CN110088160B - Resin particle, connection material, and connection structure - Google Patents
Resin particle, connection material, and connection structure Download PDFInfo
- Publication number
- CN110088160B CN110088160B CN201880005079.3A CN201880005079A CN110088160B CN 110088160 B CN110088160 B CN 110088160B CN 201880005079 A CN201880005079 A CN 201880005079A CN 110088160 B CN110088160 B CN 110088160B
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- China
- Prior art keywords
- particles
- resin
- resin particles
- connection
- liquid crystal
- Prior art date
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- 239000002245 particle Substances 0.000 title claims abstract description 317
- 229920005989 resin Polymers 0.000 title claims abstract description 198
- 239000011347 resin Substances 0.000 title claims abstract description 198
- 239000000463 material Substances 0.000 title claims description 65
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims description 57
- 239000002184 metal Substances 0.000 claims description 54
- 229920002050 silicone resin Polymers 0.000 claims description 48
- 238000007906 compression Methods 0.000 claims description 31
- 125000006850 spacer group Chemical group 0.000 claims description 31
- 230000006835 compression Effects 0.000 claims description 30
- 239000000853 adhesive Substances 0.000 claims description 12
- 230000001070 adhesive effect Effects 0.000 claims description 12
- 239000011230 binding agent Substances 0.000 claims description 11
- 238000011084 recovery Methods 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 4
- 230000002040 relaxant effect Effects 0.000 abstract description 17
- 230000002401 inhibitory effect Effects 0.000 abstract 1
- -1 polysiloxane Polymers 0.000 description 84
- 239000004973 liquid crystal related substance Substances 0.000 description 60
- 229910000077 silane Inorganic materials 0.000 description 35
- 125000004429 atom Chemical group 0.000 description 34
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 31
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 29
- 238000000034 method Methods 0.000 description 29
- 229910052710 silicon Inorganic materials 0.000 description 29
- 125000004432 carbon atom Chemical group C* 0.000 description 25
- 229920001296 polysiloxane Polymers 0.000 description 23
- 239000000758 substrate Substances 0.000 description 23
- 239000000565 sealant Substances 0.000 description 17
- 239000012790 adhesive layer Substances 0.000 description 16
- 150000002430 hydrocarbons Chemical group 0.000 description 16
- 125000000962 organic group Chemical group 0.000 description 16
- 125000001165 hydrophobic group Chemical group 0.000 description 15
- 125000004430 oxygen atom Chemical group O* 0.000 description 15
- 150000003254 radicals Chemical class 0.000 description 15
- 150000001875 compounds Chemical class 0.000 description 14
- 239000000126 substance Substances 0.000 description 14
- 239000011521 glass Substances 0.000 description 13
- 238000007789 sealing Methods 0.000 description 13
- 229910044991 metal oxide Inorganic materials 0.000 description 12
- 150000004706 metal oxides Chemical class 0.000 description 12
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 10
- 239000003638 chemical reducing agent Substances 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 10
- 229910052709 silver Inorganic materials 0.000 description 10
- 239000004332 silver Substances 0.000 description 10
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 10
- 239000010408 film Substances 0.000 description 9
- 125000005386 organosiloxy group Chemical group 0.000 description 9
- 229920001187 thermosetting polymer Polymers 0.000 description 9
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 9
- 238000006116 polymerization reaction Methods 0.000 description 8
- 238000005481 NMR spectroscopy Methods 0.000 description 7
- 150000007942 carboxylates Chemical class 0.000 description 7
- 229920001971 elastomer Polymers 0.000 description 7
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 7
- 239000002923 metal particle Substances 0.000 description 7
- 230000035699 permeability Effects 0.000 description 7
- 238000005245 sintering Methods 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 238000006073 displacement reaction Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 229920002379 silicone rubber Polymers 0.000 description 5
- 229910001923 silver oxide Inorganic materials 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000806 elastomer Substances 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 238000005304 joining Methods 0.000 description 4
- 239000011817 metal compound particle Substances 0.000 description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 4
- 239000007870 radical polymerization initiator Substances 0.000 description 4
- 229920001169 thermoplastic Polymers 0.000 description 4
- 239000004416 thermosoftening plastic Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- 229920001400 block copolymer Polymers 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 125000004122 cyclic group Chemical group 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000005060 rubber Substances 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229920002554 vinyl polymer Polymers 0.000 description 3
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- BBMCTIGTTCKYKF-UHFFFAOYSA-N 1-heptanol Chemical compound CCCCCCCO BBMCTIGTTCKYKF-UHFFFAOYSA-N 0.000 description 2
- KWVGIHKZDCUPEU-UHFFFAOYSA-N 2,2-dimethoxy-2-phenylacetophenone Chemical compound C=1C=CC=CC=1C(OC)(OC)C(=O)C1=CC=CC=C1 KWVGIHKZDCUPEU-UHFFFAOYSA-N 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 238000012674 dispersion polymerization Methods 0.000 description 2
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- GOQYKNQRPGWPLP-UHFFFAOYSA-N heptadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 2
- KEMQGTRYUADPNZ-UHFFFAOYSA-N heptadecanoic acid Chemical compound CCCCCCCCCCCCCCCCC(O)=O KEMQGTRYUADPNZ-UHFFFAOYSA-N 0.000 description 2
- MNWFXJYAOYHMED-UHFFFAOYSA-N heptanoic acid Chemical compound CCCCCCC(O)=O MNWFXJYAOYHMED-UHFFFAOYSA-N 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
- VKOBVWXKNCXXDE-UHFFFAOYSA-N icosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCC(O)=O VKOBVWXKNCXXDE-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- ISYWECDDZWTKFF-UHFFFAOYSA-N nonadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCCC(O)=O ISYWECDDZWTKFF-UHFFFAOYSA-N 0.000 description 2
- ZWRUINPWMLAQRD-UHFFFAOYSA-N nonan-1-ol Chemical compound CCCCCCCCCO ZWRUINPWMLAQRD-UHFFFAOYSA-N 0.000 description 2
- FBUKVWPVBMHYJY-UHFFFAOYSA-N nonanoic acid Chemical compound CCCCCCCCC(O)=O FBUKVWPVBMHYJY-UHFFFAOYSA-N 0.000 description 2
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- REIUXOLGHVXAEO-UHFFFAOYSA-N pentadecan-1-ol Chemical compound CCCCCCCCCCCCCCCO REIUXOLGHVXAEO-UHFFFAOYSA-N 0.000 description 2
- DPBLXKKOBLCELK-UHFFFAOYSA-N pentan-1-amine Chemical compound CCCCCN DPBLXKKOBLCELK-UHFFFAOYSA-N 0.000 description 2
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- 239000002243 precursor Substances 0.000 description 2
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- 230000009467 reduction Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
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- 238000012360 testing method Methods 0.000 description 2
- HLZKNKRTKFSKGZ-UHFFFAOYSA-N tetradecan-1-ol Chemical compound CCCCCCCCCCCCCCO HLZKNKRTKFSKGZ-UHFFFAOYSA-N 0.000 description 2
- 229920005992 thermoplastic resin Polymers 0.000 description 2
- SZHOJFHSIKHZHA-UHFFFAOYSA-N tridecanoic acid Chemical compound CCCCCCCCCCCCC(O)=O SZHOJFHSIKHZHA-UHFFFAOYSA-N 0.000 description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
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- 239000010937 tungsten Substances 0.000 description 2
- ZDPHROOEEOARMN-UHFFFAOYSA-N undecanoic acid Chemical compound CCCCCCCCCCC(O)=O ZDPHROOEEOARMN-UHFFFAOYSA-N 0.000 description 2
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- ZNGSVRYVWHOWLX-KHFUBBAMSA-N (1r,2s)-2-(methylamino)-1-phenylpropan-1-ol;hydrate Chemical compound O.CN[C@@H](C)[C@H](O)C1=CC=CC=C1.CN[C@@H](C)[C@H](O)C1=CC=CC=C1 ZNGSVRYVWHOWLX-KHFUBBAMSA-N 0.000 description 1
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 description 1
- XFRVVPUIAFSTFO-UHFFFAOYSA-N 1-Tridecanol Chemical compound CCCCCCCCCCCCCO XFRVVPUIAFSTFO-UHFFFAOYSA-N 0.000 description 1
- JPZYXGPCHFZBHO-UHFFFAOYSA-N 1-aminopentadecane Chemical compound CCCCCCCCCCCCCCCN JPZYXGPCHFZBHO-UHFFFAOYSA-N 0.000 description 1
- ZIKLJUUTSQYGQI-UHFFFAOYSA-N 1-ethoxy-2-(2-ethoxypropoxy)propane Chemical compound CCOCC(C)OCC(C)OCC ZIKLJUUTSQYGQI-UHFFFAOYSA-N 0.000 description 1
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 description 1
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 1
- VCYDUTCMKSROID-UHFFFAOYSA-N 2,2,4,4,6,6-hexakis-phenyl-1,3,5,2,4,6-trioxatrisilinane Chemical compound O1[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si]1(C=1C=CC=CC=1)C1=CC=CC=C1 VCYDUTCMKSROID-UHFFFAOYSA-N 0.000 description 1
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- JJLJEONZQSKVAT-UHFFFAOYSA-N 2-(2-ethenylbut-3-enoxy)ethenylsilane Chemical compound C(=C)C(COC=C[SiH3])C=C JJLJEONZQSKVAT-UHFFFAOYSA-N 0.000 description 1
- FPZWZCWUIYYYBU-UHFFFAOYSA-N 2-(2-ethoxyethoxy)ethyl acetate Chemical compound CCOCCOCCOC(C)=O FPZWZCWUIYYYBU-UHFFFAOYSA-N 0.000 description 1
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- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 description 1
- DRLRGHZJOQGQEC-UHFFFAOYSA-N 2-(2-methoxypropoxy)propyl acetate Chemical compound COC(C)COC(C)COC(C)=O DRLRGHZJOQGQEC-UHFFFAOYSA-N 0.000 description 1
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 1
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
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- WAEVWDZKMBQDEJ-UHFFFAOYSA-N 2-[2-(2-methoxypropoxy)propoxy]propan-1-ol Chemical compound COC(C)COC(C)COC(C)CO WAEVWDZKMBQDEJ-UHFFFAOYSA-N 0.000 description 1
