CN107207928B - 粘合性树脂层以及粘合性树脂膜 - Google Patents

粘合性树脂层以及粘合性树脂膜 Download PDF

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Publication number
CN107207928B
CN107207928B CN201680009304.1A CN201680009304A CN107207928B CN 107207928 B CN107207928 B CN 107207928B CN 201680009304 A CN201680009304 A CN 201680009304A CN 107207928 B CN107207928 B CN 107207928B
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adhesive resin
resin layer
acrylic
substrate
adhesive
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CN107207928A (zh
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藤田志朗
铃木淳史
新见洋人
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Fujimori Kogyo Co Ltd
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Fujimori Kogyo Co Ltd
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract

本发明提供一种粘合性树脂层及粘合性树脂膜，其中该粘合性树脂层即便与基材贴合后加热变形，也能够防止气泡的产生，对依次层叠基材、粘合性树脂层、及基材而成的层叠体的、基材的变形的追随性良好。更具体而言，本发明提供的粘合性树脂层为含有丙烯酸类粘合性树脂组合物的单层的粘合性树脂层(11)，其中，该粘合性树脂组合物至少含有(A)丙烯酸类聚合物、(B)丙烯酸类单体或丙烯酸类寡聚物、及(C)热聚合引发剂，粘合性树脂层(11)在常温下在两面(11a)、(11b)具有粘着性，在升温速度为10℃/分钟的差示扫描热量测定(DSC)中，在80℃以上开始确认发热，在120℃～210℃之间确认至少1个波峰。

Description

粘合性树脂层以及粘合性树脂膜
技术领域
本发明涉及一种即便贴合在基材后加热变形，也能够防止气泡产生的粘合性树脂层及粘合性树脂膜。
本申请主张以2015年7月17日申请的日本特愿2015-142880号为基础的优先权，并将其内容引用在此。
背景技术
作为使用后能够容易地将粘着剂剥离的粘着剂，使用有含有丙烯酸类粘着剂、氨酯丙烯酸酯等的光固化型丙烯酸酯化合物、异氰酸酯类固化剂(交联剂)、及光聚合引发剂的粘着剂(例如，参照专利文献1～3)。这种粘着剂由于在常温下具有粘着性，并且通过光照射使粘着性降低从而能够再剥离，所以被广泛地使用于半导体加工用或搬运用胶粘带。
另一方面，丙烯酸类粘着剂，还广泛地使用于层叠粘合触控面板、移动电话、显示器、贴合玻璃等的具有透明性或透光性的基材。但是，在基材与粘着剂之间产生空隙且残留气泡时，有减低基材之间的粘合强度的可能性。此外，在需要透明性的用途的情况下，有因气泡而致使通过基材后的光学特性降低的可能性。
现有技术文献
专利文献
专利文献1：日本特许第3764133号公报
专利文献2：日本特许第3803200号公报
专利文献3：日本特开2012-193321号公报
发明内容
本发明要解决的技术问题
本发明鉴于上述情形而成，其技术问题为提供一种粘合性树脂层及粘合性树脂膜，其中该粘合性树脂层即便与基材贴合后加热变形，也能够防止气泡的产生，且对依次层叠基材、粘合性树脂层、及基材而成的层叠体的、基材的变形的追随性良好。
解决技术问题的技术手段
为了解决上述技术问题，本发明提供一种粘合性树脂层，其为含有丙烯酸类粘合性树脂组合物的单层的粘合性树脂层，其特征在于：所述粘合性树脂组合物至少含有(A)丙烯酸类聚合物、(B)丙烯酸类单体或丙烯酸类寡聚物、及(C)热聚合引发剂，所述粘合性树脂层在常温下在两面具有粘着性，在升温速度为10℃/分钟的差示扫描热量测定(DSC)中，在80℃以上开始确认发热，在120℃～210℃之间确认至少1个波峰。
所述(C)热聚合引发剂优选为过氧化物。
所述粘合性树脂组合物，相对于所述(A)丙烯酸类聚合物100重量份，优选含有5～50重量份的所述(B)丙烯酸类单体或丙烯酸类寡聚物。
所述粘合性树脂组合物，优选含有含羟基的丙烯酸类单体作为所述(B)丙烯酸类单体或丙烯酸类寡聚物中的至少一部分。
所述粘合性树脂组合物，优选含有固化性氨酯丙烯酸酯作为所述(B)丙烯酸类单体或丙烯酸类寡聚物中的至少一部分。
此外，本发明提供一种粘合性树脂膜，其特征在于：通过在2片隔离膜之间层叠所述粘合性树脂层而成。
此外，本发明提供一种用于形成层叠体的粘合性树脂层，其中，所述层叠体通过经由所述粘合性树脂层层叠2片基材而成。
此外，本发明提供一种粘合性树脂层，其特征在于：在将经由所述粘合性树脂层层叠2片基材而得到的层叠体，夹持于2个模具之间的状态下，使所述层叠体加热变形，所述粘合性树脂层即使在加热固化后，粘着力也为10N/25mm以上。
