JP2010043211A - 高温耐性接着剤組成物、基板の接着方法、及び3次元半導体装置 - Google Patents
高温耐性接着剤組成物、基板の接着方法、及び3次元半導体装置 Download PDFInfo
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- JP2010043211A JP2010043211A JP2008209197A JP2008209197A JP2010043211A JP 2010043211 A JP2010043211 A JP 2010043211A JP 2008209197 A JP2008209197 A JP 2008209197A JP 2008209197 A JP2008209197 A JP 2008209197A JP 2010043211 A JP2010043211 A JP 2010043211A
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- QCLHXCDKGCQCDS-UHFFFAOYSA-N dimethoxy-methyl-(4-trimethoxysilylbutyl)silane Chemical compound CO[Si](C)(OC)CCCC[Si](OC)(OC)OC QCLHXCDKGCQCDS-UHFFFAOYSA-N 0.000 description 1
- YXFVGUFLCFUJSH-UHFFFAOYSA-N dimethoxy-methyl-(5-trimethoxysilylpentyl)silane Chemical compound CO[Si](C)(OC)CCCCC[Si](OC)(OC)OC YXFVGUFLCFUJSH-UHFFFAOYSA-N 0.000 description 1
- CVQVSVBUMVSJES-UHFFFAOYSA-N dimethoxy-methyl-phenylsilane Chemical compound CO[Si](C)(OC)C1=CC=CC=C1 CVQVSVBUMVSJES-UHFFFAOYSA-N 0.000 description 1
- YQGOWXYZDLJBFL-UHFFFAOYSA-N dimethoxysilane Chemical compound CO[SiH2]OC YQGOWXYZDLJBFL-UHFFFAOYSA-N 0.000 description 1
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- 125000004817 pentamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
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- GXOHBWLPQHTYPF-UHFFFAOYSA-N pentyl 2-hydroxypropanoate Chemical compound CCCCCOC(=O)C(C)O GXOHBWLPQHTYPF-UHFFFAOYSA-N 0.000 description 1
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- 238000006116 polymerization reaction Methods 0.000 description 1
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- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
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- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000013464 silicone adhesive Substances 0.000 description 1
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- 239000011734 sodium Substances 0.000 description 1
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- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
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- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
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- 239000004094 surface-active agent Substances 0.000 description 1
