以钼酸钠、硝酸铁、磷酸和三亚乙基四胺为原料, 采用水热合成法成功制备了一种还原型磷钼酸盐与FeⅡ构筑的超分子化合物, 其化学式为［C8H24N4］1.5［C6H22N4］1.5{Fe［Mo6O12(OH)3(PO4)3(HPO4)］2}·5H2O (1), 并通过单晶X射线衍射、粉末X射线衍射(PXRD)和红外光谱(FT-IR)对其结构进行了表征。结果表明, 该化合物是由{Fe［P4MoV6O31］2}22- (记为{Fe(P4Mo6)2})、质子化的三亚乙基四胺和质子化的N, N′-二(氨乙基)-哌嗪通过氢键相互作用连接形成的三维超分子结构。电催化性能的研究表明, 化合物1对铬离子(CrⅥ)、铁离子(FeⅢ)、溴酸钾(KBrO3)和抗坏血酸(AA)具有良好的电化学传感性能和低检测限(LOD)。

本文在水热条件下成功合成了一例Keggin型多酸基超分子化合物1,其分子式为H3［(3-PA)4(PW12O40)］(3-PA=3-(3-吡啶)丙烯酸)，并通过单晶X射线衍射、元素分析(EA)、红外(IR)光谱、X射线粉末衍射(PXRD)、热重(TG)和固体紫外-可见(UV-Vis)漫反射对化合物1的结构进行了表征。化合物1属于三斜晶系，P-1空间群，a=1.200 33(3) nm，b=1.216 42(3) nm，c=1.424 66(4) nm，α=75.030(1)°，β=73.452(1)°，γ=69.372(1)°，V=1.837 00(8) nm3，Z=1，Mr=3 476.78，F(000)=1 538，μ=18.815 mm-1，Dc=3.143 mg·m-3，S=1.062，R1=0.046 2,wR2=0.138 7。化合物1的结构单元包含一个［PW12O40］3-多阴离子和四个3-PA配体，并通过［PW12O40］3-多阴离子和3-PA配体之间的氢键连接形成二维超分子层。化合物1在光催化还原Cr(Ⅵ)反应中展现出良好的光催化活性，并具有较好的结构稳定性和可循环利用性。

In this study, the double-layered Aurivillius phases CaBi₂Ta₂O₉ (CBT) and PbBi₂Ta₂O₉ (PBT) were prepared through a hydrothermal route with NaOH as a mineralizer. XRD analysis confirmed that the CBT and PBT compounds were successfully formed and adopted an orthorhombic crystal structure with an A2₁am symmetry. Le Bail refinements of XRD data indicated that the unit cell volume of CBT was smaller than PBT and is associated with the smaller ionic radius of Ca2+ compared to Pb2+. The surface morphology of both samples, as determined using SEM, demonstrated plate-like grains with anisotropic grain growth. It was found that the different ionic radii of A-site cations (Ca2+ and Pb2+) strongly affected the structural, optical and electrical properties of the Aurivillius phase. The occupation of smaller Ca2+ cations induced a higher structural distortion, which resulted in higher bandgap (Eg) energy and ferroelectric transition temperature (Tc) of CBT, compared to those of PBT.In this study, the double-layered Aurivillius phases CaBi₂Ta₂O₉ (CBT) and PbBi₂Ta₂O₉ (PBT) were prepared through a hydrothermal route with NaOH as a mineralizer. XRD analysis confirmed that the CBT and PBT compounds were successfully formed and adopted an orthorhombic crystal structure with an A2₁am symmetry. Le Bail refinements of XRD data indicated that the unit cell volume of CBT was smaller than PBT and is associated with the smaller ionic radius of Ca2+ compared to Pb2+. The surface morphology of both samples, as determined using SEM, demonstrated plate-like grains with anisotropic grain growth. It was found that the different ionic radii of A-site cations (Ca2+ and Pb2+) strongly affected the structural, optical and electrical properties of the Aurivillius phase. The occupation of smaller Ca2+ cations induced a higher structural distortion, which resulted in higher bandgap (Eg) energy and ferroelectric transition temperature (Tc) of CBT, compared to those of PBT.

