TW503449B - Halogen gas plasma-resistive members and method for producing the same, laminates, and corrosion-resistant members - Google Patents
Halogen gas plasma-resistive members and method for producing the same, laminates, and corrosion-resistant members Download PDFInfo
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- TW503449B TW503449B TW90108412A TW90108412A TW503449B TW 503449 B TW503449 B TW 503449B TW 90108412 A TW90108412 A TW 90108412A TW 90108412 A TW90108412 A TW 90108412A TW 503449 B TW503449 B TW 503449B
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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五、發明說日j 曰 修正 案號 9010841^ 日月⑴ L發明所屬技術領域】 和頂ί發明係有關於適用為半導體製造裝置的反應室内壁 、#的耐鹵素氣體電漿用構件。 【習知技術】 係使為超淨(SUPer CUan)狀態之半導體製造裝置, 積用^氯系氣體、及氟素氣體等的_系腐蝕性氣體做為沈 乳體、蝕刻用氣體以及清潔用氣體。 用C1F例如μ在熱⑽裝置等的半導體製造裝置,沈積後使 *導4清心I4體HF又及St的“、腐録氣體組成之 SiHCl 札體。又,沈積的階段,也使用WF6、 刻裝置氣成膜用氣體。又,在独 蝕性氣體。’、孔-氧氣系乳體、溴系氣體等的腐 【發明欲解決之問題】 沾劣、年來,傾向於使用NF3等腐颠姓胜2丨丨一从 的為使蝕刻速度 3寻:'幻生特別南的氣體,目 的壁面被腐Ϊ此,有半導體製造裝置用反岸室 :。或者亦有堆積於壁面之反應生出::於晶圓上的間 娬粒而掉落的情 ^成物剝離而成為晶圓上 現象,成為半導體不產生絕緣不良和導通不良之 反處h 1 守篮不艮的原因。因此,兩^ Γ Μ至和頂部的壁面轉移至曰 而要可防止微粒從
去卢明之課題係為暴露:C 遊於構件,構件的腐蝕以及曰L ^之耐鹵 於谷益内的空間,難以 2日日®加工屬之微粒 _ 土隹積於容器内的其 第5頁 i 號%10fU12 η 五、發明說明(2) 習t有藉由銘等的陶究形成反應室 _ ^ 膜之?術。然而,在該情況,二二而在其表 觸气蝕*質的環境下即使重複多次埶循;人:,特刿是在接 VJt’ f須強固地附著於反應室=匕耐餘m亦不 【解決課題的手段】 的表面。 去/11明之第一觀點係為暴露於耐ϋ f# 2體電衆用構件,具傷構件的本體ί:體電裝之耐南 體表面的耐蝕膜,其特徵 太、土>、形成於該本 UMPa以上。 對本體的剥離強度為 本發明人發現藉由在構件本 ::強度的耐蝕膜,可 ::形成具有前述之 的空間,掉落、堆積於容器内的宜粒浮遊於容器内 膜的剝離強度,將減少耐蝕膜從^ 件上。也許,增加 於是發現,為了防止微產—,而減少微粒。 須在1 5MPa以上。 則述剝離強度實質上必 氣體電漿係自素氣體的電漿之耐_素 氣體接觸面形成之耐蚀膜,U對該構件本體之電漿 表面粗糙度Ra為丨· 2 “ m以上了 做為耐蝕膜的中心線平均 本發明人發現葬ώ户
Rr;的;,,可抑‘腐姓產形成具有前述之 間,掉洛、堆積於容器内的二于龟於容器内的空 猎由耐蝕膜難以產生微 牛上。 圓加工產生:::恤增大(表面保 響----的微粒,被保持1 第6頁 Λ. 曰 案號 90108419 五、發明說明(3) y膜的表面,而免除浮遊於空間,掉落堆積至其他構 留凹t此二2=表面RaA (粗)’也就是指在表面保 :膜:面術增大時,画素氣體的電聚入侵表面的凹部區 產峰=從凹部(粒子)的根部腐㈣界,將促使微粒的 。二、而,如此微粒的增加將減少,而能防止微粒浮 遊、掉洛於容器内的空間。 =述的觀點,耐蝕膜的中心線平均粗糙度^更佳為 辦:二私。x,Ra過大時,將促進耐蝕膜表面的腐蝕反而 曰加被粒,因此從該觀點Ra較佳為20 //m以下,更佳為8 v m以下。耐餘膜的相對密度較佳為95 %以下。 … 软1蝕膜的起伏度Wa (waveness)較佳為丨“m以上。當 f製程產生之副產品為氣象而不會產生微粒等的固形物 下沒有上述限制,表面粗糙度較佳為1 · 5 # m以 二’ 以下。該場合的耐#膜之相對密度較佳 為9〇 /以上,更佳為95%以上。 耐餘膜較佳是沒有長度以上、寬〇1㈣以上 痕。 亡述微粒裂痕的有無,可以掃瞄式電子顯微鏡以5〇〇 以上的倍率觀測耐蝕膜而確認。 耐蝕麼的下地面較佳為多孔質。耐蝕膜的下地面之中 心線平均粗糙度“較佳為12以上,更佳為1 5以上。 而提高耐餘膜於下地的接著性,可防止因膜的剝離心生 i
之微粒。 為了使下地面粗糙,可使下地面成為多孔質, 下 =面砥粒研磨(grain pol ishing)加工或噴砂(Swd芝 本發明之另一課題為提供鋁組成之基體,與於誃 二體上之膜的積層體,該膜不易從基體剝 特別诳腐x 蝕物質接觸後膜亦不易剝離之積層體。 衧別疋與腐 又,本發明之課題,是使用該積層體,提呈 蝕性,且可長期間穩定使用之耐蝕性構件,別= 氣體電襞用構件。 行句疋耐鹵素 A耖ίί:月之ί二觀點,係為鋁組成之基體,與形成於該 :腺的ί Ξ ί :物膜的積層胃’其特徵為在基體與釔化合 物Μ的界面存在有鋁與釔化合物的反應生成物。 ,本發明人發現藉由後述之特定的製造方法在鋁基體上 形成釔化合物膜的場合,視條件而沿著兩者的界面生成鋁 ΪΪ化ί物的反應生成物。於是,生成這樣反應生成物的 劳S 9如在8 0 〇 C與室溫之間施加熱循環後,亦沒有發 現紀化合物膜剝離,而達成本發明。 該反應生成物’通常是沿著基體與釔化合物的界面以 層狀形成’而構成中間層。但是,該層狀的釔化合物,亦 有全面延伸基體與釔化合物之界面而連續的場合,亦有在 基體^釔?合物之界面’不連續生成,而形成複數島狀的 層狀勿=%合。在該場合,島狀的層狀物互相不連續,但 整體沿著界面而以層狀存在’構成中間層。又,本發明, 剷述反應生成物亦包含在基體與釔化合物之界面呈點狀或
ΙΙΗΙIIH 第8頁 503449 案號 90108419 五、發明說明(5) 刀政狀之琢0如此般面積小的反應生成物層為點狀戍分 散狀的場合,亦包含於本發明。且,可以^線折射裝^確刀 認前述反應生成物者亦在本發明之範圍内。 圖式簡單說明: 第1圖係顯示中間層的周圍構造之概要圖。 第2圖係以掃瞄式電子顯微鏡顯示比 面之照片(倍率5000倍)。 飞1·叶的表 第3圖係以玄掃瞄式電子顯微鏡顯示比較例1之試料的表 面之照片(倍率1 0 0 0倍)。 、丁叶的表 第4圖係以知目苗式雷+顧彡 ― 埶處理3小時)之試鏡顯不實施例1 (在1 600。。 … ^/ 大枓的表面之照片(倍率50 0 0倍)。 苐5圖係以知瞄式電子顯微鏡 。 熱處理3小時)之試料的矣而夕M u ,貝她扒丄、在1 b00 C 筮fi同在斜的表面之照片(倍率1 0 0 0倍)。
回’、平瞄式電子顯微鏡顯示實施例3 (在1 70fi 熱處理3 *時)之試料的 耳她例d C在1 700 C 第7圖係以掃晦式電;ϋ率5GGG倍)。 熱處理3小時)之試料: = ; =實施例3 (在1·。。 叶的表面之照片(倍率J 〇 〇 〇倍)。 本:a月之第—較佳實施例 構件本體與耐蝕膜之間具 2孔體電水用材枓在 在耐蚀膜的埶膨^ ^ _,中間層的熱膨脹係數 隹了鄉朕扪,、、、恥脹係數與構件本體 此’可防止耐蝕膜之剝離而 ‘:U係數之間。精 熱膨脹係數的差較佳是& q /〇'中間層與耐蝕膜的 間體的熱膨脹係圭X 〇在, 層較以有彻的構件與禮:以内。 503449
