TWI737801B - 電漿處理裝置用碳化矽構件及其製造方法 - Google Patents

電漿處理裝置用碳化矽構件及其製造方法 Download PDF

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TWI737801B
TWI737801B TW106129893A TW106129893A TWI737801B TW I737801 B TWI737801 B TW I737801B TW 106129893 A TW106129893 A TW 106129893A TW 106129893 A TW106129893 A TW 106129893A TW I737801 B TWI737801 B TW I737801B
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sic
silicon carbide
weight
plasma
sintered body
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TW106129893A
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TW201833061A (zh
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鈴木智久
宮原陸人
佐佐木優
後藤哲也
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日商北陸成型工業股份有限公司
國立大學法人東北大學
鈴木智久
宮原陸人
佐佐木優
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Abstract

本發明係其目的為以低成本提供耐久性佳的電漿處理裝置用碳化矽構件。 　　本發明之電漿處理裝置用碳化矽構件係混合將金屬系雜質削減至超過20ppm、70ppm以下，且，含有50ppm以下Al雜質的平均粒徑為0.3~3μm之α構造碳化矽粉末、與由0.5~5重量份之B4 C所構成的助燒結劑或由Al2 O3 及Y2 O3 之合計量為3~15重量份所構成的助燒結劑，將已混合的α構造碳化矽粉末及助燒結劑在氬氣環境爐內或高頻感應加熱爐內進行燒結後，加工已得到的燒結體而得。

Description

電漿處理裝置用碳化矽構件及其製造方法
本發明係關於用以製造各種之半導體裝置之電漿處理裝置用碳化矽構件及其製造方法。
先前，在半導體裝置之製造步驟係進行利用了電漿的半導體晶圓之成膜處理或蝕刻處理，又，進行藉由氟系氣體所致的腔室清洗。
第1圖係反應性離子蝕刻(Reactive Ion Etching：RIE)裝置之剖面圖，具備施加蝕刻處理於半導體晶圓1的反應室2，於此反應室2之上下係相對地配置有噴頭型上部電極3與下部電極4。
作為原理係於反應室2內供給蝕刻氣體，若由高頻電源10施加電力於下部電極4，則在反應室2產生電漿。在如第1圖般的平行平板型RIE裝置之情況，若由高頻電源10施加電力於下部電極4，則於半導體晶圓1與電漿之間產生自偏壓電位，電漿中之離子或自由基等之活性種被加速於半導體晶圓1之方向(垂直於晶圓面的方向)。活性種係藉由依濺鍍所致的物理上的效果和化學反應效果，因為僅於垂直於半導體晶圓1之晶圓面的方向進行蝕刻(向異性蝕 刻)，所以可進行高精度微細加工者。
在蝕刻半導體晶圓1時，首先藉由連接於排氣板7之前的真空泵(無圖示)，將反應室2內作為真空狀態，由噴頭型上部電極3供給蝕刻氣體。
噴頭型上部電極3為圓盤狀，具有中空部5同時於下面係形成多數之氣體供給孔6為形成至蓮蓬狀。蝕刻氣體係成為由蝕刻氣體供給源(無圖示)首先供給於中空部5，以均等的流量通過氣體供給孔6而向反應室2內供給。
