CN116281986A - Preparation method, drafting device and application of three-dimensional graphene - Google Patents
Preparation method, drafting device and application of three-dimensional graphene Download PDFInfo
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- CN116281986A CN116281986A CN202310407589.6A CN202310407589A CN116281986A CN 116281986 A CN116281986 A CN 116281986A CN 202310407589 A CN202310407589 A CN 202310407589A CN 116281986 A CN116281986 A CN 116281986A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 117
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 117
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 230000009467 reduction Effects 0.000 claims abstract description 34
- 239000013067 intermediate product Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000002184 metal Substances 0.000 claims abstract description 14
- 239000003638 chemical reducing agent Substances 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 3
- 230000008901 benefit Effects 0.000 abstract description 5
- 239000004065 semiconductor Substances 0.000 abstract description 5
- 239000007791 liquid phase Substances 0.000 description 18
- 239000000243 solution Substances 0.000 description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical group I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 9
- 229910000043 hydrogen iodide Inorganic materials 0.000 description 9
- 230000005540 biological transmission Effects 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 238000011065 in-situ storage Methods 0.000 description 5
- 230000003247 decreasing effect Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000002356 single layer Substances 0.000 description 4
- 239000002390 adhesive tape Substances 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 230000005669 field effect Effects 0.000 description 2
- -1 light weight Chemical compound 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000005325 percolation Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003828 vacuum filtration Methods 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000005441 electronic device fabrication Methods 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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Abstract
The invention relates to the technical field of graphene, and particularly provides a preparation method, a drafting device and application of three-dimensional graphene. The preparation method of the three-dimensional graphene comprises the following steps: (1) Carrying out first reduction treatment on the flaky three-dimensional graphene oxide to obtain a first intermediate product; (2) Drawing the first intermediate product to obtain a second intermediate product; (3) And carrying out a second reduction treatment on the second intermediate product to obtain the three-dimensional graphene. Compared with the prior art, the method disclosed by the invention has the advantages that more fold morphology is constructed on the surface of the three-dimensional graphene through plastic drafting and reduction treatment, so that the conductive mode of the three-dimensional graphene is converted from a semiconductor type to a metal type, and meanwhile, the inherent mechanical property advantage of the graphene is maintained.
Description
Technical Field
The invention relates to the technical field of graphene, in particular to a preparation method, a drafting device and application of three-dimensional graphene.
Background
Graphene is a kind of graphene with sp 2 The carbon atoms connected by the orbital hybridization configuration are piled up to form a novel carbon material with a single-layer two-dimensional honeycomb lattice structure. Graphene has a unique "dirac cone" type band structure, which allows it to have extremely high carrier mobility at room temperature, about 1000cm 2 ·V -1 S. In addition, the graphene has mechanical characteristics of flexibility, light weight, high strength, flexible processing and the like, and provides a potential alternative scheme for the research and the manufacture of semiconductor electronic devices in the 'back-silicon' age. However, the unique zero-bandgap dirac cone-shaped band structure of graphene makes its application in the field of semiconductor electronic device fabrication very limited. The two-dimensional morphology of graphene makes it still facing a serious challenge in terms of scale preparation and application. In addition, the low-dimensional morphology of the graphene causes insufficient specific capacity, which greatly limits the application of the graphene in various fields such as the field of high-power electronic devices. To have the followingThe proposal of the concept of 'all-carbon electronics' represented by the three-dimensional graphene oxide structure with self-supporting configuration provides a feasible scheme for solving the problems, wherein the three-dimensional graphene oxide with the most representative structure is graphene sponge, graphene network, graphene film and the like.
At present, the conductivity of three-dimensional graphene oxide represented by graphene sponge, graphene network and graphene film has typical "insulation" type temperature dependence. Furthermore, the "insulating" type temperature dependence exists not only at the charge neutral point but also at carrier concentrations up to 10 19 ·cm -3 Can be observed in the doping system of (c).
For graphene having a three-dimensional spatial configuration, its internal carriers generally exhibit a semiconductor type transport characteristic, i.e., electrical conductivity exhibits a tendency to increase with an increase in temperature. How to realize a metal type carrier transport mode in three-dimensional graphene, that is, how the conductivity shows a decreasing trend with increasing temperature, is very urgent.
