CN117447937A - 半导体加工用压敏粘合片 - Google Patents
半导体加工用压敏粘合片 Download PDFInfo
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- CN117447937A CN117447937A CN202310921086.0A CN202310921086A CN117447937A CN 117447937 A CN117447937 A CN 117447937A CN 202310921086 A CN202310921086 A CN 202310921086A CN 117447937 A CN117447937 A CN 117447937A
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- Prior art keywords
- sensitive adhesive
- pressure
- semiconductor processing
- adhesive sheet
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- 239000004820 Pressure-sensitive adhesive Substances 0.000 title claims abstract description 336
- 239000004065 semiconductor Substances 0.000 title claims abstract description 105
- 238000012545 processing Methods 0.000 title claims abstract description 95
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- 239000004094 surface-active agent Substances 0.000 claims abstract description 42
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 38
- 239000000758 substrate Substances 0.000 claims abstract description 37
- 229920005601 base polymer Polymers 0.000 claims abstract description 36
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- 238000005406 washing Methods 0.000 claims description 9
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
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- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
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- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 description 2
- LRRQSCPPOIUNGX-UHFFFAOYSA-N 2-hydroxy-1,2-bis(4-methoxyphenyl)ethanone Chemical compound C1=CC(OC)=CC=C1C(O)C(=O)C1=CC=C(OC)C=C1 LRRQSCPPOIUNGX-UHFFFAOYSA-N 0.000 description 2
- HFCUBKYHMMPGBY-UHFFFAOYSA-N 2-methoxyethyl prop-2-enoate Chemical compound COCCOC(=O)C=C HFCUBKYHMMPGBY-UHFFFAOYSA-N 0.000 description 2
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- 239000004971 Cross linker Substances 0.000 description 2
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- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
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- LZHUBCULTHIFNO-UHFFFAOYSA-N 2,4-dihydroxy-1,5-bis[4-(2-hydroxyethoxy)phenyl]-2,4-dimethylpentan-3-one Chemical compound C=1C=C(OCCO)C=CC=1CC(C)(O)C(=O)C(O)(C)CC1=CC=C(OCCO)C=C1 LZHUBCULTHIFNO-UHFFFAOYSA-N 0.000 description 1
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- XIWVNXGNLGFNSO-UHFFFAOYSA-N 2-(2-dodecoxyethoxy)ethyl dihydrogen phosphate Chemical compound CCCCCCCCCCCCOCCOCCOP(O)(O)=O XIWVNXGNLGFNSO-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- 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
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
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- C09J133/062—Copolymers with monomers not covered by C09J133/06
- C09J133/066—Copolymers with monomers not covered by C09J133/06 containing -OH groups
