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研究生：	謝豐任 Sie, Fong-Ren
論文名稱：	碲化鉍基複合粉體之製備及其塊材熱電性質之研究 Powder preparation and thermoelectric properties of Bi2Te3-based bulk materials
指導教授：	黃啟祥 Hwang, Chii-Shyang
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學及工程學系 Department of Materials Science and Engineering
論文出版年：	2017
畢業學年度：	105
語文別：	中文
論文頁數：	161
中文關鍵詞：	碲化鉍基熱電材料、退火處理、無電鍍法、熱裂解法、火花電漿燒結、熱電優值
外文關鍵詞：	Bi2Te3-based thermoelectric materials, annealing treatment, electroless plating, pyrolysis, spark plasma sintering (SPS), figure of merit
相關次數：	點閱：110 下載：1
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碲化鉍基熱電材料是目前性質最優異的室溫型熱電材料，其塊材熱電性能熱穩定性對於商業熱電模組與系統的適用溫度息息相關。從實際運用於商業化量產的角度考量，碲化物塊材的熱穩定性及以粉末冶金法 (powder metallurgy) 製備具奈米微結構之碲化物塊材皆是值得研究的方向。
本論文針對以下四個部分進行研究，分別是 Bi0.5Sb1.5Te3 退火處理、 Bi0.5Sb¬1.5Te3/Sb 複合熱電塊材、Bi0.4Sb1.6Te3/TiO2-Ag複合熱電塊材及 Bi2Te3/Cu 複合熱電塊材。研究之目的旨在探討 Bi0.5Sb1.5Te3 之熱穩定性以及Bi0.5Sb1.5Te3、Bi0.4Sb1.6Te3、Bi2Te3複合熱電塊材之晶相、成分以及微觀結構，並進而關聯其熱電性質。
於 Bi0.5Sb1.5Te3 塊材熱穩定性方面，以機械合金法搭配火花電漿燒結 (SPS) 所製備之塊材經不同退火條件進行熱處理後，其缺陷型態、相對密度與熱電性質皆有明顯變化。其中，塊材經 250 ℃ 持溫 24 h 與經 200 ℃ 持溫 120 h 皆會產生 Te 第二相析出。經退火處理後之 Bi0.5Sb1.5Te3 塊材，其電傳導率及 Seebeck 係數皆分別呈現減少與增加的趨勢，雖然趨勢相同但內部缺陷型態卻不同。退火熱處理亦會使Bi0.5Sb1.5Te3 塊材具有較低之熱傳導率與晶格熱傳導率，顯示塊材內部的缺陷形成散射中心以增加聲子散射所致。Bi0.5Sb1.5Te3 塊材經 200 ℃ 持溫 72 h 退火後有最大之 ZT 值， 0.94 。相較於未退火之Bi0.5Sb1.5Te3 塊材的 ZT 值提升了約 19 % 。
於 Bi0.5Sb¬1.5Te3/Sb 複合熱電塊材方面，以無電鍍法搭配 SPS 製備 p-type Bi0.5Sb1.5Te3/Sb 複合塊材，其 Sb的添加量對顯微結構及熱電性質均有顯著影響。塊材內部可發現奈米 Sb 顆粒團聚於晶界處，此團聚會限制晶粒成長，使平均晶粒尺寸減少。Sb 的添加會使載子濃度與電傳導率增加，並且導致Fermi level 的移動，使 p-type Bi0.5Sb1.5Te3/Sb塊材工作溫度往高溫端移動。實驗結果證明，微量的 Sb 添加有助於聲子散射而獲得較低的熱傳導率與晶格熱傳導率，而過量的 Sb 添加會使熱傳導率與晶格熱傳導率大幅提升。Bi0.5Sb1.5Te3/Sb (2.8 wt%) 樣品於量測溫度500 K 時有最大ZT 值，0.54 。此值相較於 Bi0.5Sb1.5Te3 於 500 K時之 ZT 值，提升約 145%。
於 Bi0.4Sb1.6Te3/TiO2-Ag複合熱電塊材方面，以無電鍍法搭配 SPS 製備 p-type Bi0.4Sb1.6Te3/TiO2-Ag複合熱電塊材，TiO2-Ag 的添加量對缺陷型態、熱電性質及硬度值均有顯著影響。結果顯示，部分 Ag 原子可擴散進入 Bi0.4Sb1.6Te3中取代 Bi 或 Sb 原子位置且形成〖〖Ag〗_Bi^' (Ag〗_Sb^') 缺陷，此可增加載子濃度與電傳導率與導致 Fermi level 的移動使 p-type Bi0.4Sb1.6Te3/TiO2-Ag塊材的工作溫度往高溫端移動。實驗結果證明TiO2-Ag的添加因電傳導率大幅增加而導致電子熱傳導的增加，但晶格熱傳導率因塊材內部缺陷與 TiO2-Ag 形成聲子散射源而減少。Bi0.4Sb1.6Te3/TiO2-Ag (0.25 wt%) 樣品擁有最佳 ZT 值、 ZTave 值及維氏硬度值，其值分別為1.19(375 K)、 1.02 及 104.0 Hv，相較於 Bi0.4Sb1.6Te3 塊材分別提升了 19%、24% 及 21.5%。
