CN106882792A - A kind of method of Graphene in dry method transfer metal substrate - Google Patents
A kind of method of Graphene in dry method transfer metal substrate Download PDFInfo
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- CN106882792A CN106882792A CN201510933644.0A CN201510933644A CN106882792A CN 106882792 A CN106882792 A CN 106882792A CN 201510933644 A CN201510933644 A CN 201510933644A CN 106882792 A CN106882792 A CN 106882792A
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- graphene
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Abstract
The method that the present invention provides Graphene in a kind of dry method transfer metal substrate, including：1）The metal substrate that length has Graphene is placed in target substrate, and the Graphene is faced into target substrate；2）The metal substrate and target substrate that the length that will be placed has Graphene are put into reactor; under protective atmosphere; it is warming up to metal substrate fusion temperature or more; the metal substrate fusing is set to be shrunk to prill; the Graphene is attached in target substrate; room temperature is dropped in protective atmosphere after insulation Preset Time, the Graphene is transferred in target substrate.Method of the present invention repeatability is high, simple and easy to apply, and the scale batch for microelectronics and optoelectronic areas high-quality graphene is shifted；Transfer process of the present invention belongs to physical process and is aided in without other liquid or solid state reagents, and transfer process will not introduce other impurities, can be prevented effectively from unintentional doping, reduce influence of the transfer process to Graphene electric property.
Description
Technical field
The invention belongs to graphene film preparing technical field, the side of Graphene in more particularly to a kind of dry method transfer metal substrate
Method.
Background technology
Delivering first from two scientist Andre Geim and the Konstantin Novoselov in Russia's birth in 2004 has
After closing the paper of Graphene, Graphene has evoked huge great waves in scientific circles, and its appearance is expected in hyundai electronicses sciemtifec and technical sphere
Trigger new round revolution.Graphene possesses many superior performances, for example high transmission rate, high electron mobility, high current density,
High mechanical properties, be easy to modification etc..Just because of these characteristics, it be acknowledged as manufacture transparent conductive film, high frequency transistor,
Hydrogen storage battery, so integrated circuit ideal material, with wide market application foreground.
So far, in the preparation method of many Graphenes, CVD on the metallic substrate can obtain high-quality, large area
Graphene, Graphene prepared by the method is most suitable for the application of microelectronics and optoelectronic areas.Due to the electric conductivity of metal substrate,
Graphene in metal substrate is generally required to be transferred in other target substrates and could used.At present, metal substrate is eroded
Wet method transfer is the most common transfer method of CVD Graphenes in metal substrate, and recently, researcher have developed Bubbling method and turns again
Graphene is moved, this method can effectively reduce Graphene cost without corroding metal substrate.However, either traditional wet method
Transfer or Bubbling method transfer, Graphene can be all immersed in the middle of solution, cause the unintentional doping of Graphene.
The dry method transfer that the present invention is referred to, whole process can avoid Graphene from being contacted with other solution or solid matter, it is to avoid non-
Deliberately doping.And, the method is simple to operate, reproducible, is suitable to high-quality graphene needed for microelectronics and optoelectronic applications
Preparation.
The content of the invention
The shortcoming of prior art, Graphene in metal substrate is shifted it is an object of the invention to provide a kind of dry method in view of the above
Method, for solve the problems, such as in the prior art Graphene transfer easily cause unintentional doping.
In order to achieve the above objects and other related objects, the method that the present invention provides Graphene in a kind of dry method transfer metal substrate,
Including step：Step 1), the metal substrate that length has Graphene is placed in target substrate, and the Graphene is faced into target
Substrate, wherein, do not infiltrated with Graphene after the metal substrate fusing；Step 2), the length that will be placed has the gold of Graphene
Category substrate and target substrate are put into reactor, under protective atmosphere, are warming up to metal substrate fusion temperature or more, are made described
Metal substrate fusing is shrunk to prill, and the Graphene is attached in target substrate, in protective atmosphere after insulation Preset Time
Room temperature is dropped to, the Graphene is transferred in target substrate.
Used as a kind of preferred scheme of the method for Graphene in dry method of the invention transfer metal substrate, described Graphene includes stone
Black alkene separates one or two combination of domain and Graphene continuous film.
As a kind of preferred scheme of the method for Graphene in dry method of the invention transfer metal substrate, the material of the metal substrate
One or more alloy including copper, nickel, cobalt and ruthenium.
