纳米PbTiO_3温致相变的原位高温拉曼光谱研究(英文)

采用钛酸丁脂和醋酸铅和溶胶凝胶法制备了纳米PbTiO3粉体。利用扫描电镜观察了经不同温度烧结后常温下粉体形貌及晶粒尺寸,得到不同尺寸(5 0～1 0 0nm)的纳米粉体。同时观察了升温条件下的温致拉曼光谱,分析了不同温度热处理后粉体的相,高温原位拉曼光谱表明了烧绿石相是升温过程中四方相PbTiO3向立方相结构转变必须经过的过渡相。另外,对高温下挥发的粉体进行研究发现,煅烧PbTiO3粉体可以得到不同尺寸的烧绿石相结构粉体     

纳米粉体CeO_2∶Eu~(3+)的溶胶-凝胶绿色合成及其发光性质

采用溶胶-凝胶法,以硝酸铈为原料,加入适量淀粉为分散剂,并通过氨水来调节溶液p H值,合成稀土Eu~(3+)掺杂的CeO_2红色纳米粉体。通过X射线衍射仪、场发射扫描电子显微镜、荧光分光光度计等手段研究不同煅烧温度对粉体结构、形貌、发光及显色性能的影响。结果表明,所得样品为立方晶系的萤石结构,空间群为Fm3m,颗粒呈近似球形,粒径范围在10~60 nm之间。随着煅烧温度的升高,CeO2晶粒尺寸逐渐增大,荧光粉的红色发光也逐渐增强。经800℃烧结后,近紫外(370 nm)和蓝光区(468 nm)的光都能对粉体有效地激发,这有利于其在固态照明中的应用。在溶胶-凝胶制备过程中,采用淀粉作分散剂,具有工艺简单、绿色环保的优点,有利于纳米氧化铈粉体的大规模制备。     

纳米BaTiO3陶瓷的Raman光谱研究

高压能增加陶瓷烧结的致密驱动力和抑制陶瓷晶粒的长大。用高压辅助烧结的方法得到了晶粒尺寸约为60和30 nm的致密纳米BaTiO3陶瓷。BaTiO3陶瓷的晶体结构随温度的变化由变温Raman光谱来研究。在温度范围-190℃到200℃内,与粗晶的BaTiO3陶瓷相比,纳米BaTiO3陶瓷Raman散射结果表明,随着晶粒尺寸的减小,Raman峰的强度变弱,相变越来越弥散,出现了相变峰的消失;而且随着温度的升高,在纳米BaTiO3陶瓷甚至在30 nm BaTiO3陶瓷中都有与粗晶相同的从三方相到正交相到四方相到立方相的连续相变。变温Raman散射也表明,当晶粒大小减小到纳米尺寸时,纳米BaTiO3陶瓷表现出与粗晶不同的新颖性质。在一定的温度范围内,存在多种铁电相的共存。     

La1-xPrxCrO3纳米晶的结构和磁性质

我们用柠檬酸溶胶凝胶法成功制备了Pr掺杂La1-xPrxCrO3(x=0～0.6)纳米晶.在硝酸盐溶液中加入柠檬酸作为螯合剂,乙二醇为分散剂,得到干凝胶并在烧结温度为600 ℃时获得纯相钙钛矿结构纳米晶粉体,颗粒直径大约为40 nm且大小分布均匀.La0.5Pr0.5CrO3在场冷条件下的磁化强度以及在7K时的磁滞回线的测量结果表明,在260 K表现出顺磁到反铁磁转变,在200 K时磁化率达到最大值,随后磁化率随着温度的降低而急剧减小,在大约94 K的时候磁化率为0,随着温度的进一步降低,磁化率为负值.     

Tb1-xDyxFe2-y-Fe掺杂BaTiO3多层膜中的磁电耦合

用溶胶-凝胶法制备了Fe掺杂BaTiO3粉体,在1350℃下烧结成圆片状多晶样品,并与Tb1-xDyxFe2-y胶合成磁电(ME)双层膜或三层膜.实验分析表明Fe:BaTiO3依然是四方相钙钛矿结构,但是居里温度及相变潜热均略低于纯净BaTiO3.研究了Tb1-xDyxFe2-y-Fe∶BaTiO3双层膜和Tb1-xDyxFe2-y-Fe∶BaTiO3-Tb1-xDyxFe2-y三层膜的ME效应.在2.8×104 A/m的磁场下,两者的横向ME电压系数均达其峰值,分别为6.225和26.25 mV·(A·m-1)-1·cm-1.并且,用掺杂BaTiO3制备的双层膜和三层膜的横向ME电压系数均为相同条件下用纯净BaTiO3制备的双层膜和三层膜的横向ME电压系数的1.5倍.另外由于不含铅,锆等有害物质,符合环保要求,因此采用掺杂BaTiO3制备的磁电效应器件具有深入研究和应用价值.     