Disclosure of Invention
In view of the above, the invention aims to provide a preparation method, a drafting device and application of three-dimensional graphene, wherein the method constructs more fold morphology on the surface of the three-dimensional graphene, so that the conductive mode of the three-dimensional graphene is changed from a semiconductor type to a metal type, namely, the conductivity is reduced along with the temperature rise, and meanwhile, the inherent mechanical performance advantage of the graphene is maintained.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method for preparing three-dimensional graphene, comprising:
(1) Carrying out first reduction treatment on the flaky three-dimensional graphene oxide to obtain a first intermediate product;
(2) Drawing the first intermediate product to obtain a second intermediate product;
(3) And carrying out a second reduction treatment on the second intermediate product to obtain the three-dimensional graphene.
In the present invention, the first reduction treatment is specifically: mixing flaky three-dimensional graphene oxide with a reducing agent solution;
the second reduction treatment specifically comprises the following steps: the second intermediate product is mixed with a reducing agent solution.
In the present invention, the drawing is performed in a reducing agent solution; the drafting specifically comprises the following steps: sequentially wrapping and contacting the first intermediate product with a drafting shaft; the rotating speed of the drafting shaft increases progressively along the advancing direction of the second intermediate product; the number of the drafting shafts is more than or equal to 2.
In the present invention, the linear velocity difference between the adjacent two draft shafts is 0.2 to 0.3 rpm.
In the present invention, the preparation method further comprises: carrying out heat treatment on the second intermediate product after the second reduction treatment; the temperature of the heat treatment is 2500-3500K.
In the step (1), the mixing time is 3-5 min; the drafting time is 15-30 s; in the step (3), the mixing time is 3-5 min.
The invention also provides a drafting device comprising: a drawing tank for accommodating a reducing agent solution; a draft shaft provided along a forward direction of the drafted object; the number of the drafting shafts is more than or equal to 2.
In the present invention, the rotation speed of the draft shaft increases in the advancing direction of the drafted article.
The invention also provides application of the three-dimensional graphene in preparation of a material with a metal type carrier characteristic.
The invention provides a method for triggering a metal type carrier transport mode in situ in three-dimensional graphene oxide, which is characterized in that more fold morphology of a percolation network configuration is constructed on the surface of the three-dimensional graphene through plastic drafting and reduction treatment, and the fold morphology of the surface of the three-dimensional graphene can realize the metal type carrier transport mode, namely, a band structure is converted from a band gap open type to a band gap overlapped type. The embodiment of the invention proves that after the three-dimensional graphene oxide is treated by a method comprising liquid phase reduction and plastic stretching, the conductivity is reduced from 2.7-3.4 (100K) to 1.7-2.2 (300K) along with the increase of temperature.
The invention provides a method for triggering a metal carrier transport mode in situ in three-dimensional graphene oxide, which can avoid the inconvenience in execution of the traditional doping technologies such as element doping, field effect doping and the like, and realize the regulation and control of a local micro-area and a global carrier transport mode; in addition, the three-dimensional graphene containing the fold morphology still retains the inherent mechanical performance advantages of graphene, such as light weight, high strength, flexibility, and the like.
Drawings
Fig. 1 is a schematic diagram of a plasticizing and drafting device according to an embodiment of the present invention, wherein the device is composed of a roller device and a liquid phase working medium tank, and the roller device includes a driving roller 1, a driving roller 2, a driving roller 1 and a driving roller 2;
fig. 2 is a three-dimensional graphene scanning electron microscope image of embodiment 1 of the present invention;
FIG. 3 is a graph showing the conductivity as a function of temperature for example 1 of the present invention;
fig. 4 is a three-dimensional graphene scanning electron microscope diagram of embodiment 2 of the present invention;
FIG. 5 is a graph showing the change of conductivity with temperature according to example 2 of the present invention;
fig. 6 is a three-dimensional graphene scanning electron microscope image of embodiment 3 of the present invention;
FIG. 7 is a graph showing the change of conductivity with temperature in example 3 of the present invention.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention adopts the following technical scheme:
a method for preparing three-dimensional graphene, comprising:
(1) Carrying out first reduction treatment on the flaky three-dimensional graphene oxide to obtain a first intermediate product;
(2) Drawing the first intermediate product to obtain a second intermediate product;
(3) And carrying out a second reduction treatment on the second intermediate product to obtain the three-dimensional graphene.
