CN111501085A - Method for cleaning Mask in vacuum evaporation equipment - Google Patents

Method for cleaning Mask in vacuum evaporation equipment Download PDF

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Publication number
CN111501085A
CN111501085A CN202010354714.8A CN202010354714A CN111501085A CN 111501085 A CN111501085 A CN 111501085A CN 202010354714 A CN202010354714 A CN 202010354714A CN 111501085 A CN111501085 A CN 111501085A
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CN
China
Prior art keywords
mask
cleaned
cathode
electrolyte
power supply
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Pending
Application number
CN202010354714.8A
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Chinese (zh)
Inventor
熊志红
郑思温
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Shenzhen Shishang Electronic Technology Co ltd
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Shenzhen Shishang Electronic Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
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Priority to CN202010354714.8A priority Critical patent/CN111501085A/en
Publication of CN111501085A publication Critical patent/CN111501085A/en
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F1/00—Electrolytic cleaning, degreasing, pickling or descaling
    • C25F1/02—Pickling; Descaling
    • C25F1/04—Pickling; Descaling in solution
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F1/00—Electrolytic cleaning, degreasing, pickling or descaling
    • C25F1/02—Pickling; Descaling
    • C25F1/04—Pickling; Descaling in solution
    • C25F1/06—Iron or steel
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F1/00—Electrolytic cleaning, degreasing, pickling or descaling
    • C25F1/02—Pickling; Descaling
    • C25F1/04—Pickling; Descaling in solution
    • C25F1/08—Refractory metals
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Cleaning By Liquid Or Steam (AREA)

Abstract

The invention discloses a method for cleaning a Mask in vacuum evaporation equipment, wherein the Mask body is made of aluminum, titanium, stainless steel or alloy, and the method comprises the following steps: taking a nitric acid solution as an electrolyte, taking a Mask to be cleaned as an anode, respectively immersing the Mask to be cleaned and a cathode into the electrolyte, applying a power supply between the Mask to be cleaned and the cathode, connecting the Mask to be cleaned with the anode of the power supply, and connecting the cathode with the cathode of the power supply, so that a metal film on the surface of the Mask to be cleaned is dissolved in the electrolyte, and obtaining the cleaned Mask. The nitric acid solution enables a compact oxide film to be formed on the surface of the Mask body, the metal film on the Mask is preferentially removed while the Mask is protected, the cleanliness requirement is met, the Mask body is not damaged, and meanwhile, the dosage of cleaning medicines is saved.

