新型镓熔点自动复现装置

介绍了中国计量科学研究院新型镓熔点自动复现装置, 该装置的固定点炉采用半导体三段冻制及加热技术实现了镓熔点复现的自动化, 通过精密控温及合理的结构设计获得优良的温度稳定性与均匀性。该装置镓熔点使用当前最新提纯技术的99.999 99%高纯镓金属及完善的灌注技术。实验结果显示, 该固定点装置温坪持续了70 h以上,前20%～80%温坪变化小于0.15 mK,复现性为0.07 mK, 该装置的扩展不确定度为0.36 mK（k=2）。     

镓熔点温坪复现研究

镓熔点是ITS-90国际温标中重要的定义固定点,在温度计量研究中起着重要作用。由于高纯镓从液态转化为固态时,体积膨胀约3.1%,传统玻璃外壳的镓熔点容器在冻制过程中很容易造成损坏。为了解决这一难题,设计了一种具有金属外壳的镓熔点装置,以该装置为对象,开展了2种不同镓熔点复现方法和2种不同复现装置对镓相变温坪影响方面的研究,并与国外同类型装置的性能进行了比较。实验结果表明:不同镓点容器复现的镓熔点温度在0.02 mK范围内一致,高纯镓中的微量杂质是造成差异的主要原因;外液-固界面复现方法比双液-固界面复现方法得到的温坪值低0.09 mK;不同复现装置对镓熔点温坪的影响较小。     

一种新型结构的镓三相点容器

本文介绍了计量院研制的新型结构的镓三相点容器及镓三相点的复现方法。并将两个镓三相点容器与镓熔点容器进行了比对 ,结果表明 :两个镓三相点容器所复现的镓三相点温度与镓熔点温度的差值分别为1 85mK、1 71mK ;通过分析认为镓三相点容器间的温差 (0 1 4mK)主要是镓样品所含杂质成分的差异引起的。     

新型开口锌凝固点复现装置

介绍了中国计量科学研究院研制的新型开口锌凝固点复现装置,该装置采用99．99999％的高纯锌金属固定点灌注技术,固定点炉采用三段控温的方式,依靠精确控温及合理的结构设计获得优良的垂直温场。通过准确测量容器的内部气压,可以优化我国国家基准中气压修正的不确定度分量。实验结果显示：该装置复现的温坪时间大于30小时,复现的扩展不确定度为0．6mK（k=2）。     

不同复现方法对镓熔点温度的影响

镓熔点是ITS - 90国际温标中一个重要的定义固定点。本文详细介绍了温度咨询委员会 (简称CCT)第一工作组推荐国家实验室复现镓熔点的最佳方法———双液 -固界面法。同时 ,还介绍了外液 -固界面的复现方法 ,并将两种方法复现的镓熔点值进行比较。实验结果表明 ,外液 -固界面法比双液 -固界面法复现出来的镓熔点值偏低约 0 13mK。     

新型便携式镓熔点炉的研制

中国计量科学研究院最新研制的便携式镓熔点炉采用了先进的半导体制冷和控温技术及有效合理的制冷块分布方式,实现对镓熔点容器的冻制与复现自动化.实验结果显示:该固定点炉从底端起140mm范围内的垂直温场小于0.03℃,温坪时间达到80h以上,复现性优于0.06mK.     

真空镓固定点黑体辐射源研制

为满足红外遥感载荷实验室辐射定标需求,实现红外遥感辐射量值溯源到ITS-90国际温标,研制了真空镓固定点黑体辐射源.黑体腔开口直径为25 mm,深度220 mm,内部喷涂高发射率涂层,通过仿真计算黑体腔的发射率优于0.9999.在真空下测试了镓固定点相变坪台的复现性为4.4 mK,坪台稳定性优于2 mK.测量了镓固定点...     

