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。     

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。     

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.     

300℃以上热电偶量传体系问题分析及对策

针对目前300℃以上热电偶量传体系存在不确定度过大、计量能力不满足要求等问题,分析了高温共晶点和实用型固定点温度复现、纯金属热电偶温度测量和1500℃以上高温热电偶校准等技术的最新进展,提出基于固定点温度复现方法的新的量值传递体系设想,可大大减小热电偶量值传递的不确定度,使各级计量标准装置不确定度分布更为合理,能保证热电偶量值的逐级量传,满足科研生产对热电偶的溯源要求。     

Fe-C共晶点的复现与温坪特性的研究

在温度量传体系中,铜凝固点(1084.62 ℃)以上目前还没有其他纯金属固定点,而金属-碳共晶点作为新兴的固定点具备良好的复现性,可补充铜点以上的温度固定点,拓展现有的高温温度量值传递水平。尽管Fe-C共晶点非常接近铜凝固点,但其仍有较高的使用价值,可为更高温共晶点灌注及复现提供宝贵的经验。用一等标准S偶对Fe-C共晶点的温坪进行测量,其共晶点温度为1152.4 ~1152.5 ℃。     

Co-C共晶点研制及评价

根据国际温度咨询委员会辐射测温工作组(CCT-WG5)对世界各国计量机构开展Co-C共晶点研制工作的相关要求,设计并搭建了Co-C共晶点灌注系统,采用直接共晶法成功灌注了满足复现实验要求的Co-C共晶点坩埚。针对直接共晶灌注法效率低、坩埚破裂风险大的缺陷,提出了对灌注方法的改进方案,并依据该方案成功灌注了2个Co-C共晶点坩埚。对灌注的Co-C-2#共晶点进行了复现试验,结果显示:拐点温度的不确定度为5.3 mK,满足小于10 mK的CCT要求;短期重复性为9.6 mK,满足小于20 mK的CCT要求。     

一种三段加热的立式高温均热炉的研制

介绍了一种用于Fe-C高温共晶点装置复现的三段加热立式高温均热炉, 包括炉体的设计结构、 温度控制系统、 复现用腔体的密封结构设计和冷却水与充气保护系统等. 对炉体温场的测试结果表明: 该炉体能够满足设计的预期要求, 实现Fe-C高温共晶点的复现.     

一种三段加热立式高温均热炉的研制

介绍了一种用于Fe-C高温共晶点装置复现的三段加热立式高温均热炉,包括炉体的设计结构、温度控制系统、复现用腔体的密封结构设计和冷却水与充气保护系统等。对炉体温场的测试结果表明:该炉体能够满足设计的预期要求,实现Fe-C高温共晶点的复现。     

Development and Realization of Iron–Carbon Eutectic Fixed Point at NPLI

The concept of metal–carbon eutectic temperature fixed point has been introduced in 1999 and is extensively being investigated by thermometry researchers to cover the high-temperature range above copper fixed point. Metal–carbon eutectic fixed points also helped to provide direct traceability with reduced associated uncertainty in the high temperature range for thermometry and radiometry applications. In view of this, CSIR-National Physical Laboratory, India (NPLI) has developed iron–carbon (Fe–C, 1153 °C) eutectic fixed point cell in the graphite crucible and realized by using the noble metal thermocouples. The preparation parameters such as design and fabrication of a graphite crucible, Fe:C eutectic composition and filling procedure, furnace profile, melting and freezing plateau measurements, heat flux immersion, inhomogeneity, etc. have been optimized and presented in this paper. The measurement uncertainty of the Fe–C eutectic cell realized with Type-S thermocouple was estimated to be 3.04 μV (0.25 °C) at coverage factor k = 2.     

Realization of Fe–C Eutectic Point Using an Alumina Crucible

As another crucible material for metal–carbon eutectic points, alumina ceramic was used in the first trial to make an Fe–C eutectic point for the calibration of a thermocouple. Its melting and freezing behavior was tested 26 times with a type S thermocouple at various melting offset temperatures, namely, +4 °C, +9 °C, and +19 °C, and at a fixed freezing offset temperature of ?11 °C. The melting emf is reproducible independent of the melting offset temperatures, and the standard deviation of the 26 melting temperatures is 0.02 °C without breakage of the cell. The difference of melting emf between alumina Fe–C and graphite Fe–C fixed points is only 25 mK within an uncertainty of 0.39 °C (k = 2). The melting behaviors of an alumina cell are quite similar to a common graphite cell. Thus, alumina can be used as a crucible material in an Fe–C eutectic system without breakage, and it can be used at a higher temperature range. As possible application systems using alumina crucibles, Pd–C and Si–SiC eutectic points are suggested.     

一种新型高温热电偶性能测试系统的研制

热电偶在高温使用时容易受到材料相容性、氧化等多种因素的影响,产生显著的不均匀性,需要对其进行性能测试,以进一步判断其测温准确度。研制了一种新结构的高温管式炉,控温热电偶布置方式有利于提高恒温段温度均匀性;在此基础上,搭建了一套高温热电偶测试系统,并对系统性能进行了理论模拟和实验研究。测试结果显示,在400～1 000℃范围内,测试系统的温度稳定性优于±0.25℃;长度为150 mm的恒温段的温度均匀性优于±0.35℃,表明测试系统的性能够满足热电偶性能测试的需求。     

Evaluation of Cobalt–Carbon and Palladium–Carbon Eutectic Point Cells for Thermocouple Calibration

Two cobalt–carbon (Co–C) eutectic point (1,324 °C) cells and one palladium–carbon (Pd–C) eutectic point (1,492 °C) cell were constructed for thermocouple calibration. The lengths of the Co–C and Pd–C cells were 297 mm, 140 mm, and 140 mm, respectively. The melting and freezing plateaux at the Co–C and Pd–C eutectic points were observed using Pt/Pd thermocouples. The repeatability of the plateau, the effect of the surrounding temperature, and the temperature profile in the cell were measured, and the heat flux effect along the thermometer well was evaluated. When the plateaux of Co–C (297 mm height), Co–C (140 mm height), and Pd–C cells, were measured three times, seven times, and six times, respectively, the standard deviations of the melting points were 0.1 μV, 0.1 μV, and 0.4 μV, respectively. According to the temperature profiles along the thermometer well during the melting plateaux, it was found that the Pt/Pd thermocouple should be inserted at least 9.5 cm, 5 cm, and 6 cm below the surface of the eutectic alloys in the Co–C (297 mm height), Co–C (140 mm height), and Pd–C cells with the furnace set-point 16 °C above the melting 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...     

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.