CN110194448A - A kind of two-dimensional material of graphene coated or the manufacturing method of graphene - Google Patents
A kind of two-dimensional material of graphene coated or the manufacturing method of graphene Download PDFInfo
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- CN110194448A CN110194448A CN201910145173.5A CN201910145173A CN110194448A CN 110194448 A CN110194448 A CN 110194448A CN 201910145173 A CN201910145173 A CN 201910145173A CN 110194448 A CN110194448 A CN 110194448A
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
- C01B21/0648—After-treatment, e.g. grinding, purification
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- 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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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/22—Intercalation
- C01B32/225—Expansion; Exfoliation
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- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/02—Single layer graphene
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/30—Purity
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
Abstract
The invention discloses a kind of two-dimensional material of graphene coated or the manufacturing methods of graphene.Specific steps are as follows: dried after successively impregnating two-dimensional material in the weak acid solution of heat and the solution of solid-phase carbon source, dried after then being impregnated in the solution of interleaving agent again, obtain predecessor；Predecessor is put into CVD furnace and is reacted, so that solid-phase carbon source is by thermal cracking, then is purified, obtains the two-dimensional material of graphene coated；After carrying out above-mentioned steps, optionally, the two-dimensional material that the biggish surface of area is coated with graphene is subjected to surrounding trimming, removing is etched after exposing the section of material, pure two-dimensional material is made.Compared with prior art, the application beneficial effect is: the obtained material coated with two-dimensional material, at low cost, and the single layer rate of two-dimensional material is high and pollution-free.
Description
Technical field
This application involves the manufacturing field of two-dimensional material more particularly to a kind of materials coated with two-dimensional material and two-dimentional material
The manufacturing method of material.
Background technique
With the reach of science, the manufacture minute yardstick record of material is constantly refreshed, and occurs monatomic or single point recently
Sub- bistable material, represents the two-dimensional material of object such as single layer, currently manufactured or based on chemical gaseous phase deposition CVD method, low cost
Production technology be solid-phase carbon source method, it is typical as " a kind of based on template-solid-phase carbon source thermal cracking preparation two-dimensional material side
The patent of method " (application number 201810127051.9), since solid-phase carbon source is the polymer of melting, the thickness of coating is thicker, produces
The single layer rate of product is lower.In recent years since, on base powder surface, cladding two-dimensional material is directly used in plastics as conduction
The technique of reinforcing agent also occurs, and such as the patent that patent publication No. is CN107858663A, is added in CVD furnace and is deposited on surface
The p type single crystal silicon of catalyst layer carries out after carbon nano tube growth the Cu powder of catalytic growth two-dimensional material cladding again, achieves
Certain effect, but its technique is more complex, it is with high costs.
Summary of the invention
The purpose of the application is to coat very thin coating as solid-phase carbon source growth two using material surface for above-mentioned problem
Material is tieed up, provides the manufacturing method of a kind of material coated with two-dimensional material and two-dimensional material in conjunction with CVD vapor deposition apparatus.
Gas phase deposition technology is to utilize the physics occurred in gas phase, chemical process, forms functional or dress in workpiece surface
Metal, the nonmetallic or compound coat of decorations property.Gas phase deposition technology can be divided into chemical vapor deposition, object according to membrane formation mechanism
Physical vapor deposition and plasma gas phase deposition.The basic definition of chemical vapor deposition-CVD is in semi-conductor industry using the most
The extensive technology for being used to depositing multiple materials, including large-scale insulating materials, most metals material and metal alloy material
Material.In theory, it is very simple: two or more gaseous starting materials are imported into a reaction chamber, so
They chemically react between each other afterwards, form a kind of new material, deposit in wafer surface.
There are three types of the materials of small size to need coated graphite alkene by the application, is described below:
The first situation: material is metal material: including Pt, Al, Co, Ir, Ru, Ni, Cu, Au, Ag, Fe, Mo, W, Ni,
One of Zr, V, Nb, Ta or Cr or alloy.
Second situation: material is porous semiconductor or insulating materials: including glass, ceramics, silicide, clay, oxygen
One of compound, nitride, sulfide, montmorillonite or kaolin are a variety of.
