WO2013021945A1 - Composition adhésive pour une fixation temporaire - Google Patents

Composition adhésive pour une fixation temporaire Download PDF

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Publication number
WO2013021945A1
WO2013021945A1 PCT/JP2012/069851 JP2012069851W WO2013021945A1 WO 2013021945 A1 WO2013021945 A1 WO 2013021945A1 JP 2012069851 W JP2012069851 W JP 2012069851W WO 2013021945 A1 WO2013021945 A1 WO 2013021945A1
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Prior art keywords
component
adhesive composition
meth
temporary fixing
acrylate
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PCT/JP2012/069851
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English (en)
Japanese (ja)
Inventor
剛介 中島
朋之 金井
公彦 依田
大島　和宏
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Denka Co Ltd
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Denki Kagaku Kogyo KK
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Priority to JP2013528010A priority Critical patent/JP6016793B2/ja
Publication of WO2013021945A1 publication Critical patent/WO2013021945A1/fr
Anticipated expiration legal-status Critical
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16

Definitions

  • the present invention relates to a method for temporarily fixing members when various members are processed, and to a composition and an adhesive suitable for the method.
  • the present invention relates to, for example, a method for temporarily fixing a member when a silicon wafer is processed from a silicon block, and an acrylic temporary fixing adhesive composition suitable for the application.
  • Double-sided tapes, hot melt adhesives, and epoxy adhesives are used as temporary fixing adhesives for semiconductor mounting parts such as silicon wafers.
  • a member joined or laminated with these adhesives is cut into a predetermined shape, and then the adhesive is removed to produce a processed member.
  • these components are fixed to a substrate with double-sided tape, then the desired components are cut, and further, the double-sided tape is irradiated with ultraviolet rays to be peeled off from the components. .
  • a hot-melt adhesive the members are joined, and the adhesive is infiltrated into the gap by heating, and then a desired part is cut and the adhesive is peeled off in an organic solvent.
  • an epoxy adhesive the base agent and the curing agent are weighed and mixed, joined to the member, and then a desired part is cut and the adhesive is peeled off in an organic solvent.
  • the double-sided tape has a problem that it is difficult to obtain a thickness accuracy, or the adhesive strength is weak, so that the double-sided tape cannot be peeled off during processing of the component.
  • the double-sided tape has a problem that it cannot be peeled off unless heat of 100 ° C. or higher is applied.
  • the double-sided tape has a problem that it cannot be peeled off if the adherend has poor permeability.
  • Hot melt adhesive cannot be applied unless heat of 100 ° C. or higher is applied during bonding, and there are restrictions on the members that can be used. Hot-melt adhesives require the use of an organic solvent at the time of peeling, and the washing process of an alkaline solvent or a halogen-based organic solvent is complicated, which has been a problem in terms of the working environment.
  • Epoxy adhesives may cause a significant decrease in adhesion when the metering and mixing of the main agent and curing agent is insufficient. As with the hot-melt adhesive, the epoxy adhesive needs to use an organic solvent at the time of peeling. Epoxy adhesives have a complicated cleaning process for alkali solvents and halogen-based organic solvents, and have been problematic in terms of work environment. Epoxy adhesives have a slow curing speed and need to maintain a sufficient curing time until curing.
  • Patent Documents 1 to 3 have proposed a photocurable or heat curable adhesive for temporary fixing containing a water-soluble compound such as a water-soluble vinyl monomer.
  • a water-soluble compound such as a water-soluble vinyl monomer.
  • the peelability in water is solved, but the adhesive strength at the time of fixing the component is low, and there is a problem that the dimensional accuracy of the member at the time of cutting is poor.
  • the use is limited to a permeable adherend, and in the case of a thermosetting adhesive, the use is limited to a heat-resistant adherend.
  • JP-A-6-116534 JP-A-11-71553 Japanese Patent Laid-Open No. 2001-226641 JP 2010-248395 A International Publication No. WO2008 / 018252 Japanese Patent Laid-Open No. 7-153724 Japanese Patent Laid-Open No. 11-60400
  • Patent Document 4 A two-component acrylic adhesive having excellent environmental and workability has been proposed (Patent Document 4).
  • Patent Document 4 there is no description that no chipping occurs in the processed wafer even if the processing conditions are not particularly limited. If the chipping of the wafer is large, the wafer may be damaged from that point.
