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研究生：	張明宗
論文名稱：	電化學沉積技術應用於微型熱電致冷器之研製 Development of thermoelectric micro-cooler using a electrochemical deposition technique
指導教授：	楊啟榮 Yang, Chii-Rong 程金保 Cheng, Chin-Pao
學位類別：	碩士 Master
系所名稱：	機電工程學系 Department of Mechatronic Engineering
論文出版年：	2007
畢業學年度：	95
語文別：	中文
論文頁數：	112
中文關鍵詞：	碲鉍合金、銻鉍合金、熱電材料、致冷晶片、電化學技術
英文關鍵詞：	bismuth telluride, antimony telluride, thermoelectric, cooling chip, electrochemical technique
論文種類：	學術論文
相關次數：	點閱：320 下載：0
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隨著電子及光電元件產品封裝縮小化及高發熱密度的趨勢，高效率的冷卻及精確控溫技術越來越重要。微熱電元件具有體積小、無污染、控溫效率高等優點，正好符合此一趨勢。由於微電子及微機電技術的進步，使得熱電元件的設計及製程技術而有了新的發展及應用，而微小化的熱電元件更適合應用於微小的電子元件散熱，延長使用壽命及提高元件穩定度。
本研究利用電化學沉積的技術，電鍍n-type熱電材料Bi2Te3及p-type熱電材料Sb2Te3的合金電鍍，研製微型熱電致冷晶片，並探討不同金屬基板上其熱電材料的表面形貌，並找出較佳的電鍍參數，以比較在各個參數不同的情形下之改變，可達到材料之最佳匹配。利用黃光微影的製程分別將上下金屬電極及p-type及n-type腳位做連結，以完成製程整合。
本實驗以濃度為7.5 × 10-3 M 的Bi2O3與10 ×10-3 M 的TeO2，成功鍍出了緻密性良好的n-type Bi2Te3熱電材料，其鍍率約為6 um/hr，其成分為Bi約為45 %，Te成分約為55 %，故後續將再調變濃度，期望達到Bi 40 %及Te 60 %p-type Sb2Te3熱電材料已接近材料所需之成分比率，Sb成分約為42 %，Te成分約為58 %，但對於其表面粗操度仍需進ㄧ步的改善。
而由實驗結果做一實際運作，並對微熱電製冷晶片做特性量測，包括了XRD、SEM、Seebeck 係數、熱傳導係數以及電阻值的量測。

With the electronic and optoelectronic components products and packaging technology grow up, and high fever of electronic products, high-efficiency cooling and precise temperature control technology is increasingly important.
Micro thermoelectric element is small, clean, efficient, high temperature control device. By using its cooling application, we use costless electrochemical technique to fabricate micro thermoelectric cooler, in order to solution thermal problem of electronic products.
We use Bi2O3, Sb2O3 and TeO2 metal oxide powder dissolve in diluted HNO3 for preparing electrolyte. And, we use different metal based plate to electroplate thermoelectric materials, in order to find better based for electroplating n-type junction Bi2Te3 and p-type junction Sb2Te3.
We find a better electroplating conditions to electroplate Bi2Te3 material.The concentration of the metal powder choose 7.5 × 10-3 M Bi2O3 and 10 × 10-3 M TeO2 to electroplate a smooth morphology junction, and the composition of Bi near 45 % and Te 55 %, the growth rate is about 6 um/hr. The other thermoelectric material Sb2Te3 can be found that the composition of Sb is neat 42 ％, and Te 58 ％, it is very close the proportional composition. But, the smoothness of Sb2Te3 is needed to be improve.

