CN110352182A - 半导体制造装置用加热器 - Google Patents

半导体制造装置用加热器 Download PDF

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CN110352182A
CN110352182A CN201880002671.8A CN201880002671A CN110352182A CN 110352182 A CN110352182 A CN 110352182A CN 201880002671 A CN201880002671 A CN 201880002671A CN 110352182 A CN110352182 A CN 110352182A
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ceramic matrix
heater
manufacturing apparatus
semiconductor manufacturing
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CN110352182B (zh
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山名启太
曻和宏
鸟居谦悟
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NGK Insulators Ltd
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Abstract

本发明的半导体制造装置用加热器是在AlN陶瓷基体的内部埋设有发热体的半导体制造装置用加热器，AlN陶瓷基体含有O、C、Ti、Ca、Y作为杂质元素，且Ti/Ca的质量比为0.13以上，在XRD图谱中没有确认到TiN相。

Description

半导体制造装置用加热器
技术领域
本发明涉及半导体制造装置用加热器。
背景技术
作为半导体制造装置用加热器，已知有如专利文献1中所示那样具有AlN陶瓷基体和埋设于该AlN陶瓷基体内部的发热体的半导体制造装置用加热器。这样的半导体制造装置用加热器用于对载置于AlN陶瓷基体的表面的晶片进行加热。此外，作为半导体制造装置用加热器，已知有如专利文献2中所示那样在AlN陶瓷基体的内部埋设有发热体和静电电极的半导体制造装置用加热器。
另一方面，在专利文献3、4中，作为AlN陶瓷基体，公开了一种在原料中配合CaO、TiO2等并进行烧结而得的AlN陶瓷基体。例如，文献3中公开了在原料中配合了2重量％的CaO、0.5重量％的TiO2的例子(Ti/Ca质量比为0.21)，文献4中公开了在原料中配合了1重量％的CaO、0.2重量％的TiO2的例子(Ti/Ca质量比为0.15)。
现有技术文献
专利文献
专利文献1：日本特开2008-153194号公报
专利文献2：日本特开2005-281046号公报
专利文献3：日本特开平8-157261号公报
专利文献4：日本特开平8-157262号公报
发明内容
发明要解决的课题
专利文献1、2的半导体制造装置用加热器中，如果从发热体向晶片泄漏电流，或从静电电极向晶片泄漏电流，则晶片会受到损伤。因此，优选将AlN陶瓷基体的体积电阻率控制为较高的值(例如7×108Ωcm以上)。然而，AlN陶瓷基体的体积电阻率有时会受杂质的影响而变动，难以控制体积电阻率。尤其是AlN陶瓷基体有时含有O、C、Ti、Ca、Y作为杂质元素，而关于这些元素会对体积电阻率产生什么样的影响，迄今未知。
此外，专利文献3、4的AlN陶瓷基体含有Ti、Ca，但由于Ti的配合量过多，因此在烧结时会生成体积电阻率极低(2～6×10-5Ωcm)的TiN相，从而存在AlN陶瓷基体整体的体积电阻率下降这样的问题。
