。
Embodiment 2:
Aerosil is prepared by sol-gel process first:With tetraethyl orthosilicate as raw material, by tetraethyl orthosilicate:Water:
The volume ratio of alcohol is 1:4:8, water and ethanol are added, the mixed solution of three is stirred into 12 h, then use 1mol/L oxalic acid solutions
Regulation PH is 3.6, and mixed solution static 2 days at room temperature is fully hydrolyzed the silester in mixed solution, is stirred continuously down
Being slowly added to ammonia spirit controls PH to obtain silica hydrosol for 7.2, and gained silica hydrosol stands at room temperature
To generation gel, by gel aging 3 days at room temperature, the aging gel for finishing is put into n-hexane and is soaked, every 12 hours
Change n-hexane once, to extract the water in wet gel and ethanol, the n-hexane of the gel surface that will finally obtain is removed, and is used
Supercritical fluid drying technology is dried to gel, that is, obtain aerosil.
Aerosil reduction obtains nano-silicon:By aerosil:The mass ratio of magnesium powder is 1:1 accurate title
The g of the aerosil 0.38 and g of magnesium powder 0.38 is taken, then both is well mixed, nitrogen protection in tube furnace by it
Lower 6000C high-temperature calcinations, heating rate is 20C/min, room temperature is slowly dropped to after 10 h of insulation, then in air atmosphere 6000The h of C high-temperature calcinations 5, heating rate is 50C/min, is slowly dropped to room temperature, obtains magnesia/nano silicon material.
The removal of impurities of magnesia:After being fully ground, weigh 0.26 g contain oxidation magnesium addition nano-silicon be placed in 50 mL beakers
It is interior, the mL of 1.5 mol/L hydrochloric acid 25 is added, both mixed solutions are sufficiently stirred for 24 h in magnetic stirring apparatus, by what is obtained
Turbid solution passes through to be centrifugally separating to obtain the product for not containing magnesia.
The removal of impurities of silica:The nano-silicon for weighing above-mentioned removing magnesia is placed in 50 mL beakers, adds 1.0 mol/
The mL of L hydrofluoric acid 25,24 h are sufficiently stirred for by both mixed solutions in magnetic stirring apparatus, the turbid solution that will be obtained by from
The isolated nano-silicon for not containing impurity of the heart, finally 70 in vacuum drying chamber0C dries 12 h and obtains product.
According to nano-silicon:Acetylene black:Kynoar=8:1:The ratio of 1 (mass ratio) accurately weighs nano-silicon, acetylene black
It is well mixed with Kynoar, appropriate 1-METHYLPYRROLIDONE is drawn, drip has the measuring cup of Kynoar in drop in advance
In, stirred in constant-temperature heating magnetic stirring apparatus, uniform sample will be ground and be added thereto, 24 h systems are stirred together
Into slurry.With copper sheet as collector, slurry is coated uniformly on Copper Foil, circular electrode pole piece is stamped into after vacuum drying, used
Assay balance claim pole piece and metal copper sheet quality, thus can calculate the quality of active material nano-silicon, be to electricity with lithium piece
Pole nano-silicon is negative pole, and the barrier film selection standard films of Celgard 2400, electrolyte selects 1 mol/L LiPF6/EMC+DC+EC
(Volume ratio is 1:1:1), from the button cell shell of 2016 types, its assembling process is in the hand of oxygen and water content less than 1 ppm
Carried out in casing, argon gas protection.The button cell that will be completed carries out constant current charge-discharge test, and charging/discharging voltage scope is
0.01~1.0 V。
Embodiment 3:
Aerosil is prepared by sol-gel process first:With tetraethyl orthosilicate as raw material, by tetraethyl orthosilicate:Water:
The volume ratio of alcohol is 1:4:8, water and ethanol are added, the mixed solution of three is stirred into 12 h, then use 1mol/L oxalic acid solutions
Regulation PH is 3.6, and mixed solution static 2 days at room temperature is fully hydrolyzed the silester in mixed solution, is stirred continuously down
Being slowly added to ammonia spirit controls PH to obtain silica hydrosol for 7.2, and gained silica hydrosol stands at room temperature
To generation gel, by gel aging 3 days at room temperature, the aging gel for finishing is put into n-hexane and is soaked, every 12 hours
Change n-hexane once, to extract the water in wet gel and ethanol, the n-hexane of the gel surface that will finally obtain is removed, and is used
Supercritical fluid drying technology is dried to gel, that is, obtain aerosil.
Aerosil reduction obtains nano-silicon:By aerosil:The mass ratio of magnesium powder is 1:2 accurate titles
The g of the aerosil 1.52 and g of magnesium powder 3.04 is taken, then both is well mixed, nitrogen protection in tube furnace by it
Lower 6000C high-temperature calcinations, heating rate is 20C/min, room temperature is slowly dropped to after 10 h of insulation, then in air atmosphere 7000The h of C high-temperature calcinations 5, heating rate is 50C/min, is slowly dropped to room temperature, obtains magnesia/nano silicon material.
