CN106457509A - 研磨垫及其制造方法 - Google Patents
研磨垫及其制造方法 Download PDFInfo
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- CN106457509A CN106457509A CN201580013166.XA CN201580013166A CN106457509A CN 106457509 A CN106457509 A CN 106457509A CN 201580013166 A CN201580013166 A CN 201580013166A CN 106457509 A CN106457509 A CN 106457509A
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- alkoxysilyl
- grinding pad
- polyurethane resin
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Abstract
本发明以提供研磨速度快且平坦化特性优异的研磨垫及其制造方法作为目的。一种研磨垫,它是具有由聚氨酯树脂发泡体形成的研磨层的研磨垫,其中,作为所述聚氨酯树脂发泡体的形成材料的聚氨酯树脂在侧链上具有下式(1)所示的烷氧基甲硅烷基,(式中,X为OR1或OH,R1分别独立地表示碳原子数1~4的烷基)。
Description
技术领域
本发明涉及能稳定且以高研磨效率进行透镜、反射镜等的光学材料或者硅晶片、硬盘用的玻璃基板、铝基板以及一般的金属研磨加工等的要求高度的表面平坦性的材料的平坦化加工的研磨垫。本发明的研磨垫特别适用于对硅晶片及其上面形成有氧化物层、金属层等的器件,在层叠和形成这些氧化物层和金属层之前进行平坦化的工序。
背景技术
作为要求高度的表面平坦性的材料的代表,列举有制造半导体集成电路(IC、LSI)的称为硅晶片的单晶硅的圆盘。对于硅晶片,为了在IC、LSI等的制造工序中,形成在电路形成中使用的各种薄膜的可信赖的半导体接合,在层叠和形成氧化物层和金属层的各个工序中,要求对其表面进行高精度且平坦的加工。在这样的研磨加工工序中,通常将研磨垫固定在被称为台板的能旋转的支承圆盘上,半导体晶片等的加工物被固定在研磨垫上,然后通过双方运动,在台板和研磨垫之间产生相对速度,再连续供给含有研磨粒的研磨浆液到研磨垫上,实施研磨操作。
作为研磨垫的研磨特性,要求优异的研磨对象物的平坦性(可平面性)和表面内的均匀性,研磨速度快的特性。对于研磨对象物的平坦性和表面内均匀性,可通过将研磨层高弹性率化以得到一定程度的改善。对于研磨速度,通过将研磨层形成发泡体,增加浆液的保持量,或者将研磨层形成为亲水性以提高浆液的保持能力等进行提升。
例如,在专利文献1中,为了提高研磨垫对水的浸润性,提出了一种研磨垫用组合物,该研磨垫用组合物含有(A)交联弹性体,(B)具有选自羧基、氨基、羟基、环氧基、磺酸基以及磷酸基中的至少一种的官能团的物质,和水溶性物质,并且所述(A)交联弹性体是使1,2-聚丁二烯交联而成的聚合体。
在专利文献2中,为了将浆液浸入研磨垫中变得容易,提出了如下的研磨垫:它是由含有具有亲水性基团的化合物共聚而成的聚氨酯树脂、且含有亲水剂的聚氨酯组合物形成的研磨垫,该亲水剂为选自2,4,7,9-四甲基-5-二烯-4,7-二醇-二聚氧乙烯醚、以及2,4,7,9-四甲基-5-二烯-4,7-二醇中的至少一种,该具有亲水性基团的化合物为环氧乙烷单体。
在专利文献3中,为了获得平坦性、表面内均匀性、研磨速度都良好,研磨速度变化少且寿命特性优异的研磨垫,提出了如下方案:
作为聚氨酯树脂发泡体的原料成分之一,使用以亲水性高分子量多元醇成分和异氰酸酯成分作为原料成分而形成的亲水性异氰酸酯末端预聚物(B),所述亲水性高分子量多元醇成分具有25重量%以上的环氧乙烷单元(-CH2CH2O-)且数均分子量为500以上。
在专利文献4中,为了提高研磨层的亲水性,提出了如下的研磨层:
即,该研磨层含有部分酰化多糖类成分,该部分酰化多糖类成分可溶解于能将构成研磨层的树脂溶解的有机溶剂中,但难溶或不溶于水。
但是,将研磨层形成亲水性的话,虽然研磨速度增大了,但是存在研磨对象物的平坦性变差的问题。
现有技术文献
专利文献
专利文献1:日本专利第3826702号说明书;
专利文献2:日本专利第3851135号说明书;
专利文献3:日本专利第4189963号说明书;
专利文献4:日本专利第5189440号说明书。
发明内容
发明所要解决的技术问题
本发明以提供研磨速度快且平坦化特性优异的研磨垫及其制造方法作为目的。
解决技术问题所采用的技术方案
本发明人对解决前述课题进行了反复研究,结果发现通过下述研磨垫就能够解决前述课题,从而完成了本发明。
本发明涉及一种研磨垫,它是具有由聚氨酯树脂发泡体形成的研磨层的研磨垫,其中,作为所述聚氨酯树脂发泡体的形成材料的聚氨酯树脂在侧链上具有下式(1)所示的烷氧基甲硅烷基:
(式中,X为OR1或OH,R1分别独立地表示碳原子数1~4的烷基)。
如上所述,本发明具有在聚氨酯树脂的侧链上导入前述的烷氧基甲硅烷基的特征。研磨层表面所存在的前述的烷氧基甲硅烷基在研磨中被浆液中的水水解,在研磨层表面上生成硅烷醇基。该硅烷醇基具有亲水性,所以研磨层表面的亲水性提高。其结果是能提高浆液的保持能力,且能提高研磨速度。
另一方面,烷氧基甲硅烷基因被导入聚氨酯树脂的侧链上,所以聚氨酯树脂难以被浆液膨胀。研磨层内部所存在的前述烷氧基甲硅烷基因难以与浆液中的水接触,所以难以被水解。因此能仅将研磨层表面亲水化,抑制研磨层整体的硬度的下降。其结果是研磨垫的平坦化特性难以降低。
所述聚氨酯树脂较好是含有作为预聚物原料组合物的反应物的包含烷氧基甲硅烷基的异氰酸酯末端预聚物和链增长剂的聚氨酯原料组合物的反应固化体,所述预聚物原料组合物的反应物含有异氰酸酯成分和多元醇成分;所述异氰酸酯成分含有下式(2)所示的包含烷氧基甲硅烷基的异氰酸酯;所述多元醇成分含有3官能以上的多元醇:
(式中,X为OR1或OH,R1分别独立地表示碳原子数1~4的烷基,R2表示碳原子数1~6的亚烷基)。
所述包含烷氧基甲硅烷基的异氰酸酯较好为3-异氰酸酯基丙基三乙氧基硅烷。
所述包含烷氧基甲硅烷基的异氰酸酯的含量较好是聚氨酯原料组合物的1~10重量%。因烷氧基甲硅烷基被导入聚氨酯树脂的侧链,所以通过导入少量的烷氧基甲硅烷基而呈现亲水性。包含烷氧基甲硅烷基的异氰酸酯的含量不到1重量%的情况下,研磨层表面的亲水化难以产生;如果超过10重量%时,存在难以制作研磨特性优异的研磨层的倾向。
另外,本发明涉及一种研磨垫的制造方法,该制造方法是包括将含有异氰酸酯末端预聚物的第一成分和含有链增长剂的第二成分进行混合、固化,制得聚氨酯树脂发泡体的工序的制造方法,其特征在于,所述工序是如下工序:
以相对于第一成分和第二成分合计重量为0.05~10重量%的条件将聚硅氧烷类表面活性剂添加到第一成分中,再将所述第一成分与非反应性气体搅拌,调制使所述非反应性气体作为气泡分散的气泡分散液后,在所述气泡分散液中混合含有链增长剂的第二成分,固化,制得聚氨酯树脂发泡体的工序;
所述第一成分含有作为预聚物原料组合物的反应物的包含烷氧基甲硅烷基的异氰酸酯末端预聚物;所述预聚物原料组合物的反应物含有异氰酸酯成分和多元醇成分;所述异氰酸酯成分含有下式(2)所示的包含烷氧基甲硅烷基的异氰酸酯;所述多元醇成分含有3官能以上的多元醇:
(式中,X为OR1或OH,R1分别独立地表示碳原子数1~4的烷基,R2表示碳原子数1~6的亚烷基)。
所述包含烷氧基甲硅烷基的异氰酸酯较好为3-异氰酸酯基丙基三乙氧基硅烷。
所述包含烷氧基甲硅烷基的异氰酸酯的含量较好是所述第一成分和所述第二成分的合计重量的1~10重量%。
本发明涉及一种半导体器件的制造方法,其特征在于,包含使用前述研磨垫研磨半导体晶片的表面的工序。
发明效果
本发明的研磨垫是研磨速度快且平坦化特性优异的研磨垫。另外,本发明的研磨垫因在研磨操作时通过浆液将研磨层表面变化为亲水性,所以浆液中的研磨粒子的凝集变难,能有效抑制在研磨对象物上产生划痕。
附图说明
图1是显示CMP研磨中使用的研磨装置一例的示意结构图。
具体实施方式
本发明的研磨垫可以仅为由聚氨酯树脂发泡体构成的研磨层,也可以是研磨层和其他层(例如缓冲层等)的层叠体。
作为聚氨酯树脂发泡体的形成材料的聚氨酯树脂在侧链上具有下式(1)所示的烷氧基甲硅烷基。X较好为OR1,R1较好为甲基或者乙基。
(式中,X为OR1或OH,R1分别独立地表示碳原子数1~4的烷基)。
作为聚氨酯树脂的原料,使用异氰酸酯成分、多元醇成分(高分子量多元醇、低分子量多元醇)和链增长剂的同时,还使用为在聚氨酯树脂的侧链上导入上式(1)所示的烷氧基甲硅烷基的包含烷氧基甲硅烷基的化合物。对于在聚氨酯树脂的侧链上导入烷氧基甲硅烷基的方法无特别限定,例如有如下的1)~3)等方法:
1)、使3官能以上的多元醇成分和包含烷氧基甲硅烷基的异氰酸酯反应的方法;
2)、使3官能以上的异氰酸酯成分和包含烷氧基甲硅烷基的醇或包含烷氧基甲硅烷基的胺反应的方法;
3)、使包含烷氧基甲硅烷基的异氰酸酯和聚氨酯树脂反应的方法(脲基甲酸酯反应或者缩二脲反应)。
在本发明中,聚氨酯树脂较好是含有作为预聚物原料组合物的反应物的包含烷氧基甲硅烷基的异氰酸酯末端预聚物和链增长剂的聚氨酯原料组合物的反应固化体,所述预聚物原料组合物的反应物含有异氰酸酯成分和多元醇成分;所述异氰酸酯成分含有下式(2)所示的包含烷氧基甲硅烷基的异氰酸酯;所述多元醇成分含有3官能以上的多元醇:
(式中,X为OR1或OH,R1分别独立地表示碳原子数1~4的烷基,R2表示碳原子数1~6的亚烷基)。
作为上式(2)所示的包含烷氧基甲硅烷基的异氰酸酯,较好为3-异氰酸酯基丙基三乙氧基硅烷。
作为前述包含烷氧基甲硅烷基的异氰酸酯以外的异氰酸酯成分,可使用聚氨酯领域中公知的化合物,无特别限定。例如2,4-甲苯二异氰酸酯、2,6-甲苯二异氰酸酯、2,2’-二苯基甲烷二异氰酸酯、2,4’-二苯基甲烷二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯、1,5-萘二异氰酸酯、p-亚苯基二异氰酸酯、m-亚苯基二异氰酸酯、p-二甲苯二异氰酸酯、m-二甲苯二异氰酸酯等的芳香族二异氰酸酯;乙烯二异氰酸酯、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的脂肪族二异氰酸酯;1,4-环己烷二异氰酸酯、4,4’-二环己甲烷二异氰酸酯、异佛尔酮二异氰酸酯、降冰片烷二异氰酸酯等的脂环式二异氰酸酯等。这些可单独使用,也可2种以上合用。
作为前述3官能以上的多元醇(具有3个以上的羟基的多元醇),例如可为聚己内酯三醇等的官能团数为3的高分子量的多元醇、聚己内酯四醇等的官能团数为4的高分子量的多元醇、三羟甲基丙烷、甘油、双甘油、1,2,6-己三醇、三乙醇胺、季戊四醇、四羟甲基环己烷、甲基葡糖苷以及这些多元醇的环氧烷(EO、PO等)的加成物等。这些可单独使用,也可2种以上合用。其中,较好使用聚己内酯三醇。
作为前述3官能以上的多元醇以外的多元醇成分,可使用聚氨酯技术领域通常使用的高分子量多元醇,例如,聚四亚甲基醚二醇、聚乙二醇等为代表的聚醚多元醇;聚己二酸亚丁酯为代表的聚酯多元醇、聚己内酯多元醇、聚己内酯之类的聚酯二醇和亚烷基碳酸酯的反应物等例示的聚酯聚碳酸酯多元醇、使碳酸亚乙酯和多元醇进行反应,之后使有机二羧酸和所制得的反应混合物反应所得的聚酯聚碳酸酯多元醇、由多羟基化合物和芳基碳酸酯的酯交换反应所得的聚碳酸酯多元醇等。这些可单独使用,也可2种以上合用。
对于高分子量多元醇的重均分子量没有特别限定,从所制得的聚氨酯树脂的弹性特性等的观点看,较好为500~3000。重均分子量不到500时,使用该多元醇所制得的聚氨酯树脂不具有足够的弹性特性,容易形成脆的聚合物,而由这样的聚氨酯树脂形成的研磨垫变得过硬,会成为研磨对象物表面的划痕发生的原因。再者,因容易磨耗,从研磨垫的寿命的观点看也不理想。相反,重均分子量超过3000的话,由使用该多元醇所制得的聚氨酯树脂形成的研磨垫变软,很难获得充分满足的平坦性。
除了上述高分子量多元醇以外,还可合用乙二醇、1,2-丙二醇、1,3-丙二醇、1,2-丁二醇、1,3-丁二醇、1,4-丁二醇、2,3-丁二醇、1,6-己二醇、新戊二醇、1,4-环己烷二甲醇、3-甲基-1,5-戊二醇、二乙二醇、三乙二醇、1,4-双(2-羟基乙氧基)苯、二乙醇胺以及N-甲基二乙醇胺等的低分子量多元醇。另外也可合用乙二胺、三亚乙基二胺、二苯基甲烷二胺、以及二亚乙基三胺等的低分子量多胺。另外也可合用单乙醇胺、2-(2-氨基乙基氨基)乙醇、以及单丙醇胺等的醇胺。这些低分子量的多元醇、低分子量多胺等可单独使用,也可2种以上合用。
前述的包含烷氧基甲硅烷基的异氰酸酯末端预聚物通过使用前述异氰酸酯成分和多元醇成分等,以异氰酸酯基(NCO)和活性氢(H*)的当量比(NCO/H*)为1.2~8、较好为1.5~3的范围进行加热反应制得。在不到1.2的情况下,制备预聚物时会存在容易凝胶化的趋势;相反,在超过8的情况下,会存在和链增长剂反应时发热变大,很难获得均一的研磨垫的趋势。
在使用前述的包含烷氧基甲硅烷基的异氰酸酯末端预聚物同时,也可合用不包含烷氧基甲硅烷基的异氰酸酯末端预聚物。
在前述异氰酸酯末端预聚物固化时使用链增长剂。链增长剂是具有至少2个以上的活性氢基的有机化合物。作为活性氢基,例如为羟基、伯氨基或者仲氨基、巯基(SH)等。具体为:4,4’-亚甲基双(o-氯苯胺)(MOCA)、2,6-二氯-p-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、丙二醇-二-p-氨基苯甲酸酯、1,2-双(2-氨基苯基硫代)乙烷、4,4’-二氨基-3,3’-二乙基-5,5’-二甲基二苯基甲烷、N,N’-二-sec-丁基-4,4’-二氨基二苯基甲烷、3,3’-二乙基-4,4’-二氨基二苯基甲烷、m-苯二甲胺、N,N’-二-sec-丁基-p-苯二胺、m-苯二胺、以及p-苯二甲胺等例示的多胺类、或者上述低分子量多元醇或者低分子量多胺。它们可使用1种,也可以2种以上混合使用。
所述包含烷氧基甲硅烷基的异氰酸酯的含量较好是聚氨酯原料组合物的1~10重量%,更好为1~8重量%,进一步更好为1~5重量%。
聚氨酯树脂发泡体可使用熔融法、溶液法等公知的氨基甲酸酯化技术制得,但是考虑到成本和作业环境等,较好以熔融法制造。
聚氨酯树脂发泡体的制造也可用预聚物法、一次成形法的任意一种。预聚物法的情况下,前述预聚物的异氰酸酯基的数量对链增长剂的活性氢基(羟基、氨基)的数量的比例较好为0.9~1.2。
作为聚氨酯树脂发泡体的制造方法,可使用添加中空球的方法、机械发泡法(包括机械浮渣法(日文:メカニカルフロス法))、化学发泡法等。
特好是使用作为聚烷基硅氧烷和聚醚的共聚物的聚硅氧烷类表面活性剂的机械发泡法。作为聚硅氧烷类表面活性剂,可例示SH-192以及L-5340(东丽道康宁有机硅公司(東レダウコーニングシリコーン社)制造)、B8443、B8465(戈德施密特公司(ゴールドシュミット社)制造)等作为适合的化合物。聚硅氧烷类表面活性剂较好以0.05~10重量%、更好为0.1~5重量%添加到聚氨酯原料组合物中。
根据需要,在聚氨酯原料组合物中还可添加抗氧化剂等的稳定剂、润滑剂、颜料、填充剂、防静电剂、其他的添加剂。
聚氨酯树脂发泡体可以是独立气泡类型,也可以是连续气泡类型,但是为了防止浆液向研磨层内部的侵入,防止研磨层内部存在的烷氧基甲硅烷基的水解,较好是独立气泡类型。
关于制造构成研磨垫(研磨层)的微细气泡类型的聚氨酯树脂发泡体的方法的例子,进行以下说明。该聚氨酯树脂发泡体的制造方法具有如下工序:
1)、制作包含烷氧基甲硅烷基的异氰酸酯末端预聚物的气泡分散液的发泡工序
在包含烷氧基甲硅烷基的异氰酸酯末端预聚物(第一成分)中添加聚硅氧烷类表面活性剂,在非反应性气体的存在下搅拌,使非反应性气体作为气泡分散,制得气泡分散液。在前述预聚物常温下为固体的情况下,将其预热到合适温度,熔融使用。
2)、链增长剂的混合工序
在上述气泡分散液中添加链增长剂(第二成分),混合,搅拌,形成发泡反应液。
3)、浇注工序
将上述的发泡反应液流入模具内。
4)、固化工序
将流入模具内的发泡反应液加热,使其反应固化。
作为形成气泡用的非反应性气体,较好使用不可燃性的气体,具体列举为氮气、氧气、二氧化碳、氦气和氩气等惰性气体或者这些惰性气体的混合气体。使用干燥除去水分的空气在成本上也是最为理想的。
作为将非反应性气体形成气泡状分散在含有聚硅氧烷类表面活性剂的第一成分内的搅拌装置,可使用公知的搅拌装置,对其无特别限定。具体例如为均质机、溶解分散机(日文:ディゾルバー)、双轴行星型搅拌机(日文:プラネタリーミキサー)等。对于搅拌装置的搅拌叶片的形状无特别限定,搅打器型的搅拌叶片的使用能获得微细气泡,较为理想。
发泡工序中的制作气泡分散液的搅拌和混合工序中的添加链增长剂进行混合的搅拌较好使用不同的搅拌装置。特别是混合工序中的搅拌可以不是形成气泡的搅拌,较好使用不卷入大气泡的搅拌装置。作为这样的搅拌装置,适合用行星型搅拌机。发泡工序和混合工序的搅拌装置也可使用相同的搅拌装置,根据需要进行对搅拌叶片的旋转速度调整等的搅拌条件的调整来使用比较合适。
在聚氨酯树脂发泡体的制造方法中,对发泡反应液流入模具直至不能流动为止进行反应而得的发泡体进行加热且后固化的操作具有提高发泡体的物理特性的效果,极好。也可采用将发泡反应液流入模具,马上将其放入加热炉内进行后固化的条件,因为即使在这样的条件下,热也不被马上传递给反应成分,所以气泡直径不会增大。固化反应在常压下进行能稳定气泡形状,所以较为理想。
在聚氨酯树脂发泡体中即使使用叔胺类等公知的能促进聚氨酯反应的催化剂也没关系。催化剂的种类和添加量可考虑混合工序后流入规定形状的模具的流动时间来进行选择。
聚氨酯树脂发泡体的制造可以是计量各个成分,将其投入容器内进行搅拌的间歇方式,也可以是将各个成分和非反应性气体连续供给至搅拌装置,进行搅拌,送出气泡分散液,制得成品的连续生产方式。
也可以是将作为聚氨酯树脂发泡体的原料的预聚物放入反应容器内,其后投入链增长剂,搅拌后,流入规定大小的注入模具内,制成块,用刨状或者带锯状的切片器将该块切割成片的方法,或者也可以在前述的注入模具的阶段,形成为薄片形状。
聚氨酯树脂发泡体的平均气泡直径较好为30~200μm。如果不在该范围的情况下,研磨后的研磨对象物的可平面性(平坦性)会降低。
聚氨酯树脂发泡体的硬度用ASKER-D硬度计测定较好为40~70度,在ASKER-D硬度不到40度的情况下,研磨对象物的可平面性下降;另外超过70度的话,虽然可平面性良好,但是研磨对象物的均匀性(均匀性)会降低。
聚氨酯树脂发泡体的比重较好为0.5~1.3,如果比重不到0.5的话,研磨层的表面强度降低,研磨对象物的可平面性会下降;如果大于1.3的话,研磨层表面的气泡数量减少,虽然可平面性良好,但是研磨速度会降低。
在本发明的研磨垫(研磨层)的与研磨对象物接触的研磨表面较好具有保持和更新浆液的表面形状。由发泡体形成的研磨层的研磨表面上具有多个开口,具有保持和更新浆液的功能,但是为了高效进行浆液的保持性和浆液的更新,以及防止因与研磨对象物的吸附而对研磨对象物产生的破坏,在研磨表面较好具有凹凸构造。凹凸构造只要是保持和更新浆液的形状即可,对其无特别限定,例如可为XY格子槽、同心圆状槽、贯通孔、不贯通的孔、棱柱、圆柱、螺旋状槽、偏心圆状槽、放射状槽、以及这些槽的组合。另外,这些凹凸构造通常为具有规则性的构造,但是为了形成具有浆液的保持和更新性好的构造,在一定范围内也可以变化槽的间距、槽宽度和槽深度等。
对于前述凹凸构造的制作方法无特别限定,例如可用如下方法:使用了规定大小的刨刀(日文:バイト)那样的工具进行机械切削的方法;通过将树脂注入具有规定表面形状的模具,使其固化的制造方法;利用具有规定表面形状的加压板将树脂加压的制造方法;使用光刻法进行制作的方法;使用印刷手法进行制作的方法;通过使用二氧化碳激光等的激光进行制作的方法等。
本发明的研磨垫也可以是将前述的研磨层和缓冲片进行粘合而成的研磨垫。
前述的缓冲片(缓冲层)是补充研磨层特性的缓冲片。为了兼顾此消彼长的关系的可平面性和均匀性的两者,缓冲片在CMP中是必要的构件。可平面性是指在研磨具有图案形成时所产生的微小凹凸的研磨对象物时的图案部的平坦性。而均匀性是指研磨对象物的整体的均匀性。通过研磨层的特性来改善可平面性,通过缓冲片的特性来改善均匀性。在本发明的研磨垫中,缓冲片较好使用比研磨层柔软的材料。
作为前述的缓冲片,例如可使用聚酯无纺布、尼龙无纺布、丙烯酸无纺布等的纤维无纺布或者含浸有聚氨酯的聚酯无纺布这样的含浸树脂的无纺布、聚氨酯泡沫、聚乙烯泡沫等的高分子树脂发泡体、丁二烯橡胶、异丙烯橡胶等的橡胶性树脂、感光性树脂等。
作为将研磨层和缓冲片进行粘合的手段,例如是以双面胶夹持研磨层和缓冲片,进行加压的方法。
前述的双面胶是具有在无纺布或者膜等的基材的两面设置有粘附层的通常结构的材料。如果考虑到防止浆液向缓冲片渗透等问题,较好是作为基材使用膜。另外,作为粘附层的组成,例如是橡胶类粘合剂或者丙烯酸类粘合剂等。如果考虑到金属离子的含量,丙烯酸类粘合剂的金属离子含量少,所以较为理想。另外,研磨层和缓冲片在组成上也可以不同,所以可使双面胶的各个粘附层的组成不同,也可将各个层的粘附力进行优化调整。
本发明的研磨垫也可以在与台板粘附的面上设置有双面胶。作为该双面胶,与前述相同,可使用基材的两面上设置有粘附层的具有通常结构的材料。作为基材例如可为无纺布或者膜等。如果考虑到研磨垫使用后从台板剥离,较好是作为基材使用膜。另外,作为粘附层的组成,例如可为橡胶类粘合剂或者丙烯酸类粘合剂等。如果考虑到金属离子的含量,丙烯酸类粘合剂的金属离子含量少,所以较为理想。
半导体器件经过使用前述研磨垫对半导体晶片的表面研磨的工序制得。半导体晶片一般是在硅晶片上层叠了布线金属和氧化膜而成的材料。对于半导体晶片的研磨方法和研磨装置无特别限定,例如可使用图1所示的、具有支承研磨垫(研磨层)1的研磨平台2、支承半导体晶片4的支承台(抛光头)5和用于向晶片均匀施压的填充材料、和研磨剂3的供给机构的研磨装置等进行。研磨垫1例如通过双面胶粘贴装配固定在研磨平台2上。研磨平台2和支承台5以使被分别支承的研磨垫1和半导体晶片4相向的的方式配置,各自都具有旋转轴6、7。在支承台5的侧面设置有将半导体晶片4挤压到研磨垫1上的加压机构。研磨时,使研磨平台2和支承台5一边旋转,一边将半导体晶片4挤压到研磨垫1上,一边供给浆液,一边进行研磨。对浆液的流量、研磨负重、研磨平台转速以及晶片转速无特别限定,可适当调整。
由此半导体晶片4的表面突出部分被除去,被研磨成平坦状,此后通过切割、粘合、封装等制得半导体器件。半导体器件被用于演算处理装置和存储器等。
实施例
以下通过实施例说明本发明,但本发明并不受限于这些实施例。
[测定、评价方法]
(平均气泡直径的测定)
以较薄形成为厚度1mm以下的显微镜用薄片切片机(日文:ミクロトームカッター)对所制得的聚氨酯树脂发泡体进行平行切片,以作为测定用试样。使用扫描型电子显微镜(日立科学系统公司(日文:日立サイエンスシステムズ社)制、S-3500N)以100倍拍摄试样表面,然后用图像分析软件(三谷商事株式会社(日文:MITANIコーポレーション社)制、WIN-ROOF),测定任意范围的全部气泡的圆当量径,由该测定值算出平均气泡直径。
(比重的测定)
根据JIS Z8807-1976进行。将制得的聚氨酯树脂发泡体切成4cm×8.5cm的条形状(厚度:任意)以作为比重测定用试样,将其以16小时静置在温度23℃±2℃、湿度50%±5%的环境中。在测定中,用比重计(赛多利斯公司(日文:ザルトリウス社)制)测定比重。
(硬度的测定)
根据JIS K6253-1997进行。将制得的聚氨酯树脂发泡体切成2cm×2cm(厚度:任意)大小,以作为硬度测定用试样,将其以16小时静置在温度23℃±2℃、湿度50%±5%的环境中。测定时,将试样重叠形成为厚度6mm以上。用硬度计(高分子计量器公司制,ASKER-D型硬度计),测定硬度。另外,将试样浸渍在水中48小时,其后取出试样,轻轻拭去表面水分后,以同样的方法测定硬度。
(研磨特性的评价)
使用MAT-ARW-8C1A(MAT(株)制)作为研磨装置,使用制得的研磨垫进行研磨特性的评价。通过对在8英寸硅晶片上形成1μm的热氧化膜所形成的材料研磨60秒,由此时的研磨量算出研磨速度。在氧化膜的膜厚测定中,使用光干涉式膜厚测定装置(耐诺公司(ナノメトリクス社)制造,装置名:Nanospec)。作为研磨条件,在研磨中以流量120ml/分钟添加作为浆液的硅浆液(SS12、卡博特公司制造(日文:キャボット社))。作为研磨负荷为4.5psi,研磨平台转速为93rpm,晶片转速为90rpm。
平坦化特性通过磨削量进行评价。在8英寸硅晶片上堆积0.5μm的热氧化膜后,进行规定的图案化后,以p-TEOS堆积1μm的氧化膜,制成具有初期阶差(日文:段差)0.5μm的图案的晶片。以前述条件对该晶片进行研磨,研磨后,测定各阶差,算出磨削量。磨削量是指在宽270μm的线以30μm的空间排列的图案和宽30μm的线以270μm的空间排列的图案中,前述2种图案的线上部分的阶差变为以下时的270μm的空间的磨削量。270μm的空间的磨削量少的情况表示不希望磨削的部分的磨削量少,平坦性高。
划痕的评价通过如下步骤进行:
在前述条件下研磨3片8英寸的假片(dummy wafer),其后对堆积有厚度的热氧化膜的8英寸的晶片研磨1分钟,然后用科磊腾克公司(日文:KLAテンコール社)制的缺陷评价装置(Surfscan SP1)测定研磨后的晶片上存在多少条0.19μm以上的条痕。
实施例1
在反应容器内放入3-异氰酸酯基丙基三乙氧基硅烷(信越化学株式会社制造、KBE-9007)10.2重量份、甲苯二异氰酸酯(2,4-体/2,6-体=80/20的混合物、TDI-80)37.8重量份、聚己内酯三醇(大赛璐化学工业公司制造、PCL305、羟值:305mgKOH/g、官能团数为3)22.6重量份、数均分子量为650的聚四亚甲基醚二醇(PTMG650)26.5重量份、以及二乙二醇(DEG)2.9重量份,此时NCO指数为1.9,在75℃反应3小时,制得包含烷氧基甲硅烷基的异氰酸酯末端预聚物(NCO重量%为9.12重量%,以下称为Si-预聚物)。
在反应容器内添加聚醚类预聚物(有利来路公司(ユニロイヤル社)制造,アジプレンL-325)75重量份、制得的Si-预聚物25重量份以及聚硅氧烷类表面活性剂(戈德施密特公司制造、B8465)3重量份,混合,调整到70℃,减压脱泡。其后,用搅拌叶片以转速为900rpm激烈搅拌大约4分钟以将气泡搅拌入反应系统内。其后,在反应容器内添加预熔融为120℃的4,4’-亚甲基双(o-氯苯胺)(以下称为MOCA)26.4重量份,此时NCO指数为1.1。以约70秒搅拌该混合液后,流入盘型的敞口模具(浇注容器)。在该混合液失去流动性的时刻放入炉内,在100℃进行后固化16小时,制得聚氨酯树脂发泡体块。
用切片机(亚米泰克公司(日文:アミテック社)制造、VGW-125)将加热至约80℃的前述聚氨酯树脂发泡体块切片,制得聚氨酯树脂发泡体片,然后,使用抛光机(亚米泰克公司制)将该片的表面进行抛光处理直至其厚度为1.27mm,以作为调整了厚度精度的片。将经过该抛光处理的片冲压成直径61cm的大小,使用槽加工机(泰克诺公司(日文:テクノ社)制造)对表面进行槽宽0.25mm、槽间距1.50mm、槽深度0.40mm的同心圆状的槽加工,制得研磨层。使用层叠机在与该研磨层的槽加工面相反侧的面上粘贴双面胶(积水化学工业公司制造,ダブルタックテープ)。然后,对实施了电晕处理的缓冲片(东丽株式会社制、聚乙烯泡沫、トーレペフ、厚度为0.8mm)的表面进行抛光处理,使用层叠机将其粘贴在前述双面胶上。再者,使用层叠机粘贴双面胶在缓冲片的另一面上以制成研磨垫。
实施例2~8、比较例1~3
除了采用表1记载的配方以外,以与实施例1同样的方法制得研磨垫。表1中的亲水性预聚物由下述方法制得。
在反应容器内放入聚乙二醇(PEG、第一工业制药公司制、数均分子量1000)40重量份、聚乙二醇(PEG、第一工业制药公司制、数均分子量600)12.8重量份、DEG6重量份,一边搅拌一边减压脱水1~2小时。然后,将氮导入可拆式烧瓶中,氮置换后,添加TDI-80(41.2重量份)。一边将反应体系内的温度保持在70℃左右,一边搅拌到反应结束。反应结束为NCO%达到基本一定值的时刻(NCO重量%:9.96重量%)。其后,以约2个小时进行减压脱泡,制得亲水性预聚物。
