CN113862088B - Mask cleaning agent for OLED - Google Patents
Mask cleaning agent for OLED Download PDFInfo
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- CN113862088B CN113862088B CN202111255871.4A CN202111255871A CN113862088B CN 113862088 B CN113862088 B CN 113862088B CN 202111255871 A CN202111255871 A CN 202111255871A CN 113862088 B CN113862088 B CN 113862088B
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- 239000012459 cleaning agent Substances 0.000 title claims abstract description 24
- 239000002738 chelating agent Substances 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 15
- 150000007524 organic acids Chemical class 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000004094 surface-active agent Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 229930182470 glycoside Natural products 0.000 claims description 8
- LRMSQVBRUNSOJL-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)F LRMSQVBRUNSOJL-UHFFFAOYSA-N 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 229940120146 EDTMP Drugs 0.000 claims description 5
- 229940090960 diethylenetriamine pentamethylene phosphonic acid Drugs 0.000 claims description 5
- DUYCTCQXNHFCSJ-UHFFFAOYSA-N dtpmp Chemical compound OP(=O)(O)CN(CP(O)(O)=O)CCN(CP(O)(=O)O)CCN(CP(O)(O)=O)CP(O)(O)=O DUYCTCQXNHFCSJ-UHFFFAOYSA-N 0.000 claims description 5
- NFDRPXJGHKJRLJ-UHFFFAOYSA-N edtmp Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCN(CP(O)(O)=O)CP(O)(O)=O NFDRPXJGHKJRLJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000011148 porous material Substances 0.000 claims description 5
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 150000002338 glycosides Chemical class 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 3
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical compound OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229960001124 trientine Drugs 0.000 claims description 3
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 claims description 2
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 2
- 229940116254 phosphonic acid Drugs 0.000 claims 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 abstract description 8
- 238000001704 evaporation Methods 0.000 abstract description 8
- 230000008020 evaporation Effects 0.000 abstract description 7
- 238000013329 compounding Methods 0.000 abstract description 4
- 229910000073 phosphorus hydride Inorganic materials 0.000 abstract description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052731 fluorine Inorganic materials 0.000 abstract description 3
- 239000011737 fluorine Substances 0.000 abstract description 3
- 239000002736 nonionic surfactant Substances 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 description 25
- 230000000694 effects Effects 0.000 description 13
- 238000000034 method Methods 0.000 description 8
- 238000007740 vapor deposition Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- -1 alkyl glycoside Chemical class 0.000 description 4
- 239000000693 micelle Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 229910001425 magnesium ion Inorganic materials 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- 239000013585 weight reducing agent Substances 0.000 description 3
- 229920001621 AMOLED Polymers 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 229910001374 Invar Inorganic materials 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 238000011895 specific detection Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- 238000000441 X-ray spectroscopy Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000002508 compound effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 150000007529 inorganic bases Chemical class 0.000 description 1
- 238000010406 interfacial reaction Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004093 laser heating Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 description 1
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/83—Mixtures of non-ionic with anionic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/24—Organic compounds containing halogen
- C11D3/245—Organic compounds containing halogen containing fluorine
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/36—Organic compounds containing phosphorus
- C11D3/364—Organic compounds containing phosphorus containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/123—Sulfonic acids or sulfuric acid esters; Salts thereof derived from carboxylic acids, e.g. sulfosuccinates
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/662—Carbohydrates or derivatives
-
- C11D2111/22—
Abstract
The invention provides a Mask cleaning agent for an OLED (organic light emitting diode), which is formed by compounding fluorine-containing organic acid, an organic phosphine chelating agent and an anionic-nonionic surfactant, and can effectively solve the problems that the Mask is difficult to clean the surface, the edge and the open holes after Ag/Mg evaporation in the prior art, so that the yield and the performance of a product are poor, mask materials are corroded, the service life is shortened and the like.
Description
Technical Field
The invention belongs to the field of OLED manufacturing, and particularly relates to a fine metal mask cleaning agent used after Ag/Mg evaporation.
Background
Organic Light Emitting Diodes (OLEDs) have become the dominant display technology in the third generation due to their ultra-high contrast, realistic colors, thin profile, high definition, high refresh rate, etc. The vast majority of the current mainstream OLED screens refer to actively driven organic light emitting diodes (AMOLED). From the aspect of the preparation flow of the AMOLED, the key three technologies are as follows: back plate technology, vapor deposition technology, and packaging technology. In addition to the precise vapor deposition equipment, the vapor deposition technology also needs a Mask (Mask) for vapor deposition, and the Mask determines the pixel height and the size of the OLED display screen. Mask is a costly and consumable item that requires repeated use. In the evaporation process, evaporation material can be deposited on the Mask, so that the evaporation effect is affected, and the service life of the Mask is even affected by blocking the open holes. In the prior art, the Mask is cleaned after being used for a plurality of times during on-line production.