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 1
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- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- SVONRAPFKPVNKG-UHFFFAOYSA-N 2-ethoxyethyl acetate Chemical compound CCOCCOC(C)=O SVONRAPFKPVNKG-UHFFFAOYSA-N 0.000 description 1
- LTHNHFOGQMKPOV-UHFFFAOYSA-N 2-ethylhexan-1-amine Chemical compound CCCCC(CC)CN LTHNHFOGQMKPOV-UHFFFAOYSA-N 0.000 description 1
- POYODSZSSBWJPD-UHFFFAOYSA-N 2-methylprop-2-enoyloxy 2-methylprop-2-eneperoxoate Chemical compound CC(=C)C(=O)OOOC(=O)C(C)=C POYODSZSSBWJPD-UHFFFAOYSA-N 0.000 description 1
- MYTUNQXRWZGYCK-UHFFFAOYSA-N 2-penta-1,4-dien-3-yloxyethenylsilane Chemical compound C(=C)C(OC=C[SiH3])C=C MYTUNQXRWZGYCK-UHFFFAOYSA-N 0.000 description 1
- LIFHMKCDDVTICL-UHFFFAOYSA-N 6-(chloromethyl)phenanthridine Chemical compound C1=CC=C2C(CCl)=NC3=CC=CC=C3C2=C1 LIFHMKCDDVTICL-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 238000012935 Averaging Methods 0.000 description 1
- MRABAEUHTLLEML-UHFFFAOYSA-N Butyl lactate Chemical compound CCCCOC(=O)C(C)O MRABAEUHTLLEML-UHFFFAOYSA-N 0.000 description 1
- XTHGGXWMGDMZEI-UHFFFAOYSA-N C=C[SiH2]O[SiH](C=C)C1=CC=CC2=C1C3=CC4=CC=CC=C4C=C3C=C2 Chemical compound C=C[SiH2]O[SiH](C=C)C1=CC=CC2=C1C3=CC4=CC=CC=C4C=C3C=C2 XTHGGXWMGDMZEI-UHFFFAOYSA-N 0.000 description 1
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 description 1
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Images
Classifications
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- 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
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J153/00—Adhesives based on block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2353/00—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/10—Block- or graft-copolymers containing polysiloxane sequences
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention provides a resin particle capable of effectively relaxing internal stress and effectively inhibiting occurrence of rebound. The present invention provides a resin particle, wherein the resin particle is represented by the general formula [ (R) 3 SiO 1/2 ]M unit represented by the general formula [ (R) 2 SiO 2/2 ]D unit represented by the general formula [ (R) SiO) 3/2 ]T unit represented by the general formula [ SiO ] 4/2 ]The total number of the T units and the Q units is 4% or less of 100% of the total number of the Q units.
Description
Technical Field
The present invention relates to resin particles containing a silicone resin. The present invention also relates to a connection material and a connection structure using the resin particles.
Background
Miniaturization, weight saving, and thickness reduction of electric and electronic parts are rapidly advancing. Meanwhile, dimensional stability of printed wiring boards or multilayer boards, reduction of warpage, prevention of occurrence of cracks, and the like have become technical problems. As a method for solving the above-described problems, a method for relaxing internal stress and the like are mentioned. As a method for relaxing the internal stress, for example, a method of adding a stress relaxing material such as polysiloxane particles to a resin composition has been proposed.
As an example of the above polysiloxane particles, the following patent document 1 discloses spherical polysiloxane elastomer particles. The main component of the spherical silicone elastomer particles is a silicone elastomer. The average particle diameter of the spherical silicone elastomer particles is 0.1 to 500. Mu.m. The spherical silicone elastomer particles described above are substantially free of metal elements derived from the curing catalyst.
Further, patent document 2 below discloses a polysiloxane particle having 100 parts by mass of spherical particles of a polysiloxane elastomer and 0.5 to 25 parts by mass of a polyorganosilsesquioxane coating the surface thereof. The spherical particles of the silicone elastomer have a volume average particle diameter of 0.1 to 100. Mu.m. The above-mentioned polyorganosilsesquioxane is in the form of particles. The size of the polyorganosilsesquioxane is 60nm or less.
Further, the following patent document 3 discloses a sponge-like silicone particle obtained by the following method: the silane compound having three functional groups represented by the formula (1) and the silane compound having two functional groups represented by the formula (2) are copolymerized. The sponge-like silicone particles are formed by the following method: spherical polysiloxane particles having an average particle diameter of 0.1 to 50 μm are connected to form a flocculent state. The average particle diameter of the sponge-like silicone particles is 1 to 100 μm. The sponge-like silicone particles can again discharge 70% or more of the temporarily absorbed oil.
Prior art literature
Patent literature
Patent document 1: japanese patent laid-open No. 2006-104456
Patent document 2: japanese patent laid-open No. 2013-40241
Patent document 3: japanese patent application laid-open No. 2015-140356
Disclosure of Invention
Technical problem to be solved by the invention
When forming a connection portion for connecting the electrodes and an adhesive layer for bonding the two members to be connected, it is preferable to heat the connection portion or the adhesive layer to cure an adhesive such as a resin. When the connection portion or the adhesive layer is heated, internal stress may be generated due to curing shrinkage of an adhesive such as a resin. The internal stress generated is a factor of occurrence of cracks in the connecting portion or the adhesive layer, and therefore, it is necessary to alleviate the internal stress. With the conventional polysiloxane particles described in patent documents 1 to 3, it is difficult to sufficiently alleviate the internal stress generated in the connecting portion or the adhesive layer.
In addition, when the conventional silicone particles described in patent documents 1 to 3 are used as a spacer, the action of restoring the compressed silicone particles to their original shape causes a so-called rebound phenomenon. If the silicone particles mixed as the spacers in the adhesive layer rebound, peeling may occur at the interface between the adhesive layer and the adherend after a lapse of time.
The purpose of the present invention is to provide resin particles that can effectively alleviate internal stress and effectively suppress occurrence of rebound. The present invention also provides a connection material and a connection structure using the resin particles.
Technical means for solving the problems
According to a broad aspect of the present invention, there is provided a resin particle wherein the resin particle is represented by the general formula [ (R) 3 SiO 1/2 ]M unit represented by the general formula [ (R) 2 SiO 2/2 ]D unit represented by the general formula [ (R) SiO) 3/2 ]T unit represented by the general formula [ SiO ] 4/2 ]The total number of the T units and the Q units is 4% or less of 100% of the total number of the Q units.
In a specific embodiment of the resin particles of the present invention, the compression recovery rate at 40% compression deformation is 10% or less.
In a specific embodiment of the resin particles of the present invention, the 10% K value is 500N/mm 2 The following is given.
In a specific embodiment of the resin particles of the present invention, the particle diameter is 0.5 μm or more and 500 μm or less.
In a specific embodiment of the resin particles of the present invention, the resin particles are particles containing a silicone resin.
In a specific embodiment of the resin particles of the present invention, the resin particles are used as spacers.
According to a broad aspect of the present invention, there is provided a connecting material comprising the above resin particles, and further comprising a binder or particles containing a metal atom.
In a specific embodiment of the resin particles of the present invention, the connecting material comprises a binder.
In a specific embodiment of the resin particles of the present invention, the connecting material comprises particles containing a metal atom.
In a specific embodiment of the resin particles of the present invention, the thermal decomposition temperature of the resin particles is higher than the melting point of the metal atom-containing particles.
In a specific aspect of the resin particle of the present invention, the connecting material is used to form a connecting portion that connects two members to be connected;
and for forming the connection portion by a sintered body of the metal atom-containing particles.
According to an broad aspect of the present invention, there is provided a connection structure comprising:
a first connecting object member,
Second connection target member
A connection section that connects the first connection object member and the second connection object member together, wherein,
the material of the connection portion contains the resin particles.
ADVANTAGEOUS EFFECTS OF INVENTION
In the resin particles of the present invention, the resin particles are represented by the general formula [ (R) 3 SiO 1/2 ]M unit represented by the general formula [ (R) 2 SiO 2/2 ]D unit represented by the general formula [ (R) SiO) 3/2 ]T unit represented by the general formula [ SiO ] 4/2 ]The total number of the T units and the Q units is 4% or less of 100% of the total number of the Q units. The resin particles of the present invention have the above technical features, and therefore can effectively alleviate internal stress and effectively suppress occurrence of rebound.
Drawings
Fig. 1 is a cross-sectional view showing an example of a connection structure using the resin particles of the present invention.
Fig. 2 is a cross-sectional view showing an example of a liquid crystal display element using the resin particles of the present invention as spacers for the liquid crystal display element.
