CN117761969A - Stripping liquid and preparation method and application thereof - Google Patents
Stripping liquid and preparation method and application thereof Download PDFInfo
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- CN117761969A CN117761969A CN202311795162.4A CN202311795162A CN117761969A CN 117761969 A CN117761969 A CN 117761969A CN 202311795162 A CN202311795162 A CN 202311795162A CN 117761969 A CN117761969 A CN 117761969A
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- 239000007788 liquid Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 72
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 72
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 63
- 230000001105 regulatory effect Effects 0.000 claims abstract description 43
- 239000003607 modifier Substances 0.000 claims abstract description 33
- 230000000694 effects Effects 0.000 claims abstract description 29
- 239000002994 raw material Substances 0.000 claims abstract description 23
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 20
- LIIRANHZCBWPSP-UHFFFAOYSA-N 1-(methylamino)cyclopentan-1-ol Chemical compound CNC1(O)CCCC1 LIIRANHZCBWPSP-UHFFFAOYSA-N 0.000 claims abstract description 18
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 18
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims description 70
- 238000003756 stirring Methods 0.000 claims description 60
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 50
- 238000000498 ball milling Methods 0.000 claims description 25
- 229910052882 wollastonite Inorganic materials 0.000 claims description 25
- 239000010456 wollastonite Substances 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 24
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 16
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 16
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 16
- 239000012286 potassium permanganate Substances 0.000 claims description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 229920002120 photoresistant polymer Polymers 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 8
- 239000011787 zinc oxide Substances 0.000 claims description 8
- 229920001661 Chitosan Polymers 0.000 claims description 7
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims description 7
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- 239000007853 buffer solution Substances 0.000 claims description 6
- 239000004202 carbamide Substances 0.000 claims description 6
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims description 6
- 239000001509 sodium citrate Substances 0.000 claims description 6
- 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 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 230000003750 conditioning effect Effects 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000012527 feed solution Substances 0.000 claims 1
- 238000002203 pretreatment Methods 0.000 claims 1
- 239000002253 acid Substances 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 230000002301 combined effect Effects 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 9
- 238000007654 immersion Methods 0.000 description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- 239000003674 animal food additive Substances 0.000 description 4
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- PRBXPAHXMGDVNQ-UHFFFAOYSA-N 2-[2-(2-hydroxyethoxy)ethoxy]acetic acid Chemical compound OCCOCCOCC(O)=O PRBXPAHXMGDVNQ-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- OPKOKAMJFNKNAS-UHFFFAOYSA-N N-methylethanolamine Chemical compound CNCCO OPKOKAMJFNKNAS-UHFFFAOYSA-N 0.000 description 2
- 239000002798 polar solvent Substances 0.000 description 2
- 150000003141 primary amines Chemical class 0.000 description 2
- 150000003335 secondary amines Chemical class 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 description 1
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 description 1
- 229940075557 diethylene glycol monoethyl ether Drugs 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to the technical field of stripping liquid, and in particular discloses a stripping liquid which comprises the following raw materials in parts by weight: 20-30 parts of N-methylpyrrolidone, 10-20 parts of ethylenediamine, 5-10 parts of methylaminocyclopentanol and 1-4 parts of nitrilotriacetic acid. The stripping liquid adopts N-methyl pyrrolidone, ethylenediamine, methylaminocyclopentanol and nitrilotriacetic acid as matrix agents to form stripping effects, and the stripping effects can be enhanced by mutually blending the flaky graphene regulating effect inlet agent and the nano whisker modifier, so that the product formed by combined effect can be improved, and meanwhile, the high temperature resistance and acid corrosion resistance stability of the product are optimized.
Description
Technical Field
The invention relates to the technical field of stripping liquid, in particular to stripping liquid and a preparation method and application thereof.
