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TWI616401B - 微米粉體與其形成方法 - Google Patents

微米粉體與其形成方法 Download PDF

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TWI616401B
TWI616401B TW105137205A TW105137205A TWI616401B TW I616401 B TWI616401 B TW I616401B TW 105137205 A TW105137205 A TW 105137205A TW 105137205 A TW105137205 A TW 105137205A TW I616401 B TWI616401 B TW I616401B
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powder
niobium
micron
forming
minutes
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TW105137205A
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TW201819297A (zh
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蕭達慶
涂文坡
鄭楚丕
宋睦喜
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財團法人工業技術研究院
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Priority to US15/386,749 priority patent/US10059631B2/en
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Priority to US16/040,785 priority patent/US10214454B2/en

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Abstract

本揭露提供之微米粉體的形成方法，包括：(a)混合矽前驅物與碳前驅物以形成混合物後，於真空無氧條件下加熱混合物至1600℃至1800℃維持120至180分鐘，以形成碳化矽的粉體；以及(b)於無氧下加熱碳化矽的粉體至1900℃至2100℃維持5至15分鐘，再冷卻碳化矽的粉體至1800℃至2000℃維持5至15分鐘，以形成微米粉體，其中微米粉體包括碳化矽核心，以及碳膜包覆碳化矽核心。

