CN107075187A - 组合物、片的制造方法、片、层叠体及带有元件晶片的层叠体 - Google Patents
组合物、片的制造方法、片、层叠体及带有元件晶片的层叠体 Download PDFInfo
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- CN107075187A CN107075187A CN201580052955.4A CN201580052955A CN107075187A CN 107075187 A CN107075187 A CN 107075187A CN 201580052955 A CN201580052955 A CN 201580052955A CN 107075187 A CN107075187 A CN 107075187A
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- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
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- RKBCYCFRFCNLTO-UHFFFAOYSA-N triisopropylamine Chemical compound CC(C)N(C(C)C)C(C)C RKBCYCFRFCNLTO-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L53/02—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers of vinyl-aromatic monomers and conjugated dienes
-
- 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
- C09J7/10—Adhesives in the form of films or foils without carriers
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- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/06—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of natural rubber or synthetic rubber
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/04—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/04—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B25/08—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/12—Layered products comprising a layer of natural or synthetic rubber comprising natural rubber
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/14—Layered products comprising a layer of natural or synthetic rubber comprising synthetic rubber copolymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/16—Layered products comprising a layer of natural or synthetic rubber comprising polydienes homopolymers or poly-halodienes homopolymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/20—Layered products comprising a layer of natural or synthetic rubber comprising silicone rubber
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Abstract
提供一种组合物、片的制造方法、片、层叠体及带有元件晶片的层叠体,所述组合物的弹性体的溶解性良好,可提高固体成分浓度,可形成干燥性、表面状态及耐热性优异的膜。所述组合物含有:自25℃起以20℃/min升温的5%热质量减少温度为375℃以上的弹性体;下述通式(1)所表示的沸点为160℃以上的溶剂;及沸点小于120℃的溶剂。通式(1)中,R1~R6分别独立地表示氢原子或脂肪族烃基。
Description
技术领域
本发明涉及一种组合物、片的制造方法、片、层叠体及带有元件晶片的层叠体。更详细而言,本发明涉及一种在半导体装置等的制造中可优选地使用的组合物、片的制造方法、片、层叠体及带有元件晶片的层叠体。
背景技术
在集成电路(Integrated Circuit,IC)或大规模集成电路(Large ScaleIntegration,LSI)等半导体元件的制造工艺(process)中,在元件晶片上形成多个IC芯片,并通过切割(dicing)而单片化。
伴随着电子设备的进一步的小型化及高性能化的需求(needs),对搭载在电子设备上的IC芯片也要求进一步的小型化及高集成化,但元件晶片的面方向上的集成电路的高集成化已接近极限。
作为自IC芯片内的集成电路向IC芯片的外部端子的电性连接方法,一直以来打线接合(wire bonding)法广为人知,但为了实现IC芯片的小型化,近年来已知以下方法:在元件晶片中设置贯通孔,将作为外部端子的金属插塞(plug)以在贯通孔内贯穿的方式连接于集成电路的所谓形成硅贯通电极(Through Silicon Via,TSV)的方法。然而,仅形成硅贯通电极的方法无法充分应对所述近年来的对IC芯片的进一步高集成化的需求。
鉴于以上情况,已知以下技术:使IC芯片内的集成电路多层化,由此提高元件晶片的每单位面积的集成度。然而,集成电路的多层化会使IC芯片的厚度增大,故必须实现构成IC芯片的构件的薄型化。关于此种构件的薄型化,例如已研究了元件晶片的薄型化,此方法不仅有助于IC芯片的小型化,而且可使硅贯通电极的制造中的元件晶片的贯通孔制造步骤省力,故被视为有前途。另外,在功率元件(power device)、图像传感器(image sensor)等半导体元件中,就提高所述集成度或提高元件结构的自由度的观点而言,也正在尝试薄型化。
作为元件晶片,具有约700μm~900μm的厚度者已广为人知,近年来,以IC芯片的小型化等为目的,正在尝试使元件晶片的厚度变薄至200μm以下。
然而,厚度200μm以下的元件晶片非常薄,以其作为基材的半导体元件制造用构件也非常薄,故在对此种构件实施进一步的处理、或单移动此种构件的情形时,难以稳定且无损伤地支撑构件。
为了解决如上所述的问题,已知利用暂时接着剂将薄型化前的元件晶片与支撑基板暂时固定(暂时接着(temporary bonding)),将元件晶片的背面磨削而薄型化后,使支撑基板自元件晶片脱离的技术。
在专利文献1中记载:使用含有苯乙烯系弹性体、乙酸乙酯、十氢萘的接着剂组合物形成接着层,且使用形成有接着层的接着膜将晶片与晶片的支撑基板贴附。
另一方面,在专利文献2中记载:使相对于苯乙烯系弹性体100重量份而含有150重量份~2400重量份的有机溶剂、100重量份~1500重量份的水、及1重量份~20重量份的亲水性-亲油性均衡(Hydrophile-Lipophile Balance,HLB)值为6~17的非离子性表面活性剂的苯乙烯系弹性体分散溶液含浸于纤维质基材后,使其干燥而制造片状物。
现有技术文献
专利文献
专利文献1:日本专利特开2014-37458号公报
专利文献2:日本专利特开平11-117180号公报
发明内容
发明要解决的课题
在将元件晶片的表面与支撑基板暂时接着的情形时,为了稳定地支撑元件晶片,而对元件晶片的表面与支撑基板之间的暂时接着层要求一定强度的接着力,并且谋求可容易地解除元件晶片与支撑基板的暂时接着状态的特性。当形成满足此种特性的暂时接着层时,正研究使用弹性体。
另外,在使用片将元件晶片与支撑基板暂时接着的情形时,为了确保对元件晶片的表面形状(例如金属凸块(metal bump)、垫、通孔(via)等结构体)的追随性,而期望片具有某种程度的厚度。
然而,本发明人等人对专利文献1所揭示的组合物进行研究的结果可知:专利文献1的组合物的弹性体的溶解性低,难以形成具有厚度的片。进而可知,专利文献1的组合物的干燥性差,有膜中的溶剂的残留量增加的倾向。
作为提高组合物的干燥性的方法,考虑使用沸点低的溶剂,但可知若使用沸点低的溶剂,则容易产生干燥不均或厚度不均等,有膜表面的表面状态恶化的倾向。若膜表面的表面状态差,则有对元件晶片或支撑基板的接着性差的倾向。
另外,近年来,在元件的制造工艺中,有时将元件供于更高温下的处理。因此,为了应对各种制造工艺,对暂时接着膜也谋求耐热性的进一步提高。
另一方面,在专利文献2中,使苯乙烯系弹性体分散溶液含侵于纤维质基材,并快速干燥,而获得具有天然皮革的手感的片。也即,专利文献2是将苯乙烯系弹性体分散溶液用作纤维质基材的集束剂。然而,专利文献2中并未针对使用苯乙烯系弹性体分散溶液来形成片等进行记载。进而,并未针对提高弹性体的溶解性、干燥后的表面状态、耐热性进行记载。
本发明是鉴于所述背景而成,其目的在于提供一种组合物、片的制造方法、片、层叠体及带有元件晶片的层叠体,所述组合物的弹性体的溶解性良好,可提高固体成分浓度,可形成干燥性、表面状态及耐热性优异的膜。
解决问题的技术手段
本发明人等人为了解决所述课题而进行了潜心研究,结果发现,通过将自25℃起以20℃/min(20℃/分)升温的5%热质量减少(mass reduction)温度为375℃以上的弹性体、后述的通式(1)所表示的沸点为160℃以上的溶剂、与沸点小于120℃的溶剂并用,而可达成所述目的,从而完成了本发明。本发明提供以下内容。
<1>一种组合物,其含有:自25℃起以20℃/min升温的5%热质量减少温度为375℃以上的弹性体;下述通式(1)所表示的沸点为160℃以上的溶剂;及沸点小于120℃的溶剂,
[化1]
通式(1)中,R1~R6分别独立地表示氢原子或脂肪族烃基。
<2>根据<1>所记载的组合物,其中弹性体是以25质量%以上的比例而含有于组合物中。
<3>根据<1>或<2>所记载的组合物,其中弹性体为含有来源于苯乙烯的重复单元的弹性体。
