CN111847437B - Device and method for transferring graphene to net-carrying copper substrate in batch - Google Patents
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- CN111847437B CN111847437B CN202010727856.4A CN202010727856A CN111847437B CN 111847437 B CN111847437 B CN 111847437B CN 202010727856 A CN202010727856 A CN 202010727856A CN 111847437 B CN111847437 B CN 111847437B
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Abstract
The invention relates to the technical field of graphene, in particular to a device for transferring graphene to a net-carrying copper substrate in batches, which comprises a load disk and a load disk base, wherein the load disk is made of polytetrafluoroethylene; the load disc is provided with load holes of a load net copper substrate which are arranged in a matrix (linear matrix or circumferential matrix) or in a random arrangement, and the lower parts of the load holes are provided with lead-out holes which are coaxial with the load holes, have a diameter smaller than that of the load holes and penetrate through the load disc; the load disc base is provided with support columns which are equal to and coaxial with the guide-out holes and are matched with the guide-out holes. A method for transferring graphene to a net-carrying copper substrate in batches comprises the following steps of spin-coating a PMMA solution on the surface of a copper foil with the graphene, curing, pre-etching, rinsing and removing a film; by applying the device and the method, the graphene can be transferred to the mesh-loaded copper substrate in batches, the operation is simple and convenient, and the transfer process and the device can be modified and designed according to actual requirements.
Description
Technical Field
The invention relates to the technical field of graphene, in particular to a device and a method for transferring graphene to a grid-loaded copper substrate in batches.
Background
From carbon atoms with SP2The graphene two-dimensional material hybridized to form the regular hexagon is a semiconductor material with a zero band gap structure, and has high conductivity (theoretical electron transfer rate-200000 cm)2/v.s), high thermal conductivity (theoretical thermal conductivity-5000W/m.K), low light absorbance (-2.3%), and high specific surface area (-2630 m)2Per g) and the like, and has great application prospect and commercial value in the fields of integrated circuits, functional materials, display devices, sensors and the like.
At present, the preparation method of graphene comprises the following steps: physical stripping method, epitaxial growth method, graphene oxide reduction method, metal catalytic epitaxial growth method, chemical vapor deposition method and other preparation methods; the chemical vapor deposition method is considered as the most promising method for preparing single-layer graphene, the principle is that under the high-temperature atmosphere, hydrocarbons (methane and ethylene) are subjected to a thermal catalytic reaction on the surface of transition metal (Cu and Ni) to generate single-layer or few-layer graphene, and the current process for preparing graphene on a copper foil is mature; the graphene prepared on the copper foil can remove the metal copper substrate through the solution etching process, so that the separation of the metal growth substrate and the graphene is realized, and the subsequent transfer, processing and application of the graphene on different substrates are facilitated.
The graphene transfer technique is a physical transfer technique for transferring graphene from a growth substrate to a target load substrate; whether the batch or huge graphene transfer technology is mature or not determines whether the subsequent large-scale application of graphene in various fields is successful or not, so that the batch graphene transfer technology is of great importance; at present, the technical field of graphene transfer is still lack of a mature method for transferring graphene in batches.
Disclosure of Invention
The present invention addresses the above market needs by providing an apparatus and method for batch transfer of graphene to a mesh-loaded copper substrate.
The technical scheme of the invention is as follows:
a device for transferring graphene to a net-carrying copper substrate in batches comprises a load tray and a load tray base; the load disc is provided with load holes of a load net copper substrate which are arranged in a matrix (linear matrix or circumferential matrix) or in a random arrangement, and the lower parts of the load holes are provided with lead-out holes which are coaxial with the load holes, have a diameter smaller than that of the load holes and penetrate through the load disc; the load disc base is provided with support columns which are equal to and coaxial with the guide-out holes and are matched with the guide-out holes.
Preferably, when the load disk is attached to the load disk base, the supporting column passes through the leading-out hole and the load hole, and the top surface of the supporting column is 0.2-0.5mm higher than the load surface of the load disk and is used for pushing out the mesh-loaded copper substrate in the load hole.
