TW201500309A - 於高溫下用於碳化矽部件的密封方法 - Google Patents

於高溫下用於碳化矽部件的密封方法 Download PDF

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TW201500309A
TW201500309A TW103115398A TW103115398A TW201500309A TW 201500309 A TW201500309 A TW 201500309A TW 103115398 A TW103115398 A TW 103115398A TW 103115398 A TW103115398 A TW 103115398A TW 201500309 A TW201500309 A TW 201500309A
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gasket
weight
mullite
sio
niobium carbide
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Nicolas Leblond
Mehrdad Mahmoudi
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Corning Inc
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Abstract

本發明描述於高溫下可用的碳化矽物件和製作該物件的方法。方法包含提供複數個碳化矽部件；提供莫來石墊片；將墊片放在待接合部件的末端之間，從而形成組件；施加15-25磅/平方吋的負載至遠離墊片的部件末端，藉以壓合墊片；在蒙孚爐中，施以1450℃至1550℃的溫度來加熱組件；將負載提高到至少30-50磅/平方吋，及使組件保持在此溫度下2-5天的時間，以黏接莫來石墊片與碳化矽部件的末端。

Description

於高溫下用於碳化矽部件的密封方法 【交互參照之相關申請案】
本申請案主張西元2013年4月30日申請的美國專利申請案第61/817,574號的優先權權益，本申請案依賴該申請案全文內容且該申請案全文內容以引用方式併入本文中。
本發明係針對利用於高達至少1500℃的高溫下可用的機械強韌且真空密閉密封，以將碳化矽(SiC)部件接合在一起的方法。特別地，方法可用於製作長碳化矽管狀元件，該元件可用作在減壓下加固光纖預形體的真空容器。
專利申請案US2010/0055498已描述各種用於接合SiC部件的方法的現有技術狀況。通常，該等方法需在SiC部件間施加接合化合物，又因化合物會與空氣中的氧反應，以致需在還原大氣(例如氮、氬、真空)中燃燒。US2010/0055498所述方法由以下步驟組成：製備玻料(組成為SiO2/Al2O3/CaO或Al2O3/CaO/MgO)、混合玻料與有機黏結劑、將玻料/黏結劑塗鋪於待接合的SiC部件，及在空氣中、以1100℃至1650 ℃燃燒。視玻料組成而定，所得接合據稱在高達1200℃的溫度下為密閉。
上述玻料密封方法的最高操作溫度(1200℃)對一些應用係限制因素，例如光纖預形體加固，此需要高於1450℃的溫度，計數小時。就此應用而言，用於光纖預形體的SiC容器尺寸為直徑12至18吋、長度12至18呎。目前的製造製程無法製作如此大的SiC部件，因此必須組裝多個管段。故期使用能形成直徑為12至18吋、從SiC管短邊算起長度為12至18呎的SiC容器的接合材料。接合材料應可用於至少高達1500℃的溫度，並提供密閉密封。
