K; t . +2 x N ‘ . This is to certify that the thesis entitled COMPARISON OF THERMAL DIFFUSIVITY MEASUREMENT TECHNIQUES presented by XIN HUANG has been accepted towards fulfillment of the requirements for the MS. degree in MECHANICAL ENGINEERING . 34 ( Major of or’s Signature lo MAy 2'sz Date MSU is an Affirmative Action/Equal Opportunity Institution 0 ~ A ‘ _, __.'_.¢‘.. ----"-—-~. '. __ - LIBRARY Michigan State University PLACE IN RETURN BOX to remove this checkout from your record. To AVOID FINES return on or before date due. MAY BE RECALLED with earlier due date if requested. DATE DUE DATE DUE DATE DUE 6/01 c:/CIRC/DateDue.p65—p.15 COMPARISON OF THERMAL DIFFUSIVITY MEASUREMENT TECHNIQUES By Xin Huang A THESIS Submitted to Michigan State University in partial fulfillment of requirements for the degree of MASTER OF SCIENCE Department of Mechanical Engineering 2004 ABSTRACT COMPARISON OF THERMAL DIFFUSIVITY MEASUREMENT TECHNIQUES By Xin Huang Accurate knowledge of thermal diffusivity is important for thermal analysis design. Although ofien assumed to respond isotropically, many polymers and composite materials exhibit thermally anisotropic responses. Materials with unknown or changing properties especially challenge the design of experiments to measure thermal diffusivities. Three thermo—optical techniques that have been proposed to measure anisotropic thermal diffusivities are the flash, thermal wave, and flash-field methods. In this work, D- optimum criteria are applied to optimize experimental parameters such as the number of temperature sensors and sensor positions in the flash method, or the number of measurements and measurement times in the other two methods. The modification of these experimental parameters can be easily achieved after an experiment for which the temperature field history of one of the specimen surfaces is measured, such as by an infrared camera. Here, each of these methods is optimized using simulated experimental temperature responses calculated for radially symmetric thermal diffusivity; noise has been added to simulate experimental data. These optimizations are then compared to determine the preferred technique for this material symmetry. ACKNOWLEDGMENTS I am grateful to my thesis advisor, Dr. Neil Wright, for his guidance and support during my thesis study. In particular, I want to acknowledge the useful discussions with Dr. James Beck and Sean Davis. I would like to thank Dr. James Beck and Dr. Craig Somerton for serving on my thesis defense committee. I owe a debt of thanks to all my friends at Michigan State University, especially to Jian Wu, Xingkai Chi, Yanbing Li and Liping Jia, for their encouragement and help during my time at MSU. Finally, special thanks are extended to my parents and the rest of my family for their love and support. TABLE OF CONTENTS LIST OF FIGURES ....................................................................................................... v LIST OF TABLES ...................................................................................................... viii CHAPTER 1 INTRODUCTION ........................................................................... 1 CHAPTER 2 OPTIMIZATION METHOD ........................................................ 5 2.] Mathematical Model ............................................................................................... 5 2.2 Estimation Technique ............................................................................................. 8 2.3 Optimization Method ............................................................................................ 10 CHAPTER 3 OPTIMIZATION ........................................................................... 13 3.1 Flash Method ........................................................................................................ 13 3.1.1 Temperature Simulation ................................................................................ 13 3.1.2 Sensitivity Analysis ...................................................................................... 14 3.1.3 Optimization ................................................................................................. 21 3.2 Thermal Wave and Flash-field Methods ............................................................... 32 3.2.1 Temperature Simulation ................................................................................ 