Preferably, the load holes are circular, the diameter of the load holes is (D +0.1) - (3/2D), wherein D is the diameter of the mesh-carrying copper substrate, and when the diameter D =3mm, the diameter of the load holes is 3.1-4.5 mm.
Preferably, the depth of the loading hole is 0.5-5 mm.
Preferably, the leading-out hole is circular, the diameter of the leading-out hole is (D-0.2) - (1/2D), wherein D is the diameter of the mesh-carrying copper substrate, and when the diameter of the mesh-carrying copper substrate is D =3mm, the diameter of the leading-out hole is 2.8-1.5 mm.
Preferably, a plurality of support holes are formed in the load disc and penetrate through the load disc, the diameter of each support hole is not smaller than 3mm, and the distance between each support hole and the edge of the load disc is not smaller than 2 mm.
Preferably, two supporting legs are symmetrically arranged on two sides of the load disk, the supporting legs are located on the back face of the load disk and are semicircular, and the bottom area of each supporting leg is not less than 0.5 cm.
Preferably, the load disk base is provided with a detent which is matched with the load disk support foot.
Preferably, the load tray and the load tray base are both made of acid and alkali resistant material (polytetrafluoroethylene or quartz glass).
A method for transferring graphene to a net-carrying copper substrate in batch comprises the following steps:
s1, spin-coating a PMMA solution with the concentration of 1% -10% on the surface of a copper foil with graphene by a CVD method, wherein the spin-coating comprises two stages of low-speed spin-coating and high-speed spin-coating, the low-speed spin-coating speed is 500-5000 r/s;
s2, placing the copper foil coated with PMMA in a heating platform for curing, wherein the curing temperature is 50-180 ℃, and the curing time is 3-10 min;
s3, obtaining a PMMA/graphene/Cu sample through heating and curing, pre-etching by using an etching solution (one of ammonium persulfate, ferric trichloride and other etching solutions) with the concentration of 0.1-1.5M, pre-etching for 2-4 periods with 2-6min as an etching period, and slowly washing the pre-etching surface by using deionized water after each period is finished to remove a graphene layer on the etching surface;
s4, etching the PMMA/graphene/Cu sample after the pre-etching is finished by using an etching solution (ammonium persulfate or ferric trichloride) with the concentration of 0.1-1.5M, and removing the copper foil to obtain a PMMA/graphene film;
s5, rinsing the graphene/PMMA film obtained in the step S4 by using deionized water containing 2% -15% of surfactants such as isopropanol or ethanol; after rinsing, the graphene/PMMA film is loaded on the surface of a loading disc with a net-loading copper substrate by controlling the water level to drop or using an auxiliary device (a loading disc bracket and tweezers); the surfactants such as isopropanol, ethanol and the like are used for reducing the surface tension of deionized water, so that the subsequent transfer work is facilitated;
s6, pushing out the net-carrying copper substrate placed in the load hole through the support column of the load disk base to enable the net-carrying copper substrate to be closely attached to the graphene/PMMA film; naturally airing or drying the PMMA/graphene/net-carrying copper substrate sample by a heating platform at the temperature of 80-150 ℃;
s7, reversely buckling the PMMA/graphene/mesh-loaded copper substrate sample obtained in the step 6 in a mesh-loaded copper substrate loading hole of a loading disc, and removing the PMMA film on the PMMA/graphene/mesh-loaded copper substrate sample within 0.5-3h by using acetone steam obtained at 70-150 ℃; after the PMMA film is removed by acetone vapor, residual acetone on the surface of the sample is removed within 0.5-3h by using isopropanol vapor obtained at 70-150 ℃, and the remaining graphene is attached to the mesh-carrying copper substrate.
Compared with the existing graphene transfer technology, the method has the following beneficial effects:
1. the method and the device for transferring the graphene to the net-carrying copper substrate in batch can realize batch transfer of the graphene on the net-carrying copper substrate;
2. the method and the device for transferring the graphene to the grid-loaded copper substrate in batches can realize batch transfer of the graphene on different substrates;
3. the method and the device for transferring the graphene to the grid-loaded copper substrate in batches have the advantages of simple process principle and simplicity and convenience in operation, and the transfer process and the device can be modified and designed according to actual requirements.
