Pd-C和Ru-C固定点的热力学和ITS-90温度测量

卢小丰; 张婷婷; 董伟; 唐小洁; 原遵东; 王铁军

doi:10.12338/j.issn.2096-9015.2020.9034

Pd-C和Ru-C固定点的热力学和ITS-90温度测量

doi: 10.12338/j.issn.2096-9015.2020.9034

中国计量科学研究院，北京 100029

基金项目: 国家重点研发计划项目(2016YFF0200101)

详细信息

作者简介:
卢小丰(1979-)，中国计量科学研究院副研究员，研究方向：辐射温度计量，邮箱：luxf@nim.ac.cn

计量
- 文章访问数: 437
- HTML全文浏览量: 205
- PDF下载量: 52
- 被引次数: 0
出版历程
- 网络出版日期: 2021-04-21
- 刊出日期: 2021-06-24

Temperature Measurement of Pd-C and Ru-C Cells at NIM

National Institute of Metrology, Beijing 100029, China

摘要

摘要: 报告了中国计量科学研究院在参与高温固定点热力学温度国际联合研究后对Pd-C和Ru-C两个新高温固定点的研究成果，为Pd-C(1492 ℃)和Ru-C(1953 ℃)设计了两种类型坩埚，可用于校准辐射温度计和高温热电偶。Pd-C和 Ru-C的国际温标值(T₉₀)是由固定点-基准高温计外推测量，热力学温度(T)则利用精密光电高温计LP4测量获得，其中LP4经过带有热力学温度值的Co-C(1324 ℃)、Pt-C(1738 ℃)和Re-C(2474 ℃)内插分度。实验结果表明：Pd-C和Ru-C的T与T₉₀之间的差值分别为0.25 K和0.29 K；Pd-C的T和T₉₀的不确定度分别为0.32 K和0.45 K, Ru-C分别为0.49 K和0.50 K。研究成果不仅为高温固定点的校准推广应用，也为传递热力学温度建立了重要基础。
- 计量学 /
- 高温固定点 /
- 辐射测温 /
- 热力学温度 /
- 不确定度 /
- 坩埚
Abstract: The results of the research on two new eutectic fixed point cells, Palladium-Carbon (Pd-C) and Ruthenium-Carbon (Ru-C), conducted by the National Institute of Metrology (NIM) after participating in an international joint study on high-temperature fixed point cells thermodynamic temperatures are reported. Two types of crucibles were designed for Pd-C (1492 °C) and Ru-C (1953 °C), which can be used to calibrate radiation thermometers and high-temperature thermocouples. The International Temperature Scale of 1990 values (T₉₀) of Pd-C and Ru-C are measured extrapolated from a primary standard thermometer, and the thermodynamic temperature (T) is obtained using a precision photoelectric pyrometer LP4 measurement, where LP4 is interpolated and indexed by Co-C (1324 °C), Pt-C (1738 °C) and Re-C (2474 °C) with thermodynamic temperature values. The experimental results show that the differences between T and T₉₀ of Pd-C and Ru-C are 0.25 K and 0.29 K, respectively; the uncertainties of T and T₉₀ of Pd-C are 0.32 K and 0.45 K, and those of Ru-C are 0.49 K and 0.50 K. The results not only promote the application of calibration for high-temperature fixed points, but also establish an important basis for transferring thermodynamic temperature.
- metrology /
- high temperature fixed point /
- radiation thermometry /
- thermodynamic temperature /
- uncertainty /
- crucibles

HTML全文

图 1 石墨坩埚示意图

Figure 1. Schematic diagram of graphite crucible

下载: 全尺寸图片幻灯片

图 2 坩埚和石墨环的分布示意图

Figure 2. Schematic diagram of the distribution of crucible and graphite rings

下载: 全尺寸图片幻灯片

图 3 InK和NIM固定点坩埚的温度差值

Figure 3. Temperature difference between InK and NIM fixed point crucibles

下载: 全尺寸图片幻灯片

图 4 固定点T与T₉₀的测量差值及以铜点T - T₉₀外推值

Figure 4. Measured discrepancy between T and T₉₀ of fixed points , and extrapolated value from T-T₉₀of Cu

下载: 全尺寸图片幻灯片

表 1 Pd-C和Ru-C坩埚参数

Table 1. Parameters of Pd-C and Ru-C crucibles

HTFP	编号	纯度	金属来源	质量/g	空腔直径/mm
Pd-C	0318	99.999%	Alfa Aesar	44.59	3
Pd-C	0518	99.999%	Alfa Aesar	41.33	7
Ru-C	1601	99.99%	Tanaka	39.30	3
Ru-C	1602	99.99%	Tanaka	41.04	7

下载: 导出CSV

表 2 Pd-C和Ru-C固定点的T₉₀值

Table 2. T₉₀ values of Pd-C and Ru-C fixed point

HTFP	编号	T₉₀/K
Pd-C	0318	1764.78
Pd-C	0518	1764.81
Ru-C	1601	2226.59
Ru-C	1602	2226.78

下载: 导出CSV

表 3 Pd-C和Ru-C 的T₉₀值不确定度评估/K

Table 3. Uncertainty evaluation of T₉₀value of Pd-C and Ru-C

不确定度	不确定度来源	Pd-C	Ru-C
T₉₀复现的不确定度	参考固定点的不确定度	0.034	0.052
	参考固定点的测量	0.051	0.032
	光谱响应度测量	0.024	0.067
	SSE	0.029	0.045
	非线性	0.014	0.032
	漂移	0.085	0.134
	环境条件	0.001	0.003
	增益	0.020	0.033
	信噪比	0.014	0.007
	重复性	0.095	0.112
高温固定点	空腔发射率	0.041	0.069
	瞄准法向	0.033	0.045
	拐点选取	0.075	0.020
	重复性	0.050	0.040
T₉₀不确定度	合成不确定度	0.21	0.25
T₉₀不确定度	扩展不确定度(k=2)	0.42	0.50

