CN115710707A - Magnesium-silver alloy and ytterbium metal cleaning agent and cleaning method - Google Patents
Magnesium-silver alloy and ytterbium metal cleaning agent and cleaning method Download PDFInfo
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- CN115710707A CN115710707A CN202211431747.3A CN202211431747A CN115710707A CN 115710707 A CN115710707 A CN 115710707A CN 202211431747 A CN202211431747 A CN 202211431747A CN 115710707 A CN115710707 A CN 115710707A
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- silver alloy
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- ytterbium
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 71
- 239000002184 metal Substances 0.000 title claims abstract description 71
- 239000012459 cleaning agent Substances 0.000 title claims abstract description 49
- 229910001316 Ag alloy Inorganic materials 0.000 title claims abstract description 44
- SJCKRGFTWFGHGZ-UHFFFAOYSA-N magnesium silver Chemical compound [Mg].[Ag] SJCKRGFTWFGHGZ-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910052769 Ytterbium Inorganic materials 0.000 title claims abstract description 40
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000004140 cleaning Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000007797 corrosion Effects 0.000 claims abstract description 27
- 238000005260 corrosion Methods 0.000 claims abstract description 27
- 230000001590 oxidative effect Effects 0.000 claims abstract description 17
- 239000003112 inhibitor Substances 0.000 claims abstract description 16
- 239000007800 oxidant agent Substances 0.000 claims abstract description 16
- 239000002738 chelating agent Substances 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 229910001374 Invar Inorganic materials 0.000 claims description 13
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 13
- 229920000570 polyether Polymers 0.000 claims description 13
- 239000004094 surface-active agent Substances 0.000 claims description 13
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 8
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 8
- 125000002636 imidazolinyl group Chemical group 0.000 claims description 7
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 6
- 235000011054 acetic acid Nutrition 0.000 claims description 5
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 4
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 4
- 235000015165 citric acid Nutrition 0.000 claims description 4
- 235000019253 formic acid Nutrition 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- 239000011975 tartaric acid Substances 0.000 claims description 4
- 235000002906 tartaric acid Nutrition 0.000 claims description 4
- CEGPKOIWQYWDNX-UHFFFAOYSA-N 2-[bis(carboxymethyl)amino]acetic acid;sodium Chemical compound [Na].[Na].OC(=O)CN(CC(O)=O)CC(O)=O CEGPKOIWQYWDNX-UHFFFAOYSA-N 0.000 claims description 3
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 3
- 239000005695 Ammonium acetate Substances 0.000 claims description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 3
- 239000004280 Sodium formate Substances 0.000 claims description 3
- 235000019257 ammonium acetate Nutrition 0.000 claims description 3
- 229940043376 ammonium acetate Drugs 0.000 claims description 3
- VZTDIZULWFCMLS-UHFFFAOYSA-N ammonium formate Chemical compound [NH4+].[O-]C=O VZTDIZULWFCMLS-UHFFFAOYSA-N 0.000 claims description 3
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 3
- 239000008103 glucose Substances 0.000 claims description 3
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 claims description 3
- 239000001632 sodium acetate Substances 0.000 claims description 3
- 235000017281 sodium acetate Nutrition 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims 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 claims description 3
- 235000011083 sodium citrates Nutrition 0.000 claims description 3
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 claims description 3
- 235000019254 sodium formate Nutrition 0.000 claims description 3
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 claims description 3
- 229940039790 sodium oxalate Drugs 0.000 claims description 3
- 239000001433 sodium tartrate Substances 0.000 claims description 3
- 229960002167 sodium tartrate Drugs 0.000 claims description 3
- 235000011004 sodium tartrates Nutrition 0.000 claims description 3
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 3
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 239000003002 pH adjusting agent Substances 0.000 claims 2
- 229910000604 Ferrochrome Inorganic materials 0.000 claims 1
- 239000002244 precipitate Substances 0.000 abstract description 11
- 150000002739 metals Chemical class 0.000 abstract description 3