  • Patent Document 5 describes an adhesive composition containing spherical silica as a particulate material, but the amount used is 20 parts by mass or less, and the amount used is different from that of the present application.
  • the present inventor has obtained the knowledge that the chipping of the processed wafer can be reduced by filling the adhesive with an inorganic filler, thereby completing the present invention. It has come to be.
  • the present invention 1. Contains 100 parts by weight of monomer and / or oligomer having (meth) acryloyl group, (2) polymerization initiator, (3) ⁇ -diketone chelate and / or ⁇ -ketoester, (4) 25 to 300 parts by weight of inorganic filler An adhesive composition for temporary fixing. 2. Furthermore, (5) The adhesive composition for temporary fixing according to item 1 comprising an elastomer component. 3. (4) The adhesive composition for temporary fixing according to Item 1 or 2, wherein the inorganic filler is one or more members selected from the group consisting of silica, quartz, alumina, and talc. 4).
  • a monomer and / or oligomer having a (meth) acryloyl group is (1-2) a (meth) acrylic acid monomer having a bisphenol skeleton, (1-4) a (meth) acrylate having an aromatic group and (1 -5)
  • the total content of component (1-2), component (1-4) and component (1-5) is 100 parts by mass of component (1-2), component (1-4) and component (1-5)
  • the temporary fixing adhesive according to item 4, wherein the component (1-2): component (1-4): component (1-5) 1 to 20:20 to 60:30 to 70 in terms of mass ratio Agent composition. 6).
  • a monomer and / or oligomer having a (meth) acryloyl group is (1-1) an alkyl (meth) acrylate, (1-2) a (meth) acrylic acid monomer having a bisphenol skeleton, (1-4) aroma Item 4.
  • the temporary fixing adhesive composition according to any one of Items 1 to 3, comprising (meth) acrylate having a group and (1-5) hydroxyalkyl (meth) acrylate. 7).
  • the temporary fixing adhesive composition according to any one of items 1 to 8 is divided into a first agent and a second agent, wherein the first agent contains at least component (2), A two-component temporary fixing adhesive composition comprising at least the component (3). 10.
  • Item 13 The temporary fixing adhesive composition according to any one of items 1 to 12, wherein the use is one or more of the group consisting of silicon cutting, sapphire cutting, glass cutting and resin cutting object.
  • a temporary fixing adhesive composition according to any one of Items 1 to 13 is used to adhesively fix a member, cure the temporary fixing adhesive composition, and fix the temporarily fixed member.
  • a method for temporarily fixing a member, wherein the cured member of the adhesive composition for temporary fixing is removed by immersing the processed member in water.
  • 15. The method for temporarily fixing a member according to item 14, wherein the water is warm water. 16.
  • a silicon block is bonded and temporarily fixed to a base material using the temporary fixing adhesive composition according to any one of items 1 to 13, and then the silicon block is cut to produce a silicon wafer.
  • a method for producing a silicon wafer wherein the silicon wafer is removed from the substrate by immersing the substrate in water. 17. 17. The method for temporarily fixing a member according to item 16, wherein the water is hot water. 18. 14. A joined body obtained by adhering an adherend using the temporary fixing adhesive composition according to any one of items 1 to 13. 19. Item 19. The joined body according to Item 18, wherein the adherend is one or more members selected from the group consisting of silicon, sapphire, resin, and glass.
  • the present invention has the following effects, for example.
  • the temporary fixing adhesive composition of the present invention can increase hardness by containing an inorganic filler, thereby suppressing chipping of the processed member.
  • Examples of the monomer and / or oligomer having (1) (meth) acryloyl group used in the present invention include the following.
  • Alkyl (meth) acrylate examples include (meth) acrylic monomers represented by the general formula (A).
  • Formula (A) Z—O—R 1 (In the formula, Z represents a (meth) acryloyl group, and R 1 represents an alkyl group having 1 to 20 carbon atoms.)
  • R 1 is preferably an alkyl group having 1 to 20 carbon atoms, and more preferably an alkyl group having 6 to 12 carbon atoms. When the number of carbon atoms exceeds 20, the surface curability is lowered and stickiness is observed, and the curing rate may be lowered.
  • alkyl (meth) acrylates include methyl (meth) acrylate, ethyl (meth) acrylate, n-propyl (meth) acrylate, isopropyl (meth) acrylate, butyl (meth) acrylate, and 2-ethylhexyl (meth) acrylate.