The third situation: material is composite material: composite material is in one layer of metal or alloy of other body surfaces plating
Composite material is made in film, other described main bodys are can be in its surface metallization or all materials of alloy, and described answers
Condensation material is the compound of metal or alloy material, semiconductor or insulating materials one or more.
A kind of two-dimensional material of graphene coated or the manufacturing method of graphene, include the following steps:
(1) preparation of material:
Two-dimensional material is impregnated into 2~80min in 30~98 DEG C of weak acid solution, then is cleaned for several times with deionized water, then
It is dried after mass concentration is immersion in the solution of 0.1~10% solid-phase carbon source, so that the coating dry film thickness of material surface
For 1~500nm, then mass concentration be 0.1~15% interleaving agent solution in impregnate after dry, become predecessor；
(2) growth of carbon material:
Predecessor is put into CVD furnace, then by CVD stove evacuation to 10Pa hereinafter, being passed through again into the CVD furnace lazy
Property gas, inert gas flow velocity be 90~400sccm, to eliminate air, be heated to carbon source cracking generate free carbon temperature
Degree or more, heating rate is 16 DEG C/min, and the pressure in furnace is maintained normal pressure, and the graphene growth time is 5~200min, then
It closes steam supply valve and stops heating, cool to room temperature, rate of temperature fall is 18 DEG C/min；
(3) it clears up:
Several times by the air purging cleaning of the product cleaning of previous step, the two-dimensional material of graphene coated is obtained；
Optionally, after completing step (3), step (4) etching removing is carried out:
The two-dimensional material that the biggish surface of area is coated with graphene is subjected to surrounding trimming, the section for exposing material is laggard
Row etching removing, taking-up graphene is cleaned with deionized water to be dried afterwards several times, obtains graphene.
Further, two-dimensional material described in step (1) is metal, alloy, semiconductor, insulating materials or composite material
One of or it is a variety of, be prepared by CVD method.
Further, the metal or alloy include Pt, Al, Co, Ir, Ru, Ni, Cu, Au, Ag, Fe, Mo, W, Ni, Zr,
V, one of Nb, Ta or Cr or combinations thereof, preferably Cu.
Further, the semiconductor or insulating materials include glass, ceramics, silicide, clay, oxide, nitride,
One of sulfide, montmorillonite or kaolin are a variety of, preferably diatomite.
Further, the composite material is made of one layer of metal or alloy Film laminated of bulk material surface plating
Material, the material of main part are that can be metal or alloy, insulate in its surface metallization or the material of alloy, material of main part
One of body or semiconductor material or combinations thereof, such as metal or alloy, Si, SiO2、Al2O3、HfO2, quartz, mica or glass
Deng；The metal or alloy includes in Pt, Al, Co, Ir, Ru, Ni, Cu, Au, Ag, Fe, Mo, W, Ni, Zr, V, Nb, Ta or Cr
One or more kinds of alloys, preferably Ni.
Further, solid-phase carbon source described in step (1) is solid carbon object, including plastics, rubber, rubber and plastic copolymer
Or one of resin or combination, preferably PP plastics.
Further, the mass concentration of solid-phase carbon source described in (1) in a solvent is 0.1~10%, and dip-coating is in material table
The coating dry film in face is with a thickness of 1~500nm, and preferred coating dry film is with a thickness of 15nm.
Further, interleaving agent described in step (1) is with the substance for preventing graphene reunion function, including boric acid
One of sodium, sodium phosphate, sodium citrate, sodium naphthenate, sodium alkyl sulfonate or sodium alkyl benzene sulfonate are a variety of, preferred to be isolated
Agent is sodium citrate.
Further, the mass concentration of interleaving agent in the solution described in step (1) be 0.1~15%, preferably every
It is 0.5% from the mass concentration of agent in the solution.
Further, it is heated to carbon source cracking in step (2) and generates the temperature of free carbon or more, preferably material
Cu, heating temperature are 980 DEG C.
Further, the graphene growth time described in step (2) is 5~200min, preferred graphene growth time
For 30min.