料的混合物、固溶體或反應物。藉此,在高溫區域即使耐 钱膜暴露於_素氣體的電漿中,亦能防止耐蝕膜之剝離而 產生微粒。 本發明耐蝕膜的剝離強度,利用以上之基材的粗糙 度’也就是固定(ahcnoring)效果,並利用根據熱膨脹差 或化學反應和相轉移發生之膜内應力(膜内應力的發生來 源並不只限於中間層)而得。當然亦可使用多孔質材料為 構件本體’利用塗佈後的熱處理之構件本體的收縮。又, 亦可利用根據在界面之化學反應之化學的結合作用。 ,餘,的材料,其高耐蝕性而言較佳為釔的化合物, 特=是二氧化釔、含有三氧化釔之固溶體、含有三氧化釔 之複a氧化物、二氟化記為佳。具體而言,例如有三氧化 釔三氧化锆(zirconia)三氧化釔固溶體、稀土類氧化物一 二氧化釔固溶體、3Y203 ·5Α1 203、YF3、Y-Al-(0)-F、 Y2Zr207 、Y203 ·Α1203 、2Y203 ·Α1203 等。 前述反應物可舉例如下。 (1)耐蝕膜為含有釔的化合物,本體為氧化鋁製的場 合,3Υ203 .5Α1203 、Υ203 ·Α1203 、2Υ203 .Α1203 (2) 本體為鋁製的場合,Α1-γ2〇3金屬陶瓷(cermet) (3) 本體為氧化錯製的場合,Y2zr2〇7 >又耐餘膜的材料,以其高耐钱性較佳還是以化鋁與驗 土族的化>合物,具體而言可舉例如MgA12〇4、CaAi2〇4、、
BaA 1 204等。前述反應物在本體為氧化鋁製的場合可舉例 如為MgA1 204、CaA1 204、BaA1 204 與A1 203 的固溶體。 反應層與基材的邊界較佳有卜2 之微粒子與空隙
mm 第10頁 修正 曰 i號 90inR419 五、發明說明(7) 因A 1 =藉由被形成反應層之微粒子與基材包圍。該部分 剝離了低楊氏杈數(Youg, s m〇du lus),所以可防止膜的 蝕膜:t 3的下地層可為構件本體,或者中間㉟,但該耐 地層之揚氏模數較佳是在HOGpa以下。 2的材質並無特別限制。μ,較佳是不含有可能 ΐ 器嶋程有不良影響之元素。從該觀點來 物或騁鋁,亂化鋁、氧化鋁、氧化鋁與氧化釔的化合 ^洛二、氧化鋁與鹼土族氧化物的化合物或固溶體、 、口、氧化锆與氧化釔的化合物或固溶體。 定接之對本體之剝離強度,是以Sebastans試驗測 疋接者面直徑5. 2mm。 耐姓膜為含有紀化合物& #人 .„ +丄 濃度較佳為30卿以下 的场合,耐餘膜中的鐵原子的 生微:::膜I混入少量鐵原子時’ *現耐蝕膜的表面產 鐵斥:、曲;。Λ 了防止這樣的微小班點產生,耐蝕膜中的 鐵原子》辰度必須在3 〇 p p m以下。 耐钱膜中較佳係含有稀土族元素。該稀土族元素,特 佳為La、Ce、Pr、Nd、P„、Sm、Eu ,、几、d”h〇、
Er、Tm、Yb、Lu。又,化合物較佳為 氧化物之化合物。 隹穴虱甲加熱而成的 形成本發明之耐蝕膜,可舉例如以下之方法 (1) 溶射耐蝕膜的材料而形成耐餘膜。
(2) 以化學氣相沈積法或電化學氣相沈積法形成耐钱
503449 曰 號 90108419_ 五、發明說明(8) (3)使基材的成形體貼合臈 dip)、再使其共燒結。 和改聚料(slurry 在⑴的場合,藉由使用多孔 下地之令間層,可抑制揚氏模數比、、—乍為成為耐蝕膜之 附著溶射之耐蝕膜材料於中間層。牲抢體低,亦可強固地 面,若形成開口部份小且内^寻別是,在中間層的表 時粒子將進入該開氣孔中,於門$ f狀的開氣孔,在溶射 射膜於表面的作用。 乳?中固化,而有固定溶 為了形成該多孔質膜,在構 孔質膜的原料粉末與分散媒體與造孔劑=Z至少含有多 層,接著烘烤該塗佈層。此時, W之Θ材而形成塗佈 多孔質膜形成多數開氣孔,# “ j孔劑的作用,可在 部分開氣孔形成開口部較小的形:即绝孔劑的I可將大 將該表面研磨加工,閉氣孔成為開氣Π: , 分開口部份相對減小。 ’、 忒開軋孔大部 關於前述之塗佈用的客妊 (acrvn ^ ±石山私士 1"材义孔劑較佳為丙烯基 松/二 t私末、纖維質等,分散媒體較佳為水、 私月日%(turpentlne alcohol)、丁基 carbitol)等。更佳為在膏材中、天 醉、y ㈢材午’小、加黏結劑(b i n d e r ),兮 黏結,較佳為聚乙締醇、甲基纖維質、丙烯酸黏結劑 力聋m”的材料時’較佳是在低壓狀態溶射,壓 T〇rr以下。藉此,溶射膜的氣孔更加減 少,可使隶終的耐蝕臈的耐蝕性更向上提高。 形成溶射膜後,藉由熱處理溶射膜(以及視必要構件 ),更燒ϋΐ容射可、消^3減少溶射膜中的氣孔 第12頁
:中::Ξ::’藉由熱處理溶射膜、中間層以及構件本 處理、iC ’可消除或減少溶射臈中的氣孔。該熱 別限;=是在140°。°以上,熱處理溫度的上限並無特 構件2體=成中間層的場合,熱處理溫度的上限不使 本體、交I即可,從該觀點較佳是在2〇〇〇。〇以下。又, %,' ί iL質的中間層的場合,從抑制中間層的燒結之觀 …處理溫度較佳是在1 8 0 0 °C以下。 溫度 〇C時 結果 本發明人,更發現藉由140(rc以上的溶射膜之熱處理 ,可顯著增加耐蝕膜的剝離強度。熱處理溫度達1400
’本體的材質與耐姓膜的材質之間亦產生反應層,其
提高了耐蝕膜的剝離強度。 A 另一方面,溶射膜的熱處理溫度提高,接近180(rc =夺,一旦發生生成之反應層的附近之鋁元素的移動、擴 政,耐蝕膜的剝離強度反而降低。從此觀點,熱處理溫产 較佳為165CTC以下,更佳為1 6 0 0它以下,特佳為155(rc = 在反應層為大致平均的材質組成的場合,前 溫度特佳為1 550 t:以下。 …、 又,關於適當的實施型態,在反應層,耐蝕膜的材料 對本體的構成材料之濃度比,為從本體測向耐蝕麼側增 加。採用這般傾斜之組成的中間層,在熱處理時,溶^抑 制在前述反應層之附近的鋁元素的移動、擴散,藉此即使 在1 6 0 0 C的熱處理溫度剝離強度亦不會降低。 上述之反應層厚度並無特別限制,在反應層非常薄的 場合’比起未生成反應層的場合耐蝕膜的剝離強度明顯增
案號 ΘΟίΜ/ηο 五、發明說明(10) 反應層的厚度為3 為更佳。 又马3 “m以 修正 時,從剝離強度增加的觀點 膜的剝特別上限,”在2〇"m以下,耐餘 15 以下,最佳為^加^^觀點,反應層的厚度更佳肩 法堆=ί = :ί以化學氣相沈積法或電化學氣相沈利 發明-J = 可消除溶射臈表面的氣孔。為何4 此U此仔到高剝離強度之原因並一 要原因,是與基材的固定(―效;;:
=的弱壓縮應力等。在本發明該等主要因素相 而传到高剝離強度。 早 叙素氣體可舉例如C1F3、評3、CF4等的CF系氣體, WF4、ci2、BC13 等。 實施例【實驗A】 (實施例1 -1試料的製造)
準備尺寸40x 40x 0.5mm的平板形狀的金屬鋁製的基 體。該基體表面的中心線平均粗糙度Ra為1 · 3 # m。其上以 溶射法成膜鋁-釔金屬陶瓷(Al^O^lHmol%)組成之厚 度10 //m的中間層。中間層之40〜100 °C的熱膨脹係數為15 3 X 10-6 / °C。中間層的中心線平均粗糙度Ra為6· 1 。中 間層的相對密度為8 2 %。 以溶射法在中間層上形成三氧化釔膜。具體而言,使 用PLASMA TECHNIK公司製造的「VACTEK Y2〇3粉」。在溶射 時,以40L/分的流量流入氬氣,以12L/分的流量流入氫。
第14頁 503449 案號 90108412 曰 修正 五、發明說明(11) 溶射輸出為4 OkW,溶射距離為120mm。三氧化釔膜的厚度 為6 0 // m。並未發現有中間層與三氧化釔膜之間的剝離。 接著,從三氧化釔膜的裡側取出中間層以及鋁層。然 後以1 5 0 0 °C熱處理三氧化釔膜3小時後,切斷而得尺寸20 X 2 0 X 3 0 0 // m的試驗片。該試驗片的相對密度為9 7 %,中 心線平均粗糙度Ra為5.7//m,Wa (平均起伏度)為3.8// m。Ra以及Wa是使用Tayler-Hobson公司製造的「Form Talysurf Series Z54」測定掃瞄(scan)長度 4.8mm。 (比較例1 -1之試料的製造) 製造燒結陶瓷(相對密度99.8%)組成之尺寸20x20 X 3mm的試驗片。該試驗片的中心線平均粗糙度Ra為〇. 3 // m,Wa (平均起伏度)為〇· 1 。 (耐餘試驗) 將實施例卜1以及比較例卜1的試料設置於耐蝕試驗裝 置内’以下列條件進行。在評3 ( downf 1 ow p 1 asma)中, 在73 5 °C維持各試料2小時。NF3氣體流量為75 seem,媒介 氣體(carrier gas)(氮氣體)的流量為i00sccm,以ICP (13.56 Hz、輸出800W)激發(excitation ),氣體壓力為 0 · 11 〇 r r。對各試料,測定暴露(e χ p 〇 s u r e)試驗前後的各 重量,而算出重量變化。
表1 因埘蝕試驗減少重量 —實施例1_1 0.1 mg/cm2 比較例1-1 9.2 mg/cm2 第15頁 503449
