CN104404459B - A kind of preparation method of target material - Google Patents
A kind of preparation method of target material Download PDFInfo
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- CN104404459B CN104404459B CN201410626628.2A CN201410626628A CN104404459B CN 104404459 B CN104404459 B CN 104404459B CN 201410626628 A CN201410626628 A CN 201410626628A CN 104404459 B CN104404459 B CN 104404459B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
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- Inorganic Chemistry (AREA)
- Photovoltaic Devices (AREA)
- Physical Vapour Deposition (AREA)
Abstract
It is an object of the present invention to provide a kind of method for preparing cushion zinc oxide sulphur target, based on zinc oxide, add magnesium sulfide zinc and add the third oxide etc., control cushion carrier concentration, more preferable PN characteristics can be made, and the pioneering mode for adding high temperature sintering using injection forming makes the target of such a multivariant oxide, improve target uniformity and consistency, extend target life and increase utilization rate, improve sputtering thin film quality and performance, via the raising of the design and target quality of composition, improve the conversion efficiency of CIGS solar cells, reduce production cost, meet the demand of volume production.
Description
Technical field
Copper-indium-gallium-selenium photovoltaic battery buffering is prepared the present invention relates to a kind of preparation method of target material, especially one kind
The method of layer zinc oxide sulphur target.
Background technology
Global energy requirements are climbed to a higher point year by year, in the case where energy-conservation and environmental consciousness come back, and the development renewable sources of energy are that the whole world is common
Target；For the renewable sources of energy, no matter for waterpower, wind-force, geothermal power generation, it is both needed to obtain conversion effect with kinetic energy conversion regime
Rate, and solar power generation is then the electricity generation system that electric energy is converted into using sunshine, without movable part in solar power system
Point, machinery is rotated unlike that must be used in the electricity generation systems such as wind-force, waterpower, underground heat, therefore do not have HTHP and noise etc.
Puzzlement, does not cause environmental pressure in power generation process, is a cleanly green energy resource.In addition, solar source is inexhaustible to use it
Inexhaustible characteristic so that solar power system can have the big advantage of one of continuous utilization；Although the light of solar power generation now
Photoelectric transformation efficiency is not still high, but it is its advantage that solar power system, which is not required to expend extra energy cost, in other words, these
Originally not by people by the use of the energy now with fraction be used as power source.The sun is irradiated to the energy of earth's surface daily, surpasses
The energy of the whole mankind required for 30 years is crossed, solar cell has turned into the main flow of following alternative energy source.Estimate to the whole world in 2100
The energy will be up to 60% using the utilization rate of solar energy.
The huge number of solar cell, and CIGS (CIGS) thin-film solar cells possesses high conversion efficiency and hair
Open up potentiality and attracted attention, current CIGS (CIGS) thin-film solar cells highest conversion efficiency is real by U.S.'s renewable sources of energy
Test room (NREL) to be created, its efficiency is up to 20%.CIGS from nineteen ninety-five be developed so far conversion efficiency improved it is whole have 7% it
It is many, compared to CdTe in the same time 4%, monocrystalline silicon and polysilicon respectively for 3% and non-crystalline silicon 1%, it is sufficient to find out that CIGS exists
Development potentiality in conversion efficiency.CIGS belongs to polycrystalline yellow copper structure (Chalcopyrite) compound of I-III-VI race,
It is a kind of semiconductor material being derived by II-VI compounds of group zincblende lattce structure (Zinc-Blend Structure)
Material, is formed, the lattice position for belonging to II race's element originally is replaced and shape by I race and III race by the unit cell storehouse of two zincblende
Into, and lattice position residing for In can then replace by the Ga elements added inside chalcopyrite.CIGS (CIGS) has direct
The P-type characteristic of semiconductor of energy gap (Direct band-gap) property, and have at a relatively high absorption coefficient of light α (α=104~
105 cm-1), it is 100 times of monocrystalline silicon, most solar spectrum can be covered, compared with other solar cells, therefore only need 1 ~
3 μm of thickness, you can the incident sunshine of absorption more than 99%.Current CIGS thin film solar cell highest conversion efficiency is by U.S.
State's Renewable Energy Laboratory (NREL) is created, and its efficiency is up to 20%.And NREL was shown in assessment report in 2011, CIGS (copper
Indium gallium selenium) can up it grow up with annual 0.3% in conversion efficiency.
CIGS (CIGS) thin-film solar cells be developed so far its modular construction substantially part by Top electrode (AL/Ni),
Anti-reflecting layer (MgF2), optical window layer (AZO/ITO), cushion (CdS), absorbed layer (CIGS), back electrode (Mo) and substrate (SS/
GLASS/PET) constituted；In single film layer, each material composition than parameter allotment, film crystal structure, processing procedure mode with
It is the challenge in its preparation to optimize the various factors such as processing procedure, in addition, it is also necessary to take into account that each film layer is stacked into the matching, each of component
The many factors such as influence each other between film layer preparation method and processing procedure, especially from pertinent literature show CIGS (CIGS) for
It is extremely sensitive for component influences under various process parameters, more increase CIGS (CIGS) thin-film solar cells in preparation
Difficulty, while also cause technology door relatively to improve, international photovoltaic circle be considered technical difficulty than it is larger it is a kind of too
Positive electricity pond.