此外，本发明提一种层叠体，其特征在于：通过经由所述粘合性树脂层层叠2片基材而成。
此外，本发明提供一种层叠体的制造方法，其特征在于：在将经由所述粘合性树脂层层叠2片基材而得到的层叠体，夹持于2个模具之间的状态下，将所述粘合性树脂层加热固化。
在将所述粘合性树脂层的原材料组合物中所含的溶剂的沸点设为温度A，将所述热聚合引发剂具有1分钟的半衰期的温度设为温度B，将在所述粘合性树脂层的制造工序中用于将所述溶剂去除的加热时的温度设为温度C，将使所述粘合性树脂层加热固化的工序中的模具的加压温度设为温度D时，优选各温度为下述式(1)的顺序。
式(1)温度A<温度C<温度B<温度D
所述加热固化时的模具的温度优选为150～300℃的温度。
本发明的特征在于：粘合性树脂组合物含有丙烯酸类聚合物、丙烯酸类单体或丙烯酸类寡聚物、及热聚合引发剂，通过所述成分能够制造转移胶带(transfer tape)状的粘合性树脂层。粘合性树脂层通过丙烯酸类单体或丙烯酸类寡聚物而具有对基材的基材追随性。能够提供一种粘合性树脂层以及其制造方法，该粘合性树脂层中，通过热等的反应开始条件，丙烯酸类单体或丙烯酸类寡聚物进行固化，即便贴合在基材后加热变形，气泡也不会进入。特别是通过丙烯酸类单体或丙烯酸类寡聚物的添加量的手段，能够保持对基材的追随性、及转移胶带状的粘合性树脂层自身的强度。通过本发明，通过强迫地、特别是通过热压，能够使粘合性树脂层半强迫地追随基材。从气泡产生的抑制、对基材的变形的追随性的角度出发，在制造层叠体时，优选不经由空气而将热及压力这两者施加于层叠体的热压，而并非由经由空气的电子射线照射或能量线照射引起的固化。
发明效果
通过本发明，能够提供一种粘合性树脂层及粘合性树脂膜，所述粘合性树脂层即便与基材贴合后加热变形，也能够防止气泡的产生。
附图说明
图1为表示本发明的粘合性树脂膜的一个例子的剖面图。
图2为表示在2片基材之间层叠有粘合性树脂层的层叠体的一个例子的剖面图。
图3为表示粘合性树脂层被加热固化后的层叠体的一个例子的剖面图。
图4为表示粘合性树脂层被加热固化后的曲面状的层叠体的一个例子的剖面图。
具体实施方式
以下，基于优选的实施方式，参照附图对本发明进行说明。
在图1中，表示粘合性树脂膜10的一个例子的剖面图。粘合性树脂膜10具有：2片隔离膜12、13；及被层叠在它们之间的粘合性树脂层11。构成粘合性树脂层11的粘合性树脂组合物，含有(A)丙烯酸类聚合物、(B)丙烯酸类单体或丙烯酸类寡聚物、及(C)热聚合引发剂。粘合性树脂层11的两面11a、11b在常温下具有粘着性(成为粘着面)。
此外，在本说明书中，“常温”是指约3℃～约40℃，优选为约10℃～约30℃，更优选为约15℃～约25℃，最优选为约23℃。
粘合性树脂层11在遍及厚度方向的整体含有粘合性树脂组合物。只要含有满足必要条件的粘合性树脂组合物，粘合性树脂层11也可由含有同种或异种粘合性树脂组合物的2层以上而构成。粘合性树脂层11由单层的粘合性树脂层所构成时，由于能够使层构成单纯化而降低成本，因而优选。粘合性树脂组合物含有丙烯酸类粘合性树脂(聚合物)。粘合性树脂组合物的光学特性不被限定，可具有透明性，也可为半透明或不透明。
隔离膜12、13，在与粘合性树脂层11接触侧的表面12a、13a上，具有剥离性(成为剥离面)。作为隔离膜12、13的构成，可举出在树脂膜的一面或两面设置有剥离剂层的构成、及在树脂膜的树脂内含有剥离剂的构成。也能够使用纸、合成纸、金属箔、各种片材等代替树脂膜。隔离膜12、13具有透明性时，由于能够在隔离膜12、13未被剥离的粘合性树脂膜10的状态下，直接进行粘合性树脂层11的光学检查，因此优选。
图1中所示的粘合性树脂膜10，可以通过将隔离膜12、13从粘合性树脂层11上剥离而露出的粘着面11a、11b，贴合2片基材。图2表示经由粘合性树脂层11层叠2片基材21、22而成的层叠体20的一个例子。2片基材21、22在单面21a、22a与粘合性树脂层11接触，其相反侧的面21b、22b以能够利用模具进行热压的方式，不与粘合性树脂层11接触而空开。
基材21、22为通过粘合性树脂层11而被贴合的被粘物。各基材21、22可以是刚性板，也可以像膜一样具有可挠性。例如可以是玻璃、聚碳酸酯、丙烯酸树脂、各种树脂、陶瓷、金属等的单板，也可以是液晶面板、触控面板、玻璃盖片、线路基板等的由多种材料所构成的复合体。基材21、22的材质、厚度、形状等，可各自相同，也可不同。基材21、22的内表面21a、22a及外表面21b、22b，可各自平坦，也可以任一面或两面具有段差或凹凸。
将粘合性树脂层11贴合在基材21、22后，使基材21、22热变形时，作为基材21、22的材质，优选聚烯烃、聚酯、聚碳酸酯、聚酰胺、丙烯酸树脂、聚氯乙烯、纤维素酯等的热塑性树脂。使用于热变形的基材，不限定于热塑性树脂的基材(膜等)单体，也可在该基材的面上或内部，含有异种材料(金属、无机物、有机物等)的薄膜、图案、粒子、细线、微细结构物等。
形成如图2的层叠体20时，将隔离膜12、13剥离的顺序没有特别限定。可以在将一个隔离膜剥离而露出的一个粘着面上，贴合一个基材之后，再将另一个隔离膜剥离而露出的另一个粘着面上，贴合另一个基材。也可将两个隔离膜剥离而露出两个粘着面后，分别贴合基材。
由于粘合性树脂层11含有具有流动性的(B)丙烯酸类单体或丙烯酸类寡聚物，所以柔软性较高，能够利用粘合性树脂组合物湿润基材21、22的接触面21a、22a整体。因此，即便贴合在基材21、22后，使层叠体20加热变形，也能够抑制气泡。由于粘合性树脂层11含有(C)热聚合引发剂，所以可通过贴合后使其热固化，使接合更牢固。相较于照射紫外光，热固化的设备具有较简便、即便基材21、22包含透光性较低的部分时或粘合性树脂层11因着色等而不容易透射紫外光时也能够可靠地固化的优点。
