Pressure Dependence of UO2 Melting Measured by Double-Pulse Laser Heating

The melting point of uranium dioxide was measured as a function of isostatic pressure in an autoclave filled with helium up to 0.25 GPa. Containerless laser surface-heating was applied to measure the melting point by thermal arrest measurements during sample cooling. Precise control of the cooling rate, aimed at a precise determination of the freezing plateau, was obtained with a two-pulse method, where two Nd:YAG high power laser pulses are mixed within the same optical fiber and then focused on the sample surface. Calibration of the power of the two pulses permits the measurement of the melting point with very low uncertainty (0.5%). The measured melting slope of UO₂ is 170 and 200 KGPa^–1, a value which is markedly higher than that predicted by the Clausius–Clapeyron equation, which expresses this slope in terms of the enthalpy of fusion and the melting expansion. Possible reasons for this discrepancy are discussed.     

Radiative Properties of Uranium Dioxide Near Its Melting Point

A new technique for measuring radiative properties of nuclear fuel materials at high temperatures has been developed. The technique is based on pulse diffuse optical probing of the sample surface and on pyroreflectometry used in measuring radiative properties of refractory materials during laser heating or cooling. Pulse diffuse optical probing of the sample has been realized for the first time in subsecond pyrometry of the open surface heated by laser radiation. Such a procedure of sample irradiation during sample laser heating or cooling enables reflectivity and emissivity measurements near high temperature phase transitions to be performed in spite of possible sharp changes of the reflection indicatrix at phase transitions in the investigated material. With the method developed in this study, the spectral emissivity and reflectivity of uranium dioxide near its premelting and melting points have been measured. It has been found that condensation of the vapor plume formed above the sample during laser heating influenced the melting and boiling temperatures of uranium dioxide. The first-order phase transitions in uranium dioxide, such as solid–vapor–solid and liquid–vapor–liquid, have been observed in uranium dioxide for the first time during laser heating. Also, new data on the spectral emissivity of uranium dioxide at a wavelength of 0.644 m and in the temperature range of 2000 to 4200 K are presented.     

Advances in Measurements of the Melting Transition in Non-Stoichiometric UO2

This work presents a study of the melting behavior of the UO_2+x system. Self-crucible pulsed-laser melting at high pressure is realized, further improving the recently developed experimental approach. Thermograms of the heated surface of the sample, recorded by a fast pyrometer, show thermal arrests and/or points of inflection corresponding to the phase transformations. A further probe laser beam is focused onto and reflected by the sample surface, and the reflected light intensity is used to detect the exact instants at which melting/freezing transitions occur. Furthermore, a model was developed describing the complex process of laser-induced melting in a system where a solubility gap accompanies the formation of liquid, and a corresponding numerical simulation of the melting-freezing process was performed in order to depict the heat and matter transport phenomena involved. Finally, liquidus and solidus lines are proposed for the system UO_2+x in the range 0x0.21.     

Graphite Melting and Properties of Liquid Carbon

The results of fast heating (by electrical pulse current) of highly oriented pyrolytic graphite specimens are presented. Experimental data are obtained for graphite melting: the enthalpy of solid and liquid phases under melting, the heat of melting, and the heat capacity of solid and liquid phases near melting. Liquid carbon resistivity is measured under fast heating of cylindrical graphite specimens in thick-walled sapphire capillary tubes. Preliminary data for the isobaric heat capacity C _p for liquid carbon up to 10,000 K and for the isochoric heat capacity C _v up to 8000 K are presented.     