Drawings
Fig. 1 is a three-dimensional view of a load tray and load tray base assembly of a device for batch transfer of graphene to a mesh copper substrate.
Fig. 2 is a schematic structural diagram of a front side of a load tray of a device for transferring graphene to a mesh copper substrate in batch.
Fig. 3 is a schematic view of a back structure of a load tray of a device for transferring graphene to a mesh copper substrate in batch.
Fig. 4 is a schematic view of a load tray base structure of a device for transferring graphene to a mesh copper substrate in batch.
Detailed Description
The following describes the embodiments of the present invention in detail with reference to fig. 1, 2, 3, and 4.
Example 1:
as shown in fig. 1, 2, 3 and 4, an apparatus for batch transfer of graphene to a copper mesh substrate includes a carrier plate 1 made of teflon and a carrier plate base 2; the load disk 1 is provided with load holes 3 of a load net copper substrate which are arranged in a matrix (linear matrix or circumferential matrix) or in a random arrangement, and the lower parts of the load holes 3 are provided with lead-out holes 4 which are coaxial with the load holes, have a diameter smaller than that of the load holes 3 and penetrate through the load disk 1; the load disk base 2 is provided with a supporting column 5 which is equal to, coaxial with and matched with the guide-out hole 4.
When the load disk 1 is attached to the load disk base 2, the supporting column 5 passes through the guide-out hole 4 and the load hole 3, and the top surface of the supporting column 5 is 0.2mm higher than the load surface 6 of the load disk 1 and is used for pushing out the net-loaded copper substrate in the load hole 3.
The used net-carrying copper substrate is a micro-grid copper net with the diameter of 3 mm.
The load hole 3 is circular, the diameter of the load hole 3 is (D +0.1), where D is the diameter of the mesh-loaded copper substrate, and when the diameter of the circular mesh-loaded copper substrate D =3mm, the diameter of the load hole 3 is 3.1 mm.
The load port 3 and the lead-out port 4 may also have other shapes, such as oval.
The depth of the loading hole 3 is 0.6 mm.
The leading-out hole 4 is circular, the diameter of the leading-out hole 4 is (D-0.2), wherein D is the diameter of the mesh-carrying copper substrate, and when the diameter of the mesh-carrying copper substrate D =3mm, the diameter of the leading-out hole 4 is 2.8 mm.
A plurality of support holes 8 are formed in the load disc 1, the support holes 8 penetrate through the load disc 1, the diameter of each support hole 8 is 4mm, and the distance between each support hole 8 and the edge of the load disc 1 is 3 mm; the bracket hole 8 is mainly used for moving the load disk 1 by auxiliary tools such as a bracket, tweezers and the like.
Two supporting legs 7 are symmetrically arranged on two sides of the load disk 1, the supporting legs 7 are positioned on the back of the load disk 1 and are semicircular, and the bottom area of each supporting leg 7 is 0.6 cm; the supporting feet 7 mainly serve to support the load tray 1.
The load disk base 2 is provided with a clip 9 which is matched with the load disk supporting foot.
Example 2:
as shown in fig. 1, 2, 3 and 4, an apparatus for batch transfer of graphene onto a mesh-loaded copper substrate includes a load tray 1 made of quartz glass and a load tray base 2; the load disk 1 is provided with load holes 3 of a load net copper substrate which are arranged in a matrix (linear matrix or circumferential matrix) or in a random arrangement, and the lower parts of the load holes 3 are provided with lead-out holes 4 which are coaxial with the load holes 3, have a diameter smaller than that of the load holes 3 and penetrate through the load disk 1; the load disk base 2 is provided with a supporting column 5 which is equal to, coaxial with and matched with the guide-out hole 4.
Preferably, when the load tray 1 is attached to the load tray base 2, the support pillar 5 passes through the exit hole 4 and the load hole 3, and the top surface of the support pillar 5 is 0.5mm higher than the load surface of the load tray 1 for pushing out the copper mesh substrate in the load hole 3.
