JP2009235218A - Adhesive composition and cleaning method - Google Patents
Adhesive composition and cleaning method Download PDFInfo
- Publication number
- JP2009235218A JP2009235218A JP2008082489A JP2008082489A JP2009235218A JP 2009235218 A JP2009235218 A JP 2009235218A JP 2008082489 A JP2008082489 A JP 2008082489A JP 2008082489 A JP2008082489 A JP 2008082489A JP 2009235218 A JP2009235218 A JP 2009235218A
- Authority
- JP
- Japan
- Prior art keywords
- adhesive composition
- mass
- alcohol
- compound
- acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000853 adhesive Substances 0.000 title claims abstract description 71
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 71
- 239000000203 mixture Substances 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000004140 cleaning Methods 0.000 title claims abstract description 11
- 229920001577 copolymer Polymers 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 150000001875 compounds Chemical class 0.000 claims abstract description 20
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 17
- 229930195729 fatty acid Natural products 0.000 claims abstract description 17
- 239000000194 fatty acid Substances 0.000 claims abstract description 17
- 235000007586 terpenes Nutrition 0.000 claims abstract description 17
- 150000003505 terpenes Chemical class 0.000 claims abstract description 15
- 239000004094 surface-active agent Substances 0.000 claims abstract description 14
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 12
- 239000004014 plasticizer Substances 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 22
- 239000012459 cleaning agent Substances 0.000 claims description 17
- 150000001298 alcohols Chemical class 0.000 claims description 10
- 125000004432 carbon atom Chemical group C* 0.000 claims description 7
- VOWAEIGWURALJQ-UHFFFAOYSA-N Dicyclohexyl phthalate Chemical group C=1C=CC=C(C(=O)OC2CCCCC2)C=1C(=O)OC1CCCCC1 VOWAEIGWURALJQ-UHFFFAOYSA-N 0.000 claims description 5
- 125000000217 alkyl group Chemical group 0.000 claims description 4
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- 150000004671 saturated fatty acids Chemical class 0.000 claims description 2
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- 238000005498 polishing Methods 0.000 abstract description 14
- 239000002173 cutting fluid Substances 0.000 abstract description 10
- 238000005406 washing Methods 0.000 abstract description 10
- 230000007613 environmental effect Effects 0.000 abstract description 9
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- 238000005520 cutting process Methods 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 8
- 238000000576 coating method Methods 0.000 description 8
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- 239000000155 melt Substances 0.000 description 4
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Landscapes
- Adhesives Or Adhesive Processes (AREA)
Abstract
Description
本発明は、電子部品、光学部品などの部材を加工処理する際に、一時的にこれらの部材を仮止め接着しておくために使用する仮止め用の固形接着剤組成物（以下、単に「接着剤組成物」という場合がある）に関し、さらに詳しくは、アルカリ性の切削液や研磨液などの加工液に対する耐性が優れており、加工後、不要となった接着剤を環境負荷が少ないアルコール系洗浄剤で洗浄できる接着剤組成物および洗浄方法に関する。 The present invention provides a temporary adhesive solid adhesive composition (hereinafter simply referred to as “a temporary adhesive composition”) that is used for temporarily adhering these members temporarily when processing members such as electronic components and optical components. More specifically, the adhesive composition may be referred to as “adhesive composition”, and is more excellent in resistance to processing fluids such as alkaline cutting fluid and polishing fluid. The present invention relates to an adhesive composition that can be cleaned with a cleaning agent and a cleaning method.
従来、シリコンウエハーなどの電子部品、ガラスなどの光学部品などの部材は、それらを切削あるいは研磨加工処理する際に、上記部材が動かないように接着剤組成物を使用して一時的に仮止め接着しておく必要があり、加工処理が終了すると不要となった接着剤は、ハロゲン系や芳香族炭化水素系などの有機溶剤系洗浄剤、過酸化水素を用いた酸化性洗浄剤、発煙硝酸などの洗浄剤を使用して洗浄除去されていた。 Conventionally, electronic parts such as silicon wafers and optical parts such as glass are temporarily fixed temporarily using an adhesive composition so that the members do not move when they are cut or polished. Adhesives that need to be bonded and are no longer needed after processing is complete are organic solvent-based cleaners such as halogen and aromatic hydrocarbons, oxidizing cleaners using hydrogen peroxide, fuming nitric acid It was removed by washing using a cleaning agent.
近年、上記の仮止め接着に使用される接着剤組成物としては、上記の環境負荷が大きい従来の洗浄剤などに代わって、環境上の負荷の少ないアルカリ水溶液の洗浄剤で容易に洗浄除去ができるアルカリ可溶性樹脂を主成分とするものが使用されてきている。 In recent years, as an adhesive composition used for the above-mentioned temporary bonding, it can be easily washed and removed with a cleaning agent of an alkaline aqueous solution having a low environmental load instead of the conventional cleaning agent having a large environmental load. Those having an alkali-soluble resin as a main component have been used.
