CN102822116B - 半导体制造装置用耐腐蚀性构件及其制法 - Google Patents
半导体制造装置用耐腐蚀性构件及其制法 Download PDFInfo
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- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 3
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- 238000009434 installation Methods 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- 229910003440 dysprosium oxide Inorganic materials 0.000 claims description 2
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(iii) oxide Chemical compound O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims description 2
- ZXGIFJXRQHZCGJ-UHFFFAOYSA-N erbium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Er+3].[Er+3] ZXGIFJXRQHZCGJ-UHFFFAOYSA-N 0.000 claims description 2
- OWCYYNSBGXMRQN-UHFFFAOYSA-N holmium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ho+3].[Ho+3] OWCYYNSBGXMRQN-UHFFFAOYSA-N 0.000 claims description 2
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims description 2
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Abstract
秤量Yb2O3与SrCO3为摩尔比1:1，调制调合粉末。将该调合粉末单轴加压成形，制作为圆盘状成形体。将成形体在大气气氛中进行热处理，合成复合氧化物。将合成的复合氧化物用研钵粗粉碎，进行湿式粉碎。将粉碎后取出的浆料在氮气流中干燥，制为合成原料粉末。将该合成原料粉末单轴加压成形，制作为圆盘状成形体。将得到的成形体用热压法烧成，得到半导体制造装置用耐腐蚀性构件。该耐腐蚀性构件，由SrYb2O4晶相构成，开孔率为0.1%，NF3腐蚀速率值小于由Y2O3的晶相构成的。
Description
技术领域
本发明关于半导体制造装置用耐腐蚀性构件及其制法。
背景技术
半导体制造中实施干燥工序和等离子体喷涂等时所利用的半导体制造装置中，作为蚀刻、清洗用，使用的是反应性高的F、Cl系等离子体。因此，用于此种装置的构件必须有高耐腐蚀性，对于静电卡盘和加热器等与Si晶片接触的构件，需要更高耐腐蚀。作为应对此种需求的耐腐蚀性构件，专利文献1中公开了通过PVD法形成的Yb2O3和Dy2O3的薄膜。这些薄膜，在等离子体中的腐蚀速率较之于氧化铝烧结体等非常小。
专利文献1：日本专利特开2002-222803号公报
发明内容
但是，由于薄膜在成膜时内部易出现气孔和裂纹，因此等离子体易造成腐蚀，再由于与基材性质的差异和附着性问题造成的腐蚀以及重复使用所伴随的剥离等，可能对设备特性造成影响，用于静电卡盘等时存在问题。这些构件适宜使用烧结体，但上述的专利文献1中，虽然对通过PVD法形成的Yb2O3和Dy2O3的薄膜进行了评价，但没有对烧结体进行评价。此外，作为耐腐蚀性构件，虽然所知的有Y2O3和Al2O3的烧结体，但需要开发可以将腐蚀速率抑制得更小的烧结体材料。
本发明为解决此种课题，主要目的是提供较之于传统产品，腐蚀速率可抑制得更小的半导体制造装置用耐腐蚀性构件。
