改性纳米二氧化钛薄膜制备及其在模拟海水中光生阴极保护性能研究
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摘要
随着功能材料高新领域的迅猛发展,纳米二氧化钛薄膜独特的光电转换效应在金属腐蚀防护方面表现出诱人的应用前景,正日益受到人们的重视。当二氧化钛薄膜材料与金属基体相接时,受到能量大于其能隙光子的照射下,二氧化钛价带电子激发至导带,形成电子—空穴对,负电电子由导带进入金属基体,使金属的电极电位降低至不发生腐蚀的阴极保护区,可作为非牺牲性的光阴极保护材料,实现对海洋金属材料腐蚀防护。二氧化钛的光阴极保护性能取决于其光电效率,其中选择合适的掺杂改性以得到高的光电转换效率和具有可见光响应的薄膜电极材料是人们最为关注的问题。
本论文以钛酸四丁酯为前驱体,二乙醇胺为抑制剂,采用溶胶凝胶法在中性条件下在不锈钢基体上制备纳米二氧化钛薄膜,通过在制备过程中添加聚乙二醇(PEG)制备改性型二氧化钛薄膜；以硝酸铁和尿素分别作为引入铁源和氮源来制备Fe掺杂和N掺杂二氧化钛薄膜,以期望提高纳米二氧化钛薄膜材料的光电转换效率和拓宽光电响应范围。论文中采用激光粒度分析和Zeta电位来测试改性对二氧化钛溶胶性能的影响；采用X射线衍射(XRD)、热分析(DTA-TG)、红外吸收(IR)、扫描电镜(SEM)等测试方法对所制备二氧化钛晶体的物相结构、性能和表面形貌进行了表征；采用紫外可见透射光谱、荧光光谱对所制二氧化钛薄膜进行光物理性能测试；以改性二氧化钛薄膜为工作电极,利用二氧化钛半导体特性和Mott-Schottky理论对在模拟海水界面参数如二氧化钛的平带电位、空间电荷层的载流子浓度以及空间电荷层宽度进行测试；最后在模拟海水体系采用光电联用体系进行循环伏安法(U-I曲线)、开路电位测试、交流阻抗谱和极化曲线测试,综合评价其对不锈钢基体光生阴极保护性能。
(1)通过在二氧化钛溶胶中添加PEG制备改性型二氧化钛。实验表明添加PEG减小二氧化钛溶胶颗粒尺寸,促进溶胶中有序网络形成。PEG的添加使二氧化钛晶型转变温度向低温方向移动,有利于相变过程进行,改性后二氧化钛薄膜质量良好具有多孔结构。该多孔结构增加了光线在薄膜表面的反射次数,提高了薄膜对光的吸收和利用率。多孔结构增大了薄膜与电解液的接触面积,同时有利于电极/电解质溶液界面的光生载流子传输,从而大大提高了光生电荷的分离效率。在模拟海水体系光电性能测试中,改性后二氧化钛薄膜光电性能显著提高。实验中对热处理温度、多孔结构等因素综合分析,确定500℃热处理温度以下,PEG最佳添加量为1g/100mL。
(2)铁掺杂二氧化钛有利于形成粒径较小,性能稳定的二氧化钛溶胶粒子。铁掺杂后有利于二氧化钛相变过程进行,铁掺杂使纳米二氧化钛膜结晶度良好,膜表面更均一和致密,晶粒尺寸减小。通过光学性能分析,铁掺杂使二氧化钛吸收边蓝移,对可见光区响应变化不明显；掺杂铁可作为浅俘获位,有效地抑制光生电子和空穴的复合,能有效提高光电转换效率。掺铁二氧化钛薄膜在模拟海水中Mott-Schottky曲线测试分析,铁掺杂二氧化钛薄膜双电层是p-型微区和n-型微区共存,该p-n结电场有利于光电流的产生。在模拟海水中光电实验证实这一结论,掺铁二氧化钛薄膜电极有效地增大光电流,掺铁二氧化钛对光生电子驱动力的增加,增强了二氧化钛薄膜电极对不锈钢基体的光生阴极保护作用。综合对不同掺铁量的性能比较,在相同的测试条件下,掺铁量最佳值为Fe/Ti摩尔比0.5%。
(3)氮掺杂二氧化钛有利于形成粒径较小,性能稳定的二氧化钛溶胶粒子。氮掺杂对二氧化钛晶型转化未产生明显变化。氮掺杂纳米二氧化钛膜结晶度良好,晶粒尺寸减小,薄膜质量有明显改善。通过光学性能分析,氮掺杂使吸收边红移；在可见光范围内有明显吸收。在可见光光源下,光电化学测试表明,掺氮后改变了电子跃迁能级,使氮掺杂二氧化钛仍有电子跃迁,光生载流子产生阳极光电流,能对不锈钢基体进行有效的光生阴极保护。但氮掺杂量存在最佳量,实验证明最佳氮掺杂量为N/Ti的摩尔比为20%。
As the functional material develop rapidly. Nano-structured semiconductors are of vital importance on the development of functional material.The photoelective performance are essential properties for this king of materials. The investigation of titanium dioxide for photogenerated cathode protection of metals has received great attention. In addition, if illuminated titanium dioxide is in contact with metal, electrons are injected from the semiconductor to the metal via the conduction band. As a result, the potential of the metal will be shifted in the negative direction to the flatland potential of titanium dioxide. If the potential is more negative than the potential at which the metal beings to oxidize, the metal can be protected from corrosion. So titanium dioxide can realize corrosion protection of the marine material as non-sacrificial protective material. The photocathodic protection performance of titanium dioxide is dependent on the photoelectrochemical efficiency, which select the appropriate doped in order to obtain high photoelectric conversion efficiency and visible-light response of the electrode material is of the greatest concern.
