CN109133040A - A kind of preparation method of the adjustable graphene aerogel of pore-size - Google Patents
A kind of preparation method of the adjustable graphene aerogel of pore-size Download PDFInfo
- Publication number
- CN109133040A CN109133040A CN201810893167.3A CN201810893167A CN109133040A CN 109133040 A CN109133040 A CN 109133040A CN 201810893167 A CN201810893167 A CN 201810893167A CN 109133040 A CN109133040 A CN 109133040A
- Authority
- CN
- China
- Prior art keywords
- freezing
- graphene
- temperature
- preparation
- graphene aerogel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
Abstract
A kind of preparation method of the adjustable graphene aerogel of aperture size.The graphene aerogel by graphene oxide by reduction freezing method preparation, have the characteristics that aperture size adjustable extent for 5-240 μm, elasticity modulus highest 327kPa, can be with absorbing organic solvent；Freezing equipment used in freezing step is made of cooling system and temp measuring system, and reduction cryogenic temperature section is -10 DEG C to -196 DEG C, and each second cools down 0.2 DEG C to 20 DEG C.The present invention obtains the graphene aerogel of different pore size size using ice crystal as template accuracy controlling aeroge pattern.The small-bore graphene aerogel prepared under the conditions of high speed freezes has high mechanical property and thermal conductivity, can be used for being catalyzed, field of batteries.The large aperture graphene aerogel prepared under low speed freezing conditions has high oriented attachment performance, can be used for sewage treatment.The ultra-large aperture graphene aerogel prepared under Ultra-Low Speed freezing conditions has high compression reaction performance, can be used for pressure sensor.
Description
Technical field
The invention belongs to carbon material technical field, in particular to the preparation of a kind of adjustable graphene aerogel of aperture size
Method.
Technical background
Graphene is as a kind of novel two-dimentional carbon material, due to having excellent physical property and high specific surface area
Widely paid close attention to.Porous aerogel block body material is made in graphene, can further widen its application field.Graphite
The extremely-low density of alkene aeroge combination aeroge and the superior physical properties of graphene, in catalysis, electrochemistry, sewage treatment, biography
The fields such as sense have performance advantage.
Currently, the preparation method of graphene aerogel is there are larger deficiency, due to can not accuracy controlling graphene aerogel
Pattern to limiting its performance boost.In common preparation method, hydro-thermal method combination self assembly and reduction process are by graphite
Alkene lamella is assembled into three-dimensional structure [1,2], but can not prepare high-sequential and the adjustable porous structure of aperture size.Chemistry
Sedimentation can prepare the graphene aerogel [3,4] of high heat conductance, but its pattern is limited to the pattern of depositing base, from
And limit the popularization and application of this method.Ice template method passes through the forming core of ice crystal and the pattern of adjusting and controlling growth graphene aerogel
[5,6], but be constrained to freezing conditions and be difficult to control, it is difficult the shape of accuracy controlling graphene aerogel using ice template method at present
Looks.On the other hand, ultralow density and porous structure cause the mechanical property of graphene aerogel poor.Conventional schedule of reinforcement
Or the density [7] of aeroge being greatly improved, or change the chemical property [8] of aeroge, this can all reduce graphene airsetting
The performance advantage of glue itself is unable to satisfy existing demand.
Summary of the invention
For above-mentioned two problems of the existing technology, the present invention provides a kind of adjustable graphene gas of aperture size
Gel and preparation method thereof, by controlling the freezing environment of sample preparation to regulate and control forming core and the growth of ice template, and by ice
Template controls the pattern of graphene aerogel, and the graphene aerogel prepared under different freezing conditions shows different aspect
Performance advantage.This method is easy to operate, cost is relatively low, and does not change the density and chemical property of graphene aerogel, can
To bind directly existing preparation method.
A kind of preparation method of the adjustable graphene aerogel of aperture size, which is characterized in that the graphene airsetting
For glue by graphene oxide by reduction freezing method preparation, having aperture size adjustable extent is 5-240 μm, elasticity modulus highest
327kPa, can be with absorbing organic solvent the features such as；Freezing equipment used in freezing step is by cooling system and thermometric system
System composition, reduction cryogenic temperature section are -10 DEG C to -196 DEG C, and each second cools down 0.2 DEG C to 20 DEG C.
