CN104561913B - A kind of low-resistivity CIGS quaternary alloy sputtering target material and preparation method thereof - Google Patents
A kind of low-resistivity CIGS quaternary alloy sputtering target material and preparation method thereof Download PDFInfo
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- CN104561913B CN104561913B CN201410775474.3A CN201410775474A CN104561913B CN 104561913 B CN104561913 B CN 104561913B CN 201410775474 A CN201410775474 A CN 201410775474A CN 104561913 B CN104561913 B CN 104561913B
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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
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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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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Abstract
The invention discloses a kind of low-resistivity CIGS quaternary alloy sputtering target material and preparation method thereof, the thing that the target includes mutually has Cu (In0.7Ga0.3)Se2, CuInSe2And Cu2Cu (In in Se phases, the thing phase of the target0.7Ga0.3)Se2Thing mutually accounts for more than 95%, CuInSe of thing phase summation2And Cu2Se phases account for the 1~5% of total thing phase.The preparation method of the sputtering target material of the present invention includes：Prepared by powder, powder mixing, the process such as powder metallurgy sintered, and prepared by the powder include CuIn0.7Ga0.3Se2The preparation of single-phase alloy powder, the CuIn0.7Ga0.3Se2Prepared by the method that single-phase alloy powder is synthesized by vacuum reaction, vacuum >=10‑1Pa, reaction temperature is at 500~700 DEG C, and heating rate is not more than 5 DEG C/min.The sputtering target of the present invention, resistivity is low, and consistency is high, and crystallite dimension fine uniform can carry out intermediate frequency or d.c. sputtering, be greatly improved the sputtering rate of CIGS thin-film, while saving equipment investment cost.
Description
Technical field
The invention belongs to powder metallurgical technology, and in particular to a kind of low-resistivity CIGS quaternary alloy sputtering target
Material and preparation method thereof.
Background technology
CIGS (abbreviation CIGS) film occupies various thin-film solar cells first places with maximum conversion 20.3%, this
The maximum conversion record only poor 0.1%, and the characteristic not decayed with high conversion with the time, quilt of one efficiency and polysilicon
It is considered most there is the thin-film solar cells of development potentiality.Sputtering technology is the main flow system of current CIGS batteries sun light absorbing layer
Make technique, foreign countries are very ripe using sputtering-large-scale application of the selenizing method technique in FPD, but serious ask
Topic is to need to use H2Se realizes selenizing, and H by high-temperature heating2Se has severe toxicity and severe corrosive.
Because the CIGS quaternary target electric conductivity developed both at home and abroad at present is too poor, resistivity is hundreds of even Shang kilohm li
Rice, can only use rf magnetron sputtering plated film.America and Europe is used for the industrialization sputter production line for producing CIGS batteries, is worth at least thousands of
Ten thousand, it is at most more than one hundred million or several hundred million yuans.If CIGS targets are conductive, magnetically controlled DC sputtering plated film, sputtering rate can be used
By more than ten times that are that radio frequency magnetron splashes, and sputtering equipment expense is greatly reduced.Therefore the research and development of conduction CIGS targets, before it is applied
Scape will be very good.If research and development make a breakthrough, CIGS targets are expected to obtain (i.e. 3.75 hundred million U.S.s of solar absorption layer material 25%
Member), even more than 50% the market share.The preparation method of disclosed CIGS quaternary alloys target mainly has two in the prior art
Kind：One kind is dry method[1~4], i.e., by the way that above-mentioned four kinds of high purity elemental powder are carried out into mechanical mixture, then carry out cold, hot pressure and be made
Type prepares alloy target material either by the way that above-mentioned four kinds of simple substance alloy powders are mixed in synthesis under vacuum conditions two-by-two
Between compound, then again by intermediate compound by CIGS alloys stoichiometric proportion mix carry out cold, hot pressure type is made；Other one
The method of kind is wet method[5], i.e., four kinds of simple substance mixed under organic environment, and carries out synthetic reaction form single
CIGS phases, then carry out granulating powders again, hot and cold compressing.The above-mentioned electric conductivity for not considering target in the prior art.
The present inventor proposes a kind of low-resistivity CIGS quaternary alloy sputtering target material and preparation method thereof by concentrating on studies, should
Target can be used for intermediate frequency or d.c. sputtering, and promoting the use of for the target is greatly improved sputtering rate, and will substantially reduce
Equipment investment, while the also production cost for reduction CIGS thin-film, popularization and application establish solid in photovoltaic industry as early as possible
Basis.