Evaporation and Condensation of Uranium Dioxide in an Electromagnetic Field

New physical phenomena related to the interaction of laser radiation with high evaporation materials, in particular with uranium dioxide, have been experimentally revealed by a subsecond heating technique. The first phenomenon, interpreted as an absorption flash, was observed in laser heating the sample and was manifested as a sharp drop in temperature on the heating curve. The second phenomenon, interpreted as a threshold condensation of vapor on the sample, was revealed during the cooling stage of the sample initially heated by laser radiation. This was manifested as an exothermal condensation peak on the cooling curve. The study of these phenomena has shown that there was a stable vapor zone above a sample in the field of laser radiation. The size and shape of the small particles produced due to laser evaporation and mainly formed in this vapor zone depended on the power of the laser radiation and the pressure of the inert gas. A change in the parameters of the vapor zone by changing the power of the laser radiation and the pressure of the inert gas gives the potential to produce nanoparticles of targeted sizes. Thus, the study of physical processes and mechanisms of forming nanoparticles of refractory materials at high temperatures motivates further development of the method of laser evaporation for producing nano-dimensional powders of targeted sizes and properties. Paper presented at the Seventh International Workshop on Subsecond Thermophysics, October 6–8, 2004, Orléans, France.     

Melting-Point Measurements at High Static Pressures from Laser Heating Methods: Application to Uranium

Two experimental approaches dealing with the determination of melting at high static pressures are described and analyzed. With the sample squeezed inside a diamond anvil cell, high temperatures up to the solid–liquid transition are obtained using Nd:YAG laser heating. Two methods have been investigated. In the first technique, the heating is accomplished with a pulsed laser and the brief radiation variations (t<10 ms) emitted from the sample are recorded with two high-speed infrared detectors. The melting location is defined by a plateau or changes of slope of the signals, and the temperatures are calculated by assuming a constant value of emissivity factor at the end of the transition over the studied pressure range. The second system employs a continuous laser and a two-dimensional CCD detector to measure temperatures using multispectral pyrometry. Melting is detected from criteria related either to textural change in the sample involving interference contrast under a laser illumination or to the specific variations of temperature and emissivity as a function of laser power. Thermal radiation is fitted to Planck's law with temperature and emissivity as the free parameters. Advantages and drawbacks are presented from results obtained on pure uranium.     

Realization of the 3He Melting Pressure Scale, PLTS-2000

The Provisional Low Temperature Scale of 2000, PLTS-2000, which was adopted in October 2000, uses the melting pressure of ³He to provide the basis for temperature measurement in the range from the Néel temperature of the solid, T ₂₀₀₀=0.902 mK, up to 1 K. The definition and derivation of the scale has been published, and the present paper now gives guidance on the practical methods by which the melting pressures can be measured in the laboratory. Various options are described, depending on the equipment available, and the uncertainties that may be achieved are considered.      

Scanning the Melting Curve of Tungsten by a Submicrosecond Wire-Explosion Experiment

Measurements of temperature and density during a wire-explosion experiment at atmospheric pressure are described. The measurements encompass a parameter range from the solid to near the critical point. The influence of a polytetrafluoroethylene coating of the wire, necessary to prevent surface discharges, on the temperature and density measurements is investigated. The melting curve of tungsten up to 4000 K is detemined.     

超临界二氧化碳处理对铀抗大气腐蚀性能的影响

通过对经超临界二氧化碳（Super Critical Carbon Doxide,SCCO2)处理的铀样品在60℃和70％相对湿度大气环境中腐蚀增重速度进行测量，研究了SCCO2处理对铀样品抗大气腐蚀性能的影响，借助俄歇电子能谱和X射线衍射等表面分析方法，对经过SCCO2处理的铀样品在表面的结构和化学成分进行了分析。实验有明，在10MPa、60℃的SCCO2中浸泡处理3．0h和4．5h后，铀样品的抗大气腐蚀速度都较未经过SCCO2处理的样品有明显的减慢。SCCO2压力参数影响的实验结果显示：同样条例上（60℃，3h)，10MPa SCCO2处理的样品的抗大气腐蚀性能比8MPa压力处理的要好；相同压力及时间条件下（10MPa,3h),60℃处理的样品的抗腐蚀性能优于50℃处理的。在所有实验中，10MPa,60℃的SCCO2处理3h后再于2MPa的CO2中浸泡108h，样品的抗腐蚀性能最好。AES分析结果显示，经SCCO2处理后，铀表层C、O含量比未处理品高，表明处理过程中有C和O的引入；XRD分析发现，铀表面与SCCO2之间的化学反应在表层主要的产物是UO2。对超临界二氧化碳处理提高铀抗腐蚀能力的机理也进行了初步的探讨。     

