CN115678446A - UV visbreaking film for semiconductor cutting - Google Patents
UV visbreaking film for semiconductor cutting Download PDFInfo
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- CN115678446A CN115678446A CN202211251014.1A CN202211251014A CN115678446A CN 115678446 A CN115678446 A CN 115678446A CN 202211251014 A CN202211251014 A CN 202211251014A CN 115678446 A CN115678446 A CN 115678446A
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- 239000004065 semiconductor Substances 0.000 title claims abstract description 14
- 238000005520 cutting process Methods 0.000 title claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000012790 adhesive layer Substances 0.000 claims abstract description 44
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 31
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 31
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims abstract description 31
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims abstract description 31
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 31
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims abstract description 31
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 31
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims description 147
- 239000007790 solid phase Substances 0.000 claims description 115
- 239000000203 mixture Substances 0.000 claims description 80
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 78
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 70
- 239000007788 liquid Substances 0.000 claims description 62
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 56
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 52
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 claims description 47
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 claims description 47
- 239000007864 aqueous solution Substances 0.000 claims description 42
- 238000002156 mixing Methods 0.000 claims description 42
- 238000001035 drying Methods 0.000 claims description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- 238000005406 washing Methods 0.000 claims description 32
- 230000000181 anti-adherent effect Effects 0.000 claims description 28
- 229910021389 graphene Inorganic materials 0.000 claims description 27
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 25
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 24
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 24
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 24
- 239000003607 modifier Substances 0.000 claims description 24
- 238000000926 separation method Methods 0.000 claims description 24
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 claims description 18
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 18
- 229940014800 succinic anhydride Drugs 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 16
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- 229910021641 deionized water Inorganic materials 0.000 claims description 16
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- 210000004877 mucosa Anatomy 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 239000002313 adhesive film Substances 0.000 claims description 7
- 239000003292 glue Substances 0.000 claims description 5
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- 238000003848 UV Light-Curing Methods 0.000 abstract description 8
- 239000000853 adhesive Substances 0.000 abstract description 8
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- 239000000725 suspension Substances 0.000 description 18
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- 229920000139 polyethylene terephthalate Polymers 0.000 description 9
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- FKOZPUORKCHONH-UHFFFAOYSA-N 2-methylpropane-1-sulfonic acid Chemical compound CC(C)CS(O)(=O)=O FKOZPUORKCHONH-UHFFFAOYSA-N 0.000 description 3
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- 238000001723 curing Methods 0.000 description 2
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Landscapes
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a UV (ultraviolet) anti-adhesion film for semiconductor cutting, which comprises a substrate and a UV anti-adhesion adhesive layer, wherein the raw materials of the UV anti-adhesion adhesive layer comprise modified graphene, butyl acetate, acrylic acid, trimethylolpropane triacrylate, hydroxyethyl acrylate, a photoinitiator and N-methylpyrrolidone. The UV viscosity-reducing adhesive layer has good bonding strength before UV curing, has obvious viscosity-reducing effect after UV curing, and has no residual adhesive on the surface separated from an object after viscosity reduction.
Description
Technical Field
The invention relates to the technical field of UV (ultraviolet) anti-sticking films, in particular to a UV anti-sticking film for semiconductor cutting.
Background
Semiconductors are key components of digital products for home use and electronic devices. In the fabrication of large scale integrated circuits and in the fabrication of semiconductor devices, the essential base material is the semiconductor chip. Semiconductor chips are fabricated from monocrystalline silicon wafers, referred to as wafers. When a wafer material is cut and ground, a special protective film is needed for bonding and fixing. After the processing is finished, the processed wafer slices are completely stripped from the fixed adhesive film, and the wafer material is not influenced. The UV anti-sticking protective film used in the current industry can meet the performance that the adhesive force is reduced and the film is easily peeled off after the UV irradiation in the later peeling process. However, the UV anti-adhesive protective film is not resistant to high temperature, and even though the UV light irradiation adhesive force is reduced during later peeling after the high temperature, the small molecules of the adhesive layer still remain on the surface of the object to be protected.
Disclosure of Invention
Therefore, the invention provides a UV anti-adhesive film for semiconductor cutting, which comprises a substrate and a UV anti-adhesive layer, wherein the raw materials of the UV anti-adhesive layer comprise modified graphene, butyl acetate, acrylic acid, trimethylolpropane triacrylate, hydroxyethyl acrylate, a photoinitiator and N-methylpyrrolidone, and the preparation method of the modified graphene comprises the following steps:
(1) Uniformly mixing phosphoric acid and triethylamine to form a mixture, carrying out water bath on the mixture at a constant temperature of 70 +/-5 ℃, keeping the temperature for 3-4 h, adding graphene oxide into the mixture after the temperature is kept, stirring the mixture for 1-2 h at a constant temperature of 70 +/-5 ℃, then carrying out solid-liquid separation, washing a solid phase with ethanol, and drying to obtain a solid phase A;
(2) Preparing an aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid, stirring the solution, adding a solid phase A into the aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid in the stirring process, continuously stirring for 10-20 min after the feeding is finished, then adding acrylamide into the solution in the stirring state, continuously stirring for 5-8 min after the feeding is finished, then carrying out water bath at constant temperature of 70 +/-5 ℃, adding dibenzoyl peroxide into the solution in the stirring state after the constant temperature is kept, stirring for 5-7 h at constant temperature of 70 +/-5 ℃ after the feeding is finished, then stopping stirring, cooling to normal temperature, carrying out solid-liquid separation, washing the solid phase with deionized water, and drying to obtain a solid phase B;
(3) Mixing succinic anhydride, hydrogen peroxide and water, stirring for more than 4 hours at the temperature of 8-10 ℃ to obtain a mixture modifier, dispersing the solid phase B in N, N' -dimethylformamide to form turbid liquid, carrying out water bath to keep the temperature of the turbid liquid at constant temperature to 80 +/-5 ℃, then stirring the turbid liquid under the heat preservation condition, adding the mixture modifier in the stirring state, continuously stirring for more than 60 hours at constant temperature after finishing adding, then carrying out air cooling to normal temperature, carrying out solid-liquid separation, washing the solid phase with ethanol for 2 times, then washing with deionized water for 2 times, and drying to obtain the modified graphene.
