臺灣博碩士論文加值系統

本論文主要目的採用脈衝磁控濺鍍製備MZO（ZnO:Mo）薄膜，並藉由化學濕式蝕刻進行薄膜表面粗化，於不同蝕刻時間下觀察薄膜對可見光之漫透射率與光電性質之影響。首先，以ZnO靶材上置放不同位置之鉬片，藉此改變Mo元素之含量，沈積於Corning 1731玻璃基板上。並透過調變濺鍍功率、工作壓力、脈衝頻率、薄膜厚度和基板溫度等參數來製備具最佳光電結構特性之MZO薄膜。其次，以KOH及HCl兩種不同的蝕刻液，調變蝕刻時間進行MZO薄膜表面粗化使其具有陷光結構；探討薄膜蝕刻後對電性、可見光的穿透及散射之影響。研究中利用薄膜測厚儀量測其薄膜厚度及沈積率、能量分散光譜儀量測成分含量、霍爾量測儀量測電阻率、載子濃度和載子遷移率、X光繞射儀做薄膜結構性分析、X光射線光電子能譜儀量測薄膜化學態分析、熱場發射掃描式電子顯微鏡觀察薄膜表面形貌，利用光譜儀做光穿透率量測，並以可變角度多功能光學特性檢測系統做總透射率與鏡面透射率量測，藉此換算出漫透射率的光譜圖。研究結果顯示，於Mo含量1.77wt.％、濺鍍功率100W、工作壓力0.4Pa、脈衝頻率10kHz、薄膜厚度500nm於室溫下，可獲得MZO 薄膜較低的電阻率為8.9×10-4Ωcm，可見光穿透率大於80％。考量光電特性等因素，我們選用0.5％HCl在300K攪拌的環境下蝕刻MZO薄膜3秒到6秒，可得到電阻率1.74~2.75×10-3Ωcm，可見光總透射率67~73％，可見光漫透射率25.1~28.4%，霧度值為0.34~0.42，薄膜表面火山口（Crates）直徑約220~350nm，可應用於薄膜太陽能電池前透明電極。

The purpose of this discourse was prepared MZO (ZnO:Mo) thin film by PMS (Pulse magnetron sputter), and then we used chemical wet etching to observed the effect of diffuse transmittance and electrical properties. First, changed the content of Mo element by different position of molybdenum sheet on ZnO ceramic target to deposit MZO film on glass substrate (Corning 1737). The structural, electrical and optical properties as a fuction of sputtering power, working pressure, pulse frequency, thin film thickness and substrate temperature were investigated. Second, ligh trapping structure of MZO thin film can be prepared by two kinds of etchant at varying the etching time, then discussing the effect of electrical, light scattering and transmittance properties. In the experiment, the film thickness and deposited rate were measured by a profilometer. The content of composition was measured by Energy dispersive spectrometer (EDS). Resistivity, carrier density and carrier mobility were measured by Hall effect measurement system. The analyse of crystallinity was measured by X-ray diffraction (XRD). Analyse of chemical valence was measured by X-ray photoelectron spectroscope (XPS). Surface texture was observed by thermal field emission scanning electron microscope (TF-SEM). Transmittance was measured by spectrometer. Total transmittance and Specular transmittance were measured by angle changeable optical characteristic measurement system to calculated diffuse transmittance. Result, The MZO film showed with the lowest resistivity was prepared by Mo concentration 1.77 wt.%, sputtering power 100W, working pressure 0.4Pa, pulse frequency 10kHz, thin film thickness 500nm at room temperature that showed a resistivity of 8.9×10-4Ωcm and a transmittance of 80% in the visible range. 0.5％HCl and 33％KOH etched 800nm thickness of MZO thin film. At the same thickness, the surface smooth, cavitation decreased and lower resistivity were etched by 33％KOH. Considering electrical, light scattering and transmittance properties, we choosed 0.5％HCl to etch MZO film during 3~6 second. Finally, we can get resistivity of 1.74~2.75×10-3Ωcm, total transmittance of 67~73% in the visible range, diffuse transmittance of 25.1~28.4% in the visible range and haze value between 0.32 to 0.42 for front electrode application of thin film solar cells.