32 3.2.2 Sensitivity Analysis ...................................................................................... 34 3.2.3 Optimization ................................................................................................. 34 CHAPTER 4 COMPARISON OF METHODS ............................................... 45 CHAPTER 5 CONCLUSION .............................................................................. 49 REFERENCE ................................................................................................................ 51 LIST OF FIGURES Figure 2.1 Schematic representation of the mathematical model. ...................................... 6 Figure 3.1 Schematic representation of the flash method with an extended heating. Heating occurs within the radius rp on the front face. Temperature sensors are positioned at Tm] and Tmz. ................................................................................................................ 13 Figure 3.2 Simulation of temperature rise at various radii for the flash method with a short heat pulse (a) and an extended heating (b) ............................................................... 16 Figure 3.3 Normalized sensitivity coefficients of axial thermal diffusivity (a2) for the flash method with a short heat pulse (a) and an extended heating (b). ............................. 17 Figure 3.4 Normalized sensitivity coefficients of radial thermal diffiisivity (arr) for the flash method with a short heat pulse (a) and an extended heating (b). ............................. 18 Figure 3.5 Normalized sensitivity coefficients of Biot number (H ) for the flash method with a short heat pulse (a) and an extended heating (b) .................................................... 19 Figure 3.6 Normalized sensitivity coefficients of flash (Q) for the flash method with a short heat pulse (a) and of heat flux ( q") for the flash method with an extended heating (b). ..................................................................................................................................... 20 Figure 3.7 Optimization of measurement time (to, if) for the flash method with a short heat pulse (a) and an extended heating (b). The heating time (t p = 30 s) and heating area (rp =2mm)are fixed. ..................................................................................................... 23 Figure 3.8 Optimization of sensor position (rm) and final measurement time (t f ) for the extended flash method, with initial measurement time to =10 s . The heating time (t p = 30 s) and heating area (rp = 2 mm) are fixed ........................................................ 24 Figure 3.9 Optimization of the second sensor position (rm, 2) for the extended flash method, with the first sensor at the center on the rear surface and initial measurement time to =10 s . The heating time (tp = 30 s) and heating area (rp = 2 mm) are fixed. .25 Figure 3.10 Optimization of positions of both sensors (rm, 1 , rm, 2) for the extended flash method. The ATZ of each point is obtained with optimized measurement time interval. The heating time (t p = 30 s) and heating area (rp = 2 mm) are fixed. .......................... 26 Figure 3.11 Optimization of positions of the second and third sensors (rm, 2, rm,3) for the extended flash method, with the first sensor at the center on the rear surface. The AB of each point is obtained with optimized measurement time interval. The heating time (tp=3OS)andheatarea(rp=2mm)arefixed ............................................................. 27 Figure 3.12 Ratio of determinants with increasing numbers of sensors (M ) evenly positioned between the center and the edge on the rear surface for the extended flash method. The measurements start at to =10 s. The heating time (tp = 30 s) and heat area (rp = 2 mm) are fixed. ..................................................................................................... 28 Figure 3.13 Optimization of heating time (t p) and final measurement time (t f) for the extended flash method, based on a priori information about unknown parameters. The heat area (rp = 2 mm) is given. ....................................................................................... 30 Figure 3.14 Optimization of heating area (rp) and second sensor position (rm, 2) for the extended flash method, based on a priori information about unknown parameters, with one sensor at the center on the rear surface. The ATZ of each point is obtained with optimized heating time (t p) and measurement interval (to , t f ). ................................... 