冰晶石型氟化物Na_3FeF_6的水热合成、表征及磁学性质研究

采用水热法制备了冰晶石型氟化物Na3FeF6,通过粉末X射线衍射、扫描电子显微镜、差热-热重分析等手段对化合物的性质进行了表征。该化合物空间群为单斜晶系。晶胞参数为a=5.513A,b=5.728A,c=7.964A,并对其磁学性质进行了研究。     

Zn55.24Al18.86Zr25.9的晶体结构研究

采用平衡合金法制备了Zn_(55.24)Al_(18.86)Zr_(25.9)三元化合物的合金样品,利用XRD、扫描电镜(SEM)对样品进行了表征,并使用Rietveld全谱拟合方法对化合物的晶体结构进行了研究。Rietveld精修的可靠性因子为:R_p=7.15%,R_(wp)=9.56%。该化合物属立方晶系,空间群为p4/mmm,点阵常数a=b=4.070 803,c=4.073 669。精修的结果表明Zr原子占据1a位置,部分Zn原子占据2e位置,另一部分Zn原子和Al原子混合占据1c位置。最后通过理论计算验证了所得结构的合理性。     

碱性染料与磷钨酸形成的新型电荷转移盐的制备与表征

报道了用Keggin结构的磷钨酸与碱性染料结晶紫、碱性藏红T和碱性湖兰BB反应形成的3种新型电荷转移盐。利用元素分析、差热-热重、变温红外、固体漫反射电子光谱对标题化合物的组成、热稳定性和光学性质进行了表征。     

钙钛矿型氧化合物AgNbO3的水热合成与表征

采用水热法制备了钙钛矿型化合物Ag-NbO3晶体,对化合物进行粉末X射线表征。Rietveld精修结果表明化合物AgNbO3属于三方晶系,空间群为R-3C。并对化合物进行了扫描电子显微镜(SEM)、BET法测定比表面积和对固体紫外漫反射光谱进行表征。对该化合物的光催化性质进行了测试,在可见光照射下降解染料龙胆紫。结果表明此化合物在室温下具有很高的光催化性质,在光催化性能方面具有潜在的应用价值。     

直流溅射法制备SnO_2纳米薄膜及其表征

采用直流溅射法,以纯锡为靶材制备出了SnO_2纳米薄膜,并利用X射线衍射仪、透射电镜及台阶仪对纳米薄膜的物相结构及厚度进行了分析测试。结果表明:采用单晶硅作为衬底时可以制备出晶态的SnO_2纳米薄膜,该纳米薄膜由粒径几纳米到十几纳米的SnO_2小颗粒组成,而采用载玻片作为衬底时则制备出了非晶态的SnO_2纳米薄膜;通过控制溅射时间,可以得到一系列不同厚度的SnO_2纳米薄膜,直流溅射法制备SnO_2纳米薄膜的膜厚公式为d=0.29UIt(其中d为薄膜厚度,,1=0.1 nm;U为溅射电压,V;I为溅射电流,A;t为溅射时间,s)。     

PbO-CrO_3系化合物的X射线研究及声光性质予测

对 PbO-CrO_3系化合物5PbO·CrO_3和2PbO·CrO_3进行了 X 射线结晶学研究,精确测定了它们的晶胞参数和粉末衍射数据并加以指标化。确定5PbO·CrO_3为同成份熔融化合物,其三斜晶胞参数 a=8.19(3)(?),b=9.29(2)(?),c=23.79(13)(?),α=109.12(35)°,β=114.22(39)°,γ=79.82(27)°。测得2PbO·CrO_3的单斜晶胞参数为a=14.020(2)(?),b=5.6799(7)(?),c=7.1419(8)(?),β=115.21(1)°。对这两个化合物的声光性质的予测表明,它们均具有大的声光优值,可望作为新的声光晶体材料。     

Pt-M(M=Fe, Co, Ni)金属间化合物电子结构和弹性性质的第一性原理研究

通过基于密度泛函理论的第一性原理计算方法,研究了Pt-M(M=Fe,Co,Ni)各金属间化合物的结构、能量、电子结构和弹性性质。首先对Pt-M(M=Fe,Co,Ni)金属间化合物进行几何优化,对其能带结构、总态密度、分态密度、键合特征和弹性性质进行研究,并计算各金属间化合物的结合能与生成焓。计算所得晶格参数与实验值和文献计算值吻合。PtFe_3的生成焓最小,结合能最大,说明PtFe_3较其他合金相更稳定、键合力更强。通过对Pt-M(M=Fe,Co,Ni)的能带结构和电子态密度进行计算,分析了其结构稳定性的物理本质。PtFe_3-t中Pt-Fe和Fe-Fe键相比其他合金相键长较短且电荷密度较高,说明PtFe_3-t中Pt-Fe和Fe-Fe键的键能比其他合金相大,所以PtFe_3-t合金相的结构稳定性最好。对Pt-M(M=Fe,Co,Ni)弹性性质的研究表明PtFe_3为脆性相,PtFe、Pt3Fe、PtCo、Pt_3Co、PtNi和PtNi3为延性相,其中Pt_3Co的塑性最好,PtFe_3-t有较高的弹性模量,其原子间结合力相对较强,材料的强度较大。     