Further, inert gas described in step (2) is in helium, nitrogen, argon gas, neon, Krypton or xenon
It is one or more, preferably argon gas.
Compared with prior art, the application beneficial effect is: the obtained two-dimensional material with graphene coated, cost
Low, the single layer rate of obtained two-dimensional material is high and pollution-free.
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) figure of 1 product of embodiment.
Fig. 2 is transmission electron microscope (TEM) figure of 1 product of embodiment.
Fig. 3 is Raman spectrum (Raman) result figure of 1 product of embodiment.
Specific embodiment
Following specific embodiments are the further explanations to method provided by the present application and technical solution, but are not construed as
Limitation to the application.
Embodiment 1: a kind of manufacturing method of graphene, steps are as follows:
(1), the preparation of material:
By side length it is that 300 × 600mm opens with a thickness of 50 μm of Cu foil 30 and impregnates 30min in 70 DEG C of weak acid solution, then
It dries after mass content is immersion in the xylene solution of 0.2% PE, then is cleaned for several times with deionized water, obtain material table
The coating dry film in face is dried with a thickness of 4nm, then after mass concentration is immersion in the aqueous solution of 0.1~15% sodium citrate,
As predecessor；
(2), the growth of carbon material:
It will be put into CVD furnace after predecessor fitly laminate stack height, then by CVD stove evacuation to 6Pa, then Xiang Suoshu
Argon gas is passed through in CVD furnace, flow velocity 200sccm is heated to 980 DEG C, and heating rate is 16 DEG C/min, by the pressure in furnace
Power maintains normal pressure, and reaction time 30min turns off steam supply valve and stops heating, cools to room temperature, rate of temperature fall 18
DEG C/min, the upper and lower surface of Cu foil all grows the graphene for having high quality；
(3), it clears up:
Several times by the air purging cleaning of the product cleaning of previous step, the Cu foil material of graphene coated is obtained.
(4) etching removing:
The Cu foil material of two-dimensional material cladding is subjected to surrounding trimming, removing is etched after exposing the section of material, takes
Graphene film is cleaned with deionized water and is dried afterwards several times out, obtains graphene, scanning electron microscope diagram, the projection electricity of product
Sub- microscope figure and Raman spectrogram are shown in Figure of description 1-3 respectively.
Embodiment 2: a kind of manufacturing method of the diatomite with graphene coated, steps are as follows:
(1), the preparation of material:
50 μm of granularity of diatomite 500g is impregnated into 30min in 70 DEG C of weak acid solution, then cleans number with deionized water
It is secondary, then dried after mass content is immersion in the xylene solution of 1.5% PP, obtain the coating dry film thickness of material surface
It is dried for 10nm, then after being impregnated in the aqueous solution for the sodium citrate that mass concentration is 0.6% Boratex, becomes predecessor；
(2), the growth of carbon material:
Predecessor is put into CVD furnace, then by CVD stove evacuation to 3Pa, then into the CVD furnace is passed through helium,
Flow velocity is 200sccm, is heated to 1024 DEG C, and heating rate is 16 DEG C/min, the pressure in furnace is maintained normal pressure, two dimension
The Material growth time is 40min, turns off steam supply valve and stops heating, cools to room temperature, and rate of temperature fall is 18 DEG C/min；
(3), it clears up:
Several times by the air purging cleaning of the product cleaning of previous step, the diatomite material of graphene coated is obtained.
