CN104694989A - Preparation method of graphene-base metal composite material - Google Patents
Preparation method of graphene-base metal composite material Download PDFInfo
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- CN104694989A CN104694989A CN201510107704.3A CN201510107704A CN104694989A CN 104694989 A CN104694989 A CN 104694989A CN 201510107704 A CN201510107704 A CN 201510107704A CN 104694989 A CN104694989 A CN 104694989A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
Abstract
The invention provides a preparation method of a graphene-base metal composite material, which comprises the following steps: by using a graphene aerogel as a working electrode in a three-electrode system, carrying out electrodeposition to obtain a graphene-base metal composite pre-product, and carrying out heat treatment on the graphene-base metal composite pre-product to obtain the graphene-base metal composite material. By adopting the electrodeposition process, the preparation method of the graphene-base metal composite material does not relate to any high-energy-consumption high-pollution operation, and has high environment friendliness.
Description
Technical field
The invention belongs to graphene-based field of compound material, be specifically related to a kind of preparation method of graphene-based metal composite.
Background technology
Graphene is a kind of monolayer carbon atomic plane two-dimensional material separated from graphite material, is to build other dimension Carbon Materials as the basic structural unit of zero dimension soccerballene, one-dimensional nano carbon pipe and graphite etc.The structure of Graphene uniqueness makes it have much peculiar character, such as: Graphene has room-temperature quantum Hall effect; Its intensity is the highest in current all material, up to 130GPa; Its carrier mobility reaches 15000cm
2.V
-1.s
-1, exceed more than 10 times of commercial silicon chip mobility; Thermal conductivity is up to 5000W.m
-1.K
-1, being adamantine 3 times, is more than 5 times of Carbon fibe; In addition, the theoretical specific surface area of Graphene is also very high, reaches 2630m in theory
2.g
-1.
Three-dimensional grapheme not only part remains the unique excellent mechanics of Graphene, calorifics and electric property, is also changed to the research viewpoint of Graphene to macroscopical block materials by microcosmic nano material, and is that lower good basis is established in its further macroscopic view application.In three-dimensional grapheme, the advantage of graphene aerogel is maximum, it is integrated with the advantage such as Graphene and aerogel high-ratio surface, high porosity, high conductivity and good thermal conductivity, has great application potential in fields such as detector, catalyzer and carrier thereof, absorption, electrochemical energy storage and electrical condensers.
Because the intensity of simple graphite oxide aerogel is lower, constrain it to apply further, therefore, sight focuses in the modification of three-dimensional grapheme aerogel by people, and the attention rate of the matrix material with graphene aerogel and metal in numerous modifying method is higher.In prior art, prepare method many employings methane of graphene-based metal composite, ethene as carbon source, be prepared under the hot conditions of 700 ~ 1000 DEG C, not only energy consumption is high, and the tail gas produced causes pollution to environment.
Summary of the invention
The present invention carries out for solving the problem, and by providing a kind of preparation method of graphene-based metal composite newly, improves the environment friendly of graphene-based metal composite preparation process further.
Present invention employs following technical scheme:
The preparation method of graphene-based metal composite provided by the invention, has such feature, comprises the following steps:
Step one, using graphene aerogel as the working electrode in three-electrode system, pH be 1 ~ 7 with in the electrolytic solution of metal ion, galvanic deposit 0.1 ~ 24h under 25 ~ 90 DEG C of temperature condition, obtains graphene-based metal composite pre-product;
Step 2, by the graphene-based metal composite pre-product in step one in atmosphere of inert gases, is heat-treat 1 ~ 10h under the condition of 100 ~ 900 DEG C in temperature, obtains described graphene-based metal composite.
The preparation method of graphene-based metal composite provided by the invention, can also have such feature: also comprise and the graphene-based metal composite pre-product obtained in step one is dipped to the step that pH is 7 in clear water.
The preparation method of graphene-based metal composite provided by the invention, such feature can also be had: in step one, the preparation method of graphene aerogel is: configuration concentration is the graphene oxide water solution of 0.01 ~ 10mg/mL, after 100 ~ 200 DEG C of Water Under thermal treatment 20h, form Graphene hydrogel, Graphene hydrogel obtains graphene aerogel after lyophilize 72h under-60 DEG C of conditions.
