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1.
采用光化学沉积法制备了一系列不同Pt含量的新型Pt/BiOCl纳米片光催化剂,运用N2物理吸附-脱附、X射线粉末衍射、扫描电镜、透射电镜、X射线光电子能谱、光致发光光谱、紫外-可见漫反射光谱等手段对Pt/BiOCl进行了表征,并以λ=254nm的紫外灯和钨灯为光源,考察了Pt含量对Pt/BiOCl光催化降解酸性橙II活性的影响.结果表明,沉积的Pt对BiOCl样品比表面积的影响不大,但可有效增强催化剂对可见光的吸收能力,显著抑制光生电子与空穴的复合.当Pt含量为1%~2%时,能大幅度提高紫外光下BiOCl催化降解染料的活性,并产生可见光活性.这是由于Pt/BiOCl具有一定的可见光吸收能力,产生了Pt纳米粒子的等离子体光催化作用.  相似文献   

2.
ZnO纳米管的光学性质及其对甲基橙降解的光催化活性   总被引:4,自引:0,他引:4  
以十二烷基硫酸钠为模板剂采用水热法合成了ZnO纳米管,以尿素和ZnSO4为原料制备了ZnO纳米颗粒,并应用透射电镜、x射线衍射、光致发射光谱、拉曼光谱、比表面积测定、傅里叶红外光谱和紫外-可见漫反射光谱等技术对样品进行了表征.结果表明,ZnO纳米管的比表面积较大,在λ≈650nm的可见光波段ZnO纳米管开始出现吸收峰,而ZnO纳米颗粒在可见光波段几乎没有吸收.ZnO纳米管和纳米颗粒在紫外光照射下均对甲基橙有降解作用,其中ZnO纳米管的光催化活性较高.随着催化剂用量的增加和光照时间的延长,甲基橙降解率逐渐提高;甲基橙浓度的增大使甲基橙降解率降低.  相似文献   

3.
PbWO4是一类重要的半导体,广泛运用于高能物理领域无机闪烁晶体.它具有许多独特的物理性能,如衰减时间短(10 ns)、能量密度高(8.28 cm3)、低光产率(300 photons/MeV)、短辐射长度(0.9 cm)和高抗辐照损伤等. PbWO4纳米晶体的激子荧光、热荧光和其它光学性能主要取决PbWO4晶体的形貌和微观结构.目前已经合成了不同结构的PbWO4纳米/微米晶体,如四角双锥微米晶、微米球、纳米棒、纳米纺垂体等.近年来, PbWO4的光催化性能也引起人们的重视.研究发现, PbWO4晶体的光催化性能和其形貌、微观结构密切相关.如在不同形貌的十四面体、三维多尺度微米球和纳米颗粒中, PbWO4微米球表现了极高的光催化活性.此外, PbWO4微米球由于密度大,非常容易分离,从而有利于其回收利用,在循环使用时具有很高的稳定性.因此,合成具有特殊形貌的PbWO4纳米/微米晶体具有重要的理论和现实意义.此外,合成贵金属/半导体复合纳米结构是提高光催化性能的另一有效策略.在贵金属/半导体复合纳米结构中,光生电子(e–)和(h+)的复合可以在很大程度上得到抑制,因为光生e–可以快速地迁移至贵金属颗粒中心,从而加速e–和h+的分离.本文利用水热结合焙烧法首先合成了长度大于1μm的棒状PbWO4微米晶.然后利用光化学沉积法,在PbWO4微米晶表面沉积不同含量(0.5 wt%,1 wt%,和2 wt%)的Pt纳米粒子.利用X射线衍射(XRD)、N2物理吸附、扫描电镜(SEM)、透射电镜(TEM)、光电子能谱(XPS)、光致发光谱(PL)和紫外-可见漫反射吸收光谱(UV-Vis DRS)等手段对所制PbWO4和Pt/PbWO4进行了表征.表征结果表明,合成的PbWO4和Pt/PbWO4的比表面积很小(1.5–1.9 m2/g),沉积的Pt纳米粒子为金属态. UV-Vis DRS测试表明,沉积的Pt纳米粒子在光照下可以产生表面等离子共振,促进可见光的吸收.另外, PL的结果则证实Pt纳米粒子的存在还可抑制PbWO4晶体在光照下产生的光生e–和h+的分离.而XRD和高分辨TEM分析表明PbWO4微米棒的晶体生长方向为(–102)晶体方向.电子选区衍射表明,棒状PbWO4微米晶具有极高的结晶度.以氙灯为光源进行了光催化降解染料酸性橙II的光催化性能测试.结果表明,当沉积1–2 wt%Pt纳米粒子时,可使光催化活性提高2倍左右.另外, Pt/PbWO4微米棒的密度较大,非常容易进行离心分离催化剂及其循环使用.在第一次使用时酸性橙II的降解率为93%,而在第四次使用时酸性橙II的降解率仍维持在88%,表现出很好的光催化稳定性. Pt/PbWO4具有很高的光催化活性的原因,一方面是由于其具有很高的结晶度和独特的棒状结构,另一方面是由于沉积的Pt纳米粒子在光照下可以产生表面等离子共振,促进了可见光的吸收和光生e–与h+的分离.  相似文献   

