Al2O3/ZrO2/ZrSiO4复合材料的研究

在Al2O3颗粒补强锆英石陶瓷的研究基础上,探讨了Al2O3与ZrO2共同对锆英石陶瓷的协同补强增韧行为.制备的锆英石基复合材料的室温抗弯强度和断裂韧性分别可达383.31MPa、4.39 MPa·m12.采用XRD分析了复合材料的相组成,采用SEM观察复合材料的断面形貌.结果显示:ZrSiO4为主要晶相,另外还有少量Al2O3和ZrO2存在;第二种增强体ZrO2的最佳引入量为20％(质量分数);确定复合材料的强韧化是由Al2O3和ZrO2颗粒引起的裂纹偏转、微裂纹增韧与ZrO2颗粒引起的相变增韧共同作用而实现的,断裂方式主要为穿晶断裂.     

Synthesis and properties of magnetic solid superacid: SO4/ZrO2–B2O3–Fe3O4

A magnetic SO₄²⁻/ZrO₂–B₂O₃–Fe₃O₄ solid superacid catalyst is prepared via a simple chemical co-precipitation approach. The obtained materials were characterized in detailed by X-ray powder diffraction, thermogravimetric analysis–different scanning calorimetry, Fourier transform infrared spectroscopy (FTIR), electron microscopy (SEM and TEM), and Mossbauer spectra. Powder X-ray diffraction patterns show that in this composite oxide the transformation temperature of ZrO₂ from tetragonal to monoclinic phase is higher compared to the pristine SO₄²⁻/ZrO₂ material. The introduction of Fe₃O₄ endows the superacid with a super-paramagnetic property while in a ferromagnetic state after calcination. The superacid exhibits high catalytic activity in forming ethyl acetate by esterification.     

含钛磷酸盐玻璃NaTi2(PO4)3-0.9Ca3(PO4)2的析晶行为

利用差热分析、X射线衍射仪、液氮吸附BET孔经测试仪对组成为NaTi2(PO4)3-0.9 Ca3(PO4)2的含钛磷酸盐玻璃的析晶行为进行了研究.通过对该玻璃相继进行成核、析晶和酸浸泡处理制备了NaTi2(PO4)3骨架多孔微晶玻璃.证明该玻璃在646℃8h成核处理过程中产生了旋节分解特征的成分偏聚,形成了富TiO2玻璃相和富CaO玻璃相交错生长的连通结构,成核处理后的玻璃在738℃析晶过程中依次在富钛相和富钙相中析出NaTi2(PO4)3和β-Ca3(PO4)2.成核过程对析晶的促进作用是通过促进NaTi2(PO4)3的析出而实现的.     

g-C3N4及改性g-C3N4的光催化研究进展

聚合型半导体材料g-C3N4因其优异的物理性能和光电性能成为当今研究的热门材料。本文从结构分析和理论计算角度讨论了g-C3N4能够作为无金属催化剂的原因,综述了介孔g-C3N4、无机元素掺杂g-C3N4、金属负载g-C3N4、g-C3N4/金属氧化物复合物和有机改性g-C3N4等不同改性g-C3N4的制备和性质,着重分析了他们催化光解水析氢反应的机理、影响因素及研究进展,并阐述了今后的研究方向。     

3种合金在80℃H2SO4和H2SO4-HNO3溶液中的腐蚀行为

化工装置常用316L合金、804合金和Hastelloy C合金制造,使用过程中常接触65%～85%H2SO4溶液和65%～85%H2SO4与少量HNO3的混合液。采用静态挂片试验和电化学方法研究了这3种合金在80℃,72%H2SO4溶液和80℃,72%H2SO4+0.1%HNO3混合溶液中的腐蚀行为。结果表明:在80℃,72%H2SO4溶液中,804合金的耐蚀性优于Hastelloy C合金,316L的耐蚀性最差;在80℃,72%H2SO4+0.1%HNO3溶液中,804合金的耐蚀性优于316L,Hastelloy C合金的耐蚀性最差。     

FeVO4/Cu3(BTC)2(H2O)3异质结制备及光催化性能

以Cu片和1, 3, 5-苯三甲酸为原料,电化学法制备经典Cu-MOF材料Cu₃(BTC)₂(H₂O)₃,即HKUST-1,作为基底金属有机框架材料(MOFs),采用室温沉积法制备FeVO₄/HKUST-1异质结复合材料,通过XRD、SEM、BET、UV-Vis DRS等对其晶体结构、形貌、比表面积、光吸收性能等进行了表征。结果表明:FeVO₄与HKUST-1复合形成异质结后,有利于光生电子-空穴的产生和转移,对目标染料污染物罗丹明B(RhB)的降解性能显著增强。可见光照射120 min后,异质结体系中RhB的降解率可达93%,而单一FeVO₄或HKUST-1体系中仅为12%和5%。此外,对材料的组成比例进行了优化,当FeVO₄与HKUST-1摩尔比为1∶1时,制备的FeVO₄/HKUST-1复合材料具有最佳的光催化性能。进一步,考察了其循环使用的稳定性,循环5次后对RhB的降解效率仍保持在90%以上,稳定性良好。      

