CN103180262A - 堇青石质陶瓷及使用其的半导体制造装置用部件 - Google Patents
堇青石质陶瓷及使用其的半导体制造装置用部件 Download PDFInfo
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Abstract
本发明提供热膨胀系数小、机械强度优异的堇青石质陶瓷及使用其的半导体制造装置用部件。所述堇青石质陶瓷中,相对于具有以氧化物换算量计含有Mg12.6质量%以上且14.0质量%以下、以氧化物换算量计含有Al33.4质量%以上且34.4质量%以下、及以氧化物换算量计含有Si52.0质量%以上且53.6质量%以下的组成范围的主成分100质量%,含有换算成氧化物时为4.5质量%以上且15.0质量%以下的Y、Yb、Er及Ce中的任一种作为副成分,并且堇青石、二硅酸盐及尖晶石作为晶相存在。该堇青石质陶瓷的热膨胀系数在±120ppb/℃的范围内,四点弯曲强度为170MPa以上,具有低热膨胀性及优异的机械强度。
Description
技术领域
本发明涉及堇青石质陶瓷及使用其的半导体制造装置用部件。
背景技术
堇青石质陶瓷由于热膨胀系数小而被用于过滤器、蜂窝状物(honeycomb)、耐火物等中。并且,近年来,提出了将其用于真空装置结构体、基座(susceptor)、台架(stage)或者半导体制造工艺中的夹具等半导体制造装置用部件的方案,作为这样的堇青石质陶瓷,提出了如下的堇青石质陶瓷:以80~92重量%的比例含有堇青石、以2~20重量%的比例含有稀土元素(RE)的氧化物,并且,上述堇青石的晶体粒子由高温型堇青石和低温型堇青石的混合组织构成,低温型堇青石在堇青石晶体粒子中所占的面积比例为5%以上、且杨氏模量为120GPa以上(参考专利文献1)。
现有技术文献
专利文献
专利文献1:日本特开2001-39764号公报
发明内容
发明要解决的问题
在LSI等半导体的制造工序中,随着电路微细化的迅速发展,其线宽高精密化至亚微米级的水平,例如,对于在Si晶片上形成高精密电路的曝光装置所使用的台架,要求100nm(0.1μm)以下的定位精度,由部件具有的热膨胀系数引起的对位误差会对产品的品质、成品率产生很大的影响。
因此,为了提高曝光装置中使用的台架的定位精度而提高品质、成品率,要求构成上述台架的陶瓷显示出ppm级~ppb级的热膨胀系数。
进而,真空装置结构体、基座、台架或者半导体制造工艺中的夹具等半导体制造装置用部件随着半导体晶片的尺寸增大而不断大型化,需要应对自重、悬臂支撑结构等,因而,要求在低热膨胀化的同时提高机械强度(四点弯曲强度)。
本发明是为了应对上述要求而完成的发明,其目的在于,提供热膨胀系数小、机械强度优异的堇青石质陶瓷及使用其的半导体制造装置用部件。
用于解决问题的手段
本发明的堇青石质陶瓷的特征在于,相对于具有以氧化物换算量计含有Mg12.6质量%以上且14.0质量%以下、以氧化物换算量计含有Al33.4质量%以上且34.4质量%以下、及以氧化物换算量计含有Si52.0质量%以上且53.6质量%以下的组成范围的主成分100质量%,含有换算成氧化物时为4.5质量%以上且15.0质量%以下的Y、Yb、Er及Ce中的任一种作为副成分,并且堇青石、二硅酸盐及尖晶石作为晶相存在。
另外,本发明的半导体制造装置用部件的特征在于,使用了上述构成的本发明的堇青石质陶瓷。
发明效果
根据本发明的堇青石质陶瓷,通过相对于具有以氧化物换算量计含有Mg12.6质量%以上且14.0质量%以下、以氧化物换算量计含有Al33.4质量%以上且34.4质量%以下、及以氧化物换算量计含有Si52.0质量%以上且53.6质量%以下的组成范围的主成分100质量%,含有换算成氧化物时为4.5质量%以上且15.0质量%以下的Y、Yb、Er及Ce中的任一种作为副成分,并且堇青石、二硅酸盐及尖晶石作为晶相存在,从而能将显示负侧的热膨胀系数的堇青石、与显示正侧的热膨胀系数的二硅酸盐及尖晶石的晶相的存在比率最优化,能使得到的堇青石质陶瓷的热膨胀系数在±120ppb/℃的范围内。另外,通过存在作为晶相的尖晶石,从而抑制堇青石的晶相的晶粒生长,能够将堇青石质陶瓷制成由微细晶体构成的高致密体,因而,能够提高机械特性。
