CN107746052A - A kind of preparation method of the graphene aerogel of N doping - Google Patents
A kind of preparation method of the graphene aerogel of N doping Download PDFInfo
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- CN107746052A CN107746052A CN201711043034.9A CN201711043034A CN107746052A CN 107746052 A CN107746052 A CN 107746052A CN 201711043034 A CN201711043034 A CN 201711043034A CN 107746052 A CN107746052 A CN 107746052A
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- C01—INORGANIC CHEMISTRY
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- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Abstract
A kind of preparation method of the graphene aerogel of N doping, belongs to aeroge preparing technical field.After the present invention is by the way that the graphene oxide dispersion of individual layer or few layer is well mixed with nitridation B solution, ascorbic acid is added as reducing agent, reacted through low-temperature hydrothermal and reduce graphene oxide to obtain hydrogel, finally by supercritical drying, obtain the graphene aerogel of N doping.The nitrogen-doped graphene aeroge that the present invention obtains has excellent mechanical performance and electrical insulating property, effectively can prevent battery from being come off in vibration processes, the Heat Conduction Material being expected to be used in electric automobile battery box body；In addition, the nitrogen-doped graphene aeroge surface that the present invention obtains has loose structure, there is larger application prospect in adsorb and be catalyzed etc..
Description
Technical field
The invention belongs to aeroge preparing technical field, and in particular to a kind of graphene aerogel of high performance N doping
Preparation method.
Background technology
Aeroge be it is a kind of there is high-specific surface area and the porous nanometer material compared with low-density, typically pass through supercritical drying
Or the method for frozen drying hydrogel obtains.For graphene aerogel as a kind of new mesoporous and poromerics, it is more
Porosity reaches 80%~99.8%, and specific surface area is up to 200~1500m2/ g, catalyst carrier, gas filtering material, efficiently
The fields such as heat-barrier material, capacitor electrode material have been widely used.At present, graphene aerogel is with resorcinol and formaldehyde
For raw material, reducing agent is used as using hydrazine hydrate, ethylenediamine, hydroiodic acid etc., stable graphene colloid is made in the basic conditions
After solution, it is prepared by supercritical drying.However, the carbon-to-oxygen ratio for the graphene that existing method is prepared is relatively low, lead
Electrical property is poor, directly affects the final performance for the graphene aerogel to be formed；And the reducing agent used has toxicity or corruption
Corrosion, it is unfavorable for industrialization large-scale production.
The content of the invention
The defects of the invention aims to overcome background technology to exist, propose that a kind of technique is simple, it is big to be easily achieved
The preparation method of the graphene aerogel of the N doping of technical scale metaplasia production.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of the graphene aerogel of N doping, specifically includes following steps：
Step 1, by individual layer or few layer (<10 layers) graphene oxide add deionized water in, 4~8h of ultrasonic disperse until
It is well mixed, obtain the graphene oxide dispersion that mass concentration is 2~8mg/ml；
Step 2, by boron nitride powder add deionized water in, 8~12h of ultrasonic disperse to uniformly after, centrifuge, take
Layer clear liquid is as nitridation B solution；Wherein, centrifugal rotational speed is 6000~9000r/min, and the time is 8~15min；
Step 3, nitridation B solution that step 2 obtains added in the graphene oxide dispersion that step 1 is prepared, 30~
30~45min of ultrasonic disperse at a temperature of 50 DEG C, ascorbic acid (VC) is then added, obtains mixed liquor；Wherein, nitrogenized in mixed liquor
The mass concentration of boron is 0.015g/L~0.02g/L, and the mass concentration of graphene oxide is 3.2g/L~3.4g/L, ascorbic acid
Mass concentration be 6.5g/L~13g/L；
Step 4, by the mixed liquor that step 3 obtains after 20~35min of mechanical agitation at a temperature of 30~45 DEG C, stand 15~
30min, it is then placed in hydrothermal reaction kettle and carries out hydro-thermal reaction, reaction temperature is 90~100 DEG C, and the reaction time is 4~6h, instead
After the completion of answering, the graphene hydrogel of column is obtained；
Step 5, the graphene hydrogel that step 4 obtains soaked into 20~30h in ethanol, with remove unnecessary impurity and
Remaining reducing agent；Then supercritical drying is carried out, drying temperature is 30~40 DEG C, and pressure is 7.0Mpa~10.0Mpa, the time
For 15~24h, the graphene aerogel of the N doping is obtained.
Further, individual layer described in step 1 or few layer (<10 layers) graphene oxide using improve Hummers chemical methods
It is made.
Preferably, the mass concentration of graphene oxide dispersion described in step 1 is 4mg/ml.
Further, the mass concentration for B solution being nitrogenized described in step 2 is 0.015~0.05mg/ml.
