CN116515490B - Silicon oxide thinning liquid for integrated circuit and preparation method thereof - Google Patents
Silicon oxide thinning liquid for integrated circuit and preparation method thereof Download PDFInfo
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- CN116515490B CN116515490B CN202310173381.2A CN202310173381A CN116515490B CN 116515490 B CN116515490 B CN 116515490B CN 202310173381 A CN202310173381 A CN 202310173381A CN 116515490 B CN116515490 B CN 116515490B
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- 239000007788 liquid Substances 0.000 title claims abstract description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910052814 silicon oxide Inorganic materials 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 73
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 73
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000003381 stabilizer Substances 0.000 claims abstract description 35
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims abstract description 32
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000004094 surface-active agent Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 14
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 8
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 claims description 7
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000003999 initiator Substances 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 4
- MXXDSLLVYZMTFA-UHFFFAOYSA-N octadecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 MXXDSLLVYZMTFA-UHFFFAOYSA-N 0.000 claims description 4
- 125000001453 quaternary ammonium group Chemical group 0.000 claims description 4
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000003208 petroleum Substances 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- HEBRGEBJCIKEKX-UHFFFAOYSA-M sodium;2-hexadecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HEBRGEBJCIKEKX-UHFFFAOYSA-M 0.000 claims description 3
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 2
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 2
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- -1 sodium tetradecyl sulfide Chemical compound 0.000 claims description 2
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 2
- PNGBYKXZVCIZRN-UHFFFAOYSA-M sodium;hexadecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCS([O-])(=O)=O PNGBYKXZVCIZRN-UHFFFAOYSA-M 0.000 claims description 2
- GGHPAKFFUZUEKL-UHFFFAOYSA-M sodium;hexadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCOS([O-])(=O)=O GGHPAKFFUZUEKL-UHFFFAOYSA-M 0.000 claims description 2
- KBAFDSIZQYCDPK-UHFFFAOYSA-M sodium;octadecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCS([O-])(=O)=O KBAFDSIZQYCDPK-UHFFFAOYSA-M 0.000 claims description 2
- NWZBFJYXRGSRGD-UHFFFAOYSA-M sodium;octadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCOS([O-])(=O)=O NWZBFJYXRGSRGD-UHFFFAOYSA-M 0.000 claims description 2
- AYFACLKQYVTXNS-UHFFFAOYSA-M sodium;tetradecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCCCS([O-])(=O)=O AYFACLKQYVTXNS-UHFFFAOYSA-M 0.000 claims description 2
- ORLPWCUCEDVJNN-UHFFFAOYSA-N sodium;tetradecyl benzenesulfonate Chemical compound [Na].CCCCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 ORLPWCUCEDVJNN-UHFFFAOYSA-N 0.000 claims description 2
- 239000002699 waste material Substances 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 description 12
- 238000001914 filtration Methods 0.000 description 11
- 238000001556 precipitation Methods 0.000 description 11
- 238000005406 washing Methods 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 10
- 238000005530 etching Methods 0.000 description 8
- 239000011521 glass Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 7
- 239000000758 substrate Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000003513 alkali Substances 0.000 description 4
- 229940083575 sodium dodecyl sulfate Drugs 0.000 description 4
- 238000003486 chemical etching Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 231100000419 toxicity Toxicity 0.000 description 3
- 230000001988 toxicity Effects 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 description 1
- VEFXTGTZJOWDOF-UHFFFAOYSA-N benzene;hydrate Chemical compound O.C1=CC=CC=C1 VEFXTGTZJOWDOF-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K13/00—Etching, surface-brightening or pickling compositions
- C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
- C09K13/08—Etching, surface-brightening or pickling compositions containing an inorganic acid containing a fluorine compound
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Cleaning Or Drying Semiconductors (AREA)
- Silicon Compounds (AREA)
Abstract
本发明提出了一种集成电路用氧化硅减薄液及其制备方法，属于集成电路技术领域。由以下原料按重量份制备而成：聚乙烯醇季铵盐稳定剂5‑10份、氢氟酸10‑20份、硫酸5‑10份、硝酸5‑10份、表面活性剂3‑5份和水50‑90份。本发明集成电路用氧化硅减薄液的利用率的提高，废液产生量显著减少，处理简单，且制备方法简单，安全环保，工作效率高，具有广阔的应用前景。The present invention proposes a silicon oxide thinning liquid for integrated circuits and a preparation method thereof, belonging to the technical field of integrated circuits. The silicon oxide thinning liquid is prepared from the following raw materials by weight: 5-10 parts of polyvinyl alcohol quaternary ammonium salt stabilizer, 10-20 parts of hydrofluoric acid, 5-10 parts of sulfuric acid, 5-10 parts of nitric acid, 3-5 parts of surfactant and 50-90 parts of water. The utilization rate of the silicon oxide thinning liquid for integrated circuits of the present invention is improved, the amount of waste liquid generated is significantly reduced, the treatment is simple, and the preparation method is simple, safe and environmentally friendly, and the work efficiency is high, and it has broad application prospects.
