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博碩士論文 etd-0727106-154344 詳細資訊
Title page for etd-0727106-154344
論文名稱
Title
化學水浴沈積法成長硫化鎘薄膜之研究
A study of cadmium sulfide thin film grown by chemical bath deposition
系所名稱
Department
畢業學年期
Year, semester
語文別
Language
學位類別
Degree
頁數
Number of pages
109
研究生
Author
指導教授
Advisor
召集委員
Convenor
口試委員
Advisory Committee
口試日期
Date of Exam
2006-07-10
繳交日期
Date of Submission
2006-07-27
關鍵字
Keywords
薄膜、化學水浴沈積法、硫化鎘
chemical bath deposition, thin film, CdS, CBD, cadmium sulfide
統計
Statistics
本論文已被瀏覽 5691 次,被下載 8118
The thesis/dissertation has been browsed 5691 times, has been downloaded 8118 times.
中文摘要
本研究探討化學水浴沈積法成長硫化鎘薄膜條件與成膜間關係,以XRD分析晶向結構,SEM觀察薄膜表面形貌與晶粒大小,薄膜厚度是以反射式光譜量測得到。實驗發現改變反應溶液pH值,可以調變硫化鎘薄膜的晶相。pH=8.5~10.5時製備得到的CdS薄膜為具有(002)從優方位的Hexagonal結構,當pH=11時,難以判定晶向結構。在低的pH值(pH=8.5)條件下,由於OH-濃度低,使得硫脲水解量太少,造成S2-濃度低,故即使反應一小時,僅得膜厚49nm。而在高pH值區間(pH=11),由於Cd2+濃度低,因此在反應40分鐘後,所得膜厚約為100nm。但在兩區間內(pH=10.5),可在反應20分鐘時,達到450nm膜厚。改變溶液pH值,可以使薄膜厚度差異程度高達一個數量級。
但是,不同成長條件之組成晶粒大小並不如膜厚之差異般明顯。反應20分鐘之組成晶粒約為70±10nm,反應40分鐘所得之組成晶粒則為75±15nm,且晶粒大小與酸鹼值間無明顯關係。這表示說膜厚增加是由於增加晶粒密度所貢獻的,並非晶粒尺寸增大所造成的。
此外,歸納比較不同基板,以及不同條件下之成長結果,我們認為,硫化鎘是先在溶液中同質成核,再藉由基板與晶核的耦極作用力以某一方位吸附至基板上,晶粒再更進一步增大直到飽和。
Abstract
In this study , we investigate the relationship between growth condition and thin film quality of cadmium sulfide (CdS) thin films grown by chemical bath deposition (CBD) method. Thin film structures are analyzed by X-ray diffraction , morphology and grain size are obtained by scanning electronic microscopy , and film thickness measured by reflectance spectroscopy . In medium pH value ( pH=10.5) , 20 min deposition can achieve 450 nm film thickness . At lower pH (pH=8.5), low hydrolysis rate of thiourea limits the concentration of sulfur anion , film thickness is only 49 nm after one hour deposition at 70 ℃ , and the obtained thin film can not fully cover the substrate to have a pin-hole free film . At higher pH (pH=11), 40 min only deposites 100 nm film thickness. Strong binding between the cadmium ion and the complexing agent causes low free cadmium cation concentration in the solution, which limits the growing rate. By varying the growth pH condition, the difference in thickness is more than one order of magnitude.
In contrast to the film thickness relationship, grain size distribution suffers less influence from the pH consition. Our results indicate no explicitly relation between the grain size and solution pH condition. 20 minutes depositions result cadmium sulfide grain sizes to be 70±10nm , and 40 minutes result grain size to be 75±15nm . The results indicate that film thickness increases mainly due to the increasing of grain number, rather than the increasing of grain size .
By summarized the results, we propose that the deposition of cadmium sulfide film is initially formed homogeneous nucleation in the solution. The nuclea diffuse and adhere to the substrate. Intristic electric dipole momentum of the cadmium sulfide nano-particle provides an attractive force for the adhesion, and results preferred orientation. Meanwhile, the grain keeps growing up until the size saturated .
目次 Table of Contents
目錄

第一章 緒論 1
1.1前言 1
1.2 化學水浴沈積法 2
1.3 化學水浴沈積法成長硫化鎘薄膜 4
1.3.1化學水浴沈積法成長硫化鎘薄膜的配方 4
1.3.2 同質成核與異質成核 4
1.3.3化學反應機制 8
1.3.4化學水浴法成長硫化鎘薄膜的相關參數與影響 9
1.3.4.1鎘鹽濃度與種類對CBD-CDS的影響 9
1.3.4.2 硫脲濃度對硫化鎘薄膜的影響 10
1.3.4.3 氨水濃度對硫化鎘薄膜的影響 10
1.3.4.4 緩衝溶液濃度對硫化鎘薄膜的影響 11
1.3.4.5 溶液PH值對硫化鎘薄膜的影響 12
1.3.4.6 回火對硫化鎘薄膜的影響 12
1.3.4.7 反應溫度對硫化鎘薄膜的影響 13
第二章 實驗步驟 15
2.1 基板清洗 15
2.2 成長硫化鎘薄膜於矽基板表面 15
2.3 成長疏水性薄膜於矽基板上 16
2.3.1 OCTADECYLTRICHLOROSILANE 16
2.3.2 OCTADECYLTRIMETHOXYSILANE 17
2.4 實驗藥品 17
2.5分析儀器 18
2.5.1 X-光繞射儀 18
2.5.2 掃描式電子顯微鏡(SEM) 19
2.5.3 反射式光譜儀 19
第三章 結果與討論 20
3.1 化學反應機制 20
3.2反應溶液顏色變化 21
3.3 反應溶液PH值對硫化鎘薄膜厚度的影響 22
3.4 硫化鎘薄膜的表面形貌 23
3.5 硫化鎘薄膜的結構分析 26
3.6 硫化鎘薄膜的成膜條件 29
3.7 SILANE疏水性薄膜與硫化鎘薄膜成長於選擇性區域 31
第四章 結論 34
第五章 參考資料 36
第六章 附錄 46

