二氧化鈦光電特性及染料於光觸媒膜反應器之分解效率

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研究生：	王文裕 Wen-Yu Wang
論文名稱：	二氧化鈦光電特性及染料於光觸媒膜反應器之分解效率 Photoelectrochemical Properties of Titanium Dioxide and Decomposition of Dyes in Photocatalytic Membrane Reactors
指導教授：	顧洋 Young Ku
口試委員:	張祖恩 none 蔣本基 none 曾迪華 none 黃志彬 none 劉志成 none 黃炳照 none
學位類別：	博士 Doctor
系所名稱：	工程學院 - 化學工程系 Department of Chemical Engineering
論文出版年：	2006
畢業學年度：	94
語文別：	英文
論文頁數：	189
中文關鍵詞：	發光二極體、間歇性照射、Langmuir-Hinshelwood 、界達電位、pH偏移
外文關鍵詞：	light emitted diode, periodic illumination, Langmuir-Hinshelwood, zeta potential, pH drift
相關次數：	點閱：215 下載：10
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上一筆

本研究主要探討pH值對二氧化鈦的光電性質，及染料光觸媒催化反應的影響。在酸性溶液的光電化學分析中，二氧化鈦光陽極的開路光電壓及閉路光電流隨pH值減小而增高，顯示在酸性溶液會產生更多的光電子。在酸性溶液的半高開路光電壓及半高閉路光電流的反應時間，比在鹼性溶液快，顯示在酸性溶液，電子的擴散速率較快。利用自行設計的裝置量測二氧化鈦薄膜於電解質溶液中的切線流動電位及過濾流動電位，結果顯示pH值、壓力及紫外光對兩者皆有影響。量測二氧化鈦薄膜切線流動電位計算所得的界達電位，與利用電泳光散射法量測二氧化鈦懸浮液所得的界達電位，兩者數值不同；但兩者所得的等電位點都接近pH 6.8。
本研究首次發現，量測二氧化鈦薄膜切線流動電位的過程中，無論在酸性或鹼性溶液，量測前後電解質溶液pH值會產生偏移現象。利用發展出的修正模式，計算在不同pH值時，二氧化鈦薄膜與電解質溶液費米能階的平衡，能夠解釋pH偏移現象。同時，在切線流動電位量測中，發現隨pH變化的遲滯現象，在不同路徑的相同pH下，會有二個不同的切線流動電位。本研究並首次發現，於酸性溶液，照射紫外光會使切線流動電位小量減小(＜15mV)。於酸性及鹼性溶液，照射紫外光則會使過濾流動電位產生較大的變化(20~60mV)。而且，過濾流動電位隨過濾壓力增加而增高，並隨紫外光照射強度呈現指數減小。
本研究利用紫外光發光二極體(UV-LED)為光源，探討染料(RR22)在二氧化鈦薄膜光催化反應器的反應行為。結果顯示，光觸媒催化行為符合Langmuir-Hinshelwood動力模式；間歇照光的光量子效率比連續照光高。在低光強度時，QLC(石英-溶液-光觸媒)配置方式的光量子效率比QCL(石英-光觸媒-溶液)高；相反地，在高光強度時，兩種光觸媒配置方式的光量子效率接近相等。本研究亦探討二氧化鈦與其塗佈質子交換膜(Nafion)後之表面電性，及對陰離子性染料(RR22)與陽離子性染料(BR2)反應行為的影響。每克二氧化鈦塗佈0.5克Nafion溶液，會使其在pH 2~12間的界達電位下降至-20mV以下，並使二氧化鈦呈現疏水性，減少染料的吸附及光觸媒催化反應速率。吸附實驗及利用低壓汞燈的光觸媒催化結果顯示，二氧化鈦(純的或Nafion改質的)及染料在不同pH的表面電性對反應速率有極大的影響。二氧化鈦光催化分解RR22，在酸性溶液中較快，並於接近等電點時速率最低；而Nafion改質二氧化鈦光催化RR22，無論在酸性或鹼性中，皆無顯著反應。二氧化鈦及Nafion改質二氧化鈦光催化BR2，在鹼性溶液中較快；但是，在Nafion改質二氧化鈦的系統中的反應速率，比在純二氧化鈦中低。