蝕刻氣體供給後，由高頻電源10施加電力於下部電極4，在反應室2產生電漿。藉由電漿中之活性種，半導體晶圓1被蝕刻。
半導體晶圓1係藉由被設置於下部電極4之上部的圓盤狀之靜電吸盤8(Electrostatic Chuck：ESC)而以靜電吸附保持，於靜電吸盤8之上面之周圍係設有環狀之邊緣環9。 邊緣環9係在蝕刻半導體晶圓1時，以活性種為在半導體晶圓1之周緣部以相對於鉛直方向(垂直於晶圓面的方向)而言不偏向之方式調整電場而設置者。
於專利文獻1(日本特開2007-112641號公報)係記載有其目的為提供相對於高電漿密度而言具備耐電漿性的聚焦環(邊緣環)，於氧化釔粉末、鋁粉末之混合粉末加入有機黏著劑而混練、成形後，以氫氣環境或惰性環境、1520℃以下之溫度燒結而得的燒結複合體所形成的比阻抗(電阻率)為未達109Ω‧cm的聚焦環。
於專利文獻2(日本特開平11-217268號公報)係 記載有一種電漿裝置用SiC燒結體，其係耐電漿性優異，因粒子脫落所致的粒子污染少的電漿裝置用SiC燒結體，其特徵為密度為2.7g/cm3以上，結晶粒徑之平均值為20μm以上，熱傳導率為80W/m‧K以上，電阻率為10-2~102Ω‧cm，於實施例3及5係開示有將α構造碳化矽(以下稱為「α-SiC」。)設為主原料者，詳細地說明實施例1、2及比較例1、2任一均將β構造碳化矽(以下稱為「β-SiC」。)設為主原料者，關於將α-SiC設為主原料者之特性係除了表1所記載的事項以外係不清楚，關於游離碳含有率係高於其他實施例或比較例，關於電阻率係實施例3表示0.4Ω‧cm、實施例5表示5.0Ω‧cm之高的值，所以未成為具有特別優異的特性的燒結體。
又，實施例3係儘管以最高溫之2400℃燒結，但密度頂多停在3.1g/cm3，而且，因為結晶粒徑小於實施例1、2，所以電荷容易被累積，耐電漿性變差。
於專利文獻3(日本特開2003-95744號公報)係雖然記載於段落0008「如試料No.2~試料No.13所示，可了解本發明之碳化矽燒結體係緻密且實質上無氣孔，YAG相為微細地分散的強度、硬度優異的燒結材料。」(第5欄31~34行)及「將試料No.2~試料No.13及試料No.16或試料No.17之使用本發明之碳化矽燒結體的半導體製造用構件安裝於半導體製造用機器時，因為氣孔所致的散射顯著地被壓制，所以裝置精度提昇，可確認半導體製造效率之改善。」(第6欄35~39行)，但是如於同段落記載之「碳化 矽之結晶部係在α相、β相、α+β複合相之中，無關哪一相，顯現同等之物性值。」(第5欄36~38行)，未顯現對α相之碳化矽結晶相所構成的燒結體為特別優異之認識。
更進一步，最近係以電漿耐性高的碳化矽(以下稱為「SiC」。)形成的邊緣環亦普及，但為了防止反應室2內之金屬污染，所以採用由純度高的化學氣相沈積(Chemical Vapor Deposition：CVD)法所致的β-SiC或以CVD法製作的SiC粉末之熱壓燒結體，而且該主原料為β-SiC。
然後，將α-SiC設為主原料的SiC構件係相較於將使用CVD法的β-SiC設為主原料的SiC構件而言鐵等之金屬系雜質多，因為反應室內污染產生，所以不太有打算將α-SiC作為電漿處理裝置用構件而使用的想法，電漿耐性亦不被詳細地調查。
於專利文獻4(日本特開平10-120466號公報)係開示可使用用在半導體製造之電漿蝕刻裝置的高耐蝕性碳化矽質構件，其特徵為由α-SiC之含量為90重量%以上之燒結體所構成者。
於專利文獻5(日本特開2001-7082號公報)係開示耐電漿性優異，可謀求長壽命化的電漿蝕刻用電極板，其特徵為以將6H型之α-SiC設為主體的碳化矽燒結體所形成者。
但是，專利文獻4之物係使用鐵之含量為1ppm以下、鋁之含量為5ppm以下、鈣之含量為3ppm以下之金屬系雜質非常少者，在比較例1所示的包含18ppm Al的α-SiC係設 為重量減少率大(參照請求項1，段落0039~0040及表1)。