【實驗B ] (實施例1 - 2之試料的製造) a準備夕孔备之15mol%穩定化CaO錯組成之本體。具體 、曰X 1 5 m 0 1 % C a 0穩定化之錯的粉末,與水、黏結劑」 練,從直徑5〇_的印模(die)壓出成形,乾燥、、燒成 ’ 〇而得燒結體,加工該燒結體而切成尺寸3〇mmx 2〇〇mm βΧ(ΐ「mm之^奉狀的本體。該本體的氣孔率為30 %,揚氏率為 Pa ’中心線平均粗糙度Ra = l. 8 //in、Wa=l. 3 /zm。 士 f該本體之表面,以溶射法形成三氧化釔膜。具體而
口 彳用 PLASMA TECHN I K AG 公司製造的「vaCTEX Y2〇3 :丄:在溶射時,以40L/分的流量流入氬氣,以i2iy分的 机里抓入虱。溶射輸出為40kw,溶射距離為13〇 mm。三氧 1匕=3厚度為50"m。並未發現有中間層與三氧化釔膜 之間的剝離。 % v 。從二氧化釔膜的裡侧取出中間層以及鋁層。然 ^ C熱處理二氧化記膜3小時後,切斷而得尺寸2 〇 X 20 x 30(^#1„的試驗片。該試驗片中包含本體與三氧化釔 \ ^ 。該試驗片的相對密度為96 %,中心線平均粗糙度 Ra為5·9",Wa(平均起伏度)為3.8_。 (實施例1 - 3之試料的製造) _ 將實施例2之試料的 (diamond)磨石粗研磨。 平均粗糙度Ra為1.5 (比較例1-2之試料的製 —氧化在乙表面’以# 1 4 0的 粗研磨後的三氧化釔膜之中心線 ,Wa 為 1 · 4 // m 〇 造)
503449 曰 案號 90108412 五、發明說明(13) 械擠壓而製成60 X 60 X 8mm的平板狀成形體,將該成形體 以7 tonne/cm2的壓力等方靜水擠壓成形,在大氣氛團氣 中1 8 0 0 C燒成成形體而得燒結體。將該燒結體切成尺寸 2 0mm X 2 0mm X 3mm的試料,以# 240磨石研磨加工一側的主 面(另一主面不加工)。加工後的Ra為為〇·7 β m 〇 (比較例1 - 3之試料的製造) 與比較例2相同材料的燒結氧化釔(相對密度99· 8 % ),切成尺寸20mmx 20mmx 3mm的試料。以#8〇〇磨石研磨 加工試料一側的主面。該主面之Ra*〇1 “m,以為〇2# m ° (而才餘試驗) 以與前述耐蝕試驗相同條件,對實施例卜2、實施例 卜3、比較例卜2、比較例1-3進行耐蝕試驗。但是, 施例2、3,是於基材之calcia穩定化之锆部分磨去之 進行試驗。其結果並未發線各試料間有差異。 〜、 (微粒的保持量) 〃 以下列試驗方法測定實施例卜2、實施例卜3 卜2、比較例卜3,微粒保持於表面的程度。 較例 (1)在乾燥器中於1〇〇 t:加熱乾燥各試料3 置於乾燥器(desiccator)内,冷卻至室溫。 )。⑺以化學天秤測定各試料的質量(分解能1〇—紅 (3 )將各試料的試驗面向上放置,在 放置2g氧化紹微粉末(BET值30m2/g )。此瞎"☆的試驗面
I1HIIII 試驗面的 第17頁 案號 901084]? 五、發明說明(14) 整面均勻地呈載微粉末 (4) 將试料的試驗面彳
取田任下(上下顛锢)。 (5) 在試料的下側讲署势—卜顯倒) 的屮Γ7 #罢认她4 J 口又置e 0官的内徑為6· 3mm 〇將技 的出口放置於離試驗而r二人、 将官 蚪#人 曲C面向下)20mm的位置。將瞽子+ 對蜮驗面。向試驗面中 曰 J 1罝竹吕垂直 體!分鐘。 面中〜以流!10L/分的流量流出氣氣氣 (6 ) 以在微粉末為附益义 各試料的質量,算測定相同的天科再次剛定 ⑺對-各試料重複該操作5次,分別測定粉末 表2 ,4示可/、均作為各試驗面的平均粉體吸著量。 再者,表2採用略記法, 因此6· 2 X 10Ε (-4 )表示6· 2 X 10-4。 ^ 其結果,看出本發明的試料,微粉末吸著至試料的試 驗面,具有保持粉體的能力。 # 【實 數 後的數字表示10的$ _
:C 表2 平均粉體附著量 (g/cm2) 因耐餘試驗減少重量 (mg/cm2) 實施例1_2之試料 實施例1_3之試料 _ 6.2χ 1〇Ε(-4) 0.2 7·5χ 1〇e(-5) 0.1 比較例1_2之試料 無法檢測重量增加 0.1 比較例1_3之試料 無法檢測重量增加 0.2 首先’準備尺寸50x 50x 2 mm之純度99.7%的氧化鋁
第18頁 Ά 修正 曰 9010841 i? L、發明說明(15) __ :、、、本體 1砂本體。在該喷砂處理,改變喷砂壓力, (=粒的粒度,調整本體的表面粗糙度Ra = 0. 5-3. 1 本&照表3 )。對應表3所示之各表面粗糙度準備複數個各 以=酮超音波洗淨本體後,將釔電漿溶射於上 = >谷射條件為以40L/分的流量流入氬氣,以l2L/:: 。溶射輸出為40kw ’溶射距離為120_。三氧 化釔臈的厚度為200…各實驗溶射條件相同。 3小日^有^^3之各試料的一部分在大氣中以15〇〇°c執處理 ί ίϊ 1〇mmx2mm,測定剝離強度。 剝離強度的測定方法如下。 厚度1).將成膜試料切成丨。關x 10mmx 2mm (包含耐餘膜的 32.立試料於丙酮中超音波洗淨5分鐘。 rphot t '者接著劑之鋁銷針(stud…) (Phototechnica Co T十h 制、 5· 2mm的圓形。 ^ ) °邊接著區域為直徑 4 ·在成膜兩側接著針。 5·將接著試料的針裝 上拉,直到膜剝落,你胺引,,、(jlg),以,,autograph”向 算接著強度(剝離強;膜:離洛以 此時’在接著劑的部位 ;何重篁/針的接著面積)。 再者,本實驗C, Λ枓的值,不做為測定值。 耐#膜的中心線平均粗的相對密對為98.8〜99.4%, ,Wa (平均起 第19頁 503449 90108411, 干 η 五、發明說明(16) 試驗 編號 下地屠的粗糙度 (Ra、" m) 剝離強度 OlPa) 熱處理温度 CC) 1-1 0.5 0.5 無 1-2 0.7 0.8 無 1-3 1.2 2.2 無 1-4 1.6 3.5 無 1-5 2.1 3.9 無 1-6 2.4 4.2 無 1-7 2.8 4.9 無 1-8 0.5 11 1500 1-9 0.7 14.0 1500 J-10 1.2 48.0 1500 1-11 1.6 52.0 1500 1-12 2.1 45.0 1500 J.-13 2.4 29.0 1500 1-14 2.8 14 1500 1-15 3.1 10.0 1500 伏度)為3.2〜4.5//m 表3 « 之钟刺。 、衣熱慝理之試料卜7,在1 5 0 0 °C熱處理 之試=沾2 -剝離強度非常高。其原因,認為是未熱處理 處理之if是藉固定效果之物理結合,而在1 500熱 學姓^武枓的結合是經由氧化銘與三氧化釔的反應相之化 因“離:因可能為含有氣體相的場合。 提高剝離強度。 …曰曰化,因此膜材質本身被強化而 強声;fr二處理之忒料,隨著本體的表面粗糙度增加,剝離 ^曰加。另一方面,發現以1 5 0 0 °C熱處理之試料,
JM 的程度剝離強度為最高。 第20頁 503449 修正 案號 90108412 五、發明說明(Π) 未熱處理之試料,因為隨著表面粗糙度增加,在耐 膜與本體之接合界面耐蝕膜的固定效果更增強。相對於 此,在1 5 0 0 °C熱處理之試料,Ra:z丨· 6 # m附近剝離強度為 隶咼的,無法以固定效果說明。可能表面粗糙度^增加、 時’在凹凸大的本體表面,成膜時凹部殘留有空間,因 該空間成為構造缺陷。以1 5 0 〇 °c熱處理之試料,因為耐L 膜與本體的接著是以化學結合,因此構造缺陷部分開始飾 加’接合強度亦開始降低。又,表面粗糙度Ra小時,熱^ 理前不充分之區域的面積增加,而降低剝離強度。 < 從表3可看出’熱處理之試料,從剝離強度的觀點, 下地層的中心線平均粗糙度Ra較佳為1〇 以上,更佳’ 2 /z m以上。又,Ra較佳為2 · 5 # m以下,更佳為2 · 〇 “旧#、、、 下。 又1製作耐蝕性構件時,機械的剝離強度,在膜的 久性上是必要的。從此觀點,較佳是對成膜施加熱處理而。、 然而,溶射後的剝離強度,在處理上,剝離強度高 佳。總括來說本體的中心線平均粗糙她的適 2 〜2.5/zm。 ’I·
【實驗D J ^備尺寸50><50)<2111111之純度99.7%的氧化鋁作為 將各本體以丙酮超音波洗淨本體後 』電6:0為匕。 膜。溶射條# A ητ /八认士曰,冷射記電水為耐麵 旦、、六入&条件為4〇L/刀的流罝流入氬氣,以12L/分的、、六
