TiO_（2-x）N_x/NiO双层薄膜的制备及光电化学特性
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摘要
本论文以开发一种新型光电功能电极材料为目标,分别采用磁控溅射法、溶胶凝胶法先在导电玻璃(ITO)上制备N掺杂TiO_2薄膜,然后通过一种简便的化学沉积法(CBD)在TiO_(2-x)N_x薄膜上沉积一层多孔结构的NiO薄膜,构建出TiO_(2-x)N_x/NiO双层薄膜,采用XRD、SEM、XPS、紫外可见吸收光谱和电化学测试等对薄膜的微观结构、光电致色和光电化学储能等特性进行了研究。
以金属钛为靶材、O_2/N_2/Ar混合气为溅射气体,在ITO玻璃表面磁控溅射一层薄膜,再经300-500℃退火处理制备了氮掺杂TiO_2薄膜。研究表明,400℃退火处理的氮掺杂TiO_2薄膜具有最高的光电流响应,TiO_(2-x)N_x/NiO双层薄膜具有明显的光电致色特性,经氙灯照射1h后,薄膜从无色变成棕色,500nm波长处光透过率从79.0%下降至12.6%。光充电后,电极在100nA下放电时间为11h。
利用溶胶凝胶法在ITO表面制备一层薄膜,再经300-500℃退火处理制备了氮掺杂TiO_2薄膜。研究表明,所制备的ITO/TiO_(2-x)N_x/NiO双层薄膜具有明显的光电致色特性,500℃制备的氮掺杂TiO_2薄膜具有较高的光电流响应,经氙灯照射1h后,薄膜从无色变成棕色,400nm波长处光透过率从83.5%下降至32.9%。光充电后,电极在100nA下放电时间为4.2h。
此外,先在导电玻璃(ITO)表面磁控溅射一层TiN薄膜,再经300-500℃空气氛中退火处理制备了氮掺杂TiO_2薄膜。在相同的光照下,其光电流为纯TiO_2薄膜的4倍,由其构成的ITO/TiO_(2-x)N_x/NiO双层薄膜具有明显的光电致色特性。经氙灯照射3h后,薄膜从无色变成棕色,400nm波长处光透过率从71.4%下降至26.5%,在100nA下放电时间为18h。光充电后,电极在100nA下放电时间为18h。
In order to develop a new kind of photo-electric function materials, N-dopedTiO_2 thin films were synthesized on indium-tin oxide (ITO) conducting glass substrateby DC reactive magnetron sputtering and sol-gel method, respectively. Then highporous NiO was deposited onto the N-doped TiO_2 layer by chemical bath deposition(CBD) to obtain TiO_(2-x)N_x/NiO bilayer thin films electrode. The microstructure, photoelectrochromicproperties and photoelectrochemical energy storage ability of theTiO_(2-x)N_x/NiO thin film were investigated by XRD、SEM、XPS、UV-vis adsorptionspectra and eletrochemial test technology.
N-doping TiO_2 films were prepared on ITO conducting glass by dc-reactivemagnetron sputtering using Ti target in O2+N2/Ar gas mixture in combination with afollowing heat-treatment at 300-500℃. The results showed that the TiO_(2-x)N_x filmannealed at 400℃showed the highest photocurrent response under Xe lightirradiation. The bilayer films were irradiated with Xe lamps at a closed circuit for 1 h,the color of the TiO_(2-x)N_x/NiO electrode turned from colorless to brown, and thetransmittance varied from 79.0% to 12.6% at 500 nm. After photo-charging, thedischarge current was controlled at 100 nA and the duration time was about 11 h.And also, the N-doped TiO_2 film was synthesized on indium-tin oxide (ITO)conducting glass substrate by sol-gel method. As compared to the undoped TiO_2, thesynthesized N-doped TiO_2 had visible light photoresponse and exhibited a significantincrease in the photocurrent under Xe light irradiation. It was found that theTiO_(2-x)N_x/NiO electrode exhibited excellent photoelectrochromic properties. After 2 hirradiation, the color of the TiO_(2-x)N_x/NiO electrode changed from colorless to brown,and the transmittance varied from 83.5% to 32.9% at 400 nm. The discharge currentwas controlled at 100 nA and the duration time was about 4.2 h.
