CN106904600B - A method of preparing continuous single-layer graphene on an insulating substrate - Google Patents
A method of preparing continuous single-layer graphene on an insulating substrate Download PDFInfo
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- CN106904600B CN106904600B CN201510952655.3A CN201510952655A CN106904600B CN 106904600 B CN106904600 B CN 106904600B CN 201510952655 A CN201510952655 A CN 201510952655A CN 106904600 B CN106904600 B CN 106904600B
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- C01B2204/00—Structure or properties of graphene
- C01B2204/02—Single layer graphene
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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Abstract
The present invention provides a kind of method for preparing continuous single-layer graphene on an insulating substrate, comprising: 1) provides an insulating substrate, deposit germanium film in Yu Suoshu insulating substrate；2) using the germanium film as catalyst, graphene is grown at high temperature, meanwhile, germanium film constantly evaporates at high temperature, and is finally entirely removed, and obtains the continuous graphite alkene being incorporated into insulating substrate.The present invention passes through germanium film catalytic growth graphene in insulating substrate, and by germanium film evaporative removal while growth, obtain single layer continuous graphite alkene on insulator, it overcomes traditional handicraft and such as pollution, gauffer influence brought by graphene on insulator is prepared using transfer method, improve the quality and performance of grapheme material on insulator.Large area single layer continuous graphite alkene can be obtained using method of the invention.Step of the present invention is simple, significant effect, is with a wide range of applications in field of preparation of graphene.
Description
Technical field
The present invention relates to a kind of preparation methods of graphene, prepare continuous single layer on an insulating substrate more particularly to one kind
The method of graphene.
Background technique
Graphene is with unusual electric conductivity, intensity beyond steel decades of times and fabulous translucency, it
Appearance is expected to cause a wheel revolution in modern electronic technology field.In graphene, electronics can be migrated extremely efficiently, and be passed
The semiconductor and conductor of system, such as silicon and the copper graphene that is far from show well.Due to the collision of electronics and atom, traditional half
The form of conductor and conductor heat releases some energy, and general computer chip wastes 72%-81%'s in this way
Electric energy, graphene is then different, its electron energy will not be depleted, this makes it be provided with extraordinary good characteristic.
Since two scientists of Univ Manchester UK in 2004 have found graphene using the method that micromechanics is removed
Since, the appearance of graphene has evoked huge great waves.Graphene is impayable in aspect of performance such as physics, chemistry, mechanics
Advantage gathers around it in fields such as electronics, information, the energy, material and biological medicines and has broad application prospects
Obtaining the preparation method of single layer large-area graphene at present is mainly metal (nickel, copper etc.) catalytic chemical gaseous phase deposition
Method needs to transfer graphene in insulating substrate for the application of electronic field, but the presently used transfer method step arrived
It is rapid complicated, it is easy to which that fold, the pollution for causing graphene will certainly reduce the performance of graphene.
In view of the above, it how to be able to achieve a kind of method tool that can prepare large area single-layer graphene on an insulating substrate
There is important meaning.
Summary of the invention
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide a kind of companies of preparation on an insulating substrate
The method of continuous single-layer graphene is easy to make by graphene in the method preparation insulating substrate of transfer in the prior art for solving
The problem of declining at graphene performance.
In order to achieve the above objects and other related objects, the present invention provides one kind and prepares continuous single layer stone on an insulating substrate
The method of black alkene, the method includes the steps: step 1) provides an insulating substrate, deposits germanium film in Yu Suoshu insulating substrate；
Step 2) grows graphene using the germanium film as catalyst at high temperature, meanwhile, germanium film constantly evaporates at high temperature, and
It is finally entirely removed, obtains the continuous graphite alkene being incorporated into insulating substrate.
As a kind of preferred embodiment of the method for preparing continuous single-layer graphene on an insulating substrate of the invention, step 1)
In, the insulating substrate includes one of silicon substrate, Sapphire Substrate and the quartz substrate that surface has silica.
As a kind of preferred embodiment of the method for preparing continuous single-layer graphene on an insulating substrate of the invention, step 1)
In, method using magnetron sputtering is in depositing germanium film in the insulating substrate.
As a kind of preferred embodiment of the method for preparing continuous single-layer graphene on an insulating substrate of the invention, step 1)
In, the thickness range of the germanium film of deposition is 10~500nm.
As a kind of preferred embodiment of the method for preparing continuous single-layer graphene on an insulating substrate of the invention, step 2)
In, graphene is grown in the germanium film surface using gaseous carbon source as raw material.
Further, the gaseous carbon source includes the combination of one or more of methane, acetylene, ethylene.
As a kind of preferred embodiment of the method for preparing continuous single-layer graphene on an insulating substrate of the invention, step 2)
In, graphene is grown in the germanium film surface using chemical vapour deposition technique.