Description
Technical Field
The invention relates to the technical field of integrated circuits, in particular to a silicon oxide thinning liquid for an integrated circuit and a preparation method thereof.
Background
With the development of electronic technology and display technology, thinning of a glass substrate has become a premise and a motive force for thinning of a terminal display product as a core of thinning of a display product. At present, the thinning technology of the glass substrate of the display product is mainly divided into two types of physical grinding polishing thinning and chemical etching thinning, and the chemical etching thinning is gradually becoming the main stream technology of thinning the glass substrate with the technical advantages of high speed, high efficiency, low investment and the like. Taking the production of a TFT-LCD (thin film transistor liquid crystal display) as an example, the main flow thickness of the original glass substrate is 0.5mm, and the thinnest thickness which can be achieved by the production process of the TFT-LCD array substrate is not in line with the requirement of thinning the terminal display product, which also shows the value of the glass substrate thinning technology. The advantages of chemical etch thinning over physical polish thinning are apparent for process technologies that thin 0.5mm (1.0 mm on both sides after the cassette) thick glass substrates to 0.25mm (0.5 mm on both sides after the cassette) and even thinner. The existing chemical etching thinning technology adopts single hydrofluoric acid as etching liquid to carry out thinning, but the etching liquid has the following defects:
1. High toxicity and easy volatilization. In the production process, particularly in the preparation process, higher temperature conditions and hydrofluoric acid concentration are needed, so that a large amount of hydrofluoric acid gas is easily volatilized, and the toxicity and the danger are high.
2. The etching rate of the etching solution in the production process is unstable and the utilization rate is low.
3. The utilization rate of the etching solution is low, so that the waste liquid treatment capacity is large, the treatment is difficult, and the waste liquid treatment cost matched with the etching solution is high.
4. The product is difficult to remove. Hydrofluoric acid reacts with glass to generate a large amount of white indissolvable matters, which are difficult to remove from the surface of the glass, and can be further adhered to equipment, pipelines and the like, so that the problems of poor surface effect, pipeline blockage, equipment shutdown and the like of products are caused, and even safety accidents are caused.
Disclosure of Invention
The invention aims to provide a silicon oxide thinning liquid for an integrated circuit and a preparation method thereof, which have the advantages of remarkably reduced waste liquid production, simple treatment, simple preparation method, safety, environmental protection, high working efficiency and wide application prospect, and the utilization rate of the silicon oxide thinning liquid is improved. .
The technical scheme of the invention is realized as follows:
the invention provides a silicon oxide thinning liquid for an integrated circuit, which comprises the following raw materials of a polyvinyl alcohol quaternary ammonium salt stabilizer, hydrofluoric acid, sulfuric acid, nitric acid, a surfactant and water.
The invention is further improved by the following raw materials, by weight, 5-10 parts of polyvinyl alcohol quaternary ammonium salt stabilizer, 10-20 parts of hydrofluoric acid, 5-10 parts of sulfuric acid, 5-10 parts of nitric acid, 3-5 parts of surfactant and 50-90 parts of water.
As a further improvement of the invention, the sulfuric acid is concentrated sulfuric acid with a concentration of more than 98%.
As a further improvement of the present invention, the surfactant is at least one selected from the group consisting of sodium dodecylbenzenesulfonate, sodium dodecylsulfonate, sodium dodecylsulfate, sodium tetradecyl sulfide, sodium tetradecyl sulfonate, sodium tetradecyl benzenesulfonate, sodium hexadecyl sulfonate, sodium hexadecyl sulfate, sodium octadecyl sulfonate, sodium octadecyl benzenesulfonate, and sodium octadecyl sulfate.
