CN111334809A - Method for cleaning silver evaporation material - Google Patents

Method for cleaning silver evaporation material Download PDF

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Publication number
CN111334809A
CN111334809A CN202010176551.9A CN202010176551A CN111334809A CN 111334809 A CN111334809 A CN 111334809A CN 202010176551 A CN202010176551 A CN 202010176551A CN 111334809 A CN111334809 A CN 111334809A
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China
Prior art keywords
cleaning
evaporation material
silver
silver evaporation
cleaned
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CN202010176551.9A
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Inventor
姚力军
潘杰
边逸军
王学泽
慕二龙
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Ningbo Jiangfeng Electronic Material Co Ltd
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Ningbo Jiangfeng Electronic Material Co Ltd
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Priority to CN202010176551.9A priority Critical patent/CN111334809A/en
Publication of CN111334809A publication Critical patent/CN111334809A/en
Priority to PCT/CN2021/080547 priority patent/WO2021180222A1/en
Priority to KR1020217025323A priority patent/KR102641900B1/en
Pending legal-status Critical Current

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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
    • C23C14/14—Metallic material, boron or silicon
    • 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
    • C23C14/24—Vacuum evaporation
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/20—Other heavy metals
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
    • C23G5/02—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
    • C23G5/032—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing oxygen-containing compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
    • H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
    • H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
    • H01L21/28506—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers
    • H01L21/28512—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table
    • H01L21/2855—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table by physical means, e.g. sputtering, evaporation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
    • H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
    • H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
    • H01L21/28506—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers
    • H01L21/28512—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table
    • H01L21/28568—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table the conductive layers comprising transition metals

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Cleaning By Liquid Or Steam (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)

Abstract

The invention discloses a method for cleaning silver evaporation materials. The cleaning method of the silver evaporation material comprises the following steps: 1) cleaning the silver evaporation material to be cleaned by using a mixed solution containing hydrogen peroxide and ammonia water; 2) cleaning the silver evaporation material cleaned in the step 1) by using IPA liquid; 3) cleaning the silver evaporation material cleaned in the step 2) by using pure water. The method for cleaning the silver evaporation material can improve the surface quality of the silver evaporation material and reduce the loss of silver in the current silver evaporation material cleaning mode.

