静电悬浮条件下的材料典型热物理性质测量

随着对材料研究的逐渐深入,材料制备和材料分析的方法越来越重要,并且一些材料重要的物理性质是开展相关研究的基础。由于一些材料熔点高、难熔化,同时,传统手段无法避免容器壁的污染,或者无法在真空条件下进行试验避免气体的污染,或者由于实验性质原因只能测量特定的材料,这些方法很难测量材料在高温下过热过冷阶段的热物理性质。系统介绍了静电悬浮技术,这是一种新型的实现深过冷的方式,可以达到高温下对材料热物理性质进行测量的目的。静电悬浮技术使样品在两极板间悬浮,在悬浮的状态下采用激光对样品进行加热,使材料达到高温熔化,同时进行热物性的测量。对比了几种实现测量典型热物理性质的方法,了解静电悬浮的优势,并详细地介绍了静电悬浮技术对材料的熔体密度、热膨胀系数、表面张力和粘度系数以及比热的测量。     

深过冷合金中的非平衡现象分析

深过冷技术是快速凝固技术中的一种，它能实现金属或合金在慢速冷却条件下发生快速凝固，这就为研究者研究合金快速凝固中的一些非平衡现象提供了一种新的途径，讨论了影响熔体过冷度的主要因素，介绍了获得熔体深过冷的几种主要方法，分析了深过冷熔体的非平衡现象产生的原因。     

无容器凝固条件下La2O3-TiO2二元共晶陶瓷的结构演变

无容器凝固已成为制备新型功能陶瓷材料的重要手段,但直至目前对二元复相陶瓷的深过冷凝固机理研究甚少.本论文采用气动悬浮技术研究了无容器凝固条件下La2O3-TiO2二元共晶陶瓷凝固组织和结构演变.按La2O3-82.8at％ TiO2共晶组分将两种粉体混匀压片烧结成陶瓷圆柱,经激光加热熔化后在触发形核和无容器凝固两种形核模式下凝固.结果表明,烧结后的陶瓷由La4Ti9O24和TiO2两相组成;用光学显微镜和扫描电镜观察了两种形核模式的陶瓷样品形貌,均为规则共晶层片结构,前者因是触发形核,过冷度小,组织较后者粗大,由表面多个形核中心向内部辐射生长;后者为深过冷凝固,组织细小并高度取向,原因是后者是均质形核,过冷度大,晶体生长方向受热流控制.     

深过冷定向凝固工艺过程的研究

利用过冷度的遗传性，提出了将合金熔体深过冷与传统定向凝固相结合的深过冷定向凝固技术，并在自制的实验装置上，对ＳＤＳ技术进行了探索性研究，实现了Ｃｕ与ｗ（Ｎｉ）为５．０％合金的深过冷和深过冷定向凝固。     

深过冷Ni-Sn合金非规则共晶的形成机制

采用熔融玻璃净化配合循环过热使Ni-32.5%Sn(质量分数)共晶合金实现了深过冷快速凝固.当过冷度大于某一临界值时,非规则共晶在凝固组织中出现.随着过冷度的提高,最终得到完全的非规则共晶组织.通过分析Ni-Sn共晶合金中各相形核、生长、以及枝晶熔断机制随过冷度的变化,解释了非规则共晶的形成机制.在深过冷条件下熔体中初生相率先形核并长入过冷熔体中,形成枝晶骨架,再辉重熔后次生相从残余熔体中析出并包围初生相,形成非规则共晶.     

过冷度对Fe-Ni-P-B软磁合金凝固组织的影响

采用玻璃包覆法(fluxing)提纯和在不同温度下保温,获得了Fe40Ni40P14B6合金熔体的凝固组织,研究了过冷度对凝固组织的影响.结果表明,随着过冷度的增大,Fe40Ni40P14B6的凝固组织从亚共晶转变为共晶组织,晶粒尺寸明显减小.当过冷度超过某一临界值时,合金熔体发生Spinodal分解,形成网状结构的凝固组织并使晶粒显著细化,达到纳米尺度.在深过冷条件下,可获得块体纳米晶凝固组织.     