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- 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
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
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- 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
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
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- 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
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
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- 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
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
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- 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
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Abstract
本发明涉及半导体加工用压敏粘合片。提供一种对具有凹凸的被粘物的凹凸具有优异的追随性且锚固性优异的半导体加工用压敏粘合片。所述半导体加工用压敏粘合片包括由UV固化型压敏粘合剂形成的压敏粘合剂层,和基材。所述UV固化型压敏粘合剂包含基础聚合物、光聚合引发剂和磷酸酯系表面活性剂。
Description
技术领域
本发明涉及一种半导体加工用压敏粘合片。
背景技术
半导体晶片用于各种用途,例如个人计算机、智能手机和汽车。在半导体晶片的加工工序中,在加工时使用压敏粘合带来保护其表面。近年来,大规模集成电路(LSI)的微型化和高功能化一直在进行,并且晶片的表面结构变得复杂。其具体实例是通过焊料凸块(solder bump)、或电极等获得的晶片表面的复杂三维结构。因此,需要在半导体加工工序中使用的压敏粘合带具有对晶片表面的凹凸的追随性。具有柔软性的压敏粘合剂用于具有对凹凸的追随性的压敏粘合片的压敏粘合剂层。这种压敏粘合片具有优异的对凹凸的跟随性,但是在与基材的锚固力方面存在问题。
近年来,随着产品的小型化和薄型化,已经推进了半导体晶片的薄型化。在加工成薄形状的晶片中,当压敏粘合带的压敏粘合强度过高时,晶片可能在剥离压敏粘合带时断裂。因此,为了防止被粘物上的残胶和在剥离带时晶片的断裂,已经提出了使用UV固化型压敏粘合剂的压敏粘合带(例如,日本专利申请特开No.2020-017758和日本专利申请特开No.2013-213075)。当基材和压敏粘合剂层之间的锚固力不充分时,存在的问题在于:当对压敏粘合带进行UV固化以将其剥离时,发生锚固不良,导致被粘物上的残胶。为了解决这些问题,已经提出在基材上形成底涂(undercoating)层以改善压敏粘合剂层对基材的锚固力。然而,压敏粘合片的制造步骤的数量增加,因此产率可能降低。另外,半导体晶片的加工工序可以包括使用溶剂的洗涤步骤。当包括这样的步骤时,底涂层可能溶解在溶剂中,因此可能无法充分获得对压敏粘合剂层的锚固力改善效果(anchoring force-improvingeffect)。
发明内容
本发明旨在解决现有技术中的上述问题,并且本发明的目的是提供一种具有优异的对凹凸的追随性和优异的锚固性的半导体加工用压敏粘合片。
1.根据本发明的至少一个实施方案,提供一种半导体加工用压敏粘合片,其包括:由UV固化型压敏粘合剂形成的压敏粘合剂层;和基材。所述UV固化型压敏粘合剂包含基础聚合物、光聚合引发剂和磷酸酯系表面活性剂。
2.在根据上述第1项的半导体加工用压敏粘合片中,相对于100重量份的所述基础聚合物,所述磷酸酯系表面活性剂的含量可以为0.03重量份以上。
3.在根据上述第1项或第2项的半导体加工用压敏粘合片中,所述压敏粘合剂层在UV固化后的锚固力可以为1N/20mm以上。
4.在根据上述第1项至第3项中任一项的半导体加工用压敏粘合片中,所述UV固化型压敏粘合剂可以进一步包含交联剂,并且相对于100重量份的所述基础聚合物,所述交联剂的含量可以为1重量份以下。
5.在根据上述第4项的半导体加工用压敏粘合片中,所述交联剂可以是异氰酸酯系交联剂。
6.在根据上述第1项至第5项中任一项的半导体加工用压敏粘合片中,所述基础聚合物可以是具有碳-碳双键的聚合物。
7.在根据上述第1项至第6项中任一项的半导体加工用压敏粘合片中,所述基材可以包含聚烯烃系树脂。
8.根据上述第1项至第7项中任一项的半导体加工用压敏粘合片可用于包括溶剂洗涤步骤的半导体加工工序中。
附图说明
图1是根据本发明的至少一个实施方案的半导体加工用压敏粘合片的示意性截面图。
具体实施方式
A.半导体加工用压敏粘合片的整体构成
图1是根据本发明的至少一个实施方案的半导体加工用压敏粘合片的示意性截面图。在所示的实例中,半导体加工用压敏粘合片100包括基材10和配置在基材的一个表面上的压敏粘合剂层20。半导体加工用压敏粘合片可以包括任何合适的其他层(未示出)。例如,任何合适的层(例如,中间层)可以形成在基材和压敏粘合剂层之间。在所示的实例中,基材10是单层,但可以是两层以上的层叠体。在半导体加工用压敏粘合片中,为了保护压敏粘合剂层直到该片受到使用,剥离衬垫可以设置在压敏粘合剂层的外侧。
根据本发明的至少一个实施方案的半导体加工用压敏粘合片的厚度可以设定为任何合适的厚度。半导体加工用压敏粘合片的厚度例如优选为10μm至1,000μm,更优选为50μm至300μm,还更优选为100μm至300μm。
B.基材
基材可以由任何合适的树脂形成。用于形成基材的树脂的具体实例包括聚酯系树脂,例如聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚对苯二甲酸丁二醇酯(PBT)和聚萘二甲酸丁二醇酯(PBN)、乙烯-乙酸乙烯酯共聚物、乙烯-甲基丙烯酸甲酯共聚物,聚烯烃系树脂,例如聚乙烯、聚丙烯和乙烯-丙烯共聚物,聚乙烯醇,聚偏二氯乙烯,聚氯乙烯,氯乙烯-乙酸乙烯酯共聚物,聚乙酸乙烯酯,聚酰胺,聚酰亚胺,纤维素,氟系树脂,聚醚,聚苯乙烯系树脂如聚苯乙烯,聚碳酸酯和聚醚砜。其中,优选使用聚酯系树脂,例如聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚对苯二甲酸丁二醇酯(PBT)和聚萘二甲酸丁二醇酯(PBN),以及聚烯烃系树脂,例如聚乙烯、聚丙烯和乙烯-丙烯共聚物,并且更优选使用聚烯烃系树脂。当使用这些树脂时,改善了对凹凸的追随性,因此可以改善对其表面上具有凹凸的被粘物的密合性(adhesiveness)。基材可以是单层,或者可以是两层以上的层叠体。当基材是两层以上的层叠体时,优选的是,优选的树脂是用于形成作为层叠体的基材的与压敏粘合剂层接触的至少一层的树脂。