The preparation method of graphene-based metal composite provided by the invention, can also have such feature: in step 2, and electrolytic solution is made up of damping fluid and metal ion liquid,
Damping fluid comprises 0.01 ~ 1mol/L Na
3c
6h5O
72H
2o, 0.01 ~ 1mol/L H
3bO
3and 0.01 ~ 1mol/L NaH
2pO
2h
2o,
Metal ion liquid comprises 0.01 ~ 1mol/L FeSO
47H
2o, 0.01 ~ 1mol/LCoSO
47H
2o, 0.01 ~ 1mol/L CuSO
45H
2o and 0.01 ~ 1mol/L MnSO
4in any one or a few.
The preparation method of graphene-based metal composite provided by the invention, can also have such feature: in step 2, and atmosphere of inert gases is any one in nitrogen atmosphere and argon atmosphere.
The preparation method of graphene-based metal composite provided by the invention, can also have such feature: in three-electrode system, and platinized platinum and saturated dry mercury electrode are respectively as to electrode and reference electrode.
Invention effect and effect
The invention provides a kind of preparation method of graphene-based metal composite, first using graphene aerogel as the working electrode in three-electrode system, adopt the method for galvanic deposit, obtain graphene-based metal composite pre-product, then, the graphene-based metal composite pre-product obtained obtains graphene-based metal composite through Overheating Treatment again.Owing to adopting the method for galvanic deposit, make the preparation method of graphene-based metal composite provided by the invention not relate to any high energy consumption high pollution operation, environment friendly is strong.
Accompanying drawing explanation
Fig. 1 is the SEM figure of graphene aerogel in embodiments of the invention one;
Fig. 2 is the SEM figure of graphene-based metal composite in embodiments of the invention two;
Fig. 3 is the Raman collection of illustrative plates of the graphene-based metal composite in embodiments of the invention two;
Fig. 4 is the infrared spectrogram of the graphene-based metal composite in embodiments of the invention two;
Fig. 5 is the intensity map of the graphene-based metal composite in embodiments of the invention four;
Fig. 6 is the SEM figure of the graphene-based metal composite in embodiments of the invention seven.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described.
The preparation method of graphene aerogel
Embodiment one
Present embodiments provide the preparation method of graphene aerogel: configuration concentration is the graphene oxide water solution of 0.01 ~ 10mg/mL, after 100 ~ 200 DEG C of Water Under thermal treatment 20h, form Graphene hydrogel, Graphene hydrogel under-60 DEG C of conditions after lyophilize 72h to graphene aerogel.
Fig. 1 is the SEM figure of the graphene aerogel of the present embodiment.
As shown in Figure 1, in the microtexture of graphene aerogel, graphene sheet layer is continuous, is hierarchical porous structure.
The preparation method of graphene-based metal composite
Embodiment two
The preparation method of the graphene-based metal composite in the present embodiment is preferred method, comprises the following steps:
Step one, graphene aerogel in embodiment one is carried out galvanic deposit in three-electrode system, and wherein, the graphene aerogel in embodiment one is working electrode, Pt sheet and saturated dry mercury electrode are respectively electrode and reference electrode, and electrolyte is 0.24mol/L FeSO
47H
2o, 0.16mol/L CoSO
47H
2o, 0.8mol/L Na
3c
6h
5o
72H
2o, 0.2mol/LH
3bO
3and 0.8mol/L NaH
2pO
2h
2the mixed solution of O, pH is 3, and depositing temperature is 60 DEG C, and depositing time is 2h, obtains graphene-based metal composite pre-product;
Step 2, it is 7 that the graphene-based metal composite pre-product in step one is dipped to pH in clear water, obtains schungite thiazolinyl metal composite;
Step 3, by the schungite thiazolinyl metal composite in step 2 under the protection of condition of nitrogen gas, is heat-treat 5h under the condition of 500 DEG C in temperature, obtains graphene-based metal composite.
