（Sr,Ba）1—xEuxTiO3的高温高压合成及XPS研究

用高温高压法合成了Ｓｒ１－ｘＥｕｘＴｉＯ３（ｘ＝０．０，０．１，０．２，０．３，０．４，０．５）及Ｂａ０３。Ｅ０。７ＴＯ３化合物。结果表明，所有样品均为立方结构，样品中存在Ｅｕ（Ⅱ）和Ｅｕ（Ⅲ）混合价。Ｅｕ＾３＋的掺入直接影响了Ｓｒ离子与氧离子的结合。使Ｓｒ３ｐ３／２的结合能随Ｘ的增加而增加。     

A_2BO_4型催化活性材料结构与性能的研究Ⅰ．［La_（k－x）Sr_x□_（1－k）］_2Cu_（1－y）□_yO_（4－δ）体系

以硝酸盐为原料，用柠檬酸络合法按［Ｌａ１－ｋＳｒｘ□ｋ－ｘ］２ＣｕＯ４（Ｘ＝０、０．０５、０．１、０．１５、０．２，ｋ＝０．０２５）的配比制备了５个样品．应用多晶Ｘ射线衍射法研究了此Ｌａ－Ｓｒ－Ｃｕ－Ｏ系列Ａ２ＢＯ４型复合氧化物的非完整结构．结构研究表明，此系列结构空位型非完整的存在，使结构中Ｂ位的铜离子变价为Ｃｕ２＋和Ｃｕ３＋．但是，随着Ａ位Ｓｒ加入量的增加，Ａ位空位的减少，结构中Ｂ位Ｃｕ３＋量随之减少，Ｃｕ２＋量随之增加，样品对于ＣＯ氧化的催化性能缓慢下降，而ＮＯ还原的催化能力增强．高价态的Ｃｕ３＋的存在是实现对ＣＯ催化氧化的条件；而Ｃｕ２＋给电子能力促进了Ｎｏ－的生成，是ＮＯ催化还原的活性来源．从此系列样品的催化性能和精细结构的研究可得出，适当地调节Ａ２ＢＯ４型结构中Ａ位和Ｂ位的空位及Ｓｒ２＋的掺入量，使Ｂ位Ｃｕ２＋和Ｃｕ３＋保持适当的比例，可获得ＣＯ催化氧化和ＮＯｘ催化还原同时具有较高活性的催化活性材料．     

Pr_（2－x）Sr_xNiO_（4±δ）的合成、结构和电磁性质

用固相法合成了Ｐｒ＿（２－ｘ）Ｓｒ＿ｘＮｉＯ＿（４±δ）（０．０≤ｘ≤１．０）系列Ｋ＿２ＮｉＦ＿４型化合物，研究了其结构，红外光谱，电磁性质。当０．０≤ｘ＜０．１和ｘ＝１．０时以正交晶系结晶；当０．１≤ｘ＜１．０时以四方晶系结晶；Ｎｉ离子平均价态在＋２至＋３价之间。当ｘ值较小时，样品中含有过量的氧。ＮｉＯ＿６八面体中Ｎｉ￣（３＋）的Ｊａｈｎ－Ｔｅｌｌｅｒ畸变引起ｃ／ａ值在ｘ＝０．５处出现极大，在７７～２５０Ｋ之间，样品磁性质符合居里－外斯定律，并表现出反铁磁相互作用。电学性质的变化可以理解为Ｎｉ￣（３＋）离子电子组态由：变至的结果     

（CeO2）0.7—x（MO）x（La2O3）0.3（M=Mg,Ca,Sr）固体电解质及其性能的…

合成了（ＣｅＯ２）０．７－ｘ（ＭＯ）ｘ（Ｌａ２Ｏ３）０．３（Ｍ－Ｍｇ、Ｃａ、Ｓｒ）固体电解质。对其晶体结构、电导率、ＸＰＳ谱、离子迁移数及制成的燃料电池的Ｖ－Ｉ曲线进行了测定。（ＣｅＯ２）０．７（Ｌａ２Ｏ３）０．３中掺入Ｃａ＾２＋、Ｍｇ＾２＋或Ｓｒ＾２＋，可使电解质的氧离子导电性能改善，从而使制成的燃料电池的开路电压输出功率也得到提高。     

