Chemical composition analysis for laser solid forming of titanium alloys from blended elemental powders

Laser solid forming （LSF） from blended elemental powders is an advanced technique to investigate new alloy systems and to create innovative materials. Accurate composition control is critical for the applications of this technique. In this letter, the composition analysis is performed on LSF titanium alloys from blended Ti, Al, and V powders. It is found that the composition of as-deposited sample can be controlled by keeping the identity of the divergence angle of each elemental powder stream. Based on the consistency condition for divergence angles of different elemental powder streams, the matching relation among the Ti, Al, and V powder characteristics （particle size and density） can be obtained, which ensures the consistency in composition between the laser deposits and the blended elemental powders under different laser processing parameters.     

Microstructure evolution of laser solid forming of Ti-Al-V ternary system alloys from blended elemental powders

Morphology evolution of prior β grains of laser solid forming (LSF) Ti-xAl-yV (x 11,y 20) alloys from blended elemental powders is investigated. The formation mechanism of grain morphology is revealed by incorporating columnar to equiaxed transition (CET) mechanism during solidification. The morphology of prior β grains of LSF Ti-6Al-yV changes from columnar to equiaxed grains with increasing element V content from 4 to 20 wt.-%. This agrees well with CET theoretical prediction. Likewise, the grain morphology of LSF Ti-xAl-2V from blended elemental powders changes from large columnar to small equiaxed with increasing Al content from 2 to 11 wt.-%. The macro-morphologies of LSF Ti-8Al-2V and Ti-11Al-2V from blended elemental powders do not agree with CET predictions. This is caused by the increased disturbance effects of mixing enthalpy with increasing Al content, generated in the alloying process of Ti, Al, and V in the molten pool.     

Anisotropy models in precise crystallite size determination of mechanically alloyed powders

Nanocrystalline AA 4032 alloy powder was synthesized by high-energy ball milling from elemental powders for 30 h duration. XRD and TEM results reveal that the powder is cubic and nanocrystalline in nature. X-ray peak broadening analysis was used to evaluate the lattice strain and the crystallite size using the Williamson-Hall analysis with three different models viz., uniform deformation, uniform deformation stress and uniform deformation energy density. The root mean square (RMS) strain was calculated from the interplanar spacing and the strain estimated from the three models. The three models yield different strain values due to the anisotropic nature of the material. The energy density model is proposed to be the best fit model among the three as severe lattice strain is associated with ball milled powders.     

显微红外反射光谱法快速鉴别珍珠粉真伪

珍珠是名贵的装饰品和中药材,在我国对其已有2000多年的应用历史。研究发现,贝壳内层的化学组成与珍珠相似,主要含有碳酸钙和各种氨基酸。贝壳粉也可在临床上做药用,但其药用价值远低于珍珠粉。然而,珍珠粉和贝壳粉外观特性极为相似,元素组成和形貌检测无法对其进行有效地鉴别。由于贝壳粉的成本低,常常冒充珍珠粉流入市场,侵害了消费者的利益。本研究通过珍珠粉和贝壳粉在不同温度下煅烧一定时间后显微红外反射光谱的差异实现珍珠粉真伪鉴别。实验结果表明,在一个大气压下经过400 ℃煅烧30 min后,珍珠粉中文石型碳酸钙部分转化为方解石型,而贝壳粉中文石型碳酸钙完全转化为方解石型。这种不同的相转变过程可以被显微红外反射光谱很好的区别。因此,可在此条件下利用红外反射光谱鉴别珍珠粉和贝壳粉相变差异。和传统的透射式红外光谱法相比,这种显微反射红外光谱法无需压片制样、快速灵敏。本研究也讨论了该方法针对其他常见伪品的适用性,如牡蛎粉和石决明粉,结果表明该方法能够简单、高效和准确地鉴别珍珠粉真伪。     

Effect of Addition of Process Control Agent (PCA) on the Nanocrystalline Behavior of Elemental Silver during High Energy Milling

Mechanical Alloying (MA) or High Energy Milling has been a subject of great interest for last few decades. However, in the majority of the cases the investigations are confined to areas like alloying in binary or multi-component systems from premixed powders. Very little work has been reported on high-energy milling of pure metals. There are some reports on mechanical alloying of pure metals that undergo polymorphic transformation on milling, but relatively few papers have been reported in the literature pertaining to attrition milling of pure metals, which do not fall under this category. One such attempt has been made in this investigation by subjecting a noble metal like silver with fcc crystal structure to attrition milling. The present work deals with the investigation of the effect of addition of a process control agent (PCA) on the nanocrystalline behavior of elemental silver powder subjected to high energy milling in an attritor. Elemental silver powder was subjected to attrition milling with and without addition of stearic acid as PCA. The powder samples drawn at periodic intervals during the course of milling were subjected to characterization using techniques like XRD, SEM and DSC. The variation in particle shape morphology, crystallite size and lattice strain as a function of PCA was studied.     

Comparison of ball milling of Fe/Cr powders and Fe-Cr crystalline alloy

Using the mechanical attrition technique (MA), we have prepared a Fe-Cr alloy starting with a mixture of elemental iron and chromium powders with a nominal composition of 28 at% of Fe and 72 at% of Cr. MA was also performed on solid solutions of Fe₂₈Cr₇₂ crystalline alloy. The Mössbauer effect of the mechanically alloyed powder from Cr and Fe metals has been compared with that from crystalline alloy.     

Synthesis of Cu2ZnSnSe4 compound powders by solid state reaction using elemental powders

The solid state reaction method was used to synthesize single phase and near stoichiometric Cu₂ZnSnSe₄ compound from elemental Cu, Zn, Sn and Se powders in a quartz tube furnace under an Ar flow at atmospheric pressure. These elemental powders were initially milled using zirconia balls. The α-CuSe phase was present in all of the milled powders because of the mechanical alloying effect between the Cu and Se powders. The solid state reaction mechanism was examined for the synthesis process. The phase analysis suggested that the Cu₂ZnSnSe₄ powder crystallized into the stannite phase with a high degree of crystallinity after near stoichiometric molar ratios of the powders was reacted at 500 °C for 6 h. This study showed that the solid state reaction method was a straightforward technique for the synthesis of the Cu₂ZnSnSe₄ compound powders from the elemental powders.     

Impact and Static Consolidation of Mechanically-Alloyed Mixture of Copper and Graphite Powders

A mixture of copper and carbon powders was mechanically alloyed in a planetary ball mill. The supersaturated solid solubility of carbon in mechanically-alloyed copper is 25 v at% C, as determined from the lattice parameter change. The supersaturated powder consolidated by static compression at 1.4 v GPa, has the relative density of 95%, a Vickers hardness of 121, and a compressive strength of 1.4 v GPa. In contrast, powder consolidated dynamically by a 90.1 g projectile traveling at a velocity of 38.1 m/s and at an estimated impact compression of 2.3 GPa after 0.4 GPa static precompression has a relative density of 96.3% and a Vickers hardness of 200. X-ray diffraction patterns shift to higher angles after impact compression. The supersaturated solid solubility of 18 at% C in Cu+20 at% C mechanically-alloyed powders was reduced to 12.5 at% C by impact compression. Mechanically-alloyed powders can be consolidated by impact and static pressures while retaining the effects of mechanical alloying; for example, supersaturated solid solubility.     

粉末状态对激光立体成形Zr55Cu30Al10Ni5块体非晶合金晶化行为的影响

基于金属熔体结构的遗传性, 激光熔池的快速熔凝导致粉末的晶化状态可能会对最终成形件的晶化产生重要影响, 理清其影响规律对于制备大块非晶合金具有重要意义. 本文选取等离子旋转电极法所制粉末和1000 K退火态粉末为沉积材料, 采用激光立体成形技术沉积Zr₅₅Cu₃₀Al₁₀Ni₅块体非晶合金, 考察了粉末中已有晶化相对熔池及热影响区晶化行为的影响. 结果发现, 原始粉末组织由非晶相及粗大的Al₅Ni₃Zr₂相组成; 当激光线能量较低时, 相应熔覆层的熔池和热影响区皆含有Al₅Ni₃Zr₂相; 随着线能量的提高, 熔池中Al₅Ni₃Zr₂相消失, 保持了非晶态, 但热影响区晶化加重, 并有大量Al₅Ni₃Zr₂相析出; 当采用退火态粉末时, 即使线能量较小, 相应熔覆层仍主要由非晶构成, 几乎无Al₅Ni₃Zr₂相析出. 这是由于原始粉末在退火时其微观结构发生重排, 与Al₅Ni₃Zr₂相关的原子短程/中程有序结构减少, 导致已沉积层非晶区的热稳定性提高, 不利于Al₅Ni₃Zr₂相析出. 可见, 提高线能量将会加剧非晶沉积体的晶化, 而粉末中的Al₅Ni₃Zr₂团簇相状态对Zr₅₅Cu₃₀Al₁₀Ni₅合金沉积层的晶化有重要影响.     

Parametric X-ray radiation from powders

Parametric X-ray Radiation (PXR) produced in powders has been observed for the first time. PXR spectra were measured under observation angles of 150° and 180° during the interaction of relativistic 7 MeV electrons with a tungsten powder. All the PXR peaks that theoretically can be produced in the studied energy region were registered. The performed absolute comparison of the experiment with the PXR kinematical theory from randomly oriented crystallites showed a good accordance.     

Determining Contact Angles of Powders by Liquid Penetration

The wettability of a powder is important, especially in chemical and pharmaceutical technologies when considering the manufacturing process and the properties of the final product. However, contact angle methods for powders are problematic. The common measurement techniques are the sessile drop method and the liquid penetration method. In this work the determination of contact angles of powders by liquid penetration is considered. In particular, we investigated the influence of the sample preparation and sampling device on the wetting process. A bulk with constant properties during the measurement must be guaranteed. We postulate a packing procedure to obtain reproducible measurements by ensuring constant powder properties.     

NANOSTRUCTURED AND AMORPHOUS MATERIALS BY MECHANICAL ALLOYING

Mechanical Alloying is particularly attractive because it can be used to process structurally uniform and isotropic bulk quantities of powdered materials that have a fine length scale. Furthermore, it appears to be applicable to many combinations of elements. Here experimental results regarding the synthesis and characterization of several binary and ternary nanocrystalline and amorphous alloys of Ti, Zr, Hf, V, Nb and Fe with other transition elements and with B, C and Si are reported. The nanocrystalline and amorphous powders, with effective particle size between 7 and 30nm, were prepared by mechanical alloying in a high-energy ball-mill using commercial elemental powders and/or alloy powder.     

A new bistatic model for electromagnetic scattering from perfectly conducting random surfaces: numerical evaluation and comparison with SPM

This paper is a companion to our previous contribution deriving a new approximate bistatic model for electromagnetic scattering from perfectly conducting rough surfaces. We evaluate this model numerically and compare it with an 'exact' numerical solution of the scattering problem. This comparison shows good agreement between our approximation and numerical solution for a wide range of incident and scattering angles. However, for horizontal-incident horizontal-scattered polarization (HH-pol), the model exhibits strong deviation from the 'exact' solution for near-grazing scattering angles. The model shows a similar divergence at HH-pol when compared with the small-perturbation method (SPM). The cause of this divergence is explained. During the SPM comparison, we noticed that the integral equation method model also does not reproduce the SPM limit except for forward and backscatter geometries. We propose in this paper a simple modification of our model to ensure agreement with the bistatic SPM approximation when applicable, and show that the modified model also yields close agreement with numerical computations even when the surface roughness does not satisfy the SPM condition.     

A new method of flame temperature measurement utilizing the acoustic emissions from laser-induced plasmas

The optical emissions from laser-induced plasmas have been successfully exploited for elemental composition measurements in flames; however, the information from the accompanying plasma-generated acoustic emissions has not been well utilized. In this study, we investigated the influence of flame temperature and composition on the acoustic emissions from laser-induced plasmas in an ethylene-air premixed flame. The acoustic emissions are sensitive to temperature, and a negative correlation can be established. The effect of composition on acoustic emissions was found to be second order compared to that of temperature. Based on these findings, we introduce acoustic-based laser-induced breakdown thermometry (LIBT). A statistical analysis was performed to mitigate the bias introduced by anomalous extreme values. The spatial and temporal resolution of LIBT were also analyzed to demonstrate its potential to perform simultaneous composition and temperature measurements when used along with laser induced breakdown spectroscopy (LIBS). Finally, the temperature distribution in an ethylene-air counter-flow diffusion flame was measured; and the results compared favorably with numerical results.     

激光立体成形中熔池凝固微观组织的元胞自动机模拟

本文通过采用自适应网格技术, 将激光立体成形的宏观温度场模型和凝固微观组织的低网格各向异性元胞自动机模型(cellular automaton, CA)结合, 建立了适用于激光立体成形的集成数值模型. 模型包括基材的温度场分布, 熔池形貌和熔凝过程的凝固微观组织. 模拟了激光扫描速度为15 mm/s时, 激光作用在Fe-C单晶基材上形成熔池的形状以及熔池内凝固微观组织. 计算结果揭示了熔池内固液界面从平界面失稳到胞\枝晶的非稳态凝固过程, 并得到了平界面组织形成的白亮带. 白亮带上方形成了外延生长的枝晶列.     

光电成像系统动像光学传递函数

在论述光电成像系统时间响应特性图像运动的基础上,提出并完善了光电成像系统动像光学传递函数的数理模型,除已导出的匀速运动和简谐振动下的动像LSF和OTF公式外,又导出了匀加速运动下动像LSF和OTF公式以及椭圆、圆周运动下的两维动像PSF和OTF公式,从而可以全面计算、分析光电成像系统的动像传递特性,为更深入研究动态光电成像奠定了理论基础.     

A normalised residence time transport equation for the numerical simulation of combustion with high-temperature air

This study concerns the numerical simulation of turbulent non-premixed combustion in highly preheated air streams. One of the objectives is to settle an efficient computational procedure to proceed with the numerical simulation of large-scale industrial devices. It is also expected that the availability of such a computational framework may facilitate comprehensive sensitivity analyses as well as the development of mathematical models able to represent turbulence-chemistry interactions (TCI) in such conditions. Based on the salient physical ingredients that characterise scalar mixing, propagation, and self-ignition processes, a turbulent combustion modelling framework is thus introduced and applied to the numerical simulation of well-documented laboratory flames. In the corresponding geometries, the bulk flow velocities of the reactants streams can reach rather large values, which lead the flame to lift from the burner rim. Partially premixed flame edges thus stabilise the whole flame structure and the temperature of the oxidising stream can be increased by vitiation with burned gases so as to promote the corresponding flame-stabilisation processes. For sufficiently large values of the vitiated airstream temperature, self-ignition mechanisms may be triggered thus leading to a competition between mixing, propagation, and ignition processes. In this context, the ratio of the residence time to the self-ignition delay is thought to be a relevant variable to delineate the possible influence of ignition phenomena. Therefore, a modelled transport equation for this normalised residence time is considered. The performance of the corresponding modelling proposal is analysed with special emphasis placed on its ability to reproduce ‘memory’ or ‘lagrangian’ effects related to thermal aging processes. In this respect, it is noteworthy that the present set of computations makes use of tabulated quantities associated to (i) steady laminar one-dimensional diffusion flamelets, so as to describe the composition of combustion products, (ii) steady laminar one-dimensional premixed flamelets, to describe the flame brush propagation, and (iii) temporal evolution of zero-dimensional homogeneous mixtures to account for the possible occurrence of self-ignition phenomena. In particular, the tabulated self-ignition time value is used to evaluate the increase in the normalised residence time. Finally, two modelling parameters are put into evidence and studied through a detailed sensitivity analysis.     

Large eddy simulation of turbulent premixed combustion using tabulated detailed chemistry and presumed probability density function

A method of chemistry tabulation combined with presumed probability density function (PDF) is applied to simulate piloted premixed jet burner flames with high Karlovitz number using large eddy simulation. Thermo-chemistry states are tabulated by the combination of auto-ignition and extended auto-ignition model. To evaluate the predictive capability of the proposed tabulation method to represent the thermo-chemistry states under the condition of different fresh gases temperature, a-priori study is conducted by performing idealised transient one-dimensional premixed flame simulations. Presumed PDF is used to involve the interaction of turbulence and flame with beta PDF to model the reaction progress variable distribution. Two presumed PDF models, Dirichlet distribution and independent beta distribution, respectively, are applied for representing the interaction between two mixture fractions that are associated with three inlet streams. Comparisons of statistical results show that two presumed PDF models for the two mixture fractions are both capable of predicting temperature and major species profiles, however, they are shown to have a significant effect on the predictions for intermediate species. An analysis of the thermo-chemical state-space representation of the sub-grid scale (SGS) combustion model is performed by comparing correlations between the carbon monoxide mass fraction and temperature. The SGS combustion model based on the proposed chemistry tabulation can reasonably capture the peak value and change trend of intermediate species. Aspects regarding model extensions to adequately predict the peak location of intermediate species are discussed.     

Application of x-ray fluorescence analysis to investigation of the composition of gunshot residues

We have used x-ray fluorescence analysis to study the elemental composition of gunshot residues from smooth-bore and rifled-bore guns. We have established that it is possible to differentiate between types of projectiles (jacketed/lead), types of primers (corrosive/noncorrosive), and types of propellant powders (black/smokeless) by analysis of the elemental composition of the gunshot residues. We have shown that the mercury content in gunshot residues on the surface of the object carrying the residues steadily decreases as storage time increases. Despite this fact, mercury can be preserved as a component of gunshot residues on the object (cotton cloth) under room conditions for more than 45 days. __________ Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 73, No. 3, pp. 320–325, May–June, 2006.     

Process monitoring of powder pre-paste laser surface alloying

Instead of the continuous powder delivery method using a powder feeder for thick layer laser cladding, pre-pasting of the alloying powder on the substrate is a widely used method to supply the coating powders into the melt pool for LSA. A method to monitor the process of laser surface alloying based on the infrared emission from the melt pool using infrared photodiodes was developed. The technique is solely aimed at the process of laser surface alloying using pre-paste metal powder on the substrate surface prior to laser melting. This monitoring technique is able to distinguish the existence or the absence of the pre-paste powder and the consistency of the laser surface alloying process. The technique is of low cost and is simple to implement into the process.