CN115161650A - Neutral metal cleaning agent for MASK MASK plate - Google Patents
Neutral metal cleaning agent for MASK MASK plate Download PDFInfo
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- CN115161650A CN115161650A CN202210996884.5A CN202210996884A CN115161650A CN 115161650 A CN115161650 A CN 115161650A CN 202210996884 A CN202210996884 A CN 202210996884A CN 115161650 A CN115161650 A CN 115161650A
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- Prior art keywords
- mask
- neutral metal
- ammonium
- agent
- heavy metal
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Links
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 24
- 239000002184 metal Substances 0.000 title claims abstract description 24
- 230000007935 neutral effect Effects 0.000 title claims abstract description 21
- 239000012459 cleaning agent Substances 0.000 title claims abstract description 20
- 229910001385 heavy metal Inorganic materials 0.000 claims abstract description 26
- 239000002738 chelating agent Substances 0.000 claims abstract description 22
- 229920000642 polymer Polymers 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 7
- 239000007800 oxidant agent Substances 0.000 claims abstract description 7
- 239000004094 surface-active agent Substances 0.000 claims abstract description 7
- 239000003002 pH adjusting agent Substances 0.000 claims abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- -1 tetradecyl-dimethyl ammonium pyridinium bromide Chemical compound 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 230000001590 oxidative effect Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 claims description 5
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 4
- 239000005695 Ammonium acetate Substances 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 235000019257 ammonium acetate Nutrition 0.000 claims description 4
- 229940043376 ammonium acetate Drugs 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000011593 sulfur Substances 0.000 claims description 3
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 2
- JHWIEAWILPSRMU-UHFFFAOYSA-N 2-methyl-3-pyrimidin-4-ylpropanoic acid Chemical compound OC(=O)C(C)CC1=CC=NC=N1 JHWIEAWILPSRMU-UHFFFAOYSA-N 0.000 claims description 2
- 239000004254 Ammonium phosphate Substances 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- VZTDIZULWFCMLS-UHFFFAOYSA-N ammonium formate Chemical compound [NH4+].[O-]C=O VZTDIZULWFCMLS-UHFFFAOYSA-N 0.000 claims description 2
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 2
- 229910021538 borax Inorganic materials 0.000 claims description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 2
- UMGXUWVIJIQANV-UHFFFAOYSA-M didecyl(dimethyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCC[N+](C)(C)CCCCCCCCCC UMGXUWVIJIQANV-UHFFFAOYSA-M 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 235000010333 potassium nitrate Nutrition 0.000 claims description 2
- 239000004323 potassium nitrate Substances 0.000 claims description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 2
- 235000011151 potassium sulphates Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000010344 sodium nitrate Nutrition 0.000 claims description 2
- 239000004317 sodium nitrate Substances 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 2
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 claims description 2
- 101000928335 Homo sapiens Ankyrin repeat and KH domain-containing protein 1 Proteins 0.000 claims 7
- 101000701393 Homo sapiens Serine/threonine-protein kinase 26 Proteins 0.000 claims 7
- 102100030617 Serine/threonine-protein kinase 26 Human genes 0.000 claims 7
- LCZIQCSYIXULBD-UHFFFAOYSA-N 2-chloroacetic acid;dodecan-1-amine Chemical compound [O-]C(=O)CCl.CCCCCCCCCCCC[NH3+] LCZIQCSYIXULBD-UHFFFAOYSA-N 0.000 claims 1
- UXLDDQXHPVSLKN-UHFFFAOYSA-N S(=O)(=O)([O-])[O-].C(CCCCCCCCCCCCCCCCC)[NH3+].C(CCCCCCCCCCCCCCCCC)[NH3+] Chemical compound S(=O)(=O)([O-])[O-].C(CCCCCCCCCCCCCCCCC)[NH3+].C(CCCCCCCCCCCCCCCCC)[NH3+] UXLDDQXHPVSLKN-UHFFFAOYSA-N 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 238000004140 cleaning Methods 0.000 abstract description 11
- 229910052769 Ytterbium Inorganic materials 0.000 abstract description 10
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052709 silver Inorganic materials 0.000 abstract description 8
- 239000004332 silver Substances 0.000 abstract description 8
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 230000009102 absorption Effects 0.000 description 9
- 238000010521 absorption reaction Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 238000001704 evaporation Methods 0.000 description 7
- 230000008020 evaporation Effects 0.000 description 7
- 229910001374 Invar Inorganic materials 0.000 description 6
- 229910045601 alloy Inorganic materials 0.000 description 6
- 239000000956 alloy Substances 0.000 description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 5
- 230000000536 complexating effect Effects 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 5
