CN109368626A - A kind of electrolyte for electrochemical stripping two-dimension nano materials - Google Patents
A kind of electrolyte for electrochemical stripping two-dimension nano materials Download PDFInfo
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- CN109368626A CN109368626A CN201811538990.9A CN201811538990A CN109368626A CN 109368626 A CN109368626 A CN 109368626A CN 201811538990 A CN201811538990 A CN 201811538990A CN 109368626 A CN109368626 A CN 109368626A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/003—Phosphorus
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
Abstract
The present invention is a kind of electrolyte containing Multiple components, which is used to prepare graphene and class graphene two-dimension nano materials by electrochemical stripping effect.The electrolyte is using the mixed liquor of deionized water and ethyl alcohol as solvent, the electrolyte containing there are many, and under the action of electrochemical reaction, the electrode of layer structure material such as graphite composition can fast and efficiently be removed into two-dimension nano materials in the electrolyte.The electrolyte have many advantages, such as it is environmentally protective, at low cost, high-efficient, be suitable as removing two-dimension nano materials electrolyte.
Description
Technical field
The present invention relates to graphene and the preparation fields of class grapheme two-dimension material, and specifically one kind can be in electrification
Learn a kind of electrolyte that two-dimension nano materials are prepared under reagentia.
Background technique
Ideal graphene is two-dimensional monoatomic layer graphite, has very high specific surface area, excellent chemistry, thermostabilization
Property, good electric conductivity and heating conduction, the properties such as excellent mechanical performance are studied from the Geim of Univ Manchester UK
Since the method synthesizing graphite alkene that group was removed in 2004 by micromechanics, people are caused to graphene and its composite material
Research boom, so that graphene has great application prospect in fields such as catalysis, electronics, the energy, biological medicine, materials, together
When, class graphene two-dimension nano materials have good catalytic hydrogen evolution living such as molybdenum disulfide nano thin slice, black phosphorus nano flake
Property and storage lithium performance, had potential application in catalysis and energy storage field.
Graphene or class grapheme two-dimension material can be prepared by a variety of methods, can be broadly divided into physical method and change
Method, wherein physical method can be divided into micromechanics removing, liquid/vapor the methods of is directly removed, and chemical method can be divided into chemistry
The methods of the methods of vapor deposition (CVD), oxidation-reduction method, electrochemical stripping method.CVD method is by gas phase reaction under high temperature
And the method for being deposited on graphene in solid film substrate, this method can prepare the graphene of high quality, large area, but cost
High, complex process and process conditions are harsh constrains its development.Presently the most common oxide-reduction method, the method are producing
The strong acid and strong oxidizer for having strong corrosive, strong oxidizing property to chemical industry equipment have been used in the process, have biggish danger to environment
Evil, and the electronic structure and crystal perfection that form graphene, by serious destruction, conductivity has apparent reduction, limitation
It further develops.The method of electrochemical stripping can be shelled by the electrode that the electrochemical reaction of electrode forms layer structure
From at two-dimension nano materials, graphene and class graphene two-dimensional nano piece are prepared, but efficiency is lower, and the two dimension separated
Nanometer sheet is thicker, limits its further development.
In the electrolyte that the present invention develops, under the release effect of electrochemical reaction, the electricity of layered solid material composition
Extremely charge stripping efficiency can be greatly improved by efficient, clean removing at two-dimensional nano thin slice.
Summary of the invention
In order to efficiently, cleaning, the preparation of low cost have crystal structure complete, graphene of large specific surface area and
Class graphene two-dimension nano materials, the purpose of the present invention is to provide one kind, and height can be carried out under electrochemical reaction release effect
The electrolyte for imitating stripped laminar material, under the action of electrochemical reaction, the electrode of stratified material composition can be by efficient, clear
Clean, safe and stable removing is at two-dimension nano materials, and prepared two-dimensional material is with crystal structure is complete, thickness is thin, area
The advantages that adjustable controllable.
In order to achieve the above objectives, the technical solution of the present invention is as follows:
Ethyl alcohol is add to deionized water first, the volume content of ethyl alcohol and water is between 1-99%；Second step, by isopropyl
One of alcohol, normal propyl alcohol substance or two kinds are added among above-mentioned mixed solution liquid, wherein the volume content of every kind of substance
Between 0.01%-25%, but its total volume content is between 0.1%-30%；Third step, by lauryl sodium sulfate, hexadecane
One of base sodium sulfonate, neopelex or it is a variety of be added in above-mentioned solution, wherein the quality of every kind of substance contains
Amount is between 0.01%-15%, and gross mass content is between 0.01%-20%；4th step, will be in sodium sulphate, ammonium sulfate, potassium sulfate
One kind be added among above-mentioned solution, concentration is in 1 mg L-1-50 g L-1Between.
In electrochemical stripping two-dimension nano materials, the electrode of stratified material such as graphite or molybdenum disulfide will be mainly contained
It is inserted among the electrolyte, keeps the electrolyte constant temperature in 0-95oBetween C, with the electrode be anode, with graphite, platinum or
Other metal materials are cathode, can be by just extremely efficient, the clean stripping of stratified material composition under the action of electrochemical reaction
From at two-dimensional nano piece.
