CN115893391A - Graphene aerogel with stable structure and high elasticity and preparation method thereof - Google Patents
Graphene aerogel with stable structure and high elasticity and preparation method thereof Download PDFInfo
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- CN115893391A CN115893391A CN202110984068.8A CN202110984068A CN115893391A CN 115893391 A CN115893391 A CN 115893391A CN 202110984068 A CN202110984068 A CN 202110984068A CN 115893391 A CN115893391 A CN 115893391A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 86
- 239000004964 aerogel Substances 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 32
- 229910052802 copper Inorganic materials 0.000 claims description 32
- 239000010949 copper Substances 0.000 claims description 32
- 238000007710 freezing Methods 0.000 claims description 24
- 230000008014 freezing Effects 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 21
- 230000009467 reduction Effects 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 238000004108 freeze drying Methods 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 6
- 239000012300 argon atmosphere Substances 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 20
- 239000006185 dispersion Substances 0.000 description 16
- 239000013078 crystal Substances 0.000 description 15
- 238000006722 reduction reaction Methods 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000000463 material Substances 0.000 description 8
- 239000000523 sample Substances 0.000 description 7
- 230000006835 compression Effects 0.000 description 6
- 238000007906 compression Methods 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- -1 graphite alkene Chemical class 0.000 description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000001132 ultrasonic dispersion Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000012520 frozen sample Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 238000009777 vacuum freeze-drying Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000012669 compression test Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
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- 238000004146 energy storage Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
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- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
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- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
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Abstract
The invention relates to a graphene aerogel with a stable structure and high elasticity and a preparation method thereof. The graphene aerogel has a radial-like orientation structure inside.
Description
Technical Field
The invention relates to a graphene aerogel with a stable structure and high elasticity and a preparation method thereof, belonging to the field of nano materials.
Background
Due to the excellent performances of high ion mobility, high specific surface area, mechanics and the like, the graphene has wide application prospects in the aspects of energy storage, sensing, catalysis, composite materials and the like. However, aggregation and accumulation often occur among the graphene due to the action of pi-pi bonds, so that the comprehensive performance of the graphene is seriously reduced, and the further application of the graphene is hindered.
Mixing graphiteThe graphene aerogel with the three-dimensional network formed by the graphene is an effective way for preventing the graphene aerogel from being agglomerated and accumulated, and the excellent comprehensive performance of the graphene can be fully exerted. The unique aerogel structure will also impart other properties to the material, such as ultra-low density, low thermal conductivity, and the like. Using a sol-gel process, the molecular precursors are dried (frozen or supercritical) to remove the solvent from the wet gel. Aerogels tend to exhibit high porosity (90-99%), low density (about 3 kg/m) 3 ) Low thermal conductivity (about 0.014 W.m at room temperature) -1 ·K -1 ) And the like. Therefore, they can be applied to the fields of catalytic processes, electronic devices, sensors, and the like.
The methods commonly used to date for the preparation of graphene aerogels are chemical reduction or hydrothermal methods, both of which require the use of complex reagents or involve complex operations. Meanwhile, the aerogel has the defects of low strength, unstable structure and weak elasticity.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a high-elasticity graphene aerogel which is simple to operate, is environment-friendly, and can obtain a stable structure, and a preparation method thereof.
In one aspect, the present disclosure provides a graphene aerogel having a radially-like orientation structure inside the graphene aerogel.
In the disclosure, the graphene aerogel has a radial-like orientation structure inside, and the existence of transverse channels effectively disperses loads, provides transverse restraint, reduces stress concentration generation, and has a more stable structure and high elasticity.
Preferably, the graphene aerogel has a pore size distribution of 10-100 μm, a porosity of at least 95% (preferably at least 97%), and an apparent density of 3-6 mg/cm 3 。
Preferably, the plastic deformation of the graphene aerogel after 50 times of 50% strain cycles is less than or equal to 15%, and the maximum stress reduction amplitude after 50 times of 50% strain cycles is less than or equal to 25%. Preferably, the plastic deformation of the graphene aerogel after 50 times of 50% strain cycles is less than or equal to 6%. The maximum stress value decreased slightly at 50 cycles of 50% strain. Preferably, the maximum stress reduction after 50 cycles of 50% strain is less than or equal to 15%.