The vapor deposition is to evaporate the material to be evaporated into atoms or molecules by current heating, electron beam bombardment heating, laser heating and other methods in vacuum, and then make linear motion in a larger free path to collide with the surface of the substrate to condense, so as to form a film. It can be said that evaporation is an essential part of the OLED manufacturing process. The luminous organic material is evaporated onto the substrate through the Mask precise holes, the pixel height of the OLED display screen is directly determined by the Mask holes, the smaller the holes are, the higher the pixel is, meanwhile, the smaller the holes are, the easier the organic material is accumulated, and the cleaning frequency and the cleaning requirement are higher.
Currently, single-layer metal cathodes that find application in OLED devices are Mg, li, ca, sr, na, cs, gd, and the like. In order to prevent the adverse effect of water and oxygen on the metal cathode, alloy cathodes Ca/Al, mg/Ag, al/Li, sn/Al, ag/Al and the like are adopted in the process. Among them, alloy cathode Mg/Ag (10:1) formed by co-evaporating metal Mg and metal Ag is most widely used, and most of them are Mg which is difficult to clean due to high Mg content.
Patent CN 112609189A discloses an electronic grade CH 3 COOH, electronic grade H 2 O 2 And Ag/Mg cleaning agent for the Mask and a cleaning method thereof, wherein the Ag/Mg cleaning agent comprises more than 10MΩ pure water, but only has the effect of cleaning the surface of the Mask, has poor cleaning effect on edges and openings, and meanwhile, the addition of hydrogen peroxide brings strong oxidizing property, even if corrosion inhibitor is added, the Ag/Mg cleaning agent has obvious corrosiveness on the Mask, and can influence the service life of the Mask. The patent CN 108659997A impregnates and dissolves metal ions on the surface of Mask at room temperature by forming a powerful complex of inorganic base or quaternary ammonium base and organic acid, but the chelating agent has different chelating constants for different metal ions, and in practice, the cleaning effect on Ag/Mg, especially Mg therein, is limited.
Disclosure of Invention
In view of the defects in the prior art, the invention provides a Mask cleaning agent which can solve the problems that the Mask in the prior art is difficult to clean the surface, the edge and the open holes after Ag/Mg evaporation, so that the product yield and the performance are poor and the like.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the mask cleaning agent for the OLED comprises the following raw materials in percentage by mass: 9-11% of organic acid, 10-20% of chelating agent, 10-20% of surfactant and 50-70% of deionized water; the sum of the compositions of the raw materials is 100 percent.
Wherein the organic acid is fluorine-containing organic acid, and specifically is perfluoropropionic acid. The C-F bond of the fluorinated organic acid has strong electron withdrawing property and strong acidity. The perfluoropropionic acid and the salt thereof have higher interfacial activity, and are favorable for cleaning Ag/Mg films attached to the surfaces, edges and openings of the mask.
The chelating agent is an organic phosphine chelating agent, and specifically is one or more of triethylene tetramine hexamethylene phosphonic acid (TEMMP), diethylene triamine pentamethylene phosphonic acid (DTPMPA) and ethylene diamine tetramethylene phosphonic acid (EDTMPS). The organic phosphine chelating agents have excellent chelating performance and can be matched with Mg 2+ The chelate is stable, has high thermal stability, is easy to biodegrade, is safe and does not pollute the environment.
The surfactant is a surfactant compounded by alkyl glycoside (APG) and alkyl glycoside sulfosuccinate (APG-SS), and when the compounded molar ratio is APG: APG-SS can be 3:7, 2:8 and 1:9, wherein the proportion of 2:8 is the best. The APG-SS and the APG can form an anionic-nonionic compound effect, and bring about a better synergistic effect. APG: the APG-SS surfactant can be mixed in any proportion to reduce the surface tension of APG and improve the surface performance of APG.
The resistivity of the deionized water at 25 ℃ is not lower than 18M omega cm.
The preparation method of the mask cleaning agent comprises the steps of adding deionized water into a stirring kettle at normal temperature, adding perfluoropropionic acid at the rotating speed of 30r/min, adjusting the rotating speed to 60r/min after the addition, sequentially adding AGP-SS, APG and chelating agent (each material is stirred until the system is clarified after being added, then the next material is added), continuously stirring for 30 minutes after all the materials are added, and then filtering through a filter element with the aperture of 5 mu m and the aperture of 1 mu m.
