經濟部智慧財產局員工消費合作社印製 575536 A7 ---- B7 五、發明說明（1 ) 〔技術領域〕 本發明係有關於主要使用於晶片板與電漿鈾刻裝置之 夾具（」1g)等半導體製造用之夾具之高純度陶瓷零件 之接合方法，尤其是由碳化矽所構成之高純度陶瓷零件之 接合方法。 〔背景技術〕 氧化擴散工程或C V D (下面亦稱化學氣相成長法） 工程，以及近來之電漿蝕刻工程等之半導體製造裝置用夾 具皆使用各種陶瓷。其中由碳化砍所形成之陶瓷（下面簡 稱碳化矽質陶瓷）因爲係熱傳導性、耐熱性、耐酸性優異 之材料，所以廣泛地利用做爲半導體製造裝置用零件。 半導體製造裝置用之陶瓷製品多被要求有複雜形狀或 大型形狀。但，以碳化矽質陶瓷爲首之陶瓷通常不易加工 ，要將複雜形狀之燒結體等以整體加工製造多屬困難，另 外對於大型形狀也由於煅燒爐等之製造設備之限制，多無 法製造。 因此，通常係將企望之製品分割成多個零件（以下亦 稱爲元件）而構成，再分別接合各零件而成最終成品（接 合體成品）。 先前，一般習知之陶瓷零件之接合方法有將煅燒前之 狀態下以粘合劑類接合，或煅燒後以有機系、無機系粘合 劑類接合等，惟煅燒前之粘合劑類之接合很費工夫’且煅 燒後有無法修正之問題，另一方面煅燒後利用粘合劑類接 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐) " '^ -4 - . --------IT---------線 (請先閲讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 575536 A7 ____ B7 五、發明說明（2 ) 合，則有硬度與氣密性降低，純度劣化之大問題。此外’ 先前之接合方法中不易修復破損之成品。 此外，在特開平1 0 — 8 7 3 7 6號中，揭示了組合 具有雌雄之接合部位之碳化矽質零件，爲使該接合部位所 形成之間隙互相連通，利用毛細管作用在該間隔塡充、凝 固熔融矽以接合之方法，惟在塡充間隙之矽部分之耐熱性 及耐酸有問題。 另一方面，在特開平9 一 2 4 9 4 5 5號揭示了將碳 零件組合，並以含有碳稞粒之熱固性樹脂粘合劑接合碳零 件以做爲接合體，連同粘合劑成分將該拉始體轉化成碳化 矽，再以化學氣相成長法在其表面形成碳化矽被膜之方法 。但是該方法使用樹脂粘合劑，因此接合部分之硬度變脆 ，另外以碳零件做起始構件，所以有工程多，工夫費時之 問題。 另外，在特開平9 一 1 0 7 0 2 4號中揭示了在製造 形成有碳化矽被膜之石墨製品時，利用面接觸使石墨製品 密接粘合後，以化學氣相成長法形成碳化矽被膜之方法， 惟因所用之基體構件爲硬度低之石墨，因此不易在接觸面 強力粘合。另外，又揭示以由高溫粘合劑所構成之接縫塡 充材料塡充接合面之間隙部並熱處理以碳化，藉以確保密 接性，但是基本上基體之石墨等與碳化矽被膜之熱膨脹係 數不同，所以不易始終保持密接性。 亦即，先前不容易發現一種可以簡單地且保持純度將 高純度陶瓷零件接合，而且製得之接合體之高溫硬度、耐 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) -5- 經濟部智慧財產局員工消費合作社印製 575536 A7 ___ B7 五、發明說明（3 ) 熱性、耐蝕性優異，並可以對處複雜形狀之接合方法。 〔發明之揭示〕 本發明提供一種高純度陶瓷零件之接合方法（以下簡 稱本接合方法），其特徵爲使多個陶瓷被接合零件接近配 置於企望之接合部位，並利用化學氣相成長法，在上述陶 瓷被接合零件之表面形成碳化矽固定被覆層以接合上述陶 瓷被接合零件。 ’ 本接合方法之態樣大別之有將企望之接合部位密接配 置之情形，以及在企望之接合部位間設置間隙部配置之情 形。 圖式之簡單說明 第1圖爲表示應接合之高純度陶瓷零件之斜視圖。 第2圖爲表示將高純度陶瓷零件之側面部接觸接合之 狀態之縱剖面圖。 第3圖爲表示在組合體之表面形成C V D —碳化矽固 定被覆層之狀態之縱剖面圖。 第4圖爲表示使高純度陶瓷零件之表面部接觸並接合 之縱剖面圖。 第5圖爲表示在組合體之表面形成C V D —碳化砂固 定被覆層之狀態之縱剖面圖。 第6圖爲表示將高純度陶瓷構件保持間隔並以側面接 合之狀態之縱剖面圖。 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） —^.--------------訂--------- (請先閱讀背面之注意事項再填寫本頁) -6- 575536 經濟部智慧財產局員工消費合作社印製 A7 B7 五、發明說明（4 ) 第7圖爲表示在組合體之表面形成C VD -碳化矽固 定被覆層之狀態之縱剖面圖。 第8圖爲表示在組合體之表面形成C VD -碳化矽固 定被覆層之狀態之縱剖面圖。 〔符號之說明〕 10(1). 1 0 ( 2 )—板狀零件，1 3 ( 1 )、 1 3 ( 2 )—側面部，1 5 ( 1 )、 1 5 ( 2 )—表面部 ，2 0、2 0 > —零件之組合體，2 3、2 3 / —碳化砂 固定被覆層（外殼），30、30 / -接合體，200、 20〇/ —零件之組合體，230、230> —碳化矽固 定被覆層（外殼），230d —碳化矽塡充體，300、 3〇0 > —接合體，d —接合部位表面間距離，e —上部 開口，e — —下部開口。 實施發明之最佳形態 以下，詳細說明本發明。 適用本接合方法之高純度陶瓷零件除了非氧化物系陶 瓷與氧化物系陶瓷之外，還可使用金屬矽、石英玻璃等。 陶瓷有例如碳化砂、砂、氮化砂、碳化鈦、氮化錦、錦土 、氧化锆、石英、富鋁紅柱石（mulhe )，矽鋁氧氮（ S1al〇n )陶瓷等◦另外，在本說明書中所謂高純度陶瓷係指 大致上雜質爲小於〇 . 1 %者。 該等陶瓷也可以被複合化。例如一個陶瓷成爲基塊（ 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) ---------訂---------· -7- 經濟部智慧財產局員工消費合作社印製 575536 A7 _ B7 五、發明說明（5 ) matrix)，而在該基塊中分散以纖維狀或稞粒狀之其他陶 瓷之塡充物（filler )而形成強體也可以。 另外，該等陶瓷也可以爲多孔質，再者該空隙部分也 可以用其他陶瓷塡充。例如，使多孔質之碳化矽燒結體含 浸熔融金屬矽並以矽完全塡充該空隙，成爲精密化，氣體 不透過性之矽浸滲碳化矽等爲理想。 此外，利用化學氣相成長法所形成之碳化矽所形成之 高純度陶瓷零件由於金屬雜質特質特少，所以做爲半導體 製造裝置用之零件爲理想。 本發明之接合方法係用於接合以此種陶瓷所形成之零 件之方法，惟零件之形狀並無特別之限制，其基本形態有 例如圓柱狀、桿狀、圓筒狀、板狀、片狀、薄膜狀、角柱 狀、盤狀、圓錐狀、角錐狀、球狀等。該接合不限於同種 形態之零件間，例如板狀零件間，也可以在不同形態之零 件間進行。此外，在本說明書中，·被接合之高純度陶瓷零 件稱爲被接合陶瓷零件，而所謂接合係指多個被接合陶瓷 零件最後成爲一體之謂。 該此零件通常將其陶瓷之原料粉末依據其企望之模型 成形後，經由燒結而得，惟零件之形狀爲板狀、薄片狀、 薄片狀之情形時，也可以利用化學氣相成長法來形成。 以下，一邊參照圖式一邊說明本發明之實施形態。本 接合方法係將多個被接合陶瓷零件接近其接合部位而配置 者而大別之可分爲兩個態樣。亦即，配置於使其接合部位 接近至相接觸爲止之情形以及使其接近至具有間隙部之情 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） !!![..#--------訂---------線· (請先閱讀背面之注音？事項再填寫本頁) -8- 575536 A7 ______ B7 五、發明說明（6 ) 形。 (請先閱讀背面之注意事項再填寫本頁) 首先，要就配置於使接合部位接近至相接觸（以下簡 稱爲接觸配置）之情形加以說明。·接觸配置時，係將多個 被接合陶瓷零件配置組合俾接合部位互相接觸，以先構成 零件之組合體。 在此，對第1圖所示之高純度陶瓷零件之兩個板狀零 件1〇（1 )、 1 0 ( 2 )檢討其側面部1 3 ( 1 )、 1 3 ( 2 )或表面部1 5 ( 1 )、 1 5 ( 2 )接合之情形 〇 首先，檢查其在側面部之接合。 做爲接合部位之側面部1 3 ( 1 )、 1 3 ( 2 )被組 合成可確保其表面之密接性，如第2圖所示，構成組合體 2 0° 爲確保接合部位之接觸，雙方宜利用面接觸爲理想， 基本上如兩側面平行而無彎曲等，其表面可以毫無間隙地 重疊，即可以形成牢固接合之組合體2 0而較理想。 此外，兩表面宜硏磨處理良好，表面之平均表面粗度 R a小於1 // m，較佳爲小於0 · 5 // m，最大表面粗度 經濟部智慧財產局員工消費合作社印製 R m a X爲小於3 // m，較佳爲1 · 5 // m。平均表面粗 度R a宜小於1 // m，且最大表面粗度R m a X小於3 // m則更佳。另外，平均表面粗度R a及最大表面粗度 R m a X係利用電子表面粗度計並依照J I S B — 〇6 0 1等測定之。 更理想爲將接合部位進行鏡面加工，由於確保充分之 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） -9- 經濟部智慧財產局員工消費合作社印製 575536 A7 _ B7 五、發明說明（7 ) 平滑度與平坦度，所以接合部位之密接性更加提昇。 其次，如第3圖所示，接觸配置時，在該零件之組合 體2 0之表面，利用化學氣相成長法形成碳化矽（以下簡 稱CVD - S i C)之固定被覆層2 3。亦即，硬度高之 碳化矽被膜變成覆蓋該組合體2 0之外表面整體之高硬度 之外殼（Shell )，而內部之組合體2 0被該外殼完全地固 定’整體上形成堅固之接合體3 0。 該接合體3 0由於以側面部接合板狀零件，比具有一 定厚度者具有更寬表面積之板狀構件。 另一方面，同樣也可以進行兩個板狀零件1 0 ( 1 ) 、10 (2)之表面部15(1)、 15 (2)之接合。 由於該板狀零件之表面間之接合而形成陶瓷層壓體。此種 形態亦爲本發明之重點之一。 做爲接合部位之表面部1 5 ( 1 )、 1 5 ( 2 )被組 合成表面充分接觸而重疊，並且如第4圖所示，構成層壓 之零件之組合體2 0。 與側面接合之情形相同，兩表面越以面接觸密接時， 亦即，兩表面硏磨處理良好，表面之平均表面粗度R a小 於1 // m及/或最大表面粗度R m a X小於3 // m，則可 有充分之接觸而越理想。惟在層壓體之情形下’應使面接 觸之表面積大，所以爲使其全面接觸，表面之平坦度與平 行度越好越理想。 如第5圖所示，與側面之接合之情形相同’在該組合 體20 /之表面形成CVD — S i C固定被覆層2 3 > ° 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） Γ-------------^---------^^^1 (請先閱讀背面之注咅？事項再填寫本頁) -10- 575536 A7 _ B7 五、發明說明（8 ) 如此一來，高硬度之碳化矽被膜變成覆蓋該組合體之外表 面整體之外殼（Shell )，而內部之層壓狀之組合體完全被 固定，整體上形成堅固之接合體30/。 在本發明中，在接合高純度陶瓷零件時所形成之碳化 矽固定被覆層之厚度宜爲2 0至2 0 0 0 //m，較佳爲 3〇至1〇〇〇//m ，更佳爲5 0至8 0 0 //m 。較此爲 薄之膜厚，無法獲得充分之硬度或剛性。又如膜厚太厚時 ，則要以化學氣相成長法形成時，需要極長之時間，所以 生產性降低，成本上不利。 高純度陶瓷零件之組合體係藉由碳或矽質陶瓷之保持 夾具等所保持而設置於CVD爐內，形成CVD - S i C 膜。另外，C V D - S 1 C膜不僅形成於組合體之表面， 而且也形成於該等保持夾具之表面.，所以要利用C V D -S 1 C膜進行組合體之被覆時，組合體與保持夾具同時被 接合。因此，該等保持夾具於高純度陶瓷零件之接合後， 宜藉由噴沙或切削加工由接合體去除。 其次，要就在企望之接合部位間設置間隙部來配置（ 以下簡稱間隙部配置）之情形加以說明。