On the other hand, the invention also provides a preparation method of the graphene aerogel, which comprises the following steps:
(1) Introducing the graphene oxide aqueous solution into a hollow copper mold until the graphene oxide aqueous solution overflows and is sealed by copper;
(2) Placing the hollow copper mold filled with the graphene oxide aqueous solution in a low-temperature environment, and performing directional freezing and freeze drying to obtain graphene oxide aerogel; the freezing direction of the directional freezing is from the surface of the mold to the center of the liquid;
(3) And thermally reducing the obtained graphene oxide aerogel in an inert atmosphere at 800-1400 ℃ to obtain the graphene aerogel.
In the present disclosure, a special directional freezing manner (centripetal freezing) is utilized to prepare the high-elasticity graphene aerogel with stable structure. On one hand, the closed mould is designed so that in the initial freezing state, the temperature of the contact interface of the dispersion liquid and the mould is close to and lower than the temperature of the center of the solution, so that the temperature gradient from the surface of the solution to the center of the solution, namely the centripetal temperature gradient, is generated, and the premise is provided for centripetal freezing. The growth direction of the ice crystals is parallel to the temperature gradient, the ice crystals grow from the inner surface of the copper mould to the center under the influence of the centripetal temperature gradient, and after the solution is completely frozen, the directional growth of the ice crystals is finished. On the other hand, the graphene oxide sheets in the dispersion are extruded to the ice crystal interface during the ice crystal growth process, and the interior of the aerogel obtained thereby is integrated into the growth profile of centripetally oriented ice crystals. The diagonal line of the longitudinal section presents unique 'flower-shaped' orientation, the closed cylindrical copper mould mainly generates mutually perpendicular temperature gradients on the longitudinal section, and the ice crystal growth direction is converged to the diagonal line under the action of double gradients. The centripetal freezing can generate radial-like orientation in the material without complex reagents or complex operation flows, effective dispersed load exists in transverse channels, transverse restraint is provided, stress concentration is reduced, and the graphene aerogel has a more stable structure and high elasticity.
Preferably, the concentration of the graphene oxide aqueous solution is 2-15 mg/mL, preferably 6-12 mg/mL, and more preferably 6-10 mg/mL; the diameter of the graphene oxide sheet layer is 5-50 μm. The graphene oxide sheet layers with large sizes have larger bonding surfaces in the layer-by-layer assembling process, and the bonding is firmer.
Preferably, the freezing temperature of the directional freezing is-80 ℃ to-196 ℃ (liquid nitrogen environment), and the time is 2 minutes to 2 hours, preferably 2 minutes to 1 hour.
Preferably, the temperature of the freeze drying is-80 ℃ to-196 ℃ (liquid nitrogen environment), the environment is a vacuum environment, and the vacuum degree is 1Pa to 100Pa. The ice component is removed by utilizing the characteristic that ice is directly sublimated under the vacuum condition, higher temperature gradient is generated at lower temperature, the internal structure of the aerogel has more excellent orientation, and the graphene oxide aerogel with a stable structure is obtained.
Preferably, the size of the hollow mold is as follows: the inner diameter is 10-50 mm, the height is 10-50 mm, and the wall thickness of the die is 1-4 mm, so that the size and the internal structure of the obtained graphene aerogel sample can be adjusted, and the thinner die is favorable for establishing a higher temperature gradient inside. The hollow copper mould is a cubic hollow copper mould or a cylindrical hollow copper mould; preferably, the ratio of the height to the inner diameter of the hollow copper mold is 0.5-1.5.
Preferably, the inert atmosphere is an argon atmosphere; the time of the thermal reduction is 1 to 4 hours.