- 238000001704 evaporation Methods 0.000 description 14
- 230000008020 evaporation Effects 0.000 description 14
- 229910045601 alloy Inorganic materials 0.000 description 11
- 239000000956 alloy Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- MTNDZQHUAFNZQY-UHFFFAOYSA-N imidazoline Chemical compound C1CN=CN1 MTNDZQHUAFNZQY-UHFFFAOYSA-N 0.000 description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 8
- 229910052709 silver Inorganic materials 0.000 description 8
- 239000004332 silver Substances 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 230000005764 inhibitory process Effects 0.000 description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 4
- 229920001621 AMOLED Polymers 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- -1 carboxylic acid ammonium salt Chemical class 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 229960001484 edetic acid Drugs 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000003755 preservative agent Substances 0.000 description 2
- 230000002335 preservative effect Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 229910001923 silver oxide Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical group N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 1
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 1
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 1
- 239000004375 Dextrin Substances 0.000 description 1
- 229920001353 Dextrin Polymers 0.000 description 1
- 229910001021 Ferroalloy Inorganic materials 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229960001701 chloroform Drugs 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 235000019425 dextrin Nutrition 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- TUEYHEWXYWCDHA-UHFFFAOYSA-N ethyl 5-methylthiadiazole-4-carboxylate Chemical compound CCOC(=O)C=1N=NSC=1C TUEYHEWXYWCDHA-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000008040 ionic compounds Chemical class 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000006174 pH buffer Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 description 1
- 229940071536 silver acetate Drugs 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Landscapes
- Detergent Compositions (AREA)
Abstract
The invention discloses a magnesium-silver alloy and ytterbium metal cleaning agent and a cleaning method, and develops a metal cleaning agent which can efficiently dissolve metals such as Mask and residual magnesium-silver alloy and ytterbium on a crucible at a lower cost, does not cause loss on substrates such as Mask and the like, and reduces the generation of precipitates. The cleaning agent consists of 2-10% of oxidant, 3-12% of oxide dissolving agent, 3-15% of pH regulator, 0.1-1% of corrosion inhibitor, 0.1-1% of metal chelating agent and the balance of water. The magnesium-silver alloy and ytterbium metal cleaning agent provided by the invention can efficiently dissolve metals such as Mask and residual magnesium-silver alloy and ytterbium on a crucible at a lower cost, does not cause loss on substrates such as Mask and the like, and reduces the generation of precipitates.
Description
Technical Field
The invention belongs to the technical field of cleaning agents, and particularly relates to a magnesium-silver alloy and ytterbium metal cleaning agent for cathode materials deposited on a crucible, a metal mask and an evaporation cavity baffle in an Organic Light Emitting Diode (OLED) evaporation process, and a method for cleaning the crucible, the metal mask and the evaporation cavity baffle by using the metal cleaning agent.
Background
Currently, an active matrix organic light emitting diode (oled) or an Active Matrix Organic Light Emitting Diode (AMOLED) screen is manufactured by an evaporation process, and a cathode of the oled is made of a magnesium-silver alloy and a small amount of ytterbium. Magnesium-silver alloy and ytterbium with certain thicknesses can remain on the crucible, the metal mask plate and the evaporation cavity baffle after evaporation is finished, and the magnesium-silver alloy and ytterbium can be reused after being removed.
At present, a large number of methods are adopted, namely, residual metal is physically stripped manually by using a roller, cannot be completely removed, and can remain at the evaporation coating corner of an opening of a metal mask plate, a baffle gap and other positions to form a burr phenomenon; in addition, the Mask is easy to deform in the roller removing process, and the yield is greatly influenced.
With the rapid increase of the global demand on OLED screens and the growth of the domestic OLED industry, the magnesium-silver cleaning agent has a great growth space.
