CN104681801A - Graphene/Cu/Ni composite electrode and preparation method thereof - Google Patents
Graphene/Cu/Ni composite electrode and preparation method thereof Download PDFInfo
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- CN104681801A CN104681801A CN201510094943.XA CN201510094943A CN104681801A CN 104681801 A CN104681801 A CN 104681801A CN 201510094943 A CN201510094943 A CN 201510094943A CN 104681801 A CN104681801 A CN 104681801A
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Abstract
The invention discloses a graphene/Cu/Ni composite electrode and a preparation method thereof. The composite electrode comprises a Cu/Ni alloy layer and a graphene film covering the Cu/Ni alloy layer, wherein the Cu/Ni alloy layer is formed by mutual diffusion of Ni atoms and Cu atoms of an Ni film and a Cu film covering the Ni film, and the thickness ratio of the Ni film to the Cu film is in a range of 1:(3-10). According to the graphene/Cu/Ni composite electrode and the preparation method thereof, damage caused by a graphene transfer process and a graphical process to the quality of graphene is avoided, the number of graphene defects is decreased, thicknesses of the Ni film and the Cu film are adjusted, a temperature-gradient CVD (chemical vapor deposition) technology is adopted, the high-quality graphene is obtained, the protection capability of the graphene to a Cu/Ni alloy is enhanced, and the obtained composite electrode has the excellent corrosion resistance.
Description
Technical field
The invention belongs to metal electrode resist technology field, more specifically, relate to a kind of Graphene/Cu/Ni combination electrode and preparation method thereof.
Background technology
Cu/Ni composition metal is easy to plastotype, processing and welding, is widely used in the device such as metal interconnected, aircraft component, implanted device as electrode.Graphene is a kind of two-dimentional monoatomic layer material, is widely used, especially its good chemical stability because of its outstanding machinery, optics, electricity, chemical stability etc., can be used as anticorrosive to protect Cu/Ni clad metal electrode.
But research shows the phenomenon that serious corrosion lower metal can occur at the fault location of Graphene, and high-quality, flawless single-layer graphene can reduce the generation of corrosion phenomenon effectively.At present, CVD technology is often adopted to prepare large area, high-quality Graphene.With single transition metal (Cu, Ni etc.) for catalyst, take hydrocarbon compound as carbon source, deposit growing graphene; Then the graphene film of growth is transferred in target substrate, through steps such as graphical treatment, carries out the application of device.But the quality of complicated, destructive Graphene transfer and patterning process meeting grievous injury Graphene, causes unnecessary defect, affects the application of Graphene in metal electrode is anticorrosion.
Summary of the invention
For above defect or the Improvement requirement of prior art; the invention provides a kind of Graphene/Cu/Ni combination electrode and preparation method thereof; avoid Graphene transfer process and patterning process to the destruction of Graphene quality; decrease the number of Graphene defect; by adjusting the thickness of Ni film and Cu film, adopting the CVD technique of temperature-gradient method, obtaining high-quality Graphene; enhance the protective capability of Graphene to Cu/Ni alloy, the combination electrode obtained has excellent corrosion resistance.
For achieving the above object, according to one aspect of the present invention, provide a kind of Graphene/Cu/Ni combination electrode, it is characterized in that, comprise Cu/Ni alloy-layer and cover the graphene film on described Cu/Ni alloy-layer; Wherein, described Cu/Ni alloy-layer is by Ni film and cover Cu film on described Ni film mutually diffuseing to form of Ni atom and Cu atom occurs, and the Thickness Ratio of described Ni film and described Cu film is 1:(3 ~ 10).
Preferably, described Cu/Ni alloy-layer and described graphene film are patterned structures.