In this dissertation, Ti (OC4H9)4 was used as precursor, C4H11NO2 was used as inhibitors to prepared nano-titanium dioxide film on the stainless steel substrate by neutral sol-gel method. In the preparation process, Modified titanium dioxide thin films were prepared by adding PEG; respectively, iron-doped titanium dioxide thin films were prepared with ferric nitrate as iron source, nitrogen-doped titanium dioxide thin films were prepared with urea as nitrogen source. Modified and doped titanium dioxide thin films were prepared to look forward to enhance photoelectric conversion efficiency and to broaden the scope of photoelectric response. This paper used laser particle size analysis and Zeta potential to test the modification on the properties of titanium dioxide sol; the crystal structure, properties and surface morphology of modified titanium dioxide were characterized using X-ray diffraction (XRD), thermal analysis (DTA-TG), infrared absorption (IR), and scanning electron microscopy (SEM). The photophysical properties of samples were tested using UV-visible transmission (UV-vis) and fluorescence spectra; Using modified TiO2 thin film as the working electrode, titanium dioxide films interface parameters were calculated in simulated seawater such as flat-band potential, space charge layers carrier concentration as well as space-charge layer width by titanium dioxide semiconductor properties and Mott-Schotty theory. Finally photoelectric propertie of modified titanium dioxide is studied in a simulated seawater using cyclic voltammetry (U-I curve), open circuit potential test, Electrochemical Impedance Spectroscopy(EIS) and polarization curves with photoelectrochemical cell, comprehensive evaluation of its stainless steel substrate photogenerated protection performance.
(1) Modified titanium dioxide, which is prepared titanium dioxide sol by adding PEG experiments showed that modification reduced the particle size and increase networking structure of titanium dioxide sol, made titanium dioxide crystal transition temperature to lower temperature direction and of good quality films were successfully prepared with porous structure of titanium dioxide thin films. The porous structure increased light reflection times in the film surface to improve light absorption and utilization. The porous structure of the film increased the contact area, at the same time was conducived to photogenerated-carrier transmission, which greatly improved the efficiency of photoinduced charge separation. Photoelectrochemical properties showed that the photoelectrochemical performance of modified titanium dioxide thin-film was improved significantly in simulated seawater. Comprehensive analysis conclusion of heat treatment temperature, porous structure, Best modified experimental conditions are below 500℃,1g PEG addition.
(2)Fe-doped titanium dioxide was conducived to form small, stable particles sol. Fe-doped titanium dioxide was conducived to crystal transfer process, Fe-doped nano-titanium dioxide film decrease the grain size and crystallization excellent, film surface was more uniform and dense, Through optical performance analysis, absorption spectra of Fe-doped titanium dioxide turned red-shift; Fe-doped titanium dioxide can inhibit the photo-generated electron and hole recombination. By the Mott-Schottky curves analysis, Fe-doped titanium dioxide thin-film double-layer exist p-type and n-type micro-district co-exist; the electric field of the p-n junction is conducive to photocurrent generation in simulated sea water. Photoelectrochemical experiments confirm this conclusion, Fe-doped titanium dioxide thin film increase effectively the photocurrent and photogenerated electrons driving force, enhanced photogenerated cathode protection to stainless steel in simulated seawater. At the same test conditions, the amount of the best value is Fe/Ti ratio of 0.5% by synthesis of different quantity of the above-mentioned and comparation of properties of different Fe-doped.
