Preparation and Properties of IrO2 Thin Films Grown by Pulsed Laser Deposition Technique

Highly conductive IrO2 thin films were prepared on Si （100） substrates by means of pulsed laser deposition technique from an iridium metal target in an oxygen ambient atmosphere. Emphasis was put on the effect of oxygen pressure and substrate temperature on the structure, morphology and resistivity of IrO2 films. It was found that the above properties were strongly dependent on the oxygen pressure and substrate temperature. At 20 Pa oxygen ambient pressure, pure polycrystalline IrO2 thin films were obtained at substrate temperature in the 300-500℃ range with the preferential growth orientation of IrO2 films changed with the substrate temperature. IrO2 films exhibited a uniform and densely packed granular morphology with an average feature size increasing with the substrate temperature. The room-temperature resistivity variations of IrO2 films correlated well with the corresponding film morphology changes. IrO2 films with the minimum resistivity of （42 ±6）μΩ·cm was obtained at 500℃.     

Growth,Characterization and Micro-pattern Fabrication of Iridium/Si3N4/Si（100） Thin Films

Iridium thin films have been deposited on Si3N4（100 nm）/Si（100） substrates by magnetron sputtering. And then iridium film micro-patterns were fabricated by ion milling technique. The atomic force microscopy （AFM） measurements reveal that there is a very fiat and smooth surface with an average roughness of 0.64 nm for the iridium films. The X-ray diffraction also reveals that the deposited iridium films have a polycrystalline microstructure with （111） plane preferential orientation. The electrical resistivity of the iridium films was also measured and discussed.     

Effect of the sputtering parameters on the structure and properties of Cu<Subscript>3</Subscript>N thin film materials

Copper nitride (Cu₃N) thin films were successfully deposited on glass substrates by reactive radio frequency magnetron sputtering. The effects of sputtering parameters on the structure and properties of the films were studied. The experimental results show that with increasing of RF power and nitrogen partial pressure, the preferential crystalline orientation of Cu₃N film is changed from (111) to (100). With increasing of substrate temperature from 70 °C to 200 °C, the film phase is changed from Cu₃N phase to Cu. With increasing sputtering power from 80 W to 120 W, the optical energy decreases from 1.85 eV to 1.41 eV while the electrical resistivity increases from 1.45 ×10² Ω · cm to 2.99 × 10³ Ω · cm, respectively.     

Cu<Subscript>2</Subscript>ZnSnS<Subscript>4</Subscript> thin films prepared by sulfurizing different multilayer metal precursors

Cu₂ZnSnS₄ (CZTS) thin films were successfully fabricated on glass substrates by sulfurizing Cu-Sn-Zn multilayer precursors, which were deposited by ion beam sputtering and RF magnetron sputtering, respectively. The structural, electrical and optical properties of the prepared films under various processing conditions were investigated in detail. Results showed that the as-deposited CZTS thin films with the precursors by both ion beam sputtering and RF magnetron sputtering have a composition near stoichiometric. The crystallization of the samples, however, has a strong dependence on the atomic percent of constituents of the prepared CZTS films. A single phase stannite-type structure CZTS with a large absorption coefficient of 10₄/cm in the visible range could be obtained after sulfurization at 520°C for 2 h. The samples relative to the RF magnetron sputtering showed a low resistivity of 0.073 Ωcm and band gap energy of about 1.53 eV. The samples relative to the ion beam sputtering exhibited a resistivity of 0.36 Ωcm and the band gap energy is about 1.51 eV. Supported by the National Natural Science Foundation of China (Grant No. 10574106), the Planned Science and Technology Project of Guangdong Province (Grant No.2003C05005) and the Natural Science Fund of Zhanjiang Normal University (Grant No.200801)     

Microstructures and fatigue-free properties of the La<Superscript>3+</Superscript> and Nd<Superscript>3+</Superscript> doped Bi<Subscript>4</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> thin films prepared by modified sol-gel technique