Excellent results of the invention are:
The present invention based on ethyl alcohol, the shortcomings that avoiding solvent big using toxicity, is reduced costs, avoiding makes simultaneously with water
With strong acid and strong corrosive chemical reagent；The electrode formed based on stratified material is inserted into this electrolyte, as
Anode, using graphite, platinum or other metals as cathode, under the action of electrochemical reaction, can efficiently by anode remove at
Two-dimensional nano piece, while the Second Aggregation of removed two-dimensional nano thin slice is avoided, meanwhile, which is readily cleaned, by 1-3 times
Washing can be prepared by clean two-dimensional nano thin slice, avoid the shortcomings that organic solvent is difficult to clean.
1. the present invention under the action of electrochemical reaction, can effectively be accelerated based on the mixed solution of water and ethyl alcohol
The charge stripping efficiency of layered electrode improves the yield of two-dimension nano materials.
2. the present invention avoids the solvent big using toxicity based on the mixed solution of water and ethyl alcohol.
3. under the action of electrochemical reaction, the present invention can efficiently, the two-dimensional nano thin slice that separates of cleaning.
4. chemical stability of the present invention is good, and at low cost, it is easy to carry out industrial application.
Specific embodiment
Embodiment 1
80 ml deionized waters, 10ml isopropanol are added in the ethanol solution of 500ml first；Simultaneously by 5 grams of dodecyl sulphur
Sour sodium, 10 grams of sodium sulphate are added among above-mentioned solution, up to electrolyte after stirring evenly, with natural graphite powder dry-pressing burning
Plate shaped graphite electrode made of knot is anode, using platinized platinum as cathode, by electrolyte constant temperature about 60oC, distance is about between positive and negative anodes
1 cm, positive and negative pole tension are maintained at 10.0 V, and a large amount of bubble can be generated in the electrochemical reaction occurred on anode, by stone
The release effect of electrode ink, available thickness about 1-10 nm and the complete graphene of crystal structure.
Embodiment 2
100 ml deionized waters, 20ml normal propyl alcohol are added in the ethanol solution of 400ml first；Simultaneously by 10 grams of dodecyls
Sodium sulphate, 10 grams of ammonium sulfate are added among above-mentioned solution, are 1:1's with mass ratio up to electrolyte after stirring evenly
Molybdenum sulfide and natural graphite
Cylindrical electrode made of the molded then sintering of dried bean noodles is anode, using nickel sheet as cathode, by electrolyte constant temperature about
50oC, distance is about 1 cm between positive and negative anodes, and positive and negative pole tension is maintained at 8.0 V, is generated by the electrochemical reaction on anode
Gas is to the release effect of graphite and molybdenum disulfide combination electrode, available thickness about 1-20 nm and the complete stone of crystal structure
The composite material of black alkene nanometer sheet and molybdenum disulfide nano sheet.
Embodiment 3
10 ml deionized waters, 20 ml normal propyl alcohols are added in the ethanol solution of 500ml first；Simultaneously by 10 grams of dodecyls
Sodium sulphate, 0.1 gram of ammonium sulfate are added among above-mentioned solution, up to electrolyte after stirring evenly, with " tubbiness " metal platinum
Net is inertia anode, and wherein platinum guaze is 100 mesh, and outside and bottom coat the polypropylene screen cloth of one layer of 10000 mesh, will be about 10 gram five
V 2 O powder is added in above-mentioned " tubbiness " inert electrode, using graphite rod as cathode, by electrolyte constant temperature about 85oC, just
Distance is about 0.5 cm between cathode, and positive and negative pole tension is maintained at 12.0 V, the gas generated by the electrochemical reaction on anode
To the release effect of vanadic anhydride powder, the vanadic anhydride nanometer sheet of available thickness about 1-20 nm.
Embodiment 4
190 ml deionized waters, 10 ml normal propyl alcohols are added in the ethanol solution of 200ml first；Simultaneously by 10 grams of dodecanes
Base benzene sulfonic acid sodium salt, 10 grams of sodium sulphate are added among above-mentioned solution, up to electrolyte after stirring evenly, with " tubbiness " metal
Platinum guaze is inertia anode, and wherein platinum guaze is 100 mesh, and outside and bottom coat the polypropylene screen cloth of one layer of 12000 mesh, will be about 20 grams
Black phosphorus powder is added in above-mentioned " tubbiness " inert electrode, using nickel sheet as cathode, by electrolyte constant temperature about 35oC, positive and negative interpolar
Distance is about 1 cm, and positive and negative pole tension is maintained at 6.0 V, and the gas generated by the electrochemical reaction on anode is to black phosphorus powder
Release effect, black phosphorus nanometer sheet of the available thickness between 1-20 nm.
