臺灣博碩士論文加值系統

本論文研究的半導體奈米材料有三種，分別為SnO2/SnS2異質結構奈米片、SnxSe(1-x)奈米線以及SnSe2/SnSe異質結構奈米片。
第一部份，SnO2/SnS2異質結構奈米片以CVD製程成長並藉由調控冷卻時間來達到控制SnO2與SnS2之間的比例。本實驗總共有四種不同比例的SnO2/SnS2異質結構奈米片被製作出來，分別為純的SnO2、SnS2、SnO2/SnS2 (SnO2偏多)與SnO2/SnS2 (SnS2偏多)。接著將這些奈米片放置於甲基藍溶液中，並在5 W，475 nm LED燈的照射下觀察甲基藍的降解情形。結果顯示只要有SnO2/SnS2異質接面存在都會有效改善降解效果。透過SnO2與SnS2的能帶結構可以得知SnO2/SnS2為一個type II異質接面，能夠有效分離光生電子與電洞以增加載子壽命使催化效果上升。
第二部份，SnxSe(1-x)奈米線，為能夠容易的控制奈米線的組份，使用AAO模板輔助壓力鑄造法來製備並藉由改變前驅物組份來達到控制SnxSe(1-x)奈米線中Sn與Se空缺的含量。一共有8種不同組份的SnxSe(1-x) (x=0.47~0.53)奈米線被合成出來並製作成光感測器。這些不同缺陷濃度的SnSe奈米線被用來製備成光感測器來探測從可見光至紅外光波長的光波。結果顯示出SnxSe(1-x)的光感測性能會隨著x的增加而增加。藉由缺陷的能帶模擬得知，隨著缺陷數量的上升，SnxSe(1-x)的能帶會變小。換句話說，材料的導電率會隨著缺陷濃度的上升而增加，導電率的上升意味著自由電子的增加。也就是說在同樣光強度下，Sn0.53Se0.47的光生載子數量會比純的SnSe還多，使光響應上升。
第三部份，SnSe2/SnSe異質結構奈米片，藉由鉻酸與氫氧化鈉對於SnSe與SnSe2之間的選擇性蝕刻來得到不同組份的SnSe2/SnSe異質結構奈米片。XRD與Raman分析得知，不論是鉻酸或是氫氧化鈉，SnSe2都會優先被蝕刻。將Sn0.39Se0.61(SnSe-SnSe2共晶相)塊材溶於鉻酸中，得到純SnSe奈米片以及SnSe2/SnSe異質結構奈米片，並將奈米片應用於鋰電池。儘管SnSe2的理論電容值比SnSe要低，SnSe2/SnSe異質結構奈米片依舊展現出比SnSe奈米片還要優異的可逆電容。這可以歸因於SnSe2/SnSe異質結構奈米片具有較低的電荷傳輸電阻，其可能是因為SnSe2/SnSe異質接面的電場增加了載子的移動速率。另外，也測試了將不同熱處理後的Sn0.39Se0.61塊材(淬冷、淬冷後退火以及緩慢冷卻三種)浸泡於氫氧化鈉中以得到不同結晶度的SnSe異質結構奈米片。隨後將這三種奈米片作為光催化劑在5 W，475 nm的LED燈下降解甲基藍。由於結晶度高的SnSe奈米片的載子平均自由徑比淬火的要長，預期上退火與緩慢冷卻得SnSe奈米片會有較佳的降解能力。結果顯示淬冷後退火的SnSe奈米片確實具有最佳的降解效果。

In this thesis, three different kinds of materials were being investigated, SnO2/SnS2 heterostructure nanoflakes, SnxSe(1-x) nanowires and SnSe2/SnSe heterostructure nanoflakes.
For the first part, SnO2/SnS2 heterostructure nanoflakes was fabricated with CVD method and the composition can be controlled by adjusting the cooling time during the process. Here, four kinds of nanoflakes were being synthesized, SnO2, SnS2, SnO2/SnS2 (SnO2 rich) and SnO2/SnS2 (SnS2 rich), respectively. Afterwards, these nanoflakes were then used to photodegrade methyl blue solution under 5 W, 475 nm LED light source to probe the influence of SnO2/SnS2 heterojunction to photocatalytic performance. On the basis of the result from UV-Vis spectrometer, the SnO2/SnS2 heterojunction can improve the degraded performance. Base of the band structure of SnO2 and SnS2, the SnO2/SnS2 is a type II heterojunction that will separate electrons and holes to enhance carrier life time and further ameliorate the photodegraded property.
For the second part, SnxSe(1-x) nanowires, in order to control the composition, the AAO template supporting die casting process was being adopted, and the SnxSe(1-x) nanowires with different x were fabricated by directly changing the composition of SnxSe(1-x) bulks. In this report, 8 kinds of SnxSe(1-x) (x=0.47~0.53) nanowires have been synthesized. Those SnxSe(1-x) (x=0.47~0.53) nanowires were used to fabricate the photodetector to detect the light from visible light to infrared light. As result, the photoresponse will rise with the increasing x. To understand the mechanism, the band structure simulation with different concentration of Sn and Se vacancies were being employed and the consequence shown that the band gap will decrease when the defect concentration is ascending. Moreover, under the same defect concentration, the inducing of Se vacancies demonstrate much lower band gap than Sn vacancies. In other words, the free electrons inside SnxSe(1-x) increase as x increase, which mean Sn0.53Se0.47 can generate more electrons and holes than SnSe under the same power density of the irradiation light source and further enhance the photoresponse.
For the third part, SnSe2/SnSe heterostructure nanoflakes were prepared by using H2Cr2O7 or NaOH as an etching solution to etch Sn0.39Se0.61(SnSe-SnSe2 eutectic phase) bulk through selective etching between SnSe and SnSe2. Depend on the XRD and Raman spectrum, the SnSe2 phase is the priority etching phase even for NaOH or H2Cr2O7 solution. Here, the Sn0.39Se0.61 bulk was soaked in H2Cr2O7 solution to obtain SnSe2/SnSe and SnSe nanoflakes, and used in Li-ion battery. Even though the theoretical capacitance of SnSe2 (800 mAh/g) is lower than SnSe (847 mAh/g), SnSe2/SnSe nanoflakes also display the higher reversible capacitance than SnSe nanoflakes. It can be attributed to the build in electric field at SnSe2/SnSe heterojunction that can enhance the carrier mobility to lower charge transfer resistance of SnSe2/SnSe nanoflakes. Besides, we also investigate the influence of heat treatment on precursor Sn0.39Se0.61 bulk (3 types: quench, annealing after quench and slow cooling rate) and the obtained SnSe2/SnSe nanoflakes. These three kinds of SnSe2/SnSe nanoflakes were used as photocatalyst to degrade MB dye under 5 W, 475 nm LED. Since the carrier live time of the SnSe nanoflakes with high crystallinity is longer than the quenching sample, the annealing and slow cooling SnSe nanoflakes is expected to have better degradation ability, and the results show that the SnSe nanoflake that annealed after quenching really have the best degradation effect.

