激光闪光法测量固体材料热扩散率的实验研究
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摘要
热扩散率是表征材料内部非稳态导热过程的重要热物理参数之一,准确测量材料的热扩散率,对于了解材料的导热性能,进行材料非稳态导热过程分析以及研究新材料都具有非常重要的意义。
课题在中国计量科学研究院最新建立的激光热导仪上,重新开发了一套测量更准确、数据处理更方便的自动采集软件,并分别用不同直径的K型热电偶和S型热电偶,对五个不同厚度的316不锈钢样品以及德国物理技术研究院(PTB)标准试样的热扩散率,从常温到1000℃进行了测量。实验结果表明,直径为0.1mm的K型热电偶由于其具有灵敏度高,响应速度快,热电势大,测温范围广,易于焊接等优点,因此,在该装置上得到了较好的实验结果。
在确定测温热电偶的基础上,又分别对不同的样品厚度、不同的激光能量、不同的漏热修正方法对热扩散率测量结果所带来的差异一一进行了比较,发现样品热扩散率的测量值基本上随着样品厚度的增加而增大,并且每种样品均有其合适的厚度范围；热扩散率与激光能量大小的依赖关系并不明显；Cowan的漏热修正法、ASTM漏热修正法以及参数估计法各有其适用的温度范围,通过与参考值的比较,前两种方法更适合于本套实验系统。这些研究分析工作,对于提高该装置的性能、确定合适的测量方法等都具有重要的实际应用价值。
最后以0.1mm K型热电偶对PTB标准试样,在常温、300℃、500℃、800℃、1000℃进行了测量,测量值在各个温度点的相对标准偏差均小于2%,对实验数据进行了激光有限脉冲宽度、热膨胀、漏热以及热电偶响应时间修正,修正后的结果在常温到1000℃与欧洲比对结果(参考值)进行比较,其相对于PTB参考值的相对偏差值均小于2%,并给出了试样在各温度点的测量不确定度。
Thermal diffusivity is one of the important parameters for nonsteady heat conduction. Precise measurement of thermal diffusivity is significant for the investigation of nonsteady heat conduction, the study of thermophysical properties of materials, the development of new materials.
The current study is to investigate the measurement difference arising from different experimental conditions. New software, which is more efficient and precise, has been developed. An evualation on the effect of the K and S type thermocouples of different diameters has been made by the measurements on the 316 stainless steel samples of five different thicknesses and the reference sample of Physikalisch-Technische Bundesanstalt (PTB) over the temperature ranging from room temperature to 1000℃. The measurement results demonstrate that the K type thermocouple of the diameter of 0.1 mm has the characteristics of high sensitivity, speedy responsivity, large potential, wide temperature range and easy welding. This thermocouple is proper for measuring thermal diffusivity with the new device.
By applying K type thermocouple of 0.1 mm diameter, the effect of the thickness of tested samples, the output power of laser, the different heat loss correction methods have been investigated. The investigations demonstrate that the measured thermal diffusivity increases with increasing the thickness of samples and is nearly invariant with the output power of laser. The Cowan heat-loss correction method, the parameter estimation method and the American Society for Testing & Materials (ASTM) heat-loss method has different application temperature range. The comparison indicates that the Cowan and the ASTM correction methods are more available for the new device. The investigation is very important for the improvement of the apparatus's capability and the selection of the best metrical method.
The measurements have been conducted respectively over the room temperature,300℃, 500℃,800℃,1000℃on the PTB reference samples. The comparison with the given reference values of the tested samples presents a relative deviation less than 2%. The measurement results have been corrected for the finite pulse-time, the thermal expansion, the heat loss and the response time of thermocouple.