  • 2-ethylhexyl (meth) acrylate is preferable from the viewpoint of good adhesiveness.
  • (1-2) (Meth) acrylic acid monomer having bisphenol skeleton examples include a (meth) acrylic monomer represented by the general formula (B).
  • Such (meth) acrylic monomers include 2,2-bis (4- (meth) acryloxyphenyl) propane, 2,2-bis (4- (meth) acryloxyethoxyphenyl) propane, 2,2 -Bis (4- (meth) acryloxydiethoxyphenyl) propane, 2,2-bis (4- (meth) acryloxytetraethoxyphenyl) propane, 2,2-bis (4- (meth) acryloxypolyethoxy) Phenyl) propane, 2,2-bis (4- (meth) acryloxypropoxyphenyl) propane, and the like, and one or more of these can be used.
  • 2,2-bis (4- (meth) acryloxypolyethoxyphenyl) propane is preferable because of its great effect.
  • dicyclopentenyloxyalkyl (meth) acrylate examples include (meth) acrylic monomers represented by the general formula (C).
  • Z represents a (meth) acryloyl group
  • R 4 represents an alkylene group having 1 to 12 carbons
  • q represents an integer of 1 to 20).
  • Such (meth) acrylic monomers include dicyclopentenyloxyethyl (meth) acrylate, dicyclopentenyloxydiethylene glycol (meth) acrylate, dicyclopentenyloxytriethylene glycol (meth) acrylate and dicyclopentenyloxypropylene glycol.
  • (Meth) acrylate etc. are mentioned, These 1 type (s) or 2 or more types can be used. Among these, dicyclopentenyloxyethyl (meth) acrylate is preferable because it has good surface curability and can be easily obtained.
  • R 4 is preferably an alkylene group having 1 to 4 carbon atoms, more preferably an ethylene group, from the viewpoint of high resin strength.
  • q is preferably 1 to 3 and more preferably 1 in terms of the resin strength of the cured product.
  • (1-4) (Meth) acrylates having an aromatic group examples include (meth) acrylic monomers represented by the general formula (D).
  • Formula (D) Z—O— (R 5 O) r —R 6 (Wherein Z represents a (meth) acryloyl group, R 5 represents —C 2 H 4 —, —C 3 H 6 —, —CH 2 CH (CH 3 ) —, —C 4 H 8 — or —C 6 H 12 —, R 6 represents a phenyl group or a phenyl group having an alkyl group having 1 to 3 carbon atoms, and r represents an integer of 1 to 10)
  • Such (meth) acrylic monomers include phenoxyethyl (meth) acrylate, phenoxydiethylene glycol (meth) acrylate, phenoxypolyethylene glycol (meth) acrylate, phenoxypropyl (meth) acrylate, phenoxydipropylene glycol (meth) acrylate and Phenoxy polypropylene glycol (meth) acrylate etc. are mentioned, These 1 type (s) or 2 or more types can be used. Among these, phenoxyethyl (meth) acrylate is preferable because of its great effect.
  • Formula (E) Z—O— (R 7 O) s —H (Wherein Z represents a (meth) acryloyl group, R 7 represents —C 2 H 4 —, —C 3 H 6 —, —CH 2 CH (CH 3 ) —, —C 4 H 8 — or —C 6 H 12- represents, and s represents an integer of 1 to 10.)
  • Examples of such (meth) acrylic monomers include hydroxyalkyl (meth) acrylates such as 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, and hydroxybutyl (meth) acrylate. 1 type (s) or 2 or more types can be used. Among these, 2-hydroxyethyl (meth) acrylate and / or 2-hydroxypropyl (meth) acrylate are preferable because they are inexpensive and have good adhesiveness.
  • (meth) acrylic acid ester of polyhydric alcohol examples include 1,4-butanediol di (meth) acrylate, 1,6-hexanediol di (meth) Acrylate, 1,9-nonanediol di (meth) acrylate, tripropylene glycol di (meth) acrylate and the like. Among these, 1,9-nonanediol di (meth) acrylate and / or tripropylene glycol di (meth) acrylate is preferable in terms of low skin irritation.
