CN113444589A - 用于清除聚合物的组合物 - Google Patents
用于清除聚合物的组合物 Download PDFInfo
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- CN113444589A CN113444589A CN202110320229.3A CN202110320229A CN113444589A CN 113444589 A CN113444589 A CN 113444589A CN 202110320229 A CN202110320229 A CN 202110320229A CN 113444589 A CN113444589 A CN 113444589A
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- 239000000203 mixture Substances 0.000 title claims abstract description 69
- 229920000642 polymer Polymers 0.000 title claims abstract description 59
- -1 fluorinated alkyl compound Chemical class 0.000 claims abstract description 79
- 239000003880 polar aprotic solvent Substances 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims description 45
- 125000004432 carbon atom Chemical group C* 0.000 claims description 29
- 238000009835 boiling Methods 0.000 claims description 19
- 150000001875 compounds Chemical class 0.000 claims description 18
- 125000000217 alkyl group Chemical group 0.000 claims description 17
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 10
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 claims description 8
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 6
- 229920001296 polysiloxane Polymers 0.000 claims description 6
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- 239000010452 phosphate Substances 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 5
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 5
- IZXIZTKNFFYFOF-UHFFFAOYSA-N 2-Oxazolidone Chemical compound O=C1NCCO1 IZXIZTKNFFYFOF-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
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- VEAZEPMQWHPHAG-UHFFFAOYSA-N n,n,n',n'-tetramethylbutane-1,4-diamine Chemical compound CN(C)CCCCN(C)C VEAZEPMQWHPHAG-UHFFFAOYSA-N 0.000 claims description 4
- NJBCRXCAPCODGX-UHFFFAOYSA-N 2-methyl-n-(2-methylpropyl)propan-1-amine Chemical compound CC(C)CNCC(C)C NJBCRXCAPCODGX-UHFFFAOYSA-N 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 3
- 150000001408 amides Chemical class 0.000 claims description 3
- 239000003660 carbonate based solvent Substances 0.000 claims description 3
- 239000005453 ketone based solvent Substances 0.000 claims description 3
- DMQSHEKGGUOYJS-UHFFFAOYSA-N n,n,n',n'-tetramethylpropane-1,3-diamine Chemical compound CN(C)CCCN(C)C DMQSHEKGGUOYJS-UHFFFAOYSA-N 0.000 claims description 3
- UQKAOOAFEFCDGT-UHFFFAOYSA-N n,n-dimethyloctan-1-amine Chemical compound CCCCCCCCN(C)C UQKAOOAFEFCDGT-UHFFFAOYSA-N 0.000 claims description 3
