共沉淀法制备Sr(Fe0.5Nb0.5)O3纳米粉体及其介电性能研究

采用共沉淀法制备Sr(Fe0.5Nb0.5) O3纳米粉体,两步烧结工艺制备Sr(Fe0.5 Nb0.5) O3陶瓷.用X射线衍射仪(XRD)分析烧结温度、煅烧时间、体系温度、pH值和初始溶液浓度对前驱体粉体物相的影响,用扫描电子显微镜(SEM)分析Sr(Fe0.5 Nb0.5) O3纳米粉体和陶瓷的微观形貌,用阻抗分析仪研究陶瓷的介电性能.结果表明:当体系温度为25℃,pH值为9,初始溶液浓度为0.25 mol/L,在950℃煅烧2h后可获得颗粒分布均匀(～ 50 nm)的Sr(Fe0.5Nb05)O3纳米粉体,用该纳米粉体获得的Sr(Fe0.5Nb0.5)O3陶瓷有优异的频率和温度稳定性及高的介电常数(ε'＞2×103)和较低的介电损耗(1 kHz,tanδ=0.086).高的介电常数与陶瓷晶粒和晶界间阻挡层的形成有关,低的介电损耗来源于陶瓷致密的微观结构.     

Al2O3改性Ba(Fe0.5Nb0.5)O3复合陶瓷制备与性能研究

采用草酸盐共沉淀法成功合成了Ba(Fe0.5Nb0.5)O3 (BFN)纳米粉体,并采用sol-gel法获得Al2O3改性的BFN复合粉体,于1150℃两步烧结3h获得复合陶瓷,研究了Al2O3添加对BFN陶瓷微观形貌和介电性能的影响.结果表明:BFN · xAl2O3(x=4wt;,6wt;,8wt;)复合粉体颗粒分布均匀,粒径约为50 nm.Al2O3的加入可明显降低陶瓷的烧结温度.Al2 O3添加量为4wt;的复合陶瓷有高的介电常数,较小的介电损耗和良好的温度稳定性.BFN·xAl2O3复合陶瓷中存在的介电弛豫行为符合Arrhenius定律,是一个热激活过程,随着x的增加,复合陶瓷的激活能逐渐增大,这与无定形Al2O3增加了陶瓷的弛豫势垒,使界面极化减弱相关.     

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.     

钙钛矿型Ba0.5Sr0.5Co0.8Fe0.2O3-δ透氧膜材料的制备及其透氧性能的研究

通过甘氨酸硝酸盐法(GNP)合成了钙钛矿型Ba0.5Sr05Co0.8Fe0.2O3-δ(BSCF)复合氧化物粉体.经压制、烧结后,得到了BSCF烧结体试样,还通过硝酸溶液浸蚀处理对烧结体试样进行了表面浸蚀处理.采用X射线衍射仪(XRD)对煅烧后的粉体进行了相成分分析;采用扫描电子显微镜(SEM)及能谱仪(EDS)对烧结体和表面浸蚀后烧结体样品的微观组织和成分进行了表征;对烧结体的致密度、电导率进行了测试分析,并在自制的氧渗透装置上测定了BSCF钙钛矿膜的透氧量,分析了温度和不同氧分压差等对膜透氧性能的影响.实验结果表明,甘氨酸-硝酸盐法所制备的前驱体粉末在900℃煅烧3h后可获得具有单一钙钛矿结构的BSCF粉体,1100℃煅烧的BSCF烧结体的电导率在600℃时最大达到38.15 S·cm-1.其透氧量随着温度和氧分压差的升高而增大,且硝酸表面浸蚀处理后,BSCF膜片的透氧性能有明显提高,透氧速率提高1.6～4.5倍.850℃,20;O2-80;N2混合气体/He条件下,浸蚀后的透氧膜片的透氧量达到2.36 mL/cm2 · min,而未浸蚀透氧膜片的透氧量仅为1.36 mL/cm2·min.     

CuO对(Zn_(0.5)Mg_(0.5))Nb_2O_6陶瓷的烧结温度和微波介电性能的影响

本文研究了助烧剂CuO对(Zn0.5Mg0.5)Nb2O6陶瓷的烧结特性、微观结构、相结构及微波介电性能的影响。研究结果表明,助烧剂CuO可以将(Zn0.5Mg0.5)Nb2O6陶瓷的烧结温度降低到950℃。添加3 wt%CuO,在950℃烧结的(Zn0.5Mg0.5)Nb2O6陶瓷密度达到了理论密度的97%以上,介电常数为20,Q×f值为33556 GHz。     

TGG法制备织构化K0.5Na0.5NbO3无铅压电陶瓷的性能研究

以熔盐法制备的K4Nb6O17片状粉体为前驱体,通过质子取代法制备了片状Nb2O5粉体,并且以其为模板结合模板晶粒生长(TGG)技术制备出较高织构度的X0.5Na0.5NbO3 (KNN)织构化无铅压电陶瓷,研究了不同工艺参数(模板含量、烧结温度和保温时间)对KNN织构化陶瓷的显微结构、介电性能以及压电性能的影响规律.研究结果表明:当模板含量、烧成温度和保温时间分别为10wt;,1120℃和5h时,可以获得织构度f为0.78的KNN织构化无铅压电陶瓷,并具有优异的压电和介电性能:平行于流延方向压电常数d33=141 pC/N,介电常数ε3T/ε0=503和平面机电耦合系数kp=39.7;;垂直于流延方向d33=112 pC/N,εT33/ε0=454和kp=37.5;.     