總   目   錄
摘要      I
總目錄      III
圖目錄      V
表目錄      IX
第一章 緒論      1
1.1 前言      1
1.2 散熱元件介紹      2
1.3 研究動機與目的     5
1.4 論文架構     7
第二章 熱電效應原理介紹      16
2.1 三大熱電效應      16
2.1.1 席貝克效應      16
2.1.2 帕耳帖效應      18
2.1.3 湯姆生效應     19
2.2 熱電優值      20
2.3 熱電材料的分類與選擇      22
2.4 電化學沉積的基本原理      23
2.5影響合金電鍍之參數      28
2.6電鍍與電鑄技術的異同      29
2.7電鍍合金的特點      30
第三章 文獻回顧      35
3.1 材料備製方法之分類      35
    3.2 傳統技術製造法      35
3.2.1 布里茲曼法      35
3.2.2     CZ法      36
3.2.3 熱壓成形法      36
3.2.4 熱擠壓成形法      37
3.3 微加工技術製造法      40
    3.3.1 濺鍍/蒸鍍法      40
    3.3.2     MOCVD法      41
    3.3.3 電化學沉積法      42
第四章 實驗設計與流程      56
4.1 實驗規劃      56
    4.2 製成規劃與設備介紹      58
4.2.1 微影製程      58
4.2.2 合金電鑄      59
    4.3 熱電材料之合金電鑄      62
     4.3.1 哈爾式槽試驗      62
     4.3.2 小型電鍍槽電鍍實驗      63
    4.4 鍍層分析與量測      64
         4.4.1 掃描式電子顯微鏡      64
     4.4.2 能量分散式光譜分析儀      64
     4.4.3 表面輪廓儀      65
     4.4.4     X-ray繞射儀      65
    4.5 材料的熱電特性量測      65
             4.5.1 席貝克係數的量測方法      65
             4.5.2 熱傳導係數的量測方法      66
             4.5.3 導電率量測方法     67
             4.5.4 紅外線熱像儀      68
第五章 實驗結果與討論      80
5.1 電化學沉積鉍化碲合金      80
             5.1.1鉍化碲合金沉積於銅基板之探討      80
5.1.2鉍化碲合金沉積於銀基板之探討      81
5.1.3鉍化碲合金沉積於金基板之探討      83
    5.2 電化學沉積銻化碲合金      99
             5.2.1銻化碲合金沉積於金基板之探討      99
第六章 結論與未來展望      105

參考文獻      107

圖   目   錄
Figure 1-1    Schematic diagram of thermoacoustic refrigerator      9
Figure 1-2    Schematic of two-phase microchannel heat sink for model development      9
Figure 1-3    MEMS jets process flow chart      10
Figure 1-4    Droplet/jet impingement schematic of EDIFICE      10
Figure 1-5    Schematic chart of thermoelectric      11
Figure 1-6    Schematic chart of heat pipe      11
Figure 1-7    Schematic chart of loop heat pipe      12
Figure 1-8    Schematic chart of capillary pumped loop      12
Figure 1-9    Moore’s law      14
Figure 1-10    Commercial bulk thermoelectric cooling chip       15
Figure 2-1    Schematic chart of Seebeck effect      31
Figure 2-2    Schematic chart of Peltier effect      31
Figure 2-3    Schematic chart of Thomson effect      32
Figure 2-4    Performance of the established P-type thermoelectric materials      33
Figure 2-5    Performance of the established N-type thermoelectric materials      33
Figure 2-6    Materials dependence of electrical conductivity, Seebeck coefficient, power factor, and thermal conductivity      34
Figure 3-1    Schematic diagram of Bridgman method      38
Figure 3-2    Schematic diagram of CZ method      38
Figure 3-3    Schematic diagram of hot pressing method      39
Figure 3-4    Schematic diagram of hot extrusion method      39
Figure 3-5    (a) In-plane (lateral) Peltier cooler (b) Thermoelectric mini-device on Kapton substrate      44
Figure 3-6    The supporting membrane affects largely the performance of lateral thermoelectric cooler      45
Figure 3-7    Thermoelectric properties of Bi-Te films deposition at 260 °C on glass, mica, MgO, and Al2O3 substrate      45
Figure 3-8    (left) Bi2Te3 films deposited at (a) 130 °C (b) 260 °C, both with at. %Te of 60, and (c) 260 °C with at. % Te of 54. (right) Sb2Te3 films deposited at (a) 170 °C (b) 270 °C, both with at. %Te of 60, and (c) 260 °C with at. % Te of 50      46
Figure 3-9    A cross section SEM picture of the overgrowth of 5 mm thick p-(Bi, Sb)2Te3 layer over a contact electrode     47
Figure 3-10    Schematic diagram of experimental setup for co-sputtering      47
Figure 3-11    (a) Te contents in deposited as a function of RF power of Te target (b) Seebeck coefficient of telluride films as a finction of the deposition temperature      48
Figure 3-12    Schematic illustration of MOCVD PROCESS      48
Figure 3-13    (a) Schematic diagram of Peltier device (b) Peltier cooling device as a function of applied current      49
Figure 3-14  (a) SEM close up of a completed p-type and n-type couple(~20 mm heights) SEM overview of entire completed microdevice (b) Cooling delta (from temperature averaging) vs. applied current was plotted and illustrates a Delta-max at around 2K     51
Figure 3-15    electrochemical MEMS fabrication steps for thermoelectric microdevice       52
Figure 3-16    Surface morphology of BixTey films electrodeposited at different potentials: (a) -10 mV, (b) -60 mV, (c) -100 mV, (d) -170 mV, (e) -200 mV, (f) -300 mV, (g) -400 mV     53
Figure 3-17    SEM images of (top) antimony telluride and (bottom) antimony      54
Figure 3-18    XRD pattern of an electrodeposited (a) Sb layer and (b) Sb2Te3     54
Figure 3-19    SEM images of Sb2Te3 films deposited on (top) Ag working electrode and (bottom) Si (100) working electrode (b) XRD pattern of Sb2Te3 films deposited on (left) Ag and (right) Si (100)      55
Figure 4-1    Flow chart of research      57
Figure 4-2    Flow chart of process      61
Figure 4-3    DC & RF sputter      71
Figure 4-4    Thermal evaporator      71
Figure 4-5    Lithography process equipments (a) spin coater (b) hot plate (c) UV mask aligner (d) optical microscope      73
Figure 4-6    Schematic diagram of Hull cell equipment      74
Figure 4-7    Schematic diagram of 1L electroplating tank      75
Figure 4-8    SEM and EDS system      76
Figure 4-9    Surface profiler      76
Figure 4-10    X-ray diffraction      76
Figure 4-11    Schematic diagram of Seebeck coefficient measurement      77
Figure 4-12    Schematic diagram of thermal conductivity measurement equipment      78
Figure 4-13    Schematic diagram of electrical conductivity equipment      78
Figure 4-14    Infrared radiometer      78
Figure 5-1    (right) OM images of Bi-Te film deposited under 1 × 10-3 M, applied current (a) 100 mA (b) 50 mA      85
Figure 5-2    SEM morphology of Bi-Te alloy deposited on copper substrate      86
Figure 5-3     SEM morphology of Bi-Te alloy deposited on copper substrate     87
Figure 5-4    SEM morphology of Bi-Te alloy deposited on Ag substrate at concentration of 1 × 10-3 M      88
Figure 5-5    SEM morphology of Bi-Te alloy deposited on Ag substrate at concentration of 5 × 10-3 M      89
Figure 5-6    SEM morphology of Bi-Te alloy deposited on Ag substrate at concentration of 10 × 10-3 M      90
Figure 5-7    Thickness of Bi-Te alloy deposited for 3 hours      91
Figure 5-8    SEM morphology of Bi-Te alloy deposited on Ag substrate for 3 hours      91
Figure 5-9    Concentration of  Bi-Te mole ratio versus Bi at. %      92
Figure 5-10    SEM morphology of Bi-Te alloy deposited on Au substrate at concentration of 5 × 10-3 M      93
Figure 5-11    SEM morphology of Bi-Te alloy deposited on Au substrate at concentration of 7.5 × 10-3 M      94
Figure 5-12    SEM morphology of Bi-Te alloy deposited on Au substrate for 3 hours      95
Figure 5-13    Close view of single junction of Bi-Te alloy      95
Figure 5-14    Over view of junction of Bi-Te alloy      96
Figure 5-15    Thickness of Bi-Te alloy deposited on Au substrate for 3 hours      96
Figure 5-16    SEM morphology of Bi-Te alloy deposited on Au substrate at concentration of 10 × 10-3 M      97
Figure 5-17    Concentration of  Bi-Te mole ratio versus Bi at. %      98
Figure 5-18 SEM morphology of Sb-Te deposited on Au substrate at concentration of 5 × 10-3 M    101
Figure 5-19 SEM morphology of Sb-Te deposited on Au substrate at concentration of 10 × 10-3 M    103




