Sc2W3O12薄膜制备及其负热膨胀性能

采用脉冲激光沉积法制备了斜方相Sc₂W₃O₁₂薄膜。利用X射线衍射仪(XRD)和场发射扫描电镜(FESEM)对Sc₂W₃O₁₂靶材和Sc₂W₃O₁₂薄膜组分、表面形貌和靶材断面形貌进行表征, 研究衬底温度与氧分压对薄膜制备的影响。采用变温XRD和热机械分析仪(TMA)分析了Sc₂W₃O₁₂陶瓷靶材和薄膜的负热膨胀特性。实验结果表明: 经1000℃烧结6 h得到结构致密的斜方相Sc₂W₃O₁₂陶瓷靶材, 其在室温到600℃的温度范围内平均热膨胀系数为-5.28×10^-6 K^-1。在室温到500℃衬底温度范围内脉冲激光沉积制备的Sc₂W₃O₁₂薄膜均为非晶态, 随着衬底温度的升高, 薄膜表面光滑程度提高; 随着沉积氧压强增大, 表面平整性变差。非晶膜经1000℃退火处理7 min后得到斜方相Sc₂W₃O₁₂多晶薄膜, 在室温到600℃温度区间内, Sc₂W₃O₁₂薄膜的平均热膨胀系数为-7.17×10^-6 K^-1。     

Co掺杂钙钛矿锰氧化物La0.8Sr0.2MnO3电磁特性研究

采用传统的高温固相反应法制备了La_0.8Sr_0.2Mn_1-xCo_xO₃(x = 0, 0.1, 0.3)多晶样品。系统研究了Co掺杂量对La_0.8Sr_0.2MnO₃(LSMO)多晶样品的类Griffiths相、磁熵变、临界行为和电输运性质的影响。研究结果表明: 制备的多晶样品均具有菱形对称结构; 三样品在低温磁转变温度(T_C2)以上均存在类Griffiths相; La_0.8Sr_0.2Mn_1-xCo_xO₃(x = 0, 0.1, 0.3)样品外加磁场为7 T的最大磁熵变ΔS_max分别为-2.28、-2.05和-2.75 J/(kg·K), Co元素的掺杂使得ΔS_max先减小后增大; 母相的临界行为与平均场模型拟合得最好, 掺杂后样品的临界行为和3D海森伯模型拟合最好; 母相为半导体材料, Co元素掺杂量达到0.1时在低温磁转变温度(T_C2)附近出现金属绝缘体转变; 高温区三样品的导电方式均满足小极化子模型。     

应力对蓝宝石衬底上生长二氧化钒薄膜结构和光电性能的调控

利用脉冲激光沉积技术在蓝宝石衬底上生长不同厚度的VO₂薄膜, 对薄膜的结构、表面形貌和光电性能进行研究。结果表明: 所沉积的VO₂薄膜为具有单晶性能、表面平整的单斜晶相的VO₂薄膜, 相变前后, 方块电阻的变化可达到3~4个数量级, 在波长为2500 nm的透过率变化最高可达56%, 优化的可视透过率(T_lum)和太阳能调节率( ∆T_sol )为43.2%和8.7%。薄膜受到的应力对VO₂薄膜有重要影响, 可以通过调节薄膜的厚度对VO₂薄膜光电性能实现调控。当VO₂薄膜厚度较小时, 薄膜受到拉应力, 拉应力能使相变温度显著降低, 金属-绝缘体转变性能(MIT)不但与载流子浓度的变化相关, 而且还受载流子迁移率变化的影响;当VO₂薄膜厚度较大时, 薄膜受到压应力, VO₂薄膜的相变温度接近块体VO₂的相变温度, MIT转变主要来自于载流子浓度在相变前后的变化, 其载流子迁移率几乎不变。     

脉冲激光沉积生长单相的Nd_(1.85)Ce_(0.15)CuO_4薄膜及其激光感生热电电压效应

采用脉冲激光沉积(PLD)技术,在SrTiO3单晶衬底表面外延生长单相的1.85 Ce0.15 CuO4(NCCO)薄膜,并首次在斜切衬底上生长的NCCO薄膜中探测到激光感生热电电压(LITV)信号.实验研究表明,在低沉积温度、高沉积氧压和较大的激光脉冲重复频率下生长的NCCO薄膜中存在Nd1-xCexO<<1.75>,(NCO)杂相,是由于衬底表面吸附粒子扩散迁移困难所致;而高温下真空退火导致杂相的产生,则与NCCO的结构相变引起的热分解有关.通过提高沉积温度、降低沉积氧压和激光脉冲重复频率、并采用低温(T≤800℃)真空退火的方式,可以抑制杂相的形成.制备得到的单相的NCCO外延薄膜是一种新型的原子层热电堆材料,能量为1mJ的紫外脉冲激光的辐照,可以在倾斜的NCCO薄膜中诱导产生0.8V的LITV信号.     