Further, the temperature of the thermal reduction is preferably 800 to 1100 ℃. Wherein, suitable ground heat reduction temperature can be better with oxidation graphite alkene reduction to reduction oxidation graphite alkene, obtains high quality graphite alkene aerogel.
Has the advantages that:
in the method, graphene oxide is used as a raw material, liquid nitrogen is used as a cold source, a self-made copper mold is used, and the graphene oxide is added into deionized water and subjected to ultrasonic dispersion to prepare a uniform dispersion liquid. Pouring the mixture into a copper mould, sealing the copper mould with copper, placing the copper mould into liquid nitrogen, taking out a sample in the mould after the copper mould is completely frozen, carrying out vacuum freeze drying to obtain graphene oxide aerogel, and carrying out high-temperature thermal reduction to obtain the graphene aerogel. The prepared aerogel has stable structure and high elasticity.
Drawings
Fig. 1 shows optical images of graphene oxide aerogel and graphene aerogel in example 1;
FIG. 2 shows a structural view of a hollow copper mold used in the present invention;
fig. 3 shows a longitudinal sectional scanning electron microscope image of the graphene aerogel prepared in example 3;
fig. 4 shows stress-strain curves of the graphene aerogel prepared in example 4 under different compressive strains;
fig. 5 shows a stress-strain curve of 50 compression cycles at 50% compressive strain for the graphene aerogel prepared in example 1.
Detailed Description
The present invention is further illustrated by the following examples, which are to be construed as merely illustrative, and not a limitation of the present invention.
In the method, the ice crystal directional growth is mainly realized by utilizing a special directional freezing mode, the microstructure of the graphene aerogel is regulated and controlled, the structural stability of the material is further improved, and the high-elasticity graphene aerogel is obtained.
In this patent, only use directional freezing, can obtain the graphite alkene aerogel that has good elasticity, need not complicated high temperature and changes or utilize toxic additive etc. green high-efficient. The obtained aerogel has excellent performance. In this patent, utilize the structural advantage of mould, obtain the graphite alkene aerogel that has good elasticity. The obtained material has excellent mechanical properties. The following exemplarily illustrates a method for preparing a highly elastic graphene aerogel having a stable structure.
And (3) dispersing graphene oxide. Adding graphene oxide powder into deionized water, and performing ultrasonic dispersion to obtain a uniformly dispersed graphene oxide aqueous solution (or called graphene oxide dispersion liquid). Wherein, the power of ultrasonic dispersion can be 100-200W, and the time can be 30-40 min.
And pouring the graphene oxide dispersion liquid into a cylindrical hollow copper mold, wherein the ratio of the height (h) to the diameter (inner diameter D) of the copper mold is 1-5, and preferably 0.5-1. The mold was completely filled with the dispersion and then sealed with copper.
And (4) directional freezing. And (3) placing the sealed mould in a low-temperature environment for a period of time, and after the dispersion liquid in the mould is completely frozen, freezing and drying to obtain the graphene oxide aerogel. Wherein, the directional freezing direction is from the surface of the mold to the center of the liquid, that is, the surface of the mold is the low temperature end, and the center of the dispersion liquid is the high temperature end. The temperature for directional freezing and freeze drying is-80 deg.C to-196 deg.C. The freeze drying method is vacuum freeze drying, and specifically comprises the following steps: and placing the frozen sample in a vacuum environment with the vacuum degree of 1-100 Pa.
And (4) carrying out thermal reduction. And heating and reducing the graphene oxide aerogel at a certain temperature under the argon condition to obtain the graphene aerogel with stable structure and high elasticity. Wherein the thermal reduction temperature is preferably 800-1400 ℃.