Further, the UV visbreaking adhesive layer comprises the following raw materials in parts by weight: 3-5 parts of modified graphene, 50-60 parts of butyl acetate, 4-7 parts of acrylic acid, 5-10 parts of trimethylolpropane triacrylate, 2-4 parts of hydroxyethyl acrylate, 0.4-0.6 part of a photoinitiator and 20-30 parts of N-methylpyrrolidone.
Further, in the step (1), the phosphoric acid and the triethylamine are uniformly mixed to form a mixture, wherein the mixing mass ratio of the phosphoric acid to the triethylamine is phosphoric acid: triethylamine =10, and the solid-liquid mass ratio of graphene oxide added to the mixture is solid/liquid =1.
Further, in the step (2), the concentration of the 2-acrylamido 2-methylpropanesulfonic acid in the aqueous solution of the 2-acrylamido 2-methylpropanesulfonic acid is 10 to 15g/300mL, and the solid-liquid mass ratio of the solid phase a to the aqueous solution of the 2-acrylamido 2-methylpropanesulfonic acid added to the aqueous solution of the 2-acrylamido 2-methylpropanesulfonic acid is solid phase a/aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid =1/50; the mass ratio of the added mass of the acrylamide to the solid phase A is acrylamide: the solid phase A = 2-3, the mass ratio of the added dibenzoyl peroxide to the solid phase A is dibenzoyl peroxide: solid phase a =0.03mg:10 to 16g.
Further, in the step (3), the mixing mass ratio of succinic anhydride, hydrogen peroxide and water is succinic anhydride: hydrogen peroxide: water = 1.0-1.5; the mass fraction of solute in the hydrogen peroxide is 30 percent; the solid phase B is dispersed in N, N '-dimethylformamide to form a solid-liquid ratio of solid phase B/N, N' -dimethylformamide = 1-2 g/400mL, and the addition amount of the mixture modifier is 3-4 times of the mass of the solid phase B.
The invention also discloses a processing method of the UV anti-sticking film, which comprises the following steps:
weighing the raw materials of the UV visbreaking glue layer according to the weight parts, and uniformly mixing the butyl acetate, the acrylic acid, the trimethylolpropane triacrylate and the hydroxyethyl acrylate to obtain a mixed component I;
dispersing the modified graphene in N-methyl pyrrolidone uniformly to obtain a second mixed component;
and step three, heating the mixed component I to the temperature of 60 +/-2 ℃, preserving heat, stirring, adding the mixed component II under a stirring state, continuously stirring for 20-30 min after the addition is finished, adding the photoinitiator, continuously stirring for 10-20 min after the addition is finished, coating the mixture on the surface of the substrate, and drying for 2-3 min at the temperature of 120 ℃ to obtain the UV mucosa reducer.
The invention has the beneficial effects that: the UV visbreaking adhesive layer has good bonding strength before UV curing, the 180-degree peel strength can reach 24.8N/25mm, the visbreaking effect after UV curing is obvious, the 180-degree peel strength is reduced to 0.31N/25mm, and no residual adhesive exists on the surface separated from an object after visbreaking.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
The UV anti-adhesive film for semiconductor cutting comprises a PET substrate film and a UV anti-adhesive layer, wherein the raw materials of the UV anti-adhesive layer comprise modified graphene, butyl acetate, acrylic acid, trimethylolpropane triacrylate, hydroxyethyl acrylate, a photoinitiator and N-methylpyrrolidone, and the raw materials of the UV anti-adhesive layer comprise the following components in parts by weight: 3 parts of modified graphene, 50 parts of butyl acetate, 4 parts of acrylic acid, 5 parts of trimethylolpropane triacrylate, 2 parts of hydroxyethyl acrylate, 0.4 part of 1173 photoinitiator and 20 parts of N-methylpyrrolidone.
The preparation method of the modified graphene comprises the following steps:
(1) Uniformly mixing phosphoric acid and triethylamine to form a mixture, wherein the mixing mass ratio of the phosphoric acid to the triethylamine is phosphoric acid: triethylamine =10, keeping the temperature of the mixture constant to 70 ± 5 ℃ in a water bath, preserving the temperature for 3h, and after the preservation is finished, adding graphene oxide into the mixture, wherein the solid-liquid mass ratio of the added graphene oxide in the mixture is solid/liquid = 1; stirring the mixture for 1h at the constant temperature of 70 +/-5 ℃ at the speed of 50r/min, then carrying out solid-liquid separation, washing a solid phase by using ethanol, and drying to obtain a solid phase A;
(2) Preparing an aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid, wherein in the aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid, the concentration of 2-acrylamido 2-methylpropanesulfonic acid is 10g/300mL, and a solvent is water; stirring the solution at 50r/min, adding a solid phase A into the aqueous solution of the 2-acrylamido 2-methylpropanesulfonic acid during stirring, wherein the solid-liquid mass ratio of the solid phase A added into the aqueous solution of the 2-acrylamido 2-methylpropanesulfonic acid is that the solid phase A/the aqueous solution of the 2-acrylamido 2-methylpropanesulfonic acid =1/50; and after the addition is finished, stirring at the speed of 50r/min for 10min, and then adding acrylamide into the solution under the stirring state, wherein the mass ratio of the added acrylamide to the solid phase A is acrylamide: solid phase A =2, stirring is continued for 5min at 50r/min after the addition is completed, then the water bath is kept at a constant temperature of 70 +/-5 ℃, and dibenzoyl peroxide is added to the solution in a stirring state after the constant temperature, and the mass ratio of the added dibenzoyl peroxide to the solid phase A is dibenzoyl peroxide: solid phase a =0.03mg:10g of a mixture; stirring for 6h at the constant temperature of 70 +/-5 ℃ at 50r/min after the feeding is finished, then stopping stirring, cooling to the normal temperature in air, performing solid-liquid separation, washing a solid phase with deionized water, and drying to obtain a solid phase B;
(3) Mixing succinic anhydride, hydrogen peroxide and water, wherein the mixing mass ratio of the succinic anhydride to the hydrogen peroxide to the water is as follows: hydrogen peroxide: water = 1.0; stirring for 4 hours at the temperature of 8 ℃ at 50r/min to obtain a mixture modifier, dispersing the solid phase B in N, N '-dimethylformamide to form a suspension, wherein the solid-liquid ratio of the solid phase B dispersed in the N, N' -dimethylformamide is =1g/400mL, keeping the suspension at a constant temperature of 80 +/-5 ℃ in a water bath, stirring the suspension at the temperature of 50r/min under a stirring condition, and adding the mixture modifier in a stirring state, wherein the adding amount of the mixture modifier is 3 times of the mass of the solid phase B; and after the addition is finished, continuously stirring for 60 hours at constant temperature, then air-cooling to normal temperature, carrying out solid-liquid separation, washing a solid phase for 2 times by using ethanol, then washing for 2 times by using deionized water, and drying to obtain the modified graphene.