- 150000002825 nitriles Chemical class 0.000 claims description 3
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 claims description 3
- 150000003462 sulfoxides Chemical class 0.000 claims description 3
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 claims description 3
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 claims description 3
- IIFFFBSAXDNJHX-UHFFFAOYSA-N 2-methyl-n,n-bis(2-methylpropyl)propan-1-amine Chemical compound CC(C)CN(CC(C)C)CC(C)C IIFFFBSAXDNJHX-UHFFFAOYSA-N 0.000 claims description 2
- TXXWBTOATXBWDR-UHFFFAOYSA-N n,n,n',n'-tetramethylhexane-1,6-diamine Chemical compound CN(C)CCCCCCN(C)C TXXWBTOATXBWDR-UHFFFAOYSA-N 0.000 claims description 2
- ORSUTASIQKBEFU-UHFFFAOYSA-N n,n-diethylbutan-1-amine Chemical compound CCCCN(CC)CC ORSUTASIQKBEFU-UHFFFAOYSA-N 0.000 claims description 2
- OOHAUGDGCWURIT-UHFFFAOYSA-N n,n-dipentylpentan-1-amine Chemical compound CCCCCN(CCCCC)CCCCC OOHAUGDGCWURIT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 description 25
- 239000002184 metal Substances 0.000 description 25
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- 238000005260 corrosion Methods 0.000 description 22
- 230000007797 corrosion Effects 0.000 description 21
- FPGGTKZVZWFYPV-UHFFFAOYSA-M tetrabutylammonium fluoride Chemical compound [F-].CCCC[N+](CCCC)(CCCC)CCCC FPGGTKZVZWFYPV-UHFFFAOYSA-M 0.000 description 16
- 229920005573 silicon-containing polymer Polymers 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- 230000000694 effects Effects 0.000 description 14
- 230000002000 scavenging effect Effects 0.000 description 14
- 238000000034 method Methods 0.000 description 12
- 239000002998 adhesive polymer Substances 0.000 description 11
- 125000001931 aliphatic group Chemical group 0.000 description 11
- 229910001128 Sn alloy Inorganic materials 0.000 description 9
- 239000010408 film Substances 0.000 description 9
- 150000002222 fluorine compounds Chemical class 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 229920001187 thermosetting polymer Polymers 0.000 description 8
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- SJRJJKPEHAURKC-UHFFFAOYSA-N N-Methylmorpholine Chemical compound CN1CCOCC1 SJRJJKPEHAURKC-UHFFFAOYSA-N 0.000 description 6
- 239000004205 dimethyl polysiloxane Substances 0.000 description 6
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 5