The ultimate compression strength of the graphene-based metal composite prepared according to the method for the present embodiment is 100KPa, and resistance is 10-100 Ω.
Fig. 2 is the SEM figure of the graphene-based metal composite in the present embodiment.
As shown in Figure 2, by the electro-deposition techniques in the present embodiment, metallic particles can be made to grow uniformly in the pore structure of graphene aerogel.
Fig. 3 is the Raman spectrogram of the graphene-based metal composite in the present embodiment.
As shown in Figure 3, electro-deposition techniques makes metallic particles and graphene aerogel produce physical adsorption, does not produce new chemical bond, remains the physicochemical property that graphene aerogel is excellent.
Fig. 4 is the infrared spectrogram of the graphene-based metal composite of the present embodiment.
As shown in Figure 4, through the electro-deposition techniques process of different time, graphene aerogel does not produce new chemical bond, remains itself good physicochemical property.
Embodiment three
The preparation method of graphene-based metal composite, comprises the following steps:
Step one, graphene aerogel in embodiment one is carried out galvanic deposit in three-electrode system, and wherein, the graphene aerogel in embodiment one is working electrode, Pt sheet and saturated dry mercury electrode are respectively electrode and reference electrode, and electrolyte is 0.5mol/L FeSO
47H
2o, 0.5mol/L MnSO
4, 1.0mol/L Na
3c
6h
5o
72H
2o, 0.3mol/L H
3bO
3and 0.5mol/L NaH
2pO
2h
2the mixed solution of O, pH is 4, and depositing temperature is 60 DEG C, and depositing time is 6h, obtains graphene-based metal composite pre-product;
Step 2, it is 7 that the graphene-based metal composite pre-product in step one is dipped to pH in clear water, obtains schungite thiazolinyl metal composite;
Step 3, by the schungite thiazolinyl metal composite in step 2 under the protection of condition of nitrogen gas, is heat-treat 10h under the condition of 100 DEG C in temperature, obtains graphene-based metal composite.
The ultimate compression strength of the graphene-based metal composite prepared according to the method for the present embodiment is about 50KPa, and resistance is 10-100 Ω.
Embodiment four
The preparation method of graphene-based metal composite, comprises the following steps:
Step one, graphene aerogel in embodiment one is carried out galvanic deposit in three-electrode system, and wherein, the graphene aerogel in embodiment one is working electrode, Pt sheet and saturated dry mercury electrode are respectively electrode and reference electrode, and electrolyte is 1.0mol/L FeSO
47H
2o, 1mol/L CuSO
45H
2o, 0.5mol/L Na
3c
6h
5o
72H
2o, 0.5mol/LH
3bO
3and 0.8mol/L NaH
2pO
2h
2the mixed solution of O, pH is 2, and depositing temperature is 25 DEG C, and depositing time is 24h, obtains graphene-based metal composite pre-product;
Step 2, it is 7 that the graphene-based metal composite pre-product in step one is dipped to pH in clear water, obtains schungite thiazolinyl metal composite;
Step 3, by the schungite thiazolinyl metal composite in step 2 under the protection of condition of nitrogen gas, is heat-treat 0.1h under the condition of 900 DEG C in temperature, obtains graphene-based metal composite.
The ultimate compression strength of the graphene-based metal composite prepared according to the method for the present embodiment is about 5KPa, and resistance is 10-100 Ω.
Fig. 5 is the graphene-based metal composite stress-strain diagram in the present embodiment.
Shown in Fig. 5, graphene-based metal composite physical strength can reach 5KPa.
Embodiment five
The preparation method of graphene-based metal composite, comprises the following steps:
Step one, graphene aerogel in embodiment one is carried out galvanic deposit in three-electrode system, and wherein, the graphene aerogel in embodiment one is working electrode, Pt sheet and saturated dry mercury electrode are respectively electrode and reference electrode, and electrolyte is 0.5mol/L CoSO
45H
2o, 1mol/L MnSO
4, 0.01mol/L Na
3c
6h
5o
72H
2o, 0.8mol/L H
3bO
3and 1mol/L NaH
2pO
2h
2the mixed solution of O, pH is 2, and depositing temperature is 90 DEG C, and depositing time is 0.01h, obtains graphene-based metal composite pre-product;
Step 2, it is 7 that the graphene-based metal composite pre-product in step one is dipped to pH in clear water, obtains schungite thiazolinyl metal composite;
Step 3, by the schungite thiazolinyl metal composite in step 2 under the protection of condition of nitrogen gas, is heat-treat 5h under the condition of 500 DEG C in temperature, obtains graphene-based metal composite.