基材可以在不抑制本发明的效果的范围内进一步包括其他组分。其他组分的实例包括抗氧化剂、紫外线吸收剂、光稳定剂和热稳定剂。关于其他组分的种类和使用量,其他组分可以根据目的以任何合适的量使用。
基材的厚度优选为10μm至200μm,更优选为20μm至150μm。
C.压敏粘合剂层
压敏粘合剂层由UV固化型压敏粘合剂形成。UV固化型压敏粘合剂通常包含基础聚合物和光聚合引发剂。由UV固化型压敏粘合剂形成的压敏粘合剂层可以提供在UV固化之前对被粘物具有优异的压敏粘合强度并且在UV固化之后具有优异的剥离性的压敏粘合片。在根据本发明的至少一个实施方案的半导体加工用压敏粘合片中,用于形成压敏粘合剂层的UV固化型压敏粘合剂包含磷酸酯系表面活性剂。使用这种压敏粘合剂形成的压敏粘合剂层即使在采用软的(例如,低交联度)压敏粘合剂以改善凹凸追随性时也具有优异的对基材的锚固性。因此,抑制了在UV固化后剥离压敏粘合片时在基材和压敏粘合剂层之间的界面处的锚固不良(anchoring failure),因此可以抑制被粘物上的残胶。另外,即使当使用半导体加工用压敏粘合片的半导体加工工序包括溶剂洗涤步骤时,也抑制压敏粘合剂层溶解在溶剂中。因此,压敏粘合片也可以适当地用于包括溶剂洗涤步骤的半导体加工工序中。
压敏粘合剂层的UV固化前的弹性模量优选为0.05MPa至1.20MPa,更优选为0.10MPa至1.00MPa,还更优选为0.17MPa至0.95MPa。当压敏粘合剂层的UV固化前的弹性模量落在这样的范围内时,压敏粘合剂层可以追随被粘物的凹凸,因此可以提供具有优异的凹凸嵌入性(unevenness-embedding property)的半导体加工用压敏粘合片。压敏粘合剂层的弹性模量可以用例如纳米压痕仪测量。
压敏粘合剂层的UV固化后的锚固力优选为1N/20mm以上,更优选为1.5N/20mm至10N/20mm,还更优选为2N/20mm至8N/20mm。当UV固化后的锚固力落在这样的范围内时,可以抑制在基材和压敏粘合剂层之间的界面处的锚固不良。本文的锚固力是指通过以下方法测量的剥离力。(i)将半导体加工用压敏粘合片切割成20mm宽×150mm长的尺寸,并且经由预定的双面胶带将SUS板贴合到压敏粘合片的与其压敏粘合剂层相反的整个表面(例如,在具有“基材/压敏粘合剂层”构成的压敏粘合片的情况下,其上没有形成压敏粘合剂层的基材的表面(外表面))上。(ii)将尺寸为20mm宽×150mm长并且含有聚酯系树脂的压敏粘合性评价用片(相对于聚对苯二甲酸乙二醇酯具有10N/20mm至20N/20mm的剥离压敏粘合强度的片,例如日东电工株式会社在商品名“No.315Tape”下获得的产品)的压敏粘合剂表面贴合到已经被切割的压敏粘合剂层的外表面(不与基材接触的表面)上,以提供评价样品的压敏粘合片。(iii)通过拉伸试验测量评价样品的基材和压敏粘合剂层之间的剥离力。上述步骤(i)至(iii)各自在23℃的环境温度下进行。对于剥离力的测量,在剥离速度为50mm/min和剥离角度为180°的条件下进行拉伸试验。
C-1.UV固化型压敏粘合剂
任何合适的压敏粘合剂都可以用作UV固化型压敏粘合剂。例如,可以采用通过向任何合适的压敏粘合剂如丙烯酸系压敏粘合剂、橡胶系压敏粘合剂、有机硅系压敏粘合剂或聚乙烯醚系压敏粘合剂中添加UV固化性单体和/或低聚物而获得的压敏粘合剂,或者可以采用使用具有碳-碳双键的聚合物作为基础聚合物的压敏粘合剂。其中,优选使用包含具有碳-碳双键的聚合物作为基础聚合物的压敏粘合剂。
C-1-1.基础聚合物
具有碳-碳双键的基础聚合物可以在其主链中具有碳-碳双键,可以在其侧链中具有碳-碳双键,或者可以在其末端具有碳-碳双键。当使用具有碳-碳双键的基础聚合物时,使用具有聚合性碳-碳双键并且具有压敏粘合性的聚合物作为基础聚合物。这种聚合物的实例包括各自通过将碳-碳双键引入树脂例如(甲基)丙烯酸系树脂、乙烯基烷基醚系树脂、有机硅系树脂、聚酯系树脂、聚酰胺系树脂、聚氨酯系树脂或苯乙烯-二烯嵌段共聚物而获得的聚合物。其中,优选使用通过将碳-碳双键引入(甲基)丙烯酸系树脂而获得的(甲基)丙烯酸系聚合物。当使用(甲基)丙烯酸系聚合物时,可以获得其中压敏粘合剂层的储能弹性模量和拉伸弹性模量容易调节并且压敏粘合强度和剥离性之间的平衡优异的压敏粘合片。此外,可以减少源自压敏粘合剂的组分对被粘物的污染。“(甲基)丙烯酸”是指丙烯酸和/或甲基丙烯酸。
任何合适的(甲基)丙烯酸系树脂都可以用作(甲基)丙烯酸系树脂。(甲基)丙烯酸系树脂的一个实例是通过聚合含有一种或两种以上的各自具有直链或支链烷基的丙烯酸或甲基丙烯酸的酯的单体组合物而获得的聚合物。
直链或支链烷基优选碳原子数为30以下的烷基,更优选碳原子数为1至20的烷基,还更优选碳原子数为4至18的烷基。烷基的具体实例包括甲基、乙基、丙基、异丙基、正丁基、叔丁基、异丁基、戊基、异戊基、己基、庚基、环己基、2-乙基己基、辛基、异辛基、壬基、异壬基、癸基、异癸基、十一烷基、月桂基、十三烷基、十四烷基、硬脂基、十八烷基和十二烷基。
具有直链或支链烷基的丙烯酸或甲基丙烯酸的酯的具体实例包括(甲基)丙烯酸丙酯、(甲基)丙烯酸异丙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸仲丁酯、(甲基)丙烯酸戊酯、(甲基)丙烯酸异戊酯、(甲基)丙烯酸己酯、(甲基)丙烯酸庚酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸辛酯、(甲基)丙烯酸异辛酯、(甲基)丙烯酸壬酯、(甲基)丙烯酸异壬酯、(甲基)丙烯酸癸酯、(甲基)丙烯酸异癸酯,(甲基)丙烯酸十一烷基酯、(甲基)丙烯酸十二烷基酯、(甲基)丙烯酸十三烷基酯、(甲基)丙烯酸十四烷基酯、(甲基)丙烯酸十五烷基酯、(甲基)丙烯酸十六烷基酯、(甲基)丙烯酸十七烷基酯、(甲基)丙烯酸十八烷基酯、(甲基)丙烯酸十九烷基酯和(甲基)丙烯酸二十烷基酯。