Description

Method for cleaning silver evaporation material
Technical Field
The invention relates to the technical field of cleaning processes, in particular to a method for cleaning a silver evaporation material.
Background
Physical Vapor Deposition (PVD) refers to a technique of vaporizing a material source-solid or liquid surface into gaseous atoms, molecules or parts of them by Physical methods under vacuum conditions to form ions, and depositing a film with a specific function on the surface of a substrate by a low-pressure gas (or plasma) process. The main methods of physical vapor deposition are: vacuum evaporation, sputter coating, arc plasma coating, ion coating, molecular beam epitaxy, and the like. The vacuum evaporation is widely applied to the back gold process of the semiconductor wafer due to strong film bonding force, high deposition rate and uniform film thickness.
With the rapid development of artificial intelligence and 5G technology, the demand of semiconductor chips is increasing. The vacuum evaporation coating technology is widely applied to the back gold process of the wafer at present. The semiconductor chip has extremely high requirements on the purity and the surface quality of an evaporated material, otherwise, the semiconductor chip can generate the defects of Peeling, splashing and the like and even damage a machine table in the vacuum evaporation coating process; on the other hand, this leads to non-uniform film properties and may lead to chip scrap. The wafer back gold plating film is generally required to be plated with three metal films of Ti, Ni and Ag, wherein Ag is used as the outermost metal film, and has the function of connecting a Ni layer and excellent conductivity. The silver evaporation material cannot avoid the problems of residual impurities, dirt and the like on the surface of the silver evaporation material in the preparation process, so that in order to ensure the quality of a film in a wafer back gold process, the invention provides a cleaning liquid formula of a pure silver (the purity is more than or equal to 3N) evaporation material, which not only can improve the surface quality of the silver evaporation material, but also can reduce the silver loss in the current silver evaporation material cleaning mode.
At present, the cleaning mode of silver evaporation materials is mainly centrifugal grinding, and surface impurities and dirt are removed by utilizing mutual collision between the evaporation materials at a high rotating speed and scouring of a detergent.
CN109420638A discloses an apparatus for cleaning semiconductor equipment parts and a cleaning method, the apparatus comprises a cleaning tank, in which cleaning liquid is placed, and the parts to be cleaned are soaked in the cleaning liquid in the cleaning tank; the cleaning liquid is ammonia water or a mixed solution of ammonia water and hydrogen peroxide. The method is based on the fact that the environment of the blue-green epitaxy process is rich in nitrogen, a large amount of ammonia gas can be used, and weakly alkaline ammonia water is used for cleaning the stainless steel parts, so that the recovery of the epitaxy process cannot be influenced, and the parts cannot be damaged. The mixed solution of ammonia water and hydrogen peroxide is used as the cleaning liquid, but no specific proportion is given, and the cleaning liquid is only cleaned by the mixed solution, so that the cleaning is not thorough when the cleaning liquid is applied to cleaning of silver evaporation materials.
CN108987273A discloses a surface treatment method of silver evaporation material, comprising: providing a silver evaporation material; carrying out centrifugal grinding operation on the silver evaporation material; after the centrifugal grinding operation, carrying out cleaning operation on the silver evaporation material; and after the cleaning operation, drying the silver evaporation material. Compared with the scheme of removing the oxide layer by adopting the acid washing operation, the problem that the acid washing solution consumes the silver evaporation material can be avoided, so that the surface brightness and smoothness of the silver evaporation material are improved, the purity of the silver evaporation material is improved, the consumption of the silver evaporation material is reduced, and the preparation cost of the silver evaporation material is reduced. However, the physical cleaning method causes a large amount of silver evaporation material to be lost, and is not beneficial to the industrial production of the evaporation material.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for cleaning a silver evaporation material, which can not only improve the surface quality of the silver evaporation material, but also reduce the loss of silver in the existing silver evaporation material cleaning mode.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for cleaning silver evaporant, comprising the steps of:
1) cleaning the silver evaporation material to be cleaned by using a mixed solution containing hydrogen peroxide and ammonia water;
2) cleaning the silver evaporation material cleaned in the step 1) by using IPA liquid;
3) cleaning the silver evaporation material cleaned in the step 2) by using pure water.
The method for cleaning the silver evaporation material comprises the steps of firstly converting impurities (such as Cr, Cu, Zn, Ni, Co, Ca, Fe and Mg) or oil stains remained on the surface of the silver evaporation material into water-soluble compounds by utilizing the strong oxidation of hydrogen peroxide and the dissolution of ammonia water, then cleaning and removing the water-soluble compounds by using IPA (isopropyl alcohol) liquid and pure water, and quickly and efficiently removing the impurities or the oil stains possibly remained on the surface of the silver evaporation material in a chemical cleaning mode, so that the surface quality of the silver evaporation material is improved, the stability of the silver evaporation material during evaporation and the performance of a film are finally improved, and the loss of silver in the existing silver evaporation material cleaning mode can be reduced.