另外,根据本发明的半导体制造装置用部件,通过使用本发明的堇青石质陶瓷,从而能实现100nm(0.1μm)以下的定位精度,在Si晶片的高精密电路的形成中,能提高品质及成品率。
具体实施方式
以下,对本实施方式的堇青石质陶瓷的一例进行说明。
本实施方式的堇青石质陶瓷中,相对于具有以氧化物换算量计含有Mg12.6质量%以上且14.0质量%以下、以氧化物换算量计含有Al33.4质量%以上且34.4质量%以下、及以氧化物换算量计含有Si52.0质量%以上且53.6质量%以下的组成范围的主成分100质量%,含有换算成氧化物时为4.5质量%以上且15.0质量%以下的Y、Yb、Er及Ce中的任一种作为副成分。
并且,本实施方式的堇青石质陶瓷中,作为晶相,存在:由MgO、Al2O3和SiO2这3种成分形成的堇青石(Mg2Al4Si5O18);由Y、Yb、Er及Ce中的任一种的氧化物和SiO2形成的二硅酸盐(例如Yb2Si2O7);和由MgO和Al2O3形成的尖晶石(MgAl2O4)。
这里,本实施方式的堇青石质陶瓷通过满足上述组成范围并存在作为晶相的堇青石、二硅酸盐及尖晶石,从而能够将显示负侧的热膨胀系数的堇青石、与显示正侧的热膨胀系数的二硅酸盐及尖晶石的晶相的存在比率最优化,能使得到的堇青石质陶瓷的热膨胀系数接近0(zero)。具体而言,通过满足上述组成范围并存在作为晶相的堇青石、二硅酸盐及尖晶石,从而能够使室温(20~25℃)下的堇青石质陶瓷的热膨胀系数在±120ppb/℃的范围内。需要说明的是,在显示正侧的热膨胀系数的二硅酸盐及尖晶石中,二硅酸盐比尖晶石在正侧显示出更大的热膨胀系数的值。
另外,使副成分相对于主成分100质量%的含量在Y、Yb、Er及Ce中的任一种换算成氧化物时为4.5质量%以上且15.0质量%以下的原因在于,副成分的含量小于4.5质量%时,二硅酸盐的存在比率变少,室温(20~25℃)下的堇青石质陶瓷的热膨胀系数小于-120ppb/℃。另外,其原因还在于,副成分的含量超过15.0质量%时,二硅酸盐的存在比率变多,室温(20~25℃)下的堇青石质陶瓷的热膨胀系数超过+120ppb/℃。
另外,通过存在作为晶相的尖晶石,从而抑制堇青石的晶相的晶粒生长,能够将堇青石质陶瓷制成由微细晶体构成的高致密体,因此,能够提高机械特性。具体而言,能使四点弯曲强度为170MPa以上。若具有170MPa以上的强度,则在伴随半导体晶圆的尺寸增大的部件的大型化中成为问题的、因自重引起的破损、在悬臂支撑结构中施加载荷时的破损等的风险少,因此,能够适合用于真空装置结构体、基座、台架、半导体制造工艺中的夹具等半导体制造装置用部件中。需要说明的是,关于上述四点弯曲强度,基于JIS R1601-2008来测定即可。另外,自不必说,尖晶石适宜分散存在于堇青石的晶相间。
需要说明的是,关于构成本实施方式的堇青石质陶瓷的各成分的换算成氧化物时的含量,可以如下求出:将堇青石质陶瓷的一部分粉碎,将所得粉体溶解于盐酸等溶液中,然后,使用ICP(电感耦合等离子体,Inductively Coupled Plasma)发射光谱分析装置(岛津制作所制造:ICPS-8100)进行测定,使用所得各金属元素的含量的值,分别换算成氧化物。另外,关于堇青石、二硅酸盐、尖晶石的各晶相的确认,例如,可以如下确认:使用X射线衍射装置(PANalytical公司制造:X’PertPRO),在2θ=8°~80°、CuKα1测定的条件下测定堇青石质陶瓷的表面,将所得X射线衍射图和JCPDS卡对照,进行晶相的鉴定。