在間隙部配置法 中，係將應接合之多個高純度陶瓷零件組合成保持該接合 部位之表面間距離以構成具有間隙部之零件之組合體。 與接觸配置法之情形相同，針對第1圖所示之兩個陶 瓷板狀零件1 0 ( 1 )、1 0 ( 2 )檢查接合該側面部 13(1)、 13 (2)與表面部15(1)、 15(2 )之情形。 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） (請先閱讀背面之注咅？事項再填寫本頁) --4^裝--------訂---------· 經濟部智慧財產局員工消費合作社印製 -11 - 575536 A7 B7 五、發明說明（9 ) 首先，考慮其側面部之接合，如第6圖所示，做爲接 合部位之側面部1 3 ( 1 )、 1 3 ( 2 )組合成可以保持 (請先閱讀背面之注意事項再填寫本頁) 間隔（接合部位之表面間距離）d以構成零件之組合體 2〇〇。 間隔d如設定於1 0至1 0 〇 0 // m爲理想。間隔d 小於1 0 // m時，C V D之原料氣體無法充分進入該間隙 以致接合部位之硬度變脆，所以不理想，再者，如間隔d 超過1 0 0 0 //m時，不但需要大量之原料氣體塡充該間 隙，而且CVD時也變長，成本上不合算。 在間隙配置法時，在接合部位設置間隙d，藉由 C V D - S i C塡充該間隙，接合部位之間可以接合得更 堅牢。 在間隙部配置法之情形下，接合部位表面被硏磨處理 良好，表面之平均表面粗度R a小於1 // m，小於0 · 5 // m爲佳，如最大表面粗度R m a X爲小於3 // m，較佳 爲1 · 5 // m時，則原料氣體容易均勻進入，原料氣體之 經濟部智慧財產局員工消費合作社印製 濃度分佈會均勻化，在間隙部分之接合體不易形成空隙， 所以較爲理想。平均表面粗度R a小於1 // m而最大表面 粗度R m a X小於3 // m時更佳。 最後，製得如第7圖所示之接合體3 0 0。亦即， CVD - S 1 C固定被覆層2 3 0變成高硬度之外殼（ shell )並完全固定陶瓷板狀零件1 0 ( 1 )、 1 0 ( 2 ) ，而塡滿接合部位之間隙d之S 1 C部分（2 3 0 d )與 該固定被覆層2 3 0係在其上部開口 e及下部開口 e /連 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） -12- 575536 A7 _ B7 五、發明說明（ίο ) 接成爲一體。 (請先閱讀背面之注意事項再填寫本頁) 同樣地，也可以在表面部分接.合板狀零件，並如第8 圖所示形成層壓體（接合體）300 /。 此外，如第8圖所示，要將表面部隔開以層壓零件時 ，宜將兩者垂直放置以保持之間隔d，或在表面部間插入 碳或碳化矽質之間隔片以保持間隔d。該等間隔片如實質 上沒有問題時，亦可以直接留在成品之接合體中（碳化矽 被膜中），也可在必要時以噴沙法或切削加工法由接合體 中去除。 另外，在本發明中，可以藉由在形成接合體之零件之 一邊之表面形成突起部（凸部，雄部，突條部），而在另 一邊形成嵌合該突起部之嵌合部（‘凹部，雌部，槽部）俾 更確實進行高純度陶瓷零件間之接合。 如上配置之高純度陶瓷零件之組合體係藉由碳或碳化 矽質陶瓷之保持夾具等保持住而設置於C V D爐中形成 C V D - S 1 C膜與接觸配置法之情形相同。 經濟部智慧財產局員工消費合作社印製 用於實於本發明之C V D爐並無特別之限制，惟以橫 式、縱式、鐘罩式等較常用，而加熱法則適用直接通電法 ，高頻感應加熱或雷射加熱法。 CVD — S 1 C膜基本上係在10 00至1600°C ，較佳爲1 1 0 0至1 5 0 0 °c之非氧化性氣氛中引進原 料氣體堆積而成。 原料氣體可以使用（1 )由不同之化合物供應矽與碳 之原料氣體系，例如，S 1 C 14與CH4，s i C 14與 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） -13- 經濟部智慧財產局員工消費合作社印製 575536 A7 __ B7 五、發明說明（11) c 3 Η 8 ^ Si C 1 4 與 C6H!4，S 1 C 1 4 與 CC 1 4， S12H6與CH4等也可以，（2)或由同一化合物供應 石夕與碳之原料氣體系，例如，C Η 3 S i C 1 3， (CH3)2SiC12，( C H a ) 3 S i C 1， (CH3) 4S i ，CH3S iHC 12也可以。此等原料氣 體與氫、氦、M等載氣（earner gas) —起被輸入爐內。 對於形成C V D - S i C膜之壓力並無特別之限制， 惟爲了將原料氣體充分導入零件組合體之間隙部內並以碳 化矽實質上完全塡充該間隙部，宜設定於1至3 0 0托（ T 〇 r r )，較佳爲1〇至100托左右之減壓。 如上所述，在上述C V D條件下，可以事先形成應接 合之零件之板狀、片狀、薄膜狀、薄板狀之碳化矽。亦即 ，此時，可使用石墨與碳之基體做爲基板，在其上面形成 企望厚度之碳化矽被膜，基板之石墨等爾後可在空氣中 ，藉由1 0 0 0 °C左右之溫度進行熱分解之方法去除而製 得薄板狀之碳化矽（C V D — S 1 C )。 此外，利用本發明製得之高純度陶瓷零件之接合體做 爲半導體之製造裝置用夾具時，要接合之高純度陶瓷零件 以含雜質較少者爲理想，尤其金屬雜質之總含量少於4 0 p p m，較佳爲少於3 0 P P m，.更佳爲少於2 0 p p m ，最佳爲少於1 0 P P m爲理想。 在此所謂金屬雜質係指砂以外之鐵、銅、鎂、釩、鎳 、錳、鈉、鉀、鋁等，爲有可能被混入晶片（wafer )中而 對半導體裝置降低絕緣電阻與降低氧化矽（s i ◦ 2 )之耐 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） K--------------tr---------線 (請先閱讀背面之注意事項再填寫本頁) -14 - 575536 經濟部智慧財產局員工消費合作社印製 A7 B7____ 五、發明說明（12 ) 壓進而引起Ρ η接合漏泄不良等之有害元素。 另外，形成於該高純度陶瓷零件表面之c ν D 一 S i C被覆層之純度宜爲金屬總含量少於5 0 P P b ，較佳爲 少於3 0 p p b ，更佳爲少於1〇p p b。 〔實施例〕 以下要以實施例詳細說明本發明。 (1 )高純度陶瓷零件組合體之形成 〔實施例1〕 首先，如第1圖所示準備兩片如第2圖所示之4公分 正方而厚度爲1 m m之具/3型結晶構造之C V D — S i C 晶片做爲被接合陶瓷零件。又C V D — S i C晶片之平均 表面粗度Ra爲〇 · 2//m，最大表面粗度Rmax爲 2 · 0 // m做爲被接合陶瓷零件。 以碳夾具（未圖示）按住該等零件之兩端，再如第2 圖所示，使其側面相接觸配置。亦即，使兩個零牛密接以 形成4公分X 8公分X 1公釐之形狀之零件組合體。 〔實施例2〕 準備兩片與實施例1相同之C V D — S i C晶片做爲 被接合陶瓷零件。如第4圖所不’使其兩個表面設置成接 觸而層壓。 〔實施例3〕 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） '· —-------裝--------^--------- (請先閱讀背面之注意事項再填寫本頁) -15- 575536 A7 - B7 五、發明說明（13) 準備兩片與實施例1相同之C V D — s i C晶片。接 著’利用碳夾具將兩片晶片零件配置成T字形。 〔實施例4〕 準備兩片與實施例1相同之C V D — S 1 C晶片。如 第6圖所示，將兩片晶片配置成側面部間隔d成爲5 0 0 β m之組合體。 〔實施例5〕 除了使用矽浸滲碳化矽晶片做爲高純度陶瓷零件之外 ，與實施例1同樣地配置兩片晶片。另外，矽浸滲碳化矽 晶片之平均表面粗度R a爲〇 . 2 //m，最大表面粗度 Rmax 爲 2 · 2//m〇 (2) CVD — S i C固定被覆層之形成 接著，將實施例1至5所配置之高純度陶瓷零件之組 合體設置於CVD爐內，在真空中加熱至1 0 0 0°C以進 行烘乾（b a k 1 n g )處理。亦即，在此狀態下，引進氫氣， 壓力調整至1 0 0托並保持6 0分鐘。接著’以1 5 °C / 分鐘之昇溫速度加熱並昇溫至1 2 5 0 °C之成膜溫度。 然後，導入C Η 3 S i C 1 3做爲形成碳化矽之固定被 覆之用之料化合物，在高純度陶瓷零件之表面分別形成 250//Π1之CVD — S 1 C固定被覆層。 另外，針對實施例1至5測定接合前與接合後之表面 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） (請先閲讀背面之注咅心事項再填寫本頁) 罗裝 ----訂---------. 經濟部智慧財產局員工消費合作社印製 -16- 575536 A7 _ B7 五、發明說明（14) 之金屬雜質之濃度。實施例1至4之接合前與接合後皆爲 4 0 p P b。另外，實施例5之接合前爲1 8 p p m，接 合後爲45ppb。 (請先閱讀背面之注意事項再填寫本頁) 由碳夾具卸下形成有CVD - S i C固定被覆層之接 合體即分別獲得碳化矽接合體。雖然以精密拉伸試驗機（ Insuon )對該等接合體進行拉伸試驗，惟拉伸強度非常高 ，接合邰位之硬度與其他部分比較毫無遜色，在純度、耐 酸性亦爲優異之接合體。 〔比較例〕 與實施例1 一樣，準備兩片4公分正方1公釐厚之 C V D - S i C晶片。粘合劑係使用將變性酚醛樹脂6 5 質量％與鱗狀天然石墨粉末3 5質量％混練而成者，並使 其與實施例1 一樣地密接。 接著’在空氣中加熱至2 0 0 °C以硬化粘合劑，再於 非氧化性氣氛中昇溫至1 〇 〇 〇 t：以碳化粘合劑中之樹脂 。這樣就製得碳化矽接合體。粘合劑層之厚度成爲2〇〇 β m 。 經濟部智慧財產局員工消費合作社印製 (3 )抗彎強度與耐熱衝擊性 利用在實施例1 ，實施例4及比較例1所製得之接合 體進行抗彎強度及耐熱衝擊性之評估。 ①抗彎強度 依據J I S R 1 6 0 1所規定之方法測定碳化矽接 本紙張尺度適用中國國家標準（CNS)A4規格（21〇 χ 297公釐） -17- 575536 A7 B7 五、發明說明（15 ) 合體在室溫中之抗彎強度。 ②耐熱衝擊性 依據熱衝擊法（thermal shock )進行耐熱衝擊性之評 估。將碳化矽接合體加熱後，即投入水中驟冷以賦予溫度 差，並測定碳化矽接合體之硬度變化。 在表1中同時表示硬度變化激烈之最低溫度差（耐熱 衝擊溫度△ T )之値與抗彎強度之値。 表 1 抗彎強度（Μ P a ) 耐熱衝擊溫度△ T (°c ) 實施例1 2 5 0 4 5 0 實施例4 2 9 0 4 5 0 比較例1 1 5〇 3 0 0 〔產業上之可利用性〕 根據本發明之高純度陶瓷零件’之接合方法，比先前之 接合方法可以更簡單製得具有複雜形狀與大型形狀、高硬 度而耐熱性、耐酸性優異，且純度高之陶瓷接合體。 