矿化剂浓度和反应时间对微波水热合成高纯BiFeO3粉体的影响

以Fe(NO3)3·9H2O和Bi(NO3)3·5H2O为反应原料,KOH为矿化剂,采用微波水热法制备高纯的单相BiFeO3粉体。研究了KOH浓度和微波水热反应时间对BiFeO3粉体纯度和相变的影响。研究表明,当KOH浓度高于6 mol/L时能合成出纯相BiFeO3粉体,随着水热矿化剂浓度的提高粉体形貌逐渐由准立方演变为截角立方,最后趋于类八面体结构的团聚体。当延长微波水热反应时间,BiFeO3粉体逐渐由三方相结构(R3m)向六方相结构(R3c)转变。当KOH浓度为10 mol/L,Bi3+/Fe3+摩尔比为1,微波水热时间为30 min,反应温度在200℃就可制备出高纯BiFeO3粉体,其饱和磁化强度约为0.075 emu/g。     

Bi3.25La0.75Ti3O12纳米片的水热合成及表征

以硝酸铋、硫酸钛和硝酸镧为原料,氢氧化钠为矿化剂,采用水热法制备了镧掺杂的钛酸铋片状纳米材料,研究了水热温度和水热时间对其结构的影响.采用XRD和SEM对产品的物相和结构进行了表征.结果表明:以硫酸钛作为无机钛源,在较低的水热温度(200 ℃)、水热时间为6 h时可以制备出花状的Bi3.25La0.75Ti3O12纳米片.     

水热合成Cu-Bi2WO6及其光催化性能研究

以Bi(NO3)3·5H2O和Na2WO4·2H2O为原料,NaOH为矿化剂,CuCl2和CuSO4为铜源水热法离子掺杂合成Bi2WO6粉体,并使用XRD、SEM、UV-VIS、XPS对其进行表征,分析了不同铜源离子掺杂Bi2WO6以及掺杂量对所制备样品光催化性能的影响.结果表明,以CuCl2为铜源离子掺杂Bi2WO6的样品粒径减小,吸收边红移.掺杂后的铜以中Cu2和Cu+两种电子形式存在.光催化测试结果表明,以CuCl2为铜源且掺入量为1.5mol;时所制备的Bi2WO6样品的光催化活性最高.     

化学沉淀法制备BiVO4及其表征

以Bi(NO3)3·5H2O和NH4VO3为原料,利用化学沉淀法制备了BiVO4,并系统地研究了不同反应条件如:反应物初始浓度、溶液pH值、反应温度、反应时间等对粒径的影响.采用Malvem粒度分布仪、扫描电子显微镜和X射线衍射仪等对产品进行了表征,并得出结论:化学沉淀法制备的钒酸铋,所得粒子粒度较小,均匀性好.     

氯氧化铋晶体的制备及其表征研究

采用铋盐转化水解法制备了四方相氯氧化铋晶体,研究反应温度、水解反应用水量以及反应液滴加顺序对产物粒径、产率及表面形貌的影响.结果表明,最佳反应条件为Bi(NO3)3·5H2O与HCl摩尔比为1∶5,反应温度为25～30℃,反应液滴加顺序为A→B,用水量为35 mL.该条件下制备出片状氯氧化铋晶体颗粒粒径0.5～2 μm,产物分散性良好.利用马尔文激光粒径分析仪、X射线衍射仪(XRD)、热场发射扫描电子显微镜(SEM)对氯氧化铋的粒度分布、晶面结构和微观形貌分析可知,所制备的氯氧化铋粒径分布符合正态分布曲线,且纯度高无任何杂质,反应液滴加顺序对产物形貌影响较大.     

共沉淀法制备BiFeO_3粉体

以Bi(NO_3)_3·5H_2O和Fe(NO_3)_3·9H_2O为原料,冰醋酸做溶剂,柠檬酸为络合剂,采用共沉淀法制备前驱物,对前驱物沉淀进行退火处理,制备出BiFeO_3纳米粉体.研究了煅烧温度和冰醋酸的加入量对BiFeO_3纳米粉体的晶粒尺寸及形貌的影响.采用X射线衍射仪(XRD)、场发射扫描电子显微镜(FE-SEM)对所制备的BiFeO_3纳米粉体进行表征,用EDS确定了样品的表面成分组成.结果表明:退火温度为450 ℃时出现BiFeO_3衍射峰,但存在杂相;退火温度为600 ℃时制备出了BiFeO_3纯相粉体,粉体为立方体结构.冰醋酸加入量由1 mL增大到1.8 mL时,粉体的晶粒尺寸由14.21 nm减小到11.65 nm.通过EDS能谱分析得出BiFeO_3粉体由Bi,Fe和O 三种元素组成.     