Description

微米粉體與其形成方法
本揭露關於碳化矽粉體與其形成方法。
單晶碳化矽具有諸多優異的光，電，熱特性，比如高崩潰電壓、寬能隙、高電子飄移速度、高熱傳導係數等，因而在新世代電子基板的應用上相當看好。目前碳化矽之晶體成長技術主流為物理氣相傳輸法(Physical Vapor Transport，PVT)，乃使用高純度碳化矽粉體做為原料，於超過2000℃使粉體昇華後，藉由溫度場的設計，使昇華的氣體分子在低溫的晶種沈積下來使晶體成長。做為晶體成長的原材料，碳化矽粉體的品質對於所成長的晶體特性有直接的影響，純度一般為首要考量。因為粉體中的雜質元素在晶體成長過程中會隨之傳輸到晶體內部，進而引發缺陷產生並影響晶體電性。此外，粉體形貌也是影響晶體成長的要素之一，粉體粒徑為決定晶體成長的穩定性與速度之關鍵因子，目前碳化矽粉體的主要製作方法有二，其一為Acheson法，係將二氧化矽與石油焦在高達2500℃以上的溫度合成為碳化矽晶塊，再將此晶塊物理粉碎研磨成為碳化矽粉體。由於晶塊成長於大氣中，純度難掌控。晶塊研磨過程中，磨料造成的污染使粉體純度受限。其二為化學氣相沈 積法(Chemical Vapor Deposition，CVD)，此法使用高純度的矽前驅物與碳前驅物氣體(例如SiH4與C3H8)，在真空環境下將前驅物氣體分子分解並反應成碳化矽粉體。此法之原料氣體純度高，因此所製作出來的碳化矽粉體亦具有高純度。然而粉體顆粒過小，使晶體之成長過程操作不易。此外，以CVD法合成粉體之產率低，致使成本過高而不易大量商業化使用。
綜上所述，目前亟需新的方法形成碳化矽的微米粉體。
本揭露一實施例提供之微米粉體的形成方法，包括：(a)混合矽前驅物與碳前驅物以形成混合物後，於真空無氧條件下加熱混合物至1600℃至1800℃維持120至180分鐘，以形成碳化矽的粉體；以及(b)於無氧下加熱碳化矽的粉體至1900℃至2100℃維持5至15分鐘，再冷卻碳化矽的粉體至1800℃至2000℃維持5至15分鐘，以形成微米粉體，其中微米粉體包括碳化矽核心，以及碳膜包覆碳化矽核心。
本揭露一實施例提供之微米粉體，包括：碳化矽核心；以及碳膜包覆碳化矽核心，其中碳化矽核心之粒徑介於50微米至500微米之間，且碳膜厚度介於20nm至200nm之間。
第1A圖係本揭露一實施例中，往復式昇華前之碳化矽粉體的照片。
第1B圖係本揭露一實施例中，往復式昇華後之碳化矽粉體 的照片。
第2圖係本揭露一實施例中，往復式昇華前之碳化矽粉體的粒徑分佈圖。
第3圖係本揭露一實施例中，往復式昇華後之碳化矽粉體的粒徑分佈圖。
第4A圖係本揭露一實施例中，往復式昇華前之碳化矽粉體的SEM照片。
第4B圖係本揭露一實施例中，往復式昇華後之碳化矽粉體的SEM照片。
第5圖係本揭露一實施例中，往復式昇華後之碳化矽粉體的TEM照片。
第6圖係本揭露一實施粒中，往復式昇華後之碳化矽粉體表面之薄膜的EELS圖譜。
第7A圖係本揭露一實施例中，往復式昇華前之碳化矽粉體的照片。
第7B圖係本揭露一實施例中，往復式昇華後之碳化矽粉體的照片。
第8圖係本揭露一實施例中，往復式昇華前之碳化矽粉體的粒徑分佈圖。
第9圖係本揭露一實施例中，往復式昇華後之碳化矽粉體的粒徑分佈圖。
本揭露提供調控碳化矽粉體粒徑的技術，以達穩定且快速的晶體原料需求。習知PVD長晶之高純度碳化矽粉體 之顆粒較細時，具有較高的比表面積，即在長晶過程中具有較高的粉體昇華速度，因此容易提昇晶體成長速度。然而當粉體粒徑過小時，高表面能也往往造成粉體燒結現象，阻斷了昇華後氣體在粉體間的傳輸通道。此外，由於晶體成長乃在高真空下進行，當碳化矽粉體粒徑過小時，粉體容易隨著氣流揚起，增加了粉體操作的困難性，碳矽組成也發生變化。有鑑於此，部份習知晶體成長技術採用粒徑較大的粉體做為原料，以避免燒結問題且有利於真空下的操作。然而粉體粒徑過大則使得粉體昇華率降低，難以提升晶體成長速度。與習知技術相較，本揭露於真空環境下反應合成碳化矽粉體後，搭配往復式昇華處理碳化矽粉體。小顆粒碳化矽粉體具有較高的表面能，在高溫時因擴散而傾向於萎縮乃至消失。大顆粒碳化矽粉體因為具有較低表面能，在高溫時相對穩定，此時粉體因而得以成長，逐漸成長至粒徑數十乃至數百微米。本揭露實施例之方法可調控碳化矽粉體粒徑，進而提供合適的粒徑與分佈之碳化矽粉體。
本揭露一實施例之微米粉體的形成方法，包括：(a)混合矽前驅物與碳前驅物以形成混合物後，於真空無氧條件下加熱混合物至1600℃至1800℃維持120至180分鐘，以形成碳化矽的粉體。若上述加熱溫度過低及/或維持時間過短，則反應未完成，成品中將混有未反應物。若上述加熱溫度過高及/或維持時間過長，則除了能源損耗增加之外，也將降低坩堝與隔熱材料等使用壽命。在一實施例中，真空無氧條件的壓力為0.1Torr-50Torr之間。若上述壓力過低，則前驅物耗損增加。若上述壓力過高，則反應速度過慢，需更長時間。若步驟(a)之真空 無氧條件含有氧氣，則將干擾反應進行，致使成品中產生氧化物，並且使得坩堝與耐火材料等石墨製品壽命大幅降低。上述碳前驅物可為石墨、活性碳、瀝青、樹脂、烷類、烯類、其他合適的碳前驅物、或上述之組合。上述矽前驅物可為矽粉、氧化矽粉、矽酸乙酯、其他合適的矽前驅物、或上述之組合。在一實施例中，步驟(a)形成之碳化矽的粉體粒徑介於數百奈米至數十微米之間，平均粒徑約介於20微米至50微米。
接著(b)於無氧下加熱碳化矽的粉體至1900℃至2100℃維持5至15分鐘，再冷卻碳化矽的粉體至1800℃至2000℃維持5至15分鐘以形成微米粉體。若步驟(b)加熱碳化矽的粉體之溫度過低或維持的時間過短，則微米粉體粒徑過小。若步驟(b)加熱碳化矽的粉體之溫度過高或維持的時間過長，則能源損耗增加且降低坩堝與隔熱材料使用壽命。在一實施例中，加熱/冷卻碳化矽粉體之循環(即往復式昇華)的次數可重複多次，直到微米粉體達到所需尺寸。在一實施例中，上述步驟(b)重複多次的時間總計60至120分鐘之間。若步驟(b)重複的總計時間過短，則粉體粒徑過小。若步驟(b)重複的總計時間過長，則能源損耗增加且降低坩堝與隔熱材料使用壽命。在一實施例中，步驟(b)之無氧條件包含氬氣，且其壓力介於400Torr至760Torr之間。若無氧條件之壓力過低，則碳化矽粉體耗損將會增加。若無氧條件之壓力過高，則反應速度變慢，需要更長時間。若步驟(b)之無氧條件含有氧氣，則將干擾反應進行，致使成品中產生氧化物，並且使得坩堝與耐火材料等石墨製品壽命大幅降低。步驟(b)形成之微米粉體包括碳化矽核心，以及包覆 碳化矽核心之碳膜。上述碳化矽核心之粒徑介於50微米至500微米之間，且碳膜厚度介於20nm至200nm之間。此外，上述微米粉體具有光致發光特性，其激發波長為325nm，且其放射波長介於400nm至550nm之間。與步驟(a)之碳化矽粉體相較，步驟(b)之微米粉體表面額外包覆碳膜且其粒徑較大。
為了讓本揭露之上述和其他目的、特徵、和優點能更明顯易懂，下文特舉數實施例配合所附圖示，作詳細說明如下：
實施例
實施例1
取600g之氧化矽粉作為矽前驅物，以及240g之石墨粉作為碳前驅物，均勻混合後置於石墨坩堝中，抽真空至0.1Torr後在真空無氧的環境下加溫至1700℃後維持150分鐘，使氧化矽粉與石墨粉反應形成碳化矽粉體。此碳化矽粉體粒徑介於約數百奈米至數十微米，如第1A圖所示。將此碳化矽粉體置放於石墨坩堝中，在溫度低於1000℃時通入超高純度氩氣作為保護氣體，壓力約為660torr。在無氧的環境下，將溫度升高至1900℃進行退火處理10分鐘後，再降溫至1800℃處理10分鐘。上述升溫/降溫的循環(又稱往復式昇華)重複4次後，回溫至室溫以得微米粉體，其粒徑成長如第1B圖所示。往復式昇華前後之產物粒徑與粒徑分布(以HORIBA雷射粒徑分析儀量測)具有明顯差異，如第2圖(往復式昇華前)、第3圖(往復式昇華後)、與第1表所示。
第1表
以SEM觀察往復式昇華前後的粉體的表面形貌。往復式昇華前的粉體表面光滑如第4A圖，往復式昇華後則出現明顯紋路如第4B圖，兩者之表面形貌具有明顯差異。以TEM觀察往復式昇華後的粉體其微觀組織，往復式昇華後的粉體表面具有厚度約80nm的薄膜，如第5圖所示。如第6圖所示，上述薄膜經EELS分析，其組成以碳為主(不同於粉體之碳化矽核心)。
實施例2
取600g之氧化矽粉作為矽前驅物，以及240g之石墨粉作為碳前驅物，均勻混合後置於石墨坩堝中，抽真空至0.1Torr後在真空無氧的環境下加溫至1720℃後維持150分鐘，使氧化矽粉與石墨粉反應形成碳化矽粉體。此碳化矽粉體粒徑介於約數百奈米至數十微米，如第7A圖所示。將此碳化矽粉體置放於石墨坩堝中，在溫度低於1000℃時通入超高純度氩氣作為保護氣體，壓力約為660torr。在無氧的環境下，將溫度升高至1920℃進行退火處理10分鐘後，再降溫至1820℃處理10分鐘。上述升溫/降溫的循環(又稱往復式昇華)重複4次後，回溫至室溫以得碳化矽粉體，其粒徑成長如第7B圖所示。往復式昇華前後之產物粒徑與粒徑分布(以HORIBA雷射粒徑分析儀量測)具有明顯差異，如第8圖(往復式昇華前)、第9圖(往復式昇華後)、與第2表所示。
雖然本揭露已以數個實施例揭露如上，然其並非用以限定本揭露，任何本技術領域中具有通常知識者，在不脫離本揭露之精神和範圍內，當可作任意之更動與潤飾，因此本揭露之保護範圍當視後附之申請專利範圍所界定者為準。