通过在将经由粘合性树脂层11层叠2片基材21、22而得到的层叠体20，夹持在2个模具之间的状态下，进行加热，能够使粘合性树脂层11固化。由此，(A)丙烯酸类聚合物及(B)丙烯酸类单体或丙烯酸类寡聚物进行反应(聚合、交联等)，使得基材21、22之间的粘合力上升。此外，通过加热的同时进行加压，即便在基材21、22与粘合性树脂层11之间残留有气泡，也能填埋空隙而将气泡去除。进行加热固化时，2个模具中的至少一者被加热。
将层叠体20热压时，2个模具与层叠体(详言地，基材21、22的外表面21b、22b)之间，也可使介入垫层(cushion)(缓冲片)、剥离片、保护片等(介入物)。在2个模具在对层叠体的按压面具有凹凸时，由于模具的凸部直接接触层叠体时，压力容易集中在凸部，所以优选设置上述的介入物。
2个模具可覆盖层叠体20的侧面，也可不覆盖。例如，也可以将一个模具设作凸型，将另一个模具设作凹型，将层叠体20收纳在凹型的凹部后，使凸型的凸部朝向凹型的凹部接近。
图3中表示通过加热固化而得到的层叠体30的一个例子。在该层叠体30中，作为粘合性树脂层11热固化后的结果，在2片基材21、22之间，层叠有含有热固化后的粘合性树脂的粘合层23。由于热固化后的粘合层23的硬度增大，所以即便加热前的粘合性树脂层11柔软，也不容易再剥离。由此，作为粘合性树脂层11，能够使用即便粘合力较低、但是对基材的变形的追随性优异的树脂。粘合性树脂层11在加热固化后，粘合层23的粘着力(粘合力)优选为10N/25mm以上。
在制造层叠体30时，将2种基材21、22区分开时，可以考虑几种制造方法。层叠体30的制造中，可以采用任一种方法。
作为第一层叠方法，可举出：在第一基材21上层叠粘合性树脂层11，随后，实施热压处理，在粘合性树脂层11上层叠第二基材22，从而层叠成层叠体20之后；或是一边层叠第二基材22一边使用2个模具，使粘合性树脂层11加热固化的方法。
作为第二层叠方法，可举出：在第二基材22上层叠粘合性树脂层11，随后，实施热压处理，在粘合性树脂层11上层叠第一基材21之后；或是一边层叠第一基材21一边使用2个模具，使粘合性树脂层11加热固化的方法。
作为第三层叠方法，可举出：同时层叠第一基材21、粘合性树脂层11、及第二基材22之后；或是在进行层叠的同时，使用2个模具使粘合性树脂层11加热固化的方法。
第一或第二层叠方法，通过将基材21、22的一者与粘合性树脂层11先贴合而进行热压处理，从而粘合性树脂层容易追随于基材21、22中的一者。在一个基材表面存在段差或凹部等，而与粘合性树脂层之间容易产生空隙的情况下，由于能够通过热压处理将该空隙填埋，所以是即便热压加工的条件偏差较大，也能够形成较少气泡的方法。此外，考虑能够缩短制程这一点，第三层叠方法在成本方面是最具有优点的方法。
在基材21、22间层叠粘合性树脂层11并进行热压时，也能够使基材21、22中的一者或两者变形，而使层叠体产生凹凸。例如在2个模具的按压面上设置凹凸时，能够使树脂膜等具有可挠性的基材21、22变形为凹凸状。由于最初的粘合性树脂层11具有流动性，能够追随于基材21、22的凹凸。此外，通过在热压时进行热聚合，粘合性树脂层11固化，能够抑制产生空隙及气泡。而且，通过使基材21、22与粘合层23接合，如图4所示，能够将基材21、22的变形固定，从而实现凹凸、曲面、挠曲、弯曲等的成型。在基材的内表面形成有凸部时，也可在背侧的外表面形成凹部。在图4中，虽举出波板状的成型体作为一个例子，但并不特别地限定于此，能够成型为任意形状。
粘合性树脂层11优选在升温速度10℃/分钟的差示扫描热量测定(DSC)中，在80℃以上开始确认发热，在120℃～210℃之间确认至少1个波峰。在小于80℃下确认发热时，例如即便在常温下也有进行热固化反应的可能性，保存性下降。通过在120℃～210℃之间确认波峰，能够在与其相同程度的温度下使其进行热固化。而且，基材21、22也通过加热软化而容易变形。
为了提高粘合性树脂层11的操作性，粘合性树脂层11优选通过100～250℃的温度及30秒～10分钟的时间的加热来进行热固化。优选在这些的温度及时间范围中的至少一部分的条件下进行热固化，更优选能在全部范围下进行热固化。实际使用时的热固化条件，也可以是上述范围外。但是，从保存性的角度出发，优选在常温下实质上不进行热固化，例如优选在100℃以下的温度下，具有加热10分钟以内不会热固化的性质。
在粘合性树脂层11未固化的状态(加热前)下，在温度23℃下的储能模量优选为1×104～1×106Pa。此外，粘合性树脂层11通过加热而热固化之后，在温度23℃下的储能模量优选为1×104～1×109Pa。优选相较于加热前的在温度23℃下的储能模量，通过加热而热固化之后的在温度23℃下的储能模量变得更高。这些储能模量，分别在温度为23℃下能够对未固化的状态(加热前)的粘合性树脂层、及通过加热而热固化之后的粘合性树脂层(热固化后的粘合层)进行测定。测定储能模量时的振动频率，例如为1Hz。测定热固化后的粘合层的储能模量时，不将粘合性树脂层贴合在基材上，而通过使粘合性树脂层在隔离膜之间加热固化之后，将隔离膜剥离，由此能够得到热固化后的粘合层的单体。
接着，更详细地说明也为转移胶带的粘合性树脂层。
