稀土掺杂Pb(Mg1/3Nb2/3)O3-PbTiO3压电陶瓷的烧结特性研究

在传统的固相反应制备工艺中,固相反应的烧结温度直接影响着陶瓷的物相结构、陶瓷致密度以及介电性能等.本文采用固相反应法制备x; Sm3掺杂PMN-PT压电陶瓷,通过控制不同的烧结温度,制备了一系列Sm-PMNPT陶瓷样品.利用X射线衍射仪、介电温谱以及准静态d33测量仪对陶瓷结构、介电性能、压电系数等性能进行表征.研究结果表明:烧结温度在1250℃,x=1.875mol;～2.5mol;,陶瓷样品的钙钛矿含量最大,压电系数最高可达1254 pC/N,kp=0.58,相对介电常数高达30000左右,密度达到8.48 g/cm3.     

烧结温度和升温速率对Pb(Sb1/3Mn2/3)0.05Zr0.47Ti0.48O3压电陶瓷性能的影响

采用传统固相法制备了Pb(Sb1/3 Mn2/3)0.05Zr0.47Ti0.48 O3 (PMS-PZT)压电陶瓷.利用XRD、SEM和EDS等研究PMS-PZT陶瓷体系在烧结过程中形成的过渡液相和形成过渡液相温度(1100℃)附近的升温速率对陶瓷结构、压电和介电性能的影响.结果表明:不同烧结温度下,所有样品均为单一的钙钛矿四方相,过渡液相不会对相的结构有影响,但是当烧结温度较低时,过渡液相在烧结后期以玻璃相在晶界附近富集,对陶瓷的压电和介电性能有很大影响.随着烧结温度和升温速率的升高,PMS-PZT晶粒尺寸增大,晶粒均匀性和规则性得以改善,晶化质量得到提高;d33测试和阻抗分析测试结果表明PMS-PZT样品在1100℃附近以7 ℃·min-1升温速率并在1250℃烧结时具有最好的压电和介电性能:d33 =313 C/N,kp=0.59,Qm=1481,εr=1437,tanδ=0.53;.     

Sr和Nb复合掺杂Bi4Ti3O12基高温压电陶瓷的研究

采用传统固相法制备了Bi4Ti3O12 +0-91wt;Nb2O5+xwt; SrCO3(BTNO-Sr,0.00≤x≤1.50)层状压电陶瓷,研究了Sr掺杂对BTNO系陶瓷微观结构与电性能的影响.结果表明所有样品均为单一的铋层状结构相陶瓷.适量引入Sr能使BTNO系陶瓷的晶粒尺寸细化与均一,表现出介电弥散性,并改善其压电、机电和铁电性能.当x=0.50时,样品性能最佳:相对密度p=98.8;,压电常数d33=22 pC/N,平面机电耦合系数kp=9.5;,机械品质因子Qm =4462,剩余极化强度Pr=13.01μC/cm2,居里温度Tc=620℃.此外,介电性能和热稳定性能研究显示材料x=0.50具有好的压电稳定性,适合于制备高温高频压电器件.     

MgO掺杂对PMMN四元系压电陶瓷结构与性能的影响

采用固相烧结法制备添加过量MgO的铌镁-铌锰-锆钛酸铅(PMMN)四元系压电陶瓷材料,研究了不同MgO掺杂量对材料结构及压电介电性能的影响.实验结果表明,适量MgO掺杂,不仅不改变PMMN压电陶瓷的钙钛矿相结构,且能提高合成粉体的晶化程度,降低陶瓷的烧结温度,改善材料的压电介电性能.当MsO掺杂量为0.25;质量分数,1130℃烧结的样品性能参数为:d33=310 pC/N,Qm=1008,kp=0.61,tan δ=0.34;,ε33T/ε0=1494,是一种中温烧结功率型压电陶瓷材料,适用于多层压电变压器,超声马达等器件.     