Bi2O3助熔剂对CaO-B2O3-SiO2/Al2O3玻璃陶瓷复合材料性能的影响

以CaO-B₂O₃-SiO₂(CBS)玻璃粉体和Al₂O₃陶瓷粉体为原料,通过在CBS与Al₂O₃的质量比固定为50:50的玻璃-陶瓷复合材料中添加适量的Bi₂O₃作为烧结助熔剂,探讨了Bi₂O₃助熔剂对CBS/Al₂O₃复合材料的烧结性能、介电性能、抗弯强度和热膨胀系数的影响规律.研究表明:Bi₂O₃助熔剂能通过降低CBS玻璃的转变温度和黏度促进CBS/Al₂O₃复合材料的致密化进程,于880 ℃下烧结即能获得结构较致密、气孔较少的CBS/Al₂O₃复合材料.然而,过量添加Bi₂O₃将使玻璃的黏度过低,从而恶化CBS/Al₂O₃复合材料的烧结性能、介电性能及抗弯强度.当Bi₂O₃的添加量为CBS/Al₂O₃复合材料的1.5wt%时,于880 ℃下烧结即能获得最为致密的CBS/Al₂O₃复合材料,密度为2.82 g·cm^-3,这一材料具有良好的介电性能(介电常数为7.21,介电损耗为1.06×10^-3),抗弯强度为190.34 MPa,0~300 ℃的热膨胀系数为3.52×10^-6 K^-1.     

纳米LaFeO3-TiO2光催化还原CO2

采用柠檬酸络合-溶胶-凝胶法制备LaFeO3-TiO2纳米催化剂,并用TG-DTA、FT-IR、UV-Vis、XRD对其表征,研究煅烧温度、LaFeO3复合量对光催化催化还原CO2制甲醇性能影响及反应优化条件。结果表明,LaFeO3与TiO2的复合可以抑制TiO2的晶相转变,拓宽催化剂光响应范围,提高光催化性能。优化条件为:催化剂煅烧温度为800℃,复合质量分数为3%的LaFeO3,催化剂用量为2.0g/L,反应时间为7h,CO2流量为200mL/min,反应温度为90℃,反应液中NaOH和Na2SO3的浓度均为0.10mol/L,甲醇的产率达325.49μmol/g。并初步探讨了LaFeO3-TiO2光催化还原CO2机理。     

CoAl2O4/Al2O3纳米复合陶瓷的结构与表征

利用溶胶-凝胶方法制备了的CoAl2O4/Al2O3纳米复合陶瓷,并用X-ray分析(XRD)、红外光谱(IR)和扫描电镜分析(SEM)对其结构进行了分析.结果表明,随Al2O3含量增多,CoAl2O4尖晶石相从CoAl2O4/Al2O3凝胶中的析晶温度升高.SEM形貌也说明,随Al2O3含量增多,CoAl2O4/Al2O3陶瓷中形成一定的层状结构.     

炭黑包覆Al2O3掺杂LiMn2O4正极材料的研究

使用醋酸锂、醋酸锰和氧化铝为原料,采用高温固相法合成掺杂Al离子的LiMn2O4二级产物。合成化学计量比为n(Li)∶n(Mn)∶n(Al)=1.3∶1.9∶0.1。首次烧结温度450℃,烧结时间4h;二次烧结温度750℃,煅烧时间为40h。合成样品采用XRD进行材料表征。测试结果表明:合成样品为尖晶石结构,结晶度较高。所得样品使用炭黑包覆处理,并制成实验性电池,对其进行交流阻抗测试(EIS)分析、循环伏安特性(CV)测试、充放电及循环性能测试分析。实验结果表明:包覆后的正极材料改善了LiMn2O4的大电流充放电性能,该材料在0.5C的首次放电比容量为93mAh/g;包覆材料增强了在大电流充放电下的容量保持率,极大地改善了电池的循环性能,该材料在充放电倍率为0.2C时,32次循环后的容量保持率为92.5%。     

Precision frequency measurement of the 2S1/2 2D5/2 transition of Sr+ with a 674-nmdiode laser locked to an ultrastable cavity