Detailed Description
The present invention will be described in detail below.
(resin particles)
In the resin particles of the present invention, the resin particles are represented by the general formula [ (R) 3 SiO 1/2 ]M unit represented by the general formula [ (R) 2 SiO 2/2 ]D unit represented by the general formula [ (R) SiO) 3/2 ]T unit represented by the general formula [ SiO ] 4/2 ]The total number of the T units and the Q units is 4% or less of 100% of the total number of the Q units. The M unit, D unit, T unit, Q unit are known from the above formulae. R in the above formula represents any group. As an optional group of R, O bonded to Si other than the unit of the above formula is excluded 1/2 A group.
Since the resin particles of the present invention have the above technical features, the resin particles can effectively alleviate internal stress and effectively suppress occurrence of rebound.
Since the resin particles of the present invention have the above-described technical characteristics, the compression recovery rate is relatively low, and the effect of recovering the original shape of the compressed resin particles is relatively hard to act, and rebound is hard to occur. For example, when the resin particles of the present invention are used as spacers, the spacers can be brought into sufficient contact with a member for a liquid crystal display element or the like, and the gap can be controlled with higher accuracy.
When forming a connection portion for electrically connecting electrodes or an adhesive layer for adhering two members to be connected, it is preferable to heat the connection portion or the adhesive layer to cure an adhesive such as a resin. When the connection portion or the adhesive layer is heated, internal stress may be generated due to curing shrinkage of an adhesive such as a resin. The internal stress generated causes a crack or the like, and therefore, it is preferable to remove the internal stress. As a method for removing the internal stress, a heat treatment method and the like can be given. However, if a resin or the like is used for the connection portion or the adhesive layer, it is difficult to sufficiently remove the internal stress even by the heat treatment. Since the resin particles of the present invention have the above-described means, the compression recovery rate is relatively low, and the effect of recovering the original shape of the compressed resin particles is relatively hard to be exerted. By using the resin particles of the present invention for the connection portion or the adhesive layer, even if internal stress is generated in the connection portion or the adhesive layer by heating or the like, the internal stress of the connection portion or the adhesive layer is effectively relaxed by the deformation of the resin particles. As a result, occurrence of cracks or the like in the connection portion or the adhesive layer can be effectively suppressed.
The resin particles preferably contain silicone resin particles from the viewpoint of further effectively relaxing the internal stress and further effectively suppressing occurrence of rebound. The above-mentioned silicone resin preferably contains a specific organic siloxy unit (a unit containing a silicon bond).
The above-mentioned organosiloxy unit includes: monofunctional organo siloxy units called M units, difunctional organo siloxy units called D units, trifunctional organo siloxy units called T units, tetrafunctional organo siloxy units called Q units. The Q unit is a unit having no organic group containing a carbon atom directly bonded to a silicon atom, but in the present invention, it is an organo siloxy unit.
In the above-mentioned organosiloxane-based unit, since the siloxane bond is a bond in which two silicon atoms are bonded through one oxygen atom, the number of oxygen atoms per silicon atom in the siloxane bond is considered to be 1/2, and is generally represented as O 1/2 . Specifically, for example, in one D unit, one silicon atom contained in the D unit is bonded to two oxygen atoms, and each oxygen atom is bonded to a silicon atom of another unit. That is, the structure of the D unit is [ -O 1/2 -(R) 2 Si-O 1/2 -]Due to the presence of two O 1/2 The unit, D unit, is represented by the general formula [ (R) 2 SiO 2/2 ]。
The M unit is represented by the general formula [ (R) 3 SiO 1/2 ]An organo siloxy unit represented. Specifically, the M unit has a structure represented by the following formula (1).
[ chemical formula 1]
In the above formula (1), R1, R2 and R3 each represent an arbitrary group. R1, R2 and R3 each preferably represent an alkyl group, an aryl group, an allyl group, a hydrogen atom or a divalent organic group having 1 to 5 carbon atoms. The organic group may contain a carbon atom, a hydrogen atom, and an oxygen atom. The organic group may be a divalent hydrocarbon group having 1 to 5 carbon atoms. The main chain of the above organic group is preferably a divalent hydrocarbon group. In the above organic group, a carboxyl group, a hydroxyl group or the like may be bonded to the divalent hydrocarbon group. The structure represented by the above formula (1) may be bonded to another structure through R1, R2, R3. The oxygen atom in the above general formula (1) may form a siloxane bond with a silicon atom of another structure or may form a bond with an atom other than the silicon atom of another structure.
The structure represented by the above formula (1) is preferably bonded to other structures through a divalent hydrocarbon group from the viewpoint of further effectively relaxing the internal stress and further effectively suppressing occurrence of rebound. From the viewpoint of further effectively relaxing the internal stress and further effectively suppressing occurrence of rebound, the oxygen atom in the above formula (1) is preferably bonded to a silicon atom of another structure, and is also preferably bonded to a divalent hydrocarbon group of another structure.
The D unit is represented by the general formula [ (R) 2 SiO 2/2 ]Represented by the formula (I). Specifically, the D cell has a structure represented by the following formula (2).
[ chemical formula 2]
In the above formula (2), R4 and R5 each represent an arbitrary group. R4 and R5 are preferably alkyl, aryl, allyl, a hydrogen atom or a divalent organic group having 1 to 5 carbon atoms. The organic group may contain a carbon atom, a hydrogen atom, and an oxygen atom. The organic group may be a divalent hydrocarbon group having 1 to 5 carbon atoms. The main chain of the above organic group is preferably a divalent hydrocarbon group. In the above organic group, a carboxyl group, a hydroxyl group or the like may be bonded to the divalent hydrocarbon group. The structure represented by the above formula (2) may be bonded to another structure through R4, R5. The oxygen atom in the above general formula (2) may form a siloxane bond with a silicon atom of another structure or may form a bond with an atom other than the silicon atom of another structure.
The structure represented by the above formula (2) is preferably bonded to other structures through a divalent hydrocarbon group from the viewpoint of further effectively relaxing the internal stress and further effectively suppressing occurrence of rebound. From the viewpoint of further effectively relaxing the internal stress and further effectively suppressing occurrence of rebound, the oxygen atom in the above formula (2) is preferably bonded to a silicon atom of another structure, and is also preferably bonded to a divalent hydrocarbon group of another structure.
The T unit is represented by the general formula [ (R) SiO 3/2 ]An organo siloxy unit represented. Specifically, the T cell has a structure represented by the following formula (3).
[ chemical formula 3]
In the above formula (3), R6 represents an arbitrary group. R6 preferably represents an alkyl group, an aryl group, an allyl group, a hydrogen atom or a divalent organic group having 1 to 5 carbon atoms. The organic group may contain a carbon atom, a hydrogen atom, and an oxygen atom. The organic group may be a divalent hydrocarbon group having 1 to 5 carbon atoms. The main chain of the above organic group is preferably a divalent hydrocarbon group. In the above organic group, a carboxyl group, a hydroxyl group or the like may be bonded to the divalent hydrocarbon group. The structure represented by the above formula (3) may be bonded to another structure through R6. The oxygen atom in the above general formula (3) may form a siloxane bond with a silicon atom of another structure or may form a bond with an atom other than the silicon atom of another structure.
The structure represented by the above formula (3) is preferably bonded to other structures through a divalent hydrocarbon group from the viewpoint of further effectively relaxing the internal stress and further effectively suppressing occurrence of rebound. From the viewpoint of further effectively relaxing the internal stress and further effectively suppressing occurrence of rebound, the oxygen atom in the above formula (3) is preferably bonded to a silicon atom of another structure, and is also preferably bonded to a divalent hydrocarbon group of another structure.
The Q unit is represented by the general formula: [ SiO ] 4/2 ]Indicated as organo siloxy units (siloxane units). Specifically, the Q unit has a structure represented by the following formula (4).
[ chemical formula 4]
The oxygen atom in the above formula (4) may form a siloxane bond with a silicon atom of another structure or may form a bond with an atom other than the silicon atom of another structure. From the viewpoint of further effectively relaxing the internal stress and further effectively suppressing occurrence of rebound, the oxygen atom in the above formula (4) is preferably bonded to a silicon atom of another structure, and is also preferably bonded to a divalent hydrocarbon group of another structure.
In the resin particles of the present invention, the resin particles are represented by the general formula [ (R) 3 SiO 1/2 ]M unit represented by the general formula [ (R) 2 SiO 2/2 ]D unit represented by the general formula [ (R) SiO) 3/2 ]T unit represented by the general formula [ SiO ] 4/2 ]The total number (TnQn) of the T units and the Q units is 4% or less of the total number of the Q units represented by 100%.
From the viewpoint of further effectively relaxing the internal stress and further effectively suppressing occurrence of springback, the TnQn is preferably 3% or less, more preferably 2% or less, of 100% of the total number of the M unit, the D unit, the T unit, and the Q unit. The lower limit of TnQn is not particularly limited. The TnQn may be 0% (the number is 0) or more than 0%.
The TnQn can be obtained by 29 The resin particles were analyzed by Si-solid NMR to calculate. Specifically, the calculation can be performed as follows.
The method for calculating TnQn comprises the following steps:
using resin particles which have been sufficiently dried, and under the following measurement conditions 29 Si-solid NMR measurement (DD/MAS method) can obtain integral values of signal amounts of the respective units. From the obtained integral value of the signal quantity of each unit described above, tnQn can be calculated.