Further, supercritical drying described in step 5 is ethanol supercritical drying；The concentration of the ethanol be 0.5~
2mol/L。
Further, steps 1 and 2, the power of ultrasonic disperse described in 3 are 180~500W, supersonic frequency is 20~
65KHz。
The graphene aerogel for the N doping that the inventive method obtains, the three-dimensional net structure being made up of two-dimensional graphene
High performance graphite alkenyl aeroge, its aperture is 50nm~100um, and porosity is 65~99.9%, density is 0.02~
0.1g/cm3, specific surface area is 100~750m2/ g, electrical conductivity 10-5~10-4S/cm。
Compared with prior art, beneficial effects of the present invention are：
1st, the present invention by by individual layer or few layer (<10 layers) graphene oxide dispersion with nitridation B solution be well mixed
Afterwards, add ascorbic acid (VC) and be used as reducing agent, reacted through low-temperature hydrothermal and reduce graphene oxide to obtain hydrogel, most passed through afterwards
Supercritical drying is crossed, obtains the graphene aerogel of N doping.In the forming process of nitrogen-doped graphene aeroge of the present invention simultaneously
Any crosslinking agent is not used, and hydrogel is directly formed by hydro-thermal reaction, graphene airsetting is ensure that while cost is reduced
The intrinsic construction unit of the purity and graphene of glue, has farthest played its excellent physical and chemical performance；The present invention
(90~100 DEG C) progress hydro-thermal reactions at a lower temperature, avoid the oxygen-containing function in graphene oxide in high temperature environments
Group discharges in a gaseous form, causes collapsing for aeroge, can not be molded, and energy consumption is low pollution-free, the graphene being prepared
Aeroge has good pattern；The present invention using ethanol supercritical drying formed aeroge, by drying temperature, pressure and
The control of time, form with good pattern, without the aeroge collapsed, there is excellent mechanical performance.
2nd, the nitrogen-doped graphene aeroge that the present invention obtains has excellent mechanical performance and electrical insulating property, can effectively prevent
Only battery comes off in vibration processes, the Heat Conduction Material being expected to be used in electric automobile battery box body；In addition, what the present invention obtained
Nitrogen-doped graphene aeroge surface has loose structure, has larger application prospect in adsorb and be catalyzed etc..
Brief description of the drawings
Fig. 1 is the transmission electron microscope figure (TEM) for the graphene oxide that step 1 of the embodiment of the present invention obtains；
Fig. 2 is the X-ray photoelectron spectroscopic analysis figure (XPS) for the graphene oxide that step 1 of the embodiment of the present invention obtains；
Fig. 3 is the scanning electron microscope diagram (SEM) of the graphene aerogel for the N doping that the embodiment of the present invention obtains；
Fig. 4 is the pictorial diagram of the graphene aerogel for the N doping that the embodiment of the present invention obtains；
Fig. 5 is the pictorial diagram for the graphene aerogel that the present invention obtains at different supercritical drying temperature and pressure.
Embodiment
With reference to the accompanying drawings and examples, technical scheme is described in detail.
Embodiment
A kind of preparation method of the graphene aerogel of N doping, specifically includes following steps：
Step 1, prepare the graphene oxide of individual layer using improving Hummers chemical methods：500mL reaction flask is placed in
In ice bath, 98% concentrated sulfuric acid is added, is stirred；Then the solid mixture of 4g graphite powders and 2g sodium nitrate is added, then is added by several times
Enter 12g potassium permanganate, controlling reaction temperature is no more than 20 DEG C, and stirring reaction to temperature rises to 35 DEG C or so, continues to stir
30min, deionized water is slow added into, continued after stirring 20min, added the oxidant of hydrogen peroxide reduction residual, filter while hot；
After obtained filter cake is using 5% HCl solution and deionized water washing, it is placed in vacuum drying chamber at 60 DEG C and fully dries, obtain
The TEM and XPS of the graphene oxide of the individual layer arrived as illustrated in fig. 1 and 2, show to have obtained uniform graphene oxide；
Step 2, the graphene oxide of individual layer made from step 1 added in deionized water, ultrasonic disperse 8h is until mixing
Uniformly, the graphene oxide dispersion that mass concentration is 4mg/ml is obtained；Wherein, the power of ultrasonic disperse is 300W, supersonic frequency
Rate is 45KHz；
Step 3,2mg boron nitride powders are added in 100ml deionized waters, peeled off through ultrasonic disperse 10h into individual layer or
Few layer (<10 layers) boron nitride after, processing is centrifuged using centrifuge, take centrifuge after supernatant liquor as nitrogen
Change B solution；Wherein, centrifugal rotational speed 8000r/min, time 12min；
The nitridation B solution that step 4, the graphene oxide dispersion, the 20ml steps 3 that take 100ml steps 2 to prepare obtain, is mixed
It is put into ultrasonic agitation machine after conjunction to be sufficiently mixed, temperature is 45 DEG C, jitter time 30min；Wherein, the power of ultrasonic disperse
For 300W, supersonic frequency 45KHz；
1.5g ascorbic acid (VC) is added in step 5, the solution obtained after step 4 processing, obtained mixed liquor is 45
At a temperature of DEG C after mechanical agitation 35min, 30min is stood, is then placed in hydrothermal reaction kettle and carries out hydro-thermal reaction, reaction temperature is
90 DEG C, reaction time 6h, the heating rate that 90 DEG C are risen to by room temperature is 6 DEG C/min, after the completion of reaction, obtains the graphite of column
Alkene hydrogel；
Step 6, the graphene hydrogel that step 5 obtains soaked into 30h in 300ml ethanol, to remove unnecessary impurity
And remaining reducing agent；Then ethanol supercritical drying is carried out, drying temperature is 40 DEG C, pressure 8Mpa, time 20h, is obtained
To the graphene aerogel of the N doping.