4.
Pb WO4是一类重要的半导体,广泛运用于高能物理领域无机闪烁晶体.它具有许多独特的物理性能,如衰减时间短(10 ns)、能量密度高(8.28 cm3)、低光产率(300 photons/MeV)、短辐射长度(0.9 cm)和高抗辐照损伤等.Pb WO4纳米晶体的激子荧光、热荧光和其它光学性能主要取决Pb WO4晶体的形貌和微观结构.目前已经合成了不同结构的Pb WO4纳米/微米晶体,如四角双锥微米晶、微米球、纳米棒、纳米纺垂体等.近年来,Pb WO4的光催化性能也引起人们的重视.研究发现,Pb WO4晶体的光催化性能和其形貌、微观结构密切相关.如在不同形貌的十四面体、三维多尺度微米球和纳米颗粒中,PbW O4微米球表现了极高的光催化活性.此外,Pb WO4微米球由于密度大,非常容易分离,从而有利于其回收利用,在循环使用时具有很高的稳定性.因此,合成具有特殊形貌的PbW O4纳米/微米晶体具有重要的理论和现实意义.此外,合成贵金属/半导体复合纳米结构是提高光催化性能的另一有效策略.在贵金属/半导体复合纳米结构中,光生电子(e–)和(h+)的复合可以在很大程度上得到抑制,因为光生e–可以快速地迁移至贵金属颗粒中心,从而加速e–和h+的分离.本文利用水热结合焙烧法首先合成了长度大于1μm的棒状Pb WO4微米晶.然后利用光化学沉积法,在PbW O4微米晶表面沉积不同含量(0.5 wt%,1 wt%,和2 wt%)的Pt纳米粒子.利用X射线衍射(XRD)、N2物理吸附、扫描电镜(SEM)、透射电镜(TEM)、光电子能谱(XPS)、光致发光谱(PL)和紫外-可见漫反射吸收光谱(UV-Vis DRS)等手段对所制PbW O4和Pt/Pb WO4进行了表征.表征结果表明,合成的PbW O24和Pt/Pb WO4的比表面积很小(1.5–1.9 m/g),沉积的Pt纳米粒子为金属态.UV-Vis DRS测试表明,沉积的Pt纳米粒子在光照下可以产生表面等离子共振,促进可见光的吸收.另外,PL的结果则证实Pt纳米粒子的存在还可抑制PbW O4晶体在光照下产生的光生e–和h+的分离.而XRD和高分辨TEM分析表明Pb WO4微米棒的晶体生长方向为(–102)晶体方向.电子选区衍射表明,棒状PbW O4微米晶具有极高的结晶度.以氙灯为光源进行了光催化降解染料酸性橙II的光催化性能测试.结果表明,当沉积1–2 wt%Pt纳米粒子时,可使光催化活性提高2倍左右.另外,Pt/Pb WO4微米棒的密度较大,非常容易进行离心分离催化剂及其循环使用.在第一次使用时酸性橙II的降解率为93%,而在第四次使用时酸性橙II的降解率仍维持在88%,表现出很好的光催化稳定性.Pt/Pb WO4具有很高的光催化活性的原因,一方面是由于其具有很高的结晶度和独特的棒状结构,另一方面是由于沉积的Pt纳米粒子在光照下可以产生表面等离子共振,促进了可见光的吸收和光生e–与h+的分离.  相似文献   