氧化铁掺杂对PMnS-PZN-PZT压电陶瓷性能的影响

通过对晶体结构与压电、介电性能测试,探讨了Fe_2O_3掺杂对PMnS-PZN-PZT陶瓷压电性能的影响.结果表明,PMnS-PZN-PZT陶瓷结构位于三方、四方相共存的MPB区间,Fe_2O_3掺杂导致晶体三方、四方相结构含量发生变化.当Fe_2O_3掺杂含量为0.45 wt;时,晶体结构位于准同型相区间偏四方相结构的位置,压电与介电性能达到最佳:tanδ=0.12;,d_(33)=356 pC · N~(-1),k_p=0.60,Q_m=745,在230 ℃以下的温度范围具有很好的频率温度稳定性.     

Pb0.92Sr0.08-xBax(Sb2/3Mn1/3)0.05Zr0.48Ti0.47O3的制备与性能研究

采用传统固相烧结法制备了Pb0.92Sr0.08-xBax(Sb2/3 Mn1/3)005Zr0.48Ti0.47O3(PSBSM-PZT)压电陶瓷样品.研究了不同Sr2+、Ba2+掺杂含量对样品的相结构、微观形貌、压电和介电性能的影响.结果显示:所有样品均为钙钛矿结构.而当x=0.02～0.06时,陶瓷样品组分位于准同型相界区(MPB).由于位于准同型相界区域的陶瓷样品对于电畴的转向具有促进作用,所以处于MPB区域的陶瓷样品具有较大的压电和介电性能,但同时由于电畴转向带来的较大内摩擦和结构损耗,从而提高了材料的机械损耗和介电损耗.当x=0.02时的陶瓷样品获得最佳的综合性能:d33=346 pC/N,kp=0.58,Qm=1217,εr=1724,tanδ=0.774;.     

烧结升温速率对钛酸钡陶瓷压电性能的影响

采用固相反应方法在不同烧结升温速率下制备了BaTiO3陶瓷,并对陶瓷样品的晶体结构、表面形貌、介电、压电和铁电性能进行了测试和分析.结果表明:当烧结升温速率为3 ℃/min和5 ℃/min时陶瓷均为四方钙钛矿晶格结构,随升温速率的增大,四方相程度增强,材料平均晶粒尺寸减小,压电系数和铁电性能随之降低,但介电常数随之增大,当烧结升温速率为5 ℃/min介电常数最大,其值为3144.当烧结升温速率为1 ℃/min时陶瓷为正交钙钛矿晶格结构d33和Pr最大,其值为Pr=10 μC/cm2和d33=193 pC/N.     

Fe2O3掺杂(Ba0.7Ca0.3)TiO3-Ba(Zr0.2Ti0.8)O3无铅压电陶瓷的制备与性能

采用固相合成法制备了Fe2O3掺杂(Ba0.7Ca0.3)TiO3-Ba(Zr0.2Ti0.8)O3(简称BCZT)无铅压电陶瓷。借助XRD、SEM、阻抗分析仪等对该陶瓷的相组成、显微结构以及压电和介电性能进行了研究。结果表明,Fe2O3掺杂降低了BCZT无铅压电陶瓷的烧结温度并使居里温度Tc从85℃提高到95℃;当Fe2O3掺杂为0.02wt%～0.1wt%时,陶瓷样品均为ABO3型钙钛矿结构;少量Fe2O3掺杂促进了陶瓷晶粒的生长,但随着Fe2O3掺杂量进一步增加,陶瓷晶粒随之细化;当Fe2O3掺杂量为0.04wt%时,陶瓷样品具有最优综合电性能,其压电常数d33、机电耦合系数kp、机械品质因数Qm、介电损耗tanδ和介电常数εr分别为400 pC/N,0.40,51,0.023和3482。     

