X射线荧光光谱法测定硅酸盐中硫等20个主、次、痕量元素

本文使用新研制的偏硼酸锂和四硼酸锂混合熔剂，在１０００℃熔融制样，以Ｘ射线荧光光谱法测定硅酸盐等样品中的Ｓ，Ｎａ，Ｍｇ，Ａｌ，Ｓｉ，Ｐ，Ｋ，Ｃａ，Ｔｉ，Ｍｎ，Ｆｅ，Ｂａ，Ｃｒ，Ｖ，Ｓｒ，Ｚｒ，Ｒｂ，Ｃｕ，Ｎｉ和Ｎｂ等２０种元素，采用理论α系数和康普顿散射线作内标校正元素间的吸收－增强效应。其分析结果的精密度和准确度可与化学法相比     

偏硼酸锂熔样ICP—MS法测定土壤样品中15种痕量稀土元素

本文采用偏硼酸锂熔样，使用Ｅｌａｎ５０００型ＩＣＰ质变仪，对土壤样品１５种痕量稀土元素的测定进行了研究。选择了样品处理最佳条件和仪器的最佳测定参数。选用Ｒｅ内标元素补偿基体抑制效应和灵敏度漂移。     

偏硼酸锂熔样ICP－MS法测定土壤样品中15种痕量稀土元素

本文采用偏硼酸锂熔样，使用Ｅｌａｎ５０００型ＩＣＰ质谱仪，对土壤样品１５种痕量稀土元素的测定进行了研究。选择了样品预处理最佳条件和仪器的最佳测定参数。选用Ｒｅ内标元素补偿基体抑制效应和灵敏度漂移。检出限为０．００６～０．０２４μｇ／Ｌ。用土壤标样ＧＢＷ０７４０１作为质控样，１５种痕量稀土元素的测得值与标准值有很好的一致性。土壤样品分析的相对标准偏差（ＲＳＤ）为０．７％～３．７％。方法简便快速，适用于例行分析。     

大气压液体阴极辉光放电-原子发射光谱法应用于血清中微量锂元素的测定

含锂药剂在用于临床治疗精神疾病时需要对患者血清中锂元素浓度进行监测以在控制正常药效的同时防止锂中毒事故的发生。目前临床医学检验血清中锂元素含量主要采用火焰原子吸收光谱和基于离子选择性电极的电化学技术。但火焰原子吸收光谱技术需要使用乙炔钢瓶和空气压缩机,存在仪器不能便携,对实验室条件要求苛刻等缺点;电化学方法存在电极处理与更换繁琐,分析效率相对偏低等问题。同时,仪器可便携、操作简单且对锂元素分析具有良好分析性能的液体阴极辉光放电-原子发射光谱技术尚未应用于医疗领域血清中锂含量的测定。因此,基于自制便携液体阴极辉光放电-原子发射光谱装置,建立了血清中锂元素的高灵敏度分析方法。系统考察了10～100倍血清样品稀释倍数对血清样品测试的干扰,结果表明,当血清样品稀释20倍以上时,未发现显著的基体干扰,可以较好地保证结果的可靠性。对影响锂元素分析性能的分析谱线、试液酸度等参数进行了系统优化, 结果表明671 nm为锂元素最佳测试谱线;试液酸度对锂元素分析的灵敏度和稳定性影响显著,采用1%硝酸（V/V）试液酸度可以保证良好的分析性能。在优化的系统参数和实验条件下,锂元素标准曲线的回归方程为：Ie=7 299ρ_Li+400;R2=0.998 3。当血清样品稀释20倍时,该方法对锂元素的检出限为0.2 mg·L-1。对同一血清样品6次重复测试考察本方法的重复性,相对标准偏差小于5%。将本方法应用于血清标准样品（Trace Elements Serium L-2）中锂含量分析,测定值与证书标称值一致。表明该方法可以较好地应用于医疗检验领域实际血清样品中微量锂元素含量的测定。     