<4>根据<1>至<3>中任一项所记载的组合物,其中弹性体为氢化产物(hydrogenated product)。
<5>根据<1>至<4>中任一项所记载的组合物,其中弹性体为单末端或两末端为苯乙烯嵌段的苯乙烯嵌段聚合物。
<6>根据<1>至<5>中任一项所记载的组合物,其中弹性体的苯乙烯含有率为40质量%以上。
<7>根据<1>至<6>中任一项所记载的组合物,其中沸点为160℃以上的溶剂的SP值为19(MPa)1/2以下。
<8>根据<1>至<7>中任一项所记载的组合物,其中沸点小于120℃的溶剂的SP值为19(MPa)1/2以下。
<9>根据<1>至<8>中任一项所记载的组合物,其中沸点小于120℃的溶剂为选自芳香族烃、脂环式烃及环状醚中的一种以上。
<10>根据<1>至<9>中任一项所记载的组合物,其中沸点小于120℃的溶剂是以10质量%~60质量%的比例而含有于组合物中。
<11>根据<1>至<10>中任一项所记载的组合物,其中沸点为160℃以上的溶剂与沸点小于120℃的溶剂的质量比为80∶20~99∶1。
<12>根据<1>至<11>中任一项所记载的组合物,其还含有抗氧化剂。
<13>根据<12>所记载的组合物,其中抗氧化剂是以1质量%~7质量%的比例而含有于组合物中。
<14>根据<1>至<13>中任一项所记载的组合物,其用于片形成用途。
<15>根据<1>至<14>中任一项所记载的组合物,其为暂时接着组合物。
<16>一种片的制造方法,其将根据<1>至<15>中任一项所记载的组合物施用于支撑体上,并使其干燥。
<17>一种片,其是使根据<1>至<15>中任一项所记载的组合物干燥而获得。
<18>一种层叠体,其在使根据<1>至<15>中任一项所记载的组合物干燥而获得的片的单面或两面上具有具备脱模性的支撑体。
<19>一种带有元件晶片的层叠体,其在元件晶片与支撑基板之间具有使根据<1>至<15>中任一项所记载的组合物干燥而获得的片,且片的一个表面与元件晶片的元件面接触,另一表面与支撑基板的表面接触。
发明的效果
根据本发明,可提供一种组合物、片的制造方法、片、层叠体及带有元件晶片的层叠体,所述组合物的弹性体的溶解性良好,可提高固体成分浓度,可形成干燥性、表面状态及耐热性优异的膜。
附图说明
图1为表示半导体装置的制造方法的一实施方式的概略图。
具体实施方式
以下,对本发明的实施方式加以详细说明。
在本说明书中的基团(原子团)的表述中,未记载经取代及未经取代的表述不仅包含不具有取代基的基团(原子团),还包含具有取代基的基团(原子团)。例如所谓“烷基”,不仅包含不具有取代基的烷基(未经取代的烷基),而且还包含具有取代基的烷基(经取代的烷基)。
本说明书中的“光化射线”或“放射线”例如是指包含可见光线、紫外线、远紫外线、电子束、X射线等。
本说明书中,所谓“光”是指光化射线或放射线。
本说明书中,所谓“曝光”只要无特别说明,则不仅是指利用水银灯、紫外线、准分子激光所代表的远紫外线、X射线、极紫外线线(Extreme Ultraviolet,EUV)等的曝光,还是指利用电子束及离子束(ion beam)等粒子束的描画。
本说明书中,“(甲基)丙烯酸酯”表示丙烯酸酯及甲基丙烯酸酯,“(甲基)丙烯酸基”表示丙烯酸基及甲基丙烯酸基,“(甲基)丙烯酰基”表示“丙烯酰基”及“甲基丙烯酰基”。
本说明书中,重量平均分子量及数量平均分子量是定义为由凝胶渗透色谱法(GelPermeation Chromatography,GPC)测定所得的聚苯乙烯换算值。本说明书中,重量平均分子量(Mw)及数量平均分子量(Mn)例如可通过以下方式求出:使用HLC-8220(东曹(Tosoh)(股)制造),使用TSKgel Super AWM-H(东曹(股)制造,6.0mm ID×15.0cm作为管柱,且使用10mmol/L的溴化锂N-甲基吡咯烷酮(N-methylpyrrolidinone,NMP)溶液作为洗脱液。
本说明书中的固体成分为25℃下的固体成分。
再者,在以下所说明的实施方式中,关于已在参照附图中说明的构件等,通过在图中标注相同符号或相应符号而将说明简化或省略。
<组合物>
本发明的组合物含有:(A)自25℃起以20℃/min升温的5%热质量减少温度为375℃以上的弹性体;(B)后述的通式(1)所表示的沸点为160℃以上的溶剂;及(C)沸点小于120℃的溶剂。
本发明的组合物因含有自25℃起以20℃/min升温时的375℃下的质量减少率为5质量%以下的弹性体,故可形成耐热性优异的片等膜。因此,例如在经过了高温下的工艺的情形时,也可稳定地将元件晶片暂时接着。
另外,因含有后述的通式(1)所表示的沸点为160℃以上的溶剂,故可提高弹性体的溶解性,可提高组合物的固体成分浓度。因此,可容易地制造具有厚度的片等膜。尤其在作为弹性体使用的是含有来源于苯乙烯的重复单元的弹性体的情形时,可进一步提高弹性体的溶解性。
而且,通过将(B)后述的通式(1)所表示的沸点为160℃以上的溶剂、与(C)沸点小于120℃的溶剂并用,而可提高组合物的干燥性,并且可制造表面状态优异的片等膜。
再者,在单独使用(B)后述的通式(1)所表示的沸点为160℃以上的溶剂的情形时,因组合物的干燥速度慢,故膜中的溶剂残存量容易变多。另外,在单独使用(C)沸点小于120℃的溶剂的情形时,弹性体的溶解性不充分,且难以制造具有厚度的膜。进而,因组合物的干燥速度过快,故容易产生干燥不均或厚度不均,表面状态容易劣化。
本发明的组合物可优选地用于片形成用途。
另外,本发明的组合物可优选地用作暂时接着组合物。
以下,对本发明的组合物的各成分加以详细说明。
<<(A)弹性体>>
本发明的组合物含有弹性体。通过含有弹性体而也追随支撑基板或元件晶片的微细的凹凸,从而利用适度的固着效果(anchor effect)而可形成具有优异的接着性的片等膜。另外,在将支撑基板自元件晶片剥离时,可在不对元件晶片等施加应力的情况下将支撑基板自元件晶片简单地剥离,可防止元件晶片上的元件等的破损或剥落。
再者,本说明书中,所谓弹性体,表示显示出弹性变形的高分子化合物。即,定义为具有如下性质的高分子化合物:在施加外力时,根据所述外力而瞬间变形,且在解除外力时,短时间内恢复原本的形状。
本发明中,弹性体优选为具有如下性质:在将原本的大小设为100%时,可在室温(20℃)下利用小的外力而变形至200%,且在解除外力时,在短时间内回到130%以下。
本发明中,弹性体自25℃起以20℃/min升温的5%热质量减少温度为375℃以上,优选为380℃以上,进而优选为390℃以上,最优选为400℃以上。另外,上限值并无特别限定,例如优选为1000℃以下,更优选为800℃以下。根据所述形态,容易形成耐热性优异的片等膜。质量减少温度是指利用热重量测定装置(热重量分析仪(ThermogravimetricAnalyzer,TGA))在氮气流下在所述升温条件下测定的值。再者,在本发明的组合物含有两种以上的弹性体的情形时,是指两种以上的弹性体的混合物的值。
本发明中,弹性体的玻璃化温度(以下也称为“Tg”)优选为-50℃~300℃,更优选为0℃~200℃。若Tg为所述范围,则接着时对元件晶片表面的追随性良好,可形成无孔隙的片等膜。再者,在弹性体具有两点以上的Tg的情形时,所述Tg的值是指较低的玻璃化温度。
本发明中,弹性体的重量平均分子量优选为2,000~200,000,更优选为10,000~200,000,尤其优选为50,000~100,000。通过在所述范围内,即便在将支撑基板自元件晶片剥离后将残存于元件晶片和/或支撑基板上的来源于弹性体的残渣去除时,在溶剂中的溶解性也优异,故有不在元件晶片或支撑基板上残留残渣等优点。
本发明中,作为弹性体,可使用含有来源于苯乙烯的重复单元的弹性体(聚苯乙烯系弹性体)、聚酯系弹性体、聚烯烃系弹性体、聚氨基甲酸酯系弹性体、聚酰胺系弹性体、聚丙烯酸系弹性体、硅酮系弹性体、聚酰亚胺系弹性体等。优选为选自聚苯乙烯系弹性体、聚酯系弹性体、聚烯烃系弹性体、聚氨基甲酸酯系弹性体、聚酰胺系弹性体、聚丙烯酸系弹性体、硅酮系弹性体及聚酰亚胺系弹性体中的一种以上,就溶解性、耐热性等的观点而言,尤其优选为聚苯乙烯系弹性体。
另外,弹性体优选为氢化产物。尤其优选为聚苯乙烯系弹性体的氢化产物。若弹性体为氢化产物,则容易形成耐热性优异的片等膜。进而,容易形成剥离性及剥离后的清洗去除性优异的片等膜。在使用聚苯乙烯系弹性体的氢化产物的情形时,所述效果显著。再者,所谓氢化产物,是指弹性体经氢化的结构的聚合物。
<<<聚苯乙烯系弹性体>>>
本发明中,聚苯乙烯系弹性体并无特别限制,可根据目的而适当选择。例如可列举:苯乙烯-丁二烯-苯乙烯嵌段共聚物(SBS)、苯乙烯-异戊二烯-苯乙烯嵌段共聚物(SIS)、苯乙烯-乙烯-丁烯-苯乙烯嵌段共聚物(SEBS)、苯乙烯-丁二烯-丁烯-苯乙烯共聚物(SBBS)及这些共聚物的氢化产物、苯乙烯-乙烯-丁烯苯乙烯嵌段共聚物(SEBS)、苯乙烯-乙烯-丙烯-苯乙烯嵌段共聚物(SEPS)、苯乙烯-乙烯-乙烯-丙烯-苯乙烯嵌段共聚物等。
聚苯乙烯系弹性体中的来源于苯乙烯的重复单元的含量优选为40质量%以上,优选为45质量%以上,更优选为46质量%以上。上限例如可设为90质量%以下,也可设为85质量%以下。
聚苯乙烯系弹性体优选为苯乙烯与其他单体的嵌段共聚物,更优选为单末端或两末端为苯乙烯嵌段的嵌段共聚物,尤其优选为两末端为苯乙烯嵌段的嵌段共聚物。若将聚苯乙烯系弹性体的两端设定为苯乙烯嵌段(来源于苯乙烯的重复单元),则有耐热性进一步提高的倾向。其原因在于:来源于耐热性高的苯乙烯的重复单元存在于末端。尤其通过苯乙烯嵌段(来源于苯乙烯的重复单元的嵌段部位)为反应性的聚苯乙烯系硬嵌段,有耐热性、耐化学品性更优异的倾向,因而优选。另外,可认为通过使用为嵌段共聚物的弹性体,在200℃以上将进行硬嵌段(hard block)与软嵌段(soft block)的相分离。可认为所述相分离的形状有助于抑制元件晶片的基板表面产生凹凸。此外,此种弹性体就在溶剂中的溶解性及对抗蚀剂溶剂的耐性的观点而言也更优选。
另外,若聚苯乙烯系弹性体为氢化产物,则对热的稳定性提高,不易引起分解或聚合等变质。进而,就在溶剂中的溶解性及对抗蚀剂溶剂的耐性的观点而言也更优选。
再者,本说明书中所谓“来源于苯乙烯的重复单元”,是指将苯乙烯或苯乙烯衍生物聚合时聚合物所含的来源于苯乙烯的构成单元,也可具有取代基。苯乙烯衍生物例如可列举:α-甲基苯乙烯、3-甲基苯乙烯、4-丙基苯乙烯、4-环己基苯乙烯等。取代基例如可列举:碳数1~5的烷基、碳数1~5的烷氧基、碳数1~5的烷氧基烷基、乙酰氧基、羧基等。