本发明是为了解决这样的课题而提出的，其主要目的在于，对于使用了AlN陶瓷基体的半导体制造装置用加热器，即使AlN陶瓷基体含有O、C、Ti、Ca、Y作为杂质元素，在高温时也具有较高的体积电阻率。
解决课题的方法
本发明的半导体制造装置用加热器是在AlN陶瓷基体的内部埋设有发热体的半导体制造装置用加热器，
上述AlN陶瓷基体在含有O、C、Ti、Ca、Y作为杂质元素的同时，含有铝酸钇相作为结晶相，且Ti/Ca的质量比为0.13以上，并且在使用CuKα射线所测定的XRD图谱中没有确认到TiN相。
该半导体制造装置用加热器中，即使所使用的AlN陶瓷基体含有O、C、Ti、Ca、Y作为杂质元素，在高温时也具有较高的体积电阻率。关于其理由，考察如下。如果在铝酸钇相(例如Y4Al2O9(YAM)、YAlO3(YAL)等)中固溶Ca，则2价的Ca会置换3价的Y，从而因价数平衡关系而产生缺氧，氧离子传导通路增加，体积电阻率降低。另一方面，如果在铝酸钇相中固溶Ti，则4价的Ti会置换3价的Al，从而因价数平衡关系而填补缺氧，氧离子传导通路减少。如果Ti/Ca的质量比为0.13以上，则可认为由于Ti会适当地抑制由Ca引起的氧离子传导通路的增加，因此能够提高AlN陶瓷基体在高温时的体积电阻率。
此外，如果AlN陶瓷基体中的Ti过多，则会生成TiN。TiN在室温时的体积电阻率为2～6×10-5Ωcm，在600℃时为其室温时的体积电阻率的约1.1倍(文献1：日本陶瓷协会学术论文杂志(日本セラミックス協会学術論文誌)，99卷4号，pp286-291(1991)，文献2：电学论A(電学論A)，114卷12号，pp886-891(1994))。即，TiN是在室温和高温下体积电阻率均极低的化合物。因此，为了使AlN陶瓷基体在高温时具有较高的体积电阻率，优选不含TiN相。此外，如果生成TiN，则易于引起绝缘破坏，耐蚀性也会降低，因此，从这样的观点考虑，也优选AlN陶瓷基体不含TiN相。TiN相的XRD图谱刊登于JCPDS38-1420。如果在AlN陶瓷基体的XRD图谱中没有确认到TiN相，则由TiN引起的体积电阻率下降被抑制，因此能够提高AlN陶瓷基体在高温时的体积电阻率，还能抑制由TiN引起的绝缘破坏、耐蚀性下降。需说明的是，XRD图谱使用CuKα射线来测定(更详细地，使用CuKα射线在管电压40kV、管电流40mA的条件下进行测定)。
需说明的是，TiN相有可能以Al固溶于TiN中的相的形式存在，但即使在这种情况下，其体积电阻率也极低，认为有可能导致绝缘破坏、耐蚀性下降。
AlN陶瓷基体中的Ti/Ca的质量比优选为0.13以上0.5以下。AlN陶瓷基体的Ti含有率优选为18质量ppm以上95质量ppm以下。AlN陶瓷基体优选含有YAM和YAL，这种情况下，YAM/YAL的质量比优选为2.8以上5.3以下。AlN陶瓷基体中的O/C的质量比优选为48以上65以下。
本发明的半导体制造装置用加热器例如可以如下制作，即：使用含有O、C、Ti、Ca作为杂质元素的AlN原料粉末与作为烧结助剂的Y2O3粉末的混合粉末，在其内部埋设发热体并进行成形，从而制作成形体，并对该成形体进行烧成。优选AlN原料粉末中的O/C的质量比为20～30、Ti/Ca的质量比为0.13以上。如果这样，则在使用Y2O3粉末作为烧结助剂对AlN原料粉末进行烧成后的AlN陶瓷基体易于成为上述AlN陶瓷基体。这样的AlN原料粉末可以通过在含有O、C、Ti、Ca的Al2O3粉末中根据需要适量添加C、TiO2、CaO而得到粉末，并对所得到的粉末进行氮化、氧化来得到。AlN原料粉末中，优选含有0.70～0.75质量％的O、220～380质量ppm的C、18～95质量ppm的Ti、150～250质量ppm的Ca。
本发明的半导体制造装置用加热器中，AlN陶瓷基体在540℃时的体积电阻率优选为1.0×109Ωcm以上。如果这样，则能够充分减小从发热体向载置于AlN陶瓷基体的晶片的漏电流。
