CN105129785A - Preparation method of graphene on insulator - Google Patents
Preparation method of graphene on insulator Download PDFInfo
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- CN105129785A CN105129785A CN201510532114.5A CN201510532114A CN105129785A CN 105129785 A CN105129785 A CN 105129785A CN 201510532114 A CN201510532114 A CN 201510532114A CN 105129785 A CN105129785 A CN 105129785A
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Abstract
The invention provides a preparation method of graphene on an insulator. The preparation method comprises the following steps: providing a germanium catalyst substrate, placing the germanium catalyst substrate in a growth chamber, introducing hydrogenous atmosphere to form a Ge-H key on the surface of the germanium catalyst substrate; heating the catalyst substrate to a preset temperature, introducing a carbon source and growing on the surface of the germanium catalyst substrate to obtain graphene; providing an insulation substrate, bonding one surface, formed with the graphene, of the germanium catalyst substrate with the insulation substrate to obtain a bonding pad; performing microwave treatment of the bonding pad to break the Ge-H key, generating hydrogen to peel off the graphene from the germanium catalyst substrate, transiting to the surface of the insulation substrate to obtain the graphene on the insulator. According to the preparation method, a wet process reaction is not needed, the introduction of defects is reduced, and during the transition process, a carrier is supported all the time, so that the completeness of the graphene is maintained to the maximum extent, and the preparation method is beneficial to obtain the graphene with large size and high quality on the insulator.
Description
Technical field
The invention belongs to low-dimensional materials and field of new, relate to the preparation method of Graphene on a kind of isolator.
Background technology
Since the method discovery Graphene that two scientists of Univ Manchester UK in 2004 use micromechanics to peel off, the appearance of Graphene has evoked huge great waves.Graphene, the i.e. monoatomic layer of graphite are the two-dirnentional structure of carbon atom by honeycomb arrangement.Graphene is in impayable advantages of aspect of performance such as physics, chemistry, mechanics, especially outstanding with electrology characteristic, has the feature of three most advantages: transparent, pliable and tough, electroconductibility is strong, has even presented the trend of Graphene substituted for silicon.
The graphene preparation method of the routine of current development has: micromechanics stripping, pyrolytic silicon carbide (SiC), chemical vapour deposition (CVD) on transition metal and heavy metal and chemical graft oxidation style.Micromechanics stripping method can prepare high-quality Graphene, but the Graphene area that at present prepared by this method is less than 1mm × 1mm, can only be used for Basic Experiment Study; Graphene prepared by SiC subliming method is very large by the impact of substrate, and number of plies heterogeneity, cannot carry out substrate-transfer; CVD is a kind of method being suitable for preparing big area, high quality, continuous graphite alkene film.
Current CVD method mainly prepares Graphene on transition metal.In order to meet different application demand needs, the Graphene of preparation is transferred in corresponding insulating substrate after graphene growth completes.On isolator, Graphene shows huge application potential in transistor of future generation, nesa coating, sensor field
The transfer process of Graphene itself is a complexity and the process of high cost, and this is very disadvantageous for scale of mass production; In transfer process, defect and impurity are introduced inevitable simultaneously, and this greatly reduces Graphene quality, is unfavorable for the application of Graphene on isolator.Desirable transfer techniques should have following features: 1) guarantee that the graphene-structured after shifting is complete, harmless; 2) pollution-free to Graphene in transfer process; 3) process stabilizing, has repeatability.
Therefore, how to provide the preparation method of Graphene on a kind of isolator, to reduce breakage and the defect of Graphene, obtain Graphene on high-quality isolator, become the important technological problems that those skilled in the art are urgently to be resolved hurrily.
Summary of the invention
The shortcoming of prior art in view of the above, the object of the present invention is to provide the preparation method of Graphene on a kind of isolator, be transferred to insulating substrate for solving Graphene in prior art, Graphene can be damaged in various degree, causes the problem that Graphene on isolator is of low quality.
For achieving the above object and other relevant objects, the invention provides the preparation method of Graphene on a kind of isolator, comprising:
One germanium catalytic substrate is provided; Described germanium catalytic substrate is put into growth chamber, in described growth chamber, passes into hydrogeneous atmosphere, to form Ge-H key on described germanium catalytic substrate surface;
Described catalytic substrate is heated to preset temp, and passes into carbon source in described growth chamber, obtain Graphene in the surface growth of described germanium catalytic substrate;
One insulating substrate is provided, described germanium catalytic substrate is formed with the one side of Graphene and described insulating substrate bonding, obtains the bonding pad be formed by stacking by insulating substrate, Graphene and germanium catalytic substrate successively from bottom to top;
Bonding pad described in microwave treatment, to make described Ge-H bond rupture, generates hydrogen, described Graphene is peeled off from described germanium catalytic substrate, is transferred to described insulated substrate surface, obtains Graphene on isolator.
