TWI411467B - 金屬孔洞材料、其製備方法及含氮化合物之檢測方法 - Google Patents

金屬孔洞材料、其製備方法及含氮化合物之檢測方法 Download PDF

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TWI411467B
TWI411467B TW099132543A TW99132543A TWI411467B TW I411467 B TWI411467 B TW I411467B TW 099132543 A TW099132543 A TW 099132543A TW 99132543 A TW99132543 A TW 99132543A TW I411467 B TWI411467 B TW I411467B
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metal
preparing
hole material
nitrogen
metal hole
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Chun Nan Kuo
Shou Nan Li
Shaw Yi Yen
Yu Lun Lai
Jung Nan Hsu
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Ind Tech Res Inst
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Description

金屬孔洞材料、其製備方法及含氮化合物之檢測方法
本發明係有關於金屬孔洞材料，且特別是有關於一種金屬孔洞材料，其可用於當作氣體偵測器之感測元件。
隨著科技不斷的進步，許多新型的關鍵技術成為高科技業的發展重點，其中高科技廠房微污染監控技術已被列為未來產業競爭的關鍵技術之一。
國際半導體技術藍圖委員會(International Technology Roadmap for Semiconductors；ITRS)預估至2013年晶片關鍵尺寸(critical dimension；CD)將縮小至32奈米(nm)，微污染控制為其關鍵技術之一。以32nm的半導體製程為例，在無塵室中之製程關鍵區域，微污染敏感區對於酸、鹼、有機類、摻質(dopants)類的空氣品質建議值皆分別建議維持在10～150 ppt以下的範圍內。因此，欲確認無塵室內空氣品質是否符合半導體製程上的要求，需要的是極低濃度的氣體監測器。
對氨氣濃度進行十億分之一(ppb)等級的監測與控制，在晶圓廠是一項非重要的課題。在微影技術(lithography)製程中，製程環境的氨氣濃度只要達到百億分之一(sub-ppb)等級就會改變光阻的光化學性質，而造成光阻產生T型頂(t-topping)現象，如附件1所示。此外，氨氣為一種具光反應特性的氣體，會在黃光區的鏡片(lens)表面與硫化物(例如SO2 )反應生成(NH4 )2 SO2 而霧化鏡面造成機台的損害甚至導致設備停工。
氨氣在半導體廠的污染生成來源有CVD、晶片清潔(wafer cleaning)、光阻塗佈、CMP、乃至於作業人員呼出的氣體均含有氨氣。雖然在無塵室中與機台內部中均有空氣迴風系統配備各種不同的過濾裝置用以確保空氣的潔淨度，然而若沒有相當靈敏度的氣體感測系統與之配合，以及時提供作業與製程環境中的微污染氣體濃度變化，則無法得知機台內部的空氣是否符合作業需求以達到良率的提昇。以往在工安的考量下，為了維護作業人員的健康與環境安全所發展出的氨氣感測器零敏度往往只有介於百萬分之一(ppm)等級與千萬分之一(sub-ppm)等級之間。