31 Figure 3.15 Schematic representations of the thermal wave method (a), with temperature measurements on the front surface, and of the flash-field method (b), with temperature measurements on the rear surface. Heating occurs within the radius rp on the front face. ........................................................................................................................................... 33 Figure 3.16 Simulation of temperature rise for the thermal wave method (a) and the flash- field method (b) ................................................................................................................. 36 Figure 3.17 Normalized sensitivity coefficients for the thermal wave method (a) and the flash-field method (b). ...................................................................................................... 37 Figure 3.18 Ratio of determinants with two measurements for the thermal wave method (a) and the flash-field method (b). The heating time (t p =30s) and heating area (rp =2mm)are fixed. ..................................................................................................... 38 vi Figure 3.19 Ratio of determinants with a third measurement at various times for the thermal wave method (a) and the flash-field method (b). The heating time (t p = 30 s) and heating area (rp = 2 mm) are fixed. .......................................................................... 39 Figure 3.20 Ratio of determinants with a fourth measurement at various times for the thermal wave method (a) and the flash-field method (b). The heating time (t p = 30 s) and heating area ( rp = 2 mm) are fixed. .......................................................................... 40 Figure 3.21 Ratio of determinants with a fifth measurrnent at various times for the termal wave method (a) and the flash-field method (b). The heating time (II) = 30 s) and heating area (rp = 2 mm) are fixed. ............................................................................................. 41 Figure 3.22 Optimization of heating time (t p) and heating area (rp) for the thermal wave method (a) and the flash-field method (b), based on a priori information about unknown parameters, with four optimized measurement times. ...................................................... 43 vii LIST OF TABLES Table 3.1 Optimal position of the second sensor, rm,2/rs , for changing thermal diffusivity, with rm] /r, = 0. (a0 =1.ox10‘7 mzs“) ................................................. 29 Table 3.2 Maximum ratio of determinants ATZ , from samples of different sizes with the flash method, for materials with (12 =1.5x10—7 mzs’1 and a, = 1.0x10—7 mzs-l.... 32 Table 3.3 Maximum ratio of determinants Aiz , from samples of different sizes with the thermal wave method based on four measurements, for materials with a2 =1.5x10—7 mzs‘l and a, =1.Ox10—7 mzs’l. ....................................................... 44 Table 3.4 Maximum ratio of determinants ATZ , from samples of different sizes with the flash-field method based on four measurements, for materials with a, =1.5><10”7 mstl and a, =l.0x10T7 mzs’l. ....................................................... 44 Table 4.1 Estimation results with measurement errors of standard deviation 0‘ = 0001me. ................................................................................................................. 47 Table 4.2 Estimation results with measurement errors of standard deviation 0 = 0.01Tmax. ................................................................................................................... 47 Table 4.3 Estimation results with measurement errors of standard deviation (7:0.027’max .................................................................................................................... 