自蔓延高温合成Ti2SnC粉体及反应机理的研究

采用自蔓延高温合成技术制备了Ti_2SnC粉体材料,利用XRD、SEM、EDS、TEM及DTA等分析手段对其形貌结构进行表征,在室温条件下其晶格参数a和c分别为3.186和13.630。分析了Ti2SnC的形成机制。在Ti-Sn-C反应体系中,Sn在232℃时熔化为液态,随着温度的升高,钛包裹在碳的外面形成钛碳层,继续加热Ti和Sn反应生成Ti-Sn金属间化合物TixSny,如Ti_6Sn_5和Ti_5Sn_3,在800℃左右钛碳层形成了TiC,在1100℃左右TiC与TixSny发生反应生成类盘状的Ti_2SnC。     

持续电流作用下金属间化合物NiAl薄板热弯成形

目的 为了解决和克服现有耐高温金属间化合物成形难、传统等温热成形效率和能源利用率低的问题,开发持续电流作用下金属间化合物薄板热弯成形新技术。方法 首先,对NiAl板材进行系统的升温实验,确定热弯成形的电流密度。然后对NiAl板材进行三点弯曲实验,确定凸模下压速度。最后,在自行设计并制作的可实现电与载荷持续复合作用的热弯成形装置和陶瓷绝缘模具上对板材进行热弯成形实验。结果 在电流密度为8.5 A/mm²、加热温度为1 300 ℃、凸模下压速度为0.5 mm/min的实验条件下,成形后的热弯件尺寸精度良好、厚度均匀,无开裂和回弹产生。结论 该方法主要针对热弯曲成形工艺,解决了金属间化合物难变形及传统脉冲电流辅助热成形难以在变形过程中持续通电的问题,改善了金属间化合物成形时产生的开裂和回弹。     

LaFe_(11.4)Si_(1.6)B_y系列化合物的磁性和磁熵变

LaFe11.4Si1.6By(y=0、0.1、0.2、0.3、0.4和0.5)系列化合物,通过添加少量的B后,可以明显的缩短退火时间。晶格常数随着B含量的增加先减小后增大。该系列化合物的热滞很小,B的添加对其热滞几乎没有影响。在外加磁场变化为0～1.5T时,等温磁熵变的最大值从19.1J/(kg.K)(y=0)逐渐下降到7.1J/(kg.K)(y=0.5)。该系列化合物在B含量较低时,处于居里温度(Tc)之上,存在比较明显的场致变磁转变特性。随着B含量增加到0.5时,场致变磁转变特性明显减弱。     

Structure, magnetic and thermal properties of Gd2MnTiO6

A new perovskite compound Gd₂MnTiO₆ was synthesized and its crystal structure, magnetic and thermal properties have been investigated. The XRD patterns were refined by the Rietveld method and the refined lattice parameters with the monoclinic space group P2₁/n (No. 14) were a=0.5398 (2), b=0.5704 (2), c=0.7767 (2) nm and β=89.68 (2)°. The antiferromagnetic behavior was observed below 16.0 K and λ-type heat capacity was measured near this temperature.     

Hydrothermal synthesis, structural characterization and thermal, spectroscopic and magnetic properties of the inorganic-organic hybrid phosphate, [(C2N2H9)VF(PO4)]

The [(C₂N₂H₉)VF(PO₄)] compound has been synthesized by hydrothermal techniques under autogeneous pressure at 170°C. The compound was characterized from X-ray powder diffraction data with the Rietveld method. Its crystal structure consists of sheets linked by the ethylenediammonium cations and constructed by chains of VO₃F₂N octahedra. The thermal study indicates that the compound is stable up to 290°C. In the IR spectrum the bands of both the ethylenediammonium and phosphate ions are observed. From the reflectance diffuse spectrum the Dq and Racah parameters have been calculated. The magnetic measurements indicate the presence of antiferromagnetic interactions.     

A new compound K2Cr8O16 with hollandite type structure

A new compound, K₂Cr₈O₁₆ with the hollandite-type structure was synthesized under high temperature-pressure conditions ranging from 1100° to 1250° C and from 55 to 65 kbars. Its crystal structure was classified as C³₂h - C2/m with the lattice parameters a=13.820, b=2.941, c=9.772 A and β=135°. Ferromagnetism was observed in this compound whose Curie temperature was 225 K and magnetic moment was approaximately 18 μ_B.     

Magnetic characterization of antiferromagnetic Ba2Fe6O11

The magnetic properties of the metastable compound Ba₂Fe₆O₁₁ present in the phase subsystem BaFe₂O₄ - BaFe₁₂O₁₉ have been analyzed by means of Mössbauer and magnetic measurements. The obtained data indicate that Ba₂Fe₆O₁₁ is a complex antiferromagnet with Neél temperature T_N = 488 K. The overall features of the Mössbauer spectra and the population of the observed iron sublattices suggest for Ba₂Fe₆O₁₁ a crystalline structure related to that of perovskite like compounds, which are often present in the chemical reactions that lead to the formation of hexaferrites. The extraneous phases present in the obtained samples, one of which turned out to be barium hexaferrite, have also been characterized.     

