TWI499574B - A corrosion resistant material for a semiconductor manufacturing apparatus and fabrication method thereof - Google Patents

A corrosion resistant material for a semiconductor manufacturing apparatus and fabrication method thereof Download PDF

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TWI499574B
TWI499574B TW100110602A TW100110602A TWI499574B TW I499574 B TWI499574 B TW I499574B TW 100110602 A TW100110602 A TW 100110602A TW 100110602 A TW100110602 A TW 100110602A TW I499574 B TWI499574 B TW I499574B
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corrosion
resistant material
semiconductor manufacturing
manufacturing apparatus
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TW100110602A
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TW201139324A (en
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Morimichi Watanabe
Yuji Katsuda
Toru Hayase
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Ngk Insulators Ltd
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Description

用於半導體製造裝置的耐蝕材料及其製法
本發明係有關於用於半導體製造裝置的耐蝕材料及其製法。
實施半導體製造中乾式法(dry process)或電漿塗佈(plasma coating)等之際所利用的半導體製造裝置係將反應性高的氟系、氯系電漿用於蝕刻(etching)、清潔(cleaning)，故此類裝置所利用的材料須具高耐蝕性，且靜電夾頭(electrostatic chuck)或加熱器(heater)等與矽晶圓(Si wafer)相接之材料係要求更高的耐蝕性。作為因應此種要求之耐蝕材料，專利文獻1中揭示有採用物理氣相沉積法(Physical Vapor Deposition,PVD)形成的Yb2 O3 或Dy2 O3 薄膜。此等薄膜其電漿下的蝕刻速率(etching rate)相較於氧化鋁燒結體等為甚小。
【先前技術文獻】
【專利文獻】
【專利文獻1】日本特開2002-222803號公報
惟，薄膜在形成時氣孔或裂痕(crack)容易存在於其內部而易於持續受電漿腐蝕，且進一步有因其與基材的性質不同或密合性的問題而使之持續受腐蝕，以及因伴隨重覆使用所致之剝離等而對裝置特性造成影響的可能性，對適用於靜電夾頭等而言是有問題的。對此等材料而言係以燒結體為佳，然上述專利文獻1中雖已對採用PVD法形成的Yb2 O3 或Dy2 O3 薄膜進行評定，但卻未對燒結體進行評定。又作為耐蝕材料雖已知有Y2 O3 或Al2 O3 燒結體，但仍需開發可將蝕刻速率抑制到更低程度的燒結體材料。
本發明為用以解決如此課題而開發者，其主要目的在於提供一種相較於習知之用於半導體製造裝置的耐蝕材料，可將蝕刻速率抑制到更低程度者。
