Effect of deposition time on microstructures and growth behavior of ZrC coatings prepared by low pressure chemical vapor deposition with the Br<Subscript>2</Subscript>-Zr-C<Subscript>3</Subscript>H<Subscript>6</Subscript>-H<Subscript>2</Subscript>-Ar System

ZrC coatings were deposited on graphite substrates by low pressure chemical vapor deposition (LPCVD) with the Br₂-Zr-C₃H₆-H₂-Ar system. The effects of deposition time on the microstructures and growth behavior of ZrC coatings were investigated. ZrC coating grew in an island-layer mode. The formation of coating was dominated by the nucleation of ZrC in the initial 20 minutes, and the rapid nucleation generated a fine-grained structure of ZrC coating. When the deposition time was over 30 min, the growth of coating was dominated by that of crystals, giving a column-arranged structure. Energy dispersive X-ray spectroscopy showed that the molar ratio of carbon to zirconium was near 1:1 in ZrC coating, and X-ray photoelectron spectroscopy showed that ZrC was the main phase in coatings, accompanied by about 2.5mol% ZrO₂ minor phase.     

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)     

Thermal shock resistances of FeMnCr/Cr<Subscript>3</Subscript>C<Subscript>2</Subscript> coatings deposited by arc spraying

Arc spraying with the cored wires was applied to deposit FeMnCr/Cr₃C₂ coatings on low carbon steel substrates, namely FM1, FM2 and FM3. Thermal shock resistances of the coatings were investigated to assess the influence of Cr₃C₂ content on thermal shock resistance. Characteristics of the coatings under thermal cycling test were studied by optical microscopy, field emission scanning electron microscope (FE-SEM) and energy dispersion spectrum (EDS), X-ray diffraction (XRD). The experimental results show that hardness of the coatings increases, bonding strength decreases slightly with increase of the Cr₃C₂ content of the coatings. As a result, FM2 coating possesses the best thermal shock resistance, attributing to its better thermal expansion matches and wettability than those of FM3 coating, less oxide rate than that of FM1 coating restraining from cracks formation and propagation in coatings.     

Bipolar Resistive Switching Effect in BiFeO<Subscript>3</Subscript>/Nb:SrTiO<Subscript>3</Subscript> Heterostructure by RF Sputtering at Room Temperature

The (001) oriented BiFeO₃ thin film was deposited on the Nb: SrTiO₃ substrate by radio frequency magnetron sputtering technology, and the bipolar resistive switching effect was observed in the BiFeO₃/Nb: SrTiO₃ heterostructure. The results showed that the ratio between the high resistance and low resistance was more than two orders at a reading pulse of -0.5 V and it exhibited excellent retention over 3600 s. The current density-voltage characteristic was dominated by the space-charge-limited conduction. The resistive switching effect of the structure was attributed to the trapping/detrapping of the charge carriers.     

Microstrueturc and Mcehanieal Propcrtics of Heat-treated GeSb2Te4 Thin Films

The effect of annealing on microstructure, adhesive and frictional properties of GeSb2Te4 films were experimentally studied. The GeSb2Te4 films were prepared by radio frequency （RF） magnetron sputtering, and annealed at 200℃ and 340℃ under vacuum circumstance, respectively. The adhesion and friction experiments were mainly conducted with a lateral force microscope （LFM） for the GeSb2Te4 thin films before and after annealing. Their morphology and phase structure were analyzed by using atomic force microscopy （AFM） and X-ray Diffraction （XRD） techniques, and the nanoindention was employed to evaluate their hardness values. Moreover, an electric force microscope （EFM） was used to measure the surface potential. It is found that the deposited GeSb2Te4 thin film undergoes an amorphous-to-fcc and fcc-to-hex structure transition; the adhesion has a weaker dependence on the surface roughness, but a certain correlation with the surface potential of GeSb2Te4 thin films. And the friction behavior of GeSb2Te4 thin films follows their adhesion behavior under a lower applied load. However, such a relation is replaced by the mechanical behavior when the load is relatively higher. Moreover, the GeSb2Te4 thin film annealed at 340℃ presents a lubricative property.     

Microstructure and performance analysis of organic coating under high temperature and high CO<Subscript>2</Subscript> partial pressure

To evaluate the property of the organic coatings in oil and gas plants, the aging process was studied in high temperature and high CO₂ partial pressure environment. Correlations were developed between the macroscopic properties and microstructure of the organic coatings. The surface appearance, mechanical properties, and permeability of the organic coatings were measured. Furthermore, the crystal structure of the organic coatings was investigated through synchrotron radiation grazing incidence X-ray diffraction (GIXRD) on the BL14B1 beam line in Shanghai Synchrotron Radiation Facility. Combined with the Fourier transform infrared spectroscopy, the molecular structure of the organic coatings was investigated. The experimental results indicate that the thickness variation and weight loss of the organic coatings increase with the immersion time, and the penetration resistance of the coating obviously decreases as the temperature rises. Moreover, the degradation of the organic coatings with immersion time in high temperature and high CO₂ partial pressure environment is caused by the amorphization of the organic coatings as the groups and bonds of the organic coatings were not damaged.     