微波辅助溶胶-凝胶自蔓燃法制备纳米Na0.5Bi0.5TiO3粉体的工艺研究

采用微波辅助溶胶-凝胶自蔓燃法制备了具有准同型相界组成的0.94Na0.5 Bi0.5TiO3-0.06BaTiO3(0.94NBT-0.06BT)粉体,采用X射线粉末衍射、红外光谱、热重-差热等分析手段对粉体进行了分析表征.通过对合成工艺中溶液的pH值、不同络合剂、微波功率等参数的优化,获得了合成单相钙钛矿结构0.94NBT-0.06BT元铅压电纳米粉体的最优工艺参数:使用柠檬酸作为络合剂、溶液pH值为4～6、微波功率为520 W,热处理温度为500℃,合成后的粉体大小均匀,粒度分布在10 ～ 20 nm之间.利用红外光谱和热分析探讨了蔓燃反应的合成机理.     

凝胶浇注法制备中温固体氧化物燃料电池Sm_(0.5)Sr_(0.5)Co_(1-x)Fe_xO_(3-δ)多孔阴极材料的研究

以碳酸盐和氧化物为原料,通过凝胶浇注法制得了Sm_(0.5)Sr_(0.5)Co_(1-x)Fe_xO_(3-δ)(SSCF, x=0～1.0)粉体,对不同温度煅烧所得粉体的相组成和微观形貌进行了测定.制备的Sm_(0.5)Sr_(0.5)Co_(1-x)Fe_xO_(3-δ)粉体模压成形后烧结得到SSCF烧结体.测定了烧结体的密度和孔隙率并对烧结体的微观结构进行了观测,用直流四端子法测定了烧结样品的电导率并对其热膨胀系数及电化学性能等进行了测定.结果表明:干凝胶在1000 ℃煅烧可以得到粒度均匀细小的SSCF粉体,其晶体结构随Fe含量发生变化;一定温度烧结的Sm_(0.5)Sr_(0.5)Co_(1-x)Fe_xO_(3-δ)材料具有多孔结构,随烧结温度的增加,烧结体的密度增大,孔隙率减小;Fe的掺杂降低了Sm_(0.5)Sr_(0.5)CoO_(3-δ)材料的热膨胀系数,Sm_(0.5)Sr_(0.5)Co_(0.2)Fe_(0.8)O_(3-δ)材料在800 ℃时的热膨胀系数为16.4×10~(-6) K~(-1);SSCF材料的电导率随Fe含量的增加而减小,但在500～800 ℃,其电导率均大于100 S·cm~(-1).此外,Sm_(0.5)Sr_(0.5)Co_(1-x)Fe_xO_(3-δ)材料均表现出良好的催化活性.     

模板晶粒定向生长技术制备(Na0.8K0.2)0.5Bi0.5TiO3无铅压电陶瓷的性能研究

以熔盐法和质子取代法制备的片状Nb2O5粉体为模板晶粒,固相法合成的(Na0.8K0.2)05Bi0.5TiO3 (NKBT)粉体为基料,分别采用固相压制成型(干法)和流延成型(湿法)工艺制备出具有较高取向度的织构化NKBT无铅压电陶瓷,研究了两种成型工艺对NKBT无铅压电陶瓷的显微结构、压电性能和介电性能的影响.结果表明:采用湿法工艺制备的织构陶瓷的各项性能优于干法工艺,采用湿法工艺在1150℃保温5h时,可以获得较高织构度(f=0.66)的NKBT无铅压电陶瓷,并具有优异的压电和介电性能:压电常数d33 =149 pC/N,介电常数ε3T3/ε0=912和平面机电耦合系数kp=29.4;.     

改进的碳铵沉淀法中氧化钇粉体尺寸及形貌的调控研究

以商业氧化钇(Y2 O3)为原材料,采用改进的碳酸盐沉淀工艺合成钇碳酸盐前驱体,经随后的焙烧工艺获得Y2O3产品.X衍射技术(XRD)和扫描电镜(SEM)表征表明:合成的碳酸盐前驱体Y2(CO3)3·2H2O具有类球形形貌、粒度分布均匀,经950℃焙烧2 h,前驱体受热分解为Y2 O3粉体,粉体完整保留了前驱体的形貌特征.同时,基于对NH4 HCO3/NH4+不同摩尔比条件下NH4 HCO3/NH4 NO3混合溶液中pH值变化的理论计算,在保持其他条件不变化条件下,通过改变NH4 HCO3/NH4 NO3混合溶液的加入量以获得不同的稀土碳酸盐沉淀终点pH值,当碳酸盐沉淀过程中pH值从6.0降低至4.7时,可实现超细至大颗粒不同尺寸氧化钇粉体的制备.同时,公斤级的扩大试验证实该工艺具有良好的可推广性.进一步提出NH4+在碳酸氢铵沉淀制备氧化钇工艺中的作用机理:(1)改变反应体系中阳离子和阴离子的组成;(2)显著影响前驱体的晶型;(3)显著影响产品颗粒尺寸大小.     

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)     

Gravitational Effects on Mixing and Growth Morphology of an In0.5Ga0.5 System

A mixing experiment of multicomponents melts was performed using a uniform temperature furnace in the Second International Microgravity Laboratories (IML-2) mission. Growth morphologies and Ga concentration profiles were analyzed for the samples with the compositional ratio of 0.5 In–0.5 Ga–1.0 Sb grown under microgravity and on earth. The sample with free surface grown under microgravity was nearly spherical in shape, except some parts with projections. Ga was dispersed homogeneously in the bulk because the mixing was enhanced by Marangoni convection due to the concentration gradient. On the other hand, the sample grown on earth was a double cylindrical shape with different diameters, and Ga concentration decreased from top to bottom, showing clearly the effect of gravity. Many needle crystals were formed in both space and earth samples due to rapid cooling. The average size of the needle crystals grown in space was larger than that of the earth sample.