CN116462192A - Preparation method of modified graphene filler - Google Patents
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- CN116462192A CN116462192A CN202310515519.2A CN202310515519A CN116462192A CN 116462192 A CN116462192 A CN 116462192A CN 202310515519 A CN202310515519 A CN 202310515519A CN 116462192 A CN116462192 A CN 116462192A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 239000000945 filler Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 75
- 229910052751 metal Inorganic materials 0.000 claims abstract description 22
- 239000002184 metal Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000000151 deposition Methods 0.000 claims abstract description 16
- 230000008021 deposition Effects 0.000 claims abstract description 16
- 238000004070 electrodeposition Methods 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000576 coating method Methods 0.000 claims abstract description 10
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 229910052742 iron Inorganic materials 0.000 claims abstract description 6
- 230000003647 oxidation Effects 0.000 claims description 13
- 238000007254 oxidation reaction Methods 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 9
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 241000080590 Niso Species 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000003792 electrolyte Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 26
- 230000001590 oxidative effect Effects 0.000 abstract description 6
- 239000007769 metal material Substances 0.000 abstract description 5
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 5
- 150000004706 metal oxides Chemical class 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 5
- 230000004048 modification Effects 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 2
- 239000003990 capacitor Substances 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000004519 grease Substances 0.000 abstract description 2
- 229920001296 polysiloxane Polymers 0.000 abstract description 2
- 230000027756 respiratory electron transport chain Effects 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 abstract description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 48
- 239000011701 zinc Substances 0.000 description 32
- 239000011787 zinc oxide Substances 0.000 description 24
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 17
- 229910052725 zinc Inorganic materials 0.000 description 16
- 238000002441 X-ray diffraction Methods 0.000 description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000013078 crystal Substances 0.000 description 8
- 239000002131 composite material Substances 0.000 description 7
- 239000002086 nanomaterial Substances 0.000 description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000002194 synthesizing effect Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000643 oven drying Methods 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- RZLVQBNCHSJZPX-UHFFFAOYSA-L zinc sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Zn+2].[O-]S([O-])(=O)=O RZLVQBNCHSJZPX-UHFFFAOYSA-L 0.000 description 2
- 238000007385 chemical modification Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- -1 microwave Chemical class 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
A preparation method of modified graphene filler belongs to the technical field of surface modification of graphene. The preparation method comprises the steps of directly dispersing graphene into a deposition precursor liquid, performing electrodeposition preparation under slow stirring, taking a metal sheet as an anode, taking an iron net as a cathode, realizing electron transfer through collision between the graphene sheet and the cathode in the deposition liquid, thereby preparing a double-layer structure graphene/metal material on the surface of the graphene, further oxidizing to prepare a three-layer structure graphene/metal oxide material, and adopting the three-layer structure material prepared by the method, wherein a coating and a graphene body have good binding force, so that the defect that a metal coating is difficult to directly deposit on the surface of common graphene lacking active groups in the traditional technology is overcome. The prepared graphene/metal oxide material is expected to be applied to the fields of metal corrosion and protection, electrocatalytic materials, high-performance super capacitors, industrial analysis and separation, heat conduction silicone grease and the like.
Description
Technical Field
The invention relates to surface modification of graphene, in particular to a preparation method of modified graphene filler.
Background
Graphene, which is used as a novel two-dimensional carbon nanomaterial, has large theoretical specific surface area, excellent conductivity and mechanical properties, good chemical stability and shielding performance, and is widely applied to various fields such as nano medicine carrying, supercapacitors, electrochemical sensors, solar cells, metal corrosion and protection. However, the common graphene has higher chemical inertia and is not easy to uniformly disperse due to the lack of active groups on the surface, and the application limit of the common graphene can be broken through only by adopting a method of introducing active functional groups through surface chemical modification. At present, graphene oxide is mainly used as a raw material for surface modification of graphene, and modification is realized through abundant active functional groups. The inert surface of the common graphene is directly modified by electrochemical deposition and other methods, so that the work is very little.