Description

Method for cleaning Mask in vacuum evaporation equipment
Technical Field
The invention relates to the technical field of manufacturing of photoelectric panels, in particular to a Mask cleaning method in vacuum evaporation equipment.
Background
Electro-optical display panels, such as liquid crystal panels, electroluminescent display panels, light emitting diode display panels, organic light emitting diode display panels, touch panels, plasma display panels, field emission display panels, laser display panels, etc., are widely used in electronic devices such as mobile phones, computers, televisions, electronic display screens of household appliances, etc.
In the process of processing the photoelectric display panel, one of the processes is to plate a conductive metal film layer, such as a copper film, a molybdenum film, etc., on a photoelectric substrate, in the process of vacuum evaporation, a Mask in a vacuum evaporation device is also splashed with a small amount of conductive metal film liquid, after long-term use, conductive metal stains are accumulated on the surface of the Mask, the normal operation of the film plating is affected, and the Mask needs to be cleaned so as to be recycled.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a method for cleaning a Mask in vacuum evaporation equipment.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for cleaning a Mask in vacuum evaporation equipment is characterized by comprising the following steps of:
taking a nitric acid solution as an electrolyte, taking a Mask to be cleaned as an anode, respectively immersing the Mask to be cleaned and a cathode into the electrolyte, applying a power supply between the Mask to be cleaned and the cathode, connecting the Mask to be cleaned with the anode of the power supply, connecting the cathode with the cathode of the power supply, dissolving a metal film on the surface of the Mask to be cleaned in the electrolyte to obtain the cleaned Mask, and reducing metal ions dissolved in the electrolyte into metal at the cathode and depositing and recycling the metal ions.
The embodiment of the invention has the following beneficial effects:
the embodiment of the invention adopts an electrolysis method, a nitric acid solution is adopted as an electrolyte, so that a compact oxide film is generated on the surface of a Mask body to be cleaned, the internal body is protected, the Mask to be cleaned is used as an anode, a metal film on the surface of the Mask to be cleaned is preferentially dissolved, the Mask body is better protected, and the dissolved metal ions are precipitated and recovered at the cathode again, so that the utilization rate of metal is improved; nitric acid is not consumed in the whole electrolytic process, the nitric acid can be repeatedly used, the using amount of the nitric acid is saved, pollution of a large amount of yellow smoke generated by chemical reaction of the nitric acid to the surrounding environment is avoided, and wastewater treatment is avoided. Compared with nitric acid soaking in the prior art, the cleaning method has the advantages of low nitric acid consumption, high metal utilization rate, low Mask body loss and environmental friendliness.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The invention discloses a method for cleaning a Mask in vacuum evaporation equipment, wherein the Mask is made of aluminum or titanium, and the method comprises the following steps:
taking a nitric acid solution as an electrolyte, taking a Mask to be cleaned as an anode, respectively immersing the Mask to be cleaned and a cathode into the electrolyte, applying a power supply between the Mask to be cleaned and the cathode, connecting the Mask to be cleaned with the anode of the power supply, and connecting the cathode with the cathode of the power supply, so that a metal film on the surface of the Mask to be cleaned is dissolved in the electrolyte to obtain the cleaned Mask, and reducing metal ions dissolved in the electrolyte into metal at the cathode and depositing and recycling the metal ions.
The invention adopts the principle of the electrolytic cell, nitric acid does not generate chemical reaction and is not consumed in the whole electrolytic reaction process, and the electrolyte can be repeatedly used, thereby not only saving the use cost of the nitric acid, but also avoiding the influence of a large amount of yellow smoke generated by the reaction of the nitric acid on the environment and avoiding the treatment of wastewater. On the other hand, the Mask body is made of aluminum, titanium, stainless steel or alloy, and a layer of compact oxide film is formed on the surface of the body in the nitric acid electrolyte, so that the body inside the body can be prevented from further reacting with the nitric acid solution, the body is protected, and the loss of the Mask body is reduced.