5.
采用溶剂热-煅烧法,通过F掺杂合成了一系列具有高暴露(001)晶面的BiOCl纳米片。应用X射线衍射、N_2物理吸附、扫描电子显微镜、透射电子显微镜、X射线光电子能谱、紫外可见漫反射光谱、红外光谱和光电流响应等物理化学方法对合成的样品进行了表征分析。结果表明,掺杂适量的F可以促进BiOCl(110)优势晶面的生长,形成高暴露(001)晶面,同时可抑制BiOCl晶粒的长大,并增大BiOCl纳米片的比表面积和提高其表面羟基的数量。在模拟太阳光下,光催化降解偶氮染料罗丹明B结果表明,F掺杂能显著提高BiOCl对罗丹明B的光催化降解活性。其中F_(1.0)-BiOCl对罗丹明B的降解速率是BiOCl的2.67倍。此外,F_(1.0)-BiOCl对酸性橙Ⅱ的光催化降解活性是商业光催化剂P25(TiO_2)的1.24倍。F掺杂引起光催化活性大幅提升的主要原因是,高暴露(001)晶面的生成提升了BiOCl纳米片对染料的吸附性能,同时加快了光生e~-和h~+分离。  相似文献   

6.
在含有溴化十六烷基三甲基铵(CTAB)的水溶液中,通过水热法制备了超细钨酸锌(ZnWO4)纳米棒。用X射线衍射、扫描电子显微镜和紫外可见漫反射光谱表征了所制备的样品。在汞灯照射下,通过降解甲基橙(MO)检测了超细ZnWO4纳米棒的光催化活性。结果表明,在CTAB胶束作用下,ZnWO4纳米棒更细更长,超细ZnWO4纳米棒光催化活性比普通ZnWO4纳米棒更强,在同样条件下,前者对MO的降解率为90.2%,后者为50.%。  相似文献   

7.
采用两电极体系中恒电流电沉积在Ti基底上制得较均一的ZnO纳米棒阵列,利用SEM和XRD观察表征样品,研究Zn(NO3)2浓度及电流密度对ZnO纳米棒阵列微观形貌的影响. 以甲基橙为目标降解物,考察该电极光催化性能. 结果表明,Zn(NO3)2浓度和电流密度对纳米棒阵列的形貌有显著影响;与ITO玻璃等其他基底相比,在Ti基底上也可沉积较好均一取向的ZnO纳米棒阵列;紫外灯照射下,ZnO/Ti电极对甲基橙(10 mg·L-1)模拟印染废水降解2.5 h,降解率达到83.3%,光催化活性较佳;无光照时ZnO纳米棒的降解率仅7%.  相似文献   

8.
梁英  刘素芹 《应用化学》2014,31(1):65-68
在含有溴化十六烷基三甲基铵(CTAB)的水溶液中,通过水热法制备了超细钨酸锌(ZnWO4)纳米棒。 用X射线衍射、扫描电子显微镜和紫外可见漫反射光谱表征了所制备的样品。 在汞灯照射下,通过降解甲基橙(MO)检测了超细ZnWO4纳米棒的光催化活性。 结果表明,在CTAB胶束作用下,ZnWO4纳米棒更细更长,超细ZnWO4纳米棒光催化活性比普通ZnWO4纳米棒更强,在同样条件下,前者对MO的降解率为90.2%,后者为50%。  相似文献   