制造本发明的粘合性树脂层时所使用的粘合剂原材料组合物，由于溶解于有机溶剂的组合物，能够以厚度精确度更良好地进行涂布，因此优选含有有机溶剂。通过从粘合剂原材料组合物中干燥溶剂，能够得到粘合性树脂层。即，粘合剂原材料组合物的组成，也可以是在构成粘合性树脂层的粘合性树脂组合物的组成中添加有溶剂的组成。粘合性树脂层在常温下(热固化前)，能够起粘着剂层的功能。
构成(A)丙烯酸类聚合物的单体，可举出：具有酯基(-COO-)的丙烯酸类单体、具有羧基(-COOH)的丙烯酸类单体、具有酰胺基(-CONR2，R为氢原子或烷基等的取代基)的丙烯酸类单体、具有腈基(-CN)的丙烯酸类单体、烯烃类、苯乙烯、乙烯基酯类、乙烯基醚类、乙烯基硅烷等非丙烯酸类单体。(A)丙烯酸类聚合物优选为由2种以上的单体所构成的共聚物。光聚合前的(A)丙烯酸类聚合物的数均分子量，例如优选为50,000～1,000,000左右。粘度可举出例如1,000～10,000mPa·s左右。
作为具有酯基(-COO-)的丙烯酸类单体，可举出(甲基)丙烯酸烷基酯、具有羟基(氢氧基)的(甲基)丙烯酸酯、具有烷氧基或聚醚基的(甲基)丙烯酸酯、具有氨基或取代氨基的(甲基)丙烯酸酯等。此外，在本说明书，(甲基)丙烯酸酯是指丙烯酸酯及甲基丙烯酸酯的总称。
作为具有羧基(-COOH)的丙烯酸类单体，可举出：丙烯酸、甲基丙烯酸、具有羧基(-COOH)的(甲基)丙烯酸酯等。
作为具有酰胺基(-CONR2，R为氢原子或烷基等的取代基)的丙烯酸类单体，可举出丙烯酰胺、甲基丙烯酰胺等。
作为具有腈基(-CN)的丙烯酸类单体，可举出丙烯腈、甲基丙烯腈等。
优选(A)丙烯酸类聚合物中的结构单体的50重量％以上，由丙烯酸类单体所构成。特别是优选结构单体的50重量％以上由通式CH2＝CR1-COOR2(式中，R1表示氢或甲基，R2表示碳原子数为1～14的烷基)表示的(甲基)丙烯酸烷基酯中的1种或2种以上所构成。作为(甲基)丙烯酸烷基酯的具体例，可举出(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正丙酯、(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)丙烯酸叔丁酯、(甲基)丙烯酸正戊酯、(甲基)丙烯酸异戊酯、(甲基)丙烯酸正己酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸正辛酯、(甲基)丙烯酸异辛酯、(甲基)丙烯酸异壬酯、(甲基)丙烯酸癸酯、(甲基)丙烯酸十二酯。特别优选将烷基R2的碳原子数为4～12的(甲基)丙烯酸烷基酯设作必需而(例如50～100mol％)使用。
此外，作为含有羟基的(甲基)丙烯酸酯，例如可举出：(甲基)丙烯酸2-羟基乙酯、(甲基)丙烯酸2-羟基丙酯、(甲基)丙烯酸3-羟基丙酯、(甲基)丙烯酸4-羟基丁酯、(甲基)丙烯酸6-羟基己酯、(甲基)丙烯酸8-羟基辛酯、聚乙二醇单(甲基)丙烯酸酯、聚丙二醇单(甲基)丙烯酸酯、环己烷二甲醇单(甲基)丙烯酸酯等中的1种或2种以上。
(B)丙烯酸类单体或丙烯酸类寡聚物中，作为丙烯酸类单体，可举出：与构成(A)丙烯酸类聚合物的单体同样的单体，例如(甲基)丙烯酸烷基酯、含有羟基的(甲基)丙烯酸酯、丙烯酰胺等中的1种或2种以上。1分子中的(甲基)丙烯酰基等的聚合性官能团的数目可为1个，也可为2个以上。
特别是含有具有羟基的(甲基)丙烯酸酯单体作为(B)丙烯酸类单体或丙烯酸类寡聚物中的至少一部分时，具有极性的羟基容易分散于粘合性树脂层的整体。由此，即便在湿度较高的(进一步为高温的)环境下，水分也不容易凝聚，能够抑制粘合性树脂层的白浊，因此优选。在具有羟基的(甲基)丙烯酸酯中，1分子中的羟基的数目可为1个，也可为2个以上。
此外，作为(B)丙烯酸类单体或丙烯酸类寡聚物中的至少一部分，可以使用固化性氨酯丙烯酸酯。氨酯丙烯酸酯为在同一分子中具有氨基甲酸酯键(-NH-COO-)及(甲基)丙烯酰氧基(记作X＝H或CH3，CH2＝CX-COO-)的化合物。固化性氨酯丙烯酸酯，是指氨酯丙烯酸酯中，通过作为聚合性官能团的(甲基)丙烯酰氧基而具有固化性的化合物。1分子中的氨基甲酸酯键的数目可为1个，也可为2个以上。此外，1分子中的(甲基)丙烯酰氧基的数目可为1个，也可为2个以上。
作为氨酯丙烯酸酯，例如可举出：使具有羟基的(甲基)丙烯酸酯化合物与异氰酸酯化合物反应而得到的化合物；及使具有羟基的(甲基)丙烯酸酯化合物，与使多元醇化合物与聚异氰酸酯化合物反应而得到的氨酯预聚合物反应而得到的化合物等。作为多元醇化合物，可举出聚酯多元醇、聚醚多元醇等。
(B)丙烯酸类单体或丙烯酸类寡聚物，优选为通过由(C)热聚合引发剂引起的热固化而成为聚合物的一部分，且为比聚合物粘度低的液体(流体)。也可以同时使用丙烯酸类单体及丙烯酸类寡聚物。作为丙烯酸类寡聚物，可举出：氨酯丙烯酸酯寡聚物等丙烯酸酯寡聚物。(B)丙烯酸类单体或丙烯酸类寡聚物所具有的聚合性官能团的数目，例如为1～10个，优选为2～5个。
相对于(A)丙烯酸类聚合物100重量份，粘合性树脂组合物优选含有5～50重量份的(B)丙烯酸类单体或丙烯酸类寡聚物。若(B)丙烯酸类单体或丙烯酸类寡聚物的添加量过多，则使其热聚合时，会有粘合性树脂层的粘合力太低的情况。
作为(C)热聚合引发剂，可举出通过热而分解、使单体的聚合(自由基聚合)及树脂的固化开始的自由基引发剂。作为自由基引发剂，虽已知有在低温下起作用的氧化还原引发剂及有机金属化合物等，但是考虑粘合性树脂层的操作性这一点，优选在更高温下起作用的(有机)过氧化物类、偶氮类等。热聚合引发剂中，在转移胶带的制造过程中，特别是为了在溶剂的干燥工序中不反应或者不半衰，优选热聚合引发剂的半衰期为1分钟的温度(以下有时称为“1分钟半衰期温度”)，比粘合剂原材料组合物所含的有机溶剂的沸点更高。此外，为了使热聚合引发剂在热压时的温度下充分地反应一定时间，优选具有比热压设定温度低50℃以上的1分钟半衰期温度的材料。