尤其是，當高純度陶瓷零件係由CVD-S1C或矽 浸滲碳化矽等所構成之碳化矽質零件時，如以c V D -S i C形成固定被覆層時，則高純度陶瓷零件與固定被覆 層基本上會變成同級之高純度之碳化政質之材質，而可製 得高硬度，而耐熱性、耐酸性優異，而且純度層級高之接 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） C請先閲讀背面之注意事項存填寫本頁)Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs 575536 A7 ---- B7 V. Description of the Invention (1) [Technical Field] The present invention relates to a fixture mainly used for wafer boards and plasma uranium engraving devices ("1g) A method for joining high-purity ceramic parts such as jigs for semiconductor manufacturing, especially a method for joining high-purity ceramic parts composed of silicon carbide. [Background Art] Various ceramics are used for semiconductor manufacturing device clamps, such as an oxidation diffusion process, a CVD (hereinafter also referred to as a chemical vapor growth method) process, and a recent plasma etching process. Among them, ceramics formed by carbonization chopping (hereinafter referred to as silicon carbide ceramics) are widely used as parts for semiconductor manufacturing devices because they are materials with excellent thermal conductivity, heat resistance, and acid resistance. Ceramic products used in semiconductor manufacturing equipment are often required to have complicated shapes or large shapes. However, ceramics headed by silicon carbide ceramics are usually not easy to process. It is difficult to manufacture sintered bodies with complex shapes as a whole. In addition, large shapes cannot be manufactured due to the limitations of manufacturing equipment such as calciners. Therefore, the desired product is usually divided into a plurality of parts (hereinafter also referred to as components), and each part is then joined to form the final product (joint product). Previously, the conventional joining methods for ceramic parts include joining with adhesives in the state before firing, or joining with organic or inorganic adhesives after firing, but joining with adhesives before firing. It takes a lot of work and there are problems that cannot be corrected after calcination. On the other hand, the size of the paper used for adhesive bonding after calcination applies the Chinese National Standard (CNS) A4 specification (210 X 297 mm) " '^ -4- . -------- IT --------- line (Please read the notes on the back before filling this page) Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs 575536 A7 ____ B7 V. Invention Explanation (2) When combined, there is a problem that hardness and air tightness are reduced, and purity is deteriorated. In addition, it is difficult to repair the damaged product in the previous joining method. In addition, Japanese Patent Application Laid-Open No. 10—8 7 3 7 6 discloses the combination of silicon carbide parts with male and female joints. In order to communicate the gaps formed by the joints with each other, capillary action is used to fill the gaps. 2. The method of solidifying molten silicon to join, but the heat resistance and acid resistance of the silicon part in the gap filling problem. On the other hand, Japanese Patent Application Laid-Open No. 9-1 2 4 9 4 5 5 discloses a combination of carbon parts, and the carbon parts are bonded with a thermosetting resin adhesive containing carbon particles as a bonded body. The method of converting the starting body into silicon carbide, and then forming a silicon carbide film on the surface by chemical vapor growth. However, this method uses a resin adhesive, so the hardness of the joint portion becomes brittle, and the carbon component is used as the starting member, so there are many projects and time and labor. In addition, Japanese Patent Application Laid-Open No. 9-1 0 0 0 2 4 discloses that when a graphite product having a silicon carbide film is formed, the graphite product is closely adhered by surface contact, and then a silicon carbide film is formed by a chemical vapor growth method. This method, but because the base member used is low hardness graphite, it is not easy to adhere strongly to the contact surface. In addition, it was also revealed that a joint material made of a high-temperature adhesive was used to fill the gaps of the joint surface and heat-treated to carbonize to ensure the adhesion. However, the thermal expansion coefficient of graphite and the like of the substrate is basically different from the silicon carbide film , So it is not always easy to maintain tightness. That is to say, it was not easy to find a kind of high-purity ceramic parts that can be simply and maintain the purity, and the high-temperature hardness and resistance to the paper can be used in accordance with China National Standard (CNS) A4 (210 X 297 mm) ). -------- ^ --------- (Please read the notes on the back before filling in this page) -5- Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs 575536 A7 ___ B7 V. Description of the invention (3) A bonding method which is excellent in heat resistance and corrosion resistance, and can be used in various shapes. [Disclosure of the Invention] The present invention provides a method for joining high-purity ceramic parts (hereinafter referred to as the present joining method), which is characterized in that a plurality of ceramic parts to be joined are arranged close to a desired joining part, and a chemical vapor growth method is used. A silicon carbide fixing coating layer is formed on the surface of the ceramic bonded component to bond the ceramic bonded component. The difference between this joining method is that the desired joints are closely arranged, and the gaps are arranged between the desired joints. Brief Description of Drawings Fig. 1 is a perspective view showing high-purity ceramic parts to be joined. Fig. 2 is a longitudinal sectional view showing a state in which the side portions of the high-purity ceramic component are contact-bonded. Fig. 3 is a longitudinal sectional view showing a state where a CVD-silicon carbide fixed coating is formed on the surface of the assembly. Fig. 4 is a longitudinal sectional view showing that the surface portions of the high-purity ceramic parts are brought into contact with and joined to each other. Fig. 5 is a longitudinal sectional view showing a state where a CVD-carbide sand fixed coating layer is formed on the surface of the assembly. Fig. 6 is a longitudinal cross-sectional view showing a state where high-purity ceramic members are spaced and joined by side faces. This paper size applies to China National Standard (CNS) A4 (210 X 297 mm) — ^ .