TW574390B - Hafnium silicide target for forming gate oxide film and method for preparation thereof - Google Patents

Hafnium silicide target for forming gate oxide film and method for preparation thereof Download PDF

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Publication number
TW574390B
TW574390B TW91112590A TW91112590A TW574390B TW 574390 B TW574390 B TW 574390B TW 91112590 A TW91112590 A TW 91112590A TW 91112590 A TW91112590 A TW 91112590A TW 574390 B TW574390 B TW 574390B
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Taiwan
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ppm
powder
target
oxide film
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TW91112590A
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English (en)
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Shuichi Irumata
Ryo Suzuki
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Nikko Materials Co Ltd
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    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
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Description

574390 A7 —^ --21--- 五、發明說明（/ ) [技術領域] 本發明係關於一種對於可做爲高介電體閘極絕緣膜使 用之HfSiO膜以及HfSiON膜之形成上爲適宜之富有加工 性、耐脆化性等之給矽化物靶及其製造方法。又’於本說 明書中所使用之單位「ppm」全部代表wtppm。 [背景技術] 介電體閘極絕緣膜之膜厚會大幅地影響M0S電晶體 之性能，在與矽基板之界面必須呈現電性穩定、載體之遷 移度不致惡化。 以往，做爲此種閘極絕緣膜係使用Si〇2膜，從界面特 性來看確爲最優之材料。又，做爲閘極絕緣膜使用之Si〇2 膜其具有厚度愈薄則載體（亦即電子或電洞）的數量愈增加 而可增加汲極電流(drain current)之特性。 基於此種特性，閘極Si02膜每當因配線之微細化造成 電源電壓下降之情況，在不致損及絕緣破壞之可靠性的範 圍下，多將其薄膜化。惟，一旦閘極Si02膜成爲3mn以下 ，則會流過直接穿隧漏電流，而出現無法當作絕緣膜來作 用之問題。 另一方面，仍欲謀求電晶體之更加微細化，但只要如 前述般做爲閘極絕緣膜之Si02膜的膜厚受到限制，則電晶 體之微細化無法邁進，從而出現電晶體性能無法獲得改善 之問題。 又，爲了降低LSI之電源電壓、降低消耗電力，有必 要將閘極絕緣膜做進一步的薄層化，惟一旦Si02膜成爲 3 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） (請先閱讀背面之注意事項再填寫本頁) • 1 I I I 1 I I 訂----I I I I 一 A7 574390 ______B7 五、發明說明（>) 3nm以下則如上述般有閘極絕緣膜破壞之問題，所以在薄 膜化方面有其極限。 