糯米浆对仿生碳酸钙形貌的影响

以糯米浆为有机调控物质,二氧化碳提供碳源仿生制备出多种形貌的碳酸钙晶体.探索了矿化时间、钙离子浓度对碳酸钙晶体形貌和晶型的影响.采用扫描电子显微镜(SEM)、傅里叶红外光谱仪(FT-IR)和X射线衍射仪(XRD)对制备的碳酸钙表观形貌及结构进行表征.扫描电镜结果表明:以糯米浆为有机调控物质,钙离子浓度和矿化时间对碳酸钙晶体的形貌有一定的影响;XRD及FT-IR图谱表明制备的碳酸钙晶型为方解石和球霰石.     

硅酸钠和重烷基苯磺酸盐对碳酸钙物相和形貌的影响

研究了硅酸钠及重烷基苯磺酸盐(HABS)对碳酸钙晶型和形貌的影响,采用FESEM、XRD和FT-IR等手段,对获得的产物进行了表征.结果表明,硅酸钠可促进不同形貌和不规则聚集体状碳酸钙的形成;当硅酸钠浓度大于250 ppm时,可以抑制部分无定形碳酸钙向方解石的转化;当HABS与硅酸钠同时存在时,优先形成麦穗状方解石.     

L-天冬氨酸诱导叠层碳酸钙微晶的形成

利用气相扩散的方法得到一种特殊形貌的碳酸钙层状聚集体.探讨了L-天冬氨酸的浓度、反应时间对碳酸钙的形貌和晶型的影响.采用扫描电镜(SEM)、X射线粉末衍射(XRD)及红外吸收光谱(FT-IR)对合成出的样品的形貌、结构进行了表征.结果表明:L-天冬氨酸的浓度及反应时间对碳酸钙的形貌和晶型有着重要的影响,并对L-天冬氨酸浓度影响碳酸钙的形貌和晶型的机理进行了解释.     

水溶性壳聚糖/鸡蛋清对仿生碳酸钙晶体形貌的控制

在水溶性壳聚糖/鸡蛋清的调控下,采用气相扩散法仿生制备出多种形貌的碳酸钙晶体.研究了Ca2+起始浓度、m壳聚糖∶ m鸡蛋清质量比对碳酸钙形貌和晶型的影响.采用扫描电子显微镜(SEM)、红外光谱(FT-IR)及X射线衍射(XRD)等测试技术对获得的碳酸钙样品进行表征.XRD及FT-IR结果表明所得碳酸钙包括方解石和球霰石两种晶型,SEM观察表明Ca2+浓度及m壳聚糖∶m鸡蛋清质量比对碳酸钙形貌有重要的调控作用.     

水热条件下黄磷炉渣废料制备碳酸钙晶须

本文采用黄磷炉渣制备白炭黑后的残留废液为原料,尿素作为沉淀剂制备碳酸钙晶须,系统研究了晶型控制剂(MgCl2)的浓度、反应温度、反应时间、尿素和残留废液的体积比等因素对碳酸钙晶须形貌和物相组成的影响,所得产品通过X射线衍射、扫描电镜进行了分析与表征.研究结果表明,反应温度140℃,反应时间3 h,(NH2)2CO:CaCl2体积比为1:3,晶型控制剂为0.3 mol/L的条件之下,可获得平均长度在50 p.m,长径比为10左右的碳酸钙晶须.     

碳酸钙晶须的制备及含硫化合物对碳酸钙晶须影响的研究

在碱性环境下(pH＞ 12)采用衬底溶液双滴加法制备了形貌均匀且长径比大于10的文石型碳酸钙晶须.探讨了衬底液浓度、温度等因素对碳酸钙晶须生长的影响;研究了硫化钠、硫酸钠、硫代硫酸钠对碳酸钙晶须生长过程的影响;通过扫描电子显微镜和X射线衍射对样品的形貌和物相进行了表征.结果表明:衬底液Ca2+浓度为0.4 mol/L、温度为80 ℃时最有利于文石型碳酸钙晶须的生长;随着含硫化合物的增加,文石型碳酸钙晶须的长径比与质量分数均逐渐减小,且方解石型碳酸钙含量逐渐增加.     

