CN101855080A - 剥离片材及压敏粘合剂制品 - Google Patents
剥离片材及压敏粘合剂制品 Download PDFInfo
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Abstract
本发明提供具有良好剥离性能的非硅氧烷剥离片材,其中,即使在长时间以卷绕的辊状形式存储后也不会发生粘连。剥离片材10通过在剥离片材基底11上层压底涂层12和剥离剂层13构成。剥离剂层13由包含密度为0.800至0.905克/立方厘米且用多位点催化剂聚合的聚烯烃热塑性树脂的聚烯烃树脂组合物形成。在剥离剂层13中,在自其表面50至1000纳米深度处采用纳米压痕法在23℃下测量的剥离剂层的平均弹性模量为0.1至0.3GPa,在表面上形成粗糙以使其表面粗糙度Ra1为100至700纳米。
Description
技术领域
本发明涉及具有由聚烯烃树脂组合物形成的剥离剂层的剥离片材,尤其涉及用于诸如硬盘驱动器等的精密电子设备的名牌标签或低逸气带的应用中的剥离片材。
背景技术
用于压敏粘合剂带的剥离片材通过在基底片材上层压剥离剂层构成,硅氧烷剥离剂通常用于剥离剂层。对于硅氧烷剥离剂,尽管其剥离性能极佳,但是部分低分子硅氧烷化合物能被转移至压敏粘合剂,由此使得压敏粘合剂带粘附其上的粘附体会被硅氧烷化合物污染。因此,当将压敏片材用于固定在诸如硬盘驱动器等的电子设备上的应用时,硅氧烷污染可引起电子设备失灵。
因此,正研究将非硅氧烷剥离剂,例如长链烷基剥离剂、醇酸树脂剥离剂、氟化剥离剂、聚烯烃剥离剂等用于取代硅氧烷剥离剂以防止电子设备的硅氧烷污染。但是,使用长链烷基剥离剂和醇酸树脂剥离剂的应用由于它们的大剥离力而受到限制;此外,氟化剥离剂尽管其剥离力小但是昂贵,因此很难将其用于批量生产工艺。
另一方面,聚烯烃剥离剂广泛用于需要低剥离力的应用中,因为可使其剥离力较小(参见专利引文1至6)。最近,利用聚烯烃树脂的剥离剂已得到各种各样的改进,例如在专利引文1中讨论了在剥离剂层的表面上形成由1至3微米的表面粗糙度Ra限定的粗糙(roughness)从而改进剥离剂层的剥离性能。
专利引文1:日本未审查专利公布(KOKAI)No.2005-350650
专利引文2:日本专利公布No.3776120
专利引文3:日本未审查专利公布(KOKAI)No.2003-147295
专利引文4:日本未审查专利公布(KOKAI)No.2003-147294
专利引文5:PCT专利申请国际公布的已公开日文翻译(KOHYO):No.11-508958
专利引文6:日本已审查申请公布(KOKOKU)No.57-45790
发明内容
技术问题
顺便提一下,通常剥离片材被卷绕成辊状形式,然后在粘合至压敏粘合剂片材之前存储起来。但是,由于将其以卷绕的辊状形式进行存储,因此剥离片材(其中聚烯烃树脂用于剥离剂层)存在较难从辊卷展开成片材的问题,因为很容易发生所谓的“粘连”,即其中剥离片材的背面变得粘住剥离剂层。
此外,如专利引文2中所公开,用诸如茂金属催化剂等的单位点催化剂聚合的聚烯烃树脂通常用于剥离剂。但是,用单位点催化剂聚合的聚烯烃树脂的物理性能可以通过加热至预定的温度得以极大地改变,因为分子量的分布范围及其组成是狭窄的。因此,即使在制备后不立即发生粘连,在长期存储过程中在相对高的温度下也会发生粘连。而且,即使在刚制备后剥离性能是良好的,但在长期存储后剥离性能也会损害。
因此,鉴于以上问题产生了本发明,本发明的目的是提供一种利用聚烯烃树脂的剥离片材,其具有良好的剥离性能,但是其中即使在剥离片材以卷曲的辊状形式长期存储后也不会发生粘连。
技术方案
本发明的剥离片材包括剥离剂层,所述剥离剂层由包含密度为0.800至0.905克/立方厘米且用多位点催化剂聚合的聚烯烃热塑性树脂的聚烯烃树脂组合物形成,所述剥离剂层在自其表面50至1000纳米深度处采用纳米压痕法在23℃下测量的剥离剂层的平均弹性模量为0.1至0.3GPa,在表面上形成粗糙以使其表面粗糙度Ra1为100至700纳米。