Additionally, TiN thin films were prepared on ITO by dc reactive magnetronsputtering technique and then directly annealed in 300-500℃in air for thepreparation of TiO_(2-x)N_x thin film electrode. Under the same light irradiation, thephotocurrent of the TiO_(2-x)N_x electrode is four times larger than that of pure TiO_2 electrode. The as-fabricated TiO_(2-x)N_x/NiO electrode exhibited a noticeablephotoelectrochromism. After 3 h irradiation, the transmittance varies from 71.4% to26.5% at 400 nm. The discharge current was controlled at 100 nA and the durationtime was about 18 h.
以金属钛为靶材、O_2/N_2/Ar混合气为溅射气体,在ITO玻璃表面磁控溅射一层薄膜,再经300-500℃退火处理制备了氮掺杂TiO_2薄膜。研究表明,400℃退火处理的氮掺杂TiO_2薄膜具有最高的光电流响应,TiO_(2-x)N_x/NiO双层薄膜具有明显的光电致色特性,经氙灯照射1h后,薄膜从无色变成棕色,500nm波长处光透过率从79.0%下降至12.6%。光充电后,电极在100nA下放电时间为11h。
利用溶胶凝胶法在ITO表面制备一层薄膜,再经300-500℃退火处理制备了氮掺杂TiO_2薄膜。研究表明,所制备的ITO/TiO_(2-x)N_x/NiO双层薄膜具有明显的光电致色特性,500℃制备的氮掺杂TiO_2薄膜具有较高的光电流响应,经氙灯照射1h后,薄膜从无色变成棕色,400nm波长处光透过率从83.5%下降至32.9%。光充电后,电极在100nA下放电时间为4.2h。
此外,先在导电玻璃(ITO)表面磁控溅射一层TiN薄膜,再经300-500℃空气氛中退火处理制备了氮掺杂TiO_2薄膜。在相同的光照下,其光电流为纯TiO_2薄膜的4倍,由其构成的ITO/TiO_(2-x)N_x/NiO双层薄膜具有明显的光电致色特性。经氙灯照射3h后,薄膜从无色变成棕色,400nm波长处光透过率从71.4%下降至26.5%,在100nA下放电时间为18h。光充电后,电极在100nA下放电时间为18h。
In order to develop a new kind of photo-electric function materials, N-dopedTiO_2 thin films were synthesized on indium-tin oxide (ITO) conducting glass substrateby DC reactive magnetron sputtering and sol-gel method, respectively. Then highporous NiO was deposited onto the N-doped TiO_2 layer by chemical bath deposition(CBD) to obtain TiO_(2-x)N_x/NiO bilayer thin films electrode. The microstructure, photoelectrochromicproperties and photoelectrochemical energy storage ability of theTiO_(2-x)N_x/NiO thin film were investigated by XRD、SEM、XPS、UV-vis adsorptionspectra and eletrochemial test technology.
N-doping TiO_2 films were prepared on ITO conducting glass by dc-reactivemagnetron sputtering using Ti target in O2+N2/Ar gas mixture in combination with afollowing heat-treatment at 300-500℃. The results showed that the TiO_(2-x)N_x filmannealed at 400℃showed the highest photocurrent response under Xe lightirradiation. The bilayer films were irradiated with Xe lamps at a closed circuit for 1 h,the color of the TiO_(2-x)N_x/NiO electrode turned from colorless to brown, and thetransmittance varied from 79.0% to 12.6% at 500 nm. After photo-charging, thedischarge current was controlled at 100 nA and the duration time was about 11 h.And also, the N-doped TiO_2 film was synthesized on indium-tin oxide (ITO)conducting glass substrate by sol-gel method. As compared to the undoped TiO_2, thesynthesized N-doped TiO_2 had visible light photoresponse and exhibited a significantincrease in the photocurrent under Xe light irradiation. It was found that theTiO_(2-x)N_x/NiO electrode exhibited excellent photoelectrochromic properties. After 2 hirradiation, the color of the TiO_(2-x)N_x/NiO electrode changed from colorless to brown,and the transmittance varied from 83.5% to 32.9% at 400 nm. The discharge currentwas controlled at 100 nA and the duration time was about 4.2 h.
Additionally, TiN thin films were prepared on ITO by dc reactive magnetronsputtering technique and then directly annealed in 300-500℃in air for thepreparation of TiO_(2-x)N_x thin film electrode. Under the same light irradiation, thephotocurrent of the TiO_(2-x)N_x electrode is four times larger than that of pure TiO_2 electrode. The as-fabricated TiO_(2-x)N_x/NiO electrode exhibited a noticeablephotoelectrochromism. After 3 h irradiation, the transmittance varies from 71.4% to26.5% at 400 nm. The discharge current was controlled at 100 nA and the durationtime was about 18 h.
引文
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