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1.
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   

2.
The compound previously reported as Ba2Ti2B2O9 has been reformulated as Ba3Ti3B2O12, or Ba3Ti3O6(BO3)2, a new barium titanium oxoborate. Small single crystals have been recovered from a melt with a composition of BaTiO3:BaTiB2O6 (molar ratio) cooled between 1100°C and 850°C. The crystal structure has been determined by X-ray diffraction: hexagonal system, non-centrosymmetric space group, a=8.7377(11) Å, c=3.9147(8) Å, Z=1, wR(F2)=0.039 for 504 unique reflections. Ba3Ti3O6(BO3)2 is isostructural with K3Ta3O6(BO3)2. Preliminary measurements of nonlinear optical properties on microcrystalline samples show that the second harmonic generation efficiency of Ba3Ti3O6(BO3)2 is equal to 95% of that of LiNbO3.  相似文献   

3.
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   

4.
利用类石墨氮化碳(g-C3N4)和亚稳相钙钛氧化物(CaTi2O5)固相法制备C3N4/CaTi2O5复合材料。利用X射线衍射(XRD)、金相显微镜、扫描电子显微镜(SEM)及附带能谱分析仪(EDS)和N2吸附-脱附对样品的显微结构和比表面积进行检测分析,并用紫外-可见吸收光度计(UV-Vis)测试了样品的光吸收性能,研究C3N4与CaTi2O5物质的量之比(nC3N4/nCaTi2O5)对C3N4/CaTi2O5复合样品的物相结构和微观形貌的影响,同时考察C3N4/CaTi2O5复合样品在可见光照射下光催化降解罗丹明染料效果。实验结果表明:相比纯C3N4和CaTi2O5样品,C3N4/CaTi2O5复合样品在可见光下具有较高的光催化性能,随着nC3N4/nCaTi2O5增加,样品的光催化降解率随之增加而后降低,当nC3N4/nCaTi2O5=1:1时,样品的光催化降解率达到最大值99.5%,并且循环重复利用5次后,样品的光催化剂降解率仍几乎保持不变。复合样品光催化性能提高主要归因于复合能级结构有效地抑制了电子和空穴复合所致。  相似文献   

5.
Thin crystals of La2O3, LaAlO3, La2/3TiO3, La2TiO5, and La2Ti2O7 have been irradiated in situ using 1 MeV Kr2+ ions at the Intermediate Voltage Electron Microscope-Tandem User Facility (IVEM-Tandem), Argonne National Laboratory (ANL). We observed that La2O3 remained crystalline to a fluence greater than 3.1×1016 ions cm−2 at a temperature of 50 K. The four binary oxide compounds in the two systems were observed through the crystalline-amorphous transition as a function of ion fluence and temperature. Results from the ion irradiations give critical temperatures for amorphisation (Tc) of 647 K for LaAlO3, 840 K for La2Ti2O7, 865 K for La2/3TiO3, and 1027 K for La2TiO5. The Tc values observed in this study, together with previous data for Al2O3 and TiO2, are discussed with reference to the melting points for the La2O3-Al2O3 and La2O3-TiO2 systems and the different local environments within the four crystal structures. Results suggest that there is an observable inverse correlation between Tc and melting temperature (Tm) in the two systems. More complex relationships exist between Tc and crystal structure, with the stoichiometric perovskite LaAlO3 being the most resistant to amorphisation.  相似文献   