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- 229920002050 silicone resin Polymers 0.000 description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 125000005210 alkyl ammonium group Chemical group 0.000 description 4
- DKPFZGUDAPQIHT-UHFFFAOYSA-N butyl acetate Chemical compound CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- CATSNJVOTSVZJV-UHFFFAOYSA-N heptan-2-one Chemical compound CCCCCC(C)=O CATSNJVOTSVZJV-UHFFFAOYSA-N 0.000 description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 4
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- ZFPGARUNNKGOBB-UHFFFAOYSA-N 1-Ethyl-2-pyrrolidinone Chemical compound CCN1CCCC1=O ZFPGARUNNKGOBB-UHFFFAOYSA-N 0.000 description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 229910001316 Ag alloy Inorganic materials 0.000 description 3
- 229910001020 Au alloy Inorganic materials 0.000 description 3
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 125000003172 aldehyde group Chemical group 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- KFSZGBHNIHLIAA-UHFFFAOYSA-M benzyl(trimethyl)azanium;fluoride Chemical compound [F-].C[N+](C)(C)CC1=CC=CC=C1 KFSZGBHNIHLIAA-UHFFFAOYSA-M 0.000 description 3
- 229910052794 bromium Inorganic materials 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 125000004093 cyano group Chemical group *C#N 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000003112 inhibitor Substances 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 3
- UWHSPZZUAYSGTB-UHFFFAOYSA-N 1,1,3,3-tetraethylurea Chemical compound CCN(CC)C(=O)N(CC)CC UWHSPZZUAYSGTB-UHFFFAOYSA-N 0.000 description 2
- RXYPXQSKLGGKOL-UHFFFAOYSA-N 1,4-dimethylpiperazine Chemical compound CN1CCN(C)CC1 RXYPXQSKLGGKOL-UHFFFAOYSA-N 0.000 description 2
- HPYNZHMRTTWQTB-UHFFFAOYSA-N 2,3-dimethylpyridine Chemical compound CC1=CC=CN=C1C HPYNZHMRTTWQTB-UHFFFAOYSA-N 0.000 description 2
- BWZVCCNYKMEVEX-UHFFFAOYSA-N 2,4,6-Trimethylpyridine Chemical compound CC1=CC(C)=NC(C)=C1 BWZVCCNYKMEVEX-UHFFFAOYSA-N 0.000 description 2
- JYYNAJVZFGKDEQ-UHFFFAOYSA-N 2,4-Dimethylpyridine Chemical compound CC1=CC=NC(C)=C1 JYYNAJVZFGKDEQ-UHFFFAOYSA-N 0.000 description 2
- XWKFPIODWVPXLX-UHFFFAOYSA-N 2,5-dimethylpyridine Chemical compound CC1=CC=C(C)N=C1 XWKFPIODWVPXLX-UHFFFAOYSA-N 0.000 description 2
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 description 2
- QQZOPKMRPOGIEB-UHFFFAOYSA-N 2-Oxohexane Chemical compound CCCCC(C)=O QQZOPKMRPOGIEB-UHFFFAOYSA-N 0.000 description 2
- BSKHPKMHTQYZBB-UHFFFAOYSA-N 2-methylpyridine Chemical compound CC1=CC=CC=N1 BSKHPKMHTQYZBB-UHFFFAOYSA-N 0.000 description 2