Alternatively, described insulating substrate comprises silicon-dioxide, silicon nitride, sapphire, silicon carbide, strontium titanate, glass, hafnia, polyethylene terephthalate, polyimide or polyimide based resin.
Alternatively, described hydrogeneous atmosphere is the gas mixture of hydrogen and argon gas.
Alternatively, the scope of described preset temp is 800 ~ 920 DEG C.
Alternatively, described carbon source comprises at least one in methane, ethene, acetylene, benzene and PMMA.
Alternatively, the material at the bottom of described bonding radical comprises Si, SiGe or III-V material.
Alternatively, bonding pad described in microwave treatment under non-oxidizable protective atmosphere.
Alternatively, described non-oxide protective atmosphere comprises at least one in argon gas and nitrogen.
Alternatively, the temperature range of bonding pad described in microwave treatment is 100 ~ 300 DEG C.
Alternatively, before bonding, nitrogen plasma treatment is carried out to the face to be bonded of described insulating substrate.
Alternatively, before bonding, nitrogen plasma treatment is carried out to described graphenic surface.
Alternatively, described Graphene is gone out by thermal chemical vapor deposition method, Low Pressure Chemical Vapor Deposition or plasma reinforced chemical vapour deposition method in the surface growth of described germanium catalytic substrate.
Alternatively, described Graphene is single-layer graphene.
As mentioned above, the preparation method of Graphene on isolator of the present invention, there is following beneficial effect: the present invention, by described germanium catalytic substrate being formed with the one side of Graphene and described insulating substrate bonding, obtains the bonding pad be formed by stacking by insulating substrate, Graphene and germanium catalytic substrate successively from bottom to top; And by bonding pad described in microwave treatment, wherein, microwave treatment has the feature of high-efficiency heating, be a kind of inner overall heating, have fast, simply, all even efficient feature, described Ge-H bond rupture can be made, generate hydrogen, described Graphene is peeled off from described germanium catalytic substrate, is transferred to described insulated substrate surface, obtains Graphene on isolator.On isolator of the present invention, the preparation method of Graphene is without the need to through Wet Method Reaction process, decrease the introducing of defect, and have carrier supported all the time in Graphene transfer process, at utmost remain the integrity of Graphene, be conducive to obtaining Graphene on large-sized isolator.Graphene is peeled off rear remaining described germanium catalytic substrate and can be reused, and is conducive to saving material, more environmental protection.
Accompanying drawing explanation
Fig. 1 is shown as the process flow sheet of the preparation method of Graphene on isolator of the present invention.
Fig. 2 is shown as the schematic diagram of preparation method at germanium catalytic substrate surface formation Ge-H key of Graphene on isolator of the present invention.
The preparation method that Fig. 3 is shown as Graphene on isolator of the present invention obtains the schematic diagram of Graphene in the surface growth of germanium catalytic substrate.
Germanium catalytic substrate is formed with the one side of Graphene and the schematic diagram of insulating substrate bonding by the preparation method that Fig. 4 is shown as Graphene on isolator of the present invention.
Fig. 5 is shown as the schematic diagram of preparation method's microwave treatment bonding pad of Graphene on isolator of the present invention.
The schematic diagram that germanium catalytic substrate is taken off by the preparation method that Fig. 6 is shown as Graphene on isolator of the present invention.
The schematic diagram of Graphene on the isolator that the preparation method that Fig. 7 is shown as Graphene on isolator of the present invention obtains.
Element numbers explanation
S1 ~ S4 step
1 germanium catalytic substrate
2Ge-H key
3 Graphenes
4 insulating substrate
Embodiment
Below by way of specific specific examples, embodiments of the present invention are described, those skilled in the art the content disclosed by this specification sheets can understand other advantages of the present invention and effect easily.The present invention can also be implemented or be applied by embodiments different in addition, and the every details in this specification sheets also can based on different viewpoints and application, carries out various modification or change not deviating under spirit of the present invention.
Refer to Fig. 1 to Fig. 7.It should be noted that, the diagram provided in the present embodiment only illustrates basic conception of the present invention in a schematic way, then only the assembly relevant with the present invention is shown in graphic but not component count, shape and size when implementing according to reality is drawn, it is actual when implementing, and the kenel of each assembly, quantity and ratio can be a kind of change arbitrarily, and its assembly layout kenel also may be more complicated.