29 Measurement conditions for Si-solid NMR measurement (DD/MAS method):
the device comprises: JNM-ECX400 manufactured by Jeol Resonance Inc "
And (3) observing a core: 29 Si
and (3) probe: 8mm probe for solid NMR
MAS rotation speed: 7kHz
The measuring method comprises the following steps: single pulse (DD/MAS)
Pulse width: 3.45 mu s% 29 Si/90 degree)
Delay time: 315 seconds
Acquisition time: 21 ms of
Number of scans: 500 times
In addition, derived from the units described above 29 The chemical shift of Si-solid NMR is generally as follows. Derived from the units mentioned 29 The chemical shift of Si-solid NMR can be appropriately determined in consideration of any group bonded to Si group.
M unit: 5ppm to 15ppm
D unit: -30ppm to-5 ppm
T unit: -75ppm to-50 ppm
Q unit: -120ppm to-100 ppm
From the viewpoint of further effectively relaxing the internal stress and further effectively suppressing occurrence of springback, the compression recovery rate at the time of compression deformation of the resin particles by 40% is preferably 10% or less, more preferably 9% or less, and preferably 0.1% or more, more preferably 1% or more.
The compression recovery rate at 40% compression deformation of the resin particles can be measured as follows.
The resin particles are spread on the sample stage. For each of the dispersed resin particles, a micro compression tester was used, and a load was applied in the center direction of the resin particles at 25 ℃ on the smooth end face of a cylinder (diameter 100 μm, made of diamond) until the resin particles were compressively deformed 40% (reverse load value). Then, the charge was removed until the original load value (0.40 mN). The load-compression displacement during this period was measured, and the compression recovery rate at 40% compression set at 25℃was obtained from the following equation. The load speed was set to 0.33mN/sec. As the micro compression tester, for example, "micro compression tester MCT-W200" manufactured by Shimadzu corporation, "Fischer Scope H-100" manufactured by Fischer company, etc. may be used.
Compression recovery (%) = [ L2/L1] ×100
L1: compression displacement from origin load value to reverse load value when load is applied
L2: load shedding displacement from reverse load value to origin load value when releasing load
The 10% K value of the resin particles is preferably 5N/mm 2 The above is more preferably 10N/mm 2 Above, and preferably 500N/mm 2 Hereinafter, more preferably 200N/mm 2 Hereinafter, 150N/mm is more preferable 2 Hereinafter, it is particularly preferably 100N/mm 2 The following is given. When the 10% k value of the resin particles is not less than the lower limit and not more than the upper limit, the internal stress can be relaxed more effectively, and the occurrence of springback can be suppressed more effectively.
The 10% K value of the above resin particles can be measured as follows.
One resin particle was compressed on a smooth end face of a cylinder (diameter 100 μm, made of diamond) using a micro compression tester at 25℃under conditions of a compression rate of 0.3mN/sec and a maximum test load of 20 mN. The load value (N) and the compression displacement (mm) at this time were measured. From the obtained measurement value, a 10% K value at 25℃can be obtained by the following formula. As the micro compression tester, for example, "micro compression tester MCT-W200" manufactured by Shimadzu corporation, "Fischer Scope H-100" manufactured by Fischer company, etc. may be used. The 10% K value of the above resin particles is preferably calculated by arithmetically averaging 10% K values of 50 optional resin particles.
10% K value (N/mm) 2 )＝(3/2 1/2 )·F·S -3/2 ·R -1/2
F: load value (N) at 10% compression set of resin particles
S: compression displacement (mm) at 10% compression deformation of resin particles
R: radius (mm) of resin particle
The K value generally and quantitatively represents the hardness of the resin particles. By using the K value, the hardness of the resin particles can be quantitatively and clearly expressed.
The particle diameter of the resin particles may be appropriately set according to the application. The particle diameter of the resin particles is preferably 0.5 μm or more, more preferably 1 μm or more, and preferably 500 μm or less, more preferably 450 μm or less, still more preferably 100 μm or less, still more preferably 50 μm or less, and particularly preferably 20 μm or less. When the particle diameter of the resin particles is not less than the lower limit and not more than the upper limit, the internal stress can be relaxed more effectively, and the occurrence of rebound can be suppressed more effectively. When the particle diameter of the resin particles is 0.5 μm or more and 20 μm or less, the resin particles can be suitably used for a stress relaxation material. When the particle diameter of the resin particles is 1 μm or more and 100 μm or less, the resin particles can be suitably used for a gap control material.
The particle diameter of the resin particles represents the diameter when the resin particles are spherical, and the maximum inner diameter when the resin particles are not spherical.
The particle diameter of the resin particles is preferably an average particle diameter, and more preferably a number average particle diameter. The particle diameter of the resin particles can be obtained by using a particle size distribution measuring apparatus or the like. For example, a particle size distribution measuring apparatus using the principles of laser scattered light, resistance change, image analysis after imaging, and the like can be used. Specifically, examples of the method for measuring the particle diameter of the resin particles include the following methods: the particle size of about 100000 resin particles was measured using a particle size distribution measuring apparatus (Multisizer 4 manufactured by Beckman Coulter Co., ltd.) and an average value was calculated. The particle diameter of the resin particles is preferably determined by the following method: 50 arbitrary resin particles were observed by an electron microscope or an optical microscope, and an average value was calculated.
From the viewpoint of further effectively relaxing the internal stress, the coefficient of variation (CV value) of the particle diameter of the resin particles is preferably 10% or less, more preferably 7% or less, and still more preferably 5% or less. When the coefficient of variation (CV value) of the particle diameter of the resin particles is equal to or less than the upper limit, the resin particles can be suitably used as a stress relaxation material or a gap control material.
The coefficient of variation (CV value) can be measured as follows.
CV value (%) = (ρ/Dn) ×100
ρ: standard deviation of particle diameter of resin particles
Dn: average value of particle diameter of resin particles
The shape of the resin particles is not particularly limited. The resin particles may have a spherical shape or a flat shape other than a spherical shape.
The use of the above resin particles is not particularly limited. The resin particles are suitable for various applications. The above resin particles are preferably used as spacers. The method of using the spacer includes: spacers for liquid crystal display elements, spacers for gap control, spacers for stress relaxation, and the like. The spacer for gap control can be used for gap control of stacked chips for ensuring a gap height and flatness, and for gap control of optical members for ensuring smoothness of a glass surface and thickness of an adhesive layer. The spacer for stress relaxation can be used for stress relaxation of a sensor chip or the like, and stress relaxation of a connecting portion connecting two members to be connected together. The spacer for stress alleviation can be used for connecting materials of power devices, adhesives for sensors, and the like. The spacer is preferably used for a connecting material for a power unit, and is preferably used for an adhesive for a sensor.
The resin particles are preferably used as spacers for liquid crystal display elements, and are preferably used as a peripheral sealing agent for liquid crystal display elements. In the peripheral sealing agent for a liquid crystal display element, the resin particles preferably function as spacers. Since the resin particles have good compression set characteristics, when the resin particles are used as spacers and disposed between substrates, the spacers can be effectively disposed between the substrates. Further, since the resin particles can suppress scratches on the members for liquid crystal display elements, display defects are less likely to occur in the liquid crystal display elements using the spacers for liquid crystal display elements.
Further, the above resin particles are suitably used as an inorganic filler, an additive for toner, an impact absorber or a vibration absorber. For example, the above resin particles can be used as a substitute for rubber, springs, or the like.
(other details of resin particles)
The resin particles are preferably particles containing a silicone resin from the viewpoint of further effectively relaxing the internal stress and further effectively suppressing occurrence of rebound.
The material of the above-mentioned silicone resin is preferably a silane compound having a radical polymerizable group and a silane compound having a hydrophobic group having 5 or more carbon atoms, preferably a silane compound having a radical polymerizable group and a hydrophobic group having 5 or more carbon atoms, preferably a silane compound having radical polymerizable groups at both ends. When these materials are reacted, siloxane bonds are formed. In the silicone resin obtained, a radical polymerizable group and a hydrophobic group having 5 or more carbon atoms generally remain. By using such a material, particles containing the silicone resin having a particle diameter of 1 μm or more and 200 μm or less can be easily obtained, and the chemical resistance of the particles containing the silicone resin can be improved and the moisture permeability thereof can be reduced.
In the silane compound having the above radical polymerizable group, the radical polymerizable group is preferably directly bonded to a silicon atom. One kind of the above silane compound having a radical polymerizable group may be used alone, or two or more kinds may be used in combination.
The silane compound having a radical polymerizable group is preferably an alkoxysilane compound. The silane compound having a radical polymerizable group includes: vinyl trimethoxysilane, vinyl triethoxysilane, dimethoxymethylvinylsilane, diethoxymethylvinylsilane, divinylmethoxyvinylsilane, divinylethoxyvinylsilane, divinyldimethoxysilane, divinyldiethoxysilane, 1, 3-divinyltetramethyldisiloxane, and the like.
In the above-mentioned silane compound having a hydrophobic group having 5 or more carbon atoms, it is preferable that the hydrophobic group having 5 or more carbon atoms is directly bonded to a silicon atom. One kind of the above silane compound having a hydrophobic group having 5 or more carbon atoms may be used alone, or two or more kinds may be used in combination.