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- HWWYDZCSSYKIAD-UHFFFAOYSA-N 3,5-dimethylpyridine Chemical compound CC1=CN=CC(C)=C1 HWWYDZCSSYKIAD-UHFFFAOYSA-N 0.000 description 2
- ITQTTZVARXURQS-UHFFFAOYSA-N 3-methylpyridine Chemical compound CC1=CC=CN=C1 ITQTTZVARXURQS-UHFFFAOYSA-N 0.000 description 2
- HCFAJYNVAYBARA-UHFFFAOYSA-N 4-heptanone Chemical compound CCCC(=O)CCC HCFAJYNVAYBARA-UHFFFAOYSA-N 0.000 description 2
- FKNQCJSGGFJEIZ-UHFFFAOYSA-N 4-methylpyridine Chemical compound CC1=CC=NC=C1 FKNQCJSGGFJEIZ-UHFFFAOYSA-N 0.000 description 2
- FFWSICBKRCICMR-UHFFFAOYSA-N 5-methyl-2-hexanone Chemical compound CC(C)CCC(C)=O FFWSICBKRCICMR-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 2
- QCOGKXLOEWLIDC-UHFFFAOYSA-N N-methylbutylamine Chemical compound CCCCNC QCOGKXLOEWLIDC-UHFFFAOYSA-N 0.000 description 2
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- IPTNXMGXEGQYSY-UHFFFAOYSA-N acetic acid;1-methoxybutan-1-ol Chemical compound CC(O)=O.CCCC(O)OC IPTNXMGXEGQYSY-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
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- QUKGYYKBILRGFE-UHFFFAOYSA-N benzyl acetate Chemical compound CC(=O)OCC1=CC=CC=C1 QUKGYYKBILRGFE-UHFFFAOYSA-N 0.000 description 2
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- 238000002845 discoloration Methods 0.000 description 2
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- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 2
- NGAZZOYFWWSOGK-UHFFFAOYSA-N heptan-3-one Chemical compound CCCCC(=O)CC NGAZZOYFWWSOGK-UHFFFAOYSA-N 0.000 description 2
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- 229910052740 iodine Inorganic materials 0.000 description 2
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- MBHINSULENHCMF-UHFFFAOYSA-N n,n-dimethylpropanamide Chemical compound CCC(=O)N(C)C MBHINSULENHCMF-UHFFFAOYSA-N 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- YLYBTZIQSIBWLI-UHFFFAOYSA-N octyl acetate Chemical compound CCCCCCCCOC(C)=O YLYBTZIQSIBWLI-UHFFFAOYSA-N 0.000 description 2
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- 238000001556 precipitation Methods 0.000 description 2
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- CMUTXJXHVDKYAN-UHFFFAOYSA-L tetrabutylazanium difluoride Chemical compound [F-].[F-].CCCC[N+](CCCC)(CCCC)CCCC.CCCC[N+](CCCC)(CCCC)CCCC CMUTXJXHVDKYAN-UHFFFAOYSA-L 0.000 description 2