（CeO_2）_（0．7－x）（MO）_x（La_2O_3）_（0．3）（M＝

合成了（ＣｅＯ＿２）＿（０．７－ｘ）（ＭＯ）＿ｘ（Ｌａ＿２Ｏ＿３）＿（０．３）（Ｍ＝Ｍｇ、Ｃａ、Ｓｒ）固体电解质。对其晶体结构、电导率、ＸＰＳ谱、离子迁移数及制成的燃料电池的Ｖ－Ｉ曲线进行了测定。（ＣｅＯ＿２）＿（０．７）（Ｌａ＿２Ｏ＿３）＿（０．３）中掺入Ｃａ￣（２＋）、Ｍｇ￣（２＋）或Ｓｒ￣（２＋），可使电解质的氧离子导电性能改善，从而使制成的燃料电他的开路电压输出功率也得到提高。     

NdSr_（1－x）M_xNiO_4（M＝Ca，Ba）的合成，结构和电学磁学性

用固相法首次合成了ＮｄＳｒ＿（１－ｘ）Ｍ＿ｘＮｉＯ＿４（Ｍ＝Ｃａ：０．０≤１．０；Ｍ＝Ｂａ：０．０≤ｘ≤０．６）系列复合氧化物，并研究了其结构，红外光谱，电学性质和磁学性质。除ＮｄＣａＮｉＯ以正交晶系结晶外，其它试样的结构均属于四方晶系。ＩＲ谱显示随Ｃａ￣（２＋）离子含量的增加，ＮｄＳｒ＿（１－ｘ）Ｍ＿ｘＮｉＯ＿４的Ｎｉ－Ｏ键缩短，Ｃａ￣（２＋）和Ｂａ￣（２＋）引入ＮｄＳｒＮｉＯ＿４以取代Ｓｒ￣（２＋），使试样由金属性导电转变为半导体性导电；随Ｃａ￣（２＋）含量增加，试样的室温电阻率增大。７７～３００Ｋ磁化率与温度关系曲线显示，所有试样的Ｎｉ￣（３＋）都以低自旋状态存在。     

纳米晶La_（1－_x）Sr_xFeO_3的合成及气敏特性的研究

用柠檬酸盐法合成出Ｌａ_（１－_ｘ）Ｓｒ_ｘＦｅＯ_３（ｘ＝０．１，０．２，０．３，０．４）原粉，再经固相反应得到纳米晶粉末，用ＴＧ、ＤＴＡ、ＸＲＤ、ＩＲ进行了表征，确证复合氧化物Ｌａ_（１－_ｘ）Ｓｒ_ｘＦｅＯ_３为钙钛矿型结构，粒径在１０～２５ｎｍ之间。实验结果表明，随着固相反应条件不同，产物粒径呈规律性变化．气敏特性研究表明，该纳米晶材料对乙醇有较高的选择性和灵敏度，其选择性顺序为Ｌａ_（０．９）Ｓｒ_（０．１）ＦｅＯ_３＞ＬａＦｅＯ_３＞ＬａＦｅＯ_３（大晶粒）。     

Syntheses，Structures and Properties of Some New Composition Perovskite Compounds：Sr_（0．6）Bi_（0．4）FeO_（2．7），Sr_（1－x）Bi_xFeO_（3－y） and Ba_（1．5）Pt_（0．5）Mn_2O_6

Ｓｙｎｔｈｅｓｅｓ，ＳｔｒｕｃｔｕｒｅｓａｎｄＰｒｏｐｅｒｔｉｅｓｏｆＳｏｍｅ　ＮｅｗＣｏｍｐｏｓｉｔｉｏｎＰｅｒｏｖｓｋｉｔｅＣｏｍｐｏｕｎｄｓ：Ｓｒ_（０．６）Ｂｉ_（０．４）ＦｅＯ_（２．７），Ｓｒ_（１－ｘ）Ｂｉ_ｘＦｅＯ_（３－ｙ）　ａｎｄ　Ｂａ...     

溶胶－凝胶法合成（Mg，Ca）O－SiO_2∶Eu~（3＋），Bi~（3＋）发

以Ｍｇ（ＮＯ３）２、Ｃａ（ＮＯ３）２、Ｅｕ（ＮＯ３）３、Ｂｉ（ＮＯ３）３、ＬｉＮＯ３和Ｓｉ（ＯＣ２Ｈ５）４为反应物，采用溶胶－凝胶法，在比较低的温度下，首次合成０．７０１ｍｏＩＭｇＯ－０．１７５ｍｏｌＣａＯ－１．２５ｍｏＩＳｉＯ２∶０．０６ｍｏｌＥｕ（３＋），０．００２ｍｏＩＢｉ（３＋）（加入Ｌｉ＋作为电荷补偿剂）发光体。得到了最佳合成条件。研究了由溶胶向凝胶转变和凝胶向发光晶体的转变过程。探讨了发光体在不同激发波长激发下的发光特性以及在激活剂、敏化剂不同掺杂量下的发光行为。讨论了在（Ｍｇ（ａ）Ｏ－ＳｉＯ２基质中Ｂｉ（３＋）对Ｅｕ（３＋）的能量传递和敏化作用。     