为了改变例如内聚强度、耐热性或交联性,单体组合物可以根据需要包含可与(甲基)丙烯酸烷基酯共聚的其他单体。这种单体的实例包括:含羧基的单体,如丙烯酸和甲基丙烯酸;酸酐单体,如马来酸酐和衣康酸酐;含羟基的单体,如(甲基)丙烯酸羟乙酯和(甲基)丙烯酸羟丙酯;含磺酸基团的单体,如苯乙烯磺酸和烯丙基磺酸;含氮单体,如(甲基)丙烯酰胺、N,N-二甲基(甲基)丙烯酰胺和丙烯酰吗啉;(甲基)丙烯酸氨基烷基酯系单体,如(甲基)丙烯酸氨基乙酯;(甲基)丙烯酸烷氧基烷基酯系单体,如(甲基)丙烯酸甲氧基乙酯;马来酰亚胺系单体,如N-环己基马来酰亚胺和N-异丙基马来酰亚胺;衣康酰亚胺系单体,如N-甲基衣康酰亚胺和N-乙基衣康酰亚胺;琥珀酰亚胺系单体;乙烯基系单体,例如乙酸乙烯酯、丙酸乙烯酯、N-乙烯基吡咯烷酮和甲基乙烯基吡咯烷酮;氰基丙烯酸酯单体,如丙烯腈和甲基丙烯腈;含环氧基团的丙烯酸系单体如(甲基)丙烯酸缩水甘油酯;二醇系丙烯酸酯单体,如聚乙二醇(甲基)丙烯酸酯和聚丙二醇(甲基)丙烯酸酯;各自具有杂环、卤素原子、或硅原子等的丙烯酸酯系单体,如(甲基)丙烯酸四氢糠酯、氟代(甲基)丙烯酸酯和有机硅(甲基)丙烯酸酯;烯烃系单体,如异戊二烯、丁二烯和异丁烯;和乙烯基醚系单体如乙烯基醚。这些单体组分可以单独使用或组合使用。相对于100重量份的单体组合物的所有单体,单体的含量优选为1重量份至30重量份,更优选为3重量份至25重量份。
(甲基)丙烯酸系树脂的重均分子量优选为300,000以上,更优选为500,000以上,还更优选为600,000至2,000,000。当重均分子量落在这样的范围内时,可以防止低分子量组分的渗出(bleeding),因此可以获得具有低污染性的压敏粘合片。(甲基)丙烯酸系树脂的分子量分布(重均分子量/数均分子量)优选为1至20,更优选为3至10。当使用具有窄分子量分布的聚合物时,可以防止低分子量组分的渗出,因此可以获得具有低污染性的压敏粘合片。重均分子量和数均分子量可以通过凝胶渗透色谱法测量(溶剂:四氢呋喃,聚苯乙烯换算)来确定。
具有碳-碳双键的聚合物可以通过任何合适的方法获得。聚合物可以通过例如使通过任何合适的聚合方法获得的树脂和具有聚合性碳-碳双键的化合物进行反应(例如缩合反应或加成反应)来获得。具体地,当使用(甲基)丙烯酸系树脂时,可以通过使具有衍生自具有任何合适的官能团的单体的结构单元的(甲基)丙烯酸系树脂(共聚物)在任何合适的溶剂中进行聚合,然后使所得丙烯酸系树脂的官能团和具有可与该官能团反应的聚合性碳-碳双键的化合物进行反应来获得树脂。相对于100重量份的上述树脂,进行反应的具有聚合性碳-碳双键的化合物的量优选为4重量份至30重量份,更优选为4重量份至20重量份。任何合适的溶剂都可以用作溶剂。其实例包括各种有机溶剂,例如乙酸乙酯、甲基乙基酮和甲苯。
如上所述,当树脂和具有聚合性碳-碳双键的化合物进行反应时,树脂和具有聚合性碳-碳双键的化合物优选具有可以彼此反应的官能团。官能团的组合例如是羧基/环氧基团、羧基/氮丙啶基、或羟基/异氰酸酯基团。在这些官能团的组合中,从易于反应跟踪的角度来看,羟基和异氰酸酯基团的组合是优选的。
具有碳-碳双键的化合物的实例包括甲基丙烯酸2-异氰酸基乙酯、甲基丙烯酰异氰酸酯、2-甲基丙烯酰氧基乙基异氰酸酯(甲基丙烯酸2-异氰酸基乙酯)和间异丙烯基-α,α-二甲基苄基异氰酸酯。
当使用通过添加UV固化性单体和/或低聚物获得的压敏粘合剂时,任何合适的单体或低聚物都可以用作UV固化性单体和低聚物中的每一种。UV固化性单体的实例包括氨基甲酸酯(甲基)丙烯酸酯、三羟甲基丙烷三(甲基)丙烯酸酯、四羟甲基甲烷四(甲基)丙烯酸酯、季戊四醇三(甲基)丙烯酸酯、季戊四醇四(甲基)丙烯酸酯、二季戊四醇单羟基五(甲基)丙烯酸酯、二季戊四醇六(甲基)丙烯酸酯和1,4-丁二醇二(甲基)丙烯酸酯。UV固化性低聚物的实例包括氨基甲酸酯系低聚物、聚醚系低聚物、聚酯系低聚物、聚碳酸酯系低聚物和聚丁二烯系低聚物。优选使用分子量为约100至约30,000的低聚物作为低聚物。单体和低聚物可以单独使用或组合使用。
单体和/或低聚物可以根据要使用的压敏粘合剂的种类以任何合适的量使用。相对于100重量份的用于形成压敏粘合剂的基础聚合物,单体和/或低聚物的用量例如优选为5重量份至500重量份,更优选为40重量份至150重量份。
C-2.光聚合引发剂
任何合适的引发剂都可以用作光聚合引发剂。光聚合引发剂的实例包括:酰基氧化膦系光聚合引发剂,如2,4,6-三甲基苄基苯基次膦酸乙酯和(2,4,6-三甲基苯甲酰基)-苯基氧化膦;α-酮醇系化合物,如4-(2-羟基乙氧基)苯基(2-羟基-2-丙基)酮、α-羟基-α,α′-二甲基苯乙酮、2-甲基-2-羟基苯丙酮和1-羟基环己基苯基酮;苯乙酮系化合物,如甲氧基苯乙酮、2,2-二甲氧基-2-苯基苯乙酮、2,2-二乙氧基苯乙酮和2-甲基-1-[4-(甲硫基)-苯基]-2-吗啉代丙烷-1;苯偶姻醚系化合物,如苯偶姻乙醚、苯偶姻异丙醚和茴香偶姻甲醚(anisoin methyl ether);缩酮系化合物,如苄基二甲基缩酮;芳香族磺酰氯系化合物,如2-萘磺酰氯;光活性肟系化合物,如1-酰苯-1,1-丙二酮-2-(o-乙氧羰基)肟;二苯甲酮系化合物,如二苯甲酮、苯甲酰苯甲酸和3,3′-二甲基-4-甲氧基二苯甲酮;噻吨酮系化合物,例如噻吨酮、2-氯噻吨酮、2-甲基噻吨酮、2,4-二甲基噻吨酮、异丙基噻吨酮、2,4-二氯噻吨酮、2,4-二乙基噻吨酮和2,4-二异丙基噻吨酮;樟脑醌;卤代酮;和酰基膦酸酯,以及α-羟基苯乙酮类,如2-羟基-1-(4-(4-(2-羟基-2-甲基丙酰基)苄基)苯基-2-甲基丙烷-1。其中,可以优选使用苯乙酮系化合物。光聚合引发剂可以单独使用或组合使用。
市售品可以用作光聚合引发剂。其实例包括可从IGM Resins B.V.在商品名Omnirad 127D、Omnirad 379EG和Omnirad 651下可得的产品。
光聚合引发剂可以以任何合适的量使用。相对于100重量份的上述UV固化型压敏粘合剂,光聚合引发剂的含量优选为0.5重量份至20重量份,更优选为0.5重量份至10重量份。当光聚合引发剂的含量小于0.5重量份时,UV固化型压敏粘合剂在UV照射时可能不能充分固化。当光聚合引发剂的含量大于10重量份时,压敏粘合剂的储存稳定性会降低。
C-3.磷酸酯系表面活性剂
磷酸酯系表面活性剂的实例包括聚氧乙烯烷基醚或聚氧乙烯烷基芳基醚的磷酸单酯、聚氧乙烯烷基醚或聚氧乙烯烷基芳基醚的磷酸二酯、聚氧乙烯烷基醚或聚氧乙烯烷基芳基醚的磷酸三酯、烷基磷酸酯、烷基醚磷酸酯及其盐。盐的实例包括钠盐和钾盐。其中,可以优选使用聚氧乙烯烷基醚磷酸酯及其盐、单酯、二酯或其混合物。这些磷酸酯系表面活性剂可以单独使用或组合使用。
聚氧乙烯烷基醚磷酸酯是通过环氧乙烷与高级醇的加成聚合获得的产物的磷酸酯。高级醇的碳原子数优选为8至22,更优选为10至20,还更优选为12至18。环氧乙烷的加成摩尔数优选为1至15,更优选为2至12,还更优选为2至10。使用这种聚氧乙烯烷基醚磷酸酯,即使在采用具有优异的凹凸追随性的软的压敏粘合剂时,也获得可以形成与基材的锚固力优异的压敏粘合剂层的压敏粘合剂组合物。结果,即使在对压敏粘合剂层进行UV固化之后,也可以抑制被粘物上的残胶。