- RAOIDOHSFRTOEL-UHFFFAOYSA-N tetrahydrothiophene Chemical compound C1CCSC1 RAOIDOHSFRTOEL-UHFFFAOYSA-N 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000004634 thermosetting polymer Substances 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 description 1
- GFKCWAROGHMSTC-UHFFFAOYSA-N trimethoxy(6-trimethoxysilylhexyl)silane Chemical compound CO[Si](OC)(OC)CCCCCC[Si](OC)(OC)OC GFKCWAROGHMSTC-UHFFFAOYSA-N 0.000 description 1
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 description 1
- HTGSSSRYYQJTLN-UHFFFAOYSA-N tris(2-dimethylsilyl-2-methoxyethyl)-methylsilane Chemical compound COC(C[Si](C)(CC(OC)[SiH](C)C)CC(OC)[SiH](C)C)[SiH](C)C HTGSSSRYYQJTLN-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on 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; Adhesives based on derivatives of such polymers
- C09J183/02—Polysilicates
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on 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; Adhesives based on derivatives of such polymers
- C09J183/14—Adhesives based on 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; Adhesives based on derivatives of such polymers in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/48—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
- C08G77/50—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms by carbon linkages
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/48—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
- C08G77/50—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms by carbon linkages
- C08G77/52—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms by carbon linkages containing aromatic rings
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/48—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
- C08G77/54—Nitrogen-containing linkages
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
- C09J5/06—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving heating of the applied adhesive
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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Abstract
【解決手段】環状構造を含んでいてもよい直鎖状もしくは分岐状、又は環状の脂肪族炭化水素基、複素環含有基、又は芳香環含有炭化水素基による架橋により結ばれた1対以上のケイ素原子を有すると共に、3つ以上の水酸基及び/又は加水分解性基を有するシラン化合物を含む縮合物前駆体の単体又は混合物を加水分解・縮合して得たケイ素系高分子化合物であり、かつ該ケイ素系高分子化合物に含まれる全ケイ素原子に対し、前記脂肪族炭化水素基、複素環含有基、又は芳香環含有炭化水素基による架橋との直接の結合を持つケイ素原子の割合が90モル%以上であるケイ素系高分子化合物を熱硬化性結合剤として含有する高温耐性接着剤組成物。