As a kind of preferred scheme of the method for Graphene in dry method of the invention transfer metal substrate, the fusing point of the target substrate
Higher than the fusing point of corresponding metal substrate, including surface have in silicon substrate, silicon substrate and the Sapphire Substrate of silica one
Kind.
As a kind of preferred scheme of the method for Graphene in dry method of the invention transfer metal substrate, step 1) in, if described
The metal substrate back side also has Graphene, then be first removed the Graphene oxygen plasma lithographic method at the back side.
As a kind of preferred scheme of the method for Graphene in dry method of the invention transfer metal substrate, the placement of the target substrate
Direction can be level to vertical arbitrarily angled.
Used as a kind of preferred scheme of the method for Graphene in dry method of the invention transfer metal substrate, the protective atmosphere is to avoid
The mixing of a kind of gas or two or more gases that Graphene is etched in hot environment.
As dry method of the invention transfer metal substrate on Graphene method a kind of preferred scheme, step 2) in liter it is gentle
Cooling rate is 0.01~1000 degrees celsius/minute.
As a kind of preferred scheme of the method for Graphene in dry method of the invention transfer metal substrate, step 2) in, by target
Substrate tilting certain angle is placed, so that the region beyond the prill after fusing is rolled into Graphene in the presence of self gravitation.
As dry method of the invention transfer metal substrate on Graphene method a kind of preferred scheme, step 2) in, by with
Mechanical external force or the method for chemical attack remove the prill.
As described above, the method that dry method of the invention shifts Graphene in metal substrate, has the advantages that：
1) method of the present invention repeatability is high, simple and easy to apply, for microelectronics and the scale of optoelectronic areas high-quality graphene
Batch is shifted；
2) transfer process of the present invention belongs to physical process and is aided in without other liquid or solid state reagents, and transfer process will not be introduced
Other impurities, can be prevented effectively from unintentional doping, reduce influence of the transfer process to Graphene electric property.
Brief description of the drawings
The step of Fig. 1 is shown as the method for Graphene in dry method transfer metal substrate of the invention schematic flow sheet.
The structure that each step that Fig. 2~Fig. 6 is shown as the method for Graphene in dry method transfer metal substrate of the invention is presented is shown
It is intended to.
Fig. 7 is shown with conventional wet transfer and Graphene in copper substrate is transferred into SiO2The light microscopic figure of Graphene on/Si substrates
Piece.
Fig. 8 is shown with dry method transfer of the present invention and Graphene in copper substrate is transferred into SiO2The light microscopic of Graphene on/Si substrates
Picture.
Fig. 9 is shown with the light microscopic that Graphene in copper substrate is transferred to Graphene in Sapphire Substrate for dry method transfer of the present invention
Picture.
Component label instructions
101 metal substrates
102 Graphenes
103 target substrates
104 prills
S11~S12 steps 1)~step 2)
Specific embodiment
Embodiments of the present invention are illustrated below by way of specific instantiation, those skilled in the art can be as disclosed by this specification
Content understand other advantages of the invention and effect easily.The present invention can also add by way of a different and different embodiment
To implement or apply, the various details in this specification can also be based on different viewpoints and application, without departing from essence of the invention
Various modifications or alterations are carried out under god.
Refer to Fig. 1~Fig. 9.It should be noted that the diagram provided in the present embodiment only illustrates of the invention in a schematic way
Basic conception, component count, shape when only display is with relevant component in the present invention rather than according to actual implementation in illustrating then and
Size is drawn, and it is actual when the implementing kenel of each component, quantity and ratio can be a kind of random change, and its assembly layout type
State is likely to increasingly complex.
Embodiment 1
As shown in Fig. 1~Fig. 8, the method that the present embodiment provides Graphene in a kind of dry method transfer metal substrate, including step：
As shown in Figure 1 to 4, step 1 is carried out first) S11, the metal substrate 101 that length has Graphene 102 is placed in target lining
On bottom 103, and the Graphene 102 is faced into target substrate 103, wherein, with graphite after the fusing of the metal substrate 101
Alkene 102 does not infiltrate.
As an example, described Graphene 102 includes that Graphene separates one or two combination of domain and Graphene continuous film.
In the present embodiment, the Graphene 102 is Graphene continuous film.
As an example, the material of the metal substrate 101 includes one or more alloy of copper, nickel, cobalt and ruthenium.