另外,关于热膨胀系数的测定,可以如下测定:准备长度10~20mm、边长或直径为5mm左右的棱柱或圆柱试样,依据JIS R1618-2002,使用例如激光热膨胀计LIX-1(真空理工(株)制造)作为测定装置,以等速升温测定的模式在升温速度:1℃/min的条件下测定所需温度范围的热膨胀系数。
并且,本实施方式的堇青石质陶瓷中,将二硅酸盐的含量设为A、将尖晶石的含量设为B时,A和B的比率A/B优选为0.5以上且24.0以下。
如上所述,二硅酸盐和尖晶石的含量的比率A/B为0.5以上且24.0以下时,能够将显示负侧的热膨胀系数的堇青石、与显示正侧的热膨胀系数的二硅酸盐及尖晶石的晶相的存在比率进一步最优化,因此,能使室温(20~25℃)下的堇青石质陶瓷的热膨胀系数在±100ppb/℃的范围内。
需要说明的是,关于二硅酸盐及尖晶石的含量,例如,使用X射线衍射装置(PANalytical公司制造:X’PertPRO),在2θ=8°~80°、CuKα1测定的条件下实施X射线衍射测定,使用Rietveld解析程序RIETAN,对X射线衍射测定结果进行解析,由此从堇青石、二硅酸盐及尖晶石的各晶相的比例算出即可。关于二硅酸盐和尖晶石的含量的比率A/B,由算出的各自的含量算出即可。
另外,作为构成将二硅酸盐的含量设为A、将尖晶石的含量设为B时A和B的比率A/B为0.5以上且24.0以下的堇青石质陶瓷的晶相的具体的含量,二硅酸盐为2.6~12.7质量%左右,尖晶石为0.53~5.1质量%左右,余量为堇青石。
进而,优选使二硅酸盐的含量为4.5质量%以上且7.0质量%以下、尖晶石的含量为1.4质量%以上且3.3质量%以下。由此,能使室温(20~25℃)下的堇青石质陶瓷的热膨胀系数的绝对值更小。另外,二硅酸盐的含量为4.9质量%以上且5.6质量%以下、尖晶石的含量为2.2质量%以上且2.8质量%以下时,能使室温(20~25℃)下的堇青石质陶瓷的热膨胀系数的绝对值较小并接近零。
另外,本实施方式的堇青石质陶瓷优选还含有颜料成分。像这样含有颜料成分时,通过与其它色调的陶瓷组合,能带来如谋求色彩的调和或显眼等视觉效果。另外,在将堇青石质陶瓷作为例如会受到光的散射影响的分析用镜筒等光学系支撑部件使用时,如果使用形成灰色系等色调的颜料成分制作堇青石质陶瓷,则由于堇青石质陶瓷呈现灰色系色调而能够使光的散射受到抑制而使分析精度的降低较少。
另外,在半导体制造装置内的加工产品状态的确认中,在半导体制造装置用部件的作用下光发生散射时,会给以小型照相机等光学设备进行的确认带来障碍,因此,作为需要抑制光的散射的部件使用时,优选形成呈灰色系色调的堇青石质陶瓷。
这里,为了形成呈现能抑制光的散射的灰色系色调的堇青石质陶瓷,优选的是,含有Mn、Cr及Co作为颜料成分且Mn、Cr及Co分别换算成MnO2、Cr2O3及CoO后的总含量相对于主成分100质量%为0.05质量%以上且3质量%以下。
如上所述,在含有Mn、Cr及Co作为颜料成分并且Mn、Cr及Co分别换算成MnO2、Cr2O3及CoO后的总含量相对于主成分100质量%为0.05质量%以上且3质量%以下时,对热膨胀系数、机械特性的影响小,并且,不会出现因颜料成分之间的反应、主成分和颜料成分之间的反应而异相(例如MnAl2O4,MnCr2O4)量增加,色调不均,从而导致外观受损的情况,能够形成呈现能抑制光散射的灰色系色调的堇青石质陶瓷。
需要说明的是,色调过暗时,存在吸收光能(以下记为吸光。),温度升高,因该温度升高而使堇青石质陶瓷膨胀,导致尺寸发生变化的风险,因此,为了抑制光的散射并抑制吸光,优选使CIE1976L*a*b*色空间中的亮度指数L*为50以上且70以下。需要说明的是,关于该亮度指数L*,可以依据JIS Z8722-2000来测定。
