CN108598384A - A kind of preparation method of composite aerogel negative material - Google Patents
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Abstract
The present invention discloses a kind of preparation method of composite aerogel negative material, butyl titanate is dissolved in ethanol in proper amount and forms solution A, it dissolves chitosan in acetic acid aqueous solution, form solution B, glutaraldehyde is dissolved in absolute ethyl alcohol and forms solution C, carbon nanotube through acid processing is dissolved in lauryl sodium sulfate aqueous solution and obtains suspension D, continue under stirring condition in 50 DEG C of water-baths, by solution B, C and D is slowly added in solution A simultaneously, a small amount of sulfuric acid is added dropwise again, lasting stirring, after completion of the reaction, filtering, first it is washed with distilled water again with ethyl alcohol, it is dried to obtain gel, finally by the xerogel high-temperature calcination, it crushes, sieving, obtain target product.Composite aerogel negative material is made using atmosphere pressure desiccation in the present invention, have it is at low cost, it is simple for process, industrialization large-scale production and the good major advantage of chemical property are easily realized, and synergistic effect can be played, to improve the capacity and cyclical stability of cathode.
Description
Technical field
The present invention relates to negative material field technologies, refer in particular to a kind of preparation method of composite aerogel negative material.
Background technology
New-energy automobile is all being greatly developed in countries in the world, but new-energy automobile is difficult in the presence of charging at present, the charging time is long
Etc. technical problem.Fast charging type lithium ion battery negative material must have the ability for quickly receiving a large amount of Li+, otherwise Li+ meetings
Li dendrite is formed in negative terminal surface deposition, precipitation, generating short circuit leads to security risk.
Traditional graphite cathode material interlamellar spacing is smaller, hinders the quick deintercalations of Li+, analysis lithium and charging are easy under fast charge pattern
Amount substantially reduces, therefore simple graphite cannot function as fast charging type lithium cell cathode material.And the amorphous of porous nano particle
Carbon materials become the ideal material of fast charge negative electrode of lithium ion battery.
Carbon nanotube（CNT）It is the One-dimensional Quantum material with special construction, there is good electric conductivity, excellent mechanics
The specific surface area of performance and super large.Specific capacity is higher for the first time separately as lithium cell negative pole by CNT, but there is irreversible appearance of discharging for the first time
Amount is big, charge and discharge platform unobvious, the shortcomings of after voltage, has both been contributed in charge and discharge process using the one-dimensional porous structures of CNT
Lithium ion being embedded in and moving out, and can be TiO2(B)/carbon aerogels build three-dimensional conductive network.
In recent years, the TiO of nanostructure2It is most popular function energy material, TiO2(B) it is monoclinic phase state layer structure,
And there are small duct, Li+Embedded quantity has preferable charge-discharge characteristics, can be used as a kind of property up to 0.5~1.0Li/Ti
The excellent lithium ion battery negative material of energy.But TiO2(B) loosely organized, specific surface area is small, and conductivity is relatively relatively low, prepares
Of high cost, therefore, adding carbon nanotube by design enhances electric conductivity, and by conventional sol-gel method by outer bread
One layer of carbon is covered, CNT/TiO is constituted2(B)/C composite aerogels.
Chinese invention patent application publication No. CN 105540658A disclose a kind of titanium dioxide cathode material and its preparation
Method, method are：
(1) butyl titanate is added in the mixed liquor of urea-choline chloride ionic liquid, water and glacial acetic acid composition and is carried out instead
Answer, washing filtering, will filter object it is freeze-dried after, roasting, both target product.
(2) the more excellent volume ratio of butyl titanate, ionic liquid, water and glacial acetic acid is：2-4:3-8:3-4:1-2.