鑒於以上情事，近來乃取代Si02膜改針對高介電體閘 極絕緣膜進行探討。此高介電體閘極絕緣膜中受到矚目者 有HfSiO膜以及HfSiON膜。 此高介電體閘極絕緣膜能以較厚之膜來得到與Si02膜 同等之電容，可抑制穿隧漏電流之發生，此爲其特徵所在 。又，由於可視爲在Si02添加Hf，所以預期在界面特性 上也和Si02接近。 是以，乃需要得到一種濺鍍靶，來輕易、安定地形成 品質優良之HfSiO以及HfSiON高介電體閘極絕緣膜。 [發明之揭示] 本發明爲了解決上述問題，其課題在於提供一種對於 可做爲高介電體閘極絕緣膜(具備替代Si02膜之特性)使用 之HfSiO膜以及HfSiON膜之形成上爲適宜之富有加工性 、耐脆化性等之給矽化物靶及其製造方法。 本發明係提供： 1. 一種閘極氧化膜形成用給矽化物靶，係由HfSiu^ 2.〇〇所構成(在此組成比中，不包含Si : 1.02。亦即，僅Si 之下限値超過1.02。此於本說明書中皆同樣）。 2. —種閘極氧化膜形成用飴矽化物靶，係由 2.00所構成’且具備以HfSi相以及HfSi2相爲主之混相。 3. 如上述第1或2項之閘極氧化膜形成用給矽化物靶 ，其相對密度在95%以上。 4 本紙張尺度適用中國國家標準（CNS)A4規格（210 x 297公爱^ (請先閱讀背面之注意事項再填寫本頁) ί I I--— —訂 --------線- A7 574390 ___B7__ 五、發明說明（f ) 則是和做爲基材之Si基板的整合性佳，又由於容易成爲非 晶性結構，所以有漏電流減少之特徵。 基於以上之情事，依據使用目的來考慮並決定介電係 數與漏電流之平衡是必要的。又，於元件之製造程序中被 要求分別固有之相容性(適合性），所以必須有可依必要性 來任意變更Hf與Si之組成比的材料。 將給與矽之混合物粉加以燒結之情況，依組成比之不 同，會成爲HfSi相、HfSi2相等之矽化物相與Hf相、Si相 等之混晶，一般，這些當中之化合物給矽化物，因其熔點 高而於燒結時無法充分地提升密度，成爲孔洞之組織燒結 體，而有產生許多粒子之問題。 再者，若不依照組成比來調整熱壓條件(亦即加熱溫度 與壓力），則無法得到最適密度之靶。 本發明基於密度提升之目標進而硏究改良，終於成功 地獲得可適宜當作閘極絕緣膜形成用給矽化物靶之物。 本發明，係採用了考量到介電係數與漏電流之平衡之 由HfSihOW.QQ所構成之聞極絕緣膜形成用給砂化物祀。此 給矽化物靶係具備以HfSi相以及HfSi2相爲主之混相，可 得到孔洞組織消失、相對密度在95%以上之給矽化物靶。 若相對密度未滿95%，則密度不足、脆性下降且加工 性也變差。再者脆性結晶會因爲破壞飛散引起粒子增加。 是以，以上述範圍爲佳。 閘極氧化膜形成用給矽化物靶中之氧含量以 500〜lOOOOppm爲佳。若氧未滿500ppm，則耙製造中有起 6 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） (請先閱讀背面之注意事項再填寫本頁) >1裝 ί n n 一：OJ· 1 1MI ϋ I ϋ ϋ A7 574390 五、發明說明（(） 火之危險性，相反地若超過l〇〇〇〇ppm則祀中之氧會以氧 化物的形式析出而成爲濺鍍中之異常放電的原因，粒子會 增加導致製品良率下降。 又’靶中之锆的含有量以抑制在2.5重量％以下爲佳 。若錐量超過2.5重量％，則用以形成氧化膜之反應性濺鍍 時之電壓、電流、基板溫度等的程序條件會大幅變動，非 所喜好者。 再者，閘極氧化膜形成用給矽化物靶中之雜質以C : 300ppm 以下、Ti : lOOppm 以下、Mo : 100ppnl 以下、W :lOppm 以下、Nb : lOppm 以下、Fe : lOppm 以下、Ni ·· lOppm 以下、Cr : lOppm 以下、Na : O.lppm 以下、K : O.lppm 以下、U ·· O.Olppm 以下、Th : O.Olppm 以下爲佳 。因爲這些雜質會成爲閘極與下部Si基板部之污染源。 在製造由HfSiiow.oo所構成之在耐脆化性優異之閘極 氧化膜形成用給矽化物靶之時，係合成出由HfSh .02-2.00 所 構成之組成的粉末，將之以1400°C〜1535°C做熱壓來製造 。