CN108039379B - A kind of zinc oxide combination electrode film and preparation method thereof that metal foil surface is metal-doped - Google Patents
A kind of zinc oxide combination electrode film and preparation method thereof that metal foil surface is metal-doped Download PDFInfo
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- CN108039379B CN108039379B CN201711205257.0A CN201711205257A CN108039379B CN 108039379 B CN108039379 B CN 108039379B CN 201711205257 A CN201711205257 A CN 201711205257A CN 108039379 B CN108039379 B CN 108039379B
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 76
- 239000002184 metal Substances 0.000 title claims abstract description 62
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 55
- 239000011888 foil Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000001301 oxygen Substances 0.000 claims abstract description 20
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 20
- 239000000758 substrate Substances 0.000 claims abstract description 20
- 238000004544 sputter deposition Methods 0.000 claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 14
- 229910052786 argon Inorganic materials 0.000 claims abstract description 11
- 239000011701 zinc Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 238000002294 plasma sputter deposition Methods 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- 238000005516 engineering process Methods 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 3
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 3
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 3
- 230000001360 synchronised effect Effects 0.000 claims abstract description 3
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 3
- 239000011159 matrix material Substances 0.000 claims description 52
- 238000000576 coating method Methods 0.000 claims description 7
- 239000013077 target material Substances 0.000 claims description 6
- 230000007547 defect Effects 0.000 claims description 5
- 230000002708 enhancing effect Effects 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims 2
- 230000002269 spontaneous effect Effects 0.000 claims 2
- 239000010408 film Substances 0.000 description 50
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 11
- 238000000034 method Methods 0.000 description 11
- 229960001296 zinc oxide Drugs 0.000 description 9
- 230000005284 excitation Effects 0.000 description 5
- 230000005611 electricity Effects 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- VVTSZOCINPYFDP-UHFFFAOYSA-N [O].[Ar] Chemical compound [O].[Ar] VVTSZOCINPYFDP-UHFFFAOYSA-N 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000005622 photoelectricity Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022466—Electrodes made of transparent conductive layers, e.g. TCO, ITO layers
- H01L31/022483—Electrodes made of transparent conductive layers, e.g. TCO, ITO layers composed of zinc oxide [ZnO]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1884—Manufacture of transparent electrodes, e.g. TCO, ITO
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Condensed Matter Physics & Semiconductors (AREA)
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Abstract
The invention discloses a kind of zinc oxide combination electrode films that metal foil surface is metal-doped.It is to realize the preparation of metal foil/ZnO film electrode using one step of double-deck glow plasma physics sputter-deposition technology on metal foil.It is specifically cleaned metal foil as substrate acetone, high pressure nitrogen drying and processing；Metallic element sputtering source of high-purity low-melting-point metal Zn target as ZnO, is cleaned with acetone, while being passed through the synthesis atmospheric condition of argon gas and oxygen as metal oxide；The substrate pre-processed and target sample are put into double-deck glow plasma sputtering chamber, the synchronous doping for realizing basic metallic element in sull and the oxidate compound film that is formed.
Description
Technical field
Metal-doped zinc oxide composite coating and its system are formed the present invention relates to a kind of flexible metal paillon sputtering surface
Preparation Method belongs to technical field of film preparation.
Background technique
Zinc oxide (ZnO) is that a kind of broad stopband with biggish exciton binding energy and higher electron mobility is direct
Bandgap compound semiconductors material, the excellent properties having make its as electrode material be expected to photodetection, photocatalysis and
Area of solar cell is widely applied.Previous ZnO film often with FTO glass (SnO2Film), ito glass (In2O3Film) it is compound
It is used as photoelectric device light anode, however ITO and FTO glass higher cost, quality is frangible, is easy to limit the problems such as failure
Its application under specific condition.Nickel (Ni), aluminium (Al), etc. metals have relatively excellent electrical properties, if can be with metal
Paillon replaces electro-conductive glass and the compound flexible electrode material for obtaining superior performance of ZnO film, then can be expanded with save the cost
Application value of the ZnO in photoelectric field.
Existing metal foil/ZnO film electrode preparation method has thermal evaporation, chemical vapour deposition technique and electrochemistry
Sedimentation etc., but above-mentioned preparation method, there are at high cost, complicated for operation, ZnO film is not close in conjunction with substrate, leads to electrode
The problems such as photoelectricity performance is bad.
Goal of the invention
The present invention aiming at the problem that in terms of large area, quick preparation, photoelectric properties, is mentioned metal foil/ZnO film electrode
For a kind of zinc oxide combination electrode film and preparation method thereof that metal foil surface is metal-doped.Especially by double-deck brightness etc. from
The completion of one step of muon physics sputter deposition prepares ZnO film in metal foil surface and obtains flexible light electrode material, so that should
Process controllability is good, speed is fast, high-quality, at low cost, is especially suitable for large area preparation.