Effect of salt spray corrosion on tribological properties of HVOF sprayed NiCr-Cr<Subscript>3</Subscript>C<Subscript>2</Subscript> coating with intermediate layer

The objective of the present work was to determine the influence of the neutral salt spray corrosion on the wear resistance of HVOF sprayed NiCr-Cr₃C₂ coating with intermediate layer. Ni-Zn-Al₂O₃ coatings as interlayers were prepared by low pressure cold spray (LPCS) between NiCr-Cr₃C₂ cermet coatings to form a sandwich structure to enhance the corrosion resistance properties. The tribological properties were examined using the UMT-3 fricition and wear tester by line-contact reciprocating sliding under dry and salt spray one week corrosion. The morphology, element distribution, and phase compositions of the coating and worn sufaces were analyzed by using scanning electron microscopy, energy dispersive spectrometry, and X-ray diffraction respectively. The corrosion behavior of the coating was studied by the open-circuit potential, the electrochemical impedance spectroscopy, potentiodynamic polarization, and salt spray corrosion methods. It is found that the sandwich structured coating has better corrosion resistance than the single layer coating. The results show that under dry wear conditions, the wear mechanism is abrasive and adhesive wear, whereas under salt spray corrosion conditions it becomes corrosion wear. The friction coefficient of the sandwich structured coating after salt spray corrosion is slightly lower than the dry friction coefficient, but the weight of the wear loss is lower than that under dry condition.     

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.     

Moisture-proof and enhanced effect of inorganic coating on porous Si<Subscript>3</Subscript>N<Subscript>4</Subscript> ceramic

Inorganic coating was fabricated on the surface of the porous Si₃N₄ ceramic by polymer derived (PD) and spraying technology, via using vinyl-polysilazane (PSN-1) as a preceramic polymer and Si₃N₄ and lithium aluminosilicate (LAS) powders as fillers. The phase and microstructure of the coatings were analyzed by X-ray diffraction (XRD) analysis and scanning electron microscopy (SEM), respectively. The effect of the coatings on mechanical property and humidity resistance of the porous Si₃N₄ ceramic was investigated. The experimental results showed that we successfully fabricated the uniform and dense coating which preferably combined with the substrate upon the addition of fillers. The bending strength of the porous Si₃N₄ ceramic sprayed the coating increased by more than 18%, and the surface hardness increased by 1.7 times. The apparent porosity of the materials reduced by an average of 97.7%, and water absorption was below 0.5%. Therefore, the prepared coating with preferable density had an obviously moisture-proof and enhanced effect on the porous Si₃N₄ ceramic.     

Improved visible transparency of SIO<Subscript>2</Subscript>/ZNO:AL /CEO<Subscript>2</Subscript>-TIO<Subscript>2</Subscript>/SIO<Subscript>2</Subscript> multilayer films with high UV absorption and infrared reflection rate

New visible transparent, UV absorption, and high infrared reflection properties have been realized by depositing multilayer SiO₂/ZnO: Al/CeO₂-TiO₂/SiO₂ films onto glass substrates at low temperature by radio frequency magnetron sputtering. Optimum thickness of SiO₂, ZnO: Al (ZAO) and CeO₂-TiO₂ (CTO) films were designed with the aid of thin film design software. The degree of antireflection can be controlled by adjusting the thickness and refractive index. The outer SiO₂ film can diminish the interference coloring and increase the transparency; the inner SiO₂ film improves the adhesion of the coating on the glass substrate and prevents Ca²⁺, Na⁺ in the glass substrate from entering the ZAO film. The average transmittance in the visible light range increases by nearly 18%-20%, as compared to double layer ZAO/CTO films. And the films display high infrared reflection rate of above 75% in the wavelength range of 10-25 μm and good UV absorption (> 98%) properties. These systems are easy to produce on a large scale at low cost and exhibit high mechanical and chemical durability. The triple functional films with high UV absorption, antireflective and high infrared reflection rate will adapt to application in flat panel display and architectural coating glass, automotive glass, with diminishing light pollution as well as decreasing eye fatigue and increasing comfort.     

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.     