CN113881944A discloses a magnesium-silver alloy cleaning agent and a cleaning method, which aim to rapidly dissolve magnesium-silver alloy without damaging a metal mask. The cleaning agent mainly comprises hydrogen peroxide and carboxylic acid ammonium salt. The magnesium-silver alloy cleaning agent provided by the invention has low cost, can efficiently and thoroughly dissolve and clean the magnesium-silver alloy without damaging a metal substrate. However, the cleaning agent is a neutral cleaning agent, has poor dissolving capacity for metal ytterbium, causes the metal ytterbium to remain on substrates such as a metal mask and the like, and generates precipitates to pollute devices when excessive magnesium is dissolved.
CN109881204A discloses a magnesium-silver alloy cleaning agent and a cleaning method, aiming at providing a cleaning agent which has low cost, can efficiently and thoroughly dissolve and clean magnesium-silver alloy without damaging a metal substrate. The magnesium-silver alloy cleaning agent comprises 3-10wt% of main oxidant, 5-15wt% of auxiliary oxidant, 1-10wt% of pH buffer agent, 0.3-1.0wt% of preservative and the balance of water; the primary oxidant is selected from one or more of nitric acid, hydrogen peroxide and perchloric acid; the auxiliary oxidant is selected from one or more of phosphoric acid and sulfuric acid; the preservative is selected from one or more of sucrose, sorbitol, dextrin and bipyridyl. The magnesium-silver alloy cleaning agent provided by the invention has low cost, can efficiently and thoroughly dissolve and clean the magnesium-silver alloy without damaging a metal substrate. However, the formula of the cleaning agent provided by the invention uses strong acid, which inevitably damages the Mask made of ferroalloy.
With the rapid increase of the global demand on OLED screens and the growth of the domestic OLED industry, the magnesium-silver alloy and ytterbium metal cleaning agent has a great growth space. Therefore, there is a need in the art to develop a method for removing mg-ag alloy from the surface of a metal Mask simply, rapidly and effectively, while removing yb metal, without causing deformation and damage to the Mask, thereby improving the yield of the product.
Disclosure of Invention
In view of the defects of the prior art, an object of the present invention is to provide a cleaning agent and a cleaning method capable of removing mg-ag alloy and yb metal deposited in an evaporation process. The method can quickly and effectively remove the metal magnesium silver alloy and the metal ytterbium, and cannot deform the metal mask plate.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the magnesium-silver alloy and ytterbium metal cleaning agent comprises the following raw materials in percentage by mass: 2-10% of oxidant, 3-12% of oxide dissolving agent, 3-15% of pH regulator, 0.1-1% of corrosion inhibitor, 0.1-1% of metal chelating agent and the balance of water; the oxidant is hydrogen peroxide, and the concentration of the oxidant is 2-10wt%; the oxide dissolving agent is one or more of acetic acid, citric acid, formic acid, oxalic acid, malonic acid and tartaric acid;
the pH regulator is one or more of sodium acetate, ammonium acetate, sodium citrate, ammonium citrate, sodium formate, ammonium formate, sodium oxalate, ammonium oxalate and sodium tartrate; the metal chelating agent is one or more selected from ethylene diamine tetraacetic acid, disodium ethylene diamine tetraacetic acid, nitrilotriacetic acid, disodium nitrilotriacetic acid, sodium tripolyphosphate and glucose.
The corrosion inhibitor is an imidazoline-based polyether surfactant MZ-EO-n, and the structural formula is as follows:
The pH range of the magnesium-silver alloy and ytterbium metal cleaning agent is 4-6.
Meanwhile, the invention also provides a cleaning method which comprises the step of cleaning the evaporation device attached with the magnesium-silver alloy and ytterbium by adopting the metal cleaning agent.