葡萄糖的加入量对C/Bi2WO6微晶的结构及可见光催化性能的影响

以葡萄糖(C6H12O6),分析纯硝酸铋(Bi(NO3)3·5H2O)和钨酸钠(Na2 WO4·2H2O)为原料,在简单的微波水热-煅烧条件下成功制备了形貌可控的交叉薄片状C/Bi2 WO6微晶.研究了反应体系中前驱物的不同摩尔比对产物的结构形貌以及光催化性能的影响.采用X-射线衍射仪(XRD)、EDS能谱分析、扫描电子显微镜(SEM),Perkin Elmer Larnbda 950型紫外可见漫反射光谱仪和康塔公司NOVA 2200e型表面空隙度分析仪分别对产物的结构、形貌,光学性能以及氮吸附-脱附等温线进行表征.结果表明:当前驱物葡萄糖,硝酸铋和钨酸钠的摩尔比为1∶10∶5时,合成了形貌可控且具有较好可见光催化性能的C/Bi2WO6微晶,其禁带宽度为3.055 eV,在可见光照射240 min后对罗丹明B的降解效率可达到94.8;.     

水热法制备BiFeO_3粉体的相变研究

本文以Fe(NO_3)_3·9H_2O 和Bi(NO_3)_3·5H_2O为反应原料,以KOH为矿化剂, 利用水热方法在矿化剂浓度4.5 mol/L至12.0 mol/L区域内制备出钙钛矿结构的BiFeO_3粉体材料.经过XRD慢扫(扫描速率为0.008°/s)及peakfit软件模拟分析得知,在KOH浓度由4.5～12.0 mol/L转变的过程中,产物的物相由三方相BiFeO_3向六方相BiFeO_3的转变.同时BiFeO_3铁电性能研究也证实了以上相变的存在.     

Bi2O3/g-C3N4/TiO2三元复合物的制备及其可见光催化活性研究

以工业纳米TiO2,三聚氰胺(C3H6 N6)和硝酸铋(Bi(NO3)3·5H2O)为原料,通过高温煅烧制备Bi2O3/g-C3 N4/TiO2三元复合物,采用XRD、XPS、FT-IR、UV-vis、PL光谱等对其结构进行了表征.结果表明g-C3 N4和Bi2O3分散覆盖在TiO2表面,形成具有异质结结构的Bi2O3/g-C3N4/TiO2三元复合物,其带隙降低,对可见光的吸收增强,电子和空穴通过在Bi2O3、g-C3N4和TiO2三者界面间的转移有效延长了光生载流子的寿命,从而提高光催化效率.以亚甲基蓝为目标污染物评价其光催化活性.结果表明,当TiO2与C3H6N6质量比为1∶2.5,Bi(NO3)3·5H2O含量为0.35;,煅烧温度为520℃,煅烧时间为5h时制得的Bi2O3/g-C3 N4/TiO2三元复合物(即0.35Bi/C/T)活性最高,LED灯(12 W)光照180 min后对10mg/L亚甲基蓝溶液降解率达98.1;.     

钨酸锌微纳米材料的水热合成及发光性能研究

以Zn(NO3)2·6H2O和Na2WO4·2H2O为原料,草酸为沉淀剂,采用水热法在180℃反应4h制备了ZnWO4粉体,并考察了前驱体溶液pH值对ZnWO4发光性能的影响.通过X射线衍射(XRD),场发射扫描电子显微镜(SEM)和荧光光谱(PL)等测试手段对样品的物相、微观形貌和发光性能进行表征.结果表明:pH值为7～9时适宜合成ZnWO4粉体,pH =7、8时,得到的是星状结构ZnWO4粉体;pH =9时分别得到的是由长度为500 nm,直径为100 nm的纳米棒交叉组装而成的镂空结构ZnWO4粉体.相比之下,由纳米棒交叉组装而成的镂空片的发光性能最佳.     