  • oligomer having (meth) acryloyl group for example, 1,2-polybutadiene-terminated urethane (meth) acrylate (for example, “TE-2000” manufactured by Nippon Soda Co., Ltd.) , “TEA-1000”), hydrogenated products thereof (for example, “TEAI-1000” manufactured by Nippon Soda Co., Ltd.), 1,4-polybutadiene-terminated urethane (meth) acrylate (for example, “BAC-” manufactured by Osaka Organic Chemical Co., Ltd.) 45 "), polyisoprene-terminated (meth) acrylate, polyester urethane (meth) acrylate (for example," UV-3000B "manufactured by Nippon Gosei Co., Ltd.), polyether urethane (meth) acrylate, polyester (meth) acrylate, bisphenol Type A epoxy (me
  • the (meth) acrylic monomers it is preferable to contain (1-5) a (meth) acrylic monomer having a hydroxyl group in terms of great effect.
  • the content ratio of the (meth) acrylic monomer having (1-5) hydroxyl group in the (meth) acrylic monomer is preferably 5 to 70 parts by mass in 100 parts by mass of the (meth) acrylic monomer. 60 parts by mass is more preferable.
  • (X) (1-2) A combination of a (meth) acrylic acid monomer having a bisphenol skeleton, (1-4) a (meth) acrylate having an aromatic group, and (1-5) a hydroxyalkyl (meth) acrylate.
  • the content ratio of the component (1-2), the component (1-4) and the component (1-5) is 100 parts by mass in total of the component (1-2), the component (1-4) and the component (1-5).
  • the component (1-2): component (1-4): component (1-5) is preferably 1 to 20:20 to 60:30 to 70 in terms of mass ratio, and 5 to 15:30 to 55:35. ⁇ 60 is more preferred.
  • Polymerization initiators used in the present invention include cumene hydroperoxide, paramentane hydroperoxide, tertiary butyl hydroperoxide, diisopropylbenzene dihydroperoxide, methyl ethyl ketone peroxide, benzoyl peroxide and tertiary butyl.
  • Organic peroxides such as peroxybenzoate are preferred, and one or more of these can be used.
  • cumene hydroperoxide is preferable in terms of reactivity with the component (1) and the component (3).
  • the amount of the component (2) used in the present invention is not particularly limited, but is preferably 0.5 to 10 parts by mass, preferably 1 to 7 parts by mass with respect to 100 parts by mass of the component (1). . If the amount of component (2) used is too small, the curing rate may be slow, while if too large, the storage stability may be slow.
  • Examples of (3) ⁇ -diketone chelate and / or ⁇ -ketoester used in the present invention include ⁇ -diketone chelate and / or ⁇ -ketoester.
  • Examples of ⁇ -diketone chelates include vanadyl acetylacetonate, cobalt acetylacetonate, and copper acetylacetonate.
  • Examples of the ⁇ -ketoester include vanadyl naphthenate, vanadyl stearate, copper naphthenate, cobalt octylate and the like, and one or more of these can be used.
  • a metal salt having a reducing property is preferable, and one or two of the group consisting of vanadium acetylacetonate, copper naphthenate, and cobalt octylate are used.
  • the above is more preferable, and vanadyl acetylacetonate is most preferable.
  • the amount of the component (3) used is not particularly limited, but is preferably 0.05 to 5 parts by mass, more preferably 0.1 to 2 parts by mass with respect to 100 parts by mass of the component (1). If the amount of the component (3) used is too small, the curing rate may be slow and the adhesiveness may be small. On the other hand, if too large, the unreacted component may remain and the adhesiveness may deteriorate.
  • fused silica is preferable.
  • alumina is preferable, and spherical alumina is more preferable.
  • one or more members selected from the group consisting of silica, quartz, alumina, and talc are preferable, in that heat dissipation can be imparted.
  • One or two of quartz and alumina are more preferable.
  • Component (4) is preferably used in an amount of 25 to 300 parts by weight, more preferably 50 to 200 parts by weight, per 100 parts by weight of component (1). If the amount of the component (4) used is too small, the effect of increasing the hardness may be difficult to obtain. On the other hand, if the amount is too large, the viscosity is too high, causing problems in operation, and reducing the peelability in water. There is a case to do.
  • the average particle diameter of the component (4) by the laser diffraction / scattering method is preferably 1 to 100 ⁇ m, and more preferably 3 to 20 ⁇ m. If the average particle size is too small, the amount of increase in viscosity becomes large and it is difficult to fill with high viscosity. On the other hand, if it is too large, the inorganic filler may precipitate.