作为(有机)过氧化物类的热聚合引发剂的具体例，可举出过氧化苯甲酰、过氧化乙酰、过氧化癸酰、过氧化月桂酰等二酰基过氧化物、过氧化二异丙苯、过氧化二叔丁基等二烷基过氧化物、过氧化苯甲酸叔丁酯、过氧化-2-乙基己酸叔丁酯等过氧化烷基酯；异丙苯过氧化氢、叔丁基过氧化氢等的过氧化氢等。尤其，优选上述的1分钟半衰期温度为100℃以上的有机过氧化物，更优选以1分钟半衰期温度在100℃～200℃的范围内的有机过氧化物。作为这样的有机过氧化物，可举出过氧化新癸酸叔己酯、过氧化新癸酸叔丁酯、过氧化新庚酸叔丁酯、过氧化新戊酸叔戊酯、过氧化新戊酸叔丁酯、过氧化二月桂酰、过氧化-2-乙基己酸1,1,3,3-四甲基丁酯、过氧化二琥珀酸、叔己基过氧化-己酸2-乙酯、过氧化-2-乙基己酸叔丁酯、1,1-双(叔己基过氧化)环己烷、1,1-双(叔丁基过氧化)环己烷、过氧化异丙基单碳酸叔己酯、叔丁基过氧化马来酸、叔丁基过氧化己酸3,5,5-三甲酯、叔丁基过氧化单碳酸异丙酯、叔丁基过氧化单碳酸2-乙基己酯、过氧化月桂酸叔丁酯、过氧化苯甲酸叔己酯、过氧化乙酸叔丁酯、过氧化苯甲酸叔丁酯、4,4-双(叔丁基过氧化)戊酸正丁酯、过氧化二异丙苯、过氧化二叔己基、过氧化二叔丁基、过氧化氢对孟烷等。
作为偶氮类的热聚合引发剂，可举出2,2'-偶氮双(异丁腈)、2,2'-偶氮双(2-甲基丁腈)、2,2'-偶氮双(2,4-二甲基戊腈)、2,2'-偶氮双(4-氰基戊腈)、2,2'-偶氮双(4-甲氧基-2,4-二甲基戊腈)、2,2'-偶氮双(甲基异丁酸酯)、1,1'-偶氮双(1-环己烷腈)等。此外，本发明的聚合引发剂，为了控制反应性，能够使用被封入具有笼状分子的分子胶囊中的热聚合引发剂。笼状分子优选为蒽结构。
相对于(A)丙烯酸类聚合物100重量份，(C)热聚合引发剂的添加量优选为0.001～0.5重量份。
在本发明的粘合性树脂层中，也能够添加聚合延迟剂。通过使用聚合延迟剂，能够容易地控制聚合度。此外，从使对基材的变形的追随性提高的角度出发而优选。
粘合性树脂组合物，可以进一步含有除(A)～(C)以外的任意成分。例如，为了使(A)丙烯酸类聚合物、或通过(B)丙烯酸类单体或丙烯酸类寡聚物的聚合而生成的聚合物交联，优选使用异氰酸酯类交联剂、环氧类交联剂、金属螯合物等的(D)交联剂(固化剂)。此时，根据需要，作为(A)丙烯酸类聚合物或(B)丙烯酸类单体或丙烯酸类寡聚物中的至少一部分，可以使用具有与(D)交联剂反应的官能团的聚合物或单体。与(D)交联剂反应的官能团，例如采用异氰酸酯类交联剂时，为羟基或羧基等。相对于聚合物的官能团，(D)交联剂的添加量例如优选为1.5当量以下。
通过由(D)交联剂(固化剂)引起的(A)丙烯酸类聚合物的固化，也可在贴合在被粘物前的制造粘合性树脂层的阶段，通过熟化而使其进行。
作为其他任意成分，例如可举出抗氧化剂、填充剂、增塑剂等。制造粘合性树脂层时所使用的粘合剂原材料组合物，可含有水或有机溶剂等的溶剂，也可为无溶剂的浆状组合物。在基材上存在ITO等的氧化物导电膜或贱金属等的有被腐蚀可能性的材料，且其与粘合性树脂层接触时，作为粘合性树脂组合物的材料，优选使用减少酸等的腐蚀性成分的聚合物，例如优选使用酸值低的聚合物。
本发明的粘合性树脂层的制造中，优选尽量使作为进行固化的成分的丙烯酸类单体或丙烯酸类寡聚物固化。此外，使用丙烯酸类寡聚物时，丙烯酸类聚合物及丙烯酸类寡聚物的分子量均较大，作为涂料的相容性变差的情况常常发生。因此，优选添加增容剂。虽为无反应性的增容剂也无妨，但是由于有在粘着剂层产生分离的可能性，所以能够使用的材料受到限定的可能性较高，并且根据种类或添加量，有在耐久试验中发生发泡等问题的可能性，通用性较低。因此，若为在热反应时与丙烯酸类寡聚物一起固化的增容剂，则由于进行高分子化，也能够抑制发泡等的缘故，因此，优选选择保有反应基团的材料。而且，使用如热反应后会***的丙烯酸类单体作为增容剂时，可期待涂料的稳定性，同时也能够期待固化后粘着剂层***的效果。丙烯酸类单体，除了相容性良好以外，相较于丙烯酸类聚合物或丙烯酸类寡聚物，由于粘度较低，因此可通过在涂料的粘度太高时进行添加，以使在制膜时调整到最适合的粘度，从而有助于生产率的提高。
(粘合性树脂层的制造方法)
本发明的粘合性树脂层(转移胶带)，能够通过将粘合剂原材料组合物在含有溶剂的状态下涂布在隔离膜上，进行干燥，进一步被隔离膜保护而制造。粘合剂原材料组合物，优选使用模具或管刮刀(pipe doctor)而涂布。在溶剂的干燥中，优选使用干燥机等使其干燥。关于溶剂的干燥时间，考虑生产率时，优选为10分钟以下，进一步优选为2～5分钟。此外，由于必须将有机溶剂充分地干燥，所以优选在有机溶剂的沸点以上的温度下使其干燥，优选在热聚合引发剂的1分钟半衰期温度以下进行干燥。
以上，基于优选的实施方式对本发明进行了说明，但是本发明并不限定于上述的实施方式，在不脱离本发明的要旨的范围可以进行各种改变。
层叠体也可在3片以上的基材之间，分别具有粘合性树脂层。优选层叠体中所含的2层以上的粘合性树脂层中的1层以上(优选为全部)为本实施方式的粘合性树脂层。
将层叠体热压时，也可在一对模具之间设置2个以上的层叠体。该设置没有特别限定，可在模具的压缩方向层叠2个以上的层叠体，也可在与压缩方向垂直的面内(例如任一模具的按压面上)排列2个以上的层叠体。也可使上述的介入物介于2个以上的层叠体之间。
