TW201416327A - 奈米銀線之製備方法 - Google Patents
奈米銀線之製備方法 Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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Abstract
本發明之主要目的係在提供一種奈米銀線之製備方法,係以醛類衍生物作為還原劑,將正一價之銀鹽於有機促進劑的存在下還原成奈米銀線,其步驟包括:(A)提供包含有機促進劑以及醛類衍生物之水溶液,加熱水溶液後加入酸類,反應形成第一溶液;(B)加入具正一價之銀鹽水溶液至第一溶液,反應完成後得到奈米銀線之產物。
Description
本發明係關於一種奈米銀線之製備方法,尤指一種使用水作為溶劑,以及醛類衍生物作為還原劑之奈米銀線製備方法。
奈米級的銀材料,由於表面積大幅提升,其所具有的特殊性質,可被廣泛地用在各種領域,例如高導電性奈米銀塗料、奈米銀觸媒、以及高抗菌性奈米銀殺菌劑等等。在光電材料中,透明導電薄膜為光電元件中不可或缺的材料,而現階段的光電產品所使用的透明導電薄膜大多為氧化銦錫薄膜(ITO),不過考量到未來銦礦短缺及軟性電子應用的問題,許多新興導電材料迅速的崛起,如奈米碳管、石墨烯及金屬奈米線等。其中,奈米銀線目前具有以下之製備方法:模板合成法、零維奈米結構自組裝法、光還原法、熱還原法、固-液相界面反應法、晶種合成法、以及多元醇合成法。
目前製備奈米銀線之技術主要係由多元醇合成法製備,其製備過程必須使用大量的有機溶劑,並使用貴重金屬作為催化劑,如鈀、以及鉑金屬等,且必須於高溫狀態(>160℃)下進行反應,故目前奈米銀線製備方法不適合大量製造,其製備成本也相對昂貴,不利於工業上的量產。
因此,目前急需一種新的奈米銀線製備方法,取代先前製備方法中作為還原劑之有機溶劑,以及作為催化劑之
貴重金屬,以達成降低製備成本,符合環保要求之製程,並且利於大量生產。
本發明之主要目的係在提供一種奈米銀線之製備方法,係以醛類衍生物作為還原劑,將正一價之銀鹽於有機促進劑的存在下還原成奈米銀線,其步驟包括:(A)提供包含有機促進劑以及醛類衍生物之水溶液,加熱水溶液後加入酸類,反應形成第一溶液;(B)加入具正一價之銀鹽水溶液至第一溶液,反應完成後得奈米銀線之產物。
如上述奈米銀線之製備方法中,步驟(A)中,有機促進劑係為聚乙烯吡咯烷酮,其分子量範圍係在20000~50000之間,其濃度範圍係在0.05~1 M之間,較佳為0.1~0.5 M之間;醛類衍生物係為含碳數1~20之醛類,如甲醛、乙醛、糠醛、3,4,5-三甲氧基苯甲醛等,其濃度範圍係在0.01~1 M間,較佳為0.03~0.07 M之間,更佳為0.05~0.07 M之間;而酸類係為硝酸、鹽酸、或硫酸,其濃度範圍係在0.001~0.01 M之間,較佳為0.002~0.007 M之間,更佳為0.003~0.005 M之間。此外,步驟(A)中,加熱水溶液係加熱至70℃至120℃,較佳為80~100℃;反應時間係為1~10分鐘,較佳為1~5分鐘。
如上述奈米銀線之製備方法中,步驟(B)中,正一價之銀鹽係為硝酸銀;反應時間係為1~6小時,較佳為2~5小時。
本發明之奈米銀線之製備方法係使用水作為溶劑,製程相較於習知製備方法環保,且具有低溫製程,以及反應速率快之優點,適合大量生產製造,並且相對環保。