Ferroelectric Bi_3.25La_0.75Ti₃O₁₂ (BLT) and Bi_3.15Nd_0.85Ti₃O₁₂ (BNT) thin films were fabricated on Pt/TiO₂/SiO₂/Si (100) substrates by a modified sol-gel technique. X-ray diffraction indicated that these films were of single phase with random polycrystalline orientations. The surface morphologies of the films were observed by scanning electron microscope, showing uniform, dense films with grain size of 50–100 nm. Well-saturated hysteresis loops of the films were obtained in metal-ferroelectric-metal type capacitors with Cu top electrodes at an applied voltage of 400 kV/cm, giving the remanent polarization (2P _r) and coercive field (2E _c) values of the films of 25.1 μC/cm² and 203 kV/cm for BLT, and 44.2 μC/cm² and 296 kV/cm for BNT, respectively. Moreover, these capacitors did not show fatigue behaviors after up to 1.75×10¹⁰ switching cycles at the test frequency of 1 MHz, suggesting a fatigue-free character. The influences of the La³⁺ and Nd³⁺ doping on the properties of the films were comparatively discussed. Supported by the National Key Basic Research and Development Program of China (Grant No. 2006CB932305) and the Natural Science Foundation of Hubei Province, China (Grant No. 2004ABA082)     

Preparation and ferroelectric properties of Bi<Subscript>3.4</Subscript>Ce<Subscript>0.6</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> thin films grown by sol-gel method

We have investigated the preparation and properties of Bi_3.4Ce_0.6Ti₃O₁₂ thin films. The Bi_3.4Ce_0.6Ti₃O₁₂ thin films were fabricated on the Pt/Ti/SiO₂/Si substrates using sol-gel method. The structure and morphology of the films were characterized using X-ray diffraction and atomic force microscopy. The thin films showed a perovskite phase and dense microstructure. The dielectric constant and the dissipation factor of the Bi_3.4Ce_0.6Ti₃O₁₂ thin films were about 172 and 0.031 at 1 kHz, respectively. The 2P _r and 2E _c of the Bi_3.4Ce_0.6Ti₃O₁₂ thin films were 67.1 μC/cm² and 299.7 kV/cm, respectively, under an applied field of 600 kV/cm. The Bi_3.4Ce_0.6Ti₃O₁₂ film did not show fatigue up to 4.46×10⁹ switching cycles at a frequency of 1 MHz, and showed good insulating behavior according to the test of leakage current. Supported by the Natural Science Foundation of Hubei Province (Grants No. 2004ABA082)     

Fabrication of GaN epitaxial films on Al2O3/Si (001) substrates

Single crystal GaN films of hexagonal modification have been fabricated on Al₂O₃/Si (001) substrates via a low pressure metalorganic chemical deposition (LP-MOCVD) method. the full width at half-maximum of (0002) X-ray diffraction peak for the GaN film 1.1 μm thick was 72 arcmin, and the mosaic structure of the film was the main cause of broadening to the X-ray diffraction peak. At room temperature, the photoluminescence (PL) spectrum of GaN exhibited near band edge emission peaking at 365 nm. Project supported by the “863” Advanced materials Committee of China and the Planning Commission of China.     

Optical waveguide and nonlinear properties of Bi<Subscript>3</Subscript>NdTi<Subscript>3</Subscript>O<Subscript>12</Subscript> thin films

Neodymium-substituted bismuth titanate (Bi₃NdTi₃O₁₂, BNT) thin films were prepared on quartz substrates by a metal-organic solution deposition process. The crystalline structure was evaluated by X-ray diffraction. Waveguide property was investigated by using prism coupling technique and optical transmittance measurement. The optical nonlinearities of the film were measured by the top-hat Z-scan techniques and a large positive nonlinear refractive index, nonlinear refractive coefficient and two-photon absorption coefficient were determined to be 3.84 × 10⁻⁷ esu, 0.7523 cm²/GW and 4.81 × 10⁴ cm/GW, respectively. These results reveal that the BNT film may be a kind of new multifunctional materials.     

Orientation of Bi<Subscript>3.2</Subscript>La<Subscript>0.8</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> ferroelectric thin films with different annealing schedules

Fatigue-free Bi_3.2La_0.8Ti₃O₁₂ ferroelectric thin films were successfully prepared on p-Si (100) substrates using metalorganic solution deposition process. The orientation and formation of 5-layers thin films were studied under different processing conditions using XRD. Experimental results indicate that increase in annealing time at 700 °C after preannealing for 10 min at 400 °C can remarkably increase (200)-orientation of the films derived from the precursor solutions with two contents of citric acid. Meanwhile, high content of citric acid increases the film thickness and is conducive to the a-orientation of the films with the preannealing, and low concentration of the solution is conducive to the c-orientation of the films without the preannealing.     

Effect of annealing temperature on the ferroelectric properties of BiFeO<Subscript>3</Subscript> thin films prepared by sol-gel process

Sol-gel process was adopted to prepare BiFeO₃ films. BiFeO₃ films were deposited on LaNiO₃ coated Si(100) substrates annealed at 500 and 550 °C, respectively. The X-ray diffraction results reveal that BiFeO₃ film has a rhombohedrally distorted perovskite structure with space group R3c. The film annealed at 500 °C has larger remnant polarization (P _r) of 35.3 μC/cm². For the film annealed at 550 °C, smaller remnant polarization of P _r=4.8 μC/cm² is observed for its low breakdown electric field. Lower leakage conduction is observed in the film annealed at 500 °C at low applied field.     

Crystallization and Electrical Properties of （Ba0.4Pb0.3）Sr0.3TiO3 Thin Film by Pulsed Laser Deposition

（Ba0.4Pb0.3）Sr0.3TiO3 thin films were fabricated via pulsed laser deposition （PLD） technique on Pt/TiO2/SiO2/Si substrate. The crystallization of the films was characterized by XRD and FSEM, and the experimental results suggested deposition parameters, especially the deposition temperature was the key factor in forming the perovskite structure. The dielectric properties of the film deposited with optimized parameters were studied by an Agilent 4294A impedance analyzer at 1 MHz. The dielectric constant was 772, and the loss tangent was 0.006. In addition, the well-shaped hysteresis loop also showed that the film had a well performance in ferroelectric. The saturated polarization P, remnant polarization Pr and coercive field E were about 4.6 μC/cm2, 2.5 μC/cm2 and 23 kV/cm （the coercive voltage is 0.7 V）, respectively. It is suggested the film should be a promising candidate for microwave applications and nonvolatile ferroelectric random access memories （NvFeRAMs）.     

Preparation and characterization of SrTiO<Subscript>3</Subscript> thin film on functional organic self-assembled monolayers

SrTiO₃ thin film was successfully prepared on the functionalized organic self-assembled monolayers (SAMs) by the Liquid Phase Deposition (LPD) method. The as-prepared samples were characterized by X-ray diffraction (XRD), atomic force microscope (AFM), scanning electron microscopy (SEM) and metallographic microscope. Measurement of contact angle showed that the hydrophobe substrate was changed into hydrophile by UV irradiation. AFM photographs of octadecyl-trichloro-silane self-assembled monolayer (OTS-SAM) surface approved that UV irradiation did change the morphology of OTS monolayer and provided evidence for the conversion of hydrophilic characteristic. Photographs of Metallographic Microscope showed that OTS-SAM had an active effect on the deposition of SrTiO₃ thin film. XRD and SEM indicated that the thin film was of pure cubic phase SrTiO₃ and composed of nanosized grains with a size in the range of 100–500 nm. The formation mechanism of the SrTiO₃ film was proposed.     

Preparation of MgO films as buffer layers by laser-ablation at various substrate temperatures

MgO thin films were deposited on Si(100) substrates by laser ablation under various substrate temperatures (Tsub),expecting to provide a candidate buffer layer for the textured growth of functional perovskite oxide films on Si substrates.The effect of Tsub on the preferred orientation,crystallinity and surface morphology of the films was investigated.MgO films in single-phase were obtained at 473-973 K.With increasing Tsub,the preferred orientation of the films changed from (200) to (111).The crystallinity and surface morphology was different too,depending on Tsub.At Tsub=673 K,the MgO film became uniform and smooth,exhibiting high crystallinity and a dense texture.     

Study on the thermal stability and electrical properties of the high-k dielectrics (ZrO2)x(SiO2)1?x

(ZrO₂) _x (SiO₂)_1−x (Zr-Si-O) films with different compositions were deposited on p-Si(100) substrates by using pulsed laser deposition technique. X-ray photoelectron spectra (XPS) showed that these films remained amorphous after annealing at 800°C with RTA process in N₂ for 60 s. The XPS spectra indicated that Zr-Si-O films with x=0.5 suffered no obvious phase separation after annealing at 800°C, and no interface layer was formed between Zr-Si-O film and Si substrate. While Zr-Si-O films with x >0.5 suffered phase separation to precipitate ZrO₂ after annealing under the same condition, and SiO₂ was formed at the interface. To get a good interface between Zr-Si-O films and Si substrate, Zr-Si-O films with bi-layer structure (ZrO₂)_0.7(SiO₂)_0.3/(ZrO₂)_0.5(SiO₂)_0.5/Si was deposited. The electrical properties showed that the bi-layer Zr-Si-O film is of the lowest equivalent oxide thickness and good interface with Si substrate. Supported by the National Nature Science Foundation of China (Grant No. 60636010) and the National Basic Research Program of China (“973” Program) (Grant No. 2004CB619004)     

Preparation and characterization of CeO<Subscript>2</Subscript>-TiO<Subscript>2</Subscript>/SnO<Subscript>2</Subscript>:Sb films deposited on glass substrates by R.F. sputtering

CeO2-TiO2 films and CeO2-TiO/SnO2：Sb （6 mol%） double films were deposited on glass substrates by radio-frequency magnetron sputtering （R.F. Sputtering）, using SnO2：Sb（6 mol%） target, and CeO2- TiO2 targets with different molar ratio of CeO2 to TiO2 （CeO2：TiO2-0：1.0; 0.1：0.9; 0.2：0.8; 0.3：0.7; 0.4：0.6; 0.5：0.5; 0.6：0.4; 0.7：0.3; 0.8：0.2; 0.9：0.1; 1.0：0）. The films are characterized by UV-visible transmission and infrared reflection spectra, scanning electron microscopy （SEM）, Raman spectroscopy, X-ray photoelectron spectroscopy （XPS） and X-ray diffraction （XRD）, respectively. The obtained results show that the amorphous phases composed of CeO2-TiO2 play an important role in absorbing UV, there are Ce^3-, Ce^4- and Ti^4- on the surface of the films; the glass substrates coated with CeO2-TiO2 （Ce/Ti=0.5：0.5; 0.6：0.4）/SnO2：Sb（6 mol%） double films show high absorbing UV（〉99）, high visible light transmission （75%） and good infrared reflection （〉70%）. The sheet resistance of the films is 30-50 Ω/□. The glass substrates coated with the double functional films can be used as window glass of buildings, automobile and so on.     

Effects of Si and Ce on the microstructure and hydrogen storage property of Ti<Subscript>26.5</Subscript>Cr<Subscript>20</Subscript>V<Subscript>45</Subscript>Fe<Subscript>8.5</Subscript>Ce<Subscript>0.5</Subscript> alloy

In this paper, the effects of Si and Ce on the microstructure and hydrogen storage property of Ti_26.5Cr₂₀V₄₅Fe_8.5Ce_0.5 alloy were studied, respectively. First of all, effects of Si on the microstructure and hydrogen storage properties of Ti_26.5Cr₂₀(V₄₅Fe_8.5)_1−x Si _x Ce_0.5 (x = 0, 0.5, 1.0, 1.5 and 2.0 at%) alloys were studied by X-ray diffraction, scanning electron microscopy and P-C isotherm measurements. As the Si addition increases, the hydrogen absorption capacities of alloys decrease but the equilibrium pressure increases, due to the formation of Laves phase. Secondly, the effect of Ce on Ti_26.5Cr₂₀ (V₄₅Fe_8.5)_0.98Si₂ alloy was studied. It was found that Ce addition is an effective way to eliminate the effect of Si on the hydrogen storage properties of the alloy. Supported by the National Hi-Tech Research and Development Program of China (“863” Project) (Grant No. 2006AA05Z144)     

Structure and properties of TiB<Subscript>2</Subscript> thin films deposited at low temperatures using RF magnetron sputtering

The TiB2 thin films were deposited on steel substrates using RF magnetron sputtering technique with the low normalized substrate temperature （0.1〈Ts/Tm〈0.2）. Microstructure of these films was obtained by field emission scanning electron microscope （FESEM） and the grazing incidence X-ray diffraction （GIXRD） characterization, while the composition of films was obtained using Auger emission spectroscopy （AES） analysis. It was found that the TiB2 thin films were overstoichiometric with the B/Ti ratio at 2.33 and the diffusion of Ti and B atoms on the substrate surface was greatly improved at 350 ℃. Moreover, a new dense structure, named ＂equiaxed＂ grain structure was observed by FESEM at this substrate temperature, Combined with FESEM and AES analysis, it was suggested that the ＂equiaxed＂ grain structure was located in Zone 2 at the normalized substrate temperature as low as 0.18.     

Influence of thickness on the properties of solution-derived LiMn<Subscript>2</Subscript>O<Subscript>4</Subscript> thin films

LiMn₂O₄ thin films of different thickness were derived from solution deposition and heat treated by rapid thermal annealing. The phase identification and surface morphology were studied by X-ray diffraction and scanning electron microscopy. The electrochemical properties of the films were examined by galvanostatic charge-discharge experiments and electrochemical impedance spectroscopy. LiMn₂O₄ thin films of different thickness derived from solution deposition and rapid thermal annealing are homogeneous and crack free with the grain size between 20 nm and 50 nm. The specific capacity of these films is between 42 and 47 μAh·cm²·μm⁻¹. The capacity decreases with the increase of discharge current density. The capacity loss per cycle increases from 0.012% to 0.16% after being cycled 50 times as the film thickness increases from 0.18 μm to 1.04 μm. The lithium diffusion coefficients of these films are in the same order of 10⁻¹¹ cm²·s⁻¹.     

Two-step synthesis of TiC<Subscript>0.7</Subscript>N<Subscript>0.3</Subscript>@WC-MoC<Subscript>2</Subscript> core-shell microspheres and fabrication of TiC<Subscript>0.7</Subscript>N<Subscript>0.3</Subscript>@WC-MoC<Subscript>2</Subscript>-based cermets by SPS

The precursor with TiC0.7N0.3@WO3-MO3 microspheres were prepared by a novel method from the WO3-MoO3 sol dipping. Subsequently, TiC0.7N0.3@WC-MoC2 core-shell structural microspheres were successfully obtained by carburizing the precursor at 900 °C in a flowing mixture of CH4 (20 ml·min-1) and H2 (200 ml·min-1) for 2 h. Then TiC0.7N0.3@WC-MoC2-15Co cermets were prepared utilizing the core-shell powders by spark plasma sintering (SPS). Powders of the precursors with TiC0.7N0.3@WO3-MO3 microspheres, TiC0.7N0.3@WC-MoC2 microspheres and TiC0.7N0.3@WC-MoC2-15Co cermets were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). The obtained TiC0.7N0.3@WC-MoC2 microspheres have a dense WC-MoC2 coatings shell. The thickness of the shell could be easily controlled by adjusting the number of sol dipping cycles. It was found that the TiC0.7N0.3@WC-MoC2 microspheres were more beneficial to fabricate the "core-rim" structures by SPS.     

Facile synthesis of nanocrystalline Cr<Subscript>2</Subscript>O<Subscript>3</Subscript> thin film

A novel and facile synthesis route for the manufacture of transparent and uniform self-assembled nanocrystalline Cr2O3 (nc-Cr2O3) thin films with different morphology was reported, utilizing chromium nitrate as the inorganic source and triblock copolymer F127 as the morphology-directing agent by the evaporation-induced assembly (EIA) method. X-ray powder diffraction (XRD), thermogravimetry-differential scanning calorimetry (TG-DSC), N2-sorption, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to characterize the as-prepared nc-Cr2O3 thin films. The Cr2O3 thin film with different morphology was obtained by changing the relative humidity. The possible formation mechanism of the nc-Cr2O3 thin films with different morphologies was discussed.