應用微型加熱器金屬封裝於濕式TEM樣品乘載元件之製作

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研究生：	朱正熹 Chu, Cheng-Hsi
論文名稱：	應用微型加熱器金屬封裝於濕式TEM樣品乘載元件之製作 Fabrication of metal sealing Wet-Cell by localized heating method
指導教授：	陳福榮 Chen, Fu-Rong 曾繁根 Tseng, Fan-Gang
口試委員:
學位類別：	碩士 Master
系所名稱：	原子科學院 - 工程與系統科學系 Department of Engineering and System Science
論文出版年：	2010
畢業學年度：	98
語文別：	中文
論文頁數：	67
中文關鍵詞：	環境腔體、金屬凸塊
外文關鍵詞：	Wet-Cell, UBM
相關次數：	點閱：3 下載：0
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摘要

　　本研究主旨在於發展一個可以封裝液態活體生物樣品之元件(Wet-Cell)，使得一般電子顯微鏡可做為環境電子顯微鏡觀測生物試片。製程上我們使用微系統製程技術製作可直接用於一般電子顯微鏡樣品試片載台之元件，同時並不需要任何的改裝樣品試片載台以及外加其他機具。製程是以KOH蝕刻250um厚度的矽晶圓，並有一層100nm的氮化矽薄膜作為電子顯微鏡電子束穿透之觀測窗口。並在薄膜上鍍有一層金屬，使元件可以排除電子束轟擊下產生的電子累積，同時增強薄膜的機械強度。液態試片則以銲錫合金做為封裝材料。
　　捨棄過去常用之環氧樹酯做為封裝材料，而使用銲錫合金取代之，最主要因素則是金屬擁有最低的透氣率。為了使用銲錫金屬做為封裝材料，則必需在元件上鍍上一層潤濕層，增加元件與銲錫金屬的附著性。除此之外，為使銲錫合金熔化封裝，在此使用Localized Heating法，大大的降低在封裝時，元件以及液態活體生物樣品受到熱的損傷。
　　封裝結果可以從螢光光學顯微鏡中發現，封裝完畢後仍有活體大腸桿菌存活，但液體剩餘量大幅減少。但因目前還有許多封裝問題尚未克服，所以未來之目標則是增加封裝的成功良率，並且放進穿透式電子顯微鏡中，觀測液態活體生物試片。

Abstract

The purpose of this research is to develop a Wet-Cell sealing the liquid biological sample to carry out Environmental Electron Microscopy observation. The device fabricated with MEMS technology can be used in conventional TEM holder directly, need not install any hardware additional. Fabrication is KOH etching through 250um thick silicon wafer is used to form the chamber and to release the 100nm thick Si3N4 membrane for electron beam passing through. Metal grids is used to remove the electric charge and improve the mechanical strength. Liquid sample is sealed between two cells with solder.
We use solder alloy to replace epoxy as the seal material because the metal has the lower permeability. We need a wetting layer to connect Wet-Cell and solder material because we want to improve the ability of combine with tin and silicon wafer. And we use localized heating reflow solder material, to reduce the heat damage of the Wet-Cell and liquid biological sample.
The result after we seal the Wet-Cell, we can find the living E.coli by fluorescence optical microscopy. But now we still have some problem did not solve, so the future goal is improve the yield, and use Transmission Electron Microscopy to observe living biological sample.

章節目錄
摘要.............................................................................................................................................i
Abstract.......................................................................................................................................ii
致謝...........................................................................................................................................iii
章節目錄...................................................................................................................................iv
表目錄.......................................................................................................................................vi
圖目錄......................................................................................................................................vii
Chapter 1 前言...........................................................................................................................1
1.1 Wet-Cell簡介................................................................................................................1
1.2 Wet-Cell研究動機........................................................................................................2
1.3 Environmental TEM的發展.........................................................................................2
1.4孔隙限制Environmental TEM.....................................................................................3
1.5薄膜限制Environmental TEM.....................................................................................3
1.6 Wet-Cell製作想法........................................................................................................5
Chapter 2 實驗原理及儀器.....................................................................................................16
2.1電阻式加熱器應用Localized heating法....................................................................16
2.2 UBM............................................................................................................................16
2.3封裝材料之選擇..........................................................................................................17
2.4 E-gun............................................................................................................................17
2.5 RIE...............................................................................................................................18
2.6 LPCVD........................................................................................................................20
2.7 PECVD........................................................................................................................21
Chapter 3 實驗步驟.................................................................................................................26
    3.1 Wet-Cell改良設計概念..............................................................................................26
　　3.2 試片製備....................................................................................................................27
　　　3.2.1 Inframe製程........................................................................................................27
　　　3.2.2 Outframe製程......................................................................................................29
　　3.3 試片封裝....................................................................................................................31
Chapter 4 結果與討論.............................................................................................................45
　　4.1微機電製程問題討論.................................................................................................45
　　　4.1.1微影問題..............................................................................................................45
　　　4.1.2金屬掀離問題......................................................................................................45
　　　4.1.3兩次KOH體型微加工濕蝕刻問題....................................................................46
　　　4.1.4薄膜破損問題......................................................................................................46
　　　4.1.5薄膜結構上光阻塗佈..........................................................................................47
　　　4.1.6 PECVD Si3N4覆蓋問題......................................................................................47
　　　4.1.7 UBM掀離問題....................................................................................................48
　　　4.1.8 UBM濕蝕刻問題................................................................................................48
　　4.2加熱結果討論.............................................................................................................48
　　　4.2.1基本參數..............................................................................................................48
　　　4.2.2 IR..........................................................................................................................48
　　4.3封裝測試.....................................................................................................................49
　　　4.3.1銲錫與UBM測試................................................................................................49
　　　4.3.2 Wet-Cell封裝測試...............................................................................................49
      4.3.3 Wet-Cell封裝問題...............................................................................................49
      4.3.4 Wet-Cell封裝問題解決方法...............................................................................50
4.4以傳統epoxy封裝Wet-Cell並於SEM中觀測E.coli............................................51
Chapter 5 總結.........................................................................................................................64
Chapter 6 未來研究展望.........................................................................................................65
文獻...........................................................................................................................................66

