CN107107307A - 研磨垫 - Google Patents

研磨垫 Download PDF

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Publication number
CN107107307A
CN107107307A CN201680006010.3A CN201680006010A CN107107307A CN 107107307 A CN107107307 A CN 107107307A CN 201680006010 A CN201680006010 A CN 201680006010A CN 107107307 A CN107107307 A CN 107107307A
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CN
China
Prior art keywords
polyurathamc
phase
grinding pad
ratio
glycol
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Granted
Application number
CN201680006010.3A
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English (en)
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CN107107307B (zh
Inventor
村上阳平
大嶋伸之
中野裕之
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Nitta DuPont Inc
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Nitta Haas Inc
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Publication of CN107107307A publication Critical patent/CN107107307A/zh
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • B24B37/11—Lapping tools
    • B24B37/20—Lapping pads for working plane surfaces
    • B24B37/24—Lapping pads for working plane surfaces characterised by the composition or properties of the pad materials
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/14—Manufacture of cellular products
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08G18/30—Low-molecular-weight compounds
    • C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
    • C08G18/3203—Polyhydroxy compounds
    • C08G18/3206—Polyhydroxy compounds aliphatic
    • C—CHEMISTRY; METALLURGY
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    • C08G18/3212—Polyhydroxy compounds containing cycloaliphatic groups
    • C—CHEMISTRY; METALLURGY
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Abstract