深过冷熔体激发快速定向凝固

阐述了深过冷的方法，深过冷的遗传性，深过冷度的理论极限以及深过冷熔体激发发快速定向凝固的试验方法及其凝固过程，给出了深过冷熔体（Ｃｕ－５ｗｔ％）激发快速定向凝固与铸态试验激发快速定向凝固的初步试验结果。     

熔体深过冷过共晶铝硅合金的凝固组织研究

本工作采用熔体急冷装置对过共晶铝硅熔体进行深过冷处理,采用光学显微镜、扫描电子显微镜和X射线衍射仪等手段,研究了硅含量和熔炼工艺对熔体深过冷过共晶铝硅合金凝固组织的影响。研究结果表明,合金在800℃熔炼,保温时间为30 min时,熔体深过冷处理可抑制Al-(14～18) Si合金熔体在凝固过程中初晶硅的析出。当Al-18Si合金在800℃熔炼,保温时间超过30 min时,深过冷Al-18Si合金熔体在室温金属模型中凝固时可完全抑制初晶硅的析出,获得无初晶硅的凝固组织。     

深过冷合金中的晶粒细化

深过冷熔体在一个临界过冷度下凝固,在很窄的过冷区间内晶粒尺寸将急剧减小,称之为晶粒细化.从研究过冷Ni基合金的晶粒细化现象入手,对迄今为止关于产生晶粒细化的各种机制做了较为系统的归纳和分析.并在此基础上,提出了存在的问题和今后的发展方向.     

深过冷Fe85B15亚共晶合金晶粒的细化机制

采用熔融玻璃与循环过热相结合的方法使Fe85 B15 合金熔体获得了320K的大过冷度,并在共晶组织中获得了晶粒尺寸为100～200nm的共晶相.理论分析和实验结果表明,合金熔体的大过冷为晶粒细化提供了驱动力,而形核率和晶粒生长速度随过冷度的变化决定了晶粒的细化.实验结果为通过深过冷快速凝固技术制备块体纳米晶材料提供了新的思路和重要的实验依据.     

Measurements of thermophysical properties of liquid metals by noncontact techniques

With the advent of containerless processing techniques such as electromagnetic levitation, it is now possible to study the properties of high-temperature liquid metalsin situ by applying sophisticated noncontact diagnostics, such as pyrometry and high-speed videography. Thermophysical properties of interest are, e.g., specific heat, thermal conductivity, and viscosity. Applying containerless processing, it is also possible to undercool the melt because of the lack of container-induced nucleation sites. This gives access to a metastable region of the phase diagram. The knowledge of thermophysical data in this region is very important, because undercooling plays a major role in any solidification process. The degree of undercooling not only determines the growth velocity, but also is crucial in selecting the eventually obtained metastable solid phase. In this paper, some recent developments are surveyed relating to the noncontact measurements of emissivity, specific heat, electrical conductivity, density, surface tension, and viscosity, as well as a discussion of possible experiments in microgravity.Paper presented at the Third Workshop on Subsecond Thermophysics, September 17–18, 1992, Graz, Austria.     

Undercooling and crystallization behaviour of antimony droplets

The level of liquid undercooling below the equilibrium melting point experienced typically in a bulk material is limited by the presence of potent heterogeneous nucleation sites. By subdividing the material into a collection of fine (10 to 150m) droplets the most potent nucleants are isolated into a small fraction of the droplet population, allowing the remainder to reach deep levels of undercooling prior to the onset of solidification. Droplet surface coating characteristics influence both the level and uniformity of the undercooling and, in addition, may alter the nucleation kinetics thereby encouraging the formation of a metastable crystalline phase from the undercooled liquid. An effective means of both creating a stable dispersion of fine droplets and influencing the surface coating is through the droplet emulsion technique. This approach has allowed the level of undercooling for pure antimony to be extended from 0.08 to 0.237T _m through proper control of droplet size, surface coating and applied cooling rate. The formation of a metastable simple cubic phase from the melt has been confirmed using both differential thermal analysis and X-ray diffraction techniques. The simple cubic phase is retained in droplets to temperatures approaching the melting point at a heating rate of 20° C min^–1. Drop tube treatment of emulsified samples has also been successful at producing the metastable simple cubic structure by containerless processing.     

Role of sample size in the nucleation kinetics of phase transformations in steel alloys

Certain commercial steel alloys exhibit a two-step phase transformation process during solidification when substantial undercooling of the liquid allows access to the metastable phase. This two-step transformation leads to a desirable microstructure under certain conditions. Electrostatic Levitation (ESL) and Electromagnetic Levitation (EML) are two methods of containerless processing used to study how nucleation and growth kinetics influence the transformation delay between phases. Because the two facilities show substantially different delay results, the test environment differences have been analyzed to determine the root cause of this deviation. In particular, the difference in sample size between ESL and EML is examined and modeling shows that this difference is not the controlling factor in determining transformation delay behavior.     