The cleaning agent containing hydrogen peroxide and organic weak acid can oxidize silver into silver oxide and then react with acid to generate soluble ionic compounds, and meanwhile, magnesium and ytterbium can react to generate divalent magnesium ions and trivalent ytterbium ions under the condition of weak acid to be dissolved in solution. The cleaning agent has weak acidity, and the existence of the corrosion inhibitor can not cause corrosion to the evaporation device. The addition of the metal chelating agent forms a soluble complex with metal ions, reduces the generation of precipitates and avoids secondary pollution to devices such as a metal mask plate and the like. Meanwhile, the chemical cleaning method can not deform the metal mask plate, and the chemical is safe and can not damage the surface of the evaporation device.
The invention has the remarkable advantages that:
the oxidant is hydrogen peroxide; the oxide dissolving agent is one or more of acetic acid, citric acid, formic acid, oxalic acid, malonic acid and tartaric acid. In the invention, the magnesium-silver alloy and the ytterbium metal are oxidized into the metal oxide by using the oxidant, and the metal oxide is dissolved by using the oxide dissolving agent, so that the residual metal on the Mask or the crucible is cleaned.
According to the invention, the adopted oxide dissolving agent is organic weak acid, and the pH regulator is added, so that the risk of corrosion of the acid cleaning agent to the Mask is reduced. In order to reduce the generation of precipitate, a metal ion chelating agent is added, and the chelating agent forms a soluble complex with metal ions to reduce the generation of precipitate. The cleaning is carried out under the heating condition, and the generation of the precipitate can also be avoided.
The corrosion inhibitor adopts an imidazoline-based polyether surfactant MZ-EO-n, and the surfactant mainly comprises imidazoline groups and polyether chains. The imidazoline group and the polyether chain both have acid resistance and can be used under an acidic condition, and the imidazoline group can be adsorbed on the surface of steel to form a compact protective film, so that the corrosion inhibitor has excellent corrosion inhibition on metals such as steel. The use of imidazoline polyether surfactant can reduce the surface tension of the solution, make the cleaning agent spread on Mask more easily, improve the cleaning effect, and the existence of imidazoline group further protects the Mask and other steel substrates.
Detailed Description
The following description will clearly and completely describe the embodiments of the present invention in conjunction with the accompanying drawings. It is to be understood that the disclosed embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention.
The magnesium-silver alloy and ytterbium metal cleaning agent provided by the invention comprises the following raw materials in percentage by mass: 2-10% of oxidant, 3-12% of oxide dissolving agent, 3-15% of pH regulator, 0.1-1% of corrosion inhibitor, 0.1-1% of metal chelating agent and the balance of water; the pH range of the magnesium-silver alloy and ytterbium metal cleaning agent is 4-6.
The oxidant is hydrogen peroxide, and the concentration of the oxidant is 2-10wt%; the oxide dissolving agent is one or more of acetic acid, citric acid, formic acid, oxalic acid, malonic acid and tartaric acid;
the pH regulator is one or more of sodium acetate, ammonium acetate, sodium citrate, ammonium citrate, sodium formate, ammonium formate, sodium oxalate, ammonium oxalate and sodium tartrate;
the metal chelating agent is selected from one or more of ethylenediamine tetraacetic acid, disodium ethylenediamine tetraacetic acid, nitrilotriacetic acid, disodium nitrilotriacetic acid, sodium tripolyphosphate and glucose;
the corrosion inhibitor is an imidazoline-based polyether surfactant MZ-EO-n, and the structural formula is as follows:
wherein n is an integer from 2 to 20.
The synthetic route of the imidazoline-based polyether surfactant is as follows:
the preparation method of the magnesium-silver alloy and ytterbium metal cleaning agent comprises the following steps: adding an oxide dissolving agent, a pH regulator, a metal chelating agent and a corrosion inhibitor into ultrapure water, completely dissolving the ultrapure water under mechanical stirring, then adding hydrogen peroxide, and continuously stirring until the solution is a clear homogeneous system.
The invention also discloses a cleaning method, which comprises the step of cleaning the metal substrate attached with the magnesium-silver alloy and ytterbium by adopting the metal cleaning agent. The cleaning is carried out under the heating condition, and the generation of the precipitate can be avoided.