對半導體廠而言，偵測極限僅至百萬分之一(ppm)等級的氨氣感測器並無法滿足對製程監測的要求，因此為了達到可以測量氨氣濃度為十億分之一(ppb)等級的要求，目前在半導體廠對低濃度氨氣偵測的方式採用了包括離子機動性測譜(Ion Mobility Spectroscopy、IMS)、化學螢光法(Chemiluminescence)、腔體振盪吸收光譜法(Cavity Ring-Down Spectroscopy、CRDS)以及傳統採樣分析的離子層析法(Impinger+ion chromatography、IC)。然而，這些分析方法不是需要高單價的儀器設備，就是會有冗長的分析時間，進而導致高科技廠常面臨良率損失之威脅。
因此，業界需要的是一種量測氨氣的新穎材料及技術。
本發明提供一種金屬孔洞材料的製備方法，包括：混合一矽氧烷、一金屬或金屬化合物、及水，攪拌後得到一混合物；調控該混合物使其具有一pH值，其中該pH值小於7；在調整完pH值後，對該混合物進行一第一乾燥處理，得到一固體；以及，對該固體進行研磨，進行一第二乾燥處理後得到該金屬孔洞材料。值得注意的是，該製備金屬孔洞材料的方法無使用任何鍛燒製程。本發明提供一種金屬孔洞材料，係由上述方法所製備而得。
本發明所述之金屬孔洞材料，包含以下原子所組成：金屬原子，該金屬原子合包鐵、銅、釩、錳、鉻、鈷、或其組合，其中該金屬原子之原子數比率佔該金屬孔洞材料之1~10%；矽原子，該矽原子之原子數比率佔該金屬孔洞材料之20~40%；氧原子，該氧原子之原子數比率佔該金屬孔洞材料之50~70%，其中該金屬多孔材料在製程中經任何鍛燒製程，並具有一分解溫度介於150~250℃。
本發明亦提供一種含氮化合物之檢測方法，包含：提供如上述之金屬孔洞材料導入一待測氣體與該屬孔洞材料反應；以及，分析反應結果。
為讓本發明之上述和其他目的、特徵、和優點能更明顯易懂，下文特舉出較佳實施例，並配合所附圖式，作詳細說明如下：
本發明提供一種金屬孔洞材料，其對含氮化合物具呈色感測特性。該金屬孔洞材料，由於其製備方式，可使金屬或金屬化合物能夠穩定的存在於矽孔洞材料之中，提供足夠的空間增加其與目標氣體(例如：NH3 )結合之機會，進而提高偵測極限。該金屬孔洞材料對含氮化合物具呈色感測特性的原理在於金屬化合物與含氮化合物結合會產生特定之顏色變化。本發明亦提供一種含氮化合物之檢測方法，可利用紫外光-可見光光譜將金屬孔洞材料之光吸收強度予以量化，進而建立含氮化合物濃度與光吸收強度變化之線性關係，最終達到測量含氮化合物濃度之目的。
本發明之金屬孔洞材料，在一實施例中，係由以下步驟所製備，請參照第1圖所示之金屬孔洞材料製備流程圖：首先，將矽氧烷、金屬或金屬化合物與水混合(步驟11)，攪拌後得到一混合物(步驟12)。接著，調控該混合物使其pH值小於7(步驟13)。在調整完pH值後，靜置該混合物一段時間(例如：24小時)，並對該混合物進行一第一乾燥處理(例如：在室溫下進行)，得到一固體(步驟14)。接著，對該固體進行研磨(步驟15)後，進行一第二乾燥處理(例如：在60℃下進行)得到該金屬孔洞材料，其中，本發明所述之乾燥處理(包含第一及第二乾燥處理)係指放置於室溫或是不高於60℃的溫度下(相對溼度較佳係小於RH=50%)，進行自然乾燥，且該製備金屬孔洞材料的方法無使用任何鍛燒製程。(該金屬孔洞材料的整體製程溫度不會高於60℃)。
本發明所述之金屬孔洞材料，其組成比例(Atomic%)為：金屬原子(源於所使用之金屬或金屬化合物(例如：鐵、銅、釩、錳、鉻等金屬)佔1~10%；矽原子(源於矽氧烷)佔20~40%；氧原子佔50~70%。值得注意的是，本發明所述之金屬多孔材料由於未加以鍛燒，所以其物性的分解溫度係介於150~250℃，不同於一般經煅燒的金屬氧化材料(分解溫度>300℃)。
在此，上述矽氧烷之化學結構係為Si(OR4 )，R係為含1-8個碳原子的烷基，可例如為四異丙烷氧化鈦(titanium (IV)isopropoxide;TTIP)、四甲基矽氧烷(TMOS)、四乙基矽氧烷(TEOS)或前述之組合。該金屬係為含鐵、銅、釩、錳、鉻、鈷、或其組合，此外，該金屬化合物係為含鐵、銅、釩、錳、鉻、或鈷之鹵化物、硫化物、硝酸鹽、氮酸鹽、硫酸鹽、或其組合，例如為硝酸鐵、硝酸鈷、硝酸鉻、或具有結晶水之前述化合物。該金屬孔洞材料所含之矽與金屬的重量比係介於0.95:0.05至0.05:0.95之間。金屬比例大於0.95以上，易形成較大的顆粒，降低活性位置表面積，導致反應活性下降。金屬比例低於0.05，則可能因活化位置不足而降低反應速率。