温度对钛酸盐纳米管水热转化的TiO_2纳米晶形貌演变的影响机制

钛酸纳米管水热转化是制备晶相组成和形貌可调控TiO2纳米晶的工艺易控及成本低且收率高的途径。本文研究了两种pH值体系中,水热处理温度对钛酸纳米管水热转化的TiO2纳米晶形貌演变的影响。当钛酸悬浮液的pH值为2.0时,钛酸纳米管水热转化为锐钛矿相纳米晶,且随着水热温度的升高,纳米晶的形貌向规则的双锥形演变;对于pH为0.5的强酸性体系,钛酸纳米管水热转化为金红石相纳米棒,并随着水热温度的升高,其形貌向带有两锥形尖端的长方体纳米棒演变。最后,结合TEM和HRTEM分析,探讨了钛酸纳米管向不同晶相组成和形貌的TiO2纳米晶的水热转化及其形貌演变机制。     

硫酸软骨素/L-谷氨酸对碳酸钙形貌及晶体生长影响的研究

根据生物矿化原理,通过CO2的缓慢扩散,在硫酸软骨素(CSB)/L-谷氨酸二元体系中,与富集在有机/无机界面钙离子的结合,合成了不同形貌的碳酸钙.系统地研究了室温下各种因素对碳酸钙晶体形貌和晶型的影响.产物用XRD、SEM和FT-IR进行表征,FT-IR和XRD分析表明:所得的晶体为方解石的晶型,SEM表明体系中CSB的浓度,pH值,CSB/L-谷氨酸的浓度比对碳酸钙形貌起着重要作用.通过改变实验条件得到了椭球型,哑铃型等形貌碳酸钙晶体,并对其可能的形成机理进行了分析.     

球形方解石的合成和表征

25℃下,用豆腐废水作为碳酸钙形貌调节剂,用Na2 CO3和CaCl,·6H2O作为原料合成碳酸钙,研究豆腐废水对产物组成和粒子形貌的影响.用粉末X-射线衍射仪(XRD)和红外光谱仪(FT-IR)对合成的产品晶型进行了表征,用扫描电子显微镜(SEM)观察研究粒子的形貌.研究结果显示,合成得到的产物是纯的方解石,粒子的形状是球形的或者是接近球形的.结果 说明,豆腐废水虽然不会影响碳酸钙的晶型,但是会影响碳酸钙粒子的形貌.     

电石渣可控制备多晶型、多形貌纳米碳酸钙的研究进展

碳酸钙有不同的晶体特征，使其在各个领域发挥不同的作用，对碳酸钙晶型、形貌和尺寸的控制是无机材料制备的研究热点。以电石渣为原料制备纳米碳酸钙能够实现变废为宝，是含钙固废综合利用的研究方向之一。因此在电石渣制备纳米碳酸钙过程中同步实现晶型、形貌的调控，能够将低附加值的电石渣固废转化为高附加值的纳米碳酸钙产品，具有良好的环境效应和经济效益。本文总结了电石渣制备纳米碳酸钙的方法，重点讨论了制备过程中晶型和形貌控制方面的研究进展。结果表明，在碳酸钙晶体成核和生长的过程中，控制工艺条件可以通过影响过饱和度进一步实现对晶型和形貌的调控，且不同种类的添加剂作用机理也不尽相同。热力学、动力学作为控制结晶各过程平衡的基础，可以用来解释各影响因素的作用机理。     