Further, the present invention to graphene oxide hydrogel when carrying out supercritical drying, first with ethanol to corresponding
Solvent and other impurities in hydrogel enter line replacement, then again using ethanol supercritical drying method to the hydrogel after processing
It is dried, the SEM and pictorial diagram for obtaining the graphene aerogel of N doping distinguish as shown in Figures 3 and 4.Can from figure
Go out, the graphene aerogel for the N doping that embodiment obtains has a large amount of holes, and generally uniform distribution, is advantageous to mitigate its matter
Amount, improve the stability of mechanical structure.
Further, the present invention to graphene oxide hydrogel when carrying out supercritical drying, in order to ensure obtained oxygen
Graphite alkene aeroge has good pattern and without collapsing, and the temperature and pressure scope of supercritical drying is regulated and controled.
On the premise of other specification condition in keeping embodiment is constant, the temperature of supercritical drying and pressure are divided into 3 scopes, point
It is not：(1) temperature<30 DEG C, pressure<7.0Mpa；(2) temperature>40 DEG C, pressure>10Mpa；(3) 30 DEG C~40 DEG C of temperature, pressure
7.0Mpa~10.0Mpa.It is (1) " temperature in temperature and pressure range<30 DEG C, pressure<Under conditions of 7.0Mpa ", obtained oxygen
Shown in graphite alkene aeroge such as Fig. 5 (c), obtained aeroge is expanded, more loose, is easily collapsed；In temperature and pressure
Scope be (2) " temperature>40 DEG C, pressure>Under conditions of 10Mpa ", obtained graphite oxide aerogel such as Fig. 5 (a, b) institutes
Show, obtained aeroge is there occurs polycondensation phenomenon, and density increase, porosity reduces, brittle；It is in the scope of temperature and pressure
(3) " 30 DEG C~40 DEG C of temperature, under conditions of pressure 7.0Mpa~10.0Mpa ", obtained graphite oxide aerogel such as Fig. 5
(d) shown in, obtained aeroge has good pattern, and density is light, and nothing collapses.
The graphene aerogel of the N doping obtained to embodiment applies pressure in the axial direction, its can bear 500g~
The pressure of 1000g sizes.The graphene aerogel of the N doping obtained to embodiment carries out electrical insulation capability test, obtains its electricity
Conductance is 10-5~10-4S/cm, there is good electrical insulation capability.
Claims (5)
1. a kind of preparation method of the graphene aerogel of N doping, comprises the following steps：
Step 1, the graphene oxide of individual layer or few layer added in deionized water, 4~8h of ultrasonic disperse is obtained until well mixed
To the graphene oxide dispersion that mass concentration is 2~8mg/ml；
Step 2, by boron nitride powder add deionized water in, 8~12h of ultrasonic disperse to uniformly after, centrifuge, take upper strata clear
Liquid is as nitridation B solution；Wherein, centrifugal rotational speed is 6000~9000r/min, and the time is 8~15min；
In step 3, the graphene oxide dispersion for preparing the nitridation B solution addition step 1 that step 2 obtains, at 30~50 DEG C
At a temperature of 30~45min of ultrasonic disperse, then add ascorbic acid, obtain mixed liquor；Wherein, in mixed liquor boron nitride quality
Concentration is 0.015g/L~0.02g/L, and the mass concentration of graphene oxide is 3.2g/L~3.4g/L, and the quality of ascorbic acid is dense
Spend for 6.5g/L~13g/L；
Step 4, after the mixed liquor that step 3 obtains is stirred into 20~35min at a temperature of 30~45 DEG C, 15~30min is stood, so
After be put into hydrothermal reaction kettle and carry out hydro-thermal reaction, reaction temperature is 90~100 DEG C, and the reaction time be 4~6h, reaction completion
Afterwards, the graphene hydrogel of column is obtained；
Step 5, the graphene hydrogel that step 4 obtains soaked into 20~30h in ethanol, then carry out supercritical drying, done
Dry temperature is 30~40 DEG C, and pressure is 7.0Mpa~10.0Mpa, and the time is 15~24h, obtains the graphene gas of the N doping
Gel.