CeOx与ZnO纳米复合粉体的制备及其发光性能

通过溶胶-凝胶法制备CeOx／ZnO纳米复合粉体,并对其结构和光致发光特性进行了研究。发现500℃烧结出的复合粉体在502nm处的绿光发射同纯ZnO的相比有显著的增强;600℃烧结的样品在603nm出现新的发光峰。通过XRD和XPS分析认为荧光增强的主要原因同粉体中铈主要以Ce^3 形式存在有关,新的发光峰可能来源于ZnO／CeO2界面处形成的新的能级跃迁。     

EDTA络合溶胶-凝胶法制备Y2O2S:Eu3+,Mg2+,Ti4+红色长余辉材料

采用EDTA(乙二胺四乙酸)络合溶胶-凝胶法制备了Y2O2S:Eu3+,Mg2+,Ti4+粉体。采用X射线衍射仪、扫描电子显微镜和荧光分光光度计对不同温度合成的样品性能进行测试与表征。结果表明:当硫化温度低于1 000℃时,样品为Y2O3与Y2O2S的混合相;当温度在1 050～1 100℃时,样品为纯相的Y2O2S;当温度升高到1 150℃时,再次出现Y2O3的相。硫化温度在950～1 100℃时,产物的粒径为50～300 nm。用波长为330 nm的紫外光激发样品时,626 nm处的发射对应于Eu3+的5D0-7F2跃迁。硫化温度为1 100℃时,样品的余辉时间最佳,为95 min(≥1 mcd/m2)。相比于以乙酰丙酮为络合剂的溶胶-凝胶法,EDTA络合溶胶-凝胶法制备的样品的发光性能具有较大提高。     

纳米氧化锌的IR及其薄膜的UV光谱研究

采用溶胶-凝胶浸渍提拉法制备了纳米氧化锌薄膜。ZnO为六方晶系纤锌矿型,薄膜表面均匀致密,粒径尺寸约为10nm,400℃焙烧后的粉体在451cm-1处出现Zn-O伸缩振动,较体相材料向低波数移动了约29cm-1,膜中ZnO粒子的带边吸收位于363nm,其吸光度值与膜层数间的较好线性关系说明可以将氧化锌溶胶中的纳米粒子较好地转移到基片上。     

溶胶-凝胶法制备YAG∶Ce,Yb纳米荧光粉及其发光性质研究

使用溶胶-凝胶法在不同煅烧温度下制备了不同掺杂的YAG∶Ce,Yb荧光粉。使用扫描电镜、X射线衍射仪对其形貌、结构进行了表征;采用光致发光、荧光寿命等技术,对其发光性质进行了研究。结果表明:粉体粒径随煅烧温度上升而增大,在1 000℃下,得到平均尺寸~84 nm的纳米荧光粉。溶胶-凝胶法产物与高温固态法产物相比,Yb~(3+)离子发光的猝灭浓度由10%下降至5%。这可能是由于溶胶-凝胶反应产物体系中掺杂离子分布更加均匀所致。     

溶胶-凝胶法制备钕钡铜氧超导粉

采用溶胶-凝胶（Sol—Gel）法制备钕钡铜氧（NdBCO）超导原粉，并在不同的温度下进行烧结。用X射线衍射（XRD）分析表明烧结后的NdBCO超微粉在不同的温度下获得不同的相，其中800℃烧结得到的是Nd～123相，粒度计算结果表明粒径约为150nm左右。差热-热重（TGDTA）分析结果表明，在500℃柠檬酸分解，800℃时NdBCO超导原粉结晶，为超导靶材的制备奠定了良好的基础。     

Effect of titanium alkoxides on the properties of barium-strontium-calcium titanate powders obtained by a sol-gel method

This is a study of the effect of titanium alkoxides on the properties of barium-strontium-calcium titanate powders produced by a sol-gel method. Sols were synthesized using titanium tetraethoxide, titanium tetraisoproxide, and titanium tetrabutoxide. Xerogels of titanium oxide doped with barium, strontium, and calcium in a proportion of 60:30:10 were obtained by drying the sols at a temperature of 70°C. Thermogravimetric analysis, along with differential scanning calorimetry, IR spectroscopy, and x-ray phase analysis, were used to study the changes in the xerogel and the crystallite dimensions in the powder induced by thermal processing. The morphology and specific surface area of the powders were determined by scanning electron microscopy and low-temperature physical adsorption-desorption of nitrogen. These studies lead us to recommend sols based on Ti(OC₃H₇)₄ with a crystallite particle size in the powder of ∼63 to 40 nm for creating homogeneous ceramic materials from barium-strontium-calcium titanate.     

Dielectric losses in submicrometer barium titanate near the Curie temperature

Low-frequency dielectric losses (tanδ) in barium titanate ceramics with crystallite sizes of ~100 nm near the Curie temperature are studied. It is shown that the observed tanδ maximum is described by a low-frequency fluctuation mechanism of dielectric losses. An analysis of experimental data shows that the critical nucleus size in ultrafine material is smaller than the one in bulk barium titanate.     