Embodiment 3: a kind of manufacturing method of the aluminum oxide composite ceramic powder with Ni layers of graphene coated plating metal,
Steps are as follows:
(1) preparation of material:
Taking granularity is the aluminum oxide composite ceramic powder that less than or equal to 40 μm surfaces have vacuum evaporation W metal layer
500g impregnates 30min in 70 DEG C of weak acid solution, then is cleaned for several times with deionized water, then the PMMA for being 2% in mass content
Chloroformic solution in impregnate after dry, obtain the coating dry film of material surface with a thickness of 8nm, then in mass concentration be 0.4%
It is dried after being impregnated in the aqueous solution of sodium sulfonate, becomes predecessor；
(2), the growth of carbon material:
Predecessor is put into CVD furnace, then by CVD stove evacuation to 4Pa, then into the CVD furnace is passed through neon,
Flow velocity is 200sccm, is heated to 1020 DEG C, and heating rate is 16 DEG C/min, the pressure in furnace is maintained normal pressure, two dimension
The Material growth time is 35min, turns off steam supply valve and stops heating, cools to room temperature, and rate of temperature fall is 18 DEG C/min；
(3), it clears up:
Several times by the air purging cleaning of the product cleaning of previous step, Ni layers of plating metal of graphene coated are obtained
Aluminum oxide composite ceramic powder material.
Embodiment 4: a kind of surface is coated with the manufacturing method of the Ti of graphene film carefully short silk, and steps are as follows:
(1) preparation of growth substrate:
Take diameter be less than or equal to 200nm, length less than or equal to 3mm Ti carefully short silk 800g in 78 DEG C of room temperature of weak acid
40min is impregnated, then is cleaned for several times with deionized water, then is dried after mass content is immersion in the aqueous emulsion of 0.8% PU
It is dry, obtain the coating dry film of material surface with a thickness of 12nm, then mass concentration be 0.7% sodium benzoate aqueous solution after in
Drying is impregnated, predecessor is become；
(2), the growth of carbon material:
Predecessor is put into CVD furnace, then by CVD stove evacuation to 1Pa, then into the CVD furnace is passed through nitrogen,
Flow velocity is 100sccm, is heated to 1094 DEG C, and heating rate is 16 DEG C/min, the pressure in furnace is maintained normal pressure, two dimension
The Material growth time is 40min, turns off steam supply valve and stops heating, cools to room temperature, and rate of temperature fall is 18 DEG C/min；
(3), it clears up:
Several times by the air purging cleaning of the product cleaning of previous step, it is carefully short to obtain the Ti for being coated with graphene to surface
Wire material.
The method of the present invention that the above embodiments are only used to help understand and its core concept.It should be pointed out that for
For those skilled in the art, without departing from the principle of the present invention, if can also be carried out to the present invention
Dry improvement and modification, these improvement and modification are also fallen into the claims in the present invention protection scope.
Claims (10)
1. a kind of two-dimensional material of graphene coated or the manufacturing method of graphene, which comprises the steps of:
(1) preparation of material:
Two-dimensional material is impregnated into 2~80min in 30~98 DEG C of weak acid solution, then is cleaned for several times with deionized water, then in matter
Dried after being impregnated in the solution for the solid-phase carbon source that amount concentration is 0.1~10% so that the coating dry film of material surface with a thickness of 1~
500nm, then dried after mass concentration is immersion in the solution of 0.1~15% interleaving agent, become predecessor；
(2) growth of carbon material:
Predecessor is put into CVD furnace, then by CVD stove evacuation to 10Pa hereinafter, being passed through indifferent gas into the CVD furnace again
Body, inert gas flow velocity be 90~400sccm, to eliminate air, be heated to carbon source cracking generate free carbon temperature with
On, heating rate is 16 DEG C/min, and the pressure in furnace is maintained normal pressure, and the graphene growth time is 5~200min, is turned off
Steam supply valve and stopping heating, cool to room temperature, and rate of temperature fall is 18 DEG C/min；
(3) it clears up:
Several times by the air purging cleaning of the product cleaning of previous step, the two-dimensional material of graphene coated is obtained；
Optionally, after completing step (3), step (4) etching removing is carried out:
The two-dimensional material that the biggish surface of area is coated with graphene is subjected to surrounding trimming, is lost after exposing the section of material
Removing is carved, taking-up graphene is cleaned with deionized water to be dried afterwards several times, obtains graphene.
2. the manufacturing method according to claim 1, which is characterized in that two-dimensional material described in step (1) is metal, closes
One of gold, semiconductor, insulating materials or composite material are a variety of, are prepared by CVD method.
3. manufacturing method described according to claim 1~any one of 2, which is characterized in that solid phase described in step (1)
Carbon source is one of solid carbon object, including plastics, rubber, rubber and plastic copolymer or resin or combination.