Background
Conventional stripping compositions are often formulated with organic amines such as primary or secondary amines in combination with polar solvents or diols; such as Monoethanolamine (MEA) as a primary amine, 2-methylaminoethanol and the like as a secondary amine, N-methylpyrrolidone (NMP), sulfolane, dimethylsulfoxide (DMSO) and the like as a polar solvent, diethylene glycol monoethyl Ether (EDG), diethylene glycol monobutyl ether (BDG), triethylene glycol ether (TEG) and the like as a glycol, and the stripping liquid is poor in stripping performance and poor in stability under high-temperature, acid corrosion conditions, thereby limiting stripping efficiency, based on which the present invention further improves the treatment thereof.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide stripping liquid, a preparation method and application thereof, so as to solve the problems in the prior art.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides a stripping liquid which comprises the following raw materials in parts by weight:
20-30 parts of N-methylpyrrolidone, 10-20 parts of ethylenediamine, 5-10 parts of methylaminocyclopentanol and 1-4 parts of nitrilotriacetic acid.
Preferably, the stripping liquid comprises the following raw materials in parts by weight:
25 parts of N-methylpyrrolidone, 15 parts of ethylenediamine, 7.5 parts of methylaminocyclopentanol and 2.5 parts of nitrilotriacetic acid.
Preferably, the stripping liquid further comprises 5-10 parts of flaky graphene regulating effect agent and 3-6 parts of nano whisker modifier;
the preparation method of the flaky graphene regulating effect agent comprises the following steps:
s01: uniformly dispersing flaky graphene in a sufficient amount of potassium permanganate solution by ultrasonic, washing, drying, and performing heat improvement adjustment treatment to obtain a heat-adjusted graphene agent;
s02: adding 5-5% of lanthanum chloride solution with the mass fraction of 5-5% of the total mass of the sodium dodecyl benzene sulfonate solution and 1-3% of citric acid with the mass fraction of 5-10% of the total mass of the sodium dodecyl benzene sulfonate solution into the sodium dodecyl benzene sulfonate solution, and fully stirring to obtain a pre-mixed solution;
s03: stirring the thermally regulated graphene agent in a preset solution which is 5-10 times of the total amount of the thermally regulated graphene agent, and after stirring, washing and drying to obtain preset graphene;
s04: and (3) carrying out ball milling improvement treatment on the pre-adjusted graphene and the effect feed liquid according to a weight ratio of 5:2, wherein the ball milling rotating speed is 1000-1500r/min, the ball milling time is 1-2h, and after ball milling, washing and drying are carried out to obtain the graphene-like effect feed agent.
Preferably, the mass fraction of the potassium permanganate solution is 10% -15%; the power of ultrasonic dispersion is 300-350W, and the ultrasonic time is 1-2h.
Preferably, the specific operation steps of the heat improvement conditioning process are:
heat treating at 210-230deg.C for 5-10min, cooling to 150-160deg.C at 2-3deg.C/min, maintaining for 2-5min, and cooling to room temperature at 1-2deg.C/min.
Preferably, the stirring rotation speed of the stirring pre-adjustment treatment is 750-850r/min, and the stirring time is 1-2h.
Preferably, the effective feed liquid comprises the following raw materials in parts by weight:
2-5 parts of nano silica sol, 1-3 parts of phosphoric acid buffer solution with pH value of 5.0, 4-7 parts of urea and 8-12 parts of sodium citrate solution with mass fraction of 10%, and 1-2 parts of nano zinc oxide.
Preferably, the preparation method of the nano whisker modifier comprises the following steps:
s101: preheating wollastonite at 55-60 ℃ for 10-15min, then immersing in 3-5 times of yttrium nitrate solution with mass fraction of 5%, wherein the immersing pressure is 10-15MPa, the immersing time is 1-2h, and the wollastonite agent is obtained after immersing;
s102: uniformly stirring the nano calcium sulfate whisker in a chitosan solution with the mass fraction of 5% which is 3-5 times of the total amount of the nano calcium sulfate whisker, then adding wollastonite with the mass fraction of 2-5% of the total amount of the nano calcium sulfate whisker and sodium lignin sulfonate with the mass fraction of 2-5% of the nano calcium sulfate whisker, fully stirring, and finally washing and drying to obtain the nano whisker modifier.
