Al2O3/YSZ Composite Coatings Prepared by a Novel Sol–Gel Process and Their High-Temperature Oxidation Resistance

In this study, a novel sol–gel process has been utilized to fabricate Al₂O₃/YSZ (6 wt% yttria partially stabilized zirconia) composite coatings on Ni-based superalloy. The green coatings were obtained by electrophoretic deposition (EPD) in a suspension containing aluminium oxide sol, nano-Al₂O₃ and micro-YSZ particles, and then treated by so-called pressure filtration microwave sintering (PFMS) process. The as-sintered composite coatings were dense, uniform and crack-free and the phases mainly present α-Al₂O₃, m-ZrO₂ and t-ZrO₂ as aluminium oxide sol content decreasing. The cyclic oxidation tests at 1000 °C for 200 h demonstrate that both of high-temperature oxidation and spallation resistance for the coated samples were remarkably improved. These beneficial effects could be attributed to the special microstructure that micro-YSZ particles embedded in nano/submicron Al₂O₃ matrix. Meanwhile, the mechanisms of the inhibition of the oxygen diffusion and thermal match are further discussed.     

Preparation of Y_(1-x)Ho_xBa_2Cu_3O_(7-δ) Superconductive Thin Films

ＰｒｅｐａｒａｔｉｏｎｏｆＹ＿（１－ｘ）Ｈｏ＿ｘＢａ＿２Ｃｕ＿３Ｏ＿（７－δ）ＳｕｐｅｒｃｏｎｄｕｃｔｉｖｅＴｈｉｎＦｉｌｍｓＰｅｎｇＺｈｅｎｇｓｈｕｎ，ＹａｎｇＢｉｎｇｃｈｕａｎ，ＷａｎｇＸｉａｏｐｉｎｇ（彭正顺）（杨秉川）（王小平）ＳｈｉＤｏｎｇ...     

Texture Analysis of Thin Titanium(TA1)Strip by Maximum-entropy Method

The Maximum-entropy Method(MEM)for determining the complete ODF(orientation distributionfunction),accompanied with the equal-volume partitioning technique for quantitative texture analysis,was firsttested in analysing the texture of a commercial purity titanium strip.The experimentally measured results indi-cate that the rolling planes of most grains in this sample are parallel to the{1010}and the{1210}with about~±10°spread while the rolling directions nearly distribute uniformly and their volume fractions are 19.46％and 18.70％ respectively.Besides,there are still two weaker texture components,(7526)[1544]and(1105)[2311],with 3.24％and 4.17％respectively.     

Effects of Annealing Temperature on the Structural,Optical,and Electrical Properties of ZnO Thin Films Grown on n-Si<100>Substrates by the Sol–Gel Spin Coating Method

The effects of annealing temperature on the sol–gel-derived ZnO thin films deposited on n-Sh100 i substrates by sol–gel spin coating method have been studied in this paper.The structural,optical,and electrical properties of ZnO thin films annealed at 450,550,and 650 °C in the Ar gas atmosphere have been investigated in a systematic way.The XRD analysis shows a polycrystalline nature of the films at all three annealing temperatures.Further,the crystallite size is observed to be increased with the annealing temperature,whereas the positions of various peaks in the XRD spectra are found to be red-shifted with the temperature.The surface morphology studied through the scanning electron microscopy measurements shows a uniform distribution of ZnO nanoparticles over the entire Si substrates of enhanced grain sizes with the annealing temperature.Optical properties investigated by photoluminescence spectroscopy shows an optical band gap varying in the range of 3.28–3.15 eV as annealing temperature is increased from 450 to 650 °C,respectively.The fourpoint probe measurement shows a decrease in resistivity from 2:1 10 2to 8:1 10 4X cm with the increased temperature from 450 to 650 °C.The study could be useful for studying the sol–gel-derived ZnO thin film-based devices for various electronic,optoelectronic,and gas sensing applications.     

