CN115354375A - Preparation method of graphene/diamond composite film - Google Patents
Preparation method of graphene/diamond composite film Download PDFInfo
- Publication number
- CN115354375A CN115354375A CN202210992097.3A CN202210992097A CN115354375A CN 115354375 A CN115354375 A CN 115354375A CN 202210992097 A CN202210992097 A CN 202210992097A CN 115354375 A CN115354375 A CN 115354375A
- Authority
- CN
- China
- Prior art keywords
- graphene
- diamond
- powder
- composite film
- diamond powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
Abstract
The invention provides a preparation method of a graphene/diamond composite film. The method comprises the following process steps: 1. treating diamond powder by utilizing piranha washing liquor to remove impurities on the surface of the powder, and carrying out hydroxylation treatment on the surface of the powder; 2. ultrasonically dispersing the washed diamond powder in deionized water, and adding a proper amount of graphene oxide aqueous solution; 3. under magnetic stirring, dropwise adding a sodium borohydride solution with a certain concentration into the diamond powder/graphene oxide mixed solution, and continuously stirring until the graphene oxide is completely reduced; 4. centrifugally washing the diamond powder/graphene composite for multiple times; 5. filtering the clear solution, and drying to obtain diamond powder/graphene mixed powder; 6. and depositing diamond powder/graphene mixed powder with different proportions on a steel substrate through electrodeposition to obtain the graphene/diamond composite film. The process flow is simple and easy to operate, and graphene/diamond composite films with different mass ratios can be obtained by pretreating diamond powder with piranha washing liquid.
Description
Technical Field
The invention relates to a method for preparing a graphene/diamond composite film, belonging to the technical field of chemical preparation of materials.
Background
Graphene is a polymer made of carbon atoms in sp 2 The two-dimensional nano material with a honeycomb crystal structure formed by hybridization has excellent mechanical, thermal, electrical and electric conductivity and thermal conductivity due to the unique lattice structure. The method has wide application prospect in the aspects of field effect transistors, high-frequency electronic devices, transparent conductive films, composite materials, energy storage materials, electrochemical sensors and the like. Diamond is a simple substance composed of carbon element, and is ground state electricThe structure of the seed is 1s 2 2s 2 2p 2 The 2s layer electrons of the carbon atom form sp with the electrons in the 2p layer 3 The hybrid orbit of (1), therefore every carbon atom and adjacent carbon atom around form the saturated covalent bond with the sp3 hybrid orbit, form the regular tetrahedron structure, the crystal structure of diamond determines it has a series of excellent physical and chemical properties, such as excellent mechanical properties, good heat conductivity, chemical stability, high thermal conductivity and high insulating property, etc., have wide application in fields such as electron, traffic and engineering, etc.
The graphene/diamond composite film is expected to fully utilize the excellent performances of diamond and graphene, obtain more excellent comprehensive performances, and has wide application prospects in the fields of electronics, engineering, civil use and the like.
Disclosure of Invention
The technical problem is as follows: the invention aims to provide a preparation method of a graphene/diamond composite film, which comprises the steps of treating diamond powder by utilizing piranha washing liquid, removing impurities on the surface of the powder, carrying out hydroxylation treatment on the surface of particles, mixing the particles with graphene oxide, reducing by utilizing sodium borohydride, carrying out centrifugal washing, and depositing diamond powder/graphene mixed powder with different proportions on a steel substrate by adopting electrodeposition to obtain the graphene/diamond composite film.
The technical scheme is as follows: according to the invention, piranha washing liquor is adopted to treat the diamond powder, impurities on the surface of the diamond powder are removed, and the surface of the diamond powder particles is subjected to hydroxylation modification, so that the combination of the diamond powder particles and the reduced graphene is firmer and more stable. And mixing the graphene oxide powder and the graphene oxide powder, performing original treatment by using sodium borohydride, and depositing diamond powder/graphene mixed powder with different proportions on a steel substrate through electrodeposition to obtain the graphene/diamond composite film.
