Ti-6A1-4V表面激光熔覆钛基复合涂层的微观组织及形成机制

Titanium matrix composite coatings were fabricated on Ti-6A1-4V substrate by laser cladding using powder mixtures of Ti Cr3C2 and Ti TiB2, respectively. The chemical compositions and mi-crostructures of the coatings were analyzed using scanning electron microscope (SEM), energy dispersive spectrometer (EDS) and X-ray diffraction (XRD). Microhardness was measured by a microhardness tester. The results showed that Cr3C2 particles were dissolved and deposited to form dendritic TiC in the upper section and spherical grain TiC in the bottom of Cr3C2 Ti coating. Most of TiB2 was dissolved in the molten pool by laser irradiation, then formed TiB with fine needles and coarse needles in the TiB2 Ti coating. A few quasi-melted TiB2 particles with irregular shape at the bottom of the coating were observed. The average microhardnesses were approximately HV850-V1000, HV800-V1050 in the Cr3C2 Ti and TiB2 Ti coating, respectively, which were 2-3 times higher than that of Ti-6A1-4V substrate.     

Growth Mechanism,Microstructure, and Surface Modification of Nanostructured CeO2 Films by Chemical Solution Deposition

The evolution from a partially oriented granular microstructure to a dense epitaxial one in CeO₂ films deposited from chemical solutions on Y₂O₃‐stabilized cubic ZrO₂ (YSZ) has been investigated using cross‐section transmission electron microscopy (XTEM), electron energy‐loss spectroscopy (EELS), X‐ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), X‐ray diffraction (XRD), and X‐ray reflectometry (XRR). In crystallization from chemical solutions, undercoolings are typically high enough to promote homogeneous and heterogeneous nucleation with equal probability. The desired texture is then transmitted from heterogeneously nucleated epitaxial grains throughout the volume of the film upon sintering. Crystallization of CeO₂ under the reducing atmospheric conditions of Ar/5 % H₂ results in a nanometric granular microstructure with a high concentration of C impurities decorating grain boundaries and interstitial cavities, which unexpectedly prevails after high‐temperature annealing. Post‐processing in oxidizing conditions removes C impurities and promotes grain growth resulting in a fully epitaxial film, as well as stabilizing the otherwise energetically prohibitive polar (001) planes. Misfit stresses in the post‐processed epitaxial films are completely relieved by interfacial dislocations with b = (a/2) < 110 > and b = (a/2) < 011 > Burgers vectors. A mechanism that considers impurity‐induced grain‐boundary blocking and the stabilization of (001) planes via surface oxidation is proposed. Processing conditions to obtain high‐quality CeO₂ buffer layers can be adapted to YBa₂Cu₃O₇‐coated conductors.     

Effects of oxygen on crystallization of amorphous silicon films and polysilicon TFT characteristics

Oxygen ions were implanted into the amorphous silicon film deposited at 540°C in order to study the effects of oxygen on the solid phase crystallization of silicon films. The resulting films were investigated using transmission electron microscopy, x-ray diffraction (XRD), and also by measuring the electrical characteristics of polycrystalline silicon thin film transistors (TFTs) fabricated in the crystallized films. The development of {111} texture as a function of annealing time is similar to films implanted with Si, with higher oxygen samples showing more texture. Transmission electron microscopy shows that the grain size of completely crystallized films varies little with oxygen concentration. The electrical performances of TFTs are found to degrade with increasing oxygen dose. The trap state density increases from 5.6 × 10¹²/cm² to 9.5 × 10¹²/cm² with increasing oxygen dose. It is concluded that for a high performance TFT, oxygen incorporation in the Si film should be kept to 10¹⁹/cm³ or less.     

Characterization of the YbBa2Cu3O7-y and YBa2Cu3O7-y thin superconducting films prepared by chemical solution deposition on MgO(001) substrate

Thin superconducting films of the YbBa2Cu3O7-y (Yb123) and YBa2Cu3O7-y (Y123), prepared by post-deposition annealing of the metal naphthenates gels spin-coated on MgO(001) substrate, have been characterized by cross-sectional high-resolution electron microscopy and X-ray diffraction. It was found that the c-axis Yb123 films were epitaxially grown on the MgO(001) substrate at the temperature range from 700 degrees C to 775 degrees C in a gas mixture containing Ar and O2 with the oxygen partial pressure of p(O2) = 10(-4) atm. In contrast to the Yb123 films, it was found that Y123 films could be derived at a wider temperature range from 750 degrees C to 950 degrees C. Randomly oriented Y123 films were also grown on the MgO(001) substrate besides the majority of in-plane c-axis oriented growth.     