- 229910052749 magnesium Inorganic materials 0.000 description 5
- 239000007769 metal material Substances 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 229920002125 Sokalan® Polymers 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- SJCKRGFTWFGHGZ-UHFFFAOYSA-N magnesium silver Chemical compound [Mg].[Ag] SJCKRGFTWFGHGZ-UHFFFAOYSA-N 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000001509 sodium citrate Substances 0.000 description 3
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000004584 polyacrylic acid Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 241001268993 Heterochrosis Species 0.000 description 1
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 1
- 229920002873 Polyethylenimine Polymers 0.000 description 1
- NGOVNSCURCOLBI-UHFFFAOYSA-N azanium;octadecyl sulfate Chemical compound N.CCCCCCCCCCCCCCCCCCOS(O)(=O)=O NGOVNSCURCOLBI-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- DKVNPHBNOWQYFE-UHFFFAOYSA-N carbamodithioic acid Chemical group NC(S)=S DKVNPHBNOWQYFE-UHFFFAOYSA-N 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000011086 high cleaning Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000003334 secondary amides Chemical class 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000176 sodium gluconate Substances 0.000 description 1
- 229940005574 sodium gluconate Drugs 0.000 description 1
- 235000012207 sodium gluconate Nutrition 0.000 description 1
- 230000002195 synergetic effect Effects 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
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
-
- 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
- C23G1/24—Cleaning or pickling metallic material with solutions or molten salts with neutral solutions
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/34—Introducing sulfur atoms or sulfur-containing groups
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Detergent Compositions (AREA)
Abstract
The invention discloses a neutral metal cleaning agent for a MASK MASK plate, and belongs to the technical field of OLED (organic light emitting diode) cleaning agents. The neutral metal cleaning agent comprises the following components in percentage by weight: 5-30% of an oxidizing agent, 10-20% of an inorganic salt, 5-15% of a polymeric heavy metal chelating agent, 1-10% of a pH adjusting agent, 5-15% of a surfactant, 55-75% of deionized water. The neutral metal cleaning agent disclosed by the invention has strong chelating capacity on heavy metals such as silver, ytterbium and the like by adopting the polymer heavy metal chelating agent prepared by synthesis, and can effectively improve the cleaning efficiency and cleaning effect. The cleaning agent has good component compatibility, small smell, environmental friendliness and no corrosiveness, and cannot damage MASK MASK plates.
Description
Technical Field
The invention belongs to the technical field of OLED (organic light emitting diode) cleaning agents, and particularly relates to a neutral metal cleaning agent for a MASK (MASK) plate.
Background
Evaporation is one of the core processes of the OLED, and is also the second stage in the OLED process. The evaporation must be performed in a vacuum environment, and when the mask is ready, an evaporation source (e.g., a commonly used cathode material) is placed under it and heated to an appropriate temperature. When heating begins, small organic molecules in the molecular units pass through a Metal MASK (Fine Metal MASK) and are deposited in the desired locations. The evaporation source is mainly metal particles, and the composition of the evaporation source is 70-90% of silver, 10-20% of magnesium and a small amount of ytterbium. After the evaporation is finished, a large amount of cathode metal materials are attached to the mask plate, so that the service life of the mask plate is influenced.
The common cleaning agent in the market at present has the problems of cleaning residue, slow dissolving rate, turbid solution, precipitate, corrosion to a mask plate, high liquid medicine cost and the like. CN202010834449.3 discloses an effective stripping cleaning agent for metal magnesium and silver, which is prepared by mixing 16% of hydrogen peroxide, 18% of oxalic acid, 2% of nonylphenol polyoxyethylene ether, 8% of acetic acid, 3% of tetrasodium ethylene diamine tetraacetate, 3% of sodium gluconate and 50% of pure water into a solution, and the stripping cleaning agent for magnesium and silver has the advantages of high cleaning speed, high efficiency, simple waste liquid treatment and environmental protection; however, from the view of the formula structure, the corrosion to the mask is strong, the damage is easy to cause, and secondly, the complexing ability to heavy metal is poor, a stable complex can not be formed, the dissolution balance is influenced, the continuous proceeding of the reaction is inhibited, and simultaneously, a plurality of precipitates are easy to generate.
