本實驗利用金屬輔助化學蝕刻法製備多孔矽，探討不同的鍍金時間及蝕刻時間對於多孔矽孔洞分佈的影響，再以化學氣相沉積法於孔洞中成長氧化鋅奈米結構。而在金屬輔助化學蝕刻中，金為蝕刻時的催化劑，矽基板上有金分佈的區域會優先被蝕刻，因此，矽基板上金的形貌分佈會直接影響蝕刻的位置，所以，選擇鍍金於基板上，形貌分佈最均勻的35秒作為蝕刻的最佳參數。由於接著會再以化學氣相沉積法的氣-液-固生長機制，成長氧化鋅奈米結構於多孔矽中，因此，氧化鋅成長的位置取決於多孔矽的孔洞分佈。所以，選擇鍍金時間35秒，蝕刻孔洞形貌分佈均勻的3分鐘和5分鐘，作為成長氧化鋅奈米結構的最佳參數。蝕刻3分鐘成長30分鐘長出來的氧化鋅奈米線結構分佈最均勻，氧化鋅奈米線平均長度約10 um。蝕刻3分鐘成長30分鐘長出來的氧化鋅奈米線結構分佈最均勻，氧化鋅奈米線平均長度約為10 um。鍍金35秒蝕刻3分鐘，氧化鋅奈米結構成長時間為30分鐘的多孔矽基板的X光繞射圖(XRD)量測結果顯示，氧化鋅沿著(002)、(101)、(110)、(103)與(002)的晶面方向成長，優選晶相為(002)晶面。而在光致螢光光譜圖(PL)量測結果中，可以得知材料有無本質缺陷存在，氧化鋅奈米結構成長時間為30分鐘的多孔矽基板在近能隙發光區段處有發光，此即為氧化鋅的本質發光，而在可見光區沒有發光，這代表沒有氧化鋅的缺陷存在。鍍金35秒蝕刻3分鐘，氧化鋅奈米結構成長時間為30分鐘的多孔矽基板的場發射量測結果顯示，施加的電場大小為30 V/um，存在最低起始電壓為10 V/um，最大的電流密度為9x10-6 mA/cm2，場發射增強因子β為884。另外，還發現99%的鋅粉長出來的氧化鋅大多為奈米花結構；而99.999%的鋅粉長出來為均勻的氧化鋅奈米線結構，所以，鋅粉的純度會影響氧化鋅奈米結構的形貌。








關鍵字：氧化鋅、奈米線、多孔矽、金屬輔助化學蝕刻、化學氣相沉積法、場發特性。

In this study, the porous silicon were prepared by metal-assisted chemical etching method, and the effect of different gold coating time and etching time on the distribution of porous pores was discussed. Since gold is a catalyst for metal-assisted chemical etching, the area with gold coating will preferentially etched. In this way, the best distribution of the topography was chose for 35 seconds as the best parameter for etching. As well as the chemical vapor deposition method to grow zinc oxide nanostructures in porous silicon, therefore, the growth of zinc oxide depends on the location of porous silicon holes distribution. The etching time 3 and 5 minutes, the holes morphology is uniform. The etching time is chose here for 3 and 5 of minutes as the optimum parameter for growing zinc oxide. when the zinc oxide's growth time was 30 minutes of etching time of 3 minutes the distribution of zinc oxide nanowires the most uniform distribution, and zinc oxide nanowires average length of about 10um.The X-ray measurement showed that the zinc oxide nanowires were grown for 30 minutes in the pores having 3 minutes etching time grow in the crystal plane direction of (100), (101),(103),(110) and (002), and the crystal phase is ZnO(002) highly-preferred orientation. In the photoluminescence spectrum (PL), the zinc oxide nanowires emit light at the near-energy band gap, which is the essential luminescence of zinc oxide, and there is no light in the visible region, which means that there is no defect of zinc oxide. The Porous silicon with a etching time of 3 minutes and growth time of zinc oxide is 30 minutes had a field emission result. The available applied field size is 30 V / um, the turn-on field is 24 V / um, the maximum current density is 9x10-6 mA/cm2, and the field emission enhancement factor β is 884. In addition, the experiment can be found 99% of the zinc powder grow out of zinc oxide mostly were nanometer flower structures, , and zinc powder of 99.999% the nanowire structures were the distribution uniform. Therefore, that the purity of zinc powder will affect the morphology of zinc oxide nanostructures.