聚苯乙烯系弹性体的市售品例如可列举:塔釜普兰(Tufprene)A、塔釜普兰(Tufprene)125、塔釜普兰(Tufprene)126S、索尔普兰(Solprene)T、阿萨普兰(Asaprene)T-411、阿萨普兰(Asaprene)T-432、阿萨普兰(Asaprene)T-437、阿萨普兰(Asaprene)T-438、阿萨普兰(Asaprene)T-439、塔釜泰克(Tuftec)H1272、塔釜泰克(Tuftee)P1500、塔釜泰克(Tuftee)P5051、塔釜泰克(Tuftec)H1052、塔釜泰克(Tuftec)H1062、塔釜泰克(Tuftee)M1943、塔釜泰克(Tuftec)M1911、塔釜泰克(Tuftec)H1041、塔釜泰克(Tuftec)MP10、塔釜泰克(Tuftec)M1913、塔釜泰克(Tuftec)H1051、塔釜泰克(Tuftec)H1053、塔釜泰克(Tuftec)P2000、塔釜泰克(Tuftec)H1043(以上为旭化成(股)制造),弹性体AR-850C、弹性体AR815C、弹性体AR-840C、弹性体AR-830C、弹性体AR860C、弹性体AR-875C、弹性体AR-885C、弹性体AR-SC-15、弹性体AR-SC-0、弹性体AR-SC-5、弹性体AR-710、弹性体AR-SC-65、弹性体AR-SC-30、弹性体AR-SC-75、弹性体AR-SC-45、弹性体AR-720、弹性体AR-741、弹性体AR-731、弹性体AR-750、弹性体AR-760、弹性体AR-770、弹性体AR-781、弹性体AR-791、弹性体AR-FL-75N、弹性体AR-FL-85N、弹性体AR-FL-60N、弹性体AR-1050、弹性体AR-1060、弹性体AR-1040(亚龙化成(Aron Kasei)制造),科腾(Kraton)D1111、科腾(Kraton)D1113、科腾(Kraton)D1114、科腾(Kraton)D1117、科腾(Kraton)D1119、科腾(Kraton)D1124、科腾(Kraton)D1126、科腾(Kraton)D1161、科腾(Kraton)D1162、科腾(Kraton)D1163、科腾(Kraton)D1164、科腾(Kraton)D1165、科腾(Kraton)D1183、科腾(Kraton)D1193、科腾(Kraton)DX406、科腾(Kraton)D4141、科腾(Kraton)D4150、科腾(Kraton)D4153、科腾(Kraton)D4158、科腾(Kraton)D4270、科腾(Kraton)D4271、科腾(Kraton)D4433、科腾(Kraton)D1170、科腾(Kraton)D1171、科腾(Kraton)D1173、卡里弗莱克斯(Cariflex)IR0307、卡里弗莱克斯(Cariflex)IR0310、卡里弗莱克斯(Cariflex)IR0401、科腾(Kraton)D0242、科腾(Kraton)D1101、科腾(Kraton)D1102、科腾(Kraton)D1116、科腾(Kraton)D1118、科腾(Kraton)D1133、科腾(Kraton)D1152、科腾(Kraton)D1153、科腾(Kraton)D1155、科腾(Kraton)D1184、科腾(Kraton)D1186、科腾(Kraton)D1189、科腾(Kraton)D1191、科腾(Kraton)D1192、科腾(Kraton)DX405、科腾(Kraton)DX408、科腾(Kraton)DX410、科腾(Kraton)DX414、科腾(Kraton)DX415、科腾(Kraton)A1535、科腾(Kraton)A1536、科腾(Kraton)FG1901、科腾(Kraton)FG1924、科腾(Kraton)G1640、科腾(Kraton)G1641、科腾(Kraton)G1642、科腾(Kraton)G1643、科腾(Kraton)G1645、科腾(Kraton)G1633、科腾(Kraton)G1650、科腾(Kraton)G1651、科腾(Kraton)G1652、科腾(Kraton)G1654、科腾(Kraton)G1657、科腾(Kraton)G1660、科腾(Kraton)G1726、科腾(Kraton)G1701、科腾(Kraton)G1702、科腾(Kraton)G1730、科腾(Kraton)G1750、科腾(Kraton)G1765、科腾(Kraton)G4609、科腾(Kraton)G4610(科腾(Kraton)制造),TR2000、TR2001、TR2003、TR2250、TR2500、TR2601、TR2630、TR2787、TR2827、TR1086、TR1600、SIS5002、SIS5200、SIS5250、SIS5405、SIS5505、代那隆(Dynaron)6100P、代那隆(Dynaron)4600P、代那隆(Dynaron)6200P、代那隆(Dynaron)4630P、代那隆(Dynaron)8601P、代那隆(Dynaron)8630P、代那隆(Dynaron)8600P、代那隆(Dynaron)8903P、代那隆(Dynaron)6201B、代那隆(Dynaron)1321P、代那隆(Dynaron)1320P、代那隆(Dynaron)2324P、代那隆(Dynaron)9901P(捷时雅(JSR)(股)制造),电化STR(Denka STR)系列(电气化学工业(股)制造),可因塔克(Quintac)3520、可因塔克(Quintac)3433N、可因塔克(Quintac)3421、可因塔克(Quintac)3620、可因塔克(Quintac)3450、可因塔克(Quintac)3460(日本瑞翁(Zeon)制造),TPE-SB系列(住友化学(股)制造),拉巴隆(Rabalon)系列(三菱化学(股)制造),赛普顿(Septon)S1001、赛普顿(Septon)S8004、赛普顿(Septon)S4033、赛普顿(Septon)S2104、赛普顿(Septon)S8007、赛普顿(Septon)S2007、赛普顿(Septon)S2004、赛普顿(Septon)S2063、赛普顿(Septon)HG252、赛普顿(Septon)S8076、赛普顿(Septon)S2002、赛普顿(Septon)S1020、赛普顿(Septon)S8104、赛普顿(Septon)S2005、赛普顿(Septon)S2006、赛普顿(Septon)S4055、赛普顿(Septon)S4044、赛普顿(Septon)S4077、赛普顿(Septon)S4099、赛普顿(Septon)S8006、赛普顿(Septon)V9461、海布拉(Hybrar)7311、海布拉(Hybrar)7125、海布拉(Hybrar)5127、海布拉(Hybrar)5125(以上为可乐丽(Kuraray)制造),苏米弗莱克斯(Sumiflex)(住友电木(Sumitomo Bakelite)(股)制造),莱奥斯托马(Leostomer)、爱克提马(Actymer)(以上为理研乙烯基工业制造)等。
<<<聚酯系弹性体>>>
聚酯系弹性体并无特别限制,可根据目的而适当选择。例如可列举使二羧酸或其衍生物与二醇化合物或其衍生物进行缩聚所得的聚酯系弹性体。
二羧酸例如可列举:对苯二甲酸、间苯二甲酸、萘二羧酸等芳香族二羧酸及这些二羧酸的芳香核的氢原子经甲基、乙基、苯基等取代而成的芳香族二羧酸,己二酸、癸二酸、十二烷二羧酸等碳数2~20的脂肪族二羧酸,及环己烷二羧酸等脂环式二羧酸等。这些二羧酸可单独使用一种,也可并用两种以上。
二醇化合物例如可列举:乙二醇、1,3-丙二醇、1,4-丁二醇、1,6-己二醇、1,10-癸二醇、1,4-环己二醇等脂肪族二醇,脂环式二醇,下述结构式所表示的二元酚等。
[化2]
所述式中,YDO表示碳原子数1~10的亚烷基、碳原子数4~8的亚环烷基、-O-、-S-及-SO2-的任一个,或表示苯环彼此的直接键结(单键)。RDO1及RDO2分别独立地表示卤素原子或碳原子数1~12的烷基。pdo1及pdo2分别独立地表示0~4的整数,ndol表示0或1。
聚酯系弹性体的具体例可列举:双酚A、双-(4-羟基苯基)甲烷、双-(4-羟基-3-甲基苯基)丙烷、间苯二酚等。这些聚酯系弹性体可单独使用一种,也可并用两种以上。
另外,也可使用以芳香族聚酯(例如聚对苯二甲酸丁二酯)部分作为硬段(hardsegment)成分、以脂肪族聚酯(例如聚四亚甲基二醇)部分作为软段(soft segment)成分的多嵌段共聚物作为聚酯系弹性体。多嵌段共聚物中,可根据硬段与软段的种类、比率及分子量的差异而列举各种级别(grade)。具体例可列举:海特莱(Hytrel)(东丽杜邦(TorayDupont)(股)制造),佩尔普兰(Pelprene)(东洋纺织(股)制造),普利马罗(Primalloy)(三菱化学制造),奴贝兰(Nouvelan)(帝人化成制造),艾斯佩尔(Espel)1612、艾斯佩尔(Espel)1620(日立化成工业(股)制造),普利马罗(Primalloy)CP300(三菱化学公司制造)等。
<<<聚烯烃系弹性体>>>
聚烯烃系弹性体并无特别限制,可根据目的而适当选择。例如可列举:乙烯、丙烯、1-丁烯、1-己烯、4-甲基-戊烯等碳数2~20的α-烯烃的共聚物等。例如可列举乙烯-丙烯共聚物(EPR)、乙烯-丙烯-二烯共聚物(EPDM)等。另外可列举:二环戊二烯、1,4-己二烯、环辛二烯、亚甲基降冰片烯、亚乙基降冰片烯、丁二烯、异戊二烯等碳数2~20的非共轭二烯与α-烯烃共聚物等。另外可列举:在丁二烯-丙烯腈共聚物上共聚合甲基丙烯酸而成的羧基改性腈橡胶。具体可列举:乙烯·α-烯烃共聚物橡胶、乙烯·α-烯烃-非共轭二烯共聚物橡胶、丙烯·α-烯烃共聚物橡胶、丁烯·α-烯烃共聚物橡胶等。
市售品可列举:米拉斯托马(Milastomer)(三井化学(股)制造)、赛墨兰(Thermorun)(三菱化学制造)爱克赛特(EXACT)(艾克森(Exxon)化学制造)、英佳吉(ENGAGE)(陶氏化学(The Dow Chemical)制造)、艾斯伯莱克斯(Espolex)(住友化学制造)、沙林(Sarlink)(东洋纺制造)、纽康(Newcon)(日本聚丙烯(Polypro)制造)、爱克赛林(EXCELINK)(捷时雅(JSR)制造)等。
<<<聚氨基甲酸酯系弹性体>>>
聚氨基甲酸酯系弹性体并无特别限制,可根据目的而适当选择。例如可列举:含有包含低分子的二醇及二异氰酸酯的硬段、与包含高分子(长链)二醇及二异氰酸酯的软段的结构单元的弹性体等。
高分子(长链)二醇可列举:聚丙二醇、聚四亚甲基氧化物、聚(1,4-亚丁基己二酸酯)、聚(亚乙基·1,4-亚丁基己二酸酯)、聚己内酯、聚(1,6-亚己基碳酸酯)、聚(1,6-亚己基·亚新戊基己二酸酯)等。高分子(长链)二醇的数量平均分子量优选为500~10,000。
低分子的二醇可使用乙二醇、丙二醇、1,4-丁二醇、双酚A等短链二醇。短链二醇的数量平均分子量优选为48~500。
聚氨基甲酸酯系弹性体的市售品可列举:潘德克斯(PANDEX)T-2185、潘德克斯(PANDEX)T-2983N(迪爱生(DIC)(股)制造)、美拉龙(Miractran)(日本美拉龙(Miractran)制造),爱拉丝托兰(Elastollan)(巴斯夫(BASF)制造)、赖萨明(Resamine)(大日精化工业制造)、佩莱散(Pellethane)(陶氏化学(The Dow Chemical)制造)、爱昂来巴(IronRubber)(诺克(NOK)公司制造)、莫比龙(Mobilon)(日清纺化学(Nisshinbo Chemical)制造)等。