In the invention, the obtained graphene aerogel has the apparent density of 3-7 mg/cm 3 The material has excellent rebound property, after 50% compression strain for 50 times, the rebound rate reaches more than 95%, and the material has important application prospect.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
(1) Adding 320mg of graphene oxide (the thickness is 1nm, the diameter is 10-50 mu m) into 40mL of deionized water, and performing ultrasonic dispersion for 30min under the power of 100W to obtain a uniformly dispersed graphene oxide dispersion liquid with the concentration of 8 mg/mL;
(2) A self-made cylindrical copper mould with the inner diameter of phi 15mm multiplied by 35mm is adopted, evenly-dispersed graphene oxide dispersion liquid is poured into the mould until the mould is full, a copper end cover is utilized to seal the mould, and the inside of the mould is ensured to be full of the dispersion liquid. Placing the mold in liquid nitrogen for directional freezing (-196 ℃), taking out after 2min, naturally thawing in air for 20min until the mold can be opened, and taking out the sample;
(3) Putting the frozen sample into a freeze dryer for vacuum drying, wherein the vacuum degree is 1Pa, and the vacuum drying time is 48h, so as to obtain graphene oxide aerogel;
(4) And (3) placing the graphene oxide aerogel in a vacuum furnace, heating to 1000 ℃ at a speed of 5 ℃/min under an argon atmosphere, and preserving heat for 2h, wherein the cooling mode is natural cooling. And obtaining the elastic graphene aerogel. Apparent density of about 3.6mg/cm 3 ；
(5) The obtained aerogel is subjected to compression test by using a compression tester, and the maximum stress value of the prepared aerogel after 50 times of 50% strain compression is slightly reduced compared with the initial stress, and the plastic deformation is 4%.
Example 2
Example 2 differs from example 1 only in that: 160mg of graphene oxide powder is added in the step (1), and the concentration of the obtained dispersion liquid is 4mg/mL.
Example 3
Example 3 differs from example 1 only in that: 240mg of graphene oxide powder is added in the step (1), and the concentration of the obtained dispersion liquid is 6mg/mL.
Example 4
Example 4 differs from example 1 only in that: 400mg of graphene oxide powder is added in the step (1), and the concentration of the obtained dispersion liquid is 10mg/mL.
Example 5
Example 5 differs from example 1 only in that: 480mg of graphene oxide powder is added in the step (1), and the concentration of the obtained dispersion liquid is 12mg/mL.
Example 6
Example 6 differs from example 1 only in that: the ratio of the height (h) to the diameter (D) of the copper mold was 0.5.
Example 7
Example 7 differs from example 1 only in that: the ratio of the height (h) to the diameter (D) of the copper mold was 1.5.
Comparative example 1
Comparative example 1 differs from example 1 only in that: the lower surface of the hollow cylinder is-196 ℃, and unidirectional freeze drying is carried out.
Table 1 shows the performance parameters of the graphene aerogel prepared according to the present invention:
fig. 1 shows optical images of graphene oxide aerogel and graphene aerogel before and after thermal reduction, after which the aerogel changes from yellow-brown to black graphene aerogel.
Fig. 2 shows the structural design of the hollow copper mould, the double end-cap design facilitates sample extraction after freezing, and the concave structure is designed to leave enough room for the volume expansion caused by water freezing. And ensures that the dispersion in the mold is in full contact with the inner surface of the mold.
Fig. 3 shows a longitudinal sectional scanning electron microscope image of the prepared graphene aerogel. The diagonal direction presents unique 'flower-shaped' orientation, the graphene sheet layers are converged in the diagonal direction of 47 degrees, and the convergence angle is continuously reduced. When the longitudinal ice crystals meet the transverse ice crystals at the diagonal, the longitudinal ice crystals are influenced by the temperature gradient caused by the transverse ice crystals, and the growth direction of the ice crystals is changed under the action of the double gradient, so that the approach-compromise trend is caused. The closer to the center of the block the growth trend is, the closer to the common diagonal position, the smaller the convergence angle becomes. Specifically, we can observe a special structure of "Y" type as shown in FIG. 3. The crystal growth is generated by the fact that part of the ice crystals meet when converging and jointly move to the growth end point, and the growth end point is a Y-shaped node. The material has the advantages that the material generates radial-like orientation inside, the transverse pore channels effectively disperse loads, transverse restraint is provided, stress concentration is reduced, and the graphene aerogel has a more stable structure and high elasticity.