Implementation is as follows:
A kind of zinc oxide combination electrode film that metal foil surface is metal-doped is that the double-deck brightness is utilized on metal foil
One step of optical plasma sputter deposition technology realizes the preparation of metal foil/ZnO film electrode.Specifically by metal foil
It is cleaned as substrate acetone, high pressure nitrogen drying and processing；Metal member of high-purity low-melting-point metal Zn target (99.99%) as ZnO
Plain sputtering source, is cleaned with acetone, while being passed through the synthesis atmospheric condition of argon gas and oxygen as metal oxide；It will locate in advance
The substrate and target sample managed are put into double-deck glow plasma sputtering chamber, synchronous to realize basic metallic element in oxide
Doping in film and the oxidate compound film formed.
The present invention also provides the preparation method of the metal-doped zinc oxide combination electrode film of above-mentioned metal foil surface, tools
Body step are as follows:
(1) pretreatment of target and matrix: using high pure metal Zn target (99.99%) as the metallic element sputtering source of ZnO,
Itself and parent metal paillon are pre-processed with acetone, then with high pressure nitrogen drying and processing；It adjusts between matrix and target frame
Distance, respectively from substrate, target and vacuum furnace cavity draw three electrodes, substrate and target are all made of the pulse power and add
Heat, and matrix and target material surface are respectively formed a floor plasma glow discharge area in coating process, are put by two layers of plasma glow
The film forming efficiency of the overlapping enhancing metal in electric area.
(2) metal foil/ZnO film electrode preparation: argon is filled with into furnace body, that is, double-deck glow plasma sputtering chamber
Gas and oxygen, by matrix voltage pressure regulation to 380-420V, control matrix electric current to 1.5- so that air pressure reaches 20Pa in furnace body
2.0A carries out preheating in 10-20 minutes and bombardment to matrix, so that metal foil matrix surface increased activity, is carrying out ZnO film
When growth, not only matrix surface there are a large amount of Lacking oxygen defects and also realize simultaneously parent metal in ZnO film from
Hair doping；Then adjusting matrix voltage is 300-350V, and target voltage is adjusted to 650-700V, controls matrix electric current in 1.5-
2.2A, source current is in 0.3-0.6A, and plated film time is according to required thickness control in 20-40min.
Further, the distance between matrix and target frame are adjusted in step (1), are maintained at 20-25mm.
Further, the argon gas and oxygen of 3:1-9:1 are filled in step (2), so that air pressure reaches 20Pa in furnace body.
The present invention is by adjusting sull of the argon oxygen than obtaining different ratio.Specifically on later period substrates of different surface
Argon oxygen is realized than different by gas flowmeter when preparing sull, in the situation for keeping total gas pressure constant
Under, required total gas pressure is obtained by adjusting the flow of argon oxygen ratio.Argon oxygen is than different, oxygen and metal in the sull of acquisition
The mass percent of element is different, and the difference of oxygen content finally influences whether electron-transport and photoelectric response characteristic.
The utility model has the advantages that
(1) present invention is using high-purity Zn target as target, in order to improve the supply and efficiency of supply of element reaction, in substrate and
Double-deck glow plasma discharge is formed around target, film forming only needs 20-40min..
(2) present invention forms metal foil/ZnO film electrode electricity of large-area high-quality by the sputtering reaction of element
Pole, film surface is uniform, quality is good.
(3) since the doping of basic metallic element can be achieved at the same time in film, so that the electrode photoelectric stream that the present invention obtains
Intensity is higher, and speed of photoresponse is fast and photoelectric properties are stablized.
(4) present invention is using the double-deck brightness plasma physics sputter deposition in original single layer glow plasma sputtering technology
On the basis of the sputtering of one layer of glow plasma surface is increased so that deposition efficiency and quality in metal foil surface are excellent to substrate
In conventional coating technique, and individually designed metal-doped oxide target material is not needed, utilizes double-deck glow sputtering process
In high-energy can be directly realized by diffusing, doping of the fund metallic element in sull, improve photoelectric response performance, because
This is expected to carry out the large-scale application of composite film electrode on flexible material surface.
Detailed description of the invention
Fig. 1 be the present invention prepared by metal foil/ZnO film electrode surface (a) scanning electron microscope (SEM) and
(b) EDS power spectrum.By SEM figure it can be seen that column structure is presented in the electrode surface ZnO that the present invention is made, and is evenly distributed,
Quality is good.It can be seen that Zn element and O Elements Atom percentage close to 1:1, exist simultaneously a certain amount of nickel member by EDS power spectrum
Element doping.