<<<聚酰胺系弹性体>>>
聚酰胺系弹性体并无特别限制,可根据目的而适当选择。例如可列举:将聚酰胺-6、聚酰胺-11、聚酰胺-12等聚酰胺用于硬段且将聚氧乙烯、聚氧丙烯、聚四亚甲基二醇等聚醚和/或聚酯用于软段的弹性体等。所述弹性体大致分为聚醚嵌段酰胺型、聚醚酯嵌段酰胺型这两种。
市售品可列举:优贝(UBE)聚酰胺弹性体、优贝斯达(UBESTA)XPA(宇部兴产(股)制造),带阿米德(Daiamide)(大赛璐-赫斯(Daicel-Huls)(股)制造),佩巴克斯(PEBAX)(东丽(Toray)(股)制造),葛丽伦(Grilon)ELY(日本艾曼斯(EMS-Group Japan)(股)制造),诺瓦米德(Novamid)(三菱化学(股)制造),葛丽拉克斯(Grilax)(迪爱生(DIC)(股)制造),聚醚酯酰胺PA-200、聚醚酯酰胺PA-201、聚醚酯酰胺TPAE-12、聚醚酯酰胺TPAE-32、聚酯酰胺TPAE-617、聚酯酰胺TPAE-617C(T&K托卡(T&K TOKA)(股)制造)等。
<<<聚酰亚胺系弹性体>>>
聚酰亚胺系弹性体并无特别限制,可根据目的而适当选择。例如可优选地使用:包含芳香族聚酰亚胺等工程塑料(engineering plastic)、及作为软段的分子量为几百~千的聚醚或聚酯或聚烯烃等橡胶成分,且硬段与软段交替缩聚而成的嵌段聚合物。市售品的具体例例如可列举优贝斯达(UBESTA)XPA9040F1(宇部兴产(股)制造)等。
<<<聚丙烯酸系弹性体>>>
聚丙烯酸系弹性体并无特别限制,可根据目的而适当选择。例如可列举:以丙烯酸乙酯、丙烯酸丁酯、丙烯酸甲氧基乙酯、丙烯酸乙氧基乙酯等丙烯酸酯作为主成分的聚丙烯酸系弹性体,
或丙烯酸酯与甲基丙烯酸缩水甘油酯、烯丙基缩水甘油醚等。更可列举将丙烯腈或乙烯等交联点单体共聚合而成的聚丙烯酸系弹性体等。具体可列举:丙烯腈-丙烯酸丁酯共聚物、丙烯腈-丙烯酸丁酯-丙烯酸乙酯共聚物、丙烯腈-丙烯酸丁酯-甲基丙烯酸缩水甘油酯共聚物等。
<<<硅酮系弹性体>>>
硅酮系弹性体并无特别限制,可根据目的而适当选择。例如可列举:以有机聚硅氧烷作为主成分的硅酮系弹性体,且其为聚二甲基硅氧烷系、聚甲基苯基硅氧烷系、聚二苯基硅氧烷等。市售品的具体例可列举:KE系列(信越化学工业(股)制造)、SE系列、CY系列、SH系列(以上为东丽道康宁硅酮(Toray-Dow coming silicone)(股)制造)等。
<<<其他弹性体>>>
本发明中,可使用经橡胶改性的环氧树脂(环氧系弹性体)作为弹性体。环氧系弹性体例如是通过以下方式而获得:利用两末端羧酸改性型丁二烯-丙烯腈橡胶、末端氨基改性硅酮橡胶等,将双酚F型环氧树脂、双酚A型环氧树脂、水杨醛型环氧树脂、苯酚酚醛清漆型环氧树脂或甲酚酚醛清漆型环氧树脂的一部分或全部的环氧基加以改性。
本发明的组合物优选为在组合物中以25质量%以上的比例而含有弹性体,更优选为28质量%以上,进而更优选为30质量%以上。本发明的组合物因弹性体的溶解性良好,故可提高弹性体浓度。通过提高组合物的弹性体浓度,可形成具有厚度的片等膜。
另外,优选为本发明的组合物的总固体成分的80质量%以上为弹性体,更优选为85质量%以上。
弹性体也可含有多种上述所列举的种类。
另外,弹性体优选为含有50质量%~100质量%的苯乙烯系弹性体,更优选为含有80质量%~100质量%,进而优选为含有90质量%~100质量%,进而更优选为含有95质量%~100质量%,尤其优选为实质上仅由苯乙烯系弹性体所构成。
<<(B)通式(1)所表示的沸点为160℃以上的溶剂>>
本发明的组合物含有(B)通式(1)所表示的沸点为160℃以上的溶剂(以下也称为溶剂(B))。
[化3]
通式(1)中,R1~R6分别独立地表示氢原子或脂肪族烃基。
再者,通式(1)的R1~R6不相互键结。也即,通式(1)所表示的化合物为单环的芳香族烃。
R1~R6所表示的脂肪族烃基可列举烷基、烯基、炔基等,优选为烷基。
烷基的碳数优选为1~20,更优选为1~10,进而优选为1~5。烷基优选为直链或分支。
烯基的碳数优选为2~20,更优选为2~10,进而优选为2~5。烷基优选为直链或分支。
炔基的碳数优选为2~20,更优选为2~10,进而优选为2~5。烷基优选为直链或分支。
R1~R6中优选为2个~4个为脂肪族烃基,更优选为2个~3个为脂肪族烃基。
溶剂(B)的沸点为160℃以上,优选为160℃~250℃,更优选为160℃~220℃。若为所述范围,则组合物的干燥性良好。进而容易形成干燥不均或厚度不均得到抑制的表面状态良好的片等膜。
溶剂(B)的SP值(溶解度参数(solubility parameter))优选为19(MPa)1/2以下,优选为18.5(MPa)1/2以下。下限例如优选为16.5(MPa)1/2以上。若溶剂(B)的SP值为19(MPa)1/2以下,则可进一步提高弹性体的溶解性。
再者,本发明中,SP值使用利用Hoy法所得的值。Hoy法的文献可优选地列举《H.L.霍伊:涂料技术杂志(H.L.Hoy:J.PaintTech.)》(42(540)、76-118(1970))或《SP值基础·应用与计算方法》(山本;信息机构;2005)。
溶剂(B)的具体例可列举:均三甲苯(mesitylene)(沸点165℃,SP值18.0(MPa)1/2)、对二异丙基苯(沸点210℃,SP值17.6(MPa)1/2)、对二乙基苯(沸点181℃,SP值18.0(MPa)1/2)、间二乙基苯(沸点182℃,SP值17.8(MPa)1/2)、1,3,5-三乙基苯(沸点218℃,SP值18.0(MPa)1/2等。
本发明的组合物优选为在组合物中以50质量%~75质量%的比例而含有溶剂(B),更优选为55质量%~70质量%,进而更优选为60质量%~70质量%。若溶剂(B)的含量为所述范围,则弹性体的溶解性及干燥性良好。
<<(C)沸点小于120℃的溶剂>>
本发明的组合物含有(C)沸点小于120℃的溶剂(以下也称为溶剂(C))。
溶剂(C)的沸点小于120℃,优选为110℃以下,进而更优选为105℃以下。下限优选为60℃以上,更优选为65℃以上,进而优选为70℃以上。若为所述范围,则组合物的干燥性良好。进而容易形成干燥不均或厚度不均得到抑制的表面状态良好的片等膜。
溶剂(C)的SP值优选为19(MPa)1/2以下,优选为18.5(MPa)1/2以下。下限例如优选为16.5(MPa)1/2以上。若溶剂(C)的SP值为19(MPa)1/2以下,则可进一步提高弹性体的溶解性。
溶剂(C)可使用选自芳香族烃、脂环式烃及环状醚中的一种以上。
芳香族烃可列举甲苯(沸点111℃,SP值18.2(MPa)1/2)、苯(沸点80℃,SP值18.5(MPa)1/2)等。
脂环式烃可列举环己烷(沸点81℃,SP值16.8(MPa)1/2)、甲基环己烷(沸点101℃,SP值16.0(MPa)1/2)等。
环状醚可列举四氢呋喃(沸点66℃,SP值19.5(MPa)1/2)等。
本发明的组合物优选为在组合物中以5质量%~65质量%的比例而含有溶剂(C),更优选为5质量%~60质量%,进而更优选为10质量%~60质量%。若溶剂(C)的含量为所述范围,则弹性体的溶解性及干燥性良好。
本发明的组合物中溶剂(B)与溶剂(C)的质量比优选为溶剂(B)∶溶剂(C)=80∶20~99∶1,更优选为85∶15~99∶1,进而优选为90∶10~99∶1。若溶剂(B)与溶剂(C)的质量比为所述范围,则弹性体的溶解性良好,容易形成提高干燥性并且表面状态良好的片等膜。
<<抗氧化剂>>
本发明的组合物优选为含有抗氧化剂。通过含有抗氧化剂,可进一步提高所获得的膜的耐热性。进而容易形成层压性优异的片等膜。
抗氧化剂可使用:酚系抗氧化剂、硫系抗氧化剂、磷系抗氧化剂、醌系抗氧化剂、胺系抗氧化剂等。
酚系抗氧化剂例如可列举:对甲氧基苯酚、2,6-二-叔丁基-4-甲基苯酚,巴斯夫(BASF)(股)制造的“易加乐斯(Irganox)(注册商标)1010”、“易加乐斯(Irganox)(注册商标)1330”、“易加乐斯(Irganox)(注册商标)3114”、“易加乐斯(Irganox)(注册商标)1035”,住友化学(股)制造的“苏米莱泽(Sumilizer)(注册商标)MDP-S”、“苏米莱泽(Sumilizer)(注册商标)GA-80”等。
硫系抗氧化剂例如可列举:3,3′-硫代二丙酸二硬脂酯,住友化学(股)制造的“苏米莱泽(Sumilizer)(注册商标)TPM”、“苏米莱泽(Sumilizer)(注册商标)TPS”、“苏米莱泽(Sumilizer)(注册商标)TP-D”等。
磷系抗氧化剂例如可列举:亚磷酸三(2,4-二-叔丁基苯基)酯、双(2,4-二-叔丁基苯基)季戊四醇二亚磷酸酯、聚(二丙二醇)苯基亚磷酸酯、亚磷酸二苯基异癸基酯、亚磷酸-2-乙基己基二苯基酯、亚磷酸三苯酯,巴斯夫(BASF)(股)制造的“艳佳佛(Irgafos)(注册商标)168”、“艳佳佛(Irgafos)(注册商标)38”等。
醌系抗氧化剂例如可列举对苯醌、2-叔丁基-1,4-苯醌等。
胺系抗氧化剂例如可列举二甲基苯胺或吩噻嗪等。
抗氧化剂优选为易加乐斯(Irganox)(注册商标)1010、易加乐斯(Irganox)(注册商标)1330、3,3′-硫代二丙酸二硬脂酯、苏米莱泽(Sumilizer)(注册商标)TP-D,更优选为易加乐斯(Irganox)(注册商标)1010、易加乐斯(Irganox)(注册商标)1330,尤其优选为易加乐斯(Irganox)(注册商标)1010。
另外,所述抗氧化剂中,优选为将酚系抗氧化剂与硫系抗氧化剂或磷系抗氧化剂并用,最优选为将酚系抗氧化剂与硫系抗氧化剂并用。尤其在使用聚苯乙烯系弹性体作为弹性体的情形时,优选为将酚系抗氧化剂与硫系抗氧化剂并用。通过设定为此种组合,可期待可高效地抑制由氧化反应所致的弹性体的劣化的效果。进而容易形成层压性优异的片等膜。
在将酚系抗氧化剂与硫系抗氧化剂并用的情形时,酚系抗氧化剂与硫系抗氧化剂的质量比优选为酚系抗氧化剂∶硫系抗氧化剂=95∶5~5∶95,更优选为25∶75~75∶25。若为所述范围,则可有效地防止将膜暴露于高温下时的分解。
抗氧化剂的组合优选为易加乐斯(Irganox)(注册商标)1010与苏米莱泽(Sumilizer)(注册商标)TP-D、易加乐斯(Irganox)(注册商标)1330与苏米莱泽(Sumilizer)(注册商标)TP-D、及苏米莱泽(Sumilizer)(注册商标)GA-80与苏米莱泽(Sumilizer)(注册商标)TP-D,更优选为易加乐斯(Irganox)(注册商标)1010与苏米莱泽(Sumilizer)(注册商标)TP-D、易加乐斯(Irganox)(注册商标)1330与苏米莱泽(Sumilizer)(注册商标)TP-D,尤其优选为易加乐斯(Irganox)(注册商标)1010与苏米莱泽(Sumilizer)(注册商标)TP-D。