并且,使用上述热膨胀系数小、机械强度优异的堇青石质陶瓷作为半导体制造装置用部件时,能实现100nm(0.1μm)以下的定位精度,在Si晶片的高精密电路的形成中,能提高品质及成品率。
以下,对本实施方式的堇青石质陶瓷的制造方法进行说明。
作为本实施方式的堇青石质陶瓷的制造方法,首先,作为1次原料,准备预先合成的平均粒径为0.5~5μm的合成堇青石粉末、平均粒径为0.5~3μm的尖晶石粉末和平均粒径为0.5~2μm的Y、Yb、Er及Ce中的任一种的氧化物粉末。
需要说明的是,合成堇青石粉末及尖晶石粉末构成本实施方式的主成分,Y、Yb、Er及Ce中的任一种的氧化物粉末构成副成分。另外,合成堇青石粉末是从主成分100质量%减去尖晶石粉末的添加量、并按照以氧化物换算量计含有Mg11.7质量%以上且13.3质量%以下、以氧化物换算量计含有Al29.1质量%以上且33.8质量%以下、及以氧化物换算量计含有Si52.0质量%以上且53.6质量%以下的组成范围预先合成的粉末。
然后,称量规定量的合成堇青石粉末及尖晶石粉末,例如,称量93.5质量%以上且99.9质量%以下的合成堇青石粉末、0.01质量%以上且6.5质量%以下的尖晶石粉末。然后,相对于合成堇青石粉末和尖晶石粉末的总和100质量%,以4.5质量%以上且15.0质量%的范围的量称量副成分,添加纯水及各种粘结剂,使用球磨机进行5~30小时湿式混合及粉碎直至平均粒径达到2μm以下,得到浆液。
需要说明的是,通过设为上述添加量,从而使烧成后的堇青石质陶瓷的组成范围为:以氧化物换算量计含有Mg12.6质量%以上且14.0质量%以下、以氧化物换算量计含有Al33.4质量%以上且34.4质量%以下、及以氧化物换算量计含有Si52.0质量%以上且53.6质量%以下。
另外,添加颜料成分时,相对于主成分100质量%,称量例如0.05质量%以上且3.0质量%以下的颜料成分,与合成堇青石粉末、尖晶石粉末及Y、Yb、Er及Ce中的任一种的氧化物粉末一起加入球磨机内,用上述方法进行湿式混合即可。作为颜料成分,尤其优选含有Mn、Cr及Co。
然后,用喷雾造粒法(喷雾干燥法)使浆液喷雾,进行造粒,形成2次原料。然后,使用该2次原料,用静压成形(橡胶压制)法、粉末压制成形法进行成形,根据需要实施切削加工后,将其用烧成炉在大气氛围中以1340~1440℃的最高温度保持1小时以上且10小时以下。其后,通过设成以10℃/min以下降温至1000℃的烧成条件,从而能够存在通过副成分与合成堇青石中的SiO2反应而生成的二硅酸盐。尤其是为了使烧成后的堇青石质陶瓷的二硅酸盐的含量A和尖晶石的含量B的比率A/B在0.5以上且24.0以下的范围内,设为1350~1420℃的最高温度即可。
然后,通过根据需要实施磨削加工,从而能够得到本实施方式的堇青石质陶瓷。另外,也可以在烧结后利用HP法(热压制法)、HIP法(热等静压法、Hot Isostatic Pressing)来实现进一步的致密化。由此,能够使四点弯曲强度为190MPa以上。
需要说明的是,作为1次原料,也可以代替Y、Yb、Er及Ce中的任一种的氧化物粉末、或者其一部分,而以二硅酸盐(Y2Si2O7、Yb2Si2O7、Er2Si2O7、Ce2Si2O7)的形式添加。
实施例1
制作如表1所示那样分别改变了调配组成、副成分的种类、添加量等的试样,实施堇青石质陶瓷的各成分的质量比率、晶相的确认、热膨胀系数的测定。
首先,作为1次原料,准备平均粒径为2μm的合成堇青石粉末(以表1所示的MgO、Al2O3及SiO2的组成范围预先合成)、平均粒径为1μm的尖晶石粉末和作为副成分的平均粒径为1μm的Yb2O3、Y2O3、Er2O3及Ce2O3的粉末。然后,以表1所示的添加量称量尖晶石粉末,并以从100质量%减去尖晶石粉末的添加量而得的量称量合成堇青石粉末。