如果表面粗糙度Ra2为将剥离片材在40℃的环境条件下静置30天后所述剥离剂层的表面粗糙度,则表面粗糙度比Ra2/Ra1优选为0.9至1.1。聚烯烃树脂组合物的熔体流动速率优选地为1至20克/10分钟。
例如,上述聚烯烃热塑性树脂包含至少一种选自聚乙烯、聚丙烯、聚丁烯、聚(4-甲基-1-戊烯)或乙烯与碳数为3至10的α-烯烃的共聚物的聚烯烃树脂。
剥离片材可以通过将剥离剂层经底涂层层压在基底上构成,优选地所述剥离片材基本上不含硅氧烷化合物。
本发明的压敏粘合剂制品包括基底,层压在基底上的剥离剂层,以及层压在剥离剂层上并与其接触的压敏粘合剂层,其中所述剥离剂层由包含密度为0.800至0.905克/立方厘米且用多位点催化剂聚合的聚烯烃热塑性树脂的聚烯烃树脂组合物形成,所述剥离剂层在自其表面50至1000纳米深度处采用纳米压痕法在23℃下测量的剥离剂层的平均弹性模量为0.1至0.3GPa,在表面上形成粗糙以使其表面粗糙度Ra1为100至700纳米。
例如,压敏粘合剂层优选地由丙烯酸类压敏粘合剂形成,压敏粘合剂制品优选地基本上也不包含硅氧烷化合物。
有益效果
在利用聚烯烃树脂的剥离片材中,在保持良好的剥离性能的同时,即使长期存储也能防止粘连的发生。
附图说明
图1为显示在本发明具体实施方案中的剥离片材的截面示意图。
图2为显示在本发明具体实施方案中的压敏粘合剂制品的截面示意图。
具体实施方式
下文参照附图说明了本发明的具体实施方案。
图1为显示在本发明具体实施方案中的剥离片材的截面示意图。图2为显示在本发明具体实施方案中的压敏粘合剂制品的截面示意图。如图1所示,剥离片材10通过在剥离片材基底11的一个表面上依次层压底涂层12和剥离剂层13构成。剥离剂层13由聚烯烃树脂组合物形成,且在其表面13A上形成大量凹面和凸面(粗糙)。
如图2所示,压敏粘合剂制品20通过使压敏粘合剂片材23粘合至剥离片材10构成,由此压敏粘合剂层22与剥离剂层13的表面13A接触,其中压敏粘合剂片材23通过在压敏粘合剂片材基底21的表面上层压压敏粘合剂层22形成。剥离片材10可以单独卷绕成辊状形式然后存储,或者可在通过将其粘合至压敏粘合剂片材23而制成压敏粘合剂制品20后再将其卷绕成辊状形式然后存储。
用于形成剥离剂层13的聚烯烃树脂组合物至少包含密度为0.800至0.905克/立方厘米且用多位点催化剂聚合的聚烯烃热塑性树脂。此处,根据JIS K7112-1999测量密度。上述聚烯烃热塑性树脂的密度优选地为0.850至0.905克/立方厘米,最优选为0.880至0.905克/立方厘米。
上述多位点催化剂的一个例子包括齐格勒(Ziegler)催化剂,菲利普(Phillips)催化剂和标准(Standard)催化剂。齐格勒催化剂包括由诸如钛化合物、钒化合物等过渡金属化合物组成的主催化剂,由诸如有机铝等有机金属化合物组成的助催化剂,以及由硅、钛、镁或其它的氧化物组成的催化剂载体。菲利普催化剂包括由氧化铬组成的主催化剂和由铝或其它的氧化物组成的催化剂载体。标准催化剂包括由氧化钼组成的主催化剂,以及由铝或其它的氧化物组成的催化剂载体。
上述聚烯烃热塑性树脂通过凝胶渗透色谱法(GPC)测得的重均分子量(Mw)与数均分子量(Mn)之比(Mw/Mn)优选大于或等于3,Mw/Mn更优选为3至10,Mw/Mn最优选为3.6至8。
例如,聚乙烯、聚丙烯、聚丁烯、聚(4-甲基-1-戊烯)、乙烯与碳数为3至10的α-烯烃的共聚物,或者选自其中的两种或多种的混合物可用作上述聚烯烃热塑性树脂。其中,尤其优选乙烯与碳数为3至10的α-烯烃的共聚物。此外,剥离片材10的剥离性能通过限定上述热塑性树脂的密度在上述范围内得以改进。此外,如果上述热塑性树脂用多位点催化剂聚合,则很容易限定Mw/Mn在上述范围内;从而保持预定的剥离性能,且即使剥离片材10在被卷绕成辊状形式的状态下长期存储后也几乎不会发生粘连,因为在剥离剂层表面形成的粗糙很难改变。