上記の接着剤組成物としては、ある種のウエハーの仮着用接着剤（特許文献１）が開示されている。しかしながら、特許文献１に開示の接着剤は、ロジン、その他のアビエチン酸を主成分とする樹脂、該樹脂の誘導体、該樹脂の二塩基酸との変性物などのアルカリ可溶性樹脂を主成分としているために、電子部品、光学部品などの部材を、アルカリ性の切削液や研磨液などを使用して、加工処理した場合に、加工中に仮止め接着剤が上記の加工液によって侵され、支持台に仮止めされている上記部材が動く危険性があり、精密な精度を有する切削や研磨が出来ない。 As said adhesive composition, the adhesive for temporary wearing of a certain wafer (patent document 1) is disclosed. However, the adhesive disclosed in Patent Document 1 is mainly composed of an alkali-soluble resin such as rosin, other resins containing abietic acid as a main component, derivatives of the resin, and modified products of the resin with dibasic acids. Therefore, when a member such as an electronic component or an optical component is processed using an alkaline cutting liquid or polishing liquid, the temporary fixing adhesive is attacked by the above processing liquid during the processing, and the support base There is a risk that the above-mentioned member temporarily fixed to the metal will move, and cutting and polishing with precise accuracy cannot be performed.
また、加工処理後、不要となった接着剤をアルカリ水溶液で洗浄除去するが、比較的に高濃度のアルカリ剤を使用するために作業環境がよくなく、さらに、洗浄除去後、洗浄液中のアルカリ成分が残る危険性があるために、さらに、水洗を充分に行う必要があり、洗浄工程で水を使用するために乾燥に時間がかかるという難点がある。 In addition, after processing, the unnecessary adhesive is washed away with an alkaline aqueous solution, but the working environment is not good due to the use of a relatively high concentration alkaline agent. Since there is a risk that the components remain, it is necessary to sufficiently perform washing with water, and there is a problem that it takes time to dry because water is used in the washing process.
上述のことから、アルカリ性の切削液や研磨液などの加工液に対する耐性が優れており、加工後、不要となった接着剤を環境負荷が少ない洗浄剤を用いて容易に洗浄除去できる接着剤組成物および洗浄方法が要望されている。 Because of the above, the adhesive composition has excellent resistance to processing fluids such as alkaline cutting fluid and polishing fluid, and can be easily cleaned and removed after processing using a cleaning agent with less environmental impact Things and cleaning methods are desired.
従って、本発明の目的は、塗布性、仮止めの接着性を損なわず、アルカリ性の切削液や研磨液などの加工液に対する耐性が優れており、環境負荷が少ないアルコール系洗浄剤で容易に洗浄除去できる接着剤組成物および洗浄方法を提供することである。 Therefore, the object of the present invention is to easily wash with an alcohol-based cleaning agent that does not impair applicability and adhesiveness of temporary fixing, has excellent resistance to processing fluids such as alkaline cutting fluid and polishing fluid, and has a low environmental impact. It is to provide an adhesive composition and cleaning method that can be removed.
本発明者は、前記の課題を解決すべく鋭意検討した結果、下記の特定成分からなる接着剤組成物が、塗布性、仮止めの接着性を損なわず、切削液や研磨液など加工液に対する耐アルカリ性が優れており、環境負荷が少ないアルコール系洗浄剤で容易に洗浄除去できることを見出した。すなわち、本発明は、軟化点が９０℃〜１６０℃のテルペンフェノール共重合体（ａ）と、高級脂肪酸、高級アルコール、および可塑剤から選ばれる少なくとも１種の化合物（ｂ）と、界面活性剤（ｃ）とを含有することを特徴とする仮止め用の固形接着剤組成物を提供する。 As a result of intensive studies to solve the above problems, the present inventor has found that the adhesive composition composed of the following specific components does not impair the applicability and the adhesiveness of the temporary fixing, and can be applied to machining fluids such as cutting fluid and polishing fluid. It has been found that it can be easily washed and removed with an alcohol-based cleaning agent having excellent alkali resistance and low environmental impact. That is, the present invention relates to a terpene phenol copolymer (a) having a softening point of 90 ° C. to 160 ° C., at least one compound (b) selected from higher fatty acids, higher alcohols, and plasticizers, and a surfactant. A solid adhesive composition for temporary fixing, comprising (c).
また、本発明の好ましい実施形態では、前記化合物（ｂ）が、接着剤組成物総量中に１０質量％〜７０質量％を占める量で含有されており、前記高級脂肪酸が、アルキル基の炭素数が１４〜２２の飽和脂肪酸であり、前記高級アルコールが、炭素数が１６〜２６の飽和アルコールであり、前記可塑剤が、ジシクロヘキシルフタレートであり、および前記界面活性剤（ｃ）が、非イオン界面活性剤であり、接着剤組成物総量中に０．１質量％〜２質量％を占める量で含有されていることが好ましい。 Moreover, in preferable embodiment of this invention, the said compound (b) is contained in the quantity which occupies 10 mass%-70 mass% in adhesive composition total amount, and the said higher fatty acid is carbon number of an alkyl group. Is a saturated fatty acid having 14 to 22, the higher alcohol is a saturated alcohol having 16 to 26 carbon atoms, the plasticizer is dicyclohexyl phthalate, and the surfactant (c) is a nonionic interface It is an activator and is preferably contained in an amount occupying 0.1% by mass to 2% by mass in the total amount of the adhesive composition.