二;的ί。溶射輸出為4〇kW,溶射距離為120mm。三氣:L -—^予度為20G"m 〇各實驗溶射條件相同。接著對形成 503449 案號 9010S419 五、發明說明(18) 溶射膜後的各試料在800〜;1 6 0 0玄 )熱處理。 C (表4所示之各處理溫度 從以各溫度熱處理之各試料, 料(i〇mmxl〇mmx2mm)以及膜Hi剥離^纟測定用試 X 1 Omm X 0 1 η 1 g ^ 、 耽率測疋用试料(5mm X iUmmx (J· :1〜〇· l5mm,·僅從膜部切出)。 X * ^(Archi.edean) S : = ί。#著,對剝離強度測定用試料,垂直切 斷膜將剖面鏡面研磨後,以;^ , 盘财餘膜的双而、丨… 田t電子顯微鏡觀察本體 相定應層的厚度。又,反應物的結晶 Ϊ面 裝置測定剝離試驗時的膜試料以及針的剝 為4 9〜6 6纟本實驗D ’耐蝕膜的中心線平均粗糙度Ra是 為U 6.6㈣,Wa (平均起伏度)為3 2 4 2p。疋
第22頁 叫449 五、發明說明(19) 案號 90108412 Λ__3 曰 修正 表4 熱處理盈度 CC) 剝離強度 (MPa) 開氣孔率 (容量%) 反應層膜厚 (㈣ 無 3.4 5.1 無 800 4.6 5.1 無 1000 2.1 5 無 1200 18.0 2.5 無 1400 42.0 1.4 3 1500 50.2 1.1 9 1550 31,5 0.9 15 1600 1.8 0.8 25 其結果,剝離強度在熱處理1 5 〇 〇 °c的試料為最高。其 因’是熱處理溫度在1 4 0 0 C以上氧化銘與紀反應,而強原 界面的結合力。然而,超過1 550 °C,反應相的厚度增知化 因此原子的擴散過多,而在界面有空隙,因此剝離強声’ 於降低。因此,反應層的厚度在3 與20 //m之間的場八趨 m 合’剝離強度為最高。從此觀點,反應層的厚度最佳為3 // m 到 1 5 // m 〇 反應相是3Y203 ·5Α1 203、2Υ203 ·Α1 203、Y203 · A1 2 Ο 3中之一個或混合物。 隨著熱處理溫度增高,耐蝕膜的氣孔率減小。考慮财蝕膜 的耐蝕性的場合,必須同時有剝離強度與緻密性。因此, 熱處理溫度农佳疋在1 4 0 0〜1 5 5 0 °c熱處理,此時反應層的
第23頁 ^03449 修正 案號 90108412 五、發明說明(20) 厚度為3〜15 //m。 【實驗E】 準備尺寸50 X 50 X 2mm之純度9 9. 7 %的氧化鋁作為本 體。噴砂本體,整個本體的表面粗糙度以二丨· 6 ± 〇. 1 。 將各本體以丙酮超音波洗淨本體後,改變以如下粉體的組 ,溶射為中間層(Total 5 passes )(第1 pass :氧化銘 粉,第2 pass :氧化鋁80%釔2〇%粉,第3 pass :氧化銘 60%紀40%粉,第4 pass :氧化鋁40%釔60%粉,第5 Pass :氧化鋁2〇 %釔8〇 %粉)。之後,電漿溶射釔作為 射膜。 曰’容射條件為以4 0 L /分的流量流入氬氣,以1 2 L /分的流 昼机入氫。溶射輸出為4〇kW,溶射距離為1 20mm。三氧化 紀膜的厚度為200 //m。各本體溶射條件相同。 接著’在1 5 0 0〜1 6 0 0。(:熱處理形成耐蝕膜後之試料, 將在各溫度熱處理之試料切成剝離強度測定用試料(丨〇_ x lOmmx 2mm )以及膜開氣孔率測定用試料(5jnm>< 1〇mm>< 〇·卜〇· 15mm ;僅從膜部切出)。 、’、實驗C同樣地測定剝離強度。又,以(a r c h i m e d e a η) 法測疋開氣孔率。接著,對剝離強度測定用試料,垂直切 斷膜’將剖面鏡面研磨後,以掃瞄型電子顯微鏡觀察本體 ^膜的界面,以X線折射裝置分析。其結果,本試驗的試 料,在1 60 0億可得到35MPa之高剝離強度,此時膜的氣孔 率為0. 5 %。
第24頁 503449 修正
案號 90108419 五、發明說明(21) 表5 熱處理溫度 ΓΟ 剝離強度 (MPa) 開氣孔率 (容量%) 1500 42.0 1 1550 48.0 0.8 1600 --------- 35.0 0.5 【實驗F】 準備尺寸50x 5〇x 2 mm之純度99.7%的氧化鋁作盘 體。喷砂本體,整個本體的表面粗糙度Ra=1. 6 土 〇… 將各本體以丙酮超音波洗淨本體後,電漿溶射表6·所::。 各種稀土族氧化物為溶射膜。又,—部份的稀 混入氧化锆,而進行溶射。 、虱化物 ,f射條件為,中間層、对钱膜同時以4GL/分的流旦法 理形成耐餘膜後Λ土料膜的厚度為3 0 0 在16_熱處 1 · 1 η各式=切成耐鹵素氣體耐蝕性評價用試料(僅膜 ^ · 1 0mm X 1 Omm y n λ 、丨里联 驗。 · )’以實驗Α的方法進行耐蝕試 的气:成:ί Ϊ氧化物組成之耐蝕膜的試料,卜匕單氧化鋁 的忒枓’ _ _素氣體顯示有非 ::化鋁 氧化物添加氧化梦的w ^非*问耐蝕性。又,在稀土類 蝕性。 ^、、 膜,氣孔率變小,顯示更好的耐
503449 _案號90108412_年月曰 修正_ 五、發明說明(22) 4.8〜6.4//m,Wa (平均起伏度)為3.8〜4.5//m。多成分系 的場合有成為複數結晶相的情況。37. 5mol % Y2 03與 62. 5mo 1 e % Α 12 03的組合時比單一相時剝離強度高,得到 較佳的結果。
第26頁 503449 案號 90108412 A_η 曰 修正 五、發明說明(23) 表6 耐蝕膜的組成 耐蝕膜 的 μιη 剝離強度 MPa 開氣孔孛 容曼% 因耐蝕試驗 減少重曼 mg/cm Y2〇3 3.2 35 0.6 0.2 10mol%La2O3 90 mol % Y203 3.5 24 0.5 0.3 Ce〇2 2.8 23 1.2 0.2 Pr203 3.1 32 0.9 0.3 Nd2〇3 3.2 30 0.8 0.2 Sm203 4.3 29 0.9 0.2 Gd2〇3 3.8 31 1 0.3 Dy2〇3 2.9 28 1.2 0.2 37.5mol% Y203 糸1 62.5 mol %A1203 3.4 22 0.9 0.1 37.5 mol% Y203 浓2 62.5 mol %A1203 3.4 32 8 0.0 37.5 mol% Y203 ※之 62.5 mol %Α12Ο3(150μιη) +Y2〇3(中間層150μηι) 3.3 52 7 0.0 90 mol % Y203 10mol%ZrO2 3.0 34 0.3 0.1 95mol%(10mol%La2O3 · 90 mol% Y203) 5 mol%Zr02 2.9 36 0.2 0 90 mol % Ce02 10mol%ZrO2 3.5 30 0.6 0 90 mol % Nd203 10mol%ZrO2 3.2 28 0.4 0 90 mol % Sm203 10mol%ZrO2 3.1 29 0.3 0 A1203 2.7 38 0.1 9.5 系1 僅測出5Α12〇3 _ 3Υ2〇β 糸2 測出 5Α12〇3 3Υ2〇3,Al2〇3 Υ2〇3,Al2〇3 2Υ2〇3 # # 從以上所述,根據本發明,係為暴露於鹵素氣體的電 漿的耐i素氣體電漿用構件,難以發生因腐蝕之微粒浮游
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修正 於電漿容器内的空間,掉落、堆積於容器内的其他構件 接著,說明本發明之第2觀點。 根據本發明之第2觀點的積層體,前述反應生成物較 佳是含有三氧化釔與氧化鋁的複合氧化物組成之結晶相。 該複合氧化物的種類沒有限定,但舉例如以下者。 (1) YaA 15012 ( YAG ) ’含有三氧化紀與氧化銘以3 : $ 的比例,具有石權石(g a r n e t)結晶構造。 (2) YAl〇3(YAP),(perovskite)結晶構造。 (3) Y4A 12 09 (YAM),單斜晶系。 特佳為中間層含有三氧化釔•氧化鋁石權石組成之結 晶層,以及/或還含有Υ4Α12〇9(2Υ2〇3 ·Α12〇3)組成之結晶構" 造〇 構成纪化合物膜之紀化合物’舉例例如三氧化紀、人 有三氧化釔之固溶體、含有三氧化釔之固溶體(錐-三氧 化釔固溶體、稀土族氧化物固溶體)、含三氧化記之複人 氧化物(三氧化釔•鋁石榴石、Y4Al2〇9(2Y2〇3 · Al2〇3) 口 ΥΑ1〇3(Υ2〇3 ·Α 12 03 )等、三氟化在乙、Υ-Α1〜(〇) —ρ、Yzr〇 等。特別是紀化合物膜至少含有三氧化釔為佳,^ ^含
