Synthesis,crystal structure and thermal analysis of a new stilbazolium salt crystal

A new organic crystal of 4-N, N-dimethylamino-4′-N′-methyl-stilbazolium benzene sulfonate (DASBS) was synthesized and characterized for the first time. It is a derivative of 4-N, N-dimethylamino-4′-N′-methyl-stilbazolium tosylate (DAST) with the benzene sulfonate replacing p-toluenesulfonate. Single crystal XRD demonstrated that the crystal structure of DASBS·H₂O was triclinic. The thermal analysis of this new crystal was also conducted, and the melting point was obtained to be 232°C.     

Synthesis and structure of a new cobalt-containing aluminophosphate

We report on the synthesis and single-crystal structure of a novel cobalt-substituted aluminophosphate. Crystal data: monoclinic, space group $\text{P2}{}_1\text{c}$ (no. 14), a = 8.593(1), b = 15.540(1), c = 7.736(1)Å, β = 110.65(1)°, V = 966.7(4)ų, Z = 4, R = 0.037, and R_w = 0.029 for 2280 contributing reflections and 182 variables. Refined framework-atom bond distances and angles exhibited regular tetrahedral coordination of Al and P [d_ave(AlO) = 1.74(1)Å, d_ave(PO) = 1.54(2)Å] and distorted Co-centered octahedra. The Co substituted every second aluminum in the ordered AlP distribution and was coordinated to five framework oxygen atoms and to one nitrogen atom from a template ethylenediamine molecule located in an eight-member ring opening. Structure collapsed in the absence of template.     

含侧甲基液晶双马来酰亚胺的合成及表征

通过甲基对苯二酚和对马来酰亚胺基苯甲酸,制得了一种低熔点的酯类液晶双马来酰亚胺.应用FT-IR、1H-NMR、DSC、HSPM对液晶双马来酰亚胺的结构和液晶行为进行了表征.结果表明,这类液晶双马来酰亚胺具有较低的熔点,侧甲基的存在使得液晶双马来酰亚胺的熔点下降了39℃.由HSPM观察到所合成的液晶单体具有向列型液晶所具有的典型的纹影织构,呈现出较好的热致液晶行为,并且液晶织构可以通过端基的交联聚合反应固定在交联网络中.     

Synthesis,crystal structure and properties of a new lead fluoride borate,Pb3OBO3F

A new compound, Pb₃OBO₃F, has been grown by the high temperature solution method from the PbO–PbF₂–B₂O₃ system. It crystallizes in the orthorhombic system, space group Pbcm with unit-cell parameters a = 7.6313(14) Å, b = 6.5229(12) Å, c = 11.906(2) Å, Z = 4, volume = 592.66(19) Å³. The structure of the compound is solved by the direct methods and refined to R₁ = 0.0528 and wR₂ = 0.1400. Pb₃OBO₃F consists of Pb(1)O₃F tetrahedra, Pb(2)O₄ tetrahedra and BO₃ triangles which build up the symmetrical chains extended along the c-axis. The powder X-ray diffraction pattern of the Pb₃OBO₃F has been measured. Functional groups presented in the sample were identified by Fourier transform infrared spectrum.     

Synthesis and crystal structure of tetramethylammonium fluoride octadecasil

Octadecasil, a clathrate-type inclusion compound, has been synthesized hydrothermally at 453 K with a gel having the composition 1.0SiO₂:0.53tetramethylammonium (TMA⁺):0.54fluoride:86H₂O. The crystal structure has been determined based on powder X-ray diffraction data taken at 298 K, and has been refined using Rietveld method. The result confirms the AST-type, all-silica framework model developed by Caullet et al. [P. Caullet, J.L. Guth, J. Hazm, J.M. Lamblin, H. Gies, Eur. J. Solid State Inorg. Chem. 28 (1991) 345]. Furthermore, by using a rigid body model the position and orientation of the occluded TMA⁺ cation in the rhombododecahedral [4⁶6¹²] cage can be determined; F⁻ anion has been located in the hexahedral [4⁶] cage. The unit cell parameters, in the tetragonal space group I4/m, have been refined as: a = b = 9.07 Å, c = 13.44 Å, cell volume = 1104.97 Å³. The refined unit cell composition is |[N(CH₃)₄⁺]_2.0F⁻_1.9|[Si₂₀O₄₀], i.e., both TMA⁺ and F⁻ ions possess near full occupancies, and compensate each other's electronic charges. The crystallization of the AST framework structure is the result of a cooperative structure-directing effect of both ions.     

