CN115710131B - Method for cleaning ITO target material burning-supporting gasket - Google Patents
Method for cleaning ITO target material burning-supporting gasket Download PDFInfo
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- CN115710131B CN115710131B CN202211468271.0A CN202211468271A CN115710131B CN 115710131 B CN115710131 B CN 115710131B CN 202211468271 A CN202211468271 A CN 202211468271A CN 115710131 B CN115710131 B CN 115710131B
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- heat preservation
- gasket
- furnace
- cleaning
- ito
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- 238000004140 cleaning Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000013077 target material Substances 0.000 title claims abstract description 9
- 238000004321 preservation Methods 0.000 claims abstract description 79
- 238000005245 sintering Methods 0.000 claims abstract description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 11
- 239000001301 oxygen Substances 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000009423 ventilation Methods 0.000 claims description 9
- 238000005086 pumping Methods 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- 238000000227 grinding Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 6
- 230000000052 comparative effect Effects 0.000 description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 125000006850 spacer group Chemical group 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
Classifications
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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
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Physical Vapour Deposition (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to a method for cleaning an ITO target material burning-supporting gasket, which comprises the following main steps: placing the sintering pad with the ITO residues attached to the surface into a vacuum furnace, heating at a high temperature of 1550-1650 ℃, and keeping a certain vacuum degree; then cooling to 1300-1400 ℃, introducing air or oxygen for heat preservation, then heating to 1550-1650 ℃ again, and keeping a certain vacuum degree; and after the heat preservation is finished, cooling to room temperature and cleaning. The invention adopts the high-temperature sintering gasket, removes ITO residues on the gasket through high temperature, has good cleaning effect, and has the advantages of no gasket loss, clean and suitability for mass cleaning compared with the prior method for grinding and cleaning the gasket.
Description
Technical Field
The invention relates to the field of ceramic target sintering kiln furniture cleaning, in particular to a method for cleaning an ITO target sintering pad.
Background
An Indium Tin Oxide (ITO) target is a target material for magnetron sputtering coating, is used for plating a transparent conductive ITO film, and is widely applied to the fields of display screens, touch screens, solar cells and the like.
The purity of the ITO target material is required to be more than 99.99 percent. Therefore, when sintering in the sintering kiln, the high-purity gasket is needed to support, so that the high-purity gasket is prevented from directly contacting with the sintering bearing plate.
The sintering temperature of the ITO target is typically above 1550 ℃. After long-time sintering, an ITO shell layer is adhered to the gasket, the shell layer is uneven and has different thickness, the flatness of the ITO target material can be seriously affected, and the yield of the product is reduced. Meanwhile, the adhesion layer can also cause the gasket to adhere to the target, so that the surface pits appear on the target, and the product is directly scrapped.
The existing solution is that after the gasket is used each time, the gasket is manually ground by using a grinding stone or mechanically ground by using a grinding machine, and the production efficiency is greatly reduced due to the fact that the gasket is small in size, large in quantity, labor-consuming and time-consuming in grinding. Moreover, the grinding amount is small, and the cleaning is not clean; the grinding amount is large, the abrasion of the gasket is large, the consumption is fast, and the cost is high. There is an urgent need for a better method of cleaning the pad.
Disclosure of Invention
The invention aims to solve the technical problems that: the method for cleaning the ITO target material burning-bearing gasket adopts the high-temperature sintering gasket, removes the ITO residues on the gasket through pyrolysis, has good cleaning effect, and has the advantages of no loss of the gasket, clean and suitability for mass cleaning compared with the conventional method for grinding the cleaning gasket.
The technical scheme for solving the technical problems is as follows: a method for cleaning an ITO target material burning-in pad comprises the following steps:
(1) Placing the sintering pad with the ITO residues attached to the surface into a vacuum furnace;
(2) Heating the vacuum furnace to 1550-1650 ℃, and preserving heat for 4-10 hours, wherein the vacuum degree in the heat preservation period is minus 0.09-minus 0.04MPa;
(3) After the heat preservation is finished, the furnace temperature is reduced to 1300-1400 ℃, then the heat preservation is carried out for 1-4 hours, and air or oxygen is introduced during the heat preservation period, so that the furnace pressure is between 50Pa and 120 Pa;
(4) After the heat preservation is finished, the furnace temperature is increased to 1550-1650 ℃, the heat preservation is carried out for 4-10 hours, ventilation is stopped when the heat preservation is carried out, vacuum pumping is carried out, and the vacuum degree in the heat preservation period is-0.09-0.04 MPa;
(5) And after the heat preservation is finished, cooling to room temperature along with the furnace, and taking out the gasket to finish the cleaning of the ITO residues of the gasket.
