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研究生:王尹男
研究生(外文):Yin-nan Wang
論文名稱:奈米碲化鉛之水熱法合成及其火花電漿燒結體性質研究
論文名稱(外文):Spark plasma sintering of PbTe nanoparticles derived from hydrothermal method
指導教授:黃啟祥黃啟祥引用關係
指導教授(外文):Chii-Shyang Huang
學位類別:碩士
校院名稱:國立成功大學
系所名稱:材料科學及工程學系碩博士班
學門:工程學門
學類:材料工程學類
論文種類:學術論文
論文出版年:2009
畢業學年度:97
語文別:中文
論文頁數:68
中文關鍵詞:火花電漿燒結水熱法碲化鉛
外文關鍵詞:PbTespark plasma sinteringhydrothermal
相關次數:
  • 被引用被引用:2
  • 點閱點閱:345
  • 評分評分:
  • 下載下載:88
  • 收藏至我的研究室書目清單書目收藏:0
PbTe系列合金為中溫域最著名之熱電材料,為提升PbTe塊材的熱電轉換效率,本研究旨在檢討如何製備出奈米晶粒尺寸之PbTe塊材。研究項目包括: (1) 如何結合化學法及水熱法之優點而合成奈米大小的PbTe粒子,並提高其產粉效率, (2) 探討火花電漿燒結的燒結溫度與持溫時間對燒結體粒徑之影響及其氧化物之生成關係 (3) 探討奈米塊材之微觀結構對載子傳輸之影響。
本研究利用水熱爐的高壓還原特性及化學法的分段化學反應提出二階段水熱法,此法以600 ml的高壓釜,反應物Pb(NO3)2、Te各為0.06 mole時可於110 oC反應1小時而合成出單一相的PbTe奈米粉末,其粒子大小在10~40 nm,每次產量可達20 g。但粉體表面有氧化現象,氧含量約25 at%。合成的粉體經200 oC持溫3分鐘的SPS燒結,可製備出平均粒徑129 nm之緻密燒結體(相對密度 > 95 %);更高的燒結溫度則會使原本附著在粉體表面的非晶質氧化物結晶成PbTeO3而析出於PbTe晶界。而載子在PbTe奈米塊材中的移動是由晶界散射所主導。
PbTe based alloys are one of the best intermediate temperature thermoelectric materials. This research focus on fabricating dense PbTe bulk with nano-sized grains to enhance the thermoelectric conversion efficiency; including three items . (1) Combing the advantages of hydrothermal method and low temperature wet chemical route to synthesize PbTe nanoparticles and to enhance the yield. (2) To investigate the relationship between the microstructures and the sintering parameters (sintering temperature and holding time) of SPS. (3) To investigate the relationship between the microstructure and the electrical properties.
Two steps hydrothermal method was proposed to synthesize PbTe nanoparticles. This method reproducibly synthesizes 10-40 nm nanocrystals at 110 oC for 2 h and has a high yield over 20 g per batch. The result also indicates surface oxidation on the nanocrystals, and the average oxygen content is about 25 at%. Dense PbTe nanocomposites were obtained by spark plasma sintering of as-synthesized nanoparticles at 200 oC for 3 min. The average grain size of this nanocomposite is 129 nm and the relative density is over 95%. The electrical properties are related to the microstructure which suggests that the transport properties are dominated by grain boundary potential barrier scattering.
摘要 I
Abstract II
目錄 III
表目錄 V
圖目錄 VI
第一章 緒論 1
1-1前言 1
1-2研究目的 2
第二章 相關文獻回顧與整理 3
2-1 奈米塊材 3
2-1-1熱電轉換效率之提升 3
2-1-2 奈米塊材於熱電之應用 6
2-2 碲化鉛基化合物奈米塊材製備 14
2-2-1碲化鉛基化合物簡介 14
2-2-2碲化鉛基化合物奈米塊材製備 18
2-2-3化學法製備碲化鉛奈米粉末 19
2-2-4火花電漿燒結 21
第三章 實驗方法與步驟 23
3-1 實驗材料 23
3-2 實驗流程 23
3-2-1碲化鉛粉末的製備 23
3-2-2 碲化鉛燒結塊材製備 24
3-3 樣品分析方法 27
3-3-1產物結晶相分析 27
3-3-2 顯微結構觀察 27
3-3-3 燒結體密度量測 27
3-3-4 電導率量測 28
3-3-5 載子濃度量測 28
第四章 結果與討論 32
4-1 粉末分析 32
4-1-1 粉末結晶性分析 32
4-1-2 粉末表面形貌分析 37
4-1-3粉體成分分析 37
4-2 燒結體分析 40
4-2-1 燒結體結晶相分析 40
4-2-2 燒結體微結構分析 45
4-2-3燒結參數對微結構之影響 54
4-3 燒結體電性質分析 57
4-3-1晶粒尺寸對電傳導特性之影響 57
4-3-2晶粒尺寸對載子濃度之影響 59
4-3-3晶粒尺寸對載子遷移率之影響 61
第五章 結論 64
參考文獻 65
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