Syntheses and structures of N-phenylmaleimidetriazoles and by-products

The syntheses, properties, and structures of N-phenylmaleimidetriazole derivatives are described. Intermediates and by-products are also discussed. 1b. a = 43.997(7) Å, 5.7610(9) Å, 8.245(1) Å, = 99.339(4), C₂/c; 2a. a = 13.646(4) Å, b = 7.744(2) Å, c = 10.612(3) Å, = 91.979(6), P2₁/c. 3a. a = 22.245(1) Å, b = 22.245(1) Å, 10.010(1) Å, P42/n. 3a. a = 11.727(2) Å, b = 14.075(3) Å, c = 16.080(3) Å, = 105.859(3), = 105.331(3), = 98.187(3), P-1. 3b. a = 8.561(3) Å, b = 14.755(5) Å, c = 22.771(7) Å, = 97.006(5), P2₁/c. 3c. a = 10.500(2) Å, b = 12.189(2) Å, c = 13.040(2) Å, = 109.091(3), = 106.089(3), = 101.022(3), P-1. 8a. a = 16.389(8) Å, b = 5.749(3) Å, c = 19.316(3) Å, = 97.467(9), P2₁/n. 8b. a = 5.822(2) Å, b = 10.114(3) Å, c = 16.705(4) Å, = 84.681(5), = 82.840(5), = 75.769(4), P-1. 9b. a = 11.251(1) Å, 13.335(3) Å, 13.376(3) Å, = 102.456(4), P2₁/n. 9c. a = 15.836(3) Å, b = 8.236(2) Å, c = 5.447(3) Å, = 92.551(3), P2₁/c. 10a. a = 13.177(2) Å, b = 14.597(2) Å, c = 5.5505(8) Å, = 110.979(2), Cc. 11a. a = 14.720(2) Å, b = 13.995(2) Å, c = 38.245(6) Å, = 94.430(3), P2₁/n. 12b. a = 15.067(5) Å, b = 20.378(6) Å, c = 8.669(5) Å, = 99.16(4), = 99.32(3), = 105.23(3), P-1. 13b. a = 8.2824(6) Å, b = 10.5245(7) Å, c = 15.518(1) Å, = 92.305(1), = 100.473(1), = 100.124(1), P-1. 15a. a = 15.357(3) Å, b = 7.778(2) Å, c = 22.957(2) Å, Pbca. 16b. a = 18.0384(4) Å, b = 12.474(3) Å, c = 20.078(5) Å, Pbca.     

Sol-gel synthesis and characterization of adsorbent and photoluminescent nanocomposites of starch and silica

Using sol-gel method, mesoporous and photoluminescent silica nanocomposites of soluble starch have been synthesized and characterized. Different ratios of H₂O, TEOS and EtOH were used at fixed template (soluble starch) and catalyst (NH₄OH) concentrations to obtain materials of different performances in terms of heavy metal binding from a solution which has been monitored using Cd(II) as representative divalent heavy metal ion. Optimum material was obtained when H₂O, TEOS and EtOH were used in 14:1:2 ratio. This sample was not only an efficient metal ion adsorbent but also had an intense luminescence in ultra-violet region and potentially may be used in silicon-based UV-emitting devices. Metal binding by the material was further enhanced after calcination (at 800 °C in air) while its luminescence had a multipeak profile in UV-visible region. In a batch adsorption study, calcined hybrid composite (0.25 g/L) could remove 98.5% Cd(II) from 100 mg/L Cd(II) solution in 2 h. The chemical, structural and textural characteristics of the synthesized materials have been investigated using Fourier Transform Infrared Spectroscopy (FTIR), X-rays Diffraction (XRD), Thermal Analysis (TGA/DTA), Photoluminescence (PL), Brunauer-Emmett-Teller Analysis (BET) and Scanning Electron Microscopy (SEM).     

Chemistry and Electrocrystallization of Organic Metals and Superconductors

Abstract

Considerable variation in the conditions of electrochemical crystal growth of TMTSF₂X (i.e., constant current versus constant potential, ambient versus inert atmosphere, etc.) and in the purity of the constituents (donor, electrolyte, solvent) does not significantly affect the unusual low-temperature properties of this class of materials. Our results suggest that the electrocrystallization procedure may be self-purifying by selecting for conducting crystal phases with constituents having specific oxidation potentials and solubility properties. However, doping solutions with structurally and chemically similar constituents (i.e., TMTTF, and IO^? ₄ in CIO^? ₄) leads to their incorporation in the crystal structure where they have a profound effect. Several mole percent of these dopants suppress superconductivity in the PF^? ₆ and CIO^? ₄ salts, and increase and broaden the metal-insulator phase transition.     