秦油2号油菜高产栽培中喷肥优化配方研究

采用二次饱和－Ｄ最优设计的方法，研究Ｓｒ（ＮＯ３）２（ｘ１）、ＫＨ２ＰＯ４（ｘ２）和Ｎａ２Ｂ４Ｏ７·１０Ｈ２Ｏ（ｘ３）叶面喷施对秦油２号油菜的产量效应，获得回归方程：ｙ＝２４７．４８５＋７．００４８ｘ１＋２．２９２４４ｘ２—９．８２６４６ｘ３—０．２５３５ｘ１ｘ２—１３．８５２４ｘ１ｘ３：—３．３７４７５ｘ２ｘ３＋２７．０５７５Ｘ２１—１６．３０３６ｘ２２—８．７６７８ｘ２３结果表明Ｓｔ（ＮＯ３）２。有明显的增产作用．ｘ１ｘ３的交互作用（效应）最大．通过计算机模拟．其最佳因子组合为Ｓｒ（ＮＯ３），０．１％、ＫＨ２ＰＯ４０．３％和硼砂０．０１％，预计产量可达２９６．４６ｋｇ／６６７ｍ２．     

Conductive Composite Materials of Polyethylene and Polypyrrole with High Modulus and High Strength

Composite films of polyethylene (PE) and polypyrrole (PPy) were prepared by polymerization of PPy on an ultradrawn polyethylene film with high modulus and high strength in ferric chloride (FeCl₃) aqueous solution. The electrical conductivity of the composite film was found to be related to the polymerization conditions, such as polymerization temperature, polymerization time, the concentration and the oxidation potential of the FeCl₃ solution. Scanning electron microscopy, FTIR and ¹³C NMR spectra were used to elucidate the morphological and structural variations of PPy prepared under different conditions, which lead to the differences in the electrical properties of the resultant composite films. The best electrical conductivity of the composite was about 5.5 S/cm for the film prepared under optimum conditions. The Young's modulus and the tensile strength reached 80 GPa and 3.2 GPa, respectively, which indicated the successful production of a conductive polymer with high strength and high modulus.     

高模量高强度聚合物的分子设计与加工技术

对高模量高强度聚合物材料的结构与其力学性能的关系,以及近年来在这方面研究中出现的一些新的加工手段进行了介绍。     

基于高分辨质谱的甲基化心磷脂高通量分析方法的建立和应用

该文基于心磷脂标准品的甲基化反应,建立了高灵敏度高通量分析甲基化心磷脂的液相色谱 - 高分辨质谱方法。由于甲基化后的心磷脂具有特征性的碎片,因此建立了包含780个分子特征片段的模拟数据库用于脂质鉴定。衍生化后,CL（14∶0/14∶0/14∶0/14∶0）信号提高了10倍,定量下限（LOQ）达到10 ng/mL。将该方法应用于小鼠衰老过程中心磷脂的调控研究,通过Tracefinder本地二级数据库共鉴定了43个心磷脂分子,其中21个心磷脂在衰老的大脑中有差异变化。结果发现：含有FA（20∶4）、FA（22∶6）长链多不饱和脂肪酸的心磷脂在衰老过程中呈下降趋势。高分辨质谱平台为甲基化的心磷脂分析提供了一种高通量筛选方法,对于低丰度心磷脂的检测具有很大潜力。     

高温高压水中干酪根热解的拉曼光谱原位研究

利用对顶砧压腔装置,以金刚石作为顶砧,通过观测和采用拉曼光谱对干酪根在高温高压水中热解的具体过程进行了原位研究.由于金刚石顶砧只在约1 332 cm-1波数出现一个很强很尖锐的峰,因此用于压 标的石英、介质水以及样品干酪根的拉曼峰都未受影响.测试了在450℃和850 MPa条件下干酪根变化的拉 曼峰.随着温度和压力的增加,干酪根在1 600 cm-1波数附近由于芳香环振动引起拉曼峰的最大峰位置 (vmax)和半高宽(FWHM)存在转折变化.在干酪根热解之前,其芳香环结构和无序结构之间的缺陷向有序化变化.而对于干酪根的热解过程,先是热解为液相碳氢化合物,随后进一步热解为更小分子的成分,如 CH4.干酪根的热解过程与压力密切相关,增加压力对热解存在抑制作用.     