The removal of impurities of magnesia:After being fully ground, weigh 0.52 g contain oxidation magnesium addition silica aerogel be placed in 50 mL burning
In cup, the mL of 1.5 mol/L hydrochloric acid 25 is added, both mixed solutions are sufficiently stirred for 24 h in magnetic stirring apparatus, will obtained
Turbid solution pass through to be centrifugally separating to obtain the product that does not contain magnesia.
The removal of impurities of silica:The nano-silicon for weighing above-mentioned removing magnesia is placed in 50 mL beakers, adds 1.0 mol/
The mL of L hydrofluoric acid 25,24 h are sufficiently stirred for by both mixed solutions in magnetic stirring apparatus, the turbid solution that will be obtained by from
The isolated nano-silicon for not containing impurity of the heart, finally by the nanometer silica gel 70 in vacuum drying chamber0C dries 12 h and obtains
Product.
According to nano-silicon:Acetylene black:Kynoar=8:1:The ratio of 1 (mass ratio) accurately weighs nano-silicon, acetylene black
It is well mixed with Kynoar, appropriate 1-METHYLPYRROLIDONE is drawn, drip has the measuring cup of Kynoar in drop in advance
In, stirred in constant-temperature heating magnetic stirring apparatus, uniform sample will be ground and be added thereto, 24 h systems are stirred together
Into slurry.With copper sheet as collector, slurry is coated uniformly on Copper Foil, circular electrode pole piece is stamped into after vacuum drying, used
Assay balance claim pole piece and metal copper sheet quality, thus can calculate the quality of active material nano-silicon, be to electricity with lithium piece
Pole nano-silicon is negative pole, and the barrier film selection standard films of Celgard 2400, electrolyte selects 1 mol/L LiPF6/EMC+DC+EC
(Volume ratio is 1:1:1), from the button cell shell of 2016 types, its assembling process is in the hand of oxygen and water content less than 1 ppm
Carried out in casing, argon gas protection.The button cell that will be completed carries out constant current charge-discharge test, and charging/discharging voltage scope is
0.01-1.0 V。
Embodiment 4:
Aerosil is prepared by sol-gel process first:With tetraethyl orthosilicate as raw material, by tetraethyl orthosilicate:Water:
The volume ratio of alcohol is 1:4:8, water and ethanol are added, the mixed solution of three is stirred into 12 h, then with 1 mol/L oxalic acid solutions
Regulation PH is 3.6, and mixed solution static 2 days at room temperature is fully hydrolyzed the silester in mixed solution, is stirred continuously down
Being slowly added to ammonia spirit controls PH to obtain silica hydrosol for 7.2, and gained silica hydrosol stands at room temperature
To generation gel, by gel aging 3 days at room temperature, the aging gel for finishing is put into n-hexane and is soaked, every 12 hours
Change n-hexane once, to extract the water in wet gel and ethanol, the n-hexane of the gel surface that will finally obtain is removed, and is used
Supercritical fluid drying technology is dried to gel, that is, obtain aerosil.
Aerosil reduction obtains nano-silicon:By aerosil:The mass ratio of magnesium powder is 1:1 accurate title
The g of the aerosil 0.76 and g of magnesium powder 0.76 is taken, then both is well mixed, nitrogen protection in tube furnace by it
Lower 6000C high-temperature calcinations, heating rate is 20C/min, room temperature is slowly dropped to after 10 h of insulation, then in air atmosphere 7000The h of C high-temperature calcinations 5, heating rate is 50C/min, is slowly dropped to room temperature, obtains magnesia/nano silicon material.
The removal of impurities of magnesia:After being fully ground, weigh 0.52 g contain oxidation magnesium addition nano-silicon be placed in 50 mL beakers
It is interior, the mL of 1.5 mol/L hydrochloric acid 25 is added, both mixed solutions are sufficiently stirred for 24 h in magnetic stirring apparatus, by what is obtained
Turbid solution passes through to be centrifugally separating to obtain the product for not containing magnesia.
The removal of impurities of silica:The nano-silicon for weighing removing magnesia is placed in 50 mL beakers, adds 1.0 mol/L hydrogen
The mL of fluoric acid 25,24 h are sufficiently stirred for by both mixed solutions in magnetic stirring apparatus, and the turbid solution that will be obtained is by centrifugation point
From the nano-silicon for obtaining not containing impurity, finally by the nano-silicon 70 in vacuum drying chamber0C dries 12 h and obtains product.
