Na+对制备Al4SiC4/Al4O4C复合耐火材料的影响

以焦宝石、活性炭和铝粉为原料,添加Na2CO3制备Al4SiC4/Al4O4C复合耐火材料.采用化学分析、XRD和SEM等测试技术,研究了Na+对材料物相组成和显微结构的影响.结果表明:添加Na2CO3加速了Al2O3和活性炭的反应,促进了Al4O4C的生成.未添加Na2CO3时生成的Al4SiC4晶粒表面光滑,添加Na2CO3后Al4SiC4晶粒粗糙、凹凸,缺陷明显增加.此外,未添加Na2CO3的试样中生成的Al4O4C呈短纤维状,添加Na2CO3后全部转变为细小颗粒.     

Surface Order Parameter of 4-n-Heptyl-4′-Cyanobiphenyl

We measured the order parameter near the interface between a liquid crystal and the solid substrate treated by several methods. The interfacial order parameter is different according to the surface treatment, and is larger than the bulk order parameter. Moreover, in the temperature above the clearing point, the interfacial order still has a finite value.     

Liquid Crystalline Phases in 4-Acetyl-4′-n-Alkanoyloxy-Azobenzenes

Abstract

The preparation and melting behaviour of the homologous series of 4-acetyl-4′-n-alkanoylox-azobenzenes, CH₃-CO-C₆H₄-N?N-C₆H₄-O-CO-(CH₂) _n -CH₃, (with n ranging from zero to 16) is reported. The melting behaviour has been investigated by means of thermal microscopy and differential scanning calorimetry. The experimental results indicate for almost all the compounds the presence of solid state polymorphism and a type A smectic; for one compound a type B smectic phase is also present. Some homologs present, in addition, a nematic phase.     

Molecular and crystal structures of 4-acylphenyl 4′-alkyloxybenzoates

The crystal structures of four liquid-crystal (LC) compounds belonging to 4-acylphenyl 4′-alkyloxybenzoates with the general formula C _n H_{2n + 1}-C(O)-C₆H₄-O-C(O)-C₆H₄-O-C _m H_{2m + 1} numbered as 1/6, 1/7,2/7, and 3/7 (the numbers in the code indicate the ratios of the numbers of alkyl-chain units, n/m) are determined. Compounds 1/6 and 1/7 form smectic and nematic phases, but they are monotropic mesogens, whereas compounds 2/7 and 3/7 form only an enantiotropic smectic phase. Compound 3/7 crystallizes in two crystal modifications—triclinic with Z′ = 2 (3/7 _tr ) and monoclinic with Z′ = 4 (sp. gr. P2, 3/7 _mon ). All crystals consist of alternating aromatic and aliphatic regions and are characterized by the presence of weak directional interactions, such as C-H...O hydrogen bonds and π-stacking interactions. This provides the necessary conditions for the formation of a mesophase, and the existence of two types of structure-forming units is in line with the formation of a smectic phase. An explanation is proposed for the monotropic properties of 1/6 and 1/7.     

Crystal and molecular structure of 4′-hexyloxyphenyl 4-pentylbenzoate

The molecular and crystal structure of 4??-hexyloxyphenyl 4-pentylbenzoate, C₆H₁₃O-C₆H₄-COO-C₆H₄-C₅H₁₁, which is a liquid-crystal compound, was determined by X-ray diffraction. This compound forms a nematic phase upon melting. The crystal contains three crystallographically independent molecules. In one of them, the alkyl chain is disordered. This is indicative of the looseness of the crystal packing in the aliphatic region. The crystal structure is stabilized by the following two types of weak directional interactions: hydrogen bonds with the participation of the terminal O atom of the ester group and the C-H group of one of the benzene rings and C-H????-system interactions. Only one of the three independent molecules is involved in the latter type of interactions. Hence, the structurization of the mesophase is most likely determined by hydrogen bonding.     

New Crystals in the CsHSO4–CsH2PO4–NH4H2PO4–H2O System

Crystallography Reports - The phase equilibria in the CsHSO4–CsH2PO4–NH4H2PO4–H2O four-component aqueous salt system have been studied. The crystallization ranges and solubilities...     

X-ray diffraction study of mesogenic 4-methoxyphenyl-4′-n-nonyloxybenzoate

4-methoxyphenyl-4′-n-nonyloxybenzoate have been investigated by single crystal X-ray structural analysis. Crystal packing of the compounds does not represent a precursor of the mesophse although the typical for liquid crystal compounds separation of crystal packing on aromatic and aliphatic areas is observed here. Possible reason for monotropic properties are discussed.     