As a further improvement of the invention, the preparation method of the polyvinyl alcohol quaternary ammonium salt stabilizer comprises the following steps:
s1, dissolving polyvinyl alcohol in an aqueous solution to obtain a polyvinyl alcohol solution;
S2, mixing the polyvinyl alcohol solution prepared in the step S1, dimethylaminoethyl methacrylate and an initiator, heating and stirring for reaction, adding ethanol for precipitation, filtering and washing to obtain modified polyvinyl alcohol;
s3, adding the modified polyvinyl alcohol prepared in the step S2 into an organic solvent, adding alkali and epoxy chloropropane, heating and stirring for reaction, adding water for precipitation, filtering, washing and drying to obtain the polyvinyl alcohol quaternary ammonium salt stabilizer.
As a further improvement of the present invention, the polyvinyl alcohol solution in step S1 is contained in an amount of 30 to 40% by weight.
As a further improvement of the invention, the mass ratio of the polyvinyl alcohol solution to the dimethylaminoethyl methacrylate to the initiator in the step S2 is 100:10-12:0.5-1, the initiator is at least one selected from sodium persulfate, potassium persulfate and ammonium persulfate, the temperature of the heating and stirring reaction is 60-70 ℃ and the time is 1-2h.
As a further improvement of the invention, in the step S3, the organic solvent is selected from at least one of dichloromethane, chloroform, ethyl acetate, methyl acetate, butyl acetate, petroleum ether, cyclohexane and n-hexane, the alkali is selected from at least one of triethylamine, diethylamine, naOH and KOH, the mass ratio of the modified polyvinyl alcohol to the alkali to the epichlorohydrin is 10:2-3:2-4, and the stirring reaction temperature is 40-60 ℃ and the stirring reaction time is 2-3h.
As a further improvement of the invention, the preparation method of the polyvinyl alcohol quaternary ammonium salt stabilizer specifically comprises the following steps:
s1, dissolving polyvinyl alcohol in an aqueous solution to obtain a 30-40wt% polyvinyl alcohol solution;
s2, mixing 100 parts by weight of the polyvinyl alcohol solution prepared in the step S1, 10-12 parts by weight of dimethylaminoethyl methacrylate and 0.5-1 part by weight of an initiator, heating to 60-70 ℃, stirring and reacting for 1-2 hours, adding equal volume of ethanol for precipitation, filtering and washing to obtain modified polyvinyl alcohol;
S3, adding 10 parts by weight of the modified polyvinyl alcohol prepared in the step S2 into 50 parts by weight of an organic solvent, adding 2-3 parts by weight of alkali and 2-4 parts by weight of epichlorohydrin, heating to 40-60 ℃, stirring and reacting for 2-3 hours, adding equal volume of water for precipitation, filtering, washing and drying to obtain the polyvinyl alcohol quaternary ammonium salt stabilizer.
The invention further provides a preparation method of the silicon oxide thinning liquid for the integrated circuit, which comprises the following steps of uniformly stirring and mixing hydrofluoric acid, sulfuric acid, nitric acid, a surfactant and water, adding a polyvinyl alcohol quaternary ammonium salt stabilizer, and stirring and mixing to obtain the silicon oxide thinning liquid for the integrated circuit.
The silicon oxide thinning liquid for the integrated circuit has the advantages that the polyvinyl alcohol quaternary ammonium salt stabilizer is added, and hydrofluoric acid and nitric acid can be fixed through forming macromolecular gel, so that high-temperature volatilization of the hydrofluoric acid and the nitric acid is effectively avoided, pollution to the environment is reduced, meanwhile, high-concentration hydrofluoric acid is maintained, and the working efficiency of the thinning liquid is greatly improved.
The polyvinyl alcohol quaternary ammonium salt stabilizer provided by the invention contains a long-chain quaternary ammonium salt structure, plays a role in stabilizing hydrofluoric acid, and can further reduce the surface tension of a thinning liquid and improve the etching effect.
The invention uses acids with smaller toxicity to cooperate with hydrofluoric acid to play a role, so that the concentration and the dosage of the hydrofluoric acid are greatly reduced, and the toxicity and the volatility of acids such as sulfuric acid, nitric acid and the like relative to the hydrofluoric acid are much smaller, thereby obviously improving the safety and the environmental protection of etching liquid.
