用于分度热电偶的Co-C高温共晶点的制作和复现性研究

介绍了中国计量科学研究院研制的用于分度热电偶的Co-C高温共晶点,以及使用铂/钯热电偶对共晶点进行的复现测量的结果。实验数据表明,Co-C高温共晶点的熔点复现性已达到了0.03 ℃。Co-C高温共晶点坩埚在1300 ℃以上温度经历了累计时间500 h、110多次的熔化和凝固实验后依然完好。     

高温共晶固定点的建立与复现

金属(碳)-碳(M-C和M(C)-C)高温共晶固定点(以下简称高温固定点)的出现给温标复现方法带来了一次变革,并有可能成为下届温标新的定义固定点.文中介绍了目前常见的高温固定点坩埚的典型结构,描述了高温固定点的灌注工艺及灌注方法.为对固定点的不同灌注方法及其效果进行研究,使用石墨衬套和碳纤维石墨材料作内衬,灌注了Co-C和Pt-C高温固定点.对灌注的高温固定点初步的复现实验结果显示,Co-C、Pt-C的短期复现重复性均优于50 mK,进一步证明了高温固定点作为新温标定义固定点的可行性.     

Pd-C高温共晶点复现技术研究

设计了Pd-C高温共晶点复现装置,包括复现用高温均热炉炉体、温度控制系统、真空泵、充气保护装置、水冷系统、复现用的石墨坩埚、二等B型标准热电偶和Pt-Pd热电偶等。在此基础上进行了石墨坩埚的灌注和共晶点复现,并对复现的试验数据进行了相应的分析。结果表明本装置温度复现性可以达到0.2℃以下。     

高温共晶点坩埚耐用性研究

高温共晶点坩埚因采用石墨材料制作,结构强度较低,在复现试验后易发生破裂,造成高温共晶点的损坏。坩埚耐用性问题已成为制约高温共晶点加入下一代温标的主要障碍之一。为了解决上述问题,本文依据ANSYS对坩埚受力情况进行分析,明确了坩埚主要受力点的理论位置,之后结合多种高温共晶点的实际破裂情况,分析了不同种类共晶点坩埚破裂的原因,并有针对性的提出了两种高温共晶点坩埚改进方案：改进型Hybrid结构和导流盖结构。最后使用改进结构的坩埚灌注了新的高温共晶点/包晶点,复现试验后未出现损坏问题,初步验证了方案的有效性。     

Pd-C高温共晶点复现装置研制

主要针对Pd-C高温共晶点复现装置的组成进行介绍,其中包括复现用高温均热炉炉体、温度控制系统、真空泵、充气保护装置、水冷系统、复现用的石墨坩埚、二等B型标准热电偶和Pt-Pd热电偶等。针对石墨坩埚的灌注和共晶点复现过程进行了描述,根据复现的试验数据进行了相应的分析。     

Re-C共晶高温固定点的研制与评价

基于直接共晶的灌注方法,研制了混合结构的Re-C共晶高温固定点.利用高温固定点实验系统对其进行了复现实验研究.依据国际温度咨询委员会辐射测温工作组第二工作包(CCT-WG5-WP2)——关于遴选最优高温固定点用于最终热力学温度赋值的标准,对本文灌注的Re-C进行了评价,结果表明其熔化温度短期重复性为3mK、熔化结束温度...     

Ga-In-Sn微型共晶点相变特性研究

以Ga-In-Sn三元合金为研究对象,研制了可用于现场及在线标定的微型Ga-In-Sn共晶点容器,开展了3种不同配比对相变温度和温坪复现影响的研究。结果表明:3种配比的共晶点温坪可持续1.2~2 h,实验的复现性优于4.5 mK,合成扩展不确定度为9.3 mK(k=2),3种配比的共晶点相变温度平均值为10.748 ℃;在相同热工况下Ga-In-Sn合金发生共晶反应的相变温度不受配比的影响;改变合金熔体的降温速率可改变微型共晶点过冷度。     