The invention provides the preparation method of Graphene on a kind of isolator, refer to Fig. 1, be shown as the process flow sheet of the method, comprise the steps:
S1: a germanium catalytic substrate is provided; Described germanium catalytic substrate is put into growth chamber, in described growth chamber, passes into hydrogeneous atmosphere, to form Ge-H key on described germanium catalytic substrate surface;
S2: described catalytic substrate is heated to preset temp, and carbon source is passed in described growth chamber, obtain Graphene in the surface growth of described germanium catalytic substrate;
S3: provide an insulating substrate, is formed with the one side of Graphene and described insulating substrate bonding, obtains the bonding pad be formed by stacking by insulating substrate, Graphene and germanium catalytic substrate successively from bottom to top by described germanium catalytic substrate;
S4: bonding pad described in microwave treatment, to make described Ge-H bond rupture, generates hydrogen, described Graphene is peeled off from described germanium catalytic substrate, is transferred to described insulated substrate surface, obtains Graphene on isolator.
First refer to Fig. 2, perform step S1: provide a germanium catalytic substrate 1; Described germanium catalytic substrate 1 is put into growth chamber, in described growth chamber, passes into hydrogeneous atmosphere, to form Ge-H key 2 on described germanium catalytic substrate 1 surface.
Concrete, described germanium catalytic substrate 1 refers to that surface has the substrate of Ge material, to include but not limited on body germanium, germanium on insulator, body silicon in epitaxial Germanium or III-V material epitaxial Germanium etc.Exemplarily, described germanium catalytic substrate 1 adopts germanium wafer.Before described germanium catalytic substrate 1 is put into growth chamber, conventional clean can be carried out to described germanium catalytic substrate 1.
Described hydrogeneous atmosphere preferably adopts the gas mixture of hydrogen and argon gas, its effect mainly contains four aspects: (1) is warming up in the process of graphene growth temperature in follow-up described germanium catalytic substrate, the reaction on hydrogen and germanium catalytic substrate surface, forms described Ge-H key 2; (2) as the carrier gas of subsequent chemistry vapour deposition process growing graphene, promote the growth of Graphene, reduce Graphene defect; (3) in growth chamber, form hydrogen saturation pressure, make germanium catalytic substrate in intensification and graphene growth process, surface is formed with Ge-H key all the time; (4) zone of oxidation and other impurity on germanium catalytic substrate surface is removed, for graphene growth provides clean surface.
Then refer to Fig. 3, perform step S2: described catalytic substrate 1 is heated to preset temp, and passes into carbon source in described growth chamber, obtain Graphene 3 in the surface growth of described germanium catalytic substrate 1.
Concrete, the method obtaining Graphene 3 in the surface growth of described germanium catalytic substrate 1 is chemical Vapor deposition process, includes but not limited to thermal chemical vapor deposition method, Low Pressure Chemical Vapor Deposition or plasma reinforced chemical vapour deposition method etc.Described Graphene 3 is single-layer graphene, a kind of Two-dimensional Carbon material be namely made up of with the closelypacked carbon atom of benzene ring structure (i.e. hexagonal honeycomb structure) periodicity one deck.
Exemplarily, using tube furnace as described growth chamber, graphene growth temperature is 800 ~ 920 DEG C, and hydrogen flowing quantity is 2 ~ 100sccm, carbon source flow 0.01 ~ 50sccm, graphene growth time 1 ~ 1000min.Described carbon source can be gaseous state, liquid state or solid-state carbon source, includes but not limited at least one in methane, ethene, acetylene, benzene and PMMA.Adopt the technology of chemical Vapor deposition process growing graphene to be well known to those skilled in the art, in other embodiments, also can adopt other processing condition according to actual needs, should too not limit the scope of the invention herein.
It is pointed out that in graphene growth process, even if part Ge-H bond rupture, also supply can be obtained immediately from described hydrogeneous atmosphere, regenerate Ge-H key, as shown in Figure 3, final described Graphene 3 is formed at the layer of hydrogen atoms surface of described germanium catalytic substrate 1.
Refer to Fig. 4 again, perform step S3: provide an insulating substrate 4, described germanium catalytic substrate 1 is formed with the one side of Graphene 3 and described insulating substrate 4 bonding, obtains the bonding pad be formed by stacking by insulating substrate 4, Graphene 3 and germanium catalytic substrate 1 successively from bottom to top.
