TWI540635B - Corrosion resistant member for semiconductor manufacturing apparatus and method for making the same - Google Patents

Corrosion resistant member for semiconductor manufacturing apparatus and method for making the same Download PDF

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TWI540635B
TWI540635B TW100110600A TW100110600A TWI540635B TW I540635 B TWI540635 B TW I540635B TW 100110600 A TW100110600 A TW 100110600A TW 100110600 A TW100110600 A TW 100110600A TW I540635 B TWI540635 B TW I540635B
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corrosion
resistant member
semiconductor manufacturing
sintered body
manufacturing apparatus
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TW100110600A
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TW201145386A (en
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Morimichi Watanabe
Yuji Katsuda
Toru Hayase
Asumi Jindo
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Ngk Insulators Ltd
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Description

用於半導體製造裝置的耐蝕構件及其製法
本發明係有關於用於半導體製造裝置的耐蝕構件及其製法。
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構件須具高耐蝕性，且靜電夾頭(electrostatic chuck)或加熱器(heater)等與矽晶圓(Si wafer)相接之構件係要求更高的耐蝕性。作為因應此種要求之耐蝕性構件，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Yb2O3或Dy2O3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甚小。
【先前技術文獻】
【專利文獻1】日本專利特開第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。對此等構件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Yb2O3或Dy2O3薄膜進行評定，但卻未對燒結體進行評定。作為耐蝕性構件雖已知有Y2O3或Al2O3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，其主要目的在於提供一種相較於迄今已知之燒結體，可將蝕刻速率抑制到更低程度之用於半導體製造裝置的耐蝕構件。
本發明者等人對稀土類氧化物燒結體作為用於半導體製造裝置的耐蝕構件的可適用性戮力進行研究的結果發現，當其中一部分的稀土類氧化物燒結體滿足特定物性時便可格外提升抑制蝕刻速率的效果，本發明即臻完成。
即，本發明之用於半導體製造裝置的耐蝕構件係由開孔隙率為0.3%以下且包括選自氧化鐿、氧化鈥、氧化鏑及氧化鉺所組成之群組的至少一種燒結體構成。
又，本發明之用於半導體製造裝置的耐蝕構件的製法為：將選自氧化鐿、氧化鈥、氧化鏑及氧化鉺所組成之群組的至少一種氧化物原料，(a)在未使用燒結助劑(sintering aid)的情況下，成形作為標的之用於半導體製造裝置的耐蝕構件的形狀後，在鈍氣環境下，於既定煅燒溫度下進行熱壓煅燒，或是(b)隨同選自Mg、Ca及Sr所組成之群組的至少一種元素之氟化物的燒結助劑，成形為作為標的之用於半導體製造裝置的耐蝕構件的形狀後，在鈍氣環境下，於低於所述既定煅燒溫度的溫度下進行熱壓煅燒，由此燒結所述氧化物原料而製得開孔隙率為0.3%以下的燒結體。