本发明是一种研磨垫，其由发泡聚氨酯形成，通过25℃下的脉冲NMR测定求出的所述发泡聚氨酯中的S相的含有比例大于70％。

Description

研磨垫
相关申请的相互参照
本申请主张日本特愿2015-068387号的优先权，通过引用并入本申请说明书的记载。
技术领域
本发明涉及一种研磨垫。
背景技术
为了对用作半导体基板的硅晶片等被研磨物进行研磨，广泛使用由发泡聚氨酯形成的研磨垫(例如，专利文献1)。
现有技术文献
专利文献
专利文献1：日本特开2015-6729号公报。
发明内容
发明要解决的问题
但是，对于以往的研磨垫而言，用研磨垫研磨被研磨物，则产生摩擦热，其结果是，由于该摩擦热使硬度变化。
因此，以往的研磨垫存在不能充分地研磨被研磨物的情况、损伤被研磨物的情况，存在不能稳定地研磨被研磨物的问题。
因此，本发明鉴于上述问题，其课题在于，提供一种由温度变化引起的硬度的变化小的研磨垫。
用于解决问题的方案
本发明是一种研磨垫，其由发泡聚氨酯形成，
通过25℃下的脉冲NMR测定求出的所述发泡聚氨酯中的S相的含有比例大于70％。
而且，本发明的研磨垫的一实施方式中，通过在60℃下的脉冲NMR测定求出的所述发泡聚氨酯中的S相的含有比例与通过25℃下的脉冲NMR测定求出的所述发泡聚氨酯中的S相的含有比例之比为80％以上。
具体实施方式
以下，对本发明的一实施方式进行说明。
本实施方式的研磨垫由发泡聚氨酯形成。
通过25℃下的脉冲NMR测定求出的所述发泡聚氨酯中的S相的含有比例大于70％，优选为80～100％，更优选为90～100％。
另外，在脉冲NMR测定中，将发泡聚氨酯分为自旋-自旋弛豫时间小于0.03ms的相(短相)(S相)、自旋-自旋弛豫时间为0.03ms以上且小于0.2ms的相(中间相)(M相)、自旋-自旋弛豫时间为0.2ms以上的相(长相)(L相)，分别求出各个相的含有比例。
自旋-自旋弛豫时间能够通过，例如，使用JEOL制造的“JNM-MU25”，实施采用固体回波(Solid Echo)法的测定而求出。
在脉冲NMR中，将施加了脉冲磁场后的经过时间设为t(ms)，将t＝0时的磁化设为M0，将时间t时的磁化设为M(t)，基于下述数学式求出自旋-自旋弛豫时间(T2)。
另外，下述数学式中的“W”表示威布尔系数(Weibull Modulus)。
[数学式1]
并且，将测定对象分解成n个成分时，关于第i个(i＜n)的成分，将t＝0时的该i成分的磁化设为M0i，将i成分的威布尔系数设为Wi，基于下述数学式求出i成分的自旋-自旋弛豫时间(T2i)、以及i成分的比例Fi。
例如，威布尔系数Wi能够使用WS＝2、WM＝1、WL＝1。
关于这种弛豫时间的求出方法，在S.Yamasakiet al Polymer 48 4793(2007)等中有所公开。
[数学式2]
[数学式3]
另外，关于S相、M相、以及L相的含有比例，例如，在脉冲NMR测定中，观测到主要结晶相为S相，主要非晶相为L相。而且，在脉冲NMR测定中，观测到主要硬链段部分为S相，主要软链段部分为L相。
而且，作为发泡聚氨酯，已知“结晶相的比例”、“硬链段部分的比例”为各种比例的发泡聚氨酯。另外，通过增加氨基甲酸酯键、脲键，能够提高“硬链段部分的比例”。关于发泡聚氨酯的材料，在下文进行描述，例如，能够在使异氰酸酯与多元醇键合时，通过增加短链二醇(例如，二乙二醇(DEG)、分子量小的聚乙二醇(PEG)等)的使用量增加氨基甲酸酯键。此外，例如，在使异氰酸酯末端预聚物与4,4’-亚甲基双(2-氯苯胺)(MOCA)键合时，通过增加MOCA的使用量，或者降低用于反应的加热温度，能够增加脲键。而且，例如，通过抑制化学交联，硬链段彼此变得容易接近，能够提高“结晶化相的比例”。
因此，通过提高结晶相的比例，提高硬链段部分的比例，能够提高S相的含有比例。
通过在60℃下的脉冲NMR测定求出的所述发泡聚氨酯中的S相的含有比例与通过25℃下的脉冲NMR测定求出的所述发泡聚氨酯中的S相的含有比例之比优选为80％，更优选为90～100％。
所述发泡聚氨酯能够通过对含有异氰酸酯基的含异氰酸酯基化合物、含有活性氢的含活性氢有机化合物、以及发泡剂进行混合加热而得到。
作为所述含异氰酸酯基化合物，能够使用，例如，芳香族二异氰酸酯、脂肪族二异氰酸酯、脂环族二异氰酸酯等。另外，作为这些含异氰酸酯基化合物，能够使用单独物或者组合多种的物质。