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- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了用于清除聚合物的组合物,所述组合物包含:氟化烷基化合物、极性非质子溶剂和胺化合物,其中,所述胺化合物包括非环状仲胺化合物或非环状叔胺化合物。
Description
相关申请的交叉引用
本申请要求2020年3月26日提交的日本专利申请No.10-2020-0036615的权益,其全部内容通过引用方式并入本申请中。
技术领域
本发明涉及用于清除硅酮聚合物的组合物。
背景技术
在制造半导体装置时,在半导体晶片(以下,简称为“晶片”)的前表面(以下,称为“电路表面”)上形成电子电路等之后,存在进行背研磨(这是对晶片的背表面进行研磨的过程)以减小晶片的厚度的情况。在这种情况下,为了保护晶片的电路表面或防止晶片移动,通常通过粘合聚合物(例如,硅酮聚合物)将支撑物粘附到晶片的电路表面。粘附到晶片的电路表面的支撑物具有以下优点:增强通过背研磨而变薄的晶片,并且允许在晶片的经研磨的背表面上形成背电极。
在执行背研磨和形成背电极之后,从晶片的电路表面去除支撑物,剥离粘合聚合物,并且对晶片进行切割以生产半导体芯片。
近年来,已经开发并使用了采用作为形成为延伸穿过晶片的电极的贯通电极(例如,硅贯通电极)的芯片堆叠技术。根据芯片堆叠技术,由于多个芯片的电子电路通过贯通电极而不是典型的导线电连接,所以实现电子电路的高密度集成和高速操作是可能的。当使用这种芯片堆叠技术时,经常执行背研磨以减小其中堆叠有多个芯片的组件的厚度。因此,支撑物和粘合聚合物的使用正在增加。
关于此问题,通常通过粘合聚合物将支撑物粘附到晶片的电路表面,然后将粘合聚合物热固化以将支撑物牢固地粘附到晶片。因此,当剥离粘合聚合物时,固化的粘合聚合物可能残留在晶片的电路表面上。因此,需要一种有效清除残留在晶片电路表面上的固化的粘合聚合物的手段。另外,当清除粘合聚合物时,存在的问题是金属膜或凸球(bumpball)可能由于金属腐蚀而被损坏。
专利文献1公开了一种用于清除粘合聚合物的组合物。但是,该组合物的问题在于对于网状聚合物的清除速率慢。
现有技术的文献
专利文献
(专利文献1)韩国专利申请公布No.10-2014-0060389
发明内容
为了解决上述现有技术中出现的问题而完成本发明,并且本发明的目的在于提供一种用于清除聚合物的组合物,该组合物能够有效且快速地清除在半导体装置制造过程中残留在晶片的电路表面上的粘合聚合物,而不引起金属腐蚀。
本发明的效果、特征和目的不限于上述的那些,并且本领域普通技术人员根据以下描述可以清楚地理解上文未提及的其他效果、特征和目的。
为了实现本发明的目的,提供了一种用于清除聚合物的组合物,该组合物包括氟化烷基化合物、极性非质子溶剂和胺化合物。胺化合物包括非环状仲胺化合物或非环状叔胺化合物。
根据本发明,提供了一种清除聚合物的组合物,其能够通过包括非环状仲胺或非环状叔胺来提高聚合物清除速率。特别地,本发明的清除聚合物的组合物能够高速清除基于硅酮的聚合物,并且能够通过防止金属腐蚀而最小化对金属膜或凸球的损坏。
具体实施方式
本发明涉及一种清除聚合物的组合物,该组合物包含氟化合物、溶剂和胺化合物。氟化合物是氟化烷基化合物,溶剂是极性非质子溶剂,且胺化合物是非环状仲胺化合物或非环状叔胺化合物。
在本发明中,烷基是指与单键结合的烃基。
<用于清除聚合物的组合物>
根据本发明,用于清除聚合物的组合物包含氟化烷基化合物、极性非质子溶剂和胺化合物。该组合物可以进一步包含其他添加剂,并且可以用于清除硅酮聚合物。
用该组合物清除的聚合物没有特别限制,但优选为硅酮聚合物。具体地,硅酮聚合物包括线性聚合物和网状聚合物。例如,硅酮聚合物包括通过固化形成网状聚合物的基于聚有机硅氧烷的树脂以及线性非反应性聚二甲基硅氧烷聚合物。
特别地,本发明的组合物具有不仅清除线性聚合物而且清除网状聚合物的优点,因为氟化烷基化合物分解并溶解硅酮聚合物。
根据本发明,由于胺化合物将组合物的pH调节至合适的水平,因此可以在聚合物清除期间获得防止金属腐蚀的效果。因此,可以防止对金属膜或凸球的损坏。具体地,该组合物可以通过防止金属腐蚀来保护金属(诸如Sn、Sn/Ag合金和Sn/Au合金)。在这种情况下,可以保护的金属不限于此。
此外,根据本发明的清除聚合物的组合物不包含有意添加的水。优选地,清除聚合物的组合物不含水。但是,如果需要,可以使用氟化烷基化合物的水合物。在这种情况下,清除聚合物的组合物可以包含少量水。在这种情况下,相对于组合物的总重量,水可以按重量计小于4%的量包含在组合物中。当水的含量超过该范围时,聚合物清除性降低并且金属腐蚀增加。
此外,优选地,根据本发明的清除聚合物的组合物在其分子结构中不包含具有羟基(-OH)基团的化合物,例如基于醇的化合物。在化合物的分子结构中具有羟基基团的情况下,存在羟基基团抑制氟化合物的活性而使硅酮树脂的清除性降低的问题。
(A)氟化烷基化合物
根据本发明的清除聚合物的组合物包含氟化烷基化合物。氟化烷基化合物通过断开聚合物(例如硅酮聚合物)的环来降低分子量。
在本发明中,氟化烷基化合物的实例是烷基氟化铵。具体地,氟化烷基化合物的实例包括一种或多种由式4-1或式4-2表示的化合物。
[式4-1]
在式4-1中,R6至R9各自为具有3至10个碳原子(C3至C10)的烷基。当R6至R9各自为具有两个或更少个碳原子(C2或更少)的烷基时,由于氟化合物在溶剂中的溶解度降低,因此在混合后立即发生沉淀,或者在混合后经过一定时间发生沉淀。
[式4-2]
在式4-2中,R10至R12各自为具有1至10个碳原子(C1至C10)的烷基。
例如,作为氟化烷基化合物,单独地或组合地使用一种或多种选自四丁基二氟化铵(TBAF·HF)、四丁基氟化铵(TBAF)、四辛基氟化铵(TOAF)、以及苄基三甲基氟化铵(BTMAF)中的化合物。