Recrystallization by annealing in SiC amorphized with Ne irradiation

Alpha-silicon carbide was irradiated with Ne+ ions at room temperature to various fluences up to 7.5 x 10(20) Ne+ m(-2) and then isochronally annealed under observation with a transmission electron microscope. In all cases, thin regions were completely amorphized by irradiation and epitaxial growth occurred from the residual crystalline region by subsequent annealing. Crystal nucleation occurred with annealing at 1000 degrees C in the cases of 3.8 x 10(20) and 7.5 x 10(20) Ne+ m(-2) irradiation, and at 1100 degrees C in the cases of 1.3 x 10(20) and 2.3 x 10(20) Ne+ m(-2) irradiation. Growth or formation of bubbles was observed with annealing at 1000 degrees C after 1.3 x 10(20), 2.3 x 10(20), and 3.8 x 10(20) Ne+ m(-2) irradiation.     

Nanostructure of Er3+ doped silicates

We demonstrate nanostructural evolution resulting in highly increased photoluminescence in silicates doped with Er3+ ions. High-resolution transmission electron microscopy (HRTEM) imaging, nano-energy dispersed X-ray (NEDX) spectroscopy, X-ray diffraction (XRD) and photoluminescence analysis confirm the local composition and structure changes of the Er3+ ions upon thermal annealing. We studied two types of amorphous nanopowder: the first is of the composition SiO2/18Al2O3/2Er2O3 (SAE), synthesized by combustion flame-chemical vapor condensation, and the second is with a composition of SiO2/8Y2O3/2Er2O3 (SYE), synthesized by sol-gel synthesis (composition in mol%). Electron diffraction and HRTEM imaging clearly show the formation of nanocrystallites with an average diameter of approximately 8 nm in SAE samples annealed at 1000 degrees C and SYE samples annealed at 1200 degrees C. The volume fraction of the nanocrystalline phase increased with each heat treatment, eventually leading to complete devitrification at 1400 degrees C. Further XRD and NEDX analysis indicates that the nanocrystalline phase has the pyrochlore structure with the formula Er(x)Al(2-x)Si2O7 or Er(x)Y(2-x)Si2O7 and a surrounding silica matrix.     

Tuning the Dimensions of C60‐Based Needlelike Crystals in Blended Thin Films

A new ordered structure of the C₆₀ derivative PCBM ([6‐6]‐phenyl C₆₁‐butyric acid methyl ester) is obtained in thin films based on the blend PCBM:regioregular P3HT (poly(3‐hexylthiophene)). Rapid formation of needlelike crystalline PCBM structures of a few micrometers up to 100 μm in size is demonstrated by submitting the blended thin films to an appropriate thermal treatment. These structures can grow out to a 2D network of PCBM needles and, in specific cases, to spectacular PCBM fans. Key parameters to tune the dimensions and spatial distribution of the PCBM needles are blend ratio and annealing conditions. The as‐obtained blended films and crystals are probed using atomic force microscopy, transmission electron microscopy, selected area electron diffraction, optical microscopy, and confocal fluorescence microscopy. Based on the analytical results, the growth mechanism of the PCBM structures within the film is described in terms of diffusion of PCBM towards the PCBM crystals, leaving highly crystalline P3HT behind in the surrounding matrix.     

Textural and microstructural transformation of Cu damascene interconnects after annealing

Influence of annealing on the textural and microstructural transformation of Cu interconnects having various line widths is investigated. Two types of annealing steps have been considered here: room temperature over 6 months and 200°C for 10 min. The texture was determined by x-ray diffraction (XRD) of various cross-sectional profiles after electropolishing, and the surface, microstructure, and grain boundary character distribution (GBCD) of Cu interconnects were characterized using electron backscattered diffraction (EBSD) techniques. In order to analyze a relationship between the stress distribution and textural evolution in the samples, microstresses were calculated with decreasing line widths at 200°C using finite element modeling (FEM). In this investigation, it was found that the inhomogeneity of stress distribution in Cu interconnects is an important factor, which is necessary for understanding textural transformation after annealing. A new interpretation of textural evolution in damascene interconnects lines after annealing is suggested, based on the state of stress and the growth mechanisms of Cu electrodeposits.     