本发明的半导体制造装置用加热器中，AlN陶瓷基体的弯曲强度优选为300MPa以上，更优选为310MPa以上。如果这样，则充分地具有作为用于半导体制造装置的结构部件所要求的强度。
本发明的半导体制造装置用加热器中，AlN陶瓷基体的热导率优选为170W/m·K以上。如果这样，则载置于AlN陶瓷基体的晶片的均热性提高。
附图说明
图1是概略地显示静电卡盘加热器10的构成的纵截面图。
图2是表示O/C质量比与体积电阻率的关系的图表。
图3是表示Ti/Ca质量比与体积电阻率的关系的图表。
图4是表示YAM/YAL质量比与体积电阻率的关系的图表。
图5是显示实验例1的AlN烧结体的XRD图谱的图表。
图6是显示实验例7的AlN烧结体的XRD图谱的图表。
具体实施方式
以下，一边参照附图一边说明本发明的优选实施方式。图1是概略地显示静电卡盘加热器10的构成的纵截面图。
静电卡盘加热器10是本发明的半导体制造装置用加热器的一个例子，具有陶瓷基体12、发热体14和静电电极16。
陶瓷基体12是AlN制的圆盘部件，直径例如为200～450mm。陶瓷基体12的上表面成为用于载置晶片W的晶片载置面12a。陶瓷基体12是以AlN为主成分的基体，但含有O、C、Ti、Ca、Y作为杂质元素，同时含有铝酸钇相作为结晶相，且Ti/Ca的质量比为0.13以上，并且在XRD图谱中没有确认到TiN相。在XRD图谱中是否确认到TiN相，是通过将陶瓷基体12的XRD图谱与TiN相的全部峰进行比对来确定的。陶瓷基体12中的Ti/Ca的质量比优选为0.13以上0.5以下。陶瓷基体12的Ti含有率优选为18质量ppm以上95质量ppm以下。陶瓷基体12优选含有YAM和YAL作为铝酸钇相，这种情况下，YAM/YAL的质量比优选为2.8以上5.3以下。陶瓷基体12中的O/C的质量比优选为48以上65以下。
发热体14埋设于陶瓷基体12的内部。发热体14是将金属线圈通过一笔画的方法在晶片载置面12a的整面配线成预定的图案。发热体14不限于金属线圈，还可以采用例如带状、网状、片状等各种形态。作为发热体的材料，优选为Mo、W、Nb等高熔点导电材料。
静电电极16埋设于陶瓷基体12的内部。静电电极16配置于晶片载置面12a与发热体14之间。静电电极16的形状没有特别限定，除了例如平面状、网状之外，还可以是冲孔金属。作为静电电极16的材料，优选为Mo、W、Nb等高熔点导电材料。
接着，对静电卡盘加热器10的使用例进行说明。首先，将静电卡盘加热器10设置于未图示的腔室内。然后，在静电卡盘加热器10的晶片载置面12a上载置晶片W，通过对静电电极16施加电压而使静电电极16与晶片W之间产生约翰生·拉别克等静电吸附力，从而将晶片W吸附固定于晶片载置面12a上。此外，将外部端子连接于作为发热体14的金属线圈并施加电压而使发热体14发热，从而将晶片W加热至预定温度。在该状态下，对晶片W实施用于制作半导体芯片所需要的各种处理。处理结束后，结束对静电电极16施加电压、对发热体14施加电压，从晶片载置面12a上取下晶片W。
接着，对静电卡盘加热器10的制造例进行说明。首先，准备含有O、C、Ti、Ca作为杂质元素的AlN原料粉末。AlN原料粉末优选O/C的质量比为20～30、Ti/Ca的质量比为0.13以上。这样的AlN原料粉末可以通过在含有O、C、Ti、Ca的Al2O3粉末中根据需要适量添加C、TiO2、CaO而得到粉末，并对所得到的粉末进行氮化、氧化来获得。AlN原料粉末中优选含有0.70～0.75质量％的O、220～380质量ppm的C、18～95质量ppm的Ti、150～250质量ppm的Ca。
接下来，在所准备的AlN原料粉末中添加作为烧结助剂的Y2O3粉末并混合，制成混合粉末，通过喷雾干燥将该混合粉末制成颗粒。Y2O3以相对于混合粉末全体成为4.5～5.5质量％的方式添加。作为混合方法，可以采用使用了有机溶剂的湿式混合，也可以采用例如球磨、振动磨、干式袋混合等干式混合。