The processing method of the UV anti-sticking film comprises the following steps:
step one, weighing the raw materials of the UV anti-adhesive layer according to the weight parts, and uniformly mixing butyl acetate, acrylic acid, trimethylolpropane triacrylate and hydroxyethyl acrylate to obtain a mixed component I;
dispersing the modified graphene in N-methyl pyrrolidone uniformly to obtain a second mixed component;
and step three, heating the mixed component I to the temperature of 60 +/-2 ℃, preserving heat, stirring (50 r/min), adding the mixed component II under the stirring state, continuing to stir for 30min after the material addition is finished, then adding the photoinitiator, continuing to stir for 20min after the material addition is finished, then coating the mixture on the surface of the substrate, and drying for 3min at the temperature of 120 ℃ to obtain the UV mucosa reducer.
Example 2
The UV anti-adhesive film for semiconductor cutting comprises a PET substrate film and a UV anti-adhesive layer, wherein the raw materials of the UV anti-adhesive layer comprise modified graphene, butyl acetate, acrylic acid, trimethylolpropane triacrylate, hydroxyethyl acrylate, a photoinitiator and N-methylpyrrolidone, and the raw materials of the UV anti-adhesive layer comprise the following components in parts by weight: 4 parts of modified graphene, 54 parts of butyl acetate, 5 parts of acrylic acid, 7 parts of trimethylolpropane triacrylate, 3 parts of hydroxyethyl acrylate, 0.5 part of 1173 photoinitiator and 25 parts of N-methylpyrrolidone.
The preparation method of the modified graphene comprises the following steps:
(1) Uniformly mixing phosphoric acid and triethylamine to form a mixture, wherein the mixing mass ratio of the phosphoric acid to the triethylamine is phosphoric acid: triethylamine =10, keeping the temperature of the mixture constant to 70 ± 5 ℃ in a water bath, preserving the temperature for 3h, and after the preservation is finished, adding graphene oxide into the mixture, wherein the solid-liquid mass ratio of the added graphene oxide in the mixture is solid/liquid = 1; stirring the mixture for 1h at the constant temperature of 70 +/-5 ℃ at the speed of 50r/min, then carrying out solid-liquid separation, washing a solid phase by using ethanol, and drying to obtain a solid phase A;
(2) Preparing an aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid, wherein in the aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid, the concentration of 2-acrylamido 2-methylpropanesulfonic acid is 12g/300mL, and a solvent is water; stirring the solution at 50r/min, adding a solid phase A into the aqueous solution of the 2-acrylamido 2-methylpropanesulfonic acid during stirring, wherein the solid-liquid mass ratio of the solid phase A added into the aqueous solution of the 2-acrylamido 2-methylpropanesulfonic acid is that the solid phase A/the aqueous solution of the 2-acrylamido 2-methylpropanesulfonic acid =1/50; and after the feeding is finished, stirring at 50r/min for 10min, and then adding acrylamide into the solution in a stirring state, wherein the mass ratio of the added acrylamide to the solid phase A is acrylamide: solid phase A =2, stirring is continued for 5min at 50r/min after the addition is completed, then the water bath is kept at a constant temperature of 70 +/-5 ℃, and dibenzoyl peroxide is added to the solution in a stirring state after the constant temperature, and the mass ratio of the added dibenzoyl peroxide to the solid phase A is dibenzoyl peroxide: solid phase a =0.03mg:12g; stirring for 6h at the constant temperature of 70 +/-5 ℃ at 50r/min after the feeding is finished, then stopping stirring, cooling to the normal temperature in air, performing solid-liquid separation, washing a solid phase with deionized water, and drying to obtain a solid phase B;
(3) Mixing succinic anhydride, hydrogen peroxide and water, wherein the mixing mass ratio of the succinic anhydride to the hydrogen peroxide to the water is as follows: hydrogen peroxide: water = 1.2; stirring for 4 hours at the temperature of 8 ℃ at 50r/min to obtain a mixture modifier, dispersing the solid phase B in N, N '-dimethylformamide to form a suspension, wherein the solid-liquid ratio of the solid phase B dispersed in the N, N' -dimethylformamide is =1g/400mL, keeping the suspension at a constant temperature of 80 +/-5 ℃ in a water bath, stirring the suspension at the temperature of 50r/min under a stirring condition, and adding the mixture modifier in a stirring state, wherein the adding amount of the mixture modifier is 3 times of the mass of the solid phase B; and continuously stirring for 60 hours at constant temperature after the addition is finished, then air-cooling to normal temperature, performing solid-liquid separation, washing a solid phase with ethanol for 2 times, then washing with deionized water for 2 times, and drying to obtain the modified graphene.
The processing method of the UV visbreaking film comprises the following steps:
weighing the raw materials of the UV visbreaking glue layer according to the weight parts, and uniformly mixing the butyl acetate, the acrylic acid, the trimethylolpropane triacrylate and the hydroxyethyl acrylate to obtain a mixed component I;
dispersing the modified graphene in N-methyl pyrrolidone uniformly to obtain a second mixed component;
and step three, heating the mixed component I to the temperature of 60 +/-2 ℃, preserving heat, stirring (50 r/min), adding the mixed component II under the stirring state, continuing to stir for 30min after the material addition is finished, then adding the photoinitiator, continuing to stir for 20min after the material addition is finished, then coating the mixture on the surface of the substrate, and drying for 3min at the temperature of 120 ℃ to obtain the UV mucosa reducer.