又，在專利文獻5係作為原料SiC粉末，使用金屬元素含量合計為40ppm以下，理想為30ppm以下，更理想為20ppm以下，最理想為10ppm以下者為最佳(段落0027)。
[先前技術文獻] [專利文獻]
[專利文獻1]日本特開2007-112641號公報
[專利文獻2]日本特開平11-217268號公報
[專利文獻3]日本特開2003-95744號公報
[專利文獻4]日本特開平10-120466號公報
[專利文獻5]日本特開2001-7082號公報
記載於專利文獻1的邊緣環係比阻抗(電阻率)為未達109Ω‧cm之非常大的程度，關於雜質之擴散未驗證。然後，關於相較於以SiC形成的邊緣環而言，電漿耐性是否較優異亦不清楚。
又，以SiC形成的邊緣環係相較於以多晶矽或SiO2等形成的邊緣環而言，在電漿耐性或純度之高度等之面具有優異的特性，但為了防止反應室2內之金屬污染，採用以純度高的CVD法所致的SiC或以CVD法作成的β-SiC粉末之 熱壓燒結體，所以生產成本相較於以多晶矽或SiO2等形成的邊緣環而言，花費接近10倍，在性能之比例上非常昂貴。
更進一步，以此等之CVD法所致的SiC或將以CVD法作成的β-SiC粉末進行熱壓的SiC係不僅金屬系雜質為由1位數至2位數以上之少的0.1ppm以下之超高純度，而且電漿耐性未高到及於非常昂貴的比例，所以成為推高運轉成本的主要原因，又，在使用以將α-SiC設為主體的碳化矽燒結體形成的電漿蝕刻裝置用構件時係有必要更提昇耐電漿性。
本發明係其目的為解決如此的問題，可以較低成本製作，且，提供電漿耐性高的SiC構件及該製造方法。
關於請求項1的發明之電漿處理裝置用碳化矽構件係其特徵為由α構造碳化矽與氧化物系助燒結劑之燒結體所構成，前述α構造碳化矽中在燒結前金屬系雜質之含量為超過20ppm、70ppm以下，Al雜質之含量為超過20ppm、50ppm以下，且，SiO2之含量為0.3%以下，前述氧化物系助燒結劑由Al2O3與Y2O3所構成，該合計量為3~15重量份，且，Y2O3之重量為Al2O3之重量之1~2倍，於α構造碳化矽結晶之晶界存在有YAM相成分。
藉由關於請求項1的發明之電漿處理裝置用碳化矽構件，則不僅由α構造碳化矽與氧化物系助燒結劑之燒結體所構成，而且鐵等之金屬系雜質不對電漿處理裝置帶來不良影響，可廉價地製造電漿耐性高的構件，前述α構造碳化矽中在燒結前金屬系雜質之含量為超過20ppm、70ppm以下，Al雜質之含量為超過20ppm、50ppm以下，且，SiO2之含量為0.3%以下，。
然後，由於氧化物系助燒結劑由Al2O3與Y2O3所構成，該合計量為3~15重量份，且，Y2O3之重量為Al2O3之重量之1~2倍，於α構造碳化矽結晶之晶界存在有YAM相成分，故電漿處理裝置用碳化矽構件之耐電漿特性可成為更良好者。
因此，可提昇以邊緣環為首的各種電漿處理裝置內所使用的碳化矽構件之耐久性，且，可實現量產化及低成本化。
1:半導體晶圓
2:反應室
3:噴頭型上部電極
4:下部電極
5:中空部
6:氣體供給孔
7:排氣板
8:靜電吸盤
9:邊緣環
10:高頻電源
[第1圖]反應性離子蝕刻裝置之剖面圖。
[第2圖]表示電漿照射時間和每單位表面積之質量減少量之關係的線圖。
[第3圖]關於本發明的將Al2O3及Y2O3作為助燒結材料的α-SiC燒結體之X光繞射圖。
[第4圖]表示現在作為邊緣環而採用的純正品(CVD-SiC)與由本發明之燒結體所構成的邊緣環而透過蝕刻而形成於多層層合膜的孔之剖面形狀的圖。
以下，藉由實施例而說明本發明之實施形態(邊緣環之製造步驟)。
[實施例1] <第1步驟>
微量地包含週期表第4列之I~VIII族之各元素及該各元素之氧化物、碳化物、氮化物或硼化物等之雜質(以下，稱為「第4列金屬系雜質」。)，而且自由之SiO2成分成為0.3%以下以方式進行化學洗淨，作為主原料採用平均粒徑為0.6μm之α-SiC(純度98.5%左右者)。