火焰原子吸收光谱法测定光学新材料钛酸钡锶中钡和锶

本文介绍了火焰原子吸收光谱法测定光学新材料钛酸钡锶中钒和锶，研究样品制备、测试条件和共存元素干扰，本法的准确度和精密度均满意。     

硼酸锂系列晶体的高压拉曼散射研究

本文进行了硼酸锂系列晶体的高压拉曼散射及其压致相变的研究。对于三硼酸锂（ＬｉＢ３Ｏ５），我们发现在５．０ＧＰａ有一可逆的晶态到晶态的相变，在２７．０ＧＰａ有一不可逆的晶态到非晶态的相变。二硼酸锂（Ｌｉ２Ｂ４Ｏ７）不可逆压致非晶相变发生在３２．０ＧＰａ附近。对于一硼酸锂，我们研究了０—５５．８ＧＰａ范围内的高压拉曼光谱，只在２．０ＧＰａ发现了一个晶态到晶态的相变，但未发现不可逆压致非晶化现象。在硼酸锂系列晶体中，不可逆压致非晶化的压力随Ｌｉ２Ｏ的含量的增加而升高。硼酸锂晶体中Ｌｉ２Ｏ的含量越高，压致非晶化越不容易发生，这与熔体急冷法制备硼酸锂玻璃的规律是一致的。     

X射线荧光分析钒钛铁矿中主次量元素

四硼酸锂为熔剂 ,硝酸锂为氧化剂防止硫元素挥发损失 ,溴化锂作脱模剂 ,玻璃熔片法制备样品。干扰曲线法结合理论α系数法对谱线重叠干扰和基体效应进行校正 ,建立了 XRF测定钒钛铁矿中 Mg,Al,Si,P,S,Ca,Ti,V,Mn,TFe等主次量元素的分析方法。该方法经标准样品验证 ,与推荐值符合较好。 10次制样测量各组分 RSD在 0 .2 7%— 5 .2 4 %范围内     

钽掺杂对钛酸钡导热性能影响的研究

利用光热检测技术测量了钛酸钡材料的导热性能，得到了不同成型压力、烧结温度以及不同 掺杂量下的钛酸钡材料的热扩散率.研究了钽掺杂对钛酸钡材料导热性能的影响，发现了钽 元素掺杂量小于1.5mol%时，钛酸钡材料的热扩散率随掺杂量的增加而增大，当钽元素掺杂 量大于1.5mol%时，热扩散率随掺杂量的增加而减少.对钛酸钡材料的导热性能做了进一步的 分析. 关键词： 光热检测 钛酸钡 导热性能 钽掺杂     

纳克量级锂同位素的高精度质谱测量

锂作为最轻的金属元素，在质谱测量中会发生显著的同位素分馏效应。国内外有关锂同位素的质谱分析研究，多针对的是地质、环境、宇宙学等领域，测定的样品中锂含量都在微克以上量级。针对特殊要求，需要发展纳克量级的痕量锂质谱分析技术。     

X荧光光谱分析法测定含铬不定形耐火材料

含铬耐火材料中的SiO2,Al2O3,Fe2O3,TiO2,CaO,MgO和Cr2O3等直接影响着产品质量,属于需控制成分。文章用市售耐火材料标准品和基准试剂配制出适当含量范围且有一定梯度的系列标准样,以四硼酸锂-偏硼酸锂(质量比67∶33)作熔剂、熔样过程中添加碘化铵固体脱模剂的方法制备样品玻璃熔片,通过X射线荧光光谱法(XRF)测定元素的荧光强度,并以理论α系数基体校正法消除吸收与增强效应,从而得到测量上述组分的定量校正曲线。该方法应用于耐火材料标准品的测定,所得结果与标准值吻合。应用于实际样品的测定并和化学法比较,结果准确,精密度好,操作简单、快速,具有良好的实用性。     

BaTiO_3纳米粉体的制备及结构的光谱表征

采用钛酸丁脂和八水氢氧化钡为原料的溶胶-凝胶法制备了纳米BaTiO3粉体。经不同温度烧结,并利用X射线衍射和Raman光谱分析进行结构表征。实验表明,经1073K烧结后粉体粒径为26 2nm,颗粒分布均匀,还有少量BaCO3存在。在这个温度下得到的晶粒主要是立方相,并含有少量的四方相。经1273K烧结后,BaTiO3完全是四方相,粉体粒径为80 0nm,此时BaCO3已完全分解。另外探讨了溶胶-凝胶制备纳米BaTiO3粉体的反应机理,解释了BaTiO3物相的形成。     

ICP-AES内标法测定硅铝钡合金中铝和钡

研究了以电感耦合等离子体发射光谱仪测定硅铝钡合金中铝和钡的方法。考查了方法的线性范围,检测限和RSD等指标,实验表明,方法简便,结果准确。     

Dielectric properties of barium titanate ceramics modified by SiO2 and by BaO-SiO2

The influence of SiO₂ on the dielectric properties of barium titanate ceramics was investigated. SiO₂ had been doped solely and together with BaO into barium titanate before calcination. X-ray diffraction showed that all the ceramics were of a pure perovskite phase after sintering at 1275 °C for 2 h. For SiO₂-doping, there was about 2.5 °C increase in Curie temperature per molar percentage of doping and the leakage current was obviously increased, especially at low voltages for relatively high doping levels. While for the co-doping of SiO₂ and BaO, there was little change in Curie temperature. The point defects formed through the dopings were proposed responsible for the effects. It was suggested that SiO₂ is important to barium titanate ceramics not only for sintering but also for modifying their properties.     