Target is to be used for the mother metal of sputter coating with solid shape.If target can be simply divided into metal according to materials classification
With ceramic two major class, if according to processing procedure classification can generally divide into melting processing procedure and the major class of powder metallurgy processing procedure two generally.It is most of
Metal targets adopt melting processing procedure, a small number of targets in view of when using grain size control, alloy composition fusing point gap too it is big etc. it is all because
Element just uses powder metallurgy processing procedure.It is to re-sinter processing procedure, material with hot pressing processing procedure or cold pressure for oxide target material tradition
Mixing uniformity is poor, and stress distribution is uneven in sintering process, is difficult to produce the large-sized oxide target material of high density.Current light
Such as touch screen, integrated circuit, liquid crystal display, building glass, optical film and thin-film solar cells in electricity and semiconductor industry, be
Large-area uniformity and production are obtained, associated film largely uses vacuum magnetic control sputter process.
Absorbed layer and cushion are to influence the important film layer of battery efficiency and the mode of production, tradition research in CIGS film layers
Display can show preferably battery efficiency using the CdS film layers of immersion method.Absorbed layer typically uses vacuum evaporation and vacuum
Magnetic control sputtering plating adds two kinds of main processing procedures of rear selenizing heat treatment, the characteristic with large area film forming and the preferable uniformity of acquisition.It is slow
Layer function is rushed, metal and semiconductor contact formation parallel resistance, protection absorbed layer and the planarizing of absorbed layer passive surface is prevented.It is slow
Rushing layer demand characteristics needs high light transmittance, efficiently controls film thickness (30 nm ~ 100 nm) and film uniform fold.If but
Cadmium sulfide (CdS) using immersion method as cushion, then have that processing procedure is discontinuous, Cd pollution problems are big and large-area uniformity not
Good the shortcomings of.Today there is also many research the slow of the different energy ranks of manufacture is waited using various oxides such as ZnO, ZnS, MgO, ZnSe ...
Rush layer, it is desirable to replace CdS and preferably efficiency can be obtained.The targets such as conventionally manufactured ZnO, ZnS, MgO, ZnSe using pressure sintering and
Deng isostatic pressing, equipment investment is costly, and be difficult large scale manufacture and density it is relatively low.
The content of the invention
It is an object of the present invention to provide a kind of method for preparing cushion zinc oxide sulphur target, based on the zinc oxide, addition sulphur
Change zinc and add the third oxide etc., control cushion carrier concentration, can make more preferable PN characteristics, and it is pioneering using slip casting into
Type makes the target of such a multivariant oxide plus the mode of low temperature sintering, and target is improved using the various powder of wet-mixing
Consistency after the uniformity and sintering of base substrate, extension the sputtered target material life-span and increase utilization rate, improve sputtering thin film quality and
Performance, improves the conversion efficiency of CIGS solar cells.
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 10.0-45.0wt% in zinc oxide, or
Continue to add the third oxide formation dusty material, then be sufficiently mixed with zirconia ball, pure water, dispersant grinding, its quality
Than for：Dusty material:Zirconia ball:Pure water:Dispersant=0.8-1.2:2.5-3.5:0.20-0.30:0.005；Grind 4-24
Slurry is formed after hour, is then poured into slurry in porous mould, after the drying of 12-36 hours, demoulding forms polynary
The solid density of Oxide and sulfide mixing is 5.0-5.2 g/cm3Idiosome, then by 800-1200 DEG C and 3-24 it is small
When sintering, that is, form sputter high density target idiosome, it is cleaved with surface grinding into vacuum magnetic control sputtering plating target, with Ah
Base rice, which is done in the proper way, measures target density；Using glass as base material, it is put into vacuum magnetic control sputtering machine, vacuum-pumping system first is by sputter
Cavity background pressure is evacuated to 0.7 × 10-5-0.9×10-5, will be logical through choke valve using argon gas as working gas after torr
Entering argon gas controls the operating pressure of sputter cavity to be 2 × 10-3-5×10-3Torr, first with D/C power sputter first layer 500-
Mo films thick 800nm, then thick evaporation manufacture second layer 1500-2000nm CIGS absorbs layer film altogether, is then coated with the
Three-layer thin-film, 0.7 × 10 is evacuated to vacuum-pumping system by sputter cavity background pressure-5-0.9×10-5After torr, argon is utilized
Gas will be passed through argon gas as working gas, through choke valve and control the operating pressure of sputter cavity to be 2 × 10-3-5×10- 3Torr, sputter process is carried out with RF powers, and the transparent buffer layer zinc oxide sulphur that film thickness 80-150nm or so is made is thin
Film, the 4th layer is coated with the thick nesa coatings of 600-1000nm using pulsed DC source and AZO targets, that is, completes CIGS solar energy
The film of the primary structure of battery is made, and conversion efficiency test is carried out after wire mark the superiors ag paste electrode.