若未滿1400°C密度無法充分提升，若超過1535°C則開始 出現部份熔解，固非所喜好者。 於合成出由HfSii^^.oo所構成之組成的粉末之際，係 讓氫化給粉與Si粉以1 : 1.02〜1 : 2.00之莫爾比來調製、 混合之後，在600°C〜800°C進行燒成。 雖也曾考慮使用Hf粉，惟Hf粉具強氧化力，一經粉 末化會出現起火的問題，故非所好者。 是以，爲了防止此種起火，係使用氫化給。氫化給粉 7 紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公楚) (請先閱讀背面之注意事項再填寫本頁) --------訂---------線成 A7 574390 ____B7_ 五、發明說明（^ ) 以及矽粉以微粉碎至低於100網眼來使用爲佳。藉由使用 此種微細粉，可達成燒結時之高密度化。 藉由上述燒成之際的加熱來進行脫氫與矽化物化。脫 氫係自約600°c起發生。燒結係在真空中（ΐχΐ〇_4〜ΐχΐ〇_ 2Torr)進行，爲了脫氫呈現若干氫環境氣氛。 又，加熱到800°C來結束脫氫，且因Hf金屬而有起火 之虞的部分係進行矽化物化或是使之燒結到無起火之虞之 地步(大約3μπι以上）。 如上述般，在加熱合成之際，藉由在低溫下進行脫氫 與矽化物化，可抑制粒子生長，燒成粉之一次粒子仍呈現 微細狀態，於成型之際可高密度化。燒成粉一旦巨大化， 則燒結前之微粉碎困難，會引發巨大粒子之殘存以及密度 下降。 如上所述，由於在低溫進行燒成，乃具有可抑制結晶 粒子之生長的重大特徵，可將閘極氧化膜形成用給矽化物 靶之平均結晶粒徑調整成爲5〜200μιη。於是，於燒結之際 可達成高密度化。 平均結晶粒徑未滿5μιη之粑，其氧含量要控制在 lOOOOppm以下係困難的，又在製程中有起火之虞，另超過 200μηι的情況下，由於粒子會增加，製品良率會降低，所 以上述平均結晶粒徑以控制在5〜200μηι爲佳。 藉由上述之由HfSiuw.oo所構成之組成的粉末之合成 、以及使其於1400°C〜1535°C進行熱壓，可達成燒結時之 高密度化。 8 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） (請先閱讀背面之注意事項再填寫本頁) 裝 ----訂---------線秦 A7 574390 ___B7_—____ _ 五、發明說明（j ) 上述熱壓之溫度爲合成粉之液相生成正下方之溫度’ 在此溫度範圍之燒結係重要的。藉此，可得到相對密度達 95%以上之高密度化之給矽化物靶。 經高密度化之本發明的給矽化物靶，具有可防止濺鍍 中因孔洞而產生粒子等之效果。 實施例 以下說明實施例。又，本實施例僅代表發明之一例， 本發明並不受限於該等實施例。亦即，於本發明之技術思 想所含之其他的態樣以及變形亦包含在本發明中。 (實施例1) 將100網眼以下之HfH2粉與100網眼以下之Si粉混 合，在真空中、800°C加熱，藉此一倂進行脫氫反應與矽化 物合成反應，得到HfSi^之合成粉。 將此給矽化物粉加以粉碎，得到100網眼以下之給矽 化物粉末。此時，亦可加入事先合成完畢之給矽化物粉。 此給矽化物粉末經XRD可確認爲由HfSi相以及HfSi2相 之混相所構成。 使用該矽化物粉末，於1500°C以300kg/cm2x2小時之 條件藉由熱壓法來得到密度99.3%之燒結體。將該燒結體 進一步以機械加工製作出(|)300mmx6.35mm t之耙。可得到 幾乎沒有孔洞之組織。 使用以上述方式所製作之靶進行濺鍍，測定6英吋型 晶圓上之粒子，結果發現，0.2μπι以上之尺寸的粒子合計 爲12個，粒子產生顯著地降低了。 9___ 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） (請先閱讀背面之注意事項再填寫本頁) 裝 ϋ I ϋ n^0J· I ϋ n ϋ ϋ ϋ I # A7 574390 ____B7__ 五、發明說明（f ) (請先閱讀背面之注意事項再填寫本頁) 由以上可知，本發明可得到富有加工性、耐脆化性等 之給矽化物靶。再者由於可適用於濕式加工，所以在加工 中完全沒有起火的危險性。 (實施例2) 將100網眼以下之HfH2粉與1〇〇網眼以下之Si粉混 合，在真空中、800°C加熱，藉此一倂進行脫氫反應與矽化 物合成反應，得到HfSih5之合成粉。 將此給矽化物粉加以粉碎，得到100網眼以下之給矽 化物粉末。此時，亦可加入事先合成完畢之給矽化物粉。 此給矽化物粉末經XRD可確認爲由HfSi相以及HfSi2相 之混相所構成。 使用該給矽化物粉末，於1420°C以300kg/cm2x2小時 之條件藉由熱壓法來得到密度99.8%之燒結體。將該燒結 體進一步以機械加工製作出φ300ηπηχ6.35mm t之耙。 使用以上述方式所製作之給矽化物靶進行濺鍍，測定 6英吋型晶圓上之粒子，結果發現，0.2μιη以上之尺寸的粒 子合計爲18個，粒子產生顯著地降低了。 由以上可知，本發明可得到富有加工性、耐脆化性等 之給矽化物靶。再者在加工中完全沒有起火的危險性。 (實施例3) 將100網眼以下之HfH2粉與100網眼以下之Si粉混 合，在真空中、800°C加熱，藉此一倂進行脫氫反應與矽化 物合成反應，得到HfSi^之合成粉。 將此給矽化物粉加以粉碎，得到1〇〇網眼以下之飴矽 10 一 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） A7 574390 五、發明說明（jo 化物粉末。此時，亦可加入事先合成完畢之給矽化物粉。 此給矽化物粉末經XRD可確認爲由HfSi相以及HfSi2相 之混相所構成。 使用該給矽化物粉末，於1520°C以300kg/cm2x2小時 之條件藉由熱壓法來得到密度98.4%之燒結體。將該燒結 體進一步以機械加工製作出(|)300mmx6.35mm t之耙。 使用以上述方式所製作之給矽化物靶進行濺鍍，測定 6英吋型晶圓上之粒子，結果發現，〇.2μηι以上之尺寸的粒 子合計爲20個，粒子產生顯著地降低了。 由以上可知，本發明可得到富有加工性、耐脆化性等 之給矽化物靶。再者在加工中完全沒有起火的危險性。 (比較例1) 將100網眼以下之HfH2粉與100網眼以下之Si粉混 合，在真空中、80(TC加熱，藉此一倂進行脫氫反應與矽化 物合成反應，得到HfSiu之合成粉。將此給矽化物粉加以 粉碎，得到100網眼以下之給矽化物粉末。此給矽化物粉 末經XRD可確認爲由HfSi相以及HfSi2相之混相所構成 〇 使用該給矽化物粉末，於1500°C以120kg/cm2x2小時 之條件藉由熱壓法來得到燒結體。以此方式所得之燒結體 ，爲92.7%之低密度物。將該燒結體進一步以機械加工製 作出(j)300mmx6.35mm t 之耙。 本靶之密度低，所以存在著孔洞。是以，在製作於實 用元件製作上所使用之靶之際的加工，對於加工液之污染 _ 11 ___ 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） <請先閱讀背面之注意事項再填寫本頁) 裝
H ϋ ϋ n 一一OJ· ·.1 n ϋ ϋ H ϋ I 574390 A7 _____B7 _ 五、發明說明（ft)) 的去除極爲困難，所以無法以濕式磨削來進行。因此，爲 了防止加工粉之起火，必須採用在惰性環境氣氛中進行乾 式磨削此種特別的對策。 使用以上述方式所製作之靶進行濺鍍，測定6英吋型 晶圓上之粒子’結果發現，〇.2μιη以上之尺寸的粒子合計 爲270個。再者，靶面外圍部出現了許多被稱爲結球之突 起。 如上所述，在超過本發明之範圍的高溫下進行燒結， 無法達成密度提升，又會產生許多粒子、 (比較例2) 將100網眼以下之HfH2粉與1〇〇網眼以下之Si粉混 合，在真空中、800°C加熱，藉此一倂進行脫氫反應與矽化 物合成反應，得到HfSi^之合成粉。 將此給矽化物粉加以粉碎，得到100網眼以下之給矽 化物粉末。此鉛矽化物粉末經XRD可確認爲由HfSi相以 及HfSi2相之混相所構成。 使用該給矽化物粉末，於1380°C以300kg/cm2x2小時 之條件藉由熱壓法來得到燒結體。以此方式所得之燒結體 ，爲90.6%之低密度物。將該燒結體進一步以機械加工製 作出(|)300mmx6.35mm t 之耙。 本靶之密度低，所以存在著貫通孔洞。