2. the preparation method of the graphene aerogel of N doping according to claim 1, it is characterised in that described in step 1
The graphene oxide of individual layer or few layer is made using Hummers chemical methods are improved.
3. the preparation method of the graphene aerogel of N doping according to claim 1, it is characterised in that described in step 1
The mass concentration of graphene oxide dispersion is 4mg/ml.
4. the preparation method of the graphene aerogel of N doping according to claim 1, it is characterised in that described in step 5
Supercritical drying is ethanol supercritical drying.
5. the preparation method of the graphene aerogel of N doping according to claim 1, it is characterised in that steps 1 and 2,3
Described in the power of ultrasonic disperse be 180~500W, supersonic frequency is 20~65KHz.
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Cited By (10)
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| CN108946711A (en) * | 2018-09-20 | 2018-12-07 | 安徽理工大学 | A kind of preparation method of N doping redox graphene aeroge absorbing material |
| CN109279598A (en) * | 2018-11-16 | 2019-01-29 | 中科院合肥技术创新工程院 | A kind of method of liquid laser auxiliary synthesis heteroatom doped graphene aeroge |
| CN110255534A (en) * | 2019-06-06 | 2019-09-20 | 江苏大学 | It is a kind of to adulterate three-dimensional porous graphene aerogel and preparation method and application |
| CN112156753A (en) * | 2020-09-23 | 2021-01-01 | 中国石油大学(华东) | Graphene aerogel and preparation method and application thereof |
| CN112480609A (en) * | 2020-11-06 | 2021-03-12 | 裴佩 | Preparation method of insulating and heat-conducting composite material |
| CN112607726A (en) * | 2020-12-17 | 2021-04-06 | 泉州博银信息科技有限公司 | Graphene composite material, preparation method and application thereof |
| CN109399619B (en) * | 2018-12-31 | 2021-06-04 | 太原理工大学 | Preparation method of nitrogen-doped graphene aerogel |
| CN114085530A (en) * | 2021-11-10 | 2022-02-25 | 华东理工大学 | Low-thermal-resistance high-thermal-conductivity graphene silicone rubber composite material and preparation method thereof |
| CN114597560A (en) * | 2022-02-28 | 2022-06-07 | 陕西科技大学 | Graphene/boron nitride aerogel and preparation method thereof |
| CN115413270A (en) * | 2020-01-21 | 2022-11-29 | 普林斯顿大学理事会 | Ultra-light graphene-HBN nanoparticle aerogel |
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| CN108946711A (en) * | 2018-09-20 | 2018-12-07 | 安徽理工大学 | A kind of preparation method of N doping redox graphene aeroge absorbing material |
| CN109279598A (en) * | 2018-11-16 | 2019-01-29 | 中科院合肥技术创新工程院 | A kind of method of liquid laser auxiliary synthesis heteroatom doped graphene aeroge |
| CN109399619B (en) * | 2018-12-31 | 2021-06-04 | 太原理工大学 | Preparation method of nitrogen-doped graphene aerogel |
| CN110255534A (en) * | 2019-06-06 | 2019-09-20 | 江苏大学 | It is a kind of to adulterate three-dimensional porous graphene aerogel and preparation method and application |
| CN115413270A (en) * | 2020-01-21 | 2022-11-29 | 普林斯顿大学理事会 | Ultra-light graphene-HBN nanoparticle aerogel |
| CN115413270B (en) * | 2020-01-21 | 2024-02-13 | 普林斯顿大学理事会 | Ultra-light graphene-HBN nanoparticle aerogel |
| CN112156753A (en) * | 2020-09-23 | 2021-01-01 | 中国石油大学(华东) | Graphene aerogel and preparation method and application thereof |
| CN112480609A (en) * | 2020-11-06 | 2021-03-12 | 裴佩 | Preparation method of insulating and heat-conducting composite material |
| CN112607726A (en) * | 2020-12-17 | 2021-04-06 | 泉州博银信息科技有限公司 | Graphene composite material, preparation method and application thereof |
| CN114085530A (en) * | 2021-11-10 | 2022-02-25 | 华东理工大学 | Low-thermal-resistance high-thermal-conductivity graphene silicone rubber composite material and preparation method thereof |
| CN114597560A (en) * | 2022-02-28 | 2022-06-07 | 陕西科技大学 | Graphene/boron nitride aerogel and preparation method thereof |
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