Some metal coatings, such as metal zinc, have excellent atmospheric corrosion resistance, a protective film is easy to form on the surface at normal temperature, most of the current researches report that metal zinc is electroplated on metal, and graphene shows that the work of electroplating metal zinc is less. Meanwhile, zinc oxide has the advantages of no toxicity and harm, easy preparation, stable chemical property, low cost and the like, and becomes a semiconductor material with better development prospect. ZnO is used in a number of fields such as: photocatalytic, dye sensitized solar cells, perovskite solar cells, and the like. The composite material of the synthetic ZnO can change the physical properties of the composite material and meet the application requirements of the composite material in various fields. Graphene, as a novel carbon nanomaterial, has been widely studied since discovery of advantages such as a large specific surface area, good electrical conductivity, excellent chemical stability, and easiness in synthesizing a novel composite material with other materials. For the ZnO nanomaterial, various excellent properties of graphene are beneficial to improving defects existing in the ZnO nanomaterial, so that various properties of the ZnO nanomaterial are improved. Researchers have developed various methods for synthesizing ZnO and graphene composites, such as microwave, hydrothermal, chemical vapor deposition, spray pyrolysis, and the like. However, most methods for synthesizing ZnO/graphene composite films are too complex and involve severe conditions such as high temperature and high pressure. The electrodeposition method is a simple preparation method which is green, environment-friendly, controllable and does not involve conditions such as high temperature, high pressure and the like, and has better development prospects in actual production and application compared with other methods.
Disclosure of Invention
The invention aims to solve the problems that the existing method for synthesizing a ZnO/graphene composite film is too complex and involves severe conditions such as high temperature and high pressure, and the like, and provides a preparation method of a modified graphene filler.
The aim of the invention is realized by the following technical scheme:
a method of preparing a modified graphene filler, the method comprising the steps of:
(1) Preparing an electrodeposition precursor solution;
(2) Uniformly dispersing graphene in an electrodeposition precursor solution;
(3) Taking the mixed solution obtained in the step (2) as electrolyte, taking a metal sheet as an anode and an iron mesh as a cathode, and electrodepositing a metal coating on the surface of the graphene;
(4) Purifying and drying the modified graphene obtained by electrodeposition;
(5) And (3) carrying out surface high-temperature oxidation on the modified graphene in a muffle furnace to obtain the modified graphene filler.
Further, in the step (1), the precursor solution comprises 0.1-1mol/L of metal salt, 1-10g/L of additive PEG and 0.1-0.3g/L of sodium dodecyl sulfate, wherein the metal salt is CoSO 4 ·7H 2 O、Al 2 (SO 4 ) 3 、NiSO 4 ·7H 2 O、ZnSO 4 ·7H 2 O、MgSO 4 ·7H 2 O、CuSO 4 ·5H 2 One of O.
Further, in the step (1), the precursor solution further comprises 1-10g/L KCl.
Further, in the step (2), the concentration of the graphene is 0.5-2 g/L.
Further, in the step (3), the electrodeposition potential is controlled to be 0-30.0V, the rotating speed is controlled to be 10-100 rmp, the deposition temperature is controlled to be 25-65 ℃, and the deposition time is controlled to be 2-10 min.
Further, in the step (5), the temperature of the oxidation is 150-500 ℃ and the time is 2-8 hours.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a method for directly realizing batch deposition of metal coating on common graphene powder, preparing a double-layer structure graphene/metal material, and oxidizing the double-layer structure graphene/metal material into a three-layer structure graphene/metal oxide material. The method is simple and controllable, environment-friendly and safe, low in cost and expected to realize large-scale industrial application.
Drawings
Fig. 1 is an SEM photograph of pure graphene;
FIG. 2 is an SEM photograph of graphene electrodeposited to prepare a graphene/Zn material;
FIG. 3 is an SEM photograph of graphene electrodeposited to prepare a graphene/Zn/ZnO material;
FIG. 4 is an XRD pattern of pure graphene, graphene/Zn/ZnO materials;
figure 5 shows XRD patterns of different oxidation temperatures and oxidation times.
Detailed Description
The following description of the present invention refers to the accompanying drawings and examples, but is not limited to the same, and modifications and equivalents of the present invention can be made without departing from the spirit and scope of the present invention.
