溶胶—凝胶法制备纳米二氧化钛薄膜及其光致特性研究
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摘要
本论文主要对纳米二氧化钛光催化与超亲水性薄膜的制各及性能研究和过
渡金属掺杂对纳米二氧化钛薄膜的微观结构、光致特性、电化学性质及在酸碱条
件下的稳定性等进行了研究。薄膜的制各主要由两部分组成:1.室温下Si02-T
iO2 复合薄膜的制各;2.掺杂Sb的纳米二氧化钛薄膜的制备。
1.在纳米二氧化钛薄膜的室温制备与研究中,用正硅酸乙脂和四氯化钛分
别作为二氧化硅和二氧化钛的前驱体,室温下采用溶胶.凝胶法在玻璃基板上制
备厚度约为100nm均匀、透明的纳米Si02-Fi02复合薄膜。
通过xPs对薄膜表面及近表面元素的化学态的研究发现,Ti在薄膜表面及
近表面不仅以TI4+形式存在。同时也存在少量的Ti3+。经一定时间的紫外光照射
后,Ti2p3/2谱线发生了明显的变化,拟合结果显示:紫外光长时间(24h)照射后,
Ti3+峰明显增强;从Ols峰形也可看到光照前后有着显著的区别:紫外光照射后,
相对于Ti3+的Ols峰明显增强,上述结果说明紫外光照射后部分Ti4+转变成了
Ti3+。
XRD研究表明,该薄膜中的Ti02主要以锐钛矿形式存在,晶粒大小为
14— 20nm。薄膜的表面形貌及不同的温度处理对Ti02颗粒大小的影响通过AFM
进行表征。由于Sio2溶胶的作用,室温固化及200.C热处理l小时后的薄膜表面
呈板块状结构,其颗粒尺寸约为0.2um,经450。C小时的热处理后,表面颗粒
尺寸减小到50一100nm。
在室温下制备、固化的薄膜具有良好的光致超亲水性、光催化能力和较高的
可见光透射率,且薄膜厚度均匀。无论热处理与否,样品经254nm紫外光照射
40min后对水的接触角均显著减小,接近于O。:在停止光照24小时后,接触角
仍为15— 3。,即能较长时间保持其亲水性。温度低于200℃的热处理,对薄膜的
光致特性基本没有影响,两种不同温度(室温和200。C)下处理的薄膜对罗丹明B
和亚甲基蓝水溶液的一级反应速率常数k分别为O.0229h-1.cm-2、0.0244h-1cm-2、
0.0220 h-1cm-2和0.0233 h-1-cm-2,即室温固化的薄膜与较低温度(<=200。C)处理过
的薄膜对罗丹明B和亚甲基蓝的降解没有明显的差异,较低温度处理并不影响
薄膜的光催化性。高温(>=450℃)处理1小时后,薄膜的光催化性能明显降低,
对罗丹明B和亚甲基蓝水溶液的一级反应速率常数k分别为O.0108 H-1.cm-2和
0.0097 h-1.cm-2。同时,随着厚度的增加,薄膜的光催化性能也相应提高。
通过沸水处理方法研究了不同温度下处理后薄膜与基板的附着力性能。室温
固化及200℃下处理的薄膜经沸水煮20分钟后仍具有良好的超亲水性。在波长
为254nm,功率密度为200gW/cm2的紫外光下照射40min后,薄膜对水的接触
角小于1。,表明薄膜与基板有良好的附着力及稳定性。
2.通过溶胶.凝胶法制各的掺杂sb的纳米二氧化钛光催化薄膜,在可见光
区的平均透射率大于80%。掺入适量的Sb后,由于Sb替代了Ti02的部分Ti,
形成sb-O-Ti结构,改变了Ti02的晶格结构参数(a,c),进而提高了薄膜的结晶效
率,使薄膜中锐钛矿结构的Ti02:Sb含量明显提高。但掺入过量的sb后,由于
sb相互间作用,形成Sb-Sb键,降低了晶格的有序度,使薄膜的结晶效率降低。
实验表明,Sb的最佳掺杂含量为0.2%,此时薄膜的结晶效率最高。
掺杂sb后明显提高了薄膜的光电转换效率,当掺杂含量为0 2%时,用254nm
紫外光作光源(功率密度为375uw·cm-2)时.其产生的光电流密度可达
42 49uA.cm-2,是用同种方法制备的纯Ti02薄膜电极的近ll倍。
用电化学方法研究了紫外光照射下Ti02薄膜电极表面Ti3+的产生与积累,
并提出了Tio2光致特性产生过程中的两个过程:即光电流和Ti3+产生的快过程
和Ti3+积累的慢过程,进而对Ti02薄膜光致亲水性的机理进行了一定的探讨。
含0.2%Sb的薄膜对亚甲基蓝具有较高分解性能和良好的光致亲承性。对亚
甲基蓝溶液光催化分解的一级反应速率常数k为0.078h-1.cm-2,是未掺杂的纯
Ti02薄膜在相同条件下的反应常数(0.040 h-1cm-2)的近2倍。经90-95uw的
254nm紫外光照射l小时后,掺杂0.2%的薄膜对水的接触角趋于00,表现出良
好的光致亲水性。
Ti02 Sb光催化薄膜在酸性条件下具有较强的的附着力。掺0.2%sb的薄膜
在0.2M的盐酸中浸泡48小时或在沸水中处理40分钟后对亚甲基蓝的光催化反
应常数分别为0.0338 h-1. cm-2和O.0283 h-1.cm-2,仍具有较强的光催化活性:经紫
外光照射15分钟后,水接触角均接近于0。。
电化学分析结果表明,掺杂sb后薄膜的稳定性得到显著提高,而未掺杂的
纯Ti02薄膜在盐酸中并不稳定。
最后还对用直流磁控溅射法制备锐钛矿结构的Ti02-xNx薄膜进行了初步的