本發明者等人著眼於以氧化釔(yttria)為首之稀土類氧化物的耐蝕性高，且為尋求更高耐蝕性而對稀土類化合物進行探究的結果發現2族(II族)金屬(Mg(鎂)除外)及稀土類元素(La(鑭)除外)的複合氧化物的耐蝕性極高，本發明即臻完成。
即，本發明之用於半導體製造裝置的耐蝕材料係由主相為2族元素(Mg除外)及3族(III族)元素(La除外)的複合氧化物所構成。
又，本發明之用於半導體製造裝置的耐蝕材料的製法為：將含有2族元素(Mg除外)及3族元素(La除外)的粉末成形為作為標的之用於半導體製造裝置耐蝕構件的形狀，並對該成形體進行熱壓煅燒，即製得由主相為所述2族元素及所述3族元素的複合氧化物構成的耐蝕材料。
根據本發明之用於半導體製造裝置的耐蝕材料，由於相較於習知之氧化釔或氧化鋁可將蝕刻速率抑制到更低程度，故可降低耐蝕材料的發塵量，並可長期耐受半導體製程中所使用之反應性高的氟系、氯系電漿。又，本發明之用於半導體製造裝置的耐蝕材料的製法係適於製造此種耐蝕材料。
本發明之用於半導體製造裝置的耐蝕材料係包含有2族元素(Mg除外)及3族元素(La除外)的複合氧化物的結晶相。
本發明之用於半導體製造裝置的耐蝕材料中，所述複合氧化物的結晶相亦可為主相。又、由複合氧化物的製作難易度觀點而言，複合氧化物中的2族元素較佳為Ca、Sr，特佳為Sr。又由耐蝕性與複合氧化物的製作難易度觀點而言，則複合氧化物中的3族元素較佳為Y(釔)、Yb(鏡)、Ho(鈥)、Dy(鏑)、Er(鉺)。此外，迄今仍未知有Mg與3族元素的複合氧化物或2族元素與La的複合氧化物。
本發明之用於半導體製造裝置的耐蝕材料中，除所述複合氧化物之外，還可存在3族元素的氧化物的結晶相。此種3族元素的氧化物其不僅耐蝕性高，還具有抑制所述複合氧化物晶粒成長的效果，故可提高所得之耐蝕材料的強度。此種3族元素的氧化物以設為選自氧化鏡、氧化鈥、氧化釔、氧化鉺及氧化鏑所組成之群組的至少一種為佳。
本發明之用於半導體製造裝置的耐蝕材料中，開孔隙率以0.1%以下為 佳。開孔隙率係為採用以純水為介質之阿基米得法(Archimedes’method)所測定的值。開孔隙率若超過0.1%時，則會使蝕刻速率升高或使強度降低而不佳。開孔隙率儘可能愈接近零愈佳，因此未特別存在下限值。
本發明之用於半導體製造裝置的耐蝕材料的製法為：將含有2族元素(Mg除外)及3族元素(La除外)的粉末成形為所要作之用於半導體製造裝置的耐蝕材料的形狀，並對該成形體進行熱壓煅燒，即製得由主相為所述2族元素及所述3族元素的複合氧化物所構成的耐蝕材料。該製法係適於製得本發明之用於半導體製造裝置的耐蝕材料。
於該製法中，所述粉末亦可含有多於3族元素(La除外)與2族元素(Mg除外)反應而形成複合氧化物之化學計算量的量。如此一來，即可製得含有複合氧化物的結晶相且進一步含有3族元素的氧化物的結晶相的耐蝕材料。
於此，熱壓煅燒以在鈍氣環境下實施為佳。鈍氣環境係指：只要是未對氧化物原料的煅燒造成影響的氣體環境即可，可列舉如氮氣環境、氬氣環境、氦氣環境等。又，熱壓時之煅燒溫度及擠壓壓力，只要是如可製得緻密之燒結體的溫度及壓力即可，可依據氧化物原料的種類來適當設定。例如，亦可將煅燒溫度設於1500~1800℃之間，擠壓壓力設於100~300kgf/cm2 之間。成形時之壓力並未特別限制，只要適當設為能保持形狀的壓力即可。更且，亦可在含2族元素(Mg除外)及3族元素(La除外)的粉末中添加燒結助劑(sintering aid)後成形為既定形狀，再對該成形體進行熱壓煅燒。於此情況下，相較於未使用燒結助劑的場合可降低煅燒溫度之故而能夠減少製造成本。惟，會對耐蝕性造成影響的助劑較為不佳，而例如選自Mg、Ca及Sr所組成之群組的至少一種元素的氟化物其耐蝕性高而較佳。
【實施例】
以下對本發明之較佳實施例進行說明。Yb2 O3 、Ho2 O3 、Y2 O3 原料係使用純度99.9%以上、平均粒徑1μm以下的市售粉末。SrCO3 使用純度99.9%以上、平均粒徑1μm以下的市售粉末。Al2 O3 原料則使用純度99.5%以上、平均粒徑0.5μm的市售粉末。
〔實施例1~8〕