-------------- Order --------- (Please read first Note on the back, please fill in this page again) -6- 575536 Printed by A7 B7, Consumer Cooperative of Intellectual Property Bureau of the Ministry of Economic Affairs 5. Description of Invention (4) Figure 7 shows the formation of C VD on the surface of the assembly-silicon carbide fixed coating Vertical sectional view of the state of the layer. Fig. 8 is a longitudinal sectional view showing a state where a CVD-silicon carbide fixed coating layer is formed on the surface of the assembly. [Explanation of symbols] 10 (1). 1 0 (2) —plate parts, 1 3 (1), 1 3 (2) —side parts, 1 5 (1), 1 5 (2) —surface parts, 2 0, 2 0 > — assembly of parts, 2 3, 2 3 / — fixed coating (shell) of carbonized sand, 30, 30 /-joints, 200, 20 0 / — assembly of parts, 230, 230 >-Silicon carbide fixed coating (shell), 230d-Silicon carbide filler, 300, 300 >-Joints, d-Distance between surfaces of joints, e-Upper opening, e-Lower opening. Best Mode for Carrying Out the Invention The present invention will be described in detail below. In addition to non-oxide-based ceramics and oxide-based ceramics, high-purity ceramic parts to which this joining method is applicable can also include metallic silicon, quartz glass, and the like. Ceramics include, for example, carburized sand, sand, nitrided sand, titanium carbide, brominated nitride, bronzing earth, zirconia, quartz, mullite, and silicon aluminum oxide (S1alon) ceramics. The so-called high-purity ceramic in this specification means those whose impurities are substantially less than 0.1%. Such ceramics can also be compounded. For example, a ceramic becomes a base block (this paper size applies to Chinese National Standard (CNS) A4 specification (210 X 297 mm) (Please read the precautions on the back before filling this page) --------- Order- -------- · -7- 575536 A7 _ B7 printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs 5. Description of the invention (5) matrix), and the fibers are dispersed in a fibrous or granular form in the base. Other ceramic fillers can also be used to form strong bodies. The ceramics may be porous, and the voids may be filled with other ceramics. For example, a porous silicon carbide sintered body is impregnated with molten metal silicon, and the gap is completely filled with silicon, so that the silicon carbide is impregnated with silicon that is impervious to gas and impermeability. In addition, high-purity ceramic parts made of silicon carbide formed by the chemical vapor growth method are ideal as parts for semiconductor manufacturing devices because they have very few metal impurities. The joining method of the present invention is a method for joining parts formed of such ceramics, but the shape of the parts is not particularly limited, and its basic forms include, for example, a cylindrical shape, a rod shape, a cylindrical shape, a plate shape, and a sheet shape. , Film-like, angular pillar-like, disc-like, conical, pyramid-like, spherical, etc. The joining is not limited to parts of the same form, for example, plate parts, but also between parts of different forms. In addition, in this specification, a high-purity ceramic part to be joined is referred to as a joined ceramic part, and the so-called joining means that a plurality of joined ceramic parts finally become integrated. This part is usually formed by sintering the raw material powder of ceramics according to its desired model, but when the shape of the part is plate, sheet, or sheet, it can also be formed by chemical vapor growth . Hereinafter, embodiments of the present invention will be described with reference to the drawings. This joining method is a method in which a plurality of ceramic parts to be joined are arranged close to their joints and can be divided into two aspects. That is, it is arranged in a situation where the joints are brought close to contact and when they are brought close to each other with gaps. The paper size applies the Chinese National Standard (CNS) A4 specification (210 X 297 mm) !!! [. . # -------- Order --------- Line · (Please read the note on the back? Matters before filling out this page) -8- 575536 A7 ______ B7 V. Description of the invention (6) shape. (Please read the precautions on the back before filling out this page.) First, explain how to place the joints in close contact with each other (hereinafter referred to as the contact arrangement). • In the contact arrangement, a