The purpose of this research was to study the effects of solution pH on the photoelectrochemical properties of TiO2 photoelectrode and the photocatalytic reactions of dyestuffs in aqueous solution using photocatalyst membranes. The open circuit voltage and the short circuit photocurrent of TiO2 photoelectrode increased as solution pH decreased and indicated more photoelectrons were generated in acidic solutions. The response times reaching half maximum photovoltage and photocurrent were determined to be faster in acidic solutions than those in alkaline solutions, indicating higher electron diffusion occurred in acidic solutions. The effect of electrolyte solution pH, fluid pressure and UV irradiation on the tangential streaming potential (TSP) and filtration streaming potential (FSP) of Degussa P-25 titanium dioxide membrane were examined. Both TSP and FSP measuring systems for TiO2 membrane were developed. Experimental results depicted TSP and FSP measurements were sensitive to solution pH, temperature, fluid pressure and UV irradiation. Zeta potentials of TiO2 membranes calculated with TSP data were different from those of TiO2 suspensions measured by electrophoretic light-scattering technique, but the isoelectric point (pHiep) was measured to be almost the same value of 6.8.
The pH drifts (difference of initial and final pH) were observed during the TSP measurements of TiO2 membranes. A modified model was developed to calculate the change in Fermi energy of the electrolyte/TiO2 membranes system presented at different solution pH levels. A hysteresis phenomenon was found that two zeta potentials were observed at the same pH through different pH adjustment paths. Slight decreases of TSP (<15mV) were observed in acidic solutions under UV irradiation; however, more considerable decreases of FSP (20~60mV) were examined in both acidic and alkaline solutions. The FSP increased with increasing filtration pressures and exhibited an exponential decay with increasing light intensity.
The ultraviolet light emitting diode (UV-LED) was used as the UV light source for the photocatalytic decomposition of Reactive Red 22 (RR 22). The temporal behavior of the photocatalytic decomposition of RR 22 in aqueous solution by the UV-LED/TiO2 with a rectangular planar fixed-m reactor operated in a recirculation mode was studied under various conditions including initial dye concentration, periodic illumination, light intensity, and arrangements of TiO2 coating. The decomposition of RR 22 in aqueous solution by TiO2 photocatalytic processes with the UV-LED was found to be technically feasible with a high TiO2 coated weight (1.135g) and low pH value (pH 2). A Langmuir-Hinshelwood type kinetic equation was adequate for modeling the photocatalytic decomposition of RR 22 by the UV-LED/TiO2 photocatalytic processes. The experimental results indicated that the photonic efficiency with periodic illumination was much higher than those with continuous illumination. The photonic efficiencies with the QLC (quartz-liquid-catalyst) arrangement were higher than those with the QCL (quartz-catalyst-liquid) arrangement for experiments conducted at lower applied light intensity; however the photonic efficiencies for these two arrangements were nearly identical for experiments conducted at higher light intensities. The coating of 0.5 gram of Nafion per gram of TiO2 was enough to reduce the zeta potential of Nf/TiO2 to less than -20mV in aqueous solution and exhibited a hydrophobic surface that might decrease the adsorption and photocatalytic decomposition of dye. Experimental results on the adsorption and photocatalytic decomposition of RR22 and BR2 indicating that the charges of TiO2 surface and reactant dye markedly influence the reaction rate. The photocatalytic decompositions of RR22 using TiO2 were favored to occur in acidic conditions and exhibited a minimum decomposition rate near the isoelectric point of TiO2. Nevertheless, no obvious RR22 decompositions were found in experiments conducted using Nf/TiO2. Decompositions of BR2 using both TiO2 and Nf/TiO2 were more favorable in alkaline conditions; however, decompositions of BR2 were found to be decreased in experiments conducted using Nf/TiO2.

