直流磁控反应溅射制备IrO2薄膜

为研究氧化依（ＩｒＯ_２）对ＰＺＴ铁电薄膜疲劳性能的影响,利用直流（ＤＣ）磁控反应溅射（ｓｐｕｔｔｅｒｉｎｇ）工艺成功地在ＳｉＯ_２／Ｓｉ（１００）衬底上制得了高度取向的ＩｒＯ_２薄膜．并在其上制成ＰＺＴ铁电薄膜．讨论了溅射参数（溅射功率、 Ａｒ／Ｏ_２比、衬底温度）以及退火条件对氧化铱薄膜的结晶、取向和形态的影响．     

直流磁控反应溅射制备IrO2薄膜

为研究氧化铱（ＩｒＯ２）对ＰＺＴ铁电薄膜疲性能的影响。利用直流（ＤＣ）磁控反应溅射（ｓｐｕｔｔｅｒｉｎｇ）工艺成功地在ＳｉＯ２／Ｓｉ（１００）衬底上制得了高度取向的ＩｒＯ２薄膜,并在其上制成ＰＺＴ铁电薄膜,讨论了溅射参数（溅射功率、Ａｒ／Ｏ２比、衬底温度）以及退火条件对氧化铱薄膜的结晶,取向和形态的影响。     

Preparation of strontium titanate thin films by mirror-confinement-type electron cyclotron resonance plasma sputtering

Using mirror-confinement-type electron cyclotron resonance (ECR) plasma sputtering method, strontium titanate (SrTiO₃) thin films have been prepared on Si and Pt/Ti/SiO₂/Si substrates at a low substrate temperature (below 450 K) in a low pressure (2.7×10⁻² Pa) environment of pure Ar and Ar/O₂ mixture. Prepared film surfaces were very smooth regardless of high deposition rate (8.5 nm/min). The composition ratio Sr/Ti of Sr to Ti in the films varied with the distance between the target and the substrate. All as-deposited films on Si substrates were found to be amorphous and were crystallized by post-deposition annealing using an electric furnace at 650 K, i.e. approximately 250 K lower than annealing for films obtained by conventional RF magnetron sputtering. Post-deposition annealing of these films using millimeter-wave radiation decreased the crystallization temperature to a value of 550 K. Furthermore, all as-deposited films on Pt/Ti/SiO₂/Si substrates by a plasma of Ar and O₂ gas mixture were found to be crystallized regardless of no substrate heating.     

溅射工艺参数对PZT铁电薄膜相变过程的影响

采用射频磁控溅射工艺,在（１１１）Ｐｔ／Ｔｉ／ＳｉＯ２／Ｓｉ衬底上用ＰＺＴ（５３／４７）陶瓷靶制备铁电薄膜。用快速光热退火炉对原位沉积的薄膜进行ＲＴＡ处理。     

Radio frequency sputtered zinc oxide thin films with application to metal-semiconductor-metal photodetectors

Zinc oxide (ZnO) films were successfully deposited on silicon, silicon dioxide, and glass substrates by radio frequency magnetron sputtering at different deposition conditions. Field emission scanning electron microscopy, X-ray photoelectron spectroscopy, transmission and photoluminescence measurements were employed to analyze the effect of the deposition conditions and the postdeposition annealing treatment on the surface morphology, structure, chemical deposition and optical properties of ZnO thin films. It was found that the thickness of ZnO films decreased with increased ratio of oxygen/argon and increased temperature. The crystalline and stoichiometric quality of the film was improved by depositing at high temperature and low pressure. Crystals formed more tightly and uniformly with heat treatment under air ambient. The dark current of the ZnO metal-semiconductor-metal photodetector was reduced from 3.06 μA to 96.5 nA at 5 V after postdeposition annealing when compared with that of as-deposited ZnO. Its magnitude was found to be at least two orders lower than that of the as-deposited sample.     

直流反应溅射TiO2薄膜的制备及其性能研究

采用直流反应磁控溅射的方法,溅射高纯钛靶在ITO石英衬底上制备了TiO2薄膜.用XRD、Raman光谱、AFM和紫外-可见光分光光度计分别测试了TiO2薄膜的结构、表面形貌和紫外-可见光透射谱,研究了工艺因素中溅射气压、氧氩比和退火温度对薄膜结构的影响.采用C(胶)/TiO2/ITO三层结构研究了锐钛矿TiO2薄膜的紫外光响应.实验结果表明较低的溅射气压、合适的氧氩比和较高的退火温度有利于锐钛矿TiO2薄膜的结晶.在2 V的偏压下,锐钛矿TiO2薄膜的紫外光响应上升迟豫时间约为3 s,稳定光电流可达到2.1 mA,对紫外光的灵敏性和稳定的光响应表明TiO2薄膜有可能成为一种新的紫外光探测器材料.     

The tunable amorphous-crystalline transition temperature by indium-doping on GeTe thin films

Amorphous germanium telluride (GeTe) thin films were fabricated on SiO2/Si subtracts by RF sputtering at room temperature. The thickness of the as-deposited films is about 200 nm. Indium-doping on GeTe thin films were prepared by solution doping method. The GeTe thin films were dipped into InCl3 solution with 1 mol/L, 0.8 mol/L, 0.5 mol/L and 0.1 mol/L for an hour at 100 degrees C, respectively. Then the thin films were annealed at 200 degrees C for 10 min. The I-T measurements show that the amorphous-crystalline transition temperature of In-GeTe films is lower than that of the undoped thin films. XRD reveals the formation of rock salt structure after annealing at 280 degrees C. XPS indicates that In-Te bond which may correspond to In2Te3 exists in the doped thin film. The results of calculating density of states (DOS) show that the changes of electronic states are mainly located around Fermi energy level with the increasing Indium content. These results indicate that the transition temperature of GeTe films can be effectively tuned by solution process doping indium, which may be useful to decrease set current.     

Effect of Ar gas pressure on growth, structure, and mechanical properties of sputtered Ti, Al, TiAl, and Ti3Al films

Single layers of Ti, Al, TiAl and Ti₃Al were sputter deposited on to 2″ oxidized Si 111 wafers and 7059 Corning Glass to study the effect of film thickness, temperature, and sputtering gas pressure on the mechanical and physical properties. In the present investigation, sputtering gas pressure was varied from 2 mT to 10 mT. The film thickness was varied from 1000 Å to 2 μm. The as-deposited Ti, Al and Ti₃Al films are well crystallized over the entire thickness range. Ti and Ti₃Al films show preferred orientation in the 0002 direction. On the other hand, Al films are random polycrystalline. TiAl films are nearly amorphous for all the thicknesses under consideration. TiAl films show formation of Ti (Al) solid solution phase with increasing Ar pressure. All the materials under consideration, show average film stress to be independent of thickness for thicker films. The nature of the stress (compressive or tensile) depends upon working gas pressure, sputtering power and the target material used. A definite trend is observed in the film stress as a function of Ar gas pressure. Both power and gas pressure influence the energetic bombardment of ions/atoms which in turn influence the average film stress. The nature of the intrinsic stress is explained by the atomic peening model. The Young's modulus of thin films is calculated by using the slope of the stress-temperature plots. The E values seem to change with deposition conditions, however, there is no obvious trend between the sputtering gas pressure and the Young's modulus of these thin films.     

The influences of rapid-thermal annealing on the characteristics of Sr0.6Ba0.4Nb2O6 thin film

The Sr0.6Ba0.4Nb2O6 (SBN) thin films were successfully prepared on Pt/Ti/Si and SiO2/Si/Al substrates and crystallized subsequently using rapid thermal annealing (RTA) process in ambient atmosphere for 1 min. The surface morphologies and thicknesses of as-deposited and annealed SBN thin films were characterized by field emission scanning electron microscopy, and the thickness was about 246 nm. As compared with the as-deposited SBN thin films, the RTA-treated process had improved the crystalline structures and also had large influence on the crystalline orientation. When the annealing temperatures increased from 700 degrees C to 900 degrees C, the diffraction intensities of (410) and (001) peaks apparently increased. Annealed at 900 degrees C, the (001) peak had the maximum texture coefficient and SBN thin films showed a highly c-axis (001) orientation. The influences of different RTA-treated temperatures on the polarization-applied electric field (P-E) curves and the capacitance-voltage (C-V) curves were also investigated.     

N掺杂Cu2O薄膜的低温沉积及快速热退火研究

采用氧化亚铜(Cu_2O)陶瓷靶,利用射频磁控溅射沉积法在氮气和氩气的混合气氛下制备了N掺杂Cu_2O(Cu_2O∶N)薄膜,并在N_2气氛下对薄膜进行了快速热退火处理,研究了N_2流量和退火温度对Cu_2O∶N薄膜的生长行为、物相结构、表面形貌及光电性能的影响。结果显示,在衬底温度300℃、N_2流量12sccm条件下生长的薄膜为纯相Cu_2O薄膜;在N_2气氛下对预沉积薄膜进行快速热退火处理不影响薄膜的物相结构,薄膜的结晶质量随退火温度(450℃)的升高而显著改善;快速热退火处理能改善薄膜的结晶质量和缺陷,降低光生载流子的散射,增强载流子的传输,预沉积Cu_2O∶N薄膜经400℃退火处理后展示出较好的电性能,薄膜的霍尔迁移率(μ)为27.8cm~2·V~(-1)·s~(-1)、电阻率(ρ)为2.47×10~3Ω·cm。研究表明低温溅射沉积和快速热退火处理能有效改善Cu_2O∶N薄膜的光电性能。     

Low temperature preparation of transparent, antireflective TiO2 films deposited at different O2/Ar ratios by microwave electron cyclotron resonance magnetron sputtering

A serial of crystalline titanium oxide ceramic films were deposited at low temperature using microwave electron cyclotron resonance (MW-ECR) magnetron sputtering with different O₂/Ar ratios. The influences of O₂/Ar ratio on the deposition rate, morphology, crystalline nature, optical adsorption property of the obtained titanium oxide thin films were investigated by means of X-ray diffraction (XRD), atomic force microscopy (AFM) and UV-Vis spectra. Therefore, the optimum O₂/Ar ratio for deposition of anatase TiO₂ thin films on unheated glass substrate was realized in a MW-ECR magnetron sputtering process. The as-deposited anatase TiO₂ films were transparent and were antireflective in the visible region.     

Effect of annealing treatment on structural, electrical, and optical properties of Ga-doped ZnO thin films deposited by RF magnetron sputtering

The effect of annealing on structural, electrical, and optical properties of Ga-doped ZnO (GZO) films prepared by RF magnetron sputtering was investigated in air and nitrogen. GZO films are polycrystalline with a preferred 002 orientation. The resistivities of annealed films are larger than the as-deposited. The transmittance in the near IR region increases greatly and the optical band gap decreases after annealing. The photoluminescence spectra is composed of a near band edge emission and several deep level emissions (DLE) which are dominated by a blue emission. After annealing, these DLEs are enhanced evidently.     

退火处理对SnO2:F薄膜光电性能的影响

SnO2∶F薄膜作为low-e玻璃的表面功能层材料,广泛应用于节能镀膜玻璃。Low-e玻璃在后期退火(深加工)后,其性能的变化已经引起了学术研究和实际应用方面的的关注。我们对于用化学气相沉积法在玻璃表面沉积的约250nm厚的SnO2∶F薄膜进行不同的退火处理。并通过一系列的研究,结果发现,薄膜的结构、组成、电学、光学性能在氮气和空气两种不同的退火气氛下会有显著的变化。SnO2∶F薄膜的Low-e性能经过空气中高温退火后下降明显。通过计算对比退火后SnO2∶F薄膜的晶格常数和晶胞尺寸,提出了一种对于薄膜Low-e性能下降的合理解释。     

Morphological changes induced by thermal anneals in NiFe/Ag multilayers; their relation to the resistive and magnetoresistive properties

(Ti, Al)N films have drawn much attention as alternatives for TiN coatings, which are oxidized easily in air above 500 °C. We have investigated the effect of Al content on the oxidation resistance of (Ti_{1 − x}Al_x)N films prepared by r.f. reactive sputtering.

(Ti_{1 − x}Al_xN films (O ≤ x ≤ 0.55) were deposited onto fused quartz substrates by r.f. reactive sputtering. Composite targets with five kinds of Al-to-Ti area ratio were used. The sputtering gas was Ar (purity, 5 N) and N₂ (5 N). The flow rate of Ar and N₂ gas was kept constant at 0.8 and 1.2 sccm, respectively, resulting in a sputtering pressure of 0.4 Pa. The r.f. power was 300 W for all experiments. Substrates were not intentionally heated during deposition. The deposited films (thickness, 300 nm) were annealed in air at 600 900 °C and then subjected to X-ray diffractometer and Auger depth profiling.

The as-deposited (Ti_{1 − x}Al_x)N films had the same crystal structure as TiN (NaCl type). Al atoms seemed to substitute for Ti in lattice sites. The preferential orientation of the films changed with the Al content of the film, x. Oxide layers of the films grew during annealing and became thicker as the annealing temperature increased. The thickness of the oxide layer grown on the film surface decreased with increasing Al content in the film. For high Al content films an Al-rich oxide layer was grown on the surface, which seemed to prevent further oxidation. All of the films, however, were oxidized by 900 °C annealing, even if the Al content was increased up to 0.55.     

氧氩比和热处理对ZnO：Eu^3＋薄膜的结构及其发光性质的影响

用射频磁控溅射法在石英衬底上制备了ZnO：Eu^3＋薄膜,通过X射线衍射仪和荧光光谱仪对样品进行了表征,考察了氧氩比和退火工艺对其结构及发光性能的影响。结果表明：样品均呈现ZnO的六角纤锌矿结构,适当的氧氩比有利于ZnO的C轴择优取向的形成,高温退火会使晶粒尺寸增大;合适的氧氩比,尤其是退火工艺（700℃）可以促进ZnO基质（372nm）到Eu^3＋离子（^5Do-^7F2）之间的能量传递,但过多的氧及高温退火不利于稀土Eu^3＋离子465nm（^7Fo-^5D2）到611nm（^5Do-^7F2）的直接能量传递。     

Electrical and optical properties of nanostructured VOX thin films prepared by direct current magnetron reactive sputtering and post-annealing in oxygen

Nanostructured vanadium oxide (nano-VO_X) thin films were prepared by direct current magnetron reactive sputtering in mixed O₂/Ar discharges and subsequent annealing in oxygen atmosphere. X-ray diffraction and field emission scanning electron microscope were employed to characterize the crystal structures and morphologies, respectively. Fourier transform infrared spectroscopy was applied to analyze the vanadium-oxygen bonds of films. X-ray photoelectron spectroscopy revealed the compositions of the surface and inner portion of nano-VO_X thin films. It was shown that the as-deposited films were amorphous, and in-situ annealing of these films in ambient oxygen for 10 min can lead to the growth of nano-VO_X thin films. Results of electrical studies indicated that the absolute values of temperature coefficient of resistance and activation energy of films increased significantly after oxygen annealing. Optical investigations carried out in the UV-visible range showed that the absorption edges of nano-VO_X films exhibited large red shifts compared with as-deposited film, and that dual optical absorptions were observed in nano-VO_X films.     

Influence of deposition parameters on preferred orientation of RF magnetron sputtered BST thin films

Ba_0.65Sr_0.35TiO₃ (BST) thin films have been deposited by radio frequency magnetron sputtering. The effects of the deposition parameters on the crystallization and microstructure of BST thin films were investigated by X-ray diffraction and field emission scanning electron microscopy, respectively. The crystallization behavior of these films was apparently affected by the substrate temperature, annealing temperature and sputtering pressure. The as-deposited thin films at room temperature were amorphous. However, the improved crystallization is observed for BST thin films deposited at higher temperature. As the annealing temperature increased, the dominant X-ray diffraction peaks became sharper and more intense. The dominant diffraction peaks increased with the sputtering pressures increasing as the films deposited at 0.37–1.2 Pa. With increasing the sputtering pressure up to 3.9 Pa, BST thin films had the (110) + (200) preferred orientation. Possible correlations of the crystallization with changes in the sputtering pressure were discussed. The SEM morphologies indicated the film was small grains, smooth, and the interface between the film and the substrate was sharp and clear.     

退火处理对TiO2薄膜结构和透射的影响

在常温下,采用射频反应磁控溅射方法在不同溅射功率下于K9双面抛光玻璃基底上制备二氧化钛薄膜.将制备的样品进行450℃退火6h热处理.利用X射线衍射仪(XRD)对比分析了退火前后薄膜的微观结构,采用光栅光谱仪测试了退火前后薄膜样品的透射谱.实验结果表明,退火前薄膜样品是非晶态,退火后薄膜晶化为晶态,但不同溅射功率下制备的薄膜结晶取向有差异;退火热处理对薄膜的折射率有一定影响,表现为退火前后透射谱偏移.     

Ge-Si-O phase separation and Ge nanocrystal growth in Ge:SiO(x)/SiO(2) multilayers--a new dc magnetron approach

Ge:SiO(x)/SiO(2) multilayers are fabricated using a new reactive dc magnetron sputtering approach. The influence of the multilayer stoichiometry on the ternary Ge-Si-O phase separation and the subsequent size-controlled Ge nanocrystal formation is explored by means of x-ray absorption spectroscopy, x-ray diffraction, electron microscopy and Raman spectroscopy. The ternary system Ge-Si-O reveals complete Ge-O phase separation at 400?°C which does not differ significantly to the binary Ge-O system. Ge nanocrystals of < 5?nm size are generated after subsequent annealing below 700?°C. It is shown that Ge oxides contained in the as-deposited multilayers are reduced by a surrounding unsaturated silica matrix. A stoichiometric regime was found where almost no GeO(2) is present after annealing. Thus, the Ge nanocrystals become completely embedded in a stoichiometric silica matrix favouring the use for photovoltaic applications.     

Preparation of SiO2 films with embedded Si nanocrystals by reactive r.f. magnetron sputtering

SiO_x films with a nominal x-value (1≤x≤2) were deposited on flat-surface silicon substrates by reactive r.f. magnetron sputtering at substrate temperatures of 20 and 500°C, respectively. X-ray diffraction and high resolution TEM investigations of SiO_x films with x=1.45 and x=1 show that as-deposited films have an amorphous structure. After annealing, a nucleation of Si nanocrystals was found with increasing size at increasing initial Si concentration and annealing temperature. The weak photoluminescence in the visible region of as-deposited SiO_x films increases remarkably by annealing with dependence on x.