就防止加热中的升华的观点而言,抗氧化剂的分子量优选为400以上,更优选为600以上,尤其优选为750以上。
抗氧化剂优选为以1质量%~7质量%的比例而含有于组合物中。下限更优选为1.2质量%以上,进而优选为1.5质量%以上。上限优选为6质量%以下,进而优选为5质量%以下。若为所述范围,则容易形成表面状态良好且耐热性及层压性优异的片等膜。
抗氧化剂可仅为一种,也可为两种以上。在抗氧化剂为两种以上的情形时,优选为其合计为所述范围。
<<<高分子化合物>>>
本发明的组合物视需要也可含有除上文所述的弹性体以外的高分子化合物。
本发明中,高分子化合物可使用任意者。高分子化合物为重量平均分子量为2000以上的化合物,通常为不含聚合性基的化合物。高分子化合物的重量平均分子量优选为10,000~1,000,000,优选为50,000~500,000,更优选为100,000~300,000。
高分子化合物的具体例例如可列举:烃树脂、酚醛清漆树脂、酚树脂、环氧树脂、三聚氰胺树脂、脲树脂、不饱和聚酯树脂、醇酸树脂、聚氯乙烯树脂、聚乙酸乙烯酯树脂、铁氟龙(Teflon)(注册商标)、聚酰胺树脂、聚缩醛树脂、聚碳酸酯树脂、聚对苯二甲酸丁二酯树脂、聚对苯二甲酸乙二酯树脂、聚砜树脂、聚醚砜树脂、聚芳酯树脂等合成树脂,或天然橡胶等天然树脂。其中,优选为烃树脂、酚醛清漆树脂,更优选为烃树脂。高分子化合物视需要也可组合使用两种以上。
烃树脂可任意使用。
烃树脂是指基本上仅包含碳原子及氢原子的树脂,但若基本骨架为烃树脂,则也可含有其他原子作为侧链。即,仅包含碳原子及氢原子的烃树脂中,如丙烯酸系树脂、聚乙烯醇树脂、聚乙烯基缩醛树脂、聚乙烯基吡咯烷酮树脂般烃基以外的官能基直接键结于主链的情形也包含在本发明的烃树脂中,在所述情形时,相对于树脂的所有重复单元,烃基直接键结于主链而成的重复单元的含量优选为30mol%(摩尔百分比)以上。
符合所述条件的烃树脂例如可列举:萜烯树脂、萜烯酚树脂、改性萜烯树脂、氢化萜烯树脂、氢化萜烯酚树脂、松香、松香酯、氢化松香、氢化松香酯、聚合松香、聚合松香酯、改性松香、松香改性酚树脂、烷基酚树脂、脂肪族石油树脂、芳香族石油树脂、氢化石油树脂、改性石油树脂、脂环族石油树脂、苯并呋喃(coumarone)石油树脂、茚石油树脂、聚苯乙烯-聚烯烃共聚物、烯烃聚合物(例如甲基戊烯共聚物)、及环烯烃聚合物(例如降冰片烯共聚物、二环戊二烯共聚物、四环十二烯共聚物)等。
其中,烃树脂优选为萜烯树脂、松香、石油树脂、氢化松香、聚合松香、烯烃聚合物或环烯烃聚合物,更优选为萜烯树脂、松香、烯烃聚合物或环烯烃聚合物,更优选为萜烯树脂、松香、烯烃聚合物或环烯烃聚合物,进而优选为萜烯树脂、松香、环烯烃聚合物或烯烃聚合物,尤其优选为环烯烃聚合物。
环烯烃聚合物可列举:降冰片烯系聚合物、单环的环状烯烃的聚合物、环状共轭二烯的聚合物、乙烯基脂环式烃聚合物及这些聚合物的氢化物(hydride)等。环烯烃聚合物的优选例可列举:含有至少一种下述通式(II)所表示的重复单元的加成(共)聚合物、及还含有至少一种通式(I)所表示的重复单元而成的加成(共)聚合物。另外,环烯烃聚合物的其他优选例可列举含有至少一种通式(III)所表示的环状重复单元的开环(共)聚合物。
[化4]
式中,m表示0~4的整数。R1~R6分别表示氢原子或碳数1~10的烃基,X1~X3及Y1~Y3分别表示氢原子、碳数1~10的烃基、卤素原子、经卤素原子取代的碳数1~10的烃基、-(CH2)nCOOR11、-(CH2)nOCOR12、-(CH2)nNCO、-(CH2)nNO2、-(CH2)nCN、-(CH2)nCONR13R14、-(CH2)nNR15R16、-(CH2)nOZ、-(CH2)nW,或者由X1与Y1、X2与Y2或X3与Y3所构成的(-CO)2O、(-CO)2NR17。R11、R12、R13、R14、R15、R16及R17分别表示氢原子或烃基(优选为碳数1~20的烃基),Z表示烃基或经卤素取代的烃基,W表示SiR18 pD3-p(R18表示碳数1~10的烃基,D表示卤素原子,表示-OCOR18或-OR18,p表示0~3的整数)。n表示0~10的整数。
降冰片烯系聚合物是揭示于日本专利特开平10-7732号公报、日本专利特表2002-504184号公报、US2004/229157A1号公报或WO2004/070463A1号公报等中。降冰片烯系聚合物可通过使降冰片烯系多环状不饱和化合物彼此进行加成聚合而获得。另外,视需要也可使降冰片烯系多环状不饱和化合物与以下化合物进行加成聚合:乙烯、丙烯、丁烯;丁二烯、异戊二烯般的共轭二烯;亚乙基降冰片烯般的非共轭二烯。所述降冰片烯系聚合物是由三井化学(股)以爱佩尔(APL)的商品名而销售,有玻璃化温度(Tg)不同的例如爱佩尔(APL)8008T(Tg为70℃)、爱佩尔(APL)6013T(Tg为125℃)或爱佩尔(APL)6015T(Tg为145℃)等级别。由宝理塑料(Poly plastics)(股)销售托帕斯(TOPAS)8007、托帕斯(TOPAS)5013、托帕斯(TOPAS)6013、托帕斯(TOPAS)6015等的颗粒。进而,由费拉尼亚(Ferrania)公司销售爱比亚(Appear)3000。
如日本专利特开平1-240517号公报、日本专利特开平7-196736号公报、日本专利特开昭60-26024号公报、日本专利特开昭62-19801号公报、日本专利特开2003-1159767号公报或日本专利特开2004-309979号公报等所揭示般,降冰片烯系聚合物的氢化物可通过使多环状不饱和化合物进行加成聚合或复分解(metathesis)开环聚合后,加以氢化而制造。
通式(III)中,R5及R6优选为氢原子或甲基,X3及Y3优选为氢原子,其他基团可适当选择。所述降冰片烯系聚合物是由捷时雅(JSR)(股)以雅顿(Arton)G或雅顿(Arton)F等商品名而销售,另外由日本瑞翁(Zeon)(股)以瑞奥(Zeonor)ZF14、瑞奥(Zeonor)ZF16、瑞诺(Zeonex)250、瑞诺(Zeonex)280、瑞诺(Zeonex)480R等商品名而市售,可使用这些商品。
在本发明的组合物含有高分子化合物的情形时,相对于本发明的组合物的总固体成分,高分子化合物的含量优选为5质量%以上,更优选为10质量%以上,进而优选为20质量%以上。另外,相对于本发明的组合物的总固体成分,高分子化合物的含量的上限优选为70质量%以下,更优选为60质量%以下,进而优选为50质量%以下,尤其优选为40质量%以下。
本发明的组合物也可设定为实质上不含弹性体以外的高分子化合物的构成。所谓“实质上不含高分子化合物”,例如相对于弹性体的总固体部,高分子化合物的含量优选为1质量%以下,更优选为0.1质量%以下,进而更优选为不含高分子化合物。
<<<表面活性剂>>>
本发明的组合物也可含有表面活性剂。表面活性剂可使用氟系表面活性剂、非离子系表面活性剂、阳离子系表面活性剂、阴离子系表面活性剂、硅酮系表面活性剂等各种表面活性剂,优选为氟系表面活性剂。通过含有表面活性剂,溶液特性(特别是流动性)提高,在涂布形成接着膜的情形时,可进一步改善涂布厚度的均匀性或省液性。
氟系表面活性剂的氟含有率优选为3质量%~40质量%,更优选为5质量%~30质量%,进而优选为7质量%~25质量%。氟含有率为所述范围内的氟系表面活性剂在涂布膜的厚度的均匀性或省液性的方面有效果。进而,溶解性也良好。
氟系表面活性剂例如可列举:迪爱生(DIC)(股)制造的美佳法(Megafac)F-251、美佳法(Megafac)F-281、美佳法(Megafac)F-430、美佳法(Megafac)F-444、美佳法(Megafac)F-477、美佳法(Megafac)F-510、美佳法(Megafac)F-552、美佳法(Megafac)F-553、美佳法(Megafac)F-554、美佳法(Megafac)F-555、美佳法(Megafac)F-556、美佳法(Megafac)F-557、美佳法(Megafac)F-558、美佳法(Megafac)F-559、美佳法(Megafac)F-560、美佳法(Megafac)F-561、美佳法(Megafac)F-562、美佳法(Megafac)F-563、美佳法(Megafac)F-565、美佳法(Megafac)F-567、美佳法(Megafac)F-568、美佳法(Megafac)F-569、美佳法(Megafac)F-570、美佳法(Megafac)F-571、美佳法(Megafac)R-40、美佳法(Megafac)R-41、美佳法(Megafac)R-43、美佳法(Megafac)R-94,住友3M(股)制造的FC-4430、FC-4432,AGC清美化学(AGC Seimi Chemical)(股)制造的沙福隆(Surflon)S-242、沙福隆(Surflon)S-243、沙福隆(Surflon)S-386、沙福隆(Surflon)S-651、沙福隆(Surflon)S-611、沙福隆(Surflon)S-420,欧诺法(OMNOVA)公司制造的PF-636、PF-656、PF-6320、PF-6520、PF-7002等。
非离子系表面活性剂可列举:甘油、三羟甲基丙烷、三羟甲基乙烷以及这些化合物的乙氧基化物及丙氧基化物(例如丙氧基化甘油、乙氧基化甘油等)、聚氧亚乙基月桂基醚、聚氧亚乙基硬脂基醚、聚氧亚乙基油基醚、聚氧亚乙基辛基苯基醚、聚氧亚乙基壬基苯基醚、聚乙二醇二月桂酸酯、聚乙二醇二硬脂酸酯等。
阳离子系表面活性剂可列举:森下产业(股)制造的EFKA-745,共荣社化学(股)制造的宝理弗洛(Polyflow)No.75、No.90、No.95等。
硅酮系表面活性剂可列举:迈图高新材料日本有限公司(Momentive PerformanceMaterials Japan LLC)制造的TSF-4440、TSF-4300、TSF-4445、TSF-4460、TSF-4452,信越硅酮(股)制造的KP-341、KF-6001、KF-6002,毕克化学(BYK Chemie)(股)制造的BYK-307、BYK-323、BYK-330等。
在本发明的组合物含有表面活性剂的情形时,表面活性剂优选为以0.001质量%~2.0质量%的比例而含有于本发明的组合物中,更优选为0.005质量%~1.0质量%。
表面活性剂可仅为一种,也可为两种以上。在表面活性剂为两种以上的情形时,优选为其合计为所述范围。
<<其他添加剂>>
本发明的组合物可在不损及本发明的效果的范围内,视需要而调配各种添加物,例如硬化剂、硬化催化剂、填充剂、密接促进剂、紫外线吸收剂、抗凝聚剂等。在调配这些添加剂的情形时,其合计调配量优选为组合物的总固体成分的3质量%以下。
<组合物的制备>
本发明的组合物可混合所述各成分来制备。通常在0℃~100℃的范围下进行各成分的混合。另外,在混合各成分后,例如优选为利用过滤器进行过滤。过滤可以多阶段来进行也可重复进行多次。另外,也可对经过滤的液体进行再过滤。