6.
利用类石墨氮化碳(g-C_3N_4)和亚稳相钙钛氧化物(CaTi_2O_5)固相法制备C_3N_4/CaTi_2O_5复合材料。利用X射线衍射(XRD)、金相显微镜、扫描电子显微镜(SEM)及附带能谱分析仪(EDS)和N2吸附-脱附对样品的显微结构和比表面积进行检测分析,并用紫外-可见吸收光度计(UV-Vis)测试了样品的光吸收性能,研究C_3N_4与CaTi_2O_5物质的量之比(nC_3N_4/nCaTi_2O_5)对C_3N_4/CaTi_2O_5复合样品的物相结构和微观形貌的影响,同时考察C_3N_4/CaTi_2O_5复合样品在可见光照射下光催化降解罗丹明染料效果。实验结果表明:相比纯C_3N_4和CaTi_2O_5样品,C_3N_4/CaTi_2O_5复合样品在可见光下具有较高的光催化性能,随着nC_3N_4/nCaTi_2O_5增加,样品的光催化降解率随之增加而后降低,当nC_3N_4/nCaTi_2O_5=1∶1时,样品的光催化降解率达到最大值99.5%,并且循环重复利用5次后,样品的光催化剂降解率仍几乎保持不变。复合样品光催化性能提高主要归因于复合能级结构有效地抑制了电子和空穴复合所致。  相似文献   

7.
选用B3LYP方法在LanL2MB水平下, 对双帽α-Keggin型杂多阴离子[H4As3Mo12O40]-的电子结构和质子的定位进行了密度泛函理论(DFT)研究. 结果表明, 双帽的形成大大影响了杂多阴离子[As3Mo12O40]5-的电子结构和性质, NBO分析显示参与成帽的三桥氧上的电子密度比双桥氧上的要大, 简单地从电荷密度来看, 质子将首先在三桥氧上定域成键, 但通过比较质子定域在几种桥氧上质子化稳定化能的大小, 发现[H4As3Mo12O40]-中的四个质子将在八个双桥氧中的其中四个氧原子上定位, 而不是如文献中报道的在四个三桥氧上定域成键. 对杂多酸H3PM12O40 (M=Mo, W)中质子的定位也进行了理论计算并与文献进行了比较, 结果显示, H3PMo12O40中质子是定位在双桥氧上; 而H3PW12O40中质子将优先在双桥氧上定位, 但也可在端氧上定位; 这一结果与文献报道的相一致.  相似文献   

8.
The ternary system Li2O-Al2O3-B2O3 is reinvestigated with solid-state reaction and X-ray powder diffraction technique to clarify some long-standing uncertainties. The phase relations are constructed based on the phase identifications of 51 ternary samples. Six ternary compounds, Li2AlB5O10, LiAlB2O5, Li3AlB2O6, Li2AlBO4, LiAl7B4O17 and a compound with a composition close to 0.66Li2O·0.06Al2O3·0.28B2O3, are observed or confirmed in this system, and the thermal stability of these ternary compounds is also discussed on the basis of DTA experimental results.  相似文献   

9.
Single crystals of Ca3CuRhO6, Ca3Co1.34Rh0.66O6 and Ca3FeRhO6 were synthesized by high temperature flux growth in molten K2CO3 and structurally characterized by single crystal X-ray diffraction. While Ca3Co1.34Rh0.66O6 and Ca3FeRhO6 crystallize with trigonal (rhombohedral) symmetry in the space group , Z=6: Ca3Co1.34Rh0.66O6a=9.161(1) Å, c=10.601(2) Å; Ca3FeRhO6a=9.1884(3) Å, c=10.7750(4) Å; Ca3CuRhO6 adopts a monoclinic distortion of the K4CdCl6 structure in the space group C2/c, Z=4: a=9.004(2) Å, b=9.218(2) Å, c=6.453(1) Å, β=91.672(5). All crystals of Ca3CuRhO6 examined were twinned by pseudo-merohedry. Ca3CuRhO6, Ca3Co1.34Rh0.66O6, and Ca3FeRhO6 are structurally related and contain infinite one-dimensional chains of alternating face-sharing RhO6 octahedra and MO6 trigonal prisms. In the monoclinic modification, the copper atoms are displaced from the center of the trigonal prism toward one of the rectangular faces adopting a pseudo-square planar configuration. The magnetic properties of Ca3CuRhO6, Ca3Co1.34Rh0.66O6, and Ca3FeRhO6 are discussed.  相似文献   