The adjustable graphene aerogel preparation method of aperture size as described above, comprising the following steps:
(1) graphene oxide suspension is prepared, takes graphite flake that a small amount of sodium nitrate is added, the concentrated sulfuric acid is added in ice bath, stirs
It is slowly added to a small amount of potassium permanganate after mixing a few hours, and is stirred under water bath with thermostatic control；It is slowly added to low temperature deionized water, is cooled to
A small amount of hydrogen peroxide is slowly added dropwise after room temperature and stirs a period of time；A small amount of concentrated hydrochloric acid is added and stands 12h or more, drains
Clear liquid, the process are repeated twice, and the suspension of remaining dark yellow is transferred in bag filter and is dialysed, until pH value be greater than 6,
The process continues 4 days or more, and multiple Centrifugal dispersion removes unoxidized graphite under 8000-10000rpm revolving speed, takes out supernatant
Liquid is graphene oxide suspension；Graphite flake used in the reaction process, sodium nitrate, the concentrated sulfuric acid, potassium permanganate, dioxygen
The amount of water, calculates in mass ratio, i.e. graphite flake: sodium nitrate: the concentrated sulfuric acid: potassium permanganate: 20~40% aqueous hydrogen peroxide solution is 4
~5.5:0.8~1.2:240~270:19~22:19~22；
(2) ultrasonic agitation mixing is equal in the glass beaker for being put into the graphene oxide suspension of suitable ascorbic acid sum
After even, beaker sealing is put into chamber type electric resistance furnace and is reacted one hour or more at 50 DEG C to 90 DEG C, cylindrical type graphene is formed
Hydrogel；Ion exchange is carried out to graphene hydrogel using enough deionized waters and filters residual impurity；
(3) start freezing equipment, use liquid nitrogen as cold source, select suitable material to make according to required chilling rate
For freezing plate, and freezing plate is fixed on by specific cryogenic temperature by control cold source；
(4) it will be connected with inside the thermocouple insertion graphene hydrogel of temperature measurer, open thermograph switch, wait until temperature
After curve is stablized, graphene hydrogel is put on freezing plate and is oriented freezing, observes the variation of hydrogel internal temperature in real time；
(5) until graphene hydrogel internal temperature is consistent with freezing plate temperature and is no longer changed, in hydrogel
When the liquid water in portion is completely reformed into ice, graphene hydrogel is put into vacuum freeze drier of the vacuum degree less than 20kPa
It is dried 40h to 80h, obtains black cylindrical type graphene aerogel.
Further, in step (1), the graphene oxide suspension concentration is 2-5mg/ml.
Further, in step (2), the mass ratio of the ascorbic acid and graphene oxide is 4:1.
Further, in step (3), the freezing plate are as follows: PMMA plate, 6061 aluminium alloy plates, pure aluminum plate, fine copper plate.
Further, in step (3), the preset temperature of the freezing plate are as follows: -10 DEG C, -20 DEG C, -40 DEG C, -70 DEG C, -
100℃、-196℃。
Further, the graphene aerogel obtained under -196 DEG C of freezing environments has high Young's modulus
(327kPa) and thermal conductivity (0.062W/mK) and lower resistance (1.85k Ω).
Further, the graphene aerogel obtained under -20 DEG C of freezing environments has high absorption property (adsorbable
Organic solvent of 100 times more than self weight).
Further, the graphene aerogel obtained under -10 DEG C of freezing environments has high compression reaction, and (compression follows
Do not change property ring 10 times or more) and heat-insulating property (0.031W/mK).
It is used to prepare the freezing equipment of the adjustable graphene aerogel of aperture size as described above, its feature is as follows:
(1) it is made of refrigeration system and temp measuring system；
(2) refrigeration system includes liguefied nitrogen and freezing plate, and changing freezing plate can be changed at a distance from cold source with regulating and controlling temperature
Turn cold and freezes plate material and can regulate and control cooling velocity；
(3) temp measuring system includes T-type thermocouple, high frequency temperature measurer and computer, and wherein sample can be inserted in T-type thermocouple
To obtain sample temperature data, high frequency temperature measurer can recorde sample temperature variation, and sends data to computer and draw for inside
Temperature variation curve processed；
By observation temp measuring system draw freezing curve and regulate and control refrigeration system, may be implemented specific cryogenic temperature and
Chilling rate.
The present invention proposes a kind of adjustable graphene aerogel of aperture size and preparation method thereof, using ice crystal as template
Accuracy controlling aeroge pattern obtains the graphene aerogel of different pore size size.The aperture prepared under the conditions of high speed freezes
Diameter graphene aerogel has high mechanical property and thermal conductivity, can be used for being catalyzed, field of batteries.It is cold in low speed
The large aperture graphene aerogel prepared under the conditions of jelly has high oriented attachment performance, can be used for sewage treatment.Super
The ultra-large aperture graphene aerogel prepared under low speed freezing conditions has high compression reaction performance, can be used for pressure biography
Sensor.The present invention does not change graphene chemical property and simple and easy graphene aerogel preparation method as one kind, has
Good application prospect.