Na0.5Bi0.5TiO3-K0.5Bi0.5TiO3-BaMnO3无铅压电陶瓷的结构与电性能

采用固相法制备了(0.8 -x)Na0.5 Bi0.5TiO3 -0.2K0.5Bi0.5TiO3-xBaMnO3(简称NBT-KBT-BM)无铅压电陶瓷,研究了不同BM含量(x=0,0.25％,0.50％,0.75％,1.00％,1.25％,物质的量分数)样品的物相组成、显微结构及电性能.结果表明:所制备的NBT-KBT-BM陶瓷样品均为单一的钙钛矿结构.与纯NBT-KBT陶瓷相比,掺BM陶瓷的烧结温度降低,相对密度ρr得到提高.随x的增加,材料的压电常数d33、平面机电耦合系数kp与机械品质因子Qm先增大后减小,而介电损耗tanδ以及退极化温度Td一直降低.BM的掺入降低了材料的矫顽场Ec,提高了剩余极化强度Pr,从而增强了铁电性.当x=0.75％时,陶瓷获得最佳性能:d33=167 pC/N,kp=0.269,Qm=133,εr=774,tanδ=2.93％.     

Y2O3掺杂对(Ba0.85Ca0.15)Zr0.1Ti0.896Sm0.004O3无铅压电陶瓷介电弛豫与电性能的影响

采用固相法制备了(Ba0.85Ca0.15)1-xYxZr0.1Ti0.896Sm0.004O3(BCZTS-Yx)无铅压电陶瓷.研究了Y2O3含量对BCZTS-Yx无铅压电陶瓷相结构、压电与介电性能的影响.结果表明:Y3+作为施主掺杂物占据A位.当0.004≤x≤0.006时,陶瓷存在三方相与四方相共存的准同型相界结构.当x=0.006时,陶瓷具有最佳的电性能,分别为d33=384 pC/N,kp=37.2;,εr～6775,tanδ ～ 2.04;.利用Curie-Weiss定律对该实验结果进行拟合,发现x为0.006的样品的介电弛豫特征更为明显.     

X-ray crystal structures ofcis-bis(diphenylphosphinamide)tetracarbonylmolybdenum(0) andtrans-bis(N-methyl diphenylphosphinamide)tetracarbonylmolybdenum(0)

The X-ray crystal structures ofcis-Mo(CO)₄(Ph₂PNH₂)₂,I, andtrans-Mo(CO)₄(Ph₂PNHMe)₂,II, are presented. ComplexI crystallizes in the monoclinic space groupP2₁/c(a=13.433(1),b=12.2719(8),c=17.318(2)Å;=109.79(1)°;V=2686.1(8)ų;Z=4). ComplexII crystallizes in the triclinic space groupP¯1 (a=6.9986(8),b=10.328(1),c=11.241(2)Å,=107.58(1)°,=91.76(1)°, =101.28(1)°,V=756.1(4)ų,Z=1). The molybdenum coordination geometry in each complex is a slightly distorted octahedron. The molybdenum-carbon bond lengths for the carbonyls trans to phosphorus in complexI are shorter than those the carbonyls trans to other carbonyls. The average molybdenum-phosphorus distance inI (2.525(5)Å) is similar to those in other diphenylphosphinamide complexes and longer than the molybdenum-phosphorus distance inII in 2.4585(7)Å). The distance between two nitrogen atoms incis Mo(CO)₄(Ph₂PNH₂)₂ (3.74(3)Å) is significantly larger than the sum of their van der Waals radii (3.10 Å) indicating that the two nitrogens are not hydrogen bonded.     

Crystal and molecular structure of Bis(glyoxal-bis-tert.butylimine)nickel(0)

The crystal structure determination of the title compound was undertaken to determine the coordination geometry of nickel atom. Bis(glyoxal-bis-tert.butylimine)nickel(0) (C₂₀H₄₀NiN₄) crystallizes in the space group Pna2₁ with Z = 4, a = 18.546(6), b = 9.331(8), and c = 13.505(8) Å. The structure was solved by the heavy atom method and refined to R = 0.065. The molecule has four-coordinate nickel atom. The coordination geometry about the nickel atom is tetragonal.     