Disclosure of Invention
The neutral metal cleaning agent disclosed by the invention aims to improve the cleaning performance of a cathode metal material, promotes the dissolution reaction rate through stronger complexing capacity, and meanwhile, has the advantages of good component compatibility, small smell, environmental friendliness, no corrosiveness and no damage to a MASK MASK plate.
In order to realize the purpose, the invention adopts the following technical scheme:
a neutral metal cleaning agent applied to a MASK MASK plate comprises the following components in percentage by mass:
5-30% of an oxidant;
10-20% of inorganic salt;
5-15% of a polymer heavy metal chelating agent;
1-10% of pH regulator;
5-15% of a surfactant;
55-75% of deionized water;
the sum of the weight percentages of the components is 100 percent.
Further, the oxidant is at least one of hydrogen peroxide, hydrochloric acid, sulfuric acid, acetic acid, peracetic acid and sodium dichromate; the inorganic salt is at least one of sodium sulfate, ammonium phosphate, potassium sulfate, sodium borate, ammonium nitrate, sodium nitrate and potassium nitrate.
Further, the structural formula of the polymer heavy metal chelating agent is as follows:
wherein n =10-13,x is CS 2 Mole ratio to mer, x =2,3 or 4.
Further, the preparation method of the polymer heavy metal chelating agent comprises the following steps:
1) Adding tetraethylenepentamine into a container, adding concentrated sulfuric acid serving as a catalyst, protecting by using nitrogen, heating to 130 ℃, and dropwise adding acrylic acid; and (3) keeping the temperature in the container at 130-140 ℃ in the dripping process, then heating to 180 ℃ for 6 hours, stopping the reaction, standing and cooling to room temperature to obtain yellow viscous liquid, wherein the intermediate is polyacrylic acid-tetraethylenepentamine.
2) Dissolving polyacrylic acid-tetraethylenepentamine by absolute ethyl alcohol, and respectively adding the solution according to CS 2 Addition of CS in a molar ratio of x to the units 2 Reacting with NaOH; adding NaOH, stirring to dissolve, and adding CS 2 Reacting with absolute ethyl alcohol at 25 ℃ for 8 h, removing the solvent after the reaction is finished, and drying in vacuum to obtain the polymer heavy metal chelating agent with different sulfur contents; wherein x =2,3 or 4.
Further, the pH regulator is one of triethanolamine, acetic acid, ammonium acetate, sodium citrate, ammonium formate, potassium carbonate and sodium carbonate; the surfactant is one of octadecyl sulfate ammonium, dodecyl chloroacetate ammonium, didecyl dimethyl ammonium bromide, tetradecyl-dimethyl pyridinium ammonium bromide and triethanolamine distearate methyl ammonium sulfate; the deionized water has a resistivity of not less than 15M omega at 25 ℃.
The invention has the beneficial effects that:
(1) The polymer heavy metal chelating agent adopted by the neutral metal cleaning agent is prepared by taking polyacrylic acid as a main chain, linking tetraethylenepentamine side chains on the polyacrylic acid, and then utilizing CS 2 The side chain of tetraethylenepentamine is modified, and the complex has strong complexing ability to silver, ytterbium and other heavy metal materials which are difficult to complex. The present invention relates to a method for synthesizing a heavy metal ion chelating agent, and more particularly to a method for synthesizing a heavy metal ion chelating agent, which is characterized in that chelating groups such as carboxyl, hydroxyl, aminodithioformic acid and the like are introduced into linear polymer chains such as polyvinylamine or polyethyleneimine, and the chelating groups on the flocculant molecules can not be effectively chelated with heavy metal ions and are idle due to steric hindrance.
(2) The neutral metal cleaning agent can improve the cleaning performance of the cathode metal material, promotes the dissolution reaction rate through stronger complexing ability, does not cause corrosion damage to a mask plate, and is environment-friendly, small in smell and stable in components.