探讨。结果表明,用磁控溅射制各的TiN薄膜,经一定时间的湿氧氧化后形成锐
钛矿结构的Ti02-xNx薄膜。该薄膜具有很好的光催化和光致亲水性能,对亚甲基
蓝的反应速率常数k达到0.107h-1.cm-2:经254nm紫外光照射30分钟后,薄膜
对水的接触角趋于0。:吸收光谱表明,TiO2-xNx薄膜的吸收边为460nm,对应的
禁带宽度为2.70eV。
While the annoseale photocatalyfie activity and the photo— induced properties of
titanium dioxide thin films were characterized,the effect of transitinnal metal Sb
doped into titanium dioxide thin films upon the microstructuse,photo-indeced
charaetars,electrochemical pmpertias and the stabilization in acid or alkaline
environment were studied in this paper.The preparation of the thin films includes two
parts One is the preparation of Si02一Ti02 composite thin films at room temperature
in air.Another is the deposition of Sb doped nanoscalc Ti02 thin films
1.In the section of photocatalytic Ti02 thin films were prepared at room
temperature in air,Ethyl delicate((C2Hs)4Si04)and TiCl4 were used as the precursor
0f Si02 and Ti02 respectively.The Nanoscale silicon dioxide and titanium dioxide
composite(si02-Tio2)thin films wem uniform and transparent with the thickness of
about 100nm were prepared.
Thc chemieal states of the elements on the surface or near the surface were
measured by XPS.The msults indieated that the Ti on/nearthe surface of the thin
films existed not only as Ti4+ but also aS Ti3+.After ultraviolet(UV)irradiation for
some time,the spectra of Ti2p3/2 changed obviously.Fitted results showed that the
spectra of Ti3+ risen drastically after UV irradiation for long time(about 24h)
accompaniedbyan up-forward tendency in the intensity of Ols spectra corresponded
to Ti3+. These illustrated that part of the Ti4+was changed to Ti3+ after UV irradiation
The crystalline stnlctore ofthe Si02-Ti02 thin films were characterized by X-ray
diffraction(XRD).The crystalline structure of the Ti02 in the Si02-Ti02 thin films
was in a majority of anatase state with the crystallite size of 14— 20nm.The AFM was
used to study the morphology of the thin films annealed at different temperature and
it effected onthe crystalline size of titanium dioxide For Si02 effect,the surfaces of
the samples treated at below 200。C were lumpish strucure with grain size of 0.2pm.