本發明描述碳化矽元件和用於製作該元件的方法與材料。方法和以該方法製作的元件可用於許多高溫製造製程，以製作許多不同的物件。在一態樣中，本發明係針對接合及密封至少二成型碳化矽部件的方法，特別係利用莫來石材料來接合及密封碳化矽部件，使SiC部件結合在一起而形成SiC容器。方法包含提供複數個碳化矽部件；將莫來石墊片放在待接合部件的末端之間，從而形成組件；及加熱組件，使碳化矽部件彼此黏附。在一實施例中，方法進一步包含在加熱步驟期間，施加15-25磅/平方吋的負載至遠離墊片的部件末端，藉以壓合墊片。在一實施例中，方法亦包含在蒙孚爐中，施以1400℃至1600℃的溫度來加熱組件。在一實施例中，依每分鐘3℃至8℃的加熱速率使溫度達1400℃至1600℃的範圍。在一實施例中，方法包含將組件上的負載提高到 30-60磅/平方吋，及使組件保持在該溫度下2-5天的時間，以黏接莫來石墊片與碳化矽部件的末端。在一實施例中，組件在50-60磅/平方吋的負載下，經加熱達1500℃±20℃，計2天。在一實施例中，加熱係在空氣中完成。
本發明更針對接合及密封碳化矽管的方法，方法包含提供複數個碳化矽管，碳化矽管具有長度、內徑與外徑和第一末端與第二末端，內徑與外徑間的差異定義管壁厚度；莫來石墊片，墊片尺寸適配待接合末端的壁厚。墊片放在待接合管末端與所得管組件之間，且墊片黏貼在各墊片/管接合處，使墊片保持在適當位置。15-25磅/平方吋的負載施加至遠離墊片的管末端，以將墊片壓合在一起。在空氣中，施以1400℃至1600℃的溫度來加熱組件，使碳化矽管彼此黏附。在一實施例中，依每分鐘3℃至8℃的加熱速率達到溫度範圍。在一實施例中，在加熱步驟期間，將負載提高到30-60磅/平方吋，及使組件保持在該溫度下2-5天的時間，以黏接莫來石墊片與碳化矽管的末端。在一實施例中，組件經加熱達1500℃±20℃。在一實施例中，使組件保持在1500℃±20℃，計3-4天。在另一實施例中，複數個管的外徑大於4吋，各管長度超過2呎。在一實施例中，管係在蒙孚爐中的垂直位置加熱，且管重量提供至少部分負載。當接合及密封管抽空成0.05大氣壓力時，進行測漏，洩漏率小於4sccm。
接合材料和所得接合的優點為：
1.材料不會與SiC反應，並含有最少量的鹼與鹼土材料，在高於1200℃的溫度下，鹼與鹼土材料可能造成氣泡及腐蝕SiC 材料。
2.與氧化大氣相容，例如空氣，故可簡化應用而不需昂貴的大氣控制爐。
3.與SiC部件有良好的黏附性，從而形成機械強韌結合，此媲美與大塊SiC材料的強度。
4.熱膨脹係數(CTE)相容於SiC的CTE(4.3ppm/℃)，因而容許所得組件在如最高溫度與室溫之間熱循環(冷卻及加熱)，又不會破裂。
5.接合材料在高達至少1500℃的操作溫度下具化學及物理穩定性，故可維持接合及密封的完整性。
6.接合材料可構成密閉密封，即防止氣體從接合一側遷移到另一側。本發明描述的碳化矽部件接合方法符合上述所有要求。方法尤其可應用到各種形狀的大型部件，例如管、板、凹凸部件、管向板(tubes to plates)、嚙合鋸齒部件和具其他形狀且能利用所述方法接合及密封的部件。本發明優於先前技術的附加優點在於使用固體墊片材料，以防止接合材料被擠出接合處，此乃黏糊型接合材料可能發生的情況。此外，本文所述莫來石墊片方法不配合使用有機黏結劑。該等有機黏結劑通常為黏糊型接合材料所需，且在燃燒後會於接合處形成氣泡，進而導致結構失效及/或洩漏。
10‧‧‧設備
11‧‧‧間隙
12‧‧‧SiC管(道)
14‧‧‧SiO管
16‧‧‧爐壁
18‧‧‧密封件/墊片
20‧‧‧玻璃棒
22‧‧‧毛坏
30‧‧‧鋁蓋
32‧‧‧墊片
40‧‧‧埠口
50‧‧‧支架
第1圖係設備10的基礎特徵結構示意圖，設備可用於脫水、除氣及將光纖煙灰毛坏加固成光纖玻璃預形體的一 或更多步驟；設備10包括長SiC管，SiC管係利用本文所述莫來石密封件18，由複數個小型管12製成。
第2圖係莫來石密封件18的圖片，在加熱達1500℃數天後，即自SiC管移除之；圖片顯示莫來石已融入SiC管，從而說明莫來石密封件與SiC部件間為強韌機械密封。
第3A圖至第3C圖圖示可使用所述莫來石墊片的示例性接合形狀。