It needs to consume larger amount of ionic liquid in the above-mentioned methods, and the mode being freeze-dried is not easy to realize scale
Production, gained titanium dioxide product are Detitanium-ore-type, are assembled into button cell as lithium ion battery negative material, as a result
Show that the cycle performance figure at 0.5C, reversible discharge specific capacity only have 193.2mAh g-1.Specific discharge capacity after 50 circle of cycle
There are 171.9mAh g-1, capacity retention ratio 89.0%.
Chinese invention patent application publication No. CN 105609741A disclose a kind of lithium cell cathode material silica/
The preparation method of titanium dioxide composite aerogel, method are：
（1）By estersil, titanium esters and solvent mixed solution（Solution A）With ethanol/water mixed solution（Solution B）The lower mixing of stirring is equal
It is even, and the precursor solution C of complete clear is obtained by salt acid for adjusting pH value；
（2）Solution will be subtracted and be slowly dropped to above-mentioned precursor solution C, and to obtain earth silicon/titanic oxide compound for control ph
Hydrogel；
（3）The compound hydrosol of gained earth silicon/titanic oxide is stood to generation gel, by gel under certain temperature and solvent
Then sample is carried out supercritical fluid drying to get to earth silicon/titanic oxide composite aerogel by ageing；
（4）Aerosil is prepared by above-mentioned steps (1), (2) and (3) first, then aerosil is added
In the mixed solution of titanium esters, ethyl alcohol and deionized water, by controlling the speed of pH value adjustment titanium esters hydrolysis, make the titanium dioxide of generation
Titanium uniform deposition forms earth silicon/titanic oxide composite aerogel on aerosil.
The above method uses supercritical fluid drying, and complex process is with high costs, and generates a large amount of solvent waste liquids, unfavorable
In environmental protection.The electro-chemical activity of silica is low, which is used as negative electrode of lithium ion battery
When material, the results showed that charging and discharging capacity is 270mAh/g after 500 cycles, and capacity is held only in 71.4%.
Invention content
In view of this, in view of the deficiencies of the prior art, the present invention aims to provide a kind of composite aerogels
The preparation method of negative material can effectively solve existing cathode material preparation method complex process, with high costs and electric
The bad problem of chemical property.
To achieve the above object, the present invention is using following technical solution：
A kind of preparation method of composite aerogel negative material, includes following steps：
（1）It weighs 20-30g butyl titanates to be dissolved in 40-60mL absolute ethyl alcohols, adds 80-120mL nitric acid and form solution
A；
（2）The chitosan 8-12g for weighing deacetylation 90%, it is that 2% acetic acid is molten to be added with stirring 130-170mL mass concentrations
It is dissolved in liquid, forms transparent solution B；
（3）It weighs 1-2g glutaraldehydes and is dissolved in 80-120mL ethyl alcohol and prepare solution C；
（4）After carbon nanotube is ultrasonically treated with nitration mixture, weighs 0.08-0.12g carbon nanotubes and be added in 170-230mL water, then
0.01-0.03g lauryl sodium sulfate is added, is sufficiently stirred and ultrasonic wave dispersion 50-70min forms suspension D；
（5）Under 40-60 DEG C of stirred in water bath, solution B and C and suspension D are slowly added into solution A simultaneously, fully stirred
It mixes 20-40 minutes, then the 8-12mL concentrated sulfuric acids is slowly added dropwise, be sufficiently stirred 6-10 hours, reaction finishes, and stands 3-5 hours, mistake
Filter, is then washed with ethyl alcohol, then is washed to pH=5~7 with distillation；
（6）70-90 DEG C of vacuum drying obtains xerogel in 8-12 hours, which is crushed, is fitted into tube furnace, under argon gas protection
It is preheated to 400-600 DEG C with 2 °/min, insulation reaction 2-8 hours then cools to room temperature, obtains final products.
As a preferred embodiment, the step（4）Middle carbon nanotube is multi-walled carbon nanotube.
As a preferred embodiment, the nitration mixture is the concentrated sulfuric acid and concentrated nitric acid, volume ratio 1:1.