According to another aspect of the present invention, provide the preparation method of a kind of Graphene/Cu/Ni combination electrode, it is characterized in that, comprise the steps:
(1) deposit layer of Ni film in substrate, then on Ni film deposit one deck Cu film, obtain the substrate of Cu/Ni composition metal; Wherein, the Thickness Ratio of Ni film and Cu film is 1:(3 ~ 10);
(2) CVD method is utilized, growing graphene film in the substrate of Cu/Ni composition metal;
Described step (2) comprises the steps: further
(A1) at Ar and H
2mixed atmosphere in, be warming up to 400 DEG C ~ 800 DEG C, and be incubated 3h ~ 5h;
(A2) continue to be warming up to 1000 DEG C ~ 1050 DEG C;
(A3) hydrocarbon is passed into as carbon source, insulation 15min ~ 30min;
(A4) at Ar and H
2mixed atmosphere in, be cooled to room temperature.
According to another aspect of the present invention, provide the preparation method of a kind of Graphene/Cu/Ni combination electrode, it is characterized in that, comprise the steps:
(1) in substrate, patterned photoresist is prepared;
(2) deposit layer of Ni film, then on Ni film deposit one deck Cu film; Wherein, the Thickness Ratio of Ni film and Cu film is 1:(3 ~ 10);
(3) remove photoresist, obtain patterned Cu film and Ni film;
(4) CVD method is utilized, growing graphene film on patterned Cu film;
Described step (4) comprises the steps: further
(A1) at Ar and H
2mixed atmosphere in, be warming up to 400 DEG C ~ 800 DEG C, and be incubated 3h ~ 5h;
(A2) continue to be warming up to 1000 DEG C ~ 1050 DEG C;
(A3) hydrocarbon is passed into as carbon source, insulation 15min ~ 30min;
(A4) at Ar and H
2mixed atmosphere in, be cooled to room temperature.
In general, the above technical scheme conceived by the present invention compared with prior art, has following beneficial effect:
1, direct growing graphene on metal, achieves growth in situ and the application of single-layer graphene, avoids the destruction of Graphene transfer process to Graphene quality, decrease the number of Graphene defect, enhance the protective capability to Cu/Ni alloy.
2, the Ni atom in composition metal at high temperature with the counterdiffusion of Cu atom phase; serve smooth metallic substrate surface; increase the effect of crystallite dimension; be conducive to the growth of individual layer, zero defect Graphene; by adjusting the thickness of Ni film and Cu film; can high-quality Graphene be obtained, to lower metal, there is better protected effect.
3, growing patterned single-layer graphene, avoids Graphene patterning process in device application to the destruction of Graphene quality, decreases the number of Graphene defect, enhance the protective capability to Cu/Ni alloy.
4, utilize the CVD technique growing graphene of temperature-gradient method, decrease the destruction of high temperature to Cu/Ni alloy, and further increase the growth quality of Graphene.
Accompanying drawing explanation
Fig. 1 is preparation technology's schematic flow sheet of the Graphene/Cu/Ni combination electrode of one embodiment of the invention;
Fig. 2 is preparation technology's schematic flow sheet of the Graphene/Cu/Ni combination electrode of another embodiment of the present invention;
Fig. 3 is the Raman spectrogram of the Graphene that embodiment 6 grows;
Fig. 4 is the SEM figure of the Graphene that embodiment 6 grows.
In all of the figs, identical Reference numeral is used for representing identical element or structure, wherein: 1-substrate, and 2-photoresist, 3-Ni film, 4-Cu film, 5-graphene film.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.In addition, if below in described each execution mode of the present invention involved technical characteristic do not form conflict each other and just can mutually combine.
Graphene/Cu/Ni the combination electrode of the embodiment of the present invention comprises Cu/Ni alloy-layer and covers the graphene film on Cu/Ni alloy-layer; Wherein, Cu/Ni alloy-layer is by Ni film and cover Cu film on Ni film mutually diffuseing to form of Ni atom and Cu atom occurs, and the Thickness Ratio of Ni film and Cu film is 1:(3 ~ 10).Preferably, Cu/Ni alloy-layer and graphene film are patterned structures.