Example 3
The UV anti-adhesive film for semiconductor cutting comprises a PET substrate film and a UV anti-adhesive layer, wherein the raw materials of the UV anti-adhesive layer comprise modified graphene, butyl acetate, acrylic acid, trimethylolpropane triacrylate, hydroxyethyl acrylate, a photoinitiator and N-methylpyrrolidone, and the raw materials of the UV anti-adhesive layer comprise the following components in parts by weight: 4 parts of modified graphene, 56 parts of butyl acetate, 6 parts of acrylic acid, 8 parts of trimethylolpropane triacrylate, 3 parts of hydroxyethyl acrylate, 0.5 part of 1173 photoinitiator and 25 parts of N-methylpyrrolidone.
The preparation method of the modified graphene comprises the following steps:
(1) Uniformly mixing phosphoric acid and triethylamine to form a mixture, wherein the mixing mass ratio of the phosphoric acid to the triethylamine is phosphoric acid: triethylamine =10, keeping the temperature of the mixture constant to 70 ± 5 ℃ in a water bath, preserving the temperature for 3h, and after the preservation is finished, adding graphene oxide into the mixture, wherein the solid-liquid mass ratio of the graphene oxide added into the mixture is solid/liquid = 1; stirring the mixture for 1h at the constant temperature of 70 +/-5 ℃ at the speed of 50r/min, then carrying out solid-liquid separation, washing a solid phase by using ethanol, and drying to obtain a solid phase A;
(2) Preparing an aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid, wherein in the aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid, the concentration of 2-acrylamido 2-methylpropanesulfonic acid is 13g/300mL, and a solvent is water; stirring the solution at 50r/min, adding a solid phase A into the aqueous solution of the 2-acrylamido 2-methylpropanesulfonic acid during stirring, wherein the solid-liquid mass ratio of the solid phase A added into the aqueous solution of the 2-acrylamido 2-methylpropanesulfonic acid is that the solid phase A/the aqueous solution of the 2-acrylamido 2-methylpropanesulfonic acid =1/50; and after the feeding is finished, stirring at 50r/min for 10min, and then adding acrylamide into the solution in a stirring state, wherein the mass ratio of the added acrylamide to the solid phase A is acrylamide: and (3) solid phase A =3, stirring is continued for 5min at 50r/min after the addition is finished, then the water bath is kept at a constant temperature of 70 +/-5 ℃, and after the constant temperature is reached, dibenzoyl peroxide is added into the solution in a stirring state, wherein the mass ratio of the added dibenzoyl peroxide to the solid phase A is dibenzoyl peroxide: solid phase a =0.03mg:14g of a reaction product; stirring for 6 hours at the constant temperature of 70 +/-5 ℃ at 50r/min after feeding, stopping stirring, cooling in air to normal temperature, performing solid-liquid separation, washing a solid phase with deionized water, and drying to obtain a solid phase B;
(3) Mixing succinic anhydride, hydrogen peroxide and water, wherein the mixing mass ratio of the succinic anhydride to the hydrogen peroxide to the water is as follows: hydrogen peroxide: water = 1.4; stirring for 4 hours at the temperature of 8 ℃ at 50r/min to obtain a mixture modifier, dispersing the solid phase B in N, N '-dimethylformamide to form a suspension, keeping the solid-liquid ratio of the solid phase B dispersed in the N, N' -dimethylformamide =1g/400mL, keeping the temperature of the suspension at 80 +/-5 ℃ in a water bath, stirring the suspension at the temperature of 50r/min under the condition of heat preservation, and adding the mixture modifier under the stirring state, wherein the adding amount of the mixture modifier is 3 times of the mass of the solid phase B; and after the addition is finished, continuously stirring for 60 hours at constant temperature, then air-cooling to normal temperature, carrying out solid-liquid separation, washing a solid phase for 2 times by using ethanol, then washing for 2 times by using deionized water, and drying to obtain the modified graphene.
The processing method of the UV visbreaking film comprises the following steps:
step one, weighing the raw materials of the UV anti-adhesive layer according to the weight parts, and uniformly mixing butyl acetate, acrylic acid, trimethylolpropane triacrylate and hydroxyethyl acrylate to obtain a mixed component I;
dispersing the modified graphene in N-methyl pyrrolidone uniformly to obtain a second mixed component;
and step three, heating the mixed component I to the temperature of 60 +/-2 ℃, preserving heat, stirring (50 r/min), adding the mixed component II under the stirring state, continuing to stir for 30min after the material addition is finished, then adding the photoinitiator, continuing to stir for 20min after the material addition is finished, then coating the mixture on the surface of the matrix, and drying for 3min at the temperature of 120 ℃ to obtain the UV mucosa reduction film.
Example 4
The UV anti-adhesive film for semiconductor cutting comprises a PET (polyethylene terephthalate) substrate film and a UV anti-adhesive layer, wherein the raw materials of the UV anti-adhesive layer comprise modified graphene, butyl acetate, acrylic acid, trimethylolpropane triacrylate, hydroxyethyl acrylate, a photoinitiator and N-methylpyrrolidone, and the raw materials of the UV anti-adhesive layer are as follows in parts by weight: 5 parts of modified graphene, 60 parts of butyl acetate, 7 parts of acrylic acid, 10 parts of trimethylolpropane triacrylate, 4 parts of hydroxyethyl acrylate, 0.6 part of 1173 photoinitiator and 30 parts of N-methylpyrrolidone.