以下詳細說明提及許多特定細節，以對本發明的實施例有更徹底的瞭解。然熟諳此技術者將明白，本發明實施例可不按照部分或所有特定細節實行。在其他情況下，並未詳述已知特徵結構或製程，以免讓本發明變得晦澀難懂。此外，類似或相同的元件符號用來表示共同或相仿的元件。在此，SiC管將做為以下所述的示例性接合部件。如所述，接合的管末端可具有不同的形狀。若「n」個管道代表待接合的管道數量，則形成接合管道組件需要「n-1」個墊片。故如第1圖所示，為將4個管道12結合在一起，需要3個莫來石密封件(墊片)18。
本發明描述碳化矽物件和用於製作該物件的方法與材料。方法和以該方法製作的物件可用於許多高溫製造製程，以製作許多不同的物件。
本發明係針對接合及密封碳化矽管的方法，碳化矽管用作不同目的，包括在高於1400℃的高溫與減壓下，將光纖煙灰毛坏加固成光纖玻璃預形體，但不以此為限。預形體 加固可在高溫蒙孚爐中進行。實施上述方法的主要挑戰在於判別材料夠強韌而能在預形體加固溫度下承受真空條件，預形體加固溫度通常高於1450℃。
目前，SiC係唯一具成本效益的材料，SiC夠強韌而能在1450℃下維持真空，又不會變形。然目前並無法取得具有如12-16吋大的外徑和如12-16呎長的長度的碳化矽管，因此必須接合數個短管，以獲得預定的全尺寸管。目前，可製造的最長SiC圓柱管為4呎長，故需堆疊至少3或4個管段，以製作全長12-16呎的管。接下來問題是要找到方法將該等管段密閉地密封在一起，以於加固製程期間達到適當真空度。
相較於其他方法，利用莫來石墊片密封方法的優點為：
1.密封製程不需惰性大氣，且可在空氣中、於約1500℃下完成。
2.莫來石墊片/碳化矽組件在冷卻至室溫及重新加熱至製程溫度後可維持氣密性，此非一些玻璃基礎密封方法的情況。
3.不像一些溫度需為1600℃-2000℃的焊接方法，莫來石墊片密封方法不需要高於加固爐可達到的溫度(1500℃或略高)。
4.莫來石材料很少且非常局部地與碳化矽反應。密封化合物與碳化矽反應會造成孔蝕、蝕刻及最終導致密封失效。
5.玻璃基礎密封需舌榫接合，使液態玻璃保持在接合區內。較佳的莫來石墊片材料係高矽石莫來石材料。做為墊片材料以接合SiC管道的莫來石材料包含結合至少95重量%的Al2O3 加SiO2與5重量%或以下的改質劑和雜質。墊片材料中的改質劑包括鹼與鹼土金屬氧化物和選定過渡金屬氧化物，例如鈉、鉀、鈣、鎂、鋇、鈦、鐵、鈦和鋯的氧化物。在一實施例中，莫來石材料包含結合至少97重量%的Al2O3加SiO2與3重量%或以下的改質劑和雜質。
第1圖係加固設備的示意圖，其中四個SiC管12利用莫來石墊片材料18接合在一起。第1圖的其他元件為內部SiC管14；蒙孚爐壁16，用以加熱爐內的設備元件；光纖煙灰毛坏22：煙灰沉積在玻璃棒20上，且在加固煙灰及抽拉後將形成光纖核心；水冷卻鋁蓋30和Grafoil墊片32；至少一對埠口40，用以注入選定氣體與煙灰形成蒸汽；及位於組合SiC組件上的支架50，蒙孚爐圍繞支架，支撐件(未圖示)使爐保持在適當位置。未編號的彎曲箭頭表示在脫水、除氣及加固期間，光纖煙灰預形體的旋轉方向。
本發明亦描述接合複數個碳化矽管段的方法，以形成供高溫操作的氣密密封。接合可由完全緻密的莫來石墊片製成，墊片置於二SiC管段之間。接著在空氣中、在輕微負載下(若管段很大，則管段重量可提供足夠負載)，加熱組件達約1500℃，計3-4天。在此溫度下，莫來石慢慢蠕變及順應SiC面。莫來石的組成(鋁矽酸鹽)提供與碳化矽的絕佳黏附性和足夠的熱膨脹性(CTE)，以於廣泛溫度循環過程保持完整。
在本發明的一實例中，兩個碳化矽部件或管用於製作具對接(平面)接合的長管。所用部件的外徑(「o.d.」) 為2吋(50.8毫米(mm))，長度為24吋(635mm)，壁厚為0.19吋(4.8mm)，且末端為封閉。各管從封閉端切割4吋，及使用125微米鑽石研磨盤來研磨切割面，以提供平面。由CoorsTek(Fremont，美國加州)、o.d.2吋(50.8mm)的莫來石管切割7mm薄片，以製作莫來石墊片，並使用60粒度SiC紙來消除粗糙點而拋光成6mm厚。墊片放在管段面之間，且利用膠帶固定位置。將組件裝載至管爐內，施以15-25磅的負載至組件上，使墊片於加熱期間保持在適當位置。依5℃/分鐘的速率使爐溫上升達1500℃(空氣大氣)，此時，將負載提高至50磅。在空氣中、於1500℃下經過10天後，進行測漏，然後依5℃/分鐘在1250℃與1500℃之間進行溫度循環，一天12次，以提供加固製程的加速模式。經過166次循環後，依5℃/分鐘的速率使爐冷卻至20℃，及依5℃/分鐘的速率重新加熱達1500℃。額外測漏3天。