Texture and microstructure of thin copper films

Microstructure is an important factor influencing the reliability of thin film interconnects. The microstructure of copper films is of particular interest because of its use in numerous electronic applications. Pole figure x-ray diffraction and transmission electron microcopy were conducted on copper films deposited by several techniques: sputtering, partially ionized beam deposition, chemical vapor deposition, evaporation, and electroplating. Quantitative texture data are determined from fiber texture plots. A typical copper film consists of three texture components: (111), (200), and random. (220) and (511) texture components are possible under some deposition conditions. Compared to aluminum films, the fraction of the random texture component and the distribution of the (hkl) components in copper films are relatively large. Bimodal grain size distributions are observed in some films.     

原位背散射电子衍射研究压缩变形过程中AZ31合金的微观组织演变

本文采用原位背散射电子衍射(原位-EBSD)方法研究了AZ31合金在压缩应力下的微观组织演变。结果表明{10 12}[1011]孪生是主要的变形模式。该孪生模式导致了变形后晶体取向发生了明显的转变,由原始取向为其C轴垂直于挤压方向ED的丝织构,转变为其C轴平行于ED及压缩应力方向。同时位错滑移也提供了一定的变形量。AZ31合金中RD和TD织构组分的梯度对于压缩变形条件下的孪生变形没有明显的影响。     

Investigation of polycrystalline silicon layers by electron microscopy and x-ray diffraction

The structure of polycrystalline Si layers deposited by pyrolysis of silane in a hydrogen ambient has been investigated by replica electron microscopy and X-ray diffraction. When the gas flow ratio (SiH₄/H₂) is 3·64 × 10⁻⁴ the temperature region below 900°C is a surface reaction control region and the activation energy of the chemical surface reaction rate is 1·6 eV. The temperature range above 900°C is a mass transfer region and the deposition rate is about 500 Å/min. The grains become larger and the texture of the surface of the poly Si layers becomes coarser with the deposition temperature. Some phase change was found to occur around 900°C by replica electron microscopy. The X-ray diffraction experiments show that there exist three preferred orientations of (220), (111) and (311) in the poly Si layers. The decrease of the relative intensity of the (311) orientation might have a relation to the phase change around 900°C.     

Iron-Doped,Mullite-Impregnated PVDF Composite: An Alternative Separator for a High Charge Storage Ceramic Capacitor

In this communication, the formation mechanism of the electroactive β phase, morphology and the dielectric activities of increasing doping concentration (0–1.2 M.W % of mullite) of Fe²⁺ ion-doped, mullite-impregnated polyvinylidene fluoride (PVDF) nanocomposite have been investigated. Differential thermal analysis (DTA) confirms the formation of an electroactive β phase, and Fourier transform infrared spectroscopy (FTIR) showed that the β phase increases simultaneously and attains the maximum increment of 2.6 times compared to pristine PVDF. X-ray diffraction (XRD) spectra also agreed well with the β-phase increment behaviour and also confirmed the presence of required mullite phases. Field emission scanning electron microscopy (FESEM) images indicate the strong interaction between the polymer matrix and different concentrations of Fe²⁺ ion-doped mullite particles, resulting in enhanced electroactive β phase formation and large dielectric constant of the nanocomposite films followed by significant low dielectric loss with high ac conductivity compared to pristine PVDF films at room temperature. This doped polymer composite can be used as a high dielectric separator and, using this separator, we have successfully fabricated a high-charge-storage device. This paper also demonstrates that the loading of conductive Fe²⁺ ions within the highly insulating mullite matrix has a critical concentration for the enhancement and nucleation of the electroactive β phase of the PVDF polymer. In this critical concentration, the highest formation of a β network and maximum numbers of homogeneously distributed iron-doped mullite (FeM) particles in PVDF matrix improves the effective interfacial polarization by Maxwell–Wagner–Sillar (MWS) polarization effect which is responsible for the enhancement of dielectric constant and ac conductivity followed by significant tangent loss. So, it can be concluded that the incorporation of Fe²⁺-doped mullite into PVDF matrix is an effective way to fabricate a high dielectric separator of high-charge-storage electronic devices.     