并且,相对于合成堇青石粉末和尖晶石粉末的总和100质量%,分别称量表1所示的比例的副成分,相对于纯水及主成分和副成分的总和100质量%,添加2质量%以下的粘结剂,使用球磨机进行24小时湿式混合及粉碎直至平均粒径达到2μm以下,得到浆液。
接着,使用喷雾造粒法(喷雾干燥法)使该浆液喷雾,进行造粒,得到2次原料。然后,使用该2次原料,利用粉末压制成形法进行成形,在大气氛围中以1415℃的最高温度保持5小时,然后,以10℃/min降温至1000℃,进行烧成。然后,实施磨削加工,从而得到具有纵3mm、横4mm、长45mm的尺寸的试样No.1~15、17~23、25~35、37~39、41~45。
另外,除不添加尖晶石粉末以外,利用上述同样的制造方法得到试样No.24、36、40、46。进而,除不添加作为副成分的Yb2O3、Y2O3、Er2O3及Ce2O3以外,利用上述同样的制造方法得到试样No.16。
然后,对于试样No.1~46,粉碎试样的一部分,将所得粉体溶解在盐酸等溶液中后,使用ICP发射光谱分析装置(岛津制作所制造:ICPS-8100)进行测定,使用所得各金属元素的含量的值,分别换算成氧化物。之后,使用该换算成氧化物而得到的值,求出该氧化物在烧成后的MgO、Al2O3及SiO2的总和100质量%中的质量比率、以及副成分相对于MgO、Al2O3及SiO2的总和100质量%的质量比率。结果示于表2。
另外,使用X射线衍射装置(PANalytical公司制造:X’PertPRO),在2θ=8°~80°、CuKα1测定的条件下实施各试样表面的X射线衍射测定,得到X射线衍射图,然后,与JCPDS卡对照,进行鉴定,由此确认到堇青石、二硅酸盐、尖晶石的有无。需要说明的是,确认到的情况记为“○”,确认不到的情况记为“-”,将结果示于表2。
另外,关于热膨胀系数,准备将各试样切断为10mm长度、并对切断的试样的两个端面进行R加工而得到的试验片,使用激光热膨胀计LIX-1(真空理工(株)制造),以等速升温测定的模式,在升温速度:1℃/min的条件下测定20~25℃的温度范围的热膨胀系数,算出其平均值,由此求出热膨胀系数,将结果示于表2。
[表1]
[表2]
由表2的结果可知,试样No.1、5、6、10、11、15、31~34虽然存在作为晶相的堇青石、二硅酸盐及尖晶石,但堇青石质陶瓷的主成分组成不满足以氧化物换算量计含有Mg12.6质量%以上且14.0质量%以下、以氧化物换算量计含有Al33.4质量%以上且34.4质量%以下、及以氧化物换算量计含有Si52.0质量%以上且53.6质量%以下的范围,因而热膨胀系数超出了±120ppb/℃的范围。
另外,试样No.17、23、35、38、39、42、43、46虽然存在作为晶相的堇青石、二硅酸盐及尖晶石,但不含有换算成氧化物时相对于主成分100质量%为4.5质量%以上且15.0质量%以下的作为副成分的Y、Yb、Er及Ce中的任一种,因而热膨胀系数超出了±120ppb的范围。
另外,试样No.16没有添加副成分,因而副成分没有作为烧结助剂起作用而未实现致密化,因而无法测定热膨胀系数。另外,在晶相的确认中没有确认到二硅酸盐。
另外,试样No.24、36、40、44在晶相的确认中没有确认到尖晶石,热膨胀系数超出了±120ppb/℃的范围。
相对于此,试样No.2~4、7~9、12~14、18~22、25~30、37、41、45中,相对于具有以氧化物换算量计含有Mg12.6质量%以上且14.0质量%以下、以氧化物换算量计含有Al33.4质量%以上且34.4质量%以下、及以氧化物换算量计含有Si52.0质量%以上且53.6质量%以下的组成范围的主成分100质量%,含有换算成氧化物时为4.5质量%以上且15.0质量%以下的Y、Yb、Er及Ce中的任一种作为副成分,并且堇青石、二硅酸盐及尖晶石作为晶相存在,因而显示负侧的热膨胀系数的堇青石、与显示正侧的热膨胀系数的二硅酸盐及尖晶石的晶相的存在比率得到最优化,能使所得堇青石质陶瓷的热膨胀系数为±120ppb/℃这样非常小的值。