在本发明中，在制造如图1的粘合性树脂层11之后，制造如图2的层叠结构，而且经过热压等的热处理，能够制造如图3的层叠体30。在制造图1的粘合性树脂层11时，优选设置通过加热从含有溶剂的粘合剂原材料组合物中将溶剂去除的工序。此外，在之后的贴合后的制程条件下，需要对粘合性树脂层11进行加热，从而使聚合开始。
在本发明的加压时，为了对层叠体施加加热温度为100～250℃的热，模具的温度需要以比所需的加热温度更高的温度进行加热。模具的温度优选为100～300℃。
关于本发明中的加压时间，从生产率的角度出发，优选在短时间反应结束，例如优选在5分钟以内结束。此外，可对加压温度及时间进行设定，以使层叠体的强度变得充分。
实施例
以下，通过实施例对本发明进行具体的说明。
(实施例1)
使用作为含有丙烯酸类聚合物的聚合物溶液的SK-Dyne(注册商标)2094(SokenChemical&Engineering CO.,Ltd.)、作为交联剂的E-AX(Soken Chemical&EngineeringCO.,Ltd.)，相对于丙烯酸类聚合物100重量份，以交联剂为0.2重量份的比例混合。在所得到的混合物中，添加作为具有反应性的流动性树脂成分的丙烯酸类单体的丙烯酸4-羟基丁酯(OSAKA ORGANIC CHEMICAL INDUSTRY LTD.；4HBA)40重量份、作为热聚合引发剂的过氧化-2-乙基己酸叔丁酯(NOF CORPORATION制造；制品名：PERBUTYL(注册商标)O)0.08重量份，调制粘合剂原材料组合物。粘合剂原材料组合物，含有作为溶剂的乙酸乙酯(沸点77℃)，作为用于涂布的涂料，粘度等性状得到改善。
以在干燥后的粘合剂树脂层(粘着剂层)的厚度为50μm的方式，使用涂布器将该粘合剂原材料组合物涂布在隔离膜(FUJIMORI KOGYO CO.,LTD.制造；制品名：125E-0010DG2.5AS、厚度125μm)的上表面后，在干燥工序中于90℃、2分钟的条件下使溶剂干燥，制造层叠有粘合性树脂层的层叠体。
接着，在得到的层叠体的粘合性树脂层的上表面，贴合隔离膜(FUJI MORI KOGYOCO.,LTD.制造；制品名：38E-0010BDAS、厚度38μm)，制造实施例1的粘合性树脂膜。
随后，通过进行1星期的熟化，使丙烯酸类聚合物与交联剂(环氧类)的反应结束，形成存在经交联的丙烯酸类聚合物、具有反应性的流动性树脂成分、及热聚合引发剂这3种的粘合性树脂层。
关于实施例1～19及比较例1～8，以表1中记载的粘合剂原材料组合物的组成及表2中记载的粘合剂树脂层的厚度，制造在隔离膜之间包含粘合性树脂层的层叠体。表1或表2中未记载的事项，与实施例1相同。但是，在实施例2及实施例6～9中，异氰酸酯类的交联剂(TD-75、COR ONATE HX)不仅与丙烯酸类聚合物的官能团反应，也与含有羟基的丙烯酸类单体(4HBA)的一部分反应，从而形成经交联的丙烯酸类聚合物，此时，也与实施例1同样地，粘合性树脂层中存在经交联的丙烯酸类聚合物、具有反应性的流动性树脂成分、及热聚合引发剂这3种。
[表1]
此外，在表1中，商品以溶液的形式在市场上销售时，重量份的数值为表示其中构成粘合性树脂层的各成分的重量份。
“SK-Dyne 2094”及“SK-Dyne 2147”分别表示丙烯酸类聚合物的商品名称：SK-Dyne(注册商标)2094(Soken Chemical&Engineering CO.,Ltd.)、酸值：33、数均分子量7万、固体成分浓度25％)、SK-Dyne(注册商标)2147(Soken Chemical&Engineering CO.,Ltd.)、酸值：33)。“N-7136”表示丙烯酸类聚合物的商品名称：COPONYL(注册商标)N-7136(The Nippon Synthetic Chemical Industry Co.,Ltd.、固体成分浓度32％)。在表1中，将各成分的换算成固体成分量的重量设作添加量重量份而记载。
“CORONATE HX”表示聚异氰酸酯类固化剂的商品名称：CORONATE(注册商标)HX(TOSOH CORPORATION)。“E-AX”表示环氧类固化剂的商品名称(Soken Chemical&Engineering CO.,Ltd.)。“TD-75”表示异氰酸酯类固化剂的商品名称(Soken Chemical&Engineering CO.,Ltd.)。
“UV-3310B”及“UV-1700”为表示氨酯丙烯酸酯的商品名称(The NipponSynthetic Chemical Industry Co.,Ltd.)。UV-3310B的物性为，在60℃下的粘度：40000～70000mPa·s；重均分子量Mw：5000；寡聚物官能团数：2；玻璃化转变温度Tg：22℃。
“PERHEXA(注册商标)V”表示以4,4-双(叔丁基过氧化)戊酸正丁酯作为有效成分的热聚合引发剂。“PEROCTA(注册商标)O”表示以过氧化-2-乙基己酸1,1,3,3-四甲基丁酯作为有效成分的热聚合引发剂。“PERBUTYL(注册商标)O”为以过氧化-2-乙基己酸叔丁酯作为有效成分的热聚合引发剂。“PERHEXA(注册商标)HC”表示以1,1-双(叔己基过氧化)环己烷作为有效成分的热聚合引发剂。“PERHEXA(注册商标)Z”为以过氧化苯甲酸叔己酯作为有效成分的热聚合引发剂。“Irg651”为以2,2-二甲氧基-2-苯基苯乙酮(别名苄基二甲缩酮)作为有效成分的光聚合引发剂。“PERCUMYL(注册商标)ND”为以1分钟半衰期温度较低(约94℃)的过氧化新癸酸异丙苯酯作为有效成分的热聚合引发剂。“PERCUMYL(注册商标)P”为以1分钟半衰期温度非常高(约232℃)的二异丙苯过氧化氢作为有效成分的热聚合引发剂。热压温度被设定为210℃以下，使用比其高的1分钟半衰期温度的热聚合引发剂时，由于热反应引发剂的一部分以未反应的状态而残留，有在耐久试验等中成为发泡原因的可能性，因此不优选。