作为所述芳香族二异氰酸酯，能够使用：通过在非活性溶剂中使缩合苯胺与甲醛而得到的胺混合物与光气反应等而得到的粗二苯甲烷二异氰酸酯(粗MDI)、对该粗MDI进行纯化而得到的二苯甲烷二异氰酸酯(纯MDI)、聚亚甲基聚亚苯基聚异氰酸酯(聚合MDI)、以及它们的改性物等，而且，能够使用甲苯二异氰酸酯(TDI)、1，5-萘二异氰酸酯、苯二亚甲基二异氰酸酯、1，3-苯二异氰酸酯、1，4-苯二异氰酸酯等。另外，这些芳香族二异氰酸酯能够使用单独物或者组合多种的物质。
作为二苯甲烷二异氰酸酯的改性物，例如，可举例碳二亚胺改性物、氨基甲酸酯改性物、脲基甲酸酯改性物、脲改性物、缩二脲改性物、异氰尿酸酯改性物、噁唑烷酮改性物等。作为这种改性物，具体而言，例如，可举例碳二亚胺改性二苯甲烷二异氰酸酯(碳二亚胺改性MDI)。
作为所述脂肪族二异氰酸酯，例如，即使用二异氰酸乙二酯、2，2，4-三甲基六亚甲基二异氰酸酯、1，6-六亚甲基二异氰酸酯等。
作为所述脂环族二异氰酸酯，例如，可使用1，4-环己烷二异氰酸酯、4，4’-二环己基甲烷二异氰酸酯、异佛尔酮二异氰酸酯、降冰片烷二异氰酸酯、亚甲基双(4，1-亚环己基)＝二异氰酸酯等。
作为所述含异氰酸酯基化合物，由于其蒸气压较低，难以挥发，从容易控制操作环境的方面出发，优选二苯甲烷二异氰酸酯(纯MDI)、聚合MDI、或其改性物。而且，从粘度较低，容易处理的方面出发，优选碳二亚胺改性MDI、聚合MDI、或它们与MDI的混合物。
所述含活性氢有机化合物是在分子内具有能够与异氰酸酯基反应的活性氢基的有机化合物。作为该活性氢基，具体而言，可举例羟基、伯氨基、仲氨基、硫醇基等官能团，所述含活性氢有机化合物可以在分子中仅具有一种该官能团，也可以在分子中具有多种该官能团。
作为所述含活性氢有机化合物，例如，能够使用在分子中具有多个羟基的多元醇化合物、在分子内具有多个伯氨基或仲氨基的聚胺化合物等。
作为所述多元醇化合物，能够举例分子量为400以下的多元醇、分子量大于400的多元醇预聚物等。
作为分子量为400以下的多元醇，例如，可举例乙二醇、丙二醇、1，3-丙二醇、1，3-丁二醇、1，5-戊二醇、3-甲基-1，5-戊二醇、1，6-己二醇、二乙二醇、三乙二醇、四乙二醇、二丙二醇、三丙二醇、分子量为400以下的聚乙二醇、1，8-辛二醇、1，9-壬二醇等直链脂肪族二醇，可举例新戊二醇、3-甲基-1，5-戊二醇、2-甲基-1，3-丙二醇、2-丁基-2-乙基-1，3-丙二醇、2-甲基-1，8-辛二醇等支化脂肪族二醇，可举例1，4-环己烷二醇、1，4-环己烷二甲醇、氢化双酚A等的脂环族二醇，可举例甘油、三羟甲基丙烷、三羟丁基丙烷、季戊四醇、山梨糖醇等多官能多元醇等。
作为分子量大于400的多元醇预聚物，可举例聚醚多元醇、聚酯多元醇、聚酯聚碳酸酯多元醇以及聚碳酸酯多元醇等。另外，作为多元醇预聚物，还可举例在分子中具有三个以上的羟基的多官能多元醇预聚物。
具体而言，作为所述聚醚多元醇，可举例聚亚甲基二醇(PTMG)、聚丙二醇(PPG)、聚乙二醇(PEG)、环氧乙烷加成聚丙烯多元醇等。
作为所述聚酯多元醇，可举例聚己二酸丁二酯、聚六亚甲基己二酸酯以及聚己内酯多元醇等。
作为所述聚酯聚碳酸酯多元醇，可举例聚己内酯多元醇等聚酯二醇与碳酸亚烷基酯的反应生成物、将使碳酸亚乙酯与多元醇反应而得的反应混合物进一步与有机二羧酸反应而得的反应生成物等。
作为所述聚碳酸酯多元醇，可举例1，3-丙二醇、1，4-丁二醇、1，6-己二醇、二乙二醇、聚乙二醇、聚丙二醇、或聚四亚甲基二醇等二醇与光气、碳酸二烯丙酯(例如碳酸二苯酯)或环式碳酸酯(例如碳酸丙二酯)的反应生成物等。
所述多元醇化合物可以单独使用或者组合两种以上使用。
作为所述多元醇，从反应时的强度更容易升高，制造的包含发泡聚氨酯的研磨垫的刚性更容易升高，比较廉价的方面出发，优选乙二醇、二乙二醇。
作为所述多元醇预聚物，从容易得到具有弹性的发泡聚氨酯的方面出发，优选数均分子量为800～8000的多元醇预聚物，具体而言，优选聚四亚甲基二醇(PTMG)、环氧乙烷加成聚丙烯多元醇。
作为所述聚胺化合物，可举例4，4’-亚甲基双(邻氯苯胺)(MOCA)、2，6-二氯-对苯二胺、4，4’-亚甲基双(2，3-二氯苯胺)、3，5-双(甲硫基)-2，4-甲苯二胺、3，5-双(甲硫基)-2，6-甲苯二胺、3，5-二乙基甲苯-2，4-二胺、3，5-二乙基甲苯-2，6-二胺、三乙二醇-二-对氨基苯甲酸酯、1，2-双(2-氨基苯硫基)乙烷以及4，4’-二胺基-3，3’-二乙基-5，5’-二甲基二苯甲烷等。
作为所述发泡剂，在所述发泡聚氨酯成型时，产生气体，成为气泡，只要是在所述发泡聚氨酯中形成气泡的发泡剂，就没有特别的限定，例如，能够单独地或组合使用通过加热分解产生气体的有机化学发泡剂、沸点为-5～70℃的低沸点烃、卤化烃、水、液化二氧化碳等。