Fabrication and optical reflection behavior of a two-dimensional barium titanate ceramic photonic crystal

We demonstrate a method for fabricating a two-dimensional hexagonal array of nanoscale barium titanate ceramic pillars. A precursor array was prepared by introducing a sol solution into an electron-beam resist mold with air holes and subsequently dry etching the unnecessary gel layer formed on the mold. A ceramic array, consisting of barium titanate ceramic pillars with a radius of 85 nm, a lattice constant of 450 nm, and a height of 500 nm, was fabricated by sintering the precursor array at 1073 K. The reflection spectra for the ceramic array in the visible range revealed the underlying photonic band gaps, which were in good agreement with results calculated using a plane-wave method. PACS 77.84.-s; 42.70.-a; 42.70.Qs     

钛酸铋钡陶瓷的介电性、铁电性及对晶格结构的依赖性

采用溶胶-凝胶工艺成功制备出BaBi₄Ti₄O₁₅微细粉料，并利用此微粉烧结出成瓷良好的BaBi₄Ti₄O₁₅陶瓷.研究了BaBi₄Ti₄O₁₅陶瓷的铁电 顺电相 变，测定了BaBi₄Ti₄O₁₅的介 电特性和饱和状态下的铁电特性.所作测量表明B 关键词： 铁电性 介电性 晶格结构 溶胶 凝胶法     

Semiconducting ceramic barium lanthanum titanate doped with iron

The formation of semiconductive properties in polycrystalline barium titanate when doped simultaneously with lanthanum and iron is brought about by a substitution mechanism similar to that proved to work in BaTiO₃ doped with bismuth and iron. A broader validity has thus been confirmed of the substitution model previously proposed to explain the considerable change in internal electric resistance of barium titanate containing trivalent ions in barium positions when iron ions are introduced. In contrast to barium bismuth titanate, with barium lanthanum titanate an increasing addition of iron leads to the successive formation and destruction of several types of perovskite crystals differing in electrical conductivity and Curie temperature.The author thanks his collaborators from the Research Institute of Electrotechnical Ceramics for effective help: Ing. L. Plocek for the X-ray analyses and Mr. V. tefek for preparing the electron microscope pictures.     

Photorefractive BaTiO(3) spheres and spherical disks

We have produced single-crystal spheres and spherical disks of photorefractive barium titanate (BaTiO(3)) . The spheres and disks allow direct fiber-to-fiber two-beam coupling without additional optical elements. We also investigate the spontaneous oscillation of triangles and other whispering-gallery modes in these spherical structures.     

微波消解-电感耦合等离子体-原子发射光谱法测定油墨中的铅、铬和钡

建立了微波消解-电感耦合等离子体-原子发射光谱法(ICP-AES)测定油墨中铅、钡和铬元素的分析方法.实验选用钇作为内标物,以减少背景干扰.结果表明,各元素校准曲线的相关系数均为0.9999,样品相对标准偏差小于5％,加标回收率在96.7％-98.8％之间.实验具有较好的精密度和准确性,适合油墨中铅,铬,钡元素的分析.     

Second Harmonic Generation in Microstructured Barium Titanate

We investigate the second harmonic generation under femtosecond pulse-periodic laser radiation in barium titanate in the form of ceramics, in pores of a globular photonic crystal, and in a water colloidal suspension. We measure the dependence of the second harmonic radiation intensity on the incident laser power. Excitation of the second harmonic was carried out by powerful (10⁸ W) pulses of a solid-state Yb:KGW laser (wavelength, 1,026 nm) operating at 200 kHz. We estimate the efficiency of the second harmonic generation in various microstructured phases of barium titanate and show that the threshold of plasma formation in a suspension of barium titanate microparticles in water is substantially higher than in ceramics and in the ferroelectric photonic crystal. The second-harmonicgeneration power can be significantly increased in a water suspension of barium titanate microparticles.