於 Bi2Te3/Cu 複合熱電塊材方面，以熱裂解法搭配 SPS 製備 n-type Bi2Te3/Cu 複合塊材，其 Cu含量對顯微結構及熱電性質皆有顯著影響。 SEM 與 TEM 結果顯示，Cu-rich 奈米顆粒均勻散佈於 Bi2Te3 基材中，其粒徑尺寸介於 50-100 nm。 Bi2Te3/Cu (0~1.0 wt%) 塊材皆呈現 n 型傳導， Cu 的添加明顯減少塊材的電傳導率，但同時增加塊材的 Seebeck 係數使功率因子因此增加。Bi2Te3/Cu (1.0 wt%) 於室溫有最大功率因子值，2.37 mW/mK2 ，此值相較於 Bi2Te3 塊材之功率因子提升了約 87%。 Cu 的添加有助於減少熱傳導率，其降幅約 29% 。Bi2Te3/Cu (1.0 wt%) 塊材於室溫具有最小的熱傳導率與最大的功率因子，因而具有最大ZT 值， 0.60 。此值相較於 Bi2Te3 塊材之室溫 ZT 值，提升約 94%。
上述四部分的實驗結果，可以進一步證明適當的退火熱處理與複合的製程有助於增加塊材的熱電性質。其提升 ZT 值的共同原因為透過製程參數的改變，使塊材具有適當的電傳導率及 Seebeck 係數。此外，缺陷濃度的調整與複合 Sb 、 TiO2-Ag 與 Cu 有助降低熱傳導率的功效， ZT 值因此而增加。

To investigate the thermal stability of Bi0.5Sb1.5Te3 and improve the thermoelectric performance of p-type Bi0.5Sb1.5Te3, p-type Bi0.4Sb1.6Te3 and n-type Bi2Te3, the various annealing conditions for Bi0.5Sb1.5Te3, Sb and TiO2-Ag addition in Bi0.5Sb1.5Te3 and Bi0.4Sb1.6Te3, and Cu addition in Bi2Te3 were chosen and investigated in this work. The crystal structure and microstructure of bulk specimens were confirmed by XRD and SEM, respectively. The results indicated that the secondary phase of Te is found in the samples annealed at 250 ℃ for 24 h and 200 ℃ for 120 h. Sb and TiO2-Ag aggregation were found in the grain boundary of Bi0.5Sb1.5Te3 and Bi0.4Sb1.6Te3, and Cu nanoparticles were well dispersed in the Bi2Te3 matrix and pinned at Bi2Te3 grain boundary by SEM results. The electrical conductivity trends for Bi0.5Sb1.5Te3 annealed at the various annealing conditions, Bi0.5Sb1.5Te3/Sb, Bi0.4Sb1.6Te3/TiO2-Ag and Bi2Te3/Cu were different, indicating that Sb and TiO2-Ag aggregation could help to increase the electrical conductivity, whereas the annealing process and Cu addition caused the decrease in electrical conductivity. On the other hand, all process were efficient decrease in thermal conductivity, which means that electronic thermal conductivity or lattice thermal conductivity could be decreased because of scattering the carrier or phonon. The ZT were improved in dfifferent process due to the appropriate power factor and the decreasing of thermal conductivity. The maximum ZT values for Bi0.5Sb1.5Te3 sample annealed at 200 ℃ for 72 h at 300 K, Bi0.5Sb1.5Te3/Sb (0.8 wt.%) at 300 K and Bi0.5Sb1.5Te3/Sb (4.3 wt.%) at 500 K, Bi0.4Sb1.6Te3/TiO2-Ag (0.25 wt.%) at 375 K and the Bi2Te3/Cu (1.0 wt.%) at 300 K were 0.94, 0.8, 0.54, 1.19 and 0.6, respectivity.