10.
用液相反应-前驱物烧结法制备了Cr2(WO4)3和Cr2(MoO4)3粉体。298~1 073 K的原位粉末X射线衍射数据表明Cr2(WO4)3和Cr2(MoO4)3的晶胞体积随温度的升高而增大, 本征线热膨胀系数分别为(1.274±0.003)×10-6 K-1和(1.612±0.003)×10-6 K-1。用热膨胀仪研究了Cr2(WO4)3和Cr2(MoO4)3在静态空气中298~1 073 K范围内热膨胀行为,即开始表现为正热膨胀,随后在相转变点达到最大值,最后表现为负热膨胀,其负热膨胀系数分别为(-7.033±0.014)×10-6 K-1和(-9.282±0.019)×10-6 K-1。  相似文献   

11.
通过沉积法和离子交换法成功地制备了Ag_3PO_4/Ag_2S/g-C_3N_4复合型光催化剂。利用X射线多晶粉末衍射仪(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)、N_2吸附-脱附等温线、紫外-可见漫反射光谱、荧光光谱等手段对样品进行了表征。通过降解罗丹明B考察其可见光催化活性及稳定性,研究了硫化钠与磷酸银物质的量的比值(n_(Na_2S)/n_(Ag_3PO_4))、g-C_3N_4添加量对所制备复合光催化材料性能的影响,同时对光催化机理进行了探讨。结果表明,随着n_(Na2S)/n_(Ag3PO4)的增加,所得复合催化材料活性先增加后降低;当n_(Na2S)/n_(Ag_3PO_4)为1.5%、g-C_3N_4与Ag_3PO_4的质量比为3∶7时制备的催化剂ASC1.5的光催化活性最好,在可见光照射下,40 min内可将罗丹明B完全降解,且5次循环使用后仍保持较高的催化活性。和Ag_3PO_4相比,Ag_3PO_4/Ag_2S/g-C_3N_4复合型光催化材料的活性与稳定性都得到明显提高,这主要归因于复合催化剂比表面积和孔结构的增加,载流子分离效率的提高。光催化机理研究表明,空穴(h~+)、超氧阴离子自由基(·O~(2-))和羟基自由基(·OH)都是光催化过程中的主要活性物种。三者作用大小依次为:h~+·O~(2-)·OH。  相似文献   

12.
Magnetic diphase nanostructures of ZnFe2O4/γ-Fe2O3 were synthesized by a solvothermal method. The formation reactions were optimized by tuning the initial molar ratios of Fe/Zn. All samples were characterized by X-ray diffraction, thermogravimetric analysis, infrared spectroscopy, and Raman spectra. It is found that when the initial molar ratio of Fe/Zn is larger than 2, a diphase magnetic nanostructure of ZnFe2O4/γ-Fe2O3 was formed, in which the presence of ZnFe2O4 enhanced the thermal stability of γ-Fe2O3. Further increasing the initial molar ratio of Fe/Zn larger than 6 destabilized the diphase nanostructure and yielded traces of secondary phase α-Fe2O3. The grain surfaces of diphase nanostructure exhibited a spin-glass-like structure. At room temperature, all diphase nanostructures are superparamagnetic with saturation magnetization being increased with γ-Fe2O3 content.  相似文献   

13.
The ferroelectric ceramics of Bi4Ti3O12, SrBi4Ti4O15, and lanthanum-doped Bi4Ti3O12-SrBi4Ti4O15 were synthesized, and their Raman spectra were investigated. La-doping resulted in the enlargement of remnant polarization of Bi4Ti3O12-SrBi4Ti4O15. The structure of the Bi2O2 layers and TiO6 octahedra of the intergrowth was found to be different from those of Bi4Ti3O12 and SrBi4Ti4O15. La3+ ions exhibit pronounced selectivity for the occupation of A site as La content is lower than 0.50, and tend to be incorporated into Bi2O2 layers when the La content is higher than 0.50. Lanthanum substitution brings about the structural phase transition in Bi4Ti3O12-SrBi4Ti4O15. The variation of ferroelectric property may be attributed to combined contribution from the decreasing of the oxygen vacancies, the relaxation of the lattice distortion, the destroying of the insulation and the space charge compensation effects of the Bi2O2 slabs.  相似文献   