过滤器只要为一直以来用于过滤用途等的过滤器,则可无特别限定地使用。例如可列举由聚四氟乙烯(polytetrafluoroethylene,PTFE)等氟树脂;尼龙-6、尼龙-6,6等聚酰胺系树脂;聚乙烯、聚丙烯(polypropylene,PP)等聚烯烃树脂(包含高密度、超高分子量)等而得的过滤器。这些原材料中,优选为聚丙烯(包含高密度聚丙烯)及尼龙。
过滤器的孔径例如适宜为0.003μm~5.0μm左右。通过设为所述范围,而可抑制过滤堵塞,且可确实地去除组合物中所含的杂质或凝聚物等微细的异物。
在使用过滤器时,也可将不同的过滤器组合。此时,利用第1过滤器的过滤可仅进行一次,也可进行两次以上。在将不同的过滤器组合而进行两次以上的过滤的情形时,优选为第2次以后的孔径与第1次过滤的孔径相同或较第1次过滤的孔径小。另外,也可将在所述范围内孔径不同的第1过滤器组合。此处的孔径可参照过滤器厂商(filter maker)的标称值。市售的过滤器例如可自日本颇尔(pall)股份有限公司、爱德万东洋(Advantec Toyo)股份有限公司、日本英特格(Entegris)股份有限公司(原日本密科理(Mykrolis)股份有限公司)或北泽微滤器(KITZ Micro Filter)股份有限公司等提供的各种过滤器中选择。
本发明的组合物优选为固体成分浓度为25质量%~40质量%。下限更优选为26质量%以上,进而优选为27质量%以上。上限更优选为38质量%以下,进而优选为36质量%以下。
本发明的组合物的弹性体的溶解性良好,可提高固体成分浓度。通过将固体成分浓度设为所述范围,也可形成具有厚度的片。
<片、层叠体、片的制造方法>
本发明的片的制造方法包括将所述组合物施用于支撑体上,并使其干燥的步骤。
另外,本发明的片是使所述组合物干燥而获得者。
另外,本发明的层叠体在使所述组合物干燥而获得的片的单面或两面上具有具备脱模性的支撑体。
以下,使用本发明的片的制造方法也一并对片及层叠体进行说明。
在本发明的片的制造方法中,组合物的施用方法可列举:利用压力自狭缝状的开口中挤出组合物而施用的方法;利用凹版或网纹辊转印组合物而施用的方法;一面自喷雾器(spray)或分注器(dispenser)中喷出组合物一面扫描而施用的方法;将组合物蓄积于槽(tank)中,使支撑体在其中通过,由此进行浸渍涂布的方法;利用线棒一面推动组合物一面刮取,由此而施用的方法等。
施用组合物的支撑体可列举转筒(drum)、带(band)等。另外,支撑体也可使用脱模膜(具有脱模性的支撑体)。
将组合物施用于支撑体上后,加以干燥而成为经固体化的片后,将片自支撑体上机械剥离,由此可获得单体的片(膜)。
干燥条件优选为在100℃~210℃下进行120秒~900秒。干燥温度更优选为105℃~200℃,进而优选为110℃~190℃。干燥时间更优选为150秒~800秒,进而优选为180秒~600秒。
干燥也可分成两阶段而阶段性地提升温度来实施。
另外,在使用脱模膜作为供施用组合物的支撑体的情形时,也可不将片自支撑体上剥离而残留,制成带有脱模膜的片(层叠体)。
通过连续地进行这些处理,可获得辊状的长条片。长条片的长度并无特别限定,下限例如优选为5000mm以上,更优选为1000mm以上。上限例如优选为500000mm以下,更优选为200000mm以下。
另外,也可在片的两面上贴合脱模膜(具有脱模性的支撑体),制成两面带有脱模膜的片(层叠体)。
通过在片的单面或两面上贴合脱模膜,可防止对片的表面造成损伤、或在保管中贴附的困扰(trouble)。脱模膜可在使用时剥离去除。例如于在两面上贴合有脱模膜的情形时,可将单面的脱模膜剥下,将片表面层压于元件晶片或支撑体等上后,将剩余的脱模膜剥下,由此可尽可能地保持片表面的清洁。
本发明中,片的平均厚度并无特别限定,例如优选为40μm~140μm,更优选为50μm~130μm,进而优选为60μm~120μm。若片的平均厚度为所述范围,则对元件晶片的表面形状的追随性良好,可均匀地贴合于元件晶片的元件面。进而,也不易产生暂时接着后的加工时的逸气增加、或贴合时的偏移等。
再者,本发明中,片的平均厚度是定义为利用测微计(micrometer)在沿着片的一方向的剖面中自一个端面向另一端面以等间隔对5处的厚度进行测定所得的值的平均值。
再者,本发明中,所谓“沿着片的一方向的剖面”,在片为多边形状的情形时,是指与长边方向正交的剖面。另外,在片为正方形状的情形时,是指与任一边正交的剖面。另外,在片为圆形或椭圆形的情形时,是指通过重心的剖面。
片优选为在沿着片的一方向的剖面中,最大膜厚与最小膜厚的差为平均膜厚的10%以下,更优选为5%以下。
本发明中,片的溶剂含有率优选为1质量%以下,更优选为0.1质量%以下,理想的是实质上不含有,例如为0质量%。
<接着性支撑基板>
继而,对使用本发明的片的接着性支撑基板加以说明。
接着性支撑基板在支撑基板的表面上具有本发明的片。
可在支撑基板上层压上文所述的本发明的片而形成暂时接着用层叠体。例如可列举:将片安置于真空层压机中,利用所述装置使片位于支撑基板上,在真空下使片与支撑基板接触,利用辊等压接而将片固定(层叠)于支撑基板上的方法等。另外,固定于支撑基板的片也可切割成例如圆形状等所需形状。
接着性支撑基板中,支撑基板并无特别限定,例如可列举硅基板、玻璃基板、金属基板、化合物半导体基板等。其中,鉴于不易污染作为半导体装置的基板而代表性地使用的硅基板的方面、或可使用于半导体装置的制造步骤中广泛使用的静电夹盘(chuck)的方面等,优选为硅基板。
支撑基板的厚度并无特别限定,例如优选为300μm~100mm,更优选为300μm~10mm。
也可在支撑基板的表面上设置脱模层。脱模层优选为含有氟原子和/或硅原子的低表面能量层,优选为具有含有氟原子和/或硅原子的材料。脱模层的氟含有率优选为30质量%~80质量%,更优选为40质量%~76质量%,尤其优选为60质量%~75质量%。
<带有元件晶片的层叠体>
继而,对本发明的带有元件晶片的层叠体加以说明。
本发明的带有元件晶片的层叠体是在元件晶片与支撑基板之间具有上文所述的本发明的片,且片的一个表面与元件晶片的元件面接触,另一表面与支撑基板的表面接触。
元件晶片可无限制地使用公知者,例如可列举硅基板、化合物半导体基板等。化合物半导体基板的具体例可列举:SiC基板、SiGe基板、ZnS基板、ZnSe基板、GaAs基板、InP基板、GaN基板等。
也可在元件晶片的表面上形成有机械结构或电路。形成有机械结构或电路的元件晶片例如可列举:微机电***(Micro Electro Mechanical Systems,MEMS)、功率元件、图像传感器(image sensor)、微传感器(microsensor)、发光二极管(Light Emitting Diode,LED)、光学元件、内插器(interposer)、嵌埋型元件、微元件等。
元件晶片优选为具有金属岸堤(bank)等结构。根据本发明,对在表面上具有结构的元件晶片,也可稳定地暂时接着,并且可容易地解除对元件晶片的暂时接着。结构的高度并无特别限定,例如优选为1μm~150μm,更优选为5μm~100μm。
实施机械处理或化学处理之前的元件晶片的膜厚优选为500μm以上,更优选为600μm以上,进而优选为700μm以上。上限例如优选为2000μm以下,更优选为1500μm以下。
实施机械处理或化学处理而薄膜化后的元件晶片的膜厚例如优选为小于500μm,更优选为400μm以下,进而优选为300μm以下。下限例如优选为1μm以上,更优选为5μm以上。
在本发明的带有元件晶片的层叠体中,支撑基板与上文所述的接着性支撑基板中说明的支撑基板为相同含意,优选范围也相同。
本发明的带有元件晶片的层叠体也可在支撑基板与元件晶片之间配置上文所述的本发明的片,进行加热压接而制造。
<半导体装置的制造方法>
以下,一面参照图1,一面对经过制造带有元件晶片的层叠体的步骤的半导体装置的制造方法的一实施方式加以说明。再者,本发明不限定于以下的实施方式。
图1(A)~图1(E)分别为对支撑基板与元件晶片的暂时接着加以说明的概略剖面图(图1(A)、图1(B))、表示暂时接着于支撑基板上的元件晶片经薄型化的状态(图1(C))、将支撑基板与元件晶片剥离的状态(图1(D))、自元件晶片上去除接着层后的状态(图1(E))的概略剖面图。
所述实施方式中,如图1(A)所示,首先准备在支撑基板12上设置片11而成的接着性支撑基板100。接着性支撑基板100可利用上文所述的方法来制造。接着性支撑基板100优选为实质上不含溶剂的形态。
元件晶片60是在硅基板61的表面61a上设置多个元件芯片62而成。
硅基板61的厚度例如优选为200μm~1200μm。元件芯片62例如优选为金属结构体,高度优选为10μm~100μm。
继而,如图1(B)所示,使接着性支撑基板100与元件晶片60压接,使支撑基板12与元件晶片60暂时接着。
片11优选为将元件芯片62完全覆盖,在将元件芯片的高度设为X μm、片的厚度设为Yμm的情形时,优选为满足“X+100≥Y>X”的关系。
片11将元件芯片62完全被覆的情况在欲进一步减小薄型元件晶片的总厚度变动(Total Thickness Variation,TTV)的情形(即,欲进一步提高薄型元件晶片的平坦性的情形)时有效。
即,在将元件晶片加以薄型化时,通过利用片11来保护多个元件芯片62,可使与支撑基板12的接触面中几乎不存在凹凸形状。因此,即便在如此般支撑的状态下加以薄型化,也减少将来源于多个元件芯片62的形状转印至薄型元件晶片的背面61b1的担忧,结果可进一步减小最终获得的薄型元件晶片的TTV。
继而,如图1(C)所示,对硅基板61的背面61b实施机械处理或化学处理(并无特别限定,例如滑动或化学机械研磨(Chemical-Mechanical Polishing,CMP)等薄膜化处理,化学气相成长(Chemical Vapor Deposition,CVD)或物理气相成长(Physical VaporDeposition,PVD)等高温·真空下的处理,使用有机溶剂、酸性处理液或碱性处理液等化学品的处理,镀敷处理,光化射线的照射,加热·冷却处理等),如图1(C)所示,使硅基板61的厚度变薄(例如优选为平均厚度小于500μm,更优选为1μm~200μm),获得薄型元件晶片60a。
另外,也可进行以下处理作为机械处理或化学处理:在薄膜化处理后,形成自薄型元件晶片60a的背面61b1贯穿硅基板的贯通孔(未图示),在所述贯通孔内形成硅贯通电极(未图示)。具体而言,加热处理中的最高到达温度优选为130℃~400℃,更优选为180℃~350℃。加热处理的最高到达温度优选为设定为低于片的软化点的温度。加热处理优选为最高到达温度下的30秒钟~30分钟的加热,更优选为最高到达温度下的1分钟~10分钟的加热。