また、本発明は、上記の接着剤組成物を、イソプロピルアルコールが５０質量％〜１００質量％含有されている洗浄剤で洗浄除去することを特徴とする洗浄方法を提供する。 Moreover, this invention provides the washing | cleaning method characterized by carrying out washing | cleaning removal of said adhesive composition with the washing | cleaning agent which contains 50 mass%-100 mass% of isopropyl alcohol.
本発明によれば、従来の接着剤組成物に比べて、切削液や研磨液など加工液に対する耐性が優れていることから、精密な精度を有する切削や研磨などの加工ができ、また、加工処理後、環境負荷が少ない洗浄剤で洗浄除去できる接着剤組成物および洗浄方法が提供される。 According to the present invention, compared to conventional adhesive compositions, it has superior resistance to machining fluids such as cutting fluids and polishing fluids, so that processing such as cutting and polishing with high precision can be performed. Provided are an adhesive composition and a cleaning method that can be cleaned and removed with a cleaning agent having a low environmental load after the treatment.
次に発明を実施するための最良の形態を挙げて、本発明をさらに詳しく説明する。本発明の接着剤組成物は、軟化点が９０℃〜１６０℃のテルペンフェノール共重合体（ａ）と、高級脂肪酸、高級アルコール、および可塑剤から選ばれる少なくとも１種の化合物（ｂ）と、界面活性剤（ｃ）とを含有することにより前記の特性が得られる。 Next, the present invention will be described in more detail with reference to the best mode for carrying out the invention. The adhesive composition of the present invention comprises a terpene phenol copolymer (a) having a softening point of 90 ° C. to 160 ° C., at least one compound (b) selected from higher fatty acids, higher alcohols, and plasticizers, The said characteristic is acquired by containing surfactant (c).
本発明で使用するテルペンフェノール共重合体としては、テルペン系化合物とフェノール系化合物とを公知の方法で重合反応させた軟化点が９０℃〜１６０℃である反応生成物が挙げられる。上記のテルペンフェノール共重合体は、好ましくは軟化点が９０℃〜１５０℃（数平均分子量が５００〜１，１００）、より好ましくは軟化点が１００℃〜１５０℃（数平均分子量が５００〜８００）である反応生成物が挙げられる。上記の軟化点が高過ぎると、得られる接着剤組成物の塗布性が低下する。一方、上記の軟化点が低過ぎると、得られる接着剤組成物に粘着性が発生して保存安定性が低下する。なお、本発明の軟化点は、ＪＩＳ Ｋ２２０７の環球法に準拠した測定値である。また、数平均分子量は、ＧＰＣ法により測定したポリスチレン換算分子量である。 Examples of the terpene phenol copolymer used in the present invention include a reaction product having a softening point of 90 ° C. to 160 ° C. obtained by polymerizing a terpene compound and a phenol compound by a known method. The terpene phenol copolymer preferably has a softening point of 90 ° C to 150 ° C (number average molecular weight of 500 to 1,100), more preferably a softening point of 100 ° C to 150 ° C (number average molecular weight of 500 to 800). ) Is a reaction product. When said softening point is too high, the applicability | paintability of the adhesive composition obtained will fall. On the other hand, if the softening point is too low, the resulting adhesive composition is tacky and storage stability is lowered. The softening point of the present invention is a measured value based on the ring and ball method of JIS K2207. The number average molecular weight is a molecular weight in terms of polystyrene measured by GPC method.
上記のテルペン系化合物としては、例えば、α−ピネン、β−ピネン、ジペンテン、リモネン、カンフェン、ミルセン、アロオシメン、オシメン、α−フェランドレイン、α−テルピネン、γ−テルピネン、テルピノーレン、１，８−シネオール、１，４−シネオール、α−テルピネオール、β−テルピネオール、γ−テルピネオール、サビネン、パラメンタジエン類、カレン類など、好ましくはα−ピネン、β−ピネン、ジペンテン、リモネンなどが挙げられる。 Examples of the terpene-based compound include α-pinene, β-pinene, dipentene, limonene, camphene, myrcene, alloocimene, ocimene, α-ferrane drain, α-terpinene, γ-terpinene, terpinolene, 1,8-cineole. 1,4-cineole, α-terpineol, β-terpineol, γ-terpineol, sabinene, paramentadienes, and carenes, preferably α-pinene, β-pinene, dipentene, limonene, and the like.
