CN103819178B - A kind of preparation method of IGZO target - Google Patents
A kind of preparation method of IGZO target Download PDFInfo
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- CN103819178B CN103819178B CN201310669559.9A CN201310669559A CN103819178B CN 103819178 B CN103819178 B CN 103819178B CN 201310669559 A CN201310669559 A CN 201310669559A CN 103819178 B CN103819178 B CN 103819178B
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Abstract
The present invention relates to a kind of preparation method of target, particularly a kind of preparation method of high-performance IGZO target.Comprise the following steps: (1) is by Ga
2o
3nano-powder, ZnO nano powder and In
2o
3nano-powder is mixed to get IGZO powder by the even ball milling in atomic ratio In:Ga:Zn=1:1 ~ 5:1 ~ 5, and the PVA adding IGZO powder quality 1%-5% carries out granulation; (2) IGZO powder is loaded compression moulding under 40 ~ 80MPa in mould, by the biscuit shaping first time, post forming is carried out again with 200-300MPa, then release is carried out with 4-8MPa/ min, the biscuit of forming is taken out to normal pressure, (3) biscuit is placed in sintering oven sinters, sintering condition refers to and to heat up with the temperature rise rate not higher than 1 DEG C/min, to 1300 ~ 1550 DEG C of heat preservation sinterings 4 ~ 10 hours, 950 ~ 1050 DEG C are cooled to afterwards, Temperature fall afterwards by rate of temperature fall 0.5 ~ 1 DEG C/min; Obtain IGZO target.The present invention can prepare high-performance IGZO target (high-compactness, relative density >98%, high conductivity), makes up the blank that domestic high-performance IGZO target is manufactured.
Description
Technical field
The present invention relates to a kind of preparation method of target, particularly a kind of preparation method of high-performance IGZO target.
Background technology
By In(indium), Ga(gallium), Zn(zinc), O(oxygen) semiconductor material that forms for the pixel drive transistor (TFT: thin film transistor) of liquid-crystal display and OLED display, significantly can cut down the current consumption of these indicating meters.The homogeneity of traditional polycrystalline SiTFT is poor, complex manufacturing technology; Metal oxide IGZO TFT mobility is high, homogeneity good, transparent, manufacture craft simple, can meet the demand of large scale liquid crystal indicating meter and active organic electroluminescent better.Electronic mobility due to IGZO is approximately 20 ~ 50 times of a-Si TFT, improves the utilization ratio of backlight, therefore can realize more than 2 times of general T FT screen in resolving power.In addition the electronic mobility of IGZO exceedes 40 times of traditional material, and it also can reduce the time of response of LCD screen greatly like this.And the IGZO film of the overwhelming majority deposits gained by IGZO target as sputter, therefore, the development of manufacturing for above-mentioned field of high-performance IGZO target has very important pushing effect.
The preparation method of existing IGZO target mainly prepares IGZO powder by coprecipitation method, and then carry out granulation, suppress and sinter and obtain IGZO target, because coprecipitation method is when Determination of multiple metal elements (more than two kinds of elements) precipitates, precipitation can not be carried out simultaneously, cannot ensure fully precipitate and cause component proportions improper, cause the characteristic of powder activity that is unstable and powder can be lower, therefore the target relative density that the IGZO powder obtained by this method burns out is on the low side, substantially be all at 90-95%, the IGZO target (relative density >98%) of high relative density cannot be obtained.
Summary of the invention
The technical problem to be solved in the present invention is: the preparation method providing a kind of reliable IGZO target, the method can prepare high-performance IGZO target (relative density >98%, electroconductibility is good), make up the blank that domestic high-performance IGZO target is manufactured.
The technical scheme solved the problems of the technologies described above is: a kind of preparation method of IGZO target, comprises the following steps:
(1) by Ga
2o
3nano-powder, ZnO nano powder and In
2o
3nano-powder obtains IGZO powder by atomic ratio In:Ga:Zn=1:1 ~ 5:1 ~ 5 Homogeneous phase mixing, and the binding agent PVA then adding IGZO powder quality 1%-5% carries out granulation;
(2) IGZO powder is loaded compression moulding under 40 ~ 80MPa in mould, by the biscuit shaping first time, then carry out post forming with 200-300MPa, then carry out release with 4-8MPa/ min, to normal pressure, take out the biscuit of forming;
(3) biscuit is placed in sintering oven sinters, sintering condition refers to and to heat up with the temperature rise rate not higher than 1 DEG C/min, to 1300 ~ 1550 DEG C of heat preservation sinterings 4 ~ 10 hours, be cooled to 950 ~ 1050 DEG C by rate of temperature fall 0.5 ~ 1 DEG C/min afterwards, Temperature fall afterwards; Obtain IGZO target.
Further technical scheme of the present invention is: described first time is shaping is compression moulding in hydropress, and second time is shaping is compression moulding in cold isostatic press.
Described sintering sinters in the oxygen atmosphere of normal pressure-sintered stove.