The silane compound having a hydrophobic group having 5 or more carbon atoms is preferably an alkoxysilane compound. The silane compound having a hydrophobic group having 5 or more carbon atoms includes: phenyl trimethoxysilane, dimethoxymethylphenyl silane, diethoxymethylphenyl silane, dimethylmethoxyphenyl silane, dimethylethoxyphenyl silane, hexaphenyl disiloxane, 1,3, 5-tetramethyl-1, 5-tetraphenyl trisiloxane, 1,1,3,5,5-pentaphenyl-1, 3, 5-trimethyltrisiloxane, hexaphenyl cyclotrisiloxane, phenyl tris (trimethylsiloxy) silane, octaphenyl cyclotrisiloxane, and the like.
Among the above-mentioned silane compounds having a radical polymerizable group and a hydrophobic group having 5 or more carbon atoms, the radical polymerizable group is preferably directly bonded to a silicon atom, and the hydrophobic group having 5 or more carbon atoms is preferably directly bonded to a silicon atom. The silane compound having a radically polymerizable group and a hydrophobic group having 5 or more carbon atoms may be used singly or in combination.
The silane compound having a radical polymerizable group and a hydrophobic group having 5 or more carbon atoms is exemplified by: phenyl vinyl dimethoxy silane, phenyl vinyl diethoxy silane, phenyl methyl vinyl methoxy silane, phenyl methyl vinyl ethoxy silane, diphenyl vinyl methoxy silane, diphenyl vinyl ethoxy silane, phenyl divinyl methoxy silane, phenyl divinyl ethoxy silane, 1, 3-tetraphenyl-1, 3-divinyl disiloxane and the like.
In the case of using the above-mentioned silane compound having a radical polymerizable group and the above-mentioned silane compound having a hydrophobic group having 5 or more carbon atoms to obtain particles containing a silicone resin, the following weight ratio is preferably used. The silane compound having a radical polymerizable group and the silane compound having a hydrophobic group having 5 or more carbon atoms are preferably used in a weight ratio of 1:1 to 1:20, more preferably 1:5 to 1:15.
Among all the silane compounds used to obtain the above-mentioned particles containing the silicone resin, the ratio of the number of radical polymerizable groups to the number of hydrophobic groups having 5 or more carbon atoms is preferably 1:0.5 to 1:20m, more preferably 1:1 to 1:15.
The particles containing the silicone resin preferably have a dimethylsiloxane skeleton in which two methyl groups are bonded to one silicon atom, and the material of the silicone resin is preferably a silane compound in which two methyl groups are bonded to one silicon atom. In this case, the internal stress can be relaxed more effectively, and occurrence of rebound can be suppressed more effectively.
In the silicone resin-containing particles, it is preferable that the silane compound is reacted with a radical polymerization initiator to form a siloxane bond, from the viewpoint of further effectively relaxing the internal stress and further effectively suppressing occurrence of rebound. In general, when the above-mentioned particles containing a silicone resin are synthesized by polycondensation using an acid or base catalyst, it is difficult to obtain particles containing a silicone resin having a particle diameter of 10 μm or more and 500 μm or less, and particularly it is difficult to obtain particles containing a silicone resin having a particle diameter of 100 μm or less. In contrast, by using the radical polymerization initiator and the silane compound having the above technical characteristics, particles containing a silicone resin having a particle diameter of 1 μm or more and 500 μm or less can be obtained, particles containing a silicone resin having a particle diameter of 10 μm or more can be obtained, and particles containing a silicone resin having a particle diameter of 100 μm or less can be obtained.
In order to obtain the above-described particles containing a silicone resin, a silane compound having a hydrogen atom bonded to a silicon atom may not be used. In this case, a radical polymerization initiator may be used to polymerize the silane compound without using a metal catalyst. As a result, the particles containing the silicone resin can be made free of the metal catalyst, the content of the metal catalyst in the particles containing the silicone resin can be reduced, and the internal stress can be relaxed more effectively, and the occurrence of rebound can be suppressed more effectively.
From the viewpoint of reducing the moisture permeability, the above resin particles are preferably the following: comprises a silicone resin and a resin different from the silicone resin, and the outer surface of the silicone resin is coated with the resin different from the silicone resin. From the viewpoint of reducing the moisture permeability, the above-mentioned silicone resin-containing particles are preferably particles as follows: comprises a silicone resin and a resin different from the silicone resin, and the outer surface of the silicone resin is coated with the resin different from the silicone resin.
When the resin particles include a silicone resin and a resin other than a silicone resin, the entire outer surface of the silicone resin may be coated with the resin other than a silicone resin, or there may be a portion not coated with the resin other than a silicone resin.
Examples of the resin other than the silicone resin include a resin having a vinyl group (vinyl resin). As the above-mentioned resin other than the silicone resin, one kind may be used alone, or two or more kinds may be used in combination.
From the viewpoint of further reducing the moisture permeability, the resin other than the silicone resin is preferably a resin having a vinyl group, more preferably divinylbenzene or styrene.
The specific preparation method of the particle containing the organic silicon resin comprises the following steps: a method of polymerizing a silane compound by suspension polymerization, dispersion polymerization, miniemulsion polymerization, emulsion polymerization, or the like to prepare particles containing a silicone resin, and the like. After the polymerization of the silane compound is performed to obtain an oligomer, the polymerization of the silane compound as a polymer (oligomer or the like) is performed by a suspension polymerization method, a dispersion polymerization method, a miniemulsion polymerization method, an emulsion polymerization method, or the like, to prepare particles containing the silicone resin. For example, a silane compound having a vinyl group may be polymerized to obtain a silane compound having a vinyl group bonded to a silicon atom at the terminal. The silane compound having a phenyl group may be polymerized to obtain a silane compound having a phenyl group bonded to a silicon atom in a side chain as a polymer (oligomer or the like). The silane compound having a vinyl group and the silane compound having a phenyl group are polymerized to obtain a silane compound having a vinyl group bonded to a silicon atom at the terminal and a phenyl group bonded to a silicon atom in the side chain as a polymer (oligomer or the like).
In order to obtain resin particles in which the outer surface of the silicone resin is coated with a resin other than the silicone resin, after the silicone resin is prepared, the silicone resin may be polymerized with the resin other than the silicone resin.
(connecting Material)
The connecting material is used to form a connecting portion for connecting two members to be connected. The connecting material contains the resin particles, and further contains a binder or particles containing a metal atom. The connection material is preferably used for forming the connection portion by a sintered body of particles containing metal atoms. The binder does not contain the resin particles of the present invention. The resin particles of the present invention are not contained in the particles containing a metal atom.
The thermal decomposition temperature of the resin particles is preferably higher than the melting point of the metal atom-containing particles. The thermal decomposition temperature of the resin particles is preferably 10℃or higher, more preferably 30℃or higher, and most preferably 50℃or higher than the melting point of the metal atom-containing particles.
The metal atom-containing particles include: metal particles, metal compound particles, and the like. The metal compound particles contain a metal atom and an atom other than the metal atom. As specific examples of the above metal compound particles, there may be mentioned: metal oxide particles, metal carbonate particles, metal carboxylate particles, metal complex particles, and the like. The metal compound particles are preferably metal oxide particles. For example, the metal oxide particles are sintered after being heated in the presence of a reducing agent to form metal particles during joining. The metal oxide particles are precursors of the metal particles. Examples of the metal carboxylate particles include metal acetate particles.
Examples of the metal constituting the metal particles and the metal oxide particles include: silver, copper, gold, and the like. The metal constituting the metal particles and the metal oxide particles is preferably silver or copper, and particularly preferably silver. Therefore, the metal particles are preferably silver particles or copper particles, and more preferably silver particles. The metal oxide particles are preferably silver oxide particles or copper oxide particles, and more preferably silver oxide particles. In the case of using silver particles and silver oxide particles, residues after connection can be reduced, and the volume reduction ratio can be made very small. As examples of silver oxide in the above silver oxide particles, there may be mentioned: ag (silver) 2 O and AgO.
The above-mentioned metal atom-containing particles are preferably sintered by heating at a temperature of less than 400 ℃. The sintering temperature (sintering temperature) of the metal atom-containing particles is more preferably 350 ℃ or less, and preferably 300 ℃ or more. When the sintering temperature of the metal atom-containing particles is not lower than the lower limit and not higher than the upper limit, sintering can be efficiently performed, energy required for sintering can be further reduced, and environmental load can be reduced.
When the above-mentioned metal atom-containing particles are metal oxide particles, a reducing agent is preferably used. As examples of the above reducing agent, there may be mentioned: alcohol compounds (compounds having an alcoholic hydroxyl group), carboxylic acid compounds (compounds having a carboxyl group), amine compounds (compounds having an amino group), and the like. The above reducing agents may be used singly or in combination of two or more.
Examples of the alcohol compound include alkyl alcohols. As specific examples of the above alcohol compound, there may be mentioned, for example: ethanol, propanol, butanol, pentanol, hexanol, heptanol, octanol, nonanol, decanol, undecanol, dodecanol, tridecanol, tetradecanol, pentadecanol, hexadecanol, heptadecanol, octadecanol, nonadecanol, icosanol, and the like. The alcohol compound is not limited to primary alcohol compounds, and secondary alcohol compounds, tertiary alcohol compounds, alkanediol, and alcohol compounds having a cyclic structure may be used. Further, as the alcohol compound, a compound having a plurality of alcohol groups such as ethylene glycol and triethylene glycol can be used. Further, as the alcohol compound, a compound such as citric acid, ascorbic acid, and glucose can be used.
