CN106927459A - A kind of method for directly preparing number of plies controllable grapheme on an insulating substrate - Google Patents
A kind of method for directly preparing number of plies controllable grapheme on an insulating substrate Download PDFInfo
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- CN106927459A CN106927459A CN201511019588.6A CN201511019588A CN106927459A CN 106927459 A CN106927459 A CN 106927459A CN 201511019588 A CN201511019588 A CN 201511019588A CN 106927459 A CN106927459 A CN 106927459A
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- plies
- insulating substrate
- graphene
- metal layer
- grapheme
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/26—Bombardment with radiation
- H01L21/263—Bombardment with radiation with high-energy radiation
- H01L21/265—Bombardment with radiation with high-energy radiation producing ion implantation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/324—Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering
Abstract
The present invention provides a kind of method for directly preparing number of plies controllable grapheme on an insulating substrate, using ion implanting precise control carbon ion dosage, the Graphene of the different numbers of plies is directly prepared in various dielectric substrates.Deposited metal nickel film on an insulating substrate, is then used by ion implanting and the corresponding carbon ion dosage of the different numbers of plies is injected separately into nickel film first, and relatively thick Copper thin film is then deposited on nickel.Making ambrose alloy at high temperature can be dissolved each other, and substantial amounts of copper constantly can down push away carbon, finally be released from nickel, and Graphene is formed in the interface of dielectric substrate and monel.The present invention can directly obtain the controllable high-quality continuous graphite alkene of the large area number of plies in different dielectric substrates, need not further shift, substantially increase the quality of Graphene, the high―temperature nuclei time of the present invention is extremely short, preparation efficiency can be greatly improved, for high-quality graphene and Graphene application provide effective and feasible ground approach on preparation of industrialization insulator.
Description
Technical field
It is more particularly to a kind of directly to prepare the controllable stone of the number of plies on an insulating substrate the present invention relates to a kind of preparation method of Graphene
The method of black alkene.
Background technology
Graphene is first stable two dimensional crystal successfully prepared, and is considered as the base of the allotrope for constituting other carbon
This material.Graphene surmounts graphite and the excellent properties of CNT are caused in nanometer mechanics, nanoelectronics and nanophotonics
Etc. the substantial amounts of exploration upsurge of aspect.Therefore since finding Graphene from 2004, the research to Graphene synthetic method is never interrupted,
The Graphene of the different numbers of plies possesses different properties, and such as single-layer graphene has high transmission rate, high conductivity etc., double-layer graphite
Alkene can open band gap under magnetic fields.
The subject matter that the synthesis of current Graphene faces is controllable to the number of plies of Graphene and direct prepares on an insulating substrate.In advance
To first be annealed in carbon ion implantation to nickel-copper laminar structured substrate, can be with by the precise control to carbon ion implantation dosage
The Graphene of the different numbers of plies is successfully obtained on monel substrate.Although however, the different numbers of plies can be obtained based on the above method
Graphene, but, the Graphene for being obtained is to be grown on monel surface, in actual applications, resulting Graphene
Need to be transferred to could be realized in dielectric substrate further application, in the process of multi-layer graphene transfer, inevitably draw
Enter defect, impurity, fold and crack, consequently, it is possible to reducing the performance of graphene device.
In view of the above, how to realize that a kind of method of the Graphene for directly obtaining the controllable number of plies on an insulating substrate is remained
One greatly challenge.
The content of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide a kind of preparation number of plies direct on an insulating substrate
The method of controllable grapheme, the Graphene for solving to be difficult to directly to prepare on an insulating substrate in the prior art the controllable number of plies is asked
Topic.
In order to achieve the above objects and other related objects, present invention offer is a kind of directly prepares the controllable graphite of the number of plies on an insulating substrate
The method of alkene, methods described includes step:Step 1), there is provided a dielectric substrate, in forming the first gold medal in the dielectric substrate
Category layer;Step 2), inject carbon ion in the first metal layer;Step 3), form the in the first metal layer surface
Two metal levels, first metal can dissolve each other at high temperature with the second metal;Step 4), carrying out annealing process makes described first
Metal level dissolves each other to form alloy with the second metal layer, and causes that the carbon ion is pushed out to institute from the first metal layer
Insulated substrate surface is stated, graphene layer is formed;Step 5), remove the alloy, stone on the insulator controllable to obtain the number of plies
Black alkene.