表目錄
表1.1 Environmental chamber和Wet-Cell比較表.................................................................15
表1.2 MEMS Film-limit type和Wet-Cell比較表...................................................................15

























圖目錄
圖1.1開放系統示意圖...............................................................................................................6
圖1.2封閉系統示意圖...............................................................................................................6
圖1.3開放系統裝置...................................................................................................................7
圖1.4封閉系統裝置...................................................................................................................7
圖1.5 H. Hashimoto製造之(a)氣體反應試片腔體的截面圖 (b)試片載台............................8
圖1.6 H. Hashimoto製造之氣體反應試片腔體放入TEM腔體內..........................................9
圖1.7 K. Fukushima製造之示意圖.........................................................................................10
圖1.8 Tyrone L. Daulton製造之環境試片載台示意圖..........................................................11
圖1.9 Tyrone L. Daulton製造之環境試片載台實際照片......................................................11
圖1.10 Tyrone L. Daulton環境裝置複雜之管線圖................................................................12
圖1.11 Tyrone L. Daulton製造之環境試片載台截面圖........................................................12
圖1.12 Tyrone L. Daulton製造之環境試片載台氣體及液體管線圖....................................13
圖1.13使用Tyrone L. Daulton裝置拍攝之E. coli.................................................................13
圖1.14 K. Kaznacheyev以OM觀測被兩層Si3N4薄膜包住之水膜.................................14
圖2.1材料密封性之比較.........................................................................................................22
圖2.2 SnPb相圖.......................................................................................................................22
圖2.3熱蒸鍍示意圖.................................................................................................................23
圖2.4 E-gun示意圖..................................................................................................................23
圖2.5 RIE示意圖.....................................................................................................................24
圖2.6 LPCVD示意圖..............................................................................................................24
圖2.7 PECVD示意圖..............................................................................................................25
圖3.1上圖為微型加熱器之示意圖，下圖為微型加熱器上方有UBM...............................33
圖3.2微型加熱器熱傳model.................................................................................................34
圖3.3 Inframe製程流程圖.......................................................................................................34
圖3.4 Outframe製程流程圖....................................................................................................35
圖3.5封裝流程圖.....................................................................................................................36
圖3.6 Wet-Cell Outframe觀測窗口蝕刻至一半時.................................................................37
圖3.7 Wet-Cell Outframe觀測窗口蝕刻至一半之放大圖.....................................................37
圖3.8 Wet-Cell Outframe觀測窗口蝕刻完成.........................................................................38
圖3.9 Wet-Cell Outframe觀測窗口蝕刻完成之放大圖.........................................................38
圖3.10 Wet-Cell Outframe加熱器之完成圖...........................................................................39
圖3.11 Wet-Cell Outframe Al電極..........................................................................................39
圖3.12 Wet-Cell Outframe包覆完PECVD之Si3N4之圖.......................................................40
圖3.13 Wet-Cell Outframe完成UBM第一層第二層之鉻與鎳聚焦於薄膜時.....................40
圖3.14 Wet-Cell Outframe完成UBM第一層第二層之鉻與鎳聚焦於UBM上...................41
圖3.15 Wet-Cell Outframe完成UBM第三層第四層之銅與金.............................................41
圖3.16 Wet-Cell Inframe結構完成圖......................................................................................42
圖3.17 Wet-Cell InframeUBM完成圖.....................................................................................42
圖3.18 Wet-Cell Inframe SEM圖............................................................................................43
圖3.19 Wet-Cell Inframe SEM 45o側視圖..............................................................................43
圖3.20 Wet-Cell Outframe SEM圖..........................................................................................44
圖3.21 Wet-Cell Outframe SEM 45o側視圖............................................................................44
圖4.1矽晶圓上有汙染物，或是矽晶圓沒有和光阻有很好的附著性.................................52
圖4.2光罩與試片沒有contact好，造成pattern被顯影掉....................................................53
圖4.3金屬未掀離成功.............................................................................................................54
圖4.4底部開孔較大且為圓形之圖形.....................................................................................55
圖4.5薄膜破的例子.................................................................................................................55
圖4.6噴筆示意圖.....................................................................................................................56
圖4.7光阻無法形成一完整的膜.............................................................................................56
圖4.8改良的方式旋佈光阻之示意圖.....................................................................................57
圖4.9 PECVD Si3N4沒鍍好之情形.........................................................................................57
圖4.10 UBM完全掀離不不起來............................................................................................58
圖4.11 UBM雖掀離起，但只有一小段存活下來.................................................................58
圖4.12濕蝕刻方式蝕刻UBM造成表面髒汙........................................................................59
圖4.13 IR紅外線熱像儀溫度分析..........................................................................................59
圖4.14銲錫合金厚度約20μm.................................................................................................60
圖4.15 UBM厚度與實際上之厚度差不多............................................................................60
圖4.16 Wet-Cell封裝完成SEM圖..........................................................................................61
圖4.17螢光OM觀測E.coli.....................................................................................................61
圖4.18另一螢光OM觀測E.coli.............................................................................................62
圖4.19液體多寡影響封裝示意圖...........................................................................................62
圖4.20適當液體封裝示意圖...................................................................................................63
圖4.21 E.coli於SEM中飄動...................................................................................................63

                                

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