金属碳共晶及包晶高温固定点研究
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摘要
随着科学技术的发展，人们对高温温度测量的准确性提出了更高的要求。作为温度量值源头的国际温标，目前在铜凝固点以上的高温区缺乏参考固定点，导致高温测量的不确定度随温度升高迅速增大。建立基于金属和碳共晶和包晶相变的高温固定点是解决这一问题的有效途径。论文从高温固定点的建立、国际温标赋值、影响赋值的关键因素以及国际温标一致性比对等方面，围绕应用高温固定点技术改善高温区国际温标开展研究。
建立了高温固定点的灌注和复现系统，改进了核心设备高温炉，延伸上限使用温度至2800℃，满足了WC-C包晶超高温固定点的灌注和复现需求。通过改进坩埚结构和灌注方法，研制了耐用稳定、具备优良计量特性的Co-C (名义温度1324℃)、 Pt-C (1738℃)、Re-C (2474℃)、WC-C(2747℃)系列高温固定点。
开展了对高温固定点的ITS-90赋值研究。针对温标复现的主要不确定度贡献项之一，光电高温计的非线性，建立了基于光通量倍增法和LED光源的新测量系统，实现了光电高温计在更高温度下的非线性测量。
研究了高温固定点相变温度赋值模型及关键影响因素。建立了基于凝固实验的外推至0速率的平衡相变温度理论模型，选择Pt-C进行了实验验证，理论与实验吻合良好。本模型将被国际温度计量委员会采用，用于高温固定点的热力学温度赋值。理论上研究了杂质对共晶相变温度的作用机理，建立了修正杂质效应的理论模型和修正方法。实验研究了Co-C高温固定点复现中的高温炉温度梯度效应。
基于英国国家物理实验室(NPL)的ITS-90温标，实验研究了中国、英国、西班牙三国提供的Co-C（1324℃）, Pt-C（1738℃），Re-C（2474℃）高温固定点的复现性；并利用固定点比对了三国高温温标一致性。结果表明：三种高温固定点的复现性良好，均优于0.1度。三国温标的差异在Co-C和Pt-C均小于0.1℃，在Re-C小于0.4℃。良好的一致性说明高温固定点技术将成为未来高温区关键比对的可靠技术。
With the evolution of science and technology, accurate measurement ofhigh temperature is vital and imminently required. However, the uncertaintyin high temperature measurement increases rapidly with increasingtemperature, since the currently implemented international temperature scale(ITS-90), relying upon radiation thermometry above the silver point (962C)is in lack of reference fixed points above the copper point (1084C). Thediscovery of high-temperature fixed points (HTFPs) based upon metal-carboneutectics and peritectics will drastically change the situation. In this paper wewill f℃us on research of improving the temperature scale above the copperpoint by using these HTFPs.The construction of HTFPs, the ITS-90temperature assignment to them, key factors influencing the implementationof HTFPs, international comparisons of the ITS-90, as locally realized, bymeans of HTFPs will be studied in turn in this thesis, in Chapters2to6,respectively.
Experimental systems-crucibles, ingots and furnaces-were developed tofill and subsequently realize HTFPs, i.e. providing the conditions toreproducibly realize melting and freezing curves. A high temperature furnacewas modified for use up to2800℃to satisfy the demand of filling andrealizing the WC-C peritectic fixed point. Several sets of Co-C (nominaltemperature1324℃), Pt-C (1738℃), Re-C (2474℃), WC-C(2747℃) fixedpoints of different structure were filled by different filling methods, and theyall showeds robust, stable and accurate metrological characteristics.
The T90assignments to HTFPs were studied. Non-linearity of radiationthermometers, one of the main components in the uncertainty budgetass℃iated with the realization of ITS-90by radiation thermometry-above thesilver point-was studied, using the superposition method and involving LEDswith high radiance output.
In any temperature scale, to get a unique point for reference, the phase transition temperature to be referred to, is that of the system inthermodynamic equilibrium, in its pure state. How to extrapolate to thisunique point, in the case of the selected HTFPs, and the key influence factorsto be taken into account, are important subjects discussed in this thesis. Pt-Cwas chosen and experimentally studied through freezing rate experiments tovalidate the procedures and models involved. The model will be adopted byCCT-WG5to assign thermodynamic temperature to HTFPs. The effect ofimpurities on the eutectic phase transition temperature was studiedtheoretically, and the method to correct for the impurity effect is reported here.Finally, the furnace-gradient effect on the realization of the Co-C point wasexperimentally studied as reported in this thesis.
The reproducibility of the Co-C, Pt-C, and Re-C HTFPs–in terms ofmelting characteristics filled by NIM, China,NPL, UK and CEM, Spain,were studied at NPL with NPL’s ITS-90as a reference, with as result that forall the three kinds of HTFPs the reproducibility was better than0.1℃. Aprototype comparison of the ITS-90, as realised by NIM, NPLand CEM, usingCo-C, Pt-C, and Re-C as transfer standards is reported. From thesemeasurements a comparison reference value (CRV) was derived. At the Co-Cand Pt-C points the deviation from the CRV was <0.1℃for all threeinstitutes, at the Re-C point the deviation was <0.4℃. Given the consistentperformance of the HTFPs they should be seriously considered as scalecomparison artefacts of choice when comparing l℃al realisations of theITS-90and of l℃al measurements of thermodynamic temperature.