As a preferred embodiment, the step（6）In be preheated to 450 DEG C, insulation reaction 6 hours.
The present invention has clear advantage and advantageous effect compared with prior art, specifically, by above-mentioned technical proposal
Known to：
Composite aerogel negative material is made using atmosphere pressure desiccation in the present invention, has at low cost, simple for process, easily realization industry
The major advantage that change mass produces and chemical property is good, and synergistic effect can be played, to improve the capacity and cycle of cathode
Stability.
Specific implementation mode
Present invention is disclosed a kind of preparation methods of composite aerogel negative material, include following steps：
（1）It weighs 20-30g butyl titanates to be dissolved in 40-60mL absolute ethyl alcohols, adds 80-120mL nitric acid and form solution
A。
（2）The chitosan 8-12g for weighing deacetylation 90%, it is 2% second to be added with stirring 130-170mL mass concentrations
It is dissolved in acid solution, forms transparent solution B.
（3）It weighs 1-2g glutaraldehydes and is dissolved in 80-120mL ethyl alcohol and prepare solution C.
（4）After carbon nanotube is ultrasonically treated with nitration mixture, weighs 0.08-0.12g carbon nanotubes and be added to 170-230mL water
In, 0.01-0.03g lauryl sodium sulfate is added, is sufficiently stirred and ultrasonic wave dispersion 50-70min forms suspension D.Institute
It is multi-walled carbon nanotube to state carbon nanotube, and the nitration mixture is the concentrated sulfuric acid and concentrated nitric acid, volume ratio 1:1.
（5）Under 40-60 DEG C of stirred in water bath, solution B and C and suspension D are slowly added into solution A simultaneously, filled
Dividing stirring 20-40 minutes, then the 8-12mL concentrated sulfuric acids are slowly added dropwise, is sufficiently stirred 6-10 hours, reaction finishes, and stands 3-5 hours,
Filtering, is then washed with ethyl alcohol, then is washed to pH=5~7 with distillation.
（6）70-90 DEG C of vacuum drying obtains xerogel in 8-12 hours, which is crushed, is fitted into tube furnace, argon gas is protected
It is preheated to 400-600 DEG C with 2 °/min under shield, insulation reaction 2-8 hours then cools to room temperature, obtains final products.
With multiple embodiments, invention is further described in detail below：
Embodiment 1：
A kind of preparation method of composite aerogel negative material, includes following steps：
（1）It weighs 25.2g butyl titanates to be dissolved in 50mL absolute ethyl alcohols, adds 100mL nitric acid and form solution A.
（2）The chitosan 10g for weighing deacetylation 90%, it is 2% acetic acid solution to be added with stirring 150mL mass concentrations
Middle dissolving forms transparent solution B.
（3）It weighs 1.5g glutaraldehydes and is dissolved in 100mL ethyl alcohol and prepare solution C.
（4）After carbon nanotube is ultrasonically treated with nitration mixture, weighs 0.1g carbon nanotubes and be added in 200mL water, add
0.02g lauryl sodium sulfate, is sufficiently stirred and ultrasonic wave dispersion 60min forms suspension D.The carbon nanotube is multi wall carbon
Nanotube, the nitration mixture are the concentrated sulfuric acid and concentrated nitric acid, volume ratio 1:1.
（5）Under 50 DEG C of stirred in water bath, solution B and C and suspension D are slowly added into solution A simultaneously, fully stirred
It mixes 30 minutes, then the 10mL concentrated sulfuric acids is slowly added dropwise, be sufficiently stirred 8 hours, reaction finishes, and stands 4 hours, and second is then used in filtering
Alcohol washs, then is washed to pH=5~7 with distillation.