The ultimate compression strength of the graphene-based metal composite prepared according to the method for the present embodiment is about 30KPa, and resistance is 10-100 Ω.
Embodiment six
The preparation method of graphene-based metal composite, comprises the following steps:
Step one, graphene aerogel in embodiment one is carried out galvanic deposit in three-electrode system, and wherein, the graphene aerogel in embodiment one is working electrode, Pt sheet and saturated dry mercury electrode are respectively electrode and reference electrode, and electrolyte is 1mol/L CoSO
45H
2o, 0.5mol/L CuSO
45H
2o, 0.5mol/L Na
3c
6h
5o
72H
2o, 0.9mol/LH
3bO
3and 0.01mol/L NaH
2pO
2h
2the mixed solution of O, pH is 2, and depositing temperature is 60 DEG C, and depositing time is 10h, obtains graphene-based metal composite pre-product;
Step 2, it is 7 that the graphene-based metal composite pre-product in step one is dipped to pH in clear water, obtains schungite thiazolinyl metal composite;
Step 3, by the schungite thiazolinyl metal composite in step 2 under the protection of argon gas condition, is heat-treat 5h under the condition of 500 DEG C in temperature, obtains graphene-based metal composite.
The ultimate compression strength of the graphene-based metal composite prepared according to the method for the present embodiment is about 70KPa, and resistance is 10-100 Ω.
Embodiment seven
The preparation method of graphene-based metal composite, comprises the following steps:
Step one, graphene aerogel in embodiment one is carried out galvanic deposit in three-electrode system, and wherein, the graphene aerogel in embodiment one is working electrode, Pt sheet and saturated dry mercury electrode are respectively electrode and reference electrode, and electrolyte is 0.75mol/L FeSO47H
2o, 0.75mol/L CoSO
47H
2o, 0.01mol/L MnSO
4, 0.8mol/L Na
3c
6h
5o
72H
2o, 0.01mol/L H
3bO
3and 0.8mol/L NaH
2pO
2h
2the mixed solution of O, pH is 7, and depositing temperature is 60 DEG C, and depositing time is 12h, obtains graphene-based metal composite pre-product;
Step 2, it is 7 that the graphene-based metal composite pre-product in step one is dipped to pH in clear water, obtains schungite thiazolinyl metal composite;
Step 3, by the schungite thiazolinyl metal composite in step 2 under the protection of argon gas condition, is heat-treat 5h under the condition of 500 DEG C in temperature, obtains graphene-based metal composite.
The ultimate compression strength of the graphene-based metal composite prepared according to the method for the present embodiment is about 20KPa, and resistance is 10-100 Ω.
Fig. 6 is the SEM figure of the graphene-based metal composite in the present embodiment.
As shown in Figure 6, graphenic surface is covered completely by metallics.
Embodiment eight
The preparation method of graphene-based metal composite, comprises the following steps:
Step one, graphene aerogel in embodiment one is carried out galvanic deposit in three-electrode system, and wherein, the graphene aerogel in embodiment one is working electrode, Pt sheet and saturated dry mercury electrode are respectively electrode and reference electrode, and electrolyte is 0.01mol/L FeSO47H
2o, 0.75mol/L CuSO
45H
2o, 1mol/L MnSO
4, 0.25mol/L Na
3c
6h
5o
72H
2o, 1mol/L H
3bO
3and 0.25mol/L NaH
2pO
2h
2the mixed solution of O, pH is 1, and depositing temperature is 60 DEG C, and depositing time is 12h, obtains graphene-based metal composite pre-product;
Step 2, it is 7 that the graphene-based metal composite pre-product in step one is dipped to pH in clear water, obtains schungite thiazolinyl metal composite;
Step 3, by the schungite thiazolinyl metal composite in step 2 under the protection of argon gas condition, is heat-treat 5h under the condition of 500 DEG C in temperature, obtains graphene-based metal composite.