首先調製合成原料粉末。即，以表1所示之莫耳比秤量表1所示的稀土類氧化物及碳酸鍶，以異丙醇為溶媒(溶劑)，使用尼龍(nylon)製罐(pot)、φ10mm的球狀體進行濕式混合4小時。取出混合後之漿料(slurry)，於氮氣氣流中、110℃下乾燥之，之後通過30網目(mesh)的篩網而製成調合粉末。接著，以120kgf/cm2 的壓力對該調合粉末進行單軸加壓成形，製作出φ50mm、厚度20mm左右的圓盤狀成形體。在大氣環境中、1000～1200℃下對成形體實施熱處理12小時來進行CO2 成分的去除及複合氧化物的合成。以研鉢及杵粗粉碎所合成的複合氧化物，並視需求予以濕式粉碎至平均粒徑1μm以下。濕式粉碎係以異丙醇為溶媒，並以一般的球磨機(pot mill,罐形磨機)進行粉碎。在氮氣氣流中、110℃下對粉碎後取出的漿料進行乾燥，再通過30網目(mesh)的篩網即製成合成原料粉末。
其次，將合成原料粉末成形為既定形狀。亦即，以200kgf/cm2 的壓力對合成原料粉末進行單軸加壓成形來製作φ50mm、厚度10mm左右的圓盤狀成形體。
最後煅燒所得之成形體，即製得用於半導體製造裝置的耐蝕材料。亦即，將圓盤狀成形體收納於煅燒用石磨模具中，並在既定煅燒溫度下進行煅燒。煅燒係採用熱壓法。將擠壓壓力設為200kgf/cm2 ，至煅燒結束為止設為氬氣環境，煅燒溫度(最高溫度)下的保持時間設為4小時。
[比較例1、2]
比較例1係使用Al2 O3 原料粉末、比較例2則使用Y2 O3 原料粉末來取代實施例1～8之合成原料粉末並進行成形及煅燒。此外，比較例1係將煅燒溫度設為1700℃，比較例2則將煅燒溫度設為1500℃。
[評定方法]
將所得的各燒結體加工成各種評定用，並進行以下評定。將各評定結果示於表1。
(1)開孔隙率/體積密度
係採用以純水為介質之阿基米得法來測定。試料形狀係使用加工成3mm×4mm×40mm者。
(2)結晶相評定
以研缽及杵(mortar and pestle)粉碎燒結體，並利用X光繞射裝置鑑定結晶相。測定條件係設為CuKα、40kV、40mA、2θ=10－70°(使用密封管式(sealed-tube type)X光繞射裝置(Bruker AXS製D8 ADVANCE))。
(3)蝕刻速率
將各燒結體表面研磨成鏡面，並利用ICP(感應耦合電漿(Inductively Coupled Plasma))電漿耐蝕試驗裝置進行下述條件的耐蝕試驗。將由表面粗度計所測定之非暴露面與暴露面間的段差除以試驗時間來算出各材料的蝕刻速率。
(ICP：800W、偏壓：450W、導入氣體：NF3 /O2 /Ar=75/35/100sccm,0.05Torr、暴露時間：10h，試料溫度：室溫)
(4)強度
依據日本工業規格(JIS)R1601來進行四點彎曲試驗，並算出強度。
(5)體積電阻率
採用依據日本工業規格(JIS)C2141之方法，於室溫下、大氣中進行測定。試片形狀係製成φ50mm、厚度1mm，並以銀糊料(paste)形成各個電極，使主電極直徑為20mm，保護電極(guard electrode)內徑為30mm，保護電極外徑為40mm，施加電極直徑為40mm。將施加電壓設為500V/mm，讀取施加電壓後1分鐘時的電流值並算出室溫體積電阻率。
[評定結果]
如表1所示，實施例1係使Yb2 O3 與SrCO3 (莫耳比50：50)反應來合成氧化物原料SrYb2 O4 ，並以上述程序對其進行成形、煅燒而製得用於半導體製造裝置的耐蝕材料。該耐蝕材料係以SrYb2 O4 結晶相為主相，且其蝕刻速率係低於比較例1、2，故其耐蝕性較比較例1、2更為優異。
實施例2係使Yb2 O3 與SrCO3 (莫耳比55：45)反應來合成含有SrYb2 O4 與Yb2 O3 (莫耳比82：18)的氧化物原料，實施例3則使Yb2 O3 與SrCO3 (莫耳比67：33)反應來合成含有SrYb2 O4 與Yb2 O3 (莫耳比1：1)的氧化物原料。以上述程序對此等進行成形、煅燒所得之耐蝕材料係混有SrYb2 O4 結晶相與Yb2 O3 結晶相，且其蝕刻速率因係低於比較例1、2，由此可知其耐蝕性較比較例1、2更為優異。又實施例2、3之耐蝕材料其強度高於實施例1，此認為是因存有Yb2 O3 而使得燒結粒徑微小化。此外，眾所皆知當燒結粒徑微小化時可提高強度。更且，實施例3之耐蝕材料其體積電阻率高於實施例1，此認為是因存有體積電阻率高於SrYb2 O4 的Yb2 O3 之故。