Key words: zinc oxide, nanowires, porous silicon, metal-assisted chemical etching, chemical vapor deposition, field characteristics.

目錄

摘要 2
第一章 緒論 12
1-1 前言 12
1-2 研究動機及目的 13
第二章 文獻回顧 14
2-1多孔矽的性質 14
2-2 多孔矽的形成機制 17
2-3氧化鋅的基本性質與應用 27
2-4氧化鋅的發光機制 28
2-5成長氧化鋅的方法 31
2-6化學氣相沉積(Chemical Vapor Deposition，CVD) 31
2-7氣液固成長機制(Vapor Liquid Solid，VLS) 32
2-8 氣固成長機制(Vapor Solid，VS) 33
第三章 實驗方法與步驟 35
3-1 實驗流程 35
3-2 基板準備 36
3-3 以金屬輔助化學蝕刻法製備多孔矽基板的製程儀器 37
3-4 成長氧化鋅奈米結構於多孔矽基板 39
3-5製程儀器 39
3-6量測儀器 41
第四章 實驗結果與討論 48
4-1不同鍍金時間於P型(100)晶面的矽基板上 48
4-2 鍍金35秒經不同蝕刻時間於P型(100)晶面的矽基板 50
4-3成長氧化鋅於鍍金35秒經蝕刻3 和5分鐘的P型(100)晶面的矽基板上 53
4-4 X光量測之結構特性分析 57
4-5光激螢光光譜量測之光學特性分析 58
4-6場發射量測之場發特性分析 59
第五章 結論 61
第六章 未來工作 63
第七章 參考文獻 64








