YBCO涂层导体CeO2,Y2O3缓冲层的生长研究

采用反应溅射的方法在具有立方织构的Ni基底上制备了CeO2,Y2O3缓冲层.Ar/H2气氛下预沉积的引入,有效地抑制了基底的氧化.同时,为保证薄膜的外延取向,预沉积时间必须和总沉积时间满足线性关系.对比CeO2,Y2O3的生长条件,发现CeO2的外延生长区间比Y2O3宽,Y2O3的生长对温度、气压等条件更为敏感.最终制备的CeO2缓冲层是纯的(100)取向,其平面内φ扫描半高宽(FWHM)为8.5°;而Y2O3存在两种平面取向,一种是Y2O3(110)‖Ni(100),另一种是Y2O3(100)‖ Ni(100).俄歇能谱观察表明,CeO2/Ni界面优于Y2O3/Ni界面.扫描电镜照片显示,CeO2,Y2O3缓冲层的表面均匀致密,无裂纹生成,但两种薄膜中,都有呈三角形的胞状突起.     

声表面波器件用〈110〉取向ZnO薄膜的MOCVD生长

Zn O是具有纤锌矿晶体结构的多功能半导体材料 ,它具有 3 .3 7e V的禁带宽度和高达 60 me V的激子束缚能 ,是很有希望的紫外发光材料 .由于具有 c轴的择优取向性 ,因此目前人们的注意力主要集中在对 c轴取向 Zn O薄膜的特性研究上 [1～ 3] .但其它取向的 Zn O薄膜也可在某些衬底的特定面上 ,通过特定的条件进行生长 ,如〈1 1 0〉取向的 Zn O薄膜可在特定的条件下生长在蓝宝石 R面衬底上[4～ 7] .由于 (1 1 0 )面的 Zn O薄膜具有一些 c轴取向薄膜所不具备或无法比拟的特性 ,如 :机电耦合系数高达6% (C面薄膜的机电耦合系数却不足 1 % )…     

单一混合固态源PE-MOCVD法制备YSZ薄膜及其表征

采用等离子体增强的MOCVD技术,以均匀混合的金属β-二酮鳌合物固态源Y(DPM)₃和Zr(DPM)₄作为前驱物,在NiO/SDC多孔阳极和多孔-αAl₂O₃衬底上制备了氧化钇稳定的氧化锆(YSZ)薄膜.研究了两种衬底对成膜过程和膜的结构以及微结构的影响,讨论了源区输运机制及薄膜生长动力学.XPS分析结果表明,薄膜中Y和Zr元素的摩尔比低于原始混合源中的Y和Zr元素的摩尔比,当混合源中的Y和Zr元素的摩尔比约为0.35:1时,可以获得无定形态的8%YSZ薄膜,经高温焙烧转化为单一立方相,其晶粒大小约为100nm,薄膜的生长速率约为7nm/min.     

强磁场辅助TFA-MOD法制备YBCO厚膜的理论分析

为了实现YBa2Cu3O7-x(YBCO)涂层导体在电力工业中的实际应用，必须有效增加YBCO超导层的厚度。提出一个强磁场辅助TFAMOD法制备YBCO厚膜的新工艺，并从磁热力学和磁性物理出发理论分析其可行性。沿垂直基底平面方向施加强磁场时，磁场将促进c轴取向YBCO晶核的形成，诱导厚膜中非c轴取向晶核转动到c轴平行磁场取向的位置。另外，取向晶粒间磁性相互作用力使晶粒沿磁场方向定向聚合，有利于获得致密的厚膜。因此，强磁场辅助TFA—MOD法有望制备高临界电流密度的YBCO织构厚膜。     