用黑体辐射法复现铝凝固点

本文叙述用精密直流光电温度计昨现纯金属铝凝固点的实验装置和实验方法，复现铝凝固点的总不确定度小于50mK，置信度为99%。实验中对3个铝点黑体石墨坩埚容器的凝固温度进行了多次测量，3个容器的铝凝固点温度之差不大于10mK。在8个月的时间内，对同一铝点坩埚容器的铝凝固点温度进行了11次测量，其标准偏差为15mK，长期重复性也很好。     

高温共晶点灌注方法研究

在高温共晶点研制过程中,目前常用的灌注方法包括直接共晶法和预共晶法两种,但直接共晶法存在效率低下的不足,预共晶法存在粘附问题。本文对高温共晶点灌注方法进行研究,设计了两种填充配件,一种为采用长石墨衬套的直接共晶坩埚;另一种为具有特殊结构的预共晶坩埚。经试验验证,前者可明显提高直接共晶法的灌注效率,后者有效避免了预共晶法的共晶体粘结问题,二者均达到了设计目的,为高温共晶点研制技术的完善发展起到了促进作用。     

微型双温度固定点容器研制

基准固定点传递技术应用于现场温度校准已成为提高工业温度测量水平的一种重要途径。采用多孔石墨坩埚半包围结构,内部对称填充了高纯铟(In)和锡(Sn)2种金属,研制了一种应用于现场校准的微型双温度固定点容器。实验结果表明,In点熔化温坪持续时间约为2 h,Sn点熔化温坪持续时间约为3 h,In和Sn的温坪复现的扩展不确定度分别为4.0 mK 和4.4 mK(k=2),可满足工业现场对精密铂电阻温度计的校准需求。     

Investigation of TiC–C Eutectic and WC–C Peritectic High-Temperature Fixed Points

TiC–C eutectic (2,761°C) and WC–C peritectic (2,749°C) fixed points were investigated to compare their potential as high-temperature thermometric reference points. Two TiC–C and three WC–C fixed-point cells were constructed, and the melting and freezing plateaux were evaluated by means of radiation thermometry. The repeatability of the TiC–C eutectic within a day was 60 mK with a melting range roughly 200 mK. The repeatability of the melting temperature of the WC–C peritectic within 1 day was 17 mK with a melting range of ∼70 mK. The repeatability of the freezing temperature of the WC–C peritectic was 21 mK with a freezing range less than 20 mK. One of the TiC–C cells was constructed from a TiC and graphite powder mixture. The filling showed the reaction with the graphite crucible was suppressed and the ingot contained less voids, although the lack of high-purity TiC powder poses a problem. The WC–C cells were easily constructed, like metal–carbon eutectic cells, without any evident reaction with the crucible. From these results, it is concluded that the WC–C peritectic has more potential than the TiC–C eutectic as a high-temperature reference point. The investigation of the purification of the TiC–C cell during filling and the plateau observation are also reported.     

Establishment of the Co-C Eutectic Fixed-Point Cell for Thermocouple Calibrations at NIMT

In 2015, NIMT first established a Co-C eutectic temperature reference (fixed-point) cell measurement capability for thermocouple calibration to support the requirements of Thailand’s heavy industries and secondary laboratories. The Co-C eutectic fixed-point cell is a facility transferred from NPL, where the design was developed through European and UK national measurement system projects. In this paper, we describe the establishment of a Co-C eutectic fixed-point cell for thermocouple calibration at NIMT. This paper demonstrates achievement of the required furnace uniformity, the Co-C plateau realization and the comparison data between NIMT and NPL Co-C cells by using the same standard Pt/Pd thermocouple, demonstrating traceability. The NIMT measurement capability for noble metal type thermocouples at the new Co-C eutectic fixed point (\(1324.06\,{^{\circ }}\hbox {C}\)) is estimated to be within \(\pm 0.60\,\hbox {K}\) (\(k=2\)). This meets the needs of Thailand’s high-temperature thermocouple users—for which previously there has been no traceable calibration facility.     