The ultimate compression strength of the graphene-based metal composite prepared according to the method for the present embodiment is about 80KPa, and resistance is 10-100 Ω.
Embodiment nine
The preparation method of graphene-based metal composite, comprises the following steps:
Step one, graphene aerogel in embodiment one is carried out galvanic deposit in three-electrode system, and wherein, the graphene aerogel in embodiment one is working electrode, Pt sheet and saturated dry mercury electrode are respectively electrode and reference electrode, and electrolyte is 1mol/L CoSO
47H
2o, 0.01mol/L CuSO
45H
2o, 0.25mol/L MnSO
4, 0.5mol/L Na
3c
6h
5o
72H
2o, 0.9mol/L H
3bO
3and 0.01mol/L NaH
2pO
2h
2the mixed solution of O, pH is 2, and depositing temperature is 60 DEG C, and depositing time is 12h, obtains graphene-based metal composite pre-product;
Step 2, it is 7 that the graphene-based metal composite pre-product in step one is dipped to pH in clear water, obtains schungite thiazolinyl metal composite;
Step 3, by the schungite thiazolinyl metal composite in step 2 under the protection of argon gas condition, is heat-treat 5h under the condition of 500 DEG C in temperature, obtains graphene-based metal composite.
The ultimate compression strength of the graphene-based metal composite prepared according to the method for the present embodiment is about 100KPa, and resistance is 10-100 Ω.
Embodiment ten
The preparation method of graphene-based metal composite, comprises the following steps:
Step one, graphene aerogel in embodiment one is carried out galvanic deposit in three-electrode system, and wherein, the graphene aerogel in embodiment one is working electrode, Pt sheet and saturated dry mercury electrode are respectively electrode and reference electrode, and electrolyte is 0.25mol/L FeSO47H
2o, 0.25mol/L CoSO
45H
2o, 0.25mol/L CuSO
45H
2o, 0.25mol/LMnSO
4,0.8mol/L Na
3c
6h
5o
72H
2o, 0.2mol/L H
3bO
3and 0.8mol/LNaH
2pO
2h
2the mixed solution of O, pH is 3, and depositing temperature is 60 DEG C, and depositing time is 2h, obtains graphene-based metal composite pre-product;
Step 2, it is 7 that the graphene-based metal composite pre-product in step one is dipped to pH in clear water, obtains schungite thiazolinyl metal composite;
Step 3, by the schungite thiazolinyl metal composite in step 2 under the protection of argon gas condition, is heat-treat 5h under the condition of 500 DEG C in temperature, obtains graphene-based metal composite.
The ultimate compression strength of the graphene-based metal composite prepared according to the method for the present embodiment is about 100KPa, and resistance is 10-100 Ω.
Embodiment effect and effect
Embodiment provides a kind of preparation method of graphene-based metal composite, using graphene aerogel as the working electrode in three-electrode system, adopt the method for galvanic deposit, obtain graphene-based metal composite pre-product, graphene-based metal composite pre-product obtains graphene-based metal composite through immersion and thermal treatment again.Owing to adopting the method for galvanic deposit, make the preparation process of graphene-based metal composite not relate to any high energy consumption high pollution operation, environment friendly is strong.
The graphene-based metal composite prepared according to the method for embodiment is except having the bigger serface of general gel, also there is good physical strength, its anti-pressure ability can graphene-based metal composite more of the prior art anti-pressure ability improve several to tens times, and this composite shapes is controlled, electroconductibility is strong, resistance becomes 10 ~ 100 Ω from a kilo-ohm level for graphene aerogel, make this graphene-based metal composite have larger application prospect in absorption and catalysis, also can be used as electrode of super capacitor.
