CN108285141A - A kind of graphene wet type transfer method of corrugationless non-polymer - Google Patents
A kind of graphene wet type transfer method of corrugationless non-polymer Download PDFInfo
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- CN108285141A CN108285141A CN201810212651.5A CN201810212651A CN108285141A CN 108285141 A CN108285141 A CN 108285141A CN 201810212651 A CN201810212651 A CN 201810212651A CN 108285141 A CN108285141 A CN 108285141A
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- graphene
- heptane
- etchant solution
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Abstract
The invention discloses a kind of graphene wet type transfer methods of corrugationless non-polymer, include the following steps：There is the copper foil of graphene to clean growth and dries up；Configuration concentration etchant solution has anti wrinkling agent in etchant solution；Heptane is added in etchant solution and obtains heptane anti wrinkling agent, heptane anti wrinkling agent is added dropwise on graphene copper foil；Graphene copper foil with heptane layer is swum on the liquid level of etchant solution, copper foil is located at etchant solution on liquid level, and graphene is located on copper foil；Heptane anti wrinkling agent is added on graphene copper foil on etchant solution；It waits for copper foil dissolving to finish, the oxide layer of substrate is flatly placed in above graphene；Substrate is slowly pressed into graphene, until graphene and substrate come into full contact with, graphene is attached to substrate, forms graphene-based bottom；It obtains graphene-based bottom and cleans；It is dry to obtain clean graphene-based bottom.The present invention avoids graphene itself folding from leading to breakage when shifting graphene.
Description
Technical field
The present invention relates to a kind of graphene wet type transfer methods.
Background technology
Graphene, a kind of novel two-dimensional film carbon material, because it surmounts the excellent properties of many materials so that the world
On rapidly started one graphene research overbearing tide.So far, the preparation method of graphene and its mechanics, electricity, change
The research of Xue Deng each side surface properties all achieves extraordinary progress.But graphene is wanted application and is just needed on the other devices
Growth large scale continuous graphite alkene film is obtained using CVD method, but graphene growth made from CVD method is on copper-based bottom
It cannot directly use, so needing corresponding transfer method that graphene is put into target substrate.
Graphene film has excellent mechanical property, if the sufficiently complete of graphene growth, is theoretically not required to
Polymer as such as PMMA is used to go to make protective layer, graphene can also maintain own form to float after copper substrate corrosion
Float on the integrality for keeping certain on liquid level of solution.Using this imagination, the boundary point side of PMMA label graphenes is used first
Just the position of transparent graphene film still can be determined after copper-based bottom etches, and then directly use silicon base from graphene
Directly extract graphene film in the top of film.It has cleaned after etchant solution with regard to completing displaced.This method can actually
Clean graphene film is obtained, but the integrality of graphene is difficult to ensure, it is first that this, which is primarily due to copper foil corrosion process,
A series of hole is formed along copper foil boundary, finally with the expansion in hole, gradually corrosion finishes copper foil, and this corrosion process can be made
At copper foil due to the release of solution surface tension and itself residual stress cause the part not reconnected occur relative motion from
And graphene is torn, and graphene, in order to keep minimum energy state that can carry out bending fold, last shrinkage is together.So real
It is poor to test repeatability, accuracy requirement is high, and environmental suitability is poor, and disturbance is slightly larger will to destroy graphene film, can not be used as general
Suitable common transfer method uses.
Invention content
The purpose of the present invention is to provide a kind of to avoid graphene itself from folding when shifting graphene leads to damaged stone
Black alkene wet type transfer method.
A kind of graphene wet type transfer method of corrugationless non-polymer, includes the following steps：
Step 1：There is the copper foil of graphene to clean growth and dries up；Configuration concentration etchant solution has in etchant solution anti-
Wrinkle agent；
Step 2：Heptane is added in etchant solution and obtains heptane-anti wrinkling agent, it is anti-that heptane-is added dropwise on graphene-copper foil
Graphene surface is completely covered in wrinkle agent, heptane-anti wrinkling agent, and graphene surface forms one layer of crease-resistant oxidant layer of heptane-；
Step 3：Graphene-copper foil with heptane layer is swum on the liquid level of etchant solution, copper foil and etchant solution
On liquid level, graphene is located on copper foil；Heptane-anti wrinkling agent is added on graphene-copper foil on etchant solution；
Step 4：It waits for copper foil dissolving to finish, the oxide layer of substrate is flatly placed in above graphene, substrate and stone are made
Black alkene face contact；
Step 5：Substrate is slowly pressed into graphene, until graphene and substrate come into full contact with, graphene is attached to base
Bottom forms graphene-substrate；
Step 6：It obtains graphene-substrate and cleans, removal etchant solution, remaining metal and heptane；Dry acquisition is clean
Net graphene-substrate.
