CN105931846A - Graphene electrode with nitride protection layer and preparation method of graphene electrode - Google Patents

Graphene electrode with nitride protection layer and preparation method of graphene electrode Download PDF

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Publication number
CN105931846A
CN105931846A CN201610442729.3A CN201610442729A CN105931846A CN 105931846 A CN105931846 A CN 105931846A CN 201610442729 A CN201610442729 A CN 201610442729A CN 105931846 A CN105931846 A CN 105931846A
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matrix
graphene
film
microscope slide
preparation
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CN105931846B (en
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周艳文
佟欣儒
高健波
孟见成
吴法宇
赵�卓
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HAIAN INSTITUTE OF HIGH-TECH RESEARCH NANJING UNIVERSITY
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University of Science and Technology Liaoning USTL
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/04—Electrodes or formation of dielectric layers thereon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/36—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the electrodes
    • H01L33/40—Materials therefor
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/04—Electrodes or formation of dielectric layers thereon
    • H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention relates to a graphene electrode with a nitride protection layer and a preparation method of the graphene electrode. A TiN or GaN thin film coats a glass slide substrate or a PET substrate, wherein the thickness of the thin film is 30-50nm; the graphene electrode coated with the nitride protection layer is prepared by a vacuum thermal evaporation method; an evaporation material is heated to be gasified in vacuum evaporation coating equipment; the gasified particles are emitted to the substrate and are simultaneously deposited on the substrate to form a solid thin film; and a nitride thin film is prepared on the surface of the substrate. The graphene electrode has the advantages that the graphene electrode coated with the nitride protection layer is prepared by the vacuum evaporation method, so that the problem that composite thin film graphene is exposed on the outer surface layer and is easily scratched to lose the optimal conductivity is solved; and protection on the graphene surface is achieved on the basis of not destroying the original light transmission and conductivity of the graphene, so that the service lifetime of the graphene electrode is prolonged.