Claims (8)

  1. 一種微米粉體的形成方法，包括：(a)混合矽前驅物與碳前驅物以形成一混合物後，於真空無氧條件下加熱該混合物至1600℃至1800℃維持120至180分鐘，以形成碳化矽的粉體；以及(b)於無氧下加熱碳化矽的粉體至1900℃至2100℃維持5至15分鐘，再冷卻碳化矽的粉體至1800℃至2000℃維持5至15分鐘以形成一微米粉體，其中該微米粉體包括一碳化矽核心，以及一碳膜包覆該碳化矽核心。
  2. 如申請專利範圍第1項所述之微米粉體的形成方法，其中步驟(b)重複多次。
  3. 如申請專利範圍第1項所述之微米粉體的形成方法，其中步驟(b)重複多次的總計時間為60至120分鐘。
  4. 如申請專利範圍第1項所述之微米粉體的形成方法，其中步驟(a)之真空無氧條件的壓力為0.1Torr-50Torr。
  5. 如申請專利範圍第1項所述之微米粉體的形成方法，其中步驟(b)之無氧條件包含氬氣氣氛，且其壓力為400Torr-760Torr。
  6. 如申請專利範圍第1項所述之微米粉體的形成方法，其中該碳前驅物包括石墨、活性碳、瀝青、樹脂、烷類、烯類、或上述之組合。
  7. 如申請專利範圍第1項所述之微米粉體的形成方法，其中該矽前驅物包括矽粉、氧化矽粉、矽酸乙酯、或上述之組合。
  8. 一種微米粉體，包括：一碳化矽核心；以及一碳膜包覆該碳化矽核心，其中該碳化矽核心之粒徑為50微米-500微米，且該碳膜厚度為20nm-200nm，其中該微米粉體的放射波長介於400nm至550nm之間。
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