摘要 III
Abstract V
致謝 VIII
List of Abbreviations and Acronyms 1
List of Figures and Tables 2
Chapter 1. Introduction 10
1.1 Nanomaterials 10
1.2 The Structure of SnS2 11
1.2.1 Characteristics of SnS2 Nanoflake 13
1.3 The Structure and Characteristics of SnSe 14
1.4 The Structure and Applications of SnSe2 16
1.5 Flow Chart of Research 18
1.6 Overview of Nanowires Photodetector 22
1.7 Introduction of Photocatalyst 23
1.8 Li-Ion Battery Review 24
Chapter 2. Experimental Section 25
2.1 Manufacture of SnxSe(1-x) Nanowires 25
2.1.1 Preparation of SnxSe(1-x) Bulks 25
2.1.2 Fabrication of SnxSe(1-x) Nanowires 25
2.1.3 AAO Template Removing Process 28
2.1.4 SnxSe(1-x) Nanowires Photodetector Fabrication 28
2.1.5 SnxSe(1-x) Nanowires Photodetector Measurement 28
2.2 Production of SnSe2/SnSe Heterostructure Naoflakes 29
2.2.1 Sn0.39Se0.61 Bulks Preparation 29
2.2.2 H2Cr2O7 Solution Etching Sn0.39Se0.61 Nanoflakes 30
2.2.3 Fabrication of Li-Ion Battery with Sn0.39Se0.61 Nanoflakes 31
2.2.4 NaOH Solution Etching SnSe Nanoflakes 31
2.2.5 NaOH Solution Etching In6Se7/SnSe Heterostructure Nanoflakes 32
2.2.6 Measurement of SnSe Nanoflakes Photocatalytic Property 32
2.3 Synthesis of SnO2/SnS2 Nanoflakes 33
2.3.1 Measurement of Photocatalytic Property 36
Chapter 3. Results and Discussions 37
3.1 The Investigation of SnxSe(1-x) Nanowires (x=0.47~0.53) and Application in Photodetector 37
3.1.1 Motivation of SnxSe(1-x) Nanowires Photodetector 37
3.1.2 Characterization of SnxSe(1-x) Nanowires 38
3.1.3 Photosensing Property of SnxSe(1-x) Nanowires 49
3.1.4 Band Structure Simulation of SnxSe(1-x) Nanowires 70
3.2 The Investigation of SnSe and SnSe2/SnSe Nanoflakes 75
3.2.1 Motivation of SnSe2/SnSe Heterostructure Nanoflakes Li-Ion Battery and SnSe Nanoflakes Photocatalyst 75
3.2.2 Characterization of H2Cr2O7 Etched SnSe2/SnSe Nanoflakes 78
3.2.3 The Li Ions Storage Property of H2Cr2O7 Etched SnSe and SnSe2/SnSe Nanoflakes 90
3.2.4 Characterization of NaOH Etched SnSe Nanoflakes 102
3.2.5 The Photocatalytic Property of SnSe Nanoflakes with Distinct Heating Treatment. 114
3.3 The Application of SnO2/SnS2 Heterostructure Nanoflakes on Photocatalyst 121
3.3.1 Motivation of SnO2/SnS2 Heterostructure Nanoflakes Photocatalyst 121
3.3.2 Relationship Between Cooling Time and Obtained SnO2/SnS2 Heterostructure Nanoflakes 123
3.3.3 Characterization of SnO2/SnS2 Nanoflakes 126
3.3.4 The Photodegraded Efficiency of SnO2/SnS2 Heterostructure Nanoflakes 133
Chapter 4. Summary and Conclusions 142
4.1 The Influence of Intrinsic Defects on SnxSe(1-x) Nanowires Photodetector 142
4.2 The Research of SnSe, SnSe2/SnSe Nanoflakes and Its Application 143
4.3 The Investigation of SnO2/SnS2 Heterostructure Nanoflakes on Photocatalyst 144
Chapter 5. Future Works 145
5.1 The Future Works of SnxSe(1-x) Nanowires Photodetector 145
5.2 The Future Works of SnSe Nanoflakes 145
References 146
Appendix 160

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