CN115710131B

CN115710131B - Method for cleaning ITO target material burning-supporting gasket

Info

Publication number: CN115710131B
Application number: CN202211468271.0A
Authority: CN
Inventors: 陆映东; 宋春华; 黄誓成; 梁盈祥; 覃丽莉; 黄作; 莫斌; 薛超; 张倍维
Original assignee: Guangxi Crystal Union Photoelectric Materials Co ltd
Current assignee: Guangxi Crystal Union Photoelectric Materials Co ltd
Priority date: 2022-11-22
Filing date: 2022-11-22
Publication date: 2023-10-13
Anticipated expiration: 2042-11-22
Also published as: CN115710131A

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

Method for cleaning ITO target material burning-supporting gasket

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. A method for cleaning an ITO target material burning-supporting gasket is characterized by comprising the following steps: the method comprises the following steps:

(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.