目 次

摘要 I　
謝誌 IV
目次 V
表次 VIII
圖次 IX

第一章 緒論 1
1-1 研究動機 1
1-2 研究貢獻 2
1-3 名詞解釋 3

第二章 理論分析與文獻回顧 4
2-1 透明導電膜材料與製程 4
2-1-1 透明導電膜材料 4
2-1-2 鉬的基本性質 4
2-1-3 MZO透明導電膜 5
2-2 濺鍍原理 9
2-2-1 磁控濺鍍法 11
2-2-2 直流脈衝式磁控濺鍍 12
2-2-3 脈衝頻率對薄膜性質之影響 17
2-3 太陽能電池 20
2-3-1 太陽能電池基本原理 20
2-3-2 薄膜太陽能電池之材料與結構設計 21
2-3-3 透明導電膜於太陽能電池之應用 22
2-4 太陽能電池之TCO表面粗化原理與製程 23
2-4-1表面粗化原理 23
2-4-2表面粗化製程 25
2-4-3不同參數對透明導電膜濕蝕刻性質之影響 27

第三章 研究方法 34
3-1 實驗流程 34
3-2 實驗材料與試片準備 36
3-3 實驗步驟 36
3-3-1 基板準備與前處理準備 36
3-3-2 濺鍍製程系統 38
3-3-3 濺鍍參數與步驟 39
3-4 薄膜特性分析 40
3-4-1 沈積率量測 40
3-4-2 薄膜表面成分分析 41
3-4-3 薄膜化學性質分析 43
3-4-4 四點探針量測 44
3-4-5 霍爾量測儀電性量測 45
3-4-6 SEM表面影像 46
3-4-7 微結構分析 47
3-4-8 可見光穿透率量測 48
3-4-9 光學能隙計算 48
3-5 MZO透明導電膜表面粗化 49
3-5-1 蝕刻實驗 49
3-5-2 可見光漫透射率量測 50

第四章 結果與討論 52
4-1 不同鉬片位置之化學成分 52
4-2 Mo含量對MZO薄膜光穿透率及電阻率之影響 53
4-3 濺鍍參數對MZO光穿透率及電阻率之影響 58
4-3-1 功率對MZO薄膜光穿透率及電阻率之影響 58
4-3-2 工作壓力對MZO薄膜光穿透率及電阻率之影響 62
4-3-3頻率對MZO薄膜光穿透率及電阻率之影響 66
4-3-4 MZO薄膜厚度對MZO薄膜光穿透率及電阻率之影響 70
4-3-5 基板溫度對MZO薄膜電性之影響 74
4-4 表面粗化MZO薄膜對光電性質之影響 78
4-4-1 表面粗化MZO薄膜對電阻率之影響 78
4-4-2 表面粗化MZO薄膜對透射光之影響 82
4-4-3 表面粗化MZO薄膜對表面形貌之影響 88