48 viii CHAPTER 1 INTRODUCTION The standard flash method, proposed by Parker et a1. [1], is a widely used approach to measure thermal diffusivities of isotropic materials. The top surface of a cylindrical sample is subjected to a short heat pulse from a laser or a flash lamp and the temperature rise at the center of the rear surface is measured. As originally proposed, the time at which the temperature rise reaches one-half of its maximum is inversely proportional to the thermal diffusivity. An ASTM standard now exists for the implementation of the flash method [2]. Maillet et a1. [3] extended the standard flash method to measure simultaneously the axial and radial thermal diffusivities of anisotropic materials. Only the central area of the upper surface of a disk—shaped specimen was exposed to a heat pulse. The temperature histories at two locations on the opposite face were measured with thermocouples. One thermocouple was placed at the center and the other was placed at an optimal position, as determined by calculation, outside of the projected illumination. The geometric parameters of heated area and specimen size were also adjusted to improve the quality of measurements. The high temperature rise at the heated face of the sample after the very short flash limits the utility of these techniques in the measurements of materials with low thermal diffusivities or in large samples. Vozar et al. [4] replaced the heat flash with an extended heating to reduce heating intensity and thus the maximum temperature rise at the heated area. Instead of using two thermocouples, they demonstrated that one temperature sensor at the center of rear surface was enough to identify both axial and radial thermal diffusivities, heat flux, and heat transfer coefficients at the boundaries. To improve the estimation quality, they applied a sensitivity analysis, the D-optimization method, to optimize heating duration and measurement time. Their analysis revealed several important design considerations, but the number and positions of thermocouples used to measure the temperature rise of the specimen were fixed, leaving unconsidered adjustment of temperature sensors. Applying D-optimality to set the positions of thermocouples requires assuming values for thermal diffusivities. The quality of optimal design then depends on the values initially guessed for thermal diffusivities. Materials with unknown or changing thermal diffusivities challenge the design of experiments intended for optimal measurements of the components of thermal diffusivity tensors. Thermal diffusivities of some isotropic materials, such as polymers, have been shown to become anisotropic under deformation [5]. Wright et a1. [6] proposed to expand the method of Maillet et a1. [3] to measure the three principal components of thermal diffusivity of elastomer subject to biaxial finite stretching. Doss and Wright [7] used the expanded flash method to measure the thermal diffusivity of polyvinylchloride. LeGall [8] then substituted an extended laser pulse of about four seconds for the flash and measured the thermal diffusivities of several elastomers subject to biaxial stretching. LeGall demonstrated that the thermal diffusivities of elastomers change under biaxial deformation. Highly accurate estimation of thermal diffusivities is especially important for this kind of materials because the differences in the components of thermal diffusivity tensor caused by deformation may be small, especially for small deformation, but could yield insight into thermomechanical behavior. To improve the estimation accuracy, either additional experiments with improved design of sensor positions, based on the estimated thermal diffusivity from the first experiment, may be needed or the number and positions of temperature sensors must be adjustable a postori in order to enhance the quality of the measurements that may result from material property change. Such movable sensor positions are easily implemented if the temperature field history is measured, as with an infrared camera. An advantage of substituting an infrared camera for the thermocouples used, for example, by Doss and Wright [7], is that the entire temperature at one surface can be recorded and the choice of pixels, or sets of pixels, used to determine the thermal diffusivity may be adjusted optimally. Applying infrared cameras to measure temperature is also a non-contact method, which is preferred for easily deformed materials, such as rubber and biological soft tissue. The analysis presented in this thesis seeks to optimize the number and positions of temperature sensors in the extended flash method of LeGall [8] for given parameters of heating duration and geometry, which are fixed prior to the experiment. This is a step to improve the quality in measuring anisotropic thermal diffusivity. Two other methods of thermal diffusivity measurement will be examined in addition to the extended flash method examined above. With the use of