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.     

NiFe2O4/g-C3N4的制备及可见光催化降解甲基橙

采用浸渍法制备不同负载量NiFe2 O4的负载型光催化剂NiFe2 O4/g-C3 N4,利用XRD、FT-IR、N2-adsorption、ICP-OES、TEM及XPS等手段表征NiFe2 O4/g-C3 N4样品,并考察其对甲基橙的可见光催化降解性能.结果表明,与NiFe2 O4和g-C3 N4样品相比,负载型NiFe2 O4/g-C3 N4样品对甲基橙具有更好的光催化降解活性,且催化活性随着NiFe2 O4负载量增大(0.5~5.0wt;)而呈现先增大再减小的趋势.NiFe2 O4负载量2.0wt;的样品2-NiFe/CN在可见光照射下对浓度5 mg·L-1的甲基橙表现出最好的降解活性和稳定性.这是因为能带宽度小(1.5 eV)的NiFe2 O4与能带宽度大(2.7 eV)的g-C3 N4形成的异质结催化剂NiFe2 O4/g-C3 N4,有效地促进光生载流子在二者界面快速传递和光生电子-空穴对的有效分离.     

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。     

The Synthesis of Fluorine Containing Phenyl Benzoates and Their Properties as Liquid Crystals

A new series of fluorine containing phenyl benzoates has been synthesized and the transition temperatures of these compounds have been determined. A series of 4-trifluoromethylphe 4nyl 4-n-alkybenzoates showed no liquid crystalline behaviour, but the 4-trifluoromethylphenyl 4-n-alkoxybenzoates series, with six carbons or more in alkoxy chain, was mesomorphic. The 4-cyanophenyl 4-perfluoroalkylbenzoates showed smectic liquid crystalline properties.     

非线性光学晶体δ-LiZnPO4的制备、结构及光学性能

研究了LiF为助熔剂体系下的δ-LiZnPO4的结晶特性,通过自发结晶得到了尺寸为1~3 mm的透明块状δ-LiZnPO4和Li4Zn(PO4)2共晶体,通过PXRD衍射分析和元素分析确定了共晶体的相组成,并对从共晶体中分离出的δ-LiZnPO4晶体结构进行了分析.结果表明:δ-LiZnPO4晶体具有非中心对称结构,属于正交晶系,空间群为Pna21,晶格常数a=1.00085 nm,b=0.49390 nm,c=0.66545 nm,Z=4;δ-LiZnPO4是由PO4、ZnO4和LiO4四面体构筑成的具有类似ABW型分子筛结构的化合物.采用水热法制备了尺寸约为10 μm的纯相透明的δ-LiZnPO4晶体.粉末倍频测试表明,δ-LiZnPO4晶体倍频效应约为KDP的1.7倍,紫外截止边约为218 nm,是一种有潜在应用价值的紫外非线性光学晶体.     

New compounds with re-entrant nematic phases

Some derivatives of the homologous series of 4-cyanophenyl-3-methyl-4-(4-n-alkoxycinnamoyloxy) benzoates and of 4-cyanophenyl-4-(4-n-alkoxy-α-methyl cinnamoyloxy) benzoates have been synthesises. The higher homologs of these series exhibit reentrant nematic phases at atmospheric pressure.     

Reentrant nematic phase with the new pentamorphism n sa sc nre sare in a mixture

Three homologues of the new series 4 - cyanobenzylidene - 4′ - [4″ - alkoxybenzoyloxy] anilinie are presented. One of them exhibits a reentrant nematic and a reentrant smectic A phases. A diagram of state with 4 - cyanobenzylidene - 4′ - [4″ - decyloxybenzoyloxy] aniline and 4 - [4″ - decyloxybenzoyloxy] benzylidene - 4′ - cyanoaniline has been studies. In the system studies, the following new phase sequence was found with decreasing temperature N S_A S_C N S_A.     