【選択図】なし
Description
炭素数1〜10の環状構造を含んでいてもよい直鎖状もしくは分岐状、又は環状の脂肪族炭化水素基、炭素数4又は8の複素環含有基、又は炭素数6〜12の芳香環含有炭化水素基による架橋により結ばれた1対以上のケイ素原子を有すると共に、3つ以上の水酸基及び/又は加水分解性基を有するシラン化合物
を含む縮合物前駆体の単体あるいは混合物を加水分解・縮合して得たケイ素系高分子化合物であり、
かつ該ケイ素系高分子化合物に含まれる全ケイ素原子に対し、前記脂肪族炭化水素基、複素環含有基、又は芳香環含有炭化水素基による架橋との直接の結合を持つケイ素原子の割合が90モル%以上であるケイ素系高分子化合物を熱硬化性結合剤として含有する高温耐性接着剤組成物である(請求項1)。
上記のような、高分子化合物に含まれる90モル%以上のケイ素原子が炭素との結合による架橋を少なくとも1つ有するケイ素系高分子化合物を、上記のようなケイ素化合物を用いて調製し、熱硬化性結合剤として用いることにより、高温における熱耐性という要求と、ヒートショック等に対する耐性という要求を同時に満たす高温耐性接着剤を得ることができる。
で示される構造を有することが好ましい(請求項2)。
で示されるシラン化合物を挙げることができる(請求項4)。
好ましく利用できる芳香族炭化水素基(芳香環含有炭化水素基)としては、ベンゼン環、ナフタレン環、アントラセン環を持つものが同様に例示される。芳香族炭化水素基の場合、熱安定性を挙げる設計とするためには、芳香環に直接ケイ素原子が結合したものが有利であり、弾性率を低く抑えるためにはケイ素原子と環の間には1以上のメチレン基を介したものであることが好ましいが、熱安定性を考慮した場合には2以上のメチレン基を介したものであることが好ましい。なお、上記例示のものでは、熱安定性と低い弾性率で広くバランスをとりやすいという意味では、多環式のものを除く脂肪族炭化水素基の選択が最も好ましいものである。
で示される構造を有することが好ましい。上記Rで示される基は炭素数1〜12の置換基を有していてもよい脂肪族あるいは芳香環を含有する1価炭化水素基であるが、このRは比較的炭素数の多い直鎖の脂肪族である場合には焼結膜の弾性率をある程度低くする効果はあるものの、重要な効果となるものではない。また、熱安定性の点から見ると、メチル基など分岐のない単鎖のものが優れる。しかし、側鎖の分解自体は接着性に極めて重大な問題を発生させるものではないため、比較的自由に選択しても問題がない。材料の入手と熱安定性の点からバランスがとれているものとしてメチル基、エチル基、プロピル基、ブチル基、ペンチル基、ヘキシル基、シクロペンチル基、シクロヘキシル基や、フェニル基を挙げることができるが、上記の通り、それに限定されるものではない。
で示されるシラン類等が例示される。
で示されるものを挙げることができる。本成分は主要材料ではないためRは上記要件の中で広く選択することができ、また、Yは好ましくは水素原子、水酸基、あるいは炭素数1〜4のアルコキシ基である。これらのうち、熱耐性を改善したい場合にはsが3あるいは4のものを用いることによって改善効果を得ることができる。
この中で特に好ましいのは、沸点が100℃以下のものである。
これらは1種又は2種以上を混合して使用することができる。
また、上記加水分解・縮合により得られるケイ素系高分子化合物の重合度は、ゲルパーミエーションクロマトグラフィー(GPC)によるポリスチレン換算重量平均分子量で、300〜100000、より好ましくは500〜50000であることが好ましい。
濃硝酸0.16gを223gの超純水中に溶解した溶液を室温で撹拌しながら、1,2−ビス(メチルジメトキシシリル)エタン51.1gと1−(メチルジメトキシシリル)−2−(ジメチルメトキシシリル)エタン47.6gと4−メチル−2−ペンタノン13gの溶液を添加した。反応液は徐々に発熱し50℃に達したが、30分後には室温に戻った。12時間この状態で撹拌を続けた。この反応液にプロピレングリコールモノメチルエーテルアセテート(以下PGMEA)300gを加え、低沸点溶媒を減圧で留去した。この間エバポレータのバス温度は30℃以下に保った。得られた残留溶液に酢酸エチル500ml、超純水500mlを加え、分液ロートに移して水層を除去した。有機層は超純水200mlで更に2回洗浄した。得られた有機層にプロピレングリコールモノメチルエーテルアセテート300gを加え、エバポレータで溶媒留去した結果210gの溶液が得られ、これを接着剤組成物母液とした。なお、この溶液の不揮発残分は14.7質量%であり、ゲルパーミエーションクロマトグラフィー(GPC)によりその重量平均分子量を測定したところ、1952であった。
合成例1の1,2−ビス(メチルジメトキシシリル)エタン51.1gと1−(メチルジメトキシシリル)−2−(ジメチルメトキシシリル)エタン47.6gの混合物を、1,2−ビス(メチルジメトキシシリル)エタン102.2gに変更した以外は、合成例1に記述した方法に従って接着剤組成物母液を得た。なお、この溶液の不揮発残分は20.4質量%であり、ゲルパーミエーションクロマトグラフィー(GPC)によりその重量平均分子量を測定したところ、2092であった。