中文摘要	I
Extended Abstract	IV
致謝		XV
總目錄		XVIII
表目錄		XXI
圖目錄		XXII
第一章	緒論	1
1-1	前言	1
1-2	研究動機及目的	3
第二章	基礎理論與文獻回顧	5
2-1 基本熱電效應及其應用	5
2-1-1 熱電現象[1]	5
2-1-2 Seebeck 效應	5
2-1-3 Peltier 效應	6
2-1-4 Thomson 效應	6
2-1-4熱電優值 (Figure of merit) 與能源轉換效率	7
2-2 熱電材料的介紹	15
2-2-1 熱電材料的種類	15
2-2-2提升材料熱電性能的方法	21
2-3 熱電塊材的製備方法	34
2-3-1 熔煉法	34
2-3-2 粉末冶金法	35
2-3-3 熱壓燒結技術	35
2-4 碲化鉍熱電材料之相關背景與研究動態	40
2-4-1 碲化鉍化合物簡介	40
2-4-2 相關研究之最新發展	41
第三章	實驗方法與步驟	59
3-1 實驗藥品及原料	59
3-2 實驗方法及流程	60
3-2-1 Bi0.5Sb1.5Te3 塊材熱穩定性測試	60
3-2-2 Bi0.5Sb1.5Te3/Sb 複合熱電塊材製備	60
3-2-3 Bi0.4Sb1.6Te3/TiO2-Ag 複合熱電塊材製備	61
3-2-4 Bi2Te3/Cu複合熱電塊材製備	61
3-3 碲化鉍基材料塊材的製備	67
3-3-1 生胚成形	67
3-3-2 火花電漿燒結 (Spark Plasma Sintering, SPS)	67
3-4 碲化鉍基材料的材料特性測定	67
3-4-1相鑑定分析	67
3-4-2顯微結構觀察	68
3-4-3塊材密度量測	68
3-4-4塊材成分分析	69
3-4-5塊材硬度分析	69
3-5 碲化鉍基塊材之熱電性質量測	71
3-5-1電傳導率與 Seebeck 係數量測	71
3-5-2載子濃度與遷移率量測	72
3-5-3熱傳導率量測	72
第四章	結果與討論	77
4-1 Bi0.5Sb1.5Te3 塊材之熱穩定性	77
4-1-1 合成粉體的相鑑定與顯微結構	77
4-1-2 不同退火條件的Bi0.5Sb1.5Te3 塊材相鑑定	78
4-1-3 不同退火條件的Bi0.5Sb1.5Te3 塊材顯微結構	79
4-1-4 不同退火條件的Bi0.5Sb1.5Te3 塊材熱電性質	80
4-1-4-1載子濃度、遷移率以及電傳導率	80
4-1-4-2 Seebeck 係數及功率因子	82
4-1-4-3熱傳導率及熱電優值	83
4-1-5 結論	85
4-2 Bi0.5Sb1.5Te3/Sb 複合熱電材料	98
4-2-1 Bi0.5Sb1.5Te3/Sb塊材相鑑定與顯微結構	98
4-2-2 Bi0.5Sb1.5Te3/Sb塊材熱電性質	98
4-2-2-1載子濃度、遷移率以及電傳導率	98
4-2-2-2 Seebeck 係數及功率因子	100
4-2-2-3熱傳導率及熱電優值	101
4-2-3 結論	102
4-3 Bi0.4Sb1.6Te3/TiO2-Ag 複合熱電材料	109
4-3-1 TiO2-Ag 粉體相鑑定與顯微結構	109
4-3-2 Bi0.4Sb1.6Te3/TiO2-Ag 塊材相鑑定與顯微結構	109
4-3-3 Bi0.4Sb1.6Te3/TiO2-Ag 塊材熱電性質	110
4-3-3-1 載子濃度、遷移率以及電傳導率	110
4-3-3-2 Seebeck 係數及功率因子	112
4-3-3-3 熱傳導率及熱電優值	113
4-3-4 Bi0.4Sb1.6Te3/TiO2-Ag 塊材機械性質(硬度分析)	114
4-3-5	結論	115
4-4 Bi2Te3/Cu複合熱電材料	124
4-4-1 Bi2Te3/Cu塊材相鑑定與顯微結構	124
4-4-2 Bi2Te3/Cu塊材熱電性質	126
4-4-2-1載子濃度、遷移率以及電傳導率	126
4-4-2-2 Seebeck 係數及功率因子	128
4-4-2-3 熱傳導率及熱電優值	129
4-4-3 結論	130
第五章	總結論	140
第六章	未來研究方向	143
參考文獻	144
作者自述	158

                                    

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