基于微型镓固定点的精密铂电阻温度计原位校准的研究

基于固定点温标传递技术,设计可在镓熔点原位校准的精密铂电阻温度计,并对微型固定点相变温坪特性进行实验分析.实验结果表明:微型镓固定点温坪可持续最大时长为1.2h,温坪在20 min内稳定性优于2.8 mK,复现性优于2.3 mK;微型固定点温坪值与加热温度之间存在线性关系,并且随着加热温度的升高,固定点温坪值越高,通过...     

准绝热法微型镓固定点相变特性研究

介绍了可用于原位校准的微型镓相变固定点形成过程,准绝热测试系统的结构和工作原理,测量了微型镓相变固定点在准绝热测试系统中的相变特性。实验结果表明微型相变镓固定点的相变温度与加热功率之间存在强线性关系,其线性拟合因子R2为0.995 7,并且随着功率越降低,其相变熔化温度越接近镓固定点的标准值。在相同的准绝热复现条件下,其相变温度的复现性优于2 mK。     

基于闭环制冷机的平衡氢三相点复现装置

为了解决平衡氢三相点复现装置复现难度大、耗时长、效率低的问题,研制了基于闭环GM制冷机的新型平衡氢三相点复现装置。采用准绝热方法复现平衡氢三相点;基于Labview程序,实现了复现过程的自动测量与控制。该套装置不仅提高了工作效率,而且提升了复现性。实验结果表明:该套系统平衡氢三相点的复现性优于0.05 mK,标准不确定度优于0.1 mK。     

基于微型镓基共晶固定点的温度传感器在轨校准方法研究

介绍了微型镓基共晶固定点的灌注工艺和准绝热相变特性测量系统;结合空腔黑体和非近位安装的温度传感器,研究了Ga-Sn和Ga-Zn共晶固定点的相变温坪重复性和Ga固定点的相变温坪长期稳定性;通过特定的热环境下镓及2个镓基共晶固定点三者熔化过程中温度传感器测量到的相变温坪值,对嵌入空腔黑体底部的温度传感器进行校准,其校准结果与实验室常规校准方法得到的结果差异均小于2mK。实验结果表明:在热环境保持不变的条件下,随着相变时间的增加,相变温坪值就越靠近理论上相变物质的熔化温度,即固定点与温度传感器测孔之间的异位温差越小;对于Ga-Sn和Ga-Zn共晶固定点,温度传感器测量到的相变温坪值与加热功率呈线性关系,零功率下的单点校准温度分别为20.352℃和25.187℃。     

Realization of the Gallium Triple Point at NMIJ/AIST

The triple point of gallium has been realized by a calorimetric method using capsule-type standard platinum resistance thermometers (CSPRTs) and a small glass cell containing about 97 mmol (6.8 g) of gallium with a nominal purity of 99.99999%. The melting curve shows a very flat and relatively linear dependence on 1/F in the region from 1/F = 1 to 1/F = 20 with a narrow width of the melting curve within 0.1 mK. Also, a large gallium triple-point cell was fabricated for the calibration of client-owned CSPRTs. The gallium triple-point cell consists of a PTFE crucible and a PTFE cap with a re-entrant well and a small vent. The PTFE cell contains 780 g of gallium from the same source as used for the small glass cell. The PTFE cell is completely covered by a stainless-steel jacket with a valve to enable evacuation of the cell. The melting curve of the large cell shows a flat plateau that remains within 0.03 mK over 10 days and that is reproducible within 0.05 mK over 8 months. The calibrated value of a CSPRT obtained using the large cell agrees with that obtained using the small glass cell within the uncertainties of the calibrations.     