infrared cameras becoming common, thermal imaging method is an emerging nondestructive technology for thermal property characterization. Philippi et al. [9] and Kulkarni and Brady [10] applied a heat pulse on one surface of the sample and recorded the entire transient temperature images on the opposite surface. This method is here called as the flash-field method. Telenkov et al. [11], for example, applied the thermal wave method to measure the thermal diffusivity of tissue; thermal wave method records the temperature field on the surface subjected to heat at two times after heating. Thus, the goal here is to compare the flash-field and thermal wave methods with the extended flash method using D- optimality. Results that are shown are representatives of elastomers with radially symmetric thermal diffusivity under deformation. CHAPTER 2 OPTIMIZATION METHOD 2.1 Mathematical Model Similar to the work of Maillet et a1. [3], the physical model considered here consists of a cylindrical specimen of radius rs and thickness e , with uniform and constant mass density p , heat capacity c, and axial and radial components of thermal diffusivity az , a,. The sample is initially at uniform temperature T; , equal to the ambient temperature. The central part of the upper face (2 = O , r S rp) is exposed to a constant heat flux q" for time t S 1,, (Figure 2.1). By defining the temperature excess T(z,r,t)=r*(z,r,r)—Tg, (1) the diffusion equation may be written as «2 ~2 “flan—0 Tug—0 H191), (2a) 3 " arz rar 0t 522 with the initial condition T = O at t = O , (2b) where k, and k, are the axial and radial components of thermal conductivity, respectively. The sample has convective heat loss through its upper, lower and lateral surfaces. Assuming that the upper ho , lower he and lateral h, heat transfer coefficients are constant and uniform on each surface, then the boundary conditions may be written _%Z:_(HO/e)T+g/kz at 2:0, (7—0) 2 6T ——a—Z—=(He/e)T at 226, (2d) -Z—:=(Hr/rs)T at r=rS. (26) The surface heat flux may be treated as a source term " OSrSr,OStSt ,z=0 g = q p p , (2f) 0 others where H 0 , H e and H r are the upper, lower and side Biot numbers, respectively h i, h H0: 06, He: "6, H,= ”S. (3a-c) k2 Figure 2.1 Schematic representation of the mathematical model. The temperature excess may be expressed in the form of a Fourier series [4] 2 2 u a- w a 1_ex _ n z. + m rt T(z,r,t)=— Z ZA)1(HO’Hea-)Bm(Hra—a_) 2 2 pcen=lm=l e rs rs u" a, Wm (1r ‘ + e2 rs2 OStStp, (4a) or m (X) z r r T(z,r,t) =—‘-’— z 2AnB,,,(H..—p.—) pcen=1m=l e rs rs 2 2 u" a: Wm al’ uza, w 2a CXp[( e2 + r2 )t] exp[( I1 .. + m I‘)t ]_1 S 2 2 p 2 e rs u” a- wm a, e2 rs2 t>tp, (4b) Here 2. k- a2 :L a}: :4“, (53,b) PC PC with 2 2 2 Z HO . z 7 21.4,, (un +He )[cos(u,,;)+Z—-sm(u,, ;)] An(H0,He,:)= ” (6a) (14,,2 + H02)(u,,2 + H} ) + (H0 + He)(u,,2 + HOHe) r r r 2Wm iJMWm ’rfl)‘]0(wm 7—) rP r rs s s 3,, (H,,—,—) = 2 2 2 , (6b) rs rs JO (wm)(wm +Hr ) and u" and wm are the positive roots of equations (u2 —- H0H8)tan(u) = (HO + He)u, (7a) mm) = 11,100.», (7b) where J 0 and J1 are Bessel functions of the first kind, of order 0 and 1. If the sample is subjected to an instantaneous heat pulse (i.e., a flash) instead of an extended heating, an expression for the temperature excess can be obtained by differentiating Equation 4a, for the extended heating, with respect to time [12]. The result may be written as 2 2 0° 0° 2 r r u a T(errt): Q 2 ZAn(HO’He’_—)Bm(Hr’ P,_)exp[_( n .. + m r)t], (8) pcen=lm=l e r5 r3 3 ’3 where Q is the energy absorbed per unit area from the flash. 2.2 Estimation Technique The goal here is to estimate the thermal diffusivity components 612 and a,. In this problem, H 0 , H e , H r and q" (or Q) are difficult to be identified a priori, and thus are taken as additional (or nuisance) parameters to be estimated. We will assume that the heat transfer coefficients ho, he and h, are equal, then the parameters to be estimated are thermal diffusivity components a: and a, , Biot number H 2 H0 = He = Hrarre/az /rs and heat flux q" (or energy Q). Following the development in Beck and Arnold [l3], assume that M sensors are used to record the transient temperature rise Y(z,r,t) at I different times, and that the error in temperature measurement is random, additive, uncorrelated and normally distributed with a zero mean and a known constant standard deviation 0'. The four unknown parameters may be obtained by minimizing the ordinary least-squares