在調整pH值的過程中，可以酸性溶液來調整上述溶液之pH值。在一實施例中，該酸性物質可為鹽酸、硫酸、氮酸、硝酸或前述之組合。例如，加入的金屬或金屬化合物包含鈷時，較佳為使用鹽酸來調整該溶液之pH值。在一些實施例中，上述溶液之pH值可為在7.0~1.0之間，較佳係介於5.0~2.0之間，以增進金屬與鹼性分子ammonia結合之友善環境。
根據本發明另一實施例，本發明亦提供一種利用上述金屬孔洞材料對含氮化合物之檢測方法，包含：提供本發明所述之金屬孔洞材料，並導入一待測氣體與該金屬孔洞材料反應。最後，分析反應結果。可檢測的含氮化合物例如氨氣(NH3 )。相對於傳統偵測氨氣的方法，本發明所述之金屬孔洞材料對於氨氣具有高度靈敏性。因此，其更可作為含氮分子的偵測器之感測元件，該感測元件的偵測下限可達100ppt。
在一實施例中，該感測元件更可與紫外光-可見光光譜(ultraviolet-visible spectroscopy)系統連結作為含氮分子之氣體偵測器。測試方法可包含：將待測之氣體及載送氣體(carrier flow)分別經由不同的質量流量控制器後，混合並由閥門控制是否送進具有金屬孔洞材料的測試腔體中。送進測試腔體中的氣流，需確保其貫穿金屬孔洞材料粉體後再排出。由於該金屬孔洞材料在吸收含氮化合物後會改變其自身顏色，因此搭配紫外光-可見光光譜系統後，可即時量測該金屬孔洞材料在一特定波長範圍的光吸收強度。值得注意的是，由於紫外-可見光光譜系統所測得之在特定波長範圍的該吸收強度係與該金屬孔洞材料所吸附的含氮化合物濃度成正比，因此可介由金屬孔洞材料其光吸收強度的變化，得到待測氣體其含氮化合物的濃度。
以下藉由下列實施例來說明本發明所述之金屬孔洞材料之合成方式及其性質量測，用以進一步闡明本發明之技術特徵。
【實施例1】
首先，取Co(NO3 )2 ‧6 H2 O(0.4g)、及TEOS(8ml)混合於4ml水(H2 O)中，並充分攪拌。接著，將2MHCl(2ml)加入上述混合物中並充分攪拌，使所得溶液之pH值小於7。接著將上述溶液於室溫下靜置24小時乾燥後，將所得之固體進行研磨。最後，將研磨所得之粉未置於60℃下乾燥6小時，得到具有鈷金屬之矽孔洞材料1。
以EDX(能量分散光譜儀、energy disperse X-ray)對該奈米結構材料進行表面元素分析，得到鈷及矽的重量比為12:88。
【實施例2】
首先，取Co(NO3 )2 ‧6 H2 O(0.4g)、及TEOS(8ml)混合於4ml水(H2 O)中，並充分攪拌。接著，將0.1MHCl(0.12ml)加入上述混合物中並充分攪拌，使所得溶液之pH值小於7。接著將上述溶液於室溫下靜置24小時乾燥後，將所得之固體進行研磨。最後，將研磨所得之粉未置於60℃下乾燥6小時，得到具有鈷金屬之矽孔洞材料2。
【實施例3】
首先，取Co(NO3 )2 ‧6 H2 O(0.8g)、及TEOS(8ml)混合於4ml水(H2 O)中，並充分攪拌。接著，將0.1MHCl(0.12ml)加入上述混合物中並充分攪拌，使所得溶液之pH值小於7。接著將上述溶液於室溫下靜置24小時乾燥後，將所得之固體進行研磨。最後，將研磨所得之粉未置於60℃下乾燥6小時，得到具有鈷金屬之矽孔洞材料3。
【實施例4-8】
實施例4-8分別如實施例1之相同方式進行，但以不同的金屬氧化物前驅物取代Co(NO3 )2 ‧6H2 O。實施例4-8分別所使用的金屬化合物，如表1所示。
【實施例9】