三氧化紀、含有三氧化紀之固溶體。特佳為三氧ς釔 或氟化钇。 本發明人更確認沿著中間層與基體的界面,且有配 著與中間層相同材質組成之微粒子’與在該微粒子之間步 成之空隙的細微構造。各空隙是被形成中間層之微粒子^ 基體包圍。具有如此特有的細微構造’向上提高三氧化: 303449 曰 _修正 -^^90^8412^ 五、發明說明(25) 膜與基體的密著性。認為是〃 ' 化合物膜的楊氏率之差。 σ 77緩和基體的揚氏率與釔 中間層的厚度之τ限並I 、 場合,比沒生成中間層的場限制,中間層非常薄的 大。中間層的厚度在3 _以 _的剝離強度明顯增 為更佳。 、,以提高剝離強度的觀點 又’中間層的後步上限介+ m以下的製造容易。中間層的厚^ ^別限制,實際上3〇 # 的剝離強度特別增加,從該 X在腋下,釔化合物膜 以下。 ”、、’中間層的厚度更佳為1 5 釔化合物膜用於要求高純 造裝置用途時,纪化合物中,::】4 ’特別是半導體製 金屬的含有量較佳為少,合:杜、鹼土族金屬、遷移 ⑽卿以下。再者,該含有十量值是車父以佳^00_以下’更佳 量分析測定。 有里疋以誘導結合電漿(ISP)定 特別是釔化合物膜中的鏺眉曲 原子單體的含有量)。、载原子浪度在3〇pPm以下(鐵 測的:纪T合物ΐ中混入少許鐵原子,膜的表面生成可目 班點:為了防止這樣的微小班點,耐蚀膜中的鐵 原子的》辰度必須在2Oppm以下。 士了製造本發明之積層冑,在基體或其前驅體上溶射 釔化合物膜而形成溶射膜,熱處理該溶射膜。 基體由燒結後的緻密質氧化鋁組成為佳,但亦可為氧 化銘的多孔質燒結體。又,亦可在其他基材上形成含有氧 ^5膏材層或塗佈層之後的熱處理推該膏材層和 臟謙觀猶,聊臞 :------ 月 _#號 曰 五、發明說明(26) 塗佈層燒結,形忐备# 制,板狀、膜狀等為佳基體。基體的形狀亦沒有特別限 蝕膜與下地的接著& 為1,2/^以上)。藉此提高耐 藉由使用多孔皙驊敫装麟 洌離而產生微粒。 比,可相對抑制λ辦沾”、、土體,使用緻密體的場合相 化合物膜於基體。特別是氏:=#又可更強固地附著紀 小且内部大之p # 、&面,若形成開口部份 氣孔中,’在溶射時溶融之粒子進入開 ί射固化’有固定溶射膜於表面的作用 令射釔化合物膜於基體上時,較 6 射,該壓力較佳為l00Torr以下。_疋在低壓狀悲洛 更減少,可更提高最終膜的耐敍性d ’使溶射膜的氣孔 形成溶射膜之後,藉由埶# W 體,至少使溶射腔诗姓ί:處 射膜與基體或其前驅 生成中門= 消除或減少溶射膜中的氣孔。 上限較佳是18〇〇t:以下t熱處理蹲物的 熱處理時的昇温L:ii; 乂圭為1小時以上。 防止二ί ί 上2GGt/小時。降溫速度為了 膜的裂痕,較佳是20(rc/小時以下。埶處理八 ί為佳。_間層的厚度以及記化合物膜的、結晶: 門長"以熱處理時間以及熱處理溫度控制。埶處理時 間長,溫度增加,中間層增厚,結晶粒增大。…時 續夫ί ΐ,由於三氧化釔與氧化鋁熱膨脹係數相近,為了 級和兩者之間的熱膨脹差特別進行熱處理,在這之後將^ 案號 9mnfui9 五、發明說明(27) 意其差異 h ΐϊϋ,還發現溶射膜的熱處理溫度在1 400 °c以 時,1 e二二ί耐蚀膜的剝離強度。熱處理溫度達1400 °c =里f體的材質與耐蝕膜的材質之間容易生成反庫層,苴 結果提鬲耐蝕膜的剝離強度。 心 ’、
昉,^曰^面,浴射膜的熱處理溫度增加,接近1 8 0 0 °C :蝕:Li之反應層的附近產生鋁元素的移動、擴散, 1 650 °C以下強度將降低。從此觀點,熱處理溫度較佳在 165〇: 乂下,更佳為160(rc以下,特佳為155代以下。 接著面的基體之剝離強度,以後樹枝試驗測定 接者面的^徑5. 2mm時較佳為丨5肝&以上。 剝離G 熱處理之積層體’對釔化合物膜的基體之 1 500 ^3 上’例如可達35MPa以上。特別是在 的高剝離強度熱處理時,可得2曝以上,甚至35胸以上 紀化iμ本發明之積層體可藉由依序積層氧化銘粉末層、 合粉末 > 的粉纟(例如二氧化記粉末)與氧化銘粉末的混 而乙化合物的粉末(例如三氧化記粉末)層 而得。、θ成形體,將邊積層成形體在1 500 1 800 1共燒結 導體ϊϊπ耐:性構件,有熱,裝置等的半 性氣體ϊί ΐ 導體製造裝置,使用_系腐蝕 中:二成之半導體清潔用氣體。不僅是鹵素氣體電漿 氣中且:能在㈣氣體肖氧素氣體混合《氣體的電漿雾團 耐蝕性之半導體製造裝置。 503449 _ 案號 90108412 五、發明說明(28) 鹵素氣體可舉例如C1F3、nf 、 等。 3、 紀化合物膜的中心線平均粗輪 Wa較佳為1 以上。藉此,半導^ 腐餘以及晶圓加工屑之微粒,較難 掉落、堆積於容器内的其他構件。 這是因為釔化合物膜難以產生 化合物膜的Ra增加(表面留有凹凸 加工產生之少量的微粒,保持於紀 於二間’掉洛堆積於其他構件。 在此,耐蝕膜的表面的Ra大( 凹凸。微細觀察該表面,存在著凹 部,該凸部是由從凹部突出之粒子 表面Ra增大時,由於齒素氣體的電 域’粒界從凸部(粒子)的根部部 產生。然而’如此造成之微粒的增 遊、掉落於容器内的空間。 Ra過大時,促進膜表面的腐蝕 觀點Ra在6 //m以下為較佳,膜的Wa (比較例2-1 ) ' (製造方法) 以丙酮將純度99· 6重量%、開 基體(尺寸lOmmx l〇mmx厚度2mm) 純度9 9 · 9重量%的三氧化紀,溶射 4 0 L /分的流量流入氬氣,以1 2 l /八 曰 WF,
Cl2、bci3 度R a較佳a 马3 //ra以上, ^裝置w各構件的 龟於容器内的空間, 微粒之作用的同時,釔 )了避免腐餘和晶圓 化&物臈的表面,浮遊 粗糙),是指表面留有 部,與鄰接該凹部的凸 組成。因此,耐蝕膜的 漿入侵表面的凹部區 分腐蝕,將促進微粒的 加少,可防止微粒浮 而增加微粒,因此從此 較佳在3 // m以下。 » » 氣孔率0 · 1 %的氧化鋁 以超音波洗淨’溶射 條件如下所述。即,以 的流量流入1 °溶射輸
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出為40kW ’溶射距離為120min。以下的欠叙 1列谷實施例 比較 例,溶射條件亦相同。 洛射膘厚為4…。再者’溶射臈的厚度 (micrometer)測定溶射前與溶射後的試料之,、1叶 點的測定平均值算出溶射前後的試料的厚度。^ , 的測定值之最大值與最小值的差為q " m ^ ^ 膜厚 熱處理。 μ為對溶射者不進行 (評價結果) 以掃猫型電子顯微鏡、能量分散型1線分光鏡 (spectroscope)、Χ線折射裴置觀測膜的狀熊。 (表面) 以X線折射裝置分析三氧化在乙膜的結晶相。從膜的上 方入射X線。三氧化釔的結晶相為立方晶系(cubic),豆他 為單斜晶系(Monoclinic)。在溶射膜的表面,發現長度 5〜10//m、寬0.;!〜〇.5//m左右的裂痕。該裂痕每丨⑽以…有 3〜5個(參照第2圖)。 (剖面) 二氧化釔膜内發現為層狀構造(第3圖)。因為具有 層狀的構造,預測為容易剝離的結構。發現有大約卜5 # m 的氣孔。然而,沒有從膜表面到基材的貫通孔。 (表面粗糙度) 膜之表面的中心線平均粗糙度Ra為3.5 。 (起伏度)
Wa(平均起伏度)為2· 5。但是,Ra&Wa是以 Tayler - Hobson 公司製造的「Forin Talystur f 2 S4」以掃 503449 修正 λ_η 曰 案號 9010S419 五、發明說明(30) 瞒長度4· 8mm測定。 (剝離試驗) 將1 chlban公司製造的「Nice tack」貼附於膜上,進 行亲j離w式驗。其結果’膜全面剝離,而貼附於上。 (剝離強度) 1 ·將成膜试料切成1 〇mm X 1 Qmin X 2mm (包含纪化合物 膜的厚度)的厚度。 2·將切斷之試料以丙顯I進行超音波洗淨5分鐘。 3·準備附有環氧系接著劑的A1柱拴(stud pin) 圓(p形hM〇technica&司製造)。該接著區域為直徑5 2_的 4.使柱拴接觸釔化合物膜,在150 t:加熱處理!小 日、,以%氧系接著劑接著固定柱拴與釔化合物膜。 及下5部ch=拾及f層體於張力試驗裝製的上部-Ck以 “:Γ/八。Λ ograph ’將紀化合物膜從柱拴與積 分鐘的速度向上剥離。從剝離臈時的負荷重 里以及接者面積計算接著強度(剝離強度1 ^
Pin的接著面積)。此時,在接著、5Γ里 的值不做為測定值。 剜的邛位有剝離之試料 (研磨) 以#H〇磨石粗研磨膜表面,剝離該膜。 (耐姓試驗) 、 在C1F3 (downflow plasma)中,為认 小時。C1F3氣體流量為75sccm, C維持本試料2 (氮氣體)的流量為l〇0sccin ’以續:= gas)
I
--------導結合電漿ICP
