多孔氮化硅陶瓷的微观结构、力学性能和气体透气性的研究

本研究中,以石油焦为造孔剂、Y2O3-Al2O3为烧结助剂,通过注浆成型制备出多孔氮化硅陶瓷.研究石油焦的加入量对多孔氮化硅陶瓷微观结构、力学性能及气体透气性的影响.结果表明:多孔氮化硅陶瓷的微孔是由长棒状的β-Si3N4晶粒互相搭接而成,大孔是由石油焦燃烧而成.随着石油焦加入量的增加,气孔率及达西渗透系数(μ)增大,但试样的抗弯强度降低.在起始α-Si3N4粉末中添加10wt;～50wt;石油焦、5wt; Y2O3-3wt;Al2O3 1800℃下保温2h制备出气孔率为37.08;～59.40;、抗弯强度为52.00～154.27 MPa、μ值为(3.04 ～6.87)×10-13m2的多孔氮化硅陶瓷.     

pH值对ZrO2超细粉体料浆性能的影响

研究了不同pH值时超细ZrO2粉体料浆的Zeta电位、沉降速度和粘度等性能.测试了加入柠檬酸三铵作分散剂和A型分散剂(聚丙烯酸盐)以及不加分散剂时料浆的Zeta电位,结果证明采用A型分散剂分散效果最好,在pH=10.53时Zeta电位具有最大负值-44.28mV,研究了不同pH值时料浆的沉降情况,在pH=10.55时料浆沉降速度最慢,同时研究了pH值对料浆粘度的影响,在pH=10.66时料浆粘度最低.料浆呈现出剪切变稀特性,在pH值为10～11范围内,成型的坯体网络结构稳定,最大弯曲强度达到53.90MPa.     

高固相含量纳米ITO水基浆料流变性能的研究

以PAA为分散剂制备高固相含量纳米ITO水基浆料,研究了pH值、分散剂用量、固相含量对浆料流变性能的影响.结果表明:PAA对改善纳米ITO粉体的表面电动特性有显著作用,PAA的加入使粉体Zeta电位从-16mV降到-38 mV;高固相含量的浆料均呈现出明显的剪切变稀行为;浆料粘度随固相含量增加而急剧增大;最佳的PAA用量及pH值范围分别为0.06 mg/m2和10～11.55wt;固相含量的浆料在150 s-1剪切速率下粘度为0.38 Pa·s,以此为原料采用胶态成型技术制备出微观结构均匀的ITO陶瓷素坯.     

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;.     

分散剂对CSLST微波介质陶瓷水系流延浆料稳定性的影响

分别采用聚乙烯吡咯烷酮(PVP)、聚乙烯酸(PAA)、聚丙烯酰胺为分散剂,以苯丙乳液为粘结剂,丙三醇为增塑剂,去离子水为分散介质,水系流延成型法制备添加B2O3-CuO-LiCO3(BCL)玻璃料为烧结助剂的(Ca0.9375Sr0.0625)03(Li0.5Sm0.5)07TiO3 (CSLST)微波介质陶瓷,研究了分散剂种类及含量对陶瓷粉体浆料分散稳定性以及流延膜片的影响.结果表明:当以PVP为分散剂,添加量为0.8;,调节浆料的pH=10时,浆料的分散稳定性最佳,经流延后可制备得到表面光滑,均匀无裂纹的延膜片.     

多孔陶瓷负载TiO2光催化降解甲基橙溶液的研究

采用有机先驱体浸渍法及无压烧结工艺,制备了Al2O3多孔陶瓷载体。利用溶胶-凝胶法在多孔陶瓷上负载Sm3+掺杂Ti O2光催化材料。研究了煅烧温度、涂层次数等工艺因素对多孔陶瓷负载Ti O2光催化降解甲基橙溶液的影响规律。结果表明,借助于多孔陶瓷高的气孔率,Ti O2负载在Al2O3颗粒表面或进入颗粒间的孔隙内,使材料具有较大的比表面积。掺入Sm3+使材料的光催化活性提高。在煅烧温度为600℃、四次涂层、甲基橙溶液p H值为2时,多孔陶瓷负载Ti O2光催化降解甲基橙溶液效果最佳。     

共沉淀法制备CoAl2 O4陶瓷颜料及其呈色机理研究

采用共沉淀法制备CoAl2 O4陶瓷颜料,并通过XRD、SEM和XPS表征陶瓷颜料的组成、形貌和元素价态,研究Co/Al比、溶液pH值和煅烧温度对CoAl2 O4陶瓷颜料呈色的影响,并探讨其呈色机理。结果表明：所得CoAl2 O4陶瓷颜料均具有典型的尖晶石结构,当Co/Al比为0.7∶2、溶液pH值为11、煅烧温度为1200℃时可以获得彩度较高的蓝色CoAl2 O4陶瓷颜料。 CoAl2 O4陶瓷颜料的呈色变化主要与所得产物中Co元素的价态有关,当Co含量过高或者前驱体溶液的pH值较大时,产物中含有Co3 O4( Co4+),进入CoAl2 O4后形成固溶体导致其晶格发生畸变,从而使得陶瓷颜料呈现绿色。     

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.     