The temperature rise rate of described sintering is 0.3-1 DEG C/min.
Described Ga
2o
3nano-powder, ZnO nano powder and In
2o
3the purity of nano-powder is more than 99.99%.
The present invention utilizes three kinds of polymolecularity oxidation powders to carry out abundant ball milling and mixes, namely abundant hybrid system is utilized to obtain the IGZO pelletizing of high sintering character and polymolecularity, then control is optimized to sintering process, make the dispersed and abundant sintering of various atoms metal, obtain highdensity IGZO target.The component proportions that before present method solves, coprecipitation method prepares IGZO powder cannot precisely control, and powder sintering activity is on the low side, the problem that the target relative density of acquisition is on the low side.
Adopt the present invention can prepare high-performance IGZO target (high-compactness, relative density >98%, high conductivity), make up the blank that domestic high-performance IGZO target is manufactured.
Below, the technical characteristic of the preparation method of a kind of IGZO target of the present invention is further described in conjunction with the embodiments.
Embodiment
Embodiment 1: by Ga
2o
3(gallium oxide) nano-powder, ZnO(zinc oxide) nano-powder and In
2o
3(Indium sesquioxide, specific surface area is 25m
2/ g) nano-powder by atomic ratio In:Ga:Zn=1:1:1 put into ball mill evenly ball milling be mixed to get IGZO(Indium sesquioxide gallium zinc) powder, then add the binding agent PVA(polyvinyl alcohol of IGZO powder quality 2%) carry out mist projection granulating; IGZO prilling powder is loaded in mould and suppresses with 50MPa in hydropress, by the biscuit shaping first time, in cold isostatic press, post forming is carried out again with 270MPa, after isostatic cool pressing terminates, carry out unloading press operation, during release, slow release is carried out, finally to normal pressure with 5MPa/min, and take out the biscuit of forming, obtain the IGZO biscuit of high-compactness (relative density 55%-60%).Be placed in the normal pressure-sintered stove of oxygen by the biscuit suppressed and sinter, sintering condition is for heating up with the temperature rise rate of 0.3 DEG C/min, to 1550 DEG C of heat preservation sinterings 4 hours, is cooled to 1000 DEG C afterwards, Temperature fall afterwards by rate of temperature fall 0.5 DEG C/min.Obtain the IGZO target that relative density is 98.4%.
Embodiment 2: by Ga
2o
3(gallium oxide) nano-powder, ZnO(zinc oxide) nano-powder and In
2o
3(Indium sesquioxide) nano-powder is put into the even ball milling of ball mill by atomic ratio In:Ga:Zn=1:1:2 and is mixed to get IGZO(Indium sesquioxide gallium zinc) powder, then add the binding agent PVA(polyvinyl alcohol of IGZO powder quality 4%) carry out mist projection granulating; IGZO prilling powder is loaded in mould and suppresses with 70MPa in hydropress, by the biscuit shaping first time, in cold isostatic press, post forming is carried out again with 250MPa, after isostatic cool pressing terminates, carry out unloading press operation, during release, slow release is carried out, finally to normal pressure with 8MPa/min, and take out the biscuit of forming, obtain the IGZO biscuit of high-compactness (relative density 55%-60%).Be placed in the normal pressure-sintered stove of oxygen by the biscuit suppressed and sinter, sintering condition is for heating up with the temperature rise rate of 0.5 DEG C/min, to 1500 DEG C of heat preservation sinterings 6 hours, is cooled to 1000 DEG C afterwards, Temperature fall afterwards by rate of temperature fall 0.5 DEG C/min.Obtain the IGZO target that relative density is 98%.
In described in various embodiments of the present invention
2o
3can be use chemical precipitation method to prepare polymolecularity, high purity (being better than 4N) and high sintering active nano In
2o
3powder, specific surface area is 10-30m
2/ g.Ga
2o
3the purity of nano-powder and ZnO nano powder is more than 99.99%, and specific surface area all requires 10-30m simultaneously
2/ g.Described mould can be square also can be other shapes.Described sintering oven also can adopt other can meet the sintering oven of sintering requirement.
Claims (4)
1. a preparation method for IGZO target, is characterized in that: comprise the following steps:
(1) by Ga
2o
3nano-powder, ZnO nano powder and In
2o
3nano-powder is put into the even ball milling of ball mill by atomic ratio In:Ga:Zn=1:1 ~ 5:1 ~ 5 and is mixed to get IGZO powder, and the binding agent PVA then adding IGZO powder quality 1%-5% carries out granulation; Described Ga
2o
3nano-powder, ZnO nano powder and In
2o
3the specific surface area of nano-powder is 10-30m
2/ g, purity is more than 99.99%;
(2) IGZO powder is loaded compression moulding under 40 ~ 80MPa in mould, by the biscuit shaping first time, then carries out post forming with 200-300MPa, then carry out release with 4-8MPa/ min, to normal pressure, take out the biscuit of forming,
(3) biscuit is placed in sintering oven sinters, sintering condition refers to and to heat up with the temperature rise rate not higher than 1 DEG C/min, to 1300 ~ 1550 DEG C of heat preservation sinterings 4 ~ 10 hours, be cooled to 950 ~ 1050 DEG C by rate of temperature fall 0.5 ~ 1 DEG C/min afterwards, Temperature fall afterwards; Obtain IGZO target.