<试验结果>
接着，对评价方法及其结果进行说明。
(DSC测定方法)
通过升温速度10℃/分钟的差示扫描热量测定(DSC)，来测定粘合性树脂层的发热起始温度及波峰温度。波峰温度为发热波峰(发热量成为最大的波峰)的温度的测定值。发热起始温度为波峰温度为最低的发热波峰从基线开始上升时的温度的测定值。测定范围至少为20℃～210℃，在该范围内未能确认到发热波峰时，粘合性树脂层不含有热聚合引发剂时记作“无”，粘合性树脂层含有热聚合引发剂时记作“未能观察到”。
(通过多维形状制造的粘合性树脂层的评价方法)
作为基材，准备2片裁断为15cm×15cm的厚度100μm的平坦聚对苯二甲酸乙二醇酯(PET)膜。它们的厚度可相同，也可不同，但是在该评价方法中，设为相同厚度。从粘合性树脂膜上将一侧的隔离膜剥离，贴合至第一片的PET膜上，进一步将相反侧的隔离膜剥离，贴合第二片的PET膜，制造经由粘合性树脂层以2片PET膜夹持而成的层叠膜。将至此为止的工序称为层叠工序。
使用能够形成多维形状的模具，将层叠膜设置在上下的模具之间，将模具的温度上升至设定温度为止。将该设定温度(实施例9为150℃，实施例1～8、12～19为200℃，实施例10为250℃，实施例11为300℃)作为热压温度，将到达热压温度之前的状态设作预热。在热量上升至热压温度为止时，将上下的模具进行加压而使层叠膜变形。将上下的模具合闭的时间设作加压时间，在本评价方法中设定为2分钟。经过2分钟后将模具打开，将层叠膜取出。
关于多维形状层叠膜及其制造过程，对于层叠工序不良、边缘浮起、粘合强度、微小的追随性这4个项目，采用◎(非常优异)、○(优异)、△(稍微优异)、×(差)这4个级别进行评价。
关于层叠工序不良，根据在热压前的层叠工序中的粘合不良的有无、程度等，如下所述进行评价。
◎：通过目视对层叠膜未观察到气泡、缺陷，且外观良好。
○：通过目视对层叠膜观察到一点点气泡、或缺陷，但为对外观没有实际损害的程度。
△：通过目视对层叠膜观察到一点点气泡、或缺陷，但为容许范围内。
×：通过目视对层叠膜观察到气泡、或缺陷，且外观为容许范围外。
关于边缘浮起，对热压后的层叠膜，通过目视进行外观确认，且如下所述进行评价。
◎：对层叠膜未确认到边缘浮起。
○：对层叠膜确认到极小的边缘浮起。
△：对层叠膜确认到边缘浮起但为容许范围内。
×：对层叠膜确认到边缘浮起且为容许范围外。
关于粘合强度，对由热压后的层叠膜所制成的测定试料，测定2片PET膜间的粘合强度，以下述方式进行评价。使用岛津制作所的剥离试验机，将2片PET膜之中的一个剥掉，以剥离角度180度、拉伸速度300m/min，剥下100mm的长度，且将数值稳定的部分的平均值设作粘合强度。根据该测定值，如下所述进行评价。
◎：粘合强度为30N/25mm以上
○：粘合强度为20N/25mm以上且小于30N/25mm
△：粘合强度为10N/25mm以上且小于20N/25mm
×：粘合强度小于10N/25mm
此外，关于微小的追随性，对热压后的层叠膜，通过目视进行外观确认，来确认是否有气泡等的发泡，如下所述进行评价。
◎：对层叠膜未确认到气泡。
○：对层叠膜确认到极小的气泡。
△：对层叠膜确认到气泡，但为容许范围内。
×：对层叠膜确认到气泡，且为容许范围外。
将使用上述评价方法得到的结果，显示在下述的表2中。
[表2]
(评价结果)
在实施例中均未确认到在层叠体有气泡等的外观上的不良。认为这是由于，在粘合性树脂组合物中，除了(A)丙烯酸类聚合物以外，粘合性树脂组合物中还含有作为流动性较高的成分的(B)丙烯酸类单体或丙烯酸类寡聚物的缘故。
在比较例1、5中，通过热压后的外观确认，在使基材变形后的部分中，在粘合性树脂层与PET膜之间确认到剥离。认为这是由于，粘合性树脂组合物中不含具有反应性的流动性树脂成分(丙烯酸类单体或丙烯酸类寡聚物)，致使粘合性树脂层未追随材料的变形的缘故。
在比较例2～4及6～8中，通过热压后的外观确认可知，虽然使基材变形了的部分进行了良好地追随，但是在整个面上确认到发泡。
在比较例2中，认为虽然在粘合性树脂组合物中含有具有反应性的流动性树脂成分，但是由于引发剂为光聚合引发剂，在热压中不进行固化反应，且一部分的低分子成分气化，在从模具释放压力时，由于温度引起的挥发及密合性的降低，因而发生了剥离。该例子的情况下，若能够在热压中利用某些方法进行照射紫外线，从而进行固化反应，则能够解决该技术问题，但是对不透明的模具内照射紫外线是困难的。
在比较例3、7中，认为虽然在粘合性树脂组合物中含有具有反应性的流动性树脂成分，但是由于不含引发剂，所以在热压时固化反应不进行，基于与比较例2同样的理由而发生了剥离。
在比较例4中，认为由于使用1分钟半衰期温度较低的过氧化物作为引发剂，发热起始温度太低而在热压中不进行固化反应，基于与比较例2同样的理由而发生了剥离。
在比较例8中，认为由于使用1分钟半衰期较高的过氧化物作为引发剂，在利用DSC进行的测定中，在210℃以下未能观察到波峰，在热压时的温度下未开始聚合反应，基于与比较例2同样的理由而发生了剥离。