As a kind of preferred scheme of the method for directly preparing number of plies controllable grapheme on an insulating substrate of the invention, described second
Carbon ion solubility of the carbon ion solubility of metal less than the first metal layer.
As a kind of preferred scheme of the method for directly preparing number of plies controllable grapheme on an insulating substrate of the invention, by control
The implantation dosage of the carbon ion controls the number of plies of the Graphene.
As a kind of preferred scheme of the method for directly preparing number of plies controllable grapheme on an insulating substrate of the invention, described first
Metal level is nickel dam, and second metal layer is layers of copper.
Preferably, thickness of the thickness of the layers of copper more than the nickel dam.
Preferably, the thickness range of the nickel dam is 100~500nm.
Preferably, the thickness range of the layers of copper is 1~10 μm.
Preferably, the temperature range of the annealing process is 700~1000 DEG C.
Preferably, the time range of the annealing process is 5~30min.
Preferably, the implantation dosage scope for often increasing increased carbon ion corresponding to a layer graphene is 3.5 × 1015~4 × 1015
atoms/cm2。
As a kind of preferred scheme of the method for directly preparing number of plies controllable grapheme on an insulating substrate of the invention, step 1)
In, method using electron beam evaporation or magnetron sputtering in the dielectric substrate in forming the first metal layer.
As a kind of preferred scheme of the method for directly preparing number of plies controllable grapheme on an insulating substrate of the invention, step 3)
In, the second metal layer is formed in the first metal layer surface using electron beam evaporation, magnetron sputtering or electric plating method.
As a kind of preferred scheme of the method for directly preparing number of plies controllable grapheme on an insulating substrate of the invention, step 5)
In, the alloy is removed using tape-stripping and the method for removing, or using the method removal alloy of wet etching.
As a kind of preferred scheme of the method for directly preparing number of plies controllable grapheme on an insulating substrate of the invention, the insulation
Substrate has the one kind in silicon substrate, Sapphire Substrate and the quartz glass substrate of silica including surface.
As described above, the method for directly preparing number of plies controllable grapheme on an insulating substrate of the invention, has the advantages that:
1) present invention design is ingenious, and carbon atom does not lose substantially, therefore can be by the dosage precise control Graphene of ion implanting
The number of plies;
2) present invention can directly obtain the controllable high-quality continuous graphite alkene of the large area number of plies in different dielectric substrates, be not required to
Further to shift, it is to avoid Graphene introduces in transfer process the defect in defect, impurity, fold and crack, so that significantly
Improve the performance of graphene device;
3) present invention can avoid using the hazardous gases such as hydrogen, methane;
4) the high―temperature nuclei time of the present invention is extremely short (5 minutes~30 minutes), can greatly improve preparation efficiency;
5) present invention on preparation of industrialization insulator high-quality graphene and Graphene application provide effective and feasible ground approach.
Brief description of the drawings
Fig. 1~Fig. 6 is shown as what each step of method for preparing number of plies controllable grapheme direct on an insulating substrate of the invention was presented
Structural representation.
Fig. 7~Fig. 9 is respectively indicated as using prepared by the method for preparing number of plies controllable grapheme direct on an insulating substrate of the invention
Single-layer graphene, bilayer graphene and three layer graphenes Raman spectrogram.
Component label instructions
101 dielectric substrates
102 the first metal layers
103 second metal layers
104 alloys
105 Graphenes
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.
As shown in Fig. 1~Fig. 9, the present embodiment offer is a kind of directly to prepare number of plies controllable grapheme 105 on the insulating substrate 101
Method, methods described includes step:
As shown in Fig. 1~Fig. 2, step 1 is carried out first), there is provided a dielectric substrate 101, in shape in the dielectric substrate 101
Into the first metal layer 102.
As an example, the dielectric substrate 101 has silicon substrate, Sapphire Substrate and the quartz glass of silica including surface
One kind in substrate.In the present embodiment, the dielectric substrate 101 has the silicon substrate of silica for surface, selects the substrate
The structure for eventually forming is the structure of Graphene 105 on the insulator of silicon substrate-top layer of insulating barrier-Graphene 105, and the structure can be with
Replacement traditional SOI substrate, and every excellent properties of Graphene 105 are played, meet existing semiconductor fabrication process demand.