Wherein dispersant is 18-22g/L aqueous sodium polyacrylate.
Wherein the third oxide be silica 0.1-2.0wt%, bismuth oxide 0.1-2.0wt%, vanadium oxide 0.1-2.0wt%,
Any one in aluminum oxide 0.1-2.0wt%, gallium oxide 0.1-2.0wt%, boron oxide 0.1-2.0wt%.
The grinding most preferably time is 6-16 hours.
900-1100 DEG C of preferably temperature is sintered, the most preferably time is 3-8 hours.
It is characteristic of the invention that in a kind of cushion zinc oxide sulphur target and its method for preparation, it is pioneering to use injection forming
Mode various Oxide and sulfides are sufficiently mixed uniformly extend target service life to improve the uniformity of target, and
By the third oxide is added in zinc oxide and zinc sulphide, reduction sintering temperature improves target density, develops applicable
In the zinc oxide sulphur target of cushion so that the procedure for producing of CIGS photovoltaic cells can be carried out in a vacuum completely, and not
The problem of Cd pollutes is avoided using cadmium sulfide (CdS) so that the volume production of CIGS thin film solar cell is more feasible, can
The CIGS batteries of high conversion efficiency are obtained, the requirement of production is met.
Embodiment：
Embodiment 1：
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 10.0wt% formation powder in zinc oxide
Material, then be sufficiently mixed with zirconia ball, pure water, dispersant grinding, its mass ratio is：Dusty material:Zirconia ball:Pure water:
Dispersant=0.8:2.5:0.20:0.005；Grinding forms slurry after 4 hours, then pours into slurry in porous mould, passes through
After the drying of 12 hours, the solid density that demoulding formation multivariant oxide is mixed with sulfide is 5.0g/cm3Idiosome, then
By 800 DEG C and the sintering of 3 hours, that is, form sputter high density target idiosome, it is cleaved with surface grinding into vacuum magnetic control
Sputter target, target density is measured with Archimedian method；Using glass as base material, it is put into vacuum magnetic control sputtering machine, first very
Sputter cavity background pressure is evacuated to 0.7 × 10 by empty extract system-5After torr, using argon gas as working gas, through throttling
Valve will be passed through argon gas and control the operating pressure of sputter cavity to be 2 × 10-3Torr, first thick with D/C power sputter first layer 500nm
Mo films, then the CIGS of evaporation manufacture second layer 1500nm thickness absorbs layer film altogether, third layer film is then coated with, with vacuum
Sputter cavity background pressure is evacuated to 0.7 × 10 by extract system-5After torr, using argon gas as working gas, through choke valve
Argon gas, which will be passed through, controls the operating pressure of sputter cavity to be 2 × 10-3Torr, sputter process is carried out with RF powers, is made thin
Film thickness 80nm or so transparent buffer layer oxidation zinc-sulfur membrane, the 4th layer is coated with 600nm using pulsed DC source and AZO targets
Thick nesa coating, that is, the film for completing the primary structure of CIGS solar cells makes, after wire mark the superiors ag paste electrode
Carry out conversion efficiency test.
Wherein dispersant is 18g/L aqueous sodium polyacrylate.
Embodiment 2：
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 25.0wt% formation powder in zinc oxide
Material, then be sufficiently mixed with zirconia ball, pure water, dispersant grinding, its mass ratio is：Dusty material:Zirconia ball:Pure water:
Dispersant=1.0:3.0:0.25:0.005；Grinding forms slurry after 14 hours, then pours into slurry in porous mould, passes through
After the drying for spending 24 hours, the solid density that demoulding formation multivariant oxide is mixed with sulfide is 5.1 g/cm3Idiosome, so
Afterwards by 1000 DEG C and the sintering of 5 hours, that is, form sputter high density target idiosome, it is cleaved with surface grinding into Vacuum Magnetic
Sputter target is controlled, target density is measured with Archimedian method；Using glass as base material, it is put into vacuum magnetic control sputtering machine, first
Sputter cavity background pressure is evacuated to 0.8 × 10 by vacuum-pumping system-5After torr, using argon gas as working gas, through section
Stream valve will be passed through argon gas and control the operating pressure of sputter cavity to be 4 × 10-3Torr is first thick with D/C power sputter first layer 600nm
Mo films, then thick evaporation manufacture second layer 1800nm CIGS absorbs layer film altogether, third layer film is then coated with, with true
Sputter cavity background pressure is evacuated to 0.8 × 10 by empty extract system-5After torr, using argon gas as working gas, through throttling
Valve will be passed through argon gas and control the operating pressure of sputter cavity to be 3 × 10-3Torr, sputter process is carried out with RF powers, is made
Film thickness 120nm or so transparent buffer layer oxidation zinc-sulfur membrane, the 4th layer is coated with using pulsed DC source and AZO targets
Nesa coating thick 800nm, that is, the film for completing the primary structure of CIGS solar cells makes, wire mark the superiors silver paste electricity
Conversion efficiency test is extremely carried out afterwards.