（6）80 DEG C of vacuum drying obtain xerogel in 10 hours, which is crushed, is fitted into tube furnace, under argon gas protection
450 DEG C are preheated to 2 °/min, insulation reaction 6 hours then cools to room temperature, obtains final products.
It is anode with composite aerogel negative material obtained above, lithium piece is cathode, and electrolyte is 1mol/L's
LiPF6 solution, diaphragm are 2400 standard films of Celgard, and button cell is made in glove box, carries out constant current charge-discharge test,
Charging/discharging voltage is 0.01V~2.5V, current density 200mA.g-1's.It measures the composite aerogel negative material and puts for the first time and fill
Capacitance is respectively 352mAh/g, and reversible capacity is 315mAh/g after 400 cycles, and discharge capacity cycle is kept for the first time relatively
Rate is 96%, shows that the negative material has preferable chemical property.
Embodiment 2：
A kind of preparation method of composite aerogel negative material, includes following steps：
（1）It weighs 20g butyl titanates to be dissolved in 58mL absolute ethyl alcohols, adds 80mL nitric acid and form solution A.
（2）The chitosan 12g for weighing deacetylation 90%, it is 2% acetic acid solution to be added with stirring 160mL mass concentrations
Middle dissolving forms transparent solution B.
（3）It weighs 1.3g glutaraldehydes and is dissolved in 90mL ethyl alcohol and prepare solution C.
（4）After carbon nanotube is ultrasonically treated with nitration mixture, weighs 0.08g carbon nanotubes and be added in 220mL water, add
0.03g lauryl sodium sulfate, is sufficiently stirred and ultrasonic wave dispersion 52min forms suspension D.The carbon nanotube is multi wall carbon
Nanotube, the nitration mixture are the concentrated sulfuric acid and concentrated nitric acid, volume ratio 1:1.
（5）Under 45 DEG C of stirred in water bath, solution B and C and suspension D are slowly added into solution A simultaneously, fully stirred
It mixes 28 minutes, then the 8mL concentrated sulfuric acids is slowly added dropwise, be sufficiently stirred 6 hours, reaction finishes, and stands 3 hours, and ethyl alcohol is then used in filtering
Washing, then it is washed to pH=5~7 with distillation.
（6）70 DEG C vacuum drying 8 hours xerogel, which is crushed, is fitted into tube furnace, argon gas protect under with
2 °/min is preheated to 500 DEG C, and insulation reaction 2 hours then cools to room temperature, obtains final products.
It is anode with composite aerogel negative material obtained above, lithium piece is cathode, and electrolyte is 1mol/L's
LiPF6 solution, diaphragm are 2400 standard films of Celgard, and button cell is made in glove box, carries out constant current charge-discharge test,
Charging/discharging voltage is 0.01V~2.5V, current density 200mA.g-1's.It measures the composite aerogel negative material and puts for the first time and fill
Capacitance is respectively 340mAh/g, and reversible capacity is 302mAh/g after 400 cycles, and discharge capacity cycle is kept for the first time relatively
Rate is 91%, shows that the negative material has preferable chemical property.
Embodiment 3：
A kind of preparation method of composite aerogel negative material, includes following steps：
（1）It weighs 30g butyl titanates to be dissolved in 48mL absolute ethyl alcohols, adds 110mL nitric acid and form solution A.
（2）The chitosan 11g for weighing deacetylation 90%, it is 2% acetic acid solution to be added with stirring 130mL mass concentrations
Middle dissolving forms transparent solution B.
（3）It weighs 1g glutaraldehydes and is dissolved in 80mL ethyl alcohol and prepare solution C.
（4）After carbon nanotube is ultrasonically treated with nitration mixture, weighs 0.12g carbon nanotubes and be added in 210mL water, add
0.01g lauryl sodium sulfate, is sufficiently stirred and ultrasonic wave dispersion 50min forms suspension D.The carbon nanotube is multi wall carbon
Nanotube, the nitration mixture are the concentrated sulfuric acid and concentrated nitric acid, volume ratio 1:1.
