利用高铝粉煤灰制备多孔陶瓷工艺研究

以脱硅高铝粉煤灰为主要原料、石墨为造孔剂制备多孔陶瓷.利用X射线衍射仪和扫描电子显微镜分析多孔陶瓷的物相组成和微观结构,万能试验机测试抗弯强度,阿基米德排水法测定显气孔率和体积密度,采用渗透通量评价其过滤性能.研究结果表明:随着烧结温度的升高,多孔陶瓷的莫来石含量、体积密度和抗弯强度逐步增大,刚玉和石英的含量、显气孔率、吸水率和对水的渗透通量逐渐减小.随着石墨添加量的增加,多孔陶瓷的物相组成变化不大,体积密度和抗弯强度逐步降低,显气孔率、吸水率和对水的渗透通量相应增加.添加30wt;石墨、1450℃烧结的多孔陶瓷,抗弯强度为9 MPa,显气孔率为48.28;,大气压下,对水的渗透通量达到714 L·m-2·h-1.     

NiO对白云石烧结性能的影响

以天然白云石为原料,采用二步煅烧工艺,研究了NiO对白云石烧结性能的影响,并采用扫描电子显微镜和X射线衍射仪对试样进行分析.研究结果表明:NiO添加到白云石中,高温烧结后,NiO完全固溶到MgO晶格中,改变MgO晶格常数,导致MgO晶格畸变,促进白云石的烧结.烧结温度为1600℃,无NiO添加剂时,白云石熟料的体积密度为3.30 g/cm3,显气孔率为3.4;,MgO晶粒尺寸为3.26 μm.当NiO添加量为0.75;时,白云石熟料的体积密度提高到3.33 g/cm3,显气孔率为2.7;,MgO晶粒尺寸达到3.54μm.     

透辉石改性粉煤灰基莫来石的性能和微观结构

为提高粉煤灰基莫来石的力学性能,以透辉石为烧结助剂,低温条件下采用无压烧结法制得了致密高强的莫来石.通过对莫来石线收缩率、体积密度、抗折强度、孔结构的测试,并借助X射线衍射、显微镜观察、扫描电镜微观分析等方法,研究了不同烧结温度时透辉石掺量对莫来石性能和结构的影响.结果表明:烧结温度为1400℃、透辉石掺量为8;时制得的莫来石性能最佳.此时,莫来石试样的线收缩率、体积密度和抗折强度最大,分别为13.3; 、2.88 g/cm3和160.6 MPa;试样的显气孔率仅为2.5;,莫来石试样致密程度高.透辉石在高温(≥1250℃)下熔融成液相,不但可填补莫来石烧结形成的孔洞,提高了试样结构的致密性,且有利于莫来石液相烧结,促进莫来石晶相的形成,莫来石晶相由细针状发育成短柱状,晶粒交叉生长,形成致密高强的粉煤灰基莫来石.     

保温时间对合成轻质耐高温六铝酸钙材料性能的影响

采用钙质海砂和工业γ-氧化铝为原料,经球磨、成型和无压烧结等工艺原位反应制备了六铝酸钙轻质耐高温材料,利用XRD和SEM研究了产物的物相组成和显微形貌,探讨了保温时间对制备产物体积密度、显气孔率和常温抗折强度的影响.结果表明:当合成温度为1550℃,保温时间为3～6h时,产物主要为片状六铝酸钙;保温时间由3h增加至6h时,片状晶粒的厚度和尺寸增大,当保温6h时,晶体边缘已经开始出现熔融现象;试样体积密度先减小后增大;当保温时间为5h时,试样有较优的综合性能,其显气孔率、体积密度和抗折强度值分别为55.24;和1.67 g/cm3和7.06 MPa.     

不同铝硅比对莫来石材料显微结构及性能的影响

选用铝矾土作为铝源,煤矸石为硅源,氟化铝和五氧化二钒为添加剂,通过固相反应原位制备了主晶相为莫来石相的晶体.利用X射线衍射仪和扫描电子显微镜以及相应的EDS等手段对莫来石进行了表征分析,并考察了在不同铝硅比的条件下对所制试样的显气孔率、吸水率、体积密度、抗折强度以及显微结构的变化特征.结果表明:当铝矾土与煤矸石的铝硅摩尔比为3.05:2时,显气孔率为23.6;、吸水率为10.55;、体积密度为2.3 g/cm3、抗折强度为114 MPa,试样的综合性能最优.     

MgO含量对CaZrO3-MgO陶瓷烧结特性及组成与结构的影响

采用常压烧结方法制备了CaZrO3-MgO陶瓷.研究了MgO含量对CaZrO3-MgO陶瓷的显气孔率、体积密度、抗弯强度、物相组成、显微结构和断裂方式的影响.结果表明:含有lwt;～3wt; MgO的CaZrO3-MgO陶瓷由CaZrO3单相构成,气孔率低,体积密度高,抗弯强度大,断裂方式为穿晶与沿晶共存的混合断裂;含有20wt; ～40wt; MgO的CaZrO3-MgO陶瓷由MgO和CaZrO3两相构成,气孔率高,体积密度低,抗弯强度小,CaZrO3与MgO两相间的断裂方式为沿晶断裂;当MgO含量为2wt;时CaZrO3-MgO陶瓷的烧结性能最好,当MgO含量为40wt;时CaZrO3-MgO陶瓷的烧结性能最差.少量Mg2+的引入因其向CaZrO3中单向扩散而促进材料烧结,大量Mg2+的引入因其与Zr4+互扩散导致CaZrO3分解而阻碍材料烧结.     