上述聚烯烃树脂组合物中的树脂组分仅包含密度为0.800至0.905克/立方厘米的聚烯烃热塑性树脂,但是考虑到层的成形性还可以包含密度超出此范围的聚烯烃热塑性树脂;例如其可进一步包括诸如聚乙烯树脂、聚丙烯树脂(PP)、烯烃弹性体(TPO)等的聚烯烃热塑性树脂,所述聚乙烯树脂例如低密度聚乙烯(LDPE,密度大于或等于0.910克/立方厘米且小于0.930克/立方厘米)、中密度聚乙烯(MDPE,密度大于或等于0.930克/立方厘米且小于0.942克/立方厘米)、高密度聚乙烯(HDPE,密度大于或等于0.942克/立方厘米)等。其中,优选聚乙烯树脂,尤其优选低密度聚乙烯。该聚乙烯树脂通过凝胶渗透色谱法(GPC)测得的重均分子量(Mw)与数均分子量(Mn)之比(Mw/Mn)优选大于或等于6,由此可改进层的成形性。
在上述聚烯烃树脂组合物中包含的密度为0.800至0.905克/立方厘米且用多位点催化剂聚合的聚烯烃热塑性树脂的比例,以聚烯烃树脂组合物为100重量%计优选为50至100重量%,最优选60至100重量%。当然,聚烯烃树脂组合物可以包含不同于上述聚烯烃热塑性树脂的聚烯烃树脂或其它树脂。
聚烯烃树脂组合物的熔体流动速率(MFR)优选地为1至20克/10分钟。如果MFR在1克/10分钟以下,则由于低流动性能使得形成层变得困难;如果MFR超过20克/10分钟,则由于过高的流动性能而难以形成具有均匀厚度的层。根据JISK7210-1997,在温度为190℃和负载21.2N的测量条件下测量MFR。此外,剥离剂层13的厚度优选为3至30微米。
在该具体实施方案中,通过适当混合地或单独地使用上述树脂,将自剥离剂层13的表面13A的50至1000纳米深度处在23℃下的平均弹性模量限定为0.1至0.3GPa。在23℃下的平均弹性模量通过纳米压痕法(Nano Indentation Method)测量[测量装置:纳米压入仪(NanoIndenter)(商标名称:Nano Indenter SA2;由MTS System Corp.制造)],将其计算为在70个点测得的弹性模量值的算术平均值,所述70个点均匀地位于自剥离剂层13的表面13A上20个任选点的各个表面的50纳米深度位置至1000纳米深度位置之间。
自压敏粘合剂片材23剥离开剥离片材10的剥离力可通过将在23℃下的平均弹性模量限定在上述范围内来适当确立。此外,通过将在23℃下的平均弹性模量限定为大于或等于0.1GPa,可使得当剥离片材10或压敏粘合剂制品20卷绕成辊状形状时几乎不会发生粘连。
在剥离剂层13的表面13A上形成大量凹面和凸面(粗糙),由此使得表面粗糙度Ra1为100至700纳米。当剥离片材10被剥离时的剥离力能够被确立为合适的值时,通过将表面粗糙度Ra1限定在上述范围内能够防止粘连的发生。在熔融的剥离剂层13上压印辊等(已通过例如压花在辊的表面上形成精细的粗糙)以在表面13A上产生粗糙。
表面粗糙度Ra1为基于ANSI/ASME B46.1:1995,利用光学干涉表面粗糙度仪(商标名称:WYKO NT1100,由Veeco Instruments制造),在23℃下在物镜的50倍放大率和内部透镜的1倍放大率的条件下测量的算术平均值。如果表面粗糙度Ra1通过接触法测量,则因为剥离剂层13是柔软的,存在由于接触引起的表面改变导致测量误差大的风险;但是,如果如在该具体实施方案中那样通过非接触法测量,则获得的表面粗糙度Ra1的精确度较高。
优选的是,即使将剥离片材10在高温条件下静置长时间之后,表面粗糙度的改变仍然很小。例如,如果当剥离片材10在预定的温度条件(40℃)下以卷绕的辊状形式静置长时间(30天)后再次展开成片材形式时剥离片材10的表面粗糙度为“Ra2”,则表面粗糙度比(Ra2/Ra1)优选为0.9至1.1。此外,在那些与表面粗糙度Ra1相同的条件下测量表面粗糙度Ra2。