（5）Under 40 DEG C of stirred in water bath, solution B and C and suspension D are slowly added into solution A simultaneously, fully stirred
It mixes 20 minutes, then the 11mL concentrated sulfuric acids is slowly added dropwise, be sufficiently stirred 7 hours, reaction finishes, and stands 5 hours, and second is then used in filtering
Alcohol washs, then is washed to pH=5~7 with distillation.
（6）90 DEG C vacuum drying 9 hours xerogel, which is crushed, is fitted into tube furnace, argon gas protect under with
2 °/min is preheated to 600 DEG C, and insulation reaction 4 hours then cools to room temperature, obtains final products.
It is anode with composite aerogel negative material obtained above, lithium piece is cathode, and electrolyte is 1mol/L's
LiPF6 solution, diaphragm are 2400 standard films of Celgard, and button cell is made in glove box, carries out constant current charge-discharge test,
Charging/discharging voltage is 0.01V~2.5V, current density 200mA.g-1's.It measures the composite aerogel negative material and puts for the first time and fill
Capacitance is respectively 326mAh/g, and reversible capacity is 301mAh/g after 400 cycles, and discharge capacity cycle is kept for the first time relatively
Rate is 93%, shows that the negative material has preferable chemical property.
Embodiment 4：
A kind of preparation method of composite aerogel negative material, includes following steps：
（1）It weighs 24g butyl titanates to be dissolved in 45mL absolute ethyl alcohols, adds 120mL nitric acid and form solution A.
（2）The chitosan 8g for weighing deacetylation 90%, it is in 2% acetic acid solution to be added with stirring 140mL mass concentrations
Dissolving, forms transparent solution B.
（3）It weighs 1.6g glutaraldehydes and is dissolved in 110mL ethyl alcohol and prepare solution C.
（4）After carbon nanotube is ultrasonically treated with nitration mixture, weighs 0.11g carbon nanotubes and be added in 170mL water, add
0.012g lauryl sodium sulfate, is sufficiently stirred and ultrasonic wave dispersion 68min forms suspension D.The carbon nanotube is multi wall
Carbon nanotube, the nitration mixture are the concentrated sulfuric acid and concentrated nitric acid, volume ratio 1:1.
（5）Under 55 DEG C of stirred in water bath, solution B and C and suspension D are slowly added into solution A simultaneously, fully stirred
It mixes 35 minutes, then the 12mL concentrated sulfuric acids is slowly added dropwise, be sufficiently stirred 9 hours, reaction finishes, and stands 3.8 hours, and filtering is then used
Ethyl alcohol washs, then is washed to pH=5~7 with distillation.
（6）72 DEG C of vacuum drying obtain xerogel in 11 hours, which is crushed, is fitted into tube furnace, under argon gas protection
400 DEG C are preheated to 2 °/min, insulation reaction 8 hours then cools to room temperature, obtains final products.
It is anode with composite aerogel negative material obtained above, lithium piece is cathode, and electrolyte is 1mol/L's
LiPF6 solution, diaphragm are 2400 standard films of Celgard, and button cell is made in glove box, carries out constant current charge-discharge test,
Charging/discharging voltage is 0.01V~2.5V, current density 200mA.g-1's.It measures the composite aerogel negative material and puts for the first time and fill
Capacitance is respectively 332mAh/g, and reversible capacity is 300mAh/g after 400 cycles, and discharge capacity cycle is kept for the first time relatively
Rate is 94%, shows that the negative material has preferable chemical property.
Embodiment 5：
A kind of preparation method of composite aerogel negative material, includes following steps：
（1）It weighs 28g butyl titanates to be dissolved in 55mL absolute ethyl alcohols, adds 90mL nitric acid and form solution A.
（2）The chitosan 9g for weighing deacetylation 90%, it is in 2% acetic acid solution to be added with stirring 170mL mass concentrations
Dissolving, forms transparent solution B.