The preparation method of the modified graphene comprises the following steps:
(1) Uniformly mixing phosphoric acid and triethylamine to form a mixture, wherein the mixing mass ratio of the phosphoric acid to the triethylamine is phosphoric acid: triethylamine =10, keeping the temperature of the mixture constant to 70 ± 5 ℃ in a water bath, preserving the temperature for 3h, and after the preservation is finished, adding graphene oxide into the mixture, wherein the solid-liquid mass ratio of the graphene oxide added into the mixture is solid/liquid = 1; stirring the mixture for 1h at the constant temperature of 70 +/-5 ℃ at the speed of 50r/min, then carrying out solid-liquid separation, washing a solid phase by using ethanol, and drying to obtain a solid phase A;
(2) Preparing an aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid, wherein in the aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid, the concentration of 2-acrylamido 2-methylpropanesulfonic acid is 15g/300mL, and a solvent is water; stirring the solution at 50r/min, adding a solid phase A into the aqueous solution of the 2-acrylamido 2-methylpropanesulfonic acid during stirring, wherein the solid-liquid mass ratio of the solid phase A added into the aqueous solution of the 2-acrylamido 2-methylpropanesulfonic acid is that the solid phase A/the aqueous solution of the 2-acrylamido 2-methylpropanesulfonic acid =1/50; and after the addition is finished, stirring at the speed of 50r/min for 10min, and then adding acrylamide into the solution under the stirring state, wherein the mass ratio of the added acrylamide to the solid phase A is acrylamide: solid phase A =3, stirring is continued for 5min at 50r/min after the addition is completed, then the water bath is kept at a constant temperature of 70 +/-5 ℃, and dibenzoyl peroxide is added to the solution in a stirring state after the constant temperature, and the mass ratio of the added dibenzoyl peroxide to the solid phase A is dibenzoyl peroxide: solid phase a =0.03mg:16g of a mixture; stirring for 6h at the constant temperature of 70 +/-5 ℃ at 50r/min after the feeding is finished, then stopping stirring, cooling to the normal temperature in air, performing solid-liquid separation, washing a solid phase with deionized water, and drying to obtain a solid phase B;
(3) Mixing succinic anhydride, hydrogen peroxide and water, wherein the mixing mass ratio of the succinic anhydride to the hydrogen peroxide to the water is as follows: hydrogen peroxide: water = 1.5; stirring for 4 hours at the temperature of 8 ℃ at 50r/min to obtain a mixture modifier, dispersing the solid phase B in N, N '-dimethylformamide to form a suspension, wherein the solid-liquid ratio of the solid phase B dispersed in the N, N' -dimethylformamide is =1g/400mL, keeping the suspension at a constant temperature of 80 +/-5 ℃ in a water bath, stirring the suspension at the temperature of 50r/min under a stirring condition, and adding the mixture modifier in a stirring state, wherein the adding amount of the mixture modifier is 3 times of the mass of the solid phase B; and after the addition is finished, continuously stirring for 60 hours at constant temperature, then air-cooling to normal temperature, carrying out solid-liquid separation, washing a solid phase for 2 times by using ethanol, then washing for 2 times by using deionized water, and drying to obtain the modified graphene.
The processing method of the UV anti-sticking film comprises the following steps:
weighing the raw materials of the UV visbreaking glue layer according to the weight parts, and uniformly mixing the butyl acetate, the acrylic acid, the trimethylolpropane triacrylate and the hydroxyethyl acrylate to obtain a mixed component I;
dispersing the modified graphene in N-methyl pyrrolidone, and uniformly dispersing to obtain a second mixed component;
and step three, heating the mixed component I to the temperature of 60 +/-2 ℃, preserving heat, stirring (50 r/min), adding the mixed component II under the stirring state, continuing to stir for 30min after the material addition is finished, then adding the photoinitiator, continuing to stir for 20min after the material addition is finished, then coating the mixture on the surface of the matrix, and drying for 3min at the temperature of 120 ℃ to obtain the UV mucosa reduction film.
Comparative example 1
The UV anti-sticking film used for comparison comprises a PET substrate film and a UV anti-sticking adhesive layer, wherein the raw materials of the UV anti-sticking adhesive layer comprise graphene oxide, butyl acetate, acrylic acid, trimethylolpropane triacrylate, hydroxyethyl acrylate, a photoinitiator and N-methylpyrrolidone, and the raw materials of the UV anti-sticking adhesive layer are as follows in parts by weight: 4 parts of graphene oxide, 56 parts of butyl acetate, 6 parts of acrylic acid, 8 parts of trimethylolpropane triacrylate, 3 parts of hydroxyethyl acrylate, 0.5 part of 1173 photoinitiator and 25 parts of N-methylpyrrolidone.
The processing method of the UV anti-sticking film comprises the following steps:
step one, weighing the raw materials of the UV anti-adhesive layer according to the weight parts, and uniformly mixing butyl acetate, acrylic acid, trimethylolpropane triacrylate and hydroxyethyl acrylate to obtain a mixed component I;
dispersing the graphene oxide in N-methyl pyrrolidone to be uniformly dispersed to obtain a second mixed component;
and step three, heating the mixed component I to the temperature of 60 +/-2 ℃, preserving heat, stirring (50 r/min), adding the mixed component II under the stirring state, continuing to stir for 30min after the addition is finished, then adding the photoinitiator, continuing to stir for 20min after the addition is finished, then coating the mixture on the surface of the substrate, and drying for 3min at the temperature of 120 ℃ to obtain the UV adhesive reducing film of the comparative example.
Comparative example 2
The UV anti-sticking film used for comparison comprises a PET substrate film and a UV anti-sticking adhesive layer, wherein the raw materials of the UV anti-sticking adhesive layer comprise modified graphene, butyl acetate, acrylic acid, trimethylolpropane triacrylate, hydroxyethyl acrylate, a photoinitiator and N-methylpyrrolidone, and the raw materials of the UV anti-sticking adhesive layer are as follows in parts by weight: 4 parts of modified graphene, 56 parts of butyl acetate, 6 parts of acrylic acid, 8 parts of trimethylolpropane triacrylate, 3 parts of hydroxyethyl acrylate, 0.5 part of 1173 photoinitiator and 25 parts of N-methylpyrrolidone.