合成例1の1,2−ビス(メチルジメトキシシリル)エタン51.1gと1−(メチルジメトキシシリル)−2−(ジメチルメトキシシリル)エタン47.6gの混合物を、ビス[2−(メチルジメトキシシリル)エチル]ジメトキシシラン146.0g(0.41mol)とメチルトリメトキシシラン13.6g(0.1mol)の混合物に変更した以外は、合成例1に記述した方法に従って接着剤組成物母液を得た。なお、この溶液の不揮発残分は16.2質量%であり、ゲルパーミエーションクロマトグラフィー(GPC)によりその重量平均分子量を測定したところ、2764であった。
合成例1の1,2−ビス(メチルジメトキシシリル)エタン51.1gと1−(メチルジメトキシシリル)−2−(ジメチルメトキシシリル)エタン47.6gの混合物を、1,2−ビス(メチルジメトキシシリル)エタン71.4g(0.3mol)と1,3,5−トリメトキシ−1,3,5−トリシラシクロヘキサン19.8g(0.075mol)の混合物に変更した以外は、合成例1に記述した方法に従って接着剤組成物母液を得た。なお、この溶液の不揮発残分は18.2質量%であり、ゲルパーミエーションクロマトグラフィー(GPC)によりその重量平均分子量を測定したところ、2966であった。
合成例1の1,2−ビス(メチルジメトキシシリル)エタン51.1gと1−(メチルジメトキシシリル)−2−(ジメチルメトキシシリル)エタン47.6gの混合物を、1,2−ビス(メチルジメトキシシリル)エタン71.4g(0.3mol)とトリス(2−メトキシジメチルシリルエチル)メチルシラン29.6g(0.075mol)の混合物に変更した以外は、合成例1に記述した方法に従って接着剤組成物母液を得た。なお、この溶液の不揮発残分は15.2質量%であり、ゲルパーミエーションクロマトグラフィー(GPC)によりその重量平均分子量を測定したところ、3042であった。
合成例1の1,2−ビス(メチルジメトキシシリル)エタン51.1gと1−(メチルジメトキシシリル)−2−(ジメチルメトキシシリル)エタン47.6gの混合物を、メチルトリメトキシシラン116.7gに変更した以外は、合成例1に記述した方法に従って接着剤組成物母液を得た。なお、この溶液の不揮発残分は20.8質量%であり、ゲルパーミエーションクロマトグラフィー(GPC)によりその重量平均分子量を測定したところ、2062であった。
合成例1の1,2−ビス(メチルジメトキシシリル)エタン51.1gと1−(メチルジメトキシシリル)−2−(ジメチルメトキシシリル)エタン47.6gの混合物を、メチルトリメトキシシラン58.6g(0.43mol)とジメチルジメトキシシラン51.7g(0.43mol)に変更した以外は、合成例1に記述した方法に従って接着剤組成物母液を得た。なお、この溶液の不揮発残分は22.2質量%であり、ゲルパーミエーションクロマトグラフィー(GPC)によりその重量平均分子量を測定したところ、1064であった。
エタノール188.4g、超純水93.44g、25%水酸化テトラメチルアンモニウム8.26gを混合した溶液を撹拌しながら60℃に加温した。この溶液中にメチルトリメトキシシラン19.5gとテトラエトキシシラン36.43gの混合液を6時間かけて滴下した。得られた反応液を氷水で冷却して室温にした後、シュウ酸2gとPGMEA200mlを添加し、得られた溶液をエバポレータにより溶媒留去し、残留液が161gになるまで溶媒を留去した。このようにして得られた溶液に酢酸エチル200g、超純水120gを加え、分液ロートで洗浄、静置した。分離した水層を除いてから有機層を更に2回、超純水120mlを用いて水洗した。この様にして得られた有機層にPGMEA120mlを加えた後、エバポレータにより溶媒を留去して208gまで濃縮してガス透過膜形成用組成物母液とした。なお、この溶液の不揮発残分は21.3質量%であった。
この母液を1500r.p.m.の回転速度でシリコンウェハー上に塗布し、これを120℃,2分、230℃,2分のベークを行なった後、425℃,1時間加熱して、約100nmの厚さのガス透過膜を得た。
上記ガス透過膜を成膜したシリコンウェハーに、合成例1で得られた接着剤組成物を1500r.p.m.の回転速度で塗布し、ホットプレートを用いて100℃にて1分間加熱し、溶媒を蒸発させて接着用基板を作製した。この時の接着層前駆体膜の膜厚は約500nmであった。この基板を2枚、接着層を内側にして基板接合装置EVG520(イー・ヴィー・グループ社製)にセットした。接着は10mbarの減圧下、150℃にて行い、5kNの圧力をかけながら、10℃/分で300℃まで加熱し、2分保持後、同じ速度で150℃まで冷却した。
接着後のサンプルの接着力をカミソリテストで測定したところ、接着力は約3J/m2であった。また、日立建機ファインテック製超音波映像装置FS300IIを用いた接着面の観測では、剥がれや欠陥はみられず、良好な接着面が観測された。
