硅酸铋粉体的制备与表征

以Bi2O3和SiO2为原料,采用机械合金化制备了硅酸铋(Bi12SiO20)的粉体.通过X射线衍射和扫描电子显微镜分析了合成粉体的相结构和形貌,研究了不同球磨时间对产物相组成的影响;并使用红外光谱分析和拉曼散射光谱对球磨得到的样品进行了分析.结果显示表明:球磨8h后出现了Bi12SiO20的晶相结构;随着球磨时间的延长促进了Bi12SiO20的形成,从而提供了一种可以商业化大规模生产Bi12SiO20压电粉体的方法.     

双重熔盐法制备片状BaTiO_3粉体

用双重熔盐法制备片状Bi4Ti3O12粉体,以Bi4Ti3O12为中间产物通过离子交换制备了BaTi03片状粉体,并对其工艺过程进行了优化.利用X射线衍射分析合成粉体的相结构,用扫描电子显微镜观察其显微形貌.初步探讨了BaTiO3片状粉体的生长机理.结果表明:反应温度和化学组成对中间产物Bi4Ti3O12的微观形貌具有显著影响,在1 000℃以下时,随着反应温度升高,片状尺寸增大;当相对增加Bi2O3的量时,Bi4Ti3O12片状的尺寸增大.通过离子交换制备BaTiO3时,除了模板Bi4Ti3O12的形貌对BaTiO3的晶粒生长具有影响外,反应温度和化学组成同样对BaTiO3的晶粒生长具有显著影响.合成片状Bi4Ti3O12粉体的最佳的条件为:BaTiO3与Bi4Ti3O12的摩尔比为10:1,1 000℃合成2h.     

熔盐法制备Bi4Si3O12陶瓷及其介电性能研究

以Bi2O3和SiO2为原料,利用NaCl-Na2SO4熔盐系统,在850℃保温3 h制成粉体样品,使用XRD对粉体物相进行表征,确定粉体为纯的Bi4Si3O12,然后将该粉体压片烧成Bi4Si3O12陶瓷.通过SEM和阻抗分析仪对陶瓷微观形貌和介电性能进行了分析,研究烧成温度、保温时间对硅酸铋陶瓷介电性能的影响.研究...     

Bi_4Ti_3O_(12)陶瓷的制备及微观结构

以过量的Bi2O3和TiO2为组分,采用固相烧结法制备Bi4Ti3O12陶瓷。借助XRD和SEM分析相成分和微观结构。结果表明:经750℃/2h预烧后,合成粉体由Bi4Ti3O12、少量的Bi12TiO20和Ti5O9以及Bi2O3组成。成型烧结后,Bi12TiO20和Ti5O9的衍射峰消失,出现了Bi2Ti2O7的衍射峰。1000℃烧结后,Bi2Ti2O7的衍射峰消失,产物基本为Bi4Ti3O12相。SEM分析表明,温度低时,气孔较多,晶粒较细;温度升高后,晶粒长大,气孔减少;到1000℃时,气孔显著减少,晶粒尺寸约为2～5μm。     

反应温度和时间对Bi2SiO5合成的影响

亚稳相Bi2SiO5是Bi2O3-SiO2系统最新发现的化合物晶相。利用XRD，DSC研究了反应温度和时间对Bi2SiO5合成的影响。将Bi2O3与SiO2按物质的量比1：1混合，在一定温度下处理一定时间获得生成产物。结果表明：亚稳化合物Bi2SiO3在固相反应时产生，并随温度及保温时间按一定规律变化。固相反应温度由700℃升高至900℃过程中，亚稳态Bi2SiO5逐渐转变为稳定态Bi12SiO2和Bi4Si3O12反应温度对Bi2SiO5的生成起决定性作用。750℃保温不同时间所获试样的XRD谱表明，固相反应时间延长，反应物Bi2O3的衍射峰减弱，稳定相Bi12SiO20衍射峰增强，随着反应的进行，生成物亚稳相Bi2SiO5的衍射峰减弱，反应时间过长，不利于亚稳相Bi2SiO5生成。     