是以，在製作 於實用元件製作上所使用之靶之際的加工，對於加工液之 污染的去除極爲困難，所以無法以濕式磨削來進行。因此 ，爲了防止加工粉之起火，必須採用在惰性環境氣氛中進 12 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） (請先閱讀背面之注意事項再填寫本頁) --裝 ----訂---------線Λ A7 574390 _____B7_ 五、發明說明（fj ) 行乾式磨削此種特別的對策。 使用以上述方式所製作之靶進行濺鍍，測定6英吋型 晶圓上之粒子，結果發現，〇·2μηι以上之尺寸的粒子合計 爲490個。再者，出現了許多結球。 如上所述，在超過本發明之範圍的高溫下進行燒結之 密度過低，又會產生許多粒子。 實施例1〜3之靶的相對密度爲95%以上。又，粒子數 目在20個以下。再者，於1400°C〜1535°C之最適熱壓條件 下，同樣地可達成相對密度之提升。 如此，確認Hf : Si之比爲1 ·· 1.02〜2_00之給矽化物 靶可藉由上述條件般來提升燒結體之密度，且可安定地被 製造。 相對於此，比較例1之相對密度低達92.7%。其結果 ，粒子數目爲270個，且出現結球，爲不佳之結果。 又，比較例2之相對密度低達90.6%。其結果，粒子 數目爲490個，同樣地出現結球，爲不佳之結果。 由以上可知，本發明之實施例的優越性相當明顯，可 知具有優異的特性。 [發明之效果] 本發明具有下述特徵：可得到一種給矽化物靶，其對 於可做爲高介電體閘極絕緣膜(具備替代Si02膜之特性)使 用之HfSiO膜以及HfSiON膜之形成上爲適宜，且富有加 工性、耐脆化性等。 本發明之給矽化物靶的相對密度在95%以上屬高密度 13 ^紙張尺度適用中國國家標準（CNS)A4規格（210 x 297公f (請先閱讀背面之注意事項再填寫本頁) I --------訂---------線義 574390 A7 ___B7___ 五、發明說明（|Y) V 物，擁有.優異的強度。 又，高密度化之本發明的給矽化物靶，可防止於濺鍍 中因孔洞所導致之粒子產生以及因脆性組織之破壞飛散所 導致之粒子產生，於靶之加工與製造過程中不會起火，此 爲其顯著效果所在。 (請先閱讀背面之注意事項再填寫本頁) I --------訂---------線秦 14 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） 申請曰期 __江1、c?(p、11_ 案 號 9/i/ ^rf° 類 別 C^clL·· Η〇/ύ%ί (以上各攔由本局填註） 「92. 4· 14,錄正
年 a” 'J ] 丨
It·' ·»*» 1,-., ^ 4 '* 丄.:::'」 574390 集^專利説明書 發明 一、新型名稱 中 文 閫極氬化腾形成用紿矽化物靶及其製浩卞法 英 文 HAFNIUM SILICIDE TARGET FOR FORMING GATE OXIDE FILM AND METHOD FOR PREPARATION THEREOF 姓 名 ⑴入間田修一 (2齡木了 一 發明 創作 國 籍 曰本 住、居所 (1X2)日本茨城縣北茨城市華川町臼場187番地4 曰鑛材料股份有限公司磯原工場內 姓 名 (名稱） 曰鑛材料股份有限公司 國 籍 曰本 三、申請人 住、居所 (事務所） 曰本東京都港區虎門2-KM 代表人 姓 名 鈴木孝 訂 線 本紙度適用中國國( CNS ) A4規格（ 210x197公釐） 裝
574390 A7 _B7 五、發明說明（） 4. 如上述第1或2項之閘極氧化膜形成用給矽化物靶 ，其氧含有量爲500〜lOOOOppm。 5. 如上述第1或2項之閘極氧化膜形成用鉛矽化物靶 ，其中，鉻含有量在2.5重量％以下。 6·如上述第1或2項之閘極氧化膜形成用飴矽化物靶 ，其中，雜質中之C : 300ppm以下、Ti : 100ppm以下、 Mo : lOOppm 以下、W : lOppm 以下、Nb : lOppm 以下、 Fe ·· lOppm 以下、Ni ·· lOppm 以下、Cr : lOppm 以下、Na :O.lppm 以下、K : O.lppm 以下、u : O.Olppm 以下、Th :O.Olppm 以下。 