CN111172550B - OLED mask cleaning agent and cleaning process thereof - Google Patents
OLED mask cleaning agent and cleaning process thereof Download PDFInfo
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- CN111172550B CN111172550B CN202010093828.1A CN202010093828A CN111172550B CN 111172550 B CN111172550 B CN 111172550B CN 202010093828 A CN202010093828 A CN 202010093828A CN 111172550 B CN111172550 B CN 111172550B
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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
- 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
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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
- 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
- C23G5/036—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 having also nitrogen
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Abstract
The invention belongs to the technical field of preparation of fine metal mask cleaning agents, and particularly relates to a cleaning agent for an OLED (organic light emitting diode) mask and a cleaning tool thereofA process for preparing the composite material. The composition comprises the following components in percentage by mass: 20% -50% of an alcohol ether solvent; 20% -50% of polar aprotic solvent; 1% -10% of fluorine-containing nonionic surfactant; 10% -30% of deionized water; the fluorine-containing nonionic surfactant has a structural formula shown in the specification;
n is a natural number between 8 and 14; the cleaning solution can quickly and effectively clean and remove RGB photochromic dyes attached to the FMM in the evaporation process, is easy to clean and free from residues, and effectively improves the cleaning efficiency of the FMM.
Description
Technical Field
The invention belongs to the technical field of preparation of fine metal mask cleaning agents, and particularly relates to a cleaning agent for an OLED mask and a cleaning process thereof.
Background
Flat Panel Displays (FPD) are one of the most important optoelectronic products, and the mainstream flat Panel displays can be classified into Liquid Crystal Displays (LCD) and Organic Light Emitting Diodes (OLED). The OLED display has the characteristics of self-luminescence, wide color gamut, wide viewing angle, short response time, high luminous efficiency, low working voltage, light weight, capability of manufacturing large-size and flexible panels, simple manufacturing process and the like, and is a new generation display which is acknowledged in the industry and can possibly replace the LCD.
The existing mature OLED display manufacturing process is an OLED evaporation technology, and products of the OLED display manufacturing process are widely applied to the fields of smart phones, intelligent wearing, VR (virtual reality) and the like. The evaporation technology needs a precise evaporation device and also needs a Fine Metal Mask (FMM) for evaporation, the FMM is usually bound to a Metal Mask frame after a pattern is etched from a Ni-Co alloy (iron-nickel-cobalt super Invar, Invar) with a thickness of 30-50 micrometers, and the FMM determines the height and the size of pixels of the OLED display screen. In the repeated evaporation process of the FMM, small-molecule organic materials (RGB photochromic dyes, etc.) are deposited on the FMM, causing blockage and pollution, and seriously affecting the effect of subsequent evaporation. In production, a piece of FMM typically needs to be cleaned after 20 to 30 uses to ensure its subsequent performance.
The traditional FMM cleaning front section only adopts solvent soaking cleaning, the cleaning capability is limited, the dissolving and stripping effects on small molecule RGB organic dyes are low, and even long-time improper soaking in the using process can influence the service life of the FMM, so that the preparation cost of an OLED display is increased.
Disclosure of Invention
The invention aims to provide a cleaning agent for an OLED mask, which can quickly and effectively clean and remove RGB (red, green and blue) photochromic dyes attached to an FMM in an evaporation process, is easy to clean and does not remain, and effectively improves the cleaning efficiency of the FMM.
Firstly, providing a fluorine-containing nonionic surfactant, wherein the structural formula of the fluorine-containing nonionic surfactant is shown as a formula I;
formula I
n is a natural number between 8 and 14.
Specifically, n is 10 or 12.
The fluorine-containing nonionic surfactant can be prepared by the following method:
by para-etherifying boron trifluoride (BF)3(CH3)2O) is used as a catalyst, under the protection of nitrogen, the low polyethylene glycol (1 mol) is heated to 100 ℃, difluorophenyl ethylene oxide (1.1 mol) is slowly dripped, dripping is completed within 2 hours, the target fluorine-containing nonionic surfactant can be obtained after reaction for about 4 hours, the product is washed by acidified deionized water with the pH value of 3-4 at 80 ℃, and is dried for 3 hours under the vacuum condition of 105 ℃ after being filtered, so that the target fluorine-containing nonionic surfactant can be obtained;
the invention further provides a cleaning agent for the OLED mask, which comprises the following components in percentage by mass:
20% -50% of an alcohol ether solvent;
20% -50% of polar aprotic solvent;
1% -10% of fluorine-containing nonionic surfactant;
10% -30% of deionized water;
the sum of the total mass fractions is 100%.