然後，關於各式各樣之主原料樣本，分析第4列金屬系雜質或Al雜質等之金屬系雜質的結果，該含量係在全體為37~70ppm、在Al雜質為28~45ppm、Al以外之金屬系雜質為9~25ppm。
接著作為α-SiC之助燒結劑，準備純度為99%以上且平均粒徑為1μm以下之B4C原料粉末。
在相對於上述α-SiC原料粉末而言調配0.5重量份、1.5重量份、2重量份、3重量份及5重量份助燒結劑的B4C的5 種調配粉末，各自加入助成形劑的丙烯酸系之水溶性黏著劑3重量份與作為溶媒之純水。
<第2步驟>
將此等藉由尼龍製之球磨機鍋和尼龍塗覆球，由已粉碎混合的漿液透過噴霧乾燥器而作成造粒粉末，更進一步，將此造粒粉末以加壓力1000kg/cm2進行壓製成形，作成5種50mm平方之測試片。
<第3步驟>
將5種測試片以真空環境加熱脫脂後，放入氬環境爐內，以2160℃之溫度燒結，得到5種燒結體。
計測此等之密度的結果，可了解任一之測試片均成為相對於理論密度而言的燒結體之相對密度為98.1%以上(1.5重量份調配B4C者之比重為3.14以上)之緻密的燒結體。
尚，關於理論密度係將各調配成分之比重作為SiC=3.21、Al2O3=3.987、Y2O3=5.01、B4C=2.52計算原料粉末之密度，算出燒結體之相對密度。
<第4步驟>
外徑350mm左右、內徑295mm左右，厚度5mm左右之邊緣環係藉由加工相稱於該的大小之燒結體而製作。
[實施例2] <第1步驟>
準備與在實施例1使用相同的α-SiC原料粉末和作為α-SiC之助燒結劑之一成分的Al2O3粉末，純度為99.99%以上且平均粒徑為0.5μm之微粉末。
更進一步，準備作為α-SiC之助燒結劑之其他成分的Y2O3粉末，純度為99.9%以上且平均粒徑為1μm以下之微粉末。
又，亦準備純度為99.99%之Al2O3及純度為99.9%之Y2O3之平均粒徑均為0.5μm以下之微粉末。
相對於上述α-SiC原料粉末100重量份、Al2O3原料粉末2.5重量份及Y2O3原料粉末5重量份所構成的調配粉末而言，加入助成形劑的丙烯酸系之水溶性黏著劑3重量份與作為溶媒之純水。
<第2步驟>
與實施例1相同，由已粉碎混合此等的漿液透過噴霧乾燥器而作成造粒粉末，以加壓力1000kg/cm2進行壓製成形，作成50mm平方之測試片。
<第3步驟>
將該測試片以真空環境加熱脫脂後，放入氬環境之高頻感應加熱爐內，以1860℃之溫度燒結，得到燒結體。
計測此等之密度的結果，可了解成為燒結體之比重為3.16(相對密度=96.3%)之緻密的燒結體。
又，將已使用Al2O3之平均粒徑為0.5μm且Y2O3之平均粒徑為0.5μm以下之微粉末的成形體以電阻加熱方式之氬環境爐燒結的結果，可在1800~1900℃之較低溫度範圍燒結，可得到比重為3.18(相對密度=97%)之緻密燒結體。
<第4步驟>
外徑350mm左右、內徑295mm左右，厚度5mm左右之邊緣環係藉由加工相稱於該的大小之燒結體而製作。
[實施例3] <第1步驟>
於與在實施例1使用相同而相對於α-SiC原料粉末而調配1.5重量份助燒結劑的B4C的調配粉末，不加入助成形劑而加入甲醇溶媒。
<第2步驟>
與實施例1相同，乾燥已粉碎混合此等的漿液而作成成形用粉末。
<第3步驟>
將此成形用粉末以加壓力200kg/cm2、溫度2100℃之 條件下藉由熱壓法而燒結而得到50mm平方之燒結體。
計測已得到的燒結體之密度的結果，可了解成為比重為3.193(相對密度=99.8%)之緻密的燒結體。
<第4步驟>
外徑350mm左右、內徑295mm左右，厚度5mm左右之邊緣環係藉由加工相稱於該的大小之燒結體而製作。
[實施例4]
為了研究SiC原料粉末及助燒結劑之調配量及燒結體之密度(比重)之差異與電漿耐性之關係，所以作成各種之材料。
(1)SiC原料粉末