plurality of ceramic parts to be joined are arranged and assembled, and the joints are brought into contact with each other to form a part assembly first. Here, the two plate-shaped parts 10 (1) and 10 (2) of the high-purity ceramic part shown in FIG. 1 are reviewed for the side parts 1 3 (1), 1 3 (2), or the surface part 1 5 (1), 1 5 (2) Joining condition 0 First, check the joining at the side. The side parts 1 3 (1) and 1 3 (2) as the joint part are combined to ensure the surface adhesion. As shown in FIG. 2, the assembly body 20 ° is formed to ensure the contact of the joint part. It is ideal to use surface contact. Basically, if the two sides are parallel without bending, the surfaces can overlap without gaps, that is, it can form a firmly bonded combination 20, which is ideal. In addition, the two surfaces should be well-honed. The average surface roughness R a of the surface is less than 1 // m, preferably less than 0 · 5 // m. The maximum surface roughness is printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs. ma X is less than 3 // m, preferably 1 · 5 // m. The average surface roughness R a should be less than 1 // m, and the maximum surface roughness R m a X should be less than 3 // m. In addition, the average surface roughness R a and the maximum surface roughness R m a X are measured using an electronic surface roughness meter in accordance with J I S B — 0,601, and the like. It is more ideal to perform mirror processing on the joints. To ensure that the paper size is sufficient, the Chinese National Standard (CNS) A4 (210 X 297 mm) is applied. 5. Description of the invention (7) Smoothness and flatness, so the adhesion of the joints is further improved. Next, as shown in Fig. 3, in the contact arrangement, a fixed coating layer 23 of silicon carbide (hereinafter referred to as CVD-S i C) is formed on the surface of the component assembly 20 by chemical vapor growth. That is, the silicon carbide film with high hardness becomes a high-hardness shell covering the entire outer surface of the composite body 20, and the internal composite body 20 is completely fixed by the housing, forming a solid joint as a whole. 3 0. This joint body 30 is a plate-like member having a wider surface area than a plate member having a certain thickness since the plate-like members are joined at the side portions. On the other hand, the surface portions 15 (1) and 15 (2) of the two plate-shaped members 10 (1) and 10 (2) can also be joined in the same manner. A ceramic laminate is formed by bonding between the surfaces of the plate-like parts. This form is also one of the important points of the present invention. The surface portions 1 5 (1) and 1 5 (2) as the joining portions are fully contacted and overlapped by the composite surface, and as shown in FIG. 4, a laminated body 20 is formed. As in the case of side joining, when the two surfaces are in close contact with each other, that is, the two surfaces are honing well, the average surface roughness R a of the surface is less than 1 // m and / or the maximum surface roughness R ma X is less than 3 // m, the more ideal it is to have sufficient contact. However, in the case of a laminated body, the surface area of the surface contact should be large, so that the flatness and the flatness of the surface should be as good as possible in order to make full contact. As shown in Fig. 5, the same situation as the side bonding is to form a CVD on the surface of the combined body 20 / S i C fixed coating 2 3 > ° This paper size applies the Chinese National Standard (CNS) A4 specification ( 210 X 297 mm) Γ ------------- ^ --------- ^^^ 1 (Please read the note on the back? Matters before filling out this page)- 10- 575536 A7 _ B7 V. Description of the invention (8) In this way, the high-hardness silicon carbide film becomes a shell covering the entire outer surface of the assembly, and the laminated assembly inside is completely fixed , Forming a solid joint body 30 / as a whole. In the present invention, the thickness of the silicon carbide fixing coating layer formed when joining high-purity ceramic parts is preferably 20 to 2 0 0 // m, more preferably 30 to 100 0 // m, and more It is preferably 50 to 8 0 0 // m. Compared with this, the film thickness is thin, and sufficient hardness or rigidity cannot be obtained. Also, if the film thickness is too thick, it takes a long time to form by the chemical vapor growth method, so the productivity is reduced and the cost is disadvantageous. The combination system of high-purity ceramic parts is held in a CVD furnace by carbon or silicon ceramic holding jigs, etc., to form a CVD-S i C film. In addition, the CVD-S 1 C film is formed not only on the surface of the assembly, but also on the surfaces of these holding fixtures. Therefore, when the CVD-S 1 C film is used to cover the assembly, the assembly and the holding fixture are simultaneously Being engaged. Therefore, after the holding fixtures are joined to the high-purity ceramic parts, they should be removed from the joined body by sandblasting or cutting. Next, a description will be given of a case where a gap portion is provided between the desired joint portions (hereinafter referred to as a gap