In the present embodiment, the material of the metal substrate 101 is copper.
As an example, fusing point of the fusing point of the target substrate 103 higher than corresponding metal substrate 101, including surface has two
One kind in the silicon substrate of silica, silicon substrate and Sapphire Substrate.In the present embodiment, the target substrate 103 is surface
Silicon substrate with silica.
If as an example, the back side of the metal substrate 101 also has Graphene 102, the Graphene 102 at the back side first is used into oxygen
Plasma etching method is removed.
As shown in Fig. 1 and Fig. 5~Fig. 6, step 2 is then carried out) S12, the length that will be placed has the metal substrate of Graphene 102
101 and target substrate 103 be put into reactor, under protective atmosphere, be warming up to melt temperature of metal substrate 101 or more,
Melt the metal substrate 101 and be shrunk to prill 104, the Graphene 102 is attached in target substrate 103, protect
Room temperature is dropped in protective atmosphere after warm Preset Time, the Graphene 102 is transferred in target substrate 103.
As an example, the placement direction of the target substrate 103 can be level to vertical arbitrarily angled.
As an example, the protective atmosphere is a kind of gas or two kinds for avoiding Graphene 102 from being etched in hot environment
The mixing of above gas.
As an example, step 2) in the gentle cooling rate of liter be 0.01~1000 degrees celsius/minute.
As an example, removing the prill 104 by with the method for mechanical external force or chemical attack.
Certainly, in other implementation processes, it is also possible to target substrate 103 is inclined into certain angle and is placed, so that after fusing
Prill 104 is rolled into the region beyond Graphene 102 in the presence of self gravitation.Removal gold can be saved in this way
Belong to the additional technique of bead 104, substantially reduce cost.
Below with Graphene on dry method transfer copper to SiO2Enter one as a example by/Si substrates (i.e. surface has the silicon substrate of silicon dioxide layer)
Step explanation specific implementation process of the invention：
Step 1), the copper substrate that length has Graphene is placed on SiO2/ Si substrates (SiO2Thickness is 300 nanometers) on, length has stone
The adjacent target substrate of one side of black alkene.
Step 2), the metal substrate and target substrate that will be put well are put into common CVD growth system together, are evacuated down to 1Pa,
Then pass to argon gas to normal pressure.
Step 3), it is warming up to 1200 under 1000sccm argon gas, 20sccm hydrogen, the protection of 0.1sccm methane blendeds gas
Degree Celsius, and maintain 30 minutes at this temperature, programming rate selection is 5 degrees celsius/minutes.
Step 4), fast cooling is to room under 1000sccm argon gas, 20sccm hydrogen, the protection of 0.1sccm methane blendeds gas
Temperature, the speed selection of cooling is 10 degrees celsius/minutes.
Step 5), obtain being transferred to SiO2Graphene on/Si substrates.The SiO that the present embodiment is obtained2Graphite on/Si substrates
The light microscopic figure of alkene is as shown in Figure 8, it can be seen that.Compared to the result that Fig. 7 conventional wets are shifted, result of the invention does not have glue residual
Stay, surface is cleaner.
Embodiment 2
As shown in Fig. 1~Fig. 6 and Fig. 9, the present embodiment provides a kind of method of Graphene in dry method transfer metal substrate, its base
This step such as embodiment 1, wherein, in the present embodiment, by taking Graphene on dry method transfer copper to Sapphire Substrate as an example further
Illustrate.Specifically, comprise the following steps：
Step 1), the copper substrate that length has Graphene to be put on a sapphire substrate, length has the adjacent target substrate of one side of Graphene.
Step 2), the metal substrate and target substrate that will be put well are put into common CVD growth system together, are evacuated down to 1Pa,
Then pass to argon gas to normal pressure.
Step 3), it is warming up to 1200 and takes the photograph under 1000sccm argon gas, 20sccm hydrogen, the protection of 0.1sccm methane blendeds gas
Family name's degree, maintains 30 minutes, and programming rate selection is 5 degrees celsius/minutes.
Step 4), fast cooling is to room under 1000sccm argon gas, 20sccm hydrogen, the protection of 0.1sccm methane blendeds gas
Temperature, the speed selection of cooling is 10 degrees celsius/minutes.