Drawings
FIG. 1 is an FTIR spectrum of poly (acrylic acid) -tetraethylenepentamine (a) and a polymeric heavy metal chelator (b); as can be seen, at 3272 cm -1 The strong absorption peak can be assigned as N-H stretching vibration absorption peak in the molecular structure; 2936cm -1 And 2825cm -1 Can be assigned as-CH 2 -asymmetric and symmetric stretching vibration absorption peaks; at 1646 cm -1 The peak appeared is the stretching vibration absorption peak of carbonyl in amido bond; 1559cm -1 The peak is an N-H bending vibration peak; 1471cm -1 C-N stretching vibration peak; 1373cm -1 Is the C-H bending vibration peak; 1299 cm -1 Characteristic absorption of secondary amide, which indicates successful synthesis of polyacrylic acid-tetraethylenepentamine; from the spectrogram of the polymer heavy metal chelating agent, except N-H and methylene (2940 cm) -1 ，1398 cm -1 ) And carbonyl (1635 cm) -1 ) In addition to the signal of (c), some new absorptions also appear; 1464 cm -1 The absorption of the compound is N-C = S middle N-C characteristic absorption peak and is positioned at C-N single bond (-1300 cm) -1 ) And C N double bond (. About.1600 cm) -1 ) In the nature of a double bond; at 1155 cm -1 、974 cm -1 The peaks appeared as C = S and C — S characteristic stretching vibration absorption peaks, respectively.
Detailed Description
The invention is further illustrated below with reference to preferred embodiments and comparative examples in the examples. These examples are only some of the examples of the present invention, and not all of them. All other embodiments obtained by the skilled person without inventive work are within the scope of protection. The units of parts may be grams or kilograms or tons, or other units of weight.
The invention provides a technical scheme that: a neutral metal cleaning agent for a MASK MASK plate comprises the following components in percentage by weight: 5-30% of oxidant, 10-20% of inorganic salt, 5-15% of polymer heavy metal chelating agent, 1-10% of pH regulator, 5-15% of surfactant and 55-75% of deionized water.
The preparation method of the used polymer heavy metal chelating agent comprises the following steps:
1) Adding 18.930 g of tetraethylenepentamine into a 200mL three-neck flask, adding 2-3 drops of concentrated sulfuric acid as a catalyst, using nitrogen for protection, heating to 130 ℃, and gradually dropping acrylic acid. The dropping speed is controlled well, the temperature in the bottle is kept at 130 to 140 ℃ in the dropping process, and the dropping can be finished in about 1 hour. And (3) installing a water separator, heating to 180 ℃ and keeping for 6 hours until the water amount in the water separator is not increased any more, stopping reaction, standing and cooling to room temperature. Finally, a yellow viscous liquid is obtained, and the intermediate is polyacrylic acid-tetraethylenepentamine.
2) Adding 2-3 g of polyacrylic acid-tetraethylenepentamine into a 200mL three-neck flask, dissolving the mixture by 100mL of absolute ethanol, and then respectively adding CS 2 Addition of CS at a molar ratio of x to mer (x =2,3,4) 2 And NaOH. Firstly adding NaOH, stirring and dissolving, then adding CS into a constant-pressure dropping funnel 2 And anhydrous ethanol is slowly dripped into the flask, the dripping is finished, the reaction is carried out for 8 hours at 25 ℃, after the reaction is finished, the solvent is removed, the reaction product is dried in vacuum for 5 hours at 60 ℃, and finally the polymer heavy metal chelating agent with different sulfur contents is obtained.
Examples
The neutral metal cleaning agent for the MASK MASK plate is prepared according to the formula shown in the table 1, and the specific preparation method comprises the steps of firstly adding deionized water into a stirring kettle with the rotating speed of 1200r/min at normal temperature, then sequentially adding an oxidant, inorganic salt, a polymer heavy metal chelating agent, a pH regulator and a surfactant, and adding the next material after each material is added and completely dissolved. And after all the components are added, continuously stirring for 30min, and filtering through a filter element with the diameter of 1um for 3 channels to obtain the target product.
Cleaning test on neutral metal cleaner for MASK plate:
1. cleaning test of metal magnesium, silver and ytterbium
The test method comprises the following steps: the magnesium silver film invar alloy and the ytterbium film invar alloy which are evaporated are cut into the same size, and the metal particle proportion of the magnesium silver film is 1: silver, the membrane thickness is controlled at about 5 um. Heating the equivalent solutions of the examples 1-3 and the comparative examples 1-3 to 40 ℃, respectively adding the magnesium-silver film invar alloy and the ytterbium film invar alloy, starting ultrasound with the ultrasonic frequency of 40KHZ and the ultrasonic time of 15min, rinsing with deionized water, and drying in an oven at 80 ℃ for 20min. And finally, taking out the invar alloy to observe whether the film layer residue exists on the surface of the invar alloy and the solution condition after ultrasonic treatment.