Gyrotropic and piezoelectric coefficients and attenuation of elastic waves in BaTiO3

Using Landau theory of phase transition, expressions for gyrotropic coefficients and piezoelectric coefficients are obtained for barium titanate in the tetragonal phase. Both coefficients vanish at the ferroelectric phase transition temperature. The piezoelectric coefficients tallied with the literature values. The attenuation coefficients for elastic waves propagating along the principal directions in tetragonal, orthorhombic and rhombohedral phases are derived based on Landau theory. It is predicted that there will be slight amplification for both longitudinal and transverse modes in the rhombohedral phase at a temperature close to the rhombohedral phase transition temperature.     

Dielectric Properties of Calcium,Strontium, or Barium Titanate Sintered with 5 mol.% of Lithium and Calcium Fluorides

Calcium, strontium, and barium titanates were previously synthesized then mixed and wet-ground with 5 mol.% of lithium and calcium fluorides. These mixtures were pressed into pellets and air-fired. The ceramics were investigated by X-ray diffraction, scanning electron microscopy, and dielectric measurements. Each sample is a perovskite single phase. The oxyfluoride deriving from calcium titanate exhibits a phase transition around 283 K. For strontium titanate, no phase transition is detected. On the other hand, the ceramic related to barium titanate displays a ferroelectric phase transition around 300 K and a dielectric relaxation at about 10 MHz. These oxyfluorides could be of interest for capacitor manufacturing.     

Fabrication and optical reflection behavior of a two-dimensional barium titanate ceramic photonic crystal

We demonstrate a method for fabricating a two-dimensional hexagonal array of nanoscale barium titanate ceramic pillars. A precursor array was prepared by introducing a sol solution into an electron-beam resist mold with air holes and subsequently dry etching the unnecessary gel layer formed on the mold. A ceramic array, consisting of barium titanate ceramic pillars with a radius of 85 nm, a lattice constant of 450 nm, and a height of 500 nm, was fabricated by sintering the precursor array at 1073 K. The reflection spectra for the ceramic array in the visible range revealed the underlying photonic band gaps, which were in good agreement with results calculated using a plane-wave method. PACS 77.84.-s; 42.70.-a; 42.70.Qs     

Lattice dynamics,ferroelectricity and raman spectrum of BaTiQ3 in cubic phase

A dynamical model involving non linear anisotropic polarisability of oxygen is used to calculate the phonon dispersion curves and the Raman spectrum of barium titanate at 421 K near the paraelectric-ferroelectric phase transition. The temperature phase dependence of the dispersion curves is studied and the ferroelectric soft mode is described.     

Electron microscopy of barium strontium titanate nanostructures in the aluminum oxide matrix

Electron microscopy has revealed the mechanism of formation of barium strontium titanate nanostructures during crystallization in the bulk of pores of the aluminum matrix. The nanostructures have the form of nanotubes or nanocolumns 100–200 nm in diameter and a few microns long, which are formed by barium strontium titanate crystals 3–100 nm in size.     

Dielectric properties of barium titanate ceramics modified by SiO2 and by BaO-SiO2

The influence of SiO₂ on the dielectric properties of barium titanate ceramics was investigated. SiO₂ had been doped solely and together with BaO into barium titanate before calcination. X-ray diffraction showed that all the ceramics were of a pure perovskite phase after sintering at 1275 °C for 2 h. For SiO₂-doping, there was about 2.5 °C increase in Curie temperature per molar percentage of doping and the leakage current was obviously increased, especially at low voltages for relatively high doping levels. While for the co-doping of SiO₂ and BaO, there was little change in Curie temperature. The point defects formed through the dopings were proposed responsible for the effects. It was suggested that SiO₂ is important to barium titanate ceramics not only for sintering but also for modifying their properties.     

Structural phase transitions in nanosized ferroelectric barium strontium titanate films

The lattice parameters of epitaxial barium strontium titanate films with various thicknesses (from 6 to 960 nm) were measured as a function of temperature in the normal and tangential directions with respect to the film plane using x-ray diffraction. The films were grown through the layer-by-layer mechanism by rf cathode sputtering under elevated oxygen pressure. A critical film thickness (～ 50 nm) was found to exist, below and above which the films are subjected to compressive and tensile stresses, respectively. As the temperature varies from 780 to 100 K, the films undergo two diffuse structural phase transitions of the second order over the entire thickness range. The transitions in the films under tensile stresses are likely to be transformations from the paraelectric tetragonal to aa phase and then to r phase, whereas the transitions under compressive stresses are transformations from the tetragonal paraelectric to ferroelectric c phase and then, with further decreasing temperature, to r phase.     

铁电移相器优值研究

基于双周期性电容加载共面波导传输线的移相器结构,系统研究了温度变化对铁电薄膜移相器移相能力、传输损耗的影响.调整温度可以在一定的范围内实现对移相器性能指标的微调.给出了加载因子对移相能力的示意曲线图,并在实验上,借助氩离子刻蚀技术,改变加载因子的大小,使得移相器的优值从原来的13degree/dB提升到23degree/dB.