New Filling Technique and Performance Evaluations of the Cr3C2?C Peritectic Fixed Point

The Cr₃C₂?C peritectic fixed point was investigated to test its capability to serve as a practical high-temperature fixed point. An improved filling technique where C/C sheet works as a wick and graphite paper as a hopper was applied successfully, and the long-term stability of the peritectic cell was evaluated by means of radiation thermometry. The repeatability of the melting point in one day was 7 mK with a melting range of approximately 100 mK. The cell was aged for 7 days, and the evaluated 56 melting temperatures during this period all fall within 90 mK, with a standard deviation of 19 mK. X-ray transmission photos showed that the ingot was filled uniformly in the crucible. After the evaluation of long-term stability, no clear degradation of the ingot shape and no leakage of molten metal were observed. From these results, it can be concluded that the Cr₃C₂?C peritectic cell has good stability and robustness, and the new filling technique was established. The impurity effect on the Cr₃C₂?C peritectic cell was also investigated by adding tungsten powder to another cell as the impurity component. After the observation of melting and freezing plateaux, the cell was cut in half to analyze the microstructure by means of electron probe microanalysis (EPMA) and laser ablation inductively coupled plasma mass spectrometer (LA-ICP-MS). The high concentration of impurity was observed in the area of the chromium-rich domain (eutectic mixture of Cr₇C₃ and Cr₃C₂), which suggests that impurities were rejected from the Cr₃C₂ peritectic phase during the peritectic freezing and were accumulated in the Cr₇C₃?Cr₃C₂ eutectic phase. This explains why the impurity effect is more severe for the Cr₇C₃?Cr₃C₂ eutectic point than for the Cr₃C₂?C peritectic point.     

Ga-In共晶固定点复现及赋值研究

次级固定点进一步分度温度计应用于温度校准已成为减小温度量值传递不确定度的重要方法.围绕Ga-In二元合金,以高复现水平为目标,详细介绍了大尺寸固定点容器研制、固定点灌注过程,开展了固定点复现性、亚配比剩余镓温坪验证实验研究;采用了切线交点法、均值法、三次多项式拟合法3种相变温度取值方法对Ga-In固定点进行了评价和分析...     

ZrC-C包晶固定点研制及评价

ZrC-C包晶固定点因其极高的名义相变温度(2882℃),超出了绝大多数高温加热炉的使用上限.通过改进自行设计的HT271型加热炉,使其工作温度上限提高到2900℃以上,满足了ZrC-C包晶固定点的使用要求.采用ZrC粉末和C粉末配置混合粉末,进行了ZrC-C包晶固定点的灌注和复现试验,共得到2组复现循环数据,其中第1...     

Bi-In-Sn合金熔化温坪优化方法探索

为了提高红外遥感高精度测量水平,研发适用于红外遥感测温范围的次级固定点已成为提高在轨温度标定精度的重要手段.针对红外遥感领域涉及的温度范围(190～350 K),研制了Bi-In-Sn三元合金固定点.为提高三元合金温坪复现水平,采用预熔方法对三元合金固定点进行预处理,分析不同热工况对三元合金温坪的影响,获得适用于该三元...     

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）。     

Manufacturing of MC Eutectics and Reproducibility of Pt-C Eutectic Fixed Points using a Thermogauge Furnace

National Institute of Metrology (NIM) (China) and National Physical Laboratory (NPL) (UK) have collaborated to construct metal-carbon eutectic alloy fixed points at NPL. A modified NPL Thermogauge furnace was vertically used to construct fixed points of Pd–C, Pt–C, Ru–C, and Ir–C. Breakage of Pd–C and Ru–C cells was traced to changes in furnace temperature gradients resulting from changing from horizontal to vertical operation. Subsequently, it was found that positioning the cell being filled so that the metal melting always starts from the top and freezing from the bottom to solve this problem. The constructed Pt–C cell was then compared to a Pt–C fixed point previously constructed by NIM. The results indicate that the two cells made independently agreed to be better than 40 mK.