Annealing effects on structure and laser-induced damage threshold of Ta2O5/SiO2 dielectric mirrors

The effects of annealing on structure and laser-induced damage threshold (LIDT) of Ta₂O₅/SiO₂ dielectric mirrors were investigated. Ta₂O₅/SiO₂ multilayer was prepared by ion beam sputtering (IBS), then annealed in air under the temperature from 100 to 400 °C. Microstructure of the samples was characterized by X-ray diffraction (XRD). Absorption of the multilayer was measured by surface thermal lensing (STL) technique. The laser-induced damage threshold was assessed using 1064 nm free pulsed laser at a pulse length of 220 μs.

It was found that the center wavelength shifted to long wavelength gradually as the annealing temperature increased, and kept its non-crystalline structure even after annealing. The absorbance of the reflectors decreased after annealing. A remarkable increase of the laser-induced damage threshold was found when the annealing temperature was above 250 °C.     

Defect versus nanocrystal luminescence emitted from room temperature and hot-implanted SiO2 layers

Silicon nanocrystals have been synthesized in SiO₂ matrix using Si ion implantation. Si ions were implanted into 300-nm-thick SiO₂ films grown on crystalline Si at energies of 30–55 keV, and with doses of 5×10¹⁵, 3×10¹⁶, and 1×10¹⁷ cm⁻². Implanted samples were subsequently annealed in an N₂ ambient at 500–1100°C during various periods. Photoluminescence spectra for the sample implanted with 1×10¹⁷ cm⁻² at 55 keV show that red luminescence (750 nm) related to Si-nanocrystals clearly increases with annealing temperature and time in intensity, and that weak orange luminescence (600 nm) is observed after annealing at low temperatures of 500°C and 800°C. The luminescence around 600 nm becomes very intense when a thin SiO₂ sample is implanted at a substrate temperature of 400°C with an energy of 30 keV and a low dose of 5×10¹⁵ cm⁻². It vanishes after annealing at 800°C for 30 min. We conclude that this luminescence observed around 600 nm is caused by some radiative defects formed in Si-implanted SiO₂.     

The effects of substrate temperature on the superconducting properties of Tl2Ca2Ba2Cu3O10 films sputter-deposited from stoichiometric oxide targets

The annealing characteristics and the superconducting properties of Tl₂Ca₂Ba₂Cu₃O₁₀ thin films sputter-deposited onto yttrium- stabilized ZrO₂ substrate at up to 500°C from two stoichiometric oxide targets are reported. The films deposited at 400–500°C were found to require a lower post-annealing temperature than the films deposited at lower temperatures to attain the highest T_c superconducting state, due to a more pronounced Ba diffusion toward the substrate as indicated by their secondary ion mass spectrometry depth profiles. The highest T_c achieved tends to degrade with increasing substrate temperatures, a zero resistance T_c of 121 and ≈90 K, respectively, being observed for the films deposited at -ambient temperature and at 500°C. The formation of the highest T_c phase (Tl₂Ca₂Ba₂Cu₃O₁₀) generally is associated with a sheet type of crystal growth morphology with smooth and aligned surfaces which can be obtained only from the films capable of sustaining prolonged annealing at 900°C. Annealing at lower temperatures (≈860°C) results in the formation of rod or sphere type of morphologies with rough and randomly oriented crystals and the lower T_c phases such as Tl₂Ca₁Ba₂Cu₂O₈.     

Structure and optical properties of sol–gel derived Gd2O3 waveguide films

Pure and rare earth doped gadolinium oxide (Gd₂O₃) waveguide films were prepared by a simple sol–gel process and dip-coating method. Gd₂O₃ was successfully synthesized by hydrolysis of gadolinium acetate. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) were used to study the thermal chemistry properties of dried gel. Structure of Gd₂O₃ films annealed at different temperature ranging from 400 to 750 °C were investigated by Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results show that Gd₂O₃ starts crystallizing at about 400 °C and the crystallite size increases with annealing temperature. Oriented growth of (4 0 0) face of Gd₂O₃ has been observed when the films were deposited on (1 0 0) Si substrate and annealed at 750 °C. The laser beam (λ=632.8 nm) was coupled into the film by a prism coupler and propagation loss of the film measured by scattering-detection method is about 2 dB/cm. Luminescence properties of europium ions doped films were measured and are discussed.     

Growth of β-MnO2 films on TiO2(110) by oxygen plasma assisted molecular beam epitaxy

We have used oxygen plasma assisted MBE to grow epitaxial films of pyrolusite (β-MnO₂) on TiO₂(110) for thicknesses of one to six bilayers (BL). We define a bilayer to be a layer of Mn and lattice O and an adjacent layer of bridging O within the rutile structure. The resulting surfaces have been characterized in situ by reflection high-energy electron diffraction, low-energy electron diffraction, X-ray photoelectron spectroscopy and diffraction, and atomic force microscopy. Well-ordered, pseudomorphic overlayers form for substrate temperatures between 400 and 500°C. Mn–Ti intermixing occurs over the time scale of film growth (1 BL/min) for substrate temperatures in excess of 500°C. Films grown at 400–500°C exhibit island growth, whereas intermixed films grown at temperatures of 500–600°C are more laminar. 1 BL films grown at 450°C are more laminar than multilayer films grown at the same temperature, and form a well-ordered surface cation layer of Mn on the rutile structure with at most 10% indiffusion to the second cation layer.     

ZrB2-based Ohmic contacts to p-GaN

The annealing temperature dependence of contact resistance and layer stability of ZrB₂/Ti/Au and Ni/Au/ZrB₂/Ti/Au Ohmic contacts on p-GaN is reported. The as-deposited contacts are rectifying and transition to Ohmic behavior for annealing at ≥750 °C, a significant improvement in thermal stability compared to the conventional Ni/Au Ohmic contact on p-GaN, which is stable only to <600 °C. A minimum specific contact resistance of ∼2 × 10⁻³ Ω cm⁻² was obtained for the ZrB₂/Ti/Au after annealing at 800 °C while for Ni/Au/ZrB₂/Ti/Au the minimum value was 10⁻⁴ Ω cm⁻² at 900 °C. Auger Electron Spectroscopy profiling showed significant Ti, Ni and Zr out diffusion at 750 °C in the Ni/Au/ZrB₂/Ti/Au while the Ti and Zr intermix at 900 °C in the ZrB₂/Ti/Au. These boride-based contacts show promise for contacts to p-GaN in high temperature applications.     

Synthesis and physical behaviour of In2S3 films

In₂S₃ layers have been grown by close-spaced evaporation of pre-synthesized In₂S₃ powder from its constituent elements. The layers were deposited on glass substrates at temperatures in the range, 200–350 °C. The effect of substrate temperature on composition, structure, morphology, electrical and optical properties of the as-grown indium sulfide films has been studied. The synthesized powder exhibited cubic structure with a grain size of 63.92 nm and S/In ratio of 1.01. The films grown at 200 °C were amorphous in nature while its crystallinity increased with the increase of substrate temperature to 300 °C. The films exhibited pure tetragonal β-In₂S₃ phase at the substrate temperature of 350 °C. The surface morphological analysis revealed that the films grown at 300 °C had an average roughness of 1.43 nm. These films showed a S/In ratio of 0.98 and a lower electrical resistivity of 1.28 × 10³ Ω cm. The optical band gap was found to be direct and the layers grown at 300 °C showed a higher optical transmittance of 78% and an energy band gap of 2.49 eV.     

Use of TiB2 diffusion barriers for Ni/Au ohmic contacts on p-GaN

The use of a TiB₂ diffusion barrier for Ni/Au contacts on p-GaN is reported. The annealing temperature (25-950 °C) dependence of ohmic contact characteristics using a Ni/Au/TiB₂/Ti/Au metallization scheme deposited by sputtering were investigated by contact resistance measurements and auger electron spectroscopy (AES). The as-deposited contacts are rectifying and transition to ohmic behavior for annealing at ≥500 °C . A minimum specific contact resistivity of ∼3 × 10⁻⁴ Ω cm⁻² was obtained after annealing over a broad range of temperatures (800-950 °C for 60 s). The contact morphology became considerably rougher at the higher end of this temperature range. AES profiling showed significant Ti and Ni outdiffusion through the TiB₂ at 800 °C. By 900 °C the Ti was almost completely removed to the surface, where it became oxidized. Use of the TiB₂ diffusion barrier produces superior thermal stability compared to the more common Ni/Au, whose morphology degrades significantly above 500 °C.     

The effect of annealing under hydrostatic pressure on the visible photoluminescence from si-ion implanted SiO2 films

We have studied the influence of the hydrostatic pressure during annealing on the intensity of the visible photoluminescence (PL) from thermally grown SiO₂ films irradiated with Si⁺ ions. Post-implantation anneals have been carried out in an Ar ambient at temperatures T_a of 400°C and 450°C for 10 h and 1130°C for 5 h at hydrostatic pressures of 1 bar–15 kbar. It has been found that the intensity of the 360, 460 and 600 nm PL peaks increases with rising hydrostatic pressure during low-temperature annealing. The intensity of the short-wavelength PL under conditions of hydrostatic pressure continues to rise even at T_a=1130°C. Increasing T_a leads to a shift in the PL spectra towards the ultraviolet range. The results obtained have been interpreted in terms of enhanced, pressure-mediated formation of ≡Si–Si≡ centres and small Si clusters within metastable regions of the ion-implanted SiO₂.     

Electrode contact study for SiGe thin film operated at high temperature

A study on the electrode contact of the sputtered SiGe thin film is reported for application of devices working at high temperature. Surface morphological characterization with optical microscope and AFM (atomic force microscope) together with the electrical characterization by TLM measurements (transmission line method) were performed before and after aging at 500 °C for 24 h using various sputtered multilayer electrodes, Ti/Au/Ti, Ta/Pt/Ta and Ti/Pt/Ti, on 300-nm B-doped SiGe thin film deposited by magnetron sputtering and furnace crystallisation at high temperature. After aging at 500 °C for 24 h, the Ti/Au/Ti multilayer electrodes seriously degraded to be non-ohmic contact, showing rough surface morphology. The Ti/Pt/Ti metal layers showed the lowest specific contact, resistivity before and after aging, 1.46 × 10⁻³ Ω cm² and 1.68 × 10² Ω cm² respectively.     

Superconducting Nd1.85Ce0.15CuO4 films grown by the pulsed electron deposition technique

Nd_1.85Ce_0.15CuO_4−δ superconducting thin films were prepared on (1 0 0) SrTiO₃ substrates by pulsed electron deposition technique without reducing atmosphere. Oxygen content is finely controlled by high temperature vacuum annealing, and optimal superconductivity has been obtained. The deposition conditions of the film are discussed in details. Higher deposition temperature and lower gas pressure result in the loss of copper and the appearance of the foreign phase Ce_0.5Nd_0.5O_1.75. High quality Nd_1.85Ce_0.15CuO_4−δ epitaxial films are deposited at 840–870 °C in the mixed gas with a ratio of O₂:Ar = 1:3.     

Effects of substitution of Ti for Fe in BiFeO3 films prepared by sol–gel process

Ti substituted BiFe_1−xTi_xO_3+δ films have been prepared on indium–tin oxide (ITO)/glass substrates by the sol–gel process. The films with x=0.00–0.20 were prepared at an annealing temperature of 600 °C. X-ray diffraction patterns indicate that all films adopt R3m structure and the films with x=0 and 0.10 show pure perovskite phase. Cross-section scanning shows the thickness of the films is about 300 nm. Through 0.05 Ti substitution, the 2P_r increases to 8.30 μC/cm² from 2.12 μC/cm² of the un-substituted BiFeO₃ film and show enhanced ferroelectricity at room temperature. The 2P_r values are 2.63 and 0.44 μC/cm² for the films with x=0.01 and 0.2, respectively. Moreover, the films with x=0.05 and 0.10 show enhanced dielectric property since the permittivity increases near 150 at the same measuring frequency. Through the substitution of Ti, the leakage conduction is reduced for the films with x=0.05–0.20.     

Fabrication of p-Si/β-FeSi2 balls/n-si structures by MBE and their electrical and optical properties

We report on the formation technique of single-crystalline β-FeSi₂ balls (<100 nm) embedded in a Si p–n junction region by Si molecular beam epitaxy (MBE). β-FeSi₂ films grown on Si (0 0 1) by reactive deposition epitaxy (RDE) aggregated into islands after annealing at 850°C in ultrahigh vacuum. The islands of β-FeSi₂ aggregated further into a ball shape by following the Si MBE overgrowth at 750°C. It was found from X-ray diffraction (XRD) patterns that the epitaxial relationship between the two materials, and single-crystalline nature were preserved even after the annealing and the Si overgrowth. Capacitance–voltage (C–V) characteristics and transmission electron microscope (TEM) images revealed that a lot of defects were introduced around the embedded β-FeSi₂ balls with an increase of embedded β-FeSi₂ quantity.     

Solid-phase epitaxy of CaSi2 on Si(1 1 1) and the Schottky-barrier height of CaSi2/Si(1 1 1)

Thin Ca films were evaporated on Si(1 1 1) under UHV conditions and subsequently annealed in the temperature range 200–650 °C. The interdiffusion of Ca and Si was examined by ex situ Auger depth profiling. In situ monitoring of the Si 2p core-level shift by X-ray photoemission spectroscopy (XPS) was employed to study the silicide formation process. The formation temperature of CaSi₂ films on Si(1 1 1) was found to be about 350 °C. Epitaxial growth takes place at T≥400 °C. The morphology of the films, measured by atomic force microscopy (AFM), was correlated with their crystallinity as analyzed by X-ray diffraction (XRD). According to measurements of temperature-dependent I–V characteristics and internal photoemission the Schottky-barrier height of CaSi₂ on Si(1 1 1) amounts to qΦ_Bn=0.25 eV on n-type and to qΦ_Bp=0.82 eV on p-type silicon.     

The influence of different fabrication processes on characteristics of excess Bi2O3-doped 0.95 (Na0.5Bi0.5)TiO3–0.05 BaTiO3 ceramics

In this study, we will develop the influences of the excess x wt% (x=0, 1, 2, and 3) Bi₂O₃-doped and the different fabricating process on the sintering and dielectric characteristics of 0.95 (Na_0.5Bi_0.5)TiO₃–0.05 BaTiO₃ ferroelectric ceramics with the aid of SEM and X-ray diffraction patterns, and dielectric–temperature curves. The 0.95 (Na_0.5Bi_0.5)TiO₃–0.05 BaTiO₃+x wt% Bi₂O₃ ceramics are fabricated by two different processes. The first process is that (Na_0.5Bi_0.5)TiO₃ composition is calcined at 850 °C and BaTiO₃ composition is calcined at 1100 °C, then the calcined (Na_0.5Bi_0.5)TiO₃ and BaTiO₃ powders are mixed in according to 0.95 (Na_0.5Bi_0.5)TiO₃–0.05 BaTiO₃+x wt% Bi₂O₃ compositions. The second process is that the raw materials are mixed in accordance to the 0.95 (Na_0.5Bi_0.5)TiO₃–0.05 BaTiO₃+x wt% Bi₂O₃ compositions and then calcining at 900 °C. The sintering process is carried out in air for 2 h from 1120 to 1240 °C. After sintering, the effects of process parameters on the dielectric characteristics will be developed by the dielectric–temperature curves. Dielectric–temperature properties are also investigated at the temperatures of 30–350 °C and at the frequencies of 10 kHz–1 MHz.     

低接触电阻率Ni/Ag/Ti/Au反射镜电极的研究

研究了Ag的厚度、退火时间、沉积温度对于Ni/Ag/Ti/Au电极的反射率及与p-GaN欧姆接触性能的影响. 利用分光光度计测量反射率, 采用圆形传输线模型计算比接触电阻率. 结果表明: 随着Ag厚度的增加, Ni/Ag/Ti/Au电极的反射率逐渐增大; 在氧气氛围中, 随着退火时间从1 min增至10 min, 300 ℃退火时, 比接触电阻率持续下降, 而对于400-600 ℃退火, 比接触电阻率先减小后增大; 在300和400 ℃氧气中进行1-10 min 的退火后, Ni/Ag/Ti/Au的反射率变化较小, 退火温度高于400 ℃时, 随着退火时间的增加, 反射率急剧下降; 在400 ℃氧气中3 min退火后, 比接触电阻率可以达到3.6×10^-3 Ω·cm². 此外, 适当提高沉积温度可以增加Ni/Ag/Ti/Au的反射率并降低比接触电阻率, 沉积温度为120 ℃条件下的Ni/Ag/Ti/Au电极在450 nm处反射率达到90.1%, 比接触电阻率为6.4×10^-3 Ω·cm². 综合考虑电学和光学性能, 在沉积温度为120 ℃下蒸镀Ni/Ag/Ti/Au (1/200/100/100 nm)并在400 ℃氧气中进行3 min退火可以得到较优化的电极. 利用此电极制作的垂直结构发光二极管在350 mA电流下的工作电压为2.95 V, 输出光功率为387.1 mW, 电光转换效率达到37.5%.     

Low specific contact resistivity to graphene achieved by AuGe/Ni/Au and annealing process

Low metal-graphene contact resistance is important in making high-performance graphene devices.In this work,we demonstrate a lower specific contact resistivity of Au_(0.88)Ge_(0.12)/Ni/Au-graphene contact compared with Ti/Au and Ti/Pt/Au contacts.The rapid thermal annealing process was optimized to improve AuGe/Ni/Au contact resistance.Results reveal that both pre- and post-annealing processes are effective for reducing the contact resistance.The specific contact resistivity decreases from 2.5 × 10~(-4) to 7.8 × 10~(-5) Ω·cm~2 by pre-annealing at 300 ℃ for one hour,and continues to decrease to9.5 × 10~(-7) H·cm~2 after post-annealing at 490 ℃ for 60 seconds.These approaches provide reliable means of lowering contact resistance.     

Ellipsometric spectroscopy study of photoluminescent Si/SiO2 systems obtained by magnetron co-sputtering

Si nanograins embedded in silica matrix were obtained by magnetron cosputtering of both Si and SiO₂ at different substrate temperature (200–700°C) and thermal annealing at 1100°C. The samples were characterized by ellipsometric spectroscopy, high-resolution electron microscopy observations and photoluminescence. The highest excess of Si atoms was found to be incorporated for deposition temperature near 400–500°C, giving rise to a maximum PL and a shift of the peak position towards lower energy. These features might be interpreted in terms of quantum size effects and of density of grains, even though the interface states seem to be involved in the improvement of the photoluminescence efficiency.     

Effect of Cu doping in MgB2 superconductor at various processing temperatures

The effects of Cu doping in MgB₂ superconductor has been studied at different processing temperatures. The polycrystalline samples of Mg_1−xCu_xB₂ with x = 0.05 were synthesized through the in-situ solid sate reaction method in argon atmosphere at different temperature range between 800–900 °C. The samples were characterized through X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and low temperature R–T measurement techniques for the phase verification, microstructure and superconducting transition temperature, respectively. The XRD patterns of Mg_1−xCu_xB₂ (x = 0.05) do not exhibit any impurity traces of MgB₄ or MgB₆ and they show the sharp transition in the samples prepared at 850 °C. The onset transition temperature of the prepared samples is around 39 K, which is almost the same as that for the pure MgB₂. This indicates that Cu doping in MgB₂ does not affect the transition temperature. The SEM micrograph of Mg_0.95Cu_0.05B₂ has shown that the sample is dense with grain size smaller than 1 μm.     

SiO2 passivation film effects on microwave characteristics of YBa2Cu3O7−x-based resonators

SiO₂ film coated as a passivation layer for YBa₂Cu₃O_7−x (YBCO)-based microwave devices is investigated by measuring the microwave characteristics of microstrip line resonators. The SiO₂ film is deposited with its 0.3 to 0.4 μm thickness by a sputtering method using Ar + 30%O₂ plasma. These deposition conditions do not degrade the microwave characteristics and the critical temperature (T_c). Next, the SiO₂ film coated resonators are compared with the uncoated ones for two kinds of degradation conditions: a 200°C annealing in air, and an exposure to air at 85°C and 85% RH (relative humidity). We find that the SiO₂ passivation film prevents the YBCO thin film from the surface degradation and reacting with water.