当烷基氟化铵以水合物形式存在时,烷基氟化铵的实例包括四正丁基氟化铵水合物、四正丁基氟化铵三水合物、苄基三甲基氟化铵水合物等。
相对于清除聚合物的组合物的总重量,以按重量计为0.1%至20%、优选为按重量计0.5%至17%的量包含氟化烷基化合物。当以按重量计小于0.1%的量包含氟化合物时,存在不能有效地清除粘附在电子部件上的聚合物(硅酮树脂)的问题。另一方面,当以按重量计为20%或更多的量包含氟化合物并且它以水合物型烷基氟化铵的形式存在时,含水量增加,从而使清除聚合物(诸如硅酮树脂)的效果变差。另外,金属膜由于过量的氟化物而被腐蚀。
(B)极性非质子溶剂
根据本发明的清除聚合物的组合物包含极性非质子溶剂。极性非质子溶剂溶胀硅酮聚合物并溶解氟化合物和分解的硅酮聚合物。
作为通常已知的溶剂,水和基于醇的化合物(例如,二甘醇单甲醚、乙二醇、异丙醇等)由于与氟离子的氢键结合而难以清除聚合物。因此,优选地,根据本发明的清除聚合物的组合物中的溶剂不包含水基于或醇的化合物。
极性非质子溶剂包括至少一种选自由以下组成的组的溶剂:基于酮的溶剂、基于乙酸酯的溶剂、基于酰胺的溶剂、基于吡啶的溶剂、基于吗啉的溶剂、基于吡咯烷酮的溶剂、基于脲的溶剂、基于磷酸酯的溶剂、基于亚砜的溶剂、基于腈的溶剂、基于碳酸酯的溶剂、基于噁唑烷酮的溶剂、以及基于哌嗪的溶剂。
具体地,基于酮的溶剂的实例包括由式5-1表示的化合物:
[式5-1]
在式5-1中,R13和R14各自独立地为具有1至18个碳原子(C1至C18)的线性或支化的脂族烃,并且R13和R14的碳原子数总和优选为2或更大且小于30。
酮溶剂的实例包括2-庚酮、3-庚酮、4-庚酮、3-戊酮、2-己酮、3-己酮、4-甲基-2-戊酮、5-甲基-2-己酮和2,6-二甲基-4-己酮,但不限于此。
具体地,基于乙酸酯的溶剂的实例包括乙酸甲酯、乙酸乙酯(EA)、乙酸丙酯、乙酸异丙酯、乙酸正丁酯、乙酸异丁酯、乙酸仲丁酯、乙酸戊酯(amyl acetate)、乙酸戊酯(pentyl acetate)、乙酸异戊酯、乙酸辛酯、乙酸苄酯、乙酸苯酯、乙酸乙氧基乙酯、乙酸甲氧基丁酯(MBA)、丙二醇单甲醚乙酸酯(PGMEA)、乙酸乙烯酯或乙氧基丙酸乙酯(EEP)等,但不限于此。
具体地,基于酰胺的溶剂的实例包括N,N-二甲基乙酰胺、N,N-二乙基乙酰胺、N,N-二丙基乙酰胺、N-乙基-N-甲基乙酰胺、N,N-二甲基丙酰胺(N,N-dimethylpropionamide)、N,N-二甲基丁酰胺、N,N-二甲基异丁酰胺、N,N-二甲基戊酰胺、N,N-二甲基丙酰胺(N,N-dimethylpropanamide)、N,N-二乙基丙酰胺和N,N-二丁基丙酰胺,但不限于此。
具体地,基于吡啶的溶剂的实例包括由式5-2表示的化合物:
[式5-2]
在式5-2中,R15至R17各自独立地为氢、具有1至10个碳原子(C1至C10)的线性或支化的脂族烃基、卤素(例如,F、Cl、Br、I)、醛基(-CHO)、乙醛基(-COCH3)、具有1至4个碳原子(C1至C4)的烷氧基、乙烯基、乙炔基、氰基(-CN)或甲基硫基(-SCH3)。
吡啶溶剂的实例包括吡啶、2-甲基吡啶、3-甲基吡啶、4-甲基吡啶、4-乙基吡啶、4-丙基吡啶、4-异丙基吡啶、4-戊基吡啶、2,3-二甲基吡啶、2,4-二甲基吡啶、2,5-二甲基吡啶、3,4-二甲基吡啶、3,5-二甲基吡啶和2,4,6-三甲基吡啶,但不限于此。
具体地,吗啉溶剂的实例包括由式5-3表示的化合物:
[式5-3]
在式5-3中,R18为氢,具有1至6个碳原子(C1至C6)的线性或支化的脂族烃基,乙烯基,氰基(-CN),具有1至4个碳原子(C1至C4)且被叔胺取代的脂族烃基,或被具有1至4个碳原子(C1至C4)的烷基、氰基(-CN)、卤素基团(例如,F、Cl、Br或I)或醛基(-CHO)取代的苯基或吡啶基;X是氧或-NR19-;且R19为具有1至4个碳原子(C1至C4)的脂族烃基。
基于吗啉的溶剂的实例包括N-甲基吗啉、N-乙基吗啉、N-芳基吗啉、N-丁基吗啉、N-异丁基吗啉等,但不限于此。
具体地,基于吡咯烷酮的溶剂的实例包括N-甲基吡咯烷酮(NMP)、N-乙基吡咯烷酮(NEP)和N-乙烯基吡咯烷酮(NVP),但不限于此。
具体地,基于脲的溶剂的实例包括由式5-4表示的化合物:
[式5-4]
在式5-4中,X为氧或-NR19-,并且R19和R20各自独立地为具有1至6个碳原子(C1至C6)的线性、支化或环状的脂族烃基,或具有1至4个碳原子(C1至C4)且被乙烯基、苯基、乙炔基、甲氧基或二甲基氨基取代的脂族烃基。
基于脲的溶剂的实例包括四甲基脲、四乙基脲、四丁基脲等,但不限于此。
具体地,基于磷酸酯的溶剂的实例包括由式5-5表示的化合物:
[式5-5]
在式5-5中,R21至R23各自独立地为具有1至8个碳原子(C1至C8)的线性或支化的脂族烃基、具有3至8个碳原子(C3至C8)且与相邻氧形成环的二价脂族烃基、未取代或被具有1至4个碳原子(C1至C4)的脂族烃基取代的苯基、具有2至4个碳原子且被卤素(例如F、Cl、Br或I)取代的脂族烃基、或被卤素取代的苯基。在具有1至8个碳原子(C1至C8)的线性或支化的脂族烃基中包含的基团“-CH2-”可被氧原子取代。
基于磷酸酯的溶剂的实例包括磷酸三乙酯、磷酸三丁酯、磷酸三戊酯、三芳基磷酸酯等,但不限于此。
具体地,基于亚砜的溶剂的实例包括二甲基亚砜(DMSO)、二丁基亚砜、二苯基亚砜、二苄基亚砜和甲苯基亚砜,但不限于此。
具体地,基于腈的溶剂的实例包括丙腈、丁腈、异丁腈、乙腈、三甲基乙腈和苯乙腈,但不限于此。
具体地,基于碳酸酯的溶剂的实例包括碳酸二甲酯(DMC)、碳酸二乙酯、碳酸二苯酯、碳酸二苄酯、碳酸亚乙酯、碳酸丙烯酯(PC)和碳酸亚乙烯酯,但不限于此。