また、上記のテルペン系化合物と反応させるフェノール系化合物としては、例えば、フェノール、クレゾール、キシレノール、プロピルフェノール、ノリルフェノール、ハイドロキノン、レゾルシン、メトキシフェノール、ブロモフェノール、ビスフェノールＡ、ビスフェノールＦなど、好ましくはフェノール、ビスフェノールＡなどが挙げられる。 Examples of the phenol compound to be reacted with the terpene compound include, for example, phenol, cresol, xylenol, propylphenol, norylphenol, hydroquinone, resorcin, methoxyphenol, bromophenol, bisphenol A, bisphenol F, and preferably phenol. Bisphenol A and the like.
前記のテルペンフェノール共重合体としては、例えば、α−ピネン／ビスフェノールＡ共重合体、α−ピネン／フェノール共重合体、ジペンテン／フェノール共重合体など、好ましくはα−ピネン／フェノール共重合体、ジペンテン／フェノール共重合体が挙げられる。 Examples of the terpene phenol copolymer include α-pinene / bisphenol A copolymer, α-pinene / phenol copolymer, dipentene / phenol copolymer, preferably α-pinene / phenol copolymer, A dipentene / phenol copolymer may be mentioned.
また、本発明で使用する化合物（ｂ）としては、高級脂肪酸、高級アルコール、および可塑剤から選ばれる少なくとも１種の化合物が挙げられる。すなわち、上記の化合物は、上記の各々の成分単独でも、あるいは２種以上の成分を混合して使用することができる。上記の高級脂肪酸としては、常温にて固体であるアルキル基の炭素数が１０以上、好ましくはアルキル基の炭素数が１４〜２２の直鎖飽和脂肪酸が挙げられる。上記の高級脂肪酸としては、例えば、デカン酸、ウンデカン酸、ドデカン酸、トリデカン酸、テトラデカン酸、ペンタデカン酸、ヘキサデカン酸、ヘプタデカン酸、オクタデカン酸、ノナデカン酸、エイコサン酸、ヘンエイコサン酸、ドコサン酸、トリコサン酸、テトラコサン酸、ペンタコサン酸など、好ましくはテトラデカン酸、ペンタデカン酸、ヘキサデカン酸、ヘプタデカン酸、オクタデカン酸、ノナデカン酸、エイコサン酸、ヘンエイコサン酸、およびドコサン酸が挙げられる。上記の高級脂肪酸は、単独でもあるいは２種以上を混合して使用することができる。 The compound (b) used in the present invention includes at least one compound selected from higher fatty acids, higher alcohols, and plasticizers. That is, the above-described compounds can be used alone or in combination of two or more components. Examples of the higher fatty acid include straight-chain saturated fatty acids in which the alkyl group that is solid at room temperature has 10 or more carbon atoms, and preferably the alkyl group has 14 to 22 carbon atoms. Examples of the higher fatty acid include decanoic acid, undecanoic acid, dodecanoic acid, tridecanoic acid, tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, octadecanoic acid, nonadecanoic acid, eicosanoic acid, heneicosanoic acid, docosanoic acid, and tricosanoic acid. Tetracosanoic acid, pentacosanoic acid, etc., preferably tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, octadecanoic acid, nonadecanoic acid, eicosanoic acid, heneicosanoic acid, and docosanoic acid. The above higher fatty acids can be used alone or in admixture of two or more.
また、前記の高級アルコールとしては、炭素数が６以上の一価鎖式飽和アルコール、好ましくは炭素数が１６〜２６の鎖式飽和アルコールが挙げられる。上記の高級アルコールとしては、例えば、１−ドデカノール、１−トリデカノール、１−テトラデカノール、１−ペンタデカノール、１−ヘキサデカノール、１−ヘプタデカノール、１−オクタデカノール、１−ノナデカノール、１−エイコサノール、１−ヘキサコサノール、１−ヘントリアコンタノールなど、好ましくは１−ヘキサデカノール、１−ヘプタデカノール、１−オクタデカノール、１−ノナデカノール、１−エイコサノール、１−ヘキサコサノールなどが挙げられる。上記の高級アルコールは、単独でもあるいは２種以上を混合して使用することができる。 Further, examples of the higher alcohol include monovalent chain saturated alcohols having 6 or more carbon atoms, preferably chain saturated alcohols having 16 to 26 carbon atoms. Examples of the higher alcohol include 1-dodecanol, 1-tridecanol, 1-tetradecanol, 1-pentadecanol, 1-hexadecanol, 1-heptadecanol, 1-octadecanol, 1-nonadecanol. 1-eicosanol, 1-hexacosanol, 1-hentriacontanol and the like, preferably 1-hexadecanol, 1-heptadecanol, 1-octadecanol, 1-nonadecanol, 1-eicosanol, 1-hexacosa Nord etc. are mentioned. The above higher alcohols can be used alone or in admixture of two or more.