I 503449 _ 案號90108412_年月日 修正 _ 五、發明說明(31) (13·56Ηζ、輸出800W)激發(excitation),氣體壓力為 0· 1 torr。之後以掃瞄型電子顯微鏡觀察剖面,將膜從基 體剝離。 (熱循環試驗) 實施1 0次的加熱-冷卻循環。1循環是以8 〇 〇 °c /分鐘昇 溫至800 °C,在80 0 °C加熱1小時,急速以4〇〇 °C /分鐘降至 室溫,在於8 0 0 t:加熱1小時。之後,試料的重量變化為〇 · 2mg/cm2。之後’進行前述剝離試驗,發現膜全面剝離。
(實施例2 -1 ) (製造方法) 在純度99.6重量%、開氣孔率〇1 %以下的氧化鋁基 材^尺寸· =111111 x 1 0_ X厚度2mm )之上,溶射純度99. 9 f量%的三氧化釔。溶射膜的厚度為46 " m。冑厚度的測 2值之最大值與最小值的差為j 5 " m。將該溶射 料,在1600 °C於大氣汽圃名± 礼%團軋中熱處理3小時。昇溫速唐在 1 2 0 〇 〇C以上為2 0 〇它/小眭 勺 收垃土 皮又在 r主二、 L j時。又,降溫速度為1 50 °c /小時 (表面) 1 ) 方 比 膜 之 料 圖 上 ( 之 膜 試 。以X線折射裝置八扣氧化釔粒子燒結之構造(第2~4 入射X線,檢測出:::二紀膜的結晶相。從膜之 較例2-1 )的折射^日日糸的从。比㈣加熱處理品 表面的最高點斤:半取二點的半值幅咖),熱處理 三氧化釔的結晶性择:減小。這顯示在1 60 0熱處理, (比較例1 )的立方' 本實施例1與未加熱處理之 ^系三氧化紀的主要折射最高點 503449 _案號 9010841?_年月日_ 五、發明說明(32) 的半值幅示於表7。 表7 最高點位置(2Θ) 29.1 33.7 48.5 57.6 半值幅(實施例2·1) 0.14 0.14 0.12 0.12 半值幅(比較例2_1) 0.16 0.24 0.31 0.19 (剖面) 沒有膜的剝離。發現約1〜5 // m的氣孔。然而,未發現 有從膜表面到氧化鋁基材的貫通孔(第2 - 5圖)。熱處理 前在三氧化釔膜發現之層狀構造消失。 (三氧化釔膜與氧化鋁基材的界面) 在三氧化釔膜與氧化鋁基材的邊界產生約丨〇的反應j (第5圖)。該反應層,以能量分散型X線分光裝置分析石 j ’疋氧化銘與三氧化釔反應生成者。又,依X線折射的 結果’反應層的結晶相為Al5〇i2 (YAG )以及γ4Αΐ2〇9 (YAM ^三考慮氧化銘基體的緻密性(開氣孔率〇 % )以及溶射 f化釔膜的多孔性,氧化鋁基體的氧化鋁(A 12 03 )是名 一氧化釔膜(Y2 〇3 )擴散者。反應層與氧化鋁基體的邊界有 /jn的微粒子與空隙。該空隙,是被形成反應層之微米 :,化鋁基材包圍。氧化鋁基材與反應層是經由微粒4 因此密著性不良,但是緩和反應層與氧化鋁基和 的%氏率的差異,剝離變困難。 線拚::知瞄型電子顯微鏡、能量分散型X線分光裝置、) I-i H則#果之膜的剖面之構造示於第2-1圖。 503449 _ 案號 flm〇8412__年月日__ 五、發明說明(33) 氧化鋁基材之上有氧化鋁與三氧化釔的反應層約1 〇 // m, 其上為三氧化紀膜。 (表面粗糙度) 膜之表面的中心線平均粗糙度Ra為4· 3 // m。 (起伏度)
Wa (平均起伏度)為2. 2。但是Ra以及Wa是使用
Tayler-Hobson公司製造的「Form Talysurf Series Z54」測定掃瞒(scan)長度4· 8mm。 (剝離試驗)
將ichiban公司製造的「Nice tack」貼附於膜上,進 行剝離試驗。其結果,膜沒有剝離。 (研磨) 以# 140 (diamond)磨石粗研磨膜表面,在界面沒有 膜的剝離。再以# 1 〇 〇 〇的磨石研磨,但在界面沒有膜的剝 離(以剝離試驗確認沒有膜的剝離)。 (耐蝕試驗)
與比較例2-1 同樣,在C1F3 (down-flow plasma)中 進行耐蝕試驗。試驗後以化學天秤測定試料的重量,重量 臭=在0· 2mg/cm2以下。又,以掃瞄型電子顯微鏡觀察剖 面¥ ’未發現膜的剝離。再實施前述剝離試驗,沒有發現 剝離。 C熱猶環試驗) 與比較例2 -1同樣進行熱循環。之後,訧斜的會晉繆
503449
氧化銘、YAG以及:r氧 5、8· 4以及8· 1。本實施例製广的熱膨脹係數(ppm/k)為8· 材緩緩向膜改變。推斷這是在之試料的熱膨脹係數從基 因之一。 疋 熱循環試驗沒有膜剝離的原 (實施例2 - 2〜實施例2 -1 0 ) 將溶射膜厚度約50〜100 之夂以如 、 熱處理3 *時的評價結果示於表。’刀別在16^
的基體表面喷砂處理,各基體表 對/合射月’J 奴衣面的Ra改變為如表所示。
503449 _案號90108412_年月日_ 五、發明說明(35) ΪΟ ΓΟ 'La -U ΓΟ ϋο to INJ rj〇 室赘Η υο υο UO υο υο O'! kj〇 0^1 氡化鋁 密度 Ζ, σ: 1—1 基體表面 的Ra jc/m ISJ KJ^ 00 00 熱處理前 的膜厚 jtm 1600°C 5小時 1600°C 5小時 170CTC 3小時 170CTC 3小時 1600°C 3小時 160CTC 3小時 熱處理 條样 無剝離 無剝離 無剝離 無剝離 無剝離 無剝離 剝離試驗 滴 \〇 4^ ώ bo 4^ υ〇 B ^ |SJ> 〇 CO 〇\ ΓΟ υο Lh [〇 CO B ^ ISJ K? to ΓΟ 剝離強度 MPa 1〜3jcm的燒 結微粒子β 無袈痕 1〜3jum的燒 結微粒子a 無袈痕 的燒 結微粒子。 無裂痕 1〜3j^m的燒 結微粒子。 無裂戒 1〜3/^ m的燒 結微粒子。 無裂痕 1〜3;m的燒 結微粒子。 無裂痕 表面搆造 η 1〜5牌 的氩孔 1~5 μπι 的氣孔 1~5 iim 的氣孔 1〜5"m 的氣孔 1〜5牌 的氣孔 1~5 fjim 的氣孔 别面構造 瓣 m ΓΟ 1»"« 00 反應層 的厚度 U m 1HI11 第39頁 503449 _案號90108412_年月日_ 五、發明說明(36) 表9 耐爸 k試驗 熱循環試驗 ^^的結晶相 卟觀 剝離試驗 外觀 剝離測試 Y2〇3 膜表面 反應層 實施例2-1 立方-Υ2〇3 YAG YAM 無變化 無膜的 剝離 無變化 無膜的 剝離 實施例2-2 立方孑2〇3 YAG YAM 無變化 無膜的 剝離 無變化 無膜的 剝離 實施例2-3 立方-Υ2〇3 YAG YAM 無變化 無膜的 剝離 無變化 無膜的 剝離 實施例2-4 立方-Υ2〇3 YAG YAM 無變化 無膜的 剝離 無變化 無膜的 剝離 實施例2-5 立方-Υ2〇3 YAG YAM 無變化 無膜的 剝離 無變化 無膜的 剝離 實施例2-6 立方-Υ2〇3 YAG YAM 無變化 無膜的 剝離 無變化 無膜的 剝離 ι·Βΐ 第40頁 503449 _案號90108412_年月日_ 五、發明說明(37) 比較 例2-1 實施 例 2-10 實施 例2-9 實施 例2-8 實施 例2-7 3.96 3.96 3.96 3.96 3.96 氣1匕紹 密度 1~« ΪΟ 〇 基體表面 的Ha jtm \〇 ν〇 1L 〇 〇 熱處理前 的膜厚 jUm 1600°C 10小時 1600°C 10小時 1600°C 7.5小時 160CTC 7.5小時 熱處理 條# 無剝離 無剝離 無剝離 無剝離 無剝離 剝離試驗 υο iwh ui U1 〇\ 〇 B ^ ι>ο iwh ΓΟ INJ i\j INJ 〇 &匀 3 ? ο k? H-i υΐ 00 剝離強度 Mpa 斑褰^ 為,g 1〜3jtm的燒 結微粒子。 無裂痕 1〜3/im的燒 結微粒子。 無袈飧 1〜3;m的燒 結微粒子。 無裂痕 表面搆造 舞 1〜5脾 的氣礼 1〜5脾 的氣孔 1〜5脾 的氣孔 1~5卿 的氣礼 1〜5卿 的氣礼 剖面搆造 歸 m 無反 應相 Ui 反應層 的厚度 U m 第41頁 503449 _案號90108412_年月日 修正 五、發明說明(38) 表11 耐蝕試驗 熱循環試驗 膜的結蟲相 外觀 剝離試驗 外觀 剝離測試 Y2〇3 膜表面 反應層 實施例2刀 立方-Υ2〇3 YAG YAM 無變化 無膜的 剝離 無變f匕 無膜的 剝離 實施例2-8 立方-Υ2〇3 YAG YAM 無變化 無膜的 剝離 無變(匕 無膜的 剝離 實施例2-9 立方-Υ2〇3 YAG YAM 無變化 無膜的 剝錐 無變化 無膜的 剝離 實施例2-10 立方-Υ2〇3 YAG YAM 無變化 無膜的 剝離 無變fb 無膜的 剝離 比較例2-1 立方_了2〇3 箪斜晶-ΥΡ — 有膜的剝離 φι 8〇%) 無膜的 剝離 無變化 有膜的剝離 100% 在實施例2-2,於1 6 0 0 °C進行3小時的熱處理(與實施 例2-1相同)。但是溶射膜的厚度為88 //m。該結果與實施 例2-1是相同的。在實施例2-3,在1 700 °C熱處理溶射膜3 小時。該結果與實施例2 - 1是大致相同的,但是反應層增 加若干厚度。在實施例2 - 4,熱處理條件與實施例2 - 3相 同,處理若干厚的溶射膜,其結果與實施例2-3相同。實 施例2 - 5、2 - 6,溶射膜的熱處理溫度為1 6 0 0 °C,處理時間 增長為5小時。其結果得到與實施例2 - 1、2 - 2大致相同結 果,但是反應層的厚度若干增加。 實施例2-7、2-8、2-9、2-10 ’比實施例2-5、2-6熱 處理時間更長。其結果,發現處理時間增加,中間層趨於 增厚。 實施例2-3,(在1 7 0 0 °C熱處理3小時),第2-6凸顯