Specifically, the glass substrate environment-friendly water-based cleaning solution comprises any one of the following compositions 1) to 6):
1）
30% -45% of alcohol ether solvent;
20% -50% of polar aprotic solvent;
1% -10% of fluorine-containing nonionic surfactant;
deionized water; 10% -30%;
the sum of the total mass fractions is 100%.
2）
20% -50% of an alcohol ether solvent;
30% -50% of polar aprotic solvent;
1% -10% of fluorine-containing nonionic surfactant;
deionized water; 10% -30%;
the sum of the total mass fractions is 100%.
3）
20% -50% of an alcohol ether solvent;
20% -50% of polar aprotic solvent;
3% -8% of fluorine-containing nonionic surfactant;
deionized water; 10% -30%;
the sum of the total mass fractions is 100%.
4）
20% -50% of an alcohol ether solvent;
20% -50% of polar aprotic solvent;
1% -10% of fluorine-containing nonionic surfactant;
20% -25% of deionized water;
the sum of the total mass fractions is 100%.
5）
30% -40% of alcohol ether solvent;
20% -40% of polar aprotic solvent;
1% -10% of fluorine-containing nonionic surfactant;
10% -30% of deionized water;
the sum of the total mass fractions is 100%.
6）
30% -50% of alcohol ether solvent;
25% -50% of polar aprotic solvent;
1% -10% of fluorine-containing nonionic surfactant;
15% -25% of deionized water;
the sum of the total mass fractions is 100%.
In the cleaning agent for the OLED mask, the alcohol ether solvent is one selected from the group consisting of: diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, propylene glycol monomethyl ether, dipropylene glycol monomethyl ether, of which propylene glycol methyl ether and diethylene glycol butyl ether are preferred. The alcohol ether solvent has better dissolving power for RGB photochromic dyes, can reduce the tension between the photochromic dye microparticles in a suspension state and the FMM, effectively reduces the secondary adhesion of the photochromic dyes, and is beneficial to the washing and cleaning process of the rear section.
In the cleaning agent for the OLED mask, the polar aprotic solvent is selected from one or a combination of any two of dioxane (Diox), tetrahydrofurfuryl alcohol (THFA), N-methylpyrrolidone (NMP), monomethyl formamide (NMF), dimethyl formamide (DMF) and dimethyl imidazolidinone (DMI). Among them, tetrahydrofurfuryl alcohol and dimethylimidazolidinone having a higher boiling point are preferable. The polar aprotic solvent has extremely excellent dissolving capacity for RGB photochromic dyes, is excellent in water solubility and high in boiling point, can keep the stability of a cleaning agent system, and improves the reliability of a cleaning agent and the easy rinsing property of a rear section.
In the cleaning agent for the OLED mask, the fluorine-containing nonionic surfactant is a fluorine-containing nonionic surfactant shown in a formula I:
formula I
n is a natural number between 8 and 14, and specifically, n is 10 or 12.
The hydrophilic group of the fluorine-containing nonionic surfactant molecule can form multi-point adsorption with the surface of the FMM, the permeation pressure of the photochromic dye during cleaning enables free active agent molecules in the solution and unadsorbed free parts on the hydrophilic group of the adsorbed active agent molecules to actively go deep into a contact gap between the FMM and the particles, and the dissolution of the solvent and the photochromic dye molecules is effectively reduced and improved; meanwhile, the unique C-F bond in the molecular structure enables the cleaning agent system to have high surface activity, high chemical stability and high heat-resistant stability.
In the cleaning agent for the OLED mask, the resistivity of the deionized water is not lower than 18 MOmega at 25 ℃.