As a kind of preferred embodiment of the method for preparing continuous single-layer graphene on an insulating substrate of the invention, step 2)
In, the temperature range of the high temperature is 850~937 DEG C.
As a kind of preferred embodiment of the method for preparing continuous single-layer graphene on an insulating substrate of the invention, step 2)
In, the retention time of the high temperature is at least more than the time that the germanium film all evaporates, the retention time range of the high temperature
For 30~300min.
As a kind of preferred embodiment of the method for preparing continuous single-layer graphene on an insulating substrate of the invention, step 2)
In, the graphene is the continuous graphene of single layer.
As described above, the method for preparing continuous single-layer graphene on an insulating substrate of the invention, has below beneficial to effect
Fruit: the present invention obtains germanium film evaporative removal by germanium film catalytic growth graphene in insulating substrate, and while growth
Single layer continuous graphite alkene on insulator is obtained, traditional handicraft is overcome and is prepared on insulator brought by graphene using transfer method
Such as pollution, gauffer influences, and improves the quality and performance of grapheme material on insulator.It can be obtained using method of the invention
Obtain large area single layer continuous graphite alkene.Step of the present invention is simple, significant effect, has a wide range of applications in field of preparation of graphene
Prospect.
Detailed description of the invention
Fig. 1 is shown as the step process signal of the method for preparing continuous single-layer graphene on an insulating substrate of the invention
Figure.
Each step of method for preparing continuous single-layer graphene on an insulating substrate that Fig. 2~Fig. 5 is shown as invention is presented
Structural schematic diagram.
Fig. 6 is shown as the Raman spectrogram of the continuous graphene of single layer on the insulator that the present invention obtains.
Fig. 7 is shown as the SEM figure of the continuous graphene of single layer on the insulator that the present invention obtains.
Fig. 8 is shown as the peak Raman spectrum 2D and G peak intensity of the continuous graphene of single layer on the insulator that the present invention obtains
Than figure.
Component label instructions
101 insulating substrates
102 germanium films
103 graphenes
S11~S12 step 1)~step 2)
Specific embodiment
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification
Other advantages and efficacy of the present invention can be easily understood for disclosed content.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints and application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
Please refer to FIG. 1 to FIG. 8.It should be noted that diagram provided in the present embodiment only illustrates this in a schematic way
The basic conception of invention, only shown in diagram then with related component in the present invention rather than package count when according to actual implementation
Mesh, shape and size are drawn, when actual implementation kenel, quantity and the ratio of each component can arbitrarily change for one kind, and its
Assembly layout kenel may also be increasingly complex.
As shown in fig. 1~fig. 5, the present embodiment provides the sides that one kind prepares continuous graphite alkene 103 on the insulating substrate 101
Method, the method includes the steps:
As shown in FIG. 1 to FIG. 2, progress step 1) S11 first provides an insulating substrate 101, Yu Suoshu insulating substrate 101
Upper deposition germanium film 102.
As an example, the insulating substrate 101 includes silicon substrate, Sapphire Substrate and the quartz that surface has silica
One of substrate.In the present embodiment, the insulating substrate 101 is the silicon substrate that surface has silica, made by
Substrate is graphene substrate on insulator, on the one hand the oxide layer can prevent dissolving each other for germanium and silicon, on the other hand, forms bottom
Layer silicon-insulating layer-graphene-structured substrate, more meets the demand of semiconductor fabrication process now.
As an example, using the method for magnetron sputtering in deposition germanium film 102 in the insulating substrate 101.Certainly, may be used
To prepare the germanium film 102 using other methods, therefore, however it is not limited to example recited herein.
It is needed as subsequent through germanium film 102 described in evaporative removal, the thickness of the germanium film 102 should not be too
Greatly, simultaneously as the interface that germanium film 102 is contacted with insulating substrate 101 has more defect, and as germanium film 102 is thick
The increase disadvantage of degree is gradually reduced, and therefore, the thickness of the germanium film 102 also should not be too small.As an example, the germanium film of deposition
102 thickness range is 10~500nm.One more preferably thickness range be 50~100nm.
As shown in Fig. 3~Fig. 5, step 2) S12 is then carried out, is catalyst with the germanium film 102, grows at high temperature
Graphene 103, meanwhile, the constantly evaporation at high temperature of germanium film 102, and be finally entirely removed, acquisition is incorporated into insulating substrate
Continuous graphite alkene 103 on 101.
As an example, growing stone in 102 surface of germanium film using chemical vapour deposition technique using gaseous carbon source as raw material
Black alkene 103.Further, the gaseous carbon source includes the combination of one or more of methane, acetylene, ethylene.
As an example, the temperature range of the high temperature is 850~937 DEG C.The determination basis of the temperature range is first,
It is grown suitable for graphene 103；Second, it is able to achieve the evaporation of germanium material；Third cannot be greater than the temperature (fusing point of germanium of germanium fusing
It is 937 DEG C).Preferably, selecting temperature is 920 DEG C, and the germanium that can obtain superior in quality graphene 103 and fast speed steams
Hair.