2. the preparation method of a kind of IGZO target according to claim 1, is characterized in that: described first time is shaping is compression moulding in hydropress, and second time is shaping is compression moulding in cold isostatic press.
3. the preparation method of a kind of IGZO target as claimed in claim 1 or 2, is characterized in that: described sintering sinters in the oxygen atmosphere of normal pressure-sintered stove.
4. the preparation method of a kind of IGZO target as claimed in claim 1 or 2, is characterized in that: the temperature rise rate of described sintering is 0.3-1 DEG C/min.
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|---|---|---|---|
| CN201310669559.9A CN103819178B (en) | 2013-12-11 | 2013-12-11 | A kind of preparation method of IGZO target |
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| CN201310669559.9A CN103819178B (en) | 2013-12-11 | 2013-12-11 | A kind of preparation method of IGZO target |
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| CN103819178B true CN103819178B (en) | 2015-07-29 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105239047A (en) * | 2015-10-08 | 2016-01-13 | 福建省诺希科技园发展有限公司 | Method for preparing high-conductivity indium gallium zinc oxide (IGZO) sputtering target material and product of high-conductivity IGZO sputtering target material |
| CN107522483A (en) * | 2017-06-26 | 2017-12-29 | 广西新未来信息产业股份有限公司 | A kind of preparation method of AZO targets |
| CN109053157B (en) * | 2018-07-13 | 2021-07-09 | 华南师范大学 | Ga2O3Base co-doped material target and preparation method thereof |
| CN112479683A (en) * | 2020-12-17 | 2021-03-12 | 中山智隆新材料科技有限公司 | Preparation method of doped IGZO material |
| CN112537954B (en) * | 2020-12-17 | 2022-04-15 | 中山智隆新材料科技有限公司 | Preparation method of IGZO target material |
| CN113651598B (en) * | 2021-08-11 | 2022-06-21 | 芜湖映日科技股份有限公司 | IZO doped target material and preparation method thereof |
| CN115745573A (en) * | 2022-10-31 | 2023-03-07 | 芜湖映日科技股份有限公司 | Preparation method of fine-grain IZO target material |
| CN116199496A (en) * | 2022-12-15 | 2023-06-02 | 先导薄膜材料（广东）有限公司 | Indium zinc oxide doped rare earth metal target material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1498875A (en) * | 2002-10-29 | 2004-05-26 | ס�ѽ�����ɽ��ʽ���� | Oxide sintered body and sputtering target, and prepn. process of transparent conductive oxide film used as electrode |
| CN103130493A (en) * | 2011-11-23 | 2013-06-05 | 财团法人工业技术研究院 | Indium Gallium Zinc Oxide (IGZO) nano powder and preparation method and application thereof |
| CN103193262A (en) * | 2013-04-09 | 2013-07-10 | 桂林电子科技大学 | Indium-gallium-zinc oxide powder and preparation method of ceramic target thereof |
| CN103408062A (en) * | 2013-08-02 | 2013-11-27 | 北京航空航天大学 | Aluminum-gallium co-doping zinc oxide nano-powder and preparation method for high intensity high conductivity sputtering coating target material thereof |
-
2013
- 2013-12-11 CN CN201310669559.9A patent/CN103819178B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1498875A (en) * | 2002-10-29 | 2004-05-26 | ס�ѽ�����ɽ��ʽ���� | Oxide sintered body and sputtering target, and prepn. process of transparent conductive oxide film used as electrode |
| CN103130493A (en) * | 2011-11-23 | 2013-06-05 | 财团法人工业技术研究院 | Indium Gallium Zinc Oxide (IGZO) nano powder and preparation method and application thereof |
| CN103193262A (en) * | 2013-04-09 | 2013-07-10 | 桂林电子科技大学 | Indium-gallium-zinc oxide powder and preparation method of ceramic target thereof |
| CN103408062A (en) * | 2013-08-02 | 2013-11-27 | 北京航空航天大学 | Aluminum-gallium co-doping zinc oxide nano-powder and preparation method for high intensity high conductivity sputtering coating target material thereof |
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| CN103819178A (en) | 2014-05-28 |
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Effective date of registration: 20190404 Address after: 471100 No. 66 Longhua Avenue, Luoyang Airport Industrial Cluster Area, Luoyang City, Henan Province (Matun Town, Mengjin County, Luoyang City) Patentee after: Luoyang crystal photoelectric material Co., Ltd. Address before: 545036 Yanghe Industrial Park, Liuzhou City, Guangxi Zhuang Autonomous Region Patentee before: Guangxi Crystal Union Photoelectric Materials Co., Ltd. |
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