相对于100重量份的基础聚合物,磷酸酯系表面活性剂的含量优选为0.03重量份以上,更优选为0.1重量份至1重量份,还更优选为0.3重量份至0.5重量份。当磷酸酯系表面活性剂的含量落在这样的范围内时,即使在采用具有优异的凹凸追随性的软的压敏粘合剂时,也获得可以形成与基材的锚固力优异的压敏粘合剂层的压敏粘合剂组合物。结果,即使在对压敏粘合剂层进行UV固化之后,也可以抑制被粘物上的残胶。
C-4.添加剂
压敏粘合剂层形成组合物可以根据需要包含任何合适的添加剂。添加剂的实例包括交联剂、催化剂(例如铂催化剂)、增粘剂、增塑剂、颜料、染料、填料、防老剂、导电材料、紫外线吸收剂、光稳定剂、剥离改性剂、软化剂、磷酸酯系表面活性剂以外的表面活性剂、阻燃剂、溶剂和低聚物。
在本发明的至少一个实施方案中,UV固化型压敏粘合剂还含有交联剂。交联剂的实例包括异氰酸酯系交联剂、环氧系交联剂、氮丙啶系交联剂和螯合物系交联剂。相对于100重量份的UV固化型压敏粘合剂中的基础聚合物,交联剂的含量比例优选为1重量份以下,更优选为0.01重量份至1重量份,还更优选为0.02重量份至0.6重量份,特别优选为0.03重量份至0.5重量份。压敏粘合剂层的柔软性可以通过交联剂的含量比例来控制。当交联剂的含量小于0.01重量份时,压敏粘合剂变成溶胶状,因此不能形成压敏粘合剂层。当交联剂的含量大于1重量份时,可能无法充分地获得对被粘物表面的凹凸的追随性。
在本发明的至少一个实施方案中,优选使用异氰酸酯系交联剂。异氰酸酯系交联剂是优选的,因为该交联剂可以与各种官能团反应。特别优选使用具有3个以上的异氰酸酯基团的交联剂。当使用异氰酸酯系交联剂作为交联剂并且交联剂的含量比例落在上述范围内时,可以提供对被粘物表面的凹凸具有优异的追随性并且与基材具有优异的锚固性的UV固化型压敏粘合剂。
压敏粘合剂层的厚度可以设定为任何合适的值。压敏粘合剂层的厚度优选为10μm至500μm,更优选为15μm至300μm,还更优选为20μm至250μm。当压敏粘合剂层的厚度落在上述范围内时,可以表现出对被粘物的充分的压敏粘合强度。
UV固化型压敏粘合剂的凝胶分数优选为20%至99%,更优选为50%至97%,还更优选为70%至95%。凝胶分数可以作为相对于溶剂如乙酸乙酯的不溶性成分来确定。具体地,凝胶分数确定为在将UV固化型压敏粘合剂在23℃下在乙酸乙酯中浸渍7天后不溶性组分相对于浸渍前的样品的重量分数(单位:重量%)。通常,聚合物的凝胶分数等于其交联度,聚合物中交联部分的数量越多意味着凝胶分数越大。凝胶分数(交联结构的引入量)可以通过引入交联结构的方法、或交联剂的种类和量等调节到期望的范围。
D.半导体加工用压敏粘合片的制造方法
半导体加工用压敏粘合片可以通过任何合适的方法制造。半导体加工用压敏粘合片可以通过例如涉及将压敏粘合剂溶液(UV固化型压敏粘合剂)涂布到剥离衬垫上,干燥以在剥离衬垫上形成压敏粘合剂层,并且将所得物粘合到基材的方法来获得。另外,半导体加工用压敏粘合片可以通过将UV固化型压敏粘合剂涂布到基材上,然后干燥来获得。各种方法,例如棒涂、气刀涂布、凹版涂布、凹版反转涂布、逆转辊涂布、唇涂、模涂、浸涂、胶印、柔性版印刷和丝网印刷,都可以被采用作为压敏粘合剂层形成组合物的涂布方法。可以采用任何合适的方法作为干燥方法。
E.半导体加工用压敏粘合片的用途
半导体加工用压敏粘合片可以适当地用于半导体制造工序中。如上所述,即使当根据本发明的至少一个实施方案的半导体加工用压敏粘合片与溶剂接触时,也可以抑制该片的基材和压敏粘合剂层之间的锚固力的减小。因此,半导体加工用压敏粘合片也可以适当地用于包括溶剂洗涤步骤的半导体制造工序中。溶剂洗涤步骤中使用的溶剂的实例包括半导体制造方法中通常使用的各溶剂,例如2,2-双(羟甲基)丙酸(DBPA)、丙二醇单甲醚(PGME)、丙二醇单甲醚乙酸酯(PGMEA)、异丙醇(IPA)、N,N-二甲基丙酰胺、N-甲基-2-吡咯烷酮(NMP)和乙酸丁酯。
如上所述,根据本发明的至少一个实施方案的半导体加工用压敏粘合片具有优异的对凹凸的追随性。因此,可以在制造工序中适当地保存其表面上具有凹凸的半导体晶片。例如,该片还可以适当地用于制造例如通过层叠贯通硅通孔(TSV)芯片获得的动态随机存取存储器(DRAM)等具有更复杂结构的半导体的工序。根据本发明的至少一个实施方案的半导体加工用压敏粘合片可以适当地用作其表面上具有凹凸结构的半导体晶片的切割带。
实施例
下面通过实施例具体描述本发明,但是本发明不限于这些实施例。此外,除非另有说明,实施例中的“份”和“%”是按重量计的。
[制造例1]基础聚合物1的制备
将100重量份的甲基丙烯酸十二烷基酯(LMA)、22重量份的甲基丙烯酸己酯(HMA)、0.2重量份的聚合引发剂(偶氮二异丁腈(AIBN))和500重量份的乙酸乙酯混合以制备组合物。将所得组合物装入聚合用实验装置中,该聚合用实验装置包括1升圆底可分离烧瓶,该烧瓶设置有可分离盖、分液漏斗、温度计、氮气引入管、李比希冷凝器、真空密封、搅拌棒和搅拌叶片。在搅拌组合物的同时,用氮气在常温下吹扫装置6小时。之后,当组合物在氮气流中搅拌时,将组合物在65℃下保持4小时,然后在75℃下保持2小时以用于聚合。由此,得到基础聚合物1的树脂溶液(固含量:20%)。
[制造例2]基础聚合物2的制备
将75重量份的丙烯酸2-乙基己酯(2EHA)、25重量份的丙烯酰吗啉(ACMO)、22重量份的丙烯酸2-羟乙酯(HEA)、0.2重量份的聚合引发剂(偶氮二异丁腈(AIBN))和500重量份的乙酸乙酯混合以制备组合物。将所得组合物装入聚合用实验装置中,该聚合用实验装置包括1升圆底可分离烧瓶,该烧瓶设置有可分离盖、分液漏斗、温度计、氮气引入管、李比希冷凝器、真空密封、搅拌棒和搅拌叶片。在搅拌组合物的同时,用氮气在常温下吹扫装置6小时。之后,当组合物在氮气流中搅拌时,将组合物在65℃下保持4小时,然后在75℃下保持2小时以用于聚合。由此,得到基础聚合物2的树脂溶液(固含量:20%)。
[制造例3]基础聚合物3的制备
将75重量份的丙烯酸2-甲氧基乙酯(MEA)、20重量份的ACMO、20重量份的HEA、0.2重量份的聚合引发剂(偶氮二异丁腈(AIBN))和500重量份的乙酸乙酯混合以制备组合物。将所得组合物装入聚合用实验装置中,该聚合用实验装置包括1升圆底可分离烧瓶,该烧瓶设置有可分离盖、分液漏斗、温度计、氮气引入管、李比希冷凝器、真空密封、搅拌棒和搅拌叶片。在搅拌组合物的同时,用氮气在常温下吹扫装置6小时。之后,当组合物在氮气流中搅拌时,将组合物在65℃下保持4小时,然后在75℃下保持2小时以用于聚合。由此,得到基础聚合物3的树脂溶液(固含量:19%)。
[制造例4]基础聚合物4的制备
将50重量份的丙烯酸乙酯(EA)、50重量份的丙烯酸丁酯(BA)、20重量份的HEA、0.2重量份的聚合引发剂(偶氮二异丁腈(AIBN))和500重量份的乙酸乙酯混合以制备组合物。将所得组合物装入聚合用实验装置中,该聚合用实验装置包括1升圆底可分离烧瓶,该烧瓶设置有可分离盖、分液漏斗、温度计、氮气引入管、李比希冷凝器、真空密封、搅拌棒和搅拌叶片。在搅拌组合物的同时,用氮气在常温下吹扫装置6小时。之后,当组合物在氮气流中搅拌时,将组合物在65℃下保持4小时,然后在75℃下保持2小时以用于聚合。由此,得到基础聚合物4的树脂溶液(固含量:20%)。