Concrete, described insulating substrate 4 can be the insulating substrate that semiconductor applications is conventional, such as silicon-dioxide, silicon nitride, sapphire, silicon carbide, strontium titanate, glass or hafnia etc.Described insulating substrate can be also flexible substrate, includes but not limited to high temperature resistant (more than the 100 DEG C) flexible materialss such as polyethylene terephthalate, polyimide or polyimide based resin.Can doping be had in described insulating substrate 4, also can be formed with device cell, should too not limit the scope of the invention herein.
Before bonding, nitrogen plasma treatment can be carried out to the face to be bonded of described insulating substrate, to remove its surface impurity, strengthen bonding performance.Also can carry out nitrogen plasma treatment to described graphenic surface simultaneously, adopt suitable power, nitrogen gas plasma can not injure graphenic surface while removal dirt.
Finally refer to Fig. 5 to Fig. 7, perform step S4: bonding pad described in microwave treatment, to make described Ge-H bond rupture, generate hydrogen, described Graphene 3 is peeled off from described germanium catalytic substrate 1, is transferred to described insulating substrate 4 surface, obtains Graphene on isolator.
Microwave annealing, as the novel annealing way of one, has the characteristic of high-efficiency heating, fast, simply, all efficiently even, and microwave annealing is a kind of inner overall heating, can make to be heated with being heated system uniform high-efficiency within very short time.For bonding pad of the present invention, Ge-H bond rupture after microwave treatment heating, generates a large amount of hydrogen (as shown in Figure 5), described Graphene 3 is peeled off from described germanium catalytic substrate 1, is transferred to described insulating substrate 4 surface.As shown in Figure 6, lift described germanium catalytic substrate 1, Graphene on isolator as shown in Figure 7 can be obtained.
Concrete, can under non-oxidizable protective atmosphere bonding pad described in microwave treatment, react to avoid oxygen and Graphene.Exemplarily, described non-oxide protective atmosphere comprises at least one in argon gas and nitrogen.During microwave treatment, the air pressure around bonding pad can be normal pressure.Owing to not having hydrogen supply, the hydrogen that Ge-H bond rupture generates directly is run away, and Ge catalytic substrate surface also can not regenerate Ge-H key.
In addition, due to the high efficiency of microwave heating, treatment temp does not need too high, in the present embodiment, the temperature range of bonding pad described in microwave treatment is 100 ~ 300 DEG C, is preferably 150 DEG C, at such a temperature, not only can make the effective desorption of Graphene, also can not damage Graphene because of heating.
Because Graphene is directly transferred to described insulating substrate from described germanium catalytic substrate, all the time carrier supported is had in transfer process, thus at utmost remain the integrity of Graphene, be particularly conducive to and obtain Graphene on large-sized isolator, such as, on the isolator of wafer scale Graphene.
The germanium catalytic substrate stayed after Graphene desorption can be reused, and loss is (mainly because of the loss of surface oxidation generation) seldom, therefore greatly can save material, reduce costs, and more environmental protection.
So far, by the preparation method of Graphene on isolator of the present invention, epontic for germanium catalytic substrate Graphene high quality is transferred to insulated substrate surface, on the isolator obtained, Graphene all has a good application prospect in unicircuit, LED, nesa coating, sensor field.
In sum, on isolator of the present invention, the preparation method of Graphene is by being formed with the one side of Graphene and described insulating substrate bonding by described germanium catalytic substrate, obtains the bonding pad be formed by stacking by insulating substrate, Graphene and germanium catalytic substrate successively from bottom to top; And by bonding pad described in microwave treatment, wherein, microwave treatment has the feature of high-efficiency heating, be a kind of inner overall heating, have fast, simply, all even efficient feature, described Ge-H bond rupture can be made, generate hydrogen, described Graphene is peeled off from described germanium catalytic substrate, is transferred to described insulated substrate surface, obtains Graphene on isolator.On isolator of the present invention, the preparation method of Graphene is without the need to through Wet Method Reaction process, decrease the introducing of defect, and have carrier supported all the time in Graphene transfer process, at utmost remain the integrity of Graphene, be conducive to obtaining Graphene on large-sized isolator.Graphene is peeled off rear remaining described germanium catalytic substrate and can be reused, and is conducive to saving material, more environmental protection.So the present invention effectively overcomes various shortcoming of the prior art and tool high industrial utilization.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (13)
1. the preparation method of Graphene on isolator, is characterized in that, comprising:
One germanium catalytic substrate is provided; Described germanium catalytic substrate is put into growth chamber, in described growth chamber, passes into hydrogeneous atmosphere, to form Ge-H key on described germanium catalytic substrate surface;
Described catalytic substrate is heated to preset temp, and passes into carbon source in described growth chamber, obtain Graphene in the surface growth of described germanium catalytic substrate;
One insulating substrate is provided, described germanium catalytic substrate is formed with the one side of Graphene and described insulating substrate bonding, obtains the bonding pad be formed by stacking by insulating substrate, Graphene and germanium catalytic substrate successively from bottom to top;
Bonding pad described in microwave treatment, to make described Ge-H bond rupture, generates hydrogen, described Graphene is peeled off from described germanium catalytic substrate, is transferred to described insulated substrate surface, obtains Graphene on isolator.