In the present invention, the first reduction treatment is specifically: mixing flaky three-dimensional graphene oxide with a reducing agent solution; the mixing time is 3-5 min, preferably 3min;
the second reduction treatment specifically comprises the following steps: mixing the second intermediate product with a reducing agent solution; the mixing time is 3 to 5 minutes, preferably 3 minutes.
In the present invention, the drawing is performed in a reducing agent solution; the drafting time is 5-30 s; the drafting time is preferably 5s, and the state is maintained for 10s after the drafting is completed; the drafting specifically comprises the following steps: sequentially wrapping and contacting the first intermediate product with a drafting shaft; the rotating speed of the drafting shaft increases progressively along the advancing direction of the second intermediate product; the number of the drafting shafts is more than or equal to 2.
In the present invention, the linear velocity difference between the adjacent two draft shafts is 0.2 to 0.3 rpm.
In the invention, the reducing agent solution is obtained by mixing a reducing agent and a solvent; the solvent is an organic solvent; the molecular weight of the reducing agent is less than or equal to 500; the reducing agent is preferably hydrogen iodide; in one embodiment of the present invention, the reducing agent solution is a hydrogen iodide solution, and the hydrogen iodide solution is obtained by mixing ethanol and hydrogen iodide; the volume ratio of the ethanol to the hydrogen iodide is (1-4) 1, preferably 1:1.
in the present invention, the preparation method further comprises: carrying out heat treatment on the second intermediate product after the second reduction treatment; the temperature of the heat treatment is 2500-3500K, preferably 2500K; the time of the heat treatment is preferably 5 to 8 hours, preferably 5 hours.
In the invention, the mass ratio of the three-dimensional graphene oxide to the reducing agent solution is 1 (1-100); the mass ratio of the second intermediate product to the reducing agent solution is 1 (1-100).
The invention also provides a drafting device comprising: a drawing tank for accommodating a reducing agent solution; a draft shaft provided along a forward direction of the drafted object; the number of the drafting shafts is more than or equal to 2, preferably 2.
In the invention, the drafting shaft can be arranged in the drafting groove or outside the drafting groove, and when the drafting shaft is arranged outside the drafting groove, the drafting device also comprises a transmission shaft arranged in the drafting groove; the number of the transmission shafts is preferably 2.
In the present invention, the rotation speed of the drafting shaft increases gradually along the advancing direction of the drafted object; the linear speed difference of two adjacent drafting shafts is 0.2-0.3 r/min.
In one embodiment of the present invention, the drafting device is composed of a drafting groove and 4 rollers, and the rollers arranged along the direction of the drafted object are: the driving roller 1, the driving roller 2 and the driving roller 2 are filled with a reducing agent solution, as shown in fig. 1, the driving roller 1 and the driving roller 2 are immersed in liquid phase working medium, the driving roller 1 and the driving roller 2 are arranged outside the drawing tank, the driving roller 1 and the driving roller 2 are used as drawing shafts, and the rotating speed of the driving roller 1 is V 0 The rotation speed of the driving roller 2 is V 1 ；V 1 -V 0 =0.25 rpm.
The preparation method has no special requirement on the three-dimensional graphene oxide, and the preparation method of the three-dimensional graphene oxide preferably comprises the following steps of: preparing graphene oxide dispersion liquid into three-dimensional graphene oxide by a vacuum suction filtration auxiliary template pouring method; the concentration of the graphene oxide dispersion liquid is 7-9 mg/L.
The invention also provides application of the three-dimensional graphene in preparation of a material with a metal type carrier characteristic.
The three-dimensional graphene prepared by the method has the characteristic of a metal type carrier, and can be used as an in-situ metal interconnection line in an all-carbon electronic device.