Bi2O3-SiO2系统固相反应研究

利用XRD、DSC研究了Bi2O3-SiO2系统的固相反应.按物质的量比1∶1将Bi2O3与SiO2混合物在一定温度下处理一定时间获得生成产物并探讨了不同反应条件下产物生成规律.结果表明:亚稳化合物Bi2SiO5在固相反应时产生,并随温度及保温时间按一定规律变化.750 ℃保温不同时间所获试样的XRD谱表明随着固相反应时间的延长,反应物Bi2O3的衍射峰减弱,生成物Bi12SiO20衍射峰增强,反应越完全.在固相反应过程中生成的亚稳相Bi2SiO5随着反应时间延长衍射峰减弱.固相反应温度由700 ℃升高至900 ℃过程中,Bi12SiO20逐渐转变为Bi4Si3O12.     

熔盐法制备Bi1.5ZnNb1.5O7陶瓷粉体

以Bi2O3,ZnO和Nb2O5为原料,KCl为熔盐,用熔盐法合成了单相Bi1.5ZnNb1.5O7陶瓷粉体.XRD和SEM分析表明,在950～1000 ℃,合成了单相Bi1.5ZnNb1.5O7粉体,粉体呈颗粒状,尺寸约2～5 μm.研究了合成温度、熔盐含量和保温时间对粉体颗粒形貌和尺寸的影响.结果表明,合成温度对Bi1.5ZnNb1.5O7粉体形貌和尺寸影响较大,熔盐含量和保温时间对其形貌和尺寸的影响相对较小.     

水热法合成Bi1.5ZnNb1.5O7纳米粉体

以Bi(NO3)3·5H2O,ZnO和Nb2O5为原料,KOH作为矿化剂,用水热法合成了单相Bi1 5ZnNb1.5O7粉体.用N2吸附法测定单相Bi1.5ZnNb1.5O7粉体的比表面积并计算相应的粒径.研究了KOH浓度、合成温度和反应时间对粒径的影响.用X射线衍射分析合成粉体的物相组成,并通过Scherrer公式计算粉体晶粒的尺寸.用透射电子显微镜分析合成粉体的形貌.结果表明:采用水热法可以合成单相立方焦绿石结构的Bi1.5ZnNb1.5O7纳米粉体.改变水热反应条件,可以控制合成粉体的粒径和比表面积大小.当KOH浓度为1.8 mol/L,温度为180～220 ℃,反应时间为24h时,合成的Bi1.5ZnNb1.5O7纳米粉体的最小粒径为51 nm,最大比表面积为28.8 m2/g.     

Bi4Si3O12纳米粉体的制备与表征

以正硅酸乙酯和Bi2O3为原料,采用溶胶-凝胶法制备了硅酸铋(Bi4Si3O12)纳米粉体.通过X射线衍射和电子显微镜分析了合成粉体的相结构和形貌,测定了粉体的粒度分布曲线,研究了正硅酸乙酯用量对产物相组成的影响.结果表明:干凝胶粉末在750℃热处理2 h,得到了粒径为40～100nm的粉体.正硅酸乙酯的实际用量为理论用量的6倍时,可以制备出相组成为Bi4Si3O1 2的纳米粉体.纳米尺度的Bi4Si3O12材料的激发光谱和发射光谱相对于晶体材料发生了蓝移.     

钛酸铋陶瓷靶材的热压烧结

纯相、高致密度、结晶良好的陶瓷靶材是物理气相沉积薄膜的前提.采用热压烧结方法制备钛酸铋(Bi4Ti3O12)陶瓷靶材,重点研究了制备工艺对靶材的物相、微观结构和致密度的影响.以Bi2O3和TiO2微粉为原料,采用固相反应法,在800℃合成出纯相的Bi4Ti3O12粉体;加入过量3wt%的Bi2O3,可以有效防止烧结过程中因Bi挥发所产生的杂相,得到纯相的Bi4Ti3O12陶瓷;采用热压烧结方法,进一步实现了Bi4Ti3O12粉体的致密烧结,确定了适宜的制备条件为850℃,30MPa,2b,在该条件下制备的Bi4Ti3O12陶瓷致密度达到99%,晶粒呈片层状,大小约2-4μm,可满足靶材制备薄膜的需求.     