溶胶-凝胶法制备Na0.5Bi0.5TiO3-K0.5Bi0.5TiO3体系无铅压电陶瓷的研究

采用溶胶-凝胶法制备(1-x)Na0.5Bi0.5 TiO3-xK0.5Bi0.5TiO3体系无铅压电陶瓷.XRD分析表明,用溶胶-凝胶法可以在650℃下合成具有钙钛矿结构的(1-x)Na0.5Bi0.5TiO3-xK0.5Bi0.5TiO3粉体,且在x=0.18～0.30之间存在三方-四方准同型相界(MPB).陶瓷的压电性能参数表明,该体系在MPB组成范围内具有最佳的压电性能:x=0.30时,压电常数d33达到最大值(d33=150 Pc·N-1),平面机电耦合系数kp与介电常数εH33T/ε0均在x=0.26时达到最大值,分别为36.7;和1107.     

Carrier Scattering Mechanisms in GaS0.5Se0.5 Layered Crystals

Systematic dark electrical resistivity and Hall mobility measurements have been carried out in the temperature range 150‐400 K on n‐type GaS_0.5Se_0.5 layered crystals. The analysis of temperature dependent electrical resistivity and carrier concentration reveals the extrinsic type of conduction with a donor impurity level located at 0.44 eV, donor and acceptor concentrations of 3.4 ×10¹⁷ and 4.1×10¹⁶ cm^‐3, respectively, and an electron effective mass of 0.41 m₀. The Hall mobility is limited by the electron‐phonon short‐range interactions scattering at high temperatures combined with the ionized impurity scattering at low temperatures. The electron‐phonon short‐range interactions scattering mobility analysis reveals an electron‐phonon coupling constant of 0.25 and conduction band deformation potential of 5.57 eV/Å.     

Direct preparation of K0.5Na0.5NbO3 powders

K_0.5Na_0.5NbO₃ powders have been directly synthesized by an alternative solid–state method. Stoichimometric mixture of ammonium niobium oxalate and C₄H₄O₆KNa·4H₂O were calcined in temperature range from 500 to 800 °C for 3 h. The precursor and calcination products were characterized with respect to stoichiometry, purity, crystalline structure, particle size and powder morphology using X–ray diffraction (XRD), X‐ray fluorescence (XRF) spectrometer, scanning electron microscope (SEM), Fourier transform infrared (FTIR) spectra, thermogravimetric (TG) analysis, differential scanning calorimetry (DSC) and UV–Vis diffuse reflectance (UV–Vis) spectroscopy. XRD and XRF results reveal that stoichiometric K_0.5Na_0.5NbO₃ powders could be synthesized by the method. The particle size is about 68 nm for the precursor calcined at 500 °C according to XRD data, which is in good agreement with SEM data. The average band gap energy is estimated to be 3.18 eV by UV–vis diffuse reflectance spectra. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structural analysis of amorphous Ge0.5Te0.5 by neutron diffraction

Neutron diffraction measurements have been made on a sputtered sample of amorphous Ge_0.5Te_0.5. Analysis of the radial distribution function derived from Fourier inversion of the measured structure factor gives a nearest neighbor coordination number n = 2.49. This result, compared with coordination models proposed for this composition, favors the chemically ordered 3t2-3 model (where each Ge and Te atom is threefold coordinated by the other one) analogous to a-As with n = 2.78 over the 4-2 models with n > 3.20. More detailed analysis including second neighbor atoms confirms the ordered threefold a-As model.     

Bi(Zn0.5Ti0.5)O3对Bi0.5Na0.5TiO3基陶瓷相结构及弛豫性的影响

采用固相反应合成法制备了(1-x)(0.96Bi0.5Na0.5TiO3-0.04BaTiO3)-xBi(Zn0.5 Ti0.5)O3陶瓷(x≤0.10).通过X射线衍射,介电温度谱等对该体系陶瓷的相结构及弛豫特性进行了研究.结果发现,该陶瓷在Bi(Zn0.5Ti05)O3加入量低于0.05时呈现纯钙钛矿结构.此外,随着Bi(Zn0.5Ti0.5)O3加入量的增加,其相结构由三方-四方共存向赝立方结构转变;同时,陶瓷的弥散因子上升,偶极子取向冻结活化能下降,表明BZT的加入明显地增加了0.96Bi0.5Na0.5TiO3-0.04 BaTiO3陶瓷的弛豫性.     