The cleaning temperature is 35-50 ℃, the cleaning mode is 40kHz ultrasonic cleaning, and the cleaning time is below 15min. The cleaning is carried out under the heating condition, and the generation of the precipitate can be avoided.
The evaporation device comprises a metal mask plate, a crucible and an evaporation cavity baffle, wherein the metal mask plate is generally made of invar alloy, the crucible is generally made of pyrolytic boron nitride or tantalum metal, and the evaporation cavity baffle is generally made of stainless steel.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The present invention will be further illustrated by the following examples.
The corrosion inhibitor imidazoline-based polyether surfactant MZ-EO-n has the structural formula:
wherein n is an integer of 2-20, and the preparation steps are as follows when n =4 is taken as an example:
step one, dissolving 15g of tetraethylene glycol monomethyl ether (0.072 mol) in 100mL of dichloromethane, adding 11.144g of thionyl chloride (0.094 mol), carrying out reflux reaction at 90 ℃ for 48h, adding water to quench the reaction, washing the reaction product for 3 times by using 50mL of deionized water, adding anhydrous magnesium sulfate into an organic layer to remove excessive water, and carrying out rotary evaporation to evaporate the solvent to obtain the 1-chloro-2- [2- (2-methoxyethoxy) ethoxy ] ethoxy } ethane.
And step two, dissolving 5g of 2-imidazoline (0.043 mol) in 100ml of trichloromethane, adding 10.65g of 1-chloro-2 c 2- [2- (2-methoxyethoxy) ethoxy ] ethoxy } ethane (0.047 mol), adding 2.64g of potassium hydroxide (0.047 mol) and 7.82g of potassium iodide (0.047 mol), carrying out reflux reaction at the temperature of 80 ℃ for 48h, and purifying by column chromatography to obtain the target product imidazoline-based polyether surfactant MZ-EO-4.
The structural data are characterized as follows:
IR(KBr)，σ/cm -1 :2924.82，2854.64，1655.13，1362.17，1102.64；
HRMS calculated value C 12 H 24 N 2 O 4 :260.173, found 260.1731.
Six examples are given below, with the respective components and amounts as given in table 1 below.
The examples and comparative examples are provided to illustrate the magnesium-silver alloy and ytterbium metal cleaning agents and methods disclosed herein.
Respectively taking a silver sheet with the mass of about 0.5 g, a magnesium sheet with the mass of about 0.15 g and an ytterbium block with the mass of about 0.5 g as samples (masks or residual metal film layers on crucibles are generally thin), ultrasonically cleaning for 10min at 40kHz under the condition of 40-45 ℃, weighing the mass before and after the samples, and judging the cleaning effect according to the mass difference. The test evaluation results are shown in table 1.
TABLE 1
By comparing the test results of the examples 1 to 5 and the comparative examples 1 to 6, the magnesium-silver alloy and ytterbium metal cleaning agent provided by the invention can efficiently and thoroughly dissolve the magnesium-silver alloy and ytterbium metal, no precipitate is generated, and the cleaning time is short.
It can be seen from the test results of example 1 and comparative example 1 that silver is not dissolved by a simple acidic solution because the silver is inactive, and can be dissolved only by oxidizing silver into silver oxide by adding hydrogen peroxide.
It can be seen from the test results of example 1, comparative example 4 and comparative example 5 that the addition of the metal corrosion inhibitor and the metal chelating agent does not inhibit the cleaning effect, and simultaneously reduces the corrosion of invar and the generation of silver acetate precipitate. MZ-EO-4 with surfactant property is added as a corrosion inhibitor, so that the wettability and the permeability of the cleaning agent are improved, and the dissolution rate of the cleaning agent on silver and ytterbium can be improved.
It can be seen from the test results of example 1 and comparative example 3 that when the pH is low, the hydrogen ions inhibit the oxidation of hydrogen peroxide, reducing the solubility of metallic silver.