接下来，使用混合粉末的颗粒，在其内部埋设发热体14和静电电极16并进行成形，从而制作成形体。然后，对该成形体进行烧成，从而制成AlN烧结体。由此，得到静电卡盘加热器10。烧成方法没有特别限定，例如可以使用热压烧成等。在进行热压烧成的情况下，优选烧成时的最高温度(烧成温度)设为1700～1900℃、在烧成温度的保持时间设为0.5～100小时、压制压力设为5～50MPa、气氛设为氮气气氛或真空气氛(例如0.13～133.3Pa)。
根据以上说明的本实施方式的静电卡盘加热器10，由于O/C的质量比、Ti/Ca的质量比以及YAM/YAL的质量比均处于适当的数值范围内，因此陶瓷基体12的体积电阻率提高，能够减小从发热体14、静电电极16向载置于陶瓷基体12的晶片载置面12a上的晶片的漏电流。
需说明的是，本发明不受上述实施方式的任何限定，只要属于本发明的技术范围，就可以通过各种方式来实施，这是自不待言的。
例如，上述实施方式中，作为本发明的半导体制造装置用加热器，例示了静电卡盘加热器10，但也可以省略静电电极16，还可以将静电电极16替换为RF电极。
实施例
[实验例1～11]
对于各实验例，准备表1所示的AlN原料粉末。AlN原料粉末中所含的杂质元素的质量如下测定。杂质元素的质量分析依据JIS R1675来实施。具体而言，对于氧，取约0.05g左右样品至Ni胶囊中，投入石墨坩埚中，进行加热而使其燃烧，以CO的形式提取出来，并通过非色散红外检测器进行定量。对于碳，取约0.5g左右样品，加入助燃剂(Sn等)后进行加热而使其燃烧，通过非色散红外检测器对所产生的CO+CO2进行定量。对于金属杂质，取约1g样品，添加预定量的硝酸、盐酸、双氧水，通过ICP发光分析法对加热溶解后的溶液进行测定。
在所准备的AlN原料粉末中添加作为烧结助剂的Y2O3粉末，通过球磨机来进行混合，制成混合粉末，通过喷雾干燥将该混合粉末颗粒化。Y2O3以相对于混合粉末全体成为5质量％的方式添加。接着，使用混合粉末的颗粒，制作圆盘形状的成形体。然后，对该成形体进行热压烧成，从而制作AlN烧结体。在热压烧成中，将烧成时的最高温度(烧成温度)设为1850～1890℃、在烧成温度的保持时间设为2小时、压制压力设为20MPa、气氛设为氮气气氛。对得到的AlN烧结体中所含的杂质元素的质量、YAM的质量以及YAL的质量进行测定。
AlN烧结体中的杂质元素质量通过与AlN原料粉末中的杂质元素质量同样的方法来测定。YAM和YAL的质量如下测定。首先，通过粉末X射线衍射对10deg～120deg以上的高角侧进行精确测定，得到XRD图谱，采用获得的XRD图谱进行结晶相的鉴定，假定所鉴定出的结晶相来进行里特沃尔德解析，算出各结晶相的定量值。AlN烧结体在540℃时的体积电阻率如下测定。将使用Ag糊印刷电极部而成的样品(50mm×50mm×1mm)加热至540℃后，测定施加1kV电压时的1分钟后的电流值，从而求出体积电阻率。弯曲强度通过依据JIS R1601的四点弯曲试验来测定。热导率依据JIS R1611、通过激光闪光法在室温进行测定。将它们的结果示于表2。此外，将O/C质量比与体积电阻率的关系示于图2，将Ti/Ca质量比与体积电阻率的关系示于图3，将YAM/YAL质量比与体积电阻率的关系示于图4。
X射线衍射中，通过Bruker AXS制D8ADVANCE测定0.5g左右的粉末。测定条件设为：CuKα射线源、管电压40kV、管电流40mA。对测定结果进行里特沃尔德解析，进行结晶相的鉴定和定量化。将其结果示于图5、图6和表2。图5和图6是表示实验例1、7的XRD图谱的图表。从实验例1、7的XRD图谱鉴定出的结晶相为AlN、YAM、YAL，没有确认到TiN。对于实验例2～6、8、9，虽省略了XRD图谱的图示，但得到了同样的结果。
[表1]
[表2]