4. manufacturing method described according to claim 1~any one of 2, which is characterized in that step (1) described solid-phase carbon source
Mass concentration in a solvent is 0.1~10%, and the coating dry film of dip-coating on the surface of the material is with a thickness of 20nm.
5. manufacturing method described according to claim 1~any one of 2, which is characterized in that isolation described in step (1)
Agent is with the substance for preventing graphene reunion function, including Boratex, sodium phosphate, sodium citrate, sodium naphthenate, alkyl sulfonic acid
One of sodium or sodium alkyl benzene sulfonate are a variety of.
6. manufacturing method described according to claim 1~any one of 2, which is characterized in that isolation described in step (1)
The mass concentration of agent in the solution is 0.1~15%.
7. manufacturing method according to claim 2, which is characterized in that the metal or alloy include Pt, Al, Co, Ir,
One of Ru, Ni, Cu, Au, Ag, Fe, Mo, W, Ni, Zr, V, Nb, Ta or Cr or combinations thereof.
8. manufacturing method according to claim 2, which is characterized in that the semiconductor or insulating materials include glass, make pottery
One of porcelain, silicide, clay, oxide, nitride, sulfide, montmorillonite or kaolin are a variety of.
9. manufacturing method according to claim 2, which is characterized in that the composite material is to plate in bulk material surface
It covers one layer of metal or alloy film and is made composite material, the material of main part is can be the one of its surface metallization or alloy
Cut material.
10. manufacturing method according to claim 9, which is characterized in that step (1) material of main part is metal or conjunction
Gold, Si, SiO2、Al2O3、HfO2, quartz, one kind or combinations thereof in mica or glass.
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| CN109761232B (en) * | 2019-03-28 | 2020-09-25 | 中国矿业大学(北京) | Device and method for preparing graphite intercalation compound |
| CN111606312B (en) * | 2020-06-11 | 2021-01-05 | 四川大学 | Method and apparatus for stripping hexagonal boron nitride by arc plasma pretreatment |
| CN113770356B (en) * | 2021-09-06 | 2022-04-08 | 广东工业大学 | Processing method and system for preparing metal single element two-dimensional topological material |
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| CN102502604A (en) * | 2011-11-03 | 2012-06-20 | 东南大学 | Preparation method of multifunctional graphene tube |
| CN103213980A (en) * | 2013-05-13 | 2013-07-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of three-dimensional graphene or composite system thereof |
| CN103224231A (en) * | 2013-04-23 | 2013-07-31 | 北京大学 | Transfer method of graphite film |
| CN105129763A (en) * | 2015-09-09 | 2015-12-09 | 上海大学 | Preparation method of three-dimensional graphene/mesoporous carbon sphere composite material |
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| CN104085884B (en) * | 2014-07-11 | 2016-05-18 | 中国科学院等离子体物理研究所 | A kind of with hydrogen (H2) and argon (Ar) hybrid plasma redox graphene (GO) improve the method for chemical property |
| CN107098321B (en) * | 2017-04-12 | 2019-03-19 | 天津大学 | The method that low temperature plasma prepares two-dimensional structure carboritride |
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|---|---|---|---|---|
| CN102502604A (en) * | 2011-11-03 | 2012-06-20 | 东南大学 | Preparation method of multifunctional graphene tube |
| CN103224231A (en) * | 2013-04-23 | 2013-07-31 | 北京大学 | Transfer method of graphite film |
| CN103213980A (en) * | 2013-05-13 | 2013-07-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of three-dimensional graphene or composite system thereof |
| CN105129763A (en) * | 2015-09-09 | 2015-12-09 | 上海大学 | Preparation method of three-dimensional graphene/mesoporous carbon sphere composite material |
| CN106082176A (en) * | 2016-05-25 | 2016-11-09 | 江苏科技大学 | A kind of preparation method of three-dimensional grapheme |
| CN106219521A (en) * | 2016-07-12 | 2016-12-14 | 昆明理工大学 | A kind of preparation method of three-dimensional foam Graphene |
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