临江某硅藻土酸浸煅烧增白工艺试验研究

采用酸浸-煅烧方法对临江某一级硅藻土进行了增白试验研究,探讨了酸浸温度、酸浸时间、硫酸浓度、固液比、煅烧温度、煅烧时间对硅藻土增白效果的影响,并通过扫描电镜及化学成分分析等对增白前后硅藻土进行了表征.结果表明:硅藻土增白适宜工艺条件为:酸浸温度100℃,酸浸时间4h,固液质量比1∶3.28,酸浓度5 mol/L,煅烧温度650℃,煅烧时间1.5h;优化工艺条件下,一级硅藻土白度由67.2;提升至88.4;,SiO2含量由89.78;提升至95.01;,Fe2O3含量由1.07;降低至0.21;.     

硫铁矿烧渣制备导电陶瓷的工艺研究

采用全铁含量21.89;,Fe2O3含量29.80;的硫铁矿烧渣,在高温还原气氛下以少量还原剂还原,制备了电阻率较低的高强导电陶瓷.研究了烧结温度、保温时间、矿化剂种类及掺杂量对导电陶瓷强度及电阻率的影响.结果表明:导电陶瓷的强度随烧结温度的升高而增加,保温时间的延长而降低,矿化剂掺杂量的增加而增加;而电阻率的变化趋势正好与强度变化相反.当还原剂与硫铁矿烧渣比值为0.1,1400℃保温60 min,萤石掺杂量5.4;,导电陶瓷电阻率达到58 Ω·cm,强度87 MPa;而当Na2O掺杂量达到4;,电阻率为88 Ω·cm,强度为84MPa.     

化学液相沉淀法制备过氧化银及其表征

采用化学液相沉淀工艺制备了过氧化银(AgO)粉体,研究了Na2S2O8用量、反应体系的pH值、反应时间等制备工艺参数对AgO产率的影响,并采用X射线衍射仪(XRD)及扫描电子显微镜(SEM)对制备的AgO粉体进行了表征.结果表明,优选的制备工艺是将AgNO3、Na2S2O8和SDBS的质量比定为1∶4.4∶1,然后在反应体系的温度达到60℃后通过滴加NaOH溶液调整反应体系的pH值为13.00,并维持反应时间30 min.随着AgNO3与SDBS的质量比从2.5升高到20.0,AgO粉末颗粒的形貌从近似的球形转变为球状和片状结构的混合物.     

物理法制备芒硝基复合相变材料及其性能研究

以芒硝(Na2SO4· 10H2O)为主相变材料,采用物理共混法,筛选出合适添加辅助材料组成多元混盐体系,制备出相变温度在25℃左右的Na2SO4· 10H2O基复合相变材料,研究了原料配比对相变材料相变温度和相变潜热的影响.通过热重分析、T-history曲线、差示扫描量热法等表征了制备的芒硝基相变储能材料性质.结果表明:二元相变材料相变温度随着Na2CO3·10H2O增加而先降低后增大;相变材料相变潜热密度基本不变.三元相变材料相变温度随着NaCl、KCl、NH4Cl量增加相变温度降低;相变材料相变潜热密度相比于二元体系有所减小,且在一定范围内随着成核剂硼砂含量的增加该体系相变潜热密度基本保持不变,过冷度有明显下降.当Na2SO4· 10H2O量为86.4;、Na2CO3 · 10H2O量为9.6;、NaCl量为4;,对该配方改性添加3;的硼砂和0.1;的羧甲基纤维素钠时,此相变材料的相变温度为24.6℃,过冷度为0.3℃,相变潜热密度为179.6 J/g.     

煅烧温度对络合溶胶-凝胶法制备ZnGa2O4微晶形貌及光催化性能的影响

采用EDTA络合溶胶-凝胶法制备了尖晶石结构的ZnGa2O4微晶.通过XRD、SEM等分析方法对ZnGa2O4微晶进行了测试和表征.研究了不同煅烧温度对其物相组成、显微结构及光催化性能的影响.结果表明,以乙酸锌和氧化镓为反应原料,以乙二胺四乙酸为络合剂,在650～800℃能合成单一物相的ZnGa2O4微晶.在700℃时可以成功制备八面体形的ZnGa2O4微晶,在800℃时可以合成棒状的ZnGa2O4微晶;随着温度从650～800℃逐渐升高,其对罗丹明B的光催化降解性能逐渐提高.     