On one hand, the Mask body is protected, meanwhile, metal film stains are removed, metal is recycled, and the utilization rate of the metal is improved; on the other hand, the consumption of nitric acid is avoided, the influence of the reaction of the nitric acid on the surrounding environment and the increased wastewater treatment are avoided, the use cost of the nitric acid and the wastewater treatment cost are saved, and the environmental friendliness is improved.
Preferably, the concentration of the nitric acid solution is 0.5 mol/L to 3 mol/L.
In order to reduce the overvoltage of the electrolyte and protect the Mask body, preferably, the nitric acid solution further comprises an additive, the concentration of the additive is 0.1 g/L-1 g/L, and the additive is selected from two or three of bone glue, thiourea and dry complexing agent.
Preferably, the current density of the power supply is 200A/m2～250A/m2The voltage of the power supply is 1.5V-2V, and the electrolysis time is 24 hours-96 hours.
After the Mask is cleaned by an electrolytic method, the steps of water washing, ultrasonic water washing, sand blasting and arc cleaning are sequentially carried out.
In the water washing step, electrolyte and impurities on the Mask are removed by a high-pressure water washing method, preferably, the water washing pressure is 180-260 bar, and the water washing time is 10-30 seconds.
In the ultrasonic water washing step, the ultrasonic frequency of the ultrasonic water washing is 20Hz to 40Hz, and the time of the ultrasonic water washing is 5min to 20 min.
In the step of sand blasting, a mechanical friction method is adopted to further remove the residual metal film and smooth the Mask body so as to meet the requirement of the evaporation process on roughness, preferably, the model of the sand material subjected to sand blasting is W60#, and the sand blasting pressure of the sand blasting is 3kg/cm2～4kg/cm2The time is 5 minutes to 10 minutes.
Since the Mask body has an oxide film on its surface, it is preferable to remove oxide and other organic impurities by arc cleaning. Preferably, the arc layer has a thickness of 10 to 25 μm, an air pressure of 3 to 5kg, and a current of 60 to 80A for a period of 5 to 10 minutes.
Preferably, the cathode is a stainless steel plate, and metal ions in the solution in the electrolyte are deposited on the stainless steel plate, and when the metal ions are recovered, a mechanical stripping method is adopted to recover the metal, and the stainless steel plate can be reused.
Preferably, the metal film on the Mask surface to be cleaned is a copper film or a molybdenum film, and the metal film can be cleaned by using the method.
In the following specific examples, the metal film on the Mask surface to be cleaned is a copper film, and the chemical reaction of the electrolytic cell is as follows: cathode: cu2++2e ═ Cu; anode: cu-2e ═ Cu2+。
Example 1
1) 0.5 mol/L nitric acid solution is prepared as electrolyte, 0.2 g/L of bone glue is added, 0.3 g/L of thiourea is added, and 0.5 g/L of dry complexing agent is added, so that the concentration of the additive is 1 g/L.
2) Putting a Mask to be cleaned into a titanium workpiece basket, immersing the titanium workpiece basket into electrolyte, taking a stainless steel plate as a cathode, inserting the electrolyte, connecting the titanium workpiece basket with the anode of a direct current power supply, connecting the stainless steel plate with the cathode of the direct current power supply, setting the voltage of the direct current power supply to be 2V, and outputting current with the density of 200A/cm2And electrolyzing for 60 hours.
3) Repeatedly washing the Mask obtained in the step 2) with high pressure water, wherein the washing pressure is 180 bar, and the washing time is 20 seconds.
4) Carrying out ultrasonic cleaning on the Mask obtained in the step 3), wherein the ultrasonic frequency is 20Hz, and the ultrasonic water washing time is 20 min.
5) Performing sand blasting treatment on the Mask obtained in the step 4), wherein the model of the sand material subjected to the sand blasting treatment is W60#, and the sand blasting pressure of the sand blasting treatment is 3kg/cm2The duration is 8 minutes.
6) And (3) sending the Mask obtained in the step 5) to an arc chamber for arc cleaning, setting the thickness of an arc layer to be 10 microns, the air pressure to be 3kg, the current to be 60A and the duration to be 8 minutes.
7) Cleaning and drying the Mask obtained in the step 6), and sealing and packaging for reuse.
Example 2
1) 3 mol/L nitric acid solution is prepared as electrolyte, 0.1 g/L of bone glue is added, 0.5 g/L of thiourea is added, and the concentration of the additive is 0.6 g/L.
2) Putting a Mask to be cleaned into a titanium workpiece basket, immersing the titanium workpiece basket into electrolyte, taking a stainless steel plate as a cathode, inserting the electrolyte into the titanium workpiece basket, connecting the titanium workpiece basket with the anode of a direct current power supply, connecting the stainless steel plate with the cathode of the direct current power supply, setting the voltage of the direct current power supply to be 1.5V, and outputting current with the density of 250A/cm2And electrolyzing for 60 hours.