We have measured the frequency of the 5s ²S_1/2 -4d ²D_5/2 clock transition of a single Sr ion confined in a Paul trap. A diode laser locked to an ultrastable Fabry-Perot (F-P) cavity was used to probe the transition with a resolution of 3.5 kHz. The absolute frequency was determined from heterodyne measurements referenced to an iodine stabilized HeNe laser and a CO₂ laser yielding a value for the S-D transition of (444 779 043 963±30) kHz. This work could lead to the development of a new optical frequency standard at 674 nm     

K2(Rb2,Cs2,Tl2)TeBr6(I6) and Rb3(Cs3)Sb2(Bi2)Br9(I9) perovskite compounds

We systematize available experimental data on the crystal structure of the ternary halides K₂(Rb₂,Cs₂,Tl₂)TeBr₆(I₆) and Rb₃(Cs₃)Sb₂(Bi₂)Br₉(I₉), analyze the general trends in the properties of their single crystals, and examine the key features of the physicochemical interaction in related systems.     

11B NMR Study of Pure and Lightly Carbon-Doped MgB2 Superconductors

We report a ¹¹B NMR line shape and spin-lattice relaxation rate (1/(T₁T))(1/(T_1T)) study of pure and lightly carbon-doped MgB_2-xC_x_{2-x}{\rm C}_x for x = 0,0.02x = 0,0.02, and 0.04, in the vortex state and in magnetic field of 23.5 kOe. We show that while pure MgB₂_2 exhibits the magnetic field distribution from superposition of the normal and the Abrikosov state, slight replacement of boron with carbon unveils the magnetic field distribution of the pure Abrikosov state. This indicates a considerable increase of H^c_c2H^c_{c2} with carbon doping with respect to pure MgB₂_2. The spin-lattice relaxation rate 1/(T₁T)1/(T_1T) demonstrates clearly the presence of a coherence peak right below T_cT_{\rm c} in pure MgB₂_2, followed by a typical BCS decrease on cooling. However, at temperatures lower than ?\approx 10 K strong deviation from the BCS behavior is observed, probably from residual contribution of the vortex dynamics. In the carbon-doped systems both the coherence peak and the BCS temperature dependence of 1/(T₁T)1/(T_1T) weaken, an effect attributed to the gradual shrinking of the σ hole cylinders of the Fermi surface with electron doping.     

Observation of a Sub-10-Hz Linewidth 88Sr+ 2S1/2–2D5/2 Clock Transition at 674 nm

In this paper, a pair of diode lasers at 674 nm, locked to two independent ultralow-expansion high-finesse cavities, have been characterized by monitoring the beat frequency between them. The individual laser linewidth of 1.4 Hz for a 3-s averaging time broadened to 4 Hz at 30 s. The relative frequency stability of the beat at 1s is 2.5 10^-15. One of the lasers has been used to interrogate the ⁸⁸Sr^{+ 2}Si_1/2-²D _5/2 transition at 674 nm, and a transition linewidth of 9 Hz has been observed     

Al2O3/SiO2 and HfO2/SiO2 dichroic mirrors for UV solid-state lasers

HfO₂/SiO₂ and Al₂O₃/SiO₂ multilayers to be employed as high reflectance end mirrors in Cerium-doped fluoride solid-state lasers were produced by radio frequency sputtering. The components were designed to have high transmittance at the pumping wavelength and high reflectance in a wavelength band corresponding to the active medium emission. A photoacoustic beam deflection technique and inspection of the irradiated area under a microscope were used to measure the laser induced damage threshold of the mirrors at the pumping wavelength. These coatings were tested in a laser cavity.     

Natural and persistent superhydrophilicity of SiO2/TiO2 and TiO2/SiO2 bi-layer films

Sol-gel SiO₂/TiO₂ and TiO₂/SiO₂ bi-layer films have been deposited from a polymeric SiO₂ solution and either a polymeric TiO₂ mother solution (MS) or a derived TiO₂ crystalline suspension (CS). The chemical and structural properties of MS and CS bi-layer films heat-treated at 500 °C have been investigated by Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and transmission electron microscospy. Water contact angle measurements show that MS SiO₂/TiO₂ and CS TiO₂/SiO₂ bi-layer films exhibit a natural superhydrophilicity, but cannot maintain a zero contact angle for a long time over film aging. In contrast, CS SiO₂/TiO₂ bi-layer films exhibit a natural, persistent, and regenerable superhydrophilicity without the need of UV light. Superhydrophilic properties of bi-layer films are discussed with respect to the nature of the TiO₂ single-layer component and arrangement of the bi-layer structure, i.e. TiO₂ underlayer or overlayer.     