The technical scheme adopted comprises the following steps:
step one, weighing 0.5-3 g diamond powder, adding the diamond powder into piranha washing liquid, ultrasonically dispersing, centrifugally washing for multiple times, and ultrasonically dispersing in deionized water to prepare diamond powder dispersion liquid;
adding a graphene oxide aqueous solution into the diamond powder dispersion liquid, and performing ultrasonic dispersion to prepare a diamond powder-graphene oxide dispersion liquid;
step three, dropwise adding a sodium borohydride aqueous solution in the process of magnetically stirring the diamond powder-graphene oxide dispersion liquid, and continuously magnetically stirring for 1-3 hours;
step four, centrifugally washing the dispersion liquid treated in the step three for multiple times, and drying the clear liquid after suction filtration to obtain diamond powder/graphene mixed powder;
and step five, depositing diamond powder/graphene mixed powder with different proportions on a steel substrate through electro-deposition to obtain the graphene/diamond composite film.
Wherein the piranha washing solution is a mixed solution of concentrated sulfuric acid and hydrogen peroxide, and the volume ratio is 7:3.
The graphene oxide aqueous solution is obtained by Hummers, the concentration is 10-20 mg/mL, and the adding amount is 2-8 mL. The concentration of the sodium borohydride aqueous solution is 3-8M, and the adding amount is 10-20 mL. The parameters of the electrodeposition process are as follows: 2-7A/dm < 2 >, the deposition time is 3-9 min, the deposition temperature is 45 ︒ C, the concentration of nickel sulfate in the electrolyte is nickel sulfate electrochemical deposition precursor solution is 25-100mmol/L, and the concentration of nickel chloride is 0.5-2mol/L.
Has the advantages that: diamond powder is pretreated by utilizing piranha washing liquor, so that not only can impurities on the surface of the diamond powder be removed, but also the surface of diamond powder particles is subjected to hydroxylation modification, and the combination of the diamond powder particles and the reduced graphene is firmer and more stable.
The method adopts electrodeposition to deposit the graphene/diamond mixed powder with different proportions on a steel substrate, and can obtain graphene/diamond composite films with different mass ratios. The technological process is simple to operate, and the composite material is uniformly and firmly distributed. The obtained graphene/diamond composite membrane has wide application prospect in the fields of electronics, traffic, engineering, life and the like.
Drawings
Fig. 1 is an SEM image of a graphene/diamond composite film. From the figure, the graphene and the diamond particles are uniformly and tightly combined.
Fig. 2 is a raman spectrum of the graphene/diamond composite film. From this figure it can be foundThree main distinctive peaks of graphene, D (1350 cm) -1 )，G (1680 cm -1 ) And 2D (2680 cm) -1 ). The intensity of the D peak is higher than that of the G peak, which shows that the graphene has more defects, such as folds and the like; the intensity of the 2D peak is far lower than that of the G peak, which indicates that the prepared graphene has more layers.
Detailed Description
The invention provides a preparation method of a graphene/diamond composite film. Firstly, 0.5-3 g diamond powder is dispersed in piranha washing liquid, impurities on the surface of the powder are removed, hydroxylation treatment is carried out on the surface of the powder, and the powder is centrifugally washed for many times by deionized water. Ultrasonically dispersing the washed diamond powder in 30-100 mL deionized water, and adding 2-8 mL aqueous solution of graphene oxide with the concentration of 10 mg/L. Adding 10-20 mL sodium borohydride solution with the concentration of 3.9M into the mixed solution of diamond powder and graphene oxide, and continuing to stir by magnetic force until the graphene oxide is completely reduced. The diamond powder/graphene composite is centrifugally washed for multiple times, and the graphene/diamond mixed powder with different proportions is deposited on the steel substrate by adopting electrodeposition, so that the graphene/diamond composite membranes with different mass ratios can be obtained. And observing the appearance of the sample by using a Scanning Electron Microscope (SEM), and detecting the structure of the graphene by using a Raman spectrum.
Example 1:
dispersing 1 g diamond powder in piranha washing solution, removing impurities on the surface of the powder, hydroxylating the surface of the powder, and centrifugally washing the powder for 3 times by using deionized water. Ultrasonically dispersing the treated diamond powder in 50 mL deionized water, adding 5 mL aqueous solution of graphene oxide with the concentration of 10 mg/L, and ultrasonically dispersing for 30 min. In the magnetic stirring process, a sodium borohydride solution with the concentration of 15 mL of 3.9M is added into the graphene/diamond mixed solution drop by drop, and 2 h is continuously magnetically stirred until the graphene oxide is completely reduced. And centrifuging and washing the graphene/diamond composite for multiple times, and depositing the graphene/diamond mixed powder with different proportions on a steel substrate by adopting electrodeposition to obtain the graphene/diamond composite membranes with different mass ratios.