Si衬底上生长的铁硅化合物结构和取向分析

采用分子束外延法分别在650-920℃的Si(110)和920℃的Si(111)衬底表面生长出铁的硅化物纳米结构,并主要分析了920℃高温下纳米结构的形貌、组成相及其与Si衬底的取向关系.扫描隧道显微镜(STM)研究表明,920℃高温下,Si(110)衬底上生长的铁硅化合物完全以纳米线的形式存在,且其尺寸远大于650℃低温下外延生长的纳米线尺寸;Si(111)衬底上生长出三维岛和薄膜两种形貌的铁硅化合物,其中三维岛具有金属特性且直径约300 nm、高约155 nm,薄膜厚度约2 nm.电子背散射衍射研究表明920℃高温下Si(110)衬底上生长的纳米线仅以β-FeSi2的形式存在,且β-FeSi2相与衬底之间存在唯一的取向关系:β-FeSi2(101)//Si(11 1);β-FeSi2[010]//Si[110];Si(111)衬底上生长的三维岛由六方晶系的Fe2Si相组成,Fe2Si属于164空间群,晶胞常数为a=0.405 nm,c=0.509 nm;与衬底之间的取向关系为Fe2Si(001)∥Si(111)和Fe2Si[1 20]//Si[112].     

中温平板型固体氧化物燃料电池研究

采用流延法制备Ni/YSZ阳极支撑体 YSZ电解质复合膜素坯.经等静压,共烧结而得到的复合膜,其YSZ电解质层的厚度在1530μm之间,面积大于100cm2.再将由柠檬酸盐法合成的Ce0.8Sm0.2O1.9(CSO)和固相法合成的La0.6Sr0.4CoO3(LSCO)相继沉积到YSZ膜上形成有CSO中间层的复合阴极,从而构成Ni/YSZ/CSO/LSCO的中温平板型固体氧化物燃料(单体)电池,其中Ni/YSZ为阳极,CSO是中间层,LSCO为阴极.以H2作燃料气,O2为氧化气,850℃下,该单电池开路电压达1.1V,最大输出功率密度0.2W/cm2.本文还对该单电池复数阻抗谱进行了分析讨论.     

溅射气体中氩气含量对Y1Ba2Cu3O7-δ薄膜结构和Tc的影响

采用倒筒直流磁控溅射系统在不同溅射气体组分下(氩氧比不同)原位沉积Y1Ba2Cu2O7-δ(YBCO)薄膜.样品的XRD分析发现在Ar含量过高和过低的溅射气氛下沉积的薄膜存在极少量的BaCuO2第二相, 同时显示薄膜的c轴长度, (006), (007)对(005)峰强度比随着溅射气体中Ar含量的变化而发生改变.通过薄膜超导零电阻温度检测发现, YBCO薄膜的超导零电阻温度Tc随之发生改变.这说明在磁控溅射沉积YBCO薄膜过程中, 溅射气体中Ar气含量影响薄膜各元素的化学计量比, Ar含量过高和过低导致沉积YBCO薄膜晶体结构发生畸变, 恶化超导电性.     

YSZ传导膜H_2S固体氧化物燃料电池

研究了Y2O3稳定的ZrO2(YSZ)氧离子传导膜H2S固体氧化物燃料电池性能。掺杂NiS、电解质、Ag粉和淀粉制备了双金属复合MoS2阳极催化剂,掺杂电解质、Ag粉和淀粉制备了复合NiO阴极催化剂,用扫描电镜对YSZ和膜电极组装(MEA)进行了表征,比较了不同电极催化剂的性能和极化过程,考察了不同温度对电池性能的影响。结果表明,双金属复合MoS2/NiS阳极催化剂在H2S环境下比Pt和单金属MoS2催化剂稳定,复合NiO阴极催化剂比Pt性能好,在电极催化剂中加入Ag可显著提高电极的导电性;与Pt电极相比,复合MoS2阳极和复合NiO阴极催化剂的过电位较小,阳极的极化比阴极侧小;温度升高,电池的电流密度与功率密度增加,电化学性能变好。在750℃、800℃、850℃和900℃及101.13 kPa时,结构为H2S、(复合MoS2阳极催化剂)/YSZ氧离子传导膜/(复合NiO阴极催化剂)、空气的燃料电池最大功率密度分别为30 mW/cm2、70 mW/cm2、155 mW/cm2及295 mW/cm2、最大电流密度分别为120 mA/cm2、240 mA/cm2、560 mA/cm2和890 mA/cm2。     