9.
在室温条件下,利用超声波辐射方法快速合成了四方状BiOCl(BiOBr)纳米片光催化剂。应用N2-物理吸附、X射线粉末衍射、扫描电镜、透射电镜、紫外可见光谱等手段对催化剂进行了表征,并以波长为λ=365 nm的紫外光和420 nm<λ<660 nm的可见光为光源,评价了该催化剂光催化降解酸性橙Ⅱ的活性。表征结果表明,超声波辐射可加速BiOCl和BiOBr晶化过程,显著提高BiOCl和BiOBr的结晶度,并使其晶粒发生细化,提高催化剂的比表面积。活性测试表明,声化学合成样品的光催化活性优于普通搅拌制备的样品。其中BiOCl的紫外光催化活性高于商业TiO2(P25)光催化剂。  相似文献   

10.
采用电化学阳极氧化法在钛表面构筑了海绵状纳米结构TiO2膜. 应用扫描电子显微镜(SEM)和X射线衍射(XRD)对膜层的形貌和晶型进行了分析和表征, 考察了阳极氧化时间对膜层厚度的影响, 并通过海绵状纳米结构TiO2膜对甲基橙的光催化降解研究了膜层厚度与光催化活性的关系. 结果表明, 海绵状纳米结构TiO2膜对甲基橙具有光催化降解作用, 而且随着膜层厚度的增加, 光催化降解速率显著增大, 厚度为2.2 μm的海绵状纳米结构TiO2膜对甲基橙的光催化降解速率是厚度为480 nm的6.4倍.  相似文献   

11.
K3InF6 is synthesized by a sol-gel route starting from indium and potassium acetates dissolved in isopropanol in the stoichiometry 1:3, with trifluoroacetic acid as fluorinating agent. The crystal structures of the organic precursors were solved by X-ray diffraction methods on single crystals. Three organic compounds were isolated and identified: K2InC10O10H6F9, K3InC12O14H4F18 and K3InC12O12F18. The first one, deficient in potassium in comparison with the initial stoichiometry, is unstable. In its crystal structure, acetate as well as trifluoroacetate anions are coordinated to the indium atom. The two other precursors are obtained, respectively, by quick and slow evaporation of the solution. They correspond to the final organic compounds, which give K3InF6 by decomposition at high temperature. The crystal structure of K3InC12O14H4F18 is characterized by complex anions [In(CF3COO)4(OHx)2](5−2x)− and isolated [CF3COOH2−x](x−1)− molecules with x=2 or 1, surrounded by K+ cations. The crystal structure of K3InC12O12F18 is only constituted by complex anions [In(CF3COO)6]3− and K+ cations. For all these compounds, potassium cations ensure only the electroneutrality of the structure. IR spectra of K2InC10O10H6F9 and K3InC12O12F18 were also performed at room temperature on pulverized crystals.  相似文献   

12.
The crystal structures of Bi2.5Na0.5Ta2O9 and Bi2.5Nam-1.5NbmO3m+3 (m=3,4) have been investigated by the Rietveld analysis of their neutron powder diffraction patterns (λ=1.470 Å). These compounds belong to the Aurivillius phase family and are built up by (Bi2O2)2+ fluorite layers and (Am-1BmO3m+1)2- (m=2-4) pseudo-perovskite slabs. Bi2.5Na0.5Ta2O9 (m=2) and Bi2.5Na2.5Nb4O15 (m=4) crystallize in the orthorhombic space group A21am, Z=4, with lattice constants of a=5.4763(4), b=5.4478(4), c=24.9710 (15) and a=5.5095(5), b=5.4783(5), c=40.553(3) Å, respectively. Bi2.5Na1.5Nb3O12 (m=3) has been refined in the orthorhombic space group B2cb, Z=4, with the unit-cell parameters a=5.5024(7), b=5.4622(7), and c=32.735(4) Å. In comparison with its isostructural Nb analogue, the structure of Bi2.5Na0.5Ta2O9 is less distorted and bond valence sum calculations indicate that the Ta-O bonds are somewhat stronger than the Nb-O bonds. The cell parameters a and b increase with increasing m for the compounds Bi2.5Nam-1.5NbmO3m+3 (m=2-4), causing a greater strain in the structure. Electron microscopy studies verify that the intergrowth of mixed perovskite layers, caused by stacking faults, also increases with increasing m.  相似文献   