Description

A kind of Graphene electrodes of band protective nitride layer and preparation method thereof
Technical field
The invention belongs to Graphene electrodes preparing technical field, particularly relate to the Graphene electricity of a kind of band protective nitride layer Pole and preparation method thereof.
Background technology
Since self-discovery Graphene, around preparation and the research fast development of application of Graphene, the birth of a large amount of patents of invention Raw.Investigation of materials aspect, Graphene doping boron nitride or carbonitride, it is prepared as composite, for the direction such as photocatalysis, lubrication (such as patent: Publication No. CN 105316077A, disclose a kind of Graphene/carbonitride quantum dot composite nano materials and lubrication Oil drag improving agent；Publication No. CN105396606A, discloses a kind of cerium oxide/graphene quantum dot/class Graphene phase nitrogen Change carbon composite photocatalyst material and preparation method thereof；Publication No. CN105289689A, discloses a kind of nitrogen-doped graphene amount The synthesis of sub-point/class Graphene phase carbon nitride composite and application)；Also can adulterate boron nitride or gallium nitride to prepare hetero-junctions thin Film, uses as electrode or photocatalysis membrana and (such as: Publication No. CN102392226A, discloses a kind of Graphene/boron nitride heterogeneous The preparation method of thin film；Publication No. CN105274491A, discloses a kind of Graphene-boron nitride heterogeneous phase composite film material Preparation method；Publication No. CN104944417A, discloses the preparation method of a kind of Graphene-boron nitride hetero-junctions).Graphite Alkene doping BN (boron nitride) and GaN (gallium nitride) prepare laminated film or and CNT, can as LED chip material (such as: public The number of opening is CN104966771A, discloses a kind of Graphene-boron nitride-gallium nitride based LED chip and preparation method thereof；Publication No. CN104774470A, discloses a kind of sealant for great power LED and great power LED).Especially it is worth mentioning that TiN (titanium nitride) self-supporting composite graphite alkene electrode makes the use of nitride material be no longer limited to BN (boron nitride) and GaN (nitrogen Change gallium) (such as: Publication No. CN104616896A, disclose titanium nitride/graphene combination electrode and the preparation side thereof of a kind of support Method；.
In the preparation of the above-mentioned composite enumerated or laminated film, or with nitride for supporting Film laminated Graphene, Or using Graphene as the Material cladding of doping, these complex methods all make Graphene be exposed to extexine.And preparation method Then based on the chemical method of metal catalytic.For laminated film, be exposed to the Graphene on surface be easy to be scratched from And lose its best electrical conductivity and other premium properties, it is impossible to ensure laminated film large area and the existence of stable performance.
Summary of the invention
For overcoming the deficiencies in the prior art, it is an object of the invention to provide the Graphene electrodes of a kind of band protective nitride layer And preparation method thereof, it is achieved on the basis of not destroying the original light transmission of Graphene, electric conductivity, complete the protection to graphenic surface.
For achieving the above object, the present invention is achieved through the following technical solutions:
The Graphene electrodes of a kind of band protective nitride layer, is covered with TiN or GaN thin on microscope slide matrix or PET matrix Film, described film thickness is 30～50nm.
The preparation method of the Graphene electrodes of a kind of band protective nitride layer, uses vacuum thermal evaporation preparation to be coated with nitridation The Graphene electrodes of thing protective layer, specifically comprises the following steps that
1) experiment matrix selects microscope slide matrix and the PET matrix of composite graphite alkene；Drug material selects TiN and GaN two Kind；Under same experiment condition, obtain the thickness on the PET matrix of composite graphite alkene by measuring the thickness on microscope slide matrix Predictive value；
2) pretreatment before sputtering: before plated film, microscope slide matrix needs to be cleaned by, and is placed in dehydrated alcohol by microscope slide matrix, By ultrasonic waves for cleaning 15 minutes, then matrix is placed in deionized water, ultrasonic waves for cleaning 20 minutes, finally takes out matrix, directly Dry up with nitrogen, mark on glass with marking pen, in order to the later stage measures thickness；
3) experimental technique: use vacuum thermal evaporation preparation to be coated with the Graphene electrodes of protective nitride layer: to steam in vacuum Put into microscope slide matrix and the PET matrix of composite graphite alkene in filming equipment simultaneously, be evaporated in vacuo according to the technological parameter of table 1 Carrying out plated film in filming equipment, in vacuum evaporation coating film device, heating evaporation material is allowed to gasify, the particle directive after gasification Substrate forms solid film at deposition on substrate simultaneously, prepares nitride film at matrix surface；
Table 1:TiN and the preparation technology parameter of GaN film
Compared with prior art, the invention has the beneficial effects as follows:
The method preparation using vacuum evaporation is coated with the Graphene electrodes of protective nitride layer, solves laminated film graphite Alkene is exposed to extexine and is easily scratched and the problem that loses its best electrical conductivity.Achieve and do not destroying the original printing opacity of Graphene Complete the protection to graphenic surface on the basis of property, electric conductivity, thus extend the service life of graphite electrode.
Accompanying drawing explanation
Fig. 1 is the light transmittance of monolayer and bilayer graphene.
Fig. 2 is the light transmittance of TiAlN thin film under the conditions of different evaporation voltage x current on microscope slide matrix and PET matrix.
Fig. 3 is the light transmittance of GaN film under the conditions of different evaporation voltage x current on microscope slide matrix and PET matrix.
Fig. 4 is evaporation condition 175V 200A TiAlN thin film tissue topography scanning electron microscopic picture on microscope slide matrix.
Fig. 5 is evaporation condition 175V 200A TiAlN thin film tissue topography scanning electron microscopic picture on PET matrix.
Fig. 6 is evaporation condition 180V 210A TiAlN thin film tissue topography scanning electron microscopic picture on microscope slide matrix.
Fig. 7 is evaporation condition 180V 210A TiAlN thin film tissue topography scanning electron microscopic picture on PET matrix.
Fig. 8 is evaporation condition 185V 218A TiAlN thin film tissue topography scanning electron microscopic picture on microscope slide matrix.
Fig. 9 is evaporation condition 185V 218A TiAlN thin film tissue topography scanning electron microscopic picture on PET matrix.
Figure 10 is evaporation condition 120V 150A, and the evaporation time is that 1s GaN film tissue topography on microscope slide matrix sweeps Retouch electron microscopic picture.