工艺参数对TSMTG法制备单畴YBCO样品的影响

用顶部籽晶熔融织构法(TSMTG)制备了30min直径的YBCO超导块，研究了不同的工艺条件对样品宏观形貌、织构取向和磁浮力的影响，比较了3种样品在零场冷条件下的排斥力和场冷条件下的吸引力。结果发现：由籽晶控制取向生长的单畴YBCO样品宏观形貌是以顶部籽晶为中心的4个结晶扇区，有单一的c轴取向，零场冷条件下的排斥力和场冷条件下的吸引力最大；籽晶成核但没有控制取向生长的YB-CO样品宏观形貌是以顶部籽晶为中心的多个(大于4个)扇区，相邻扇区间夹角不等，c轴取向不一致，磁浮力性能居中；非籽晶成核生长的多畴YBCO样品，上表面是以籽晶为中心的一个边长约1cm的四方结晶区，其余部分是自发成核的多晶，样品c轴取向杂乱，磁浮力很低。     

溶胶-凝胶法在聚酰亚胺衬底上制备c轴取向ZnO薄膜

通过溶胶-凝胶工艺, 采用两步加热法在聚酰亚胺表面制备了具有c轴取向的ZnO薄膜. 通过差式扫描量热-热重分析(DSC-TGA)得出最佳的前热处理温度和后热处理温度分别为300和390 ℃. 通过X射线衍射(XRD)和扫描电子显微镜(SEM)对薄膜的晶体取向和表面形貌进行了分析, 描述了ZnO薄膜在聚酰亚胺上的生长过程. 拉伸实验结果表明, ZnO薄膜与聚酰亚胺衬底有较强的附着力.     

Substrate dependent structure and in-plane dielectric properties of Ba(Sn0.15Ti0.85)O3 thin films

The structure, microstructure and in-plane dielectric properties of Barium tin titanate Ba(Sn_0.15Ti_0.85)O₃ (BTS) thin films grown on (100) LaAlO₃ (LAO) and (100) MgO single crystal substrates through sol–gel process were investigated. The films deposited on (100) LAO substrate exhibited a strong (100) preferred orientation while the film deposited on (100) MgO substrate showed polycrystalline structure. The in-plane ɛ–T measurements reveal that the films grown on (100) LAO substrate exhibited an obvious room-temperature ferroelectric state, while the film grown on MgO substrate showed paraelectric state in the temperature range of 10–130 °C. A high tunability of 52.11% was observed for the BTS films deposited on (100) LAO substrate at the frequency of 1 MHz with an applied electric field of 80 kV/cm, which is about two times larger than that of the BTS films deposited on (100) MgO substrate. The obvious differences in the dielectric properties could be attributed to the stress in the films, which come from lattice mismatch and difference in the thermal expansion coefficients between the film and substrates. This work clearly reveals the highly promising potential of BTS films for application in tunable devices.     

Synthesis and Properties of Highly Conductive Thin Films as Buffer Layer from Sol-Gel Process

We prepared epitaxial growth SrRuO₃ thin film on LaAlO₃ (001) (LAO) single crystal substrate and highly oriented BaTiO₃ ferroelectric thin film on the epitaxial SrRuO₃ thin film. A homogeneous precursor solution for preparing SrRuO₃ thin film was prepared with Sr(O—i—C₃H₇)₂ and Ru(NO)(NO₃)₃ as starting materials, and 2-methoxy ethanol as solvents. The as-coated thin films were heat treated at temperatures from 723 to 1273 K for 1 h in air. SrRuO₃ grew epitaxially on LAO(001) substrate, which were confirmed by XRD theta-2theta method and XRD pole figure analysis. The crystallographic relationship of the film and substrate was SrRuO₃(001) parallel to LAO(001) and SrRuO₃[110] parallel to LAO[100]. A homogeneous precursor solution for preparing BaTiO₃ thin film was prepared with Ti[O—n—(CH₂)₃CH₃]₄ and Ba(OCOCH₃)₂ as starting materials, and acetic acid, 2-methoxy ethanol. SrRuO₃ coated LAO substrates were coated by spin-coating method with the coating solution. The as-coated thin films were heat treated at temperatures from 973 to 1173 K in air. It was confirmed that the thin films were growing orientated for c-axis by measurement of XRD theta-2theta method.     

Optimization of the electrophoretic deposition of YBa2Cu3O7−x superconducting large area coatings

Large area coatings (>10cm²) of the high temperature superconductor YBa₂Cu₃O_7–x (x = 0.1 – 0.2) (YBCO) have been prepared by scale up an electrophoretic deposition technique using silver sheets and Si-wafers coated with Ag or Au as substrates. Several parameters, like the kind of the solvent, the applied voltage, the distance between the electrodes, the initial concentration of the suspension and the temperature during the electrophoresis were investigated in order to attain high deposition rates, as well as uniform YBCO coatings with the proper stoichiometry. To obtain a strongly adherent and dense coating a subsequent appropriate sintering and annealing procedure has been developed. The coatings obtained were characterized for their stoichiometry and superconducting properties by X-ray diffraction (XRD), Raman spectroscopy and magnetic measurements. The homogeneity and thickness of the films and the average grain size of the deposited particles have been investigated by optical and scanning electron microscopy (SEM).     

Enhancement of critical current density in superconducting YBa2Cu3O7−x films by nanostructure development of substrate surface using sol–gel method

In this paper, a simple sol–gel route has been adopted in developing substrate surface for the first time. Only by adjusting the concentration of precursor solution, LaAlO₃ (LAO) nanodot arrays were directly obtained on LAO single crystal substrate, without incorporating additional processing steps. Subsequently, YBa₂Cu₃O_7?x (YBCO) superconducting films were prepared on the nanodot arrays using a low-fluorine solution process. In contrast, J _c of YBCO films grown on the substrate developed with nanodot arrays is almost three times as large as that of YBCO films grown on undeveloped substrate in an applied magnetic field with the strength of 3 Tesla. The pinning force density (F _p ) of YBCO film on the nanodot arrays developed substrate is 2.7 GN/m³ which exceeds that (1.8 GN/m³) of YBCO films on undeveloped substrate. The results of cross-section transmission electron microscope (TEM) images show that the extended defects along the a–b planes of YBCO, induced by the developed substrate with nanodot arrays, should be the origin of the J _c enhancement.     

Crystallization of textured PbTiO3 films deposited from gels

Sol-gel processed PbTiO₃ thin films have been deposited by spin coating onto different subtrates; Si[111], Si/Al, Si/SiO₂/Cr/Pt, MgO[100], SrTiO₃[100] and sapphire. Interactions between the substrate and PbTiO₃ films after heat treatment have been studied by X-ray diffraction and Rutherford Back Scattering. When deposited onto sapphire and Si[111], PbTiO₃ films exhibit a preferred orientation with (101) perpendicular to the substrate. These films become oriented along (100) onto MgO and (001) onto SrTiO₃[100] substrates. A strong channelling effect is observed by the RBS technique when the film is oriented along the c axis on SrTiO₃[100] suggesting that these films are epitaxially grown. The diffusion of metal atoms during the thermal treatment gives rise to the formation of lead silicate on Si[111] substrates. As a result a pyrochlore phase is formed. Lead titanate films on Si/SiO₂/Cr/Pt and Si/Al substrates are polycrystalline and do not exhibit any texture.     

La2O3对Ni/γ-Al2O3甲烷化催化剂的助催化作用

我国将稀土作为助剂引入镍基甲烷化催化剂,大大提高了催化剂的活性和热稳定性,并已投入工业应用［1－3］．稀土对不同镍催化剂反应性能及其作用机理的研究已有一些报导［3－7］．谢有畅等观察到镍负载在经单层La2O3改性的γ－Al2O3表面,其晶粒要比没有La2O3时小得多．Rotgerink等认为添加La后反应速率的增加不只是由于几何效应,而是La对甲烷化本身有促进作用,单位镍表面的活性是随La含量不同而改变的,活性增加的同时表观活化能也增加［5］．作为助剂的La2O3在氢还原和反应过程中的变化及其作用的研究和讨论较少,目前一般认为添…     

Interfacial oxidation of ultrathin nickel and chromium films on yttria-stabilized zirconia

The substrate-induced oxidation upon prolonged annealing in UHV of ultrathin films of Ni and Cr vapor deposited on yttria-stabilized zirconia YSZ(100) was studied by X-ray photoelectron spectroscopy (XPS) to obtain information about the oxidation mechanism, determine the available quantity of reactive oxygen in YSZ, and investigate the thermal stability of the thin oxide films. Up to about 0.8 ML of Ni deposited at room temperature was oxidized to NiO at a constant rate at 650 K via the substrate, whereas at slightly higher coverage, the oxidation rate under identical conditions was drastically reduced. In contrast to Ni, up to 4.8 ML of Cr deposited at 275 K could be oxidized via the substrate to Cr2O3 upon extensive UHV annealing at increasing temperature up to 820 K, indicating a reactive oxygen content of at least 4 x 10(-6) with respect to the lattice oxygen in the YSZ specimen. The Cr2O3 decomposed to metallic Cr above about 800 K, whereas NiO was stable up to the maximum temperature of 875 K. These results indicate that the oxidation via the substrate is kinetically analogous to the gas-phase oxidation of bulk Ni and Cr. The reactive oxygen content of the single-crystal YSZ is larger than expected, and part of it is accommodated at the surface of the substrate. The thermal stability of the thin oxide films is determined by the oxygen exchange with YSZ and not by the respective bulk oxide thermodynamic decomposition temperature.     

金属离子修饰的Ru-Pt/γ-Al2O3催化p-CNB选择性加氢

催化还原法制备卤代苯胺因具有产品质量好、收率高和三废少等优点而日益受到重视．近年来,研究较多的是高分子化合物稳定的Pt,Pd,Ru单金属或双金属胶体催化剂以及负载型单金属或双金属催化剂．用第三金属组分修饰的胶体催化剂的催化性能更好,但反应后催化剂与产物分离     

PCVD法制备ZrO~2和YSZ薄膜

以金属β-二酮类有机螯合物Zr(DPM)~4和Y(DPM)~3为挥发性源物质, 采用微波等离子体化学气相淀积法于较低的温度下(420～560℃)成功地在多孔α-Al~2O~3陶瓷,非晶玻璃等衬底上制备出致密的ZrO~2和YSZ薄膜材料.XRD分析结果表明,纯ZrO~2薄膜中除了单斜相外还存在着亚稳态的四方相.当掺入的Y~2O~3 摩尔百分含量大于或等于7%时,ZrO~2完全被稳定成立方相.SEM观察表明, 在等离子体内的不同区域中生成的薄膜形貌有所不同.XPS检测了YSZ薄膜中Zr3d~5~/~2和Zr3d~3~/~2 的电子结合能,发现较ZrO~2的标准值低0.7eV.由TEM观察和由XRD衍射峰半宽度计算, 所制备的ZrO~2和YSZ薄膜中微晶粒径在10nm左右     

Co3O4纳米片的制备及对H2O2电还原反应的催化性能简

通过恒电势电沉积和加热处理在泡沫镍基体上制备了Co3O4纳米片. 利用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线衍射(XRD)、傅里叶变换红外光谱(FTIR)和X射线光电子能谱(XPS)等手段对纳米片的形貌和结构进行了表征. 采用线性伏安扫描和计时电流技术研究了Co3O4纳米片电极对H2O2的电还原性能. 结果表明,在3.0 mol/L KOH 和 0.4 mol/L H2O2溶液中,当电压为-0.4 V(vs. Ag/AgCl)时,线性伏安扫描电流密度达到-0.386 A/cm2,在1000 s 测试时间内,计时电流密度衰减很小,表明Co3O4纳米片电极对H2O2具有很高的活性和稳定性.