14.
通过溶胶-凝胶法合成了上转换发光材料Er~(3+)∶V_(0.01)Y_(2.99)Al_5N_(0.01)F_(0.01)O_(11.98)(Er∶YAG),然后利用水热法合成了BiPO_4,再利用高温煅烧法合成了Er∶YAG/BiPO_4/Pt复合物光催化剂.通过使用X-射线粉末衍射仪(XRD),扫描电子显微镜(SEM),透射电子显微镜(TEM),光致发光光谱(PL)和上转换发射光谱对样品的组成、形貌及光学特征进行了表征.此外,还研究了不同甘油添加量、 Er∶YAG和BiPO_4的摩尔比例和复合温度及光催化剂的循环使用次数对Er∶YAG/BiPO_4/Pt复合物光催化剂活性的影响.实验结果显示Er∶YAG/BiPO_4/Pt复合物光催化剂具有高的光催化活性和较好的稳定性,它可以作为一种高效的光催化剂用于污水中有机污染物的处理.  相似文献   

15.
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   

16.
合成了稀土(钬, Ho)-氨基酸(甘氨酸, C2H5O2N)二元配合物Ho(NO3)3(C2H5O2N)4·H2O, 并且通过化学分析、元素分析和红外(IR)光谱对配合物进行了表征. 用高精度全自动绝热量热仪, 测定了该配合物在80-390 K温度区间的定压摩尔热容(Cp,m). 利用实验测定的热容数据, 采用最小二乘法, 将热容曲线上热容峰以外的两段平滑区的摩尔热容对折合温度进行拟合, 建立了热容随折合温度变化的多项式方程. 根据热容与焓、熵的热力学关系,计算出了配合物在80-390 K温度区间内,每隔5 K,相对于298.15 K的摩尔热力学函数(HT,m-H298.15,m)和(ST,m-S298.15,m). 通过热容曲线分析, 计算出了350 K附近转变过程的焓变(ΔtrsHm)和熵变(ΔtrsSm). 用差示扫描量热法(DSC)测定了配合物的热稳定性.  相似文献   

17.
采用优化的高温固相方法制备了稀土离子Eu3+和Tb3+掺杂的La7O6(BO3)(PO42系荧光材料,并对其物相行为、晶体结构、光致发光性能和热稳定性进行了详细研究。结果表明,La7O6(BO3)(PO42:Eu3+材料在紫外光激发下能够发射出红光,发射光谱中最强发射峰位于616 nm处,为5D07F2特征能级跃迁,Eu3+的最优掺杂浓度为0.08,对应的CIE坐标为(0.610 2,0.382 3);La7O6(BO3)(PO42:Tb3+材料在紫外光激发下能够发射出绿光,发射光谱中最强发射峰位于544 nm处,对应Tb3+5D47F5能级跃迁,Tb3+离子的最优掺杂浓度为0.15,对应的CIE坐标为(0.317 7,0.535 2)。此外,对2种材料的变温光谱分析发现Eu3+和Tb3+掺杂的La7O6(BO3)(PO42荧光材料均具有良好的热稳定性。  相似文献   

