X射线粉末衍射法测定未知晶体结构

以新化合物Ba₃BPO₇为例 ,介绍了利用X射线粉末衍射技术测定未知晶体结构的方法 .首先采用分峰的方法将粉末衍射数据还原为类似单晶的数据 ,然后利用单晶结构分析的方法确定该化合物中钡、磷和硼原子的位置 ,同时结合振动光谱分析提供的硼和磷的配位多面体结构信息 ,确定了氧原子的位置 ,最后利用Rietveld方法进行了结构精修.     

EFFECT OF HIGH-ANGLE DIFFRACTION DATA ON RIETVELD STRUCTURE REFINEMENT

By utilizing the powder X-ray step-scanning diffraction data of PbSO₄, we have studied the effect of the diffraction data (with different high-angle upper-limit: 2θ_m= 160,140,120,100,80, 70 and 60°) on the precision of the Rietveld refined lattice constants, structure parameters, and agreement indices. Tbese refined results are compared with those obtained from the single crystal data. It is revealed that the deviations of the refined lattice constants, atomic positions and isotropic temperature factors decrease, and agreement indices become smaller With the increase of 2θ_m. But when 2θ_m> 120°, the deviations and agreement indices decrease very slowly. Therefore, in general cases, 2θ_m should be taken to be 120°or larger in order to get satisfactory refined results in the Rietveld crystal structure refinement.     

液相色谱-串联质谱法测定粮谷中的伏马毒素

建立了液相色谱-串联质谱同时测定玉米、小麦、大米和黄豆中伏马毒素FB1、FB2的分析方法。样品经甲醇-水-乙酸(74∶25∶1)提取,强阴离子交换柱(SAX)净化后,以0.1%乙酸水溶液-乙腈为流动相,ZORBAX Extend-C18反相色谱柱(150 mm×2.1 mm,1.8 μm)进行色谱分离,在电喷雾正离子化模式下,选择反应监测(SRM)方式进行测定。结果表明：FB1和FB2分别在2.5~1 000、5.0~1 000 μg/L范围内线性关系良好,相关系数分别为0.999 5和0.999 7。对4种空白基质分别进行0.02、0.50、2.00 mg/kg 3个水平的加标回收实验,FB1和FB2的加标回收率分别为67.5%~90.5%和70.5%~95.3%,相对标准偏差(RSD)分别为1.3%~11.4%和1.5%~10.6%,检出限分别为2.00 μg/kg和4.00 μg/kg。该方法稳定、可靠,适用于谷物中FB1和FB2的同时检测与确证。     

Bandgap narrowing in the layered oxysulfide semiconductor Ba_3Fe_2O_5Cu_2S_2: Role of FeO_2 layer

A new layered Cu-based oxychalcogenide Ba_3Fe_2O_5Cu_2S_2 has been synthesized and its magnetic and electronic properties were revealed. Ba_3Fe_2O_5Cu_2S_2 is built up by alternatively stacking [Cu_2S_2]~(2-) layers and iron perovskite oxide[(FeO_2)(BaO)(FeO_2)]~(2-)layers along the c axis that are separated by barium ions with Fe~(3+) fivefold coordinated by a square-pyramidal arrangement of oxygen. From the bond valence arguments, we inferred that in layered CuC h-based(Ch =S, Se, Te) compounds the +3 cation in perovskite oxide sheet prefers a square pyramidal site, while the lower valence cation prefers the square planar sites. The studies on susceptibility, transport, and optical reflectivity indicate that Ba_3Fe_2O_5Cu_2S_2 is an antiferromagnetic semiconductor with a Ne′el temperature of 121 K and an optical bandgap of 1.03 eV. The measurement of heat capacity from 10 K to room temperature shows no anomaly at 121 K. The Debye temperature is determined to be 113 K. Theoretical calculations indicate that the conduction band minimum is predominantly contributed by O 2p and 3 d states of Fe ions that antiferromagnetically arranged in FeO_2 layers. The Fe 3d states are located at lower energy and result in a narrow bandgap in comparison with that of the isostructural Sr_3Sc_2O_5Cu_2S_2.     