The silicon oxide thinning liquid for the integrated circuit has the advantages of improved utilization rate, remarkably reduced waste liquid yield, simple treatment, simple preparation method, safety, environmental protection, high working efficiency and wide application prospect.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The raw materials comprise (by weight parts) 5 parts of polyvinyl alcohol quaternary ammonium salt stabilizer, 10 parts of hydrofluoric acid, 5 parts of 98% concentrated sulfuric acid, 5 parts of nitric acid, 3 parts of sodium stearyl benzene sulfonate and 50 parts of water.
The preparation method of the polyvinyl alcohol quaternary ammonium salt stabilizer specifically comprises the following steps:
S1, dissolving polyvinyl alcohol in an aqueous solution to obtain a 30wt% polyvinyl alcohol solution;
s2, mixing 100 parts by weight of the polyvinyl alcohol solution prepared in the step S1, 10 parts by weight of dimethylaminoethyl methacrylate and 0.5 part by weight of potassium persulfate, heating to 60 ℃, stirring and reacting for 1h, adding equal volume of ethanol for precipitation, filtering and washing to obtain modified polyvinyl alcohol;
S3, adding 10 parts by weight of the modified polyvinyl alcohol prepared in the step S2 into 50 parts by weight of petroleum ether, adding 2 parts by weight of NaOH and 2 parts by weight of epichlorohydrin, heating to 40 ℃, stirring and reacting for 2 hours, adding equal volume of water for precipitation, filtering, washing and drying to obtain the polyvinyl alcohol quaternary ammonium salt stabilizer.
A process for preparing the silicon oxide thinning liquid for integrated circuit includes such steps as proportionally mixing hydrofluoric acid, 98% concentrated sulfuric acid, nitric acid, sodium stearyl benzene sulfonate and water, stirring, adding polyvinyl alcohol quaternary ammonium salt stabilizer, and stirring.
Example 2
The raw materials comprise (by weight parts) 10 parts of polyvinyl alcohol quaternary ammonium salt stabilizer, 20 parts of hydrofluoric acid, 10 parts of 98% concentrated sulfuric acid, 10 parts of nitric acid, 5 parts of sodium hexadecyl benzene sulfonate and 90 parts of water.
The preparation method of the polyvinyl alcohol quaternary ammonium salt stabilizer specifically comprises the following steps:
s1, dissolving polyvinyl alcohol in an aqueous solution to obtain a 40wt% polyvinyl alcohol solution;
S2, mixing 100 parts by weight of the polyvinyl alcohol solution prepared in the step S1, 12 parts by weight of dimethylaminoethyl methacrylate and 1 part by weight of sodium persulfate, heating to 70 ℃, stirring for reaction for 2 hours, adding equal volume of ethanol for precipitation, filtering and washing to obtain modified polyvinyl alcohol;
S3, adding 10 parts by weight of the modified polyvinyl alcohol prepared in the step S2 into 50 parts by weight of ethyl acetate, adding 3 parts by weight of triethylamine and 4 parts by weight of epichlorohydrin, heating to 60 ℃, stirring for reaction for 3 hours, adding equal volume of water for precipitation, filtering, washing and drying to obtain the polyvinyl alcohol quaternary ammonium salt stabilizer.
A process for preparing the silicon oxide thinning liquid for integrated circuit includes such steps as proportionally mixing hydrofluoric acid, 98% concentrated sulfuric acid, nitric acid, sodium hexadecyl benzenesulfonate and water, stirring, adding polyvinyl alcohol quaternary ammonium salt stabilizer, and stirring.
Example 3
The raw materials comprise 7 parts by weight of polyvinyl alcohol quaternary ammonium salt stabilizer, 15 parts by weight of hydrofluoric acid, 7 parts by weight of 98% concentrated sulfuric acid, 7 parts by weight of nitric acid, 4 parts by weight of sodium dodecyl sulfate and 70 parts by weight of water.