振动球磨制备的LaFe11.44Si1.56化合物的结构和磁性

利用振动球磨工艺制备了LaFe11.44Si1.56化合物,结果表明,在1100℃仅需要热处理30min,该化合物就能形成NaZn13型立方晶体结构;与电弧熔炼工艺制备的试样相比较,振动球磨工艺制备的试样的居里温度提高了15K,但最大磁熵变有所减小。因此,利用振动球磨工艺合成La(Fe,Si)13化合物有进一步研究的价值。     

New type of incommensurate magnetic ordering in Mn3TeO6

The complex metal oxide Mn₃TeO₆ exhibits a corundum related structure and has been prepared both in forms of single crystals by chemical transport reactions and of polycrystalline powders by a solid state reaction route. The crystal structure and magnetic properties have been investigated using a combination of X-ray and neutron powder diffraction, electron microscopy, calorimetric and magnetic measurements. At room temperature this compound adopts a trigonal structure, space group with a = 8.8679(1) Å, c = 10.6727(2) Å. A long-range magnetically ordered state is identified below 23 K. An unexpected feature of this magnetic structure is several types of Mn-chains. Under the action of the incommensurate magnetic propagation vector k = [0, 0, 0.4302(1)] the unique Mn site is split into two magnetically different orbits. One orbit forms a perfect helix with the spiral axis along the c-axis while the other orbit has a sine wave character along the c-axis.     

Co0.525Fe0.475MnP化合物的室温磁热效应和磁电阻效应

采用多步骤固态烧结方法合成了具有单一Co₂P相的Co_0.525Fe_0.475MnP化合物,其反铁磁有序温度在室温附近。在升温过程中,这种化合物经历两个连续的磁转变：在285 K发生反铁磁到铁磁的一级相变,在375 K发生由铁磁到顺磁的二级相变。在0~5 T的外磁场中,两个相变点温度对应的最大磁熵变分别为1.1 J/(kg·K)(303 K)和-2.0 J/(kg·K)(383 K)。外磁场为零时,随着温度的降低电阻率曲线在铁磁到反铁磁转变温度附近出现极小值,是铁磁有序与反铁磁有序的竞争所致。在35 K再次出现的电阻率极小值,可归因于由Fe替代Co引起的自旋无序所导致的金属-绝缘体转变。在5 T磁场中磁电阻率的最大值对应温度为200 K时的-2.5%,在反铁磁温度以上磁电阻率迅速减小。这表明,这种化合物的磁电阻效应源于外磁场对反铁磁有序的影响。     

Structural and magnetic properties of LaFe0.5Cr0.5O3 studied by neutron diffraction, electron diffraction and magnetometry

The structural and magnetic properties of the perovskite type compound LaFe_0.5Cr_0.5O₃ have been studied by temperature dependent neutron powder diffraction and magnetization measurements. Rietveld refinement of the neutron diffraction data shows that the compound crystallizes in an orthorhombic perovskite structure with a random positioning of the Fe and Cr cations at the B sublattice. The magnetic structure at 10 K is a collinear antiferromagnetic one with the magnetic moment per site being equal to 2.79(4) μ_B. Magnetisation measurements confirm the overall antiferromagnetic behaviour. Moreover, it indicates a weak uncompensated magnetic moment close to the transition temperature T_N ≈ 265 K. This moment can be described by a magnetic cluster state, which remains up to 550 K. Electron diffraction patterns along with high-resolution transmission electron microscopy images reveal that the crystallites are composed by domains of different orientation, which share the same cubic perovskite sub-cell reflections.     

Crystal structure, magnetic and thermal properties of LaFeTeO6

LaFeTeO₆ was prepared by solid state reaction of La₂O₃, Fe₂O₃ and TeO₂ in 1:1:2 molar ratios and characterized by powder X-ray diffraction, thermogravimetry and magnetometry. The detailed crystal structure analysis was carried out by Rietveld refinement. LaFeTeO₆ crystallizes in a trigonal lattice with unit cell parameters: a = 5.2049(1) Å and c = 10.3457(2) Å, V = 242.73(2) Å³. The crystal structure is built from sheets of the edge shared FeO₆ and TeO₆ octahedra stacked along the c-axis. These sheets are connected together by La³⁺ ions. Thermogravimetric analysis of the compound showed it to be thermally stable up to 1323 K and continuous loss of TeO₂ was observed above 1323 K leading to the formation of LaFeO₃. High temperature XRD studies revealed a normal expansion behavior of the compound. Temperature and field dependent magnetization of LaFeTeO₆ showed paramagnetic behavior in the temperature range of 3-300 K. The effective magnetic moment per Fe³⁺ ion (5.14 μB) indicates the high spin d⁵ state of Fe³⁺ ion.