The cleaning agent for the OLED mask provided by the invention can effectively remove micromolecular RGB photochromic dyes and the like deposited on the FMM after repeated evaporation process, has strong stability, can be used for cleaning at higher temperature, improves the cleaning efficiency, has higher reliability and cannot corrode the FMM. Meanwhile, the method for cleaning the FMM by using the cleaning solution is simple and has excellent cleaning effect.
In order to meet the requirement of cleaning the surface of the FMM, the invention also provides a cleaning method (as shown in figure 1) of the cleaning agent for the OLED mask, wherein the whole cleaning process of the cleaning method is completed by an ultrasonic cleaning machine, and the cleaning method comprises the following steps:
1. cleaning by using a cleaning agent for one time: fixing the FMM on a cleaning frame, putting the FMM into an ultrasonic cleaning machine added with a cleaning agent, heating to 50-60 ℃, carrying out ultrasonic frequency of 60KHz, and soaking and cleaning for 10 minutes.
2. Secondary cleaning by using a cleaning agent: and (3) putting the FMM fixed on the cleaning frame into a second ultrasonic cleaning tank added with a cleaning agent, heating to 50-60 ℃ in the same way, carrying out ultrasonic frequency of 60KHz, and soaking and cleaning for 10 minutes.
3. And (3) once washing with deionized water: and (3) putting the FMM fixed on the cleaning frame into a third ultrasonic cleaning tank added with deionized water, heating to 35-45 ℃, carrying out ultrasonic frequency of 60KHz, and soaking and cleaning for 5 minutes.
4. And (3) secondary washing with deionized water: and (3) putting the FMM fixed on the cleaning frame into a fourth ultrasonic cleaning tank added with deionized water, heating to 35-45 ℃, carrying out ultrasonic frequency of 60KHz, and soaking and cleaning for 5 minutes.
5. Drying: drying with high-pressure clean nitrogen, placing into a nitrogen protection oven, and baking at 70 ℃ for 30 minutes.
The invention has the following remarkable advantages:
(1) the cleaning agent can quickly and effectively clean and remove RGB photochromic dyes attached to the surface of the FMM in the evaporation process, is easy to clean and does not remain, and the cleaning efficiency of the FMM is effectively improved.
(2) The cleaning agent has excellent effect of removing photochromic dye attached to FMM pattern pores,
(3) the cleaning agent disclosed by the invention is strong in system stability, can be used for cleaning at a higher temperature, improves the cleaning efficiency, has higher reliability and cannot corrode FMM.
(4) The cleaning agent has high cleaning efficiency, and the cleaning yield can reach more than 95%.
Drawings
FIG. 1 is a flow chart of the cleaning of a reticle.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1: cleaning agent for OLED mask
The composite material comprises the following components in percentage by weight:
35% of diethylene glycol butyl ether, 35% of tetrahydrofurfuryl alcohol, 3.4-difluorophenyl hydroxy poly (10) ethylene oxide (in the formula I, n is 10) 3% and 27% of deionized water.
Example 2 cleaning agent for OLED mask
The composite material comprises the following components in percentage by weight:
30% of propylene glycol methyl ether, 35% of tetrahydrofurfuryl alcohol, 5% of 3, 4-difluorophenyl hydroxy poly (10) ethylene oxide (in the formula I, n is 10) and 30% of deionized water.
Example 3 cleaning agent for OLED mask
The composite material comprises the following components in percentage by weight:
dipropylene glycol monomethyl ether 40%, tetrahydrofurfuryl alcohol 35%, 3, 4-difluorophenyl hydroxy poly (12) ethylene oxide (in the formula I, n is 12) 3%, and deionized water 22%.
Example 4 cleaning agent for OLED mask
The composite material comprises the following components in percentage by weight:
25% of propylene glycol methyl ether, 45% of dimethyl imidazolidinone, 7% of 3-4-difluorophenyl hydroxy poly (12) ethylene oxide (in the formula I, n is 12) and 23% of deionized water.
Example 5 cleaning agent for OLED mask
The composite material comprises the following components in percentage by weight:
40% of propylene glycol methyl ether, 40% of dimethyl imidazolidinone, 3% of 3-4-difluorophenyl hydroxy poly (12) ethylene oxide (in the formula I, n is 12), and 17% of deionized water.