また、前記の可塑剤としては、前記のテルペンフェノール共重合体と相溶性のある公知の可塑剤であればいずれのものも使用することが出来る。上記の可塑剤としては例えば、フタル酸ジブチル、フタル酸ジエチル、フタル酸ジメチル、ジシクロヘキシルフタレートなどのフタル酸エステル、トリクレジルホスフェート、トリメチルホスフェート、トリエチルホスフェート、トリブチルホスフェート、トリフェニルホスフェート、トリキシレニルホスフェートなどのリン酸エステル、ジエチレングリコールジベンゾエート、ジプロピレングリコールジベンゾエート、ジエチレングリコールモノベンゾエート、ジプロピレングリコールモノベンゾエートなどの安息香酸エステル、およびそれらの混合物、好ましくはジシクロヘキシルフタレートが挙げられる。上記の可塑剤は、単独でもあるいは２種以上を混合して使用することができる。 As the plasticizer, any known plasticizer that is compatible with the terpene phenol copolymer can be used. Examples of the plasticizer include phthalic acid esters such as dibutyl phthalate, diethyl phthalate, dimethyl phthalate, and dicyclohexyl phthalate, tricresyl phosphate, trimethyl phosphate, triethyl phosphate, tributyl phosphate, triphenyl phosphate, and trixylenyl phosphate. And benzoic acid esters such as diethylene glycol dibenzoate, dipropylene glycol dibenzoate, diethylene glycol monobenzoate and dipropylene glycol monobenzoate, and mixtures thereof, preferably dicyclohexyl phthalate. Said plasticizer can be used individually or in mixture of 2 or more types.
前記の化合物（ｂ）は、得られる接着剤組成物の溶融塗布性および仮止めの接着性を向上させるために前記のテルペンフェノール共重合体（ａ）に配合される。前記の化合物（ｂ）の配合量は、接着剤組成物総量中に１０質量％〜７０質量％である。上記の化合物（ｂ）の配合量が多すぎると、溶融塗布粘度が下がりすぎ、適度の塗布性が得られなく、また、仮止めの接着性が低下する。一方、上記化合物（ｂ）の配合量が少なすぎると、得られる接着剤組成物の溶融塗布性および仮止めの接着性が低下する。 The compound (b) is blended with the terpene phenol copolymer (a) in order to improve the melt coatability and temporary fixability of the resulting adhesive composition. The compounding amount of the compound (b) is 10% by mass to 70% by mass in the total amount of the adhesive composition. If the compounding amount of the compound (b) is too large, the melt coating viscosity will be too low, an appropriate coating property will not be obtained, and the adhesiveness of the temporary fixing will decrease. On the other hand, when there are too few compounding quantities of the said compound (b), the melt application property of the adhesive composition obtained and the adhesiveness of temporary fixing will fall.
前記のテルペンフェノール共重合体（ａ）および化合物（ｂ）に配合される界面活性剤（ｃ）は、得られる接着剤組成物の被着体（加工部材）や加工部材を一時的に仮止め保持する支持台への濡れ性を向上させ、より仮止めの接着性をアップさせる。上記の界面活性剤（ｃ）としては、上記のテルペンフェノール共重合体（ａ）と相溶する公知の界面活性剤であればいずれでもよく、好ましくは非イオン界面活性剤であり、接着剤組成物総量中に０．１質量％〜２質量％、より好ましくは０．１質量％〜１質量％を占める量で含有されているものがよい。 The surfactant (c) blended with the terpene phenol copolymer (a) and the compound (b) is used to temporarily fix the adherend (processed member) or processed member of the resulting adhesive composition. Improves the wettability to the supporting base to hold, and further improves the adhesion of temporary fixing. The surfactant (c) may be any known surfactant that is compatible with the terpene phenol copolymer (a), preferably a nonionic surfactant, and an adhesive composition. What is contained by the quantity which occupies 0.1 mass%-2 mass% in the total amount of matter, More preferably, 0.1 mass%-1 mass% is good.
上記の非イオン界面活性剤としては、例えば、フッ素系タイプ；ポリオキシエチレンアルキレンアルキルエーテル、ポリオキシエチレンアルキルエーテル、ポリオキシエチレンアルキルフェニルエーテル、ポリオキシエチレンポリオキシプロピルアルキルエーテルなどのエーテル系タイプ；ポリオキシエチレングリセリン脂肪酸エステル、ポリオキシエチレンソルビタン脂肪酸エステルなどのエステルエーテル系タイプ；ポリエチレングリコール脂肪酸エステル、グリセリン脂肪酸エステル、ソルビタン脂肪酸エステルなどのエステル系タイプ；脂肪酸アルカノールアミド、ポリオキシエチレン脂肪酸アミドなどの含窒素系タイプなど、好ましくはフッ素系タイプが挙げられる。 Examples of the nonionic surfactant include a fluorine type; an ether type such as polyoxyethylene alkylene alkyl ether, polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene polyoxypropyl alkyl ether; Ester ether type such as polyoxyethylene glycerin fatty acid ester and polyoxyethylene sorbitan fatty acid ester; Ester type such as polyethylene glycol fatty acid ester, glycerin fatty acid ester and sorbitan fatty acid ester; including fatty acid alkanolamide and polyoxyethylene fatty acid amide Nitrogen type and the like, preferably fluorine type.