As an example, the retention time of the high temperature is at least more than the time that the germanium film 102 all evaporates, the height
The retention time range of temperature is 30~300min.
As an example, the graphene 103 that the present embodiment is grown is the continuous graphene of single layer.
Fig. 6 is shown as the Raman spectrogram of the continuous graphene of single layer on the insulator of the present embodiment acquisition, and Fig. 7 is shown as
The SEM figure of the continuous graphene of single layer, Fig. 8 are shown as on the insulator of the present embodiment acquisition on the insulator that the present embodiment obtains
The peak Raman spectrum 2D and G peak intensity of the continuous graphene of single layer are than scheming.It can be seen from Fig. 6~Fig. 8 through this embodiment
Method can obtain the continuous graphene of single layer in performance good insulating body.
As described above, the method for preparing single layer continuous graphite alkene 103 on the insulating substrate 101 of the invention, has following
The utility model has the advantages that the present invention passes through 102 catalytic growth graphene 103 of germanium film in insulating substrate 101, and by germanium while growth
102 evaporative removal of film obtains single layer continuous graphite alkene 103 on insulator, overcomes traditional handicraft and is prepared using transfer method
Such as pollution, gauffer brought by graphene 103 influences on insulator, improves the quality of 103 material of graphene on insulator
And performance.Large area single layer continuous graphite alkene 103 can be obtained using method of the invention.Step of the present invention is simple, and effect is aobvious
It writes, is with a wide range of applications in 103 preparation field of graphene.So the present invention effectively overcomes in the prior art kind
It plants disadvantage and has high industrial utilization value.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (8)
1. the method that one kind prepares continuous single-layer graphene on an insulating substrate, which is characterized in that the method includes the steps:
Step 1) provides an insulating substrate, deposits germanium film in Yu Suoshu insulating substrate；
Step 2) grows graphene using the germanium film as catalyst at high temperature, meanwhile, germanium film constantly steams at high temperature
Hair, and be finally entirely removed, the continuous graphite alkene being incorporated into insulating substrate is obtained, the temperature range of the high temperature is 850
~937 DEG C.
2. the method according to claim 1 for preparing continuous single-layer graphene on an insulating substrate, it is characterised in that: step
1) in, the insulating substrate includes one of silicon substrate, Sapphire Substrate and the quartz substrate that surface has silica.
3. the method according to claim 1 for preparing continuous single-layer graphene on an insulating substrate, it is characterised in that: step
1) in, method using magnetron sputtering is in depositing germanium film in the insulating substrate.
4. the method according to claim 1 for preparing continuous single-layer graphene on an insulating substrate, it is characterised in that: step
1) in, the thickness range of the germanium film of deposition is 10~500nm.
5. the method according to claim 1 for preparing continuous single-layer graphene on an insulating substrate, it is characterised in that: step
2) in, graphene is grown in the germanium film surface using gaseous carbon source as raw material.
6. the method according to claim 5 for preparing continuous single-layer graphene on an insulating substrate, it is characterised in that: described
Gaseous carbon source includes the combination of one or more of methane, acetylene, ethylene.
7. the method according to claim 1 for preparing continuous single-layer graphene on an insulating substrate, it is characterised in that: step
2) in, graphene is grown in the germanium film surface using chemical vapour deposition technique.
8. the method according to claim 1 for preparing continuous single-layer graphene on an insulating substrate, it is characterised in that: step
2) in, the retention time of the high temperature is at least more than the time that the germanium film all evaporates, the retention time model of the high temperature
It encloses for 30~300min.
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| CN107500277B (en) * | 2017-09-27 | 2019-12-24 | 中国科学院上海微系统与信息技术研究所 | Graphene boundary regulation and control method |
| CN109055896B (en) * | 2018-07-20 | 2021-08-20 | 中国科学院上海微系统与信息技术研究所 | Method for directly preparing graphene on insulating substrate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557017A (en) * | 2010-12-07 | 2012-07-11 | 三星电子株式会社 | Graphene structure and method of fabricating the same |
| CN105060286A (en) * | 2015-08-26 | 2015-11-18 | 中国科学院上海微系统与信息技术研究所 | Preparation method of corrugated graphene |
| CN105129785A (en) * | 2015-08-26 | 2015-12-09 | 中国科学院上海微系统与信息技术研究所 | Preparation method of graphene on insulator |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557017A (en) * | 2010-12-07 | 2012-07-11 | 三星电子株式会社 | Graphene structure and method of fabricating the same |
| CN105060286A (en) * | 2015-08-26 | 2015-11-18 | 中国科学院上海微系统与信息技术研究所 | Preparation method of corrugated graphene |
| CN105129785A (en) * | 2015-08-26 | 2015-12-09 | 中国科学院上海微系统与信息技术研究所 | Preparation method of graphene on insulator |
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