The invention also provides a preparation method of the stripping liquid, which comprises the following steps:
step one: weighing the raw materials:
step two: and pouring N-methylpyrrolidone, ethylenediamine, methylaminocyclopentanol, nitrilotriacetic acid, a flaky graphene regulating effect feed agent and a nano whisker modifier into a stirrer for stirring treatment, and stirring fully to obtain stripping liquid.
The invention also provides an application of the stripping liquid in stripping of the chip photoresist.
Compared with the prior art, the invention has the following beneficial effects:
the stripping solution adopts N-methyl pyrrolidone, ethylenediamine, methylaminocyclopentanol and nitrilotriacetic acid as matrix agents to form stripping effects, and the stripping effects can be enhanced by mutually blending the flaky graphene regulating effect inlet agent and the nano whisker modifier, and the product formed by combined effect can be improved by optimizing the high temperature resistance and acid corrosion resistance stability of the product; the flaky graphene regulating effect feed agent adopts the flaky graphene to be uniformly dispersed in a sufficient potassium permanganate solution in advance, then is washed and dried, is subjected to thermal improvement regulating treatment, is optimized by the step, optimizes the activity efficiency and dispersity of graphene, and is matched with the pre-adjustment liquid for pre-adjustment improvement, so that the better matching effect feed liquid ball milling improvement can be realized, the raw materials of the effect feed liquid are mutually matched and combined, the obtained flaky graphene regulating effect feed agent is more stable in distribution in a system, the obtained product performance effect is stronger, and the nano whisker modifier is matched with the flaky graphene regulating effect feed agent by nano calcium sulfate whisker through chitosan liquid, wollastonite agent and sodium lignin sulfonate, so that the obtained nano whisker modifier is better in synergistic effect with the flaky graphene regulating effect feed agent, the product performance stability is more remarkable, and the stripping performance of the product is more obvious.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. 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.
The stripping liquid comprises the following raw materials in parts by weight:
20-30 parts of N-methylpyrrolidone, 10-20 parts of ethylenediamine, 5-10 parts of methylaminocyclopentanol and 1-4 parts of nitrilotriacetic acid.
The stripping liquid of the embodiment comprises the following raw materials in parts by weight:
25 parts of N-methylpyrrolidone, 15 parts of ethylenediamine, 7.5 parts of methylaminocyclopentanol and 2.5 parts of nitrilotriacetic acid.
The stripping liquid of the embodiment also comprises 5-10 parts of flaky graphene regulating effect feed agent and 3-6 parts of nano whisker modifier;
the preparation method of the flaky graphene regulating effect agent in the embodiment comprises the following steps:
s01: uniformly dispersing flaky graphene in a sufficient amount of potassium permanganate solution by ultrasonic, washing, drying, and performing heat improvement adjustment treatment to obtain a heat-adjusted graphene agent;
s02: adding 5-5% of lanthanum chloride solution with the mass fraction of 5-5% of the total mass of the sodium dodecyl benzene sulfonate solution and 1-3% of citric acid with the mass fraction of 5-10% of the total mass of the sodium dodecyl benzene sulfonate solution into the sodium dodecyl benzene sulfonate solution, and fully stirring to obtain a pre-mixed solution;
s03: stirring the thermally regulated graphene agent in a preset solution which is 5-10 times of the total amount of the thermally regulated graphene agent, and after stirring, washing and drying to obtain preset graphene;
s04: and (3) carrying out ball milling improvement treatment on the pre-adjusted graphene and the effect feed liquid according to a weight ratio of 5:2, wherein the ball milling rotating speed is 1000-1500r/min, the ball milling time is 1-2h, and after ball milling, washing and drying are carried out to obtain the graphene-like effect feed agent.