课题在中国计量科学研究院最新建立的激光热导仪上,重新开发了一套测量更准确、数据处理更方便的自动采集软件,并分别用不同直径的K型热电偶和S型热电偶,对五个不同厚度的316不锈钢样品以及德国物理技术研究院(PTB)标准试样的热扩散率,从常温到1000℃进行了测量。实验结果表明,直径为0.1mm的K型热电偶由于其具有灵敏度高,响应速度快,热电势大,测温范围广,易于焊接等优点,因此,在该装置上得到了较好的实验结果。
在确定测温热电偶的基础上,又分别对不同的样品厚度、不同的激光能量、不同的漏热修正方法对热扩散率测量结果所带来的差异一一进行了比较,发现样品热扩散率的测量值基本上随着样品厚度的增加而增大,并且每种样品均有其合适的厚度范围；热扩散率与激光能量大小的依赖关系并不明显；Cowan的漏热修正法、ASTM漏热修正法以及参数估计法各有其适用的温度范围,通过与参考值的比较,前两种方法更适合于本套实验系统。这些研究分析工作,对于提高该装置的性能、确定合适的测量方法等都具有重要的实际应用价值。
最后以0.1mm K型热电偶对PTB标准试样,在常温、300℃、500℃、800℃、1000℃进行了测量,测量值在各个温度点的相对标准偏差均小于2%,对实验数据进行了激光有限脉冲宽度、热膨胀、漏热以及热电偶响应时间修正,修正后的结果在常温到1000℃与欧洲比对结果(参考值)进行比较,其相对于PTB参考值的相对偏差值均小于2%,并给出了试样在各温度点的测量不确定度。
Thermal diffusivity is one of the important parameters for nonsteady heat conduction. Precise measurement of thermal diffusivity is significant for the investigation of nonsteady heat conduction, the study of thermophysical properties of materials, the development of new materials.
The current study is to investigate the measurement difference arising from different experimental conditions. New software, which is more efficient and precise, has been developed. An evualation on the effect of the K and S type thermocouples of different diameters has been made by the measurements on the 316 stainless steel samples of five different thicknesses and the reference sample of Physikalisch-Technische Bundesanstalt (PTB) over the temperature ranging from room temperature to 1000℃. The measurement results demonstrate that the K type thermocouple of the diameter of 0.1 mm has the characteristics of high sensitivity, speedy responsivity, large potential, wide temperature range and easy welding. This thermocouple is proper for measuring thermal diffusivity with the new device.
By applying K type thermocouple of 0.1 mm diameter, the effect of the thickness of tested samples, the output power of laser, the different heat loss correction methods have been investigated. The investigations demonstrate that the measured thermal diffusivity increases with increasing the thickness of samples and is nearly invariant with the output power of laser. The Cowan heat-loss correction method, the parameter estimation method and the American Society for Testing & Materials (ASTM) heat-loss method has different application temperature range. The comparison indicates that the Cowan and the ASTM correction methods are more available for the new device. The investigation is very important for the improvement of the apparatus's capability and the selection of the best metrical method.
The measurements have been conducted respectively over the room temperature,300℃, 500℃,800℃,1000℃on the PTB reference samples. The comparison with the given reference values of the tested samples presents a relative deviation less than 2%. The measurement results have been corrected for the finite pulse-time, the thermal expansion, the heat loss and the response time of thermocouple.
引文
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[3]刘雄飞,傅友军,ALN热扩散率测试方法的研究,计量技术,1999,No.9,19.
[4]唐大伟,荒木信幸,应用激光闪光法测量簿膜材料的热扩散率,锦州师范学院学报(自然科学版)2002年3月,第23卷,第1期,1-7。
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[6]王培吉,范素华,激光光热辐射技术测量不透明符合材料的热扩散率,中国激光,2000年12月,第27卷,第12期,1129。
[7]王昆林,非稳态法测定不良导体的热导率,广西民族学院学报(自然科学版),2002年8月,第8卷,第3期,19。
[8]童文辉,沈峰满,柴田浩幸,王文忠,杨院生,早稻田嘉夫,高桥礼二郎,八木顺一郎,高炉常用耐火材料导热系数的测定,金属学报,2002年9月,第38卷,第9期,983-988。
[9]张文华,王学泽,等静压金属铍材料热常数测试,稀有金属,2003年1月,第27卷,第1期,219。
[10]何小瓦,何凤梅,卫锦先,簿膜材料和纤维材料的热扩散率测量,宇航材料工艺,1997年,第2期,49-53。
[11]张立,孙宝琦,WC-Co-Ni硬质合金热扩散率的研究,硬质合金,1994,第11卷,第2期。
[12]Shen Zhu, C.Li, Ching-Hua Su, B.Lin, H.Ban, R.N.Scripa, S.L.Lehoczky, Thermal diffusivity,thermal conductivity,and specicific heat capacity measurements of molten tellurium, Journal Crystal Growth., 2003,250,269-273.