The alkalinity of the ammonia water is weak, in order to enhance the cleaning effect, the hydrogen peroxide which has strong oxidizability and does not cause pollution is added, but the volume ratio of the hydrogen peroxide to the ammonia water in the hydrogen peroxide-ammonia water mixed solution needs to be reasonably controlled, so that the silver evaporation material is not lost while the impurities and the oil stains on the surface of the silver evaporation material are efficiently and thoroughly removed. Cleaning with mixed solution of hydrogen peroxide and ammonia water to convert residual impurities (such as Cr, Cu, Zn, Ni, Co, Ca, Fe, Mg) or oil stain on the surface of the silver evaporation material into water-soluble compounds.
In the step 1), the volume ratio of the hydrogen peroxide to the ammonia water in the hydrogen peroxide-ammonia water mixed solution is (1-3) - (5-7), for example, the volume ratio of the hydrogen peroxide to the ammonia water is 1:5, 1:6, 1:7, 2:5, 2:6, 2:7, 3:5, 3:6, 3:7, and the like. If the volume ratio of the hydrogen peroxide to the ammonia water is too low and is lower than 1:7, impurities remained on the surface of the silver evaporation material cannot be thoroughly removed, and if the volume ratio of the hydrogen peroxide to the ammonia water is too high and is higher than 3:5, raw materials of the silver evaporation material are lost to a certain extent.
In step 1), the cleaning is performed in an automatic rotary cleaning tank.
Wherein the purity of the silver evaporation material is more than or equal to 99.9 percent.
In the step 1), the cleaning time is 1-3 min, for example, the cleaning time is 1min, 1.5min, 2min, 2.5min, and 3 min.
In the step 2), the IPA liquid is cleaned, and the subsequent pure water cleaning is matched, so that the water-soluble compound converted after the cleaning in the step 1) can be removed, and the cleaning effect is further improved.
In the step 2), the cleaning with the IPA liquid is ultrasonic cleaning, preferably, the time of the ultrasonic cleaning is 10-15 min, for example, the time of the ultrasonic cleaning is 10min, 11min, 12min, 13min, and 14 min. Ultrasonic cleaning cooperates with IPA liquid, can effectively improve cleaning performance.
In the step 3), the time for cleaning with pure water is 5-10 min, for example, the time for cleaning with pure water is 5min, 6min, 7min, 8min, 9min, 10 min.
Above-mentioned abluent time needs strict control, can solve silver evaporation material surface quality problem high-efficiently through reasonable control cleaning time, under the prerequisite of guaranteeing high-efficient edulcoration, reduces the loss to silver evaporation material.
And 4) drying the silver evaporation material cleaned in the step 3) after the step 3). In step 4), the drying is vacuum drying.
In the step 4), the temperature of the vacuum drying is 60-80 ℃, for example, the temperature of the vacuum drying is 60 ℃, 65 ℃, 70 ℃, 75 ℃ and 80 ℃; the vacuum drying time is 60-80 min, for example, the vacuum drying time is 60min, 65min, 70min, 75min, 80 min; the vacuum degree of the vacuum drying is below 0.01 MPa.
And 4) after vacuum drying, the step of vacuumizing and packaging the silver evaporation material is also included.
As a preferable embodiment of the present invention, the method for cleaning the silver evaporation material comprises the following steps:
1) putting the silver evaporation material to be cleaned into an automatic rotary cleaning tank containing hydrogen peroxide-ammonia water mixed liquid with the volume ratio of hydrogen peroxide to ammonia water being (1-3) to (5-7) for cleaning for 1-3 min;
2) transferring the silver evaporation material cleaned in the step 1) into an IPA liquid tank for ultrasonic cleaning for 10-15 min;
3) transferring the silver evaporation material cleaned in the step 2) into a pure water tank for cleaning for 5-10 min;
4) putting the silver evaporation material cleaned in the step 3) into a vacuum drying oven, performing vacuum drying for 60-80 min at the temperature of 60-80 ℃ and under the vacuum degree of below 0.01MPa, and performing vacuum-pumping packaging.
Compared with the prior art, the invention has the beneficial effects that:
the method for cleaning the silver evaporation material can quickly and efficiently remove impurities or oil stains remained on the surface of the silver evaporation material, improve the surface quality of the silver evaporation material, finally improve the stability of the silver evaporation material during evaporation and the performance of a film, and also reduce the silver loss of the current silver evaporation material cleaning mode.
Drawings
FIG. 1 is a surface quality appearance of a silver evaporant after being cleaned by the cleaning method of example 1;
FIG. 2 is a surface quality appearance of a silver evaporant after being cleaned by the cleaning method of example 2;
FIG. 3 is a surface quality appearance of the silver evaporant after being cleaned by the cleaning method of example 3;
FIG. 4 is a surface quality appearance of the silver evaporant after being cleaned by the cleaning method of example 4;
FIG. 5 is a surface quality appearance of the silver evaporant after being cleaned by the cleaning method of example 5;
FIG. 6 is a surface quality appearance of the silver evaporant after being cleaned by the cleaning method of example 6;
FIG. 7 is a surface quality appearance of the silver evaporant after being cleaned by the cleaning method of example 7;
FIG. 8 is a surface quality appearance of a silver evaporant after being cleaned by the cleaning method of comparative example 1;
FIG. 9 is a surface quality appearance of a silver evaporant after being cleaned by the cleaning method of comparative example 2;
FIG. 10 is a surface quality appearance of a silver evaporant after being cleaned by the cleaning method of comparative example 3;
fig. 11 is a surface quality appearance diagram of the silver evaporant after being washed by the washing method of comparative example 4.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
Unless otherwise specified, various starting materials of the present invention are commercially available or prepared according to conventional methods in the art.
Example 1
The method for cleaning the silver evaporation material comprises the following steps:
1) putting the silver evaporation material to be cleaned into an automatic rotary cleaning tank containing hydrogen peroxide-ammonia water mixed liquid with the volume ratio of 1:7 of hydrogen peroxide to ammonia water for cleaning for 2 min;