The mass fraction of the potassium permanganate solution in the embodiment is 10% -15%; the power of ultrasonic dispersion is 300-350W, and the ultrasonic time is 1-2h.
The specific operation steps of the heat improvement adjustment process of this embodiment are:
heat treating at 210-230deg.C for 5-10min, cooling to 150-160deg.C at 2-3deg.C/min, maintaining for 2-5min, and cooling to room temperature at 1-2deg.C/min.
The stirring rotation speed of the stirring pre-adjustment treatment is 750-850r/min, and the stirring time is 1-2h.
The effective feed liquid of the embodiment comprises the following raw materials in parts by weight:
2-5 parts of nano silica sol, 1-3 parts of phosphoric acid buffer solution with pH value of 5.0, 4-7 parts of urea and 8-12 parts of sodium citrate solution with mass fraction of 10%, and 1-2 parts of nano zinc oxide.
The preparation method of the nano whisker modifier in the embodiment comprises the following steps:
s101: preheating wollastonite at 55-60 ℃ for 10-15min, then immersing in 3-5 times of yttrium nitrate solution with mass fraction of 5%, wherein the immersing pressure is 10-15MPa, the immersing time is 1-2h, and the wollastonite agent is obtained after immersing;
s102: uniformly stirring the nano calcium sulfate whisker in a chitosan solution with the mass fraction of 5% which is 3-5 times of the total amount of the nano calcium sulfate whisker, then adding wollastonite with the mass fraction of 2-5% of the total amount of the nano calcium sulfate whisker and sodium lignin sulfonate with the mass fraction of 2-5% of the nano calcium sulfate whisker, fully stirring, and finally washing and drying to obtain the nano whisker modifier.
The preparation method of the stripping liquid comprises the following steps:
step one: weighing the raw materials:
step two: and pouring N-methylpyrrolidone, ethylenediamine, methylaminocyclopentanol, nitrilotriacetic acid, a flaky graphene regulating effect feed agent and a nano whisker modifier into a stirrer for stirring treatment, and stirring fully to obtain stripping liquid.
The application of the stripping liquid in stripping the photoresist of the chip is provided.
Example 1.
The stripping liquid comprises the following raw materials in parts by weight:
20 parts of N-methylpyrrolidone, 10 parts of ethylenediamine, 5 parts of methylaminocyclopentanol and 1 part of nitrilotriacetic acid.
The stripping liquid of the embodiment also comprises 5 parts of flaky graphene regulating effect agent and 3 parts of nano whisker modifier;
the preparation method of the flaky graphene regulating effect agent in the embodiment comprises the following steps:
s01: uniformly dispersing flaky graphene in a sufficient amount of potassium permanganate solution by ultrasonic, washing, drying, and performing heat improvement adjustment treatment to obtain a heat-adjusted graphene agent;
s02: adding 5% of lanthanum chloride solution with the mass fraction of 5% and 1% of citric acid with the mass fraction of 2% of the total mass of the sodium dodecyl benzene sulfonate solution into the sodium dodecyl benzene sulfonate solution, and stirring fully to obtain a pre-adjustment solution;
s03: stirring the thermally regulated graphene agent in a preset solution which is 5 times of the total amount of the thermally regulated graphene agent, and after stirring, washing and drying to obtain preset graphene;
s04: and (3) carrying out ball milling improvement treatment on the preset graphene and effect feed liquid according to a weight ratio of 5:2, wherein the ball milling rotating speed is 1000r/min, the ball milling time is 1h, and after ball milling, washing and drying are carried out to obtain the graphene-like effect feed agent.
The mass fraction of the potassium permanganate solution in the embodiment is 10%; the power of ultrasonic dispersion is 300W, and the ultrasonic time is 1h.