本发明者们着眼于以三氧化二钇为首的稀土类氧化物的高耐腐蚀性，追求更高耐腐蚀性，探索稀土类化合物后发现，第2族金属(除Mg以外)与稀土类元素(除La以外)的复合氧化物的耐腐蚀性极高，从而完成了本发明。
即，本发明的半导体制造装置用耐腐蚀性构件，由主晶相为第2族元素(除Mg以外)与第3族元素(除La以外)的复合氧化物构成。
此外，本发明的半导体制造装置用耐腐蚀性构件的制法是，将含有第2族元素(除Mg以外)与第3族元素(除La以外)的粉末成形为目标半导体制造装置用耐腐蚀性构件的形状，通过将该成形体热压烧成，得到主晶相为上述第2族元素与上述第3族元素的复合氧化物构成的耐腐蚀性构件。
根据本发明的半导体制造装置用耐腐蚀性构件，较之于传统产品的三氧化二钇和氧化铝，可将腐蚀速率抑制得更小，因此耐腐蚀性构件的发尘量减少，可长期承受半导体制造过程中使用的反应性高的F、Cl系等离子。此外，本发明的半导体制造装置用耐腐蚀性构件的制法适宜制造此种耐腐蚀性构件。
具体实施方式
本发明的半导体制造装置用耐腐蚀性构件，含有第2族元素(除Mg以外)与第3族元素(除La以外)的复合氧化物的晶相。
本发明的半导体制造装置用耐腐蚀性构件中，上述复合氧化物的晶相可以是主晶相。此外，作为复合氧化物中的第2族元素，基于容易制作复合氧化物的观点，优选Ca、Sr，特别优选Sr。此外，作为复合氧化物中的第3族元素，基于耐腐蚀性和容易制作复合氧化物的观点，优选Y、Yb、Ho、Dy、Er。另外，Mg与第3族元素的复合氧化物和第2族元素与La的复合氧化物目前并未所知。
本发明的半导体制造装置用耐腐蚀性构件中，除上述复合氧化物以外，也可存在第3族元素的氧化物的晶相。此种第3族元素的氧化物，不仅耐腐蚀性高，由于具有抑制上述复合氧化物的粒生长的效果，得到的耐腐蚀性构件的强度会提升。此种第3族元素的氧化物，优选为选自氧化镱、氧化钬、氧化钇、氧化铒以及氧化镝构成的群的至少1种。
本发明的半导体制造装置用耐腐蚀性构件中，优选开孔率在0.1％以下。开孔率是以纯水为介质通过阿基米德法测定的值。开孔率超过0.1％的话，腐蚀速率变高、强度下降，因此不理想。开孔率优选尽可能接近零。因此，并不特别存在下限值。
本发明的半导体制造装置用耐腐蚀性构件的制法是，将含有第2族元素(除Mg以外)与第3族元素(除La以外)的粉末成形为目标半导体制造装置用耐腐蚀性构件的形状，通过对该成形体进行热压烧成，得到主晶相为上述第2族元素与上述第3族元素的复合氧化物构成的上述耐腐蚀性构件。该制法适宜得到本发明的半导体制造装置用耐腐蚀性构件。
该制法中，上述粉末中，含有的第3族元素(除La以外)可以多于其与第2族元素(除Mg以外)反应形成复合氧化物的化学计量。这样，可以得到含有复合氧化物的晶相，还含有第3族元素的氧化物的晶相的耐腐蚀性构件。
此处，热压烧成优选在惰性气氛下进行。惰性气氛指的是不对氧化物原料的烧成产生影响的气氛即可，可举出例如，氮气氛和氩气氛、氦气氛等。此外，热压时的烧成温度以及冲压压力，只要是可以得到致密的烧结体的温度以及压力即可，可根据氧化物原料的种类适当设定。例如，烧成温度可设定为1500～１800℃间，冲压压力可设定为100～300kgf／cm2间。成形时的压力并无特别限制，适当设定为可保持形状的压力即可。另外，也可在令含有第2族元素(除Mg以外)与第3族元素(除La以外)的粉末中含有烧结助剂后，成形为规定的形状，将该成形体热压烧成。此时，较之于没有使用烧结助剂的情况，可以降低烧成温度，因此可以降低制造成本。但是，对耐腐蚀性有影响的助剂并不理想，理想的是例如，选自Mg、Ca以及Sr构成的群的至少1种的元素的氟化物，其耐腐蚀性高。
实施例
以下说明本发明的适宜的实施例。Yb2O3、Ho2O3、Y2O3原料使用纯度99.9％以上、平均粒径1μm以下的市售粉末。SrCO３原料使用纯度99.9％以上、平均粒径1μm以下的市售粉末。Al2O3原料使用纯度99.5％以上的平均粒径0.5μm的市售粉末。
[实施例1～8]