(3) N-doped titanium dioxide is conducive to form small, stable particles sol.. N doping transformation of crystalline titanium dioxide, N-doped nano-crystalline titanium dioxide film decreases the grain size and improvement significant film quality. Through optical performance analysis, Absorption spectra appear red-shift; in the context of significant absorption of visible light. Photoelectrochemical tests showed that in the visible light source, the, N-doped titanium dioxide samples had still electronic transition because N-doped changed after the electronic transition energy level, optical-carrier produced anodic photocurrent, can be effective on stainless steel substrate light cathodic protection. There exists an optimum amount of nitrogen doping. Experimental prove that the optimum N/ Ti ratio of the visible light photoelectric is 20%.
本论文以钛酸四丁酯为前驱体,二乙醇胺为抑制剂,采用溶胶凝胶法在中性条件下在不锈钢基体上制备纳米二氧化钛薄膜,通过在制备过程中添加聚乙二醇(PEG)制备改性型二氧化钛薄膜；以硝酸铁和尿素分别作为引入铁源和氮源来制备Fe掺杂和N掺杂二氧化钛薄膜,以期望提高纳米二氧化钛薄膜材料的光电转换效率和拓宽光电响应范围。论文中采用激光粒度分析和Zeta电位来测试改性对二氧化钛溶胶性能的影响；采用X射线衍射(XRD)、热分析(DTA-TG)、红外吸收(IR)、扫描电镜(SEM)等测试方法对所制备二氧化钛晶体的物相结构、性能和表面形貌进行了表征；采用紫外可见透射光谱、荧光光谱对所制二氧化钛薄膜进行光物理性能测试；以改性二氧化钛薄膜为工作电极,利用二氧化钛半导体特性和Mott-Schottky理论对在模拟海水界面参数如二氧化钛的平带电位、空间电荷层的载流子浓度以及空间电荷层宽度进行测试；最后在模拟海水体系采用光电联用体系进行循环伏安法(U-I曲线)、开路电位测试、交流阻抗谱和极化曲线测试,综合评价其对不锈钢基体光生阴极保护性能。
(1)通过在二氧化钛溶胶中添加PEG制备改性型二氧化钛。实验表明添加PEG减小二氧化钛溶胶颗粒尺寸,促进溶胶中有序网络形成。PEG的添加使二氧化钛晶型转变温度向低温方向移动,有利于相变过程进行,改性后二氧化钛薄膜质量良好具有多孔结构。该多孔结构增加了光线在薄膜表面的反射次数,提高了薄膜对光的吸收和利用率。多孔结构增大了薄膜与电解液的接触面积,同时有利于电极/电解质溶液界面的光生载流子传输,从而大大提高了光生电荷的分离效率。在模拟海水体系光电性能测试中,改性后二氧化钛薄膜光电性能显著提高。实验中对热处理温度、多孔结构等因素综合分析,确定500℃热处理温度以下,PEG最佳添加量为1g/100mL。
(2)铁掺杂二氧化钛有利于形成粒径较小,性能稳定的二氧化钛溶胶粒子。铁掺杂后有利于二氧化钛相变过程进行,铁掺杂使纳米二氧化钛膜结晶度良好,膜表面更均一和致密,晶粒尺寸减小。通过光学性能分析,铁掺杂使二氧化钛吸收边蓝移,对可见光区响应变化不明显；掺杂铁可作为浅俘获位,有效地抑制光生电子和空穴的复合,能有效提高光电转换效率。掺铁二氧化钛薄膜在模拟海水中Mott-Schottky曲线测试分析,铁掺杂二氧化钛薄膜双电层是p-型微区和n-型微区共存,该p-n结电场有利于光电流的产生。在模拟海水中光电实验证实这一结论,掺铁二氧化钛薄膜电极有效地增大光电流,掺铁二氧化钛对光生电子驱动力的增加,增强了二氧化钛薄膜电极对不锈钢基体的光生阴极保护作用。综合对不同掺铁量的性能比较,在相同的测试条件下,掺铁量最佳值为Fe/Ti摩尔比0.5%。
(3)氮掺杂二氧化钛有利于形成粒径较小,性能稳定的二氧化钛溶胶粒子。氮掺杂对二氧化钛晶型转化未产生明显变化。氮掺杂纳米二氧化钛膜结晶度良好,晶粒尺寸减小,薄膜质量有明显改善。通过光学性能分析,氮掺杂使吸收边红移；在可见光范围内有明显吸收。在可见光光源下,光电化学测试表明,掺氮后改变了电子跃迁能级,使氮掺杂二氧化钛仍有电子跃迁,光生载流子产生阳极光电流,能对不锈钢基体进行有效的光生阴极保护。但氮掺杂量存在最佳量,实验证明最佳氮掺杂量为N/Ti的摩尔比为20%。
As the functional material develop rapidly. Nano-structured semiconductors are of vital importance on the development of functional material.The photoelective performance are essential properties for this king of materials. The investigation of titanium dioxide for photogenerated cathode protection of metals has received great attention. In addition, if illuminated titanium dioxide is in contact with metal, electrons are injected from the semiconductor to the metal via the conduction band. As a result, the potential of the metal will be shifted in the negative direction to the flatland potential of titanium dioxide. If the potential is more negative than the potential at which the metal beings to oxidize, the metal can be protected from corrosion. So titanium dioxide can realize corrosion protection of the marine material as non-sacrificial protective material. The photocathodic protection performance of titanium dioxide is dependent on the photoelectrochemical efficiency, which select the appropriate doped in order to obtain high photoelectric conversion efficiency and visible-light response of the electrode material is of the greatest concern.