As shown in Figure 1, the preparation method of the Graphene/Cu/Ni combination electrode of one embodiment of the invention comprises the steps:
(1) film of deposit layer of Ni on the base 13, then on Ni film 3 deposit one deck Cu film 4, obtain the substrate of Cu/Ni composition metal.
Wherein, substrate can be Si, glass etc. usually.
Preferably, the Thickness Ratio of Ni film and Cu film is 1:(3 ~ 10).
(2) CVD method is utilized, growing graphene film 5 in the substrate of Cu/Ni composition metal.
Step (2) comprises the steps: further
(A1) at Ar and H
2mixed atmosphere in, be warming up to 400 DEG C ~ 800 DEG C, and be incubated 3h ~ 5h.
(A2) continue to be warming up to 1000 DEG C ~ 1050 DEG C.
(A3) hydrocarbon is passed into as carbon source, insulation 15min ~ 30min.
Wherein, hydrocarbon can be CH usually
4, C
2h
4deng.
(A4) at Ar and H
2mixed atmosphere in, be cooled to room temperature.
As shown in Figure 2, the preparation method of the Graphene/Cu/Ni combination electrode of another embodiment of the present invention comprises the steps:
(1) patterned photoresist 2 is prepared on the base 1.
(2) deposit layer of Ni film 3, then on Ni film 3 deposit one deck Cu film 4.
Wherein, substrate can be Si, glass etc. usually.
Preferably, the Thickness Ratio of Ni film and Cu film is 1:(3 ~ 10).
(3) remove photoresist, obtain patterned Cu film and Ni film.
(4) CVD method is utilized, growing graphene film 5 on patterned Cu film.
Step (4) comprises the steps: further
(A1) at Ar and H
2mixed atmosphere in, be warming up to 400 DEG C ~ 800 DEG C, and be incubated 3h ~ 5h.
(A2) continue to be warming up to 1000 DEG C ~ 1050 DEG C.
(A3) hydrocarbon is passed into as carbon source, insulation 15min ~ 30min.
Wherein, hydrocarbon can be CH usually
4, C
2h
4deng.
(A4) at Ar and H
2mixed atmosphere in, be cooled to room temperature.
For making those skilled in the art understand the present invention better, below in conjunction with specific embodiment, the preparation method of Graphene of the present invention/Cu/Ni combination electrode is described in detail.
Embodiment 1
The Ni film that sputtering deposit one deck 300nm is thick in Si substrate, then on Ni film, sputter the thick Cu film of one deck 900nm (Thickness Ratio of Ni film and Cu film is 1:3), obtain the substrate of Cu/Ni composition metal; By the substrate of Cu/Ni composition metal at Ar and H
2mixed atmosphere in, be warming up to 400 DEG C and be incubated 5h, continuing to be warming up to 1000 DEG C, pass into CH
4as carbon source, insulation 30min, finally at Ar and H
2mixed atmosphere in, be cooled to room temperature, thus in the substrate of Cu/Ni composition metal growing graphene film.
Embodiment 2
The Ni film that sputtering deposit one deck 100nm is thick in Si substrate, then on Ni film, sputter the thick Cu film of one deck 1 μm (Thickness Ratio of Ni film and Cu film is 1:10), obtain the substrate of Cu/Ni composition metal; By the substrate of Cu/Ni composition metal at Ar and H
2mixed atmosphere in, be warming up to 800 DEG C and be incubated 3h, continuing to be warming up to 1050 DEG C, pass into CH
4as carbon source, insulation 15min, finally at Ar and H
2mixed atmosphere in, be cooled to room temperature, thus in the substrate of Cu/Ni composition metal growing graphene film.
Embodiment 3
The Ni film that sputtering deposit one deck 200nm is thick in Si substrate, then on Ni film, sputter the thick Cu film of one deck 900nm (Thickness Ratio of Ni film and Cu film is 1:4.5), obtain the substrate of Cu/Ni composition metal; By the substrate of Cu/Ni composition metal at Ar and H
2mixed atmosphere in, be warming up to 600 DEG C and be incubated 4h, continuing to be warming up to 1020 DEG C, pass into CH
4as carbon source, insulation 25min, finally at Ar and H
2mixed atmosphere in, be cooled to room temperature, thus in the substrate of Cu/Ni composition metal growing graphene film.