實施例4係使Ho2 O3 與SrCO3 (莫耳比50：50)反應來合成氧化物原料SrHo2 O4 ，實施例5則使Ho2 O3 與SrCO3 (莫耳比55：45)反應來合成含有SrHo2 O4 與Ho2 O3 (莫耳比82：18)的氧化物原料。以上述程序對此等氧化物原料進行成形、煅燒所得之用於半導體製造裝置的耐蝕材料其蝕刻速率係低於比較例1、2，由此可知其耐蝕性較比較例1、2更為優異。又實施例4、5之耐蝕材料其強度雖低於實施例1，但體積電阻率卻較高。此外，實施例5之耐蝕材料其強度高於實施例4，此認為是因實施例5中存有Ho2 O3 而使得其燒結粒徑較實施例4更加微小化。
實施例6係使Y2 O3 與SrCO3 (莫耳比50：50)反應來合成氧化物原料SrY2 O4 。以上述程序對該氧化物原料進行成形、煅燒所得之用於半導體製造裝置的耐蝕材料其蝕刻速率係低於比較例1、2，由此可知其耐蝕性較比較例1、2更為優異。
實施例7係使Er2 O3 與SrCO3 (莫耳比50：50)反應來合成氧化物原料SrEr2 O4 。以上述程序對該氧化物原料進行成形、煅燒所得之用於半導體製造裝置的耐蝕材料其蝕刻速率係低於比較例1、2，由此可知其耐蝕性較比較例1、2更為優異。
實施例8係使Dy2 O3 與SrCO3 (莫耳比50：50)反應來合成氧化物原料SrDy2 O4 。以上述程序對該氧化物原料進行成形、煅燒所得之用於半導體製造裝置的耐蝕材料其蝕刻速率係低於比較例1、2，由此可知其耐蝕性較比較例1、2更為優異。
若比較實施例1、4、6～8，則稀土類氧化物之耐蝕性的順序為：SrYb2 O4 ＞SrEr2 O4 ＞SrHo2 O4 ＞SrDy2 O4 ＞SrY2 O4 。即，稀土類元素的原子量愈大則耐蝕性愈良好。又由比較例2之Y2 O3 與實施例6之SrY2 O4 的比較結果可判斷：本發明之複合氧化物較Y2 O3 更為高耐蝕。
本申請案係以2010年3月30日所申請之日本專利申請第2010-079250號為主張優先權之基礎，由於引用其所有內容皆含於本說明書中。
【產業上之可利用性】
本發明可利用於實施半導體製造中之乾式法或電漿塗佈等之際所使用的半導體製造裝置。

Claims (7)

  1. 一種用於半導體製造裝置的耐蝕材料，其係包含有Mg除外之2族元素及La除外之3族元素的複合氧化物的結晶相，其中所述複合氧化物中的2族元素為Sr，所述複合氧化物中的3族元素則為選自Y、Yb、Ho、Er及Dy所構成之群組中的一種。
  2. 如申請專利範圍第1項所述之用於半導體製造裝置的耐蝕材料，其中所述複合氧化物的結晶相係為主相。
  3. 如申請專利範圍第1項所述之用於半導體製造裝置的耐蝕材料，其中除所述複合氧化物之外，還存有3族元素的氧化物的結晶相。
  4. 如申請專利範圍第3項所述之用於半導體製造裝置的耐蝕材料，其中所述3族元素的氧化物係為選自氧化鐿、氧化鈥、氧化釔、氧化鉺及氧化鏑所組成之群組的至少一種。
  5. 如申請專利範圍第1項至第4項任一項所述之用於半導體製造裝置的耐蝕材料，其中所述耐蝕材料的開孔隙率為0.1%以下。
  6. 一種用於半導體製造裝置的耐蝕材料的製法，其特徵為：將含有Mg除外之2族元素及La除外之3族元素的粉末成形為作為標的之用於半導體製造裝置耐蝕構件的形狀，並對該成形體進行熱壓煅燒，即製得由主相為由所述2族元素及所述3族元素的複合氧化物所構成的所述耐蝕材料，其中所述複合氧化物中的2族元素為Sr，所述複合氧化物中的3族元素則為選自Y、Yb、Ho、Er及Dy所構成之群組中的一種。
  7. 如申請專利範圍第6項所述之用於半導體製造裝置的耐蝕材料的製法，其中所述粉末係含有多於所述La除外之3族元素與所述Mg除外之2族元素反應而形成所述複合氧化物之化學計算量的量。
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