Chapter 1 Introduction
1.1 Background	1
1.2 Objective and scope	2
Chapter 2 Literature Survey
2.1 Dye wastewater	4
2.2 photocatalyst	5
2.3 UV/TiO2 photocatalytic process	12
2.4 Photocatalytic reactor	15
2.5 LED as a light source in the photocatalytic processss	27
2.6 Photocatalytic reaction kinetics	30
2.7 Operation parameters for the UV/TiO2 process	36
2.8 Photoelectrochemical and electrokinetic properties of TiO2	49
2.9 TiO2 surface charge modification	54
Chapter 3 Experimental Procedure and Analysis
3.1 Apparatus and materials	58
3.2 Photoelectrochemical property and optical spectroscopy measurements	69
3.3 Setup of the streaming potential measurements system	71
3.3.1 Setup of the TSP measurement system		71
3.3.2 Setup of the FSP measurement system	72
3.4 Streaming potential and zeta potential measurements	73
3.5 UV-LED/TiO2 photocatalytic membrane system	75
3.5.1 Preparation of TiO2 membranes	75
3.5.2 UV-LED/TiO2 photocatalytic process	77
3.6 UV/Nf/TiO2 photocatalytic membrane system	84
3.6.1 Preparation and zeta potential measurement of the Nafion-coated TiO2 (Nf/TiO2)	84
3.6.2 UV/Nf/TiO2 photocatalytic process	86
Chapter 4 Results and Discussions
4.1 Photoelectrochemical property and optical spectroscopy of titanium dioxide	88
4.2 Hydrodynamic parameters of the TSP flow cell	99
4.3 Streaming potential measurements of TiO2 membranes	102
4.3.1 TSP measurements	102
4.3.2 pH drifts and Fermi energy equilibriums	106
4.3.3 Zeta potential and pHiep	112
4.3.4 Effect of UV on surface charges of TiO2 membranes	114
4.4 Decomposition of dye in the UV-LED/TiO2 photocatalytic membrane reactor	125
4.4.1 Kinetics of dye decomposition	125
4.4.2 Effect of periodic illumination	132
4.4.3 Effect of UV light intensity and arrangements of TiO2 coating	136
4.5 UV/Nf/TiO2 photocatalytic membrane system	142
4.5.1 Adsorption and zeta potential measurement of the Nafion-coated TiO2 (Nf/TiO2)	142
4.5.2 UV/Nf/TiO2 photocatalytic membrane reactor	148
Chapter 5 Conclusions	152
References	155
Appendix A	166
Appendix B	167

