此論文為有機複合物吸附二氧化鈦作為光催化材料應用於裂解水
產氫之研究，主要選用蠶絲蛋白作為有機載體，二氧化鈦作為吸附
材料，而二氧化鈦結構分別以奈米顆粒、奈米柱及介孔晶體附著於
孔洞內，並比較三種異質結構之產氫效果。本實驗先使用氫氧化鈉
與溴化鋰溶解蠶絲蛋白，由透析法萃取出蠶絲溶液，經由膠化作用
後低溫乾燥得到多孔之蠶絲外殼;製作出載體後，再使用水熱法在不
同前驅物及改變加熱溫度和持溫時間下，得到三種不同結構之二氧
化鈦，主要以掃描式及穿透式電子顯微鏡觀察其結構變化、X-射線
繞射儀鑑定晶體結構，最後利用氣相層析儀比較在太陽光下不同形
態之二氧化鈦附著於有機體的光催化能力。結果顯示介孔晶體之二
氧化鈦整體表現能力最佳，其製程手法簡易、光催化能力良好並且
能高密度附著於孔洞有機複合物內。
除了不同結構之二氧化鈦研究外，如何增加二氧化鈦吸附在孔洞
表面也是另一項探討的議題，本研究分別在蠶絲溶液膠化前後加入
二氧化鈦及改變二氧化鈦濃度比較附著情形，結果顯示在膠化前二
氧化鈦(1.063 g/L)能達到最高密度的吸附，進而增加接觸面積提升
光催化能力之效果。

This thesis has been carried out at the National Tsing Hua University (Hsinchu,
Taiwan), in the Department of Materials Sciences and Engineering. This thesis consisted
of the study and development of an organic porous structure used as a matrix
for the incorporation of titanium dioxide in the purpose of water photo-catalysis to
produce hydrogen. The main organic compound studied was silk fibroin from silkworm.
The titanium dioxide has been synthesized in different forms: nanoparticles,
nanorods and mesocrystals. The working steps were:
• Theoretical study: chemical/physical reaction, existing photocatalysts, previous
work.
• Extraction, purification of the fibroin, gelation and lyophilisation.
• Characterization: SEM, TEM, XRD, spectrophotometer and measure of the
hydrogen production by gas chromatography.
The main issue is the design of a system linking the ease of production of the nanoparticles,
of the organic matrix, and allowing a surface yield increased by the high threedimensional
density of the photo-catalysts.

Introduction 1
1 Theory of photo-chemical water splitting 3
1.1 Chemical reaction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
1.2 System design . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
1.2.1 Efficiency . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
1.2.2 Stability . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
1.2.3 Scalability . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
1.3 Choice of the photo-catalyst . . . . . . . . . . . . . . . . . . . . . . . 7
1.4 Design prospect . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
2 Photo-catalysts 10
2.1 Nanorods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
2.1.1 Synthesis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
2.1.2 Characterization . . . . . . . . . . . . . . . . . . . . . . . . . 12
2.2 Mesocrystals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
2.2.1 Synthesis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
2.2.2 Characterization . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.3 Nanowires . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2.3.1 Synthesis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2.3.2 Characterization . . . . . . . . . . . . . . . . . . . . . . . . . 16
2.4 Titanium dioxide doping . . . . . . . . . . . . . . . . . . . . . . . . . 17
2.4.1 Hydrogen treatment . . . . . . . . . . . . . . . . . . . . . . . 18
2.4.2 Modified mesocrystals . . . . . . . . . . . . . . . . . . . . . . 20
3 Porous materials 24
3.1 Inorganic materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
3.2 Organic materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
3.3 Silk biofoam . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
3.3.1 Synthesis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
3.3.2 Characterization . . . . . . . . . . . . . . . . . . . . . . . . . 27
3.4 Bacterial nanocellulose . . . . . . . . . . . . . . . . . . . . . . . . . . 29
3.4.1 Synthesis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
3.4.2 Characterization . . . . . . . . . . . . . . . . . . . . . . . . . 30
4 Combinations of composites materials 31
4.1 Gelation with photo-catalysts . . . . . . . . . . . . . . . . . . . . . . 31
4.2 Photo-catalysts solution incubation . . . . . . . . . . . . . . . . . . . 35
5 Performance Evaluation 37
5.1 Hydrogen production . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
5.2 Photo-degradation of dye . . . . . . . . . . . . . . . . . . . . . . . . 38
5.2.1 Manual experiment . . . . . . . . . . . . . . . . . . . . . . . . 39
5.2.2 Automated experiment . . . . . . . . . . . . . . . . . . . . . . 40
6 Economics and cost analysis 46
6.1 Raw materials availability . . . . . . . . . . . . . . . . . . . . . . . . 46
6.1.1 Titanium dioxide . . . . . . . . . . . . . . . . . . . . . . . . . 46
6.1.2 Silk fibroin . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
6.2 Cost estimation of the raw materials . . . . . . . . . . . . . . . . . . 47
Conclusions 49
Appendices 51
A Photo-catalysts 51
B Porous materials 52
B.1 Silk biofoam . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
B.2 Bacterial nanocellulose synthesis . . . . . . . . . . . . . . . . . . . . 53
C Combination of composites materials 54
D Performance evaluation 54
D.1 Hydrogen measurement . . . . . . . . . . . . . . . . . . . . . . . . . 54
D.2 Automatic photo-degradation measurement . . . . . . . . . . . . . . 56
E Cost analysis 62
F Equipments 63
References 64

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