The invention has the remarkable advantages that: according to the Mask cleaning agent, the fluorine-containing organic acid is selected, so that the interfacial reaction activity of the acid and Ag/Mg is effectively improved, and the Ag/Mg film on the Mask can be effectively and rapidly removed; by adding the optimized organic phosphine chelating agent, the chelating performance of Mg ions is effectively improved, the problems of incomplete cleaning or secondary pollution caused by a large amount of Mg ions in the past cleaning are solved, and the surface tension is effectively reduced by excellent synergistic effect of the compounded anionic-nonionic compound surfactant of the alkyl glycoside and the alkyl glycoside derivative, so that the cleaning rate of Ag/Mg films at the Mask edge and the open pore is remarkably improved. The use of the product does not affect the existing Mask cleaning process, the production yield can be effectively improved, and the production cost of enterprises is reduced.
Detailed Description
In order to make the contents of the present invention more easily understood, the technical scheme of the present invention will be further described with reference to the specific embodiments, but the present invention is not limited thereto.
The experimental methods used in the examples are conventional methods unless otherwise specified.
Materials, reagents and the like used in the examples are commercially available unless otherwise specified.
The preparation method comprises the steps of adding deionized water into an experimental kettle at normal temperature, adding perfluoropropionic acid at a rotating speed of 30r/min, adjusting the rotating speed to 60r/min after the addition, sequentially adding AGP-SS, APG and chelating agent (each material is added and stirred until the system is clear and then the next material is added), continuously stirring for 30 minutes after the addition is completed, and sequentially filtering through a filter element with a pore diameter of 5 mu m and a pore diameter of 1 mu m.
TABLE 1 Components and dosage form of mask cleaning agent
Material shorthand description:
triethylene tetramine hexamethylenephosphonic acid (TETHMP)
Diethylene triamine pentamethylene phosphonic acid (DTPMPA)
Ethylenediamine tetramethylene phosphonic acid (EDTMPS)
Alkyl glycoside (APG)
Alkyl glycoside sulfosuccinate (APG-SS)
Tetra sodium ethylenediamine tetraacetate (EDTA 4 Na)
Alkylphenol ethoxylates (Tx-10)
Lauryl alcohol ether phosphate potassium (MAEPK)
All of the above materials are commercially available.
The cleaning agents prepared in the examples and the comparative examples were subjected to performance evaluation, and the specific test method thereof was as follows:
1. optical microscope for detecting cleaning ability
The Mask cleaning ability test of the cleaning agent comprises the step of observing whether the surface, the edge and the open holes are cleaned or not through a microscope. The specific detection method comprises the following steps:
the cleaning agent is diluted to 20% aqueous solution by deionized water, added into an ultrasonic cleaning tank and heated to 30 ℃. Setting the parameters of the ultrasonic cleaning tank to be that the ultrasonic frequency is 60KHz and the ultrasonic energy density is 35w/inch 2 . And (3) vertically placing the Mask subjected to Mg/Ag vapor deposition on a cleaning frame, immersing the cleaning frame in an ultrasonic cleaning tank, and ultrasonically cleaning for 40min.
After the cleaning is finished, three washing ultrasonic tanks are set to have ultrasonic frequency of 60KHz and ultrasonic energy density of 35w/inch 2 Ultrasonic washing with deionized water at room temperature for 3 times, each time for 5min.
After the flushing, the Mask is placed in an isopropanol tank to remove water, and the Mask is cleaned, dried and then detected.
The surface, edges and openings of the Mask were analyzed by Scanning Electron Microscopy (SEM) for metal residue. The criteria are as follows:
o: completely cleaning Mg/Ag film
X: mg/Ag film residue
The residual Mg/Ag content on the Mask surface was detected by X-ray spectroscopy (EDS) and compared with the initial content. The criteria are as follows:
o: the Mg/Ag removal rate is more than 90 percent
Delta 75% < Mg/Ag removal rate < 90%
X: the Mg/Ag removal rate is less than 75 percent
2. Corrosiveness measurement:
the Mask is made of invar alloy (invar), and the cleaning agent is acidic and can corrode for a long time, so that the service life of the Mask is determined by the corrosiveness. The specific detection method comprises the following steps:
300mL of 20% aqueous solution of cleaning agents with different formulas is respectively filled into 500mL glass, a Mask small sample with constant weight is put into the glass, a sealing ring cover is added to prevent water volatilization, after the glass is soaked for 1 week at room temperature, pure water is washed clean, IPA is dehydrated, and the glass is weighed again after the glass is dried to constant weight. The weight change ratio was evaluated by weighing twice, and the criteria were as follows:
o: substantially corrosion-free (weight reduction < 0.05%)
Delta: slight corrosion (0.05% < weight reduction < 0.01%)
X: has corrosion (weight reduction rate > 0.01%)
The test results are shown in Table 2.