13.
Novel complex oxides Ca14Zn6Ga10O35 and Ca14Zn5.5Ga10.5O35.25 were prepared in air at 1200 °C, 72 h. Refinements of their crystal structures using X-ray powder diffraction data showed that Ca14Zn6Ga10O35 is ordered (S.G. F23, =0.0458, Rp=0.0485, Rwp=0.0659, χ2=1.88) and Ca14Zn5.5Ga10.5O35.25 disordered (S.G. F432, =0.0346, Rp=0.0601, Rwp=0.0794, χ2=2.82) variants of the crystal structure of Ca14Zn6Al10O35. In the crystal structure of Ca14Zn6Ga10O35, there are large empty voids, which could be partially occupied by additional oxygen atoms upon substitution of Zn2+ by Ga3+ as in Ca14Zn5.5Ga10.5O35.25. These oxygen atoms are introduced into the crystal structure of Ca14Zn5.5Ga10.5O35.25 only as a part of four tetrahedra (Zn, Ga)O4 groups sharing common vertex. This creates a situation where even a minor change in the chemical composition leads to considerable anion and cation disordering resulting in a change of space group from F23 (no. 196) to F432 (no. 209).  相似文献   

14.
一些具有NASICON型网格结构的固体电解质具有高的电导率和好的稳定性,NASICON的意思是Na Super Ionic Conductor[1]。当NaZr2(PO4)3中P5 被Si4 部分取代时便可以得到具有NASICON结构的Na1 xZr2SixP3-xO12体系,其具有高的钠离子电导率。然而有相同结构的Li1 xZr2SixP3-xO12体系的离子电导率却很低,这是因为Li 半径太小,而NASICON三维网格结构的离子通道太大,两者不匹配而使电导率下降[2]。但当LiZr2(PO4)3中Zr4 被离子半径小些的Ti4 取代,所得LiTi2(PO4)3的通道就与Li 半径相匹配,适合于锂离子的迁移,从而使其电导率…  相似文献   

15.
Two new compounds, La3Ru8B6 and Y3Os8B6, were synthesized by arc melting the elements. Their structural characterization was carried out at room temperature on as-cast samples by using X-ray diffractometry. According to X-ray single-crystal diffraction results these borides crystallize in Fmmm space group (no. 69), Z=4, a=5.5607(1) Å, b=9.8035(3) Å, c=17.5524(4) Å, ρ=8.956 Mg/m3, μ=25.23 mm−1 for La3Ru8B6 and a=5.4792(2) Å, b=9.5139(4) Å, c=17.6972(8) Å, ρ=13.343 Mg/m3, μ=128.23 mm−1 for Y3Os8B6. The crystal structure of La3Ru8B6 was confirmed from Rietveld refinement of X-ray powder diffraction data. Both La3Ru8B6 and Y3Os8B6 compounds are isotypic with the Ca3Rh8B6 compound and their structures are built up from CeCo3B2-type and CeAl2Ga2-type structural fragments taken in ratio 2:1. They are the members of structural series R(A)nM3n−1B2n with n=3 (R is the rare earth metal, A the alkaline earth metal, and M the transition metal). Structural and atomic parameters were also obtained for La0.94Ru3B2 compound from Rietveld refinement (CeCo3B2-type structure, P6/mmm space group (no. 191), a=5.5835(9) Å, c=3.0278(6) Å).  相似文献   

16.
采用水热合成法制备了Co3O4及复合Ag/Co3O4、CuO/Co3O4一维纳米产品。用XRD,FE-SEM和TEM手段对产品进行了表征。采用循环伏安法研究了合成产品修饰的玻碳电极在碱性溶液中对对硝基苯酚的电催化还原性能。与裸玻碳电极相比,1mmol·L-1的对硝基苯酚在用Co3O4、特别是CuO/Co3O4修饰的玻碳电极上还原的峰电流明显增大,用Ag/Co3O4(Ag/Co原子比分别为1∶5和2∶5)修饰的玻碳电极催化还原对硝基苯酚时,尽管还原峰电流增大不是太大,但其峰电位明显降低(分别降低0.265和0.371V)。  相似文献   