Figure 11 is evaporation condition 120V 150A, and the evaporation time is 1s GaN film tissue topography scanning on PET matrix Electron microscopic picture.
Figure 12 is evaporation condition 120V 150A, and the evaporation time is 5min GaN film tissue topography on microscope slide matrix Scanning electron microscopic picture.
Figure 13 is evaporation condition 120V 150A, and the evaporation time is that 5min GaN film tissue topography on PET matrix sweeps Retouch electron microscopic picture.
Figure 14 is evaporation condition 120V 150A, and the evaporation time is 10min GaN film tissue shape on microscope slide matrix Looks scanning electron microscopic picture.
Figure 15 is evaporation condition 120V 150A, and the evaporation time is that 10min GaN film tissue topography on PET matrix sweeps Retouch electron microscopic picture.
Specific implementation method
Below in conjunction with Figure of description, the present invention is described in detail, it should be noted that the enforcement of the present invention does not limits In following embodiment.
First transferring on organic flexible PET matrix by Graphene prepared by chemical catalysis, this step is complete by commodity production Become.Then in commercial PET/ graphene base body, ultra-thin TiN (titanium nitride) and GaN (gallium nitride) is prepared by the method for vacuum evaporation Thin film (30～50nm), the effect of this layer film is to complete stone on the basis of not destroying the original light transmission of Graphene, electric conductivity The protection on ink alkene surface.
Concrete operations are:
Prepare material: selection model is the commercial microscope slide matrix of SAIL7101 and is given birth to by Jiangsu Li He Photoelectric Co., Ltd. The PET matrix of the composite graphite alkene produced；Drug material selects TiN (titanium nitride) and GaN (gallium nitride) two kinds.
Under same experiment condition, obtain on the PET matrix of composite graphite alkene by measuring the thickness on microscope slide matrix The predictive value of thickness；That is: the film thickness measurements on microscope slide matrix is equal to the pre-of the thickness on the PET matrix of composite graphite alkene Measured value.
Pretreatment before sputtering: before plated film, microscope slide matrix needs to be cleaned by, and is placed in dehydrated alcohol by microscope slide matrix, uses Ultrasonic waves for cleaning 15 minutes, then matrix is placed in deionized water, ultrasonic waves for cleaning 20 minutes, ultrasonic waves for cleaning acc power is 60w, finally takes out matrix, utilizes rapidly nitrogen to dry up, marks with marking pen on glass, in order to the later stage measures thickness.Adopt Prepare the Graphene electrodes being coated with protective nitride layer: in vacuum evaporation film device, put into load glass with vacuum thermal evaporation simultaneously Sheet matrix and the PET matrix of composite graphite alkene, carry out plated film according to the technological parameter of table 1 in vacuum evaporation coating film device, In vacuum evaporation coating film device, heating evaporation material is allowed to gasify, and the particle directive substrate after gasification is simultaneously in deposition on substrate shape Become solid film, prepare nitride film at matrix surface.
Table 1:TiN and the preparation technology parameter of GaN film
Case study on implementation 1
Utilizing vacuum vapour deposition to prepare TiAlN thin film on microscope slide and Graphene/PET respectively, medicine is purity 99.99% TiN (titanium nitride) black powder, chamber pressure is 8x10-4Pa, controls electric current by adjusting different vaporization voltage, contrast The electric conductivity of TiAlN thin film prepared under the conditions of different parameters, light transmittance and surface topography, provide the optimum work of film preparation Skill parameter.
It is deposited with according to table 1 parameter:
Table 1:TiN and the preparation technology of GaN film
In table 1, TiAlN thin film uses 175V, 180V, 185V difference evaporation voltage, and the thin film prepared is carried out electric conductivity Analyze, light transmittance analysis and Analysis of Surface Topography.
Table 2: monolayer and the electric conductivity of bilayer graphene
Table 3:TiN and GaN film electric conductivity
Be shown in Table 2, table 3, on Graphene/PET matrix, vacuum evaporation is prepared the TiAlN thin film square resistance order of magnitude and is 103Ohm/sq, the single-layer graphene square resistance order of magnitude is 102Ohm/sq, on microscope slide, the TiAlN thin film square resistance of preparation is 106ohm/sq.While result explanation titanium nitride protection Graphene, there is good electric conductivity.
See Fig. 1～Fig. 3, on microscope slide matrix prepare TiAlN thin film light transmittance be better than on Graphene preparation TiN thin Film；And along with the increase of voltage, thickness increases, light transmittance declines；TiAlN thin film is prepared at thickness in 30～40nm districts on Graphene Between time light transmittance about about 85%.
Seeing Fig. 4～Fig. 9, TiAlN thin film does not has structure on glass, there is structure on Graphene, with glass is noncrystal Relevant.TiAlN thin film is prepared in vacuum evaporation on Graphene/PET, technique be 185V/218A evaporation the time be 1s, the 40nm of preparation Thin film, square resistance is 9.93E+2ohm/sq, and light transmittance is 85%, and surface topography is fine and close.
Case study on implementation 2
The implementation case utilizes vacuum vapour deposition to prepare GaN film on microscope slide and Graphene/PET matrix, and medicine is The yellow powder that purity is 99.99% of Shanghai Wu Sheng company limited, chamber pressure is 8x10-4Pa, by adjusting difference evaporation Voltage thus control electric current, the electric conductivity of GaN film, light transmittance and surface shape prepared under the conditions of contrast different parameters Looks, provide the optimal procedure parameters of film preparation.
Concrete preparation technology parameter is: 1s, 5min, 10min (evaporation time), the thin film prepared is carried out electric conductivity and divides Analysis, light transmittance analysis and Analysis of Surface Topography.
Being shown in Table 1～table 3, on Graphene/PET matrix, vacuum evaporation is prepared the GaN film square resistance order of magnitude and is 103Ohm/sq, the single-layer graphene square resistance order of magnitude is 102Ohm/sq, glass is prepared GaN film square resistance is 106While ohm/sq result explanation GaN protection Graphene, there is good electric conductivity.
See Fig. 1～Fig. 3, glass is prepared GaN film light transmittance and is better than on Graphene preparation GaN film；And along with The increase of evaporation time, thickness increases, and light transmittance declines；GaN film thickness is prepared saturating when 30～40nm interval on Graphene Light rate is about about 85%.
Seeing Figure 10～Figure 15, GaN film does not has structure on glass, there is structure on Graphene, may be with glass Noncrystal relevant.Vacuum evaporation prepares GaN film on Graphene/PET, increases over time, and crystal grain increases, and surface is more come The finest and close.