Example 2:
dispersing 0.5 g diamond powder in piranha washing solution, removing impurities on the surface of the powder, hydroxylating the surface of the powder, and centrifugally washing the powder for 3 times by using deionized water. Ultrasonically dispersing the treated diamond powder in 40 mL deionized water, adding 3mL of graphene oxide aqueous solution with the concentration of 10 mg/L, and ultrasonically dispersing for 20 min. In the magnetic stirring process, a sodium borohydride solution with the concentration of 10 mL of 3.9M is added into the mixed solution of diamond powder and graphene oxide dropwise, and the magnetic stirring is continued for 1 h until the graphene oxide is completely reduced. The graphene/diamond composite was washed several times by centrifugation. The method adopts electrodeposition to deposit the graphene/diamond mixed powder with different proportions on a steel substrate, and can obtain graphene/diamond composite films with different mass ratios.
Example 3:
dispersing 2.5 g diamond powder in piranha washing liquid, removing impurities on the surface of the powder, hydroxylating the surface of the powder, and centrifugally washing the powder for 3 times by using deionized water. The treated diamond powder is ultrasonically dispersed in 60 mL deionized water, and 3mL aqueous solution with the concentration of 10 mg/L is added for ultrasonic dispersion for 50 min. In the magnetic stirring process, a sodium borohydride solution with the concentration of 10 mL of 3.9M is added into the mixed solution of diamond powder and graphene oxide drop by drop, and the magnetic stirring is continued for 1 h until the graphene oxide is completely reduced. The graphene/diamond composite was washed several times by centrifugation. The method adopts electrodeposition to deposit the graphene/diamond mixed powder with different proportions on a steel substrate, and can obtain graphene/diamond composite films with different mass ratios.
Claims (10)
1. A method of graphene/diamond composite film, the method comprising:
step one, weighing 0.5-3 g diamond powder, adding the diamond powder into piranha washing liquid, ultrasonically dispersing, centrifugally washing for multiple times, and ultrasonically dispersing in deionized water to prepare diamond powder dispersion liquid;
adding a graphene oxide aqueous solution into the diamond powder dispersion liquid, and performing ultrasonic dispersion to prepare a diamond powder-graphene oxide dispersion liquid;
step three, dropwise adding a sodium borohydride aqueous solution in the process of magnetically stirring the diamond powder-graphene oxide dispersion liquid, and continuously magnetically stirring for 1-3 hours;
step four, after centrifugally washing the dispersion liquid treated in the step three for multiple times, carrying out suction filtration on the clear liquid and then drying to obtain diamond powder/graphene mixed powder;
and step five, depositing diamond powder/graphene mixed powder with different proportions on a steel substrate through electro-deposition to obtain the graphene/diamond composite film.
2. The method of preparing a graphene/diamond composite film according to claim 1, wherein the piranha washing solution in the first step is a mixed solution of concentrated sulfuric acid and hydrogen peroxide, and the volume ratio is (3-10) to (1-7).
3. The method for preparing the graphene/diamond composite film according to claim 1, wherein the graphene oxide aqueous solution in the second step is obtained by Hummers, the concentration is 2-15 mg/mL, and the addition amount is 2-8 mL.
4. The method for preparing the graphene/diamond composite film according to claim 1, wherein the concentration of the aqueous sodium borohydride solution in the third step is 2.0-5.6M, and the dropwise addition amount is the volume ratio of the aqueous sodium borohydride solution to the diamond powder-graphene oxide dispersion liquid.
5. The method for preparing a graphene/diamond composite film according to claim 1, wherein in the first step, the time for ultrasonic dispersion is 20-50 min.
6. The method for preparing the graphene/diamond composite film according to claim 1, wherein in the second step, the time for the ultrasonic dispersion is 10 to 60 min.
7. The method for preparing the graphene/diamond composite film according to claim 1, wherein in the third step, a sodium borohydride aqueous solution is added dropwise during the magnetic stirring of the diamond powder-graphene oxide dispersion, and the magnetic stirring is continued for 1 to 3 hours.