实验例1～9的AlN烧结体在含有O、C、Ti、Ca、Y作为杂质元素的同时含有YAM和YAL作为结晶相，Ti/Ca的质量比为0.13以上，并且在XRD图谱中没有确认到TiN相。这些AlN烧结体在540℃时的体积电阻率均高达1.0×109(＝1.0E+09)(Ωcm)以上。因此，在作为图1所示的静电卡盘加热器10的陶瓷基体12来使用时，能够减小从发热体14、静电电极16向载置于晶片载置面12a上的晶片W的漏电流。需说明的是，实验例1～9的AlN烧结体中，Ti/Ca的质量比均为0.13以上0.5以下，Ti含有率均为18质量ppm以上95质量ppm以下，YAM/YAL的质量比均为2.8以上5.3以下，O/C的质量比均为48以上65以下。
与此相对，实验例10、11的AlN烧结体中，540℃时的体积电阻率为4.5×108[Ωcm]以下的低值。实验例10、11中，尤其是Ti/Ca的质量比在适当范围之外，这被认为是体积电阻率下降的原因。即，实验例10、11中，由于Ti/Ca的质量比低至0.08、0.07，因此可认为：Ca向YAM、YAL中固溶而使氧离子传导通路增加的情形，优于Ti向YAM、YAL中固溶而使氧离子传导通路减少的情形，从而降低了体积电阻率。实验例10中，Ti含有率在适当范围之外、YAM/YAL的质量比在适当范围之外、O/C的质量比在适当范围之外等，也被认为是体积电阻率下降的原因。实验例11中，Ti含有率在适当范围之外、O/C的质量比在适当范围之外等，也被认为是体积电阻率下降的原因。
此外，实验例10、11的AlN烧结体的弯曲强度高达353MPa、328MPa，而实验例1～9的AlN烧结体的弯曲强度也为300MPa以上(详细而言为310MPa以上)，是与实验例10、11大体相同的高值。进一步，实验例10、11的AlN烧结体的热导率高达190W/m·K、180W/m·K，而实验例1～9的AlN烧结体的热导率也为170～180W/m·K，是与实验例10、11大体相同的高值。
上述实验例1～11中，实验例1～9相当于本发明的实施例，实验例10、11相当于比较例。
本申请将2018年2月8日提出的日本专利申请第2018-20637号作为优先权主张的基础，并通过引用将其全部内容包含在本说明书中。
产业上的可利用性
本发明能够用于静电卡盘加热器、陶瓷加热器等半导体制造装置用加热器中。
符号说明
10静电卡盘加热器，12陶瓷基体，12a晶片载置面，14发热体，16静电电极，W晶片。

Claims (8)

1.一种半导体制造装置用加热器，其是在AlN陶瓷基体的内部埋设有发热体的半导体制造装置用加热器，
所述AlN陶瓷基体在含有O、C、Ti、Ca、Y作为杂质元素的同时，含有铝酸钇相作为结晶相，且Ti/Ca的质量比为0.13以上，并且在使用CuKα射线所测定的XRD图谱中没有确认到TiN相。
2.如权利要求1所述的半导体制造装置用加热器，
所述Ti/Ca的质量比为0.5以下。
3.如权利要求1或2所述的半导体制造装置用加热器，
所述AlN陶瓷基体的Ti含有率为18质量ppm以上95质量ppm以下。
4.如权利要求1～3中任一项所述的半导体制造装置用加热器，
所述AlN陶瓷基体含有YAM和YAL且YAM/YAL的质量比为2.8以上5.3以下。
5.如权利要求1～4中任一项所述的半导体制造装置用加热器，
所述AlN陶瓷基体中的O/C的质量比为48以上65以下。
6.如权利要求1～5中任一项所述的半导体制造装置用加热器，
所述AlN陶瓷基体在540℃时的体积电阻率为1.0×109Ωcm以上。
7.如权利要求1～6中任一项所述的半导体制造装置用加热器，
所述AlN陶瓷基体的弯曲强度为300MPa以上。
8.如权利要求1～7中任一项所述的半导体制造装置用加热器，
所述AlN陶瓷基体的热导率为170W/m·K以上。
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