The above can be obtained from below with reference to document：
[1] Chen Hui, Zhang Jiao, Wang Jun .CuInGaSe2Solar energy film and its development of target technology of preparing and prospect [J] work(
Energy material, 2009 (40) supplementary issues, 924-928. [2] Zhang Leng, Zhang Weijia, Song Dengyuan opens the vacuum system of the CIGS thin-films such as brightness
Standby technique and target present Research [J] functional materials .2013 (44), 14:1990-1994. [3] Zhuan great Ming, draws a bow, and opens the such as peaceful
CIGS or Cu-In-Al-Se solar cell absorption layer target material and preparation method thereof [P] Tsing-Hua University .CN101397647B.
[4] Zhu Shihui, Zhu Shiming, a kind of preparation method of copper-indium-gallium-selenium alloy [P] Guangdong guide's exotic material shares of Zhu Liu are limited
Company .CN102071329A. [5] bell moistens the intelligent limited public affairs of Hao Optoelectronics Technology share of preparation method [P] of text CIGS target materials
Take charge of .CN 102199751A.
The content of the invention
It is an object of the invention to provide a kind of low-resistivity CIGS quaternary alloy sputtering target material and preparation method thereof,
The sputtering target, resistivity is low, and consistency is high, and crystallite dimension fine uniform can carry out intermediate frequency or d.c. sputtering, can carry significantly
The sputtering rate of high CIGS thin-film, while saving equipment investment cost.
The thing that the sputtering target material of the present invention is achieved in that the target and included mutually has Cu (In0.7Ga0.3)Se2,
CuInSe2And Cu2Cu (In in Se phases, the thing phase of the target0.7Ga0.3)Se2Thing mutually accounts for more than the 95% of thing phase summation,
CuInSe2And Cu2Se phases account for the 1~5% of total thing phase.
The room temperature resistivity of the target is between 0~100 Ω cm.
The room temperature resistivity of the target is between 0~50 Ω cm.
The consistency of the target is not less than 97%.
The average grain size of the target is 10~50 μm.
The present invention sputtering target material preparation method be achieved in that including：Prepared by powder, powder mixing, powder smelting
The processes such as gold sintering, prepared by the powder include CuIn0.7Ga0.3Se2The preparation of single-phase alloy powder, the CuIn0.7Ga0.3Se2
Prepared by the method that single-phase alloy powder is synthesized by vacuum reaction, vacuum >=10-1Pa, reaction temperature rises at 500~700 DEG C
Warm speed is not more than 5 DEG C/min.
Prepared by the powder also include In2Se3、Ga2Se3And Cu2Se single-phase alloys powder and In0.7Ga0.3Se2Ternary is closed
The preparation at bronze end, the In2Se3、Ga2Se3And Cu2It is prepared by the method that the single-phase phase alloy powder of Se is synthesized by vacuum reaction,
Vacuum >=10-1Pa, reaction temperature is at 400~600 DEG C, and heating rate is not more than 5 DEG C/min, and soaking time is 3~5h；It is described
In0.7Ga0.3Se2Prepared by the method that manganese ternary alloy powder is synthesized by vacuum reaction, vacuum >=10-1Pa, reaction temperature is 500
~700 DEG C, heating rate is not more than 1 DEG C/min, and soaking time is 5~20h.
The powder mixing includes In0.7Ga0.3Se2Manganese ternary alloy powder and Cu powder mixing after again with CuIn0.7Ga0.3Se2
Quaternary single-phase alloy powder is mixed after stoichiometrically matching, In0.7Ga0.3Se2With Cu mixed-powder weight summation
No more than CuIn0.7Ga0.3Se2The weight of quaternary single-phase alloy powder.
The powder mixing includes In2Se3、Ga2Se3And Cu2Tri- kinds of binary single-phase alloy powder of Se and CuIn0.7Ga0.3Se2
Quaternary single-phase alloy powder is mixed after stoichiometrically matching, In2Se3、Ga2Se3And Cu2Tri- kinds of binary single-phase alloys of Se
Powder weight summation is not more than CuIn0.7Ga0.3Se2The weight of quaternary single-phase alloy powder.
It is described powder metallurgy sintered for discharge plasma sintering or vacuum hot-pressed sintered technology, the powder metallurgy sintered work
The sintering temperature of skill is 400~800 DEG C, and sintering pressure is 20~40MPa, and sintering time is 10mins~3h.