Y2O3陶瓷凝胶注模成型工艺研究

采用凝胶注模成型工艺制备了Y2O3陶瓷部件,研究了分散剂加入量、pH值和固相含量对浆料粘度影响,单体、交联剂、引发剂、催化剂和温度对凝胶反应时间的影响,以及烧结后陶瓷制品的线收缩率.结果表明最佳工艺参数为:分散剂聚丙烯酸铵加入量为0.8vol;,pH值为9,固相含量为65vol;,浆料的粘度为1.07 Pa·s;单体丙烯酰胺为3.5wt;,交联剂N,N'-亚甲基双丙烯酰胺为0.35wt;,引发剂5wt;过硫酸铵溶液为0.9vol;,催化剂N,N,N',N'-四甲基乙二胺为0.2vol;,反应温度为50℃,凝胶反应时间为25 min.在2000℃温度下烧结后,陶瓷制品的最小线收缩率为3.0;.     

添加剂对DMH体系电沉积金的影响

在以5,5'-二甲基已内酰脲(DMH)为配位剂的镀液体系中研究了添加剂 C4H6O2、C7H4NNaO3S 和 C12H25 SO4 Na对金电沉积工艺和电结晶过程的影响。阴极极化曲线测试中,金电沉积的最佳电势区间是-0.60~-1.2 V,添加剂浓度在研究的范围内对阴极极化电势的影响较小。循环伏安曲线结果表明,反应界面上添加剂的吸附能够影响成核生长超电势,对金还原过程表现出抑制作用。电化学阻抗谱研究表明,镀液中加入添加剂后,电荷转移过程变得更加困难。 SEM观察表明,添加剂改善了镀层质量,晶粒变得细致、均匀。 XRD分析证实,两种镀液体系中获得的镀金层都沿着Au(111)和(220)晶面择优生长。     

NiFe2O4磁性纳米颗粒的制备及其催化降解孔雀石绿的研究

以溶胶-凝胶法和固相研磨法制备NiFe2O4磁性纳米颗粒,采用X射线粉末衍射仪、扫描电子显微镜、透射电子显微镜、X射线光电子能谱仪、震动样品磁强计等探讨了不同合成方法对其结构、晶型、形貌的影响,结果表明凝胶-溶胶法制得的NiFe2O4具有颗粒小、尺寸均匀、磁学性能优、催化性能好等特点.推测了NiFe2O4/H2O2类芬顿体系催化降解孔雀石绿的反应机理.考察了pH值、催化剂用量、氧化剂用量、反应时间等因素的影响,结果表明:对浓度为25 mg/L的孔雀石绿溶液,当NiFe2O4用量为0.05 g,H2O2用量为0.30 mL,pH为5,温度为298 K,反应时间为45 min,孔雀石绿脱色率在93;以上.动力学研究表明降解过程近似为一级反应,速率常数达0.057 min-1.     

HPO42-与H2PO4-在水热法制备CeO2纳米颗粒过程中的影响

以Ce(NO3)3·6H2O、Na5P3O10和Na3PO4·12H2O为原料,用水热法在180℃反应60h分别制备了CeO2纳米八面体和纳米棒,且对Na5P3O10与Na3PO4 · 12H2O系统同时调节pH =2时180℃反应12 h制备了纳米棒.通过XRD、FE-SEM、TEM等方法对CeO2纳米棒和纳米八面体进行了测试和分析.结果表明,对于Na5P3O10与Na3PO4·12H2O系统,初始时CeO2八面体与纳米棒共存,但随着水热时间的延长,Na5 P3O10系统中CeO2八面体成为主要产物,而在Na3PO4·12H2O系统中CeO2纳米棒成为主要产物.Na5P3O10水解产生的HPO42-是CeO2纳米八面体形成的主要原因,而Na3PO4·12H2O水解产生的H2PO4-是纳米棒形成的主要原因.     

溶胶-凝胶法制备尖晶石型ZnFe2O4粉体的研究

以硝酸铁、硝酸锌为原料,柠檬酸为络合剂,采用溶胶-凝胶法制备了尖晶石型ZnFe2 O4粉体.通过热重-差热分析(TG-DTA)、X射线衍射仪(XRD)、扫描电镜(SEM)、X射线能谱仪(EDS)、透射电镜(TEM)等方法对制备的ZnFe2O4粉体进行了分析测试与表征,并对其合成机理进行探讨.研究表明:滴定溶液的pH =4时最有利于柠檬酸对Fe3+、Zn2+的络合.在600 ～ 1000℃下,随着合成温度的提高,制备的ZnFe2O4粉体晶型发育逐步完整,确定较好的合成温度为900℃.相同条件下,适当延长保温时间,有助于ZnFe2O4粉体的合成.     