具体地,基于噁唑烷酮的溶剂的实例包括2-噁唑烷酮、3-甲基-2-噁唑烷酮等,但不限于此。
基于哌嗪的溶剂的实例包括二甲基哌嗪、二丁基哌嗪等,但不限于此。
另一方面,根据本发明,极性非质子溶剂不包括后文描述的非环状叔胺。
相对于清除聚合物的组合物的总重量,以按重量计为60%至99.89%、优选地按重量计为68%至99.45%的量包含极性非质子溶剂。当以按重量计小于60%的量包含极性非质子溶剂时,存在金属膜被腐蚀的问题。另一方面,当以按重量计超过99.89%的量包含极性非质子溶剂时,存在不能有效地清除粘附在电子部件上的硅酮树脂的问题。
(C)胺化合物
根据本发明的清除聚合物的组合物包含胺化合物,并且所述胺化合物是非环状仲胺化合物或非环状叔胺化合物。胺化合物促进硅酮聚合物的溶胀并改善氟化烷基化合物的溶解度,从而提高硅酮聚合物的清除速率。在本发明中,通过将清除聚合物的组合物的pH调节至适当的水平,胺化合物表现出防腐蚀作用。
就最大化清除聚合物的组合物中的胺化合物的功能效果而言,适合使用具有特定结构的胺化合物。例如,当胺的烷基中的碳原子数增加时,溶胀硅酮聚合物的作用增强,而当胺的烷基中的碳原子数减少时,改善氟化烷基化合物的溶解度的效果增强。另外,氟化烷基化合物的电离性越好,发生的腐蚀就越多。为了获得互补效果,使用胺化合物。也就是说,胺化合物改善了聚合物的清除并减轻了金属的腐蚀。具体地,优选使用具有下述特定结构的胺化合物。
具体地,用于本发明的胺化合物的实例包括由式1至式3中的任一者表示的化合物。
[式1]
在式1中,R1和R2各自独立地表示具有1至8个碳原子(C1至C8)的线性或支化的烷基。当R1和R2相同时,R1和R2优选表示具有4个或更多个碳原子的烷基。
更优选地,R1和R2各自独立地表示具有2个至8个碳原子(C2至C8)的线性或支化的烷基。当R1和R2相同时,R1和R2优选表示具有4个至8个碳原子(C4至C8)的线性或支化的烷基。
[式2]
在式2中,R3至R5各自表示具有1至8个碳原子(C1至C8)的烷基。
[式3]
在式3中,n是3、4、5和6中的正整数。
胺化合物优选为沸点为140℃或更高的胺化合物,更优选为沸点在140℃至300℃范围内的胺化合物。当胺化合物满足式1至式3中的一者并且沸点为140℃或更高时,由于挥发性组分被最小化,因此根据本发明的清除聚合物的组合物可以容易地应用于装置制造工艺中。当胺化合物的沸点为140℃或更高时,不仅可以预期提高聚合物清除性能的效果,还可以预期防止金属腐蚀的效果。当胺化合物的沸点低于140℃时,预期聚合物清除性能有很大的改善,但是防止金属腐蚀的效果不明显。因此,难以同时获得提高聚合物清除性能的效果和防止金属腐蚀的效果。
例如,胺化合物包括一种或多种选自由以下组成的组中的化合物:三丙胺(沸点为158℃)、三丁胺(沸点为215℃)、三戊胺(沸点为242℃)、三异丁胺(沸点为191℃)、二甲基辛胺(沸点为192℃)、二乙基丁胺(沸点为141℃)、二异丁胺(沸点为141℃)、N,N,N',N'-四甲基-1,3-二氨基丙烷(沸点为144℃)、N,N,N',N'-四甲基-1,4-二氨基丁烷(沸点为169℃)和N,N,N',N'-四甲基-1,6-二氨基己烷(沸点为209℃)。
相对于清除聚合物的组合物的总重量,以按重量计0.01%至20%、优选0.05%至15%的量包含胺化合物。当以小于0.01%的量包含胺化合物时,难以预期清除速率的提高。另一方面,当胺化合物的含量按重量计超过20%时,聚合物溶胀效果不与所含胺化合物的量成比例地增加,并且金属腐蚀增加。
(D)添加剂
除了上述组分外,根据本发明的清除聚合物的组合物任选地包含其他组分,诸如本领域中常用的腐蚀抑制剂和表面活性剂。
腐蚀抑制剂用于在清除树脂期间有效地抑制含金属的底膜的腐蚀。腐蚀抑制剂可从各种来源商购获得,且无需进一步纯化即可使用。
表面活性剂用于增强清除聚合物的效果。例如,可以使用阴离子表面活性剂、阳离子表面活性剂和非离子型表面活性剂。其中,优选使用具有优异的润湿性且产生少量气泡的非离子型表面活性剂。一种或多种选自这些表面活性剂中的表面活性剂可以单独使用或组合使用。
本发明还提供了一种使用根据本发明的清除聚合物的组合物从装置中清除聚合物的方法。结合根据本发明的清除聚合物的组合物描述的所有细节可以应用于根据本发明的聚合物清除方法。在下文中,尽管将不给出多余的详细描述,但是这些可以应用于根据本发明的聚合物清除方法。
具体地,聚合物清除方法是用于清除在晶片薄化工艺中使用的聚合物(诸如硅粘合剂)的方法。晶片薄化工艺包括在载体晶片和装置晶片之间形成硅酮分离层和硅酮粘合剂层的步骤以及使装置晶片变薄的步骤。硅酮分离层用作分离位置,在该分离位置处去除载体晶片,而不损坏装置晶片。硅酮粘合剂将装置晶片粘合到载体晶片上,并进行固化过程。在这样的工艺之后,使用根据本发明的清除聚合物的组合物清除固化的聚合物。
将参考下面描述的实施例更详细地描述本发明。实施例旨在更详细地描述本发明,但是本发明的范围不限于这些实施例。
实施例和比较例:制备清除聚合物的组合物
根据表1和表2中列出的成分和组成比率制备清除聚合物的组合物。
[表1]
[表2]
<氟化合物>
(A-1)TBAF·HF:四丁基二氟化铵;
(A-2)TBAF:四丁基氟化铵;
(A-3)BTMAF:苄基四甲基氟化铵;
(A-20)氟化铵(NH4HF2)
<溶剂>
(B-1)2-庚酮;(B-2)N,N-二乙基乙酰胺;
(B-3)N,N-二甲基丙酰胺(N,N-dimethylpropanamide);(B-4)N-乙基吡咯烷酮;
(B-5)N-甲基吗啉;(B-6)乙酸正丁酯;
(B-7)PGMEA:丙二醇单甲醚乙酸酯;
(B-8)4-甲基吡啶;(B-9)二甲基哌嗪;
(B-10)三乙基磷酸酯;(B-11)四乙基脲;
(B-20)乙二醇;(B-21)异丙醇
(B-22)水;(B-23)二乙二醇单甲醚