[实施例1]
1.UV固化型压敏粘合剂组合物的制备
相对于制造例1中得到的基础聚合物1的树脂溶液的固成分100重量份,加入0.5重量份的多异氰酸酯交联剂1(Nippon Polyurethane Industry Co.,Ltd.制造,商品名:“CORONATE L”)、0.3重量份的磷酸酯系表面活性剂1(Toho Chemical Industry Co.,Ltd.制造,商品名:“PHOSPHANOL RL-210”)、和3重量份的光聚合引发剂(IGM Resins B.V.制造,商品名:“Omnirad 127D”),然后混合。接下来,使用乙酸乙酯作为稀释溶剂来调节混合物的粘度。由此,得到UV固化型压敏粘合剂1。
2.半导体加工用压敏粘合片的制造
使用具有聚丙烯(PP)/乙烯乙酸乙烯酯(EVA)/聚丙烯(PP)三层结构的膜(KuraboIndustries Ltd.制造,厚度:80μm)作为基材。将上述获得的UV固化型压敏粘合剂组合物1涂布到基材的一个表面上,随后干燥以形成厚度为20μm的压敏粘合剂层。因此,制造了半导体加工用压敏粘合片。
[实施例2]
除了使用磷酸酯系表面活性剂2(Toho Chemical Industry Co.,Ltd.制造,商品名:“PHOSPHANOL ML-220”)代替磷酸酯系表面活性剂1之外,以与实施例1相同的方式制备UV固化型压敏粘合剂组合物2。除了使用UV固化型压敏粘合剂组合物2形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
[实施例3]
除了使用磷酸酯系表面活性剂3(Toho Chemical Industry Co.,Ltd.,制造,商品名:“PHOSPHANOL RL-310”)代替磷酸酯系表面活性剂1之外,以与实施例1相同的方式制备UV固化型压敏粘合剂组合物3。除了使用UV固化型压敏粘合剂组合物3形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
[实施例4]
除了使用磷酸酯系表面活性剂4(Toho Chemical Industry Co.,Ltd.制造,商品名:“PHOSPHANOL RS-410”)代替磷酸酯系表面活性剂1之外,以与实施例1相同的方式制备UV固化型压敏粘合剂组合物4。除了使用UV固化型压敏粘合剂组合物4形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
[实施例5]
除了使用磷酸酯系表面活性剂5(Toho Chemical Industry Co.,Ltd.制造,商品名:“PHOSPHANOL RS-710”)代替磷酸酯系表面活性剂1之外,以与实施例1相同的方式制备UV固化型压敏粘合剂组合物5。除了使用UV固化型压敏粘合剂组合物5形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
[实施例6]
除了将磷酸酯系表面活性剂1的添加量改变为0.03重量份之外,以与实施例1相同的方式制备UV固化型压敏粘合剂组合物6。除了使用UV固化型压敏粘合剂组合物6形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
[实施例7]
除了将磷酸酯系表面活性剂1的添加量改变为0.1重量份之外,以与实施例1相同的方式制备UV固化型压敏粘合剂组合物7。除了使用UV固化型压敏粘合剂组合物7形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
[实施例8]
除了将磷酸酯系表面活性剂1的添加量改变为0.6重量份之外,以与实施例1相同的方式制备UV固化型压敏粘合剂组合物8。除了使用UV固化型压敏粘合剂组合物8形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
[实施例9]
除了将磷酸酯系表面活性剂1的添加量改变为1重量份之外,以与实施例1相同的方式制备UV固化型压敏粘合剂组合物9。除了使用UV固化型压敏粘合剂组合物9形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
[实施例10]
除了以下之外:使用基础聚合物2代替基础聚合物1;使用0.1重量份的交联剂2(Mitsui Chemicals Inc.制造,商品名:“TAKENATE D-101A”)代替交联剂1;并且将磷酸酯系表面活性剂1的添加量改变为0.5重量份,以与实施例1相同的方式制备UV固化型压敏粘合剂组合物10。除了使用UV固化型压敏粘合剂组合物10形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
[实施例11]
除了将交联剂2的添加量改变为0.3重量份之外,以与实施例10相同的方式制备UV固化型压敏粘合剂组合物11。除了使用UV固化型压敏粘合剂组合物11形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
[实施例12]
除了将交联剂2的添加量改变为0.5重量份之外,以与实施例10相同的方式制备UV固化型压敏粘合剂组合物12。除了使用UV固化型压敏粘合剂组合物12形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
[实施例13]
除了将交联剂2的添加量改变为1重量份之外,以与实施例10相同的方式制备UV固化型压敏粘合剂组合物13。除了使用UV固化型压敏粘合剂组合物13形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
[实施例14]
除了使用基础聚合物3代替基础聚合物2之外,以与实施例12相同的方式制备UV固化型压敏粘合剂组合物14。除了使用UV固化型压敏粘合剂组合物14形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
[实施例15]
除了使用基础聚合物4代替基础聚合物2之外,以与实施例12相同的方式制备UV固化型压敏粘合剂组合物15。除了使用UV固化型压敏粘合剂组合物15形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
[实施例16]
除了使用聚乙烯(PE)的单层膜(Okura Industrial Co.,Ltd.制造,商品名:“NSOFILM”)作为基材之外,以与实施例12相同的方式制造半导体加工用压敏粘合片。
[实施例17]