Preparation of Al2O3–ZrO2–Y2O3 Composite Coatings by a Modified Sol–Gel Technique for Thermal Barrier Application

Spatial-network Al₂O₃–ZrO₂–Y₂O₃ composite coatings were prepared by a modified sol–gel technique, so-called thermal pressure and filtration of sol–gel paint. The composite coatings were derived from a composite paint of yttria partially stabilized zirconia (YSZ) particles, Al₂O₃ particles and Al₂O₃–Y₂O₃ sol. Their microstructure showed that YSZ particles were covered with spatial-network Al₂O₃–Y₂O₃ blanket. Cyclic oxidation at 1,050 °C in air for 200 h demonstrates that the oxygen diffusion rate in the coatings could be effectively inhibited. Meanwhile, suitable coefficients of thermal expansion (CTE) gave the composite coatings better spallation resistance than that of Al₂O₃–Y₂O₃ or ZrO₂–Y₂O₃ coatings. The positive results of cyclic oxidation indicated that the composite coating can be used as an interlayer between the bond coat and the top ceramic layer in traditional TBCs. Not only the depletion rate of aluminum-rich phase in MCrAlY alloy could be slowed down by spatial-network Al₂O₃–Y₂O₃, but also different thermal expansion between thermally grown oxides layer and top layer could be relieved by suitable CTE. In this paper, the mechanisms of the inhibition of oxygen diffusion and thermal match between ceramic coating and alloy are also discussed.     

High Jc Epitaxial Superconducting YBa_2Cu_3O_(7-x) Thin Films

Excellent epitaxial growth of supercon-ducting YBa_2 Cu_3 O_(7-x) thin films have beenrealized on(100)SrTiO_3 and(100)ZrO_2substrates by a planar rf or DC-magnetronsputtering apparatus with UHV system.Thequality of growth and the epitaxial orientationof the film strongly depended on substratetemperature,the substrate orientation and ox-ygen partial pressure.The films exhibitedsuperconducting onset at 92K and zero resist-ance at 90K with critical current density of     

Synthesis,Fabrication and Characterization of ZnO-Based Thin Films Prepared by Sol–Gel Process and H<Subscript>2</Subscript> Gas Sensing Performance

In this paper, an attempt is made to deposit ZnO thin films using sol–gel process followed by dip-coating method on p-silicon (100) substrates for intended application as a hydrogen gas sensor owing to the low toxic nature and thermal stability of ZnO. The thin films are annealed under annealing temperatures of 350, 450 and 550 °C for 25 min. The crystalline quality of the fabricated thin films is then analyzed by field-emission scanning electron microscopy and transmission electron microscope. The gas sensing performance analysis of ZnO thin films is demonstrated at different annealing temperatures and hydrogen gas concentrations ranging from 100 to 3000 ppm. Results obtained show that the sensitivity is significantly improved as annealing temperature increases with maximum sensitivity being achieved at 550 °C annealing temperature and operating temperature of 150 °C. Hence, the modified ZnO thin films can be applicable as H₂ gas sensing device showing to the improved performance in comparison with unmodified thin-film sensor.     

Preparation and Characterization of Cu_2ZnSn（S_xSe_（1-x））_4Thin Films by Synchronous Sulfo-Selenization of Single-Source Evaporated Metallic Precursors

Cu2ZnSn(S,Se)4(CZTSSe) thin film was prepared using a simple two-step approach based on the single-source evaporation and synchronous sulfo-selenization.Composition,microstructure,morphology,and properties of the asprepared CZTSSe thin films were investigated.XRD and Raman patterns confirmed the formation of single-phase CZTSSe solid solutions.SEM results showed that the CZTSSe thin film had a uniform morphology and large grains.EDS results revealed the composition of CZTSSe film was Cu:Zn:Sn:S:Se = 23.7:12.6:12.2:37.7:13.8(in at%),which was in accordance with the stoichiometric Cu2ZnSn(S,Se)4.The optical band gap of CZTSSe thin film evaluated from its UV–Vis spectrum was 1.33 eV.The resistivity,carrier concentration,and mobility were 0.53 X cm,7.9 9 1018cm3,and 7.5 cm2/(Vs),respectively.     

Effect of Rare Earth Doping on Impedance,Modulus and Conductivity Properties of Multiferroic Composites:0.5(BiLa_xFe_(1-x)O_3)–0.5(PbTiO_3)

The Lanthanum-doped bismuth ferrite–lead titanate compositions of 0.5(Bi LaxFe1-xO3)–0.5(Pb Ti O3)(x = 0.05,0.10,0.15,0.20)(BLxF1-x-PT) were prepared by mixed oxide method.Structural characterization was performed by X-ray diffraction and shows a tetragonal structure at room temperature.The lattice parameter c/a ratio decreases with increasing of La(x = 0.05–0.20) concentration of the composites.The effect of charge carrier/ion hopping mechanism,conductivity,relaxation process and impedance parameters was studied using an impedance analyzer in a wide frequency range(102–106Hz) at different temperatures.The nature of Nyquist plot confirms the presence of bulk effects only,and non-Debye type of relaxation processes occurs in the composites.The electrical modulus exhibits an important role of the hopping mechanism in the electrical transport process of the materials.The ac conductivity and dc conductivity of the materials were studied,and the activation energy found to be 0.81,0.77,0.76 and 0.74 e V for all compositions of x = 0.05–0.20 at different temperatures(200–300 °C).     