Wherein dispersant is 20g/L aqueous sodium polyacrylate.
Embodiment 3：
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 45.0wt% formation powder in zinc oxide
Material, then be sufficiently mixed with zirconia ball, pure water, dispersant grinding, its mass ratio is：Dusty material:Zirconia ball:Pure water:
Dispersant=1.2:3.5:0.30:0.005；Grinding forms slurry after 24 hours, then pours into slurry in porous mould, passes through
After the drying for spending 36 hours, the solid density that demoulding formation multivariant oxide is mixed with sulfide is 5.2 g/cm3Idiosome, so
Afterwards by 1200 DEG C and the sintering of 24 hours, that is, form sputter high density target idiosome, it is cleaved with surface grinding into vacuum
Magnetic control sputtering plating target, target density is measured with Archimedian method；Using glass as base material, it is put into vacuum magnetic control sputtering machine, it is first
Sputter cavity background pressure is evacuated to 0.9 × 10 by first vacuum-pumping system-5After torr, using argon gas as working gas, pass through
Choke valve will be passed through argon gas and control the operating pressure of sputter cavity to be 5 × 10-3Torr, first with D/C power sputter first layer 800nm
Thick Mo films, then the CIGS of evaporation manufacture second layer 2000nm thickness absorbs layer film altogether, is then coated with third layer film, with
Sputter cavity background pressure is evacuated to 0.9 × 10 by vacuum-pumping system-5After torr, using argon gas as working gas, through section
Stream valve will be passed through argon gas and control the operating pressure of sputter cavity to be 5 × 10-3Torr, sputter process, system are carried out with RF powers
Film thickness 150nm or so transparent buffer layer oxidation zinc-sulfur membrane is obtained, the 4th layer is coated with using pulsed DC source and AZO targets
Nesa coating thick 1000nm, that is, the film for completing the primary structure of CIGS solar cells makes, wire mark the superiors silver paste
Conversion efficiency test is carried out after electrode.
Wherein dispersant is 22g/L aqueous sodium polyacrylate.
Embodiment 4：
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 10.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, the third oxide is silica 0.1wt%.
Remaining be the same as Example 1.
Embodiment 5：
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 25.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, the third oxide is silica 1.0wt%.
Remaining be the same as Example 2.
Embodiment 6：
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 45.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, the third oxide is silica 2.0wt%.
Remaining be the same as Example 3.
Embodiment 7：
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 10.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, the third oxide is bismuth oxide 0.1wt%.
Remaining be the same as Example 1.
Embodiment 8:
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 20.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, the third oxide is bismuth oxide 1.0wt%.
Remaining be the same as Example 2.
Embodiment 9:
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 45.0wt%, the third oxygen in zinc oxide
Compound is bismuth oxide 2.0wt%.
Remaining be the same as Example 3.
Embodiment 10:
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 10.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, the third oxide is vanadium oxide 0.1wt%.
Remaining be the same as Example 1.
Embodiment 11:
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 25.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, the third oxide is vanadium oxide 1.0wt%.
Remaining be the same as Example 2.
Embodiment 12:
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 45.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, the third oxide is vanadium oxide 2.0wt%.
Remaining be the same as Example 3.
Embodiment 13：
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 10.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, the third oxide is aluminum oxide 0.1wt%.
Remaining be the same as Example 1.
Embodiment 14：
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 20.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, the third oxide is aluminum oxide 1.0wt%.
Remaining be the same as Example 2.
Embodiment 15：
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 45.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, the third oxide is aluminum oxide 2.0wt%.
Remaining be the same as Example 3.
Embodiment 16：
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 10.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, the third oxide is gallium oxide 0.1wt%.
Remaining be the same as Example 1.
Embodiment 17:
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 20.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, the third oxide is gallium oxide 1.0wt%.
Remaining be the same as Example 2.
Embodiment 18:
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 45.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, the third oxide is gallium oxide 2.0wt%.
Remaining be the same as Example 3.
Embodiment 19:
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 10.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, the third oxide is boron oxide 0.1wt%.
Remaining be the same as Example 1.
Embodiment 20:
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 25.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, the third oxide is boron oxide 1.0wt%.
Remaining be the same as Example 2.