Crystal Structure of 3′-(4-Methoxyphenyl)-2-Phenyl-4′-(4-Ethoxyphenyl)-1,2-Dihydro-4H,4′H-Spiro [Isoquinoline-3,5′-Isoxazol]-4-One

The title compound, 3′-(4-methoxyphenyl)-2-phenyl-4′-(4-ethoxyphenyl)-1,2-dihydro-4H,4′H-spiro[isoquinoline-3,5′-isoxazol]-4-one was synthesized from the reaction of dipolarophile with p-methoxybenzadoxime in the presence of sodium hypochlorite in chloroform solution. The structure of the synthesized compound was determined by IR, ¹H NMR, mass spectroscopic data, ¹³C NMR spectroscopy, elemental analysis and X-ray crystallography. The structure was solved in monoclinic, space group C2/c with a = 21.941 (4), b = 17.233 (3), c = 15.404 (3) Å, β = 122.193 (2), V = 4928.9 (16) Å³, Z = 8 and with R_int = 0.154. The geometry of the title compound showed that the piperidine ring adopts a half-chair conformation. In the crystal structure, molecules are linked by C–H···O and C–H···N contacts. Weak C–H···π interactions plays an important role in stabilizing the supramolecular structure.     

熔盐法合成片状SrBi4Ti4O15粉体

采用NaC l-KC l熔盐法合成了生长各向异性的片状SrB i4Ti4O15粉体,用XRD分析了粉体相的结构,用SEM观察了粉体的微观形貌,讨论了不同预烧温度对合成物结构和微观形貌的影响。与固相法相比,熔盐法合成的粉体具有(00l)择优生长的优点。在850~1050℃之间,合成粉体的片状结构趋于明显,粉体生长各向异性随温度的升高呈现出先增加后减小的趋势,各向异性明显的SrB i4Ti4O15粉体的最佳合成温度为900~1000℃。     

Elastic and Optical Properties of Some 4′-n-Alkyl-4-Cyanobiphenyls

The bend elastic constants (k ₃₃) and order parameters (S) derived from optical measurements in the nematic phase of pentlyl, hexyl, heptyl and octyl cyanobiphenyls (5CB, 6CB, 7CB and 8CB respectively) are reported. The odd-even effect is clearly seen in the K ₃₃ values of all four compounds and in the S values of the first three. 5CB, 6CB and 7CB show only the nematic mesophase but their elastic constants indicate the existence of smectic-like short range order. For example, even the lowest homologue, 5CB, does not obey the law k ₃₃ ∞ S ² given by the mean field throry. 7CB, has about the same order parameter as 5CB but a much higher elastic constant. 8CB, which shows a smectic A phase as well, exhibits a lower k ₃₃ than 7CB near the nematic-isotropic transition point but a pronounced pretransitional increase near the A-N transition.     

梯度掺杂的YVO4-Nd∶YVO4复合晶体

利用改进的提拉法生长了一种新型YVO₄-Nd∶YVO₄ 复合晶体,在晶体中部实现了Nd³⁺的0.10%~0.25%(原子数分数)浓度梯度掺杂。晶体中, Nd³⁺掺杂区的弱吸收系数较未掺杂区大,表现出界面吸收现象。观测了复合晶体对泵浦光的吸收和温度分布,发现晶体沿轴向的泵浦吸收相对均匀,温度梯度相对较小。未镀膜的复合晶体样品在1 064 nm波段显示了良好的连续激光性能,光-光转换效率为37.0%,斜效率为40.9%。     

Structure of a liquid crystal of 4-cyano-4′-n-octyloxybiphenyl

The structure of a liquid crystal of 4-cyano-4′-n-octyloxybiphenyl (C₂₁H₂₅NO) is determined by X-ray diffraction analysis. The compound crystallizes in the triclinic crystal system with unit cell parameters a = 7.322(1) Å, b = 12.693(3) Å, c = 20.393(2) Å, α = 92.45(1)°, β = 99.96(1)°, γ = 99.35(2)°, and space group $P\bar 1$ . The structure is solved by the direct method and refined to R = 0.057. Two independent molecules are located in the asymmetric unit. No short intermolecular contacts are observed in the crystal packing.     

YVO4晶体缺陷分析

运用同步辐射白光X射线形貌术分析了YVO4的结构和缺陷行为,也观测了YVO4晶体(001)、(100)面的缺陷.发现在(001)面出现应力生长区、沿[100]方向的位错线以及晶体中镶嵌结构.运用白光形貌术拍摄到的劳埃斑,证明晶体为四方晶系.确定了小角晶界是引起多晶的主要原因.采用电子探针仪分析了散射颗粒形成是由杂质铁和铝的引入造成.     