  • the particle size distribution is measured by a laser diffraction type particle size distribution measuring apparatus (laser diffraction / scattering method).
  • an elastomer component in order to improve the peel strength and impact strength.
  • the (5) elastomer component used in the present invention includes acrylonitrile-butadiene-methacrylic acid copolymer, acrylonitrile-butadiene-methacrylate copolymer, methyl methacrylate-butadiene-styrene copolymer, acrylonitrile-styrene-butadiene copolymer.
  • thermoplastic elastomers such as polyester-polytetramethylene glycol multiblock polymer, polyamide-based thermoplastic elastomers such as nylon-polyol block copolymer, 1,2-polybutadiene-based thermoplastic elastomers, and vinyl-based thermoplastic elastomers. It is done.
  • These elastomer components can be used alone or
  • polybutadiene having a terminal methacrylic modification can also be used.
  • methyl methacrylate-butadiene-styrene copolymer and / or acrylonitrile-butadiene rubber are preferable, and their combined use is more preferable from the viewpoint of solubility and adhesion to (meth) acrylic monomers.
  • the acrylonitrile content is preferably 36 to 45% by mass.
  • the amount of component (5) used is preferably 5 to 35 parts by weight, more preferably 10 to 30 parts by weight, per 100 parts by weight of component (1). If the amount of the component (5) used is too small, the viscosity and the adhesiveness may be lowered. On the other hand, if it is too much, the viscosity may be too high and problems may occur in work.
  • paraffins can be used in order to quickly cure the portion in contact with air.
  • paraffins include paraffin wax, microcrystalline wax, carnauba wax, beeswax, lanolin, whale wax, ceresin and candelilla wax. These 1 type (s) or 2 or more types can be used.
  • the amount of paraffins used is preferably 0.1 to 5 parts by mass and more preferably 0.3 to 2.5 parts by mass with respect to 100 parts by mass of component (1). If the amount of paraffin used is too small, the portion in contact with the air may be hardened. On the other hand, if it exceeds 5 parts by mass, the adhesive strength may decrease.
  • a polymerization inhibitor can be used for the purpose of improving storage stability.
  • Polymerization inhibitors include hydroquinone, hydroquinone monomethyl ether, 2,6-citiary butyl-p-cresol, 2,2'-methylenebis (4-methyl-6-tertiary butylphenol), triphenyl phosphate, phenothiazine and N- And isopropyl-N′-phenyl-p-phenylenediamine. These 1 type (s) or 2 or more types can be used.
  • the polymerization inhibitor includes an antioxidant.
  • the amount of the polymerization inhibitor used is preferably 0.001 to 3 parts by mass, more preferably 0.01 to 1 part by mass with respect to 100 parts by mass of the component (1). If the amount of the polymerization inhibitor used is too small, there may be no effect, while if too much, the adhesive strength may decrease.
  • a phosphate in the acrylic temporary fixing adhesive composition of the present invention, can be used for the purpose of improving adhesiveness.
  • Examples of the phosphate include a compound represented by the general formula (F).
  • R 8 is CH 2 ⁇ CR 9 CO (OR 10 ) u — group
  • R 9 is hydrogen or methyl group
  • R 10 is —C 2 H 4 —, —C 3 H 6 —, —CH 2 CH (CH 3 ) —, —C 4 H 8 —, —C 6 H 12 — or
  • U represents an integer of 1 to 10.
  • t represents an integer of 1 or 2.
  • Examples of the phosphate include acid phosphooxyethyl (meth) acrylate, acid phosphooxypropyl (meth) acrylate, and bis (2- (meth) acryloyloxyethyl) phosphate. One or more of these may be used. Can be used. Among these, acid phosphooxyethyl (meth) acrylate is preferable because of its great effect.
  • the amount of phosphate used is preferably 0.1 to 5 parts by weight, more preferably 0.2 to 1.0 part by weight, relative to 100 parts by weight of component (1). preferable. If the amount of phosphate used is too small, the adhesive strength may decrease, while if too much, the adhesive strength may decrease.
  • thermoplastic polymers such as chlorosulfonated polyethylene, polyurethane, styrene-acrylonitrile copolymer and polymethyl methacrylate may be used for the purpose of adjusting viscosity and fluidity.