首先，调制合成原料粉末。即，秤量表1所示的稀土类氧化物与碳酸锶为表1所示的摩尔比，以异丙醇为溶剂，使用尼龙制的罐、的球石进行4小时湿式混合。取出混合后浆料，于氮气流中以110℃干燥。然后通过30目的筛网，制为调合粉末。接着，将该调合粉末以120kgf/cm2的压力进行单轴加压成形，制作厚20mm左右的圆盘状成形体。将成形体在大气气氛中于1000～1200℃下热处理12小时，除去CO2成分并进行复合氧化物的合成。将合成的复合氧化物用研钵粗粉碎，根据需要湿式粉碎至平均粒径1μm以下。湿式粉碎的溶剂为异丙醇，用一般的罐式球磨机粉碎。将粉碎后取出的浆料于氮气流中以110℃干燥，通过30目的筛网，制为合成原料粉末。
接着，将合成原料粉末成形为规定形状。即，将合成原料粉末以200kgf/cm2的压力单轴加压成形，制作厚10mm左右的圆盘状成形体。
最后，将得到的成形体烧成，得到半导体制造装置用耐腐蚀性构件。即，将圆盘状成形体装入烧成用石墨铸模，以规定的烧成温度烧成。烧成使用热压法。冲压压力为200kgf/cm2、烧成终结为止为Ar气氛。烧成温度(最高温度)下的保持时间为4小时。
[比较例1、2]
比较例1中使用Al2O3原料粉末、比较例2中使用Y2O3原料粉末替代实施例1～8的合成原料粉末，进行成形·烧成。另外，比较例1中烧成温度为1700℃、比较例2中烧成温度为1500℃。
[评价方法]
将得到的各烧结体加工为各种评价用，进行以下评价。各评价结果如表1所示。
(1)开孔率·体积密度
以纯水为介质通过阿基米德法测定。试料形状使用加工为3mm×4mm×40mm的。
(2)晶相评价
将烧结体用研钵粉碎，通过X射线衍射装置鉴定晶相。测定条件为CuKα，40kV，40mA，2θ＝10-70°，使用封入管式X射线衍射装置(ブルカ一·エイエツクスエス制D8ADVANCE)。
(3)腐蚀速率
对各烧结体表面进行镜面研磨，使用ICP等离子体耐腐蚀试验装置进行下述条件的耐腐蚀试验。通过将表面粗糙度计测定的非暴露面与暴露面的差除以试验时间，算出各材料的腐蚀速率。
ICP：800W，偏压：450W，导入气体：NF3／O2／Ar＝75／35／100sccm0.05Torr，暴露时间：10h，试料温度：室温
(4)强度
根据JISR1601，进行4点弯曲试验，算出强度。
(5)体积电阻率
根据JISC2141的方法，于室温大气中测定。试验片形状为厚1mm、主电极直径为20mm、保护电极内径为30mm、保护电极外径为40mm、外加电极直径为40mm，用银浆料形成各电极。施加电压为500V／mm，读取电压施加后1分钟时的电流，算出体积电阻率。
表1
[评价结果]
如表1所示，实施例1中，通过令Yb2O3与SrCO3以摩尔比50：50反应，合成氧化物原料SrYb2O4，将其按上述顺序成形、烧成，得到半导体制造装置用耐腐蚀性构件。该耐腐蚀性构件以SrYb2O4晶相为主晶相，腐蚀速率低于比较例1、2，因此可知耐腐蚀性优于比较例1、2。
实施例2中，通过令Yb2O3与SrCO3以摩尔比55：45反应，合成含有SrYb2O4与Yb2O3为摩尔比82：18的氧化物原料，实施例3中，通过令Yb2O3与SrCO3以摩尔比67：33反应，合成含有SrYb2O4与Yb2O3为摩尔比1：1的氧化物原料。将它们按上述顺序成形、烧成，得到的耐腐蚀性构件为SrYb2O4晶相与Yb2O3晶相混杂，腐蚀速率低于比较例1、2，因此可知耐腐蚀性优于比较例1、2。此外，实施例2、3的耐腐蚀性构件的强度高于实施例1，可认为这是由于存在Yb2O3，烧结粒径变得微细。另外，众所周知的是烧结粒径微细化后强度会提高。另外，实施例3的耐腐蚀性构件，体积电阻率高于实施例1，可认为这是由于存在有体积电阻率高于SrYb2O4的Yb2O3。
实施例4中，通过令Ho2O3与SrCO3以摩尔比50：50反应，合成氧化物原料SrHo2O4，实施例5中，通过令Ho2O3与SrCO3以摩尔比55：45反应，合成含有SrHo2O4与Ho2O3为摩尔比82：18的氧化物原料。将这些氧化物原料按上述顺序成形、烧成得到的半导体制造装置用耐腐蚀性构件，腐蚀速率低于比较例1、2，因此可知其耐腐蚀性优于比较例1、2。此外，实施例4、5的耐腐蚀性构件的强度低于实施例1，但体积电阻率较高。另外，实施例5的耐腐蚀性构件的强度高于实施例4，可认为这是由于实施例5中存在Ho2O3，因此烧结粒径较实施例4微细。