Microstructure and wear behaviour of laser-induced thermite reaction Al<Subscript>2</Subscript>O<Subscript>3</Subscript> ceramic coatings on pure aluminum and AA7075 aluminum alloy

Wear-resistant laser-induced thermite reaction Al2O3 ceramic coatings can be fabricated on pure Al and AA7075 aluminum alloy by laser cladding （one-step method） and laser cladding followed by laser re-melting （two-step method） using mixed powders CuO-Al-SiO2 in order to improve the wear properties of aluminum and aluminum alloy, respectively. The microstructure of the coatings was characterized by scanning electron microscopy （SEM） and X-ray diffraction （XRD）. The wear resistance of the coatings was evaluated under dry sliding wear test condition at room temperature. Owing to the presence of hard α-Al2O3 and γ-Al2O3 phases, the coatings exhibited excellent wear resistance. In addition, the wear resistance of the coatings fabricated by two-step method is superior to that of the coatings fabricated by one-step method.     

Preparation and piezoelectric properties of CuO-added (Ag<Subscript>0.75</Subscript>Li<Subscript>0.1</Subscript>Na<Subscript>0.1</Subscript>K<Subscript>0.05</Subscript>)NbO<Subscript>3</Subscript> lead-free ceramics

CuO-doped (Ag_0.75Li_0.1Na_0.1K_0.05)NbO₃ (ALNKN-xCuO, x = 0–2mol%) lead-free piezoelectric ceramics were prepared by the solid-state reaction method in air atmosphere. The effects of CuO addition on the phase structure, microstructure, and piezoelectric properties of the ceramics were investigated. The experimental results show that the ALNKN ceramics without doping CuO possess rhombohedral phase along with K2Nb6O16-type phase and metallic silver phase. For all of the CuO-doped ALNKN ceramics, a pure perovskite structure with the orthorhombic phase was obtained by enclosing the samples in a corundum tube. A homogeneous microstructure with the grain size of about 1 μm was formed for the ceramics with 0.5mol% CuO. The grain size increases with increasing amount of CuO. The temperature dependence of dielectric properties indicates that the ferroelectric phase of the ALNKN-xCuO ceramics becomes less stable with the addition of CuO. The ceramics with x = 1mol% exhibit relatively good electrical properties along with a high Curie temperature. These results will provide a helpful guidance to preparing other AN-based ceramics by solid-state reaction method in air atmosphere.     

Ferroelectric properties of Bi<Subscript>4</Subscript>Zr<Subscript>0.5</Subscript>Ti<Subscript>2.5</Subscript>O<Subscript>12</Subscript> thin films prepared on LaNiO<Subscript>3</Subscript> bottom electrode by sol-gel method

The Bi4Zr0.5Ti2.5O12 (BZT) thin films were fabricated on the LaNiO3 bottom electrode using sol-gel method. The structure and morphology of the films were characterized using X-ray diffraction, AFM and SEM. The results show that the films have a perovskite phase and dense microstructure. The 2Pr and 2Vc of the Pt/BZT/LaNiO3 capacitor are 28.2 μC/cm2 and 14.7 V respectively at an applied voltage of 25 V. After the switching of 1×1010 cycles, the Pr value decreases to 87% of its pre-fatigue values. The dielectric constant (ε) and the dissipation factor (tanδ) of the BZT thin films are about 204 and 0.029 at 1 kHz, respectively. The films show good insulating behavior according to the test of leakage current. The clockwise C-V hysteresis curve observed shows that the Pt/BZT/LaNiO3 structure has a memory effect because of the BZT film's ferroelectric polarization.     

Improved Breakdown Strength in (Ba<Subscript>0.6</Subscript>Sr<Subscript>0.4</Subscript>)<Subscript>0.85</Subscript>Bi<Subscript>0.1</Subscript>TiO<Subscript>3</Subscript> Ceramics with Addition of CaZrO<Subscript>3</Subscript> for Energy Storage Application

(Ba_0.6Sr_0.4)_0.85Bi_0.1TiO₃ ceramics doped with x wt%CaZrO₃ (x= 0-10) were synthesized by solid-state reaction method. The effects of CaZrO₃ amount on the dielectric properties and structure of (Ba_0.6Sr_0.4)_0.85Bi_0.1TiO₃ ceramics were investigated. X-ray diffraction results indicated a pure cubic perovskite structure for all samples and that the lattice parameter increased till x=5 and then slightly decreased. A homogenous microstructure was observed with the addition of CaZrO₃. Dielectric measurements revealed a relaxor-like characteristic for all samples and that the diffusivity γ reached the maximum value of 1.78 at x=5. With the addition of CaZrO₃, the dielectric constant dependence on electric field was weakened, insulation resistivity enhanced and dielectric breakdown strength improved obviously and reached 19.9 kV/mm at x=7.5. In virtue of low dielectric loss (tan δ<0.001 5), moderate dielectric constant (ε_r >1 500) and high breakdown strength (E_b >17.5 kV/mm), the CaZrO₃ doped (Ba_0.6Sr_0.4)_0.85Bi_0.1TiO₃ ceramic is a potential candidate material for high power electric applications.     