高分子辅助沉积法制备LaNiO3外延导电薄膜

近年来LaNiO₃(LNO)作为铁电超晶格、超导异质结和催化剂材料引起了广泛关注。本研究采用简便、低成本的高分子辅助沉积法(Polymer Assisted Deposition, PAD), 在(001)取向的SrTiO₃(STO)单晶衬底上制备了导电性能优异的LNO外延薄膜, 并对其进行各种结构和电学表征。摇摆曲线半高宽为0.38°, 表明LNO薄膜结晶度良好。高分辨XRD的φ扫描进一步证实LNO薄膜在STO衬底上异质外延生长。原位变温XRD测试进一步表征了LNO薄膜的外延生长过程。结果表明, 聚合物分解之后金属阳离子在单晶基体上有序释放并外延结晶。XPS结果表明, 采用PAD制备的LaNiO₃薄膜不存在氧空位。薄膜表面光滑, 粗糙度为0.67 nm。在10~300 K温度区间内的变温电阻率表明LNO薄膜具有良好的导电性能。上述结果表明：PAD制备的LaNiO₃薄膜具有较好的综合性能, PAD在制备外延功能薄膜材料方面具有很大的潜力。     

无容器制备Er3+/Yb3+共掺La2O3-TiO2-ZrO2玻璃及其上转换发光研究

利用无容器技术制备了(La_0.94-xEr_0.06Yb_x)(Ti_0.95Zr_0.05)_2.25O₆(x=0~0.24, 间隔0.04)球状透明玻璃, 其稀土离子掺杂浓度最大值达到30%。通过DTA分析发现, 玻璃具有很好的热稳定性, x=0时玻璃化转变温度T_g和析晶起始温度T_o分别为818℃和906℃, ΔT(ΔT= T_o-T_g)为88℃, 玻璃形成能力较低。随着Yb³⁺浓度提高, T_g、T_o和ΔT逐渐下降, 说明Yb³⁺降低了玻璃的热稳定性和形成能力。利用紫外可见分光光度计测定了样品的吸收/透过光谱, 玻璃在975 nm具有很强的吸收峰, 表明Yb³⁺可以有效提高玻璃对入射光的吸收强度; 在可见光范围内除特征吸收外具有近70%的透过率, 说明玻璃具有良好的透可见光性能, 有望获得高强上转换发光输出。上转换荧光光谱研究表明: 在980 nm激光泵浦下, 获得了中心位于535、554和672 nm处的绿、红发光带, x=0.16的发光最强, 672 nm处的红光强度是x=0的近130倍。上转换发光强度与泵浦功率关系的分析表明: 535、554 nm处的绿光和672 nm处的红光发光均是双光子发光过程。     

残余应力对SrRuO3薄膜磁学及电输运性能的影响

采用射频磁控溅射法在单晶SrTiO₃ (STO)衬底和硅(Si)衬底上制备出不同取向的SrRuO₃ (SRO)薄膜, 对薄膜的残余应力进行了分析, 并研究了应力对不同取向SRO薄膜磁学性能与电输运特性的影响。根据X射线衍射(XRD)结果分析可知, Si基SRO薄膜为多晶单轴取向薄膜, 且应力来源主要为热失配拉应力; STO基SRO薄膜为外延薄膜, 其应力主要为热失配压应力和外延压应力; 磁学性能测试表明, (001)取向SRO薄膜比(110)取向薄膜拥有更高的居里温度T_C; 压应力提高了(001)取向SRO薄膜的T_C, 却降低了(110)取向薄膜的T_C。电阻性能测试表明, 对于在同种类型衬底上沉积的SRO薄膜, (001)取向的薄膜的剩余表面电阻比(RRR)高于(110)取向的薄膜。另外, 拉应力引起了薄膜微结构的无序度增加, 弱化了表面电阻率的温度依赖性, 提高了金属绝缘体转变温度(T_MI)。     