在该具体实施方案中剥离片材10用于需要相对低剥离力的应用中,当剥离片材10自压敏粘合剂片材23剥离时的剥离力优选地为50毫牛/20毫米至500毫牛/20毫米。如果剥离力超过上述上限,则剥离力变得非常大以致引发剥离问题,即其中部分压敏粘合剂与剥离片材10一起被剥离开来。此外,如果剥离力在上述下限以下,则剥离力很小以致压敏粘合剂片材23会突然从剥离片材10滑脱。此外,在该说明书中,剥离力是根据JIS Z0237测量获得的值。
底涂层12为在剥离片材基底11的一个表面上通过挤出层压、涂布或其它方法形成的层,且形成为在剥离片材基底11与剥离剂层13之间的层。底涂层12可由与在上述剥离剂层13中类似的聚烯烃树脂组合物形成,但是优选使用低密度聚乙烯从而使其如上文所限定的平均弹性模量优选地比剥离剂层13的高。而且,在底涂层12上可提供一个或多个另外的层。
通过例如聚烯烃树脂组合物的挤出层压使得剥离剂层13直接地或者经一个或多个其它层而层压在上述底涂层12上。对于剥离片材基底11和压敏粘合剂片材基底21,可以适当选择并使用可用于剥离片材10或者用于压敏片材23的被认为是常规基底的任何基底;例如,可使用由热塑性树脂等形成的树脂薄膜、纸、金属箔或其组合。作为形成压敏粘合剂层22的压敏粘合剂,可以无特定限制地使用非硅氧烷压敏粘合剂,例如使用丙烯酸类压敏粘合剂或其它粘合剂。
在该具体实施方案中,在防止辊状形式中发生粘连的同时,由于将剥离剂层13平均弹性模量和表面粗糙度Ra1以及上述树脂的密度限定在预定的范围内,因此剥离片材10的剥离力也是良好的。此外,由于剥离剂层13包含用多位点催化剂聚合的树脂,因此剥离剂的分子量和组成是不均匀的,由此当加热剥离剂层13时防止了其物理性能的改变。据此,在剥离片材转换为辊状形式之后,即使将其在相对高的环境温度条件下长时间存储,表面粗糙度和剥离力的改变仍降低,由此在防止粘连的同时保持了良好的剥离性能。
此外,在本具体实施方案中,剥离片材10和压敏粘合剂制品20基本上不包含硅氧烷化合物,因为剥离剂层13由聚烯烃树脂组合物形成,压敏粘合剂层22也由非硅氧烷树脂形成。
(实施例)
接着将参照如下的实施例更详细地说明本发明,但是本发明并不受限于如下实施例的构成。
[实施例1]
密度为0.918克/立方厘米的低密度聚乙烯(商标名称:Novatec LDLC605Y,由Japan Polyethylene Corp.制造)被挤出并涂布在通用的厚度为38微米的PET薄膜(商标名称:Lumirror S-28,由Toray IndustriesInc.制造)上从而形成厚度为15微米的底涂层。接着,通过混合70重量份密度为0.895克/立方厘米且用多位点催化剂聚合的乙烯-1-丁烯共聚物(商标名称:Excellen EUL731由Sumitomo Chemical Co.,Ltd制造;Mw/Mn=3.9)和30重量份密度为0.918克/立方厘米的低密度聚乙烯(商标名称:Novatec LD LC604,由Japan Polyethylene Corp.制造;Mw/Mn=8.0)而获得的聚烯烃树脂组合物被挤出并在280℃的温度下涂布在底涂层上从而形成厚度为20微米的剥离剂层。然后,用具有压花表面的冷却的层压辊压印剥离剂层,如此当剥离剂层被冷却时,在剥离剂层的表面上形成精细的粗糙,从而获得实施例1的剥离片材。此外,上述聚烯烃树脂组合物的MFR为8.2克/10分钟。
[实施例2]
实施例2的步骤类似于实施例1,不同的是使用通过混合70重量份密度为0.900克/立方厘米且用多位点催化剂聚合的乙烯-1-丁烯共聚物(商标名称:Excellen VL200,由Sumitomo Chemical Co.,Ltd制造;Mw/Mn=3.9)和30重量份低密度聚乙烯(商标名称:Novatec LDLC604;Mw/Mn=8.0)而得到的混合物树脂作为聚烯烃树脂组合物以形成剥离剂层。此外,聚烯烃树脂组合物的MFR为3.0克/10分钟。