接著使用直徑5.3吋、長12呎的SiC管及如上述般組裝，以大規模測試莫來石墊片密封方法。在此例中，莫來石墊片置於搭接接合內、而非對接接合，以限制墊片的蠕變量。進行測漏數天，並且包括上述溫度循環。
抽空組裝管，組裝管末端係由至少一帽蓋密封，帽蓋具有閥和Grafoil墊片、利用真空泵，將管抽空成0.05大氣壓力、關閉閥以隔離管與泵，及監控隨時間變化的管內壓力，以進行測漏。洩漏率為小於4×10-2sccm(標準立方公分每分鐘)。在一實施例中，洩漏率為小於3×10-2。取得10分鐘內壓力斜率對時間的變化，以計算洩漏率。接著將此值乘上管 體積，而得單位為atm．cm3/秒的洩漏率。接著乘上60秒/分鐘×300K/1773K，以將此值轉換成sccm。就10分鐘測漏而言，測量裝置能偵測的最小洩漏率為1.35×10-3atm．cm3/秒(1.37×10-2sccm)。利用本文所述莫來石墊片製作的密封件，就10分鐘測漏所測得的洩漏率為2.70×10-3atm．cm3/秒(2.74×10-2sccm)，此係測量裝置的最小偵測位準的兩倍，此係很好的結果，並且顯示所述密封件的實用性。為更好了解此代表意義，在隔離管與真空泵後的10分鐘內，抽空管內的測量壓力僅增加0.002大氣。使用2吋o.d.或5.3吋o.d.的SiC管的洩漏率實質相同。
如上所述，有數種方法用於接合碳化矽部件。可產生最氣密密封(例如直接燒結)的方法需在真空或惰性大氣中進行燃燒步驟，此對大型部件而言十分具挑戰性，例如加固蒙孚管，此如所述大型SiC管。玻璃基礎密封方法可在空氣中使用，但產生密封所需溫度必須比玻璃操作溫度高數百度；即，玻璃必須夠有流動性來接合管，但又必須很黏以提供穩定密封。此外，如利用SiC粉末/黏附方法的玻璃密封需要大型高溫爐。雷射焊接玻璃基礎玻料大有可為，但尚未有用於大型部件的設備/協定。使用莫來石的優點在於，材料不與碳化矽反應；材料會在目前可用加固爐的最高溫度左右蠕變；材料不透氣；且材料的CTE接近碳化矽並可與碳化矽牢牢接合。
做為墊片材料以接合SiC管道的莫來石材料包含至少95重量%的Al2O3加SiO2與5重量%或以下的改質劑和雜 質。在一實施例中，莫來石材料包含至少97重量%的Al2O3加SiO2與3重量%或以下的改質劑和雜質。在一實施例中，墊片中的Al2O3/SiO2莫耳比為0.5：1至2：1。在一實施例中，墊片中的Al2O3/SiO2莫耳比為0.8：1至1.8：1。在進一步實施例中，墊片中的Al2O3/SiO2莫耳比為1.1：1至1.8：1。莫來石墊片材料中的雜質包括鹼與鹼土金屬氧化物和選定過渡金屬氧化物，例如鈉、鉀、鈣、鎂、鋇、鈦、鐵、鈦和鋯的氧化物。在一實施例中，在氧化物方面：墊片中的鈉加鉀含量少於2重量%；鐵加鈦加鋯含量少於1.8重量%；及鈣加鎂加鋇含量少於1.2重量%。在另一實施例中，在氧化物方面：墊片中的鈉加鉀含量少於1重量%；鐵加鈦加鋯含量少於1.2重量%；及鈣加鎂加鋇含量少於0.8重量%。
利用莫來石材料將複數個部件接合在一起而形成物件，可用上述莫來石材料來製作碳化矽物件。例如，可製作管狀碳化矽物件，碳化矽物件包含複數個碳化矽管狀部件，碳化矽管狀部件具有相對端面和內徑與外徑，且莫來石墊片接合其中一個部件的至少一端面與另一部件的端面，從而形成包含複數個部件的碳化矽管狀物件，物件具有相對端面。碳化矽物件在0.5大氣範圍的減壓下具有小於4×10-2sccm的洩漏率。莫來石墊片包含至少95重量%的Al2O3加SiO2與5重量%或以下的改質劑和雜質；墊片中的Al2O3/SiO2莫耳比為0.5：1至2：1。