Realization of Low-Temperature Fixed Points of the ITS-90 at NMIJ/AIST

A new model of sealed cells with three thermometer wells for calibration of capsule-type thermometers at low-temperature fixed points of the International Temperature Scale of 1990 has been developed at the National Metrology Institute of Japan (NMIJ). The melting curves of Ar and O₂ obtained using the new cells show very flat plateaux and a linear temperature dependence as a function of the inverse liquid fraction (1/F) over the range 1/F = 1 to 1/F = 20 with a narrow melting curve width of 0.1 mK. The melting curves of Ne obtained with the new cell also show very flat plateaux and approximately linear temperature dependence versus 1/F and a narrow melting curve width of 0.1 mK, though with a slight concave structure at high 1/F. The melting temperatures with the new cells agree with previous NMIJ sealed cells within 10 μK, which is similar to the reproducibility of the realization of the triple points at NMIJ. The source dependence of the triple-point temperature of Ne was investigated by filling two of the new cells from different sources of Ne. The difference in the realized triple point temperatures between the two sources is 0.031 mK, consistent with that estimated from isotope analysis. The uncertainties in the calibration of standard platinum resistance thermometers at the low-temperature fixed points are summarized. The uncertainty of the calibration at the triple point of e-H₂ has been reduced to about one-third of its value without the correction by making the isotopic correction on the basis of the technical annex for the ITS-90 in the mise en pratique for the definition of the kelvin.     

Construction and Start-up of a Large-Volume Thermostat for Dielectric-Constant Gas Thermometry

A liquid-bath thermostat with a volume of about 800  L was designed to provide a suitable thermal environment for a dielectric-constant gas thermometer (DCGT) in the range from the triple point of mercury to the melting point of gallium. In the article, results obtained with the unique, huge thermostat without the DCGT measuring chamber are reported to demonstrate the capability of controlling the temperature of very large systems at a metrological level. First tests showed that the bath together with its temperature controller provide a temperature variation of less than ±0.5mK peak-to-peak. This temperature instability could be maintained over a period of several days. In the central working volume (diameter—500mm, height—650mm), in which the vacuum chamber containing the measuring system of the DCGT will be placed later, the temperature inhomogeneity has been demonstrated to be also well below 1mK.     

水三相点瓶自动冻制保存装置复现性研究

介绍了型号为CIMM-TH-0230的水三相点瓶自动冻制保存装置,对该装置进行水三相点温坪复现性研究,并考核装置的各项指标。实验结果显示:该装置冻制的水三相点的温坪在48 h内变化不大于0.2 m K,复现性小于0.04 m K,稳定性优于0.5 m K,不同瓶子之间复现的温度差值不大于0.4 m K。试验数据表明该装置非常适合水三相点瓶的自动冻制、保存与复现。     

Realization of the Temperature Scale in the Range from 234.3 K (Hg Triple Point) to 1084.62°C (Cu Freezing Point) in Croatia

This article describes the realization of the International Temperature Scale in the range from 234.3 K (mercury triple point) to 1084.62°C (copper freezing point) at the Laboratory for Process Measurement (LPM), Faculty of Mechanical Engineering and Naval Architecture (FSB), University of Zagreb. The system for the realization of the ITS-90 consists of the sealed fixed-point cells (mercury triple point, water triple point and gallium melting point) and the apparatus designed for the optimal realization of open fixed-point cells which include the gallium melting point, tin freezing point, zinc freezing point, aluminum freezing point, and copper freezing point. The maintenance of the open fixed-point cells is described, including the system for filling the cells with pure argon and for maintaining the pressure during the realization.     

Measurements on Melting Pressure,Metastable Solid Phases,and Molar Volume of Univariant Saturated Helium Mixture

A concentration-saturated helium mixture at the melting pressure consists of two liquid phases and one or two solid phases. The equilibrium system is univariant, whose properties depend uniquely on temperature. Four coexisting phases can exist on singular points, which are called quadruple points. As a univariant system, the melting pressure could be used as a thermometric standard. It would provide some advantages compared to the current reference, namely pure $^3$ He, especially at the lowest temperatures below 1 mK. We have extended the melting pressure measurements of the concentration-saturated helium mixture from 10 to 460 mK. The density of the dilute liquid phase was also recorded. The effect of the equilibrium crystal structure changing from hcp to bcc was clearly seen at $T=294$  mK at the melting pressure $P=2.638$  MPa. We observed the existence of metastable solid phases around this point. No evidence was found for the presence of another, disputed, quadruple point at around 400 mK. The experimental results agree well with our previous calculations at low temperatures, but deviate above 200 mK.