4H-SiC同质外延生长及Ti/4H-SiC肖特基二极管

利用台阶控制外延生长技术在偏晶向Si-面衬底上进行了4H-SiC的同质外延生长研究,衬底温度为1500℃,在厚度为32μm、载流子浓度为2～5×1015cm-3的外延材料上制备出了反向阻塞电压大于1kV的Ti/4H-SiC肖特基二极管,二极管的正向与反向电流的整流比(定义偏压为±1V时的电流比值)在室温下超过107,在265℃的温度下超过102,在20～265℃的温度范围内,利用电流电压测量研究了二极管的电学特性,室温下二极管的理想因子和势垒高度分别为1.33和0.905eV,开态电流密度在2.0V的偏压下达到150A/cm2,比开态电阻(Ron)为7.9mΩ·cm2,与温度的关系遵守Ron～T2.0规律.     

ZrSiO4∶Mn4+荧光粉的制备及光谱性能

采用固相反应制备了不同浓度Mn⁴⁺掺杂的硅酸锆粉末,研究了Mn⁴⁺对硅酸锆光致发光性能的影响。采用XRD表征 ZrSiO₄∶Mn⁴⁺的结构,结果显示在1 400 ℃粉末已被完全合成。研究了不同掺杂浓度下ZrSiO₄∶Mn⁴⁺粉末的光谱性能,在0.3%Mn⁴⁺掺杂浓度(摩尔分数)下,其发光性能最好。在激发谱中,位于363 nm的峰是由O^2--Mn⁴⁺的电荷迁移带和自旋允许的Mn⁴⁺的⁴A₂-⁴T₁的能级跃迁叠加产生的,而450 nm的激发峰则是因为Mn⁴⁺的⁴A₂-⁴T₂能级跃迁导致的。发射谱中的最强峰位于667 nm,这是由Mn⁴⁺的²E-⁴A₂的能级跃迁产生的,还有一个位于698 nm的峰则是由于反斯托克斯声子边带发射造成的。测试了ZrSiO₄∶Mn⁴⁺粉末的荧光衰减曲线,Mn⁴⁺离子浓度为0.1%时寿命为0.204 1 ms。结果表明,ZrSiO₄∶Mn⁴⁺粉末拥有良好的发光性能,是一种有望应用于白光LED的荧光粉。     

Synthesis and Some Properties of 3-Fluoro-4-Cyanophenyl 4′-n-alkylbenzoates

A series of 3-fluoro-4-cyanophenyl 4′-n-alkylbenzoates, which show monotropic nematic phases, was prepared and their transition temperatures and melting enthalpies were measured. The 3-fluoro-4-cyanophenyl 4′-n-propylbenzoate, 3-chloro-4-cyanophenyl 4′-n-propylbenzoate and 4-cyanophenyl 4′-n-propylbenzoate were mixed with a nematic mixture (A) of 4-n-alkoxyphenyl 4′-n-alkylcyclohexane-1′-carboxylates. 3-Fluoro-4-cyanophenyl 4′-n-propylbenzoate decreases the N-1 transition temperature less, increases the birefringence more, and increases the bulk viscosity less than 3-chloro-4-cyanophenyl 4′-n-propylbenzoate, and reduces the threshold voltage to the greatest extent. The dielectric anisotropies of 3-fluoro-4-cyanophenyl 4′-n-propylbenzoate and 4-cyanophenyl 4′-n-propylbenzoate determined from a series of solutions of the compounds in nematic mixture (A) are 35.9 and 29.6, respectively.     

The Metabolemeter III: Phase Behaviour Under Pressure of bis-(4-4′-n-Heptyloxybenzylidene)- 1, 4-Phenylenediamine and Terephthalylidene-bis-(4-n-Decylaniline)

By using a metabolemeter, the phase transitions of bis-[4, 4′-n-heptyloxybenzylidene]-1, 4 phenylenediamine (HBPD) and terephthalylidene-bis-[4-n-decylaniline] (TBDA) have been studied. The weakly first order phase transitions (S_G-S_F and S_F-S_I) and the narrowly separated phase transitions (S_C-S_A and S_A-I) of TBDA are detectable. For HBPD, both transitions S_G-S_I and S_I-S_C are individually observed and the enthalpy changes are deduced from pressure increments at the tranformations: two triple points are detected, one directly by a change of slope in the drawing of the equilibrium curves. The pressure-temperature phase diagrams are given; for each transiton, the volume increases on increasing the temperture.