Embodiment 21:
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 45.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, the third oxide is any one in boron oxide 2.0wt%.
Remaining be the same as Example 3.
Embodiment 22：
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 8.0wt% formation powder materials in zinc oxide
Material, then be sufficiently mixed with zirconia ball, pure water, dispersant grinding, its mass ratio is：Dusty material:Zirconia ball:Pure water:Point
Powder=0.9:2.8:0.26:0.005；Grinding forms slurry after 10 hours, then pours into slurry in porous mould, passes through
After the drying of 15 hours, the solid density that demoulding formation multivariant oxide is mixed with sulfide is 5.0 g/cm3Idiosome, then
By 900 DEG C and the sintering of 15 hours, that is, form sputter high density target idiosome, it is cleaved with surface grinding into vacuum magnetic control
Sputter target, target density is measured with Archimedian method；Using glass as base material, it is put into vacuum magnetic control sputtering machine, first very
Sputter cavity background pressure is evacuated to 0.7 × 10 by empty extract system-5After torr, using argon gas as working gas, through throttling
Valve will be passed through argon gas and control the operating pressure of sputter cavity to be 5 × 10-3Torr, first thick with D/C power sputter first layer 600nm
Mo films, then the CIGS of evaporation manufacture second layer 1900nm thickness absorbs layer film altogether, third layer film is then coated with, with vacuum
Sputter cavity background pressure is evacuated to 0.9 × 10 by extract system-5After torr, using argon gas as working gas, through choke valve
Argon gas, which will be passed through, controls the operating pressure of sputter cavity to be 3 × 10-3Torr, sputter process is carried out with RF powers, is made thin
Film thickness 100nm or so transparent buffer layer oxidation zinc-sulfur membrane, the 4th layer is coated with using pulsed DC source and AZO targets
Nesa coating thick 700nm, that is, the film for completing the primary structure of CIGS solar cells makes, wire mark the superiors silver paste electricity
Conversion efficiency test is extremely carried out afterwards.
Wherein dispersant is 19g/L aqueous sodium polyacrylate.
Embodiment 23：
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 15.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, then be sufficiently mixed with zirconia ball, pure water, dispersant grinding, its mass ratio is：Powder
Material:Zirconia ball:Pure water:Dispersant=1.1:2.9:0.22:0.005；Grinding forms slurry after 18 hours, then by slurry
Pour into porous mould, after the drying of 30 hours, the solid density that demoulding formation multivariant oxide is mixed with sulfide
For 5.2 g/cm3Idiosome, then by 1100 DEG C and the sintering of 15 hours, that is, form sputter high density target idiosome, pass through
Cutting, into vacuum magnetic control sputtering plating target, target density is measured with Archimedian method with surface grinding；Using glass as base material, it is put into
In vacuum magnetic control sputtering machine, sputter cavity background pressure is evacuated to 0.8 × 10 by vacuum-pumping system first-5After torr, argon is utilized
Gas will be passed through argon gas as working gas, through choke valve and control the operating pressure of sputter cavity to be 4 × 10-3Torr, first with DC
Mo films thick power supply sputter first layer 700nm, then the CIGS of evaporation manufacture second layer 2000nm thickness absorbs layer film altogether, connects
And be coated with third layer film, sputter cavity background pressure is evacuated to 0.9 × 10 with vacuum-pumping system-5After torr, argon gas is utilized
As working gas, it will be passed through argon gas through choke valve and control the operating pressure of sputter cavity to be 3 × 10-3Torr, with RF power supplys
Power carries out sputter process, film thickness 140nm or so transparent buffer layer oxidation zinc-sulfur membrane is made, the 4th layer uses pulse
D/C power and AZO targets are coated with the thick nesa coatings of 700nm, that is, complete the film system of the primary structure of CIGS solar cells
Make, conversion efficiency test is carried out after wire mark the superiors ag paste electrode.
Wherein dispersant is 21g/L aqueous sodium polyacrylate.
Wherein the third oxide is silica 2.2wt%.
Embodiment 24：
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 35.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, then be sufficiently mixed with zirconia ball, pure water, dispersant grinding, its mass ratio is：Powder
Material:Zirconia ball:Pure water:Dispersant=0.6:2.0:0.40:0.005；Grinding forms slurry after 14 hours, then by slurry
Pour into porous mould, after the drying of 20 hours, the solid density that demoulding formation multivariant oxide is mixed with sulfide
For 5.2 g/cm3Idiosome, then by 800 DEG C and the sintering of 15 hours, that is, sputter high density target idiosome is formed, through cutting
Cut with surface grinding into vacuum magnetic control sputtering plating target, target density is measured with Archimedian method；Using glass as base material, it is put into true
In empty magnetron, sputter cavity background pressure is evacuated to 0.9 × 10 by vacuum-pumping system first-5After torr, argon gas is utilized
As working gas, it will be passed through argon gas through choke valve and control the operating pressure of sputter cavity to be 2 × 10-3Torr, first with DC electricity
Mo films thick source sputter first layer 500nm, then the CIGS of evaporation manufacture second layer 2000nm thickness absorbs layer film altogether, then
Third layer film is coated with, sputter cavity background pressure is evacuated to 0.8 × 10 with vacuum-pumping system-5After torr, worked as using argon gas
Make working gas, will be passed through argon gas through choke valve controls the operating pressure of sputter cavity to be 2 × 10-3Torr, with RF power supply work(
Rate carries out sputter process, film thickness 130nm or so transparent buffer layer oxidation zinc-sulfur membrane is made, the 4th layer uses pulse DC
Power supply and AZO targets are coated with the thick nesa coatings of 1000nm, that is, complete the film system of the primary structure of CIGS solar cells
Make, conversion efficiency test is carried out after wire mark the superiors ag paste electrode.