Further, the etchant solution in step 1 is by a concentration of 1 mole every liter of FeCl3Solution and (the carboxylic first of 1,3- bis-
Base) urea is mixed to form according to the ratio uniform of 100ml ratios 1mg.
Further, in step 2 when heptane being added dropwise in the etchant solution containing anti wrinkling agent, first by heptane and containing crease-resistant
The etchant solution of agent is mixed, and stands a little while, heptane is layered with etchant solution, and heptane is in upper, etchant solution under.Into one
Step, substrate is silica polished silicon wafer, and in step 5, substrate presses to graphene with the speed of 1mm/s, and substrate submerges etchant solution
Afterwards, graphene comes into full contact with substrate.
Further, step 6 includes：
Step 6.1：Silica polished silicon wafer is removed from iron stand, is put into cleaning in deionized water and is remained in silica
Etchant solution in polished silicon wafer 2-3 times；
Step 6.2：Silica polished silicon wafer is put into 20：1：1 H2O：H2O2：The solution of HCl dissolves kish；
Step 6.3：Silica polished silicon wafer is put into solution 2-3 times that deionized water cleaning remains in substrate；
Step 6.4：Silica polished silicon wafer is placed to dry moisture vertically；
Step 6.5：Silica polished silicon wafer is put into cleaning remained on surface heptane in isopropanol, takes out silica polishing
Piece dries up isopropanol.
Description of the drawings
Fig. 1 is transfer result AFM datagrams.
Specific implementation mode
A kind of graphene wet type transfer method of corrugationless non-polymer, includes the following steps：
Step 1：There is the copper foil of graphene to clean growth and dries up；Configuration concentration etchant solution has in etchant solution anti-
Wrinkle agent；Etchant solution is by a concentration of 1 mole every liter of FeCl3Solution and (carboxymethyl) ureas of 1,3- bis- are according to 100ml ratios 1mg's
Ratio uniform is mixed to form；
Step 2：Heptane is added in etchant solution and obtains heptane-anti wrinkling agent, it is anti-that heptane-is added dropwise on graphene-copper foil
Graphene surface is completely covered in wrinkle agent, heptane-anti wrinkling agent, and graphene surface forms one layer of crease-resistant oxidant layer of heptane-；Containing crease-resistant
When heptane being added dropwise in the etchant solution of agent, first heptane and etchant solution containing anti wrinkling agent are mixed, stood a little while, heptan
Alkane is layered with etchant solution, and heptane is in upper, etchant solution under.
Step 3：Graphene-copper foil with heptane layer is swum on the liquid level of etchant solution, copper foil and etchant solution
On liquid level, graphene is located on copper foil；Heptane-anti wrinkling agent is added on graphene-copper foil on etchant solution；
Step 4：It waits for copper foil dissolving to finish, the oxide layer of substrate is flatly placed in above graphene, substrate and stone are made
Black alkene face contact；
Step 5：Substrate is slowly pressed into graphene, until graphene and substrate come into full contact with, graphene is attached to base
Bottom forms graphene-substrate；Substrate is silica polished silicon wafer, and substrate presses to graphene with the speed of 1mm/s, and substrate is submerged
After etchant solution, graphene comes into full contact with substrate；
Step 6：It obtains graphene-substrate and cleans, removal etchant solution, remaining metal and heptane；Dry acquisition is clean
Net graphene-substrate；
Step 6.1：Silica polished silicon wafer is removed from iron stand, is put into cleaning in deionized water and is remained in silica
Etchant solution in polished silicon wafer 2-3 times；
Step 6.2：Silica polished silicon wafer is put into 20：1：1 H2O：H2O2：The solution of HCl dissolves kish；
Step 6.3：Silica polished silicon wafer is put into solution 2-3 times that deionized water cleaning remains in substrate；
Step 6.4：Silica polished silicon wafer is placed to dry moisture vertically；
Step 6.5：Silica polished silicon wafer is put into cleaning remained on surface heptane in isopropanol, takes out silica polishing
Piece dries up isopropanol.