17.
The crystal structures of compounds with nominal compositions Bi6FeP2O15+x (I), Bi6NiP2O15+x (II) and Bi6ZnP2O15+x (III) were determined from single-crystal X-ray diffraction data. They are monoclinic, space group I2, Z=2. The lattice parameters for (I) are a=11.2644(7), b=5.4380(3), c=11.1440(5) Å, β=96.154(4)°; for (II) a=11.259(7), b=5.461(4), c=11.109(7) Å, β=96.65(1)°; for (III) a=19.7271(5), b=5.4376(2), c=16.9730(6) Å, β=131.932(1)°. Least squares refinements on F2 converged for (I) to R1=0.0554, wR2=0.1408; for (II) R1=0.0647, wR2=0.1697; for (III) R1=0.0385, wR2=0.1023. The crystals are complexly twinned by 2-fold rotation about , by inversion and by mirror reflection. The structures consist of edge-sharing articulations of OBi4 tetrahedra forming layers in the a-c plane that then continue by edge-sharing parallel to the b-axis. The three-dimensional networks are bridged by Fe and Ni octahedra in (I) and (II) and by Zn trigonal bipyramids in (III) as well as by oxygen atoms of the PO4 moieties. Bi also randomly occupies the octahedral sites. Oxygen vacancies exist in the structures of the three compounds due to required charge balances and they occur in the octahedral coordination polyhedron of the transition metal. In compound (III), no positional disorder in atomic sites is present. The Bi-O coordination polyhedra are trigonal prisms with one, two or three faces capped. Magnetic susceptibility data for compound (I) were obtained between 4.2 and 350 K. Between 4.2 and 250 K it is paramagnetic, μeff=6.1 μB; a magnetic transition occurs above 250 K.  相似文献   

18.
YBa2Cu3Ox (Y-123) and Bi2Sr2Ca1Cu2Ox (Bi-2212) films on various substrates have been prepared by Metal-Organic Deposition starting from different metallorganic fluorine-free compounds and using a very simple instrumentation. The processing conditions include a rapid pyrolysis step in air and an annealing step in oxygen for Y-123 and in air for Bi-2212. The films obtained have been characterized by X-ray diffraction (XRD) and the formation of a superconducting phase of Y-123 or Bi-2212 was confirmed measuring the critical temperature (T c) with Ac-susceptibility and resistive measurements. Microstructure and final cationic ratios have been studied by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS).  相似文献   

19.
A new aluminum silicon oxycarbonitride, (Al5.8Si1.2)(O1.0C3.5N1.5), has been synthesized and characterized by X-ray powder diffraction (XRPD), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDX) and electron energy loss spectroscopy (EELS). The title compound is hexagonal with space group P63/mmc and unit-cell dimensions a=0.322508(4) nm, c=3.17193(4) nm and V=0.285717(6) nm3. The atom ratios of Al:Si and those of O:C:N were, respectively, determined by EDX and EELS. The initial structural model was successfully derived from the XRPD data by the direct methods and further refined by the Rietveld method. The crystal is most probably composed of four types of domains with nearly the same fraction, each of which is isotypic to Al7C3N3 with space group P63mc. The existence of another new oxycarbonitride (Al6.6Si1.4)(O0.7C4.3N2.0), which must be homeotypic to Al8C3N4, has been also demonstrated by XRPD and TEM.  相似文献   

20.
A new oxide, Bi14Sr21Fe12O61, with a layered structure derived from the 2212 modulated type structure Bi2Sr3Fe2O9, was isolated. It crystallizes in the I2 space group, with the following parameters: a=16.58(3) Å, b=5.496(1) Å, c=35.27(2) Å and β=90.62°. The single crystal X-ray structure determination, coupled with electron microscopy, shows that this ferrite is the m=5 member of the [Bi2Sr3Fe2O9]m[Bi4Sr6Fe2O16] collapsed family. This new collapsed structure can be described as slices of 2212 structure of five bismuth polyhedra thick along , shifted with respect to each other and interconnected by means of [Bi4Sr6Fe2O16] slices. The latter are the place of numerous defects like iron or strontium for bismuth substitution; they can be correlated to intergrowth defects with other members of the family.  相似文献   

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