(Na0.5Bi0.5)TiO3-(K0.5Bi0.5)TiO3无铅铁电单晶的生长、结构与介电特性

采用高温自助熔剂法制备了(Na0.5Bi0.5) TiO3-(K0.5Bi0.5) TiO3(简称:NBT-KBT)无铅铁电单晶,晶体尺寸为5mm×6 mm×1 mm.利用X射线衍射(XRD)手段研究了NBT-KBT单晶的相结构,结果表明晶体样品为钙钛矿四方相结构.Raman散射结果也表明了NBT-KBT单晶的拉曼振动模式具有四方相结构特征.利用扫描电镜(SEM)和透射电镜(TEM)研究了单晶的表面形貌和微结构特征.另外,单晶介电常数随温度以及频率的变化关系显示单晶具有弛豫铁电体特性.     

Neutron and X-ray diffraction study of superstructure and localized magnetic moments in Cu0.5Fe0.5Cr2S4 and Cu0.5In0.5Cr2S4 compounds

The superstructure parameters for the Cu_0.5Fe_0.5Cr₂S₄ and Cu_0.5In_0.5Cr₂S₄ compounds have been determined by neutron and X-ray diffraction. The localized magnetic moments in different sublattices measured for Cu_0.5Fe_0.5Cr₂S₄ are equal to 3.06 ± 0.17 μB for Fe³⁺ ions in the A-site and 2.76 ± 0.22 μB for Cr³⁺ ions in the B-site (Cu⁺ possess no magnetic moment), which are much less than the magnetic moments for the ions in the purely ionic state.     

Structural study of the semimagnetic semiconductor Zn0.5Mn0.5In2Te4

The semimagnetic semiconductor alloy Zn_0.5Mn_0.5In₂Te₄ was refined from an X‐ray powder diffraction pattern using the Rietveld method. This compound crystallizes in the space group I42m (Nº 121), Z = 2, with unit cell parameters a = 6.1738(1) Å, c = 12.3572(4) Å, V = 471.00(2) Å3, c / a = 2.00. This material crystallizes in a stannite‐type structure. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

织构化K0.5Na0.5NbO3无铅压电陶瓷的性能研究

以分析纯Na2CO3、Bi2O3和Nb2O5为原料,以NaCl为熔盐,采用二次熔盐法和拓扑化学反应法合成各向异性片状NaNbO3粉体.以该片状NaNbO3粉体为模板品粒,以固相法合成的NaNbO3和KNbO3粉体为基料,采用流延工艺制备出较高取向度的织构化K0.5Na0.5NbO3(KNN)无铅压电陶瓷,系统研究了模板含量、烧结温度和保温时间等工艺参数对织构化KNN陶瓷显微结构和压电性能的影响规律.研究结果表明:随着模板含量的增加,陶瓷的取向度逐渐增加,当模板含量为15 wt;时,陶瓷的取向度可达0.69,当模板含量为10 wt;,1100 ℃下保温5 h烧结,可以获得具有一定织构度(f=0.58)的KNN陶瓷,并表现出优异的压电性能,d33=128 pC/ N.     

Crystal structure and magnetic properties of the LaCo0.5Fe0.5O3 perovskite

The magnetic and crystal structures of the LaCo_0.5Fe_0.5O₃ perovskite are investigated. It is established that the unit cell of this compound at room temperature is characterized by rhombohedral distortions. As the temperature decreases, the compound undergoes a structural phase transition from the rhombohedral phase to the orthorhombic phase in the temperature range 200–300 K. The LaCo_0.5Fe_0.5O₃ perovskite has an antiferromagnetic structure with the G _z spatial orientation of the antiferromagnetic vector. The magnetic properties of the LaCo_0.5Fe_0.5O₃ perovskite are interpreted within a model according to which the ground state of Co³⁺ ions is a low-spin state and the existence of the weak ferromagnetic component is associated with the exchange interactions between the Fe³⁺ ions.