使用與在實施例1所使用者為相同之原料粉末(以下稱為「S1」。)，作為比較用之原料準備SiC純度為98.5%、SiO2含量為0.8%、雜質(Fe)為0.03%及金屬Al為0.02%之市售之SiC原料粉末(以下稱為「S2」。)。
(2)助燒結劑
作為助燒結劑之B4C係使用與實施例1相同原料粉末。
又，氧化物系助燒結劑之一成分的Al2O3係使用與實施例2相同原料粉末。
更進一步，氧化物系助燒結劑之其他成分的Y2O3係使 用純度為99.9%以上且平均粉末粒徑為0.5μm以下之原料粉末。
(3)各種原料粉末之混合及壓製成形體之作成
與實施例1同樣地於各種調配粉末加入丙烯酸系黏著劑和溶媒(水)，將以尼龍製之球磨機鍋和尼龍塗覆球進行粉碎混合而得的造粒粉末，以加壓力1000kg/cm2進行壓製成形而作成50mm平方之各種坯體。
(4)燒結
將各種坯體以真空環境爐進行加熱脫脂後，藉由以氬環境爐調整燒結溫度，作成比重不同的燒結體，作成試料尺寸為20×20mm平方且厚度為5mm之電漿耐性評估用之測試片。
於表1，作為電漿耐性評估用之測試片，表示現在作為邊緣環構件(表示為試料No.：St)普及的以CVD法作成的β-SiC(以下，稱為「CVD-SiC」。)、在實施例4作成比較用的鐵雜質多的燒結體(表示為試料No.：#1)及以本實施例作成的燒結體(表示為試料No.：#2~#6)之調配組成和材料特性，同時作為噴淋板用之材料將專利申請的純度99.99%之Al2O3材料(表示為試料No.：#7)設為比較測試。
Figure 106129893-A0305-02-0016-1
電漿耐性試驗係將樣本面積：20×20mm、厚度：5mm之小片樣本以8吋晶圓用之微波激發裝置(Tokyo Electron公司製)進行電漿曝露，以蝕刻前後之重量變化量研究電漿耐性。電漿條件係使用電源功率：2000W(頻率：2.45GHz)、偏壓功率：30W(頻率：13.56MHz)、SF6氣體，以氣體流量：60sccm、壓力：100mTorr、照射時間(合計)5小時曝露於電漿。因為長時間之電漿照射為困難，所以進行20次15分鐘之電漿照射。
在此，試料No欄之St為CVD-SiC，#1和#2係助燒結劑之Al2O3和Y2O3為相同但SiC原料粉末相異，而且#2係藉由變低燒結溫度而將燒結體之比重設為未達3.0者。
又，#4、#5、#6係以調查藉由相同之SiC原料和相同氧化物系助燒結劑及相同燒結條件而作成燒結體的情況之再現性者，燒結體之密度係可得到幾乎相同之值。
第2圖係將表示於表1的各種之SiC材料供給於 前述的電漿耐性試驗，將電漿照射後之質量減少量除以測試試料之表面積的值進行圖表化者。
在同圖中，作為電漿處理裝置之邊緣環，由多種之SiC材料中作為粒子污染或耐電漿性優異者而經常使用的CVD-SiC為顯現最大的質量減少量。
接著，試料No.#2係藉由燒結體之比重為低至未達3.0(相對密度=未達87.3%)，電漿耐性差且顯現大的質量減少曲線。
然後，助燒結劑為B4C系之SiC材料的#3係比重為3.08(相對密度=96.3%)，儘管相對密度低可是顯現出優於CVD-SiC的耐電漿性。
#1係鐵雜質為多達0.03%(300ppm)的SiC原料，但為CVD-SiC之一半以下之質量減少量，顯現優異的耐電漿性。
作為此理由係可認為是因為燒結體之比重為3.13(相對密度=95.3%)和成為緻密燒結體及介電損耗為10-2級，而且於SiC晶界存在YAM相成分。
然而，#1係相較於本發明之碳化矽構件而言，鐵雜質多達100倍左右，所以相較於相對密度較低的#4而言，耐電漿性較差，而且因為有金屬污染之問題所以不可謂為理想的材料。
又，#4、#5、#6係各自比重值為3.13(相對密度=94.8%)、3.14(相對密度=95.2%)、3.15(相對密度=95.5%)，任一均為於SiC晶界存在YAM相成分，且，成為 相對密度越變高而依電漿照射所致的質量減少量越變少的傾向，相較於CVD-SiC而質量減少量為#4為35%、#5為29%、#6為25%，所以可了解耐電漿性係成為約3倍至4倍。