溶胶-凝胶法制备Ca0.4Sr0.6Bi4Ti4O15细晶陶瓷

采用凝胶预碳化处理工艺制备了颗粒粒径较小,无硬团聚的Ca0.4Sr0.6Bi4Ti4O15纳米粉体,以Ca0.4Sr0.6Bi4Ti4O15非晶团簇粉体为陶瓷素坯的原料,同组分高浓度的Ca0.4Sr0.6Bi4Ti4O15溶胶为粘结剂,制备了Ca0.4Sr0.6Bi4Ti4O15细晶陶瓷,研究了Ca0.4Sr0.6Bi4Ti4O15粉体的相结构和微观形貌以及陶瓷的显微结构和铁电性能.实验结果表明:700 ℃焙烧粉体呈现为非晶团簇,800 ℃焙烧粉体形成了纯层状钙钛矿结构,粒径在100～150 nm之间,无硬团聚;950 ℃烧结的Ca0.4Sr0.6Bi4Ti4O15细晶陶瓷结构致密,晶粒尺寸在0.2～0.5 μm之间,其铁电性能优良,剩余极化Pr=12.5 μC/cm2,矫顽场强Ec=50 kV/cm.     

The utility of 4-aminobenzoic acid in promotion of hydrogen bonding in crystallization processes: the structures of the cocrystals with halo and nitro subsituted aromatic compounds, and the crystal structures of the adducts with 4-nitroaniline (1:1), 4-(4-nitrobenzyl)pyridine (1:2), and (4-nitrophenyl)acetic acid (1:1)

A number of molecular adducts of 4-aminobenzoic acid (4-ABA) have been prepared and characterized using infrared spectroscopy and in three cases by X-ray diffration methods. These three compounds are with 4-nitroaniline [(4-ABA) (C₆H₆N₂O₂)], 4-(4-nitrobenzyl) pyridine, [(4-ABA)₂(C₁₂H₁₀N₂O₂)₄], and (4-nitrophenyl)acetic acid, [(4-ABA) (C₈H₇NO₄)]. Other compounds described are with 4-chlorobenzoic acid, [(4-ABA) (C₇H₅ClO₂)], 4-bromobenzoic acid, [(4-ABA) (C₇H₅BrO₂)], 4-cyanobenzoic acid, [(4-ABA) (C₇H₆N₂)], 2-nitrobenzoic acid, [(4-ABA) (C₇H₅NO₄)], and 3-nitrobenzoic acid, [(4-ABA) (C₇H₅NO₄)]. All compounds have 1:1 stoichiometry except that with 4-(4-nitrobenzyl)pyridine (1:2) which is unique in being retro-stoichiometric. A review of the systematics of the 4-aminobenzoic acid adducts is also made, particularly with respect to the infrared characterization of the cocrystalline materials and prediction of their NLO potential.     

NH4H2PO4晶体反铁电相的对称性及序参量

在反铁电晶体NH4H2PO4(ADP)顺电反铁电相变中,对称性所属点群也随之发生相应的改变.通过对实验结果的分析,我们认为NH4H2PO4(ADP)晶体反铁电相对称性所属点群为P2(C2).选用轴矢量R作为序参量来描述NH4H2PO4(ADP)晶体反铁电相变中对称性的变化,应用居里原理,恰能得到NH4H2PO4(ADP)晶体反铁电相的正确对称性所属点群P2(C2).     

GdVO4晶体的生长及其性能研究

采用提拉法沿a轴和c轴生长出无色透明的GdVO4单晶,质量均超过50g.用X射线荧光分析法测得两个主要元素Gd和V的分凝系数都接近1.室温下测量了GdVO4晶体的X射线粉末衍射图,确定所获GdVO4晶体属于四方晶系,D194h-I41/amd空间群.通过晶体的锥光干涉图确定GdVO4晶体为单轴晶,光轴方向平行于c轴且光学均匀性比较好.利用高分辨X射线衍射仪测量GdVO4晶体的摇摆曲线,结果表明生长的GdVO4晶体的晶格完整性较好.通过浮力法测得其室温下密度为5.478g/cm3.透过波谱表明透过波长大于340nm.     