2) transferring the silver evaporation material cleaned in the step 1) into an IPA liquid tank for ultrasonic cleaning for 12 min;
3) transferring the silver evaporation material cleaned in the step 2) into a pure water tank for cleaning for 6 min;
4) putting the silver evaporation material cleaned in the step 3) into a vacuum drying oven, carrying out vacuum drying for 60min at 70 ℃ under the vacuum degree of 0.005MPa, and carrying out vacuum-pumping packaging.
Example 2
The method for cleaning the silver evaporation material comprises the following steps:
1) putting the silver evaporation material to be cleaned into an automatic rotary cleaning tank containing hydrogen peroxide-ammonia water mixed liquid with the volume ratio of 1:5 of hydrogen peroxide to ammonia water for cleaning for 2 min;
2) transferring the silver evaporation material cleaned in the step 1) into an IPA liquid tank for ultrasonic cleaning for 12 min;
3) transferring the silver evaporation material cleaned in the step 2) into a pure water tank for cleaning for 6 min;
4) putting the silver evaporation material cleaned in the step 3) into a vacuum drying oven, carrying out vacuum drying for 60min at 70 ℃ under the vacuum degree of 0.005MPa, and carrying out vacuum-pumping packaging.
Example 3
The method for cleaning the silver evaporation material comprises the following steps:
1) putting the silver evaporation material to be cleaned into an automatic rotary cleaning tank containing hydrogen peroxide-ammonia water mixed liquid with the volume ratio of 2:7 of hydrogen peroxide to ammonia water for cleaning for 2 min;
2) transferring the silver evaporation material cleaned in the step 1) into an IPA liquid tank for ultrasonic cleaning for 12 min;
3) transferring the silver evaporation material cleaned in the step 2) into a pure water tank for cleaning for 6 min;
4) putting the silver evaporation material cleaned in the step 3) into a vacuum drying oven, carrying out vacuum drying for 60min at 70 ℃ under the vacuum degree of 0.005MPa, and carrying out vacuum-pumping packaging.
Example 4
The method for cleaning the silver evaporation material comprises the following steps:
1) putting the silver evaporation material to be cleaned into an automatic rotary cleaning tank containing hydrogen peroxide-ammonia water mixed liquid with the volume ratio of hydrogen peroxide to ammonia water being 3:5, and cleaning for 2 min;
2) transferring the silver evaporation material cleaned in the step 1) into an IPA liquid tank for ultrasonic cleaning for 12 min;
3) transferring the silver evaporation material cleaned in the step 2) into a pure water tank for cleaning for 6 min;
4) putting the silver evaporation material cleaned in the step 3) into a vacuum drying oven, carrying out vacuum drying for 60min at 70 ℃ under the vacuum degree of 0.005MPa, and carrying out vacuum-pumping packaging.
Example 5
The method for cleaning the silver evaporation material comprises the following steps:
1) putting the silver evaporation material to be cleaned into an automatic rotary cleaning tank containing hydrogen peroxide-ammonia water mixed liquid with the volume ratio of hydrogen peroxide to ammonia water being 3:5, and cleaning for 2 min;
2) transferring the silver evaporation material cleaned in the step 1) into an IPA liquid tank for ultrasonic cleaning for 15 min;
3) transferring the silver evaporation material cleaned in the step 2) into a pure water tank for cleaning for 8 min;
4) putting the silver evaporation material cleaned in the step 3) into a vacuum drying oven, carrying out vacuum drying for 80min at 65 ℃ under the vacuum degree of 0.008MPa, and carrying out vacuum-pumping packaging.
Example 6
The present example is different from example 1 in that the volume ratio of hydrogen peroxide to ammonia water is 1:10, and the rest is the same as example 1.
Example 7
The difference between this example and example 1 is that the volume ratio of hydrogen peroxide to ammonia water is 1:1, and the rest is the same as example 1.
Comparative example 1
The difference between this example and example 1 is that IPA cleaning, pure water cleaning and vacuum drying are only adopted, cleaning with the hydrogen peroxide-ammonia water mixed solution in step 1) is not carried out, and the rest is the same as example 1.
Comparative example 2
The difference between this example and example 1 is that in step 1), only ammonia water is used for cleaning, and hydrogen peroxide is not contained, and the rest is the same as example 1.
Comparative example 3
This example is different from example 1 in that the cleaning with IPA liquid in step 2) is not performed, and the rest is the same as example 1.
Comparative example 4
This example is different from example 1 in that the vacuum drying of step 4) is not performed, and the rest is the same as example 1.
The silver evaporation materials were cleaned by the cleaning methods of examples 1 to 7, and the surface qualities of the cleaned silver evaporation materials are shown in fig. 1 to 7, respectively.
The cleaning methods of comparative examples 1 to 4 were carried out to clean the silver evaporant, and the surface quality of the silver evaporant after cleaning is shown in fig. 8 to 11, respectively.
As can be seen from fig. 1-5, the surface of the silver evaporation material cleaned by the cleaning method of the present invention is clean and has no impurities or oil stains, and as can be seen from fig. 6 and 7, if the volume ratio of the hydrogen peroxide to the ammonia water is too large or too small, the oil stains on the surface of the silver evaporation material cannot be removed.
As can be seen from fig. 8 to 11, comparative examples 1 to 4, which lack any step in the cleaning method of the present invention, were not effective in completely removing the oily contaminants on the surface of the silver evaporant.
The present invention is illustrated by the above-mentioned examples, but the present invention is not limited to the above-mentioned detailed process equipment and process flow, i.e. it is not meant to imply that the present invention must rely on the above-mentioned detailed process equipment and process flow to be practiced. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