Table 2 cleaning agent Performance test results
As can be seen from the comparison of examples and comparative examples, each component outside the compounding ratio range adversely affects the cleaning performance evaluation. Meanwhile, the perfluoropropionic acid is more effective in cleaning the edge with poor ultrasonic action and fine holes because of strong electron withdrawing property of C-F bond and excellent interfacial activity; the chelating ability of other chelating agents to Mg ions is obviously lower than that of 3 selected chelating agents, so that the cleaning effect of Mask is affected due to incomplete cleaning and secondary pollution, and meanwhile, the residual ion of EDS detection exceeds the standard; the compounding ratio of AGP and APG-SS is also important, and the optimal cleaning effect is achieved only in a proper ratio range; in the comparative example, it can be seen that the cleaning effect of other nonionic and anionic surfactants after the anionic-nonionic compound use is also difficult to meet the process requirements.
Based on the proportion data of each component in the example 2, the surface tension of different mixed liquids is continuously measured by a K12 surface tension meter hanging piece at 20 ℃, the experimental data are measured under a cleaning agent system, the cleaning system is added with organic acid and chelating agent to directly influence the surface tension of the system, and the data measured by directly compounding APG and APG-SS are different. From the experimental data it can be seen that: APG: the APG-SS surfactant can be mixed in any proportion to reduce the surface tension of APG and improve the surface performance of APG. When (when)nAPG∶nAPG-ss=2:8, the synergistic effect is better. When the content of APG-SS is increased to a certain amount, the change in surface tension is small. This is probably due to the fact that APG and APG-SS molecules "intercalate" into APG molecules when forming mixed micelles, reducing electrostatic repulsion between APG head groups, reducing charge density on the surface of the micelles, and enhancing the ability to form micelles. The number of APG-SS molecules determines the ability to reduce electrostatic repulsion, and when the number of APGs reaches a certain amount, the reduction effect on the micelle surface charge density is reduced.
TABLE 3 Effect of different surfactant compositions in mask cleaning Agents on surface tension
The foregoing description is only of the preferred embodiments of the present invention and is not intended to limit the scope of the claims, and all equivalent modifications made by the teachings of this invention, directly or indirectly, are intended to be included within the scope of this invention.
Claims (4)
1. The mask cleaning agent for the OLED is characterized by comprising the following raw materials in percentage by mass: 9-11% of organic acid, 10-20% of chelating agent, 10-20% of surfactant and 50-70% of deionized water; the sum of the compositions of the raw materials is 100 percent;
wherein the organic acid is perfluoropropionic acid;
wherein the surfactant is a surfactant compounded by alkyl glycoside APG and alkyl glycoside sulfosuccinate APG-SS;
APG: the APG-SS compound molar ratio is one of 3:7, 2:8 and 1:9;
the chelating agent is one or more of triethylene tetramine hexamethylene phosphonic acid, diethylene triamine pentamethylene phosphonic acid and ethylenediamine tetramethylene phosphonic acid.
2. The mask cleaning agent for OLED according to claim 1, wherein APG: the compound molar ratio of APG-SS is 2:8.
3. The mask cleaning agent for an OLED according to claim 1, wherein: the resistivity of the deionized water at 25 ℃ is not lower than 18M omega cm.
4. The mask cleaning agent for an OLED according to claim 1, wherein: the preparation method comprises the steps of adding deionized water into a stirring kettle at normal temperature, adding perfluoropropionic acid at the rotating speed of 30r/min, adjusting the rotating speed to 60r/min after the addition, sequentially adding APG-SS, APG and chelating agent, stirring each material until the system is clear after the material is put into the stirring kettle, adding the next material, continuously stirring for 30 minutes after all the materials are added, and filtering through a filter element with the pore diameter of 5 mu m and the pore diameter of 1 mu m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111255871.4A CN113862088B (en) | 2021-10-27 | 2021-10-27 | Mask cleaning agent for OLED |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111255871.4A CN113862088B (en) | 2021-10-27 | 2021-10-27 | Mask cleaning agent for OLED |
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| Publication Number | Publication Date |
|---|---|
| CN113862088A CN113862088A (en) | 2021-12-31 |
| CN113862088B true CN113862088B (en) | 2023-11-10 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202111255871.4A Active CN113862088B (en) | 2021-10-27 | 2021-10-27 | Mask cleaning agent for OLED |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001005921A1 (en) * | 1999-07-15 | 2001-01-25 | Rhodia Chimie | Use of an amphoteric polymer for treating a hard surface |
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