The preparation method of the modified graphene comprises the following steps:
(1) Preparing an aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid, wherein in the aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid, the concentration of 2-acrylamido 2-methylpropanesulfonic acid is 13g/300mL, and a solvent is water; stirring the solution at 50r/min, adding graphene oxide into the aqueous solution of the 2-acrylamide-based 2-methylpropanesulfonic acid during stirring, wherein the solid-liquid mass ratio of the graphene oxide added into the aqueous solution of the 2-acrylamide-based 2-methylpropanesulfonic acid is that the aqueous solution of graphene oxide/2-acrylamide-based 2-methylpropanesulfonic acid =1/50; and after the feeding is finished, continuing stirring for 10min at a speed of 50r/min, and then adding acrylamide into the solution under a stirring state, wherein the mass ratio of the added acrylamide to the graphene oxide is acrylamide: 1, graphene oxide =3, stirring for 5min at 50r/min after the completion of the addition, then keeping the temperature of the water bath constant to 70 ± 5 ℃, and adding dibenzoyl peroxide into the solution in a stirring state after keeping the temperature, wherein the mass ratio of the added dibenzoyl peroxide to the mass of the graphene oxide is dibenzoyl peroxide: graphene oxide =0.03mg:14g of a mixture; stirring for 6h at the constant temperature of 50r/min at 70 +/-5 ℃ after the feeding is finished, then stopping stirring, cooling to the normal temperature in air, performing solid-liquid separation, washing a solid phase with deionized water, and drying to obtain a solid phase B in the comparative example;
(2) Mixing succinic anhydride, hydrogen peroxide and water, wherein the mixing mass ratio of the succinic anhydride to the hydrogen peroxide to the water is as follows: hydrogen peroxide: water =1.4, 1.0, the mass fraction of solute in the hydrogen peroxide being 30%; stirring for 4 hours at the temperature of 8 ℃ at 50r/min to obtain a mixture modifier, dispersing the solid phase B in N, N '-dimethylformamide to form a suspension, keeping the solid-liquid ratio of the solid phase B dispersed in the N, N' -dimethylformamide =1g/400mL, keeping the temperature of the suspension at 80 +/-5 ℃ in a water bath, stirring the suspension at the temperature of 50r/min under the condition of heat preservation, and adding the mixture modifier under the stirring state, wherein the adding amount of the mixture modifier is 3 times of the mass of the solid phase B; and (3) continuously stirring for 60h at constant temperature after the addition is finished, then carrying out air cooling to normal temperature, carrying out solid-liquid separation, washing a solid phase for 2 times by using ethanol, then washing for 2 times by using deionized water, and drying to obtain the modified graphene in the comparative example.
The processing method of the UV visbreaking film comprises the following steps:
step one, weighing the raw materials of the UV anti-adhesive layer according to the weight parts, and uniformly mixing butyl acetate, acrylic acid, trimethylolpropane triacrylate and hydroxyethyl acrylate to obtain a mixed component I;
dispersing the modified graphene in N-methyl pyrrolidone uniformly to obtain a second mixed component;
and step three, heating the mixed component I to the temperature of 60 +/-2 ℃, preserving heat, stirring (50 r/min), adding the mixed component II under the stirring state, continuing to stir for 30min after the addition is finished, then adding the photoinitiator, continuing to stir for 20min after the addition is finished, then coating the mixture on the surface of the substrate, and drying for 3min at the temperature of 120 ℃ to obtain the UV mucosa reduction film of the comparative example.
Comparative example 3
The UV anti-sticking film used for comparison comprises a PET substrate film and a UV anti-sticking adhesive layer, wherein the raw materials of the UV anti-sticking adhesive layer comprise modified graphene, butyl acetate, acrylic acid, trimethylolpropane triacrylate, hydroxyethyl acrylate, a photoinitiator and N-methylpyrrolidone, and the raw materials of the UV anti-sticking adhesive layer are as follows in parts by weight: 4 parts of modified graphene, 56 parts of butyl acetate, 6 parts of acrylic acid, 8 parts of trimethylolpropane triacrylate, 3 parts of hydroxyethyl acrylate, 0.5 part of 1173 photoinitiator and 25 parts of N-methylpyrrolidone.
The preparation method of the modified graphene comprises the following steps:
(1) Uniformly mixing phosphoric acid and triethylamine to form a mixture, wherein the mixing mass ratio of the phosphoric acid to the triethylamine is phosphoric acid: triethylamine =10, keeping the temperature of the mixture constant to 70 ± 5 ℃ in a water bath, preserving the temperature for 3h, and after the preservation is finished, adding graphene oxide into the mixture, wherein the solid-liquid mass ratio of the graphene oxide added into the mixture is solid/liquid = 1; stirring the mixture for 1h at the constant temperature of 70 +/-5 ℃ at the speed of 50r/min, then carrying out solid-liquid separation, washing a solid phase by using ethanol, and drying to obtain a solid phase A;
(2) Mixing succinic anhydride, hydrogen peroxide and water, wherein the mixing mass ratio of the succinic anhydride to the hydrogen peroxide to the water is that: hydrogen peroxide: water =1.4, 1.0, the mass fraction of solute in the hydrogen peroxide being 30%; stirring for 4 hours at the temperature of 8 ℃ at 50r/min to obtain a mixture modifier, dispersing the solid phase A in N, N '-dimethylformamide to form a suspension, keeping the solid-liquid ratio of the solid phase A dispersed in the N, N' -dimethylformamide =1g/400mL, keeping the temperature of the suspension at 80 +/-5 ℃ in a water bath, stirring the suspension at the temperature of 50r/min under the condition of heat preservation, and adding the mixture modifier under the stirring state, wherein the adding amount of the mixture modifier is 3 times of the mass of the solid phase A; and continuously stirring for 60 hours at constant temperature after the addition is finished, then air-cooling to normal temperature, performing solid-liquid separation, washing a solid phase with ethanol for 2 times, then washing with deionized water for 2 times, and drying to obtain the modified graphene of the comparative example.
The processing method of the UV visbreaking film comprises the following steps:
step one, weighing the raw materials of the UV anti-adhesive layer according to the weight parts, and uniformly mixing butyl acetate, acrylic acid, trimethylolpropane triacrylate and hydroxyethyl acrylate to obtain a mixed component I;
dispersing the modified graphene in N-methyl pyrrolidone uniformly to obtain a second mixed component;
and step three, heating the mixed component I to the temperature of 60 +/-2 ℃, preserving heat, stirring (50 r/min), adding the mixed component II under the stirring state, continuing to stir for 30min after the addition is finished, then adding the photoinitiator, continuing to stir for 20min after the addition is finished, then coating the mixture on the surface of the substrate, and drying for 3min at the temperature of 120 ℃ to obtain the UV mucosa reduction film of the comparative example.