Embodiment 4
Patterned photoresist is prepared in Si substrate, then sputters the thick Ni film of one deck 300nm, then on Ni film, sputter the thick Cu film of one deck 900nm (Thickness Ratio of Ni film and Cu film is 1:3); Remove photoresist, obtain patterned Cu film and Ni film; By substrate at Ar and H
2mixed atmosphere in, be warming up to 400 DEG C and be incubated 5h, continuing to be warming up to 1000 DEG C, pass into CH
4as carbon source, insulation 30min, finally at Ar and H
2mixed atmosphere in, be cooled to room temperature, thus on patterned Cu film growing graphene film.
Embodiment 5
Patterned photoresist is prepared in Si substrate, then sputters the thick Ni film of one deck 100nm, then on Ni film, sputter the thick Cu film of one deck 1 μm (Thickness Ratio of Ni film and Cu film is 1:10); Remove photoresist, obtain patterned Cu film and Ni film; By substrate at Ar and H
2mixed atmosphere in, be warming up to 800 DEG C and be incubated 3h, continuing to be warming up to 1050 DEG C, pass into CH
4as carbon source, insulation 15min, finally at Ar and H
2mixed atmosphere in, be cooled to room temperature, thus on patterned Cu film growing graphene film.
Embodiment 6
Patterned photoresist is prepared in Si substrate, then sputters the thick Ni film of one deck 200nm, then on Ni film, sputter the thick Cu film of one deck 900nm (Thickness Ratio of Ni film and Cu film is 1:4.5); Remove photoresist, obtain patterned Cu film and Ni film; By substrate at Ar and H
2mixed atmosphere in, be warming up to 600 DEG C and be incubated 4h, continuing to be warming up to 1020 DEG C, pass into CH
4as carbon source, insulation 25min, finally at Ar and H
2mixed atmosphere in, be cooled to room temperature, thus on patterned Cu film growing graphene film.
Test Raman spectrogram and the SEM figure of the Graphene of above-described embodiment growth respectively; result shows; method of the present invention can grow individual layer, flawless graphene film; thus have better protected effect to the Cu/Ni alloy-layer of lower floor, the Graphene obtained/Cu/Ni combination electrode has excellent corrosion resistance.For the Raman spectrogram that embodiment 6, Fig. 3 is the Graphene that embodiment 6 grows, wherein, the ratio I of the intensity at 2D peak and G peak
2D/ I
g>1, illustrates that Graphene is individual layer; And the intensity representing the D peak of Graphene defect counts is zero, illustrates that the defect of Graphene is few.Fig. 4 is the SEM figure of the Graphene that embodiment 6 grows, and can find out that individual layer continuous print Graphene grows on Cu film.
Those skilled in the art will readily understand; the foregoing is only preferred embodiment of the present invention; not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (4)
1. Graphene/Cu/Ni combination electrode, is characterized in that, comprises Cu/Ni alloy-layer and covers the graphene film on described Cu/Ni alloy-layer; Wherein, described Cu/Ni alloy-layer is by Ni film and cover Cu film on described Ni film mutually diffuseing to form of Ni atom and Cu atom occurs, and the Thickness Ratio of described Ni film and described Cu film is 1:(3 ~ 10).
2. Graphene/Cu/Ni combination electrode as claimed in claim 1, it is characterized in that, described Cu/Ni alloy-layer and described graphene film are patterned structures.