Magnetic,Dielectric and Complex Impedance Properties of xBa_(0.95)Sr_(0.05)TiO_3–(1-x)BiFe_(0.9)Gd_(0.1)O_3Multiferroic Ceramics

xBa_(0.95)Sr_(0.05)TiO_3–(1-x)BiFe_(0.9)Gd_(0.1)O_3[x BST–(1-x)BFGO](x = 0.00, 0.10, 0.20 and 0.25) multiferroic ceramics were prepared by the standard solid-state reaction technique. Structural characterization was performed by X-ray diffraction. All the samples showed rhombohedral distorted perovskite structure. Surface morphology of the ceramics was studied by the field emission scanning electron microscope(FESEM). From the FESEM observation, the grain size was observed to be decreased with increasing BST content. Enhanced magnetic properties were observed in BFGO with the increase in BST content because of large lattice distortion. The complex initial permeability increased with the increasing of BST content. The study of dielectric properties showed that the dielectric constant increased, whereas dielectric loss decreased with increasing of BST content due to the reduction of oxygen vacancies. An analysis of the electric impedance and modulus with frequency was performed at different temperatures. Non-Debye-type relaxation processes occur in the compound which was confirmed from the nature of the Cole–Cole plot. The DC conductivity was found to increase with the rise in temperature which indicates the semiconducting behavior of the compound with characteristics of the negative temperature coefficient of resistance. The activation energy, responsible for the relaxation determined from the modulus spectra(0.246 eV), was found to be almost same as the value obtained from the impedance study(0.240 eV), indicating that charge carriers overcome the same energy barrier during relaxation. The frequency response of imaginary parts of electric impedance and modulus suggested that the relaxation in xB ST–(1-x)BFGO ceramics follows the same mechanism at various temperatures.     

化学液相法制备BiFeO3薄膜

以硝酸铋、硝酸铁以及柠檬酸为原料通过化学液相法在普通载玻片、（100）Si片和（100）ITO玻璃上分别制备了不同厚度的BiFeO3薄膜，研究了热处理温度对BiFeO3的形成以及微观形貌的影响。Si片上的薄膜由于与衬底之间的反应，得到纯BiFeO3相热处理温度需低于650℃，而在普通载玻片和ITO玻璃衬底上，525℃到650℃均可以得到结晶良好的纯BiFeO3薄膜。550℃热处理得到的BiFeO3薄膜中的晶粒尺寸大约在70～80nm之间，650℃热处理得到的晶粒尺寸约有140nm。磁性能测试证明薄膜有弱铁磁性，饱和磁化强度约在7000-9000A／m。     

溶胶一凝胶法制备掺铝氧化锌薄膜

采用溶胶-凝胶工艺在普通玻璃片上制备了掺铝氧化锌薄膜.通过X-射线衍射(XRD)、原子力显微镜(AFM)对薄膜的组织结构和形貌进行了表征,结果表明:用溶胶-凝胶法制得的掺铝氧化锌薄膜为纤锌矿型结构,呈c轴方向择优生长,表面均匀、致密.通过紫外-可见透射光谱(UV)和标准四探针法对薄膜的光电性能进行了研究.试验发现,当铝离子掺杂浓度为4%(摩尔分数)、溶胶物质的量浓度为0.6mol/L、前处理温度为300℃时,薄膜在可见光区的透过率超过80%,且具有较好的导电性,电阻率为8.0×10-4Ω·cm.     

铌酸钾纳米棒的新型溶胶-凝胶法合成

采用一种新的可溶性铌来代替价格昂贵的乙醇铌作为铌源,用溶胶-凝胶法合成铌酸钾(KN)纳米粉体。通过XRD、FTIR和TEM等技术手段对KN超细粉体的成相过程、相结构和微观形貌进行表征。结果表明,干凝胶在600℃煅烧可制得纯正交相的KN纳米粉体,合成温度比固相法降低了200℃以上;该粉体呈棒状,直径大约为100～200nm,长度大约为1～3μm,并对KN纳米棒的合成机制进行探讨。     

MOD法制备YBa2Cu3O7—x超导薄膜

用Ｙ、Ｂａ、Ｃｕ的三氟乙酸盐溶液，通过ＭＯＤ法在ＳｒＴｉＯ３（１００）衬底上成功地制得了黑色的、表面光滑的ＹＢＣＯ超导薄膜。研究了两种理想的成膜烧结工艺，对膜进行了物相研究。结果表明：在８５０℃，潮湿氧气氛中烧结的薄膜具有一定的择优取向；而在７５０℃，潮湿的低氧气氛中烧结的薄膜则具有高度的ｃ轴织构，前者的Ｔｃ（ｏｎｓｅ）≈９０Ｋ，Ｔｃ０≈７９Ｋ，较低的氧分压似乎有利于ｃ轴结构。     

柠檬酸盐溶胶-凝胶法合成LiZn(P_(1-x)V_x)O_4及其离子导电性

采用柠檬酸盐溶胶 -凝胶法合成了组成为 Li Zn(P1- x Vx) O4 (x=0 ,0 .1 ,0 .2 ,0 .3,0 .4,0 .5)的离子导体 ,并对合成材料进行了差示热分析 (DTA)、热重分析 (TG)、X射线衍射 (XRD)和透射电镜 (TEM)等表征。实验结果表明 ,组成为 Li Zn PO4 的烧结体结构为 α- L i Zn PO4 ;x=0 .4,0 .5的烧结体具有 Li Zn VO4 结构 ,为固溶体 (Li Zn VO4 )单相 ;而 x=0 .1 ,0 .2 ,0 .3的烧结体是由 α- Li Zn PO4 和 Li Zn VO4 两相组成的。由于 α- Li Zn PO4 烧结体的相对密度极小 ,样品在室温下几乎不显示导电性 ;而掺杂了 V以后的样品 ,随着结构和组成不同显示出不同程度的导电性 ,其中以 x=0 .4时值最大 ,T=30℃时 σ=4.55× 1 0 - 7S· cm- 1。     

Co1_(-x)Pt_x薄膜的结构与磁学性能

采用直流磁控溅射法制备了Co1_(-x)Pt_x合金薄膜,并详细研究了其结构和磁学性能随x变化的规律。通过XRD结构分析可知:溅射态的薄膜当x≤28%时,为hcp结构;x=35%和40%时,为hcp和fcc的混合结构;x≥46%以后,为fcc结构。VSM测试结果表明:随x的增大,溅射态薄膜的矫顽力先增大后减小,当x=23%时,矫顽力达到最大值2147×79.6A/m,在x=46%处矫顽力急剧下降至100×79.6A/m左右,x>46%以后,矫顽力随x的增大不再明显变化。退火后,hcp结构的薄膜矫顽力基本不变,而接近等原子比的fcc结构的CoPt薄膜,由于部分转变为fct结构,矫顽力有很大提高;fcc结构的CoPt3薄膜矫顽力有所增大,但是增大不多。     

溶胶凝胶法合成尖晶石型Li_(1 x)Mn_(2-x)O_4的工艺优化

通过引入水热合成对Pechini法进行改进 ,合成了锂离子正极材料Li1 xMn2 -xO4 。讨论了反应物的摩尔比、烧结温度、烧结时间和回火工艺对产物结构和粒度的影响。结果表明 ,烧结温度和时间以及Li/Mn摩尔比对产物的结构有较大影响 ,回火工艺可改善产物的粒度分布。优化的工艺条件为 :x =0 .0 6 ,烧结温度 6 5 0℃ ,烧结 6h ,再在 42 0℃回火 3h。得到的产物结构完整 ,颗粒均匀 ,放电容量为 118mAh/g。     

Li_(1 2x)Zn_(1-x_PO_4的合成及其锂离子的导电性

以Li2 CO3,ZnO和NH4 H2 PO4 为原料 ,采用传统固相合成法和柠檬酸盐溶胶凝胶法制备了组成为Li1 2xZn1-xPO4 (x =0～ 0 .5 )的固体粉末和烧结体。对合成材料作了DTA ,TG ,XRD和SEM等分析 ,并用交流阻抗技术测定了样品的导电性。实验结果表明 ,与传统的固相合成方法相比 ,溶胶凝胶法可以使样品合成温度降低约 40 0℃ ,并且具有较高的导电率。