List of figures
Figure 2.1	Energy band diagram: (a) metal, (b) semiconductor, (c) insulator.	6
Figure 2.2	Structure of rutile and anatase TiO2.	9
Figure 2.3	Applications of photocatalyst.	11
Figure 2.4	Schematic illustrations of the semiconductor photocatalysis.	13
Figure 2.5	Energetics and reactions involved in semiconductor photocatalysis. The values in parentheses are for TiO2.	13
Figure 2.6	Schematic diagram of the batch thin membrane photocatalytic reactor.	18
Figure 2.7	Schematic diagram of the optical fiber photoreactor.	21
Figure 2.8	The UV light intensity distribution on and within the optical fiber modeled by Snell’s law and UV light energy balance.	22
Figure 2.9	Schematic of the photocatalytic membrane reactor used with the TiO2 porous filtration membranes.	26
Figure 2.10	LED structure.	29
Figure 2.11	Schematic representation of periodic illumination.	39
Figure 2.12	Photoefficiency vs. tlight (=τL) for the photocatalytic oxidation of formate.	40
Figure 2.13	Comparison of surface speciation distribution of: (a) TiO2 surface groups, (b) speciation distribution of phthalic acid in solution, and (c) the adsorption dependence of phthalic acid on pH.	45
Figure 2.14	Structure of the electrochemical double layer on a particle surface in a system containing electrolytes.	51
Figure 2.15	Illustration of the four electrokinetic effects and their principles.	52
Figure 2.16	Cluster-network model for the morphology of hydrated Nafion.	57
Figure 2.17	Schematic structure of Nafion film: H, hydrophobic fluorocarbon region; C, hydrophilic ionic cluster region; I, interfacial region; ○─: ─SO3─ group of polymer.
57
Figure 3.1	In-house-built SPS measurement system.	63
Figure 3.2	Three-electrode electrochemical cell.	64
Figure 3.3	Schematic representation of the tangential streaming potential measurement system.	65
Figure 3.4	Schematic representation of the tangential streaming potential measurement flow cell.	66
Figure 3.5	Schematic representation of the filtration streaming potential measurement system.	67
Figure 3.6	Experimental setup of the UV-LED/TiO2 photocatalytic process	68
Figure 3.7	Scanning electron micrographs of TiO2 membrane coated on quartz plat. (a) 500X, (b) 150,000X.	76
Figure 3.8	Spectrum of B5-437-CVD.	80
Figure 3.9	Luminous intensity of B5-437-CVD at various forward current.	81
Figure 3.10	Two different arrangements of TiO2 coating for UV-LED/TiO2 photocatalytic process.	82
Figure 3.11	The chemical structure of RR 22 and the proposed photocatalytic reaction pathway.	83
Figure 3.12	The chemical structure of BR2.	85
Figure 4.1	Dependence of open circuit voltage (Voc) on pH without UV irradiation.	93
Figure 4.2	Dependence of open circuit voltage (Voc) on pH with UV irradiation.	94
Figure 4.3	Dependence of the half time on pH to reach the maximum photovoltage and photocurrent.	95
Figure 4.4	The temporal curve of photocurrent under UV irradiation at difference pH.	96
Figure 4.5	Diffuse reflectance spectrum of the Degussa P-25 powder.	97
Figure 4.6	Surface photovoltage spectrum of the Degussa P-25 powder.	98
Figure 4.7	Volumetric flow rates as a function of applied pressure in the tangential streaming potential measurements cell.	101
Figure 4.8	Time dependence of the tangential streaming potential measurement.	104
Figure 4.9	The conductivity of the electrolyte and the hysteresis loop of the dependence of tangential streaming potential on pH.	105
Figure 4.10	The pH drifts within the measurement of tangential streaming potential.	109
Figure 4.11(a)	Fermi energy values of TiO2 membrane calculated in the initial and equilibrium pH for electrolyte solutions and titanium dioxide membranes. 	110
Figure 4.11(b)	Fermi energy values of Electrolyte calculated in the initial and equilibrium pH for electrolyte solutions and titanium dioxide membranes.	110
Figure 4.12	Scheme of electron transfer model proposed at the initial pH of 8 and 5.6 respectively.	111
Figure 4.13	Effect of pH on zeta potential of titanium dioxide suspensions and membranes.	113
Figure 4.14	The tangential streaming potential with and without UV irradiation.	117
Figure 4.15	The differences of tangential streaming potential before and after UV irradiation.	118
Figure 4.16	Dependence of filtration streaming potential on trans-membrane pressure and electrolyte pH in a TiO2 layer supported on a porous stainless steel tube. (Before UV irradiation)	119
Figure 4.17	Dependence of filtration streaming potential on trans-membrane pressure and electrolyte pH in a TiO2 layer supported on a porous stainless steel tube. (After UV irradiation)	120
Figure 4.18	Dependence of filtration streaming potential on trans-membrane pressure and electrolyte pH in a TiO2 layer supported on a porous stainless steel tube. (Difference of FSP before and after UV irradiation)	121
Figure 4.19	Illustration of the streaming potential variation (ΔV) of titanium dioxide membranes before and after UV irradiation in acidic solutions.	122
Figure 4.20	Illustration of the streaming potential variation (ΔV) of titanium dioxide membranes before and after UV irradiation in alkaline solutions.	123
Figure 4.21	Dependence of filtration streaming potential on light intensity and trans-membrane pressure in a TiO2 layer supported on a porous stainless steel tube.	124
Figure 4.22	Effect of initial dye concentration on the decomposition of dye.	130
Figure 4.23	Effect of initial dye concentration on the photonic efficiency.	131
Figure 4.24	Effects of continuous and periodic illumination on the decomposition of dye.	134
Figure 4.25	Effect of light intensity on the photonic efficiency for the decomposition of dye in continuous and periodic illuminations.	135
Figure 4.26	Effects of the arrangements of TiO2 coating on the decomposition of dye.	138
Figure 4.27	Effects of light intensity and arrangements of TiO2 coating on the apparent pseudo first-order decomposition rate constants.	139
Figure 4.28	Effect of light intensity on the photonic efficiency for the decomposition of dye with QCL and QLC arrangements at pH 2 with 0.475 g of TiO2 membrane.	140
Figure 4.29	The light intensity profiles within the photoreactor operated with QCL and QLC arrangements	141
Figure 4.30	Effect of pH on zeta potential of different coated amounts of Nf/TiO2 suspensions.	144
Figure 4.31	Adsorption of Nafion on TiO2 surface.	145
Figure 4.32	Effect of pH on zeta potential of dyes adsorbed on TiO2 and Nf/TiO2 suspensions.	146
Figure 4.33	Effect of pH on the adsorption amounts of dyes on TiO2.	147

Figure 4.34
Temporal distribution of R22 for the photocatalytic reaction by TiO2 at different pH.	150
Figure 4.35	Effect of pH on the apparent pseudo first-order decomposition rate constants.
151





List of tables
		Page
Table 2.1	Classification of solids according to their energy gap EG and carrier density N at room temperature.	5
Table 2.2	Basic properties of anatase and rutile structures of TiO2.	7
Table 3.1	Absolute maximum ratings and optical-electrical characteristics of B5-437-CVD.	79
Table 4.1	The key parameters of photoelectrochemical properties, optical spectroscopy, electrokinetic properties, and their relation with the decomposition of dyes in photocatalytic membrane reactors.	92
Table 4.2	The apparent pseudo-first order rate constant calculated at various operation parameters	129

                                

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