Examples of the carboxylic acid compound include alkyl carboxylic acids. Specific examples of the above carboxylic acid compounds include: butyric acid, valeric acid, caproic acid, enanthic acid, caprylic acid, pelargonic acid, capric acid, undecanoic acid, dodecanoic acid, tridecanoic acid, tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, octadecanoic acid, nonadecanoic acid, eicosanoic acid, and the like. The carboxylic acid compound is not limited to a primary carboxylic acid compound, and a secondary carboxylic acid compound, a tertiary carboxylic acid compound, a dicarboxylic acid, and a carboxylic compound having a cyclic structure may be used.
As examples of the above amine compound, there may be mentioned: alkylamines, and the like. Specific examples of the above-mentioned amine compound include: butylamine, pentylamine, hexylamine, heptylamine, octylamine, nonylamine, decylamine, undecylamine, dodecylamine, tridecylamine, tetradecylamine, pentadecylamine, hexadecylamine, heptadecylamine, octadecylamine, nonadecylamine, eicosanamine, and the like. Further, the above amine compound may have a branched structure. Examples of amine compounds having a branched structure include: 2-ethylhexyl amine and 1, 5-dimethylhexyl amine. The amine compound is not limited to primary amine compounds, and secondary amine compounds, tertiary amine compounds, and amine compounds having a cyclic structure can be used.
The reducing agent may be an organic substance having an aldehyde group, an ester group, a sulfonyl group, a ketone group, or the like, or an organic substance such as a metal carboxylate. The metal carboxylate may be used as a precursor of the metal particles, and may also be used as a reducing agent for the metal oxide particles because it contains an organic substance.
The content of the reducing agent is preferably 1 part by weight or more, more preferably 10 parts by weight or more, and preferably 1000 parts by weight or less, more preferably 500 parts by weight or less, and even more preferably 100 parts by weight or less, based on 100 parts by weight of the metal oxide particles. When the content of the reducing agent is not less than the lower limit, the metal atom-containing particles can be further densified and sintered. As a result, the heat release and heat resistance at the joint formed by the sintered body of the metal atom-containing particles are increased.
When a reducing agent having a melting point lower than the sintering temperature (joining temperature) of the metal atom-containing particles is used, aggregation occurs at the time of joining, and voids tend to be easily generated in the joined portion. Since the metal carboxylate is used, the metal carboxylate is not melted by heating at the time of connection, and thus generation of voids can be suppressed. In addition, a metal compound containing an organic substance may be used as a reducing agent in addition to the metal carboxylate.
The above-mentioned connecting material preferably contains an adhesive from the viewpoint of further effectively improving the connecting strength. The above adhesive is not particularly limited. Known insulating resins can be used as the above adhesive. The adhesive preferably contains a thermoplastic component (thermoplastic compound) or a curable component, and more preferably contains a curable component. Examples of the curable component include: a photocurable component and a thermosetting component. The photocurable component preferably contains a photocurable compound and a photopolymerization initiator. The thermosetting component preferably contains a thermosetting compound and a thermosetting agent. As examples of the above-mentioned binders, there may be mentioned: vinyl resins, thermoplastic resins, curable resins, thermoplastic block copolymers, and elastomers. The above binders may be used singly or in combination of two or more.
Examples of the vinyl resin include: vinyl acetate resin, acrylic resin, styrene resin, and the like. Examples of the thermoplastic resin include: polyolefin resins, ethylene-vinyl acetate copolymers, polyamide resins, and the like. Examples of the curable resin include: epoxy resins, polyurethane resins, polyimide resins, unsaturated polyester resins, and the like. The curable resin may be a room temperature curable resin, a thermosetting resin, a photo curable resin, or a moisture curable resin. The curable resin may be used in combination with a curing agent. Examples of the thermoplastic block copolymer include: styrene-butadiene-styrene block copolymers, styrene-isoprene-styrene block copolymers, hydrogenated products of styrene-butadiene-styrene block copolymers, hydrogenated products of styrene-isoprene-styrene block copolymers, and the like. Examples of the elastomer include: styrene-butadiene copolymer rubber, acrylonitrile-styrene block copolymer rubber, and the like.
In addition, the above-mentioned binder may be a solvent. Examples of the solvent include water and an organic solvent. The solvent is preferably an organic solvent from the viewpoint of further improving the removability of the solvent. The organic solvents include: alcohol compounds such as ethanol; ketone compounds such as acetone, methyl ethyl ketone, and cyclohexanone; aromatic compounds such as toluene, xylene and tetramethylbenzene; glycol ether compounds such as cellosolve, methyl cellosolve, butyl cellosolve, carbitol, methyl carbitol, butyl carbitol, propylene glycol monomethyl ether, dipropylene glycol diethyl ether, and tripropylene glycol monomethyl ether; ester compounds such as ethyl acetate, butyl lactate, cellosolve acetate, butyl cellosolve acetate, carbitol acetate, butyl carbitol acetate, propylene glycol monomethyl ether acetate, dipropylene glycol monomethyl ether acetate, and propylene carbonate; aliphatic hydrocarbon compounds such as octane and decane; and petroleum solvents such as petroleum ether and naphtha.
The above-mentioned connecting material preferably contains an epoxy resin from the viewpoint of further effectively improving the connection strength.
In the case where the connecting material contains particles containing metal atoms, the content of the particles containing metal atoms in the connecting material is preferably higher than the content of the resin particles, more preferably higher than 10% by weight or higher, and even more preferably higher than 20% by weight or higher, because the effects of the resin particles of the present invention can be effectively exerted.
The content of the resin particles in the connecting material is preferably 0.1 wt% or more, more preferably 1 wt% or more, and preferably 50 wt% or less, more preferably 30 wt% or less, based on 100 wt% of the connecting material. When the content of the resin particles is not less than the lower limit and not more than the upper limit, the internal stress in the connecting portion can be relaxed more effectively.
When the connecting material contains the metal atom-containing particles, the content of the metal atom-containing particles in 100 wt% of the connecting material is preferably 0.3 wt% or more, more preferably 3 wt% or more, and preferably 50 wt% or less, more preferably 40 wt% or less. When the content of the metal atom-containing particles is not less than the lower limit and not more than the upper limit, the connection resistance is further reduced.
When the joining material contains a binder, the content of the binder in 100% by volume of the joining material is preferably 5% by volume or more, more preferably 10% by volume or more, and preferably 40% by volume or less, more preferably 20% by volume or less. When the content of the binder is not less than the lower limit and not more than the upper limit, the connection strength can be further effectively improved.
(connection Structure)
The connection structure can be obtained by connecting the members to be connected using a connection material containing the resin particles, an adhesive or particles containing metal atoms.
The connection structure includes: the first connecting object member, the second connecting object member, and a connecting portion for connecting the first connecting object member and the second connecting object member together. The material of the connection portion includes the resin particles. The material of the connection portion is preferably the connection material. The connection portion is preferably a connection structure formed of the connection material.
Fig. 1 is a cross-sectional view showing an example of a connection structure using the resin particles of the present invention.
The connection structure 51 shown in fig. 1 includes: a first member to be connected 52, a second member to be connected 53, and a connecting portion 54 connecting the first member to be connected 52 and the second member to be connected 53.
The connection portion 54 contains the resin particles 1. The resin particles 1 do not contact both the first member to be connected 52 and the second member to be connected 53. The resin particles 1 serve as spacers for stress relaxation. In fig. 1, for convenience of explanation, resin particles 1 are schematically shown.
The connection portion 54 includes a gap controlling particle 61 and a metal connection portion 62. In the connection portion 54, one gap control particle 61 is in contact with both the first connection object member 52 and the second connection object member 53. The gap controlling particles 61 may be conductive particles or particles having no conductivity. The metal connection portion 62 is a sintered body of particles containing metal atoms. The metal connection portion 62 is formed by sintering particles containing metal atoms. The metal connection portion 62 is formed by melting particles containing metal atoms and then solidifying the same. The metal connecting portion 62 is a melt-solidified product of particles containing metal atoms.
The first connection object member may have a first electrode on a surface thereof. The second connection object member may have a second electrode on a surface thereof. The first electrode and the second electrode are preferably electrically connected by the connection portion.
The method for manufacturing the connection structure is not particularly limited. As an example of a method for manufacturing the connection structure, there is given: in the first and second connection target membersAnd a method in which the above-mentioned joining material is disposed therebetween to obtain a laminate, and then the laminate is heated and pressed. The pressure of the pressurization is 9.8X10 4 ～4.9×10 6 About Pa. The heating temperature is about 120-220 ℃. The pressurizing pressure for connecting the electrode of the flexible printed board, the electrode arranged on the resin film and the electrode of the touch control board is 9.8X10 4 ～1.0×10 6 About Pa.
Specific examples of the above-described connection object members include: electronic components such as semiconductor chips, capacitors, and diodes, electronic components such as printed boards, flexible printed boards, glass epoxy boards, and circuit boards such as glass substrates. The connection target member is preferably an electronic member. At least one of the first connection object member and the second connection object member is preferably a semiconductor wafer or a semiconductor chip. The connection structure is preferably a semiconductor device.
The connecting material is also suitable for the touch control plate. Therefore, the connection target member is preferably a flexible substrate or a connection target member in which an electrode is disposed on the surface of a resin film. The connection target member is preferably a flexible substrate, and is preferably a connection target member in which an electrode is disposed on a surface of a resin film. In the case where the flexible substrate is a flexible printed board or the like, the flexible substrate generally has an electrode on its surface.