As an example, using the method for electron beam evaporation or magnetron sputtering in forming the first metal layer in the dielectric substrate 101
102.In the present embodiment, using the method for magnetron sputtering in formation the first metal layer 102 in the dielectric substrate 101, and institute
The first metal layer 102 is stated to select as nickel.
As an example, the thickness range of the nickel dam is 100~500nm.In the present embodiment, the thickness of the nickel dam is 300nm.
As shown in figure 3, then carrying out step 2), inject carbon ion in the first metal layer 102.
As an example, the present invention can be by the number of plies that controls the implantation dosage of the carbon ion to control the Graphene 105.
Specifically, nickel is selected with the first metal layer 102, second metal layer 103 from as a example by copper, its carbon ion implantation dosage and final
The relation of the number of plies of the Graphene 105 of acquisition is as shown in the table:
As seen from the above table, the number of plies of Graphene 105 is in proportionate relationship substantially with the implantation dosage of carbon ion, thus, it is only required to pass through
The implantation dosage of control carbon ion just can very easily control the number of plies of the Graphene 105 of final acquisition.
As an example, the implantation dosage scope for often increasing increased carbon ion corresponding to a layer graphene 105 is 3.5 × 1015
~4 × 1015atoms/cm2.In the present embodiment, the implantation dosage of increased carbon ion corresponding to a layer graphene 105 is often increased
Scope is 3.8 × 10158atoms/cm2。
As described in Figure 4, step 3 is then carried out), second metal layer 103 is formed in the surface of the first metal layer 102, it is described
First metal can dissolve each other at high temperature with the second metal.
As an example, carbon ion solubility of the bimetallic carbon ion solubility less than the first metal layer 102.It is excellent
Selection of land, the bimetallic carbon ion solubility selection is more low better, it is furthermore preferred that the bimetallic carbon ion is molten
Xie Du selections are zero or close to zero, also, second metal and the first metal alloy 104 that dissolves each other formed carbon ion
It is more low better that solubility is preferably also, to ensure that carbon ion forms the conversion ratio of Graphene 105.
As an example, forming institute in the surface of the first metal layer 102 using electron beam evaporation, magnetron sputtering or electric plating method
State second metal layer 103.In the present embodiment, described is formed in the surface of the first metal layer 102 using electric plating method
Two metal levels 103, and it is copper that the second metal layer 103 is selected, the Carbon Solubility of copper is very low, can cause that metal dissolves each other
During, carbon atom does not lose substantially.
As an example, thickness of the thickness of the layers of copper more than the nickel dam, to ensure to make carbon ion try one's best during subsequently dissolving each other
Many is pushed out to the surface of dielectric substrate 101.
As an example, the thickness range of the layers of copper is 1~10 μm.In the present embodiment, the thickness of the layers of copper is 5 μm.
As shown in figure 5, then carrying out step 4), carrying out annealing process makes the first metal layer 102 with second metal
Layer 103 dissolves each other to form alloy 104, and causes that the carbon ion is pushed out to the insulation lining from the first metal layer 102
The surface of bottom 101, forms 105 layers of Graphene;
As an example, the temperature range of the annealing process is 700~1000 DEG C.
As an example, the time range of the annealing process is 5~30min.The high―temperature nuclei time of the present invention extremely short (5 minutes~30
Minute), can greatly improve preparation efficiency.
Specifically, during cupro-nickel is dissolved each other, nickle atom is up moved, and copper atom moves down, due to the Carbon Solubility of copper
It is very low, therefore substantial amounts of copper constantly can down push away carbon, finally be released from nickel, on dielectric substrate and the boundary of monel
Graphene is formed at face.
As shown in fig. 6, finally carrying out step 5), remove the alloy 104, Graphene on the insulator controllable to obtain the number of plies
105。
As an example, the alloy 104 can be removed using tape-stripping and the method for removing, or using the side of wet etching
Method removes the alloy 104.In the present embodiment, the alloy 104, the method are removed using tape-stripping and the method for removing
With efficiency high, it is not necessary to chemical attack, the advantage that Graphene 105 can be avoided to damage.
Fig. 7~Fig. 9 is respectively indicated as single-layer graphene 105, the Raman spectrum of the layer graphene 105 of bilayer graphene 105 and three
Figure, from Fig. 7~Fig. 9, Graphene 105 on the controllable insulator of the high-quality number of plies can be obtained using the method for the present invention.