除了使用聚对苯二甲酸乙二醇酯(PET)的单层膜(Toray Industries,Inc.制造,商品名:“Lumirror#50S105”)作为基材之外,以与实施例12相同的方式制造半导体加工用压敏粘合片。
[实施例18]
除了以下之外:使用基础聚合物1代替基础聚合物2;并且进一步加入3重量份的轻剥离剂(聚丙二醇)和5重量份的多官能低聚物(氨基甲酸酯丙烯酸酯,The NipponSynthetic Chemical Industry Co.,Ltd.制造,商品名:“UV-3000TL”),以与实施例12相同的方式制备UV固化型压敏粘合剂组合物18。除了使用UV固化型压敏粘合剂组合物18形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
(比较例1)
除了不添加磷酸酯系表面活性剂1之外,以与实施例1相同的方式制备UV固化型压敏粘合剂组合物C1。除了使用UV固化型压敏粘合剂组合物C1形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
(比较例2)
除了加入0.3重量份的烷基硫酸盐型表面活性剂1(Toho Chemical IndustryCo.,Ltd.制造,商品名:“ALSCOAP NS-230”)代替磷酸酯系表面活性剂1之外,与实施例1相同的方式制备UV固化型压敏粘合剂组合物C2。除了使用UV固化型压敏粘合剂组合物C2形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
(比较例3)
除了加入0.3重量份的烷基硫酸盐型表面活性剂2(Toho Chemical IndustryCo.,Ltd.制造,商品名:“ALSCOAP TH-330K”)代替磷酸酯系表面活性剂1之外,与实施例1相同的方式制备UV固化型压敏粘合剂组合物C3。除了使用UV固化型压敏粘合剂组合物C3形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
(比较例4)
除了加入0.3重量份的磺酸型表面活性剂(Toho Chemical Industry Co.,Ltd.制造,商品名:“LUNOX S-40TD”)代替磷酸酯系表面活性剂1之外,以与实施例1相同的方式制备UV固化型压敏粘合剂组合物C4。除了使用UV固化型压敏粘合剂组合物C4形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
(比较例5)
除了加入0.3重量份的聚氧乙烯烷基醚型表面活性剂(Toho Chemical IndustryCo.,Ltd.制造,商品名:“PEGNOL S-4DV”)代替磷酸酯系表面活性剂1之外,以与实施例1相同的方式制备UV固化型压敏粘合剂组合物C5。除了使用UV固化型压敏粘合剂组合物C5形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
(比较例6)
除了将交联剂2的添加量改变为0.01重量份之外,以与实施例10相同的方式制备UV固化型压敏粘合剂组合物C6。除了使用UV固化型压敏粘合剂组合物C6形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
(比较例7)
除了不添加磷酸酯系表面活性剂之外,以与实施例12相同的方式制备UV固化型压敏粘合剂组合物C7。除了使用UV固化型压敏粘合剂组合物C7形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
(比较例8)
除了以下之外:不添加磷酸酯系表面活性剂;并且将交联剂2的添加量改变为3重量份,以与实施例12相同的方式制备UV固化型压敏粘合剂组合物C8。除了使用UV固化型压敏粘合剂组合物C8形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
(比较例9)
除了以下之外:不添加磷酸酯系表面活性剂;并且将交联剂2的添加量改变为5重量份,以与实施例12相同的方式制备UV固化型压敏粘合剂组合物C9。除了使用UV固化型压敏粘合剂组合物C9形成压敏粘合剂层之外,以与实施例1相同的方式制造半导体加工用压敏粘合片。
(比较例10)
除了不添加磷酸酯系表面活性剂之外,以与实施例16相同的方式制备UV固化型压敏粘合剂组合物C10。除了使用UV固化型压敏粘合剂组合物C10形成压敏粘合剂层之外,以与实施例17相同的方式制造半导体加工用压敏粘合片。
(比较例11)
除了不添加磷酸酯系表面活性剂之外,以与实施例17相同的方式制备UV固化型压敏粘合剂组合物C11。除了使用UV固化型压敏粘合剂组合物C11形成压敏粘合剂层之外,以与实施例18相同的方式制造半导体加工用压敏粘合片。
(比较例12)
除了不添加磷酸酯系表面活性剂之外,以与实施例18相同的方式制备UV固化型压敏粘合剂组合物C12。除了使用UV固化型压敏粘合剂组合物C12形成压敏粘合剂层之外,以与实施例18相同的方式制造半导体加工用压敏粘合片。
<评价>
使用在实施例和比较例中获得的压敏粘合片进行以下评价。结果如表1所示。
1.压敏粘合剂层的弹性模量
使用纳米压痕仪(Hysitron,Inc.制造,商品名:“TriboIndenter”)测量在每个实施例或比较例中获得的压敏粘合片的压敏粘合剂层的弹性模量。使用圆锥形(球形;半径:10μm)压头,并且进行单次压痕测量。通过将测量温度设置为25℃,压痕深度设置为2,000nm,压痕速度和拉伸速度设置为1000nm/s,在遮光(light-shielding)环境下进行测量。通过JKR法分析所得的载荷(μN)和位移(nm),并且通过下式计算弹性模量。
Er:弹性模量
R:压头半径
h:位移
P:载荷
2.剥离强度
(1)UV照射前的压敏粘合强度(UV之前)
将每个实施例或比较例中获得的压敏粘合片切割成测量为150mm长×20mm宽的条状。在23℃下,使2千克的辊往复运动一次,以将压敏粘合片的压敏粘合剂层贴合到镜面精加工(mirror-finished)的硅晶片(Shin-Etsu Handotai Co.,Ltd.制造,商品名:“CZN<100>2.5-3.5”,直径:4英寸)上。该片和晶片之间的贴合部形成测量为80mm长×20mm宽。然后,将贴合的产物在23℃的气氛下无载荷静置30分钟。接下来,在以下条件下,通过按照JISZ0237进行90°剥离试验来测量压敏粘合片的压敏粘合强度。
<90°剥离试验>
试验重复次数:3次
温度:23℃
剥离角度:90°
拉伸速度:300mm/min
初始长度(卡盘间距):150mm
(2)UV照射后的压敏粘合强度(UV之后)