The invention is not restricted to the scope of embodiment; to those skilled in the art; as long as various change to limit and in the spirit and scope of the present invention determined in described claim; these changes are apparent, and all innovation and creation utilizing the present invention to conceive are all at the row of protection.
Claims (6)
1. a preparation method for graphene-based metal composite, is characterized in that, comprises the following steps:
Step one, using graphene aerogel as the working electrode in three-electrode system, pH be in 1 ~ 7 with galvanic deposit 0.1 ~ 24h in the electrolytic solution of metal ion, under 25 ~ 90 DEG C of temperature condition, obtain graphene-based metal composite pre-product;
Step 2, heat-treats 1 ~ 10h in atmosphere of inert gases, temperature under being the condition of 100 ~ 900 DEG C by the described graphene-based metal composite pre-product in step one, obtains described graphene-based metal composite.
2. the preparation method of graphene-based metal composite according to claim 1, is characterized in that:
In described step 2, before the heat treatment, also comprise the described graphene-based metal composite pre-product obtained in step one is dipped to the step that pH is 7 in clear water.
3. the preparation method of graphene-based metal composite according to claim 1, is characterized in that:
Wherein, in step, the preparation method of described graphene aerogel is: configuration concentration is the graphene oxide water solution of 0.01 ~ 10mg/mL, after hydrothermal treatment consists 20h, form Graphene hydrogel under 100 ~ 200 DEG C of conditions, described Graphene hydrogel obtains described graphene aerogel after lyophilize 72h under-60 DEG C of conditions.
4. the preparation method of graphene-based metal composite according to claim 1, is characterized in that:
Wherein, in step one, described electrolytic solution is made up of damping fluid and metal ion liquid,
Described damping fluid comprises 0.01 ~ 1mol/L Na
3c
6h5O
72H
2o, 0.01 ~ 1mol/LH
3bO
3and 0.01 ~ 1mol/L NaH
2pO
2h
2o,
Described metal ion liquid comprises 0.01 ~ 1mol/L FeSO
47H
2o, 0.01 ~ 1mol/LCoSO
47H
2o, 0.01 ~ 1mol/L CuSO
45H
2o and 0.01 ~ 1mol/L MnSO
4in any one or a few.
5. the preparation method of graphene-based metal composite according to claim 1, is characterized in that:
Wherein, in described step 2, described atmosphere of inert gases is any one in nitrogen atmosphere and argon atmosphere.
6. the preparation method of graphene-based metal composite according to claim 1, is characterized in that:
Wherein, in described three-electrode system, platinized platinum and saturated dry mercury electrode are respectively as to electrode and reference electrode.
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| CN104973594A (en) * | 2015-06-26 | 2015-10-14 | 江苏大学 | Preparation method and applications of graphene aerogel |
| CN105420794A (en) * | 2015-11-13 | 2016-03-23 | 上海应用技术学院 | Preparation method for graphene/ferroferric oxide composite material |
| CN105800597A (en) * | 2016-02-26 | 2016-07-27 | 成都新柯力化工科技有限公司 | Method for preparing mechanically peeled high-conductivity composite graphene |
| CN105923627A (en) * | 2016-06-07 | 2016-09-07 | 南京邮电大学 | Preparation method of porous graphene |
| CN107256803A (en) * | 2017-06-29 | 2017-10-17 | 天津师范大学 | A kind of preparation method of graphene/carbon aerogel composite |
| CN107513745A (en) * | 2016-06-15 | 2017-12-26 | 中国科学院兰州化学物理研究所苏州研究院 | A kind of preparation method of the three-dimensional porous composite of graphene metal oxide |
| CN110106534A (en) * | 2019-05-15 | 2019-08-09 | 南京理工大学 | A method of it prepares with the super-hydrophobic nickel surface of timber mirror surface structure |
| CN111101172A (en) * | 2019-12-31 | 2020-05-05 | 新疆烯金石墨烯科技有限公司 | Graphene-aluminum composite material and preparation method thereof |
| CN113235130A (en) * | 2021-04-12 | 2021-08-10 | 中山大学 | Low-platinum composite material based on tungsten oxide/graphene aerogel and preparation method and application thereof |
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