继而,如图1(D)所示,使支撑基板12自薄型元件晶片60a脱离。脱离的方法并无特别限定,优选为不进行任何处理而自薄型元件晶片60a的端部相对于薄型元件晶片60a沿垂直方向上拉而剥离。此时,关于剥离界面,优选为在支撑基板12与片11的界面上剥离。在所述情形时,若将支撑基板12与片11的界面的剥离强度设为A、元件晶片表面61a与片11的剥离强度设为B,则优选为满足以下的式子。
A<B…·式(1)
另外,也可使片11与后述剥离液接触,其后,视需要使薄型元件晶片60a相对于支撑基板12而滑动后,自薄型元件晶片60a的端部相对于元件晶片沿垂直方向上拉而剥离。
<剥离液>
以下,对剥离液加以详细说明。
剥离液可使用水及溶剂(有机溶剂)。
另外,剥离液优选为溶解片11的有机溶剂。有机溶剂例如可列举:脂肪族烃类(己烷、庚烷,艾索帕(Isopar)E、艾索帕(Isopar)H、艾索帕(Isopar)G(埃索化学(EssoChemical)(股)制造)等)、芳香族烃类(甲苯、二甲苯等)、卤化烃(二氯甲烷、二氯乙烯、三氯乙烯、单氯苯等)、极性溶剂。极性溶剂可列举:醇类(甲醇、乙醇、丙醇、异丙醇、1-丁醇、1-戊醇、1-己醇、1-庚醇、1-辛醇、2-辛醇、2-乙基-1-己醇、1-壬醇、1-癸醇、苄醇、乙二醇单甲醚、2-乙氧基乙醇、二乙二醇单***、二乙二醇单己醚、三乙二醇单甲醚、丙二醇单***、丙二醇单甲醚、聚乙二醇单甲醚、聚丙二醇、四乙二醇、乙二醇单丁醚、乙二醇单苄醚、乙二醇单苯醚、丙二醇单苯醚、甲基苯基原醇、正戊醇、甲基戊醇等)、酮类(丙酮、甲基乙基酮、乙基丁基酮、甲基异丁基酮、环己酮等)、酯类(乙酸乙酯、乙酸丙酯、乙酸丁酯、乙酸戊酯、乙酸苄酯、乳酸甲酯、乳酸丁酯、乙二醇单丁基乙酸酯、丙二醇单甲醚乙酸酯、二乙二醇乙酸酯、邻苯二甲酸二乙酯、乙酰丙酸丁酯等)、其他(磷酸三乙酯、磷酸三甲苯酯、N-苯基乙醇胺、N-苯基二乙醇胺、N-甲基二乙醇胺、N-乙基二乙醇胺、4-(2-羟基乙基)吗啉、N,N-二甲基乙酰胺、N-甲基吡咯烷酮等)等。
进而,就剥离性的观点而言,剥离液也可含有碱、酸及表面活性剂。在调配这些成分的情形时,调配量分别优选为剥离液的0.1质量%~5.0质量%。
进而,就剥离性的观点而言,将两种以上的有机溶剂及水、两种以上的碱、酸及表面活性剂混合的形态也优选。
碱例如可使用:磷酸三钠、磷酸三钾、磷酸三铵、磷酸氢二钠、磷酸氢二钾、磷酸氢二铵、碳酸钠、碳酸钾、碳酸铵、碳酸氢钠、碳酸氢钾、碳酸氢铵、硼酸钠、硼酸钾、硼酸铵、氢氧化钠、氢氧化铵、氢氧化钾及氢氧化锂等无机碱剂,或单甲胺、二甲胺、三甲胺、单乙胺、二乙胺、三乙胺、单异丙胺、二异丙胺、三异丙胺、正丁胺、单乙醇胺、二乙醇胺、三乙醇胺、单异丙醇胺、二异丙醇胺、亚乙基亚胺、乙二胺、吡啶、氢氧化四甲基铵等有机碱剂。这些碱剂可单独使用或组合使用两种以上。
酸可使用:卤化氢、硫酸、硝酸、磷酸、硼酸等无机酸,或甲磺酸、乙磺酸、苯磺酸、对甲苯磺酸、三氟甲磺酸、乙酸、柠檬酸、甲酸、葡萄糖酸、乳酸、草酸、酒石酸等有机酸。
表面活性剂可使用阴离子系、阳离子系、非离子系、两性离子系的表面活性剂。在所述情形时,相对于碱性水溶液的总量,表面活性剂的含量优选为1质量%~20质量%,更优选为1质量%~10质量%。
通过将表面活性剂的含量设定为所述范围内,有可进一步提高片11与薄型元件晶片60a的剥离性的倾向。
阴离子系表面活性剂并无特别限定,可列举:脂肪酸盐类、松香酸盐类、羟基烷烃磺酸盐类、烷烃磺酸盐类、二烷基磺基琥珀酸盐类、直链烷基苯磺酸盐类、分支链烷基苯磺酸盐类、烷基萘磺酸盐类、烷基二苯基醚(二)磺酸盐类、烷基苯氧基聚氧亚乙基烷基磺酸盐类、聚氧亚乙基烷基磺基苯基醚盐类、N-烷基-N-油基牛磺酸钠类、N-烷基磺基琥珀酸单酰胺二钠盐类、石油磺酸盐类、硫酸化蓖麻油、硫酸化牛脂油、脂肪酸烷基酯的硫酸酯盐类、烷基硫酸酯盐类、聚氧亚乙基烷基醚硫酸酯盐类、脂肪酸单甘油酯硫酸酯盐类、聚氧亚乙基烷基苯基醚硫酸酯盐类、聚氧亚乙基苯乙烯基苯基醚硫酸酯盐类、烷基磷酸酯盐类、聚氧亚乙基烷基醚磷酸酯盐类、聚氧亚乙基烷基苯基醚磷酸酯盐类、苯乙烯-马来酸酐共聚物的部分皂化物类、烯烃-马来酸酐共聚物的部分皂化物类、萘磺酸盐***缩合物类等。其中,可尤其优选地使用烷基苯磺酸盐类、烷基萘磺酸盐类、烷基二苯基醚(二)磺酸盐类。
阳离子系表面活性剂并无特别限定,可使用以前公知的阳离子系表面活性剂。例如可列举烷基胺盐类、四级铵盐类、烷基咪唑鎓盐、聚氧亚乙基烷基胺盐类、聚乙烯多胺衍生物。
非离子系表面活性剂并无特别限定,可列举:聚乙二醇型的高级醇环氧乙烷加成物、烷基苯酚环氧乙烷加成物、烷基萘酚环氧乙烷加成物、苯酚环氧乙烷加成物、萘酚环氧乙烷加成物、脂肪酸环氧乙烷加成物、多元醇脂肪酸酯环氧乙烷加成物、高级烷基胺环氧乙烷加成物、脂肪酸酰胺环氧乙烷加成物、油脂的环氧乙烷加成物、聚丙二醇环氧乙烷加成物、二甲基硅氧烷-环氧乙烷嵌段共聚物、二甲基硅氧烷-(环氧丙烷-环氧乙烷)嵌段共聚物、多元醇型的甘油的脂肪酸酯、季戊四醇的脂肪酸酯、山梨醇及山梨醇酐的脂肪酸酯、蔗糖的脂肪酸酯、多元醇的烷基醚、烷醇胺类的脂肪酸酰胺等。其中,优选为具有芳香环及环氧乙烷链,更优选为经烷基取代或未经取代的苯酚环氧乙烷加成物或者经烷基取代或未经取代的萘酚环氧乙烷加成物。
两性离子系表面活性剂并无特别限定,可列举:烷基二甲基氧化胺等氧化胺系、烷基甜菜碱等甜菜碱系、烷基氨基脂肪酸钠等氨基酸系。尤其可优选地使用可具有取代基的烷基二甲基氧化胺、可具有取代基的烷基羧基甜菜碱、可具有取代基的烷基磺基甜菜碱。具体可使用:日本专利特开2008-203359号公报的段落编号[0256]的式(2)所表示的化合物,日本专利特开2008-276166号公报的段落编号[0028]的式(I)、式(II)、式(VI)所表示的化合物,日本专利特开2009-47927号公报的段落编号[0022]~段落编号[0029]所表示的化合物。
进而,视需要也可含有如消泡剂及硬水软化剂般的添加剂。
继而,如图1(E)所示,将片11自薄型元件晶片60a去除,由此可获得薄型元件晶片。
片11的去除方法例如可列举:将片11保持膜状而剥离去除(机械剥离)的方法;利用剥离液使片11膨润后剥离去除的方法;对片11喷射剥离液而破坏去除的方法;使片11溶解于剥离液中而溶解去除的方法;利用光化射线、放射线或热的照射使片11分解、气化而去除的方法等。可优选地使用将片11保持膜状而剥离去除的方法、使片11溶解于水溶液或有机溶剂中而溶解去除的方法。就减少溶剂的使用量的观点而言,优选为保持膜状而去除,为了保持膜状而去除,优选为元件晶片表面61a与片11的剥离强度B满足以下的式(2)。
B≤4N/cm…·式(2)
本发明中,将支撑基板12自薄型元件晶片60a剥离时,优选为不加任何处理而自薄型元件晶片60a的端部相对于元件晶片沿垂直方向上拉而剥离,将元件晶片表面61a上的片11去除的方法优选为保持膜状而去除。
若将支撑基板12与片11的界面的剥离强度设为A、元件晶片表面61a与片11的剥离强度设为B,则通过一并满足上文所述的式(1)及式(2),可将支撑基板12、片11以如上所述的形态自元件晶片去除。
再者,在自元件晶片剥离支撑基板时的在元件晶片与片11的界面上剥离的情形(即,在元件晶片侧不残留片11的情形)中,图1(E)的步骤也可省略。
使支撑基板12自薄型元件晶片60a脱离后,视需要对薄型元件晶片60a实施各种公知的处理,制造具有薄型元件晶片60a的半导体装置。
另外,在片11附着于支撑基板上的情形时,可通过将片11去除而再生支撑基板。关于将片11去除的方法,若保持膜状,则可列举:利用毛刷、超声波、冰粒子、气雾剂(aerosol)的喷附而物理去除的方法;溶解于水溶液或有机溶剂中而溶解去除的方法;利用光化射线、放射线、热的照射而使其分解、气化的方法等化学去除的方法,也可对应于支撑基板而利用以前已知的清洗方法。
例如在使用硅基板作为支撑基板的情形时,可使用以前已知的硅晶片的清洗方法,例如化学去除的情形时可使用的水溶液或有机溶剂可提高强酸、强碱、强氧化剂或这些物质的混合物,具体可列举:硫酸、盐酸、氢氟酸、硝酸、有机酸等酸类,四甲基铵、氨、有机碱等碱类,过氧化氢等氧化剂,或氨与过氧化氢的混合物、盐酸与过氧化氢水的混合物、硫酸与过氧化氢水的混合物、氢氟酸与过氧化氢水的混合物、氢氟酸与氟化铵的混合物等。
就使用再生的支撑基板的情形的接着性的观点而言,优选为使用清洗液。
清洗液优选为含有pKa小于0的酸(强酸)及过氧化氢。pKa小于0的酸是选自碘化氢、过氯酸、溴化氢、氯化氢、硝酸、硫酸等无机酸、或烷基磺酸、芳基磺酸等有机酸中。就清洗性的观点而言,优选为无机酸,最优选为硫酸。
过氧化氢可优选地使用30质量%过氧化氢水,所述强酸与30质量%过氧化氢水的混合比以质量比计而优选为0.1∶1~100∶1,更优选为1∶1~10∶1,最优选为3∶1~5∶1。
[实施例]
以下,利用实施例对本发明进行更具体说明,但本发明只要不超出其主旨,则不限定于以下的实施例。另外,只要无特别说明,则“份”、“%”为质量基准。
在将以下的原料混合而制成均匀的溶液后,使用具有5μm的细孔径的聚四氟乙烯制过滤器进行过滤来制备组合物。
<组合物的组成>
·表1记载的(A)聚合物:表1记载的质量份
·表1记载的(B)沸点为160℃以上的溶剂:表1记载的质量份
·表1记载的(C)沸点小于120℃的溶剂:表1记载的质量份
·(D)抗氧化剂(易加乐斯(Irganox)(注册商标)1010(巴斯夫(BASF)公司制造)与苏米莱泽(Sumilizer)(注册商标)TP-D(住友化学(股)制造)的1∶1混合物):表1中所示的质量份
·代付利(DAIFREE)FB-962(大金工业(股)制造):0.05质量份
·美佳法(Megafac)F-557(迪爱生(DIC)(股)制造):0.1质量份
[表1]
表中记载的化合物如以下所述。
<(A)聚合物>
(A-1)赛普顿(Septon)S2104(聚苯乙烯系弹性体,苯乙烯含量65%,氢化,5%热质量减少温度=400℃,可乐丽(Kuraray)(股)制造)
(A-2)塔釜泰克(Tuftec)P2000(聚苯乙烯系弹性体,苯乙烯含量67%,氢化,5%热质量减少温度=400℃,旭化成(股)制造)
(A-3)塔釜泰克(Tuftec)P5051(聚苯乙烯系弹性体,苯乙烯含量47%,氢化,5%热质量减少温度=396℃,旭化成(股)制造)
(A-4)赛普顿(Septon)S2006(聚苯乙烯系弹性体,苯乙烯含量35%,氢化,5%热质量减少温度=392℃,可乐丽(Kuraray)(股)制造)
(A-5)赛普顿(Septon)S2007(聚苯乙烯系弹性体,苯乙烯含量30%,氢化,5%热质量减少温度=390℃,可乐丽(Kuraray)(股)制造)
(A-6)赛普顿(Septon)S2005(聚苯乙烯系弹性体,苯乙烯含量20%,氢化,5%热质量减少温度=380℃,可乐丽(Kuraray)(股)制造)
(A-7)阿萨普兰(Asaprene)T-439(聚苯乙烯系弹性体,苯乙烯含量45%,非氢化,5%热质量减少温度=380℃,旭化成(股)制造)
(A-8)PSJ聚苯乙烯HF-77(聚苯乙烯,苯乙烯含量100%,非氢化,5%热质量减少温度=400℃,PS日本(股)制造)