ARer treated at 450℃ for 1 hour,the grain size reduced to 50-100mn.
The samples prepared at room temperature had excellent photo-induced
superhydrophilicity and superior photocatalysis.After ander UV irradiation for 40min,
the contact angles for all samples were drastically reduced to 0。and it also was
between 1.5。t0 3。after storage in dark for 24 hour.There was few or none effcct on
photocatalysis of the thin films heat treated below 200。C,the staircase reaction speed
constant(k) of?
0.0220 h-1·cml-2 and 0.0233 h-1.cm-2.respectively.But the photocatalysis of thin films
treated at or over 450℃ for l hour was reduced obviously,which staircasereaction
speed constant(k)was about 0.0108h-1.cm-2 and 0.0097 h-1.cm-2.
The adherence between the thin films treated at different temperature and
substrate was characterized byboiling water trtatment The samplestreated below
200℃showed superior photo-induced supethydrophilicity after treated in boiling
water for 20min.The contact angle was less than 1。under UV(k=254nm,
P=200pW/cm2)irradiated for 40min.It illuminated that the thin films had strength
adherence and stabilization
The Ti02:Sb thin films with thc transparent larger than 80%were prepared by
dip-coating sol-gel method.After doping proper amount of Sb,a part of Ti4+ in Tio2
were replaced by Sb3+ and Sb combined with the O in Ti02 to form the structure of
Sb-O-Ti,the crystal lattice parameters a and c were changed,and the crystalline rate
of the Tio2 in the thin films is enhanced so that the content of anatasc Ti02:Sb were
increased.When the concentration of dopant Sb was excessive.Sb interacted wim
itself to form Sb-Sb structure,ruining the original anatase structure.So the
optimization content of Sb is aboutO.2%.
The photoelectric conversion character of TiO2 thin films are improved after Sb
doping in it.When the content of Sb reached 0.2‰the photocurrent density was.
about 42.49uA·cm-2 that was 11 times to the non-doped Ti02 thin films subjecting
渡金属掺杂对纳米二氧化钛薄膜的微观结构、光致特性、电化学性质及在酸碱条
件下的稳定性等进行了研究。薄膜的制各主要由两部分组成:1.室温下Si02-T
iO2 复合薄膜的制各;2.掺杂Sb的纳米二氧化钛薄膜的制备。
1.在纳米二氧化钛薄膜的室温制备与研究中,用正硅酸乙脂和四氯化钛分
别作为二氧化硅和二氧化钛的前驱体,室温下采用溶胶.凝胶法在玻璃基板上制
备厚度约为100nm均匀、透明的纳米Si02-Fi02复合薄膜。
通过xPs对薄膜表面及近表面元素的化学态的研究发现,Ti在薄膜表面及
近表面不仅以TI4+形式存在。同时也存在少量的Ti3+。经一定时间的紫外光照射
后,Ti2p3/2谱线发生了明显的变化,拟合结果显示:紫外光长时间(24h)照射后,
Ti3+峰明显增强;从Ols峰形也可看到光照前后有着显著的区别:紫外光照射后,
相对于Ti3+的Ols峰明显增强,上述结果说明紫外光照射后部分Ti4+转变成了
Ti3+。
XRD研究表明,该薄膜中的Ti02主要以锐钛矿形式存在,晶粒大小为
14— 20nm。薄膜的表面形貌及不同的温度处理对Ti02颗粒大小的影响通过AFM
进行表征。由于Sio2溶胶的作用,室温固化及200.C热处理l小时后的薄膜表面
呈板块状结构,其颗粒尺寸约为0.2um,经450。C小时的热处理后,表面颗粒
尺寸减小到50一100nm。