[比较实施例1]
比较实施例1的步骤类似于实施例1,不同的是使用通过混合50重量份密度为0.870克/立方厘米且用单位点催化剂聚合的乙烯-丙烯共聚物(商标名称:Tafmer P0280G,由Mitsui Chemical Inc.制造;Mw/Mn=2.0)和50重量份密度为0.916克/立方厘米的低密度聚乙烯(商标名称:Novatec LD LC800,由Japan Polyethylene Corp.制造)而得到的混合物树脂作为聚烯烃树脂组合物以形成剥离剂层。此外,聚烯烃树脂组合物的MFR为5.9克/10分钟。
[比较实施例2]
比较实施例2的步骤类似于实施例1,不同的是使用密度为0.919克/立方厘米的低密度聚乙烯(商标名称:Novatec LD LC605Y,由JapanPolyethylene Corp.制造)作为聚烯烃树脂组合物以形成剥离剂层。此外,聚烯烃树脂组合物的MFR为7.4克/10分钟。
[对物理性能的评价]
通过上述测量方法测量每个实施例和比较实施例中在剥离片材中的剥离剂层的表面粗糙度Ra1和在23℃下的平均弹性模量。
此外,利用试验涂布机将丙烯酸类压敏粘合剂(商标名称:PL shin,由Lintec Corp.制造)涂布在厚度为50微米的PET薄膜上使其厚度为23微米,然后在120℃下干燥1分钟,从而形成压敏粘合剂层以获得压敏粘合剂片材。将每个实施例和比较实施例中的剥离片材粘合至压敏粘合剂片材,使得剥离剂层与压敏粘合剂层接触,从而制得压敏粘合剂制品,然后测量压敏粘合剂制品中剥离片材的剥离力。各物理性能的测量值如图1和2中所示。
[在热加速后对物理性能的评价]
绕着直径为92毫米的中心轴卷绕宽度为340毫米、长度为1000毫米的剥离片材以制得辊状形式的剥离片材。采用热加速方式通过使辊状形式的剥离片材在40℃的恒温室中静置30天来处理辊状形式的剥离片材。在已用热加速处理的剥离片材从辊展开至片状形式之后,测量热加速后的表面粗糙度Ra2。此外,在热加速后的剥离片材从辊展开来之后,将压敏粘合剂片材粘合至已经展开的片状剥离片材,从而以在上述评价物理性能中所述的类似方式制备压敏粘合剂制品。然后,测量压敏粘合剂制品中在热加速后的剥离片材的剥离力。热加速后的表面粗糙度Ra2和剥离力、表面粗糙度比Ra2/Ra1以及通过如下公式计算的剥离力变化率示于表1和2中。
剥离力变化率=[(在热加速之前的剥离力-在热加速之后的剥离力)/在热加速之前的剥离力]×100(%)
[对防粘连性能的评价]
通过自辊展开已经用热加速处理的剥离片材来评价防粘连性能。在表1中,将剥离片材由于小的粘连能够被顺利展开的情况记录为“○”。另一方面,将剥离片材由于大的粘连难以展开的情况记录为“×”。
表1
表2
如表1和2中所示,在实施例1和2中,剥离力的合适值可以通过将表面粗糙度Ra1限定为100至700纳米、将在23℃下的平均弹性模量限定为0.1至0.3GPa,并通过使用用预定的多位点催化剂聚合的树脂加以确定。此外,由于诸如表面粗糙度等的物理性能的改变即使当进行热加速时也能够得以减缓,可保持良好的防粘结性能和剥离力。
比较而言,在比较实施例1中,可将表面粗糙度Ra1和在23℃下的平均弹性模量限定为合适的值,但是,由于组合物不包含密度为0.800至0.905克/立方厘米且用多位点催化剂聚合的树脂,因此由于诸如表面粗糙度等的物理性能的改变,当进行热加速时会发生粘连。此外,应该理解的是,在热加速后剥离力下降的事实表明,在长期存储过程中极好的剥离性能不会得到保持。另一方面,在比较实施例2中,尽管可以通过限定在23℃下的平均弹性模量为较高值来使得防粘连性能良好,但由于过高的剥离力而不能获得具有极好剥离性能的剥离片材。
Claims (8)
1.一种剥离片材,其包括:
剥离剂层,所述剥离剂层由包含密度为0.800至0.905克/立方厘米且用多位点催化剂聚合的聚烯烃热塑性树脂的聚烯烃树脂组合物形成,所述剥离剂层在自其表面50至1000纳米深度处采用纳米压痕法在23℃下测量的剥离剂层的平均弹性模量为0.1至0.3GPa,在表面上形成粗糙以使其表面粗糙度Ra1为100至700纳米。
2.根据权利要求1所述的剥离片材,其中表面粗糙度比Ra2/Ra1为0.9至1.1(其中“Ra2”为将剥离片材在40℃的环境条件下静置30天后所述剥离剂层的表面粗糙度)。
3.根据权利要求1所述的剥离片材,其中所述聚烯烃树脂组合物的熔体流动速率为1至20克/10分钟。
4.根据权利要求1所述的剥离片材,其中所述聚烯烃热塑性树脂包含至少一种选自聚乙烯、聚丙烯、聚丁烯、聚(4-甲基-1-戊烯)或乙烯与碳数为3至10的α-烯烃的共聚物的聚烯烃树脂。
5.根据权利要求1所述的剥离片材,其中所述剥离剂层经底涂层层压在基底上。
6.根据权利要求1所述的剥离片材,其基本上不包含硅氧烷化合物。
7.一种压敏粘合剂制品,其包括:
基底;
层压在所述基底上的剥离剂层;以及
层压在所述剥离剂层上并与所述剥离剂层接触的压敏粘合剂层,所述剥离剂层由包含密度为0.800至0.905克/立方厘米且用多位点催化剂聚合的聚烯烃热塑性树脂的聚烯烃树脂组合物形成,所述剥离剂层在自其表面50至1000纳米深度处采用纳米压痕法在23℃下测量的剥离剂层的平均弹性模量为0.1至0.3GPa,在表面上形成粗糙以使其表面粗糙度Ra1为100至700纳米。
8.根据权利要求7所述的压敏粘合剂制品,其中所述压敏粘合剂层由丙烯酸类压敏粘合剂形成。
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PCT/JP2008/070257 WO2009060924A1 (ja) | 2007-11-08 | 2008-10-30 | 剥離シート及び粘着体 |
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- 2008-10-30 JP JP2009540092A patent/JP5284976B2/ja active Active
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- 2008-10-30 WO PCT/JP2008/070257 patent/WO2009060924A1/ja active Application Filing
- 2008-10-30 KR KR1020107010063A patent/KR101479477B1/ko active IP Right Grant
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CN108271381A (zh) * | 2016-03-04 | 2018-07-10 | 琳得科株式会社 | 半导体加工用片 |
CN108243616B (zh) * | 2016-03-04 | 2022-10-28 | 琳得科株式会社 | 半导体加工用片 |
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JP5284976B2 (ja) | 2013-09-11 |
WO2009060924A1 (ja) | 2009-05-14 |
KR101479477B1 (ko) | 2015-01-06 |
KR20100075614A (ko) | 2010-07-02 |
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JPWO2009060924A1 (ja) | 2011-03-24 |
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