  • a two-component adhesive composition As an embodiment of the present invention, use as a two-component adhesive composition is exemplified.
  • the adhesive composition is divided into the first agent and the second agent, and at least the component ( 2) is stored separately in the second agent at least component (3). It is preferable to store the phosphate in the second agent.
  • both agents can be applied to the adherend simultaneously or separately, and contacted and cured to be used as a two-component temporary fixing adhesive composition.
  • either or both of the first agent and the second agent are preliminarily incorporated with a monomer and / or oligomer having a (meth) acryloyl group and other optional components, and both are mixed at the time of use. By doing so, it can be used as a one-component adhesive composition for temporary fixing.
  • the temporary fixing adhesive composition of the present invention As a method of using the temporary fixing adhesive composition of the present invention, a method of applying an appropriate amount of the adhesive composition on the adhesive surface of one member to be fixed or the supporting substrate, and then superimposing the other member, A large number of members to be temporarily fixed are laminated in advance, the adhesive composition is applied by a method of infiltrating the adhesive composition into the gap and applied, the temporary fixing adhesive composition is cured, and the members are temporarily attached to each other. Examples include fixing methods.
  • the temporary fixing adhesive composition of the present invention is preferably obtained by using approximately the same amount of the two agents, but does not require accurate measurement of the two agents, incomplete measurement or mixing, Sometimes even two-part contact cures at room temperature. Ultraviolet rays are not required for curing the temporary fixing adhesive composition of the present invention.
  • the temporary fixing adhesive composition of the present invention is excellent in workability.
  • the acrylic temporary fixing adhesive composition of the present invention temporarily fixes various adherends, cuts the member into a desired shape, performs grinding, polishing, etc., and then immerses the member in water.
  • the composition can be peeled from the member.
  • the temporary fixing adhesive composition of the present invention is used to temporarily bond the member, to produce a cured body of the temporary fixing adhesive composition, and to process the temporarily fixed member And the temporary fixing method etc. which immerse the processed member in water and remove the hardening body of the said adhesive composition for temporary fixing are mentioned.
  • the temporary fixing method of the present invention as water used for removing the cured body, for example, moderately heated warm water, preferably 90 ° C. or less, is used, so that the peelability required for removal in water can be obtained. It is preferable in that it can be achieved in a short time and productivity is improved.
  • the method of contact with the hardening body of adhesive composition for temporary fixing, and water the method of immersing the whole joined body in water is preferable at the point which is simple.
  • the temperature of the hot water is preferably 30 to 100 ° C, more preferably 50 to 95 ° C.
  • the temporarily fixed member is processed into a desired shape by cutting, grinding, polishing, drilling, etc., and then the member is heated to water, preferably hot water. By dipping, the cured body of the adhesive can be peeled from the member.
  • the acrylic temporary fixing adhesive composition of the present invention can be used for bonding one or more of the group consisting of silicon, resin, carbon, metal, sapphire and glass. When used for bonding one or more of the group consisting of silicon, sapphire, glass and resin, it has a greater effect. When used for bonding silicon, it has the greatest effect.
  • the acrylic temporary fixing adhesive composition of the present invention When used for bonding silicon, particularly when the silicon block is cut to produce a silicon wafer, the acrylic temporary fixing adhesive composition of the present invention has a great effect.
  • the adhesive composition for temporary fixing of the present invention is used to temporarily fix the silicon block to the base material, and then the silicon block is cut to produce the silicon wafer.
  • Examples include a method of immersing in water and removing the silicon wafer from the substrate.
  • the silicon block is obtained by a method of melting and solidifying solid silicon in a heating furnace.
  • the silicon block is cut with a wire saw or the like. Examples of the wire saw include a piano wire (see Patent Documents 6 to 7). Silicon wafers are used for solar cells and semiconductors.
  • Example 1 Each use material was mixed with the composition of Table 1, and the adhesive composition for temporary fixing which consists of a 1st agent and a 2nd agent was prepared. The results are shown in Table 1.
  • test piece 100 mm x 25 mm x 1.6 mmt, SPCC-D blasted
  • the samples were stacked and bonded together as a sample.
  • the sample fixing time (unit: minute) is the time from when the strength of 0.4 MPa or more is measured immediately after pulling and bonding with a push-pull gauge in an environment of temperature 23 ° C. and humidity 50% RH. did.