本発明の接着剤組成物は、前記のテルペンフェノール共重合体（ａ）と、化合物（ｂ）と、界面活性剤（ｃ）とを適宜に配合し、好ましくは上記の化合物（ｂ）および界面活性剤（ｃ）が前記の接着剤組成物総量中の配合割合になるように配合し、１００〜１５０℃の加熱条件下で３０〜９０分間溶融しながら公知の方法で均一に混練混合して均質化する。上記の溶融混合物を成形型に流し込み、冷却して固形化して調製される。 The adhesive composition of the present invention suitably comprises the terpene phenol copolymer (a), the compound (b), and the surfactant (c), preferably the above compound (b) and the interface. The active agent (c) is blended so as to have a blending ratio in the total amount of the adhesive composition, and kneaded and mixed uniformly by a known method while melting for 30 to 90 minutes under a heating condition of 100 to 150 ° C. Homogenize. The molten mixture is poured into a mold, cooled and solidified.
本発明の接着剤組成物を使用する仮止め接着の事例としては、電子部品、光学部品、医療部品などに使用されるシリコン、ガラス、セラミック、磁性体などの材料からなるウエハー、丸管、円筒体などの形状の部材を、アルカリ性の研磨液や切削液を用いてポリシング加工あるいは切削・切断加工する際に、これらの部材を一時的に仮止めする支持台であるカーボンプレートを１００℃〜１８０℃に加熱し、当該支持台に上記の接着剤組成物を手塗り、あるいは通常のホットメルトアプリケーターを使用して、１０μｍ〜１００μｍの厚みに溶融塗布する。次に、溶融状態にある該接着剤塗布面に上記の加工部材を加熱圧着し、圧着後、常温まで冷却して仮止め接着する。仮止め接着後、上記の仮止めされた部材を、例えば、ダイヤモンドカッターなどを使用して、アルカリ性の切削液をかけながら切断加工する。 Examples of temporary bonding using the adhesive composition of the present invention include wafers, round tubes, and cylinders made of materials such as silicon, glass, ceramics, and magnetic materials used for electronic parts, optical parts, medical parts, etc. When a member having a shape such as a body is subjected to polishing processing or cutting / cutting processing using an alkaline polishing liquid or cutting fluid, a carbon plate which is a support base for temporarily fixing these members is set to 100 ° C. to 180 ° C. It heats at (degreeC) and the said adhesive composition is hand-coated on the said support stand, or it melt-coats to the thickness of 10 micrometers-100 micrometers using a normal hot-melt applicator. Next, the processed member is heat-pressed to the adhesive-coated surface in a molten state, and after press-bonding, it is cooled to room temperature and temporarily bonded. After the temporary fixing adhesion, the temporarily fixed member is cut using a diamond cutter or the like while applying an alkaline cutting fluid.
上記の切断加工が終了後、部材を仮止めした接着剤組成物の洗浄除去は、アルコール系洗浄剤を用いて行うことができ、好ましくはイソプロピルアルコールが５０質量％〜１００質量％含有されている洗浄剤を使用して洗浄除去する。上記のアルコール系洗浄剤は、イソプロピルアルコール単独でも、あるいは、上記範囲内においてイソプロピルアルコールと他のアルコールを併用してもよい。 After the above cutting process is completed, the adhesive composition with the members temporarily fixed can be removed by washing with an alcohol-based detergent, and preferably contains 50% by mass to 100% by mass of isopropyl alcohol. Wash away with detergent. The alcohol-based cleaning agent may be isopropyl alcohol alone, or isopropyl alcohol and other alcohols may be used in combination within the above range.
上記のアルコール系洗浄剤としては、例えば、ｎ−プロパノール、イソプロパノール、ｎ−ブタノール、ヘキサノール、オクタノール、メタノール、エタノールなど、好ましくはイソプロパノールが挙げられる。上記のアルコール系洗浄剤は、アセトン、酢酸メチル、酢酸エチル、酢酸ブチル、メチルイソブチルケトン、メチルエチルケトンなどを本発明の目的を妨げない範囲において配合して使用することができる。 Examples of the alcohol-based cleaning agent include n-propanol, isopropanol, n-butanol, hexanol, octanol, methanol, ethanol, and preferably isopropanol. The alcohol-based cleaning agent can be used by blending acetone, methyl acetate, ethyl acetate, butyl acetate, methyl isobutyl ketone, methyl ethyl ketone, and the like within a range not impeding the purpose of the present invention.
次に実施例および比較例を挙げて本発明をさらに具体的に説明する。文中「部」または「％」とあるのは特に断りのない限り質量基準である。なお、本発明は下記の実施例に限定されるものではない。 Next, the present invention will be described more specifically with reference to examples and comparative examples. In the text, “part” or “%” is based on mass unless otherwise specified. In addition, this invention is not limited to the following Example.