The invention provides a method for triggering a metal type carrier transport mode in situ in three-dimensional graphene oxide, which is characterized in that more fold morphology of a percolation network configuration is constructed on the surface of the three-dimensional graphene through plastic drafting and reduction treatment, and the fold morphology of the surface of the three-dimensional graphene can realize the metal type carrier transport mode, namely, a band structure is converted from a band gap open type to a band gap overlapped type. The embodiment of the invention proves that after the three-dimensional graphene oxide is treated by a method comprising liquid phase reduction and plastic stretching, the conductivity is reduced from 2.7-3.4 (100K) to 1.7-2.2 (300K) along with the increase of temperature.
The invention provides a method for triggering a metal carrier transport mode in situ in three-dimensional graphene oxide, which can avoid the inconvenience in execution of the traditional doping technologies such as element doping, field effect doping and the like, and realize the regulation and control of a local micro-area and a global carrier transport mode; in addition, the three-dimensional graphene containing the fold morphology still retains the inherent mechanical performance advantages of graphene, such as light weight, high strength, flexibility, and the like.
In order to further illustrate the present invention, the following examples are provided. The raw materials used in the following examples of the present invention are all commercially available.
Example 1
In this embodiment, a drafting device is used to prepare three-dimensional graphene, the drafting device is composed of a drafting groove and 4 rollers, and the rollers arranged along the direction of the drafted object are sequentially: as shown in fig. 1, a liquid phase working medium (reducing agent solution) is filled in a drawing groove, the driving roller 1 and the driving roller 2 are immersed in the liquid phase working medium, the driving roller 1 and the driving roller 2 are arranged outside the drawing groove, the driving roller 1 and the driving roller 2 are the drawing shafts, and the linear speed of the driving roller 1 is V 0 The linear velocity of the driving roller 2 is V 1 ；V 1 -V 0 =0.25 rpm.
The preparation method of the three-dimensional graphene in the embodiment comprises the following steps:
(1) And (3) selecting graphene oxide dispersion liquid with the concentration of 7mg/L (graphene oxide single layer rate is more than 90%, the characteristic dimension is 12 mu m (the position with the largest in-plane linear distance) and the ZETA potential is 30 mV) as raw materials, placing the graphene oxide dispersion liquid into a suction filtration device under the environment with the relative humidity of 60%, and preparing the three-dimensional graphene oxide by a vacuum suction filtration auxiliary template pouring method, wherein the macroscopic shape of the three-dimensional graphene oxide is a film, and the thickness of the three-dimensional graphene oxide is about 50 mu m.
(2) Loading the flaky three-dimensional graphene oxide obtained in the step (1) into a driving roller device, fixing the linking position through a double-sided adhesive tape, and standing the three-dimensional graphene oxide between a driving roller 1 and a driving roller 2 in a liquid phase working medium for 3 minutes as shown in figure 1.
(3) Mechanical load drafting process: the drive roller 1 and the drive roller 2 were synchronously turned on, and both maintained a linear velocity difference of 0.25 revolutions per minute (rotational velocity V of the drive roller 1 0 Is 1 revolution/min, the rotational speed V of the driving roller 2 1 Is 1.25 revolutions per minute). The single operation time of the driving roller is 5s, and the driving roller is kept in a mechanical state for 10s after the driving roller is completed.
(4) Carrying out liquid phase reduction treatment on the three-dimensional graphene oxide after plasticizing and drafting treatment: and (3) completely immersing the three-dimensional graphene oxide in a mixed solution of absolute ethyl alcohol and hydrogen iodide for reduction treatment (the volume ratio of the absolute ethyl alcohol to the hydrogen iodide is 1:1), wherein the duration of the liquid phase reduction treatment is 3 minutes.
(5) And carrying out high-temperature heat treatment on the three-dimensional graphene subjected to the liquid-phase reduction treatment, wherein the temperature of the heat treatment is 2500K, and the heat treatment time is 5 hours.