表目錄
表3-1 硫化鎘薄膜的反應條件 46
表3-2 硫化鎘薄膜厚度 47
表3-3 反應溶液PH值對晶粒大小分佈的影響 48
表3-4 JCPDS 06-0314 (HEXAGONAL,WURTZITE) 49
表3-5 JCPDS 10-0454 (CUBIC,SPHALERITE) 49
表3-6 硫化鎘薄膜的XRD PATTERN相關數據 50
表3-7 硫化鎘薄膜的實驗條件 53

圖目錄
圖2-1 實驗流程 58
圖2-2 矽基板清洗流程 59
圖2-3 化學水浴法生長硫化鎘薄膜流程圖 60
圖3-1 不同PH值所造成的硫化鎘反應溶液顏色變化(0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 61
圖3-2 硫化鎘反應溶液顏色變化( 0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 62
圖3-3. 硫化鎘試片在SI基板上的顏色呈現( 0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 63
圖3-4 硫化鎘薄膜厚度與反應溶液PH值關係圖(0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 65
圖3-5 PH=8.49,反應時間40分鐘的SEM IMAGE (0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 66
圖3-6 PH= 8.49,反應時間1小時的SEM IMAGE (0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 67
圖3-7 PH=9.03,反應時間20分鐘的SEM IMAGE ( 0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 68
圖3-8 PH=9.03,反應時間40分鐘的SEM IMAGE(0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 69
圖3-9 PH=9.50,反應時間20分鐘的SEM IMAGE ( 0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 70
圖3-10 PH=9.50,反應時間40分鐘的SEM IMAGE (0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 71
圖3-11 PH=10.00,反應時間20分鐘的SEM IMAGE ( 0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 72
圖3-12 PH=10.00,反應時間40分鐘的SEM IMAGE (0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 73
圖3-13 PH=10.51,反應時間20分鐘的SEM IMAGE ( 0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 74
圖3-14 PH=10.51,反應時間40分鐘的SEM IMAGE (0.002M氯化鎘 , 0.06M硫脲, 0.003M氯化銨) 75
圖3-15 PH= 11.00,反應時間20分鐘的SEM IMAGE (0.002M氯化鎘 , 0.06M硫脲, 0.003M氯化銨) 76
圖3-16 PH= 11.00,反應時間40分鐘的SEM IMAGE(0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 77
圖3-17 晶粒大小分佈(氯化鎘0.002M,硫脲0.06M,氯化銨0.03M) 78
圖3-18 反應溶液PH值變化對晶粒平均大小的影響 84
圖3-19 反應溶液PH值變化對晶粒大小分佈半高寬的影響 85
圖3-20 PH=12.15 時的XRD PATTERN (0.001M氯化鎘 , 0.075M硫脲) 未加緩衝溶液 86
圖3-21 PH=10時的XRD PATTERN (0.001M氯化鎘 , 0.075M硫脲) 未加緩衝溶液 86
圖3-22 PH=9.19時的XRD PATTERN (0.001M氯化鎘 , 0.075M硫脲) 未加緩衝溶液 87
圖3-23 PH=8.49時的硫化鎘薄膜的XRD PATTERN (0.003M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 87
圖3-24 PH=9.03時的硫化鎘薄膜的XRD PATTERN (0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 88
圖3-25 PH=9.5時的硫化鎘薄膜的XRD PATTERN (0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 88
圖3-26 PH=10時的硫化鎘薄膜的XRD PATTERN (0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 89
圖3-27 PH=10.51時的硫化鎘薄膜的XRD PATTERN (0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 89
圖3-28 PH=11時的硫化鎘薄膜的XRD PATTERN (0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 90
圖3-29 PH=8.49~11時的硫化鎘薄膜的XRD PATTERN (0.002M氯化鎘 , 0.06M硫脲, 0.03M氯化銨) 91
圖3-30 硫化鎘薄膜生長於玻璃基板上的情形 92
圖3-31 塗佈SILANE於玻璃基板上的情形 94
圖3-32 疏水性SILANE於化學水浴沈積法法成長硫化鎘薄膜時被氨水腐蝕的情形 95
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58.Rusu, M., Rumberg, A., Schuler, S., Nishiwaki, S., Würz, R., Babu, S.M., Dziedzina, M., Kelch, C., Siebentritt, S., Klenk, R., Schedel-Niedrig, Th. and Lux-Steiner, M.Ch. (2003). "Optimisation of the CBD CdS deposition parameters for ZnO/CdS/CuGaSe 2/Mo solar cells " Journal of Physics and Chemistry of Solids 64(9-10): 1849-1853.
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64.Metin, H.; Esen, R. (2003). "Annealing studies on CBD grown CdS thin films " Journal of Crystal Growth 258(1-2): 141-148.
65.Cui, H.-N., Teixeira, V., Meng, L.J. and Zhang, H.-J. (2004). "Studies on microstructure bilayer film of ultrasonic dipped cadmium sulfide and d.c. sputtered indium tin oxide " Thin Solid Films 447-448: 663-668.
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67.Lee, J. (2004). "Raman scattering and photoluminescence analysis of B-doped CdS thin films " Thin Solid Films 451-452: 170-174
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