8. The method of preparing a graphene/diamond composite film according to claim 1, wherein in the fourth step, the dispersion is centrifugally washed several times, and the supernatant is filtered and dried.
9. The method of manufacturing a graphene/diamond composite film according to claim 1, wherein in the fifth step, the diamond powder/graphene mixed powder is deposited on the steel substrate by electrodeposition in various ratios to obtain the graphene/diamond composite film, wherein the conductive substrate other than the steel substrate is also in a protective range.
10. The method for preparing a graphene/diamond composite film according to claim 1, wherein in the fifth step, electrodeposition process parameters are as follows: 2-7A/dm < 2 >, the deposition time is 3-9 min, the deposition temperature is 45 ︒ C, the concentration of nickel sulfate in the electrolyte is nickel sulfate electrochemical deposition precursor solution is 25-100mmol/L, and the concentration of nickel chloride is 0.5-2mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210992097.3A CN115354375A (en) | 2022-08-18 | 2022-08-18 | Preparation method of graphene/diamond composite film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210992097.3A CN115354375A (en) | 2022-08-18 | 2022-08-18 | Preparation method of graphene/diamond composite film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115354375A true CN115354375A (en) | 2022-11-18 |
Family
ID=84003445
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210992097.3A Pending CN115354375A (en) | 2022-08-18 | 2022-08-18 | Preparation method of graphene/diamond composite film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115354375A (en) |
-
2022
- 2022-08-18 CN CN202210992097.3A patent/CN115354375A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Yang et al. | Plasma-modified Ti 3 C 2 T x/CdS hybrids with oxygen-containing groups for high-efficiency photocatalytic hydrogen production | |
| Xia et al. | Designing N-doped graphene/ReSe2/Ti3C2 MXene heterostructure frameworks as promising anodes for high-rate potassium-ion batteries | |
| CN104445167B (en) | A kind of preparation method of water-soluble graphene | |
| US10807872B2 (en) | Graphene oxide quantum dot, material composed of same and graphene-like structure, and preparation method therefor | |
| Li et al. | Hierarchical graphene oxide/polyaniline nanocomposites prepared by interfacial electrochemical polymerization for flexible solid-state supercapacitors | |
| CN110117049B (en) | Preparation method of metal-organic framework/polypyrrole hybrid conductive electrode | |
| CN112758950B (en) | Boron alkene nanosheets and preparation method thereof | |
| CN103614902B (en) | A kind of preparation method of graphene/carbon fiber composite | |
| CN106700136B (en) | A kind of graphene/Chitosan Composites and preparation method thereof | |
| Shi et al. | Superior carbon belts from Spirogyra for efficient extracellular electron transfer and sustainable microbial energy harvesting | |
| CN101003909A (en) | Electrochemical combined deposition method for preparing structure of composite membrane of Nano carbon tube - metal | |
| CN107934965B (en) | Ti3C2-Co(OH)(CO3)0.5Process for preparing nano composite material | |
| CN102674337A (en) | Self-extension graphene and preparation method thereof | |
| CN110451615B (en) | Preparation method of metal-organic framework carbon nanotube hybrid desalination electrode | |
| CN109534335A (en) | A kind of preparation method of large scale graphene oxide and thus obtained large scale graphene oxide | |
| CN114917861B (en) | High-conductivity three-dimensional composite material, preparation method and application thereof in treatment of nitrogen-phosphorus organic wastewater | |
| CN109592684A (en) | A kind of petal spherical carbide titanium and its preparation method and application | |
| Zhang et al. | Facile synthesis of carbon nanotube-supported NiO//Fe2O3 for all-solid-state supercapacitors | |
| CN115354375A (en) | Preparation method of graphene/diamond composite film | |
| CN105420794B (en) | A kind of preparation method of graphene/ferriferrous oxide composite material | |
| CN112133926A (en) | Preparation method of platinum/titanium carbide nanosheet/graphene three-dimensional composite electrode catalyst | |
| KR100797775B1 (en) | Diamond/carbon nano-materials hybrid film and the fabrication method thereof | |
| CN113529047A (en) | Preparation method of MXene/C composite material | |
| KR20130105063A (en) | Method for preparing grephene oxide thin layer by radio frequency magnetron sputtering and grephene oxide thin layer produced by the same | |
| CN111203243A (en) | Preparation and application of nickel selenide/graphene composite material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication |