CN113264775A - 致密质复合材料、其制法、接合体及半导体制造装置用构件 - Google Patents

致密质复合材料、其制法、接合体及半导体制造装置用构件 Download PDF

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CN113264775A
CN113264775A CN202110081654.1A CN202110081654A CN113264775A CN 113264775 A CN113264775 A CN 113264775A CN 202110081654 A CN202110081654 A CN 202110081654A CN 113264775 A CN113264775 A CN 113264775A
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composite material
dense composite
titanium
less
mass
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CN113264775B (zh
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永井明日美
西村升
山口浩文
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NGK Insulators Ltd
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Abstract

本发明提供一种致密质复合材料、其制法、接合体及半导体制造装置用构件。本发明的致密质复合材料含有43～63质量％的硅化钛，并且含有分别比硅化钛的质量％少量的碳化硅和碳化钛，碳化硅的粒子间距离的最大值为40μm以下，标准偏差为10以下，开口气孔率为1％以下。

Description

致密质复合材料、其制法、接合体及半导体制造装置用构件
技术领域
本发明涉及致密质复合材料、其制法、接合体及半导体制造装置用构件。
背景技术
在半导体工艺中高温化的静电卡盘为了散热而接合有冷却板。在该情况下，有时作为静电卡盘的材料使用氧化铝，作为冷却板的材料使用铝，作为接合材料使用树脂。氧化铝与铝的线热膨胀系数差非常大，例如，氧化铝的线热膨胀系数为7.9ppm/K(RT-800℃：内田老鹤圃“陶瓷的物理”)，铝的线热膨胀系数为31.1ppm/K(RT-800℃：日本热物性学会编，“新编热物性手册”)。在将静电卡盘与冷却板接合的情况下，作为冷却板所需的特性，可以举出与静电卡盘的线热膨胀系数差小、为了维持散热性而热导率高、为了使冷却液或冷却气体通过而致密性高、为了耐受加工、安装等而强度高等。作为满足这样的特性的材料，可举出专利文献1所公开的复合材料。该复合材料含有37～60质量％的碳化硅粒子，并且含有分别比碳化硅粒子的质量％少量的硅化钛、碳硅化钛和碳化钛，开口气孔率为1％以下。该复合材料与氧化铝的线热膨胀系数差极小，热导率、致密性及强度足够高。
现有技术文献
专利文献
专利文献1：日本专利第6182082号公报
发明内容
发明所要解决的课题
然而，专利文献1的复合材料有时根据批次的不同而产生烧结不良部。其理由可考虑如下。专利文献1的复合材料中的硅化钛相、碳硅化钛相以及碳化钛相的分布反映了烧成前的成型体中的金属钛粒子的配置。因此，如果存在大量粒径大的金属钛粒子，则金属钛粒子的配置变得不均匀，产生含钛相与碳化硅粒子的偏析部。其结果，认为钛成分无法充分进入碳化粒子彼此的间隙而产生烧结不良部(空隙)。
本发明是为了解决这样的课题而完成的，其主要目的在于提供一种具有与氧化铝的线热膨胀系数差极小、热导率、致密性及强度充分高这样的特性的烧结性高的材料。
用于解决课题的方案
本发明的致密质复合材料含有43～63质量％的二硅化钛，并且含有分别比二硅化钛的质量％少量的碳化硅和碳化钛，碳化硅的粒子间距离的最大值为40μm以下，标准偏差为10以下，开口气孔率为1％以下。
需要说明的是，在本说明书中，表示数值范围的“～”作为包含其前后所记载的数值作为下限值及上限值的含义而被使用。
本发明的接合体是将由这样的致密质复合材料构成的第1材料和由氧化铝构成的第2材料接合而成的，本发明的半导体制造装置用部件是利用这样的接合体而成的。
本发明的致密质复合材料的制法包括：(a)制备含有平均粒径为10～25μm的碳化硅24～45质量％、平均粒径小于10μm的硅化钛42～67质量％，并且含有平均粒径小于20μm的金属钛或平均粒径小于10μm的碳化钛的粉体混合物的工序；以及(b)将上述粉体混合物在非活性气氛下通过热压在1350～1430℃烧结的工序。
发明效果
本发明的致密质复合材料是具有与氧化铝的线热膨胀系数差极小、热导率、致密性及强度充分高这样的特性的烧结性高的材料。因此，将由这样的致密质复合材料构成的第1材料和由氧化铝构成的第2材料接合而成的接合体能够用作半导体制造装置用构件，即使在低温与高温之间反复使用，第1材料与第2材料也不会剥离，因此在维持高散热性能的状态下耐用期限变长。另外，本发明的致密质复合材料的制法适于制造上述致密质复合材料。
附图说明
图1为各实验例的复合材料的SEM照片。
具体实施方式
本实施方式的致密质复合材料含有43～63质量％的硅化钛，并且含有分别比硅化钛的质量％少量的碳化硅和碳化钛，碳化硅的粒子间距离的最大值为40μm以下，标准偏差为10以下，开口气孔率为1％以下。
本实施方式的致密质复合材料含有43～63质量％的硅化钛。含量为通过里特沃尔德(Rietveld)解析而得到的值。在仅含有小于43质量％的硅化钛的情况下，有时根据制造批次的不同而产生烧结不良部，因此不优选。另外，在硅化钛含量超过63质量％的情况下，致密质复合材料的热膨胀系数变得过大，与氧化铝的热膨胀系数差变大，存在接合体的第1材料与第2材料剥离的可能性，因此不优选。作为硅化钛，可举出TiSi2、TiSi、Ti5Si4、Ti5Si3等，其中优选TiSi2。
本实施方式的致密质复合材料含有分别比硅化钛的质量％少量的碳化硅(SiC)和碳化钛(TiC)。碳化硅的质量％优选大于碳化钛的质量％。碳化硅优选含有29～46质量％。碳化硅的平均粒径优选为10～25μm。碳化钛优选含有5～15质量％。
本实施方式的致密质复合材料中，碳化硅的粒子间距离的最大值为40μm以下且碳化硅的粒子间距离的标准偏差为10以下。若不满足该条件，则有时无法得到充分高的强度或烧结性变得不充分，因此不优选。碳化硅的粒子间距离的平均值优选为4～10μm。碳化硅的粒子间距离可以通过解析致密质复合材料的SEM图像而求出。
本实施方式的致密质复合材料的开口气孔率为1％以下。开口气孔率为通过将纯水作为介质的阿基米德法测定的值。开口气孔率优选为0.1％以下。
本实施方式的致密质复合材料的线热膨胀系数与氧化铝为相同程度。因此，在将由本实施方式的致密质复合材料制作的构件与由氧化铝制作的构件接合(例如金属接合)的情况下，即使在低温与高温之间反复使用，也难以剥离。具体而言，本实施方式的致密质复合材料与氧化铝的40～570℃的平均线热膨胀系数之差的绝对值优选为0.5ppm/K以下，更优选为0.3ppm/K以下。另外，本实施方式的致密质复合材料的40～570℃的平均线热膨胀系数优选为7.2～8.2ppm/K，更优选为7.4～8.0ppm/K。
本实施方式的致密质复合材料的导热性优异，具体而言，热导率优选为70W/mK以上。这样，在将由本实施方式的致密质复合材料制作的构件与由氧化铝制成的构件进行金属接合的情况下，能够高效地释放氧化铝所具有的热。
本实施方式的致密质复合材料的强度优异，具体而言，4点弯曲强度优选为250MPa以上。这样，容易将由本实施方式的致密质复合材料制作的构件应用于冷却板等。
本实施方式的致密质复合材料也可以含有碳硅化钛。在含有碳硅化钛的情况下，其含有率优选为10质量％以下，更优选为0.5～9质量％。作为碳硅化钛，优选为Ti3SiC2(TSC)。
本实施方式的接合体是将由上述致密质复合材料制作的第1材料和由氧化铝制成的第2材料接合(例如金属接合)而成的。这样的接合体例如能够应用于半导体制造装置用构件。作为半导体制造装置用构件，例如可列举出利用以铝或其合金为主要成分的接合材料将由上述致密质复合材料制作的冷却板(第1材料)与由氧化铝制作的静电卡盘(第2材料)接合而成的构件等。第1材料与氧化铝的线热膨胀系数差极小，因此即使在低温和高温下反复使用，也难以从第2材料剥离。另外，由于第1材料的热导率足够高，因此能够高效地冷却由氧化铝制作的第2材料。进而，第1材料的致密性充分高，因此能够使冷却液、冷却气体通过内部，冷却效率进一步提高。此外，由于第1材料的强度足够高，因此也能够充分耐受因制造上述半导体制造装置用构件时的加工、接合、作为构件使用时的温度差而产生的应力。
本实施方式的致密质复合材料的制法包括：(a)制备含有平均粒径为10～25μm的碳化硅24～45质量％、平均粒径小于10μm的硅化钛42～67质量％，并且含有平均粒径小于20μm的金属钛或平均粒径小于10μm的碳化钛的粉体混合物的工序；以及(b)将上述粉体混合物在非活性气氛下通过热压在1350～1430℃烧结的工序。
在工序(a)中，在制备粉体混合物时，将各成分(碳化硅、硅化钛、金属钛和碳化钛)的平均粒径设定为落入上述的数值范围，将各成分的含有率设定为落入上述的数值范围，因此在工序(b)中烧结该粉体混合物后得到的致密质复合材料容易成为具有与氧化铝的线热膨胀系数差极小、热导率、致密性及强度充分高这样的特性的烧结性高的材料。该制法适于制造本实施方式的致密质复合材料。
在工序(a)中，关于粉体混合物中的源自除碳化硅以外的原料的Si和Ti，Si/(Si+Ti)的质量比优选为0.40～0.50。
在工序(b)中，作为非活性气氛，可以举出真空气氛、氩气气氛、氦气气氛、氮气气氛等。热压烧成时的压制压力没有特别限定，优选设定为50～300kgf/cm2。另外，烧成时间根据烧成条件适当设定即可，例如只要在1～10小时之间适当设定即可。
需要说明的是，本发明不受上述实施方式的任何限定，不言而喻，只要属于本发明的技术范围，能够以各种方式实施。
【实施例】
以下，对本发明的优选的应用例进行说明。SiC原料使用纯度97％以上、平均粒径15.5μm的市售品。金属Ti原料使用纯度99.5％以上、平均粒径12.9μm的粉末。二硅化钛使用纯度99％以上、平均粒径6.9μm的市售品。碳化钛使用纯度99％以上、平均粒径4.3μm的市售品。需要说明的是，以下的实施例并不对本发明进行任何限定。
[实验例1～11]
1.制造顺序
·调配
以成为表1所示的质量％的方式称量各原料成分，使用异丙醇作为溶剂，使用尼龙制的罐、直径10mm的含铁芯尼龙球湿式混合4小时。混合后取出浆料，在氮气流中在110℃干燥。然后，通过30目的筛子，制成调配粉末。需要说明的是，确认了在将称量的原料约500g投入到高速流动混合机(粉体投入部的容量1.8L)中，以搅拌叶片的转速1500rpm进行混合的情况下，也能够得到与湿式混合同样的材料特性。
·成形
将调配粉末以200kgf/cm2的压力进行单轴加压成形，制作直径50mm、厚度17mm左右的圆盘状成型体，收纳于烧成用石墨模具中。
·烧成
通过热压烧成圆盘状成型体，得到致密质烧结材料。在热压烧成中，将压制压力设为200kgf/cm2，以表1所示的烧成温度(最高温度)进行烧成，直至烧成结束为止设为真空气氛。烧成温度下的保持时间为4小时。
2.表的说明
表1中，a：各实验例的起始原料组成(调配比)、b：原料中，源自除SiC以外的成分(Si、Ti、TiSi2、TiC)的、Si相对于Si、Ti的总量的质量比(Si/(Si+Ti))、c：烧成条件(热压烧成温度及压制载荷)、d：由里特沃尔德解析求出的复合材料的构成相及其质量比、e：复合材料的基本特性(与体积密度、开口气孔率、4点弯曲强度、线热膨胀系数、热导率、碳化硅的粒子间距离相关的参数)。需要说明的是，实验例1～11中，实验例1～9相当于本发明的实施例，剩余的实验例相当于比较例。
表1
Figure BDA0002909553310000071
3.构成相的定量
用研钵将致密质复合材料粉碎制成粉末，在2θ＝5°～70°的范围内进行该粉末的XRD测定，将得到的XRD衍射图案作为对象进行里特沃尔德解析。作为解析软件，使用BrukerAXS制的TOPAS。
4.基本特性的测定
(1)原料的平均粒径
使用堀场制作所制造的LA950V2，将纯水作为分散介质进行测定。
(2)开口气孔率及体积密度
通过使用纯水作为介质的阿基米德法测定。
(3)4点弯曲强度
按照JIS-R1601求出。
(4)线热膨胀系数(40～570℃的平均线热膨胀系数)
按照JIS-R1618求出。具体而言，使用理学制造的Thermo plus EVO(立式差示膨胀测定方式)，在氩气气氛中，在升温速度10℃/分钟的条件下2次升温至600℃，根据第2次的测定数据算出40～570℃的平均线热膨胀系数。标准试样使用了装置附带的氧化铝标准试样(纯度99.7％、体积密度3.9g/cm3、长度20mm)。准备另1根该氧化铝标准试样，在相同条件下测定线热膨胀系数而得到的值为7.7ppm/K。
(5)热导率
按照JIS-R1611通过激光闪光法测定。
(6)SEM观察
进行致密质复合材料的SEM观察。在SEM观察中，对致密质复合材料的截面进行镜面研磨，利用电子显微镜(SEM；日本电子制JSM-IT500LA)以反射电子图像进行观察。反射电子图像的观察在加速电压10～15kV、PC30～45的条件下进行。将各实验例的SEM图像(倍率500倍)示于图1。
(7)碳化硅的粒子间距离的平均值、标准偏差及最大值
使用株式会社日本Roper制造的图像解析软件“Image–Pro ver.9.3.2”对图1所示的SEM图像进行图像解析，由此求出碳化硅的粒子间距离。具体而言，在SEM图像中，排列平行延伸的5条直线。各直线的宽度设为0.2μm。另外，该SEM图像的1个像素对应于0.2μm×0.2μm。接着，自动算出在直线上与明亮部分(即，Ti-Si矩阵)重复的区域(以下，称为“明区域”。)的面积。此时，由于各直线配置在像素列的边界线上，因此在明区域的面积计算中，通过直线提取宽度0.4μm的区域(即，具有2个像素的宽度的区域)。宽度0.2μm的直线配置于在宽度方向上相邻的2列像素列(即，在与宽度方向垂直的方向上排列的多个像素的列)的边界线上，具有与直线重叠部分的全部像素成为面积计算的对象。在明区域的面积计算中，不对1个像素(即0.04μm2)以下的区域进行计数，因此小于0.05μm2的区域作为噪声而忽略。然后，求出明区域的面积作为碳化硅粒子间的矩阵面积。矩阵面积是将碳化硅的粒子间距离和作为明区域提取的直线宽度(即0.4μm)相乘而得到的。因此，通过将上述明区域的面积除以0.4μm，从而算出碳化硅的粒子间距离。使用算出的所有粒子间距离，求出其平均值、标准偏差及最大值。
5.结果
实验例1～9的致密质复合材料中，碳化硅的粒子间距离的最大值为40μm以下(具体而言为20～40μm)，标准偏差为10以下(具体而言为4～8)。另外，碳化硅的粒子间距离的平均值为4～10μm(具体为4～9μm)。这些致密质复合材料的开口气孔率为1％以下且充分致密化，4点弯曲强度为250MPa以上，强度足够高，热导率为70W/mK以上，具有良好的热传导性，线热膨胀系数为7.2～8.2ppm/K，与氧化铝大致同等(与氧化铝的线热膨胀系数之差的绝对值为0.5ppm/K以下)。
另一方面，实验例10的致密质复合材料中，碳化硅的粒子间距离的最大值为59.9μm，标准偏差为11.6，平均值为8.3μm，但具有与实验例1～9同等的特性(开口气孔率、4点弯曲强度、热导率、线热膨胀系数)。认为这是由于碳硅化钛的含有率为比较高的13.1质量％。即，认为实验例10的致密质复合材料由于碳化硅的粒子间距离长，其偏差也大，因此特别担心强度降低，但通过高强度的碳硅化钛分布在碳化硅的粒子间，从而能够得到良好的特性。但是，由于碳硅化钛是在烧结工序中生成的，因此其生成量、分布有时根据批次的不同而产生偏差，并不是绝对能够得到良好的特性。例如，在实验例11中，原料的成分和调配比与实验例10相同，但将烧成温度从实验例10的1400℃变更为1370℃。因此，开口气孔率增大为4.14％，强度也仅为239MPa。观察实验例11的SEM图像(图1的(k))可知，局部产生了全黑的部位(箭头所指的部位)。该全黑的部位是烧结不良部(气孔)。与此相对，在实验例1～9中，认为通过改善致密质复合材料的微结构(即控制碳化硅的粒子间距离)，从而即使不生成碳硅化钛也能够得到良好的特性，因此无论批次如何都能够稳定地得到良好的特性。
6.关于接合体
在实验例1中得到的致密质复合材料样品(直径50mm、厚度8mm)上依次层叠以铝为主构成材料的厚度200μm的金属箔(纵、横与上述的样品相同)和厚度5mm的致密质氧化铝烧结体，收纳于烧成用石墨模具中，在100kgf/cm2的压力、600℃真空下热压烧成。结果，能够得到在界面没有剥离、空隙的接合体(金属接合体)。另外，使用实验例2和实验例9中得到的致密质复合材料样品代替实验例1中得到的致密质复合材料样品，同样地操作来制作接合体，结果在界面均未观察到剥离、空隙。
产业上的利用可能性
本发明的致密质复合材料例如能够用于与氧化铝制的静电卡盘、基座等进行金属接合的冷却板。
本申请将2020年1月29日申请的日本专利申请第2020-012343号作为优先权主张的基础，通过引用将其内容全部包含在本说明书中。

Claims (12)

1.一种致密质复合材料，含有43～63质量％的硅化钛，并且含有分别比硅化钛的质量％少量的碳化硅和碳化钛，碳化硅的粒子间距离的最大值为40μm以下，标准偏差为10以下，开口气孔率为1％以下。
2.根据权利要求1所述的致密质复合材料，碳化硅为29～46质量％、碳化钛为5～15质量％。
3.根据权利要求1或2所述的致密质复合材料，碳化硅的粒子间距离的平均值为4～10μm。
4.根据权利要求1～3中任一项所述的致密质复合材料，与氧化铝的40～570℃的平均线热膨胀系数差的绝对值为0.5ppm/K以下。
5.根据权利要求1～4中任一项所述的致密质复合材料，热导率为70W/mK以上。
6.根据权利要求1～5中任一项所述的致密质复合材料，4点弯曲强度为250MPa以上。
7.根据权利要求1～6中任一项所述的致密质复合材料，含有碳硅化钛。
8.一种接合体，将由权利要求1～7中任一项所述的致密质复合材料构成的第1材料和由氧化铝构成的第2材料接合而成。
9.根据权利要求8所述的接合体，所述第1材料和所述第2材料进行了金属接合。
10.一种半导体制造装置用构件，由权利要求8或9所述的接合体构成。
11.一种致密质复合材料的制法，包括：
(a)制备含有平均粒径为10～25μm的碳化硅24～45质量％、平均粒径小于10μm的硅化钛42～67质量％、并且含有平均粒径小于20μm的金属钛或平均粒径小于10μm的碳化钛的粉体混合物的工序；以及
(b)将所述粉体混合物在非活性气氛下通过热压在1350～1430℃烧结的工序。
12.根据权利要求11所述的致密质复合材料的制法，在工序(a)中，对于所述粉体混合物的源自除碳化硅以外的原料的Si和Ti，Si/(Si+Ti)的质量比为0.40～0.50。
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