Wherein dispersant is 22g/L aqueous sodium polyacrylate.
Wherein the third oxide is bismuth oxide 0.8wt%.
Embodiment 25：
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 40.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, then be sufficiently mixed with zirconia ball, pure water, dispersant grinding, its mass ratio is：Powder
Material:Zirconia ball:Pure water:Dispersant=1.1:3.2:0.26:0.005；Grinding forms slurry after 10 hours, then by slurry
Pour into porous mould, after the drying of 20 hours, the solid density that demoulding formation multivariant oxide is mixed with sulfide
For 5.2 g/cm3Idiosome, then by 900 DEG C and the sintering of 17 hours, that is, sputter high density target idiosome is formed, through cutting
Cut with surface grinding into vacuum magnetic control sputtering plating target, target density is measured with Archimedian method；Using glass as base material, it is put into true
In empty magnetron, sputter cavity background pressure is evacuated to 0.7 × 10 by vacuum-pumping system first-5After torr, argon gas is utilized
As working gas, it will be passed through argon gas through choke valve and control the operating pressure of sputter cavity to be 3 × 10-3Torr, first with DC electricity
Mo films thick source sputter first layer 600nm, then the CIGS of evaporation manufacture second layer 1700nm thickness absorbs layer film altogether, then
Third layer film is coated with, sputter cavity background pressure is evacuated to 0.9 × 10 with vacuum-pumping system-5After torr, worked as using argon gas
Make working gas, will be passed through argon gas through choke valve controls the operating pressure of sputter cavity to be 4 × 10-3Torr, with RF power supply work(
Rate carries out sputter process, film thickness 110nm or so transparent buffer layer oxidation zinc-sulfur membrane is made, the 4th layer uses pulse DC
Power supply and AZO targets are coated with the thick nesa coatings of 700nm, that is, complete the film system of the primary structure of CIGS solar cells
Make, conversion efficiency test is carried out after wire mark the superiors ag paste electrode.
Wherein dispersant is 16g/L aqueous sodium polyacrylate.
Wherein the third oxide is vanadium oxide 1.5wt%.
Embodiment 26:
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 35.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, then be sufficiently mixed with zirconia ball, pure water, dispersant grinding, its mass ratio is：Powder
Material:Zirconia ball:Pure water:Dispersant=0.8:3.5:0.26:0.005；Grinding forms slurry after 3 hours, then by slurry
Pour into porous mould, after the drying of 10 hours, the solid density that demoulding formation multivariant oxide is mixed with sulfide
For 4.8 g/cm3Idiosome, then by 1300 DEG C and the sintering of 26 hours, that is, form sputter high density target idiosome, pass through
Cutting, into vacuum magnetic control sputtering plating target, target density is measured with Archimedian method with surface grinding；Using glass as base material, it is put into
In vacuum magnetic control sputtering machine, sputter cavity background pressure is evacuated to 0.7 × 10 by vacuum-pumping system first-5After torr, argon is utilized
Gas will be passed through argon gas as working gas, through choke valve and control the operating pressure of sputter cavity to be 2 × 10-3Torr, first with DC
Mo films thick power supply sputter first layer 500nm, then the CIGS of evaporation manufacture second layer 1500nm thickness absorbs layer film altogether, connects
And be coated with third layer film, sputter cavity background pressure is evacuated to 0.7 × 10 with vacuum-pumping system-5After torr, argon gas is utilized
As working gas, it will be passed through argon gas through choke valve and control the operating pressure of sputter cavity to be 2 × 10-3Torr, with RF power supplys
Power carries out sputter process, film thickness 80nm or so transparent buffer layer oxidation zinc-sulfur membrane is made, the 4th layer uses pulse
D/C power and AZO targets are coated with the thick nesa coatings of 600nm, that is, complete the film system of the primary structure of CIGS solar cells
Make, conversion efficiency test is carried out after wire mark the superiors ag paste electrode.
Wherein dispersant is 20g/L aqueous sodium polyacrylate.