Detailed description of the invention
The microscopic appearance of the graphene aerogel prepared under Fig. 1 difference freezing conditions,
(a) graphene aerogel prepared under -10 DEG C of freezing conditions；(b) graphite prepared under -20 DEG C of freezing conditions
Alkene aeroge；(c) graphene aerogel prepared under -40 DEG C of freezing conditions；(d) stone prepared under -70 DEG C of freezing conditions
Black alkene aeroge；(e) graphene aerogel prepared under -100 DEG C of freezing conditions；(f) it is prepared under -196 DEG C of freezing conditions
Graphene aerogel.
Specific embodiment
Goal of the invention and technical solution is further described below by specific embodiment and in conjunction with attached drawing, but is not intended to limit this
Invention.
Embodiment 1
A method of it preparing the graphene aerogel of electric-conductivity heat-conductivity high and strong mechanical performance using specific freezing equipment, wraps
Include following steps:
(1) graphene oxide suspension is prepared, takes 3g graphite flake that 1.5g sodium nitrate is added, the dense sulphur of 90ml is added in ice bath
Acid is slowly added to 9g potassium permanganate after stirring 4h, and stirs for 24 hours at 30 DEG C；It is slowly added to 200ml40 DEG C of deionized water,
The hydrogen peroxide of 10ml is slowly added dropwise after being cooled to room temperature and stirs 15min；30ml concentrated hydrochloric acid is added and stands 12h or more, drains
Supernatant, the process are repeated twice, and the suspension of remaining dark yellow is transferred in bag filter and is dialysed, until pH value is greater than
6, which continues 4 days or more, the unoxidized graphite of multiple Centrifugal dispersion removal under 8000-10000rpm revolving speed, in taking-up
Clear liquid is graphene oxide suspension；
(2) graphene oxide suspension of suitable ascorbic acid and 5ml ultrasound in the glass beaker of 10ml is put into stir
It mixes 15min after evenly mixing, beaker sealing is put into chamber type electric resistance furnace at 70 DEG C and reacts 120min, forms cylindrical type graphite
Alkene hydrogel；Ion exchange is carried out to graphene hydrogel using enough deionized waters and filters residual impurity；
(3) start freezing equipment, use liquid nitrogen as cold source, select fine copper plate as freezing plate, and pass through control cold source
Freezing plate will be fixed on -196 DEG C；
(4) it will be connected with inside the thermocouple insertion graphene hydrogel of temperature measurer, open thermograph switch, until temperature
After curve is stablized, graphene hydrogel is put on freezing plate and is oriented freezing, keep thermograph and observes water-setting in real time
The variation of glue internal temperature；
(5) until graphene hydrogel internal temperature is consistent with freezing plate temperature and is no longer changed, in hydrogel
When the liquid water in portion is completely reformed into ice, graphene hydrogel is put into vacuum freeze drier of the vacuum degree less than 20kPa
It is dried 72h, obtains black cylindrical type graphene aerogel；
(6) using XRD XPS the characterization methods test material object phase such as Raman, it is seen that the graphene oxide after reduction
Object mutually change, C-C key is repaired, and functional group is removed；
(7) graphene aerogel of preparation is freezed at -196 DEG C as seen from Figure 1 using SEM characterization material microscopic appearance
In, graphene platelet is intensive and uniform, and this pattern assigns the higher mechanical property of aeroge and thermal conductivity.