実施例1と同様の方法によりに合成例2〜5で得られた接着剤組成物を同様の方法によって用いて接着試験を行ったところ、接着力はそれぞれ、約2、3、1.5、1.5J/m2であり、接着面の観察でも剥がれや欠陥がみられず、良好な接着面が観測された。
実施例1と同様の方法により、比較合成例1及び2で得られた接着剤組成物を用いて接着試験を行ったところ、接着力はそれぞれ0.5、1.5J/m2であった。一方、接着面の観察では何れの接着面にも剥がれや欠陥が観測され、良好な接着面とはいえなかった。
弾性率の測定は上記合成例1〜5及び比較合成例1,2で得た接着剤組成物をそれぞれシリコンウェハー上に塗布、400℃,1時間焼成した膜(膜厚約500nm)に関して薄膜機械的特性評価システム(MTS社製Nano Indenter SA2)を用いて行った。結果を表1に示す。
質量減少量の測定は、Rigaku社製THERMO FLEX TAS300 TG8101Dを用いて窒素気流中で行い、400℃に昇温直後の質量を100%とし、400℃を維持し、1時間経過後の質量減少を測定する手法で行った。結果を表2に示す。
Claims (10)
- 炭素数1〜10の環状構造を含んでいてもよい直鎖状もしくは分岐状、又は環状の脂肪族炭化水素基、炭素数4又は8の複素環含有基、又は炭素数6〜12の芳香環含有炭化水素基による架橋により結ばれた1対以上のケイ素原子を有すると共に、3つ以上の水酸基及び/又は加水分解性基を有するシラン化合物
を含む縮合物前駆体の単体又は混合物を加水分解・縮合して得たケイ素系高分子化合物であり、
かつ該ケイ素系高分子化合物に含まれる全ケイ素原子に対し、前記脂肪族炭化水素基、複素環含有基、又は芳香環含有炭化水素基による架橋との直接の結合を持つケイ素原子の割合が90モル%以上であるケイ素系高分子化合物を熱硬化性結合剤として含有する高温耐性接着剤組成物。 - 上記ケイ素系高分子化合物に含まれる上記脂肪族炭化水素基、複素環含有基、又は芳香環含有炭化水素基による架橋との直接の結合を持つケイ素原子は、下記一般式(1)
で示される構造を有することを特徴とする請求項1記載の高温耐性接着剤組成物。 - 上記一般式(1)において、p+q≧3であるケイ素原子数は、一般式(1)に含まれる全ケイ素原子数に対し70モル%以上である請求項2記載の高温耐性接着剤組成物。
- 上記架橋により結ばれた1対以上のケイ素原子を有すると共に、3つ以上の水酸基及び/又は加水分解性基を有するシラン化合物は、下記一般式(2),(3)又は(4)
で示されるいずれかを含むものである請求項1乃至3のいずれか1項記載の高温耐性接着剤組成物。 - 上記一般式(2)〜(4)において、少なくとも1つのrはr≧2であり、少なくとも1つのsはs≧1であり、少なくとも1つのtはt≧1である請求項4記載の高温耐性接着剤組成物。
- 請求項1乃至5のいずれか1項に記載の高温耐性接着剤組成物を基板上に塗布して接着層前駆体膜を形成し、接着層前駆体膜を挟んで接着を行う基板同士を合わせ、接着層前駆体膜を加熱により硬化させて基板同士の接着を行うことを特徴とする基板の接着方法。
- ケイ素系高分子材料を用いて形成した接着層前駆体膜により基板を接着する基板の接着方法において、1μm以上の粒径を持つ粒子を含まず、400℃以下の温度で硬化を行った後に得られる硬化膜の弾性率は4GPa以下であり、かつ該硬化膜を400℃に昇温した後400℃で60分間加熱した際の質量減少が3%以下である接着層前駆体膜を用いて基板同士の接着を行う基板の接着方法。
- 接着層前駆体膜が請求項1乃至5のいずれか1項に記載の高温耐性接着剤組成物から形成されたものである請求項7記載の基板の接着方法。
- 上記接着を行う基板は半導体製造用基板である請求項6乃至8のいずれか1項に記載の基板の接着方法。
- 請求項6乃至9のいずれか1項に記載の接着方法を用いて製造した3次元半導体装置。
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Publication number | Publication date |
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CN101649177A (zh) | 2010-02-17 |
KR20100021353A (ko) | 2010-02-24 |
EP2154708A1 (en) | 2010-02-17 |
JP4911143B2 (ja) | 2012-04-04 |
US8277600B2 (en) | 2012-10-02 |
TWI464227B (zh) | 2014-12-11 |
US20100040895A1 (en) | 2010-02-18 |
CN101649177B (zh) | 2013-08-21 |
KR20140146029A (ko) | 2014-12-24 |
TW201022395A (en) | 2010-06-16 |
KR101623655B1 (ko) | 2016-05-23 |
EP2154708B1 (en) | 2017-07-26 |
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