（3）It weighs 2g glutaraldehydes and is dissolved in 120mL ethyl alcohol and prepare solution C.
（4）After carbon nanotube is ultrasonically treated with nitration mixture, weighs 0.09g carbon nanotubes and be added in 180mL water, add
0.018g lauryl sodium sulfate, is sufficiently stirred and ultrasonic wave dispersion 70min forms suspension D.The carbon nanotube is multi wall
Carbon nanotube, the nitration mixture are the concentrated sulfuric acid and concentrated nitric acid, volume ratio 1:1.
（5）Under 60 DEG C of stirred in water bath, solution B and C and suspension D are slowly added into solution A simultaneously, fully stirred
It mixes 40 minutes, then the 9mL concentrated sulfuric acids is slowly added dropwise, be sufficiently stirred 10 hours, reaction finishes, and stands 4.5 hours, and filtering is then used
Ethyl alcohol washs, then is washed to pH=5~7 with distillation.
（6）76 DEG C of vacuum drying obtain xerogel in 12 hours, which is crushed, is fitted into tube furnace, under argon gas protection
450 DEG C are preheated to 2 °/min, insulation reaction 5 hours then cools to room temperature, obtains final products.
It is anode with composite aerogel negative material obtained above, lithium piece is cathode, and electrolyte is 1mol/L's
LiPF6 solution, diaphragm are 2400 standard films of Celgard, and button cell is made in glove box, carries out constant current charge-discharge test,
Charging/discharging voltage is 0.01V~2.5V, current density 200mA.g-1's.It measures the composite aerogel negative material and puts for the first time and fill
Capacitance is respectively 343mAh/g, and reversible capacity is 306mAh/g after 400 cycles, and discharge capacity cycle is kept for the first time relatively
Rate is 91%, shows that the negative material has preferable chemical property.
Embodiment 6：
A kind of preparation method of composite aerogel negative material, includes following steps：
（1）It weighs 23g butyl titanates to be dissolved in 52mL absolute ethyl alcohols, adds 95mL nitric acid and form solution A.
（2）The chitosan 10.5g for weighing deacetylation 90%, it is that 2% acetic acid is molten to be added with stirring 168mL mass concentrations
It is dissolved in liquid, forms transparent solution B.
（3）It weighs 1.8g glutaraldehydes and is dissolved in 118mL ethyl alcohol and prepare solution C.
（4）After carbon nanotube is ultrasonically treated with nitration mixture, weighs 0.095g carbon nanotubes and be added in 230mL water, add
0.025g lauryl sodium sulfate, is sufficiently stirred and ultrasonic wave dispersion 64min forms suspension D.The carbon nanotube is multi wall
Carbon nanotube, the nitration mixture are the concentrated sulfuric acid and concentrated nitric acid, volume ratio 1:1.
（5）Under 58 DEG C of stirred in water bath, solution B and C and suspension D are slowly added into solution A simultaneously, fully stirred
It mixes 32 minutes, then the 9.8mL concentrated sulfuric acids is slowly added dropwise, be sufficiently stirred 7.8 hours, reaction finishes, and stands 3.2 hours, filtering, then
It is washed with ethyl alcohol, then pH=5~7 is washed to distillation.
（6）85 DEG C of vacuum drying obtain xerogel in 8.8 hours, which is crushed, is fitted into tube furnace, under argon gas protection
550 DEG C are preheated to 2 °/min, insulation reaction 3 hours then cools to room temperature, obtains final products.
It is anode with composite aerogel negative material obtained above, lithium piece is cathode, and electrolyte is 1mol/L's
LiPF6 solution, diaphragm are 2400 standard films of Celgard, and button cell is made in glove box, carries out constant current charge-discharge test,
Charging/discharging voltage is 0.01V~2.5V, current density 200mA.g-1's.It measures the composite aerogel negative material and puts for the first time and fill
Capacitance is respectively 341mAh/g, and reversible capacity is 308mAh/g after 400 cycles, and discharge capacity cycle is kept for the first time relatively
Rate is 94%, shows that the negative material has preferable chemical property.