The gasket is made of aluminum oxide or zirconium oxide.
ITO is easy to decompose and gasify at high temperature. The invention adopts the high-temperature sintering gasket to decompose and gasify the ITO residues on the gasket at high temperature so as to remove the ITO residues. The gasket body cannot be melted at high temperature, and the gasket is free from loss in the cleaning process; in addition, the size of the currently used gasket is small, a plurality of gaskets can be simultaneously placed into a vacuum furnace for cleaning, and the cleaning efficiency is high. Compared with the existing method for grinding and cleaning the gasket, the method has the advantages of no gasket loss, clean and low labor cost, and is suitable for mass cleaning.
The technical features of a method for cleaning an ITO target burning pad according to the present invention will be further described with reference to the accompanying drawings and examples.
Drawings
Fig. 1: schematic diagram of a burn-in pad with ITO residues attached before cleaning.
Fig. 2: schematic diagram of a clean-all burn-in pad cleaned by the method of example 1 of the present invention.
Fig. 3: schematic of a partially cleaned setter pad after cleaning in accordance with comparative example 2 of the present invention.
Detailed Description
Example 1:
stacking the sintering pad with the ITO residues attached to the surface into a vacuum furnace, heating to 1650 ℃, preserving heat for 4 hours, and keeping the vacuum degree in the furnace at-0.04 MPa during heat preservation. After the heat preservation is finished, the furnace temperature is reduced to 1400 ℃, the heat preservation is carried out for 1 hour, oxygen is introduced during the heat preservation, the pressure in the furnace is increased to 50Pa, and the furnace is maintained. After the heat preservation is finished, the furnace temperature is increased to 1650 ℃, the heat preservation is carried out for 4 hours, ventilation is stopped when the heat preservation is carried out, and vacuum is pumped, so that the vacuum degree in the furnace is minus 0.04MPa. And after the heat preservation is finished, cooling the gasket to room temperature along with a furnace, and thus finishing cleaning of ITO residues of the gasket.
Example 2:
stacking the sintering pad with the ITO residues attached to the surface into a vacuum furnace, heating to 1550 ℃, preserving heat for 10 hours, and keeping the vacuum degree in the furnace at-0.09 MPa during heat preservation. After the heat preservation is finished, the furnace temperature is reduced to 1300 ℃, the heat preservation is carried out for 4 hours, oxygen is introduced during the heat preservation, the pressure in the furnace is increased to 120Pa, and the furnace is maintained. After the heat preservation is finished, the furnace temperature is increased to 1550 ℃, the heat preservation is carried out for 10 hours, ventilation is stopped when the heat preservation is carried out, and vacuum pumping is carried out, so that the vacuum degree in the furnace is minus 0.09MPa. And after the heat preservation is finished, cooling the gasket to room temperature along with a furnace, and thus finishing cleaning of ITO residues of the gasket.
Example 3:
stacking the sintering pad with the ITO residues attached to the surface into a vacuum furnace, heating to 1600 ℃, preserving heat for 7 hours, and keeping the vacuum degree in the furnace at-0.07 MPa during heat preservation. After the heat preservation is finished, the furnace temperature is reduced to 1350 ℃, the heat preservation is carried out for 3 hours, and air is introduced during the heat preservation, so that the pressure in the furnace is increased to 80Pa, and the furnace is maintained. After the heat preservation is finished, the furnace temperature is increased to 1600 ℃, the heat preservation is carried out for 6 hours, ventilation is stopped when the heat preservation is carried out, and vacuum pumping is carried out, so that the vacuum degree in the furnace is minus 0.06MPa. And after the heat preservation is finished, cooling the gasket to room temperature along with a furnace, and thus finishing cleaning of ITO residues of the gasket.
Comparative example 1:
the firing pad with the ITO residues attached to the surface was stacked in a vacuum furnace, heated to 1650℃and kept at the temperature for 4 hours, while keeping the vacuum in the furnace at-0.04 MPa (this procedure is the same as in example 1). After the heat preservation is finished, the gasket is cooled to the room temperature along with the furnace, the gasket is taken out, and part of the surface of the gasket still remains an ITO layer.
Comparative example 2:
compared with the embodiment 1, the basic process is the same, and the temperature point of heat preservation when oxygen is introduced is only changed, and the specific process is as follows: stacking the sintering pad with the ITO residues attached to the surface into a vacuum furnace, heating to 1650 ℃, preserving heat for 4 hours, and keeping the vacuum degree in the furnace at-0.04 MPa during heat preservation. After the heat preservation is finished, the furnace temperature is reduced to 1280 ℃, the heat preservation is carried out for 1 hour, oxygen is introduced during the heat preservation, the pressure in the furnace is increased to 50Pa, and the furnace is maintained. After the heat preservation is finished, the furnace temperature is increased to 1650 ℃, the heat preservation is carried out for 4 hours, ventilation is stopped when the heat preservation is carried out, and vacuum is pumped, so that the vacuum degree in the furnace is minus 0.04MPa. After the heat preservation is finished, the gasket is cooled to the room temperature along with the furnace, the gasket is taken out, and a small amount of ITO layer remains on the surface of part of the gasket.