2. Corrosivity test
The test method comprises the following steps: and respectively putting the MASK MASK plate which is not subjected to evaporation into the equivalent solution of the above examples 1-3 and comparative examples 1-3, soaking for 72h, taking out, rinsing with deionized water, and putting into an oven to dry at 80 ℃ for 20min. And finally, taking out the MASK MASK plate, and comparing and observing the surface expanded mesh structure of the MASK MASK plate by using a metallographic microscope to see whether the phenomena of heterochrosis, fracture, deformation and the like occur.
According to experimental results, in the embodiments 1 to 3, the cleaning requirements on magnesium, silver and ytterbium can be met within a proper proportion range, and the MASK MASK plate is not corroded. The introduction of the polymer heavy metal chelating agent can improve the cleaning performance of the cathode metal material, promote the dissolution reaction rate through stronger complexing capacity, and meanwhile, the cleaning agent has good component compatibility, small smell, no precipitation, no corrosiveness and no damage to a MASK MASK plate.
From comparative examples 1 to 3, it can be further found that the cleaning effect of ytterbium is reduced because sodium citrate is not added in comparative example 1, which shows that sodium citrate has a certain synergistic effect in the aspect of cleaning ytterbium. Secondly, the polymer heavy metal chelating agent is not added in the comparative example 2, the pH regulator is replaced by ammonium acetate, large-area film residues are found, the solution is turbid, black precipitates are formed at the bottom of the solution, and the MASK MASK plate is locally corroded after being soaked, so that the polymer heavy metal chelating agent plays a key role in ytterbium dissolution and chelation performance. Comparative example 3 increased the proportion of ammonium acetate, which was found to cause significant corrosion of the MASK.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made therein without departing from the spirit and scope of the invention.
Claims (8)
1. A neutral metal cleaning agent for a MASK MASK plate is characterized by comprising the following components in percentage by mass:
5-30% of an oxidant;
10-20% of inorganic salt;
5-15% of polymer heavy metal chelating agent;
1-10% of pH regulator;
5-15% of a surfactant;
55-75% of deionized water;
the sum of the weight percentages of the components is 100 percent.
2. The neutral metal cleaner for MASK MASKs according to claim 1, wherein the oxidizing agent is at least one of hydrogen peroxide, hydrochloric acid, sulfuric acid, acetic acid, peracetic acid, sodium dichromate.
3. The neutral metal cleaner for MASK MASKs according to claim 1, wherein the inorganic salt is at least one of sodium sulfate, ammonium phosphate, potassium sulfate, sodium borate, ammonium nitrate, sodium nitrate, and potassium nitrate.
4. The neutral metal cleaner for MASK MASKs according to claim 1, wherein the polymeric heavy metal chelating agent has the following structural formula:
wherein n =10-13, x is CS 2 Molar ratio to mer, x =2,3 or 4.
5. The neutral metal cleaner for MASK MASKs according to claim 4, wherein the preparation method of the polymer heavy metal chelating agent comprises the following steps:
1) The method comprises the following steps of (1) taking tetraethylenepentamine as a raw material, adding concentrated sulfuric acid as a catalyst, protecting with nitrogen, heating to 130 ℃, and dropwise adding acrylic acid; keeping the temperature at 130-140 ℃ in the dropping process, then heating the temperature to 180 ℃ for 6h, stopping the reaction, standing and cooling to room temperature to obtain yellow viscous liquid, wherein the intermediate is polyacrylic acid-tetraethylenepentamine;
2) Dissolving polyacrylic acid-tetraethylenepentamine by absolute ethyl alcohol, and respectively adding the solution according to CS 2 Adding CS at a molar ratio of x to chain units 2 Reacting with NaOH; firstly adding NaOH, stirring and dissolving, then adding CS 2 And reacting with absolute ethyl alcohol at 25 ℃ for 8 hours, removing the solvent after the reaction is finished, and drying in vacuum to finally obtain the polymer heavy metal chelating agent with different sulfur contents.
6. The neutral metal cleaner for MASK MASKs according to claim 1, wherein the pH adjuster is one of triethanolamine, acetic acid, ammonium acetate, ammonium formate, potassium carbonate, and sodium carbonate.
7. The neutral metal cleaner for MASK MASKs according to claim 1, wherein the surfactant is one of octadecyl ammonium sulfate, dodecyl ammonium chloroacetate, didecyl dimethyl ammonium bromide, tetradecyl-dimethyl ammonium pyridinium bromide, triethanolamine distearate methyl ammonium methyl sulfate.
8. The neutral metal cleaner for MASK MASKs according to claim 1, wherein the deionized water has a resistivity of not less than 15M Ω at 25 ℃.
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Cited By (1)
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