3) Repeatedly washing the Mask obtained in the step 2) with high-pressure water at the pressure of 260 bar for 20 seconds.
4) Carrying out ultrasonic cleaning on the Mask obtained in the step 3), wherein the ultrasonic frequency is 40Hz, and the ultrasonic water washing time is 5 min.
5) Performing sand blasting treatment on the Mask obtained in the step 4), wherein the model of the sand material subjected to the sand blasting treatment is W60#, and the sand blasting pressure of the sand blasting treatment is 4kg/cm2The duration is 8 minutes.
6) And (3) sending the Mask obtained in the step 5) to an arc chamber for arc cleaning, setting the thickness of an arc layer to be 25 microns, the air pressure to be 4kg, the current to be 80A and the duration to be 8 minutes.
7) Cleaning and drying the Mask obtained in the step 6), and sealing and packaging for reuse.
Example 3
1) 0.5 mol/L nitric acid solution is prepared as electrolyte, 0.03 g/L of bone glue, 0.03 g/L of thiourea and 0.04 g/L of colchicine are added, so that the concentration of the additive is 0.1 g/L.
2) Putting a Mask to be cleaned into a titanium workpiece basket, immersing the titanium workpiece basket into electrolyte, taking a stainless steel plate as a cathode, inserting the electrolyte, connecting the titanium workpiece basket with the anode of a direct current power supply, connecting the stainless steel plate with the cathode of the direct current power supply, setting the voltage of the direct current power supply to be 2V, and outputting current with the density of 200A/cm2And electrolyzing for 60 hours.
3) Repeatedly washing the Mask obtained in the step 2) with high pressure water, wherein the washing pressure is 180 bar, and the washing time is 20 seconds.
4) Carrying out ultrasonic cleaning on the Mask obtained in the step 3), wherein the ultrasonic frequency is 20Hz, and the ultrasonic water washing time is 20 min.
5) Adding the Mask obtained in the step 4) intoPerforming sand blasting treatment, wherein the model of the sand material subjected to the sand blasting treatment is W60#, and the sand blasting pressure of the sand blasting treatment is 3kg/cm2The duration is 8 minutes.
6) And (3) sending the Mask obtained in the step 5) to an arc chamber for arc cleaning, setting the thickness of an arc layer to be 10 microns, the air pressure to be 3kg, the current to be 60A and the duration to be 8 minutes.
7) Cleaning and drying the Mask obtained in the step 6), and sealing and packaging for reuse.
Comparative example 1
1) The Mask to be cleaned was soaked in a nitric acid solution having a concentration of 6 mol/L for 16 hours.
The rest of the procedure was the same as in example 1, but the procedure was as follows:
2) repeatedly washing the Mask obtained in the step 1) with high pressure water, wherein the washing pressure is 180 bar, and the washing time is 20 seconds.
3) Carrying out ultrasonic cleaning on the Mask obtained in the step 2), wherein the ultrasonic frequency is 20Hz, and the ultrasonic water washing time is 20 min.
4) Performing sand blasting treatment on the Mask obtained in the step 3), wherein the model of the sand material subjected to the sand blasting treatment is W60#, and the sand blasting pressure of the sand blasting treatment is 3kg/cm2The duration is 8 minutes.
5) And (3) sending the Mask obtained in the step 4) to an arc chamber for arc cleaning, setting the thickness of an arc layer to be 10 microns, the air pressure to be 3kg, the current to be 60A and the duration to be 8 minutes.
6) Cleaning and drying the Mask obtained in the step 5), and sealing and packaging for reuse.
By adopting the electrolysis method, water is substantially electrolyzed, the consumption of the nitric acid in the electrolyte is very low, only the concentration of the nitric acid needs to be kept, metal ions dissolved in the electrolyte are deposited and recovered at the cathode, the recovered metal can generate benefits, no metal-containing waste water or waste gas exists, and the pollution discharge cost is reduced. According to statistics, in example 1, the electricity consumption per ton of copper recovered by electrolysis is 2000 degrees, and the electricity consumption cost is about 1600 yuan, however, the commercial value per ton of copper can reach 4 ten thousand yuan.
The method for chemically removing copper in the comparative example 1 needs to consume a large amount of nitric acid, is easy to generate a large amount of waste gas, and the copper-containing waste liquid needs to be treated by waste water, so that copper cannot be recovered. According to statistics, in comparative example 1, the process cost comprises alkali consumption (sodium hydroxide) of 600 Kg/ton copper, the consumption cost is about 1500 yuan, nitric acid (concentration is 68%) of 3000 Kg/ton copper, the consumption cost is about 7500 yuan, and the total consumption cost reaches 9000 yuan/ton copper.
Therefore, the method of the invention not only can save cost, but also brings great benefit, and is environment-friendly.