尚，測定介電損耗的#4係因為是1×10-1級，所以推定#5、#6亦表示大致相同的值。
然而，作為噴淋板之材料開示於先前專利的#7之Al2O3係因電漿照射所致的質量減少量表示近乎0的值，但在質量減少可見的等級係雖然未被蝕刻，但是藉由來自電漿之離子照射而微少量之Al被濺鍍而飛濺於氣相中，附著於晶圓。
因此，Al2O3係於製造的裝置帶來洩漏電流增大等之不良影響。
相對於此，SiC係母材為Si而與晶圓為相同的材料所以為理想，C係相較於Al而言容易藉由氟氣體而揮發，所以不對於裝置帶來不良影響。
#1、#4、#5及#6之燒結體，作為在電漿耐性顯現高的值的理由係任一者相對密度均成為大致95%以上之緻密燒結體，而且於SiC之晶界存在YAM相成分而使結晶粒強固地鍵結，同時可認為因為YAM相本身具有耐電漿性。
附帶一提，#2係燒結體之比重為2.87(相對密度=87%)，藉由未緻密地燒結之情事及YAM相成分未存在之情事而推定為成為耐電漿性差的原因。
另一方面，使用非氧化物系之助燒結劑的B4C，與#3之測試試料係另外製作燒結體之比重為3.14(相對密度=98.2%)之緻密燒結體，以與實施例4相同之條件進行合計5小時照射電漿的測試的結果，得到質量減少量為0.026mg/mm2之資料，可了解相對於CVD-SiC而成為60%之值而相較於#3而大幅地提昇耐電漿性。
在電漿處理裝置之噴淋板或邊緣環等之構件最成為問題的鐵(Fe)及鎳(Ni)雜質濃度係在試料No.St之CVD-SiC為0.01ppm左右，又，以熱壓法燒結的β-SiC用之原料粉末係Fe及Ni被設為0.05ppm及0.05ppm以下，任一均藉由採用超高純度之構件而成為不產生雜質之不良影響。
相對於此，由使用於試料No.#4、#5及#6等的α-SiC所構成的Si之原料粉末係在Fe含有3~10ppm、在Ni含有0.5~1ppm之雜質，但藉由以相對密度成為93%以上之方式進行燒結，燒結體之雜質含量為減少至一半以下之情事為以輝光放電質譜法確認。
特別是，藉由使用高頻感應加熱法作為燒結體製造時之加熱方法，了解鐵系雜質之削減幅度大。
作為助燒結劑使用B4C的試料No.#3及相對密度為98.2%之燒結體係在電漿耐性試驗得到相較於#4、#5及#6而言有若干差的結果，但由B4C助燒結劑係藉由氟系氣體而揮發之情事，因為相較於#3而言可將助劑調配量削減至3分之1之0.5重量份，可使因電漿照射所致的質量減少量降低，同時因為無以氟系氣體揮發的B及C係作為粒 子附著於半導體晶圓之情事，所以可合適地使用作為電漿處理裝置之構件。
接著，試料No.#7之高純度Al2O3係因為由電漿照射所致的質量減少量幾乎為0，所以可認為作為電漿裝置用構件為最優異，但藉由來自電漿之離子照射而微少量之Al被濺鍍而飛濺至氣相中，附著於半導體晶圓，成為對於所製造的裝置帶來洩漏電流增大等之不良影響。
又，Al2O3係因為比熱大所以熱容量大，更進一步係熱傳導率較小而熱膨脹係數亦大，所以對於進行為了提昇電漿裝置之運轉率之急速加熱或急速冷卻係未合適。
在將本發明之SiC原料粉末和助燒結劑所構成的成分之調配粉末以相對密度成為93%以上之方式燒結的材料，適用於噴淋板的情況係介電損耗為10-1~10-2左右，而且因為金屬不純物少，所以來自高頻電源之施加電力消耗於噴淋板之自我發熱的比例少，因為彎曲強度或熱傳導率亦為充分，所以可對應急速加熱或急速冷卻，而且因為電漿耐性相較於CVD-SiC更優異，所以可較廉價地製造複雜形狀之噴淋板，可供給先前並無的高度之電漿裝置用構件。
尚，在此情況，第1圖之噴淋板3係成為由內壁電性絕緣，施加高頻電力而作為電漿激發電極使用。
[實施例5]