第42頁 503449 案號 90108412 五 、發明說明(39) 是試料之表面的掃瞄型電子顯微鏡照片,在二 ^ ^ ^ % ^ #二乳4匕在乙膜斑 氧化銘基材的界面附近的剖面之掃目苗型雷早祐 、/、 % 丁释貝微鏡昭Η + 於第2-7圖。在三氧化釔膜内,為2-5 #ιη系的:# /、、、乃 子燒結之構造,比起在1 6 0 0 t熱處理的場人,私山e 外口 ,粒成長更為 提升。又,膜、中間層以及基體的細微構造與實施例2一/、、 (實施例2 -1 1〜2 - 1 2 ) (製造方法) 將市售的氧化鋁粉末成形、燒成,而製作密度 3· 5 6g/cm3、氣孔率約10 %的(實施例2 —^ )與密^3 76 藝 g/cm3、氣孔率約5 %的(實施例2-12 ),(實施例& · 2-卜2-10,比較例密度為3. 96 g/cin3 )的氧化鋁基體。在 該氧化紹基體上溶射純度99.9wt %的三氧化釔。氧化銘基 體的大小為1 Omm X 1 0mm X 2mm。溶射膜厚度為91 # m。溶射 膜的厚度,是以測微計測定溶射前與溶射厚的試料厚^, 根據5點的測疋平均值鼻出溶射前厚的試料之厚度的差。 又,膜厚度的測定值之最大值與最小值的差為1 m。將 該溶射後之試料,在1 6 0 0 °C於大氣氛團氣中熱處理3小 時。昇溫速度在1 2 0 0 °C以上為2 0 0 °C /小時。又,降溫速度 為1 50 °C /小時。 ® 對所得之試料進行與實施例2-1〜2-10相同的試驗。結 果示於表2-6、2-7。從表2-6、2-7的結果可發現以下所 述。在1600 °C加熱時,氧化鋁基體的密度變成3.9g/cm3以 上。即使引起熱處理之氧化鋁基體的收縮,亦沒有三氧化 釔膜的剝離。又,與實施例2 -卜2 -1 2同樣地實施剝離試
第43頁 503449 案號 90108412 Λ:_3. 曰 修正 五、發明說明(40) 驗,但是沒有發現剝離。藉由緩和在反應層之YAG以及YAM 組成之微粒子與空隙之構造因氧化鋁基體與三氧化釔膜的 熱處理之收縮,可提高膜的密著性。 〇〇 υο \〇 \〇 ^ ^ 〆 〇 * r? ^ 5: 上 〇 〆 〇 1 r? %ι ]Πβ. 篛 輮 1 # 〇 〇\ 3 货 INJ Lh ^ <J B ? 菩i &)输 總萍, 雜 g ΐΙ 雜 > Si 雜 藤 m S T ^ 3 S Τ ^ 3 & 铱 1~i »—> 3辦勒
第44頁 503449 _案號90108412_年月日_ 五、發明說明(41) 表13 耐1: 試驗 熱循環試驗 膜的結晶相 外觀 剝離試驗 卟觀 剝離測試 Y2〇3 膜表面 反應層 實施例2-11 立方-Υ2〇3 YAG YAM 無變化 無膜的 剝離 無變化 無膜的 剝離 實施例2-12 立方-γ2〇3 YAG YAM 無變化 無膜的 剝離 無變化 無膜的 剝離 (實施例2 - 1 3〜2 - 1 6 ) 以與實施例2- 1相同溶射條件製作各試料,施予下述 熱處理而得各試料,與實施例2- 1同樣地評價特性。氧化 铭的密度,熱處理前的溶射膜的膜厚度,兩者皆與實施例 2 - 1相同。 表14 熱處理條件 膜的物性 °C X hr 剝離試驗 剝離強度 Ra Wa 反應層厚度 MPa # m jX m 實酬2-13 1400χ 3 無剝離 41 4.8 2.6 2 實翻2-14 1450χ 3 無剝離 45 4.2 2.1 3 實施(列2-15 1500χ 3 無剝離 50 4.9 2.5 5 實翻2-16 1550χ 3 無剝離 41 4.4 2.3 7 熱處理後的膜,實施例2-13〜2-16,於剝離試驗都沒 有剝離。膜的表面,由粒徑卜3 // m的燒結粒子構成,是沒 有裂痕的構造。膜的剖面,有1〜5 // m的氣孔。表面、剖面
第45頁 503449 _案號 9010841? 五、發明說明(42) 曰 修正 構造亦與實施例2 - 1相同。 膜的表面粗糙度(Ra )、奴 疮、釗触%由- ^ 吳伏度(Wa)、反應層的厚 度、剝離強度示於表1 4。熱處理、w — 。 4JlQ . niL …、处理溫度在1 40 0 °C到1 5 50 t:保 持3小時,可得到40MPa以上的高剝離強度。 (釔化合物膜中的雜質金屬元素的定量) 藉由電暈放電質5分析裝置(GDMS),定量實施例 2一1的構件的膜中雜質金屬元素。定量值示於表15。 表15 元紊 含有量(ppm) 元t 含有量(ppm) Li <01 Mn 0.5 Na 4 Fe 10 — Mg 1 Co 1 A1 18 Ni 6 Si 10 Cu 3 K 0.7 Zn 3 Ca 2.1 Mo <0.1 Sc <01 W <1 Ί1 0.3 缔土族金屬 <2 (除Y之外) V <0.1 Cr 1
驗金屬元素、鹼土族元素,總含有量分別在1 〇 ppm以
第46頁
、了紀之過渡金屬元素的總含有量在50ppm以下。 ("、燒結法製造之積層體)
在圓筒内徑6〇咖之模型内,放入三氧化釔粉末,在 一 8^的負荷重量成形。當模型内有三氧化釔成形體,放 ^ 一氧化紀粉末與氧化鋁粉末的混合粉末(莫耳比3 ·· 5 一,形、積層。再投入氧化鋁粉末,成形並積層。使用 ^ —氧化紀粉末的平均粒徑為2 Α ^,氧化鋁粉末的平均粒 為〇.6//m。二氧化紀層的厚度為imm,混合粉末層的厚 度為〇· 8mm ’氧化鋁層的厚度為5mn]。如此製作之成形體, 在於20〇MPa之壓力下以靜水擠壓(hydr〇static press; CIP )成形處理。在大氣中丨70 0燒成3小時,而製作燒結 體。 、對所得之燒結體進行微構造觀察、結晶相的認定、剝 離忒驗以及剝離強度測定。表面及剖面的觀察結果,未發 現一氧化紀層到氧化鋁基材層的貫通裂痕。剖面微構造觀 察以及X線折射裝置之結晶相測定,三氧化紀層與氧化銘 層之間確定為YAG(Y3A15012)相的生成。剝離試驗確認沒 有剝離。剝離強度為40MPa。 【發明效果】 如上所述,根據本發明,可提供氧化鋁組成之基體 與’形成於4基體上的紀化合物膜之積層體,膜很難從美 體剝離,特別是與腐蝕物質接觸後,亦難以剝離之積層土 體。 、曰
Claims (1)
- 503449六、申請專利範圍 _ 1. 一種耐豳素氣體電漿用構件,該構件為暴露 氣體的電漿中之耐鹵素氣體電漿用構件,1且 二圏素 體’與至少形成於該本體之表面的耐蝕膜,其中的本 膜之對前述本體之剝離強度為15肿3以上,且前述耐魅耐餘 的表面粗糙度Ra在1 · 5以下。 ^膜 件 2·如:請專利範圍第丨項所述之耐_素氣體電漿 其中前述耐蝕臈的相對密度在9〇%以上。 件 3·如申請專利範圍第丨項所述之耐函素氣體電漿 其中前述耐敍膜的表面粗糙度在以上。 ^ 4· 一種耐_素氣體電漿用構件,該構件為暴露於處去 乳體的電漿中之耐鹵素氣體電漿用構件,其具備構的女、 :的:至:::於該本體之表面的耐蝕膜,其中前述耐蝕 臈的中心線平均粗糙度Ra為1·2 以上。 了蝕 5 ·如申明專利範圍第4項所述之耐鹵素氣體電漿 件,其中刚述耐蝕性膜的相對密度為9 〇 %以上。 6 ·如申請專利範圍第丨〜5項之任一項所述之 體電漿用構件,其中前述耐餘性膜的Wa (起伏度)二2乳 m以上。 巧· L以 7·如申請專利範圍第卜5項之任一項所述之 體電襞用構件,其中前述耐钕性膜的下地面為多孔質孔 t 1 t明專利範圍第1〜5項之任一項所述之耐_辛氣 體電漿用構件,i中兪、+、Λ , J國京乱 粗糙度以i耐㈣膜的下地面的中心線平均 棹,9立ΐ::: Γ範圍第8項所述之耐齒素氣體電漿用構 虫性膜jjF地面的中心線平均粗糙度Ra為 肥ΙϋΐΜΚΙ/ΙΙΗΐ ΙΚν.Ιίΐν^^ΓΙΓ/ΜΡ it r JI !