Victrex® poly(ethersulfone) (PES) and Victrex® poly(etheretherketone) (PEEK)

Properties of two high performance engineering thermoplastics, amorphous polyethersulfone (PES) and semicrystalline polyetheretherketone (PEEK), are discussed. Both resins can be processed by conventional techniques, compounded with high performance fibers, and have high service temperature (up to 300°C). Due to the amorphous character PES can be dissolved and spray coated into metals.     

Photopyroelectric Spectroscopic Studies of ZnO-MnO(2)-Co(3)O(4)-V(2)O(5) Ceramics

Photopyroelectric (PPE) spectroscopy is a nondestructive tool that is used to study the optical properties of the ceramics (ZnO + 0.4MnO(2) + 0.4Co(3)O(4) + xV(2)O(5)), x = 0-1 mol%. Wavelength of incident light, modulated at 10 Hz, was in the range of 300-800 nm. PPE spectrum with reference to the doping level and sintering temperature is discussed. Optical energy band-gap (E(g)) was 2.11 eV for 0.3 mol% V(2)O(5) at a sintering temperature of 1025 °C as determined from the plot (ρhυ)(2)versushυ. With a further increase in V(2)O(5), the value of E(g) was found to be 2.59 eV. Steepness factor 'σ(A)' and 'σ(B)', which characterize the slope of exponential optical absorption, is discussed with reference to the variation of E(g). XRD, SEM and EDAX are also used for characterization of the ceramic. For this ceramic, the maximum relative density and grain size was observed to be 91.8% and 9.5 μm, respectively.     

(Ba_(1-α)Sr_α)_(4.8)(Sm_(0.7)La_(0.3))_(8.8)Ti_(18)O_(54)陶瓷的微波介电性能

采用固相合成法制备了(Ba(1-α)Srα)4.8(Sm0.7La0.3)8.8Ti18O54(α=0.1～0.5)系陶瓷,表征了该陶瓷的相组成和显微结构,测试了微波介电性能.结果表明:α=0.3时,(Ba(1-α)Srα)4.8(Sm0.7La0.3)8.8Ti18O54系陶瓷为单相的新钨青铜结构固溶体.α>0.3时,相继出现了第二相BaLa2Ti4O12和La0.66TiO2.993.随α的增加,(Ba(1-α)Srα)4.8(Sm0.7La0.3)8.8Ti18O54系陶瓷的相对介电常数(εr)先增大后有所波动,品质因数(Qf)先增大后减小,谐振频率温度系数(τf)单调减小.α=0.3时,在1 350℃烧结的陶瓷的微波介电性能最佳:εr=98.77,Qf=5184GHz,τf=10.9×10-6/℃,优于不掺杂的BaO-Sm2O3-TiO2陶瓷的.     

Calcium silicate hydrate (II) (“C-S-H(II)”)

This semicrystalline phase, originally named ‘calcium silicate hydrate(II)’ by Taylor (1950), has been studied with X-rays, electron optics, chemical investigation of silicate anion type, infrared spectra, and thermal methods. It is structurally related to jennite (C₉S₆H₁₁) and probably also to the fibrous CSH of cement pastes, the three phases forming a sequence of decreasing crystallinity. The specimen studied had approximate composition C₂SH_3.2 after standing over saturated CaCλ₂ at about 15°C. CSH(II) contains metasilicate chains and pyrosilicate groups and has a disordered layer structure. Much of the water can be lost reversibly without significant change in lattice parameters.     

Poly(butadiene-acrylic acid(g)acrylonitrile(g)acrylic acid)

Summary In the present work we describe, the synthesis and characterization of a new gel obtained by crosslinking a cooligomer of butadiene-acrylic acid (BuAA), by reaction with acrylonitrile and acrylic acid. The purified product was characterized by FTIR, elemental analyses and scanning electronic microscopy. The thermal properties were studied and swelling indexes were determined in different solvents and at different pH values. The capacity of poly(butadiene-acrylic acid(g)acrylonitrile(g)acrylic acid) [gel A] to separate different organic substances, such as amino acids and colorants, was determined.     