Embodiment 2
A method of it preparing the graphene aerogel of electric-conductivity heat-conductivity high and strong mechanical performance using specific freezing equipment, wraps
Include following steps:
(1) graphene oxide suspension is prepared, takes 3g graphite flake that 1.5g sodium nitrate is added, the dense sulphur of 90ml is added in ice bath
Acid is slowly added to 9g potassium permanganate after stirring 4h, and stirs for 24 hours at 30 DEG C；It is slowly added to 200ml40 DEG C of deionized water,
The hydrogen peroxide of 10ml is slowly added dropwise after being cooled to room temperature and stirs 15min；30ml concentrated hydrochloric acid is added and stands 12h or more, drains
Supernatant, the process are repeated twice, and the suspension of remaining dark yellow is transferred in bag filter and is dialysed, until pH value is greater than
6, which continues 4 days or more, the unoxidized graphite of multiple Centrifugal dispersion removal under 8000-10000rpm revolving speed, in taking-up
Clear liquid is graphene oxide suspension；
(2) graphene oxide suspension of suitable ascorbic acid and 5ml ultrasound in the glass beaker of 10ml is put into stir
It mixes 15min after mixing, beaker sealing is put into chamber type electric resistance furnace at 70 DEG C and reacts 120min, forms cylindrical type graphite
Alkene hydrogel；Ion exchange is carried out to graphene hydrogel using enough deionized waters and filters residual impurity；
(3) start freezing equipment, use liquid nitrogen as cold source, select 6061 aluminium sheets as freezing plate, and is cold by controlling
Freezing plate will be fixed on -20 DEG C by source；
(4) it will be connected with inside the thermocouple insertion graphene hydrogel of temperature measurer, open thermograph switch, until temperature
After curve is stablized, graphene hydrogel is put on freezing plate and is oriented freezing, keep thermograph and observes water-setting in real time
The variation of glue internal temperature；
(5) until graphene hydrogel internal temperature is consistent with freezing plate temperature and is no longer changed, in hydrogel
When the liquid water in portion is completely reformed into ice, graphene hydrogel is put into vacuum freeze drier of the vacuum degree less than 20kPa
It is dried 72h, obtains black cylindrical type graphene aerogel；
(6) using XRD XPS the image characterization method test material such as Raman, it is seen that by the object of redox graphene
As being changed, C-C key is repaired, and functional group is removed；
(7) sample microscopic appearance, the visible graphene aerogel graphene freezed at -20 DEG C of Fig. 1 are characterized using SEM
Thin presentation tubular structure, this makes graphene aerogel have higher absorption property.
Embodiment 3
A method of it preparing the graphene aerogel of electric-conductivity heat-conductivity high and strong mechanical performance using specific freezing equipment, wraps
Include following steps:
(1) graphene oxide suspension is prepared, takes 3g graphite flake that 1.5g sodium nitrate is added, the dense sulphur of 90ml is added in ice bath
Acid is slowly added to 9g potassium permanganate after stirring 4h, and stirs for 24 hours at 30 DEG C；It is slowly added to 200ml40 DEG C of deionized water,
The hydrogen peroxide of 10ml is slowly added dropwise after being cooled to room temperature and stirs 15min；30ml concentrated hydrochloric acid is added and stands 12h or more, drains
Supernatant, the process are repeated twice, and the suspension of remaining dark yellow is transferred in bag filter and is dialysed, until pH value is greater than
6, which continues 4 days or more, the unoxidized graphite of multiple Centrifugal dispersion removal under 8000-10000rpm revolving speed, in taking-up
Clear liquid is graphene oxide suspension；
(2) graphene oxide suspension of suitable ascorbic acid and 5ml ultrasound in the glass beaker of 10ml is put into stir
It mixes 15min after mixing, beaker sealing is put into chamber type electric resistance furnace at 70 DEG C and reacts 120min, forms cylindrical type graphite
Alkene hydrogel；Ion exchange is carried out to graphene hydrogel using enough deionized waters and filters residual impurity；
(3) start freezing equipment, use liquid nitrogen as cold source, select PMMA plate as freezing plate, and pass through control cold source
Freezing plate will be fixed on -10 DEG C；
(4) it will be connected with inside the thermocouple insertion graphene hydrogel of temperature measurer, open thermograph switch, until temperature
After curve is stablized, graphene hydrogel is put on freezing plate and is oriented freezing, keep thermograph and observes water-setting in real time
The variation of glue internal temperature；
(5) until graphene hydrogel internal temperature is consistent with freezing plate temperature and is no longer changed, in hydrogel
When the liquid water in portion is completely reformed into ice, graphene hydrogel is put into vacuum freeze drier of the vacuum degree less than 20kPa
It is dried 72h, obtains black cylindrical type graphene aerogel；
(6) using XRD XPS the image characterization method test material such as Raman, it is seen that by the object of redox graphene
As being changed, C-C key is repaired, and functional group is removed；
(7) sample microscopic appearance, the visible graphene aerogel graphene freezed at -10 DEG C of Fig. 1 are characterized using SEM
Club shaped structure is presented in thin slice, this makes graphene aerogel have higher compression cycle performance, and compression circulation is being repeated several times
Still there is very strong mechanical property afterwards.