將實施例1所得到之具有鈷金屬之矽孔洞材料1置於如第2圖所示裝置之測試腔體106中，以量測其對於NH3 的吸附能力，量測方式如下：以質量流量控制器103及104分別控制待測氣體(NH3 )101及載送氣體(氮氣)102的流量，充分混合後(混合後NH3 濃度為500ppb)，藉由閥門105來控制送進具有金屬孔洞材料107的測試腔體106進行吸附，氣流由腔體上方進入，貫穿金屬孔洞材料107後由腔體106下方排出氣體109，氣流貫穿期間以每2.5分鐘一筆數據的速度，以紫外光-可見光(UV-Vis)光譜系統記錄粉體表面紫外光-可見光(UV-Vis)吸收特性圖譜(溫度為21.3℃、溼度為44.1%)，並記錄100次，吸收度變化結果請參照第3圖。在500ppbNH3 氣體以每分鐘1700cc的流速貫穿的測試條件下，粉體表面由粉紅色(附件2)轉為藍紫色(附件3)。請參照第3圖，在波長600~700 nm之間，吸收度隨著通入氨氣量的增加而逐漸變大，此結果證實，該金屬孔洞材料可確實可作為NH3 之呈色感測材料，搭配紫外光-可見光光譜系統的即時量測，可作為NH3 氣體監測器。
【實施例10-11】
實施例10-11分別如實施例9之相同方式進行，但分別以實施例2及3所得之金屬孔洞材料取代實施例1所得之金屬孔洞材料。實施例9-11所述之金屬孔洞材料其吸收氨氣前後的吸收強度(在640nm)差異結果如表2所示。
【實施例12-14】
實施例12-14分別如實施例9之相同方式進行，但分別以60ppbNH3 、115ppbNH3 、及230ppbNH3 取代實施例9所使用之500ppbNH3 濃度。實施例12-14所述之金屬孔洞材料其吸收氨氣前後的吸收強度(在640nm)差異結果如表3所示。
接著，將表3所得之結果進行作圖，繪示出在不同NH3 濃度(ppb)下，金屬孔洞材料吸收氨氣前後的吸收度差異(ΔA)(在640nm下)，如第4圖所示。由圖可知，吸收度差異(ΔA)與氨氣濃度成正比，且其通入之氨氣濃度與吸收度變化呈現良好之線性關係。由此可知，本發明所述之金屬孔洞材料不僅可對氨氣進行定性分析，若與一紫外光-可見光光譜儀(UV-Vis spectrometer)系統連結時，亦可進行即時量測的氨氣定量分析。
【實施例15】
將實施例1所得到之具有鈷金屬之矽孔洞材料1(金屬孔洞材料)置於如測試腔體中，以紫外光-可見光光譜儀系統量測該金屬孔洞材料未進行NH3 吸收前的紫外光-可見光吸收光譜。接著，將含有NH3 的氣體(濃度為46ppm、50sccm)，送進具有金屬孔洞材料的測試腔體進行吸附，氣流由腔體上方進入，貫穿金屬孔洞材料後由腔體下方排出，持續進行60分鐘後，以紫外光-可見光光譜儀系統量測該金屬孔洞材料的吸收光譜。接著，停止送入含有NH3 的氣體進入腔體，30分鐘後，再以紫外光-可見光光譜儀系統量測該金屬孔洞材料的吸收光譜。接著，當停止送入含有NH3 的氣體進入腔體24小時後，再以紫外光-可見光光譜儀系統量測該金屬孔洞材料的吸收光譜。最後，再次通入含有NH3 的氣體(濃度為46ppm、50sccm)，並持續兩小時，再以紫外光-可見光光譜儀系統量測該金屬孔洞材料的吸收光譜，上述量測之結果如第5圖所示。由圖可知，本發明所述之金屬孔洞材料具有可重覆使用性，非常合用於對氨氣的偵測。
綜合上述，由於本發明所述之金屬孔洞材料其上的金屬化合物中帶正電的金屬中心原子，可與含氮化合物中帶有孤對電子對的胺基結合成為過渡金屬化合物，導致吸收光強度的改變，因此可再以紫外-可見光譜儀及予以定性及定量分析。此外，本發明所述之金屬孔洞材料，由於具有高靈敏度、高選擇性、可重覆性、及低偵測極限，因此可進一步用於含氮化合物之檢測方法及裝置上，非常適合用於監測低濃度氨氣。請參照表4，係為本發明所述之含氮化合物之檢測方法與習知離子機動性測譜(Ion Mobility Spectroscopy、IMS)、化學螢光法(Chemiluminescence)、腔體振盪吸收光譜法(Cavity Ring-Down Spectroscopy、CRDS)、以及傳統採樣分析的離子層析法(Impinger+ion chromatography、IC)的比較。