晶体中负离子配位多面体结晶方位、形变与晶体压电、铁电性

本文研究了压电、铁电晶体中负离子配位多面体的结晶方位与形变,提出了压电晶体中同一种负离子配位多面体的结晶方位是一致的.在铁电晶体中,负离子配位多面体发生形变,伴随着晶体发生顺电-铁电相变,并从这一基本过程出发,对铁电体相变的形成机理进行了讨论.     

Structural and spectral studies of N-trans-cinnamylidene-m-toluidine and N-trans-cinnamylidene-m-chloroaniline

N-trans-cinnamylidene-m-toluidine (1) C₁₆H₁₅N, and N-trans-cinnamylidene-m-chloroaniline (2) C₁₅H₁₂NCl form isomorphous crystals which are monoclinic, space group P2_l/c, with unit cell dimensionsa=5.967(2),b=13.793(3),c=15.048(5) Å, =91.97(3)° anda=5.868(2),b=13.788(4),c=15.191(4) Å, =91.87(3)°, respectively. The single-crystal X-ray structure determinations of the title compounds revealtrans structures. Ring (A) C_10–15 and ring (B) C_1–6, are practically planar in both structures with dihedral angels of 61.3(3) and 63.6(2)°, respectively.¹H nmr, u.v. and i.r. spectra are also reported.     

Di- and triindolylmethanes: molecular structures and spectroscopic characterization of potentially bidentate and tridentate ligands

4-Bromophenyldi(3-methylindol-2-yl)methane (2) and 2-methoxyphenyldi(3-methylindol-2-yl)methane (3) were prepared by sulfuric-acid-catalyzed reactions of 3-methylindole with 4-bromobenzaldehyde and o-anisaldehyde, respectively. Di(3-methylindol-2-yl)phenylmethane (1) and tri(3-methylindol-2-yl)methane (4) were similarly prepared as described previously. Spectroscopic data (¹H, ¹³C NMR) and the X-ray crystal structures for 1 C₂H₅OH and 2–4 are reported. The molecular structure of 1 C₂H₅OH shows hydrogen bonding of both indolyl NH protons to the oxygen of an ethanol molecule. Crystal data for 1 C₂H₅OH: Orthorhombic, Pca2₁, a = 23.9782(17) Å, b = 8.4437(7) Å, c = 11.3029(9) Å, V = 2288.4(3) ų, R ₁ = 0.0597. Crystal data for 2: Orthorhombic, P2₁2₁2₁, a = 8.911(3) Å, b = 9.584(4) Å, c = 24.040(11) Å, V = 2053.0(14) ų, R ₁ = 0.0454. Crystal data for 3: Monoclinic, P2₁/c, a = 9.737(2) Å, b = 25.035(6) Å, c = 9.359(2) Å, = 114.853(4), V = 2070.2(8) ų, R ₁ = 0.0511. Crystal data for 4: Trigonal, R3, a = 14.2214(10) Å, c = 9.6190(10) Å, V = 1684.8(2) ų, R ₁ = 0.0425.     

Synthesis and crystal structure of indium arsenate and phosphate dihydrates with variscite and metavariscite structure types

The hydrothermal synthesis, crystal structure analysis, and spectroscopic studies of InPO₄·2H₂O (1) and InAsO₄·2H₂O (2) are reported. Compound 1 is isomorphic with metavariscite: monoclinic P2₁/n (No. 14), a = 5.4551(3) Å, b = 10.2293(4) Å, c = 8.8861(3) Å, = 91.489(4)°, Z = 4, and compound 2 is isomorphic with variscite: orthorhombic Pbca (No. 61), a = 10.478(1) Å, b = 9.0998(8) Å, c = 10.345(1) Å, Z = 8. Their three-dimensional frameworks are built of corner sharing InO₄(H₂O)₂ octahedra and MO₄ (M = P⁵⁺ or As⁵⁺) tetrahedra. The water molecules in both compounds have different environments and are involved in different types of hydrogen bonding. Infrared spectroscopy indicates that water molecules are true H₂O species.     