高纯钽交叉轧制过程中微观结构和织构梯度的演变

高纯钽板在交叉轧制过程中,通过控制轧制的道次,得到了70％,82％和87％变形量的样品.应用X-射线衍射(XRD)技术测量了轧制样品1/8厚度层,1/4厚度层和中间层的宏观织构,并对样品沿厚度方向上的变形组织与微织构进行电子背散射衍射(EBSD)表征.结果表明,随着交叉轧制变形量的增加,{111} 和{100}取向晶粒的取向分裂程度增加,并且{111}取向的晶粒分裂程度高于{100}取向的晶粒.变形量为70％时,高纯钽板沿厚度方向存在强烈的微观组织和织构梯度,中间层具有强烈的{111}取向晶粒,而1/8厚度层主要为{100} 取向.随着变形量增加,高纯钽板沿厚度方向的微观组织和织构均匀性得到改善.当变形量达到87％时,表面和中心的{100} 和{111} 取向晶粒都为长条状且交互分布在一起,使得钽板沿厚度方向织构梯度得到减弱,同时获得均一的晶粒尺寸.     

Cover Picture: Tuning the Dimensions of C60‐Based Needlelike Crystals in Blended Thin Films (Adv. Funct. Mater. 6/2006)

A new ordered structure of the C₆₀ derivative PCBM is obtained in thin films based on the blend PCBM:P3HT, as detailed by Swinnen, Manca, and co‐workers on p. 760. Needlelike crystalline PCBM structures, whose dimensions and spatial distribution ca be tuned by adjusting the blend ratio and annealing conditions, are formed. In typical solar‐cell applications of these blended films, these results indicate that during long‐term operation under normal conditions (50–70 °C) morphology changes and a decrease in cell performance could occur. A new ordered structure of the C₆₀ derivative PCBM ([6‐6]‐phenyl C₆₁‐butyric acid methyl ester) is obtained in thin films based on the blend PCBM:regioregular P3HT (poly(3‐hexylthiophene)). Rapid formation of needlelike crystalline PCBM structures of a few micrometers up to 100 μm in size is demonstrated by submitting the blended thin films to an appropriate thermal treatment. These structures can grow out to a 2D network of PCBM needles and, in specific cases, to spectacular PCBM fans. Key parameters to tune the dimensions and spatial distribution of the PCBM needles are blend ratio and annealing conditions. The as‐obtained blended films and crystals are probed using atomic force microscopy, transmission electron microscopy, selected area electron diffraction, optical microscopy, and confocal fluorescence microscopy. Based on the analytical results, the growth mechanism of the PCBM structures within the film is described in terms of diffusion of PCBM towards the PCBM crystals, leaving highly crystalline P3HT behind in the surrounding matrix.     

Effect of annealing temperature on structural,electrical and optical properties of spray pyrolytic nanocrystalline CdO thin films

Nanocrystalline CdO thin films were prepared onto a glass substrate at substrate temperature of 300 °C by a spray pyrolysis technique. Grown films were annealed at 250, 350, 450 and 550 °C for 2.5 h and studied by the X-ray diffraction, Hall voltage measurement, UV-spectroscopy, and scanning electron microscope. The X-ray diffraction study confirms the cubic structure of as-deposited and annealed films. The grain size increases whereas the dislocation density decreases with increasing annealing temperature. The Hall measurement confirms that CdO is an n-type semiconductor. The carrier density and mobility increase with increasing annealing temperature up to 450 °C. The temperature dependent dc resistivity of as-deposited film shows metallic behavior from room temperature to 370 K after which it is semiconducting in nature. The metallic behavior completely washed out by annealing the samples at different temperatures. Optical transmittance and band gap energy of the films are found to decrease with increasing annealing temperature and the highest transmittance is found in near infrared region. The refractive index and optical conductivity of the CdO thin films enhanced by annealing. Scanning electron microscopy confirms formation of nano-structured CdO thin films with clear grain boundary.     