聚乙二醇对自反应淬熄法制备空心陶瓷微珠的影响

以Al+ Fe2O3+ BaO2+蔗糖+环氧树脂为反应体系、聚乙二醇为表面活性剂,运用将火焰喷涂技术与自蔓延高温合成技术(Self-propagating High-temperature Synthesis,缩写SHS)及快速冷却凝固技术相结合的自反应淬熄法,制备了空心复相陶瓷微珠.通过SEM、EDS、XRD等手段,研究了聚乙二醇的加入对团聚粉及制备的空心陶瓷微珠的影响.结果表明,与未加聚乙二醇相比,加入聚乙二醇后,团聚粉颗粒分布均匀,具有良好的流动性;所制备的空心微珠粒径趋于一致,成球率得到了明显提升,相结构中Fe3O4转变成了Fe2O3,且出现了具有尖晶石结构的BaFe2O4,这有助于提高空心微珠的吸波性能.     

淀粉固结工艺制备多孔氮化硅基陶瓷复合材料

本文以氮化硅,氮化硼,二氧化硅作为陶瓷基体材料,通过淀粉固结工艺,采用常压部分氧化烧结制备了氮化硅基多孔陶瓷。通过Zeta电位测试确定了制备陶瓷坯体的最佳pH值在9.42~10.76之间。混合浆料的浆料流变性能测试表明陶瓷浆料体系呈现剪切变稀特征。XRD分析结果表明在烧结样品组成成分为α-Si3N4、β-Si3N4、BN、Quartz low,sys以及Moganite。SEM的显示氮化硅基多孔陶瓷呈现片层型微观结构。显气孔率随淀粉含量增加而增加,试验制得多孔陶瓷显气孔率最大值高达73.2%。     

CsI-LiCl共晶材料的坩埚下降法生长与闪烁性能研究

本文采用坩埚下降法,在真空密封的石英坩埚中成功生长出CsI-LiCl与CsI-LiCl:Na共晶闪烁体。通过扫描电子显微镜(SEM)观察晶体微结构表明该共晶中LiCl相与CsI相存在周期性的层状排列,CsI相的厚度在5 μm左右。共晶样品的X射线激发发射谱显示在CsI-LiCl和CsI-LiCl:Na共晶样品存在缺陷发光,在CsI-LiCl样品中还观察到了纯CsI的自陷激子(STE)发光。CsI-LiCl样品在α粒子激发下的多道能谱中观察到明显的全能峰,这一结果证明CsI-LiCl共晶可用于热中子探测的潜力。     

静电纺丝法制备CeO2微纳米纤维及其除氟性能

以聚丙烯腈(PAN)为载体,六水合硝酸铈[Ce(NO₃)₃·6H₂O]为原料,采用静电纺丝法制备了Ce(NO₃)₃/PAN纤维,在空气中热处理得到CeO₂微纳米纤维,通过XRD、BET和SEM对CeO₂微纳米纤维进行表征。采用静态吸附实验探讨了CeO₂微纳米纤维去除水溶液中氟离子的性能,考察了溶液pH值、初始氟离子浓度及共存阴离子等对吸附性能的影响。结果表明,pH=3时,CeO₂微纳米纤维对F^-的吸附性能最佳,CeO₂吸附量随着F^-浓度的增大呈上升趋势。CeO₂微纳米纤维对F^-的吸附等温线遵循Langmuir模型,二级动力学模型能很好地描述CeO₂微纳米纤维对F^-的吸附过程。CeO₂微纳米纤维的除氟性能优良,可为其实际应用提供理论参考。     

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.     

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.     

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.     

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).     

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.     

Phase Properties of Hexanedioldiacrylate/E7 Blends

Abstract

Equilibrium phase diagrams of uncured and UV-cured difunctional hexanedioldiacrylate and the eutectic mixture of low molecular weight liquid crystals E7 are established by polarized optical microscopy and differential scanning calorimetry. Data are analyzed using the Maier-Saupe model of nematic order. In the case of the uncured system the Flory-Huggins free energy of isotropic mixing is applied while for the cured system, the Flory-Rehner elastic free energy model is used. A good correlation between experimental and theoretical phase diagrams is found in both systems.