Fig. 2 is perseverance electricity of the metal foil/ZnO film working electrode prepared by the present invention under periodical ultraviolet excitation
Position VA characteristic curve.It can be seen that electrode photoresponse is rapid under period ultraviolet excitation, and photoelectric current is highly stable.
Fig. 3 is metal foil/ZnO film working electrode prepared by the present invention under dark situation and ultraviolet excitation
Scan volt-ampere curve.It can be seen that electrode photo-current intensity under ultraviolet excitation is higher.
Fig. 4 is scanning volt-ampere of the metal foil/ZnO film working electrode prepared by the present invention under ultraviolet broken light excitation
Curve.For comparison diagram 3 it can be seen that electrode stability is good under different illumination conditions, photocurrent response is rapid.In illumination condition
Lower photoelectron can be received rapidly by metallic matrix Ni by ZnO column structure and be oriented to circuit, illustrate that Ni paillon and ZnO are thin
Film combines preferably and electrode photoelectric response is obvious.
Specific embodiment
The present invention is further explained in the following with reference to the drawings and specific embodiments.
Embodiment 1
The present invention is that one kind passes through a step using double-deck glow plasma physics sputter-deposition technology on W metal paillon
Realize the preparation of Ni paillon/ZnO film electrode.The preparation of zinc-oxide film is realized using following one-step method.
(1) pretreatment of target and matrix: using high pure metal Zn target (99.99%) as the metallic element sputtering source of ZnO,
Itself and parent metal Ni paillon are pre-processed with acetone, then with high pressure nitrogen drying and processing；Adjust matrix and target frame it
Between distance, be maintained at 20mm；Three electrodes are drawn from substrate, target and vacuum furnace cavity respectively, substrate and target are adopted
It is heated with the pulse power, and matrix and target material surface are respectively formed a floor plasma glow discharge area in coating process, by two layers
The film forming efficiency of the overlapping enhancing metal in plasma glow discharge area.
(2) Ni paillon/ZnO film electrode preparation: being filled with the argon gas and oxygen of 7:1 to furnace body, so that air pressure in furnace body
Reach 20Pa, by matrix voltage pressure regulation to 400V, controls matrix electric current to 1.8A and preheating in 10 minutes and bombardment are carried out to matrix, make
It obtains Ni paillon matrix surface and Lacking oxygen defect occurs so as to the growth of ZnO film；Then adjusting matrix voltage is 325V, target electricity
Pressure is adjusted to 680V, controls matrix electric current in 1.7A, source current is in 0.5A, plated film time 20min.Obtained by the technique
Column structure is presented in ZnO film surface, and is evenly distributed, and quality is good, sees that shown in Fig. 1 (a), Fig. 1 (b) shows thin film composition
The laminated film system that phase counterdiffusion has occurred between basic metallic element, and then forms with W metal doping zinc-oxide.
Fig. 2-4 is the ultraviolet light photo respondent behavior of the working electrode, and result of study shows electrode film made from this method and flexible base
It is combined between body, photoelectric respone is rapid, and the photoelectric current in ultraviolet lighting is higher.
Embodiment 2
The present invention is that one kind passes through a step using double-deck glow plasma physics sputter-deposition technology on metal Al paillon
Realize the preparation of Al paillon/ZnO film electrode.The preparation of zinc-oxide film is realized using following one-step method.
(1) pretreatment of target and matrix: using high pure metal Zn target (99.99%) as the metallic element sputtering source of ZnO,
Itself and parent metal Al paillon are pre-processed with acetone, then with high pressure nitrogen drying and processing；Adjust matrix and target frame it
Between distance, be maintained at 25mm；Three electrodes are drawn from substrate, target and vacuum furnace cavity respectively, substrate and target are adopted
It is heated with the pulse power, and matrix and target material surface are respectively formed a floor plasma glow discharge area in coating process, by two layers
The film forming efficiency of the overlapping enhancing metal in plasma glow discharge area.
(2) Al paillon/ZnO film electrode preparation: being filled with the argon gas and oxygen of 9:1 to furnace body, so that air pressure in furnace body
Reach 20Pa, by matrix voltage pressure regulation to 380V, controls matrix electric current to 1.6A and preheating in 10 minutes and bombardment are carried out to matrix, make
It obtains Al paillon matrix surface and Lacking oxygen defect occurs so as to the growth of ZnO film；Then adjusting matrix voltage is 280V, target electricity
Pressure is adjusted to 600V, controls matrix electric current in 1.60A, source current is in 0.4A, plated film time 20min.The working electrode is in purple
Result of study under outer photoelectric respone shows to be combined between electrode film and flexible substrate obtained by this method, and photoelectricity is rung
Should rapidly, the photoelectric current in ultraviolet lighting is higher, as in Figure 2-4.