(A-9)尼珀(Nipol)1043(丙烯腈丁二烯橡胶,苯乙烯含量0%,非氢化,5%热质量减少温度=370℃,日本瑞翁(Zeon)(股)公司制造)
<(B)沸点为160℃以上的溶剂>
(B-1)均三甲苯(沸点165℃,SP值18.0(MPa)1/2,东洋合成工业(股)制造)
(B-2)对二异丙基苯(沸点210℃,SP值17.6(MPa)1/2,东京化成工业(股)制造)
(B-3)对二乙基苯(沸点181℃,SP值18.0(MPa)1/2,东丽(股)制造)
(B-4)间二乙基苯(沸点182℃,SP值17.8(MPa)1/2,东丽(股)制造)
(B-5)1,3,5-三乙基苯(沸点218℃,SP值18.0(MPa)1/2,东京化成工业(股)制造)
(B-6)对二甲苯(沸点139℃,SP值17.9(MPa)1/2,三菱气体化学(股)制造)
(B-7)十氢萘(沸点186℃,SP值18.0(MPa)1/2,新日铁住金化学(股)制造)
(B-8)1,2,3,4-四氢萘(沸点207℃,SP值19.9(MPa)1/2,新日铁住金化学(股)制造)
<(C)沸点小于120℃的溶剂>
(C-1)环己烷(沸点81℃,SP值16.8(MPa)1/2,出光兴产(股)制造)
(C-2)甲苯(沸点111℃,SP值18.2(MPa)1/2,JX日矿日石能源(股)制造)
(C-3)四氢呋喃(沸点66℃,SP值19.5(MPa)1/2,岸田化学(Kishida Chemical)(股)制造)
(C-4)甲基环己烷(沸点101℃,SP值16.0(MPa)1/2,三协化学(股)制造)
(C-5)乙酸丁酯(沸点126℃,SP值17.4(MPa)1/2,岸田化学(Kishida Chemical)(股)制造)
再者,(A)聚合物的5%热质量减少温度通过以下方法而测定。
<5%热质量减少温度>
利用热重量分析装置Q500(TA公司制造),使2mg的试样在铝锅上在60mL/min的氮气流下、自初始温度25℃起在20℃/min的一定升温条件下升温,测定试样的质量减少5质量%时的温度。
<片的制造>
利用线棒将各组合物以速度1m/min的速度涂布于厚度75μm的聚对苯二甲酸乙二酯膜(脱模膜)上,在140℃下干燥10分钟,由此制作厚度100μm的片。使脱模膜残留而制成带有脱模膜的片。
关于表面粘性强的片,进而在片的经涂布的面上贴合厚度75μm的聚对苯二甲酸乙二酯膜(脱模膜)。
<接着性支撑基板的制造>
将利用所述方法获得的片(带有脱模膜的片)安置于真空层压机中,在两面具有聚对苯二甲酸乙二酯膜(脱模膜)的情形时将单侧的膜剥离后,使片位于100mm的硅(Si)晶片上,在真空下使片表面与Si晶片接触,利用辊将片与Si晶片固定,由此制作接着性支撑基板。此处,不将接着性支撑基板的最上部所残留的聚对苯二甲酸乙二酯膜(脱模膜)剥离而残留。
<试片的制作>
将接着性支撑基板的聚对苯二甲酸乙二酯膜(脱模膜)剥离后,对接着性支撑基板的片表面与元件晶片的元件面在真空下、110℃下以0.11 MPa的压力进行3分钟压接,制作试片。元件晶片是使用于100mm的Si晶片上以200μm的间距形成有直径80μm、高度40μm的包含铜的凸块者。
<评价>
<<溶解度的评价>>
以表1记载的比例将组合物混合。进而,在表1中添加(A)聚合物,制备固体成分浓度31质量%的试样。
再者,关于未溶解的试样,添加以下溶剂而使其完全溶解。
(追加添加的溶剂)
在添加有(B)溶剂与(C)溶剂的组合物中,添加以添加至各组合物的质量比例将(B)溶剂与(C)溶剂混合而得的混合溶剂。
在单独添加有(B)溶剂的组合物中追加(B)溶剂。
在单独添加有(C)溶剂的组合物中追加(C)溶剂。
(评价基准)
A:可制备固体成分浓度31质量%的试样。
B:可制备固体成分浓度30质量%以上且小于31质量%的试样。
C:可制备固体成分浓度29质量%以上且小于30质量%的试样。
D:可制备固体成分浓度小于29质量%的试样。
<<表面状态>>
以干燥后的膜厚成为100μm的方式将组合物涂布于聚对苯二甲酸乙二酯膜(脱模膜)上,目测观察在140℃下干燥10分钟后的表面状态,按照以下基准进行评价。
A:未观察到干燥不均或厚度不均。
B:在一部分观察到干燥不均或厚度不均。
C:在整个面观察到干燥不均或厚度不均。
<<干燥性>>
以干燥后的膜厚成为100μm的方式将组合物涂布于聚对苯二甲酸乙二酯膜(脱模膜)上,按照以下基准对在140℃下干燥10分钟后的干燥性进行评价。
A:完全干燥,表面无粘性。
B:在一部分溶剂未挥发,在所述部位确认到表面的粘性。
C:在整个面溶剂未挥发,确认到表面的粘性。
D:溶剂残存,表面仍为高粘度的液体。
<<耐热性>>
使用烘箱将试片在250℃下加热1小时。将加热后的试片与切割框架一起安置于切割胶带安装机(dicing tape mounter)的中央,使切割胶带位于上方。利用辊(及真空)将试片与切割胶带固定,在切割框架上将切割胶带切割,在切割胶带上安装试片。
将试片以500mm/min的条件朝片的垂直方向拉伸,确认剥离性,按照以下基准进行评价。再者,目测确认Si晶片有无破损。
A:能以小于10N的最大剥离力剥离。
B:能以10N以上且小于15N的最大剥离力剥离。
C:能以15N以上且小于20N的最大剥离力剥离。
D:能以20N以上的最大剥离力剥离,或Si晶片破损。
<<层压性>>
在接着性支撑基板的制造时,按照以下基准对将片层压于Si晶片上时的层压性进行评价。
A:片完全熔融,无孔隙地贴合于Si晶片上。
B:片的熔融不充分,在片的一部分确认到孔隙。
C:片的熔融不充分,在片的整个面确认到孔隙。
[表2]
溶解度 | 表面状态 | 干燥性 | 耐热性 | |
实施例1 | A | A | A | A |
实施例2 | A | A | A | A |
实施例3 | A | A | A | A |
实施例4 | A | A | B | A |
实施例5 | A | A | C | A |
实施例6 | A | A | A | A |
实施例7 | A | A | A | A |
实施例8 | A | A | A | A |
实施例9 | A | A | A | A |
实施例10 | A | A | A | B |
实施例11 | A | A | A | B |
实施例12 | A | A | A | B |
实施例13 | A | A | A | B |
实施例14 | A | A | A | A |
实施例15 | A | A | A | A |
实施例16 | B | B | A | A |
实施例17 | B | A | A | A |
实施例18 | A | A | A | A |
实施例19 | A | A | A | A |
实施例20 | A | A | A | B |
实施例21 | B | B | A | A |
实施例22 | A | A | A | C |
比较例1 | A | C | A | A |
比较例2 | A | C | D | A |
比较例3 | B | C | A | A |
比较例4 | B | C | C | A |
比较例5 | C | B | D | A |
比较例6 | A | A | A | D |
比较例7 | A | A | A | D |
比较例8 | C | A | C | A |
比较例9 | C | A | C | A |
[表3]
层压性 | |
实施例1 | A |
实施例19 | B |
实施例20 | B |
实施例21 | A |
实施例22 | C |
根据所述结果,实施例的组合物的溶解性良好,可形成干燥性、表面状态及耐热性优异的片。另外,通过含有抗氧化剂,也可提高层压性。
相对于此,比较例1~比较例9的溶解性、干燥性、表面状态、耐热性中的任一者差。
符号的说明
11:片
12:支撑基板
60:元件晶片
60a:薄型元件晶片
61:硅基板
61a:表面
61b:、61b1:背面
62:元件芯片
63:结构体
100:接着性支撑基板
Claims (19)
1.一种组合物,其含有:
自25℃起以20℃/min升温的5%热质量减少温度为375℃以上的弹性体;
下述通式(1)所表示的沸点为160℃以上的溶剂;及
沸点小于120℃的溶剂,
[化1]
通式(1)中,R1~R6分别独立地表示氢原子或脂肪族烃基。
2.根据权利要求1所述的组合物,其中所述弹性体是以25质量%以上的比例而含有于所述组合物中。
3.根据权利要求1或2所述的组合物,其中所述弹性体为含有来源于苯乙烯的重复单元的弹性体。
4.根据权利要求1至3中任一项所述的组合物,其中所述弹性体为氢化产物。
5.根据权利要求1至4中任一项所述的组合物,其中所述弹性体为单末端或两末端为苯乙烯嵌段的苯乙烯嵌段聚合物。
6.根据权利要求1至5中任所述的组合物,其中所述弹性体的苯乙烯含有率为40质量%以上。
7.根据权利要求1至6中任一项所述的组合物,其中所述沸点为160℃以上的溶剂的溶解度参数值为19(MPa)1/2以下。
8.根据权利要求1至7中任一项所述的组合物,其中所述沸点小于120℃的溶剂的溶解度参数值为19(MPa)1/2以下。
9.根据权利要求1至8中任一项所述的组合物,其中所述沸点小于120℃的溶剂为选自芳香族烃、脂环式烃及环状醚中的一种以上。
10.根据权利要求1至9中任一项所述的组合物,其中所述沸点小于120℃的溶剂是以10质量%~60质量%的比例而含有于所述组合物中。
11.根据权利要求1至10中任一项所述的组合物,其中所述沸点为160℃以上的溶剂与所述沸点小于120℃的溶剂的质量比为80:20~99:1。
12.根据权利要求1至11中任一项所述的组合物,其还含有抗氧化剂。
13.根据权利要求12所述的组合物,其中所述抗氧化剂是以1质量%~7质量%的比例而含有于所述组合物中。
14.根据权利要求1至13中任一项所述的组合物,其用于片形成用途。
15.根据权利要求1至14中任一项所述的组合物,其为暂时接着组合物。
16.一种片的制造方法,其将根据权利要求1至15中任一项所述的组合物施用于支撑体上,并使其干燥。
17.一种片,其是使根据权利要求1至15中任一项所述的组合物干燥而获得。
18.一种层叠体,其在使根据权利要求1至15中任一项所述的组合物干燥而获得的片的单面或两面上具有具备脱模性的支撑体。
19.一种带有元件晶片的层叠体,其在元件晶片与支撑基板之间具有使根据权利要求1至15中任一项所述的组合物干燥而获得的片,且所述片的一个表面与所述元件晶片的元件面接触,另一表面与所述支撑基板的表面接触。
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TW201613989A (en) | 2016-04-16 |
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US20170198176A1 (en) | 2017-07-13 |
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