下载: 导出CSV

表 4 中国计量院自制高温固定点的T值与不确定度 /K

Table 4. T value and uncertainty of high temperature fixed point made by NIM

固定点	编号	△T_(InK-NIM)	T	U（k=2）
Co-C	5	0.015	1597.38	0.29
Pt-C	5	0.101	2011.33	0.36
Re-C	3	−0.092	2747.93	0.48

下载: 导出CSV

表 5 LP4测量Pd-C和Ru-C的T值

Table 5. T value of Pd-C and Ru-C measured by LP4

HTFP	编号	热力学温度值/K
HTFP	编号	650 nm	800 nm
Pd-C	0318	1764.98	1765.03
Pd-C	0518	1765.06	1765.10
Ru-C	1601	2226.91	2226.92
Ru-C	1602	2227.03	2227.07

下载: 导出CSV

表 6 Pd-C和Ru-C的热力学温度不确定度评价/K

Table 6. Evaluation of thermodynamic temperature uncertainty of Pd-C and Ru-C

不确定度	不确定度来源	Pd-C	Ru-C
LP4不确定度	Co-C固定点	0.07	0.03
	Pt-C固定点	0.10	0.19
	Re-C固定点	0.01	0.04
	SSE测量与修正	0.03	0.04
	非线性	0.02	0.05
	漂移	0.05	0.08
	环境条件	0.01	0.01
	增益	0.03	0.04
	信噪比	0.01	0.01
高温固定点	空腔发射率	0.04	0.07
	瞄准法向	0.03	0.04
	拐点选取	0.02	0.03
	重复性	0.05	0.04
T不确定度	合成不确定度	0.16	0.245
T不确定度	扩展不确定度(k=2)	0.32	0.49

下载: 导出CSV

表 7 中国计量院自制固定点T、T₉₀值以及T - T₉₀值/K

Table 7. The fixed point T, T₉₀ value and T-T₉₀ of NIM

HTFP	No.	T	T₉₀	T - T₉₀
Cu	01	1357.80	1357.73	0.07
Co-C	5	1597.38	1597.19	0.19
Pd-C	0318	1765.01	1764.78	0.23
Pd-C	0518	1765.08	1764.81	0.27
Pt-C	5	2011.33	2011.12	0.21
Ru-C	1601	2226.92	2226.59	0.33
Ru-C	1602	2227.05	2226.78	0.27
Re-C	3	2747.93	2747.32	0.61

下载: 导出CSV

参考文献(12)

[1]	YAMADA Y, SAKATE H, SAKUMA F, et al. Radiometric observation of melting and freezing plateaus for a series of metal-carbon eutectic points in the range 1330 °C to 1950 °C[J]. Metrologia, 1999, 36: 207-210. doi: 10.1088/0026-1394/36/3/6
[2]	WOOLIAMS E R, MACHIN G, LOWE D H, et al. Metal (carbide)–carbon eutectics for thermometry and radiometry: a review of the first seven years[J]. Metrologia, 2006, 43: 11-25.
[3]	SADLI M, BLOEMBERGEN P, KHLEVNOY B, et al. An International Study of the Long-Term Stability of Metal–Carbon Eutectic Cells[J]. Int. J. Thermophys, 2011, 32: 1786-99. doi: 10.1007/s10765-011-1009-8
[4]	PEARCE J V, OGURA H, IZUCHI M, et al. Evaluation of the Pd–C eutectic fixed point and the Pt/Pd thermocouple[J]. Metrologia, 2009, 46: 473-479. doi: 10.1088/0026-1394/46/5/011
[5]	OGURA H, IZUCHI M, ARAI M. Evaluation of cobalt–carbon and palladium–carbon eutectic point cells for thermocouple calibration[J]. Int. J. Thermophys, 2008, 29: 210-221. doi: 10.1007/s10765-007-0320-x
[6]	Elliott C J, Large M J, Pearce J V. Compatibility of Materials for Use at High Temperatures with W–Re Thermocouples[J]. Int J Thermophys, 2014, 35: 1202-1214. doi: 10.1007/s10765-014-1703-4
[7]	YUAN Z, LU X, WANG J, et al. Realization of ITS-90 Above the Silver Point at the NIM[J]. Int. J. Thermophys, 2011, 32: 1611-1621. doi: 10.1007/s10765-011-0970-6
[8]	WOOLLIAMS E R, ANHALT K, M. BALLICO, et al. Thermodynamic temperature assignment to the point of inflection of the melting curve of high-temperature fixed points[J]. Phil. Trans. R. Soc. A, 2015, 374: 44.
[9]	SAKUMA F, HATTORI S. Temperature: Its Measurement and Control in Science and Industry[J]. New York: AIP, 1982, 15: 421 - 427.
[10]	卢小丰, 原遵东, 董伟, 等, 应用高温固定点校准精密光电高温计[J]. 计量学报, 2017, 38 (5): 584 – 588.
[11]	ANHALT K, HARTMANN J, LOWE D, et al. Thermodynamic temperature measurement of Co-C, Pd-C, Pt-C and Ru-C eutectic fixed-point cells[J]. Metrologia, 2006, 43: S78-S83. doi: 10.1088/0026-1394/43/2/S16
[12]	YUAN Z, WANG T, LU X, et al. T90 Measurement of Co-C, Pt-C, and Re-C High-Temperature Fixed Points at the NIM[J]. Int. J. Thermophys, 2011, 32: 1744-1752. doi: 10.1007/s10765-011-0993-z