Claims (5)
1. a kind of graphene wet type transfer method of corrugationless non-polymer, includes the following steps：
Step 1：There is the copper foil of graphene to clean growth and dries up；Configuration concentration etchant solution has anti wrinkling agent in etchant solution；
Step 2：Heptane is added in etchant solution and obtains heptane-anti wrinkling agent, heptane-anti wrinkling agent is added dropwise on graphene-copper foil,
Graphene surface is completely covered in heptane-anti wrinkling agent, and graphene surface forms one layer of crease-resistant oxidant layer of heptane-；
Step 3：Graphene-copper foil with heptane layer is swum on the liquid level of etchant solution, copper foil is located at etchant solution
On liquid level, graphene is located on copper foil；Heptane-anti wrinkling agent is added on graphene-copper foil on etchant solution；
Step 4：It waits for copper foil dissolving to finish, the oxide layer of substrate is flatly placed in above graphene, substrate and graphene are made
Face contacts；
Step 5：Substrate is slowly pressed into graphene, until graphene and substrate come into full contact with, graphene is attached to substrate, shape
At graphene-substrate；
Step 6：It obtains graphene-substrate and cleans, removal etchant solution, remaining metal and heptane；Dry acquisition cleaning
Graphene-substrate.
2. a kind of graphene wet type transfer method of corrugationless non-polymer according to claim 1, it is characterised in that：Step
Etchant solution in rapid 1 is by a concentration of 1 mole every liter of FeCl3Solution and (carboxymethyl) ureas of 1,3- bis- are according to 100ml ratios 1mg
Ratio uniform be mixed to form.
3. a kind of graphene wet type transfer method of corrugationless non-polymer according to claim 2, it is characterised in that：Step
In rapid 2 when heptane being added dropwise in the etchant solution containing anti wrinkling agent, first heptane and etchant solution containing anti wrinkling agent are mixed
Stirring is stood a little while, and heptane is layered with etchant solution, and heptane is in upper, etchant solution under.
4. a kind of graphene wet type transfer method of corrugationless non-polymer according to claim 3, it is characterised in that：Base
Bottom is silica polished silicon wafer, and in step 5, substrate presses to graphene with the speed of 1mm/s, after substrate submerges etchant solution, stone
Black alkene comes into full contact with substrate.
5. a kind of graphene wet type transfer method of corrugationless non-polymer according to claim 4, it is characterised in that：Step
Rapid 6 include：
Step 6.1：Silica polished silicon wafer is removed from iron stand, is put into cleaning in deionized water and is remained in silica polishing
The etchant solution of on piece 2-3 times；
Step 6.2：Silica polished silicon wafer is put into 20：1：1 H2O：H2O2：The solution of HCl dissolves kish；
Step 6.3：Silica polished silicon wafer is put into solution 2-3 times that deionized water cleaning remains in substrate；
Step 6.4：Silica polished silicon wafer is placed to dry moisture vertically；
Step 6.5：Silica polished silicon wafer is put into cleaning remained on surface heptane in isopropanol, silica polished silicon wafer is taken out and blows
Dry isopropanol.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109534327A (en) * | 2019-01-28 | 2019-03-29 | 哈尔滨工业大学（威海） | A kind of preparation method of graphene |
| CN110143588A (en) * | 2019-04-18 | 2019-08-20 | 浙江大学 | A method of graphene is shifted based on liquid adhesive bandage protective layer |
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| CN109534327A (en) * | 2019-01-28 | 2019-03-29 | 哈尔滨工业大学（威海） | A kind of preparation method of graphene |
| CN110143588A (en) * | 2019-04-18 | 2019-08-20 | 浙江大学 | A method of graphene is shifted based on liquid adhesive bandage protective layer |
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Application publication date: 20180717 |