另外,关于不存在尖晶石的晶相的试样No.24、36、40、44,包括试验片的制作在内,基于JIS R1601-2008测定了四点弯曲强度,结果小于170MPa。相对于此,试样No.2~4、7~9、12~14、18~22、25~30、37、41、45中四点弯曲强度为170MPa以上,本实施方式的堇青石质陶瓷的热膨胀系数小、四点弯曲强度的值大,在伴随半导体晶片的尺寸增大的部件的大型化中成为问题的、因自重引起的破损、在悬臂支撑结构中施加载荷时的破损等的风险少,因而可以适合用于真空装置结构体、基座、台架、半导体制造工艺中的夹具等半导体制造装置用部件中。进而,关于试样No.2~4、7~9、12~14、18~22、25~30、37、41、45,利用HIP法(热等静压法)实施了处理,结果四点弯曲强度为190MPa以上,机械特性更优异。
实施例2
然后,制作表3所示的分别改变了调配组成及烧成条件的试样No.47~78。需要说明的是,关于制作方法,利用与实施例1同样的制造方法来制作。然后,利用与实施例1同样的方法,实施堇青石质陶瓷的各成分的质量比率、热膨胀系数的测定。
另外,算出各试样中二硅酸盐的含量(A)和尖晶石的含量(B)的比率A/B。需要说明的是,二硅酸盐的含量(A)和尖晶石的含量(B)的比率A/B如下算出:使用X射线衍射装置(PANalytical公司制造:X’PertPRO),在2θ=8°~80°、CuKα1测定的条件下实施X射线衍射测定,使用Rietveld解析程序RIETAN对X射线衍射测定结果进行解析,由此从堇青石、二硅酸盐及尖晶石各晶相的比例算出含量。然后,用算出的二硅酸盐的含量(A)除以尖晶石的含量(B),从而算出比率A/B。
MgO、Al2O3及SiO2在烧成后的MgO、Al2O3及SiO2的总和100质量%中的质量比率、副成分相对于MgO、Al2O3及SiO2的总和100质量%的质量比率、二硅酸盐的含量(A)、尖晶石的含量(B)、比率A/B、热膨胀系数如表4所示。
[表3]
[表4]
由表4的结果可知,将二硅酸盐的含量设为A、将尖晶石的含量设为B时,A和B的比率A/B为0.5以上且24.0以下的试样No.48~77与比率A/B小于0.5或超过24.0的试样No.47、78相比,热膨胀系数的绝对值小,能使热膨胀系数在±100ppb/℃的范围内。
另外,二硅酸盐的含量为4.5质量%以上且7.0质量%以下、尖晶石的含量为1.4质量%以上且3.3质量%以下的试样No.54~61中,热膨胀系数更小,在±50ppb/℃的范围内。
进而,二硅酸盐的含量为4.9质量%以上且5.6质量%以下、尖晶石的含量为2.2质量%以上且2.8质量%以下的试样No.55~57中,热膨胀系数在±20ppb/℃的范围内,能使热膨胀系数接近零。
另外,制作除表3所示的调配组成以外的、相对于具有以氧化物换算量计含有Mg12.6质量%以上且14.0质量%以下、以氧化物换算量计含有Al33.4质量%以上且34.4质量%以下、及以氧化物换算量计含有Si52.0质量%以上且53.6质量%以下的组成范围的主成分100质量%,含有换算成氧化物时为4.5质量%以上且15.0质量%以下的Y、Yb、Er及Ce中的任一种作为副成分的各种堇青石质陶瓷,进行热膨胀系数的确认,结果比率A/B为0.5以上且0.24以下,由此确认能使热膨胀系数在±100ppb/℃的范围内。
实施例3
然后,在与实施例2的表3所示的试样No.56同样的调配组成的基础上,分别添加换算成氧化物后的总量为1质量%的表5所示的颜料成分,制作试样No.79~86。之后,对这些试样实施色调的目视确认和亮度指数L*的测定。
需要说明的是,除与合成堇青石粉末、尖晶石粉末及Yb的氧化物粉末一起添加颜料成分以外,利用和实施例1同样的制造方法制作试样。