The used net-carrying copper substrate is a micro-grid copper net with the diameter of 3 mm.
The load hole 3 is circular, the diameter of the load hole 3 is (3/2D), where D is the diameter of the mesh-loaded copper substrate, and when the diameter of the circular mesh-loaded copper substrate D =3mm, the diameter of the load hole 3 is 4.5 mm.
The load port 3 and the lead-out port 4 may also have other shapes, such as oval.
The depth of the loading hole 3 is 5 mm.
The exit hole 4 is circular, and the diameter of the exit hole 4 is (1/2D), where D is the diameter of the mesh-loaded copper substrate, and when the diameter of the mesh-loaded copper substrate D =3mm, the diameter of the exit hole 4 is 1.5 mm.
A plurality of support holes 8 are formed in the load disc 1, the support holes 8 penetrate through the load disc 1, the diameter of each support hole 8 is 4mm, and the distance between each support hole 8 and the edge of the load disc 1 is 3 mm; the bracket hole 8 is mainly used for moving the load disk 1 by auxiliary tools such as a bracket, tweezers and the like.
Two supporting legs 7 are symmetrically arranged on two sides of the load disk 1, the supporting legs 7 are positioned on the back of the load disk 1 and are semicircular, and the bottom area of each supporting leg 7 is 0.6 cm; the supporting feet 7 mainly serve to support the load tray 1.
The load disk base 2 is provided with detents 9 which are adapted to the support feet 7 of the load disk 1.
Example 3:
as shown in fig. 1, 2, 3 and 4, an apparatus for batch transfer of graphene to a copper mesh substrate includes a carrier plate 1 made of teflon and a carrier plate base 2; the load disk 1 is provided with load holes 3 of a load net copper substrate which are arranged in a matrix (linear matrix or circumferential matrix) or in a random arrangement, and the lower parts of the load holes 3 are provided with lead-out holes 4 which are coaxial with the load holes 3, have a diameter smaller than that of the load holes 3 and penetrate through the load disk 1; the load disk base 2 is provided with a supporting column 5 which is equal to, coaxial with and matched with the guide-out hole 4.
When the load disk 1 is attached to the load disk base 2, the supporting column 5 passes through the guide-out hole 4 and the load hole 3, and the top surface of the supporting column 5 is 0.3mm higher than the load surface of the load disk 1 and is used for pushing out the net-loaded copper substrate in the load hole 3.
The used net-carrying copper substrate is a micro-grid copper net with the diameter of 3 mm.
The load hole 3 is circular, the diameter of the load hole 3 is (D +0.4), where D is the diameter of the mesh-loaded copper substrate, and when the diameter of the circular mesh-loaded copper substrate D =3mm, the diameter of the load hole 3 is 3.4 mm.
The load port 3 and the lead-out port 4 may also have other shapes, such as oval.
The depth of the loading hole 3 is 0.8 mm.
The leading-out hole 4 is circular, the diameter of the leading-out hole 4 is (D-0.2), wherein D is the diameter of the mesh-carrying copper substrate, and when the diameter D =3mm, the diameter of the leading-out hole 4 is 2.8 mm; the diameter of the supporting column 5 matched with the supporting column is 2.5 mm.
A plurality of support holes 8 are formed in the load disc 1, the support holes 8 penetrate through the load disc 1, the diameter of each support hole 8 is 4mm, and the distance between each support hole 8 and the edge of the load disc 1 is 3 mm; the bracket hole 8 is mainly used for moving the load disk 1 by auxiliary tools such as a bracket, tweezers and the like.
Two supporting legs 7 are symmetrically arranged on two sides of the load disk 1, the supporting legs 7 are positioned on the back of the load disk 1 and are semicircular, and the bottom area of each supporting leg 7 is not less than 0.6 cm; the supporting feet 7 mainly serve to support the load tray 1.
The load disk base 2 is provided with detents 9 which are adapted to the support feet 7 of the load disk 1.
Example 4:
the graphene can be transferred to the mesh-loaded copper substrate in batch by the following method using the apparatuses of example 1, example 2, and example 3.