Claims (10)

1. A method for cleaning a Mask in vacuum evaporation equipment is characterized in that the Mask body is made of aluminum, titanium, stainless steel or alloy, and comprises the following steps:
taking a nitric acid solution as an electrolyte, taking a Mask to be cleaned as an anode, respectively immersing the Mask to be cleaned and a cathode into the electrolyte, applying a power supply between the Mask to be cleaned and the cathode, connecting the Mask to be cleaned with the anode of the power supply, connecting the cathode with the cathode of the power supply, dissolving a metal film on the surface of the Mask to be cleaned in the electrolyte to obtain the cleaned Mask, and reducing metal ions dissolved in the electrolyte into metal at the cathode and depositing and recycling the metal ions.
2. The cleaning method according to claim 1, wherein the concentration of the nitric acid solution is 0.5 mol/L to 3 mol/L.
3. The cleaning method according to claim 2, wherein the nitric acid solution further comprises an additive, the concentration of the additive is 0.1 g/L-1 g/L, and the additive is two or three selected from bone glue, thiourea and synuclein.
4. The cleaning method according to any one of claims 1 to 3, wherein the current density of the power supply is 200A/m2～250A/m2And the voltage of the power supply is 1.5V-2V.
5. The cleaning method according to claim 1, further comprising the step of sequentially performing water washing, ultrasonic water washing, sand blasting and arc cleaning on the cleaned Mask.
6. The cleaning method according to claim 5, wherein the pressure of the water washing is 180 to 260 bar.
7. The cleaning method according to claim 5, wherein the ultrasonic frequency of the ultrasonic water washing is 20Hz to 40Hz, and the time of the ultrasonic water washing is 5min to 20 min.
8. The cleaning method according to claim 5, wherein the blasting material model number is W60#, and the blasting pressure of the blasting is 3kg/cm2～4kg/cm2。
9. The cleaning method according to claim 5, wherein in the arc cleaning, the thickness of the arc layer is 10 to 25 μm, the gas pressure is 3 to 5kg, and the current is 60 to 80A.
10. The cleaning method according to claim 1, wherein the cathode is a stainless steel plate, and the metal film is a copper film or a molybdenum film.
CN202010354714.8A 2020-04-29 2020-04-29 Method for cleaning Mask in vacuum evaporation equipment Pending CN111501085A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010354714.8A CN111501085A (en) 2020-04-29 2020-04-29 Method for cleaning Mask in vacuum evaporation equipment

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Application Number Priority Date Filing Date Title
CN202010354714.8A CN111501085A (en) 2020-04-29 2020-04-29 Method for cleaning Mask in vacuum evaporation equipment

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CN111501085A true CN111501085A (en) 2020-08-07

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112680749A (en) * 2020-12-21 2021-04-20 江苏时代华宜电子科技有限公司 Noble metal recovery process based on vacuum sputtering chamber

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB756040A (en) * 1953-04-14 1956-08-29 Sydney John Patmore Improvements in the electro-chemical cleaning of metals
CN1489161A (en) * 2003-08-21 2004-04-14 上海交通大学 Method for removing residual copper of aluminium corroding foil surface of negative electrode for aluminium electrolytic capacitor
CN101031672A (en) * 2005-05-30 2007-09-05 株式会社爱发科 Surface treatment method
CN102817061A (en) * 2012-09-07 2012-12-12 佛山市三水凤铝铝业有限公司 Method for cleaning cathode tubes of electrolysis coloring troughs of aluminum profiles
CN103451712A (en) * 2013-08-11 2013-12-18 唐军 Mask plate cleaning equipment
CN109440117A (en) * 2018-12-29 2019-03-08 深圳仕上电子科技有限公司 The surface treatment method of workpiece

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB756040A (en) * 1953-04-14 1956-08-29 Sydney John Patmore Improvements in the electro-chemical cleaning of metals
CN1489161A (en) * 2003-08-21 2004-04-14 上海交通大学 Method for removing residual copper of aluminium corroding foil surface of negative electrode for aluminium electrolytic capacitor
CN101031672A (en) * 2005-05-30 2007-09-05 株式会社爱发科 Surface treatment method
CN102817061A (en) * 2012-09-07 2012-12-12 佛山市三水凤铝铝业有限公司 Method for cleaning cathode tubes of electrolysis coloring troughs of aluminum profiles
CN103451712A (en) * 2013-08-11 2013-12-18 唐军 Mask plate cleaning equipment
CN109440117A (en) * 2018-12-29 2019-03-08 深圳仕上电子科技有限公司 The surface treatment method of workpiece

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112680749A (en) * 2020-12-21 2021-04-20 江苏时代华宜电子科技有限公司 Noble metal recovery process based on vacuum sputtering chamber
CN112680749B (en) * 2020-12-21 2021-09-28 江苏时代华宜电子科技有限公司 Noble metal recovery process based on vacuum sputtering chamber

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Application publication date: 20200807