According to nano-silicon:Acetylene black:Kynoar=8:1:The ratio of 1 (mass ratio) accurately weighs nano-silicon, acetylene black
It is well mixed with Kynoar, appropriate 1-METHYLPYRROLIDONE is drawn, drip has the measuring cup of Kynoar in drop in advance
In, stirred in constant-temperature heating magnetic stirring apparatus, uniform sample will be ground and be added thereto, 24 h systems are stirred together
Into slurry.With copper sheet as collector, slurry is coated uniformly on Copper Foil, circular electrode pole piece is stamped into after vacuum drying, used
Assay balance claim pole piece and metal copper sheet quality, thus can calculate the quality of active material nano-silicon, be to electricity with lithium piece
Pole nano-silicon is negative pole, and the barrier film selection standard films of Celgard 2400, electrolyte selects 1 mol/L LiPF6/EMC+DC+EC
(Volume ratio is 1:1:1), from the button cell shell of 2016 types, its assembling process is in the hand of oxygen and water content less than 1 ppm
Carried out in casing, argon gas protection.The button cell that will be completed carries out constant current charge-discharge test, and charging/discharging voltage scope is
0.01~1.0 V。
Claims (9)
1. the preparation method of aerosil, it is characterised in that:Suitable estersil is selected, is added according to certain mol ratio
Distilled water and solvent, positive silicic acid is made by three after well mixed with static for a long time at room temperature after certain acid solution regulation PH
Ethyl ester is fully hydrolyzed, and is stirred continuously down and is slowly added to aqueous slkali, and silica hydrosol is obtained by controlling PH, stood to
Generation gel, is soaked during the aging gel for finishing under the uniform temperature and solvent is put into n-hexane, and solvent three is changed in 72 h
It is secondary, to remove the water in wet gel and ethanol, supercritical fluid drying is carried out after liquid is removed, that is, obtain silica airsetting
Glue.
2. the preparation of nanometer silica aerogel, it is characterised in that:Aerosil and magnesium powder are mixed by certain mass ratio
Uniformly, first by it in the tube furnace high-temperature calcination some hours under nitrogen protection, after being slowly dropped to room temperature, then in air atmosphere
High-temperature calcination some hours, obtain magnesia/nano silicon material;After being fully ground, the magnesia in mixture is removed with hydrochloric acid
Impurity, vacuum drying obtains pure nanometer silica aerogel.
3. application of nanometer silica aerogel in lithium ion battery, it is characterised in that with nanometer silica aerogel as lithium-ion electric
The techniques such as pond Electrode material, addition conductive agent and binding agent are by sizing mixing, being coated with, compressing tablet prepare electrode slice, are made with lithium piece
It is that, to electrode, assembling obtains button cell and tests its chemical property.
4. according to claim 1 aerosil preparation, it is characterised in that:The nanometer of aerosil
The average grain diameter of particle is between 100 ~ 150 nm, density is 0.5 ~ 3 mg/cm3。
5. the preparation of silica aerogel according to claim 2, it is characterised in that:The quality of aerosil and magnesium powder
Than being 1:2 and 1:1.
6. the preparation of silica aerogel according to claim 2, it is characterised in that:The particle diameter of magnesium powder used is 200 nm.
7. the preparation of silica aerogel according to claim 2, it is characterised in that:Argon gas atmosphere high-temperature calcination is 10 h, is risen
Warm speed is 20C/min, the h of air atmosphere high-temperature calcination 5, heating rate is 50C/min。
8. the preparation of silica aerogel according to claim 2, it is characterised in that:The concentration of hydrochloric acid is used by removing magnesia
1.5 mol/L, the concentration for removing the hydrofluoric acid used by silica is 1.0 mol/L.
9. the according to claim 3 nanometer of preparation of silica aerogel, it is characterised in that:Using gained nano-silicon as lithium ion
Cell negative electrode material, its first discharge specific capacity is 1720 mAhg-1, capacity is maintained at left and right 51.3% or so after circulating 50 times.
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CN109755507A (en) * | 2018-12-18 | 2019-05-14 | 湘潭大学 | A kind of preparation method of lithium ion battery silicon/carbon composite aerogel negative electrode material |
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CN108565441A (en) * | 2018-05-29 | 2018-09-21 | 郑州中科新兴产业技术研究院 | A kind of preparation method of silica plural gel and the three-dimensional porous silicium cathode material prepared using the gel |
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CN109638269A (en) * | 2018-12-29 | 2019-04-16 | 湖南中科星城石墨有限公司 | A kind of silicon/expanded graphite/agraphitic carbon composite material and preparation method |
CN109950493A (en) * | 2019-03-27 | 2019-06-28 | 东莞东阳光科研发有限公司 | Silica aerogel/micro- swollen graphite composite material, preparation method and application |
CN109950493B (en) * | 2019-03-27 | 2022-02-15 | 东莞东阳光科研发有限公司 | Silicon aerogel/micro-expansion graphite composite material, preparation method and application thereof |
CN110562985A (en) * | 2019-09-23 | 2019-12-13 | 北京化工大学 | preparation method and application of porous silicon nanowire |
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