不同磷源制备磷酸铋及其光催化性能研究

三种不同磷源在超声作用下制备磷酸铋,磷酸氢二钠为磷源制备棒状磷酸铋,咪唑磷酸盐离子液为磷源制备梭状磷酸铋,三乙烯四胺磷酸盐离子液为磷源制备颗粒状磷酸铋.XRD表征分析表明三乙烯四胺磷酸离子液为磷源制备的磷酸铋衍射峰最高,咪唑磷酸盐离子液制备磷酸铋次之,磷酸二氢钠制备的磷酸铋衍射峰最低.紫外-可见分析表明离子液中合成的磷酸铋向低波数发生移动.BET分析表明在磷酸二氢钠、咪唑磷酸盐、三乙烯四胺磷酸盐中合成的磷酸铋的比表面积分别为3.9472 m2/g,11.548 m2/g和24.063 m2/g.三种磷酸铋在紫外光下对亚甲基蓝匀有光催化作用,其中三乙烯四胺磷酸盐离子液为磷源制备的磷酸铋光催化性能最佳,同时考察了三乙基四胺磷酸盐离子液制备磷酸铋以及光催化的条件.     

钴铁氧体亚微米球吸波性能与成分的关系研究

用溶剂热方法制备CoxFe3-xO4 (0≤x≤1)亚微米球, 可看作不同比例Fe3O4和CoFe2O4的混合物.实验发现:当原料中钴铁原子比为1∶1、1∶2、1∶4和0时,反应得到的球分别为CoFe2O4、Co0.9Fe2.1O4、Co0.73Fe2.27O4和Fe3O4.Fe3O4与石蜡混合物(质量分数75wt;)厚度为5.5 mm时,反射率最低为-38 dB,对应频率为4 GHz;Co0.9Fe2.1O4与石蜡混合物在3~14 GHz频率范围内介电损耗大于磁损耗,计算出来的反射率分贝值(-41.1 dB,12.08 GHz,2 mm)低于相关报道.比较四种成分的钴铁氧体球可以看出:当x值不同时,由于成分Fe3O4和CoFe2O4的自然共振频率不同,引起磁性能随微波频率发生变化,而且由于二价铁离子被钴离子取代,结晶性也发生改变,进而改变了材料的介电和吸波性能.     

基于聚合反应制备的钛离子掺杂LiFePO4/C复合材料

首先基于聚合反应合成FePO4/PANI前驱体,再以为LiOH·H2O,FePO4/PANI 和 PVA原料制备了LiFePO4正极材料,此外再对其进行碳包覆以及Ti4+掺杂,三种试样分别标记为LiFePO4,LiFePO4/C及LiFe0.96Ti0.02PO4/C.通过XRD、EDS及充放电测试等手段表征了材料的微观结构与电化学性能.实验结果证明:试样的XRD图谱均与标准LiFePO4图谱一致,不存在无定形碳衍射峰.与未掺杂试样LiFePO4/C相比,LiFe0.96Ti0.02PO4/C的电子电导率与其相近,但离子扩散系数有所改善,Ti4+在晶格中均匀分布,因此与其他两试样相比,其电化学性能更好.试样在C/10、C/2、1C、3C及5C倍率下的放电比容量为158.7 mAh·g-1、153.3 mAh·g-1、147.6 mAh·g-1、136.4 mAh·g-1及123.5 mAh·g-1,具有良好的倍率性能与电位稳定性.     