根據本發明之用於半導體製造裝置的耐蝕構件，由於相較於迄今已知之氧化釔(yttria)燒結體或氧化鋁燒結體可將蝕刻速率抑制到更低程度，故可降低耐蝕性構件的發塵量，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。此等材料其體積電阻率高達1×1015Ω‧cm以上，亦適用為靜電夾頭或加熱器的材料。又，本發明之用於半導體製造裝置的耐蝕構件的製法係適於製造此種耐蝕性構件，特別是添加燒結助劑時可於低溫下製得緻密體，故可降低製造成本。
本發明之用於半導體製造裝置的耐蝕構件係由開孔隙率為0.3%以下且包括選自氧化鐿、氧化鈥、氧化鏑及氧化鉺所組成之群組的至少一種燒結體構成。
作為燒結體係採用選自氧化鐿、氧化鈥、氧化鏑及氧化鉺所組成之群組的至少一種燒結體。此等係為稀土類氧化物燒結體，但即便是稀土類氧化物燒結體，例如氧化釓燒結體仍有緻密化的問題，氧化銪燒結體雖可緻密化但仍無法充分抑制蝕刻速率而不佳，氧化釹燒結體被保存於大氣中時仍會崩解而不佳。又，作為燒結體雖可採用選自所述群組的多種燒結體，惟亦可採用選自該群組的單一種燒結體。製作燒結體之際所採用的氧化物原料其雜質金屬量愈少愈佳，例如氧化物較佳為0.1wt%以下。
此處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0.3%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構件中，亦可使含有選自Mg、Ca及Sr所組成之群組的至少一種、以及O與F的至少一種的粒界相(grain boundary phase,晶界相)分散於燒結體中。例如亦可使含MgO的粒界相分散，或使含Ca、F的粒界相分散。此種粒界相係為與含Mg、Ca或Sr之燒結助劑(例如MgF2或CaF2等)共同煅燒時所生成者，若採用此種燒結助劑時則可降低煅燒溫度，由此可降低耗能而減少製造成本。
作為本發明之用於半導體製造裝置的耐蝕構件，可列舉由體積密度為8.8～9.2g/cm3的氧化鐿燒結體所構成作為較佳例子。此時，不僅可充分抑制蝕刻速率，又可使所述粒界相分散來提高強度。又可列舉由體積密度為8.1～8.4g/cm3的氧化鈥燒結體所構成作為較佳例子。
本發明之用於半導體製造裝置的耐蝕構件的製法為：將選自氧化鐿、氧化鈥、氧化鏑及氧化鉺所組成之群組的至少一種氧化物原料，(a)在未使用燒結助劑的情況下，成形為作為標的之用於半導體製造裝置的耐蝕構件的形狀後，在鈍氣環境下，於既定煅燒溫度下進行熱壓煅燒，或是(b)隨同選自Mg、Ca及Sr所組成之群組的至少一種元素的氟化物燒結助劑，成形為作為標的之用於半導體製造裝置的耐蝕構件的形狀後，在鈍氣環境下，於低於所述既定煅燒溫度的溫度下進行熱壓煅燒，由此燒結所述氧化物原料而製得開孔隙率為0.3%以下的燒結體。該製法係適於製得本發明之用於半導體製造裝置的耐蝕構件。
於此，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，只要是如可製得開孔隙率為0.3%以下之緻密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。更且，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。
【實施例】
以下對本發明之較佳實施例進行說明。Yb2O3、Er2O3、Ho2O3、Dy2O3、Gd2O3、Nd2O3、Eu2O3、Y2O3原料係使用純度99.9%以上、平均粒徑1μm以下的市售粉末。Al2O3原料使用純度99.5%以上、平均粒徑0.5μm的市售粉末。MgF2原料則使用視需求將純度99.9%以上的市售粉末預粉碎成0.5～1μm者，CaF2原料亦同上使用。此外，預粉碎係以異丙醇(isopropyl alcohol)為溶媒(溶劑)並使用二氧化鋯(zirconia)製球狀體，以球磨機(pot mill,罐形磨機)進行粉碎。
[實施例1～7，比較例1～6]
實施例1～5、比較例1～6中係使用單種稀土類氧化物原料來製造用於半導體製造裝置的耐蝕構件。具體而言，係首先以200kgf/cm2的壓力對表1所示之稀土類氧化物原料粉末進行單軸加壓成形，製作出φ50mm、厚度10mm左右的圓盤狀成形體並將其收納於煅燒用石墨模具中。接著，採用熱壓法在既定煅燒溫度(參照表1)下進行煅燒，即製得用於半導體製造裝置的耐蝕構件。煅燒時之擠壓壓力係設為200kgf/cm2、至煅燒結束為止設為氬氣環境、煅燒溫度(最高溫度)下的保持時間則設為4小時。
實施例6、7中係使用兩種稀土類氧化物原料來製作用於半導體製造裝置的耐蝕構件。具體而言，係首先秤量表1所示之兩種稀土類氧化物原料粉末，以異丙醇為溶媒，使用尼龍(nylon)製罐(pot)、φ5mm的氧化鋁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。使用該調合粉末，與實施例1～5、比較例1～6同樣進行成形及煅燒。此外，表1之表記「Yb2O3/25mol%Ho2O3」係指「100mol%的Yb2O3中添加有25mol%的Ho2O3的調合粉末」。