The specific operation steps of the heat improvement adjustment process of this embodiment are:
heat-treating at 210 deg.C for 5min, cooling to 150 deg.C at 2 deg.C/min, maintaining for 2min, and cooling to room temperature at 1 deg.C/min.
The stirring rotation speed of the stirring pre-adjustment treatment in this embodiment is 750r/min, and the stirring time is 1h.
The effective feed liquid of the embodiment comprises the following raw materials in parts by weight:
2 parts of nano silica sol, 1 part of phosphoric acid buffer solution with the pH value of 5.0, 4 parts of urea and 8 parts of sodium citrate solution with the mass fraction of 10%, and 1 part of nano zinc oxide.
The preparation method of the nano whisker modifier in the embodiment comprises the following steps:
s101: preheating wollastonite at 55 ℃ for 10min, then immersing the wollastonite in 3 times of 5% yttrium nitrate solution with the immersion pressure of 10MPa and the immersion time of 1h, and obtaining wollastonite agent;
s102: uniformly stirring the nano calcium sulfate whisker in a chitosan solution with the mass fraction of 5% which is 3 times of the total amount of the nano calcium sulfate whisker, then adding wollastonite with the total amount of 2% of the nano calcium sulfate whisker and sodium lignin sulfonate with the total amount of 2% of the nano calcium sulfate whisker, fully stirring, and finally washing and drying to obtain the nano whisker modifier.
The preparation method of the stripping liquid comprises the following steps:
step one: weighing the raw materials:
step two: and pouring N-methylpyrrolidone, ethylenediamine, methylaminocyclopentanol, nitrilotriacetic acid, a flaky graphene regulating effect feed agent and a nano whisker modifier into a stirrer for stirring treatment, and stirring fully to obtain stripping liquid.
The application of the stripping liquid in stripping the photoresist of the chip is provided.
Example 2.
The stripping liquid comprises the following raw materials in parts by weight:
30 parts of N-methylpyrrolidone, 20 parts of ethylenediamine, 10 parts of methylaminocyclopentanol and 4 parts of nitrilotriacetic acid.
The stripping liquid of the embodiment also comprises 10 parts of flaky graphene regulating effect agent and 6 parts of nano whisker modifier;
the preparation method of the flaky graphene regulating effect agent in the embodiment comprises the following steps:
s01: uniformly dispersing flaky graphene in a sufficient amount of potassium permanganate solution by ultrasonic, washing, drying, and performing heat improvement adjustment treatment to obtain a heat-adjusted graphene agent;
s02: adding 5% of lanthanum chloride solution with the mass fraction of 5% of the total mass of the sodium dodecyl benzene sulfonate solution and 3% of citric acid with the mass fraction of 10% of the sodium dodecyl benzene sulfonate solution into the sodium dodecyl benzene sulfonate solution, and stirring fully to obtain a pre-adjustment solution;
s03: stirring the thermally regulated graphene agent in preset liquid which is 10 times of the total amount of the thermally regulated graphene agent, and after stirring, washing and drying to obtain preset graphene;
s04: and (3) carrying out ball milling improvement treatment on the preset graphene and effect feed liquid according to a weight ratio of 5:2, wherein the ball milling rotating speed is 1500r/min, the ball milling time is 2h, and after ball milling, washing and drying are carried out to obtain the graphene-like effect feed agent.
The mass fraction of the potassium permanganate solution in the embodiment is 15%; the power of ultrasonic dispersion is 350W, and the ultrasonic time is 2h.
The specific operation steps of the heat improvement adjustment process of this embodiment are:
heat-treating at 230deg.C for 10min, cooling to 160deg.C at 3deg.C/min, maintaining for 5min, and cooling to room temperature at 2deg.C/min.
The stirring rotation speed of the stirring pre-adjustment treatment in the embodiment is 850r/min, and the stirring time is 2h.
The effective feed liquid of the embodiment comprises the following raw materials in parts by weight:
5 parts of nano silica sol, 3 parts of phosphoric acid buffer solution with the pH value of 5.0, 7 parts of urea and 12 parts of sodium citrate solution with the mass fraction of 10%, and 2 parts of nano zinc oxide.