建立了高温固定点的灌注和复现系统，改进了核心设备高温炉，延伸上限使用温度至2800℃，满足了WC-C包晶超高温固定点的灌注和复现需求。通过改进坩埚结构和灌注方法，研制了耐用稳定、具备优良计量特性的Co-C (名义温度1324℃)、 Pt-C (1738℃)、Re-C (2474℃)、WC-C(2747℃)系列高温固定点。
开展了对高温固定点的ITS-90赋值研究。针对温标复现的主要不确定度贡献项之一，光电高温计的非线性，建立了基于光通量倍增法和LED光源的新测量系统，实现了光电高温计在更高温度下的非线性测量。
研究了高温固定点相变温度赋值模型及关键影响因素。建立了基于凝固实验的外推至0速率的平衡相变温度理论模型，选择Pt-C进行了实验验证，理论与实验吻合良好。本模型将被国际温度计量委员会采用，用于高温固定点的热力学温度赋值。理论上研究了杂质对共晶相变温度的作用机理，建立了修正杂质效应的理论模型和修正方法。实验研究了Co-C高温固定点复现中的高温炉温度梯度效应。
基于英国国家物理实验室(NPL)的ITS-90温标，实验研究了中国、英国、西班牙三国提供的Co-C（1324℃）, Pt-C（1738℃），Re-C（2474℃）高温固定点的复现性；并利用固定点比对了三国高温温标一致性。结果表明：三种高温固定点的复现性良好，均优于0.1度。三国温标的差异在Co-C和Pt-C均小于0.1℃，在Re-C小于0.4℃。良好的一致性说明高温固定点技术将成为未来高温区关键比对的可靠技术。
With the evolution of science and technology, accurate measurement ofhigh temperature is vital and imminently required. However, the uncertaintyin high temperature measurement increases rapidly with increasingtemperature, since the currently implemented international temperature scale(ITS-90), relying upon radiation thermometry above the silver point (962C)is in lack of reference fixed points above the copper point (1084C). Thediscovery of high-temperature fixed points (HTFPs) based upon metal-carboneutectics and peritectics will drastically change the situation. In this paper wewill f℃us on research of improving the temperature scale above the copperpoint by using these HTFPs.The construction of HTFPs, the ITS-90temperature assignment to them, key factors influencing the implementationof HTFPs, international comparisons of the ITS-90, as locally realized, bymeans of HTFPs will be studied in turn in this thesis, in Chapters2to6,respectively.
Experimental systems-crucibles, ingots and furnaces-were developed tofill and subsequently realize HTFPs, i.e. providing the conditions toreproducibly realize melting and freezing curves. A high temperature furnacewas modified for use up to2800℃to satisfy the demand of filling andrealizing the WC-C peritectic fixed point. Several sets of Co-C (nominaltemperature1324℃), Pt-C (1738℃), Re-C (2474℃), WC-C(2747℃) fixedpoints of different structure were filled by different filling methods, and theyall showeds robust, stable and accurate metrological characteristics.
The T90assignments to HTFPs were studied. Non-linearity of radiationthermometers, one of the main components in the uncertainty budgetass℃iated with the realization of ITS-90by radiation thermometry-above thesilver point-was studied, using the superposition method and involving LEDswith high radiance output.
In any temperature scale, to get a unique point for reference, the phase transition temperature to be referred to, is that of the system inthermodynamic equilibrium, in its pure state. How to extrapolate to thisunique point, in the case of the selected HTFPs, and the key influence factorsto be taken into account, are important subjects discussed in this thesis. Pt-Cwas chosen and experimentally studied through freezing rate experiments tovalidate the procedures and models involved. The model will be adopted byCCT-WG5to assign thermodynamic temperature to HTFPs. The effect ofimpurities on the eutectic phase transition temperature was studiedtheoretically, and the method to correct for the impurity effect is reported here.Finally, the furnace-gradient effect on the realization of the Co-C point wasexperimentally studied as reported in this thesis.
The reproducibility of the Co-C, Pt-C, and Re-C HTFPs–in terms ofmelting characteristics filled by NIM, China,NPL, UK and CEM, Spain,were studied at NPL with NPL’s ITS-90as a reference, with as result that forall the three kinds of HTFPs the reproducibility was better than0.1℃. Aprototype comparison of the ITS-90, as realised by NIM, NPLand CEM, usingCo-C, Pt-C, and Re-C as transfer standards is reported. From thesemeasurements a comparison reference value (CRV) was derived. At the Co-Cand Pt-C points the deviation from the CRV was <0.1℃for all threeinstitutes, at the Re-C point the deviation was <0.4℃. Given the consistentperformance of the HTFPs they should be seriously considered as scalecomparison artefacts of choice when comparing l℃al realisations of theITS-90and of l℃al measurements of thermodynamic temperature.
引文
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