Crystal Structure of (H3O)2[(UO2)2(SeO4)3(H2O)2](H2O)3.5

Crystals of (H₃O)₂[(UO₂)₂(SeO₄)₃(H₂O)₂](H₂O)_3.5 were prepared from aqueous solutions by evaporation. The crystal structure [monoclinic system, space group P2₁/m, a = 11.9402(11), b = 13.6452(14), c = 13.7271(12) Å, β = 109.436(7)°, V = 2109.1(3) ų] was solved by the direct method and refined to R ₁ = 0. 048 (wR ₂ = 0. 082) for 3677 reflections with |F _hkl |F _hkl |. The structure consists of [(UO₂)₂(SeO₄)₃(H₂O)₂]₂₋ layers arranged parallel to the (010) plane. The layers are formed by uranium and selenium coordination polyhedra sharing common vertices and are linked with each other by hydrogen bonds through the H₂O and H₃O⁺ groups arranged between the layers. __________ Translated from Radiokhimiya, Vol. 47, No. 5, 2005, pp. 412–414. Original Russian Text Copyright ? 2005 by Krivovichev, Kahlenberg.     

Syntheses and structures of Ta2(WO2)0.87H0.26(PO4)4 and Ta2(MoO2)(PO4)4

Tantalum hydrogen phosphate, β-TaH(PO₄)₂, has a three-dimensional structure that is stable to remarkably high temperature (∼600 °C) presumably due to the presence of strong hydrogen bonds. Impedance measurements indicate a low conductivity, 2.0 × 10⁻⁶ S/cm at 200 °C in 5% H₂. In further studies aimed at enhancing the conductivity by aliovalent doping, we have investigated systematically the synthesis of compounds in the TaH(PO₄)₂-W₂P₂O₁₁ system at 380 °C. As a result, a new phase, Ta₂(WO₂)_0.87H_0.26(PO₄)₄, was identified and subsequently the molybdenum analog Ta₂(MoO₂)(PO₄)₄ was also prepared. The structures were determined by single crystal X-ray diffraction techniques. The structures of Ta₂(WO₂)_0.87H_0.26(PO₄)₄ and Ta₂(MoO₂)(PO₄)₄ can be formally derived from the structure of β-TaH(PO₄)₂ by the replacement of two P-OH protons with an MO₂²⁺ (M = Mo and W) group together with a change in the orientation of some phosphate tetrahedra.     

The role of TiO2 and ZrO2 in Na2OMO2SiO2 glasses

The glass transition temperatures of $\text{(1?x)}\text{Na}{}_2\text{O}\text{·}\text{1}\text{2}\text{x}\text{MO}{}_2\text{·2}\text{SiO}{}_2$ and Na₂O·xMO₂·(2 ?x)SiO₂ glasses, with M = Ti or Zr, have been related to the structural role and coordination of Ti and Zr. The role of network-former, intermediate or modifier of a cation has been fundamentally linked to ionic field strength; T_g values depend on ionic field strength and coordination. Titanium behaves like an intermediate oxide; its coordination ranges between four and six, depending on $\text{Ti}\text{Si}$ ratio. The role of zirconium changes according to the degree of substitution for Na or Si and progressively approaches that of a modifier ion.     

超临界流体干燥法制备TiO2/ Fe2O3 和TiO2/ Fe2O3/ SiO2 复合纳米粒子及光催化性能

以TiCl₄ 、Fe (NO₃ )₃·9H₂O 和Na₂SiO₃19H₂O 为原料, 采用溶胶凝胶法结合超临界流体干燥法(SCFD)制备了纳米级TiO₂/ Fe₂O₃ 和TiO₂/ Fe₂O₃/ SiO₂ 复合光催化剂。以光催化降解苯酚对所得催化剂的催化活性进行了评价。结果表明, 纳米TiO₂/ Fe₂O₃ 复合粒子与单组分TiO₂ 比较, 复合粒子光催化活性高于单组分的TiO₂, 6h 苯酚降解率高达95.9 %。SiO₂ 的加入可以抑制纳米粒子粒径的长大和晶相的转变, 增强TiO₂ 纳米粒子的热稳定性。复合光催化剂中Fe₂O₃ 最佳掺入量为0.06 %, SiO₂ 最佳掺入量为10 %(摩尔分数) 。并用XRD、TEM 和FTIR 等手段进行了表征。TiO₂ 以锐钛矿型形式存在, SiO₂ 以无定性形式存在。比较了不同制备方法制得的TiO₂/ Fe₂O₃ 复合光催化剂, 得出超临界干燥法制备的光催化剂具有粒径小、比表面积大、分散性好、光催化活性高等特点。采用超临界流体干燥可直接得锐钛型纳米复合光催化剂。