Citation
[1] Mao Hanping, Yan Yuting, Wang Kun wait a kind of preparation method and its usage of graphene aerogel of,
CN104973594A[P],2015.
[2] Wei Dongshan, Zhou Lina, Sun Tai wait a kind of three-dimensional graphite oxide aerogel preparation side of high-specific surface area of
Method, CN104828807A [P], 2015.
[3] Li Feng, Hu Guangjian, Yan Chuanwei wait a kind of redox graphene/graphite of oxygen-containing functional group gradient distribution of
Alkene foamed composite and its application in vanadium cell, 106207201 A of CN [P], 2016.
[4] appoint literary talent, Xu Chuan, Hu Guangjian wait graphene/redox graphene hydridization nesting porous network structure material
Material and preparation and application, CN106803592A [P], 2017.
[5] a kind of preparation method of graphene aerogel of Zhang Yingtao, CN104843676A [P], 2015.
[6] Liu Jiaqi, Luo Qiaomei, Zhang Yimeng wait a kind of preparation method of spongy light graphite alkene aeroge of,
CN105384165A[P],2016.
[7] a kind of preparation method of high-strength graphite oxide aerogel of the red of Yang Junhe, Han Zhuo, Tang Zhi, CN
102887508 A[P],2013.
[8] Ren Lili, Gao Bingying, He He wait a kind of method for preparing block graphene aerogel of, CN 105819440
A[P],2016.
Claims (10)
1. a kind of preparation method of the adjustable graphene aerogel of aperture size, which is characterized in that graphene aerogel is by aoxidizing
Graphene by reduction freezing method preparation, have aperture size adjustable extent be 5-240 μm, elasticity modulus highest 327kPa,
Can be with absorbing organic solvent the features such as；Freezing equipment used in freezing step is made of cooling system and temp measuring system,
Restoring cryogenic temperature section is -10 DEG C to -196 DEG C, and each second cools down 0.2 DEG C to 20 DEG C.
2. according to the adjustable graphene aerogel preparation method of aperture size described in right 1, which is characterized in that including following step
It is rapid:
(1) graphene oxide suspension is prepared, takes graphite flake that a small amount of sodium nitrate is added, the concentrated sulfuric acid is added in ice bath, stirs number
It is slowly added to a small amount of potassium permanganate after hour, and is stirred under water bath with thermostatic control；It is slowly added to low temperature deionized water, is cooled to room temperature
A small amount of hydrogen peroxide is slowly added dropwise afterwards and stirs a period of time；A small amount of concentrated hydrochloric acid is added and stands 12h or more, drains supernatant
Liquid, the process are repeated twice, and the suspension of remaining dark yellow is transferred in bag filter and is dialysed, until pH value be greater than 6, should
Process continues 4 days or more, and multiple Centrifugal dispersion removes unoxidized graphite under 8000-10000rpm revolving speed, takes out supernatant
As graphene oxide suspension；Graphite flake used in the reaction process, sodium nitrate, the concentrated sulfuric acid, potassium permanganate, hydrogen peroxide
Amount, calculate in mass ratio, i.e. graphite flake: sodium nitrate: the concentrated sulfuric acid: potassium permanganate: 20~40% aqueous hydrogen peroxide solution be 4~
5.5:0.8~1.2:240~270:19~22:19~22；
(2) it is stirred by ultrasonic and is uniformly mixed in the glass beaker for being put into the graphene oxide suspension of suitable ascorbic acid sum
Afterwards, beaker sealing is put into chamber type electric resistance furnace and is reacted one hour or more at 50 DEG C to 90 DEG C, form cylindrical type graphene water
Gel；Ion exchange is carried out to graphene hydrogel using enough deionized waters and filters residual impurity；
(3) start freezing equipment, use liquid nitrogen as cold source, select suitable material as cold according to required chilling rate
Freeze plate, and freezing plate is fixed on by specific cryogenic temperature by control cold source；
(4) it will be connected with inside the thermocouple insertion graphene hydrogel of temperature measurer, open thermograph switch, wait until temperature curve
After stabilization, graphene hydrogel is put on freezing plate and is oriented freezing, observes the variation of hydrogel internal temperature in real time；
(5) until graphene hydrogel internal temperature is consistent with freezing plate temperature and is no longer changed, inside hydrogel
When liquid water is completely reformed into ice, graphene hydrogel is put into dry in vacuum freeze drier of the vacuum degree less than 20kPa
40h to 80h is handled, black cylindrical type graphene aerogel is obtained.