The present invention has prepared the single-phase alloy powder of binary, ternary and quaternary by the method for synthesizing vacuum reaction respectively
End, simple quaternary single-phase alloy powder resistivity is higher, and the target resistivity being molded with its direct pressing is 50~100
Ω cm, and In2Se、Cu2The resistivity of Se binary single-phase alloy powder and Cu powder is relatively low, by by quaternary alloy powder with
Above-mentioned two-alloy powder or manganese ternary alloy powder and Cu powder are stoichiometrically mixed, and pass through suitable forming and sintering work
Skill, can both be obtained with CuIn0.7Ga0.3Se2Alloy target material based on phase, can ensure that target has sufficiently low resistance again
Rate, realizes intermediate frequency or d.c. sputtering, improves sputtering yield, reduces film production cost.At the same time, the target also has higher
The heterogeneous microstructure of consistency and fine uniform, the film thickness uniformity for film improves a lot.
Brief description of the drawings
Fig. 1 is the embodiment of the present invention and the XRD analysis result of comparative example.
Specific embodiment
The present invention is further illustrated below in conjunction with the accompanying drawings, but the present invention is not any limitation as in any way, base
In present invention teach that any changes and modifications made, belong to protection scope of the present invention.
Low-resistivity CIGS quaternary alloy sputtering target material of the present invention, the thing that the target includes mutually has Cu
(In0.7Ga0.3)Se2, CuInSe2And Cu2Cu (In in Se phases, the thing phase of the target0.7Ga0.3)Se2Thing mutually accounts for thing phase summation
More than 95%, In2Se3And Cu2Se phases account for the 1~5% of total thing phase.
The room temperature resistivity of the target is between 0~100 Ω cm.
The room temperature resistivity of the target is between 0~50 Ω cm.
The consistency of the target is not less than 97%.
The average grain size of the target is 10~50 μm.
The present invention is prepared for the copper-indium-gallium-selenium alloy target of above-mentioned low-resistivity, preparation method bag by following preparation methods
Include：Prepared by powder, powder mixing, the process such as powder metallurgy sintered, and prepared by the powder include CuIn0.7Ga0.3Se2Single-phase alloy
The preparation of powder, the CuIn0.7Ga0.3Se2Prepared by the method that single-phase alloy powder is synthesized by vacuum reaction, vacuum >=10-1Pa, reaction temperature is at 500~700 DEG C, and heating rate is not more than 5 DEG C/min.
Prepared by the powder also include In2Se3、Ga2Se3And Cu2Se single-phase alloys powder and In0.7Ga0.3Se2Ternary is closed
The preparation at bronze end, the In2Se3、Ga2Se3And Cu2It is prepared by the method that the single-phase phase alloy powder of Se is synthesized by vacuum reaction,
Vacuum >=10-1Pa, reaction temperature is at 400~600 DEG C, and heating rate is not more than 5 DEG C/min, and soaking time is 3~5h, described
In0.7Ga0.3Se2Prepared by the method that manganese ternary alloy powder is synthesized by vacuum reaction, vacuum >=10-1Pa, reaction temperature is 500
~700 DEG C, heating rate is not more than 1 DEG C/min, and soaking time is 5~20h.
The powder mixing includes In0.7Ga0.3Se2Manganese ternary alloy powder and Cu powder mixing after again with CuIn0.7Ga0.3Se2
Quaternary single-phase alloy powder is mixed after stoichiometrically matching, In0.7Ga0.3Se2With Cu mixed-powder weight summation
No more than CuIn0.7Ga0.3Se2The weight of quaternary single-phase alloy powder.
The powder mixing includes In2Se3、Ga2Se3And Cu2Tri- kinds of binary single-phase alloy powder of Se and CuIn0.7Ga0.3Se2
Quaternary single-phase alloy powder is mixed after stoichiometrically matching, In2Se3、Ga2Se3And Cu2Tri- kinds of binary single-phase alloys of Se
Powder weight summation is not more than CuIn0.7Ga0.3Se2The weight of quaternary single-phase alloy powder.
It is described powder metallurgy sintered for discharge plasma sintering or vacuum hot-pressed sintered technology, the powder metallurgy sintered work
The sintering temperature of skill is 400~800 DEG C, and sintering pressure is 20~40MPa, and sintering time is 10mins~3h.
With reference to preparation side of the specific embodiment to heretofore described low-resistivity CIGS quaternary alloy target
Method is specifically described.