在比较例6中，认为由于相对于具有反应性的流动性树脂成分的热聚合引发剂的量过多，因此在由DSC得到的测定值中的发热起始温度、波峰温度低，在热压前进行聚合反应，即便进行反应，聚合物的分子量也未变大，密合性未得到提高，因此发生了发泡。
由比较例1～3、5、7的结果可知，为了使实施例的功能显现，必须在粘合性树脂组合物中添加具有反应性的流动性树脂成分及热聚合引发剂。此外，由比较例4、6、8的结果可知，为了使实施例的功能显现，粘合性树脂层的通过DSC测定得到的波峰温度太低或太高均有问题。此外，波峰温度，能够通过调整热聚合引发剂的种类、或相对于丙烯酸类聚合物或流动性树脂成分的热聚合引发剂的量等来控制。
在实施例中，由于粘合性树脂层以对PET等的被贴合的基材的流动性高的状态被贴合，所以能够紧密地密合。而且，由于通过热压，具有反应性的流动性树脂成分流动，在追随基材的变形后，通过热而慢慢地进行热聚合反应，具有反应性的流动性树脂成分进行高分子化，粘合性树脂层的流动性降低，以变形后的状态进行固化，所以不仅是在变形部中不产生气泡，在基材之间也不产生发泡。
如实施例19一样地添加与丙烯酸类寡聚物相容性良好的4HBA，具有确保涂料的稳定性的效果。由于丙烯酸类聚合物的分子量越大，耐热性和耐久性有变得越良好的倾向，所以优选尽可能使用分子量较大的聚合物。发现了通过添加具有反应性的流动性树脂成分，制膜时粘合性树脂层的流平性(leveling ability)良好，且膜厚的均匀性得到提高的倾向。
在粘合性树脂层被层叠于隔离膜之间的状态下，将各实施例的粘合性树脂膜在与“(通过多维形状制造的粘合性树脂层的评价方法)”相同条件下进行热压后，通过使用FT-IR(傅立叶(Fourier)变换红外分光法)对固化后的粘合性树脂层进行分析时，几乎无法确认到碳-碳双键(丙烯酸类单体的乙烯基等)的波峰。而且在热压前后通过DSC(差示扫描热量测定)进行分析时，在热压前的DSC测定中，观察到了发热波峰，但是在热压后的DSC测定中，未能观察到发热波峰。由这些结果可认为固化反应在热压条件下结束。
在比较例1～5及7～8的粘合性树脂层中，即便进行热压，通过FT-IR也能够确认到些许被认为是源自碳-碳双键的波峰。
比较例1～3及7的在热压前的DSC中，未能确认到发热波峰。由于未能确认到由热引起的反应，所以能够判断热固化反应未进行。
在比较例5的在热压前的DSC中，只确认到热聚合引发剂的发热，由于无具有反应性的流动性树脂成分，因此未进行聚合反应。
在比较例4、8的在热压前的DSC中，虽然确认到了发热波峰，但是由于发热起始温度及波峰温度高，所以能够判断在上述的热压条件下，未进行热固化反应。
在比较例6的粘合性树脂层中，通过热压后的FT-IR，几乎未能确认到碳-碳双键的波峰。而且在热压前的DSC测定中，虽然观察到了发热波峰，但是在热压后的DSC测定中，未能观察到发热波峰。由这些结果可认为在比较例6中，固化反应在热压条件下结束。
(粘合性树脂自身的DSC测定)
在实施例15～18中，通过DSC进行粘合性树脂自身的热分析。从其结果可知，虽然也取决于热聚合引发剂的种类，但是确认到在100℃以上激烈地开始反应。由此可以看出，能够使用于粘合剂原材料组合物及粘合性树脂组合物的有机溶剂的沸点，优选为100℃以下，更优选为80℃以下。
从以上的结果可知，通过使粘合性树脂层含有作为主要成分的(A)丙烯酸类聚合物、(B)丙烯酸类单体或丙烯酸类寡聚物、及(C)热聚合引发剂，能够制造可抑制因高温的热压加工而产生气泡及剥离，制造能够形成三维形状的粘着膜。
附图标记说明
10 粘合性树脂膜
11 粘合性树脂层
11a、11b 粘合性树脂层的两面(粘着面)
12、13 隔离膜
12a、13a 隔离膜的表面(剥离面)
20、30 层叠体
21、22 基材
21a、22a 内表面
21b、22b 外表面
23 热固化后的粘合层

Claims (5)

1.一种粘合性树脂层，其为含有丙烯酸类粘合性树脂组合物的单层的粘合性树脂层，其特征在于：
所述粘合性树脂组合物仅含有(A)丙烯酸类聚合物、(B)丙烯酸类单体或丙烯酸类寡聚物、(C)热聚合引发剂及(D)交联剂，
所述粘合性树脂组合物，相对于所述(A)丙烯酸类聚合物100重量份，含有5～50重量份的所述(B)丙烯酸类单体或丙烯酸类寡聚物，且含有选自由含羟基的丙烯酸类单体及固化性氨酯丙烯酸酯组成的组中的1种以上作为所述(B)丙烯酸类单体或丙烯酸类寡聚物中的至少一部分，
所述粘合性树脂层在常温下在两面具有粘着性，在升温速度为10℃/分钟的差示扫描热量测定(DSC)中，在80℃以上开始确认发热，在120℃～210℃之间确认至少1个波峰。
2.根据权利要求1所述的粘合性树脂层，其特征在于，所述(C)热聚合引发剂为过氧化物。
3.一种粘合性树脂膜，其特征在于，通过在2片隔离膜之间层叠权利要求1或2所述的粘合性树脂层而成。
4.一种用于形成层叠体的粘合性树脂层，其中，所述层叠体通过经由权利要求1或2所述的粘合性树脂层，层叠2片基材而成。
5.一种粘合性树脂层，其特征在于：在将经由权利要求1或2所述的粘合性树脂层层叠2片基材而得到的层叠体，夹持于2个模具之间的状态下，使所述层叠体加热变形，所述粘合性树脂层即使在加热固化后，粘着力也为10N/25mm以上。
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CN102015950A (zh) * 2008-04-21 2011-04-13 Lg化学株式会社 压敏粘合剂组合物，以及包括该压敏粘合剂组合物的偏振片和液晶显示器

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