3. a preparation method for Graphene/Cu/Ni combination electrode, is characterized in that, comprise the steps:
(1) deposit layer of Ni film in substrate, then on Ni film deposit one deck Cu film, obtain the substrate of Cu/Ni composition metal; Wherein, the Thickness Ratio of Ni film and Cu film is 1:(3 ~ 10);
(2) CVD method is utilized, growing graphene film in the substrate of Cu/Ni composition metal;
Described step (2) comprises the steps: further
(A1) at Ar and H
2mixed atmosphere in, be warming up to 400 DEG C ~ 800 DEG C, and be incubated 3h ~ 5h;
(A2) continue to be warming up to 1000 DEG C ~ 1050 DEG C;
(A3) hydrocarbon is passed into as carbon source, insulation 15min ~ 30min;
(A4) at Ar and H
2mixed atmosphere in, be cooled to room temperature.
4. a preparation method for Graphene/Cu/Ni combination electrode, is characterized in that, comprise the steps:
(1) in substrate, patterned photoresist is prepared;
(2) deposit layer of Ni film, then on Ni film deposit one deck Cu film; Wherein, the Thickness Ratio of Ni film and Cu film is 1:(3 ~ 10);
(3) remove photoresist, obtain patterned Cu film and Ni film;
(4) CVD method is utilized, growing graphene film on patterned Cu film;
Described step (4) comprises the steps: further
(A1) at Ar and H
2mixed atmosphere in, be warming up to 400 DEG C ~ 800 DEG C, and be incubated 3h ~ 5h;
(A2) continue to be warming up to 1000 DEG C ~ 1050 DEG C;
(A3) hydrocarbon is passed into as carbon source, insulation 15min ~ 30min;
(A4) at Ar and H
2mixed atmosphere in, be cooled to room temperature.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106683991A (en) * | 2016-12-09 | 2017-05-17 | 华中科技大学 | Interconnection method for the carbon nanotube devices of grapheme/metal combined electrode |
CN108658037A (en) * | 2018-04-27 | 2018-10-16 | 国家纳米科学中心 | A kind of graphene functionalized nanometer pinpoint and preparation method thereof |
CN109742379A (en) * | 2019-01-28 | 2019-05-10 | 哈工大机器人(岳阳)军民融合研究院 | It is a kind of on Si/C composite material grow graphene method, utilize material made from this method and its application |
US11117804B2 (en) * | 2017-06-02 | 2021-09-14 | Center For Advanced Soft Electronics | Method of synthesizing thickness-controlled graphene through chemical vapor deposition using Cu—Ni thin film laminate |
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CN102050442A (en) * | 2009-11-10 | 2011-05-11 | 三星电子株式会社 | Methods of fabricating graphene using alloy catalyst |
CN102800419A (en) * | 2011-05-27 | 2012-11-28 | 清华大学 | Method for preparing graphene conductive film structure |
CN103745829A (en) * | 2013-12-30 | 2014-04-23 | 深圳市华星光电技术有限公司 | Preparation method of graphene composite electrode material |
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CN102050442A (en) * | 2009-11-10 | 2011-05-11 | 三星电子株式会社 | Methods of fabricating graphene using alloy catalyst |
CN102800419A (en) * | 2011-05-27 | 2012-11-28 | 清华大学 | Method for preparing graphene conductive film structure |
CN103745829A (en) * | 2013-12-30 | 2014-04-23 | 深圳市华星光电技术有限公司 | Preparation method of graphene composite electrode material |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106683991A (en) * | 2016-12-09 | 2017-05-17 | 华中科技大学 | Interconnection method for the carbon nanotube devices of grapheme/metal combined electrode |
US11117804B2 (en) * | 2017-06-02 | 2021-09-14 | Center For Advanced Soft Electronics | Method of synthesizing thickness-controlled graphene through chemical vapor deposition using Cu—Ni thin film laminate |
CN108658037A (en) * | 2018-04-27 | 2018-10-16 | 国家纳米科学中心 | A kind of graphene functionalized nanometer pinpoint and preparation method thereof |
CN109742379A (en) * | 2019-01-28 | 2019-05-10 | 哈工大机器人(岳阳)军民融合研究院 | It is a kind of on Si/C composite material grow graphene method, utilize material made from this method and its application |
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