Examples of the electrode disposed on the connection target member include: gold electrode, nickel electrode, tin electrode, aluminum electrode, copper electrode, silver electrode, molybdenum electrode, tungsten electrode, etc. In the case where the connection target member is a flexible substrate, the electrode is preferably a gold electrode, a nickel electrode, a tin electrode, or a copper electrode. In the case where the connection target member is a glass substrate, the electrode is preferably an aluminum electrode, a copper electrode, a molybdenum electrode, or a tungsten electrode. When the electrode is an aluminum electrode, the electrode may be an electrode made of aluminum alone or an electrode in which an aluminum layer is laminated on the surface of a metal oxide layer. As a material of the metal oxide layer, there can be mentioned: indium oxide doped with trivalent metal elements, zinc oxide doped with trivalent metal elements, and the like. Examples of the trivalent metal element include: sn, al, ga, and the like.
The resin particles are also useful as spacers for liquid crystal display elements. The first connection target member may be a first liquid crystal display element member. The second connection target member may be a second liquid crystal display element member. The connection portion may be a sealing portion for sealing the outer circumferences of the first liquid crystal display element member and the second liquid crystal display element member in a state where the first liquid crystal display element member and the second liquid crystal display element member are opposed to each other.
The resin particles can also be used as a sealant for liquid crystal display elements. The liquid crystal display element is provided with: the liquid crystal display device includes a first liquid crystal display element member, a second liquid crystal display element member, a sealing portion, and liquid crystal. The sealing section seals the outer peripheries of the first liquid crystal display element member and the second liquid crystal display element member in a state where the first liquid crystal display element member and the second liquid crystal display element member are opposed to each other. The liquid crystal is disposed between the first liquid crystal display element member and the second liquid crystal display element member inside the sealing portion. In this liquid crystal display element, a liquid crystal dropping process is applied, and the sealing portion is formed by thermally curing a sealing agent for the liquid crystal dropping process.
Fig. 2 is a cross-sectional view showing an example of a liquid crystal display element using the resin particles of the present invention as spacers for the liquid crystal display element.
The liquid crystal display element 81 shown in fig. 2 has a pair of transparent glass substrates 82. The transparent glass substrate 82 has an insulating film (not shown) on the opposite surface. Examples of the material of the insulating film include SiO 2 Etc. The transparent electrode 83 is formed on the insulating film of the transparent glass substrate 82. The material of the transparent electrode 83 may be ITO or the like. The transparent electrode 83 can be formed by patterning using, for example, a photolithography method. An alignment film 84 is formed on the transparent electrode 83 on the surface of the transparent glass substrate 82. Examples of the material of the alignment film 84 include polyimide and the like 。
Between the pair of transparent glass substrates 82, liquid crystal 85 is sealed. Between the pair of transparent glass substrates 82, a plurality of resin particles 1 are arranged. The resin particles 1 are used as spacers for liquid crystal display elements. The interval between the pair of transparent glass substrates 82 is limited by the plurality of resin particles 1. A sealant 86 is disposed between edges of the pair of transparent glass substrates 82. The liquid crystal 85 is prevented from flowing out to the outside by the sealant 86. The sealant 86 includes resin particles 1A having only a particle diameter different from that of the resin particles 1. In fig. 2, for convenience of explanation, the resin particles 1 and the resin particles 1A are schematically shown.
In the above liquid crystal display element, 1mm 2 The arrangement density of the spacers for a liquid crystal display element is preferably 10 pieces/mm 2 Above, and preferably 1000/mm 2 The following is given. When the above arrangement density is 10 pieces/mm 2 In the above, the cell gap becomes even further. When the above arrangement density is 1000 pieces/mm 2 In the following, the contrast of the liquid crystal display element is further improved.
Hereinafter, the present invention will be specifically described with reference to examples and comparative examples. The present invention is not limited to the following examples.
Example 1
(1) Preparation of resin particles A (polysiloxane particles A)
Solution A was prepared by dissolving 0.5 part by weight of t-butyl-2-ethyl peroxy caproate (polymerization initiator, "PERBUTYL O" manufactured by Nitro oil Co., ltd.) in 30 parts by weight of a silicone oil of acrylic acid at both ends (X-22-2445 manufactured by Xinyue chemical Co., ltd.). Further, an aqueous solution B was prepared by mixing 0.8 part by weight of a 40% by weight aqueous solution (emulsifier) of triethanolamine lauryl sulfate with 80 parts by weight of a 5% by weight aqueous solution of polyvinyl alcohol (polymerization degree: about 2000, saponification degree: 86.5 to 89 mol%, manufactured by Nippon chemical industry Co., ltd. "GOHSENOL GH-20") in 150 parts by weight of ion-exchanged water. The above solution a was added to a detachable flask placed in a warm bath, and then an aqueous solution B was added. Then, emulsification was performed using a Shirasu Porous Glass (SPG) membrane (pore average diameter about 5 μm). Then, the temperature was raised to 85℃and polymerization was carried out for 9 hours. The whole polymerized particles were washed with water by centrifugal separation, then subjected to classification operation, and then freeze-dried to obtain resin particles a (polysiloxane particles a).
(2) Preparation of the connection Material
40 parts by weight of silver particles (average particle diameter 15 nm), 1 part by weight of divinylbenzene resin particles (average particle diameter 30 μm, CV value 5%), 10 parts by weight of the above-mentioned resin particles A, and 40 parts by weight of toluene as a solvent were blended and mixed to prepare a connecting material.
(3) Preparation of connection Structure
The power semiconductor element is prepared as a first connection object member. An aluminum nitride substrate is prepared as a second connection object member.
The above-described connection material was coated on the second connection object member and made to have a thickness of about 30 μm to form a connection material layer. Then, the first joining-target member is laminated on the joining material layer, to obtain a laminate. The obtained laminate was heated at 300 ℃ for 10 minutes, whereby silver particles contained in the joining material layer were sintered to prepare a joining structure.
(4) Preparation of liquid crystal display element
Preparation of sealant for liquid crystal dropping process:
the following materials were prepared.
30 parts by weight of resin particles A (polysiloxane particles A)
50 parts by weight of bisphenol A type epoxy methacrylate (thermosetting compound, "KRM7985", manufactured by DAICEL-ALLNEX Co., ltd.)
20 parts by weight of caprolactone-modified bisphenol A type epoxyacrylate (thermosetting compound DAICEL-ALLNEX Co., ltd. "EBECRYL 3708")
30 parts by weight of a partially acrylic-modified bisphenol E-type epoxy resin (thermosetting compound, "KRM8276" manufactured by DAICEL-ALLNEX Co., ltd.)
2 parts by weight of 2, 2-dimethoxy-2-phenylacetophenone (photo radical polymerization initiator, "IRGACURE651", manufactured by BASF Japan Co., ltd.)
10 parts by weight of malonic acid dihydrazide (a thermosetting agent, "MDH" manufactured by Katsukamu chemical Co., ltd.)
20 parts by weight of silica (filler, "ADMALINE SO-C2" manufactured by ADMATECHS Co., ltd.)
2 parts by weight of 3-glycidoxypropyl trimethoxysilane (silane coupling agent, "KBM-403", from Xinyue chemical Co., ltd.)
After the above materials were mixed, stirring was performed by a planetary stirring device (AWATORIRENTARO, manufactured by THINKY Co., ltd.), and then uniform mixing was performed by a ceramic three-roll mill, to obtain a sealant (sealant) for a liquid crystal display element.
Preparation of a liquid crystal display element:
1 part by weight of spacer particles (average particle diameter: 5 μm, MICROPEARL SP-205 manufactured by water chemical Co., ltd.) was mixed with 100 parts by weight of the obtained sealant, and the spacer particles were uniformly dispersed in the sealant using a planetary stirring device. The obtained sealant containing the spacer particles was filled into a dispensing syringe (PSY-10E manufactured by MUSASHI ENGINEERING Co., ltd.) and subjected to defoaming treatment. Thereafter, a sealant containing spacer particles was applied using a dispenser (shottmaster 300 manufactured by MUSASHI ENGINEERING corporation), and drawn into a rectangular frame on the transparent electrode substrate on which the ITO thin film was formed. Then, fine droplets of a TN liquid crystal (JC-5001 LA manufactured by CHISSO Co.) were dropped onto the inside of the rectangle of the transparent electrode substrate coated with the sealant containing spacer particles by using a liquid crystal dropping device, and the coating was performed. The transparent electrode substrate coated with the sealant and the TN liquid crystal was bonded to the transparent electrode substrate not coated with the sealant and the TN liquid crystal under a vacuum of 5Pa using a vacuum bonding apparatus. Subsequently, a metal halide lamp was used at 100mW/cm 2 The part coated with the sealant was irradiated with ultraviolet rays for 30 seconds, and then heated at 120 c for 1 hour, and the sealant was thermally cured to obtain a liquid crystal display element (cellGap 5 μm).
Example 2
Resin particles B (polysiloxane particles B) were produced in the same manner as in example 1, except that "X-22-1602" manufactured by Xinyue chemical Co., ltd was used instead of "X-22-2445" manufactured by Xinyue chemical Co., ltd. A connection material, a connection structure, and a liquid crystal display element were produced in the same manner as in example 1, except that the resin particles a were changed to the resin particles B.