Example 6 cleaning agent for OLED mask
The composite material comprises the following components in percentage by weight:
diethylene glycol monobutyl ether 30%, tetrahydrofurfuryl alcohol 25%, N-methyl pyrrolidone 25%, 3-4-difluorophenyl hydroxy poly (12) ethylene oxide (in the formula I, N is 12) 2% and deionized water 18%.
Measurement of cleaning Performance of cleaning solution
The cleaning liquid compositions prepared in examples 1 to 6 were subjected to performance evaluation, and the specific test methods thereof were as follows:
1. cleaning by using a cleaning agent for one time: fixing the FMM on a cleaning frame, putting the FMM into an ultrasonic cleaning machine added with a cleaning agent, heating to 50-60 ℃, carrying out ultrasonic frequency of 60KHz, and soaking and cleaning for 10 minutes.
2. Secondary cleaning by using a cleaning agent: and (3) putting the FMM fixed on the cleaning frame into a second ultrasonic cleaning tank added with a cleaning agent, heating to 50-60 ℃ in the same way, carrying out ultrasonic frequency of 60KHz, and soaking and cleaning for 10 minutes.
3. And (3) once washing with deionized water: and (3) putting the FMM fixed on the cleaning frame into a third ultrasonic cleaning tank added with deionized water, heating to 35-45 ℃, carrying out ultrasonic frequency of 60KHz, and soaking and cleaning for 5 minutes.
4. And (3) secondary washing with deionized water: and (3) putting the FMM fixed on the cleaning frame into a fourth ultrasonic cleaning tank added with deionized water, heating to 35-45 ℃, carrying out ultrasonic frequency of 60KHz, and soaking and cleaning for 5 minutes.
5. Drying: drying with high-pressure clean nitrogen, placing into a nitrogen protection oven, and baking at 70 ℃ for 30 minutes.
The surface cleanliness of the washed FMM was observed by an electron microscope. Through detection, photochromic dyes attached to the surface and among the pores of the FMM in the evaporation process can be effectively cleaned, no stains or residual water printing detergent exist after cleaning, and the working requirement of repeated use can be met.
Comparative example 1:
20% of diethylene glycol butyl ether, 30% of tetrahydrofurfuryl alcohol, 5% of 3-4-difluorophenyl hydroxy poly (12) ethylene oxide (in the formula I, n is 12) and 45% of deionized water.
Comparative example 2:
65% of diethylene glycol butyl ether, 15% of N-methylpyrrolidone, 2% of 3-4-difluorophenyl hydroxy poly (12) ethylene oxide (in the formula I, N is 12) and 18% of deionized water.
Comparative example 3:
diethylene glycol monobutyl ether 40%, tetrahydrofurfuryl alcohol 45%, 3-4-difluorophenyl hydroxy poly (12) ethylene oxide (in the formula I, n is 12) 10%, and deionized water 5%.
Comparative example 4:
80% of tetrahydrofurfuryl alcohol, 2% of 3-4-difluorophenyl hydroxy poly (12) ethylene oxide (in the formula I, n is 12) and 18% of deionized water.
Comparative example 5:
40% of diethylene glycol butyl ether, 40% of tetrahydrofurfuryl alcohol and 20% of deionized water.
Comparative example 6:
NMP 100%
the cleaning liquid compositions prepared in comparative examples 1 to 6 were subjected to performance evaluation, and the specific test methods thereof were the same as in examples, and the test results thereof are detailed in Table 1
TABLE 1
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the claims, and all equivalent component changes that can be directly or indirectly applied to other related technical fields using the content of the present invention are also included in the scope of the present invention.
Claims (7)
1. The cleaning agent for the OLED mask is characterized in that: the composition comprises the following components in percentage by mass:
20% -50% of an alcohol ether solvent;
20% -50% of polar aprotic solvent;
1% -10% of fluorine-containing nonionic surfactant;
10% -30% of deionized water;
the sum of the total mass fraction is 100 percent;
the structural formula of the fluorine-containing nonionic surfactant is shown as a formula I;
formula I
n is a natural number between 8 and 14;
the alcohol ether solvent is one selected from the group consisting of: diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, propylene glycol monomethyl ether, dipropylene glycol monomethyl ether; the polar aprotic solvent is selected from any one or two of dioxane Diox, tetrahydrofurfuryl alcohol THFA, N-methyl pyrrolidone NMP, monomethyl formamide NMF, dimethyl formamide DMF and dimethyl imidazolidinone DMI.