Embodiment 1：CIGS quaternary alloy target of the present invention is prepared as follows：
(1) material powder prepares：CuIn is stoichiometrically prepared from 5N and above high pure raw material powder0.7Ga0.3Se2
500 grams of quaternary mixed-powder, mixed-powder is enclosed within silica ware and 10 are evacuated down to-1Pa, then by closed quartz
Vessel be placed in Muffle furnace be heated to 650 DEG C be incubated 3~5 hours, heating rate be 1 DEG C/min, the type of cooling be stove it is cold.It will obtain
The single thing phase CuIn obtained0.7Ga0.3Se2Quaternary alloy powder prepares the alloy powder below 300 mesh by Mechanical Crushing mode；
The preparation of the material powder also includes In2Se3、Ga2Se3And Cu2The preparation of tri- kinds of binary single-phase alloy powder of Se, specifically
In2Se3The sintering temperature of alloy powder is 400~500 DEG C, and heating rate is 1 DEG C/min, is incubated 3~5 hours；Ga2Se3Alloy
The sintering temperature of powder is 500~700 DEG C, and heating rate is 1 DEG C/min, is incubated 3~5 hours；Cu2The sintering of Se alloy powders
Temperature is 500~600 DEG C, and heating rate is 1 DEG C/min, is incubated 3~5 hours；
(2) preparation of alloy target material：Vacuum heating-press sintering is carried out from the above-mentioned alloy powder prepared, sintering temperature is
600~700 DEG C, pressure is 25~35Mpa, and sintering time is 2~5h.
Embodiment 2:Difference from Example 1 is：
(1) preparation of the material powder also includes In2Se3、Ga2Se3And Cu2The system of tri- kinds of binary single-phase alloy powder of Se
It is standby, specific In2Se3The sintering temperature of alloy powder is 400~500 DEG C, and heating rate is 1 DEG C/min, is incubated 3~5 hours；
Ga2Se3The sintering temperature of alloy powder is 500~700 DEG C, and heating rate is 1 DEG C/min, is incubated 3~5 hours；Cu2Se alloys
The sintering temperature of powder is 500~600 DEG C, and heating rate is 1 DEG C/min, is incubated 3~5 hours；
(2) mixing of material powder：By CuIn0.7Ga0.3Se2Quaternary alloy powder and above-mentioned three kinds of binary single-phase alloy powder
End is according to CuIn0.7Ga0.3Se2Stoichiometric proportion is mixed, quaternary alloy powder and above-mentioned three kinds of two-alloy powder summations
Weight ratio be 4:1.
Embodiment 3：Difference from Example 1 is：The preparation of the material powder also includes the In0.7Ga0.3Se2
Prepared by the method that manganese ternary alloy powder is synthesized by vacuum reaction, vacuum >=10-1Pa, reaction temperature rises at 500~700 DEG C
Warm speed is not more than 1 DEG C/min, and soaking time is 5~20h.By above-mentioned In0.7Ga0.3Se2Manganese ternary alloy powder and Cu powder are mixed
After conjunction again with CuIn0.7Ga0.3Se2Quaternary single-phase alloy powder is mixed after stoichiometrically matching, CuIn0.7Ga0.3Se2
Quaternary single-phase alloy powder and In0.7Ga0.3Se2Ratio with Cu mixed-powder weight summation is 3:1.
Embodiment 4：Difference from Example 1 is that the sintering process sinters (SPS) using discharge plasma,
Sintering temperature is 400~600 DEG C, and vacuum is 10-1Pa, the sintered heat insulating time is 5~10mins.
Comparative example 1：Difference from Example 1 is that the quaternary alloy powder is to be prepared via a method which to obtain：
(1) quaternary alloy ingot casting is obtained using the method for vacuum melting；(2) Mechanical Crushing is carried out to ingot casting and obtains quaternary alloy powder.
Comparative example 2：Difference from Example 1 is that the quaternary alloy powder is the simple substance Cu from more than 5N,
In, Ga, Se powder press CuIn0.7Ga0.3Se2Stoichiometric proportion carry out mechanical mixture acquisition.
Analysis survey is carried out to the density of target, microstructure and resistivity in above-described embodiment and comparative example respectively
Examination, phase content analysis carries out quantitative analysis using K values method, and concrete outcome is as shown in table 1.