portion arrangement). In the gap arrangement method, a plurality of high-purity ceramic parts to be joined are combined to form an assembly having parts with gaps while maintaining the distance between the surfaces of the joints. As in the case of the contact arrangement method, check that the two side surface portions 13 (1), 13 (2) and the surface portion 15 are joined to the two ceramic plate-shaped parts 10 (1) and 10 (2) shown in Fig. 1 (1), 15 (2). This paper size applies to China National Standard (CNS) A4 (210 X 297 mm) (Please read the note on the back? Matters before filling out this page) --4 ^ Pack -------- Order-- ------- · Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs -11-575536 A7 B7 V. Description of the invention (9) First, consider the joining of the side parts, as shown in Figure 6, as the joining The side parts of the parts 1 3 (1), 1 3 (2) can be combined to maintain (please read the precautions on the back before filling out this page) the interval (distance between the surfaces of the joint parts) d to form a component assembly 2 〇. The interval d is desirably set to 10 to 10 〇 0 // m. When the interval d is less than 1 0 // m, the CVD raw material gas cannot sufficiently enter the gap, so that the hardness of the joint part becomes brittle, so it is not ideal. Furthermore, if the interval d exceeds 1 0 0 0 // m, not only a large amount of The raw material gas fills the gap and becomes longer during CVD, which is not cost effective. In the gap arrangement method, a gap d is provided at a joint portion, and C V D-S i C is used to fill the gap, so that the joint portions can be more firmly joined. In the case of the gap arrangement method, the surface of the joint portion is honed well, and the average surface roughness R a of the surface is less than 1 // m, preferably less than 0 · 5 // m, such as the maximum surface roughness R ma X When it is less than 3 // m, preferably 1 · 5 // m, the raw material gas is easy to enter uniformly. The concentration distribution of the raw material gas in the consumer cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs will be uniform, and the joints in the gap part Since it is not easy to form a void, it is preferable. It is better when the average surface roughness R a is less than 1 // m and the maximum surface roughness R m a X is less than 3 // m. Finally, a joint body 3 0 0 as shown in FIG. 7 was prepared. That is, the CVD-S 1 C fixed coating layer 2 3 0 becomes a high-hardness shell and completely fixes the ceramic plate-shaped parts 10 (1), 1 0 (2), and fills the gap d of the joint portion. Part S 1 C (2 3 0 d) and the fixed covering layer 2 3 0 are at the upper opening e and the lower opening e / even the size of this paper applies Chinese National Standard (CNS) A4 (210 X 297 mm)- 12- 575536 A7 _ B7 V. Description of the invention (ίο) Connected into one. (Please read the precautions on the back before filling out this page.) Similarly, you can also join plate-shaped parts on the surface and form a laminate (joint) 300 / as shown in Figure 8. In addition, as shown in Figure 8, when the surface is to be separated by a laminated part, it should be placed vertically to maintain the interval d, or a carbon or silicon carbide spacer is inserted between the surface to maintain the interval. d. These spacers can be left in the joints of the finished product (in the silicon carbide film) if there is virtually no problem, or they can be removed from the joints by sandblasting or cutting if necessary. In addition, in the present invention, a protruding portion (a convex portion, a male portion, a protruding portion) may be formed on one surface of one side of a part forming a joint body, and a fitting portion (a protruding portion) fitted into the protruding portion may be formed on the other side ( 'Recesses, females, and grooves) 俾 It is possible to bond high-purity ceramic parts more reliably. The combination system of the high-purity ceramic parts configured as described above is held in a C V D furnace by a carbon or silicon carbide ceramic holding fixture and the like, and the C V D-S 1 C film is formed in the same manner as in the contact arrangement method. The CVD furnace printed by the employee's consumer cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs for the implementation of the present invention is not particularly limited, but horizontal, vertical, bell bell, etc. are more commonly used, while the heating method is applicable to the direct current method, high frequency Induction heating or laser heating. The CVD-S 1 C film is basically formed by introducing raw material gas in a non-oxidizing atmosphere at 100 to 1600 ° C, preferably 1100 to 1500 ° C. The raw material gas can be used (1) a raw material gas system in which silicon and carbon are supplied by different compounds, for example, S 1 C 14 and CH4, si C 14 and this paper size are applicable to China National Standard (CNS) A4 (210 X 297) %) -13- Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs 575536 A7 __ B7 V. Description of Invention (11) c 3 Η 8 ^ Si C 1 4 and C6H! 4, S 1 C 1 4 and CC 1 4, S12H6, CH4, etc. may also be used. (2) or a source gas system in which stone and