Claims (6)
1. a kind of electrolyte for electrochemical stripping two-dimension nano materials, it is characterised in that: contain deionization in the electrolyte
Water and ethyl alcohol, every kind of volume content is between 1-99%, but its total volume content is between 1%-99%.
2. electrolyte solution according to claim 1, it is characterised in that: the volume content of ethyl alcohol is higher than deionized water
Volume content.
3. electrolyte solution according to claim 1, it is characterised in that: contain normal propyl alcohol, isopropanol object in the electrolyte
One or both of matter, every kind of volume content is between 0.01-25%, but its total volume content is between 0.1%-30%.
4. electrolyte solution according to claim 1, it is characterised in that: contain dodecyl sulphate in the electrolyte
One or more of sodium, sodium cetanesulfonate, neopelex, wherein the mass content of every kind of substance exists
Between 0.01%-15%, but its quality total content is between 0.1%-20%.
5. electrolyte solution according to claim 1, it is characterised in that: contain sodium sulphate, ammonium sulfate, sulphur in the electrolyte
One of sour potassium, concentration is in 1 mg L-1-50 g L-1Between.
6. electrolyte solution according to claim 1, it is characterised in that: the electrolyte can be in 0-95oMake at a temperature of C
With preferably in 20-80oIt is used at a temperature of C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811538990.9A CN109368626A (en) | 2018-12-17 | 2018-12-17 | A kind of electrolyte for electrochemical stripping two-dimension nano materials |
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| CN201811538990.9A CN109368626A (en) | 2018-12-17 | 2018-12-17 | A kind of electrolyte for electrochemical stripping two-dimension nano materials |
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| CN109368626A true CN109368626A (en) | 2019-02-22 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109950465A (en) * | 2019-03-21 | 2019-06-28 | 合肥华思***有限公司 | A kind of method of electrochemical stripping stratified material |
| CN111591991A (en) * | 2020-04-26 | 2020-08-28 | 深圳瀚光科技有限公司 | Device for electrochemically preparing MXene |
| CN112047330A (en) * | 2020-09-23 | 2020-12-08 | 广西师范大学 | Synchronous stripping and collecting method for producing graphene by electrochemical method |
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| CN103058174A (en) * | 2011-10-19 | 2013-04-24 | 杨晓林 | Preparation method of graphene |
| CN103466603A (en) * | 2013-08-09 | 2013-12-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of graphene dispersion liquid, and preparation method of graphene film |
| CN104264179A (en) * | 2014-09-17 | 2015-01-07 | 中国科学院山西煤炭化学研究所 | Method for preparing graphene from raw graphite ores through electrolysis |
| CN105948025A (en) * | 2016-05-05 | 2016-09-21 | 德阳烯碳科技有限公司 | Method for electrochemically preparing graphene |
| CN106149041A (en) * | 2015-04-21 | 2016-11-23 | 上海上木科技有限公司 | A kind of method of electrochemical stripping porous anodic alumina films |
| CN106245104A (en) * | 2016-07-20 | 2016-12-21 | 西安交通大学 | A kind of method preparing Graphene based on electrochemical process stripping dual graphite electrodes |
| WO2017050689A1 (en) * | 2015-09-22 | 2017-03-30 | Technische Universität Dresden | Method for producing a layered (semi-)conductive material |
| WO2018217042A1 (en) * | 2017-05-25 | 2018-11-29 | 한국과학기술원 | Method for producing high-quality graphene flake through electrochemical exfoliation and solution for dispersing graphene flake |
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Patent Citations (8)
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| CN103058174A (en) * | 2011-10-19 | 2013-04-24 | 杨晓林 | Preparation method of graphene |
| CN103466603A (en) * | 2013-08-09 | 2013-12-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of graphene dispersion liquid, and preparation method of graphene film |
| CN104264179A (en) * | 2014-09-17 | 2015-01-07 | 中国科学院山西煤炭化学研究所 | Method for preparing graphene from raw graphite ores through electrolysis |
| CN106149041A (en) * | 2015-04-21 | 2016-11-23 | 上海上木科技有限公司 | A kind of method of electrochemical stripping porous anodic alumina films |
| WO2017050689A1 (en) * | 2015-09-22 | 2017-03-30 | Technische Universität Dresden | Method for producing a layered (semi-)conductive material |
| CN105948025A (en) * | 2016-05-05 | 2016-09-21 | 德阳烯碳科技有限公司 | Method for electrochemically preparing graphene |
| CN106245104A (en) * | 2016-07-20 | 2016-12-21 | 西安交通大学 | A kind of method preparing Graphene based on electrochemical process stripping dual graphite electrodes |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109950465A (en) * | 2019-03-21 | 2019-06-28 | 合肥华思***有限公司 | A kind of method of electrochemical stripping stratified material |
| CN111591991A (en) * | 2020-04-26 | 2020-08-28 | 深圳瀚光科技有限公司 | Device for electrochemically preparing MXene |
| CN112047330A (en) * | 2020-09-23 | 2020-12-08 | 广西师范大学 | Synchronous stripping and collecting method for producing graphene by electrochemical method |
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