As described above, the method for directly preparing number of plies controllable grapheme 105 on the insulating substrate 101 of the invention, with following
Beneficial effect:
1) present invention design is ingenious, and carbon atom does not lose substantially, therefore can be by the dosage precise control Graphene of ion implanting
105 number of plies;
2) present invention can directly obtain the controllable high-quality continuous graphite alkene of the large area number of plies in different dielectric substrates, be not required to
Further to shift, it is to avoid Graphene introduces in transfer process the defect in defect, impurity, fold and crack, so that significantly
Improve the performance of graphene device;
3) present invention can avoid using the hazardous gases such as hydrogen, methane;
4) the high―temperature nuclei time of the present invention is extremely short (5 minutes~30 minutes), can greatly improve preparation efficiency.;
5) present invention on preparation of industrialization insulator high-quality graphene and Graphene application provide effective and feasible ground approach.
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 (14)
1. it is a kind of on an insulating substrate directly prepare number of plies controllable grapheme method, it is characterised in that methods described include step:
Step 1), there is provided a dielectric substrate, in forming the first metal layer in the dielectric substrate;
Step 2), inject carbon ion in the first metal layer;
Step 3), second metal layer is formed in the first metal layer surface, first metal and the second metal can be in height
Dissolved each other under temperature;
Step 4), carrying out annealing process makes the first metal layer dissolve each other to form alloy with the second metal layer, and causes
The carbon ion is pushed out to the insulated substrate surface from the first metal layer, forms graphene layer;
Step 5), remove the alloy, Graphene on the insulator controllable to obtain the number of plies.
2. it is according to claim 1 on an insulating substrate directly prepare number of plies controllable grapheme method, it is characterised in that:It is described
Carbon ion solubility of the bimetallic carbon ion solubility less than the first metal layer.
3. it is according to claim 1 on an insulating substrate directly prepare number of plies controllable grapheme method, it is characterised in that:Pass through
Control the number of plies of the implantation dosage control Graphene of the carbon ion.
4. it is according to claim 1 on an insulating substrate directly prepare number of plies controllable grapheme method, it is characterised in that:It is described
The first metal layer is nickel dam, and second metal layer is layers of copper.
5. it is according to claim 4 on an insulating substrate directly prepare number of plies controllable grapheme method, it is characterised in that:It is described
Thickness of the thickness of layers of copper more than the nickel dam.
6. it is according to claim 4 on an insulating substrate directly prepare number of plies controllable grapheme method, it is characterised in that:It is described
The thickness range of nickel dam is 100~500nm.
7. it is according to claim 4 on an insulating substrate directly prepare number of plies controllable grapheme method, it is characterised in that:It is described
The thickness range of layers of copper is 1~10 μm.
8. it is according to claim 4 on an insulating substrate directly prepare number of plies controllable grapheme method, it is characterised in that:It is described
The temperature range of annealing process is 700~1000 DEG C.
9. it is according to claim 4 on an insulating substrate directly prepare number of plies controllable grapheme method, it is characterised in that:It is described
The time range of annealing process is 5~30min.
10. it is according to claim 4 on an insulating substrate directly prepare number of plies controllable grapheme method, it is characterised in that:
The implantation dosage scope for often increasing increased carbon ion corresponding to a layer graphene is 3.5 × 1015~4 × 1015atoms/cm2。
11. methods for directly preparing number of plies controllable grapheme on an insulating substrate according to claim 1, it is characterised in that:
Step 1) in, method using electron beam evaporation or magnetron sputtering in the dielectric substrate in forming the first metal layer.
12. methods for directly preparing number of plies controllable grapheme on an insulating substrate according to claim 1, it is characterised in that:
Step 3) in, form described in the first metal layer surface using electron beam evaporation, magnetron sputtering or electric plating method
Two metal levels.
13. methods for directly preparing number of plies controllable grapheme on an insulating substrate according to claim 1, it is characterised in that:
Step 5) in, the alloy is removed using tape-stripping and the method for removing, or using the method removal institute of wet etching
State alloy.
14. methods for directly preparing number of plies controllable grapheme on an insulating substrate according to claim 1, it is characterised in that:Institute
Stating dielectric substrate has one kind in silicon substrate, Sapphire Substrate and the quartz glass substrate of silica including surface.
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