Comparative example 3:
compared with the embodiment 1, the basic process is the same, and the temperature point of heat preservation when oxygen is introduced is only changed, and the specific process is as follows: stacking the sintering pad with the ITO residues attached to the surface into a vacuum furnace, heating to 1650 ℃, preserving heat for 4 hours, and keeping the vacuum degree in the furnace at-0.04 MPa during heat preservation. After the heat preservation is finished, the furnace temperature is reduced to 1420 ℃, the heat preservation is carried out for 1 hour, oxygen is introduced during the heat preservation, the pressure in the furnace is increased to 50Pa, and the furnace is maintained. After the heat preservation is finished, the furnace temperature is increased to 1650 ℃, the heat preservation is carried out for 4 hours, ventilation is stopped when the heat preservation is carried out, and vacuum is pumped, so that the vacuum degree in the furnace is minus 0.04MPa. After the heat preservation is finished, the gasket is cooled to the room temperature along with the furnace, the gasket is taken out, and a small amount of ITO layer remains on the surface of part of the gasket.
Comparative example 4:
compared with example 1, the basic process is the same, only the vacuum degree is changed, and the specific process is as follows: stacking the sintering pad with the ITO residues attached to the surface into a vacuum furnace, heating to 1650 ℃, preserving heat for 4 hours, and keeping the vacuum degree in the furnace at-0.03 MPa during heat preservation. After the heat preservation is finished, the furnace temperature is reduced to 1400 ℃, the heat preservation is carried out for 1 hour, oxygen is introduced during the heat preservation, the pressure in the furnace is increased to 50Pa, and the furnace is maintained. After the heat preservation is finished, the furnace temperature is increased to 1650 ℃, the heat preservation is carried out for 4 hours, ventilation is stopped when the heat preservation is carried out, and vacuum is pumped, so that the vacuum degree in the furnace is minus 0.03MPa. After the heat preservation is finished, the gasket is cooled to the room temperature along with the furnace, the gasket is taken out, and a small amount of ITO layer remains on the surface of part of the gasket.
Comparative example 5:
compared with example 2, the basic process is the same, only the highest temperature is changed, the specific process is: stacking the sintering pad with the ITO residues attached to the surface into a vacuum furnace, heating to 1540 ℃, preserving heat for 10 hours, and keeping the vacuum degree in the furnace at-0.09 MPa during heat preservation. After the heat preservation is finished, the furnace temperature is reduced to 1300 ℃, the heat preservation is carried out for 4 hours, oxygen is introduced during the heat preservation, the pressure in the furnace is increased to 120Pa, and the furnace is maintained. After the heat preservation is finished, the furnace temperature is increased to 1540 ℃, the heat preservation is carried out for 10 hours, ventilation is stopped when the heat preservation is carried out, and vacuum is pumped, so that the vacuum degree in the furnace is minus 0.09MPa. After the heat preservation is finished, the gasket is cooled to the room temperature along with the furnace, the gasket is taken out, and a small amount of ITO layer remains on the surface of part of the gasket.
Cleaning effect description: the burning pad with ITO residues attached before cleaning is shown in figure 1, and the 'V' indicates that the cleaning effect is good, namely, the ITO residues on all pads can be cleaned, and the approximate effect is shown in figure 2; the "x" indicates that the cleaning effect was poor, i.e., the ITO residues on a portion of the spacers could be cleaned, but the ITO residues on a portion of the spacers could not be cleaned, and the use requirement was not met, as shown in fig. 3.
The gasket material described in the examples and comparative examples of the present invention is alumina.
As a variant, the method of the invention is also suitable for cleaning zirconia materials or other gaskets for ITO target sintering, which are not melted at high temperature. The shape of the gasket may be circular, rectangular, square, etc. The size of the pad that can be cleaned can be larger or smaller.