The preparation method of the nano whisker modifier in the embodiment comprises the following steps:
s101: preheating wollastonite at 60 ℃ for 15min, then immersing the wollastonite in 5 times of 5% yttrium nitrate solution with the immersion pressure of 15MPa and the immersion time of 2h, and obtaining wollastonite agent;
s102: uniformly stirring the nano calcium sulfate whisker in a chitosan solution with the mass fraction of 5% which is 5 times of the total amount of the nano calcium sulfate whisker, then adding wollastonite with the mass fraction of 5% of the total amount of the nano calcium sulfate whisker and sodium lignin sulfonate with the mass fraction of 5% of the nano calcium sulfate whisker, fully stirring, and finally washing and drying to obtain the nano whisker modifier.
The preparation method of the stripping liquid comprises the following steps:
step one: weighing the raw materials:
step two: and pouring N-methylpyrrolidone, ethylenediamine, methylaminocyclopentanol, nitrilotriacetic acid, a flaky graphene regulating effect feed agent and a nano whisker modifier into a stirrer for stirring treatment, and stirring fully to obtain stripping liquid.
The application of the stripping liquid in stripping the photoresist of the chip is provided.
Example 3.
The stripping liquid comprises the following raw materials in parts by weight:
25 parts of N-methylpyrrolidone, 15 parts of ethylenediamine, 7.5 parts of methylaminocyclopentanol and 2.5 parts of nitrilotriacetic acid.
The stripping liquid of the embodiment also comprises 7.5 parts of flaky graphene regulating effect agent and 4.5 parts of nano whisker modifier;
the preparation method of the flaky graphene regulating effect agent in the embodiment comprises the following steps:
s01: uniformly dispersing flaky graphene in a sufficient amount of potassium permanganate solution by ultrasonic, washing, drying, and performing heat improvement adjustment treatment to obtain a heat-adjusted graphene agent;
s02: adding a lanthanum chloride solution with the mass fraction of 5% and a citric acid with the mass fraction of 2% into a sodium dodecyl benzene sulfonate solution with the mass fraction of 7.5% to obtain a sodium dodecyl benzene sulfonate solution, and stirring fully to obtain a pre-mixed solution;
s03: stirring the thermally regulated graphene agent in a preset solution which is 7.5 times of the total amount of the thermally regulated graphene agent, and after stirring, washing and drying to obtain preset graphene;
s04: and (3) carrying out ball milling improvement treatment on the preset graphene and the effect feed liquid according to a weight ratio of 5:2, wherein the ball milling rotating speed is 1250r/min, the ball milling time is 1.5h, and the graphene-like effect feed agent is obtained after water washing and drying after ball milling.
The mass fraction of the potassium permanganate solution of the embodiment is 12.5%; the power of ultrasonic dispersion is 325W, and the ultrasonic time is 1.5h.
The specific operation steps of the heat improvement adjustment process of this embodiment are:
heat-treating at 220deg.C for 7.5min, cooling to 150deg.C at a rate of 2.5deg.C/min, maintaining for 3.5min, and cooling to room temperature at a rate of 1.5deg.C/min.
The stirring rotation speed of the stirring pre-adjustment treatment in the embodiment is 800r/min, and the stirring time is 1.5h.
The effective feed liquid of the embodiment comprises the following raw materials in parts by weight:
3.5 parts of nano silica sol, 2 parts of phosphoric acid buffer solution with the pH value of 5.0, 5.5 parts of urea and 10 parts of sodium citrate solution with the mass fraction of 10 percent, and 1.5 parts of nano zinc oxide.