Structure and Electrical Properties of （Na0.5Bi0.5）0.94Ba0.06TiO3 Ceramicwith0.5wt% of MnO

The structure and electrical properties of （Na0.5Bi0.5）0.94Ba0.06TiO3 ceramic doped with 0.5 wt% of MnO were investigated in comparison with those of （Na0.5Bi0.5）0.94Ba0.06TiO3 ceramic. It was ascertained that the MnO addition did not cause remarkable change in crystal structure and microstructure. The MnO addition mainly displayed a hard effect on the electrical properties, an increase of coercive field （E） and mechanical quality factor （Qm） together with a decrease of dielectric constant （εr） and piezoelectric constant （d33）. An enhancement of electromechanical coupling factor （kp） with the MnO addition was obtained too. An essential relation between the piezoelectric properties and ferroelectric nature of the ceramics was detected. It was found that the piezoelectric properties of the ceramics highly depended on the corporative contribution of remanent polarization （Pt） and coercive field.     

Effect of water soluble PVA on the microstructure characteristics of C-S-H formed in Na<Subscript>2</Subscript>SiO<Subscript>3</Subscript>-Ca(NO<Subscript>3</Subscript>)<Subscript>2</Subscript> solution system

The structure characteristics of hydrated calcium silicate synthesized by solution reaction method with the existing of water soluble polymer polyvinyl alcohol(PVA)are investigated.Using Na 2 SO 3 and Ca(NO 3 ) 2 as the main raw materials,in the condition of 2%(in weight)addition of PVA and the water to solid ratio of 20,hydrated calcium silicate samples(Ca/Si=1.0 and 1.5)were prepared with 60℃water bath.IR,BET,XRD and SEM methods were used to study the microstructure of the hydration products.The results s...     

Preparation,structure and dielectric properties of tungsten bronze ferroelectrics in SrO-Eu<Subscript>2</Subscript>O<Subscript>3</Subscript>-TiO<Subscript>2</Subscript>-Nb<Subscript>2</Subscript>O<Subscript>5</Subscript> system

Compounds Sr4Eu2Ti4Nb6O30 and Sr5EuTi3Nb7O30 with filled tetragonal tungsten bronze structure were prepared,and the dielectric characteristics and ferroelectric transition were investigated.Both ceramics displayed weak frequency dependence in room temperature dielectric constant,which decreased from 125 to 118 for Sr4Eu2Ti4Nb6O30,from 206 to 195 for Sr5EuTi3Nb7O30 in the frequency range of 10 kHz to 1 MHz.The present ceramics showed a diffuse ferroelectric phase transition.The frequency independent transition temperature (Tm) indicated the above compounds had no relaxor property.The diffuseness (γ) was 1.45 and 1.64 for Sr4Eu2Ti4Nb6O30 and Sr5EuTi3Nb7O30 respectively.The weak ferroelectric of the present materials are indicated from the P-E hysteresis loops,and a small 2Pr of 0.596 μC/cm2 and 0.068 μC/cm2 were observed for Sr4Eu2Ti4Nb6O30 and Sr5EuTi3Nb7O30 respectively.     

Dielectric tunable properties of BaTi<Subscript>4</Subscript>O<Subscript>9</Subscript>-doped Ba<Subscript>0.6</Subscript>Sr<Subscript>0.4</Subscript>TiO<Subscript>3</Subscript> microwave composite ceramics

BaTi₄O₉-doped Ba_0.6Sr_0.4TiO₃ (BST) composite ceramics were prepared by the conventional solid-state reaction and their structure, dielectric nonlinear characteristics and microwave dielectric properties were investigated. The secondary phase of the orthorhombic structure Ba₄Ti₁₃O₃₀ is formed among BST composite ceramics with the increase of BaTi₄O₉. At the same time, a duplex or bimodal grains size distribution shows fine grains in a coarse grain matrix. The degree of frequency dispersion of dielectric permittivity below T _m is increased initially and then decreased with respect to BaTi₄O₉. As the BaTi₄O₉ content increases, the tunability of composite ceramics decreases, while the Q value increases. Interestingly, 70 wt% BaTi₄O₉-doped BST has a tunability ∼4.0% (under 30 kV/cm biasing) versus a permittivity ∼68 and quality factor ∼134.1 (at ∼3.2 GHz). Supported by the Ministry of Science and Technology of China through 973-project (Grant No. 2009CB623302), the Cultivation Fund of the Key Scientific and Technical Innovation Project, Ministry of Education of China (Grant No.707024), Shanghai Committee of Science and Technology (Grant No. 07DZ22302), and Shanghai Foundation Project under 06JC14070     

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.