Effect of Temperature on Structural and Morphologic Properties of ZnO Films Annealed in Ammonia Ambient

ZnO thin films were prepared on Si(111) substrates by pulsed laser deposition (PLD). Then, the samples were annealed at different temperatures in NH₃ ambient and their properties were investigated particularly as a function of annealing temperature. The structure, morphology, and optical properties of ZnO films were studied by x-ray diffraction (XRD), Fourier transform infrared spectroscope (FTIR), scanning electron microscope (SEM), and photoluminescence (PL). The results show that the increase of annealing temperature makes for the improvement in the crystal quality and surface morphology below the temperature of 650°C. However, when the annealing temperature is above 650°C, the ZnO films will volatilize and, especially at 750°C, ZnO will volatilize completely.     

Polymeric synthesis of silicon carbide with microwaves.

The aim of this work is conducting polymeric synthesis with microwaves for producing beta-SiC. A polymeric precursor was prepared by means of hydrolysis and condensation reactions from pheniltrimethoxysilane, water, methanol, ammonium hydroxide and chloride acid. The precursor was placed into a quartz tube in vacuum; pyrolysis was carried out conventionally in a tube furnace, and by microwaves at 2.45 GHz in a multimode cavity. Conventional tests took place in a scheme where temperature was up to 1500 degrees C for 120 minutes. Microwave heating rate was not controlled and tests lasted 60 and 90 minutes, temperature was around 900 degrees C. Products of the pyrolysis were analyzed by means of x-ray diffraction; in the microwave case the diffraction patterns showed a strong background of either very fine particles or amorphous material, then infrared spectroscopy was also employed for confirming carbon bonds. In both processes beta-SiC was found as the only produced carbide.     

Genetic-based fuzzy hit-or-miss texture spectrum for textureanalysis

A new method using a fuzzy hit-or-miss transform recognition procedure, which measures degrees of fit of specified patterns within an image, is proposed for texture analysis. For a given texture, three optimal texture patterns (structuring elements) dynamically generated by genetic algorithms are used to inspect the degrees of fit by using the fuzzy hit-or-miss transform, respectively. The distribution of these degrees of fit, converted into a texture spectrum, is used as the texture feature for texture analysis     

Interpretation of texture changes during self-annealing of electroplated copper

Electroplating of copper is widely used for the fabrication of interconnections of printed circuit boards, in which via-holes are used to connect conductive layers. Self-annealing is an important feature of electroplated copper which significantly alters its microstructures. The degradation of 〈1 1 0〉 texture and the enhancement of 〈3 1 1〉 texture in electroplated copper during self-annealing process are observed by X-ray diffraction (XRD) and electron backscattering diffraction (EBSD). The mechanism of this transformation is discussed and illustrated.     

Preferred orientation of Cu(In,Ga)Se2 thin film deposited on stainless steel substrate

The influences of process parameters and Fe diffusing into Cu(In,Ga)Se₂ (CIGS) films on the orientation of CIGS absorbers grown on the stainless steel (SS) foils are investigated. The structural properties, morphology, and elemental profiles are characterized using X‐ray diffraction, scanning electron microscopy, and second ion mass spectroscopy, respectively. The orientation of CIGS thin films on the SS substrates strongly depends on the texture of the (In,Ga)₂Se₃ precursor, determined by the substrate temperature at the first stage (Ts1) and the flux ratio of Se to (In + Ga). Among these factors, Ts1 is the prerequisite to achieve [300]‐oriented IGS layer, which will yield [200]‐oriented CIGS thin film in the later process. The results indicate that through the comparison of CIGS thin films on the Mo/SS substrates and on the Mo/ZnO/SS substrates and combined with simply calculation, Fe diffusing into the CIGS layer will hinder the growth of the CIGS grains along [112] orientation. The grazing‐incidence X‐ray diffraction results suggest that the surface of the [220]‐textured CIGS thin film on the SS substrate still has [220] predominance, whereas the surface texture of the [220]‐texture CIGS thin film on the Mo/soda‐lime glass substrate became [112] predominant, which is due to the different compensation ability between Fe and Na elements. Finally, the relations between the device parameters and the degrees of the preferred orientation of CIGS absorbers are investigated. Copyright © 2012 John Wiley & Sons, Ltd.