圖表目錄

圖2-1、比較不同的蝕刻技術[7]。 15
圖2-2、金屬輔助蝕刻不同沉積金屬催化劑的比較圖[7]。 16
圖2-3、金屬輔助蝕刻機制示意圖[12]。 17
圖2-4、比爾模型孔洞起始示意圖[13]。 19
圖2-5、量子模型孔洞起始示意圖[10]。 20
圖2-6、 矽基板蝕刻5分鐘於不同蝕刻晶面的SEM圖：(A)矽基板(100)晶面、(B)矽基板(111)晶面[25]。 21
圖2-7、奈米碳管結構不同的生長方向的SEM圖與場發射圖：(A)垂直，(B)非準直的生長方向[26]。 22
圖2-8、納米碳管結構不同的分佈密度的SEM圖與場發射圖: (A)分布密度高的，(B)分布密度低的[26]。 23
圖2-9、分別為氧化鋅的(A)納米棒陣列(B)和納米椎的SEM圖像[27]。 24
圖2-10、氧化鋅不同形貌的場發射圖，方形/三角形/星形/圓圈的符號分別代表納米柱/奈米椎/奈米柱形貌的氧化鋅和箔(PT)/奈米柱和淫(AG)[27]。 24
圖2-11、PT、AG和ZN能階和費米能階的示意圖[27]。 25
圖2-12、蝕刻30分鍾的多孔矽孔洞之SEM圖[28]。 25
圖2-13、高倍率與低倍率的氧化鋅成長於多孔矽之SEM圖[28]。 26
圖2-15、氧化鋅的鎢采結構圖[29]。 27
表2-1、氧化鋅基本性質[37]。 28
圖2-16、氧化鋅缺陷能帶的示意圖[41] 30
圖2-17、綠光區的強度、氧缺陷的含量與自由載子濃度隨著溫度變化的相應性[40]。 30
圖2-18、化學氣相沉積法成長氧化鋅示意圖[51]。 32
圖 2-19、VLS成長機制示意圖[56] 33
圖 2-20以VS機制成長氧化鎂奈米線之示意圖[57]。 34
圖3-1、實驗流程圖。 36
圖3-3、金屬輔助化學蝕刻製備多孔矽基板的實驗設備圖。 38
圖3-4、水平式高溫爐。 40
圖3-5、金屬濺鍍機。 41
圖3-6、掃描式電子顯微鏡。 42
圖3-7、X 光繞射儀。 43
圖3-10、場發射原理示意圖[58]。 46
圖3-11 場發射量測儀：(A)側面、(B)正面。 47
圖4-1、不同鍍金時間於P型矽基板(100)晶面之 SEM圖 ： (A)5秒、(B)10秒、(C)15秒、(D)20秒、(E)25秒、(F)30秒、(G)35秒、(H)40秒。 49
圖4-2、不同蝕刻時間於P型矽基板(100)晶面之SEM 俯視圖： (A)3分鐘、(B) 5分鐘、(C) 7分鐘、(D) 10分鐘、(E)12分鐘、(F) 15分鐘。 51
圖4-3、不同蝕刻時間於P型矽基板(100)晶面之SEM 側面圖： (A)3分鐘、(B) 5分鐘、(C) 7分鐘、(D) 10分鐘、(E)12分鐘、(F) 15分鐘。 52
圖4-4 蝕刻後的P型(100)晶面矽基板成長氧化鋅於60分鐘之SEM圖： 54
(A~C)蝕刻3分鐘、(D~F) 蝕刻5分鐘。 54
圖4-5、蝕刻後的P型(100)晶面矽基板成長氧化鋅於55分鐘之SEM圖 55
：(A~C)蝕刻3分鐘、(D~F) 蝕刻5分鐘。 55
圖4-6、蝕刻後的P型(100)晶面矽基板成長氧化鋅於50分鐘之SEM圖：(A~C)蝕刻3分鐘、(D~F) 蝕刻5分鐘。 56
圖4-7、蝕刻後的P型(100)晶面矽基板成長氧化鋅於45分鐘之SEM圖：(A~C)蝕刻3分鐘、(D~F) 蝕刻5分鐘。 57
圖4-8、蝕刻後的P型(100)晶面矽基板成長氧化鋅於40分鐘之SEM圖：(A~C)蝕刻3分鐘、(D~F) 蝕刻5分鐘 58
圖4-9、蝕刻後的P型(100)晶面矽基板成長氧化鋅於35分鐘之SEM 59
圖：(A~C)蝕刻3分鐘、(D~F) 蝕刻5分鐘。 59
圖4-10、蝕刻後的P型(100)晶面矽基板成長氧化鋅於30分鐘之SEM圖：(A~C)蝕刻3分鐘、(D~F) 蝕刻5分鐘。 60
圖4-11、蝕刻後的P型(100)晶面矽基板成長氧化鋅於25分鐘之 SEM圖： (A~C)蝕刻3分鐘、(D~F) 蝕刻5分鐘。 61
圖4-12、蝕刻後的P型(100)晶面矽基板成長氧化鋅於20分鐘之 SEM圖：(A~C)蝕刻3分鐘、(D~F) 蝕刻5分鐘。 62
圖4-13、蝕刻後的P型(100)晶面矽基板成長氧化鋅於15分鐘之SEM 63
圖：(A~C)蝕刻3分鐘、(D~F) 蝕刻5分。 63
圖4-14、蝕刻後的P型(100)晶面矽基板成長氧化鋅於10分鐘之SEM圖：(A~C)蝕刻3分鐘、(D~F) 蝕刻5分鐘。 54
圖4-15、蝕刻後的P型(100)晶面矽基板成長氧化鋅於 5分鐘之SEM圖： (A~C)蝕刻3分鐘、(D~F) 蝕刻5分鐘。 55
圖4-16、從孔洞中成長出氧化鋅奈米線之SEM圖：(A)低倍率、(B)高倍率。 56
圖4-17、從孔洞中成長出氧化鋅奈米線之BEI圖。 56
圖4-20、蝕刻3分鐘後成長30分鐘的氧化鋅之PL圖。 59
圖4-18、蝕刻3分鐘後成長30分鐘的氧化鋅奈米線之FIELD EMISSION圖。 60
圖4-19、純矽基板成長30分鐘的氧化鋅奈米線之FIELD EMISSION圖[66]。
60

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