含镧金属富勒烯不同溶剂的高温高压提取

将金属原子或离子置于以Ｃ６０、Ｃ８２为代表的富勒烯笼内形成金属富勒烯包合物是目前富勒烯研究的热点课题［１～３］．合成的金属富勒烯常伴随生成较难分离的空心富勒烯,传统的索氏提取法效率又较低,使得金属富勒烯的深入研究受到限制［１,２］．本文采用改进的高温...     

Analysis of Rotenoids by High Temperature High Resolution Gas Chromatography-Mass Spectrometry

A short glass capillary column coated with PS-090 (20% phenyl–80% methylpolysiloxane, of 10 m × 0.30 mm i.d.; with 0.1 μm film thickness) was used to analyze samples from Tephrosia candida; eighteen rotenoids were separated and identified without derivatization by HT-HRGC and HT-HRGC-MS. The mass spectra show the typical fragmentation pattern for rotenoids, with the base peaks either at M⁺, or originating from RDA (Retro Diels-Alder) rearrangements. HT-HRGC and HT-HRGC-MS were shown to be extremely valuable and neglected techniques for structural studies as well as the routine analysis of rotenoids in crude extracts. Possible applications to other classes of aromatic natural products, e.g. flavonoids, are envisaged.     

Application of High Temperature High Resolution Gas Chromatography to Crude Extracts of Propolis

The underivatized acetone and hexane fractions from propolis samples (predominant flora Citrus spp. and Vernonia polyanthes) were analyzed by HT-HRGC (high temperature high resolution gas chromatography) and HT-HRGC coupled to mass spectrometry (HT-HRGC-MS). Several compounds, including flavonoid aglycones, phenolic acids, and high molecular weight compounds were characterized in crude extracts by HT-HRGC-MS. HT-HRGC and HT-HRGC-MS were shown to be quick and informative tools for rapid analysis of crude extracts without need for prior derivatization and purification.     

A New Method of Measurement for Elastic Wave Velocities in Minerals and Rocks at High Temperature and High Pressure and Its Significance

We developed a new method of measurement for elastic wave velocity of rocks and minerals at high temperature and high pressure in a wedge-type cubic anvil. The shear-wave and other ultrasonic wave can be identified by full wave phase analysis (FWPA), thus the velocities of compression-wave and shear-wave can be obtained in a single experiment. We have done the measurements of elastic wave velocities on pyrophyllite, etc. at high pressure (0.1—5.5 GPa) and high temperature (ambient temperature 1600℃), the ranges of the pressure and the temperature are in the head among the methods of the wave velocites measurement in laboratory in the world.     

Well‐Defined High Molecular Weight Polystyrene with High Rates and High Livingness Synthesized via Two‐Stage RAFT Emulsion Polymerization

A highly living polymer with over 100 kg mol⁻¹ molecular weight is very difficult to achieve by controlled radical polymerization since the unavoidable side reactions of irreversible radical termination and radical chain transfer to monomer reaction become significant. It is reported that over 500 kg mol⁻¹ polystyrene with high livingness and low dispersity could be synthesized by a facile two‐stage reversible addition–fragmentation transfer emulsion polymerization. The monomer conversion reaches 90% within 10 h. High livingness of the product is ascribed to the extremely low initiator concentration and the chain transfer constant for monomer unexpectedly much lower than the well‐accepted values in the conventional radical polymerization. The two‐stage monomer feeding policy much decreases the dispersity of the product.

     

Application of High Pressure-DTA for High Pressure-liquid Phase Epitaxy of Doped Mercury and Thallium HTS Formations

The fabrication method of superconducting thin films of compositions HgBa₂Ca₂Cu₃O_8+δ (Hg-1223) and Tl₂Ba₂CuO_y (2201) on single-crystalline SrTiO₃ and LaAlO₃ substrates is reported. The highest obtained T _c was 134 K and J _c over 10⁶ A cm^–2 at 77 K. High pressure DTA(HP-DTA) was applied to grow mercury- and thallium-based high-temperature superconducting crystals and thin films, to identify melting points of particular phases within these oxide systems and determine suitable processing conditions. The DTA system operates at the: maximum temperature of 1200°C, volume up to 5 cm³, working pressure up to 1.5 GPa and at a working atmosphere — inert gas with up to 25% oxygen. This revised version was published online in August 2006 with corrections to the Cover Date.