取一三頸瓶將聚乙烯吡咯烷酮(分子量為30000)27克以及148毫升的水加入三頸瓶中,混合並加熱至85℃後再加入三聚甲醛0.3克、並緩慢滴入0.1 mL的硝酸,反應3分鐘,於反應後,將1.6 M之硝酸銀水溶液46 mL緩緩滴入三頸瓶中,於85℃下進行反應5小時後降溫,利用沉降法加入酒精或水將聚乙烯吡咯烷酮移除以得到奈米銀線,並於電子顯微鏡下觀察,得線寬約為94~223 nm,長度約16~25μm之奈米銀線,其形態如圖1所示。
取一三頸瓶將聚乙烯吡咯烷酮(分子量為30000)27.5克以及148毫升的水加入三頸瓶中,混合並加熱至85℃後,再加入糠醛2.6克並緩慢滴入0.1 mL的硝酸,反應3分鐘,於反應後,將1.5 M之硝酸銀水溶液50 mL緩緩滴入三頸瓶中,於85℃下進行反應三小時後降溫,利用沉降法加入酒精或水將聚乙烯吡咯烷酮移除以得到奈米銀線,於電子顯微鏡下觀察,得線寬約為240~360 nm,長度約6~12μm之奈米銀線。
取一三頸瓶將聚乙烯吡咯烷酮(分子量為30000)28克以及150毫升的乙醇混合並加熱至85℃後,再將使用10毫升預溶解之3,4,5-三甲氧基苯甲醛5.3克加入三頸瓶中,並緩慢滴入0.1 mL的硝酸,反應3分鐘,於反應後,將1.5 M之硝
酸銀水溶液50 mL緩緩滴入三頸瓶中,進行反應三小時後降溫,利用沉降法加入酒精或水將聚乙烯吡咯烷酮移除以得到奈米銀線,於電子顯微鏡下觀察,得線寬約為150~300 nm,長度約9~48μm之奈米銀線。
上述實施例僅係為了方便說明而舉例而已,本發明所主張之權利範圍自應以申請專利範圍所述為準,而非僅限於上述實施例。
圖1係利用電子顯微鏡觀察本發明實施例1之奈米銀線型態。
Claims (12)
- 一種奈米銀線之製備方法,其步驟包括:(A)提供包含一有機促進劑以及一醛類衍生物之水溶液,加熱該水溶液後加入一酸類,反應形成一第一溶液;(B)加入一具正一價之銀鹽水溶液至該第一溶液,反應完成後得一奈米銀線之產物。
- 如申請專利範圍第1項所述之方法,其步驟(A)中,該有機促進劑係為聚乙烯吡咯烷酮。
- 如申請專利範圍第2項所述之方法,其步驟(A)中,該聚乙烯吡咯烷酮之分子量係於20000至50000之間。
- 如申請專利範圍第1項所述之方法,其步驟(A)中,該有機促進劑之濃度係為0.05至1 M。
- 如申請專利範圍第1項所述之方法,其步驟(A)中,該醛類衍生物係為含碳數1至20之醛類。
- 如申請專利範圍第1項所述之方法,其步驟(A)中,該醛類衍生物係為至少一選自甲醛、乙醛、糠醛、以及3,4,5-三甲氧基苯甲醛所組成之群組。
- 如申請專利範圍第1項所述之方法,其步驟(A)中,該醛類衍生物之濃度係為0.01至1 M。
- 如申請專利範圍第1項所述之方法,其中,該酸類係至少一選自硝酸、鹽酸、以及硫酸所組成之群組。
- 如申請專利範圍第1項所述之方法,其步驟(A)中,加熱該水溶液係加熱至70℃至120℃。
- 如申請專利範圍第1項所述之方法,其步驟(A)中,該反應時間係為1至10分鐘。
- 如申請專利範圍第1項所述之方法,其步驟(B)中,該正一價之銀鹽係為硝酸銀。
- 如申請專利範圍第1項所述之方法,其步驟(B)中,該反應時間係為1至6小時。
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