From the test results of example 1 and comparative example 6, it can be seen that the dissolution rates of magnesium, silver and ytterbium are all reduced when the concentration of acetic acid is reduced.
In order to further observe the corrosion condition of the magnesium-silver alloy and ytterbium metal cleaning agent on the invar alloy and verify the corrosion inhibition effect of the imidazoline-based polyether surfactant MZ-EO-n in the cleaning agent, the following verification is carried out.
Shearing invar alloy sheets with proper size, recording the initial mass of the invar alloy sheets, soaking the invar alloy sheets in the magnesium-silver alloy and ytterbium metal cleaning agent for 7 days at 45 ℃, washing the invar alloy sheets clean, drying the invar alloy sheets, and weighing the invar alloy sheets. The corrosion inhibition effect was judged as a reduced mass. The test evaluation results are shown in table 2.
TABLE 2
As can be seen by comparing the test results of the above examples 1-5 and comparative examples 1-6, the magnesium-silver alloy and ytterbium metal cleaning agent provided by the invention has low corrosivity to invar alloy, and the imidazoline-based polyether surfactant MZ-EO-n has excellent corrosion inhibition effect in the cleaning agent.
It can be seen from the test results of example 1 and comparative example 3 that, when the pH is lower, the corrosion of the cleaning agent to invar alloy is still more severe than that of the sample having a pH greater than 4 even in the presence of the corrosion inhibitor, and therefore, it is important that the cleaning agent is selected in an appropriate pH range.
The test results of the example 1 and the comparative example 5 show that the imidazoline based polyether surfactant MZ-EO-n has good corrosion inhibition effect in the cleaning agent disclosed by the invention, and reduces the corrosion of the cleaning agent to the invar alloy.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (7)
1. The magnesium-silver alloy and ytterbium metal cleaning agent is characterized by comprising the following raw materials in percentage by mass: 2-10% of oxidant, 3-12% of oxide dissolving agent, 3-15% of pH regulator, 0.1-1% of corrosion inhibitor, 0.1-1% of metal chelating agent and the balance of water;
wherein the oxidant is hydrogen peroxide, and the concentration of the oxidant is 2-10wt%;
the oxide dissolving agent is one or more of acetic acid, citric acid, formic acid, oxalic acid, malonic acid and tartaric acid;
the corrosion inhibitor is an imidazoline-based polyether surfactant MZ-EO-n, and the structural formula is as follows:
the metal chelating agent is selected from one or more of ethylenediamine tetraacetic acid, disodium ethylenediamine tetraacetic acid, nitrilotriacetic acid, disodium nitrilotriacetic acid, sodium tripolyphosphate and glucose.
2. The magnesium-silver alloy and ytterbium metal cleaning agent of claim 1, wherein the hydrogen peroxide content is 3-8%, the oxide dissolving agent content is 4-9%, the pH adjusting agent content is 5-10%, the corrosion inhibitor content is 0.2-0.8%, and the metal chelating agent content is 0.2-0.8% by mass.
3. The magnesium-silver alloy and ytterbium metal cleaner of claim 1, wherein the pH adjuster is one or more of sodium acetate, ammonium acetate, sodium citrate, ammonium citrate, sodium formate, ammonium formate, sodium oxalate, ammonium oxalate, sodium tartrate.
4. The magnesium silver alloy ytterbium metal cleaner of claim 1 wherein the pH of the magnesium silver alloy ytterbium metal cleaner is in the range of 4 to 6.
5. The method of claim 1, wherein the magnesium-silver alloy and ytterbium metal cleaning agent is used to clean a metal substrate to which the magnesium-silver alloy and ytterbium metal are attached.
6. The cleaning method according to claim 5, wherein the cleaning temperature is 35-50 ℃, the cleaning mode is 40kHz ultrasonic cleaning, and the cleaning time is 15min.
7. The cleaning method of claim 5, wherein the metal substrate is made of invar or ferrochrome.
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