真空热处理对石墨涂覆铀表面氧化和电化学腐蚀的影响

为了探讨石墨涂层铀表面经真空热处理后对铀抗蚀性能的影响,通过增重法和电化学方法研究了处理样在100℃和150℃、含有一定量O2和H2O(g)气氛中的抗氧化腐蚀性和50μg/g Cl-溶液中的抗化学介质腐蚀性.抗氧化腐蚀试验表明,当热处理时间(5 h)不变时,在600℃处理要优于在500℃处理.电化学试验表明,处理样品的抗蚀性能与热处理时间(2.5～10.0 h)和温度(500～650℃)有关,且在600℃处理5 h的样品的抗化学介质腐蚀性能最佳.真空热处理可以提高石墨涂层铀表面的抗蚀性能.     

Melting and Volume Vaporization Kinetics Effects in Tungsten Wires at the Heating Rates of 1012 to 1013 K/s

Experimental results on electrically exploded tungsten wires at the heating rates of 10¹²–10¹³K · s^–1 and their interpretation in the framework of a one-dimensional magneto-hydrodynamic model are presented. The effects of both melting and volume vaporization observed in these experiments are discussed. It is shown that superheating of solid tungsten does not take place at these heating rates (within a 10% experimental uncertainty). Some direct measurements performed in this study, and comparison of different quantities measured and calculated by the model, suggest that the volume vaporization starts close to a binodal line.     

我国人造金刚石用石墨材料的研究

石墨材料是人工合成金刚石的直接原料.回顾我国人造金刚石用石墨材料的发展历程,介绍目前金刚石工业专用石墨材料的种类、制备工艺及其相关性能.同时,概要介绍掺杂石墨和采用其他种类石墨材料合成金刚石的研究进展,并对今后人造金刚石用石墨材料的发展进行了展望.     

开口镓熔点装置的复现及气压修正

中国计量科学研究院自行研制的开口镓熔点装置实现了对镓熔点冻制及复现的自动化,建立了开口镓熔点配置标准铂电阻温度计组成的基准装置。实验结果显示:镓熔点熔化温坪长达50h,镓熔点的复现性为0.1mK,闭口结构与开口结构镓熔点量值差异经过气压修正后由0.13mK减小至0.06mK,镓熔点温度-气压线性拟合曲线所得数值与90温标中给出的镓熔点气压修正系数一致。     

高温高压下超级13Cr不锈钢抗CO2腐蚀性能

为了推进超级13Cr不锈钢在油气田中的应用,用高温高压釜系统模拟了油气田腐蚀环境,研究了超级13Cr不锈钢在动静态环境中高温高压下的CO2腐蚀行为,利用扫描电镜、能谱仪和X射线衍射仪等对超级130r不锈钢表面腐蚀产物的形貌及成分进行了分析。结果表明：动态腐蚀时超级13Cr不锈钢的腐蚀速率随温度的升高而增大,150℃时最大,此后腐蚀速率随温度的升高而下降;静态腐蚀速率随温度的升高呈上升趋势;动态腐蚀速率高于静态的,动静态平均腐蚀速率均较小,属于轻度或中度腐蚀,在油气田的安全使用范围之内;动静态腐蚀时超级13Cr不锈钢表面均生成均匀、致密的钝化膜层,表现为均匀腐蚀,腐蚀产物成分为不锈钢基本成分,未发现CO2腐蚀产物,超级13Cr不锈钢具有良好的抗高温高压CO2腐蚀性能。     