在室温下制备、固化的薄膜具有良好的光致超亲水性、光催化能力和较高的
可见光透射率,且薄膜厚度均匀。无论热处理与否,样品经254nm紫外光照射
40min后对水的接触角均显著减小,接近于O。:在停止光照24小时后,接触角
仍为15— 3。,即能较长时间保持其亲水性。温度低于200℃的热处理,对薄膜的
光致特性基本没有影响,两种不同温度(室温和200。C)下处理的薄膜对罗丹明B
和亚甲基蓝水溶液的一级反应速率常数k分别为O.0229h-1.cm-2、0.0244h-1cm-2、
0.0220 h-1cm-2和0.0233 h-1-cm-2,即室温固化的薄膜与较低温度(<=200。C)处理过
的薄膜对罗丹明B和亚甲基蓝的降解没有明显的差异,较低温度处理并不影响
薄膜的光催化性。高温(>=450℃)处理1小时后,薄膜的光催化性能明显降低,
对罗丹明B和亚甲基蓝水溶液的一级反应速率常数k分别为O.0108 H-1.cm-2和
0.0097 h-1.cm-2。同时,随着厚度的增加,薄膜的光催化性能也相应提高。
通过沸水处理方法研究了不同温度下处理后薄膜与基板的附着力性能。室温
固化及200℃下处理的薄膜经沸水煮20分钟后仍具有良好的超亲水性。在波长
为254nm,功率密度为200gW/cm2的紫外光下照射40min后,薄膜对水的接触
角小于1。,表明薄膜与基板有良好的附着力及稳定性。
2.通过溶胶.凝胶法制各的掺杂sb的纳米二氧化钛光催化薄膜,在可见光
区的平均透射率大于80%。掺入适量的Sb后,由于Sb替代了Ti02的部分Ti,
形成sb-O-Ti结构,改变了Ti02的晶格结构参数(a,c),进而提高了薄膜的结晶效
率,使薄膜中锐钛矿结构的Ti02:Sb含量明显提高。但掺入过量的sb后,由于
sb相互间作用,形成Sb-Sb键,降低了晶格的有序度,使薄膜的结晶效率降低。
实验表明,Sb的最佳掺杂含量为0.2%,此时薄膜的结晶效率最高。
掺杂sb后明显提高了薄膜的光电转换效率,当掺杂含量为0 2%时,用254nm
紫外光作光源(功率密度为375uw·cm-2)时.其产生的光电流密度可达
42 49uA.cm-2,是用同种方法制备的纯Ti02薄膜电极的近ll倍。
用电化学方法研究了紫外光照射下Ti02薄膜电极表面Ti3+的产生与积累,
并提出了Tio2光致特性产生过程中的两个过程:即光电流和Ti3+产生的快过程
和Ti3+积累的慢过程,进而对Ti02薄膜光致亲水性的机理进行了一定的探讨。
含0.2%Sb的薄膜对亚甲基蓝具有较高分解性能和良好的光致亲承性。对亚
甲基蓝溶液光催化分解的一级反应速率常数k为0.078h-1.cm-2,是未掺杂的纯
Ti02薄膜在相同条件下的反应常数(0.040 h-1cm-2)的近2倍。经90-95uw的
254nm紫外光照射l小时后,掺杂0.2%的薄膜对水的接触角趋于00,表现出良
好的光致亲水性。
Ti02 Sb光催化薄膜在酸性条件下具有较强的的附着力。掺0.2%sb的薄膜
在0.2M的盐酸中浸泡48小时或在沸水中处理40分钟后对亚甲基蓝的光催化反
应常数分别为0.0338 h-1. cm-2和O.0283 h-1.cm-2,仍具有较强的光催化活性:经紫
外光照射15分钟后,水接触角均接近于0。。
电化学分析结果表明,掺杂sb后薄膜的稳定性得到显著提高,而未掺杂的
纯Ti02薄膜在盐酸中并不稳定。
最后还对用直流磁控溅射法制备锐钛矿结构的Ti02-xNx薄膜进行了初步的
探讨。结果表明,用磁控溅射制各的TiN薄膜,经一定时间的湿氧氧化后形成锐
钛矿结构的Ti02-xNx薄膜。该薄膜具有很好的光催化和光致亲水性能,对亚甲基
蓝的反应速率常数k达到0.107h-1.cm-2:经254nm紫外光照射30分钟后,薄膜
对水的接触角趋于0。:吸收光谱表明,TiO2-xNx薄膜的吸收边为460nm,对应的
禁带宽度为2.70eV。
While the annoseale photocatalyfie activity and the photo— induced properties of
titanium dioxide thin films were characterized,the effect of transitinnal metal Sb
doped into titanium dioxide thin films upon the microstructuse,photo-indeced
charaetars,electrochemical pmpertias and the stabilization in acid or alkaline
environment were studied in this paper.The preparation of the thin films includes two
parts One is the preparation of Si02一Ti02 composite thin films at room temperature
in air.Another is the deposition of Sb doped nanoscalc Ti02 thin films
1.In the section of photocatalytic Ti02 thin films were prepared at room
temperature in air,Ethyl delicate((C2Hs)4Si04)and TiCl4 were used as the precursor
0f Si02 and Ti02 respectively.The Nanoscale silicon dioxide and titanium dioxide
composite(si02-Tio2)thin films wem uniform and transparent with the thickness of
about 100nm were prepared.