X-ray structures of tris(0-cyclohexyl-dithiocarbonato)bismuth(III) and tris(0-benzyl-dithiocarbonato)bismuth(III)

The crystal structures of two Bi tris xanthates are reported, namely [Bi(S₂CO-c-C₆H₁₁)₃ J and [Bi(S₂COCH₂C₆H₅)₃]. They exist as centrosymmetric dimers, owing to the presence of bridging xanthate ligands, with seven-coordinate Bi atoms. The presence of a stereochemically active lonepair of electrons in each structure distorts the coordination geometry defined by seven S atoms and causes the elongation of some of the Bi-S bond distances. Crystals of both compounds are triclinic, space groupP¯1 with unit cell dimensions for [Bi(S₂CO-c-C₆H₁₁)₃]:a=12.417(3),b=13.571(3),c=9.681(4) Å;=102.30(2),=109.21(2), =66.23(2)° andZ=2; and for [Bi(S₂COCH₂C₆H₅)₃]:a=14.747(2),b=15.966(2),c=5.991(1) Å;=95.08(1),=98.51(1), =104.92(1)° andZ=2. The structures were refined by a full-matrix least-squares procedure to finalR=0.045 using 4274 reflections for [Bi(S₂CO-c-C₆H₁₁)₃] and toR=0.027 using 3993 reflections for [Bi(S₂COCH₂C₆H₅)₃].     

Epitaxial NiO (1 0 0) and NiO (1 1 1) films grown by atomic layer deposition

Epitaxial NiO (1 1 1) and NiO (1 0 0) films have been grown by atomic layer deposition on both MgO (1 0 0) and α-Al₂O₃ (0 0 l) substrates at temperatures as low as 200 °C by using bis(2,2,6,6-tetramethyl-3,5-heptanedionato)Ni(II) and water as precursors. The films grown on the MgO (1 0 0) substrate show the expected cube on cube growth while the NiO (1 1 1) films grow with a twin rotated 180° on the α-Al₂O₃ (0 0 l) substrate surface. The films had columnar microstructures on both substrate types. The single grains were running throughout the whole film thickness and were significantly smaller in the direction parallel to the surface. Thin NiO (1 1 1) films can be grown with high crystal quality with a FWHM of 0.02–0.05° in the rocking curve measurements.     

Structural characterization of CdTe layers grown on (0 0 0 1) sapphire by MOCVD

Crystalline ZnO nanoparticles were synthesized on Si substrates with or without a Au catalyst by a chemical vapor deposition (CVD) method using ZnS as the source material. The average sizes are in the range of 40–200 nm and the densities of 10⁴–10¹⁰ cm⁻². In the absence of an Au catalyst, the average nanoparticle size firstly decreases and then increases with increasing substrate temperature while the nanoparticle density decreases as the substrate temperature increases. In the presence of an Au catalyst, ZnO nanoparticles only grow when the substrate temperature is higher than 300°C and the higher the substrate temperature the denser the nanoparticles are deposited. The density of the ZnO nanoparticles grown on a Si (1 1 1) substrate is higher than that on a Si (1 0 0) substrate with or without Au catalyst.     

The crystal structure of tris(4-methylpyridine) tricarbonylmolybdenum(0)

The title compound, Mo(4-CH₃C₅H₄N)₃(CO)₃, is monoclinic, P2₁/c, with cell dimensionsa=10.385(1),b=13.572(2),c=15.522(2) Å, =105.08(1)°,Z=4. The complex isfac-octahedral with approximate three-fold symmetry. The Mo–C bond lengths are 1.901–1.904(7) Å, distinctly shorter than in the parent Mo(CO)₆, and the Mo–N bond lengths are 2.297–2.331(5) Å.     