超高温高压下石墨向金刚石直接转变的理论研究

根据固体和分子经验电子理论（EET理论）,分别计算了静压法和爆炸法合成金刚石过程中石墨和金刚石的价电子结构,获得了超高温高压下石墨和金刚石12组不同组合晶面间的价电子密度,结果表明,采用静压法合成金刚石．石墨／金刚石晶面的电子密度差均大于10％,说明其晶面的价电子结构差异太大,不能诱发石墨向金刚石的直接转变。而采用爆炸法合成金刚石,石墨结构理论键距和实验键距差是0．1073nm,明显大于稳定的价电子结构键距差的最大值（0．005nm）,因此,爆炸法条件下,石墨的价电子结构不稳定,主要因为超高温高压下,石墨先分解出亚稳相后再转变成金刚石结构。     

Measurement of Melting Point and Radiance Temperature (at Melting Point and at 653 nm) of Hafnium-3 (wt. %) Zirconium by a Pulse Heating Method

A subsecond duration pulse heating method is used to measure the melting point and radiance temperature (at 653 nm) at the melting point of hafnium containing 3.12 weight percent zirconium. The results yield a value of 2471 K for the melting point on the International Practical Temperature Scale of 1968. The radiance temperature (at 653 nm) of this material at its melting point is 2236 K, and the corresponding normal spectral emittance is 0.39. Estimated inaccuracies are: 10 K in the melting point and in the radiance temperature, and 5 percent in the normal spectral emittance.     

Temperature and Pressure Dependence of the Speed of Sound in Seawater

The speed of sound in sea water has been measured for various salinities over the temperature range 0.1–30°C at excess pressures of 0–60 MPa. The results are presented in tables and an equation derived by least-squares fitting that gives the difference in the speed of sound between distilled water and seawater. The data are compared with calculations on the Chen-Millero algorithm, which was used in compiling the UNESCO international tables for the speed of sound. Suggestions are made for setting up GSSSD tables Seawater: Speed of sound.     

High-pressure,high-temperature thermophysical measurements on tantalum and tungsten

A submillisecond resistive heating technique under high pressure (0.2 GPa) has been applied to the measurement of thermophysical properties of tantalum and tungsten metals in the solid and the liquid state. Agreement between previously published and most of the present results is good.Paper presented at the Ninth Symposium on Thermophysical Properties, June 24–27, 1985, Boulder, Colorado, U.S.A.     

Melting and Vaporization of the 1223 Phase in the System (Tl-Pb-Ba-Sr-Ca-Cu-O)

The melting and vaporization of the 1223 [(Tl,Pb):(Ba,Sr):Ca:Cu] oxide phase in the system (Tl-Pb-Ba-Sr-Ca-Cu-O) have been investigated using a combination of dynamic methods (differential thermal analysis, thermogravimetry, effusion) and post-quenching characterization techniques (powder x-ray diffraction, scanning electron microscopy, energy dispersive x-ray spectrometry). Vaporization rates, thermal events, and melt compositions were followed as a function of thallia loss from a 1223 stoichiometry. Melting and vaporization equilibria of the 1223 phase are complex, with as many as seven phases participating simultaneously. At a total pressure of 0.1 MPa the 1223 phase was found to melt completely at (980 ± 5) °C in oxygen, at a thallia partial pressure (p_Tl2O) of (4.6 ± 0.5) kPa, where the quoted uncertainties are standard uncertainties, i.e., 1 estimated standard deviation. The melting reaction involves five other solids and a liquid, nominally as follows: 1223→1212+(Ca,Sr)2CuO3+(Sr,Ca)CuO2+BaPbO3+(Ca,Sr)O+LiquidStoichiometries of the participating phases have been determined from microchemical analysis, and substantial elemental substitution on the 1212 and 1223 crystallographic sites is indicated. The 1223 phase occurs in equilibrium with liquids from its melting point down to at least 935 °C. The composition of the lowest melting liquid detected for the bulk compositions of this study has been measured using microchemical analysis. Applications to the processing of superconducting wires and tapes are discussed.