3. preparation method according to claim 2, which is characterized in that in step (1), the graphene oxide suspension
Concentration is 2-5mg/ml.
4. preparation method according to claim 2, which is characterized in that in step (2), the ascorbic acid and oxidation stone
The mass ratio of black alkene is 4:1.
5. preparation method according to claim 2, which is characterized in that in step (3), the freezing plate are as follows: PMMA plate,
6061 aluminium alloy plates, pure aluminum plate, fine copper plate.
6. preparation method according to claim 2, which is characterized in that in step (3), the preset temperature of the freezing plate
Are as follows: -10 DEG C, -20 DEG C, -40 DEG C, -70 DEG C, -100 DEG C, -196 DEG C.
7. preparation method according to claim 2, the graphene aerogel Young mould obtained under -196 DEG C of freezing environments
Amount reaches 0.062W/mK up to 327kPa, thermal conductivity, and resistance reaches 1.85k Ω.
8. preparation method according to claim 2, the graphene aerogel obtained under -20 DEG C of freezing environments is adsorbable super
Cross the organic solvent of 100 times of self weight.
9. preparation method according to claim 2, the graphene aerogel compression circulation obtained under -10 DEG C of freezing environments
Do not change property for 10 times or more, heat-insulating property reaches 0.031W/mK.
10. being used to prepare the freezing equipment of the adjustable graphene aerogel of aperture size according to right 1, feature is such as
Under:
(1) it is made of refrigeration system and temp measuring system；
(2) refrigeration system includes liguefied nitrogen and freezing plate, and changing freezing plate can be changed cold at a distance from cold source with regulating and controlling temperature
Cooling velocity can be regulated and controled by freezing plate material；
(3) temp measuring system includes T-type thermocouple, high frequency temperature measurer and computer, and wherein sample interior can be inserted in T-type thermocouple
To obtain sample temperature data, high frequency temperature measurer can recorde sample temperature variation, and send data to computer drawing temperature
Spend change curve；
(4) by observation temp measuring system draw freezing curve and regulate and control refrigeration system, may be implemented specific cryogenic temperature and
Chilling rate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810893167.3A CN109133040B (en) | 2018-08-07 | 2018-08-07 | Preparation method of graphene aerogel with adjustable pore size |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810893167.3A CN109133040B (en) | 2018-08-07 | 2018-08-07 | Preparation method of graphene aerogel with adjustable pore size |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109133040A true CN109133040A (en) | 2019-01-04 |
| CN109133040B CN109133040B (en) | 2020-05-12 |
Family
ID=64791872
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810893167.3A Active CN109133040B (en) | 2018-08-07 | 2018-08-07 | Preparation method of graphene aerogel with adjustable pore size |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109133040B (en) |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109904010A (en) * | 2019-03-13 | 2019-06-18 | 同济大学 | A kind of gel electrolyte supercapacitor of high-low temperature resistant and preparation method thereof |
| CN110564374A (en) * | 2019-09-18 | 2019-12-13 | 青海大学 | Graphene aerogel or carbon nano-particle phase change material and preparation method thereof |
| CN111048750A (en) * | 2019-11-12 | 2020-04-21 | 北京理工大学 | Graphene aerogel/metallic lithium composite negative electrode material and preparation method thereof |
| CN111223674A (en) * | 2020-01-10 | 2020-06-02 | 东莞理工学院 | Porous graphene-like carbon aerogel and preparation method and application thereof |
| CN111229316A (en) * | 2020-03-06 | 2020-06-05 | 浙江工业大学 | Preparation method of zinc oxide supported three-dimensional honeycomb carbon-based nano material with adjustable aperture |
| CN111252754A (en) * | 2020-03-12 | 2020-06-09 | 浙江大学 | Graphene aerogel air hole regulation and control method and graphene gradient aerogel |
| CN111346577A (en) * | 2020-03-30 | 2020-06-30 | 浙江晶鑫特种纸业有限公司 | Preparation method and application of high-elasticity layered graphene oxide composite aerogel |
| CN111847430A (en) * | 2020-07-15 | 2020-10-30 | 广东墨睿科技有限公司 | Preparation method of high-strength high-resilience graphene aerogel |