［実施例１〜４］（接着剤組成物Ｍ１〜Ｍ４）
テルペンフェノール共重合体（ａ）と、化合物（ｂ）と、界面活性剤（ｃ）とを使用し、各々の成分を表１に示すように配合し、１２０℃にて６０分間均一に熱溶融混練して均質化し、均質化後、常温まで冷却固化して本発明の接着剤組成物Ｍ１〜Ｍ４を調製した。
[Examples 1 to 4] (Adhesive compositions M1 to M4)
Using terpene phenol copolymer (a), compound (b), and surfactant (c), each component was blended as shown in Table 1, and uniformly melted at 120 ° C. for 60 minutes. It knead | mixed and homogenized, and after solidifying, it cooled and solidified to normal temperature and prepared adhesive composition M1-M4 of this invention.
上記のテルペンフェノール共重合体（ａ）、化合物（ｂ）、および界面活性剤（ｃ）は、下記の通りである。
・テルペンフェノール共重合体（ａ）
ａ１：α−ピネン／フェノール共重合体（軟化点１１５℃、数平均分子量６００）
ａ２：ジペンテン／フェノール共重合体（軟化点１２５℃、数平均分子量６００）
・化合物（ｂ）
ｂ１：ステアリルアルコール
ｂ２：ステアリン酸
ｂ３：ジシクロヘキシルフタレート
・界面活性剤（ｃ）
非イオン界面活性剤（フッ素系界面活性剤）
Said terpene phenol copolymer (a), a compound (b), and surfactant (c) are as follows.
-Terpene phenol copolymer (a)
a1: α-pinene / phenol copolymer (softening point 115 ° C., number average molecular weight 600)
a2: dipentene / phenol copolymer (softening point 125 ° C., number average molecular weight 600)
Compound (b)
b1: Stearyl alcohol b2: Stearic acid b3: Dicyclohexyl phthalate / surfactant (c)
Nonionic surfactant (fluorine surfactant)
［比較例１〜４］（接着剤組成物Ｎ１〜Ｎ４）
表２に示すように各々の成分を配合し、１２０℃にて６０分間均一に熱溶融混練して均質化し、均質化後、常温まで冷却固化して比較例の接着剤組成物Ｎ１〜Ｎ４を調製した。
[Comparative Examples 1 to 4] (Adhesive Compositions N1 to N4)
As shown in Table 2, each component was blended, uniformly melted and kneaded for 60 minutes at 120 ° C., homogenized, and after homogenization, cooled and solidified to room temperature to obtain comparative adhesive compositions N1 to N4. Prepared.
上記で得られた各々の接着剤組成物について塗布性、接着性、耐アルカリ性、およびアルコール洗浄性に関し下記の測定方法により評価した。評価結果を表３に示す。
（塗布性）
前記で得られた各々の接着剤組成物を使用して、１２０℃に加熱されたカーボンプレート上に上記接着剤組成物を手で押し付け移動させながら手塗りし、その溶融塗布状態を下記の評価方法により評価した。
○：塗布面に糸引現象がなく、均一で平滑な塗布面が得られた。
×：塗布面に糸引現象を生じ、均一で平滑な塗布面が得られない。
About each adhesive composition obtained above, applicability | paintability, adhesiveness, alkali resistance, and alcohol washability were evaluated with the following measuring method. The evaluation results are shown in Table 3.
(Applicability)
Using each of the adhesive compositions obtained above, the adhesive composition was hand-pressed and moved by hand onto a carbon plate heated to 120 ° C., and the melt coating state was evaluated as follows. The method was evaluated.
○: There was no stringing phenomenon on the coated surface, and a uniform and smooth coated surface was obtained.
X: A stringing phenomenon occurs on the coated surface, and a uniform and smooth coated surface cannot be obtained.
（接着性）
前記で得られた各々の接着剤組成物を１２０℃に加熱溶融して、ステンレス基板同士を接着し、２５℃まで冷却した後、ＪＩＳＫ６８５０に準拠して接着力を測定した。
○：引張り剪断力が２ＭＰａ以上である。
×：引張り剪断力が２ＭＰａ未満である。
(Adhesiveness)
Each adhesive composition obtained above was heated and melted to 120 ° C., the stainless steel substrates were bonded to each other, cooled to 25 ° C., and then the adhesive strength was measured according to JISK6850.
◯: The tensile shear force is 2 MPa or more.
X: The tensile shear force is less than 2 MPa.
（耐アルカリ性）
前記で得られた各々の接着剤組成物を使用して、１２０℃に加熱されたガラス基板上に手塗りにて４０μｍ〜５０μｍの厚みに塗布し塗膜を形成、常温まで冷却して試料を作成した。上記の試料を５％の水酸化カリウム水溶液（２５℃）中に５分間浸漬し、ガラス基板上の接着剤組成物塗膜の耐性を下記の評価方法により評価した。
○：接着剤組成物塗膜が、溶解や膨潤されていない。
×：接着剤組成物塗膜が、溶解や膨潤されている。
(Alkali resistance)
Using each of the adhesive compositions obtained above, a coating film was formed by hand coating on a glass substrate heated to 120 ° C. to a thickness of 40 μm to 50 μm, and the sample was cooled to room temperature. Created. Said sample was immersed in 5% potassium hydroxide aqueous solution (25 degreeC) for 5 minutes, and the tolerance of the adhesive composition coating film on a glass substrate was evaluated by the following evaluation method.