The invention discloses a method for preparing a three-layer structured graphene/metal oxide material on the surface of graphene by electrodeposition. The preparation method comprises the steps of directly dispersing graphene into a deposition precursor liquid, performing electrodeposition preparation under slow stirring, taking a metal sheet as an anode, taking an iron net as a cathode, realizing electron transfer through collision between the graphene sheet and the cathode in the deposition liquid, thereby preparing a double-layer structure graphene/metal material on the surface of the graphene, oxidizing the prepared double-layer graphene/metal material to prepare a three-layer structure graphene/metal oxide material, and adopting the three-layer structure material prepared by the method, wherein a coating and a graphene body have good binding force, so that the defect that a metal coating is difficult to directly deposit on the surface of common graphene lacking active groups in the traditional technology is overcome. The prepared material is expected to be applied to the fields of corrosion and protection of metals, electrocatalytic materials, high-performance super capacitors, industrial analysis and separation, heat conduction silicone grease and the like.
Example 1:
and electrodepositing metallic zinc on the surface of the graphene to prepare a double-layer structured graphene/Zn material, and oxidizing the double-layer structured graphene/Zn material to prepare the three-layer structured graphene/Zn/ZnO material.
(1) Preparing a precursor solution: 400mL of deionized water and 50mL of ethanol are added into a 600mL beaker, 4g of polyethylene glycol, 42g of zinc sulfate heptahydrate and 0.1g of sodium dodecyl sulfate are added, and the mixture is stirred uniformly for later use;
(2) Adding 0.5g of graphene into the precursor liquid, uniformly dispersing the graphene for 40min by ultrasonic treatment, wherein the ultrasonic power is 250W, the zinc sheet is an anode, the iron net is a cathode, the electrodeposition potential is 15V, the deposition time is 5min, and the deposition temperature is 25 ℃;
(3) Washing with deionized water and ethanol twice after deposition, centrifuging at 500rpm for 5min, and oven drying at 30deg.C;
(4) And oxidizing the prepared double-layer structural material graphene/Zn for 6 hours at 400 ℃ to prepare graphene/Zn/ZnO.
By Scanning Electron Microscope (SEM) observation and X-ray diffraction (XRD) of the obtained sample, the figure 1 shows that the surface of the pure graphene sheet layer has folds but has smoother surface and no other impurities, the figure 2 shows that the thickness of the sheet layer is obviously increased between 70 nm and 100nm, the plating layer is uniform and continuous, no defects such as obvious cracks and the like exist, and the surface of the pure graphene sheet layer is rougher than the surface of the pure graphene sheet layer in comparison with the figure 1, which shows that a layer of metal zinc with uniform thickness is successfully plated on the surface of the graphene sheet layer. Fig. 3 shows that the oxidation of the metallic zinc coating to zinc oxide, the coating shows a slight structural disruption. From the XRD pattern of fig. 4, it can be seen that a relatively distinct graphitized diffraction peak appears in the XRD pattern of graphene, which corresponds to the (002) and (004) crystal planes of graphite, and the diffraction peaks are located around 26.5 ° and 54.6 °, respectively (PDF # 41-1487). In the XRD pattern of the graphene/Zn material, the intensity of the diffraction peak of the graphite crystal face (002) is greatly reduced, and meanwhile, diffraction peaks (PDF#99-0110) which are matched with crystal faces of zinc (002), (100), (101), (103), (111), (112) and (201) appear at 36.4 degrees, 39.2 degrees, 43.4 degrees, 70.2 degrees, 70.8 degrees, 82.3 degrees and 86.7 degrees. It can be shown that metallic zinc is introduced on the surface of graphene by electrodeposition. In the XRD spectrum of the graphene/zinc oxide composite material, diffraction peaks (PDF#99-0111) which are consistent with crystal faces of zinc oxide (100), (002), (101), (102), (110), (103) and (112) appear at 31.8 degrees, 34.5 degrees, 36.4 degrees, 47.7 degrees, 56.7 degrees and 62.9 degrees and 68.1 degrees on the basis of the original diffraction peaks of graphene and zinc. Meanwhile, diffraction peak intensities of crystal faces of zinc (002), (100), (101) and the like are reduced, which shows that the graphene/Zn double-layer structure material is successfully oxidized to prepare the graphene/Zn/ZnO three-layer structure material.
Example 2:
and electrodepositing metallic zinc on the surface of the graphene to prepare a double-layer structured graphene/Zn material, and oxidizing the double-layer structured graphene/Zn material to prepare the three-layer structured graphene/Zn/ZnO material.