| CN112225204A (en) * | 2020-10-21 | 2021-01-15 | 深圳烯创先进材料研究院有限公司 | Method and equipment for controlling graphene orientation in graphene sponge |
| CN112357910A (en) * | 2020-10-12 | 2021-02-12 | 深圳烯创先进材料研究院有限公司 | Preparation method of oriented graphene composite macroscopic body |
| CN113121870A (en) * | 2019-12-30 | 2021-07-16 | 浙江大学 | Method for preparing foamed plastic by emulsion ice template method and product |
| CN113816371A (en) * | 2021-09-25 | 2021-12-21 | 凯盛石墨碳材料有限公司 | Method for preparing expandable graphite by freeze-drying |
| CN115197552A (en) * | 2022-05-26 | 2022-10-18 | 中山大学南昌研究院 | Porous material with multi-scale long-range ordered channel structure and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104788959A (en) * | 2015-03-31 | 2015-07-22 | 中国科学院化学研究所 | Thermal conductive composite material provided with orientation structure and preparation method of thermal conductive composite material |
| CN106422995A (en) * | 2015-08-11 | 2017-02-22 | 中国科学院化学研究所 | Graphene aerogel and hybrid composite material thereof as well as preparation method and application of graphene aerogel |
| CN106744908A (en) * | 2016-11-24 | 2017-05-31 | 陕西聚洁瀚化工有限公司 | Improve the method that Hummers methods prepare graphene oxide |
| CN106744912A (en) * | 2017-03-10 | 2017-05-31 | 中国科学院新疆理化技术研究所 | A kind of preparation method of super-hydrophobic graphene aerogel |
| CN108285127A (en) * | 2017-01-10 | 2018-07-17 | 空中客车防务和空间有限责任公司 | Ammonia borine limitation in graphene oxide three-dimensional structure |
-
2018
- 2018-08-07 CN CN201810893167.3A patent/CN109133040B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104788959A (en) * | 2015-03-31 | 2015-07-22 | 中国科学院化学研究所 | Thermal conductive composite material provided with orientation structure and preparation method of thermal conductive composite material |
| CN106422995A (en) * | 2015-08-11 | 2017-02-22 | 中国科学院化学研究所 | Graphene aerogel and hybrid composite material thereof as well as preparation method and application of graphene aerogel |
| CN106744908A (en) * | 2016-11-24 | 2017-05-31 | 陕西聚洁瀚化工有限公司 | Improve the method that Hummers methods prepare graphene oxide |
| CN108285127A (en) * | 2017-01-10 | 2018-07-17 | 空中客车防务和空间有限责任公司 | Ammonia borine limitation in graphene oxide three-dimensional structure |
| CN106744912A (en) * | 2017-03-10 | 2017-05-31 | 中国科学院新疆理化技术研究所 | A kind of preparation method of super-hydrophobic graphene aerogel |
Non-Patent Citations (1)
| Title |
|---|
| T.LIU ET AL.: "Highly compressible anisotropic graphene aerogels fabricated by directional freezing for efficient absorption of organic liquids", 《CARBON》 * |
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109904010A (en) * | 2019-03-13 | 2019-06-18 | 同济大学 | A kind of gel electrolyte supercapacitor of high-low temperature resistant and preparation method thereof |
| CN110564374A (en) * | 2019-09-18 | 2019-12-13 | 青海大学 | Graphene aerogel or carbon nano-particle phase change material and preparation method thereof |
| CN110564374B (en) * | 2019-09-18 | 2021-08-03 | 青海大学 | Graphene aerogel or carbon nano-particle phase change material and preparation method thereof |
| CN111048750B (en) * | 2019-11-12 | 2021-07-09 | 北京理工大学 | Graphene aerogel/metallic lithium composite negative electrode material and preparation method thereof |
| CN111048750A (en) * | 2019-11-12 | 2020-04-21 | 北京理工大学 | Graphene aerogel/metallic lithium composite negative electrode material and preparation method thereof |
| CN113121870A (en) * | 2019-12-30 | 2021-07-16 | 浙江大学 | Method for preparing foamed plastic by emulsion ice template method and product |
| CN111223674A (en) * | 2020-01-10 | 2020-06-02 | 东莞理工学院 | Porous graphene-like carbon aerogel and preparation method and application thereof |
| CN111229316A (en) * | 2020-03-06 | 2020-06-05 | 浙江工业大学 | Preparation method of zinc oxide supported three-dimensional honeycomb carbon-based nano material with adjustable aperture |
| CN111252754B (en) * | 2020-03-12 | 2020-12-29 | 浙江大学 | Graphene aerogel air hole regulation and control method and graphene gradient aerogel |
| CN111252754A (en) * | 2020-03-12 | 2020-06-09 | 浙江大学 | Graphene aerogel air hole regulation and control method and graphene gradient aerogel |
| CN111346577A (en) * | 2020-03-30 | 2020-06-30 | 浙江晶鑫特种纸业有限公司 | Preparation method and application of high-elasticity layered graphene oxide composite aerogel |