Comparative example 4
The UV anti-sticking film used for comparison comprises a PET substrate film and a UV anti-sticking adhesive layer, wherein the raw materials of the UV anti-sticking adhesive layer comprise modified graphene, butyl acetate, acrylic acid, trimethylolpropane triacrylate, hydroxyethyl acrylate, a photoinitiator and N-methylpyrrolidone, and the raw materials of the UV anti-sticking adhesive layer are as follows in parts by weight: 4 parts of modified graphene, 56 parts of butyl acetate, 6 parts of acrylic acid, 8 parts of trimethylolpropane triacrylate, 3 parts of hydroxyethyl acrylate, 0.5 part of 1173 photoinitiator and 25 parts of N-methylpyrrolidone.
The preparation method of the modified graphene comprises the following steps:
(1) Uniformly mixing phosphoric acid and triethylamine to form a mixture, wherein the mixing mass ratio of the phosphoric acid to the triethylamine is phosphoric acid: triethylamine =10, keeping the temperature of the mixture constant to 70 ± 5 ℃ in a water bath, preserving the temperature for 3h, and after the heat preservation is finished, adding graphene oxide into the mixture, wherein the solid-liquid mass ratio of the added graphene oxide in the mixture is solid/liquid = 1; stirring the mixture for 1h at the constant temperature of 70 +/-5 ℃ at the speed of 50r/min, then carrying out solid-liquid separation, washing a solid phase by using ethanol, and drying to obtain a solid phase A;
(2) Preparing an aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid, wherein in the aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid, the concentration of 2-acrylamido 2-methylpropanesulfonic acid is 13g/300mL, and a solvent is water; stirring the solution at 50r/min, adding a solid phase A into the aqueous solution of the 2-acrylamido 2-methylpropanesulfonic acid during stirring, wherein the solid-liquid mass ratio of the solid phase A added into the aqueous solution of the 2-acrylamido 2-methylpropanesulfonic acid is that the solid phase A/the aqueous solution of the 2-acrylamido 2-methylpropanesulfonic acid =1/50; and after the addition is finished, stirring at the speed of 50r/min for 10min, and then adding acrylamide into the solution under the stirring state, wherein the mass ratio of the added acrylamide to the solid phase A is acrylamide: and (3) solid phase A =3, stirring is continued for 5min at 50r/min after the addition is finished, then the water bath is kept at a constant temperature of 70 +/-5 ℃, and after the constant temperature is reached, dibenzoyl peroxide is added into the solution in a stirring state, wherein the mass ratio of the added dibenzoyl peroxide to the solid phase A is dibenzoyl peroxide: solid phase a =0.03mg:14g of a mixture; and after the addition is finished, stirring for 6 hours at the constant temperature of 70 +/-5 ℃ and 50r/min, then stopping stirring, cooling to the normal temperature in air, performing solid-liquid separation, washing a solid phase by using deionized water, and drying to obtain a solid phase B which is used as the modified graphene in the comparative example.
The processing method of the UV visbreaking film comprises the following steps:
weighing the raw materials of the UV visbreaking glue layer according to the weight parts, and uniformly mixing the butyl acetate, the acrylic acid, the trimethylolpropane triacrylate and the hydroxyethyl acrylate to obtain a mixed component I;
dispersing the modified graphene in N-methyl pyrrolidone, and uniformly dispersing to obtain a second mixed component;
and step three, heating the mixed component I to the temperature of 60 +/-2 ℃, preserving heat, stirring (50 r/min), adding the mixed component II under the stirring state, continuing to stir for 30min after the addition is finished, then adding the photoinitiator, continuing to stir for 20min after the addition is finished, then coating the mixture on the surface of the substrate, and drying for 3min at the temperature of 120 ℃ to obtain the UV adhesive reducing film of the comparative example.
Example 5
The UV release films prepared in the above examples and comparative examples (the coating thickness of the UV release adhesive layer was 50 μm) were tested for 180 DEG peel strength (before UV curing at 370nm and after UV curing) as required by the national standard GB/T2792-2014 test method for peel strength of adhesive tape), and the results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the UV visbreaking adhesive layer has good bonding strength before UV curing, the 180-degree peel strength can reach 24.8N/25mm, the visbreaking effect is obvious after UV curing, the 180-degree peel strength is reduced to 0.31N/25mm, and no residual adhesive exists on the surface separated from an object after visbreaking. Comparing example 3 with each comparative example, it can be seen that, compared with the case that unmodified graphene oxide is added into a UV viscosity-reducing adhesive layer, the graphene oxide subjected to modification treatment can not only improve the adhesive strength of the adhesive layer before curing, but also has higher viscosity-reducing degree after curing and better use effect.
While the technical solutions provided by the present invention have been described in detail, for a person skilled in the art, according to the ideas of the embodiments of the present invention, the specific implementation manners and the application ranges may be changed, and as described above, the contents of the present description should not be construed as limiting the present invention.
Claims (1)
1. The UV anti-adhesive film for semiconductor cutting comprises a substrate and a UV anti-adhesive layer, and is characterized in that the raw materials of the UV anti-adhesive layer comprise modified graphene, butyl acetate, acrylic acid, trimethylolpropane triacrylate, hydroxyethyl acrylate, a photoinitiator and N-methylpyrrolidone, and the preparation method of the modified graphene comprises the following steps:
(1) Uniformly mixing phosphoric acid and triethylamine to form a mixture, carrying out water bath on the mixture at a constant temperature of 70 +/-5 ℃, carrying out heat preservation for 3-4 h, adding graphene oxide into the mixture after the heat preservation is finished, stirring the mixture at a constant temperature of 70 +/-5 ℃ for 1-2 h, then carrying out solid-liquid separation, washing a solid phase with ethanol, and drying to obtain a solid phase A;
(2) Preparing an aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid, stirring the solution, adding a solid phase A into the aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid in the stirring process, continuously stirring for 10-20 min after the feeding is finished, then adding acrylamide into the solution in the stirring state, continuously stirring for 5-8 min after the feeding is finished, then carrying out water bath at constant temperature of 70 +/-5 ℃, adding dibenzoyl peroxide into the solution in the stirring state after the constant temperature is kept, stirring for 5-7 h at constant temperature of 70 +/-5 ℃ after the feeding is finished, then stopping stirring, carrying out air cooling to normal temperature, carrying out solid-liquid separation, washing the solid phase with deionized water, and drying to obtain a solid phase B;
(3) Mixing succinic anhydride, hydrogen peroxide and water, stirring for more than 4 hours at the temperature of 8-10 ℃ to obtain a mixture modifier, dispersing the solid phase B in N, N' -dimethylformamide to form turbid liquid, carrying out water bath to keep the temperature of the turbid liquid at constant temperature to 80 +/-5 ℃, then stirring the turbid liquid under the heat preservation condition, adding the mixture modifier in the stirring state, continuously stirring for more than 60 hours at constant temperature after finishing adding, then carrying out air cooling to normal temperature, carrying out solid-liquid separation, washing the solid phase with ethanol for 2 times, then washing with deionized water for 2 times, and drying to obtain the modified graphene.