The microstructure of the three-dimensional graphene subjected to plasticizing and drawing treatment is shown in fig. 2, and the sample has a typical wrinkled microstructure. As shown in fig. 3, the conductivity of the sample showed a monotonically decreasing trend with increasing temperature, with typical metal-type carrier transport characteristics.
Example 2
The drafting device in the embodiment 1 is adopted in the embodiment, and the preparation method of the three-dimensional graphene comprises the following steps:
(1) And (3) selecting graphene oxide dispersion liquid with the concentration of 7mg/L (the graphene oxide single-layer rate is more than 90%, the characteristic dimension is 12 mu m, the ZETA potential is 30 mV) as a raw material, preparing the three-dimensional graphene oxide by a vacuum filtration auxiliary template pouring method under the environment with the relative humidity of 60%, wherein the macroscopic shape of the three-dimensional graphene oxide is a film, and the thickness is about 50 mu m.
(2) And (3) loading the flaky three-dimensional graphene oxide prepared in the step (1) into a driving roller device, and fixing the linking position through a double-sided adhesive tape. And standing the three-dimensional graphene between the transmission roller 1 and the transmission roller 2 in the liquid phase working medium for 3 minutes.
(3) Mechanical load drafting process: the drive roller 1 and the drive roller 2 were turned on simultaneously, and they were kept at a linear velocity difference of 0.25 rpm (the rotational speed of the drive roller 1 was 0.25 rpm, and the rotational speed of the drive roller 2 was 0.5 rpm). The single operation time of the driving roller is 5s, and the driving roller is kept in a mechanical state for 10s after the driving roller is completed.
(4) And (3) carrying out liquid-phase reduction treatment on the three-dimensional graphene oxide after plasticizing and drawing treatment, and fully immersing the three-dimensional graphene oxide in a mixed solution of absolute ethyl alcohol and hydrogen iodide for reduction treatment (the volume ratio is 1:1), wherein the duration of the liquid-phase reduction treatment is 3 minutes.
(5) And carrying out high-temperature heat treatment on the three-dimensional graphene subjected to the liquid-phase reduction treatment, wherein the temperature of the heat treatment is 2500K, and the heat treatment time is 5 hours.
The microstructure of the three-dimensional graphene subjected to plasticizing and drawing treatment is shown in fig. 4, and the sample has a typical wrinkled microstructure. As shown in fig. 5, the conductivity of the sample showed a monotonically decreasing trend with increasing temperature, with typical metal-type carrier transport characteristics.
Example 3
The drafting device in the embodiment 1 is adopted in the embodiment, and the preparation method of the three-dimensional graphene comprises the following steps:
(1) And (3) selecting graphene oxide dispersion liquid with the concentration of 7mg/L (the graphene oxide single-layer rate is more than 90%, the characteristic dimension is 12 mu m, the ZETA potential is 30 mV) as a raw material, preparing the three-dimensional graphene oxide by a vacuum filtration auxiliary template pouring method under the environment with the relative humidity of 60%, wherein the macroscopic shape of the three-dimensional graphene oxide is a film, and the thickness is about 50 mu m.
(2) And (3) loading the flaky three-dimensional graphene oxide prepared in the step (1) into a driving roller device, and fixing the linking position through a double-sided adhesive tape. And (3) standing the three-dimensional graphene oxide between the transmission roller 1 and the transmission roller 2 in the liquid phase working medium for 3 minutes.
(3) Mechanical load drafting process: the drive roller 1 and the drive roller 2 were turned on simultaneously, and they were kept at a linear velocity difference of 0.25 rpm (the rotational speed of the drive roller 1 was 0.5 rpm, and the rotational speed of the drive roller 2 was 0.75 rpm). The single operation time of the driving roller is 5s, and the driving roller is kept in a mechanical state for 10s after the driving roller is completed.
(4) And (3) carrying out liquid-phase reduction treatment on the three-dimensional graphene oxide after plasticizing and drawing treatment, and fully immersing the three-dimensional graphene oxide in a mixed solution of absolute ethyl alcohol and hydrogen iodide for reduction treatment (the volume ratio is 1:1), wherein the duration of the liquid-phase reduction treatment is 3 minutes.