Fig. 4 shows stress-strain curves of the graphene aerogel prepared in example 4 at 10%, 20%, 30%, 40%, and 50% compressive strain, and it can be seen from the graph that the sample shows good resilience at 10% to 50% compressive strain, and can recover to the original height after the load is removed, that is, there is no significant plastic deformation, and shows good resilience.
Fig. 5 shows a stress-strain curve of 50 compression cycles of the graphene aerogel prepared in example 1 under 50% of compressive strain, and it can be seen from the graph that 96% of the maximum stress value still remains after the sample undergoes 50% of strain compression cycles, the sample resilience also reaches above 95%, and the stress plateau is only slightly reduced, indicating that it has good structural stability.
Claims (10)
1. The graphene aerogel is characterized in that the graphene aerogel internally has a radial-like orientation structure.
2. The graphene aerogel according to claim 1, wherein the graphene aerogel has a pore size distribution of 10 to 100 μm, a porosity of at least 95%, and an apparent density of 3 to 6mg/cm 3 。
3. The graphene aerogel according to claim 1 or 2, wherein the graphene aerogel has a plastic deformation of 15% or less after 50 cycles of 50% strain and a maximum stress reduction of 25% or less after 50 cycles of 50% strain.
4. A method for preparing the graphene aerogel according to any one of claims 1 to 3, comprising:
(1) Introducing the graphene oxide aqueous solution into a hollow copper mold until the graphene oxide aqueous solution overflows and is sealed by copper;
(2) Placing the hollow copper mold filled with the graphene oxide aqueous solution in a low-temperature environment, and performing directional freezing and freeze drying to obtain graphene oxide aerogel; the freezing direction of the directional freezing is from the surface of the mold to the center of the liquid;
(3) And thermally reducing the obtained graphene oxide aerogel in an inert atmosphere at 800-1400 ℃ to obtain the graphene aerogel.
5. The preparation method according to claim 4, wherein the concentration of the graphene oxide aqueous solution is 2 to 15mg/mL, preferably 6 to 12mg/mL; the diameter of the graphene oxide sheet is 5-50 mu m.
6. The method of claim 4 or 5, wherein the freezing temperature of the directional freezing is-80 ℃ to-196 ℃ and the time is 2 minutes to 2 hours.
7. The method according to any one of claims 4 to 6, wherein the temperature of the freeze-drying is from-80 ℃ to-196 ℃, the atmosphere is a vacuum atmosphere, and the degree of vacuum is from 1Pa to 100Pa.
8. The method of any one of claims 4-7, wherein the hollow copper mold has a size: the inner diameter is 10-50 mm, the height is 10-50 mm, and the wall thickness of the die is 1-4 mm; the hollow copper mould is a cubic hollow copper mould or a cylindrical hollow copper mould; preferably, the ratio of the height to the inner diameter of the hollow copper mold is 0.5-1.5.
9. The production method according to any one of claims 4 to 8, wherein the temperature of the thermal reduction is 800 to 1100 ℃.
10. The production method according to any one of claims 4 to 9, wherein the inert atmosphere is an argon atmosphere; the time of the thermal reduction is 1 to 4 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104661959A (en) * | 2012-08-23 | 2015-05-27 | 莫纳什大学 | Graphene-based materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104661959A (en) * | 2012-08-23 | 2015-05-27 | 莫纳什大学 | Graphene-based materials |
Non-Patent Citations (1)
| Title |
|---|
| CHUNHUI WANG ET AL: ""Freeze-Casting Produces a Graphene Oxide Aerogel with a Radial and Centrosymmetric Structure"", 《ACS NANO》, 14 May 2018 (2018-05-14), pages 5816 - 5825 * |
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