  • Si block processing test Using a mixture of equal amounts of the first agent and the second agent, a 125 mm ⁇ 125 mm ⁇ 400 mm Si block and blue plate glass (125 mm ⁇ 400 mm ⁇ 20 mmt) were bonded and cured. Only the Si block part of this adhesion test body was cut into a thickness of 200 ⁇ m using a multi-wire saw, and the presence or absence of the Si block being dropped was observed (Si block processing test (dropped state)).
  • disconnected only the Si block was immersed in 90 degreeC warm water, and the time (90 degreeC warm water peeling time) for which an Si block and a blue glass peeled was measured (Si block processing test (90 degreeC warm water peeling). time)).
  • Examples 2 to 11 A temporary fixing adhesive composition was prepared in the same manner as in Example 1 except that the raw materials of the type shown in Table 1 were used in the composition shown in Table 1. About the obtained adhesive composition for temporary fixing, the said evaluation was performed similarly to Example 1. FIG. The results are shown in Table 1.
  • Comparative Examples 1 to 4 A temporary fixing adhesive composition was prepared in the same manner as in Example 1 except that the raw materials of the type shown in Table 2 were used in the composition shown in Table 2. About the obtained adhesive composition for temporary fixing, the said evaluation was performed similarly to Example 1. FIG. The results are shown in Table 2.
  • the chipping size could be reduced by 10 to 20% by adding an inorganic filler. Even when an inorganic filler was added, there was almost no change in the adhesive strength, indicating that it could withstand the processing of silicon blocks. There was no effect on the hot water peeling time, and it was confirmed that the silicon block could be peeled by being immersed in hot water after processing.
  • the chipping size could be reduced by adding an inorganic filler (Example 8, Comparative Example 4).
  • the present invention has the following effects, for example.
  • the chipping size at the time of cutting the silicon block can be reduced.
  • the temporary fixing adhesive composition of the present invention is cured in a short time and can exhibit high adhesive strength. When the cured body comes into contact with water, the adhesive strength decreases, and the adhesive force between the members or the adhesive force between the member and the jig decreases, so that the member can be easily recovered.
  • the adhesive composition for temporary fixing of the present invention can be quickly peeled off by being immersed in water. When the silicon block is cut using the temporary fixing adhesive composition of the present invention, the silicon block does not fall off and exhibits good processability.
  • the present invention cures in a short time by mixing the two components, it is remarkably superior in terms of workability and shortening of the work time compared to the epoxy adhesive.
  • the adhesive composition for temporary fixing of the present invention the cured product comes into contact with warm water of 90 ° C. or less and swells and can be recovered from the member in the form of a film, so that an effect of excellent workability is obtained.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Processing Of Stones Or Stones Resemblance Materials (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)

Abstract

La présente invention a pour but de proposer une composition adhésive acrylique pour une fixation temporaire, qui est appropriée pour diminuer l'effritement d'une tranche de silicium lorsque la tranche de silicium est traitée à partir d'un bloc de silicium. Cette composition adhésive pour fixation temporaire contient (1) un monomère qui a un groupe (méth)acryloyle, (2) un amorceur de polymérisation, (3) un chélate de β-dicétone et/ou un β-cétoester, et (4) une charge inorganique.
PCT/JP2012/069851 2011-08-05 2012-08-03 Composition adhésive pour une fixation temporaire Ceased WO2013021945A1 (fr)

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KR20210078642A (ko) * 2019-12-18 2021-06-29 (주)이녹스첨단소재 광경화성 접착제 조성물 및 이를 이용하는 부재의 가고정 방법
KR20210078641A (ko) * 2019-12-18 2021-06-29 (주)이녹스첨단소재 광경화성 접착제 조성물 및 이를 이용하는 부재의 가고정 방법
KR102334412B1 (ko) 2019-12-18 2021-12-03 (주)이녹스첨단소재 광경화성 접착제 조성물 및 이를 이용하는 부재의 가고정 방법
KR102334413B1 (ko) 2019-12-18 2021-12-03 (주)이녹스첨단소재 광경화성 접착제 조성물 및 이를 이용하는 부재의 가고정 방법
KR102339285B1 (ko) 2019-12-18 2021-12-15 삼성디스플레이 주식회사 광경화성 접착제 조성물 및 이를 이용하는 부재의 가고정 방법

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