Photooxidative stability of substituted poly(phenylene vinylene) (PPV) and poly(phenylene acetylene) (PPA)

The addition of side groups to improve the photooxidative stability of polymers used in polymer-based light-emitting diodes (LEDs) is explored. Infrared spectroscopy and computational chemistry techniques are used to study the effects of chemical substitution of the reactive vinylene moiety in poly(phenylene vinylene) (PPV). The bond order of the vinylene group in small oligomers is calculated using semiempirical techniques to assess the improvement in stability toward oxidants such as singlet oxygen. We find that PPV dimers allow relative comparisons across a range of possible substitutions. Experimental results correlate well with these calculations. The addition of electron-withdrawing substituents, such as nitrile groups, to the vinylene moiety is found to be particularly effective in reducing the reactivity of alkoxy-substituted PPV toward singlet oxygen. The photooxidative stability of a poly(phenylene acetylene) (PPA) derivative is also studied. It appears that this family of polymers is more stable toward photooxidation than are its PPV analogs. © 1998 John Wiley & Sons, Inc. J Appl Polym Sci 69: 2451–2458, 1998     

Chemical cross-linking of conducting poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate) (PEDOT:PSS) using poly(ethylene oxide) (PEO)

Hybrid films of poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate) (PEDOT:PSS) were prepared with different molecular weights of poly(ethylene oxide) (PEO). The cross-linking reaction between PEO and PEDOT:PSS was performed at high temperature and confirmed by using differential scanning calorimeter (DSC), contact angle measurement, and solid-state ¹H NMR. The effect of chemical reaction on the conductivity and morphology of these hybrid films was studied by using 4-point probe and atomic force microscope (AFM), respectively. As-spun PEO/PEDOT:PSS films have lower electric conductivity due to the addition of nonconductive PEO, and exhibits no molecular weight dependence on conductivity. After chemical cross-linking reaction at high temperature, only PEDOT:PSS films with lowest molecular weight PEO additives show enhanced conductivity with increasing reaction time. AFM result indicates that the heat-treated PEO/PEDOT:PSS hybrid films show grain-like morphology compared to ethylene glycol treated PEDOT:PSS films which shows continuous PEDOT domain. In the present work we demonstrate that the cross-linking reaction can be used to improve the wet stability of PEDOT:PSS nanofiber, showing good water resistance and excellent dimensional stability.     

Thermal studies of blends of poly(phenylene sulfide) (PPS) with poly(phenylene sulfide sulfone) (PPSS) and with poly(phenylene sulfide ether) (PPSE)

The miscibilities of poly(phenylene) sulfide/poly(phenylene sulfide sulfone) (PPS/PPSS) and poly(phenylene) sulfide/poly(phenylene sulfide ether) (PPS/PPSE) blends were invesigated in terms of shifts of glass transition temperatures T_g of pure PPS, PPSS, a dn PPSE. The crystallization kinetics of PPS/PPSS blends was also studied as a function of molar composition. The PPS/PPSS and PPS/PPSE blends are respectively partially and fully miscible. PPSE shows a plasticizing effect on PPS as does PPS on PPSS, which necessarily improves te processibility in the respective systems. We can control T_g and melting temperature T_m of PPS by varying amounts of PPSE in blends. The melt crystallization temperature T_mc of PPS/PPSE blends was higher than that of the PPSE homopolymer. Therefore, these blends require shorter cycle times in processing than pure PPSE. The overall rate of crystallization for PPS/PPSS blends follows the Avrami equation with an exponent ?2. The maximal rate of crystallization for PPS/PPSS blends occurs at a temperatre higher by 10°C than that for PPS, while the crystallization half time t_1/2 is 4 times shorter. In the cold crystallization range, crystal growth rates increase and Avrami exponents decrease significantly as the temperature increases.