18.
Samples in the system Lu2−xYxSi2O7 (0?x?2) have been synthesized following the sol-gel method and calcined to 1300 °C, a temperature at which the β-polymorph is known to be the stable phase for the end-members Lu2Si2O7 and Y2Si2O7. The XRD patterns of all the compositions studied are compatible with the structure of the β-polymorph. Unit cell parameters are calculated as a function of composition from XRD patterns. They show a linear change with increasing Y content, which indicates a solid solubility of β-Y2Si2O7 in β-Lu2Si2O7 at 1300 °C. 29Si MAS NMR spectra of the different members of the system agree with the XRD results, showing a linear decrease of the 29Si chemical shift with increasing Y content. Finally, a correlation reported in the literature to predict 29Si chemical shifts in silicates is applied here to obtain the theoretical variation in 29Si chemical shift values in the system Lu2Si2O7-Y2Si2O7 and the results compare favorably with the values obtained experimentally.  相似文献   

19.
The basic mercury(I) chromate(VI), Hg6Cr2O9 (=2Hg2CrO4·Hg2O), has been obtained under hydrothermal conditions (200 °C, 5 days) in the form of orange needles as a by-product from reacting elemental mercury and K2Cr2O7. Hydrothermal treatment of microcrystalline Hg6Cr2O9 in demineralised water at 200 °C for 3 days led to crystal growth of red crystals of the basic mercury(I, II) chromate(VI), Hg6Cr2O10 (=2Hg2CrO4·2HgO). The crystal structures were solved and refined from single crystal X-ray data sets. Hg6Cr2O9: space group P212121, Z=4, a=7.3573(12), b=8.0336(13), , 3492 structure factors, 109 parameters, R[F2>2σ(F2)]=0.0371, wR(F2 all)=0.0517; Hg6Cr2O10: space group Pca21, Z=4, a=11.4745(15), b=9.4359(12), , 3249 structure factors, 114 parameters, R[F2>2σ(F2)]=0.0398, wR(F2 all)=0.0625. Both crystal structures are made up of an intricate mercury-oxygen network, subdivided into single building blocks [O-Hg-Hg-O] for the mercurous compound, and [O-Hg-Hg-O] and [O-Hg-O] for the mixed-valent compound. Hg6Cr2O9 contains three different Hg22+ dumbbells, whereas Hg6Cr2O10 contains two different Hg22+ dumbbells and two Hg2+ cations. The HgI-HgI distances are characteristic and range between 2.5031(15) and 2.5286(9) Å. All Hg22+ groups exhibit an unsymmetrical oxygen environment. The oxygen coordination of the Hg2+ cations is nearly linear with two tightly bonded O atoms at distances around 2.07 Å. For both structures, the chromate(VI) anions reside in the vacancies of the Hg-O network and deviate only slightly from the ideal tetrahedral geometry with average Cr-O distances of ca. 1.66 Å. Upon heating at temperatures above 385 °C, Hg6Cr2O9 decomposes in a four-step mechanism with Cr2O3 as the end-product at temperatures above 620 °C.  相似文献   

20.
以三聚氰胺和六水合氯化钴为原料,一锅法制备Co_3O_4负载的多孔石墨相氮化碳(Co_3O_4/g-C_3N_4)复合光催化材料。采用X射线衍射(XRD)、傅里叶变换红外(FT-IR)光谱、X射线光电子能谱(XPS)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、紫外-可见漫反射光谱(UV-Vis DRS)、光致发光光谱(PL)等手段对其结构和光学特性进行表征。以盐酸四环素(TC)为目标污染物,评价了不同负载量Co_3O_4/g-C_3N_4复合光催化剂的可见光催化性能。结果表明,所制备的Co_3O_4/g-C_3N_4复合光催化剂为多孔结构,其比表面积较大,并在可见光区域具有显著的吸收。利用原位生成的Co_3O_4纳米粒子在氮化碳表面形成异质结构,可有效转移光生载流子,降低光生电子-空穴的再结合率,从而提高光催化活性。并且存在最佳Co_3O_4复合量,当六水合氯化钴加入量为三聚氰胺的8%(w/w)时,所制备的复合光催化剂CoCN-8具有最佳的光催化性能。在可见光的照射下,60 min内可降解85%的TC,而同样条件下,纯g-C_3N_4仅降解23%的TC。  相似文献   

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