<胺化合物>
(C-1)三丙胺(沸点158℃);
(C-2)二异丁胺(沸点141℃);
(C-3)三丁胺(沸点215℃);
(C-4)二甲基辛胺(沸点192℃);
(C-5)N,N,N',N'-四甲基-1,3-二氨基丙烷(沸点144℃);
(C-6)三乙基胺(沸点89℃);
(C-20)辛胺(沸点176℃);
(C-21)单乙醇胺(沸点174℃);
(C-22)羟胺(沸点58℃);
(C-23)四甲基氢氧化铵水溶液(20%)(沸点102℃)
(C-24)二丙胺
(C-25)N-甲基丁胺
(测试实施例1)聚合物清除性评估1—网状聚合物
为了评价网状聚合物的清除性,将涂覆固化硅酮聚合物至80μm厚度的晶片切成尺寸为2cm×2cm的小块,并将小块用作样品。将根据实施例和比较例的各个组合物的溶液加热至25℃并以400rpm旋转。将制备的样品在各个组合物溶液中浸泡1分钟,用异丙醇(IPA)洗涤,并干燥。在将样品浸入组合物溶液中之前,通过扫描电子显微镜(SEM)测量每个样品的固化硅酮聚合物的膜厚度。在将样品浸泡、洗涤和干燥后,用扫描电子显微镜(SEM)测量每个样品中残留的硅酮树脂的厚度,并计算每种组合物溶液的清除速率,并汇总在表3和表4中。
清除速率(μm/min)=[测试前厚度(μm)-测试后厚度(μm)]/测试时间(分钟)
(测试实施例2)聚合物清除性评估2—线性PDMS
为了评估线性聚二甲基硅氧烷(PDMS)的清除性,将通过以预定的质量比混合聚二甲基硅氧烷(PDMS)的预聚物和固化剂而获得的混合物旋涂在硅晶片上且切成尺寸为2cm×2cm的小块,将小块用作样品。将根据实施例和比较例的组合物溶液加热至25℃并以400rpm旋转。将样品在各个组合物溶液中浸泡1分钟,用IPA洗涤,并干燥。测试后,用光学显微镜和SEM观察每个样品表面上的残留物。表3和表4中标出了每个样品上是否存在残留物。
○:不存在/X:存在
(测试实施例3)金属腐蚀评估1—凸球
为了评估金属腐蚀,将具有1011个由Sn、Sn/Ag合金或Sn/Au合金制成的凸球的晶片切成尺寸为2cm×2cm的小块,并将小块用作样品。将制备的样品在根据实施例和比较例的各个组合物溶液中浸泡30分钟,同时将组合物溶液加热至25℃并以400rpm旋转,用IPA洗涤,并干燥。用SEM观察各个样品。将每个样品中损坏的凸球的数量计数并汇总在表3和表4中。
(测试实施例4)金属腐蚀评估2—金属膜
将涂覆有铝薄膜的晶片切成尺寸2cm×2cm的小块,并将小块用作样品。将根据实施例和比较例的各个组合物的溶液加热至25℃并以400rpm旋转。将制备的样品在各个组合物溶液中浸泡10分钟,用异丙基醇(IPA)洗涤,并干燥。洗涤后,各个样品上的薄膜用SEM检查缺陷,并且根据下述标准将结果汇总在表3和表4中。
良好:未观察到表面形态学变化或变色。
发生:观察到表面形态学变化和变色。
[表3]
[表4]
参见表3,根据本发明的清除聚合物的组合物(实施例1至实施例21)对于基于网状硅酮的聚合物表现出23μm/min或更大的高清除速率,并且对于基于线性硅酮的聚合物表现出优异的清除性能。另外,根据本发明的组合物表现出良好的抗腐蚀作用。当使用具有低沸点的胺化合物时(实施例21),或者当以过量添加胺化合物时(实施例20),性能略有降低,但是明显优于比较例的性能。
另一方面,参考表4,在均没有使用根据本发明的胺化合物的比较例7和比较例10至比较例12对于网状聚合物表现出12μm/min或更小的清除速率。也就是说,与使用根据实施例的组合物的情况相比,清除速率显著降低且金属的腐蚀也显著增加。
另外,即使在使用根据本发明的胺化合物时,但当在使用水或基于醇的化合物作为溶剂的情况下(比较例5和比较例6),证实了聚合物清除是困难的且金属腐蚀非常高。在均使用质子溶剂的比较例8和比较例9中,聚合物清除速率低,并且在清除聚合物之后仍有残留物。
另一方面,当单独使用极性非质子溶剂时,没有清除聚合物(比较例1和比较例2)。当使用氟化铵作为氟化合物时(比较例3),在组合物的制备过程中发生沉淀,使得不能进行评估。另外,在分别使用二丙胺和N-甲基丁胺作为胺化合物的比较例13和比较例14中,网状聚合物的清除速率降低至20μm/min或更少,且在由Sn、Sn/Ag合金或Sn/Au合金制成的1011个凸球中,有40个或更多个凸球被损坏。
Claims (8)
1.一种用于清除聚合物的组合物,所述组合物包含:氟化烷基化合物、极性非质子溶剂和胺化合物,其中,所述胺化合物包括非环状仲胺化合物或非环状叔胺化合物。
4.根据权利要求1所述的组合物,其中,所述极性非质子溶剂包括至少一种选自由以下组成的组中的溶剂:基于酮的溶剂、基于乙酸酯的溶剂、基于酰胺的溶剂、基于吡啶的溶剂、基于吗啉的溶剂、基于吡咯烷酮的溶剂、基于脲的溶剂、基于磷酸酯的溶剂、基于亚砜的溶剂、基于腈的溶剂、基于碳酸酯的溶剂、基于噁唑烷酮的溶剂、以及基于哌嗪的溶剂。
5.根据权利要求1所述的组合物,其中,所述胺化合物包括至少一种选自由以下组成的组中的化合物:三丙胺、三丁胺、三戊胺、三异丁胺、二甲基辛胺、二乙基丁胺、二异丁胺、N,N,N',N'-四甲基-1,3-二氨基丙烷、N,N,N',N'-四甲基-1,4-二氨基丁烷、以及N,N,N',N'-四甲基-1,6-二氨基己烷。
6.根据权利要求1所述的组合物,其中,所述胺化合物的沸点在140℃至300℃的范围内。
7.根据权利要求1所述的组合物,其中,所述组合物用于清除基于硅酮的聚合物。
8.根据权利要求1所述的组合物,其中,相对于所述组合物的总重量,所述组合物包含按重量计0.1%至20%的所述氟化烷基化合物、按重量计60%至99.89%的所述极性非质子溶剂和按重量计0.01%至20%的所述胺化合物。
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