The preparation method of the nano whisker modifier in the embodiment comprises the following steps:
s101: preheating wollastonite at 58 ℃ for 12.5min, then immersing the wollastonite in 4 times of 5% yttrium nitrate solution with the immersion pressure of 12.5MPa and the immersion time of 1.5h, and obtaining a wollastonite agent;
s102: uniformly stirring the nano calcium sulfate whisker in a chitosan solution with the mass fraction of 5% which is 4 times of the total amount of the nano calcium sulfate whisker, then adding wollastonite with the mass fraction of 3.5% of the total amount of the nano calcium sulfate whisker and sodium lignin sulfonate with the mass fraction of 3.5% of the nano calcium sulfate whisker, fully stirring, and finally washing and drying to obtain the nano whisker modifier.
The preparation method of the stripping liquid comprises the following steps:
step one: weighing the raw materials:
step two: and pouring N-methylpyrrolidone, ethylenediamine, methylaminocyclopentanol, nitrilotriacetic acid, a flaky graphene regulating effect feed agent and a nano whisker modifier into a stirrer for stirring treatment, and stirring fully to obtain stripping liquid.
The application of the stripping liquid in stripping the photoresist of the chip is provided.
Comparative example 1.
Unlike example 3, a platelet-shaped graphene regulating effect agent was not added.
Comparative example 2.
Unlike example 3, the preparation of the platelet-shaped graphene regulating effect agent did not use the S01 treatment.
Comparative example 3.
Unlike example 3, the preparation of the graphene platelet conditioning effect agent did not use a pre-conditioning solution.
Comparative example 4.
Unlike example 3, the platelet-shaped graphene is prepared without an effect feed liquid treatment.
Comparative example 5.
The difference from example 3 is that no nano zinc oxide or nano silica sol is added in the preparation of the effective feed liquid.
Comparative example 6.
The difference from example 3 is that no nanowhisker modifier treatment was used.
Comparative example 7.
The difference from example 3 is that the nanowhisker modifier is prepared without treatment with wollastonite.
Stripping ratio (%) = [ (total area of photoresist before stripping-area of residual photoresist)/(total area of photoresist before stripping) ]x100%; meanwhile, placing the product at 65 ℃ for heat treatment for 6 hours, placing the product at 2% hydrochloric acid mist for 24 hours, and testing the temperature resistance and acid corrosion resistance of the product;
the results of the performance measurements of examples 1-3 and comparative examples 1-7 are as follows
The products of the invention have obvious stripping rate performance effects and obvious performance stability effects under the conditions of temperature resistance and acid corrosion resistance, as shown in examples 1-3 and comparative examples 1-7;
one of the adjustment effect feed agent of the flaky graphene and the treatment of the nano whisker modifier is not added, the performance of the product is obviously poor, and the performance effect of the product is obvious by adopting the cooperation of the flaky graphene and the nano whisker modifier;
the preparation of the flaky graphene regulating effect feed additive does not adopt S01 treatment, the preparation of the flaky graphene regulating effect feed additive does not adopt pre-adjustment liquid treatment, the preparation of the flaky graphene regulating effect feed additive does not adopt effect liquid treatment, the preparation of the effect feed liquid does not add nano zinc oxide, nano silica sol and wollastonite agent, the preparation of the nano whisker modifier does not adopt wollastonite agent, the performance of the product has a poor trend, and the performance effect of the product is most obvious only by adopting the flaky graphene regulating effect feed additive prepared by the method of the invention, and the effect of the product is not as obvious as that of the invention by adopting other methods.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (10)
1. The stripping liquid is characterized by comprising the following raw materials in parts by weight:
20-30 parts of N-methylpyrrolidone, 10-20 parts of ethylenediamine, 5-10 parts of methylaminocyclopentanol and 1-4 parts of nitrilotriacetic acid.
2. The stripping liquid according to claim 1, wherein the stripping liquid comprises the following raw materials in parts by weight:
25 parts of N-methylpyrrolidone, 15 parts of ethylenediamine, 7.5 parts of methylaminocyclopentanol and 2.5 parts of nitrilotriacetic acid.