高居里点(1-x)Ba_(0.998)La_(0.002)TiO_3+xBi_4Ti_3O_(12)系统陶瓷微观结构及温度特性的研究

采用传统陶瓷制备工艺制备(1-x)Ba_(0.998)La_(0.002)TiO_3+ xBi_4Ti_3O_(12) (0≤x≤0.01)系统陶瓷.对在还原气氛(氮气)中烧成的陶瓷样品在一定温度下进行再氧化处理.研究了不同Bi_4Ti_3O_(12)掺杂浓度以及再氧化过程对BaTiO_3微观结构、介电性能及居里温度Tc的影响.结果表明:掺杂Bi_4Ti_3O_(12)后,BaTiO_3陶瓷的晶粒尺寸明显减小;Bi_4Ti_3O_(12)具有提高陶瓷居里点温度的作用,当x=1.0时,居里温度提高到T_c=150 ℃.随着BIT加入量的增加,电子与缺位混合补偿,晶格中将产生金属离子缺位,以补偿多余电子,因此随着BIT掺入量的增加,电阻率逐渐增大.     

新型4d/5d基超导体的结构和物性

在强关联电子体系中,轨道、自旋和晶格等自由度之间的相互作用一直是研究的热点.这些自由度之间的竞争和共存产生了复杂新奇的物理现象,如超导现象、量子相变、自旋有序、拓扑相变、金属绝缘转变等,这些丰富的物理现象来源于不同的有序态或量子涨落之间的竞争和耦合.自旋轨道耦合作用是指粒子的自旋角动量和轨道角动量之间的相互作用,在4d/5d基化合物中,由于电子的运动速度较快,自旋轨道耦合的效应不可忽视,可能表现出与3d基化合物不同的物性.例如,在含4d/5d过渡族金属元素的超导体中,其电子配对的机制可能不同于常规的s波Bardeen-Cooper-Schrieffer超导体.本文以几种典型的4d/5d基超导体为例,对其晶体结构和超导物性及其内在联系进行了详细论述,重点探讨了阴离子共价键强弱对晶体结构、相变和超导物性的影响,希望引起相关研究者对该类超导体的重视.     

新型FeSe基超导材料研究进展

FeSe基超导体作为铁基超导材料家族的重要组成部分,已经成为凝聚态物理研究的一个热点领域,对这类超导材料的探索和制备是研究其物理性质的基础.目前,对于FeSe基超导材料的探索主要集中于插层和外延单层FeSe薄膜.其中,通过插层方法获得的FeSe基超导材料具有独特的性质,且种类众多.本文介绍了近年来发现的一系列FeSe基高温超导材料,涵盖K_xFe₂Se₂,A_xNH₃FeSe,LiOHFeSe和有机分子插层FeSe等,并针对各种材料,简述了其性质及影响.     

New Type of Nitrides with High Electrical and Thermal Conductivities

The nitrogen dimer as both a fundamental building unit in designing a new type of nitrides, and a material gene associated with high electrical and thermal conductivities is investigated by first principles calculations.The results indicate that the predicted Si N4 is structurally stable and reasonably energy-favored with a striking feature in its band structure that exhibits free electron-like energy dispersions. It possesses a high electrical conductivity(5.07 × 10~5 S/cm) and a high thermal conductivity(371 W/m·K) comparable to copper. The validity is tested by isostructural Al N4 and Si C_4. It is demonstrated that the nitrogen dimers can supply a high density of delocalized electrons in this new type of nitrides.     

PVT法SiC单晶生长传热分析

研究了PVT法生长SiC过程中的传热行为,以优化生长条件、获得高质量单晶.该研究是针对坩埚盖(籽晶粘附于坩埚盖上)和炉盖之间的传热行为进行的.研究认为,坩埚盖上部石墨毡开孔形状和大小对坩埚盖的径向温度场有很大影响.采用本文简化的模型可以估算坩埚在不同位置下、不同的石墨毡开孔形状和大小时坩埚盖和炉盖之间总的辐射热阻和传热量.对影响坩埚盖和炉盖之间传热的因素进行了讨论.另外,讨论了在生长过程中动态调整坩埚盖散热条件的可行性.     

侧边抛磨单模光纤表面等离子体传感器的设计和优化

光纤表面等离子体共振传感器具有体积小、抗电磁干扰,可以实现在线实时远距离检测的优点。为提高传感器的性能,建立了侧边抛磨光纤表面等离子体共振传感的物理模型,分别研究了侧边抛磨光纤的剩余厚度、银膜层的厚度对传感器的灵敏度、共振峰的深度和半高全宽等的影响。结果表明：光纤剩余厚度越小,表面等离子体共振现象越强;随银膜层的厚度增大,共振峰的宽度变宽,而传感器的灵敏度呈现非单调变化。通过综合表面等离子体共振传感器的折射率传感灵敏度和共振峰半高全宽,提出了质量因数作为传感器的优化指标,并最终得到最优化的设计方案为光纤剩余厚度为66.5 μm,银膜的厚度为50 nm,此时质量因数达到98.67。