The flat copper foil (4 cm 2) with the graphene growing thereon is stably attached to the gluing substrate by using an adhesive tape, and the purpose is to avoid unstable absorption and damage of the copper foil in the copper foil gluing process.
Carrying out spin coating on the surface of the copper foil by using a PMMA (polymethyl methacrylate) solution with the mass fraction of 4, wherein the spin coating comprises two stages of low-speed spin coating (900 revolutions per second and 10 seconds) and high-speed spin coating (3000 revolutions per second and 30 seconds) for 2 times; and after removing the gluing substrate, the spin-coated copper foil is placed on a heating platform at 150 ℃ to be heated for 3min, so that the PMMA film is cured, and a PMMA/graphene/copper foil sample is obtained.
The obtained PMMA/graphene/copper foil sample is pre-etched in 1M ammonium persulfate solution, deionized water is used for washing the bottom of the pre-etched foil after pre-etching is finished, graphene on the copper foil on the back (non-gluing surface) is removed, pre-etching is repeated for 2 times with 5min as a period, then the copper foil is removed in the ammonium persulfate solution through a solution etching method, separation of the graphene and the copper foil is achieved, and the PMMA/graphene film is obtained.
And rinsing the PMMA/graphene film in deionized water containing 10% of isopropanol by mass fraction to remove residual etching solution on the film, wherein the isopropanol is used for reducing the surface tension of the deionized water so as to facilitate the subsequent transfer work.
The load disc 1 is placed in a rinsing container in advance, a net-carrying copper substrate is loaded into a load hole 3 of the load disc 1 by using tweezers, one surface of the net-carrying copper substrate, which is provided with the amorphous carbon film, faces upwards, and rinsing solution is dripped on the load hole 3, so that the net-carrying copper substrate is prevented from floating from the load hole 3 in the loading process.
A hose is used for guiding out deionized water in the rinsing container, and tweezers are used for assisting a PMMA/graphene film to be stably and flatly attached to the upper surface of the load plate 1 in the water level descending process; the loading disc 1 loaded with the PMMA/graphene film is clamped into the base 2 after part of rinsing solution is sucked away by using dust-free paper, the supporting columns 5 in the base 2 support the net-loaded copper substrate in the loading holes 3, and a heating platform is used for drying a sample at 120 ℃, so that the net-loaded copper substrate and the PMMA/graphene film are stably attached.
The obtained sample is reversely buckled in the loading hole 3, and the PMMA film is placed in a design mode that one surface of the PMMA film faces downwards; introducing acetone steam obtained at 100 ℃ from the bottom of the load disk 1, and steaming for 2 hours by using the acetone steam; then introducing isopropanol vapor obtained at 100 ℃ into the loading plate 1, removing the excess acetone solution on the surface of the sample, and finally realizing the perfect removal of the PMMA film.
Thus, the graphene can be transferred on 49 mesh-carrying copper substrates at the same time.
Example 5:
the difference between this example and example 4 is that the copper foil etching solution is a 1M ferric trichloride solution, and other conditions are not changed.
Example 6:
this example differs from example 4 in that the PMMA film was cured at 100 ℃ under otherwise unchanged conditions.
Example 7:
this example differs from example 4 in that the acetone vapor is taken at 80 ℃ and the other conditions are unchanged.
Example 8:
this example differs from example 4 in that the resist was removed directly using an acetone solution at 50 ℃ without changing other conditions.
Example 9:
the difference between this example and example 4 is that the photoresist is first soaked in acetone solution for 10min and then stripped under acetone vapor, and other conditions are not changed.
The above embodiments are intended to be preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention and are equivalent to the replacement of the above embodiments are included in the scope of the present invention.
Claims (10)
1. A device for transferring graphene to a net-carrying copper substrate in batches is characterized by comprising a load disk and a load disk base; the load disc is provided with load holes of the load net copper substrate which are arranged in a matrix or in a random way, and the lower parts of the load holes are provided with lead-out holes which are coaxial with the load holes, have a diameter smaller than that of the load holes and run through the load disc; the load disc base is provided with support columns which are equal to and coaxial with the guide-out holes and are matched with the guide-out holes.