Structures and properties of 1,4-dithiins and related molecules

A series of organosulfur compounds was characterized by NMR, IR, mass spectroscopy, cyclic voltammetry, and chemical analyses. The crystal structures of six compounds were determined: 1,3-dithioleno[4,5-e]naphtho[2,3-b]1,4-dithiin-2,5, 10-trione (1b), P , a = 7.665(4), b = 7.997(4), c = 11.443(5) Å, = 91.311(8), = 92.516(8), = 117.53(7)° 6,7-dimethylbenzo[1,2-b]1,3-dithioleno[4,5-e]1,4-dithiin-2,5,8-trione (2b), P2₁/m, a = 3.933(1), b = 12.864(2), c = 11.943(3) Å, = 99.161(4)° 6-phenyl-2-thioxo-6-hydrocyclopenta[2,1-b]1,3-dithioleno[4,5-e]1,4-dithiin-5,7-dione (3a), C2/c, a = 32.408(6), b = 3.8743(8), c = 27.123(5) Å, = 125.171(7)° 6-phenyl-1,3-dithioleno[4,5-e]3-pyrrolino[3,4-b]1,4-dithiin-5,7-trione (3b), P2₁/n, a = 7.9712(9), b = 6.1976(7), c = 55.978(6) Å, = 91.096(1)° 2,3,7,8-tetramethylthianthrene-1,4,6,9-tetraone (4), P2₁/c, a = 4.195(1), b = 17.924(5), c = 9.682(3) Å, = 98.509(5)° 3H,6H-1,4-oxathiino[6,5-2,1]naphtho[3,4-e]1,4-oxathiin-2,7-dione (5), P2₁/n, a = 9.3522(7), b = 7.8782(6), c = 17.118(1) Å, = 93.171(1)°. Several structures exhibited significant S—S intermolecular interactions, suggesting that the molecules might be precursors for preparing nonmetallic conductors.     

Disorder and optical absorption in amorphous silicon and amorphous germanium

The role that disorder plays in shaping the functional form of the optical absorption spectra of both amorphous silicon and amorphous germanium is investigated. Disorder leads to a redistribution of states, which both reduces the empirical optical energy gap and broadens the optical absorption tail. The relationship between the optical gap and the breadth of the absorption tail observed in amorphous semiconductors is thus explained.     

Crystal and molecular structure of 1,2-difluoroethane and 1,2-diiodoethane

A single crystal of phase 1 of 1,2-difluoroethane was grown from the melt directly on an X-ray diffractometer close to the melting point of 169 K. It crystallizes in the monoclinic space group C2/c with lattice parameters a = 7.775(4), b = 4.4973(7), c = 9.024(3) Å, = 101.73(1)°, V = 308.9(2) ų, d _calc = 1.420 g cm^–3 for Z = 4. A second phase of 1,2-difluoroethane was obtained under similar conditions which crystallizes in the orthorhombic space group P2₁2₁2₁ with the unit cell parameters a = 8.0467(16), b = 4.5086(9), c = 8.279(2) Å,V = 300.36(11) ų, d _calc = 1.461 g cm^–3 for Z = 4. In both phases the 1,2-difluoroethane molecules adopt the gauche conformation with F–C–C–F torsion angles close to 68°. Crystals of 1,2-diiodoethane C₂H₄I₂ were grown from pentane at –30°C. A platelet single crystal of the size 0.35 × 0.25 × 0.03 mm was measured with Mo K-radiation at 153 K. 1,2-Diiodoethane crystallizes in the monoclinic space group P2₁/n with a unit cell of a = 4.6051(7), b = 12.939(2), c = 4.7318(7) Å, = 104.636(3)°, V = 272.79(7) ų, Z = 2, d _calc = 3.431 g cm^–3, (MoK) = 11.353 mm^–1. In the molecule the two neighboring iodine atoms are positioned anti. The shortest intermolecular contacts occur via iodine–iodine interactions resulting in layers of molecules in the crystal.