與在實施例1使用為相同調配α-SiC原料粉末 100重量份、純度為99.99%且平均粒徑為0.5μm之Al2O3 3.5重量份、純度為99.9%且平均粒徑為0.5μm之Y2O3 7重量份而得的造粒粉末，以1t/cm2之壓力壓製成形及脫脂後，藉由以電阻加熱方式之氬環境爐用1800~1900℃之溫度燒結，作成具有比重為3.15(相對密度=95.5%)且電阻率為7.6×105Ω‧cm之特性的邊緣環。
為了研究此邊緣環之材料特性，進行以X光繞射所致的晶體結構解析。將該X光繞射圖表示於第3圖。
由此X光繞射圖，可了解SiC成分之波峰、由Al2O3與Y2O3之助燒結劑產生的YAM相成分之波峰存在。
尚，詳細地進行以X光繞射所致的晶體結構解析的結果，稍微確認Y2O3成分之存在。
因而，本發明之α-SiC燒結體係可謂作為助燒結劑調配的Al2O3和Y2O3，但以在燒結過程集合於SiC之晶界而產生YAM相成分的材料所形成者。
又，在本發明使用的α-SiC原料粉末係因為將被包含於SiC原材料的自由之SiO2削減至0.3%以下，所以不可謂電漿耐性優異的SiO2幾乎不存在，進而SiO2與作為助燒結劑調配的Al2O3反應，可形成SiO2之數倍之分子量的3Al2O3‧2SiO2~2Al2O3‧SiO2或Al6O13Si12等之莫來石成分為未大量地產生的α-SiC燒結體。
接著，使用作為現在邊緣環採用的純正品(CVD-SiC)與以本實施例作成的邊緣環，以下述之條件進行電漿蝕刻測試。
在8吋晶圓用之電感耦合型之電漿蝕刻裝置，流過20/10sccm Ar/CF4，以1Pa之壓力蝕刻矽氧化膜和多晶矽膜之多層層合膜而形成孔洞。
尚，於電漿激發係將13.56MHz之電力施加2000W於天線，於已承載矽晶圓的基板係同樣施加1000W 13.56MHz之電力。
此構造係因為形成三維NAND快閃記憶體之縱型之閘，所以可合適地使用。
又，在本實施例作成的邊緣環係因為相較於純正品(CVD-SiC)之邊緣環而言電漿耐性優異，所以於蝕刻製程中SiC成分氣化而被放出至氣相中的量亦變少。
第4圖係表示如此地進行的孔洞之剖面形狀的圖，左側為使用純正品之邊緣環而形成的孔洞之剖面形狀，右側為以與本發明之實施例4作成的燒結體(#4、#5、#6)相同材料特性所構成的邊緣環而形成的孔洞之剖面形狀。
如由第4圖可了解，在純正品係SiC邊緣環為被F系之自由基蝕刻，以氣化為SiF4或CF4等而由邊緣環放出，電漿之密度或電位為在晶圓中央和接近邊緣環的晶圓周邊會不同。
因此，僅晶圓周邊產生蝕刻形狀之異常，微細尺寸之控制變得困難，蝕刻後之良率會變差。
另一方面，本發明品係因為相較於純正品而言邊緣環為透過電漿而氣體化的比例減少，所以電漿之密度或電位 之分布均勻化。
因此，如第4圖所示之方式可形成垂直的孔洞，可抑制蝕刻形狀異常之產生。由此良率亦改善。
然後，如此的效果係不限於上述之製程或所使用的蝕刻裝置者。
近年的半導體係越來越朝向微細化的方向開發改良，電漿蝕刻之溝槽寬度係以形成為10nm以下之方式指向。
為了微細化半導體係蝕刻圖型之正確性為不可或缺，蝕刻圖型之正確性係變為對半導體之製造良率大幅地帶來影響，但藉由本發明則可使製造良率提昇。
列記實施例之變形例。
(1)在實施例1~5係採用平均粒徑為0.6μm之α-SiC，但如為α-SiC之平均粒徑為0.3~3μm，則可得而具有相同之特性的燒結體，如為0.3~1μm，則可得到緻密的燒結體。
(2)在實施例1及3係作為助燒結劑採用平均粒徑為1μm以下之B4C原料粉末，在實施例2係作為助燒結劑採用平均粒徑為0.5μm之Al2O3微粉末及平均粒徑為1μm以下之Y2O3微粉末。
但是，反覆實驗例的結果，B4C之平均粒徑如為0.3~2μm，則可得到具有同樣之特性的燒結體，可了解如為0.3~1μm，則可得到更緻密的燒結體。
又，Al2O3微粉末及Y2O3微粉末之平均粒徑如為0.3~3μm，則可得到具有相同之特性的燒結體，如為0.3~2μm，則可得到緻密的燒結體，更進一步藉由使用1μm以 下之微粉末而可得到低溫燒結性。