carbon are supplied from the same compound, for example, C Η 3 S i C 1 3, (CH3) 2SiC12, (CH a) 3 S i C 1, (CH3) 4S i and CH3S iHC 12 are also acceptable. These raw material gases are introduced into the furnace together with carrier gases such as hydrogen, helium, and M. There is no particular limitation on the pressure for forming a CVD-S i C film, but in order to fully introduce the raw material gas into the gap portion of the component assembly and substantially completely fill the gap portion with silicon carbide, it should be set to 1 to 3 0 0 Torr (Torr) is preferably a reduced pressure of about 10 to 100 Torr. As described above, under the above-mentioned C V D conditions, plate-shaped, sheet-shaped, film-shaped, and thin-plate-shaped silicon carbide can be formed in advance for parts to be bonded. That is, at this time, a substrate of graphite and carbon can be used as a substrate, and a silicon carbide film of a desired thickness can be formed thereon. The graphite of the substrate can then be carried out in the air at a temperature of about 1000 ° C. It is removed by thermal decomposition to obtain a thin plate-shaped silicon carbide (CVD — S 1 C). In addition, when the bonded body of the high-purity ceramic part prepared by the present invention is used as a fixture for a semiconductor manufacturing device, the high-purity ceramic part to be bonded is preferably one containing less impurities, especially the total content of metal impurities is less than 4 0 ppm, preferably less than 30 PP m, more preferably less than 20 ppm, and most preferably less than 10 PP m. Here, the term “metal impurities” refers to iron, copper, magnesium, vanadium, nickel, manganese, sodium, potassium, aluminum, etc. other than sand. In order to be mixed into a wafer, it is possible to reduce the insulation resistance and silicon oxide of semiconductor devices. (Si ◦ 2) The paper size is applicable to China National Standard (CNS) A4 (210 X 297 mm) K -------------- tr -------- -Line (Please read the precautions on the back before filling this page) -14-575536 Printed by A7 B7____, Employee Cooperative of Intellectual Property Bureau of the Ministry of Economic Affairs V. Description of the invention (12) Harmful elements caused by pressure caused by poor joint leakage . In addition, the purity of the c ν D-S i C coating layer formed on the surface of the high-purity ceramic part should be less than 50 PP b, preferably less than 30 ppb, and more preferably less than 10. ppb. [Examples] The present invention will be described in detail below with reference to examples. (1) Formation of high-purity ceramic parts assembly [Example 1] First, as shown in FIG. 1, two pieces of a / 3-type crystal structure with a 4 cm square and a thickness of 1 mm as shown in FIG. 2 were prepared. CVD — S i C wafers are used as bonded ceramic parts. In addition, the average surface roughness Ra of the C V D — Si C wafer is 0 · 2 // m, and the maximum surface roughness Rmax is 2 · 0 // m as the bonded ceramic parts. Use carbon clamps (not shown) to hold both ends of these parts, and then arrange the sides to make contact as shown in Figure 2. That is, two zero-new cows are brought into close contact to form a part assembly having a shape of 4 cm x 8 cm x 1 mm. [Embodiment 2] Two C V D-Si C wafers similar to those in Embodiment 1 were prepared as ceramic parts to be joined. As shown in Figure 4, the two surfaces are laminated in contact with each other. [Example 3] This paper size applies Chinese National Standard (CNS) A4 specification (210 X 297 mm) '· --------- installation -------- ^ ------ --- (Please read the precautions on the back before filling this page) -15- 575536 A7-B7 V. Description of the invention (13) Prepare two CVD-si C wafers the same as in Example 1. Next, the two wafer parts are arranged in a T shape using a carbon jig. [Embodiment 4] Two C V D-S 1 C wafers similar to those in Embodiment 1 were prepared. As shown in Fig. 6, the two wafers are arranged in a combination having a side surface interval d of 50 0 β m. [Example 5] Two wafers were arranged in the same manner as in Example 1 except that a silicon-impregnated silicon carbide wafer was used as a high-purity ceramic part. In addition, the average surface roughness R a of the silicon-impregnated silicon carbide wafer is 0.2 2 // m, and the maximum surface roughness Rmax is 2 · 2 // m〇 (2) CVD — the formation of a Si C fixed coating Next, the assembly of the high-purity ceramic parts configured in Examples 1 to 5 was set in a CVD furnace, and heated to 1000 ° C. in a vacuum to perform a drying (bak 1 ng) process. That is, in this state, hydrogen is introduced, and the pressure is adjusted to 100 Torr and maintained for 60 minutes. Next, ′ is heated at a heating rate of 15 ° C / minute and heated to a film forming temperature of 125 ° C. Then, C Η 3 S i C 1 3 was introduced as a material compound for forming a fixed coating of silicon carbide, and a 250 // Π1 CVD-S 1 C fixed coating was formed on the surface of the high-purity ceramic part. In addition, the surface of the paper before and after joining was measured for Examples 1 to 5. The paper size applies the Chinese National Standard (CNS) A4 (210 X 297 mm) (Please read the note on the back before filling this page) Luo Zhuang ---- Order ---------. Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economy -16- 575536 A7 _ B7 V. The concentration of metal impurities in the description of the invention (14). Examples 1 to 4 were 40 p P b before and after bonding. In addition, Example 5 was 18 p p m before joining and 45 ppb after joining. (Please read the precautions on the back before filling out this page.) Remove the joints formed with the CVD-S i C fixed coating by carbon jigs to obtain silicon carbide joints. Although tensile tests were performed on these joints with a precision tensile tester (Insuon), the tensile strength is very high, and the hardness of the joints is not inferior to other parts, and the joints are excellent in purity and acid resistance. body. [Comparative Example] In the same manner as in Example 1, two CV D-S i C wafers of 4 cm square and 1 mm thick were prepared. As the binder, a mixture of 65% by mass of the denatured phenol resin and 35% by mass of the flaky natural graphite powder was used, and the same was adhered as in Example 1. Then 'heated to 200 ° C in air to harden the adhesive, and then heated to 1000 t in a non-oxidizing atmosphere: carbonizing the resin in the adhesive. In this way, a silicon carbide junction was produced. The thickness of the pressure-sensitive adhesive layer was 200 β m. Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs (3) Bending strength and thermal shock resistance The joints prepared in Examples 1, 4 and Comparative Example 1 were used to evaluate the bending strength and thermal shock resistance. ① The flexural strength is determined in accordance with the method specified in JISR 16 01. The dimensions of the silicon carbide paper are subject to the Chinese National Standard (CNS) A4 (21〇χ 297 mm) -17- 575536 A7 B7 V. Description of the invention (15 ) Flexural strength of the composite at room temperature. ② Thermal shock resistance The thermal shock resistance was evaluated according to the thermal shock method. After heating the silicon carbide joint, it was put into water and quenched to give a temperature difference, and the hardness change of the silicon carbide joint was measured. Table 1 shows both the minimum temperature difference (heat-shock temperature Δ T) and the flexural strength of the minimum temperature difference where the hardness changes drastically. Table 1 Flexural strength (M P a) Thermal shock temperature Δ T (° c) Example 1 2 5 0 4 5 0 Example 4 2 9 0 4 5 0 Comparative example 1 1 503 0 0 [Industrial Usability] According to the joining method of the high-purity ceramic parts according to the present invention, it is possible to more easily produce a ceramic joint having a complex shape and a large shape, high hardness, excellent heat resistance, and acid resistance, and high purity compared with the previous joining method. body. In particular, when a high-purity ceramic part is a silicon carbide part composed of CVD-S1C or silicon-impregnated silicon carbide, for example, when a fixed coating is formed by c VD -S i C, the high-purity ceramic part and the The fixed coating layer will basically become a high-purity carbonized material of the same grade, and can be made with high hardness, excellent heat resistance and acid resistance, and high purity grades. This paper applies the Chinese National Standard (CNS) A4 Specifications (210 X 297 mm) C. Please read the notes on the back first and fill in this page)
經濟部智慧財產局員工消費合作社印製 -18- 575536 A7 B7 五、發明說明（16) 合體。 再者，本發明之接合方法可以適用於各種大小之高純 度陶瓷零件之接合，例如由數公釐之小零件至超過1公尺 之大零件之接合皆可適用。 依據本發明，可以接合各種形狀之高純度陶瓷零件’ 適用於製造晶片板等之複雜形狀之夾具時各零件間之接合 。如上所述，以本發明之方法製得之陶瓷接合體之耐熱性 與耐酸性優異，適宜於被做爲製造高硬度而高純度之半導 體之夾具之用。 另外，依據本發明之接合方法，先前之接合方法認爲 不可能之破損之高純度之碳化矽夾具等之修理也成爲可會g 。又本發明之方法也同樣地可以利用於半導體製造工程以 外之用途。 (請先閱讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） -19-Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs -18- 575536 A7 B7 V. Description of Invention (16) Combination. Furthermore, the joining method of the present invention can be applied to joining of high-purity ceramic parts of various sizes, such as joining from small parts of several millimeters to large parts exceeding 1 meter. According to the present invention, high-purity ceramic parts of various shapes can be joined. It is suitable for the joining of parts when manufacturing jigs with complex shapes such as wafer boards. As described above, the ceramic joint produced by the method of the present invention is excellent in heat resistance and acid resistance, and is suitable for use as a jig for manufacturing a semiconductor having high hardness and high purity. In addition, according to the bonding method of the present invention, repair of a high-purity silicon carbide jig or the like which was considered impossible by the previous bonding method is also possible. Also, the method of the present invention can be similarly used for applications other than semiconductor manufacturing processes. (Please read the precautions on the back before filling out this page) Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs This paper applies the Chinese National Standard (CNS) A4 specification (210 X 297 mm)