2. The cleaning agent for the OLED mask as claimed in claim 1, wherein: specifically, n is 10 or 12.
3. The cleaning agent for the OLED mask as claimed in claim 1, wherein: the alcohol ether solvent is propylene glycol methyl ether or diethylene glycol butyl ether.
4. The cleaning agent for the OLED mask as claimed in claim 1, wherein: the polar aprotic solvent is one or two selected from tetrahydrofurfuryl alcohol and dimethyl imidazolidinone.
5. The cleaning agent for the OLED mask as claimed in claim 1, wherein: the deionized water has a resistivity of not less than 18M omega at 25 ℃.
6. A cleaning process of the cleaning agent for the OLED mask as claimed in any one of claims 1 to 5, characterized in that: comprises the following steps
a. Cleaning by using a cleaning agent for one time: fixing the FMM on a cleaning frame, putting the FMM into an ultrasonic cleaning machine added with a cleaning agent, heating to 50-60 ℃, carrying out ultrasonic frequency of 60KHz, and soaking and cleaning for 10 minutes;
b. secondary cleaning by using a cleaning agent: putting the FMM fixed on the cleaning frame into a second ultrasonic cleaning tank added with a cleaning agent, heating to 50-60 ℃ in the same way, and soaking and cleaning for 10 minutes at an ultrasonic frequency of 60 KHz;
c. and (3) once washing with deionized water: placing the FMM fixed on the cleaning frame into a third ultrasonic cleaning tank added with deionized water, heating to 35-45 ℃, carrying out ultrasonic frequency of 60KHz, and soaking and cleaning for 5 minutes;
d. and (3) secondary washing with deionized water: placing the FMM fixed on the cleaning frame into a fourth ultrasonic cleaning tank added with deionized water, heating to 35-45 ℃, and soaking and cleaning for 5 minutes at an ultrasonic frequency of 60 KHz;
e. drying: drying with high-pressure clean nitrogen, and baking in a nitrogen-protected oven.
7. The cleaning process of claim 6, wherein: the drying in the step e specifically comprises the following steps: baking at 70 deg.C for 30 min.
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| KR100207982B1 (en) * | 1996-07-19 | 1999-07-15 | 윤종용 | Cleaner & cleaning method of metalmask for improving continuance of printing in surface mounting process |
| JP3833650B2 (en) * | 2003-12-04 | 2006-10-18 | 関東化学株式会社 | Cleaning liquid composition and cleaning method for mask used in vacuum deposition process of low molecular organic EL device production |
| CN102477358B (en) * | 2010-11-29 | 2014-03-19 | 江苏协鑫硅材料科技发展有限公司 | Silicon wafer cleaning agent |
| TW201323102A (en) * | 2011-12-15 | 2013-06-16 | Dongwoo Fine Chem Co Ltd | Method for cleaning vapor deposition mask for manufacture of organic EL devices and cleaning solution composition for organic EL mask |
| CN105154821A (en) * | 2015-07-31 | 2015-12-16 | 深圳市星火辉煌系统工程有限公司 | Cleaning technology of organic evaporation MASK |
| CN108424818A (en) * | 2017-02-14 | 2018-08-21 | 东友精细化工有限公司 | Cleaning masks liquid composition |
| WO2019003605A1 (en) * | 2017-06-26 | 2019-01-03 | Ａｇｃ株式会社 | Method for washing mask for vacuum vapor deposition and rinsing composition |
| CN108085173A (en) * | 2017-12-06 | 2018-05-29 | 深圳市合明科技有限公司 | For cleaning the neutral aqueous cleaning agent of camera lens and lens assembly |
| CN109439463A (en) * | 2018-12-20 | 2019-03-08 | 深圳市众望丽华实业有限公司 | Aqueous cleaning agent and its preparation method and application |
| CN111472013A (en) * | 2020-04-08 | 2020-07-31 | 四川富乐德科技发展有限公司 | Cleaning method for surface evaporation material of Open Mask of O L ED Mask |
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