2. the preparation method of Graphene on isolator according to claim 1, is characterized in that: described insulating substrate comprises silicon-dioxide, silicon nitride, sapphire, silicon carbide, strontium titanate, glass, hafnia, polyethylene terephthalate, polyimide or polyimide based resin.
3. the preparation method of Graphene on isolator according to claim 1, is characterized in that: described hydrogeneous atmosphere is the gas mixture of hydrogen and argon gas.
4. the preparation method of Graphene on isolator according to claim 1, is characterized in that: the scope of described preset temp is 800 ~ 920 DEG C.
5. the preparation method of Graphene on isolator according to claim 1, is characterized in that: described carbon source comprises at least one in methane, ethene, acetylene, benzene and PMMA.
6. the preparation method of Graphene on isolator according to claim 1, is characterized in that: the material at the bottom of described bonding radical comprises Si, SiGe or III-V material.
7. the preparation method of Graphene on isolator according to claim 1, is characterized in that: bonding pad described in microwave treatment under non-oxidizable protective atmosphere.
8. the preparation method of Graphene on isolator according to claim 7, is characterized in that: described non-oxide protective atmosphere comprises at least one in argon gas and nitrogen.
9. the preparation method of Graphene on isolator according to claim 1, is characterized in that: the temperature range of bonding pad described in microwave treatment is 100 ~ 300 DEG C.
10. the preparation method of Graphene on isolator according to claim 1, is characterized in that: before bonding, carries out nitrogen plasma treatment to the face to be bonded of described insulating substrate.
On 11. isolators according to claim 10, the preparation method of Graphene, is characterized in that: before bonding, carries out nitrogen plasma treatment to described graphenic surface.
The preparation method of Graphene on 12. isolators according to claim 1, is characterized in that: go out described Graphene by thermal chemical vapor deposition method, Low Pressure Chemical Vapor Deposition or plasma reinforced chemical vapour deposition method in the surface growth of described germanium catalytic substrate.
The preparation method of Graphene on 13. isolators according to claim 1, is characterized in that: described Graphene is single-layer graphene.
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| CN106904600A (en) * | 2015-12-17 | 2017-06-30 | 中国科学院上海微***与信息技术研究所 | A kind of method for preparing continuous single-layer graphene on an insulating substrate |
| CN106904599A (en) * | 2015-12-17 | 2017-06-30 | 中国科学院上海微***与信息技术研究所 | A kind of method for preparing figure Graphene on an insulating substrate |
| CN109055895A (en) * | 2018-07-20 | 2018-12-21 | 中国科学院上海微***与信息技术研究所 | The method of graphene quantum lattice array is directly prepared on an insulating substrate |
| CN109879275A (en) * | 2019-01-30 | 2019-06-14 | 宁波大学 | A kind of method that the concentration of combination germanium prepares graphene with ion implantation technique |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106904600A (en) * | 2015-12-17 | 2017-06-30 | 中国科学院上海微***与信息技术研究所 | A kind of method for preparing continuous single-layer graphene on an insulating substrate |
| CN106904599A (en) * | 2015-12-17 | 2017-06-30 | 中国科学院上海微***与信息技术研究所 | A kind of method for preparing figure Graphene on an insulating substrate |
| CN106904599B (en) * | 2015-12-17 | 2019-03-01 | 中国科学院上海微***与信息技术研究所 | A method of preparing figure graphene on an insulating substrate |
| CN106904600B (en) * | 2015-12-17 | 2019-03-01 | 中国科学院上海微***与信息技术研究所 | A method of preparing continuous single-layer graphene on an insulating substrate |
| CN109055895A (en) * | 2018-07-20 | 2018-12-21 | 中国科学院上海微***与信息技术研究所 | The method of graphene quantum lattice array is directly prepared on an insulating substrate |
| CN109055895B (en) * | 2018-07-20 | 2020-09-15 | 中国科学院上海微***与信息技术研究所 | Method for directly preparing graphene quantum dot array on insulating substrate |
| CN109879275A (en) * | 2019-01-30 | 2019-06-14 | 宁波大学 | A kind of method that the concentration of combination germanium prepares graphene with ion implantation technique |
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