Example 3
(1) Preparation of resin particles C (resin-coated polysiloxane particles C)
6.5 parts by weight of the resin particles A (polysiloxane particles A) obtained in example 1, 0.6 part by weight of cetyltrimethylammonium bromide, 240 parts by weight of distilled water, and 120 parts by weight of methanol were put into a 500ml separable flask placed in a warm bath, and stirred at 40℃for 1 hour. Then, 3.0 parts by weight of divinylbenzene and 0.5 parts by weight of styrene were added to the detachable flask, and the temperature was raised to 75℃and stirred for 0.5 hours. Then, 0.4 parts by weight of dimethyl 2,2' -azobis (isobutyric acid) ester was added to a detachable flask, and stirred for 8 hours to perform polymerization reaction. After the polymerization reaction, the obtained particles were subjected to water washing by centrifugal separation to obtain resin particles C (resin-coated polysiloxane particles C).
A connection material, a connection structure, and a liquid crystal display element were obtained in the same manner as in example 1, except that the resin particles a were changed to the resin particles C.
Comparative example 1
In the same manner as in example 1 except that polysiloxane powder "KMP-605" (manufactured by singe chemical industry co., ltd.) was used instead of resin particles a in the preparation of a connection material and a liquid crystal display element, a connection material, a connection structure, and a liquid crystal display element were obtained.
Comparative example 2
In the same manner as in example 1 except that polysiloxane powder "KMP-590" (manufactured by singe chemical industry co., ltd.) was used instead of resin particles a in the preparation of a connection material and a liquid crystal display element, a connection material, a connection structure, and a liquid crystal display element were obtained.
(evaluation)
(1) Total number of T and Q units (TnQn)
By passing through 29 Si-solid NMR analysis, the total number (TnQn) of the T units and the Q units was calculated in the above-described manner, out of 100% of the total number of the M units, the D units, the T units and the Q units.
(2) Particle size
The particle size of the resin particles obtained was determined by measuring the particle size of about 100000 resin particles using a particle size distribution measuring apparatus (Multisizer 4 manufactured by Beckman Coulter Co., ltd.) and calculating an average value.
(3) Coefficient of variation (CV value)
The coefficient of variation of the obtained resin particles was measured by the above method.
(4) 10% K value
The 10% K value of the obtained resin particles was measured by the above method.
(5) Compression recovery at 40% compression set
The compression recovery rate of the obtained resin particles at 40% compression deformation was measured by the above method.
(6) Connection strength
The connection strength of the obtained connection structure at 260℃was measured using a MOUNT strength measuring apparatus. The connection strength is determined based on the following criteria.
[ criterion for connection Strength ]
O: shear strength of 150N/cm 2 Above mentioned
O: shear strength of 100N/cm 2 Above and less than 150N/cm 2
X: shear strength of less than 100N/cm 2
(7) Rebound
Whether or not springback occurred at the joint portion of the obtained joint structure was observed by a scanning electron microscope. Rebound was determined based on the following criteria.
[ criterion for rebound ]
O: no rebound occurs
X: rebound occurs
(8) Internal stress relaxation characteristics
Whether or not a crack occurred at the joint of the obtained joint structure was observed by a scanning electron microscope. The internal stress relaxation characteristics are determined based on the following criteria.
[ criterion for internal stress relaxation Properties ]
O: no cracking occurred
X: crack is generated
(9) Cold and hot cycle characteristics (connection reliability)
The obtained connection structure was subjected to a cold and hot cycle test in which the connection structure was heated from-65 ℃ to 150 ℃ and then cooled to-65 ℃ for 1000 times. Whether or not cracks and peeling occurred in the connection portion was observed by an ultrasonic flaw detector (SAT). The cold-hot cycle characteristics (connection reliability) are determined based on the following criteria.
[ criterion for judging Cold-Hot cycle characteristics (connection reliability) ]
O: the joint is not cracked or peeled
X: cracking or peeling of the joint
(10) Moisture permeability
The obtained liquid crystal display element was stored in an atmosphere of a temperature of 80 ℃ and a humidity of 90% rh for 72 hours, and then was subjected to AC 3.5V voltage driving, and the periphery of the sealing portion of the halftone was visually observed. Moisture permeability was determined based on the following criteria.
[ criterion for moisture permeability ]
O: no color unevenness around the sealing portion
Delta: slight color unevenness occurred around the sealing portion
X: obvious color unevenness occurs around the sealing part
The results are shown in Table 1 below.
TABLE 1
Symbol description
Resin particles
1a. resin particles
51. the connection structure
First connection object part
53. the second connecting object member
54. the connection part
61.
62. Metal connection
81. liquid crystal display element
82. transparent glass substrate
83. transparent electrode
84. oriented film
85. liquid crystal
86. sealant
Claims (11)
1. A resin particle, wherein,
by the general formula [ (R) 3 SiO 1/2 ]M unit represented by the general formula [ (R) 2 SiO 2/2 ]D unit represented by the general formula [ (R) SiO) 3/2 ]T unit represented by the general formula [ SiO ] 4/2 ]The total number of the T units and the Q units is not more than 4% in 100% of the total number of the Q units,
the coefficient of variation of the particle diameter is 4.5% or less,
the resin particles have a compression recovery rate of 10% or less when deformed by compression of 40%.
2. The resin particles according to claim 1, which have a 10% K value of 500N/mm 2 The following is given.
3. The resin particles according to claim 1 or 2, which have a particle diameter of 0.5 μm or more and 500 μm or less.
4. The resin particle according to claim 1 or 2, which is a particle comprising a silicone resin.
5. The resin particle according to claim 1 or 2, which is used as a spacer.
6. A connecting material comprising the resin particles according to any one of claims 1 to 5, further comprising a binder or particles containing a metal atom.
7. The connecting material of claim 6 comprising an adhesive.
8. The connecting material according to claim 6 or 7, comprising particles containing metal atoms.
9. The connecting material of claim 8, wherein,
the thermal decomposition temperature of the resin particles is higher than the melting point of the metal atom-containing particles.
10. The connecting material according to claim 8, which is used to form a connecting portion that connects two connecting object members;
and for forming the connection portion by a sintered body of the metal atom-containing particles.
11. A connection structure is provided with:
a first connecting object member,
Second connection target member
A connection section that connects the first connection object member and the second connection object member together, wherein,
the material of the connecting portion comprises the resin particles according to any one of claims 1 to 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| JP (1) | JP7092670B2 (en) |
| KR (1) | KR102584161B1 (en) |
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| WO2023090457A1 (en) * | 2021-11-22 | 2023-05-25 | 積水化学工業株式会社 | Adhesive particles and laminate |
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| CN102666620A (en) * | 2009-10-23 | 2012-09-12 | 道康宁公司 | Hydrophilically-modified silicone compositions |
| CN102918087A (en) * | 2010-05-31 | 2013-02-06 | 三洋化成工业株式会社 | Resin particle and method for producing same |
| WO2016088812A1 (en) * | 2014-12-04 | 2016-06-09 | 積水化学工業株式会社 | Silicone particles, sealing agent for liquid crystal dropping methods, and liquid crystal display element |
| JP2016108563A (en) * | 2014-12-04 | 2016-06-20 | 積水化学工業株式会社 | Base material particle, conductive particle, conductive material and connection structure |
| CN107709414A (en) * | 2015-11-11 | 2018-02-16 | 积水化学工业株式会社 | Particle, particulate material, connecting material and connection structural bodies |
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| JP4860214B2 (en) | 2004-09-07 | 2012-01-25 | モメンティブ・パフォーマンス・マテリアルズ・ジャパン合同会社 | Method for producing spherical silicone elastomer fine particles and cosmetics |
| JP5044331B2 (en) * | 2007-07-30 | 2012-10-10 | 三洋化成工業株式会社 | Production method of resin particles |
| JP5607001B2 (en) | 2011-08-11 | 2014-10-15 | 信越化学工業株式会社 | Silicone fine particles and method for producing the same |
| WO2013108842A1 (en) * | 2012-01-20 | 2013-07-25 | 積水化学工業株式会社 | Conductive particles, conductive material and connection structure |
| JP2015140356A (en) | 2014-01-27 | 2015-08-03 | 大東化成工業株式会社 | Spongy silicone fine particle, manufacturing method therefor and cosmetic |
| JP6859077B2 (en) * | 2015-11-11 | 2021-04-14 | 積水化学工業株式会社 | Particle material, connecting material and connecting structure |
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- 2018-04-25 JP JP2018532346A patent/JP7092670B2/en active Active
- 2018-04-25 CN CN202310664640.1A patent/CN116675819A/en active Pending
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102666620A (en) * | 2009-10-23 | 2012-09-12 | 道康宁公司 | Hydrophilically-modified silicone compositions |
| CN102918087A (en) * | 2010-05-31 | 2013-02-06 | 三洋化成工业株式会社 | Resin particle and method for producing same |
| WO2016088812A1 (en) * | 2014-12-04 | 2016-06-09 | 積水化学工業株式会社 | Silicone particles, sealing agent for liquid crystal dropping methods, and liquid crystal display element |
| JP2016108563A (en) * | 2014-12-04 | 2016-06-20 | 積水化学工業株式会社 | Base material particle, conductive particle, conductive material and connection structure |
| CN107709414A (en) * | 2015-11-11 | 2018-02-16 | 积水化学工业株式会社 | Particle, particulate material, connecting material and connection structural bodies |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110088160A (en) | 2019-08-02 |
| CN116675819A (en) | 2023-09-01 |
| KR20190139194A (en) | 2019-12-17 |
| JPWO2018203500A1 (en) | 2020-03-12 |
| TW201843214A (en) | 2018-12-16 |
| JP7092670B2 (en) | 2022-06-28 |
| WO2018203500A1 (en) | 2018-11-08 |
| KR102584161B1 (en) | 2023-10-04 |
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