>.. ......... — ----— __ 第48頁 ^1^90108412 六、申請專利範圍 2 // m以下。 I 0 ·如申請專利範 體電漿用構件,苴中乂、第1〜5項之任一項所述之耐鹵素氣 %以下。 則述耐蝕性膜的開氣孔率在1 · 5容量 II ·如申請專利範圍^ r 體電漿用構件,苴中义第1〜5項之任一項所述之耐鹵素氣 1 //m以上的裂痕;;前述耐蝕膜沒有長度3 以上、寬〇, 體電漿用構件'專直利φ乾^圍第1〜5項之任一項所述之耐鹵素氣 件本體與前述耐蝕膜2 $耐鹵素氣體電漿用構件在前述構 係數是在前述耐飯膜2j具備中間層,該中間層的熱膨脹 脹係數之間。 膑的熱膨脹係數與前述構件本體的熱膨 體電漿用構件,專圍第1〜5項之任一項所述之财_素氣 件本體盘前if ^ ^刚述耐鹵素氣體電漿用構件在前述構 耐上具備中間層,該嶋 14.如申迹本體的構成構件之混合物或反應物。 構件,盆中乂^、+、利乾圍第1 2項所述之耐鹵素氣體電漿用 〃 τ則逃中間層的厚度在20 Am以下。 構件,豆中申二專利範圍第1 3項所述之耐鹵素氣體電漿用 /、τ則迷中間層的厚度在20 //m以下。 構件16·直如中專利範圍第13項所述之耐齒素氣體電聚用 體之構成構中間層’前述⑯膜的構件之對前述本 加。構成構件的濃度比從前述本體側向前述耐餘膜側增 利範圍第卜5項士一項^之射南音顏 ΚΓ ΧΜίΧϊϊΐί 麵· ___________ 、〜 第49頁 體電漿用構件, 义 18.如申性直w則述耐钱膜的構件含有釔。 構件’其“Ί7項所述之耐南素氣體電漿用 下。 …膜中含有之鐵原子的濃度在30卿以 ^ #!〇 λ * * ^ 如中請專利 體電漿用構件,1中义第〜4項之任一項所述之耐鹵素氣 化合物。 ^則述耐蝕膜的材料含有稀土類元素之 體電滎用構件'專其利中乾J5第1〜5項之任一項所述之财鹵素氣 Μ —種射/述耐蝕膜的材料含有锆之化合物。 造如申請專利=第Κ電裝用構件之製造方法,是在製 漿用構件時,在製造兑、十項+之任一玄項所述之耐*素氣體電 料而形成溶射Ϊ 耐蝕膜時,溶射前述耐蝕膜之材 構件2的3 .如申,專利範圍第2 2項所述之耐齒素氣體電裝用 料。 不/去,其中是在低壓狀態溶射前述耐蝕膜的材 Μ # Μ ·如申請專利範圍第2 2項所述之耐鹵素氣體電数用 構件的製造方^法,其中熱處理前述溶射膜。 水用 構件2 5 \如S請專利範圍第2 2項所述之耐齒素氣體電漿用 物。的製造方法,其中前述耐蝕膜的材料含有釔的化合 構侔2 6 ·如申请專利範圍第2 2項所述之耐齒素氣體電漿用 〜^15造方法,其中前述熱處理是在1 400〜1 6 00 t之溫 503449 --90108412 六、申請專利範圍 年月 曰 你π: 度進行。 2 7 ·如申請專利範圍第2 2項所述之耐鹵素氣體電漿用 構件的製造方法,其中藉由以化學氣相沈積法或電化學氣 相沈積法在前述溶射膜上積層前述耐蝕膜的材料,而消除 前述溶射膜表面的氣孔。 28· 一種耐ii素氣體電漿用構件之製造方法,是在製 造如申睛專利範圍第1〜5項之任一項所述之耐鹵素氣體電 衆用構件時,是以化學氣相沈積法或電化學氣相沈積法成 膜前述耐餘膜。29· 一種積層體,係為鋁組成之基體,與形成該基體 上之紀化合物膜之積層體,其中沿著前述基體與前述釔化 合物膜之界面存在有與鋁與記化合物的反應生成物。 3 0 · 一種積層體,係為鋁組成之基體,與形成該基體 上之紀化合物膜之積層體,其中沿著前述基體與前述纪化 合物膜之界面存在有與銘與紀化合物的反應生成物組成之 中間層。 3 1 ·如申請專利範圍第2 9或3 〇項所述之積層體’其中 前述釔化合物含有三氧化二釔。 3 2 ·如申請專利範圍第2 9或3 0項所述之積層體’其中 前述紀化合物含有氟化纪。 33.如申請專利範圍第29或30項所述之積層體’其中 前述反應生成物含有三氧化二釔與鋁之複合氧化物組成之 結晶相。 34 ·如申請專利範圍第3 3項所述之積層體’其中别述 反應生成物含有Υ3Α15〇12組成之結晶相。_第51頁 503449 案號 90108412 年 修正 六、申請專利範圍 之積層體,其中前述 35 .如申請專利範圍第3 3項所速^ 反應生成物含有Y4 A 12 09組成之結晶相。 t 36. —種積層體,係為鋁組成之基體、,/、形成該基體 上之釔化合物膜之積層體,其中沿著前,基,與前述記化 合物膜之界面具備含有鋁與釔化合物的複e氧化物組成之 結晶相的中間層。 3 7 ·如申請專利範圍第3 6項所述之積層體’其中前述 釔化合物含有三氧化二釔。 38 .如申請專利範圍第3 6或3 7項所述之積層體’其中 前述纪化合物含有氟化紀。 3 9 .如申請專利範圍第3 6或3 7項所述之積層體,其中 前述反應生成物含有Y3 A15012組成之結晶相。 40 .如申請專利範圍第3 6或3 7項所述之積層體,其中 前述反應生成物含有Y4 A 1 2 〇9組成之結晶相。 41 ·如申請專利範圍第2 9、3 0或3 6項之任一項所述之 積層體,其中沿著前述中間曾與前述基體的界面,具有與 前述中間層相同材質組成之微粒子,與在該微粒子之間形 成之空隙配列的細微構造。42·如申請專利範圍第29、30或36項之任一項所述之 積層體’其中如述紀化合物膜的表面的中心線平均粗糙度 Ra為3〜6//m,Wa(起伏度)為1〜3/Zm。43·如申請專利範圍第29 3 〇或3 6項之任一項所述 w xj \j [3Γ •一 尸 積層體,其中前述耐蝕膜對前述本體之剝以 上0 Sebastans試驗測定接著面之直又 條考面之直徑為5.2111111時為15^41)&以第52頁
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- 2001-04-09 TW TW90108412A patent/TW503449B/zh not_active IP Right Cessation
- 2001-04-16 US US09/835,857 patent/US6783875B2/en not_active Expired - Lifetime
- 2001-04-17 EP EP20010303504 patent/EP1158072B1/en not_active Expired - Lifetime
- 2001-04-17 EP EP20070017724 patent/EP1892318B1/en not_active Expired - Lifetime
- 2001-04-17 DE DE60137885T patent/DE60137885D1/de not_active Expired - Lifetime
- 2001-04-17 KR KR10-2001-0020358A patent/KR100429058B1/ko active IP Right Grant
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TWI468364B (zh) * | 2008-11-12 | 2015-01-11 | Applied Materials Inc | 抗反應性電漿處理之保護塗層 |
TWI709653B (zh) * | 2018-02-15 | 2020-11-11 | 日商京瓷股份有限公司 | 電漿處理裝置用構件及具備其之電漿處理裝置 |
TWI714965B (zh) * | 2018-02-15 | 2021-01-01 | 日商京瓷股份有限公司 | 電漿處理裝置用構件及具備其之電漿處理裝置 |
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EP1892318A1 (en) | 2008-02-27 |
EP1158072A2 (en) | 2001-11-28 |
KR100429058B1 (ko) | 2004-04-29 |
KR20010098643A (ko) | 2001-11-08 |
EP1892318B1 (en) | 2011-07-13 |
US20020018921A1 (en) | 2002-02-14 |
EP1158072A3 (en) | 2004-01-07 |
EP1158072B1 (en) | 2009-03-11 |
US6783875B2 (en) | 2004-08-31 |
DE60137885D1 (de) | 2009-04-23 |
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