In this dissertation, Ti (OC4H9)4 was used as precursor, C4H11NO2 was used as inhibitors to prepared nano-titanium dioxide film on the stainless steel substrate by neutral sol-gel method. In the preparation process, Modified titanium dioxide thin films were prepared by adding PEG; respectively, iron-doped titanium dioxide thin films were prepared with ferric nitrate as iron source, nitrogen-doped titanium dioxide thin films were prepared with urea as nitrogen source. Modified and doped titanium dioxide thin films were prepared to look forward to enhance photoelectric conversion efficiency and to broaden the scope of photoelectric response. This paper used laser particle size analysis and Zeta potential to test the modification on the properties of titanium dioxide sol; the crystal structure, properties and surface morphology of modified titanium dioxide were characterized using X-ray diffraction (XRD), thermal analysis (DTA-TG), infrared absorption (IR), and scanning electron microscopy (SEM). The photophysical properties of samples were tested using UV-visible transmission (UV-vis) and fluorescence spectra; Using modified TiO2 thin film as the working electrode, titanium dioxide films interface parameters were calculated in simulated seawater such as flat-band potential, space charge layers carrier concentration as well as space-charge layer width by titanium dioxide semiconductor properties and Mott-Schotty theory. Finally photoelectric propertie of modified titanium dioxide is studied in a simulated seawater using cyclic voltammetry (U-I curve), open circuit potential test, Electrochemical Impedance Spectroscopy(EIS) and polarization curves with photoelectrochemical cell, comprehensive evaluation of its stainless steel substrate photogenerated protection performance.
(1) Modified titanium dioxide, which is prepared titanium dioxide sol by adding PEG experiments showed that modification reduced the particle size and increase networking structure of titanium dioxide sol, made titanium dioxide crystal transition temperature to lower temperature direction and of good quality films were successfully prepared with porous structure of titanium dioxide thin films. The porous structure increased light reflection times in the film surface to improve light absorption and utilization. The porous structure of the film increased the contact area, at the same time was conducived to photogenerated-carrier transmission, which greatly improved the efficiency of photoinduced charge separation. Photoelectrochemical properties showed that the photoelectrochemical performance of modified titanium dioxide thin-film was improved significantly in simulated seawater. Comprehensive analysis conclusion of heat treatment temperature, porous structure, Best modified experimental conditions are below 500℃,1g PEG addition.
(2)Fe-doped titanium dioxide was conducived to form small, stable particles sol. Fe-doped titanium dioxide was conducived to crystal transfer process, Fe-doped nano-titanium dioxide film decrease the grain size and crystallization excellent, film surface was more uniform and dense, Through optical performance analysis, absorption spectra of Fe-doped titanium dioxide turned red-shift; Fe-doped titanium dioxide can inhibit the photo-generated electron and hole recombination. By the Mott-Schottky curves analysis, Fe-doped titanium dioxide thin-film double-layer exist p-type and n-type micro-district co-exist; the electric field of the p-n junction is conducive to photocurrent generation in simulated sea water. Photoelectrochemical experiments confirm this conclusion, Fe-doped titanium dioxide thin film increase effectively the photocurrent and photogenerated electrons driving force, enhanced photogenerated cathode protection to stainless steel in simulated seawater. At the same test conditions, the amount of the best value is Fe/Ti ratio of 0.5% by synthesis of different quantity of the above-mentioned and comparation of properties of different Fe-doped.
(3) N-doped titanium dioxide is conducive to form small, stable particles sol.. N doping transformation of crystalline titanium dioxide, N-doped nano-crystalline titanium dioxide film decreases the grain size and improvement significant film quality. Through optical performance analysis, Absorption spectra appear red-shift; in the context of significant absorption of visible light. Photoelectrochemical tests showed that in the visible light source, the, N-doped titanium dioxide samples had still electronic transition because N-doped changed after the electronic transition energy level, optical-carrier produced anodic photocurrent, can be effective on stainless steel substrate light cathodic protection. There exists an optimum amount of nitrogen doping. Experimental prove that the optimum N/ Ti ratio of the visible light photoelectric is 20%.
引文
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