深过冷Ni-Cu-Si合金熔体中的快速枝晶生长

为了揭示多元合金中的枝晶生长规律,采用电磁悬浮技术实现了Ni-10%Cu-10%Si三元合金的深过冷与快速凝固,实验中合金熔体获得的最大过冷度为236K。对合金快速凝固过程中初生相-αNi的枝晶生长速度测定结果表明,其与过冷度之间存在幂函数关系:V=1.6×10-13ΔT5.7。当ΔT较小时,随着ΔT的增加V增加缓慢,当ΔT较大时,随着ΔT的增加V迅速增加。对比分析表明,溶质Si对-αNi枝晶的生长影响显著,而溶质Cu则几乎没有影响。随着过冷度的增加,未发现-αNi相的微观形态从枝晶向等轴晶转变,但-αNi晶粒尺寸均随着过冷度的增加而急剧细化。     

Noncontact temperature measurement of a falling drop

The 105-m drop tube at the Marshall Space Flight Center has been used in a number of experiments to determine the effects of containerless, microgravity processing on the undercooling and solidification behavior of metals and alloys. These experiments have been limited, however, because direct temperature measurement of the falling drops has not been available. Undercooling and nucleation temperatures are calculated from thermophysical properties based on droplet cooling models. In most cases these properties are not well known, particularly in the undercooled state. This results in a large amount of uncertainty in the determination of nucleation temperatures. If temperature measurement can be accomplished, then the thermal history of the drops could be well documented. This would lead to a better understanding of the thermophysical and thermal radiative properties of undercooled melts. An effort to measure the temperature of a falling drop is under way at Vanderbilt and Marshall Space Flight Center. The technique uses two-color pyrometry and high-speed data acquisition. The approach is presented along with some preliminary data from drop tube experiments. The results from droplet cooling models will be compared with noncontact temperature measurements.Paper presented at the Tenth Symposium on Thermophysical Properties, June 20–23, 1988, Gaithersburg, Maryland, U.S.A.     

金属凝固过冷度与热物性参数的关系

本文建立了金属在均质形核和非均质形核及压力作用下凝固时的过冷度与热物性参数之间的关系方程。从而在通常给出的金属热物性参数的基础上,解释了 Flemings给出的金属过冷度的实验结果,并预测了最大过冷度极值为2/3T_m。本文讨论了热物性参数、形核剂、压力作用对过冷度的影响,以及获得深过冷液态金属的途径。本文还给出间接确定固-液界面能或扩散激活能的方法。     

Numerical simulation of rapid solidification of a spherical sample on a metallic substrate

Since the exact analytical solutions for rapid solidification process are available only for special boundary conditions, numerical techniques have to be applied for more general boundary conditions. In this paper we will describe a finite difference method for simulation of rapid solidification that is based on control volume methodology and interface-tracking technique. Heat transfer computer study will be realized for solidification with and without melt undercooling at the interface. Such numerical method will be applied for thermal history analysis of solidifying nickel on copper substrate.     

Growth kinetics in levitated and quenched Nd-Fe-B alloys

We investigated the growth kinetics and the effect of quenching conditions on rapid solidification of undercooled Nd-Fe-B melts with compositions near the Nd-₂-Fe₁₄-B (2-14-1) phase. We prepared melt drops of various undercooling levels (up to 300 K below the liquidus temperature) were prepared by the electromagnetic levitation method and subsequently quenched them onto chill substrates. We measured the solidification kinetics of the undercooled melts in situ using a high-resolution Si photodiode. In accordance with the nucleation theory, the properitectic γ-Fe phase nucleates at first during the undercooling process. There were two different solidification routes, with the observed route depending on the undercooling level of the levitated melt prior to quenching. The peritectic reaction is favored in melts with high undercooling levels prior to quenching. Low previous undercooling levels lead to primary solidification of the 2-14-1 phase on quenching. The thickness of the homogeneous 2-14-1 phase zone, grown directly at the substrate side, depends strongly on the undercooling level prior to solidification. We estimated the growth velocity of the 2-14-1 phase from temperature-time-characteristics to be of the order of 1 mm/s. These investigations give rise to improved understanding about the high sensitivity of the microstructure of Nd-Fe-B alloys on different rapid solidification procedures     

Structure and Thermophysical Properties of Molten BaGe Using Electrostatic Levitation Technique

BaGe alloys with two compositions near their eutectic point form open framework structures called the clathrate structure. These BaGe compounds with the clathrate structure can be made by rapid solidification from their liquid state. However, the formation mechanism of the clathrate structure has not been clarified due to lack of information on their liquid-state structure and properties. Since BaGe alloy melts have very high reactivity, it is difficult to measure the thermophysical properties of them by ordinary methods using a container. Therefore, a containerless technique must be used to measure the thermophysical properties of BaGe melts. Using the electrostatic levitation (ESL) technique as a containerless technique, the thermophysical properties (density, surface tension, and viscosity) of BaGe melts around the eutectic composition were measured in order to clarify the formation mechanism of the clathrate structure, and also the structure of them was observed by using the high-energy X-ray diffraction method combined with ESL. From experimental results, it was observed that the short-range order based on the clathrate structure exists even in the liquid state at the clathrate-forming compositions.