Triethyl ammonium salt of O,O′-bis(p-tolyl)dithiophosphate, [Et3NH]+[(4-MeC6H4O)2PS2]−

Triethyl ammonium Salt of O,O′-bis(p-tolyl)dithiophosphate and O,O′-bis(m-tolyl)dithiophosphate have been obtained by reaction of p- and m-cresol, respectively with P₂S₅ in toluene and have been characterized by elemental analysis, IR, ¹H and ³¹P NMR spectroscopy. The molecular structure of O,O′-bis(p-tolyl)dithiophosphate has been determined. Crystal data: [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻: Monoclinic, P2₁/c, a=15.2441(9) ?, b=10.415(2) ?, c=3.9726(9) ?, β=91.709(7)°, V=2217.5(1) ?⁻³, Z=4.Supplementary materials Additional material available from the Cambridge Crystallographic Data Centre (CCDC no. 600927 for [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻ comprises the final atomic coordinates for all atoms, thermal parameters, and a complete listing of bond distances and angles. Copies of this information may be obtained free of charge on application to The Director, 12 Union Road, Cambridge CB2 2EZ, UK (fax: +44-1223-336033; email: deposit@ccdc.cam.ac.uk or www:http://www.ccdc.cam.ac.uk).     

First-principles coexistence simulations of supercooled liquid silicon

We perform first-principles coexistence simulations of the low-density and the high-density phases of supercooled liquid silicon and find a negative slope for the coexisting line in the temperature-pressure plane. Electron density maps and electron-localization function plots of the two phases of silicon show marked differences. The calculated differences suggest more localized electrons in the low-density liquid compared to the high-density liquid, coming from an increased population of covalent bonds, which further explain the calculated negative slope in the two phase coexistence regime. This is consistent with the presence of a pseudo-gap in low-density liquid silicon, absent in the high-density liquid which shows a metallic behavior.     

Crystal structures of thecis andtrans isomers of dithiahexahydro[3.3]metacyclophane

Structures of both thecis andtrans isomers of dithiahexahydro[3.3]metacyclophane, ?C₆H₄?CH₂SCH₂?C₆H₁₀?CH₂SCH₂?, have been determined, wherecis andtrans refer to the attachments to the cyclohexane ring. Thecis form crystallizes in the monoclinic space groupP2₁/c witha=8.4299(11)Å,b=21.772(2)Å,c=8.9724(13)Å, β=116.574(11)^o, andZ=4. Thetrans isomer packs into the monoclinic space groupP2₁ witha=8.159(16)Å,b=10.185(5)Å,c=9.558(2)Å, β=112.435(18)^o, andZ=2. The cyclohexane ring of thecis isomer is in the chair conformation, while the cyclohexane of thetrans isomer is found in a twisted boat conformation.     

CTAB与SDBS对碳酸锶粒子生长形态调控及机理研究

以表面活性剂CTAB和SDBS为化学添加剂,采用化学共沉淀法对碳酸锶晶体的生长形态进行调控,成功地制备出了实心的树枝状和花瓣为空心的花状碳酸锶粉体,并用X射线衍射(XRD)、扫描电子显微镜(SEM)和傅里叶变换红外光谱(FT-IR)等分析手段对样品进行了表征;最后重点对化学添加剂可能产生的影响机理进行了初步的探讨.结果表明,CTAB和SDBS在晶体生长的过程中能起到显著的影响作用,两者对粒子分散性能的作用效果相反,而且后者对晶体(013)和(213)晶面表面能降低的贡献明显大于前者.     

Crystal structures of the cis and trans isomers of a tetrathia[3.3.3.3]cyclophane

Both the cis and trans isomers of 3,11,18,26-tetrathiatricyclo[26.2.2.1^5,9.2^13,16.1^20,24] hexatriaconta-5,7,9,20,22,24-hexene have been prepared and structurally characterized. Each of these centrosymmetric tetrathia dimers includes two cyclohexane rings in chair conformations with either 1,4-cis or 1,4-trans bonding and two meta-substituted benzene rings. The cis isomer packs into the monoclinic space group P2₁/a with a = 10.485(3)Å, b = 10.3956(18)Å, c = 14.1343(10)Å, = 105.200(13)°, Z = 2 and refined to an R factor of 0.046. The trans isomer crystallizes in the monoclinic space group P2₁/c with a = 10.7217(12)Å, b = 5.6797(7)Å, c = 25.415(5)Å, = 96.001(12)°, Z = 2 and refined to an R factor of 0.043. In the cis structure each benzene ring faces a cyclohexane ring while in the trans structure the cyclohexane rings face one another.     