| CN111346577B (en) * | 2020-03-30 | 2022-05-03 | 浙江晶鑫特种纸业有限公司 | Preparation method and application of high-elasticity layered graphene oxide composite aerogel |
| CN111847430A (en) * | 2020-07-15 | 2020-10-30 | 广东墨睿科技有限公司 | Preparation method of high-strength high-resilience graphene aerogel |
| CN112357910A (en) * | 2020-10-12 | 2021-02-12 | 深圳烯创先进材料研究院有限公司 | Preparation method of oriented graphene composite macroscopic body |
| CN112225204A (en) * | 2020-10-21 | 2021-01-15 | 深圳烯创先进材料研究院有限公司 | Method and equipment for controlling graphene orientation in graphene sponge |
| CN113816371A (en) * | 2021-09-25 | 2021-12-21 | 凯盛石墨碳材料有限公司 | Method for preparing expandable graphite by freeze-drying |
| CN113816371B (en) * | 2021-09-25 | 2023-09-08 | 凯盛石墨碳材料有限公司 | Method for preparing expandable graphite through freeze-drying |
| CN115197552A (en) * | 2022-05-26 | 2022-10-18 | 中山大学南昌研究院 | Porous material with multi-scale long-range ordered channel structure and preparation method and application thereof |
| CN115197552B (en) * | 2022-05-26 | 2024-02-13 | 中山大学南昌研究院 | Porous material with multi-scale long-range ordered channel structure and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109133040B (en) | 2020-05-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109133040A (en) | A kind of preparation method of the adjustable graphene aerogel of pore-size | |
| Yuan et al. | Characterization and stability study of a form-stable erythritol/expanded graphite composite phase change material for thermal energy storage | |
| CN106517160B (en) | A kind of preparation method of isotropism super-elasticity graphene aerogel | |
| Mehrali et al. | Preparation and properties of highly conductive palmitic acid/graphene oxide composites as thermal energy storage materials | |
| Park et al. | Synthesis of single crystals of calcite with complex morphologies | |
| Zhang et al. | Phase change materials based on polyethylene glycol supported by graphene-based mesoporous silica sheets | |
| Jákli et al. | Reversible switching between optically isotropic and birefringent states in a bent‐core liquid crystal | |
| CN109573965A (en) | A kind of preparation method of hydroxyl modification boron nitride nanosheet dispersion liquid | |
| CN112225204B (en) | Control method and equipment for graphene orientation in graphene sponge | |
| Zou et al. | Super absorbent polymer as support for shape-stabilized composite phase change material containing Na2HPO4· 12H2O–K2HPO4· 3H2O eutectic hydrated salt | |
| CN104445153A (en) | Method for macroscopic quantity preparation of carbon nano coil from graphene | |
| CN108172793A (en) | Centrifuge the method for preparing three-dimensional carbon foam/graphene oxide based composites | |
| CN104860304A (en) | High specific surface area of silicon oxide hybridized graphene aerogel and production method thereof | |
| Fang et al. | Preparation and thermal performances of Na2HPO4· 12H2O/SiO2 hydrophilic modified expanded graphite form-stable composite phase change material for radiant floor heating system | |
| Liu et al. | Preparation and characterization of new nano-particle mixed as thermal storage material | |
| CN109128149A (en) | The method for preparing three-dimensional carbon nanomaterial in aluminium powder surface in situ using sodium chloride template | |
| CN108975308A (en) | A kind of level duct charcoal nanometer sheet and its preparation method and application | |
| CN106672942A (en) | Preparation method of porous carbon nanotube | |
| CN110655056B (en) | Preparation method of porous nano silicon-carbon composite material | |
| Wang et al. | Coaxial 3D printed anisotropic thermal conductive composite aerogel with aligned hierarchical porous carbon nanotubes and cellulose nanofibers | |
| CN108439371A (en) | A kind of preparation method of three-dimensional (3D) graphene | |
| CN110452480B (en) | Preparation method of ultra-light heat-insulating flexible aerogel | |
| CN114797747B (en) | Super-elastic and high-adsorptivity MXene aerogel and preparation method thereof | |
| CN106430147B (en) | A kind of Ultrasound-microwave preparation has the functional mesoporous hollow carbon sphere of open architecture | |
| CN110127676A (en) | Hydrophobic silica graphene aerogel and its production method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |