KTN thin films prepared by pulsed laser deposition on transparent single crystal quartz(100)

Using the Sol-Gel method to produce the KTN ultrafine powder and the sintering technique with K2O atmosphere to prepare KTN ceramics as the targets instead of the KTN single crystal, highly oriented KTN thin films were produced on the transparent single crystal quartz (100) by the pulsed laser deposition (PLD). Since the thermal stress sustained by the quartz is relatively small, the limit temperature of the quartz substrates (300℃) is much lower than that of the P-Si substrates (560℃); the prepared thin film is at amorphous state. Increasing the pulsed laser energy density in the process incorporated with annealing the film after deposition at different temperatures converts the amorphous films into crystal. The optimal pulsed laser energy density and annealing temperature were 2.0 J/cm2 and 600℃, respectively. A discussion was made to understand the mechanism of film production at relatively low substrate temperature by PLD and effects of the annealing temperatures on the forming of the perovskite p     

Formation of nano-crystalline and amorphous phases on the surface of stainless steel by Nd:YAG pulsed laser irradiation

Thin surface layers consisting of nano-crystalline and amorphous phases on the surface of stainless steel have been attained under the Nd:YAG pulsed laser irradiation. The phases and microstructures were investigated by X-ray diffraction (XRD) and high resolution transmission electron microscope (HRTEM). The phase compositions of the surface determined by XRD were α-Fe (ferrite) and γ-Fe (austenite) or only γ-Fe in the near surface region on the bases of the different laser power densities. The nano-crystalline grains with sizes of 4-100 nm could result from high cooling rate and crystallization in amorphous region by homogeneous and heterogeneous nucleation. The formation of the amorphous phase was attributed to the higher cooling rates.     

A model for the interaction of near-infrared laser pulses with metal powders in selective laser sintering

A thermal model of the interaction of pulsed near-infrared laser radiation from a Nd:YAG laser was made, taking the measured powder properties such as reflectance, optical penetration depth and thermal conductivity into account. It allows an estimation of the evolution of two different temperatures: the average temperature of the powder (taken over the grains in a volume given by the laser beam diameter and the optical penetration depth) and the temperature distinction within a single grain. It showed that in pulsed mode consolidation can be achieved at much lower average power as the surface of the powder particles are molten but their cores remain at nearly room temperature. This leads to a much lower average temperature and therefore a dramatic decrease in residual thermal stresses in the finished piece. The results of the model were experimentally tested and confirmed. Received: 26 July 2001 / Accepted: 23 November 2001 / Published online: 23 January 2002     

Modelling of the thermal processes that occur during laser sintering of reacting powder compositions

A two-dimensional mathematical model has been developed to describe simultaneous self-propagating high-temperature synthesis (SHS) and selective laser sintering (SLS) of powder compositions. The models applicability is limited by the magnitude of laser irradiation. It allows a comparison to be made between product geometry and the velocity of the laser irradiation spot. PACS 81.20.ka; 81.05.bx; 81.05.Zx     

Synthesis and characterization of precipitation hardened amorphous matrix composite by mechanical alloying and pulse plasma sintering of Al65Cu20Ti15

This study reports synthesis of Al₆₅Cu₂₀Ti₁₅ amorphous alloy by mechanical alloying and consolidation of the powder mass by pulsed plasma sintering. During sintering, several intermetallic phases precipitate from the amorphous matrix and cause a significant increase in nano-hardness and elastic modulus. Microstructure in as-milled and sintered conditions was characterized by X-ray diffraction, scanning/transmission electron microscopy and differential scanning calorimetric. Among various conditions of sintering, the composites pulse plasma, sintered at 500°C, show the high compression strength (1745 MPa) and high indentation fracture toughness (4.96 MPa m^1/2); although, the maximum density (3.73 Mg/in³), nano-hardness (14 GPa) and Young's modulus (208 GPa) in the present alloy have been obtained in the composites pulse plasma sintered at 600°C.     

Nanosize silicon nitride: characteristic of doped powders and of the related sintered materials

The paper reports on both the characteristics of ultrafine silicon nitride powder produced by plasma synthesis and the microstructure and properties of the relative sintered material. The powder, already containing yttria and alumina as sintering aids, has a bimodal particle size distribution and it is partly amorphous. The chemical composition and morphology of the particles are shown. Yttria and alumina were not found in separate particles but the elements constituting them (i.e., Y, Al, O) are either in solid solutions in the crystalline particles or dispersed within the amorphous portion of the powder. Dense materials were obtained by pressureless sintering at 1750 °C. Microstructure and composition of silicon nitride grains and of grain boundary phases are analyzed and discussed. When compared to a micro-sized Si₃N₄, nanoindentation tests clearly revealed the inverse Hall Petch relation. The nanosize Si₃N₄ shows a Young’s modulus which is almost independent on the peak load. PACS 81.05.J,M; 81.40; 81.05.Y; 81.05.J; 46.30.P     

Ceramic components manufacturing by selective laser sintering

In the present paper, technology of selective laser sintering/melting is applied to manufacture net shaped objects from pure yttria-zirconia powders. Experiments are carried out on Phenix Systems PM100 machine with 50 W fibre laser. Powder is spread by a roller over the surface of 100 mm diameter alumina cylinder. Design of experiments is applied to identify influent process parameters (powder characteristics, powder layering and laser manufacturing strategy) to obtain high-quality ceramic components (density and micro-structure).The influence of the yttria-zirconia particle size and morphology onto powder layering process is analysed. The influence of the powder layer thickness on laser sintering/melting is studied for different laser beam velocity V (V = 1250-2000 mm/s), defocalisation (−6 to 12 mm), distance between two neighbour melted lines (so-called “vectors”) (20-40 μm), vector length and temperature in the furnace. The powder bed density before laser sintering/melting also has significant influence on the manufactured samples density.Different manufacturing strategies are applied and compared: (a) different laser beam scanning paths to fill the sliced surfaces of the manufactured object, (b) variation of vector length (c) different strategies of powder layering, (d) temperature in the furnace and (e) post heat treatment in conventional furnace. Performance and limitations of different strategies are analysed applying the following criteria: geometrical accuracy of the manufactured samples, porosity. The process stability is proved by fabrication of 1 cm³ volume cube.     

Features of the microstructure of Ti–Nb alloy obtained via selective laser melting

Ti–Nb alloy with 40 wt % of Nb is obtained from a composite Ti–Nb powder by means of selective laser melting. The Ti–Nb alloy has a two-phase microstructure. The main β-phase of the solid titanium–niobium solution forms grains ranging in size from ~2 to 20 μm. A nonequilibrium α″-phase is found in the forms of lamellar, globular, and packet martensite inside the grains of the β-phase and along their boundaries.     

选区激光烧结瞬态温度场模拟与测试方法研究

采用有限元方法,考虑实际的边界条件和热物性参量的变化,对Al2O3覆膜陶瓷粉末的选区激光烧结过程瞬态三维温度场进行动态模拟.通过比色测温法对红外热成像系统的发射系数进行修正后,对选区激光烧结过程瞬态温度场进行测试.数值模拟和实测结果显示,两者吻合较好.     

Alumina-zirconium ceramics synthesis by selective laser sintering/melting

In the present paper, porous refractory ceramics synthesized by selective laser sintering/melting from a mixture of zirconium dioxide, aluminum and/or alumina powders are subjected to optical metallography and X-ray analysis to study their microstructure and phase composition depending on the laser processing parameters. It is shown that high-speed laser sintering in air yields ceramics with dense structure and a uniform distribution of the stabilizing phases. The obtained ceramic-matrix composites may be used as thermal and electrical insulators and wear resistant coating in solid oxide fuel cells, crucibles, heating elements, medical tools. The possibility to reinforce refractory ceramics by laser synthesis is shown on the example of tetragonal dioxide of zirconium with hardened micro-inclusion of Al₂O₃. By applying finely dispersed Y₂O₃ powder inclusions, the type of the ceramic structure is significantly changed.     

Titanium and aluminum nitride synthesis via layer by layer LA-CVD

The possibility of the layer-by-layer synthesis of 3D parts from nitrides of titanium or aluminum by selective laser sintering/melting is discussed. The relationship between laser processing parameters and structure and phase content of sintered/melted samples are studied by means of optical metallography, X-ray diffraction, scanning electron microscopy and energy dispersive X-ray analysis. Optimal parameters of SLM process for AlN and TiN synthesis are determined. Solid 3D parts containing a TiN phase are produced from Ti powder. Distortion of the crystalline lattice of AlN and TiN phases is observed with the laser energy input.     

Preparation and characterization of pulsed laser deposition (PLD) SiC films

Si K-edge XAFS was used to characterize a stoichiometric SiC film prepared by pulsed KrF laser deposition. The film was deposited on a p-type Si(1 0 0) wafer at a substrate temperature of 250 °C in high vacuum with a laser fluence of ∼5 J/cm². The results reveal that the film contains mainly a SiC phase with an amorphous structure in which the Si atoms are bonded to C atoms in its first shell similar to that of crystalline SiC powder but with significant disorder.     

Silicon grain arrays prepared using a pattern crystallization technique of pulsed-excimer laser irradiation

Silicon grain arrays were prepared using a pattern crystallization technique of pulsed KrF excimer laser irradiation. The precursor material was hydrogenated amorphous silicon (a-Si:H) thin films deposited on single crystal Si wafers by plasma-enhanced chemical vapor deposition. It was shown that Si grains with a uniform size and a well-defined periodicity embedded in the a-Si:H matrix were obtained by this simple technique. The grain size was less than 2 μm. Relativly strong photo-luminescence with two peaks at 720 and 750 nm was observed at room temperature. We expect to reduce Si grain sizes by optimizing the growth conditions of a-Si:H thin films and controlling the temperature distribution in the film during laser irradiation. Received: 21 November 2000 / Accepted: 12 December 2000 / Published online: 9 February 2001     

Laser sintering of green compacts

Green Compact Laser Sintering (GCLS) is a new technique for sintering powder metallurgical components by laser irradiation. After mixing; powders are pressed into a green compact; which can then be sintered by laser irradiation. The properties of powder metallurgical alloys for GCLS and conventional sintering are compared.     