Claims (10)

1. The method for cleaning the silver evaporation material is characterized by comprising the following steps of:
1) cleaning the silver evaporation material to be cleaned by using a mixed solution containing hydrogen peroxide and ammonia water;
2) cleaning the silver evaporation material cleaned in the step 1) by using IPA liquid;
3) cleaning the silver evaporation material cleaned in the step 2) by using pure water.
2. The cleaning method according to claim 1, wherein in the step 1), the volume ratio of the hydrogen peroxide to the ammonia water in the hydrogen peroxide-ammonia water mixed solution is (1-3) to (5-7).
3. The cleaning method according to claim 1 or 2, wherein in step 1), the cleaning is performed in an automatic rotary cleaning tank;
preferably, the purity of the silver evaporation material is more than or equal to 99.9 percent.
4. The cleaning method according to any one of claims 1 to 3, wherein in the step 1), the cleaning time is 1 to 3 min.
5. The cleaning method according to any one of claims 1 to 4, wherein in the step 2), the IPA liquid cleaning is ultrasonic cleaning, and the time of the ultrasonic cleaning is 10-15 min.
6. The cleaning method according to any one of claims 1 to 5, wherein in the step 3), the time for cleaning with pure water is 5 to 10 min.
7. The cleaning method according to any one of claims 1 to 6, further comprising a step 4) after the step 3), wherein the silver evaporation material cleaned in the step 3) is dried.
8. The cleaning method according to claim 7, wherein in the step 4), the drying is vacuum drying;
preferably, the temperature of the vacuum drying is 60-80 ℃, the time of the vacuum drying is 60-80 min, and the vacuum degree of the vacuum drying is below 0.01 MPa.
9. The cleaning method according to claim 7 or 8, characterized in that the step 4) of vacuum drying further comprises the step of vacuum packaging the silver evaporation material.
10. A cleaning method according to any one of claims 1-9, characterized in that the cleaning method comprises the steps of:
1) putting the silver evaporation material to be cleaned into an automatic rotary cleaning tank containing hydrogen peroxide-ammonia water mixed liquid with the volume ratio of hydrogen peroxide to ammonia water being (1-3) to (5-7) for cleaning for 1-3 min;
2) transferring the silver evaporation material cleaned in the step 1) into an IPA liquid tank for ultrasonic cleaning for 10-15 min;
3) transferring the silver evaporation material cleaned in the step 2) into a pure water tank for cleaning for 5-10 min;
4) putting the silver evaporation material cleaned in the step 3) into a vacuum drying oven, performing vacuum drying for 60-80 min at the temperature of 60-80 ℃ and under the vacuum degree of below 0.01MPa, and performing vacuum-pumping packaging.
CN202010176551.9A 2020-03-13 2020-03-13 Method for cleaning silver evaporation material Pending CN111334809A (en)

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Application Number Priority Date Filing Date Title
CN202010176551.9A CN111334809A (en) 2020-03-13 2020-03-13 Method for cleaning silver evaporation material
PCT/CN2021/080547 WO2021180222A1 (en) 2020-03-13 2021-03-12 Method for cleaning silver evaporation material
KR1020217025323A KR102641900B1 (en) 2020-03-13 2021-03-12 How to clean silver evaporation material

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Application Number Priority Date Filing Date Title
CN202010176551.9A CN111334809A (en) 2020-03-13 2020-03-13 Method for cleaning silver evaporation material

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CN111334809A true CN111334809A (en) 2020-06-26

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