第五章 結論與未來研究 93
5-1 結論 93
5-2 未來研究 94
參考文獻 95

表 次
表1 不同基板溫度對蝕刻前後電阻率之影響 30
表2 康寧玻璃1737F成份表 36
表3 蝕刻後薄膜厚度對應HCl與KOH所需之蝕刻時間 79


圖 次
圖1 氧化鋅結構圖 7
圖2 不同摻雜量對ITO薄膜吸收係數的平方與入射光能量的關 7
圖3 Burstein-Moss效應示意圖 8
圖4 不同MZO薄膜厚度對(a)電性及(b)穿透率之影響 8
圖5 電漿在腔體的各種反應示意圖 10
圖6 脈衝電源供應器提供五種電壓輸出模式示意圖 13
圖7 脈衝電源供應器避免異常放電之原理示意圖 14
圖8 脈衝循環及調控參數示意圖 15
圖9 優選濺射示意圖，(a)、(b)、(c)分別顯示正常模式、逆向模式及反轉模式三者的靶電壓及靶面發生情形 16
圖10頻率與功率及沈積率關係圖 17
圖11 不同頻率之XRD關係圖 18
圖12 不同頻率對薄膜晶粒大小影響 18
圖13 不同頻率對沈積率與電阻率之影響 19
圖14 不同頻率對薄膜穿透率之影響 19
圖15 太陽能電池的工作原理 21
圖16 (a)Superstrate架構與(b)Substrate架構於薄膜型矽基太陽能電池 22
圖17 a-Si:H/μc-Si:H電池p-i-n結構中的TCO 24
圖18 入射光經粗化過的薄膜所造成的(a)穿透與(b)反射 24
圖19 以CVD製程技術製作具有陷光結構的TCO薄膜 25
圖20 以射頻磁控濺鍍法製作ZnO薄膜，經稀鹽酸蝕刻之SEM影像圖 26
圖21 三種不同的表面形貌應用於μc-Si:H太陽能電池之量子效應與反射率圖27
圖22 (a)AFM 10×10μm2量測所得之不同三種結構與(b)不同鋁含量與基板溫度對蝕刻後的表面情況分佈圖 28
圖23 不同基板溫度與工作壓力所製程之薄膜，經稀鹽酸蝕刻後現的表面結構圖 29
圖24不同基板溫度對全透光率與漫射透光率之影響 30
圖25 不同沈積溫度對AZO薄膜之XRD與半高寬之影響 31
圖26 AZO薄膜經不同蝕刻時間(a)0秒，(b)20秒，(c)60秒之SEM表面結構 31
圖27 AZO薄膜以不同蝕刻時間對(a)太陽能電池I-V曲線之探討與(b)太陽能電池參數之影響 32
圖28 AZO薄膜蝕刻前後示意圖 32
圖29 AZO薄膜蝕刻前後應用於μc-Si:H太陽能電池之量子效應與吸收率圖 33
圖30 實驗流程圖 35
圖31 基板準備與前處理 37
圖32 薄膜濺鍍系統示意圖 39
圖33 薄膜段差測試儀 40
圖34 X光能量分散光譜 41
圖35 Mo片於靶材上之位置示意圖 42
圖36 化學分析電子能譜儀 43
圖37 四點探針電阻儀 44
圖38 霍爾量測儀 45
圖39 熱場發射掃描式電子顯微鏡 46
圖40 X-ray繞射儀 47
圖41 UV 1700紫外/可見光光譜儀 48
圖42 MFS-630 可變角度多功能光學特性檢測系統 50
圖43 入射光入射於表面粗化之薄膜示意圖 51
圖44 功率100W、工作壓力0.4Pa、膜厚500nm、頻率10kHz、脈衝反轉時間5μs時， Mo金屬片位置與Mo含量對照圖 52
圖45 功率100W、工作壓力0.4Pa、膜厚500nm、頻率10kHz、脈衝反轉時間5μs，不同Mo含量對電性之影響圖 54
圖46 Mo含量1.77wt.%、功率100W、工作壓力0.4Pa、膜厚500nm、頻率10kHz、脈衝反轉時間5μs，Mo 2p5/2之XPS能譜圖 55
圖47 功率100W、工作壓力0.4Pa、膜厚500nm、頻率10kHz、脈衝反轉時間5μs，在不同Mo含量對XRD與半高寬（FWHM）之影響圖 56
圖48 功率100W、工作壓力0.4Pa、膜厚500nm、頻率10kHz、脈衝反轉時間5μs，不同Mo含量對(a)穿透率與(b)能隙之影響圖 57
圖49 Mo含量1.77wt.%、工作壓力0.4Pa、膜厚500nm、頻率10kHz、脈衝反轉時間5μs，在不同功率對電性之影響圖 59
圖50 Mo含量1.77wt.%、工作壓力0.4Pa、膜厚500nm、頻率10kHz、脈衝反轉時間5μs，在不同功率對XRD與半高寬（FWHM）之影響圖 60
圖51 Mo含量1.77wt.%、工作壓力0.4Pa、膜厚500nm、頻率10kHz、脈衝反轉時間5μs，在不同功率對(a)穿透率與(b)能隙之影響圖 61