[13]吴清仁,奚同庚,张永兴,刘振群,PZT基铁电材料F-P相变及其热物理性质,华南理工大学学报(自然科学版),1997,第25卷,第8期,31。
[14]J.Sun, J.P.Longtin,T.F.IrvineJr, Laser-based thermal pulse measurement of liquid thermophysical properties.International Journal of Heat and Mass Transfer,2001,44,645.
[15]王亚平,丁秉钧,CuCr触头合金热扩散率的实验研究,High Voltage Apparatus, Febuary 2002Vol.38,No.1,4.
[16]Dean-Mo Liu, Effect of temperature on measuring the thermal diffusivity of ceramic of different specimen thickness by using a laser-pulse method,Materials Science and Engineering,1997, B47,191.
[17]Xue Jian and R.Taylor, The effect of sample thickness of aluminium nitride AIN on thermal diffusivity measurementsusingthelaserflashtechnique, J.CENT.-SOUTHINST.MIN.METALL,Vol.22,No.4,413.
[18]Ana Paula F.Albers,Thomaz A.G.Restivo,Luciano Pagano,Joao B.Baldo,"Effect of testing conditions on the laser flash thermal diffusivity measurements of ceramics",Thermochimica acta,370(2001),111.
[19]R.C.Heckman,Finite pulse-time and heat-loss effects in pulse thermal diffusivity measurements, J.Appl.Phys., April 1973, Vol.44,No.4,1455.
[20]J.A.Cape and GW.Lehman, Temperature and Finite Pulse-Time Effects in the Flash Method for measuring Thermal Diffusivity, Journal of Applied Physics,1963, Vol.34, No.7,1909.
[21]ASTM Designation:E1461-92,Standard test method for thermal diffusivity of solids by the flash method,1992,933.
[22]J.Xue,X.Liu,Y.Lian,and R.Taylor,The Effects of a Finite pulse Time in the Flash Thermal Diffusivity Method, International Journal of Thermophysics,1993,Vol.14,No.1,123.
[23]谭俊杰,何东明,顾毓沁,朱德忠,热电偶响应对激光脉冲法测量热扩散率的影响,宇航计测技术,1995,第15卷,第4期,35。
[24]W.J.Parker, Proceeding of the Second Conference on Thermal Conductivity,1962, p.33 (unpublished).
[25]H.S.Carslaw and J.C.Jaeger, Conduction of Heat in Solids, Oxford:Oxford University press,New York, 2nd ed,1959, pp.126.
[26]R D.Cowan,, Pulse Method of Measuring Thermal Diffusivity at High Temperatures, Journal of applied physics,1963, Vol 34, No.4,926.
[27]L.M.Clark Ⅲ and R.E.Taylor, Radiation loss in the flash method for thermal diffusivity, Journal of Applied Physics,1975, Vol.46,No.2,714-719.
[28]Watt,D.A., Theory of Thermal Diffusivity by Pulse Technique, Br.J.Apply.Phys,1966, Vol.37,231.
[29]A.R.Mendelsohn, The Effect of Heat Loss on the Flash Method of Determining Thermal Diffusivity, Applied Physics Letters,1963, Vol.2, No.1,19.
[30]J.A.McKay and J.T.Schriempf, Corrections for nonuniform surface-heating errors in flash-method thermal-diffusivity measurements, Journal of Applied Physics,1976, Vol.47, No.4,1668.
[31]奚同庚,无机材料热物性学,上海科学技术出版社,1981年12月,第一版,173。
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