7·如上述第1或2項之閘極氧化膜形成用鈴矽化物靶 ，其平均結晶粒徑爲5〜200μιη。 8·—種閘極氧化膜形成用給矽化物靶之製造方法，係 合成出由HfSi^w.oo所構成之組成的粉末，將該粉末粉碎 到1〇〇篩目以下，然後以1400°C〜1535°C予以熱壓。 9·如上述第8項之閘極氧化膜形成用飴矽化物靶之製 造方法，係以150〜2000kgf/cm2進行熱壓。 [發明之實施形態] 具備有替代Si02膜之特性的高介電體閘極絕緣膜，係 使用HfSi祀以氧反應性濺鍍所形成。此氧化物膜被視爲以 ΗίΌ2 · Si〇2所表示之氧化物膜的混成體或是其氧的一部分 被氮取代之膜，在靶方面通常係要求具有si/Hf=1.〇之組成 。一般Hf與Si之組成比被要求接近於所欲形成之膜的組 成比’富Hf之氧化膜有電容率高之傾向，富si之氧化膜 5 本紙張尺度適用中國國家標準（CNS)A4規格（21〇 x 297公釐） (請先閱讀背面之注意事項再填寫本頁) I · I I I--I I 訂-------I I .

Claims (1)

  1. 57439〇
    申請專利範圍 1· 一種閘極氧化膜形成用給矽化物靶’係由HfSh.02-2.0〇所構成，且相對密度在95%以上。 2·—種閘極氧化膜形成用給矽化物靶，係由HfSiKo^ 2.〇〇所構成，具備以HfSi相以及HfSi2相爲主之混相，且相 對密度在95%以上。 3.如申請專利範圍第1或2項之閘極氧化膜形成用飴 矽化物靶，其氧含有量爲500〜lOOOOppm。 4·如申請專利範圍第1或2項之閘極氧化膜形成用給 矽化物靶，其中，锆含有量在2.5重量％以下。 5·如申請專利範圍第1或2項之閘極氧化膜形成用給 矽化物靶，其中，雜質中之C ·· 300ppm以下、Ti ·· l〇0ppm 以下、Mo : lOOppm 以下、W : lOppm 以下、Nb : i〇ppm 以下、Fe : lOppm 以下、Ni : lOppm 以下、Cr : 10ppm 以 下、Na ·· O.lppm 以下、K ·· O.lppm 以下、U ·· 〇.〇lppm 以 下、Th : O.Olppm 以下。 6·—種閘極氧化膜形成用給矽化物靶之製造方法，係 合成出由HfSiro^.oo所構成之組成的粉末，將該粉末粉碎 到100 篩目以下，然後以1400 °C〜1535七、 150〜2000kgf/cm2進行熱壓或是熱均壓(HIP)。 (請先閲讀背面之注意事項再塡寫本頁) 本紙張尺度適用中國國家標準(CNS)A4規格(210 X 297公釐〉
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JP4203070B2 (ja) 2003-03-07 2008-12-24 日鉱金属株式会社 ハフニウム合金ターゲット及びその製造方法
JP4519773B2 (ja) 2003-07-25 2010-08-04 日鉱金属株式会社 高純度ハフニウム、同ハフニウムからなるターゲット及び薄膜並びに高純度ハフニウムの製造方法
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US7517515B2 (en) 2009-04-14
CN1258211C (zh) 2006-05-31
KR20040015359A (ko) 2004-02-18
US7674446B2 (en) 2010-03-09
WO2003009367A1 (fr) 2003-01-30
EP1408541A4 (en) 2007-07-18
KR100694482B1 (ko) 2007-03-12
EP1408541A1 (en) 2004-04-14
CN1515029A (zh) 2004-07-21
US20090194898A1 (en) 2009-08-06
EP1408541B1 (en) 2012-11-28
US20040170552A1 (en) 2004-09-02
JP2003096560A (ja) 2003-04-03

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