Stable Liquid Crystals with Large Negative Dielectric Anisotropy - III

The synthesis of 4-n-pentyl and 4-n-butoxy derivatives of 1-(2,3-dicyano phenyl)-2-(4-(4-trans-n-pentyl cyclohexyl)phenyl) ethane and 1-(2,3-dicyano phenyl)-2-(4-trans-n-pentyl-4-trans-bicyclohexyl) ethane as well as of 1-(4-n-butoxy-2,3-dicyano phenyl) -2-(4-n-pentyl-4-biphenyl) ethane is described. These ethane derivatives as well as 4-butoxy-2,3-dicyano-4-n-pentyl p-terphenyl were all high melting and no enantiotropic or monotropic mesophases could be observed. However, they can be used as additives for photochemi-cally stable LC mixtures with low viscosity and large negative Δσ. The mesomorphic properties of some intermediate thiophene and furan derivatives are described.     

草酸根作用下Co3O4八面体的控制合成

在草酸根的作用下,采用水热法合成了暴露八个(111)晶面的Co3 O4八面体.采用XRD、SEM、TEM和HRTEM等手段对产物进行了表征和分析,结果表明该Co3 O4八面体呈立方晶相且具有很高的结晶性.详细研究了反应时间、反应温度、草酸根浓度等反应条件对Co3 O4形貌的影响.研究表明草酸根可选择吸附在Co3 O4的(111)晶面,通过其较大的空间位阻限制(111)晶面的生长,从而使该晶面得以最终暴露.由于(111)晶面具有较高的能量,该Co3 O4八面体具有良好的高氯酸铵(AP)催化热分解性能.     

ZnWO4-ZnO复合光催化剂的制备及光催化性能

以ZnO及WO3为前驱反应物,制备了一系列不同ZnWO4含量的ZnWO4-ZnO复合光催化剂.利用X射线衍射、扫描电子显微镜及X射线能谱仪等手段对催化剂进行表征,并以紫外光为光源,罗丹明B为模拟污染物,评价催化剂的活性.结果表明,热处理温度及ZnWO4与ZnO摩尔比对催化剂光催化降解罗丹明B的活性影响显著.当复合4mol;ZnWO4,并于850 ℃煅烧所制得的ZnWO4-ZnO催化剂活性最高,比纯ZnO高出25;.这是因为ZnWO4的复合可抑制ZnO晶粒长大,提高光生电子与空穴的分离效率,进而改善其光催化活性.     

Synthesis and Structure of Uranyl Succinate Complexes with Cyanoguanidine and Diethylacetamide

Crystallography Reports - [UO2(suc)(C2N4H4)2] · 2H2O (I) and [UO2(Deaa)4(H2О)][(UO2)2(C4H4O4)3] · 2Deaa (II) crystals (suc2– is succinate ion, C2N4H4 is cyanoguanidine, and...     

Mg3N2在生成hBN反应中的催化作用

研究了Mg3N2在B4C和NH4Cl于常压高温下生成hBN反应中的作用,用红外光谱仪和X射线衍射仪对反应产物进行分析,实验结果表明,在950℃和N2气环境下,Mg3N2与B4C反应不成生成hBN,B4C与NH4Cl反应生成少量hBN,在B4C和NH4Cl中加入Mg3N2后hBN的生成量明显增加,说明高温高压下合成cBN的常用催化剂Mg3N2,在常温压高温生成hBN的反应表现催化作用。     

The Synthesis and Physical Properties of Some 1-n-Alkyl-4-(4-substituted phenyl) bicyclo(2.2.2)octanes

The preparation and mesomorphic properties of a number of 1-n-alkyl-4-(4-n-alkyl- and 4-n-alkoxy-phenyl)bicyclo(2.2.2)octanes and 1-n-alkyl-4-(4′-n-alkylbiphenyl-4-yl)bicyclo(2.2.2)octanes are described. The clearing temperatures reported emphasise the high thermal stability conferred upon liquid crystal phases by the presence of the bicyclo-octane ring in a mesogen. Some physical data relating to the use of such materials in mixtures for electro-optical displays have been obtained.