Low temperature nanoparticle sintering with continuous wave and pulse lasers

New manufacturing methods are being sought for electronics production. Printable electronics is a promising method for producing low cost and large-scale electronics. In printable electronics nanoparticle inks printed on the surface of substrate contain additives, such as dispersing agent and carrier fluids that provide good printing properties by changing the viscosity and separating the nanoparticles of the ink. In the sintering process ink particles are heated to a certain, ink-specific temperature. During the sintering process the carrier fluid and dispersing agents are evaporated from the ink. Additional heating after evaporation causes the nanoparticles to start to agglomerate. A small particle size allows the use of a considerably lower sintering temperature than with bulk silver, for example 220 °C. The sintering process is usually utilized with a convection oven, with a long sintering time, and the thermal load on the surrounding material can become too great as components and patterns are formed from layers of different type inks. Hence, alternative sintering methods are sought. This paper describes tests done with two different types of laser; pulsed and continuous wave lasers. Laser sintering enables short sintering times and selective sintering, making it possible for printed structures to contain fragile active components produced with other technologies.     

Synthesis of Ca-P nanoparticles and fabrication of Ca-P/PHBV nanocomposite microspheres for bone tissue engineering applications

As the first step in producing totally bioresorbable osteoconductive composite scaffolds for bone tissue engineering using the selective laser sintering technology, bioresorbable nanoparticles of calcium phosphate (Ca-P) similar in composition to β-tricalcium phosphate were synthesized and Ca-P nanoparticle filled poly(hydroxybutyrate-co-hydroxyvalerate) (PHBV) microspheres were fabricated. The pH of the chemical reaction for Ca-P particle synthesis was found to have significant effects on the morphology and chemical composition of Ca-P precipitated. Ca-P particles produced at the pH of 10.0-11.0 were amorphous, had a Ca:P molar ratio of about 1.5, were spherical in shape and had sizes in the range of 10-30 nm. The Ca-P particles were used to form Ca-P nanocomposite microspheres through a solid-in-oil-in-water (S/O/W) emulsion solvent evaporation process. Ca-P nanoparticles were mostly encapsulated inside the microspheres and some Ca-P nanoparticles were superficially embedded on the microspheres. The Ca-P/PHBV microspheres had an average diameter of about 48 μm which is suitable for selective laser sintering for constructing osteoconductive composite scaffolds.     

多晶金刚石烧结中晶粒表面石墨化的实验研究

 利用X射线微区衍射，X射线光电子谱（XPS）及激光拉曼光谱等分析，对高温高压下以金刚石微粉为原料的多晶金刚石烧结过程中，金刚石晶粒表面石墨化现象进行了考察。结果表明，虽经历了烧结过程，但在没有掺杂剂作用的区域内，没有发现金刚石晶粒表面的石墨化。晶粒表面石墨化的高峰期，处于掺杂剂刚开始液化，但尚未饱和充填金刚石晶粒间空隙的烧结初期阶段，随着液相掺杂剂的饱和充填作用，金刚石晶粒表面的石墨消失，并最终完成多晶金刚石的烧结。     

3D modeling and testing of transient temperature in selective laser sintering (SLS) process

In the process of rapid prototyping by the method of selective laser sintering (SLS), transient temperature has direct effect upon the sintering performance. In the present work, a model is developed in order to generate 3D transient temperature field. It uses Al₂O₃ coated ceramic powder and involves the finite element method (FEM) variation of thermal properties and solid–liquid two-phase interface. A high-speed charge coupled device (CCD) image temperature measurement system is used to generate for testing. The obtained test results validates the simulation data and implies that the proposed modeling method is useful in simulating the transient sintering temperature specially when the correct thermal properties and key factors of two-phase interface are main concerns. The performance characteristics of the reasonable sintering parameters are predicted by the proposed modeling method.     

First photoconductivity measurement following photoionization of rare-earth dopant in a dielectric powder

Transient response of the dielectric permittivity of dielectric powder of LSO:Ce³⁺ under pulsed laser excitation were recorded by the 8-mm microwave resonator technique at room temperature. The signal in absorption mode is the signature of Ce³⁺ photoionization and photoconductivity effect in the rare-earth-doped dielectric grains. The signal in dispersion mode results from surface defects around each grain leading to electronic traps. This opens new perspectives for photoconductivity measurements on rare-earth-doped insulating nanopowders.