The design focal point of the present invention is：Composite aerogel negative material is made using atmosphere pressure desiccation in the present invention, has
It is at low cost, it is simple for process, easily realize industrialization large-scale production and the good major advantage of chemical property, and can play to cooperate with and imitate
It answers, to improve the capacity and cyclical stability of cathode.
The above described is only a preferred embodiment of the present invention, be not intended to limit the scope of the present invention,
Therefore it is every according to the technical essence of the invention to any subtle modifications, equivalent variations and modifications made by above example, still
Belong in the range of technical solution of the present invention.
Claims (4)
1. a kind of preparation method of composite aerogel negative material, it is characterised in that：Include following steps：
（1）It weighs 20-30g butyl titanates to be dissolved in 40-60mL absolute ethyl alcohols, adds 80-120mL nitric acid and form solution
A；
（2）The chitosan 8-12g for weighing deacetylation 90%, it is that 2% acetic acid is molten to be added with stirring 130-170mL mass concentrations
It is dissolved in liquid, forms transparent solution B；
（3）It weighs 1-2g glutaraldehydes and is dissolved in 80-120mL ethyl alcohol and prepare solution C；
（4）After carbon nanotube is ultrasonically treated with nitration mixture, weighs 0.08-0.12g carbon nanotubes and be added in 170-230mL water, then
0.01-0.03g lauryl sodium sulfate is added, is sufficiently stirred and ultrasonic wave dispersion 50-70min forms suspension D；
（5）Under 40-60 DEG C of stirred in water bath, solution B and C and suspension D are slowly added into solution A simultaneously, fully stirred
It mixes 20-40 minutes, then the 8-12mL concentrated sulfuric acids is slowly added dropwise, be sufficiently stirred 6-10 hours, reaction finishes, and stands 3-5 hours, mistake
Filter, is then washed with ethyl alcohol, then is washed to pH=5~7 with distillation；
（6）70-90 DEG C of vacuum drying obtains xerogel in 8-12 hours, which is crushed, is fitted into tube furnace, under argon gas protection
It is preheated to 400-600 DEG C with 2 °/min, insulation reaction 2-8 hours then cools to room temperature, obtains final products.
2. a kind of preparation method of composite aerogel negative material according to claim 1, it is characterised in that：The step
（4）Middle carbon nanotube is multi-walled carbon nanotube.
3. a kind of preparation method of composite aerogel negative material according to claim 1, it is characterised in that：The nitration mixture
For the concentrated sulfuric acid and concentrated nitric acid, volume ratio 1:1.
4. a kind of preparation method of composite aerogel negative material according to claim 1, it is characterised in that：The step
（6）In be preheated to 450 DEG C, insulation reaction 6 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810224078.XA CN108598384A (en) | 2018-03-19 | 2018-03-19 | A kind of preparation method of composite aerogel negative material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810224078.XA CN108598384A (en) | 2018-03-19 | 2018-03-19 | A kind of preparation method of composite aerogel negative material |
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| CN110763377A (en) * | 2019-10-21 | 2020-02-07 | 华南理工大学 | Super-hydrophobic piezoresistive pressure sensor and preparation method and application thereof |
| CN112194180A (en) * | 2020-10-14 | 2021-01-08 | 北京化工大学 | Modification method for enhancing mechanical property of aerogel |
| CN113292078A (en) * | 2021-04-20 | 2021-08-24 | 西安理工大学 | Preparation method of titanium dioxide aerogel |
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| CN112194180A (en) * | 2020-10-14 | 2021-01-08 | 北京化工大学 | Modification method for enhancing mechanical property of aerogel |
| CN113292078A (en) * | 2021-04-20 | 2021-08-24 | 西安理工大学 | Preparation method of titanium dioxide aerogel |
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