The performance comparision of the embodiment of the present invention of table 1 and comparative example
| Consistency | Resistivity (Ω cm) | Average grain size (μm) | CuInSe2And Cu2The mutually total content of Se things | |
| Embodiment 1 | 98.5% | 65 | 38 | 1.5% |
| Embodiment 2 | 99.5% | 25 | 40 | 2.5% |
| Embodiment 3 | 98.0% | 7 | 15 | 4.2% |
| Embodiment 4 | 97.0% | 78 | 50 | 0 |
| Comparative example 1 | 98.0% | 1568 | 60 | 0 |
| Comparative example 2 | 98.0% | 1768 | 70 | 0 |
Claims (4)
1. a kind of preparation method of CIGS quaternary alloy sputtering target material, including：The preparation of material powder, the mixing of powder,
Sinter molding process, the thing that the target includes mutually has Cu (In0.7Ga0.3)Se2, CuInSe2And Cu2Se phases, the thing of the target
Cu (In in phase0.7Ga0.3)Se2Thing mutually accounts for more than 95%, CuInSe of thing phase summation2And Cu2Se phases account for the 1~5% of total thing phase；
The room temperature resistivity of the target is 7 Ω cm or 25 Ω cm or 65 Ω cm；The consistency of the target be 98% or
98.5% or 99.5%；The average grain size of the target is 15 μm or 38 μm or 40 μm, it is characterised in that：The raw material powder
Prepared by end include CuIn0.7Ga0.3Se2The preparation of single-phase alloy powder, the CuIn0.7Ga0.3Se2Single-phase alloy powder passes through true
Prepared by the method for sky reaction synthesis, vacuum >=10-1Pa, reaction temperature at 500~700 DEG C, heating rate be not more than 5 DEG C/
min；The preparation of the material powder also includes In2Se3、Ga2Se3And Cu2Se single-phase alloys powder and In0.7Ga0.3Se2Ternary
The preparation of alloy powder, the In2Se3、Ga2Se3And Cu2The method system that the single-phase phase alloy powder of Se is synthesized by vacuum reaction
It is standby, vacuum >=10-1Pa, reaction temperature is at 400~600 DEG C, and heating rate is not more than 5 DEG C/min, and soaking time is 3~5h,
The In0.7Ga0.3Se2Prepared by the method that manganese ternary alloy powder is synthesized by vacuum reaction, vacuum >=10-1Pa, reaction temperature
At 500~700 DEG C, heating rate is not more than 1 DEG C/min, and soaking time is 5~20h.
2. the preparation method of CIGS quaternary alloy sputtering target material according to claim 1, it is characterised in that：The powder
End mixing includes In0.7Ga0.3Se2Manganese ternary alloy powder and Cu powder mixing after again with CuIn0.7Ga0.3Se2Quaternary single-phase alloy powder
End is mixed after stoichiometrically matching, In0.7Ga0.3Se2It is not more than with Cu mixed-powder weight summation
CuIn0.7Ga0.3Se2The weight of quaternary single-phase alloy powder.
3. the preparation method of CIGS quaternary alloy sputtering target material according to claim 1, it is characterised in that：The powder
End mixing includes In2Se3、Ga2Se3And Cu2Tri- kinds of binary single-phase alloy powder of Se and CuIn0.7Ga0.3Se2Quaternary single-phase alloy powder
End is mixed after stoichiometrically matching, In2Se3、Ga2Se3And Cu2Tri- kinds of binary single-phase alloy powder weight summations of Se are not
More than CuIn0.7Ga0.3Se2The weight of quaternary single-phase alloy powder.
4. the preparation method of CIGS quaternary alloy sputtering target material according to claim 1, it is characterised in that：It is described to burn
It is discharge plasma sintering or vacuum hot-pressed sintered technology to tie process, and the sintering temperature of the powder metallurgical sintering process is 400
~800 DEG C, sintering pressure is 20~40MPa, and sintering time is 10mins~3h.
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| CN101260513A (en) * | 2008-04-23 | 2008-09-10 | 王东生 | Solar energy battery copper-indium-gallium-selenium film key target material and preparation method thereof |
| CN102741450A (en) * | 2009-11-13 | 2012-10-17 | 吉坤日矿日石金属株式会社 | Cu-in-ga-se quaternary alloy sputtering target |
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| CN101260513A (en) * | 2008-04-23 | 2008-09-10 | 王东生 | Solar energy battery copper-indium-gallium-selenium film key target material and preparation method thereof |
| CN102741450A (en) * | 2009-11-13 | 2012-10-17 | 吉坤日矿日石金属株式会社 | Cu-in-ga-se quaternary alloy sputtering target |
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