雖然本發明已以數個較佳實施例揭露如上，然其並非用以限定本發明，任何所屬技術領域中具有通常知識者，在不脫離本發明之精神和範圍內，當可作任意之更動與潤飾，因此本發明之保護範圍當視後附之申請專利範圍所界定者為準。
11-16．．．步驟
101．．．待測氣體
102．．．載送氣體
103、104．．．質量流量控制器
105．．．閥門
106．．．測試腔體
107‧‧‧金屬孔洞材料
108‧‧‧紫外光-可見光光譜系統
109‧‧‧排出氣體
第1圖係為本發明一實施例所述之金屬孔洞材料的製備流程圖。
第2圖係為實施例9所述測量含氮分子之氣體的偵測器裝置圖。
第3圖係為實施例9所述以金屬孔洞材料吸附氨氣的吸附測試結果。
第4圖係顯示在不同NH3 濃度(ppb)下，金屬孔洞材料吸收氨氣前後的吸收度差異(ΔA)。
第5圖係顯示本發明實施例15所述之金屬孔洞材料其重覆性實驗結果。
附件1係為光阻因環境的氨氣所導致的T型頂(t-topping)現象之影像。
附件2係為本發明實施例9所述之金屬孔洞材料其吸附氨氣前的影像。
附件3係為本發明實施例9所述之金屬孔洞材料其吸附氨氣後的影像。
101．．．待測氣體
102．．．載送氣體
103、104．．．質量流量控制器
105．．．閥門
106．．．測試腔體
107．．．金屬孔洞材料
108．．．紫外光-可見光光譜系統
109．．．排出氣體

Claims (12)

  1. 一種金屬孔洞材料的製備方法，包含：混合一矽氧烷、一金屬或金屬化合物、及水，攪拌後得到一混合物；調控該混合物使其具有一pH值，其中該pH值小於7；在調整完pH值後，對該混合物進行一第一乾燥處理，得到一固體；以及對該固體進行研磨，進行一第二乾燥處理後得到該金屬孔洞材料，其中，製備該金屬孔洞材料的方法無使用任何鍛燒製程。
  2. 如申請專利範圍第1項所述之金屬孔洞材料的製備方法，其中該矽氧烷之化學結構係為Si(OR4 )，R係為含1-8個碳原子的烷基。
  3. 如申請專利範圍第1項所述之金屬孔洞材料的製備方法，其中該矽氧烷係為四異丙烷氧化鈦(titanium(IV)isopropoxide；TTIP)、四甲基矽氧烷(TMOS)、四乙基矽氧烷(TEOS)、或其組合。
  4. 如申請專利範圍第1項所述之金屬孔洞材料的製備方法，其中該金屬係為含鐵、銅、釩、錳、鉻、鈷、或其組合。
  5. 如申請專利範圍第1項所述之金屬孔洞材料的製備方法，其中該金屬化合物係為含鐵、銅、釩、錳、鉻、或鈷之鹵化物、硫化物、硝酸鹽、氮酸鹽、硫酸鹽、或其組合。
  6. 如申請專利範圍第1項所述之金屬孔洞材料的製備方法，其中該金屬孔洞材料所含之矽與金屬的重量比係介於0.95：0.05至0.05：0.95之間。
  7. 如申請專利範圍第1項所述之金屬孔洞材料的製備方法，其中該第一乾燥處理及該第二乾燥處理的溫度係不大於60℃。
  8. 一種金屬孔洞材料，包含以下原子所組成：金屬原子，該金屬原子合包鐵、銅、釩、錳、鉻、鈷、或其組合，其中該金屬原子之原子數比率佔該金屬孔洞材料之1~10%；矽原子，該矽原子之原子數比率佔該金屬孔洞材料之20~40%；氧原子，該氧原子之原子數比率佔該金屬孔洞材料之50~70%，其中該金屬多孔材料在製程中未經任何鍛燒製程，並具有一分解溫度介於150~250℃。
  9. 一種含氮化合物之檢測方法，包含：提供如申請專利範圍第8項所述之金屬孔洞材料；導入一待測氣體與該奈米結構材料反應；以及分析反應結果。
  10. 如申請專利範圍第9項所述之含氮化合物之檢測方法，其中該含氮化合物包含氨氣。
  11. 如申請專利範圍第9項所述之含氮化合物之檢測方法，更包含將該金屬孔洞材料與一紫外光-可見光光譜系 統連結，以即時量測該金屬孔洞材料在一特定波長範圍的光吸收強度。
  12. 如申請專利範圍第11項所述之含氮化合物之檢測方法，其中該特定波長範圍係介於300-900nm。
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