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。試料形狀則使用加工成與(2)相同形狀者。
(2)強度
予以加工成依據日本工業規格(JIS)R1601之形狀(3mm×4mm×40mm)來進行四點彎曲試驗，並算出強度。
(3)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))。
(4)粒界相評定
複合材料中的粒界相係由SEM/EDS(掃描式電子顯微鏡附加能量散射光譜儀)觀察燒結體之結晶相與經鏡面研磨之燒結體來評定。
(5)蝕刻速率
將各燒結體表面研磨成鏡面，並利用ICP電漿耐蝕試驗裝置進行下述條件的腐蝕試驗。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)
(6)化學分析
燒結體中的雜質金屬量(除Yb、Ho、Dy、Er、Mg、Ca、Sr以外之金屬元素)係依據感應耦合電漿(Inductively Coupled Plasma,ICP)發射光譜分析及感應耦合電漿(ICP)質譜分析。
(7)體積電阻率測定
採用依據日本工業規格C2141之方法，於大氣中、室溫下進行測定。試片形狀係製成φ50mm×0.5～1mm，並以銀形成各個電極，使主電極直徑為20mm，保護電極(guard electrode)內徑為30mm、外徑為40mm，施加電極直徑為40mm。將施加電壓設為2kV/mm，讀取施加電壓後1分鐘時的電流值並由該電流值算出室溫體積電阻率。
[評定結果]
如表1所示，實施例1～4中分別使用單種Yb2O3、Er2O3、Ho2O3、Dy2O3，並在煅燒溫度1500℃下進行緻密化的結果蝕刻速率為224～252nm/h，耐蝕性高。又實施例5中，在煅燒溫度1800℃下將Yb2O3緻密化的結果蝕刻速率為210nm/h，相較於實施例1耐蝕性更為提高。實施例5中耐蝕性提高的原因可推知為：在更高溫下進行煅燒使粒徑增大並相對減少低耐蝕的粒界面積，從而提高整體的耐蝕性。實施例1～5之材料其體積電阻率高達1×10J5Ω‧cm以上，係適用為靜電夾頭或加熱器的材料。實施例6係使用Yb2O3與Ho2O3之混合粉末，實施例7則使用Yb2O3與Er2O3之混合粉末，在煅燒溫度1500℃下進行緻密化的結果可見以下趨勢：與比較例1～6相比耐蝕性更為優異，與實施例1(單種)相比則強度更為提升，且體積電阻率亦增高。此等實施例6、7中，由XRD解析，Yb2O3之峰(peak)係向低角度側位移且未檢測出Ho2O3或Er2O3之峰，由此可知已分別形成Yb2O3－Ho2O3固溶體(Yb2O3－Ho2O3 ss(solid solution))、Yb2O3－Er2O3固溶體(Yb2O3－Er2O3 ss)。
另一方面，比較例1、2中，在1500、1700℃下分別煅燒Y2O3、Al2O3的結果兩者皆緻密化，然其耐蝕性係劣於實施例1～4。比較例3中，在1300℃下煅燒Yb2O3的結果氣孔之開孔隙率多達4.6%，故耐蝕性低於實施例1～4。比較例4、5中，在1500℃下分別煅燒Gd2O3、Eu2O3的結果，因Gd2O3其氣孔之開孔隙率多達2.5%，故耐蝕性劣於實施例1～4。此認為係Eu2O3其粒界之耐蝕性甚低，氟便經由粒界滲入燒結體內部而持續進行腐蝕。可推知「Yb2O3、Er2O3、Ho2O3、Dy2O3其粒界較Eu2O3更加高耐蝕」為稀土類氧化物中耐蝕性高的主因之一。比較例6中雖於1500℃下煅燒Nd2O3，惟保存於大氣下數天燒結體即崩解而無法評定。
[實施例8～15]
實施例8～15中，係採用稀土類氧化物與2A族元素(鹼土金屬)氟化物的調合粉末來製作用於半導體製造裝置的耐蝕構件。具體而言，係首先秤量表2所示之稀土類氧化物與2A族元素氟化物，以異丙醇為溶媒，使用尼龍製罐、φ5mm的氧化鋁球狀體進行濕式混合4小時。取出混合後之漿料，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200kgf/cm2的壓力對該調合粉末進行單軸加壓成形，製作出φ35mm、厚度10mm左右的圓盤狀成形體並將其收納於煅燒用石墨模具中。次之，採用熱壓法在既定煅燒溫度(表2)下進行煅燒，即製得用於半導體製造裝置的耐蝕構件。將煅燒時之擠壓壓力設為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。此外，表2之表記「Yb2O3/1vol%MgF2」係指「100vol%的Yb2O3中添加有1vol%的MgF2的調合粉末」。
將所得之各燒結體加工成各種評定用，並進行與先前相同的評定。將各評定結果示於表2。