Further, the UV visbreaking adhesive layer comprises the following raw materials in parts by weight: 3-5 parts of modified graphene, 50-60 parts of butyl acetate, 4-7 parts of acrylic acid, 5-10 parts of trimethylolpropane triacrylate, 2-4 parts of hydroxyethyl acrylate, 0.4-0.6 part of a photoinitiator and 20-30 parts of N-methylpyrrolidone.
Further, in the step (1), the phosphoric acid and the triethylamine are uniformly mixed to form a mixture, wherein the mixing mass ratio of the phosphoric acid to the triethylamine is phosphoric acid: triethylamine =10, and the solid-liquid mass ratio of graphene oxide added to the mixture is solid/liquid =1.
Further, in the step (2), in the aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid, the concentration of 2-acrylamido 2-methylpropanesulfonic acid is 10 to 15g/300mL, and the solid-liquid mass ratio of the solid phase a to the aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid added to the aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid is solid phase a/aqueous solution of 2-acrylamido 2-methylpropanesulfonic acid =1/50; the mass ratio of the added mass of the acrylamide to the solid phase A is acrylamide: the solid phase A = 2-3, the mass ratio of the added dibenzoyl peroxide to the solid phase A is dibenzoyl peroxide: solid phase a =0.03mg:10 to 16g.
Further, in the step (3), the mixing mass ratio of the succinic anhydride to the hydrogen peroxide to the water is succinic anhydride: hydrogen peroxide: water = 1.0-1.5; the mass fraction of solute in the hydrogen peroxide is 30 percent; the solid phase B is dispersed in N, N '-dimethylformamide to form a solid-liquid ratio of solid phase B/N, N' -dimethylformamide = 1-2 g/400mL, and the addition amount of the mixture modifier is 3-4 times of the mass of the solid phase B.
The invention also discloses a processing method of the UV anti-sticking film, which comprises the following steps:
weighing the raw materials of the UV visbreaking glue layer according to the weight parts, and uniformly mixing the butyl acetate, the acrylic acid, the trimethylolpropane triacrylate and the hydroxyethyl acrylate to obtain a mixed component I;
dispersing the modified graphene in N-methyl pyrrolidone, and uniformly dispersing to obtain a second mixed component;
and step three, heating the mixed component I to the temperature of 60 +/-2 ℃, preserving heat, stirring, adding the mixed component II under a stirring state, continuously stirring for 20-30 min after the material addition is finished, then adding the photoinitiator, continuously stirring for 10-20 min after the material addition is finished, then coating the mixture on the surface of the substrate, and drying for 2-3 min at the temperature of 120 ℃ to obtain the UV mucosa reduction film.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116904127A (en) * | 2023-07-04 | 2023-10-20 | 江苏特丽亮新材料科技有限公司 | Double-sided high-temperature-resistant UV (ultraviolet) mucous membrane reducing and preparation method thereof |
| CN116904127B (en) * | 2023-07-04 | 2024-06-04 | 江苏特丽亮新材料科技有限公司 | Double-sided high-temperature-resistant UV (ultraviolet) mucous membrane reducing and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112680131A (en) * | 2020-11-25 | 2021-04-20 | 苏州赛伍应用技术股份有限公司 | PVC (polyvinyl chloride) substrate UV (ultraviolet) viscosity-reducing adhesive film for semiconductor chip film inversion and preparation method thereof |
| CN114058289A (en) * | 2020-08-07 | 2022-02-18 | 宁波安特弗新材料科技有限公司 | UV visbreaking adhesive and UV visbreaking adhesive tape |
| CN114672276A (en) * | 2022-04-26 | 2022-06-28 | 河北科技大学 | UV photo-induced strippable adhesive and preparation method thereof |
-
2022
- 2022-10-13 CN CN202211251014.1A patent/CN115678446A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114058289A (en) * | 2020-08-07 | 2022-02-18 | 宁波安特弗新材料科技有限公司 | UV visbreaking adhesive and UV visbreaking adhesive tape |
| CN112680131A (en) * | 2020-11-25 | 2021-04-20 | 苏州赛伍应用技术股份有限公司 | PVC (polyvinyl chloride) substrate UV (ultraviolet) viscosity-reducing adhesive film for semiconductor chip film inversion and preparation method thereof |
| CN114672276A (en) * | 2022-04-26 | 2022-06-28 | 河北科技大学 | UV photo-induced strippable adhesive and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 代汝泉: "《汽车车身修复技术》", vol. 1, 30 April 1999, 人民交通出版, pages: 123 - 124 * |
| 李肇强: "《现代涂料的生产及应用》", vol. 2, 31 March 2017, 上海科学技术文献出版社, pages: 65 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116904127A (en) * | 2023-07-04 | 2023-10-20 | 江苏特丽亮新材料科技有限公司 | Double-sided high-temperature-resistant UV (ultraviolet) mucous membrane reducing and preparation method thereof |
| CN116904127B (en) * | 2023-07-04 | 2024-06-04 | 江苏特丽亮新材料科技有限公司 | Double-sided high-temperature-resistant UV (ultraviolet) mucous membrane reducing and preparation method thereof |
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