3. The stripping solution as claimed in claim 1, wherein the stripping solution further comprises 5-10 parts of a platelet graphene regulating effect agent and 3-6 parts of a nanowhisker modifier;
the preparation method of the flaky graphene regulating effect agent comprises the following steps:
s01: uniformly dispersing flaky graphene in a sufficient amount of potassium permanganate solution by ultrasonic, washing, drying, and performing heat improvement adjustment treatment to obtain a heat-adjusted graphene agent;
s02: adding 5-5% of lanthanum chloride solution with the mass fraction of 5-5% of the total mass of the sodium dodecyl benzene sulfonate solution and 1-3% of citric acid with the mass fraction of 5-10% of the total mass of the sodium dodecyl benzene sulfonate solution into the sodium dodecyl benzene sulfonate solution, and fully stirring to obtain a pre-mixed solution;
s03: stirring the thermally regulated graphene agent in a preset solution which is 5-10 times of the total amount of the thermally regulated graphene agent, and after stirring, washing and drying to obtain preset graphene;
s04: and (3) carrying out ball milling improvement treatment on the pre-adjusted graphene and the effect feed liquid according to a weight ratio of 5:2, wherein the ball milling rotating speed is 1000-1500r/min, the ball milling time is 1-2h, and after ball milling, washing and drying are carried out to obtain the graphene-like effect feed agent.
4. A stripping solution as claimed in claim 3, wherein the mass fraction of the potassium permanganate solution is 10% -15%; the power of ultrasonic dispersion is 300-350W, and the ultrasonic time is 1-2h.
5. A stripping solution as claimed in claim 3, characterized in that the specific operating steps of the heat-modifying conditioning treatment are:
heat treating at 210-230deg.C for 5-10min, cooling to 150-160deg.C at 2-3deg.C/min, maintaining for 2-5min, and cooling to room temperature at 1-2deg.C/min.
6. A stripping solution according to claim 3, wherein the stirring speed of the stirring pre-treatment is 750-850r/min and the stirring time is 1-2h.
7. A stripping solution according to claim 3, wherein the effective feed solution comprises the following raw materials in parts by weight:
2-5 parts of nano silica sol, 1-3 parts of phosphoric acid buffer solution with pH value of 5.0, 4-7 parts of urea and 8-12 parts of sodium citrate solution with mass fraction of 10%, and 1-2 parts of nano zinc oxide.
8. A stripper according to claim 3, wherein the preparation method of the nanowhisker modifier is as follows:
s101: preheating wollastonite at 55-60 ℃ for 10-15min, then immersing in 3-5 times of yttrium nitrate solution with mass fraction of 5%, wherein the immersing pressure is 10-15MPa, the immersing time is 1-2h, and the wollastonite agent is obtained after immersing;
s102: uniformly stirring the nano calcium sulfate whisker in a chitosan solution with the mass fraction of 5% which is 3-5 times of the total amount of the nano calcium sulfate whisker, then adding wollastonite with the mass fraction of 2-5% of the total amount of the nano calcium sulfate whisker and sodium lignin sulfonate with the mass fraction of 2-5% of the nano calcium sulfate whisker, fully stirring, and finally washing and drying to obtain the nano whisker modifier.
9. A method of preparing the stripping solution as claimed in any one of claims 1 to 8, comprising the steps of:
step one: weighing the raw materials:
step two: and pouring N-methylpyrrolidone, ethylenediamine, methylaminocyclopentanol, nitrilotriacetic acid, a flaky graphene regulating effect feed agent and a nano whisker modifier into a stirrer for stirring treatment, and stirring fully to obtain stripping liquid.
10. Use of the stripping solution according to any one of claims 1-8 for chip photoresist stripping.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311795162.4A CN117761969B (en) | 2023-12-25 | Stripping liquid and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311795162.4A CN117761969B (en) | 2023-12-25 | Stripping liquid and preparation method and application thereof |
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