The preparation method of the polyvinyl alcohol quaternary ammonium salt stabilizer specifically comprises the following steps:
s1, dissolving polyvinyl alcohol in an aqueous solution to obtain a 35wt% polyvinyl alcohol solution;
S2, mixing 100 parts by weight of the polyvinyl alcohol solution prepared in the step S1, 11 parts by weight of dimethylaminoethyl methacrylate and 0.7 part by weight of ammonium persulfate, heating to 65 ℃, stirring and reacting for 1.5 hours, adding equal volume of ethanol for precipitation, filtering and washing to obtain modified polyvinyl alcohol;
S3, adding 10 parts by weight of the modified polyvinyl alcohol prepared in the step S2 into 50 parts by weight of dichloromethane, adding 2.5 parts by weight of KOH and 3 parts by weight of epichlorohydrin, heating to 50 ℃, stirring and reacting for 2.5 hours, adding equal volume of water for precipitation, filtering, washing and drying to obtain the polyvinyl alcohol quaternary ammonium salt stabilizer.
A process for preparing the silicon oxide thinning liquid for integrated circuit includes such steps as proportionally mixing hydrofluoric acid, 98% concentrated sulfuric acid, nitric acid, sodium laurylsulfate and water, stirring, adding the stabilizer of quaternary ammonium polyvinyl alcohol, and stirring.
Comparative example 1
The difference compared with example 3 is that step S2 is not performed in the preparation process of the polyvinyl alcohol quaternary ammonium salt stabilizer.
The raw materials comprise 7 parts by weight of polyvinyl alcohol quaternary ammonium salt stabilizer, 15 parts by weight of hydrofluoric acid, 7 parts by weight of 98% concentrated sulfuric acid, 7 parts by weight of nitric acid, 4 parts by weight of sodium dodecyl sulfate and 70 parts by weight of water.
The preparation method of the polyvinyl alcohol quaternary ammonium salt stabilizer specifically comprises the following steps:
s1, dissolving polyvinyl alcohol in an aqueous solution to obtain a 35wt% polyvinyl alcohol solution;
S2, adding 10 parts by weight of the modified polyvinyl alcohol prepared in the step S1 into 50 parts by weight of dichloromethane, adding 2.5 parts by weight of KOH and 3 parts by weight of epichlorohydrin, heating to 50 ℃, stirring and reacting for 2.5 hours, adding equal volume of water for precipitation, filtering, washing and drying to obtain the polyvinyl alcohol quaternary ammonium salt stabilizer.
A process for preparing the silicon oxide thinning liquid for integrated circuit includes such steps as proportionally mixing hydrofluoric acid, 98% concentrated sulfuric acid, nitric acid, sodium laurylsulfate and water, stirring, adding the stabilizer of quaternary ammonium polyvinyl alcohol, and stirring.
Comparative example 2
The difference compared with example 3 is that steps S2 and S3 are not carried out in the preparation process of the polyvinyl alcohol quaternary ammonium salt stabilizer.
The raw materials comprise 7 parts by weight of polyvinyl alcohol quaternary ammonium salt stabilizer, 15 parts by weight of hydrofluoric acid, 7 parts by weight of 98% concentrated sulfuric acid, 7 parts by weight of nitric acid, 4 parts by weight of sodium dodecyl sulfate and 70 parts by weight of water.
The preparation method of the polyvinyl alcohol quaternary ammonium salt stabilizer specifically comprises the following steps of dissolving polyvinyl alcohol in an aqueous solution to obtain a 35wt% polyvinyl alcohol solution.
A process for preparing the silicon oxide thinning liquid for integrated circuit includes such steps as proportionally mixing hydrofluoric acid, 98% concentrated sulfuric acid, nitric acid, sodium laurylsulfate and water, stirring, adding the stabilizer of quaternary ammonium polyvinyl alcohol, and stirring.
Test example 1
The integrated circuits prepared in examples 1-3 and comparative examples 1-2 were subjected to performance test with a silicon oxide thinner, and the results are shown in Table 1.
TABLE 1
| Group of | Thinning liquid utilization (%) | Thickness uniformity after thinning (%) | Thinning speed (mu m/min) |
| Example 1 | 35 | 1.02 | 22 |
| Example 2 | 37 | 1.08 | 24 |
| Example 3 | 40 | 0.99 | 25 |
| Comparative example 1 | 25 | 2.54 | 12 |
| Comparative example 2 | 18 | 3.14 | 6 |
As can be seen from the above table, the silicon oxide thinning liquid for integrated circuits prepared in the embodiments 1-3 of the present invention has a rapid thinning rate, and the thickness uniformity and the use ratio of the thinning liquid are high after thinning.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
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