Step 5), obtain being transferred to the Graphene in Sapphire Substrate.The Graphene in Sapphire Substrate that the present embodiment is obtained
As shown in figure 9, lower left is Graphene, upper right side is sapphire substrate surface to light microscopic figure, and it is Graphene and substrate that arrow is signified
Border, it can be seen that result of the invention does not have glue residua, and surface is cleaner.
As described above, the method that dry method of the invention shifts Graphene in metal substrate, has the advantages that：
1) method of the present invention repeatability is high, simple and easy to apply, for microelectronics and the scale of optoelectronic areas high-quality graphene
Batch is shifted；
2) transfer process of the present invention belongs to physical process and is aided in without other liquid or solid state reagents, and transfer process will not be introduced
Other impurities, can be prevented effectively from unintentional doping, reduce influence of the transfer process to Graphene electric property.
So, the present invention effectively overcomes various shortcoming of the prior art and has high industrial utilization.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any to be familiar with this skill
The personage of art all can carry out modifications and changes under without prejudice to spirit and scope of the invention to above-described embodiment.Therefore, such as
Those of ordinary skill in the art completed under without departing from disclosed spirit and technological thought all etc.
Effect modifications and changes, should be covered by claim of the invention.
Claims (10)
1. a kind of method that dry method shifts Graphene in metal substrate, it is characterised in that including step：
Step 1), the metal substrate that length has Graphene is placed in target substrate, and the Graphene is faced into target substrate,
Wherein, do not infiltrated with Graphene after the metal substrate fusing；
Step 2), the metal substrate and target substrate that the length that will be placed has Graphene are put into reactor, in protective atmosphere
Under, metal substrate fusion temperature or more is warming up to, the metal substrate fusing is shrunk to prill, the Graphene
It is attached in target substrate, room temperature is dropped in protective atmosphere after insulation Preset Time, the Graphene is transferred to target
On substrate.
2. the method that dry method according to claim 1 shifts Graphene in metal substrate, it is characterised in that：Described Graphene bag
Include one or two the combination that Graphene separates domain and Graphene continuous film.
3. the method that dry method according to claim 1 shifts Graphene in metal substrate, it is characterised in that：The metal substrate
Material includes one or more alloy of copper, nickel, cobalt and ruthenium.
4. the method that dry method according to claim 1 shifts Graphene in metal substrate, it is characterised in that：The target substrate
Higher than the fusing point of corresponding metal substrate, including surface has silicon substrate, silicon substrate and the Sapphire Substrate of silica to fusing point
In one kind.
5. the method that dry method according to claim 1 shifts Graphene in metal substrate, it is characterised in that：Step 1) in, if
The metal substrate back side also has Graphene, then be first removed the Graphene oxygen plasma lithographic method at the back side.
6. the method that dry method according to claim 1 shifts Graphene in metal substrate, it is characterised in that：The target substrate
Placement direction can be level to vertical arbitrarily angled.
7. the method that dry method according to claim 1 shifts Graphene in metal substrate, it is characterised in that：The protective atmosphere is
Avoid the mixing of a kind of gas or two or more gases that Graphene is etched in hot environment.
8. the method that dry method according to claim 1 shifts Graphene in metal substrate, it is characterised in that：Step 2) in liter
Gentle cooling rate is 0.01~1000 degrees celsius/minute.
9. the method that dry method according to claim 1 shifts Graphene in metal substrate, it is characterised in that：Step 2) in, will
Target substrate inclines certain angle and places, so that beyond the prill after fusing is rolled into Graphene in the presence of self gravitation
Region.
10. the method that dry method according to claim 1 shifts Graphene in metal substrate, it is characterised in that：Step 2) in,
The prill is removed by with the method for mechanical external force or chemical attack.
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Cited By (4)
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| CN108516541A (en) * | 2018-04-02 | 2018-09-11 | 西安工程大学 | A kind of novel C VD graphenes dry method transfer method |
| CN109142408A (en) * | 2018-08-06 | 2019-01-04 | 华东师范大学 | A kind of method of the TEM sample of dry process two-dimensional material |
| CN110184585A (en) * | 2019-06-25 | 2019-08-30 | 福建闽烯科技有限公司 | A kind of preparation method and device of graphene copper powder |
| CN111845003A (en) * | 2020-06-18 | 2020-10-30 | 华中科技大学 | Controllable hot-pressing implementation method of nano material |
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| CN111845003A (en) * | 2020-06-18 | 2020-10-30 | 华中科技大学 | Controllable hot-pressing implementation method of nano material |
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