2. The apparatus of claim 1, wherein the supporting pillars pass through the exit holes and the loading holes when the loading tray is attached to the loading tray base, and the top surfaces of the supporting pillars are 0.2-0.5mm higher than the loading surface of the loading tray for pushing out the copper mesh-loaded substrate in the loading holes.
3. The apparatus of claim 1, wherein the loading holes are circular, and the diameter of the loading holes is (D +0.1) - (3/2D), wherein D is the diameter of the copper substrate, and when the diameter of the circular copper substrate is D =3mm, the diameter of the loading holes is 3.1-4.5 mm.
4. The apparatus according to claim 1, wherein the depth of the loading hole is 0.5-5 mm.
5. The apparatus of claim 1, wherein the exit hole is circular and has a diameter of (D-0.2) - (1/2D), wherein D is the diameter of the copper substrate, and when the diameter of the copper substrate is D =3mm, the exit hole has a diameter of 2.8-1.5 mm.
6. The apparatus according to claim 1, wherein the load tray is provided with a plurality of support holes, the support holes penetrate through the load tray, the diameter of each support hole is not less than 3mm, and the distance between each support hole and the edge of the load tray is not less than 2 mm.
7. The apparatus according to claim 1, wherein two supporting legs are symmetrically disposed on two sides of the load tray, the supporting legs are located on the back of the load tray and have a semicircular shape, and a bottom area of each supporting leg is not less than 0.5 cm.
8. The apparatus of claim 1, wherein the loading tray base is provided with a detent matching with the loading tray support leg.
9. The apparatus of claim 1, wherein the load tray and the load tray base are made of acid and alkali resistant material.
10. A method for transferring graphene to a net-carrying copper substrate in batch is characterized by comprising the following steps:
s1, spin-coating a PMMA solution with the concentration of 1% -10% on the surface of a copper foil with graphene by a CVD method, wherein the spin-coating comprises two stages of low-speed spin-coating and high-speed spin-coating, the low-speed spin-coating speed is 500-5000 r/s;
s2, placing the copper foil coated with PMMA in a heating platform for curing, wherein the curing temperature is 50-180 ℃, and the curing time is 3-10 min;
s3, obtaining a PMMA/graphene/Cu sample through heating and curing, pre-etching by using an etching solution with the concentration of 0.1-1.5M, pre-etching for 2-4 periods with 2-6min as an etching period, and slowly flushing the pre-etched surface by using deionized water after each period is finished to remove a graphene layer on the etched surface;
s4, etching the PMMA/graphene/Cu sample after the pre-etching is finished by using an etching solution with the concentration of 0.1-1.5M, and removing the copper foil to obtain a PMMA/graphene film;
s5, rinsing the graphene/PMMA film obtained in the step S4 by using deionized water containing 2% -15% of isopropanol or ethanol surfactant; after rinsing, loading the graphene/PMMA film on the surface of a loading disc with a net-loading copper substrate by controlling the water level to drop or using an auxiliary device; the isopropanol and ethanol surfactants used in the method aim at reducing the surface tension of deionized water, so that the subsequent transfer work is facilitated;
s6, pushing out the net-carrying copper substrate placed in the load hole through the support column of the load disk base to enable the net-carrying copper substrate to be closely attached to the graphene/PMMA film; naturally airing or drying the PMMA/graphene/net-carrying copper substrate sample by a heating platform at the temperature of 80-150 ℃;
s7, reversely buckling the PMMA/graphene/mesh-loaded copper substrate sample obtained in the step 6 in a mesh-loaded copper substrate loading hole of a loading disc, and removing the PMMA film on the PMMA/graphene/mesh-loaded copper substrate sample within 0.5-3h by using acetone steam obtained at 70-150 ℃; after the PMMA film is removed by acetone vapor, residual acetone on the surface of the sample is removed within 0.5-3h by using isopropanol vapor obtained at 70-150 ℃, and the remaining graphene is attached to the mesh-carrying copper substrate.
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| CN112624095A (en) * | 2020-12-21 | 2021-04-09 | 西安交通大学 | Two-dimensional material transfer method based on water phase change |
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