Selective area growth of GaN microstructures on patterned (1 1 1) and (0 0 1) Si substrates

Selective MOVPE growth of GaN microstructure on silicon substrates has been investigated using SiO₂ mask having circular or stripe window. In case of (0 0 1)substrate, grooves with (1 1 1) facets at the sides were made by using the etching anisotropy of a KOH solution. On the (1 1 1) facets of patterned silicon substrate (or on the as opened window region of (1 1 1) substrate), growth of wurtzite GaN was performed, of which the c-axis is oriented along the 1 1 1 axis of silicon. The photoluminescence and X-ray diffraction analysis were performed to characterize the single crystal to reveal the effect of the growth conditions of the intermediated layer and the microstructure.     

Influence of substrate temperature on nitridation of (0 0 1) GaAs using RF-radical source

The mechanism of nitridation of (0 0 1) GaAs surface using RF-radical source was systematically studied with changing substrate temperature, nitridation time and supplying As molecular beam. It was found from atomic forth microscopy (AFM) measurements that supplying As is very important to suppress the re-evaporation of As atoms and to keep the surface smooth. Reflection high-energy electron diffraction (RHEED) measurements shows that surface lattice constant (SLC) of GaAs of 0.565 nm decreases with increasing the substrate temperature and that it finally relaxes to the value of c-GaN of 0.452 nm, at 570 °C in both [1 1 0] and [1¯ 1 0] directions without concerning with the supply of As molecular beam. But, in the medium temperature range (between 350 and 520 °C), SLC of [1 1 0] direction was smaller than that of [1¯ 1 0] direction. This suggests a relation between the surface structure and the relaxing mechanism of the lattice. The valence band discontinuity between the nitridated layer and the GaAs layer was estimated by using X-ray photoemission spectroscopy (XPS). It was between 1.7 and 2.0 eV, which coincides well with the reported value of c-GaN of 1.84 eV. This suggests that the fabricated GaN layer was in cubic structure.     

Si(0 0 1) surface oxidation by N2O

Ultra-thin homogeneous oxynitride films are prepared on Si(0 0 1). The Si surface is cleaned in UHV by heating (flashing) and is exposed to different pressures of N₂O at altered temperatures. Thus oxynitride layers of different thickness and different properties are grown depending on the N₂O pressure and the Si temperature. This is illustrated by a schematic diagram. The properties of the different oxynitride layers were studied by a combined photoemission electron microscopy (PEEM) and photoelectron spectroscopy (PES) investigation using highly monochromatic synchrotron radiation. The amount of oxygen and nitrogen incorporated in the oxynitride layers is determined from the PES measurements. The typical surface morphology for different preparation conditions is shown in PEEM images.     

Mg segregation in a (1 1¯ 0 1) GaN grown on a 7° off-axis (0 0 1) Si substrate by MOVPE

Redistribution behavior of magnesium (Mg) in the N-terminated (1 1¯ 0 1) gallium nitride (GaN) has been investigated. A nominally undoped GaN layer was grown on a heavily Mg-doped GaN template by metalorganic vapor-phase epitaxy (MOVPE). Mg dopant profiles were measured by secondary ion mass spectrometry (SIMS) analysis. A slow decay of the Mg concentration was observed in the nominally undoped GaN layer due to the surface segregation. The calculated decay lengths of the (1 1¯ 0 1) GaN are ∼75–85 nm/decade. These values are shorter than the decay length determined in the sample grown on the Ga-terminated (0 0 0 1) GaN. This result indicates that Mg exhibited weak surface segregation in the (1 1¯ 0 1) GaN as compared to the (0 0 0 1) GaN. The weak surface segregation is in agreement with the high efficiency of Mg incorporation on the (1 1¯ 0 1) face. The high density of hydrogen was obtained in the (1 1¯ 0 1) GaN, which might enhance the Mg incorporation.