然后,目视确认所得到的各试样的色调,示于表5。另外,关于亮度指数L*,基于JIS Z8722-2000,使用色彩色差计(旧MINOLTA公司(制造)CR-221),将光源设为CIE标准光源D65,将照明受光方式设为条件a((45-n)[45-0]),将测定直径设为3mm,进行测定。结果示于表5。需要说明的是,对于不含有颜料成分的试样No.56,也将色调的目视确认结果和亮度指数L*的结果示于表5。
[表5]
由表5的结果可知,含有颜料成分的试样No.79~83根据颜料成分的不同可以形成各种色调的陶瓷,通过与其它色调的陶瓷组合,能带来如谋求色彩的调和、显眼等视觉效果。另外,与不含有颜料成分的试样No.56相比,亮度指数L*的值更小,由此可以确认到能抑制光的散射。另外,含有Mn、Cr及Co作为颜料成分的试样No.85的亮度指数L*的范围为65,在能够抑制光的散射并抑制吸光的优选的亮度指数L*的值即50~70的范围内。
实施例4
然后,在与实施例2的表3所示的试样No.56同样的调配组成的基础上,制作如表6所示那样分别改变了颜料成分的含量的试样,实施亮度指数L*的测定。需要说明的是,除与合成堇青石粉末、尖晶石粉末及Yb的氧化物粉末一起添加颜料成分以外,利用和实施例1同样的制造方法制作试样。关于颜料成分的含量,利用实施例1所示的同样的方法,使用ICP发射光谱分析装置(岛津制作所制造:ICPS-8100)进行测定,算出相对于主成分100质量%的值。另外,亮度指数L*的测定利用与实施例3同样的方法进行。结果示于表6。
[表6]
由表6的结果可以确认,试样No.87~94在能够抑制光的散射并且抑制吸光的优选的亮度指数L*的值即50~70的范围内,为了使亮度指数L*在该范围内,含有Mn、Cr及Co作为颜料成分并且Mn、Cr及Co分别换算成MnO2、Cr2O3及CoO后的总含量相对于主成分100质量%为0.05质量%以上且0.3质量%以下即可。
另外,虽然试样No.95确认到若干色调不均,但试样No.87~94没有确认到色调不均,并且也没有损害外观。进而,试样No.87~94在进行热膨胀系数及四点弯曲强度的测定时,与不含有颜料成分时相比,热膨胀系数为+2ppb/℃、四点弯曲强度为-4MPa。由该结果可知,试样No.87~94能形成热膨胀系数小、机械强度优异、并且呈现能够抑制光的散射且抑制吸光的色调的堇青石质陶瓷。
Claims (6)
1.一种堇青石质陶瓷,其特征在于,相对于具有以氧化物换算量计含有Mg12.6质量%以上且14.0质量%以下、以氧化物换算量计含有Al33.4质量%以上且34.4质量%以下、及以氧化物换算量计含有Si52.0质量%以上且53.6质量%以下的组成范围的主成分100质量%,含有换算成氧化物时为4.5质量%以上且15.0质量%以下的Y、Yb、Er及Ce中的任一种作为副成分,并且堇青石、二硅酸盐及尖晶石作为晶相存在。
2.根据权利要求1所述的堇青石质陶瓷,其特征在于,将所述二硅酸盐的含量设为A、将所述尖晶石的含量设为B时,A和B的比率A/B为0.5以上且24.0以下。
3.根据权利要求1或权利要求2所述的堇青石质陶瓷,其特征在于,所述二硅酸盐的含量为4.5质量%以上且7.0质量%以下,所述尖晶石的含量为1.4质量%以上且3.3质量%以下。
4.根据权利要求1~3中任一项所述的堇青石质陶瓷,其特征在于,还含有颜料成分。
5.根据权利要求4所述的堇青石质陶瓷,其特征在于,含有Mn、Cr及CoCr作为所述颜料成分,并且Mn、Cr及Co分别换算成MnO2、Cr2O3及CoO后的总含量相对于所述主成分100质量%为0.05质量%以上且3质量%以下。
6.一种半导体制造装置用部件,其特征在于,其使用了权利要求1~5中任一项所述的堇青石质陶瓷。
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