表1
实施例1~8的研磨垫是研磨速度快且平坦化特性优异的研磨垫。另外,能有效抑制晶片上产生划痕。另一方面,比较例1~3的研磨垫研磨速度和平坦化特性不够。再者,比较例1和2的研磨垫不能抑制晶片上产生划痕。
产业上利用的可能性
本发明的研磨垫能稳定且以高研磨效率进行透镜、反射镜等的光学材料或者硅晶片、铝基板以及一般的金属研磨加工等的要求高度的表面平坦性的材料的平坦化加工。本发明的研磨垫特别适用于对于硅晶片及其上面形成有氧化物层、金属层等的器件,在层叠和形成这些氧化物层和金属层之前进行平坦化的工序。
符号说明
1:研磨垫(研磨层)
2:研磨平台
3:研磨剂(浆液)
4:研磨对象物(半导体晶片)
5:支承台(抛光头)
6、7:旋转轴
Claims (8)
1.一种研磨垫,它是具有由聚氨酯树脂发泡体形成的研磨层的研磨垫,作为所述聚氨酯树脂发泡体的形成材料的聚氨酯树脂在侧链上具有下式(1)所示的烷氧基甲硅烷基:
式中,X为OR1或OH,R1分别独立地表示碳原子数1~4的烷基。
2.如权利要求1所述的研磨垫,其特征在于,所述聚氨酯树脂是含有作为预聚物原料组合物的反应物的包含烷氧基甲硅烷基的异氰酸酯末端预聚物和链增长剂的聚氨酯原料组合物的反应固化体,所述预聚物原料组合物的反应物含有异氰酸酯成分和多元醇成分;所述异氰酸酯成分含有下式(2)所示的包含烷氧基甲硅烷基的异氰酸酯;所述多元醇成分含有3官能以上的多元醇:
式中,X为OR1或OH,R1分别独立地表示碳原子数1~4的烷基,R2表示碳原子数1~6的亚烷基。
3.如权利要求2所述的研磨垫,其特征在于,所述包含烷氧基甲硅烷基的异氰酸酯为3-异氰酸酯基丙基三乙氧基硅烷。
4.如权利要求2或3所述的研磨垫,其特征在于,所述包含烷氧基甲硅烷基的异氰酸酯的含量是聚氨酯原料组合物的1~10重量%。
5.一种研磨垫的制造方法,该制造方法是包括将含有异氰酸酯末端预聚物的第一成分和含有链增长剂的第二成分进行混合、固化,制得聚氨酯树脂发泡体的工序的制造方法,其特征在于,所述工序是如下工序:
以相对于第一成分和第二成分合计重量为0.05~10重量%的条件将聚硅氧烷类表面活性剂添加到第一成分中,再将所述第一成分与非反应性气体搅拌,调制使所述非反应性气体作为气泡分散的气泡分散液后,在所述气泡分散液中混合含有链增长剂的第二成分,固化,制得聚氨酯树脂发泡体的工序;
所述第一成分含有作为预聚物原料组合物的反应物的包含烷氧基甲硅烷基的异氰酸酯末端预聚物;所述预聚物原料组合物的反应物含有异氰酸酯成分和多元醇成分;所述异氰酸酯成分含有下式(2)所示的包含烷氧基甲硅烷基的异氰酸酯;所述多元醇成分含有3官能以上的多元醇:
式中,X为OR1或OH,R1分别独立地表示碳原子数1~4的烷基,R2表示碳原子数1~6的亚烷基。
6.如权利要求5所述的研磨垫的制造方法,其特征在于,所述包含烷氧基甲硅烷基的异氰酸酯为3-异氰酸酯基丙基三乙氧基硅烷。
7.如权利要求5或6所述的研磨垫的制造方法,其特征在于,所述包含烷氧基甲硅烷基的异氰酸酯的含量是所述第一成分和所述第二成分的合计重量的1~10重量%。
8.一种半导体器件的制造方法,其特征在于,包含使用权利要求1~4中任一项所述的研磨垫,研磨半导体晶片的表面的工序。
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JP6312471B2 (ja) | 2018-04-18 |
KR20160132883A (ko) | 2016-11-21 |
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US20170073456A1 (en) | 2017-03-16 |
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