Efficiency of the piezoelectric chemisensors may be considerably enhanced by use of zinc oxide nanorods as sensing elements. ZnO nanorod arrays being good piezoelectric materials possess large surface area, which provides extra benefits for chemisorption and photodetection. Highly oriented nanorod arrays are typically prepared onto highly crystalline substrates, whereas the nanorods growth onto metal contacts meets significant technological difficulties. In this paper, we report on carbothermal, electrochemical, and hydrothermal techniques of ZnO nanorod arrays synthesis on metal contacts. The optical and structural properties of the obtained nanorods were studied using scanning electron microscopy, X-ray diffraction (XRD), Raman spectroscopy, and luminescence spectroscopy. A reliable technique was developed for obtaining ohmic contact with the grown nanorods. I–U curves of prepared contact were studied. Carbothermal synthesis made it possible to obtain the most crystallinely perfect, homogeneous, and dense arrays of nanorods and control the concentration of point defects by changing the synthesis parameters over a wide range. The electrochemical synthesis demonstrated excellent results for synthesis of ZnO nanorods on the surface of resonator electrodes.Efficiency of the piezoelectric chemisensors may be considerably enhanced by use of zinc oxide nanorods as sensing elements. ZnO nanorod arrays being good piezoelectric materials possess large surface area, which provides extra benefits for chemisorption and photodetection. Highly oriented nanorod arrays are typically prepared onto highly crystalline substrates, whereas the nanorods growth onto metal contacts meets significant technological difficulties. In this paper, we report on carbothermal, electrochemical, and hydrothermal techniques of ZnO nanorod arrays synthesis on metal contacts. The optical and structural properties of the obtained nanorods were studied using scanning electron microscopy, X-ray diffraction (XRD), Raman spectroscopy, and luminescence spectroscopy. A reliable technique was developed for obtaining ohmic contact with the grown nanorods. I–U curves of prepared contact were studied. Carbothermal synthesis made it possible to obtain the most crystallinely perfect, homogeneous, and dense arrays of nanorods and control the concentration of point defects by changing the synthesis parameters over a wide range. The electrochemical synthesis demonstrated excellent results for synthesis of ZnO nanorods on the surface of resonator electrodes.

无水碳酸镁晶体作为一种新型无机功能材料引起了研究者们的广泛关注。以氯化镁为原料, 碳酸钠为沉淀剂, 合成了无水碳酸镁晶体, 再以甘氨酸、组氨酸、丙氨酸及L-天门冬氨酸四种不同种类氨基酸作为添加剂, 调控其结晶的粒度及形貌。采用X射线衍射仪、扫描电子显微镜、激光粒度分析仪对合成产物进行表征, 分析不同种类氨基酸对合成的无水碳酸镁晶体物相结构和形貌的影响。结果表明: 在组氨酸调控下合成的无水碳酸镁结晶纯度高, 生成的产物中n(Mg2+)∶n(CO2-3)为1∶0.94; L-天门冬氨酸调控合成的晶体纯度次之; 甘氨酸和丙氨酸调控合成的晶体中掺杂大量碱式碳酸镁晶体。在组氨酸、L-天门冬氨酸、甘氨酸及丙氨酸四种氨基酸调控作用下, 晶体结晶形貌依次呈凸面球三角形状、近球状、球状及不规则状, 且无水碳酸镁晶体粒径分布均呈先上升后振荡下降最后小粒径拖尾的趋势。以上研究结果为无水碳酸镁晶体的仿生合成提供了参考。

本文在水热条件下合成了一例同多钼酸阴离子［δ-Mo8O26］4-基配合物［Co(bipbc)(δ-Mo8O26)0.5(H2O)3］ (bipbc=4，4-双［(4-羧基吡啶)甲基］联苯)，其为一维链状结构，包含环型双核钴配合物［Co2(bipbc)2］4+和［δ-Mo8O26］4-簇。该配合物结晶于单斜晶系，P21/n空间群，a=1.147 9(8) nm，b=1.440 9(11) nm，c=2.082 9(16) nm，β=93.469(2)°，V=3.438 8(4) nm3，Z=4，Mr=1 129.18，F(000)=2 204，μ=1.979 mm-1，Dc=2.181 mg·m-3，S=1.019，R1=0.056 2，wR2=0.137 7。光催化性质研究表明，在可见光、近红外光和全光谱的光照条件下，标题配合物对龙胆紫(GV)和亚甲基蓝(MB)的降解，表现出一定的光催化活性。

以脱硫石膏为原料通过水热合成法制备硫酸钙晶须, 借助X射线衍射仪、扫描电子显微镜、能谱仪、热重分析仪等测试手段进行分析, 研究了酸化预处理、料浆浓度以及反应温度对制备硫酸钙晶须的影响。结果表明: 酸化预处理可以有效去除原料中的CaCO3杂质; 随着料浆浓度和反应温度的增加, 晶须长径比均呈现先增大后减小的趋势; 当料浆浓度为3%(质量分数), pH值为6.5, 反应温度为120 ℃, 反应时间为2 h时, 取得的硫酸钙晶须最佳平均长度为161.2 μm, 最佳平均长径比为46.06。

采用水热合成法制备合金半导体材料Mo_1-XW_XS₂(X为浓度),并应用扫描式电子显微镜(SEM)、X射线衍射(XRD)和拉曼光谱仪(Raman)对其形貌和晶体结构进行表征。实验结果表明,由SEM形貌测试发现,随着掺杂浓度的增加,Mo_1-XW_XS₂片状合金材料表面逐渐粗糙;由XRD晶体结构表征发现,随着掺杂浓度的增加,Mo_1-XW_XS₂的晶格常数逐渐增大;在合金材料的拉曼频移中,随着掺杂浓度的增加,Mo_1-XW_XS₂中A_1g振动模发生蓝移,而 E2g1振动模发生红移。通过晶格结构和拉曼频移的检测和分析,证实水热合成法可制备不同浓度的Mo_1-XW_XS₂合金半导体材料。本方法可进一步拓展为二硫族化物合金半导体材料的批量制备方法,为合金半导体器件的制作和设计提供依据。