○: The adhesive composition coating film is not dissolved or swollen.
X: The adhesive composition coating film is dissolved or swollen.
（アルコール洗浄性）
上記の耐アルカリ性評価に用いられる試料を使用して、該試料を洗浄剤であるイソプロピルアルコール中に１０分間浸漬し、接着剤組成物の上記洗浄剤に対する洗浄除去を下記の評価方法により評価した。
○：接着剤組成物が、容易に洗浄除去される。
×：接着剤組成物が、洗浄除去されない。
(Alcohol washability)
Using the sample used for the above alkali resistance evaluation, the sample was immersed in isopropyl alcohol as a cleaning agent for 10 minutes, and the cleaning removal of the adhesive composition with respect to the cleaning agent was evaluated by the following evaluation method.
○: The adhesive composition is easily removed by washing.
X: The adhesive composition is not removed by washing.
上記の評価結果より、本発明の接着剤組成物は、従来の固形タイプの仮止め接着剤に比べて、同等もしくはそれ以上の塗布性や接着性を有し、特に耐アルカリ性およびアルコール洗浄性が優れていることから、アルカリ性の切削液、研磨液に対する耐性があり、環境負荷の少ないアルコール系洗浄剤で、加工後洗浄除去できることが実証された。また、比較例４の接着剤組成物は、塗布性や接着性が著しく低下している。 From the above evaluation results, the adhesive composition of the present invention has equivalent or better applicability and adhesiveness compared to conventional solid type temporary fixing adhesives, and particularly has alkali resistance and alcohol washability. Since it is excellent, it has been proved that it is resistant to alkaline cutting fluid and polishing fluid, and can be cleaned and removed after processing with an alcohol-based cleaning agent with little environmental load. Moreover, as for the adhesive composition of the comparative example 4, applicability | paintability and adhesiveness are falling remarkably.
本発明によれば、本発明の接着剤組成物は、電子部品、光学部品などの部材をアルカリ性の切削液、研磨液を使用して精密な精度で切削・切断加工あるいはポリシング加工するのに、また、加工後、不要となった接着剤を環境負荷が少ないアルコール系洗浄剤で容易に洗浄出来る接着剤組成物として有効である。 According to the present invention, the adhesive composition of the present invention is used for cutting / cutting or polishing a member such as an electronic component, an optical component or the like with an accurate cutting accuracy using an alkaline cutting fluid or a polishing fluid. Further, it is effective as an adhesive composition that can easily clean an unnecessary adhesive after processing with an alcohol-based cleaning agent having a small environmental load.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| JP2016105452A (en) * | 2014-07-02 | 2016-06-09 | 三菱マテリアル株式会社 | Method of manufacturing conjugate, method of manufacturing multilayer conjugate, method of manufacturing substrate for power module, method of manufacturing substrate for power module with heat sink, and method of manufacturing laminate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016002804A1 (en) * | 2014-07-02 | 2016-01-07 | 三菱マテリアル株式会社 | Joined body manufacturing method, multilayer joined body manufacturing method, power-module substrate manufacturing method, heat sink equipped power-module substrate manufacturing method, and laminated body manufacturing device |
| JP2016105452A (en) * | 2014-07-02 | 2016-06-09 | 三菱マテリアル株式会社 | Method of manufacturing conjugate, method of manufacturing multilayer conjugate, method of manufacturing substrate for power module, method of manufacturing substrate for power module with heat sink, and method of manufacturing laminate |
| CN106471616A (en) * | 2014-07-02 | 2017-03-01 | 三菱综合材料株式会社 | Conjugant and many layer assemblies preparation method, power module substrate and band radiator power module substrate preparation method and laminated body producing device |
| KR20170026503A (en) * | 2014-07-02 | 2017-03-08 | 미쓰비시 마테리알 가부시키가이샤 | Joined body manufacturing method, multilayer joined body manufacturing method, power-module substrate manufacturing method, heat sink equipped power-module substrate manufacturing method, and laminated body manufacturing device |
| US20170141011A1 (en) * | 2014-07-02 | 2017-05-18 | Mitsubishi Materials Corporation | Joined body manufacturing method, multilayer joined body manufacturing method, power-module substrate manufacturing method, heat sink equipped power-module substrate manufacturing method, and laminated body manufacturing device |
| US10607915B2 (en) | 2014-07-02 | 2020-03-31 | Mitsubishi Materials Corporation | Joined body manufacturing method, multilayer joined body manufacturing method, power-module substrate manufacturing method, heat sink equipped power-module substrate manufacturing method, and laminated body manufacturing device |
| KR102300970B1 (en) * | 2014-07-02 | 2021-09-09 | 미쓰비시 마테리알 가부시키가이샤 | Joined body manufacturing method, multilayer joined body manufacturing method, power-module substrate manufacturing method, heat sink equipped power-module substrate manufacturing method, and laminated body manufacturing device |
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