Claims (2)

1. the Graphene electrodes of a band protective nitride layer, it is characterised in that be covered with on microscope slide matrix or PET matrix TiN or GaN film, described film thickness is 30～50nm.
The preparation method of the Graphene electrodes of a kind of band protective nitride layer the most according to claim 1, it is characterised in that Use vacuum thermal evaporation preparation to be coated with the Graphene electrodes of protective nitride layer, specifically comprise the following steps that
1) experiment matrix selects microscope slide matrix and the PET matrix of composite graphite alkene；Drug material selects TiN and GaN two kinds；? Under same experiment condition, obtain the pre-of thickness on the PET matrix of composite graphite alkene by measuring the thickness on microscope slide matrix Measured value；
2) pretreatment before sputtering: before plated film, microscope slide matrix needs to be cleaned by, and is placed in dehydrated alcohol by microscope slide matrix, with super Sound wave cleans 15 minutes, then is placed in deionized water by matrix, ultrasonic waves for cleaning 20 minutes, finally takes out matrix, directly uses nitrogen Air-blowing is done, and marks on glass with marking pen, in order to the later stage measures thickness；
3) experimental technique: use vacuum thermal evaporation preparation to be coated with the Graphene electrodes of protective nitride layer: at vacuum evaporation coating Put into microscope slide matrix and the PET matrix of composite graphite alkene, according to the technological parameter of table 1 at vacuum vapor plating in equipment simultaneously Carrying out plated film in equipment, in vacuum evaporation coating film device, heating evaporation material is allowed to gasify, the particle directive substrate after gasification Form solid film at deposition on substrate simultaneously, prepare nitride film at matrix surface；
Table 1:TiN and the preparation technology parameter of GaN film
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108772085A (en) * 2018-03-13 2018-11-09 合肥工业大学 A kind of preparation method of broad stopband carbon nitrogen polymer

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Publication number Priority date Publication date Assignee Title
CN103489982A (en) * 2013-09-25 2014-01-01 北京工业大学 LED based on photonic crystal-single-layer graphene structure
CN103606535A (en) * 2013-11-26 2014-02-26 深圳市华星光电技术有限公司 Flexible display module manufacturing method and flexible display module through method

Patent Citations (2)

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Publication number Priority date Publication date Assignee Title
CN103489982A (en) * 2013-09-25 2014-01-01 北京工业大学 LED based on photonic crystal-single-layer graphene structure
CN103606535A (en) * 2013-11-26 2014-02-26 深圳市华星光电技术有限公司 Flexible display module manufacturing method and flexible display module through method

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Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108772085A (en) * 2018-03-13 2018-11-09 合肥工业大学 A kind of preparation method of broad stopband carbon nitrogen polymer
CN108772085B (en) * 2018-03-13 2021-02-23 合肥工业大学 Preparation method of wide-bandgap carbon-nitrogen polymer

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