表   目   錄
Table 1-1      Microfabrication technologies in MEMS field      8
Table 1-2    Development history of thermoelectric material      13
Table 1-3    The amount of transistors development in modern times    14
Table 3-1    Room temperature values of Seebeck coefficient (a), Hall mobility (m), electrical resistivity (r), and carrier concentration (n and p) for n-type Bi2Te3, p-type (Bi1-xSbx)2Te3 (x＝0.73 and 0.77) films      50
Table 3-2    Atomic percentages as a function of the applied potential(vs. Ag/AgCl (3 M NaCl)) for deposition on Pt electrodes calculated from electron probe microanalysis. The concentration of the solution is HTeO2+ (1 × 10－2 M) and Bi3+ (0.75 × 10－2 M) in 1 M HNO3. Deposition time, 60 min except for the E ＝ －0.52 in which the growth was so fast that a thick film formed in 20 min      51
Table 4-1    Experimental facilities      69
Table 4-2    Experimental chemical medicines      70
Table 5-1      Analysis Bi-Te element of the film deposited on Cu substrate      86
Table 5-2     Analysis Bi-Te element at concentration of Bi2O3 5 × 10-3 M of the film      93
Table 5-3    Analysis Bi-Te element at concentration of
Bi2O3 7.5 × 10-3 M of the film      94
Table 5-4    Analysis Bi-Te element at concentration of
Bi2O3 10 × 10-3 M of the film      97
Table 5-5    Analysis Sb-Te element at concentration of
Sb2O3 5 × 10-3 M of the film      102
Table 5-6    Analysis Sb-Te element at concentration of
Sb2O3 10 × 10-3 M of the film      104
                                

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