Claims (1)
1. A method for cleaning an ITO target material burning-supporting gasket is characterized by comprising the following steps: the method comprises the following steps:
(1) Placing the sintering pad with the ITO residues attached to the surface into a vacuum furnace;
(2) Heating the vacuum furnace to 1550-1650 ℃, and preserving heat for 4-10 hours, wherein the vacuum degree in the heat preservation period is minus 0.09-minus 0.04MPa;
(3) After the heat preservation is finished, the furnace temperature is reduced to 1300-1400 ℃, then the heat preservation is carried out for 1-4 hours, and air or oxygen is introduced during the heat preservation period, so that the furnace pressure is between 50Pa and 120 Pa;
(4) After the heat preservation is finished, the furnace temperature is increased to 1550-1650 ℃, the heat preservation is carried out for 4-10 hours, ventilation is stopped when the heat preservation is carried out, vacuum pumping is carried out, and the vacuum degree in the heat preservation period is-0.09-0.04 MPa;
(5) After the heat preservation is finished, cooling to room temperature along with a furnace, and taking out the gasket to finish cleaning the ITO residues of the gasket;
the gasket is made of aluminum oxide or zirconium oxide.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211468271.0A CN115710131B (en) | 2022-11-22 | 2022-11-22 | Method for cleaning ITO target material burning-supporting gasket |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211468271.0A CN115710131B (en) | 2022-11-22 | 2022-11-22 | Method for cleaning ITO target material burning-supporting gasket |
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| CN115710131A CN115710131A (en) | 2023-02-24 |
| CN115710131B true CN115710131B (en) | 2023-10-13 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08187650A (en) * | 1994-12-28 | 1996-07-23 | Shikoku Electric Power Co Inc | Cleaning device for gasket surface |
| CN201149257Y (en) * | 2007-10-30 | 2008-11-12 | 上海百旭引擎机械有限公司 | High temperature decomposition type heat cleaning system |
| CN106914809A (en) * | 2017-03-15 | 2017-07-04 | 广东省陶瓷研究所 | The equipment that physics decontamination is carried out to ceramic burning-resisting board |
| CN206550821U (en) * | 2017-03-15 | 2017-10-13 | 广东省陶瓷研究所 | A kind of trash-removal device of ceramic burning-resisting board |
| CN111229736A (en) * | 2020-01-20 | 2020-06-05 | 山东伟基炭科技有限公司 | Cleaning method of graphite boat for manufacturing solar cell |
| CN113372123A (en) * | 2021-05-26 | 2021-09-10 | 芜湖映日科技股份有限公司 | Pad sintering method for improving utilization rate of ITO (indium tin oxide) planar target |
| CN214441361U (en) * | 2020-09-03 | 2021-10-22 | 江西萍乡市成宇陶瓷有限责任公司 | Cleaning device of active alumina ball in hydrogen peroxide production |
-
2022
- 2022-11-22 CN CN202211468271.0A patent/CN115710131B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08187650A (en) * | 1994-12-28 | 1996-07-23 | Shikoku Electric Power Co Inc | Cleaning device for gasket surface |
| CN201149257Y (en) * | 2007-10-30 | 2008-11-12 | 上海百旭引擎机械有限公司 | High temperature decomposition type heat cleaning system |
| CN106914809A (en) * | 2017-03-15 | 2017-07-04 | 广东省陶瓷研究所 | The equipment that physics decontamination is carried out to ceramic burning-resisting board |
| CN206550821U (en) * | 2017-03-15 | 2017-10-13 | 广东省陶瓷研究所 | A kind of trash-removal device of ceramic burning-resisting board |
| CN111229736A (en) * | 2020-01-20 | 2020-06-05 | 山东伟基炭科技有限公司 | Cleaning method of graphite boat for manufacturing solar cell |
| CN214441361U (en) * | 2020-09-03 | 2021-10-22 | 江西萍乡市成宇陶瓷有限责任公司 | Cleaning device of active alumina ball in hydrogen peroxide production |
| CN113372123A (en) * | 2021-05-26 | 2021-09-10 | 芜湖映日科技股份有限公司 | Pad sintering method for improving utilization rate of ITO (indium tin oxide) planar target |
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| CN115710131A (en) | 2023-02-24 |
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Effective date of registration: 20240725 Address after: Room 307, 3rd Floor, Guanya International Star City, No. 100 Guting Avenue, Yanghe Industrial New Area, Liuzhou City, Guangxi Zhuang Autonomous Region, 545000 Patentee after: GUANGXI CRYSTAL UNION PHOTOELECTRIC MATERIALS Co.,Ltd. Country or region after: China Patentee after: Fenglianke Optoelectronics (Luoyang) Co.,Ltd. Address before: 545036 Room 307, Floor 3, 17 #, Guanya International Star City, No. 100, Guting Avenue, Yanghe Industrial New Area, Liuzhou City, Guangxi Zhuang Autonomous Region Patentee before: GUANGXI CRYSTAL UNION PHOTOELECTRIC MATERIALS Co.,Ltd. Country or region before: China |
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