(1) Preparing a precursor solution: 700mL of deionized water and 100mL of ethanol are added into a 1000mL beaker, 4g of polyethylene glycol, 42g of zinc sulfate heptahydrate, 0.1g of sodium dodecyl sulfate and 9g of potassium chloride are added, and the mixture is stirred uniformly for later use;
(2) Adding 1g of graphene into the precursor liquid, uniformly dispersing the graphene for 40min by ultrasonic treatment, wherein the ultrasonic power is 250W, the zinc sheet is an anode, the iron net is a cathode, the electrodeposition potential is 12V, the deposition time is 10min, and the deposition temperature is 25 ℃;
(3) Washing with deionized water and ethanol twice after deposition, centrifuging at 500rpm for 5min, and oven drying at 30deg.C;
(4) And (3) placing the prepared graphene/Zn with the double-layer structure material in a muffle furnace for oxidation for 4 or 6 hours at 300 ℃ or for oxidation for 4 hours at 400 or 500 ℃ to prepare the graphene/Zn/ZnO.
When the obtained sample was subjected to X-ray diffraction (XRD), it was found from fig. 5 that the diffraction peak intensities of the crystal planes of zinc oxide (100), (002), (101), (102), (110), (103), (112) became apparent at the oxidation temperature of 300 ℃, while the diffraction peak intensities of zinc oxide were found not to significantly vary with respect to the peak intensity of metallic zinc with the increase of oxidation time from the XRD pattern, and that the diffraction peak intensities of the crystal planes of zinc oxide (100), (002), (101), (102), (110), (103), (112) became more apparent from the XRD pattern at the oxidation temperature of 400 ℃, while the ratio of the diffraction peak intensities of zinc oxide was significantly higher than the ratio of the peak intensities of metallic zinc at 300 ℃, and that the diffraction peak intensities of the crystal planes of zinc oxide (100), (002), (101), (102), (110), (103), (112) were sharp at the oxidation temperature of 500 ℃, while the diffraction peak of metallic zinc (101) was substantially not found in the XRD pattern.
Claims (6)
1. A preparation method of modified graphene filler is characterized by comprising the following steps: the method comprises the following steps:
(1) Preparing an electrodeposition precursor solution;
(2) Uniformly dispersing graphene in an electrodeposition precursor solution;
(3) Taking the mixed solution obtained in the step (2) as electrolyte, taking a metal sheet as an anode and an iron mesh as a cathode, and electrodepositing a metal coating on the surface of the graphene;
(4) Purifying and drying the modified graphene obtained by electrodeposition;
(5) And (3) carrying out surface high-temperature oxidation on the modified graphene in a muffle furnace to obtain the modified graphene filler.
2. The method for preparing the modified graphene filler according to claim 1, wherein: in step (1), the precursorThe liquid comprises 0.1-1mol/L metal salt, 1-10g/L additive PEG, 0.1-0.3g/L sodium dodecyl sulfate, wherein the metal salt is CoSO 4 ·7H 2 O、Al 2 (SO 4 ) 3 、NiSO 4 ·7H 2 O、ZnSO 4 ·7H 2 O、MgSO 4 ·7H 2 O、CuSO 4 ·5H 2 One of O.
3. The method for preparing the modified graphene filler according to claim 2, wherein: in the step (1), the precursor solution also comprises 1-10g/L KCl.
4. The method for preparing the modified graphene filler according to claim 1, wherein: in the step (2), the concentration of the graphene is 0.5-2 g/L.
5. The method for preparing the modified graphene filler according to claim 1, wherein: in the step (3), the electric deposition potential is controlled to be 0-30.0V, the rotating speed is controlled to be 10-100 rmp, the deposition temperature is controlled to be 25-65 ℃, and the deposition time is controlled to be 2-10 min.
6. The method for preparing the modified graphene filler according to claim 1, wherein: in the step (5), the temperature of the oxidation is 150-500 ℃ and the time is 2-8 hours.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550003A (en) * | 2009-04-22 | 2009-10-07 | 湖南大学 | Nano-graphite alkenyl composite wave-absorbing material and method of preparing the same |
| US20140141600A1 (en) * | 2012-11-21 | 2014-05-22 | Samsung Electronics Co., Ltd. | Methods of preparing graphene and device including graphene |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550003A (en) * | 2009-04-22 | 2009-10-07 | 湖南大学 | Nano-graphite alkenyl composite wave-absorbing material and method of preparing the same |
| US20140141600A1 (en) * | 2012-11-21 | 2014-05-22 | Samsung Electronics Co., Ltd. | Methods of preparing graphene and device including graphene |
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