替代實施例包括修改目前可用的莫來石組成物，使莫來石組成物的CTE更匹配碳化矽的CTE。此外，用與碳化 矽更相容的氧化物取代存於目前可用莫來石材料中的任何鹼金屬可提供壽命較長的接合組件。在本發明中，接合面係平面，但在替代實施例中，可塑形面，以免在完成初始密封後，莫來石蠕變太多。第3A圖至第3C圖圖示可使用莫來石墊片材料的示例性接合面；圖中，斜線區12係SiC部件，圓點區18係莫來石。第3A圖圖示對接(平面)接合，第3B圖圖示搭接接合，第3C圖圖示舌榫接合。在第3B圖及第3C圖中，區域11係間隙，以供墊片在負載下變形及產生密封。
10‧‧‧設備
11‧‧‧間隙
12‧‧‧SiC管(道)
14‧‧‧SiO管
16‧‧‧爐壁
18‧‧‧密封件/墊片
20‧‧‧玻璃棒
22‧‧‧毛坏
30‧‧‧鋁蓋
32‧‧‧墊片
40‧‧‧埠口
50‧‧‧支架

Claims (16)

  1. 一種接合及密封二或更多成型碳化矽部件的方法，該方法包含下列步驟：將一莫來石墊片放在至少二待接合部件的末端之間，從而形成一組件；及加熱該組件，使該至少二碳化矽部件彼此黏附。
  2. 如請求項1所述之方法，其中該莫來石墊片包含結合至少95重量%的Al2O3加SiO2含量與5重量%或以下的一改質劑和一雜質，且該墊片中的一Al2O3/SiO2莫耳比為0.5：1至2：1。
  3. 如請求項1所述之方法，其中該加熱步驟包含施加15-25磅/平方吋的一負載至遠離該墊片的該等部件末端，以將該墊片壓合在一起。
  4. 如請求項1所述之方法，其中該加熱步驟包含在一蒙孚爐中，施以1450℃至1600℃的一溫度來加熱該組件。
  5. 如請求項1所述之方法，其中該方法包含在該加熱步驟期間，將該等部件末端上的一負載提高到至少30-60磅/平方吋，及使該組件保持在該溫度下2-5天的時間。
  6. 如請求項1所述之方法，其中該莫來石墊片包含結合至 少97重量%的Al2O3加SiO2含量與3重量%或以下的一改質劑和一雜質，且該墊片中的一Al2O3/SiO2莫耳比為0.5：1至2：1。
  7. 如請求項2所述之方法，其中該改質劑選自由鈉、鉀、鈣、鎂、鋇、鈦、鐵、鈦和鋯的氧化物所組成的一群組。
  8. 如請求項1所述之方法，其中該等部件係多個碳化矽管，各碳化矽管具有一長度、一內徑和一外徑，該內徑與該外徑間的差異定義一管壁厚度。
  9. 一種管狀碳化矽物件，包含：複數個碳化矽管狀部件，各碳化矽管狀部件具有多個相對端面和一內徑與一外徑，且一莫來石墊片接合該等部件的其中一者的至少一端面與該等部件的另一者的一端面，從而形成包含複數個部件的一碳化矽管狀物件，該物件具有多個相對端面；其中該莫來石墊片包含結合至少95重量%的Al2O3加SiO2含量與5重量%或以下的一改質劑和一雜質，且該墊片中的一Al2O3/SiO2莫耳比為0.5：1至2：1。
  10. 如請求項9所述之管狀碳化矽物件，其中該莫來石墊片包含結合至少97重量%的Al2O3加SiO2含量與3重量%或以下的一改質劑和一雜質。
  11. 如請求項9所述之管狀碳化矽物件，其中該改質劑選自由鈉、鉀、鈣、鎂、鋇、鈦、鐵和鋯的氧化物所組成的一群組。
  12. 如請求項9所述之管狀碳化矽物件，其中在氧化物方面：該墊片中的鈉加鉀含量少於2重量%；鐵加鈦加鋯含量少於1.8重量%；及鈣加鎂加鋇含量少於1.2重量%。
  13. 如請求項9所述之管狀碳化矽物件，其中該莫來石墊片包含結合至少95重量%的Al2O3加SiO2含量與5重量%或以下的一改質劑和一雜質，且該墊片中的一Al2O3/SiO2莫耳比為0.8：1至1.8：1。
  14. 如請求項9所述之管狀碳化矽物件，其中該莫來石墊片包含結合至少95重量%的Al2O3加SiO2含量與5重量%或以下的一改質劑和一雜質，且該墊片中的一Al2O3/SiO2莫耳比為1.1：1至1.8：1。
  15. 如請求項9所述之管狀碳化矽物件，其中該物件在0.5大氣的一減壓下具有小於4×10-2的一洩漏率。
  16. 如請求項9所述之管狀碳化矽物件，其中該等面接合選自由一對接接合、一搭接接合和一舌榫接合所組成的一群組。
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