Under burst of ultraviolel, light induced electron separates zinc oxide semi-conductor with hole, and Lacking oxygen and doped metallic elements can be with
Improving electrode film electron density reduces resistivity, stores and shift electronics to a certain extent, rings to reinforce film photoelectric
Behavior is answered, this outer film situation in conjunction with conductive substrates is also to improve the key of electrode light responsing sensitivity.What this method obtained
Sull and metallic matrix are tightly combined and Lacking oxygen in basic metallic element diffusion in the film and film occur
Content is more, can improve the photoelectric respone behavior of the electrode film to a certain extent.
Claims (4)
1. a kind of zinc oxide combination electrode film that metal foil surface is metal-doped, which is characterized in that be on metal foil
The preparation of metal foil/ZnO film electrode is realized using one step of double-deck glow plasma physics sputter-deposition technology, specifically
It is to be cleaned metal foil as substrate acetone, high pressure nitrogen drying and processing；Metal of high-purity low-melting-point metal Zn target as ZnO
Element sputtering source, is cleaned with acetone, while being passed through the synthesis atmospheric condition of argon gas and oxygen as metal oxide；It will be pre-
The substrate and target sample handled well are put into double-deck glow plasma sputtering chamber, synchronous to realize that basic metallic element is aoxidizing
Doping in object film and the oxidate compound film formed, the specific steps are that:
(1) pretreatment of target and matrix: right using high pure metal Zn target (99.99%) as the metallic element sputtering source of ZnO
Itself and parent metal paillon are pre-processed with acetone, then with high pressure nitrogen drying and processing；
The distance between matrix and target frame are adjusted, draws three electrodes, base from substrate, target and vacuum furnace cavity respectively
Piece and target are all made of pulse power heating, and matrix and target material surface are respectively formed one layer of plasma glow and put in coating process
Electric area, by the film forming efficiency of the overlapping enhancing metal in two layers of plasma glow discharge area；
(2) metal foil/ZnO film electrode preparation: be filled with into furnace body, that is, double-deck glow plasma sputtering chamber argon gas and
Oxygen, by matrix voltage pressure regulation to 380-420V, controls matrix electric current to 1.5-2.0A pairs so that air pressure reaches 20Pa in furnace body
Matrix carries out preheating in 10-20 minutes and bombardment, so that metal foil matrix surface increased activity, when carrying out ZnO film growth,
Not only there are a large amount of Lacking oxygen defects but also realizes spontaneous doping of the parent metal in ZnO film simultaneously in matrix surface；
Then adjusting matrix voltage is 300-350V, and target voltage is adjusted to 650-700V, controls matrix electric current in 1.5-2.2A, source electrode
Electric current is in 0.3-0.6A, and plated film time is according to required thickness control in 20-40min.
2. a kind of preparation method for the zinc oxide combination electrode film that metal foil surface is metal-doped, which is characterized in that specific
Step are as follows:
(1) pretreatment of target and matrix: right using high pure metal Zn target (99.99%) as the metallic element sputtering source of ZnO
Itself and parent metal paillon are pre-processed with acetone, then with high pressure nitrogen drying and processing；
The distance between matrix and target frame are adjusted, draws three electrodes, base from substrate, target and vacuum furnace cavity respectively
Piece and target are all made of pulse power heating, and matrix and target material surface are respectively formed one layer of plasma glow and put in coating process
Electric area, by the film forming efficiency of the overlapping enhancing metal in two layers of plasma glow discharge area；
(2) metal foil/ZnO film electrode preparation: be filled with into furnace body, that is, double-deck glow plasma sputtering chamber argon gas and
Oxygen, by matrix voltage pressure regulation to 380-420V, controls matrix electric current to 1.5-2.0A pairs so that air pressure reaches 20Pa in furnace body
Matrix carries out preheating in 10-20 minutes and bombardment, so that metal foil matrix surface increased activity, when carrying out ZnO film growth,
Not only there are a large amount of Lacking oxygen defects but also realizes spontaneous doping of the parent metal in ZnO film simultaneously in matrix surface；
Then adjusting matrix voltage is 300-350V, and target voltage is adjusted to 650-700V, controls matrix electric current in 1.5-2.2A, source electrode
Electric current is in 0.3-0.6A, and plated film time is according to required thickness control in 20-40min.
3. preparation method according to claim 2, which is characterized in that adjusted between matrix and target frame in step (1)
Distance is maintained at 20-25mm.
4. preparation method according to claim 2, which is characterized in that be filled with the argon gas and oxygen of 3:1-9:1 in step (2)
Gas, so that air pressure reaches 20Pa in furnace body.
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