(3)在實施例1係調配相對於α-SiC原料粉末而言為助燒結劑的B4C 0.5~5重量份，在實施例2係調配α-SiC原料粉末100重量份、Al2O3原料粉末2.5重量份及Y2O3原料粉末5重量份，在實施例3係調配相對於α-SiC原料粉末而言為助燒結劑的B4C 1.5重量份，在實施例4係調配α-SiC原料粉末100重量份、Al2O3原料粉末2或3.5重量份及Y2O3原料粉末4或7重量份，在實施例5係調配α-SiC原料粉末100重量份、Al2O3原料粉末3.5重量份及Y2O3原料粉末7重量份。
但是，重複實驗的結果，可了解在將B4C作為助燒結劑使用的情況，相對於α-SiC原料粉末及B4C原料粉末全體而言的B4C之調配量係0.5~5重量份即可，1~2重量份則較佳。
又，可了解在將Al2O3及Y2O3作為助燒結劑使用的情況，相對於α-SiC原料粉末100重量份而言Al2O3原料粉末和Y2O3原料粉末之合計調配量係3~15重量份即可，6~12重量份則較佳。
具體而言，合計調配量為3重量份之情況係設為Al2O3：1重量份和Y2O3：2重量份。
藉此，在燒結後於結晶晶界存在YAM相成分。
(4)在實施例1係將B4C作為助燒結劑在氬氣環境爐內燒結(氬氣燒結)，在實施例2係將Al2O3及Y2O3作為助燒結劑在高頻感應加熱爐內燒結(高頻燒結)，在實施例 3係將B4C作為助燒結劑藉由熱壓法而燒結(熱壓燒結)，在實施例4係將Al2O3及Y2O3作為助燒結劑進行氬氣燒結，但亦可將B4C作為助燒結劑進行高頻燒結，亦可將Al2O3及Y2O3作為助燒結劑進行熱壓燒結。
(5)關於燒結方法係藉由將以惰性環境爐燒結的SiC構件進而進行HIP處理，可得到空孔極少的緻密的燒結體。
例如，調配1.5重量份B4C而以惰性環境爐燒結的比重3.144(相對密度97.9%)，以2000大氣壓、2000℃，1.5小時進行HIP處理的結果，比重可緻密化為3.185(相對密度99.3%)。
尚，本發明之SiC構件係作為高溫燒結時之環境氣體使用了氬，但亦可使用氬以外之惰性氣體或非氧化性之環境氣體。
(6)在實施例1及2係被包含於α-SiC原料粉末的金屬系雜質之量為37~70ppm、Al雜質之量為28~45ppm、Al以外之金屬系雜質之量為9~25ppm，但關於各式各樣之原料粉末進行試驗的結果，可了解被包含於α-SiC原料粉末的Al以外之金屬系雜質之量係少者為較理想，關於Al雜質亦可略多，所以可謂在全體超過20ppm、70ppm以下，在Al雜質為50ppm以下、在Al以外之金屬系雜質之量為20ppm以下即可。
然後，較理想為在全體超過20ppm、60ppm以下、Al雜質為45ppm以下、Al以外之金屬系雜質為15ppm以下為 佳，更理想為金屬系雜質為55ppm以下、Al雜質為45ppm以下、Al以外之金屬系雜質為10ppm以下為佳。
(7)由實施例1~5視之，藉由燒結體之相對密度為93.0%以上，較理想為93.9%以上，介電損耗小於1×10-1，而且於燒結體之SiC結晶晶界存在YAM相成分，依情況稍微存在YAP相成分或YAG相，SiC結晶之平均結晶粒徑為10μm以下，理想為7μm以下，較理想為5μm以下之情事，可滿足電漿處理裝置用構件所要求的諸特性。

Claims (1)

  1. 一種電漿處理裝置用碳化矽構件，其特徵為由α構造碳化矽與氧化物系助燒結劑之燒結體所構成，前述α構造碳化矽係在燒結前金屬系雜質之含量為超過20ppm、70ppm以下，Al雜質之含量為超過20ppm、50ppm以下，且，SiO2之含量為0.3%以下，前述氧化物系助燒結劑由Al2O3與Y2O3所構成，該合計量為3~15重量份，且，Y2O3之重量為Al2O3之重量之1~2倍，於α構造碳化矽結晶之晶界存在有YAM相成分。
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