圖52 Mo含量1.77wt.%、功率100W、膜厚500nm、頻率10kHz、脈衝反轉時間5μs，在不同壓力對電性之影響圖 63
圖53 Mo含量1.77wt.%、功率100W、膜厚500nm、頻率10kHz、脈衝反轉時間5μs，在不同壓力對XRD與半高寬（FWHM）之影響圖 64
圖54 Mo含量1.77wt.%、功率100W、膜厚500nm、頻率10kHz、脈衝反轉時間5μs，在不同壓力對(a)穿透率與(b)能隙之影響圖 65
圖55 Mo含量1.77wt.%、功率100W、膜厚500nm、工作壓力0.4Pa，能率循環約為95％時，在不同頻率對電性之影響圖 67
圖56 Mo含量1.77wt.%、功率100W、膜厚500nm、工作壓力0.4Pa，能率循環約為95％時，在不同頻率對XRD與半高寬（FWHM）之影響圖 68
圖57 Mo含量1.77wt.%、功率100W、膜厚500nm、工作壓力0.4Pa，能率循環約為95％時，在不同頻率對(a)穿透率與(b)能隙之影響圖 69
圖58 Mo含量1.77wt.%、功率100W、工作壓力0.4Pa、頻率10kHz、脈衝反轉時間5μs，在不同膜厚對電性之影響圖 71
圖59 Mo含量1.77wt.%、功率100W、工作壓力0.4Pa、頻率10kHz、脈衝反轉時間5μs，在不同膜厚對XRD之影響圖 72
圖60 Mo含量1.77wt.%、功率100W、工作壓力0.4Pa、頻率10kHz、脈衝反轉時間5μs，在不同膜厚對(a)穿透率與(b)能隙之影響圖 73
圖61 Mo含量1.77wt.%、膜厚500nm、功率100W、工作壓力0.4Pa、頻率10kHz、脈衝反轉時間5μs，在不同基板溫度對電性之影響圖 76
圖62 Mo含量1.77wt.%、膜厚500nm、功率100W、工作壓力0.4Pa、頻率10kHz、脈衝反轉時間5μs，在不同基板溫度對XRD與半高寬（FWHM）之影響圖 77
圖63 Mo含量1.77wt.%、膜厚800nm、功率100W、工作壓力0.4Pa、頻率10kHz、脈衝反轉時間5μs，能率循環為95％下製備MZO薄膜，經0.5%HCl腐蝕液蝕刻於300K攪拌的環境下，在不同的蝕刻時間所剩餘的膜厚對電性的影響 80
圖64 Mo含量1.77wt.%、膜厚800nm、功率100W、工作壓力0.4Pa、頻率10kHz、脈衝反轉時間5μs，能率循環為95％下製備MZO薄膜，經33%KOH腐蝕液蝕刻於300K攪拌的環境下，在不同的蝕刻時間所剩餘的膜厚對電性的影響 81
圖65 Mo含量1.77wt.%、膜厚800nm之MZO薄膜以0.5％HCl腐蝕液蝕刻於300K攪拌的環境下，在不同的蝕刻時間 (a)0秒、(b)3秒、(c)6秒和(d)9秒之SEM俯視圖 89
圖66 Mo含量1.77wt.%、膜厚800nm之MZO薄膜以0.5％HCl腐蝕液蝕刻於300K攪拌的環境下，在不同的蝕刻時間 (a)0秒、(b)3秒、(c)6秒和(d)9秒之傾斜角45°SEM圖 90
圖67 Mo含量1.77wt.%、膜厚800nm之MZO薄膜以33％KOH腐蝕液蝕刻於300K攪拌的環境下，在不同的蝕刻時間 (a)33秒、(b)66秒、(c)99秒和(d)100秒之SEM俯視圖 91
圖68 Mo含量1.77wt.%、膜厚800nm之MZO薄膜以0.5％HCl腐蝕液蝕刻於300K攪拌的環境下，在不同的蝕刻時間 (a)0秒、(b)3秒、(c)6秒和(d)9秒之傾斜角45°SEM圖 92
圖69 Mo含量1.77wt.%、膜厚800nm的MZO薄膜，經0.5%HCl腐蝕液蝕刻於300K攪拌的環境下，在不同的蝕刻時間對總透射率與漫透射率的光譜圖 83
圖70 Mo含量1.77wt.%、膜厚800nm的MZO薄膜，經0.5%HCl腐蝕液蝕刻於300K攪拌的環境下，在不同的蝕刻時間對總透射率、漫透射率與霧度的影響 84
圖71 Mo含量1.77wt.%、膜厚800nm的MZO薄膜，經33%KOH腐蝕液蝕刻於300K攪拌的環境下，在不同的蝕刻時間對總透射率與漫透射率的光譜圖 86
圖72 Mo含量1.77wt.%、膜厚800nm的MZO薄膜，經33%KOH腐蝕液蝕刻於300K攪拌的環境下，在不同的蝕刻時間對總透射率、漫透射率與霧度的影響 87

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