利用坩埚废料制备玻化砖的工艺研究

以石英坩埚废料、长石、煅烧高岭土为原料,在1180～ 1280℃下烧结制备了玻化砖,1260～ 1280℃烧结的样品达到了国标GB/T4100-2015中玻化砖的性质要求.采用X射线衍射(XRD)和扫描电镜(SEM)对样品的组分和结构进行了表征,并对样品的抗弯强度、线收缩率和气孔率进行了测量.结果表明,随着烧结温度的增加,样品致密性和抗弯强度同时增加,在1260℃达到最大值,在1280℃时,,样品中闭合气孔的膨胀导致其抗弯强度有所下降;同时,原料中的钠、钾长石均随着温度的增加,不断的分解并进入玻璃相,并分别在1220℃、1240℃时全部分解.     

La2O3对氧化铝/高岭土复合定向多孔陶瓷性能的影响

以微米级α-Al2O3、陶瓷水体分散剂为主要原料,以La2O3-水洗高岭土为烧结助剂,采用冰模板法制备了一种具有高孔隙率和较高抗压强度的氧化铝/高岭土复合定向多孔陶瓷.研究了不同添加量的La2O3对多孔陶瓷的显气孔率、体积密度、抗压强度和微观形貌的影响.结果表明:添加适量的稀土La2O3能降低多孔陶瓷烧结温度、提高体积密度和抗压强度.通过高能机械球磨法添加La2O3,在1350℃烧结制备的多孔材料样品显气孔率为82;,样品的抗压强度达到10 MPa以上.当La2O3加入量达到3;时,可使多孔陶瓷抗压强度提高到15.2 MPa,较不掺加La2O3提高了约53;.     

MoSi2-SiC复合材料制备及抗热震性能研究

本文采用直接熔渗法制备二硅化钼-碳化硅(MoSi2-SiC)复合材料.以碳化硅(SiC)(粒度为0～2.5 mm、≤240目)为主要原料,水溶性树脂为结合剂,经混炼、成型、烘干后得到SiC坯体,再用二硅化钼(MoSi2)(D50 =3μm)粉末掩埋SiC坯体,在真空条件下2000℃保温3h进行熔渗烧结,制备出MoSi2-SiC复合材料.采用阿基米德排水法研究了MoSi2-SiC复合材料的显气孔率、体积密度;采用三点抗弯法测试了MoSi2-SiC复合材料1400℃抗折强度;采用热线法测试了MoSi2-SiC复合材料导热系数;采用X射线衍射测试了MoSi2-SiC复合材料的物相组成;采用SEM测试了MoSi2-SiC复合材料的显微结构;分别采用风冷法和水冷法对比研究了MoSi2-SiC复合材料、重结晶碳化硅(R-SiC)、氮化硅-碳化硅(Si3N4-SiC)三种材料抗热震性.结果表明:MoSi2在烧结过程中部分发生分解,生成了Mo5Si3,MoSi2、Mo5Si3填充于SiC的内部并实现烧结致密化,使MoSi2-SiC复合材料的显气孔率显著降低至5.7;,体积密度为3.59 g.cm-3.MoSi2-SiC复合材料中MoSi2、Mo5Si3含量分别为10wt; ～ 15wt;、3wt; ～ 5wt;.1000℃下MoSi2-SiC的导热系数为46.5W·m-1 ·K-1,显著高于R-SiC(28.3 W.m-1.K-1)材料、Si3N4-SiC(16.8 W.m-1.K-1)材料.综上所述,MoSi2-SiC复合材料的抗热震性能显著优于R-SiC材料、Si3N4-SiC材料.     

高温烟气过滤陶瓷的制备与性能研究

本论文以堇青石为过滤陶瓷骨料,以高岭土、钾长石、锂辉石为结合剂,以木炭粉为造孔剂,通过半干压成型工艺成型,研制了高温烟气过滤陶瓷.详细研究了结合剂、造孔剂添加量以及成型压力、烧成温度对高温烟气过滤陶瓷的体积密度、显气孔率、抗压强度等性能的影响,并对原料配方进行了优化,优化配方为:堇青石75wt;、结合剂25wt;、炭粉造孔剂50wt;、三聚磷酸钠0.5wt;.研究结果表明:试样的显气孔率随造孔剂添加量的增加而升高、随结合剂添加量的增加而减小;抗压强度和烧结密度随造孔剂添加量的增加而减小、随结合剂添加量的增加而升高;随成型压力的增大,过滤陶瓷的显气孔率呈逐渐减小的趋势,抗压强度则不断增大.随烧成温度的升高,过滤陶瓷的显气孔率呈先升高后减小的趋势,而抗压强度则逐渐增大.     

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).     

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.     

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.     

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.     

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.     

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.     

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.