Crystal structure of Zn4Na(OH)6SO4Cl·6H2O

The structure of Zn₄Na(OH)₆SO₄Cl·6H₂O, a secondary mineral from Hettstedt, Germany, was determined by single-crystal X-ray diffraction. The crystals are hexagonal,a=8.413(8),c=13.095(24) Å, space group $P\bar 3$ , Z=2. The structure was refined to R=0.0554 and R_w=0.0903 for 970 reflections with I≥3σ(I). The structure can be described as zinc hydroxide layers perpendicular toc, from which sulfates and chlorides extend. The layers are held together by a system of hydrogen bonds involving hexaaquo Na⁺ ions which occupy the interlayer space.     

Synthesis and Crystal Structure of 5-[2-(6-bromonaphthalenyloxymethyl)]-3-(4-morpholinomethyl)-1,3,4-oxadiazole-2(3<Emphasis Type="Italic">H</Emphasis>)-thione

Abstract  The title compound, C₁₈H₁₈BrN₃O₃S, a derivative of 1,3,4-oxadiazole, crystallizes in the triclinic space group P-1 with unit cell parameters a = 6.8731(3), b = 8.9994(4), c = 15.7099(6) ?, α = 92.779(3)°, β = 130.575(3)°, γ = 107.868(4)°, Z = 2. The dihedral angle between the mean planes of the planar naphthyl and morpholine (chair) rings with the planar oxadiazol ring is 50.1(8) and 76.8(6)°, respectively. The planar naphthyl ring is twisted 52.2(5)° with the mean plane of the morpholine ring. A group of four intermolecular close contacts are observed between a bromine atom and hydrogen atoms from the closely packed naphthyl, morpholine and oxy–methyl groups in the unit cell. These molecular interactions in concert with an additional series of π–π stacking interactions that occur between the center of gravity of the two 6-membered rings of the naphthalene group influence the twist angles of each of these three groups. A MOPAC AM1 calculation of the conformation energy of the crystal structure [226.0128(9) kcal] compared to that of the minimum energy structure after geometry optimization [29.9744(1) kcal] reveals a significantly reduced value. The twist angles of the three groups above also change after the AM1 calculation giving support to the influence of both intermolecular C–H···Br short-range interactions and Cg π–π stacking interactions on these angles which therefore play a role in stabilizing crystal packing. Graphical Abstract  Crystal structure of 5-{[(6-bromonaphthalen-2-yl)oxy]methyl}-3-(morpholin-4-ylmethyl)-1,3,4-oxadiazole-2(3H)-thione, C₁₈H₁₈BrN₃O₃S, is reported and its geometric and packing parameters described and compared to a MOPAC computational calculation. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Crystal structure of irisolidone from the flowers of Pueraia lobata

Irisolidone (5,7-dihydroxy-6,4′-dimethoxyisoflavone) was isolated from the flowers of Pueraia lobata and its crystal structure was examined by X-ray single crystal diffraction. The crystal structure of irisolidone is monoclinic, space group P2₁/c with a = 15.491(9) ?, b = 7.895(4) ?, c = 13.321(7) ?, β = 110.546(9)° and Z = 4. Hydrogen bonding and aromatic π–π stacking assemble the title compound into a three-dimensional networking structure.     

电沉积法制备ZnO纳米棒阵列及其发光特性

本文以掺F的SnO2导电玻璃为基板,以硝酸锌水溶液为电解液,采用三电极恒电位体系电沉积制备ZnO纳米棒阵列,系统考察了硝酸锌浓度和沉积电位等工艺参数对ZnO纳米棒阵列的微观形貌及其发光性能的影响规律.结果表明,硝酸锌浓度和沉积电位对纳米棒阵列的形貌有显著影响,控制适宜的工艺条件可以制备出直径分布均匀、结晶性好且纯度高的六方纤锌矿ZnO纳米棒阵列.荧光光谱分析表明,电沉积制备出的ZnO纳米棒阵列在385 nm附近有一个强荧光发射峰,且发光性能稳定、对纳米棒阵列微观形貌的细微变化不敏感,使其在发光二极管和激光器等领域具有广阔的应用前景.