Wherein the third oxide is aluminum oxide 0.6wt%.
Embodiment 27:
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 25.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, then be sufficiently mixed with zirconia ball, pure water, dispersant grinding, its mass ratio is：Powder
Material:Zirconia ball:Pure water:Dispersant=1.0:3.0:0.25:0.005；Grinding forms slurry after 14 hours, then by slurry
Pour into porous mould, after the drying of 24 hours, the solid density that demoulding formation multivariant oxide is mixed with sulfide
For 5.1 g/cm3Idiosome, then by 1000 DEG C and the sintering of 5 hours, that is, sputter high density target idiosome is formed, through cutting
Cut with surface grinding into vacuum magnetic control sputtering plating target, target density is measured with Archimedian method；Using glass as base material, it is put into true
In empty magnetron, sputter cavity background pressure is evacuated to 0.6 × 10 by vacuum-pumping system first-5After torr, argon gas is utilized
As working gas, it will be passed through argon gas through choke valve and control the operating pressure of sputter cavity to be 1 × 10-3Torr, first with DC electricity
Mo films thick source sputter first layer 400nm, then the CIGS of evaporation manufacture second layer 1300nm thickness absorbs layer film altogether, then
Third layer film is coated with, sputter cavity background pressure is evacuated to 0.6 × 10 with vacuum-pumping system-5After torr, worked as using argon gas
Make working gas, will be passed through argon gas through choke valve controls the operating pressure of sputter cavity to be 1 × 10-3Torr, with RF power supply work(
Rate carries out sputter process, film thickness 60nm or so transparent buffer layer oxidation zinc-sulfur membrane is made, the 4th layer uses pulse DC
Power supply and AZO targets are coated with the thick nesa coatings of 500nm, that is, complete the film system of the primary structure of CIGS solar cells
Make, conversion efficiency test is carried out after wire mark the superiors ag paste electrode.
Wherein dispersant is 15g/L aqueous sodium polyacrylate.
Wherein the third oxide is gallium oxide 0.08wt%.
Embodiment 28:
A kind of method for preparing cushion zinc oxide sulphur target, will add zinc sulphide 50.0wt% in zinc oxide, continue to add
The third oxide formation dusty material, then be sufficiently mixed with zirconia ball, pure water, dispersant grinding, its mass ratio is：Powder
Material:Zirconia ball:Pure water:Dispersant=1.5:4.0:0.35:0.005；Grinding forms slurry after 26 hours, then by slurry
Pour into porous mould, after the drying of 40 hours, the solid density that demoulding formation multivariant oxide is mixed with sulfide
For 5.5 g/cm3Idiosome, then by 1500 DEG C and the sintering of 26 hours, that is, form sputter high density target idiosome, pass through
Cutting, into vacuum magnetic control sputtering plating target, target density is measured with Archimedian method with surface grinding；Using glass as base material, it is put into
In vacuum magnetic control sputtering machine, sputter cavity background pressure is evacuated to 1.0 × 10 by vacuum-pumping system first-5After torr, argon is utilized
Gas will be passed through argon gas as working gas, through choke valve and control the operating pressure of sputter cavity to be 6 × 10-3Torr, first with DC
Mo films thick power supply sputter first layer 900nm, then the CIGS of evaporation manufacture second layer 2200nm thickness absorbs layer film altogether, connects
And be coated with third layer film, sputter cavity background pressure is evacuated to 1.0 × 10 with vacuum-pumping system-5After torr, argon gas is utilized
As working gas, it will be passed through argon gas through choke valve and control the operating pressure of sputter cavity to be 6 × 10-3Torr, with RF power supplys
Power carries out sputter process, film thickness 180nm or so transparent buffer layer oxidation zinc-sulfur membrane is made, the 4th layer uses pulse
D/C power and AZO targets are coated with the thick nesa coatings of 1200nm, that is, complete the film of the primary structure of CIGS solar cells
Make, conversion efficiency test is carried out after wire mark the superiors ag paste electrode.
Wherein dispersant is 25g/L aqueous sodium polyacrylate.
Wherein the third oxide is boron oxide 2.2wt%.
Comparative example 1：
The method for preparing cushion zinc oxide target in the prior art, by pure zinc oxide, needed for being fabricated to using pressure sintering
Target.Target density is measured with Archimedian method.Using glass as base material, it is put into vacuum magnetic control sputtering machine, first vacuum suction
Sputter cavity background pressure is evacuated to 0.7 × 10 by system-5-0.9×10-5After torr, using argon gas as working gas, pass through
Choke valve will be passed through argon gas and control the operating pressure of sputter cavity to be 3 × 10-3Torr, first with D/C power sputter first layer 500nm
Thick Mo films, then the CIGS of evaporation manufacture second layer 2000nm thickness absorbs layer film altogether, is then coated with third layer film, with
Sputter cavity background pressure is evacuated to 0.7 × 10 by vacuum-pumping system-5-0.9×10-5After torr, using argon gas as work
Gas, will be passed through argon gas through choke valve and controls the operating pressure of sputter cavity to be 2 × 10-3Torr, is carried out with RF powers
Sputter process, is made film thickness 100nm or so transparent buffer layer zinc-oxide film, the 4th layer using pulsed DC source and
AZO targets are coated with the thick nesa coatings of 800nm, that is, the film for completing the primary structure of CIGS solar cells makes, wire mark
Conversion efficiency test is carried out after the superiors' ag paste electrode.