实施例6中，通过令Y2O3与SrCO3以摩尔比50：50反应，合成氧化物原料SrY2O4。将该氧化物原料按上述顺序成形、烧成得到的半导体制造装置用耐腐蚀性构件，腐蚀速率低于比较例1、2，因此可知其耐腐蚀性优于比较例1、2。
实施例7中，通过令Er2O3与SrCO3以摩尔比50：50反应，合成氧化物原料SrEr2O4。将该氧化物原料按上述顺序成形、烧成得到的半导体制造装置用耐腐蚀性构件，腐蚀速率低于比较例1、2，因此可知其耐腐蚀性优于比较例1、2。
实施例8中，通过令Dy2O3与SrCO3以摩尔比50：50反应，合成氧化物原料SrDy2O4。将该氧化物原料按上述顺序成形、烧成得到的半导体制造装置用耐腐蚀性构件，腐蚀速率低于比较例1、2，因此可知其耐腐蚀性优于比较例1、2。
比较实施例1、4、6～8，稀土类氧化物的耐腐蚀性顺序为SrYb2O4>SrEr2O4>SrHo2O4>SrDy2O4>SrY2O4。即，稀土类元素的原子量越大，耐腐蚀性越良好。此外，通过比较例2的Y2O3与实施例6的SrY2O4比较可判断，本发明的复合氧化物的耐腐蚀性高于Y2O3。
本申请以2010年3月30日提交的日本国专利申请第2010-079250号为优先权主张的基础，通过引用，其所有内容均包含于本说明书。
工业可利用性
本发明可用于半导体制造中的干燥工序和等离子体喷涂等实施时所利用的半导体制造装置。
Claims (7)
1.一种半导体制造装置用耐腐蚀性构件，含有除Mg以外的第2族元素和除La以外的第3族元素的复合氧化物的晶相，所述复合氧化物中的第2族元素为Sr，所述复合氧化物中的第3族元素为选自Y、Yb、Ho、Er以及Dy构成的群的1种。
2.根据权利要求1所述的半导体制造装置用耐腐蚀性构件，其中，所述复合氧化物的晶相为主晶相。
3.根据权利要求1或2所述的半导体制造装置用耐腐蚀性构件，其中，除所述复合氧化物以外，还存在第3族元素的氧化物的晶相。
4.根据权利要求3所述的半导体制造装置用耐腐蚀性构件，其中，所述第3族元素的氧化物为选自氧化镱、氧化钬、氧化钇、氧化铒以及氧化镝构成的群的至少1种。
5.根据权利要求1～4任意一项所述的半导体制造装置用耐腐蚀性构件，其中，开孔率在0.1％以下。
6.一种半导体制造装置用耐腐蚀性构件的制法，将含有除Mg以外的第2族元素和除La以外的第3族元素的粉末成形为目标半导体制造装置用耐腐蚀性构件的形状，通过将该成形体热压烧成，得到主晶相由所述第2族元素和所述第3族元素的复合氧化物构成的所述耐腐蚀性构件，所述复合氧化物中的第2族元素为Sr，所述复合氧化物中的第3族元素为选自Y、Yb、Ho、Er以及Dy构成的群的1种。
7.根据权利要求6所述的半导体制造装置用耐腐蚀性构件的制法，其中，所述粉末中，含有的所述除La以外的第3族元素多于其与所述除Mg以外的第2族元素反应形成所述复合氧化物的化学计量。
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- 2011-03-18 CN CN201180015911.6A patent/CN102822116B/zh active Active
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| JPWO2011122376A1 (ja) | 2013-07-08 |
| US8685313B2 (en) | 2014-04-01 |
| JP5767209B2 (ja) | 2015-08-19 |
| KR101371640B1 (ko) | 2014-03-06 |
| KR20120136373A (ko) | 2012-12-18 |
| WO2011122376A1 (ja) | 2011-10-06 |
| CN102822116A (zh) | 2012-12-12 |
| US20130022526A1 (en) | 2013-01-24 |
| TWI499574B (zh) | 2015-09-11 |
| TW201139324A (en) | 2011-11-16 |
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