Thc chemieal states of the elements on the surface or near the surface were
measured by XPS.The msults indieated that the Ti on/nearthe surface of the thin
films existed not only as Ti4+ but also aS Ti3+.After ultraviolet(UV)irradiation for
some time,the spectra of Ti2p3/2 changed obviously.Fitted results showed that the
spectra of Ti3+ risen drastically after UV irradiation for long time(about 24h)
accompaniedbyan up-forward tendency in the intensity of Ols spectra corresponded
to Ti3+. These illustrated that part of the Ti4+was changed to Ti3+ after UV irradiation
The crystalline stnlctore ofthe Si02-Ti02 thin films were characterized by X-ray
diffraction(XRD).The crystalline structure of the Ti02 in the Si02-Ti02 thin films
was in a majority of anatase state with the crystallite size of 14— 20nm.The AFM was
used to study the morphology of the thin films annealed at different temperature and
it effected onthe crystalline size of titanium dioxide For Si02 effect,the surfaces of
the samples treated at below 200。C were lumpish strucure with grain size of 0.2pm.
ARer treated at 450℃ for 1 hour,the grain size reduced to 50-100mn.
The samples prepared at room temperature had excellent photo-induced
superhydrophilicity and superior photocatalysis.After ander UV irradiation for 40min,
the contact angles for all samples were drastically reduced to 0。and it also was
between 1.5。t0 3。after storage in dark for 24 hour.There was few or none effcct on
photocatalysis of the thin films heat treated below 200。C,the staircase reaction speed
constant(k) of?
0.0220 h-1·cml-2 and 0.0233 h-1.cm-2.respectively.But the photocatalysis of thin films
treated at or over 450℃ for l hour was reduced obviously,which staircasereaction
speed constant(k)was about 0.0108h-1.cm-2 and 0.0097 h-1.cm-2.
The adherence between the thin films treated at different temperature and
substrate was characterized byboiling water trtatment The samplestreated below
200℃showed superior photo-induced supethydrophilicity after treated in boiling
water for 20min.The contact angle was less than 1。under UV(k=254nm,
P=200pW/cm2)irradiated for 40min.It illuminated that the thin films had strength
adherence and stabilization
The Ti02:Sb thin films with thc transparent larger than 80%were prepared by
dip-coating sol-gel method.After doping proper amount of Sb,a part of Ti4+ in Tio2
were replaced by Sb3+ and Sb combined with the O in Ti02 to form the structure of
Sb-O-Ti,the crystal lattice parameters a and c were changed,and the crystalline rate
of the Tio2 in the thin films is enhanced so that the content of anatasc Ti02:Sb were
increased.When the concentration of dopant Sb was excessive.Sb interacted wim
itself to form Sb-Sb structure,ruining the original anatase structure.So the
optimization content of Sb is aboutO.2%.
The photoelectric conversion character of TiO2 thin films are improved after Sb
doping in it.When the content of Sb reached 0.2‰the photocurrent density was.
about 42.49uA·cm-2 that was 11 times to the non-doped Ti02 thin films subjecting
引文
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