Preparation and crystal structure of a new tin titanate containing Sn; Sn2TiO4

Single crystals of a new tin titanate containing Sn²⁺, Sn₂TiO₄ was prepared by high temperature reaction in an evacuated quartz tube and its crystal structure was determined by single crystal X-ray diffraction data. The tin titanate crystallizes in the tetragonal space group P4₂/mbc with a = 8.490(2) and c = 5.923(3) Å, Z = 4 and the final R factors are R = 0.0497 and R_w = 0.0676 for 354 unique reflections. This tin titanate is isostructural with the low temperature form of Pb₃O₄(Pb₂²⁺Pb⁴⁺O₄). This compound was oxidized above 600 °C accompanying the mass gain and finally changed to rutile-type solid solution (Sn,Ti)O₂.     

侧链含芘丁酸酯结构单元的聚氧硅烷合成与氧猝灭特性

采用氢化硅烷化反应，合成了侧链含芘丁酸结构单元的聚氧硅烷荧光高分子。用FTIR和^1HNMR表征了它们的分子结构，采用荧光分光光度计测定了它们在溶液中的激发光谱、发射光谱和氧猝灭系数。结果表明，在聚氧硅烷侧链上引入长链烷烃芘衍生物后，由于侧基上芘环的相互作用，在高波长的受激态发射区（Excimer Emssion）具有强的发射峰，而低波长的分子态发射区（Monomer Emission）的强度较弱。聚氧硅烷荧光高分子对氧气敏感，具有较高的氧猝灭系数，在ME区和EE区的氧猝灭系数分别为59％和54％。随着溶液浓度的降低，在ME区的强度增加，氧猝灭系数增大，而在EE区的强度减弱，氧猝灭系数增加不大。     

Synthesis of PbZr0.7Ti0.3O3 nanoparticles in a new tetragonal crystal structure with a polymer precursor

Nanoparticles (16- to 25-nm diameter) of PbZr_0.7Ti_0.3O₃, lead zirconate titanate (PZT), are synthesized by a controlled reconstructive thermal decomposition and crystallization from an amorphous polymer precursor with polyvinyl alcohol (PVA) and sucrose at 400 to 700 °C in air. When adding through a mixed acidic solution (with stirring) the ingredients of Pb²⁺ (nitrate) and Zr⁴⁺/Ti⁴⁺ (oxyhydroxides) cations mix-up with PVA-sucrose polymer molecules (dissolved in water) and reorganize in a dispersed structure of precursor. A dispersed structure of the cations through the polymer molecules retain on evaporating (at 50 to 80 °C in air) the excess water in a solid polymer precursor. It is found that a single phase compound of PbZr_0.7Ti_0.3O₃ forms on heating it at 400 to 700 °C temperature in air. It has a new tetragonal crystal structure in comparison to the rhombohedral bulk structure in the Zr-rich or the tetragonal structure in the Ti-rich PZTs. The PbZr_0.7Ti_0.3O₃ nanoparticles calcined under selected conditions in this polymorph are characterized by X-ray diffraction and microstructure in correlation with thermal analysis of the polymer precursor.     

Synthesis and photopolymerization kinetics of a photoinitiator containing in-chain benzophenone and amine structure

A photoinitiator HTD bearing in-chain benzophenone (BP) and coinitiator tertiary amine, based on 4-hydroxybenzophenone (HBP), toluene-2,4-diisocyanate (TDI) and N,N-dimethylethanolamine (DMEA), was synthesized and characterized by ¹H-NMR and UV-vis absorption spectroscopy. HTD had longer absorption wavelength in the UV-vis absorption spectra than the low molecular counterpart BP. The kinetics of photopolymerization was studied by real-time Fourier transformation infrared (FTIR) spectroscopy. It showed that HTD was a more effective photoinitiator than BP. When this photointiator was used to initiate polymerization of acrylates, both rate of polymerization and final conversion increased with increase of initiator concentration and light intensity. UV-vis extract analysis showed that the extractability of HTD was much lower than BP/DMEA on the same environment condition.     

Synthesis and photopolymerization kinetics of a photoinitiator containing in-chain benzophenone and amine structure

A photoinitiator HTD bearing in-chain benzophenone (BP) and coinitiator tertiary amine, based on 4-hydroxybenzophenone (HBP), toluene-2,4-diisocyanate (TDI) and N,N-dimethylethanolamine (DMEA), was synthesized and characterized by ¹H-NMR and UV-vis absorption spectroscopy. HTD had longer absorption wavelength in the UV-vis absorption spectra than the low molecular counterpart BP. The kinetics of photopolymerization was studied by real-time Fourier transformation infrared (FTIR) spectroscopy. It showed that HTD was a more effective photoinitiator than BP. When this photointiator was used to initiate polymerization of acrylates, both rate of polymerization and final conversion increased with increase of initiator concentration and light intensity. UV-vis extract analysis showed that the extractability of HTD was much lower than BP/DMEA on the same environment condition.     