The performance of transparent conductive zinc oxide film is as shown in the table made from each embodiment and comparative example：
New composition zinc oxide sulphur target energy made from the filling forming method that the present invention is used is can be seen that from upper table result
Target density is enough effectively improved, and made CIGS thin film solar cell can improve conversion efficiency, and the target of the present invention
Material density and conversion efficiency are substantially better than embodiment 22（Zinc sulphide ratio over range）, embodiment 23（The third oxide ratios
Over range）, embodiment 24（Dusty material, zirconia ball, pure water, the ratio over range of dispersant）, embodiment 25（Polyacrylic acid
The concentration over range of sodium water solution）, embodiment 26（Target preparation technology parameter over range）, embodiment 27（Sputtering process parameter
Over range）, embodiment 28（Whole technological parameter over range, comparative example 1（Prior art）, it is seen that each operation stage of the invention
There is substantial connection with the target density and conversion efficiency of preparation, employ specific preparation technology of the invention, then by addition
The third oxide results in the target of greater density and high conversion efficiency is subsequently made in zinc oxide and zinc sulphide
CIGS batteries.
Claims (1)
1. a kind of method for preparing cushion zinc oxide sulphur target, it is characterized in that：
Will in zinc oxide add zinc sulphide 10.0-45.0wt%, or continue add the third oxide formation dusty material, then with
Zirconia ball, pure water, dispersant grinding are sufficiently mixed, and its mass ratio is：Dusty material:Zirconia ball:Pure water:Dispersant=
0.8-1.2:2.5-3.5:0.20-0.30:0.005；Grinding forms slurry after 4-24 hours, and slurry then is poured into porous mould
In tool, after the drying of 12-36 hours, the solid density that demoulding formation multivariant oxide is mixed with sulfide is 5.0-5.2
g/cm3Idiosome, then by 800-1200 DEG C and the sintering of 3-24 hours, that is, form sputter high density target idiosome, pass through
Cutting, into vacuum magnetic control sputtering plating target, target density is measured with Archimedian method with surface grinding；Using glass as base material, it is put into
In vacuum magnetic control sputtering machine, sputter cavity background pressure is evacuated to 0.7 × 10 by vacuum-pumping system first-5-0.9×10-5
After torr, using argon gas as working gas, through choke valve will be passed through argon gas control the operating pressure of sputter cavity for 2 ×
10-3-5×10-3Torr, first with Mo films thick D/C power sputter first layer 500-800nm, then evaporation manufactures the second layer altogether
CIGS thick 1500-2000nm absorbs layer film, is then coated with third layer film, with vacuum-pumping system by sputter cavity background
Pressure is evacuated to 0.7 × 10-5-0.9×10-5After torr, using argon gas as working gas, argon gas control will be passed through through choke valve
The operating pressure of sputter cavity processed is 2 × 10-3-5×10-3Torr, sputter process is carried out with RF powers, film is made thick
80-150nm transparent buffer layers oxidation zinc-sulfur membrane is spent, the 4th layer is coated with 600-1000nm using pulsed DC source and AZO targets
Thick nesa coating, that is, the film for completing the primary structure of CIGS solar cells makes, after wire mark the superiors ag paste electrode
Carry out conversion efficiency test；
Dispersant is 18-22g/L aqueous sodium polyacrylate；
The third oxide is silica 0.1-2.0wt%, bismuth oxide 0.1-2.0wt%, vanadium oxide 0.1-2.0wt%, aluminum oxide
Any one in 0.1-2.0wt%, gallium oxide 0.1-2.0wt%, boron oxide 0.1-2.0wt%.
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| CN106676487B (en) * | 2016-10-09 | 2019-03-08 | 宁波森利电子材料有限公司 | A kind of zinc oxide-based ceramic sputtering target material and its preparation method and application |
| CN108658472A (en) * | 2017-03-31 | 2018-10-16 | 深圳市景创科技电子有限公司 | A kind of preparation method of intelligent glass cathodic electrochromic layer Coating Materials |
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| "Zn(O,S) layers for chalcoyprite solar cells sputtered from a single target";A. Grimm et al.;《EPJ Photovoltaics》;20121231;第3卷;摘要，第30302-2页左栏第1-2段，第30302-3页表2 * |
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