作为所述有机化学发泡剂，例如，可举例偶氮系化合物(偶氮二甲酰胺、偶氮二异丁氰、重氮氨基苯、偶氮二羧酸钡等)、亚硝基化合物(N,N’-二亚硝基五亚甲基四胺、N,N’-二亚硝基-N,N’-二甲基对苯二甲酰胺等)、磺酰氨基脲化合物[p,p’-氧基双(苯磺酰氨基脲)、对甲苯磺酰氨基脲等]等。
作为所述低沸点烃，例如，可举例丁烷、戊烷、环戊烷、以及它们的混合物等。
作为所述卤化烃，可举例二氯甲烷、HFC(氢氟碳类)等。
本实施方式的研磨垫由于由上所述地构成，所以具有以下优点。
本发明人等进行了致力研究，结果发现：由发泡聚氨酯形成的、通过25℃下的脉冲NMR测定求出的所述发泡聚氨酯中的S相的含有比例在规定范围内的研磨垫由温度变化引起的硬度的变化减小，从而想到本实施方式。
即，本实施方式的研磨垫是由发泡聚氨酯形成的、通过25℃下的脉冲NMR测定求出的所述发泡聚氨酯中的S相的含有比例大于70％的研磨垫。
本实施方式的研磨垫通过具有所述构成，成为由温度变化引起的硬度的变化小的研磨垫。
对于本实施方式的研磨垫而言，如果通过25℃下的脉冲NMR测定求出的所述发泡聚氨酯中的S相的含有比例大于70％，则认为由温度变化引起的硬度的变化减小的原因是以下的理由。
所述发泡聚氨酯的所述S相的含有比例大于70％。因此，认为所述发泡聚氨酯的硬链段结晶化的部分变多，硬链段结晶化的部分密集存在。另一方面，认为软链段存在于硬链段结晶化的部分之间，或者连接存在于硬链段结晶化的部分的端部。
如此地，认为所述发泡聚氨酯由于硬链段结晶化的部分密集，因此，硬链段间的分子间力升高，即使加热，硬链段彼此变得难以分离，其结果是，硬度变得难以下降。
而且，认为即使在存在硬链段结晶化的部分的密集度小的位置的情况下，该密集度小的位置与密集度高的位置相比，如果加热，则硬链段彼此能够具有容易分离的性质，但是通过周围的密集度的高的位置抑制活动，其结果是，硬度难以下降。
进一步地，认为所述发泡聚氨酯中即使存在少量软链段，由于软链段短，因此即使加热，软链段想要进行活动，但由于硬链段结晶化的部分使得活动被抑制，其结果是，硬度变得难以降低。
另外，对于本实施方式的研磨垫而言，通过在60℃下的脉冲NMR测定求出的所述发泡聚氨酯中的S相的含有比例与通过25℃下的脉冲NMR测定求出的所述发泡聚氨酯中的S相的含有比例之比优选为80％以上。
另外，本发明的研磨垫不限定于上述实施方式。另外，本发明的研磨垫不限定于上述作用效果。本发明的研磨垫在不脱离本发明的主旨的范围内能够进行各种变更。
实施例
接下来，举出试验例对本发明进行更具体的说明。
准备试验例1～6的发泡聚氨酯。
然后，通过脉冲NMR对各个发泡聚氨酯进行测定。脉冲NMR测定的条件如下所述。
并且，测定各个发泡聚氨酯的储能弹性模量。储能弹性模量根据JIS K7244-4:1999“塑料-动态机械特性的试验方法-第4部：拉伸振动-非共振法”进行测定。储能弹性模量的测定条件如下所述。
＜脉冲NMR测定的条件＞
测定装置：JEOL制造、JNM-MU25
测定方法：固体回波(Solid Echo)法
脉冲宽度：90°脉冲，2.0μs
重复时间：4sec
累计次数：8次
测定温度：室温(RT)(25℃)、60℃、80℃、100℃
＜储能弹性模量的测定条件＞
测定装置：SII纳米技术(Nanotechnology)制造，动态粘弹性测定装置DMS6100
频率：1Hz
初期荷重：300mN
测定模式：拉伸-正弦波控制模式
温度：10～130℃
升温：5℃/min
在表1中表示在各温度下的S相的含有比例和各温度下的S相的含有比例与25℃下的S相的含有比例之比(在表1中，表示为“各温度/RT”)。
并且，在表2中表示各温度下的储能弹性模量(E’)和各温度下的E’与25℃下的E’之比(在表2中，表示为“各温度/RT”)。
[表1]
[表2]
如表1、2所示，通过25℃下的脉冲NMR测定求出的S相的含有比例大于70％的试验例3～6发泡聚氨酯与试验例1的发泡聚氨酯相比，各温度下的E’与25℃下的E’之比表现出高的值。
即，可知根据本申请发明，能够提供由温度变化引起的硬度的变化小的研磨垫。

Claims (2)

1.一种研磨垫，其由发泡聚氨酯形成，
通过25℃下的脉冲NMR测定求出的所述发泡聚氨酯中的S相的含有比例大于70％。
2.根据权利要求1所述的研磨垫，其中，通过在60℃下的脉冲NMR测定求出的所述发泡聚氨酯中的S相的含有比例与通过25℃下的脉冲NMR测定求出的所述发泡聚氨酯中的S相的含有比例之比为80％以上。
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