脉冲激光沉积法在Si(111)衬底上生长高c轴取向LiNbO3薄膜

在氧压20Pa,衬底温度600℃,靶材与衬底距离4cm的最优化条件下,利用脉冲激光沉积(PLD)技术首次在无诱导电压和任何缓冲层的情况下,在单晶Si(111)衬底上生长具有优良结晶品质和高c轴取向的LiNbO3晶体薄膜.利用X射线衍射(XRD)、扫描电子显微镜(SEM)和原子力显微镜(AFM)对LiNbO3薄膜的结晶品质,择优取向性以及表面形貌进行了系统的分析.结果表明生长出了具有优异晶体质量的c轴取向LiNbO3薄膜,表面光滑平整且无裂纹产生,表面粗糙度约4.8nm,有利于硅基光电子器件的制备和利用.     

偏轴磁控溅射法外延BiFeO3薄膜的介电性能与阻变效应

利用偏轴射频磁控溅射法, 在(001) SrTiO₃(STO)单晶基片上制备了Pt/BiFeO₃/La_0.5Sr_0.5CoO₃/STO (Pt/BFO/ LSCO/STO)异质结电容器。研究了BiFeO₃薄膜的结构和物理性能。原子力显微镜(AFM)和X射线衍射(XRD)分析表明: BFO薄膜结晶质量良好, 且为单相(00l)外延钙钛矿结构。介电性能测试结果发现: 在5 V驱动电压下, Pt/BFO/LSCO电容器呈现饱和的蝶形回线, 调谐率和介电损耗分别为14.1%和0.19。此外, 阻变机制研究表明: 在0→5→0 V正向电压和0→-5→0 V负向电压下, 阻变均为高阻向低阻转变规律, 呈现为铁电二极管的阻变开关行为。通过I-V曲线拟合, 得到0→5→0→-5 V时阻变机制为空间电荷限制电流陷阱能级的填充和脱陷, 而-5→0 V时符合界面限制的F-N隧穿机制。     

温度控制织构金属基带上YBCO外延薄膜生长及缺陷研究

采用直流溅射法在Y₂O₃/YSZ/CeO₂(YYC)缓冲层的织构NiW基带上, 通过基片温度调制YBa₂Cu₃O_7-δ(YBCO)外延薄膜生长。X射线衍射仪(XRD)表征显示, 基片温度强烈地影响YBCO薄膜的外延生长: 在较低的基片温度下薄膜趋于a轴取向生长, 随基片温度升高薄膜逐渐变为纯c轴取向生长。由于a轴晶粒引起的大角度晶界会阻碍超导电流在a-b面内的传输, 因此YBCO薄膜的微观结构和超导电性能随温度升高而得到改善, 但是随着基片温度继续升高, 基带的氧化程度加剧, YBCO与缓冲层间发生界面反应, 从而导致薄膜质量衰退。本     

PLZST陶瓷衬底上La0.7Sr0.3MnO3薄膜生长及其磁性能和电输运特性研究

采用磁控溅射法在PLZST陶瓷衬底上制备了不同厚度的LSMO薄膜, 并对其微结构、磁性能及电输运特性进行了研究。结果表明, LSMO薄膜具有单一钙钛矿结构, 晶粒均匀, 表面平整, 其中20 nm厚LSMO薄膜粗糙度仅为2.93 nm。在10~300 K温度范围内, LSMO薄膜均具有大的磁电阻效应, 20 nm厚的LSMO薄膜磁电阻温度稳定性优异。随着薄膜厚度的增加, 薄膜的居里温度、金属绝缘体转变温度、磁化强度和导电性能降低。这可能是由于Pb、Sn、Zr等离子扩散进入LSMO薄膜中, 导致MnO₆八面体畸变造成的。     

Investigation of the Effect of Microstructure and Grain Boundaries in Nanostructured CMR Thin Films Using Scanning Tunneling Microscopy (STM) and Local Conductance Map (LCMAP)

We have investigated the spatially resolved local electronic properties of a nanostructured film of a colossal magnetoresistive (CMR) material by local conductance mapping (LCMAP) using a variable temperature scanning tunneling microscope (STM) operating in a magnetic field. The nanostructured thin films (thickness ap500 nm) of the CMR material La_0.67Sr_0.33MnO₃ (LSMO) on silicon substrates were prepared using chemical solution deposition (CSD) process. These films have a large density of natural incoherent grain boundaries (GBs) which leads to significantly different behavior compared to oriented and epitaxial films of the same composition. Due to the presence of the GBs, these films show substantial low field magnetoresistance (LFMR) followed by a slower and almost linear decrease at higher fields and this is found to be strictly dependent on particle size. Most of the mechanisms proposed to explain the LFMR in the GB are based on tunneling through the GB. The purpose of this study is to use different STM based techniques to image these inhomogeneities and quantify them to the extent possible. In particular, we study the effect of grain size and the grain boundaries and their role in the electrical transport in nanostructured films of CMR materials     

Structure and electrical properties of (100)-oriented Pb(Zn1/3Nb2/3)O3–Pb(Mg1/3Nb2/3)O3–PbTiO3 thin films on La0.7Sr0.3MnO3 electrode by chemical solution deposition

(100)-oriented 0.462Pb(Zn_1/3Nb_2/3)O₃–0.308Pb(Mg_1/3Nb_2/3)O₃–0.23PbTiO₃ (PZN-PMN-PT) perovskite ferroelectric thin films were prepared on La_0.7Sr_0.3MnO₃/LaAlO₃ (LSMO/LAO) substrate via a chemical solution deposition route. The perovskite LSMO electrode was found to effectively suppress the pyrochlore phase while promote the growth of the perovskite phase in the PZN-PMN-PT film. The film annealed at 700 °C exhibited a high dielectric constant of 2130 at 1 kHz, a remnant polarization, 2P_r, of 29.8 μC/cm², and a low leakage current density of 7.2 × 10^− 7 A/cm² at an applied field of 200 kV/cm. The ferroelectric polarization was fatigue-free at least up to 10¹⁰ cycles. Piezoelectric coefficient, d₃₃, of 48 pm/V was also demonstrated. The results showed that much superior properties could be achieved with the PZN-PMN-PT thin films on the solution derived LSMO electrode than on Pt electrode by sputtering.     

Pulsed laser deposition of La0.67Ca0.33MnO3 thin films on LiNbO3 and surface acoustic wave studies

Surface Acoustic Waves on piezoelectric substrates can be used to investigate the dynamic conductivity of thin films in a non-contact and very sensitive way, especially at low conductivities. Here, we report on such surface acoustic wave studies to characterize thin manganite film like La_0.67Ca_0.33MnO₃, exhibiting a Jan Teller effect with a strong electron phonon interaction and a metal insulator transition at high temperatures.

We report on the deposition of La_0.67Ca_0.33MnO₃ on piezoelectric substrates (LiNbO₃ in different crystal cuts, employing a pulsed laser deposition technique. The structural quality of the thin films are examined by X-Ray Diffraction, Scanning Electron Microscope and Energy Dispersive X-ray spectroscopy. For the electrical characterization, we employ the surface acoustic wave technique, accompanied by conventional direct current resistance measurements for comparison.     

Application of pulsed liquid-injection MOCVD to the growth of ultrathin epitaxial oxides for magnetic heterostructures

We illustrate the capabilities of pulsed-liquid injection metal–organic chemical vapor deposition in the nano-engineering of complex oxides with results obtained on (La_0.7Sr_0.3MnO₃/SrTiO₃)₁₅ (LSMO/STO) superlattices. Superlattices with ultrathin films of a few monolayers have been successfully prepared, as shown by synchrotron radiation diffraction experiments. Laue oscillations were observed between the satellite peaks, indicating a smooth upper surface. Sets of superlattices with varying LSMO or STO thickness were synthesized on different substrates (LaAlO₃, SrTiO₃, MgO). By varying the relative thickness of each compound and changing the substrate, the strain in the stackings could be changed.     

Fabrication and Optical Properties of Pb(Mg/sub 1/3/Nb/sub 2/3/)O/sub 3/-PbTiO/sub 3/Thin Films on Si Substrates Using the PLD Method

Epitaxial 0.67Pb(Mg_1/3Nb_2/3)O₃-0.33PbTiO₃ (PMN-PT) thin films with electro-optic effects were fabricated on (La_0.5Sr_0.5)CoO₃(LSCO)/CeO₂/YSZ-buffered Si(001) substrates using double-pulse excitation pulsed laser deposition (PLD) method with a mask placed between the target and the substrate. Epitaxial growth of PMN-PT thin films was undertaken using the two-step growth method of PMN-PT film. The PMN-PT seed layer was deposited at 500degC on the LSCO/CeO₂/YSZ/Si, which temperature was the same as that used for LSCO deposition. The PMN-PT thin films were deposited on the PMN-PT seed layer at 600degC, which enables growth of high-crystallinity PMN-PT films with smooth surfaces. We obtained optimum fabrication conditions of PMN-PT film with micrometer-order thickness. Resultant films showed high crystallinity with full width at half maximum (FWHM)=0.73 deg and 1.6 mum thickness. Electro-optic properties and the refractive index value were measured at 633 nm wavelength using the prism coupling method. The obtained refractive index was 2.59. The electro-optic coefficients r₁₃ and r₃₃ were determined by applying the electrical field between a semitransparent, thin top electrode of Pt and a bottom LSCO electrode. The electro-optic coefficient was r₁₃=17 pm/V at transverse electric field (TE) mode and r₃₃=55 pm/V at transverse magnetic field (TM) mode.     

Linearly shifting ferromagnetic resonance response of La0.7Sr0.3MnO3 thin film for body temperature sensors

Human body temperature not only reflects vital signs, but also affects the state of various organs through blood circulation, and even affects lifespan. Here a wireless body temperature detection scheme was presented that the temperature was extracted by investigating the out-of-plane (OP) ferromagnetic resonance (FMR) field of 10.2 nm thick La_0.7Sr_0.3MnO₃ (LSMO) film using electron paramagnetic resonance (EPR) technique. Within the range of 34–42 °C, the OP FMR field changes linearly with the increasing or decreasing temperature, and this variation comes from the linear responses of magnetization to the fluctuant temperature. Using this method, a tiny temperature change (<0.1 °C) of organisms can be detected accurately and sensitively, which shows great potential in body temperature monitoring for humans and mammals.     

Spin-dependent tunnelling in La0.7Sr0.3MnO3/SrTiO3 superlattices

La_0.7Sr_0.3MnO₃ is predicted to show half-metallic behaviour at low temperature, which gives rise to a metallic character for one spin direction and an insulating character for the other. This 100% polarisation of the conduction band should enhance the spin dependent tunnelling in manganite-based tunnel junctions. La_0.7Sr_0.3MnO₃/SrTiO₃ epitaxial superlattices were grown on LaAlO₃(001) substrates by metal–organic chemical vapour deposition (MOCVD). These multilayers consist of 15 epitaxial bilayers of La_0.7Sr_0.3MnO₃ and SrTiO₃. The junctions were patterned using UV lithography and Ar ion milling to carry out transport measurements in the current perpendicular-to-plane geometry (CPP). A temperature-independent non-linear I–V curve, which is characteristic of a tunnelling conduction mechanism, was observed below 50 K. At higher temperatures, the I–V curves are found to become linear and temperature-dependent. Up to 30 K, a constant tunnel magnetoresistance (TMR) (3%) is measured. The switching field is consistent with the film coercive field (a few 10s of mT). At higher temperatures, the TMR decreases rapidly. This temperature dependence is compared to the expected behaviour of a spin tunnel junction with half-metallic electrodes, with thermal activation or the loss of spin polarisation taken into account.     

Electrical transport and magnetic properties in La0.67Ca0.33MnO3 and CuFe2O4 composites

The (1 − x) La_0.67Ca_0.33MnO₃/xCuFe₂O₄ (x = 0, 0.04, 0.07, 0.10 and 0.15) composites have been prepared and investigated systematically for their microstructure, electrical and magnetic properties. The X-ray diffraction and scanning electronic microscopy analysis reveal that both La_0.67Ca_0.33MnO₃ (LCMO) and CuFe₂O₄ phases are distributed in the composites. Compared with pure LCMO, an obvious enhancement of magnetoresistance is observed over a wide temperature range for the composites. Under 3 T field, the magnetoresistance rises from a base value 44.5% for pure LCMO, to a maximum value of 66.7% for x = 0.1 composite. Meanwhile, a weak temperature-dependent MR platform is observed in the temperature range from 210 K to 240 K. The MR enhancement is discussed in terms of spin-polarized intergrain tunneling due to enhanced magnetic disorder and magnetic coupling near boundaries between LCMO and CuFe₂O₄ grains.