将每个实施例或比较例中获得的压敏粘合片切割成测量为150mm长×20mm宽的条状。在23℃下,使2千克的辊往复运动一次,以将剥离了其隔膜(separator)的压敏粘合片贴合到镜面精加工的硅晶片(Shin-Etsu Handotai Co.,Ltd.制造,商品名:“CZN<100>2.5-3.5”,直径:4英寸)上。该片和晶片之间的贴合部形成测量为80mm长×20mm宽。然后,将贴合的产物在23℃的气氛下无载荷静置30分钟。在静置30分钟后,在以下UV照射条件下,从压敏粘合片的基材的背面侧用UV光照射贴合的产物。之后,将贴合的产物静置30分钟,并且按照JIS Z 0237以与上述部分(1)的评价中相同的方式进行90°剥离试验。
<UV照射条件>
UV照射装置:Nitto Seiki Co.,Ltd.制造,商品名:UM810
光源:高压汞灯
照射强度:46mW/cm2(测量装置:Ushio Inc.制造的“UV强度计UT-101”)
照射时间:10秒
累积光量:460mJ
3.锚固力
(1)UV照射前的锚固力(UV之前)
将每个实施例或比较例中获得的半导体加工用压敏粘合片切割成20mm宽×150mm长的尺寸。将SUS板经由双面胶带(日东电工株式会社制造,商品名:“No.5000NS”)贴合到切下的压敏粘合片的基材的整个背面(其上未形成压敏粘合剂层的表面)上。接下来,将尺寸为20mm宽×150mm长的压敏粘合带(日东电工株式会社制造,商品名:“No.315Tape”(BT-315))的压敏粘合剂表面贴合到压敏粘合片的压敏粘合剂层(不与基材接触的表面)上,以提供评价样品。接下来,通过拉伸试验测量评价样品的基材和压敏粘合剂层之间的剥离力。评价样品的制备和拉伸试验均在23℃的环境温度下进行。对于剥离力的测量,在拉伸速度为300mm/min和剥离角度为180°的条件下进行拉伸试验。
(2)UV照射后的锚固力(UV之后)
将每个实施例或比较例中获得的半导体加工用压敏粘合片切割成20mm宽×150mm长的尺寸。将SUS板经由双面胶带(日东电工株式会社制造,商品名:“No.5000NS”)贴合到切下的压敏粘合片的基材的整个背面(其上未形成压敏粘合剂层的表面)上。接下来,将尺寸为20mm宽×150mm长的压敏粘合带(日东电工株式会社制造,商品名:“No.315Tape”(BT-315))的压敏粘合剂表面贴合到压敏粘合片的压敏粘合剂层(不与基材接触的表面)上,以提供评价样品。接下来,在以下UV照射条件下,从压敏粘合带侧用UV光照射贴合的产物。然后,将产物静置30分钟,并且通过拉伸试验测量评价样品的基材和压敏粘合剂层之间的剥离力。评价样品的制备和拉伸试验均在23℃的环境温度下进行。对于剥离力的测量,在拉伸速度为300mm/min和剥离角度为180°的条件下进行拉伸试验。另外,目视观察剥离后的压敏粘合片的断裂模式,并且如下评价:其中在每个实施例或比较例中获得的半导体加工用压敏粘合片和贴合到压敏粘合剂层的压敏粘合带之间的界面处发生剥离的情况(其中发生界面不良的情况)由“界面”表示,并且其中在每个实施例或比较例中获得的半导体加工用压敏粘合片和压敏粘合剂层附着到压敏粘合带(贴合到压敏粘合剂层)的压敏粘合剂层侧的情况(其中发生锚固不良的情况)由“锚固”表示。
<UV照射条件>
UV照射装置:Nitto Seiki Co.,Ltd.制造,商品名:UM810
光源:高压汞灯
照射强度:46mW/cm2(测量装置:Ushio Inc.制造,商品名:“UV强度计UT-101”)
照射时间:10秒
累积光量:460mJ
4.基材包埋
使用显微镜(Keyence Corporation制造,商品名:VK-X200,10×物镜)从每个实施例或比较例中获得的半导体加工用压敏粘合片的基材侧观察基材和压敏粘合剂层之间的层间区域中空气间隙的存在与否。
5.被粘物包埋
用真空贴片机(vacuum mounter)(Nitto Seiki Co.,Ltd.制造,商品名:“MSA-840V3”)将每个实施例或比较例中获得的压敏粘合片贴在TSV晶片(柱:5μmt,)上。接下来,用显微镜(Keyence Corporation制造,商品名:“VK-X200”,10×物镜)从压敏粘合片的基材的背面观察压敏粘合剂层和柱之间的空气间隙的存在与否。
6.拾取(粘合剂残留物)
用真空贴片机(Nitto Seiki Co.,Ltd.制造,商品名:“MSA-840V3”)将压敏粘合带贴在TSV晶片(柱:5μmt,)上。接下来,用切割机(DISCO Corporation制造,商品名:“DFD6450”)进行TSV晶片的切割,从而将晶片切割成10mm×10mm的小块。接下来,用芯片分选机(Canon Machinery Inc.制造,商品名:“BESTEM-S500”)进行已经切割成小块的晶片的拾取。用显微镜(Keyence Corporation制造,商品名:“VK-X200”,10×物镜)观察已经进行了拾取的芯片的背面(与压敏粘合带的压敏粘合剂层接触的表面),观察芯片上残胶的存在与否。
表1
*PP/EVA/PP的三层结构
表2
*PP/EVA/PP的三层结构
本发明的半导体加工用压敏粘合片具有优异的对凹凸的追随性和优异的锚固性。因此,压敏粘合片可以适当地用于其表面上具有凹凸的半导体的加工工序中。此外,抑制了溶剂中的锚固力的减小,因此,压敏粘合片可以适当地用于包括溶剂洗涤步骤的半导体制造工序中。
根据本发明的至少一个实施方案,可以提供具有优异的对凹凸的追随性和优异的锚固性的半导体加工用压敏粘合片。在根据本发明的至少一个实施方案的半导体加工用压敏粘合片中,即使在通过UV照射固化压敏粘合剂层之后,也可以保持基材和压敏粘合剂层之间的锚固性。因此,当剥离UV照射后的半导体加工用压敏粘合片时,可以防止被粘物(例如半导体晶片)上的残胶。此外,即使在包括溶剂洗涤步骤的半导体加工工序中使用压敏粘合片时,也可以抑制压敏粘合剂层对基材的锚固力的减小。
Claims (8)
1.一种半导体加工用压敏粘合片,其包括:
由UV固化型压敏粘合剂形成的压敏粘合剂层;和
基材,
其中所述UV固化型压敏粘合剂包含基础聚合物、光聚合引发剂和磷酸酯系表面活性剂。
2.根据权利要求1所述的半导体加工用压敏粘合片,其中相对于100重量份的所述基础聚合物,所述磷酸酯系表面活性剂的含量为0.03重量份以上。
3.根据权利要求1所述的半导体加工用压敏粘合片,其中所述压敏粘合剂层在UV固化后的锚固力为1N/20mm以上。
4.根据权利要求1所述的半导体加工用压敏粘合片,
其中所述UV固化型压敏粘合剂还包含交联剂,并且
其中相对于100重量份的所述基础聚合物,所述交联剂的含量为1重量份以下。
5.根据权利要求4所述的半导体加工用压敏粘合片,其中所述交联剂是异氰酸酯系交联剂。
6.根据权利要求1所述的半导体加工用压敏粘合片,其中所述基础聚合物是具有碳-碳双键的聚合物。
7.根据权利要求1所述的半导体加工用压敏粘合片,其中所述基材包含聚烯烃系树脂。
8.根据权利要求1至7中任一项所述的半导体加工用压敏粘合片,其中所述半导体加工用压敏粘合片用于包括溶剂洗涤步骤的半导体加工工序中。
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