實施例8、9中，於Yb2O3中添加表2所示之既定量的MgF2並在煅燒溫度1300℃下進行緻密化的結果，於燒結中MgF2與Yb2O3反應而在Yb2O3基體(matrix)中形成粒狀的MgO、YbOF相(參照圖1)。相較於實施例1儘管煅燒溫度較低，但仍可藉由添加氟化物來進行緻密的燒結，其耐蝕性係等同於實施例1。又，透過分散導入粒界相可使其強度高於實施例1。
實施例10、11中，於Yb2O3中添加表2所示之既定量的CaF2並在煅燒溫度1200～1300℃下進行緻密化的結果，在Yb2O3基體中形成以Ca、F為主的粒界相(參照圖2)。相較於實施例1儘管煅燒溫度較低，但仍可藉由添加氟化物來進行緻密的燒結，其耐蝕性係等同於實施例1。又，透過分散導入粒界相可使其強度高於實施例1。
實施例12、13中，於Ho2O3中添加表2所示之既定量的MgF2並在煅燒溫度1300℃下進行緻密化的結果，其與實施例8、9相同，於燒結中MgF2與Ho2O3反應而在Ho2O3基體中形成粒狀的MgO、HoOF相。實施例12、13相較於實施例3儘管煅燒溫度較低，但仍可藉由添加氟化物來進行緻密的燒結，其耐蝕性係等同於實施例3。又，透過分散導入粒界相可使其強度高於實施例3。
實施例14、15中，於Ho2O3中添加表2所示之既定量的CaF2並在煅燒溫度1300℃下進行緻密化的結果，其與實施例10、11相同，在Yb2O3基體中形成以Ca、F為主的粒界相。實施例14、15相較於實施例3儘管煅燒溫度較低，但仍可藉由添加氟化物來進行緻密的燒結，其耐蝕性係等同於實施例3。又，透過分散導入粒界相可使其強度高於實施例3。
實施例9～11、13～15之材料其體積電阻率高達1×1015Ω‧cm以上，係適用為靜電夾頭或加熱器的材料。又，實施例8、12亦具有同樣特性。
[實施例16～20]
實施例16、17中，係將實施例1中所得之燒結體(Yb2O3－1500℃煅燒成品)加工成厚度1mm，並分別在1100℃、1200℃下進行大氣退火(annealing)處理10小時、10小時。又，實施例18中，係將實施例5中所得之燒結體(Yb2O3－1800℃煅燒成品)加工成厚度1mm，實施例19、20中則將實施例6、7中所得之燒結體(分別為Yb2O3－Ho2O3固溶體、Yb2O3－Er2O3固溶體)加工成厚度1mm，並在1200℃下進行大氣退火處理10小時。
將所得之各大氣退火處理成品加工成各種評定用，進行與先前相同的評定(除強度以外)。將各評定結果示於表3。
實施例16～20中，相較於進行大氣退火處理前的燒結體，其耐蝕性皆提升且體積電阻率皆提高。又，相較於進行大氣退火處理前的燒結體，其皆轉為帶有白色的色調。具體而言，Yb2O3煅燒成品係由象牙色轉為白色(實施例16～18)，Yb2O3－Ho2O3固溶體由橙褐色轉為橙白色(實施例19)，Yb2O3－Er2O3固溶體則由紅褐色轉為桃紅色(粉紅色)(實施例20)。此可推知：煅燒後實施大氣退火處理可降低燒結體中所含的缺氧(oxygen deficiency)等並提高結晶性，由此即進一步提高耐蝕性、體積電阻率。
本申請案係以2010年3月30日所申請之日本專利申請第2010-079251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。
圖1為對在Yb2O3基體(matrix)中形成粒狀的MgO、YbOF相的燒結體的剖面(研磨面)進行拍攝後的反向散射電子像；以及圖2為對在Yb2O3基體中形成以Ca、F為主的粒界相的燒結體的剖面(研磨面)進行拍攝後的二次電子像。

Claims (5)

  1. 一種用於半導體製造裝置的耐蝕構件，係由開孔隙率為0.3%以下且包括選自氧化鐿、氧化鈥、氧化鏑及氧化鉺所組成之群組的至少一種燒結體構成，使含有選自Mg、Ca及Sr所組成之群組的至少一種、以及O與F的至少一種的粒界相分散於燒結體中，該粒界相係為與含Mg、Ca或Sr之燒結助劑共同煅燒時所生成者。
  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構件，其中，其由體積密度為8.8~9.2g/cm3的氧化鐿燒結體所構成。
  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構件，其中，其由體積密度為8.1~8.4g/cm3的氧化鈥燒結體所構成。
  4. 一種用於半導體製造裝置的耐蝕構件的製法，其特徵在於：將選自氧化鐿、氧化鈥、氧化鏑及氧化鉺所組成之群組的至少一種氧化物原料，隨同選自Mg、Ca及Sr所組成之群組的至少一種元素之氟化物的燒結助劑，成形為作為標的之用於半導體製造裝置的耐蝕構件的形狀後，在鈍氣環境下，於低於既定煅燒溫度的溫度下進行熱壓煅燒，由此燒結該氧化物原料而製得開孔隙率為0.3%以下的燒結體。
  5. 如申請專利範圍第4項所述之用於半導體製造裝置的耐蝕構件的製法，其中，燒結該氧化物原料而製得開孔隙率為0.3%以下的該燒結體後，於1000℃以上實施大氣退火處理。
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