端基为磺酸基的希夫碱型侧链聚硅氧烷液晶的合成及表征

首先以对羟基苯甲醛、对氨基苯磺酸合成希夫碱化合物;然后将对羟基苯甲酸、氯乙醇、丙烯酸、含氢硅油通过取代、酯化、硅氢化反应合成聚硅氧烷化合物;聚合物再经过酰化反应后,与希夫碱发生酚解反应合成了目标液晶.通过红外光谱对液晶化合物的结构进行表征,并利用偏光显微镜和DSC测试目标产物的液晶性能.结果表明:此液晶具有近晶A型液晶...     

含长链烷基芘类衍生物的合成与氧猝灭特性

采用酯化反应,合成了系列芘丁酸烷基酯和烷基酸芘丁酯,用IR和1HNMR表征分子结构,采用荧光分光光度计测定了它们在溶液中的荧光特性.结果表明,芘类衍生物的取代基、键桥对激发波长、发射波长和氧猝灭系数的影响较大,以OOC键结方式的烷基酸芘丁酯具有更高的氧猝灭性能,烷基链长短对荧光强度和氧猝灭系数影响不大.     

Synthesis and crystal structure of InP3

Higher indium phosphide InP₃ is obtained under high pressure of 3 GPa at 1200°C. The crystal structure was analyzed to be isomorphous with SnP₃, and GeP₃ having lattice parameters of $\text{a}\text{= 7.449}\text{A}\text{?}$ and $\text{c}\text{= 9.885}\text{A}\text{?}$. InP₃ is a metallic conductor although it is less in the amount of valence electrons than its isomorphous MP₃ of Ge and of Sn.     

The crystal structure of a new ternary silicide in the system rare-earth-ruthenium-silicon

The structural properties of a new group of ternary silicides in the system M-Ru-Si (M = Y, La, Th and RE) have been investigated. The structure is presented as determined from X-ray powder diffraction.     

Synthesis and properties of a new [60] fullerene-donor system containing dicyanovinyl groups

C₆₀ covalently connected with dicyanovinyl functionalized tris[4-(2-thienyl)phenyl]amine [C₆₀-TTPA(DCV)] (compound 1) has been successfully prepared and it was found to exhibit excellent solubility in common organic solvents with a broad visible-light harvest. The theoretical calculation of its molecular geometry and electronic structure indicates that the TTPA(DCV) moiety and C₆₀ part are acting as donor and acceptor respectively; By comparing with the UV-visible absorption spectra of amine 2, the slight red shift of compound 1 could explain the existence of a small portion of charge transport between the two parts; and the fluorescence spectra of compound 1 show that the intramolecular photo-induced electron transfer from the TTPA(DCV) to C₆₀ is the main pathway for the emission quenching.     

Synthesis and crystal growth of new antimony(III)-oxide-iodides

In the system Sb₂O₃1bSbI₃, compounds with Sb₂O₃:SbI₃ ratios of 14:2, 11:2 and 8:2, i.e. Sb₅O₇I, Sb₈O₁₁I₂ and Sb₃O₄I have been synthesized. Colorless single crystals of mm dimensions were grown by vapour transport and characterized by chemical, thermal and X-ray analysis. The latter revealed the existence of at least two more phases with higher iodine contents.     

Synthesis of bulk metallic glass composites using high oxygen containing Zr sponge

The effect of large concentration of oxygen on the microstructural development of Zr–Cu–Al–Ni bulk metallic glass (BMG) alloys, prepared from commercially available Zr sponge, has been studied. Apart from promoting crystallization, increased concentration of oxygen (∼8000 ppm) spawns additional phases. In particular, we report the appearance of α-Zr, dendritic Zr₂Cu phase and the Zr₂Ni type cubic phases. Addition of oxygen scavenger like Yttrium only partially solves the problem. Phase evolution was also found to be sensitive to the cooling rate and hence to the thickness of the cast sample. Thus it is possible to produce a gradient microstructure with predominantly amorphous phase at the outer layer.     

Gd2O2SO4粉体的合成及其晶体结构确定

通过750℃,2h煅烧Gd2O3和H2SO4(摩尔比1:1)的前驱体方法合成了Gd2O2SO4粉体.利用Gd2O2SO4的X射线粉末衍射数据和Material Studio 4.0 Reflex模块中Powder solve技术和Rietveld精修方法对Gd2O2SO4的晶体结构进行了研究.研究表明:Gd2O2SO4具有空间群为PMNB(62)的正交晶系,晶胞参数为a=1.2996nm,b=0.8117nm,c=0.4184nm,V=0.440698nm3,Z=4,计算密度为6.6949g/cm3,并确定了晶胞中原子的位置,Rietveld精修得到的Rwp=9.15%.