(5) And carrying out high-temperature heat treatment on the three-dimensional graphene subjected to the liquid-phase reduction treatment, wherein the temperature of the heat treatment is 2500K, and the heat treatment time is 5 hours.
The microstructure of the three-dimensional graphene subjected to plasticizing and drawing treatment is shown in fig. 6, and the sample has a typical wrinkled microstructure. As shown in fig. 7, the conductivity of the sample showed a monotonically decreasing trend with increasing temperature, with typical metal-type carrier transport characteristics.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The preparation method of the three-dimensional graphene is characterized by comprising the following steps of:
(1) Carrying out first reduction treatment on the flaky three-dimensional graphene oxide to obtain a first intermediate product;
(2) Drawing the first intermediate product to obtain a second intermediate product;
(3) And carrying out a second reduction treatment on the second intermediate product to obtain the three-dimensional graphene.
2. The method for preparing three-dimensional graphene according to claim 1, wherein the first reduction treatment specifically comprises: mixing flaky three-dimensional graphene oxide with a reducing agent solution;
the second reduction treatment specifically comprises the following steps: the second intermediate product is mixed with a reducing agent solution.
3. The method for preparing three-dimensional graphene according to claim 1, wherein the drawing is performed in a reducing agent solution.
4. The method for preparing three-dimensional graphene according to claim 1 or 3, wherein the drafting specifically comprises:
sequentially wrapping and contacting the first intermediate product with a drafting shaft;
the rotating speed of the drafting shaft increases progressively along the advancing direction of the second intermediate product;
the number of the drafting shafts is more than or equal to 2.
5. The method for preparing three-dimensional graphene according to claim 4, wherein the linear velocity difference between two adjacent drafting axes is 0.2 to 0.3 rpm.
6. The method for preparing three-dimensional graphene according to claim 1, further comprising: carrying out heat treatment on the second intermediate product after the second reduction treatment;
the temperature of the heat treatment is 2500-3500K.
7. The method for preparing three-dimensional graphene according to claim 1, wherein in the step (1), the mixing time is 3 to 5 minutes;
the drafting time is 15-30 s;
in the step (3), the mixing time is 3-5 min.
8. A drafting apparatus comprising:
a drawing tank for accommodating a reducing agent solution;
a draft shaft provided along a forward direction of the drafted object;
the number of the drafting shafts is more than or equal to 2.
9. Drafting device according to claim 8, characterized in that the rotation speed of the drafting shaft increases in the advancing direction of the drafted article.
10. Use of the three-dimensional graphene prepared by the preparation method of the three-dimensional graphene according to any one of claims 1 to 7 for preparing a material with a metal type carrier characteristic.
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Citations (3)
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|---|---|---|---|---|
| CN107032329A (en) * | 2016-02-03 | 2017-08-11 | 全球能源互联网研究院 | A kind of three-dimensional grapheme of nano-micrometre classification pore passage structure and preparation method thereof |
| CN108530073A (en) * | 2017-10-08 | 2018-09-14 | 北京化工大学 | A kind of preparation method of the three-dimensional porous graphene film of flexible self-supporting |
| CN111003703A (en) * | 2019-11-29 | 2020-04-14 | 杭州高烯科技有限公司 | Structure function integrated graphene material and preparation method thereof |
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2023
- 2023-04-17 CN CN202310407589.6A patent/CN116281986A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107032329A (en) * | 2016-02-03 | 2017-08-11 | 全球能源互联网研究院 | A kind of three-dimensional grapheme of nano-micrometre classification pore passage structure and preparation method thereof |
| CN108530073A (en) * | 2017-10-08 | 2018-09-14 | 北京化工大学 | A kind of preparation method of the three-dimensional porous graphene film of flexible self-supporting |
| CN111003703A (en) * | 2019-11-29 | 2020-04-14 | 杭州高烯科技有限公司 | Structure function integrated graphene material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| PENG LI: "Continuous crystalline graphene papers with gigapascal strength by intercalation modulated plasticization", 《NATURE COMMUNICATIONS》, vol. 11, 27 May 2020 (2020-05-27), pages 1 - 10 * |
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