norm 5m = [Y -T(P)]T[Y -T(P)1, (9) where P is the vector of unknown parameters PT =[P/. P2 ----- P~1=taz. ar. H. q"], (10) and [Y -T(P)IT = [Y1 —T1(P),Y2 —T2(P>....,Yi 4m]. (11) Each element [Yi — Ti (P) ] is a row vector such that [Yi 'Ti (1’)] = [Yil — 731(1’), Yi2 ‘ 712(P),--»Y1M — TIM (P)], (12) where Yim is the temperature rise measured by sensor m at time ti, for m =1,...,M and i = 1,...,1 . The estimated temperature rise Tim(P) is obtained from Equation 4 or 8 by using the current estimate of P. The Levenberg-Marquardt method is applied to calculate the unknown parameter vector P and the iterative procedure is given by [14] Pk” =P" +((J")TJ" +yknk)‘1JT[Y—T(P")], (13) where k is the iteration superscript, Jk is the sensitivity matrix, 52" is a diagonal matrix and ,uk is a positive scalar damping parameter [14]. Matrix ,ukflk is set to damp the oscillations and instabilities caused by the ill-conditioned character of this problem [15]. The sensitivity matrix is defined as - QZL fl .5__T1 1 5P1 6P2 6m .52. 37:2. 9L2 T 6‘31 6’37- 6p!" Jan-simi’: = = = (14) 61) 8T5 5T5 6T5 ’ 51.91 5132 BEN arm arm arm [ 6171 6P2 61w - where s=(i—1)M+m for i=1, 2,...,I and m=1,2,...,M . The elements of the sensitivity matrix may be denoted as sensitivity coefficients 5T, an :52, (15) where n =1, 2, ..., N. 2.3 Optimization Method Recall that the error in temperature measurement has been assumed to be random, additive, uncorrelated and normally distributed with a zero mean and a known constant standard deviation 0'. It is also assumed that there are no errors in the measurement of sensor location r , z and that the parameters to be estimated are constant. Several optimal criteria have been proposed based on the information of matrix J TJ , defined as Fisher Matrix F [13]: (1) maximization of the determinant of JTJ [15] [13]; (2) maximization of the minimum eigenvalue of J TJ [16]; (3) maximization of the trace of J TJ [13]; (4) minimization of the condition number of .1 TJ [16]. The criterion applied here is D-optimality, similar to [15], namely max A = max det(F). (16) 10 Maximizing the determinant of F is equivalent to minimizing the hypervolume of the confidence region. A small confidence region ensures a small variance for the estimation, which means high precision of the measurement [15]. Since more than one parameter are measured, it is desirable to write the D- optimum design of experiment in the dimensionless form as [15] max N =max det(J+TJ+), (17) + . . . . . . . . . . . . where J IS the dmrensronless sensrtrvrty matrix composed of dimensronless sensrtrvrty coefficients, which are defined as P 5T. an+ = n _—S" (18) Tmax apt: where Tmax is the maximum temperature rise within the sample. This allows the different experimental techniques and parameters, with different T max , to be compared. If a large but fixed number of equally spaced measurements are recorded, it is more convenient to design the experiment by maximizing the determinant of G , instead of F [13]. In the extended flash method, the elements in G are given by 1 M’Zf’ 57 [G]x,y= Wmélt 11:0(JraP—T-fl)(ygpy Tmax ) 2(It for x,y=l, 2, ...,n, (19a) where to and t f are the start and end times of measurement, respectively. In the thermal wave and flash-field methods, the elements in G are given by l’zrm (357‘ Zl(P:x—;i-Py-S-)(-)( ”mi: Ir: 0 yap), Tmax [G]x,y= ) 2dr for x, yzl, 2. (19b) where rm is the radius of temperature field measured. 11 For cases where only some of the estimated parameters are of interest, and thus need to be estimated accurately, the estimated parameters can be partitioned into two parts, P] and P2 , as T T T P =[P1 P2 ]- (20) Here, the vector P1 consists of the unknown parameters of primary interest (az , a,) and P2 contains the other unknown parameters (H , q" ). Then, the sensitivity matrix may be partitioned as J“ =1JiJ‘2‘1 (21) Accordingly, the optimal design is obtained by maximizing the ratio of det(J+T J +) to det(JgTig) [13], which is det(J+TJ+) det(JJZ'T .13) max ATZ = max (22) 12 CHAPTER 3 OPTIMIZATION 3.1 Flash Method 3.1.1 Temperature Simulation In the flash method as expanded to 2D, the transient temperature rise at either one position [4] or two [3] on the rear surface is recorded after the front surface has been subjected to heating over part of its area (Figure 3.1). Figure 3.2 presents the simulated temperature rise at different positions, for the flash method with a short heat pulse (Equation 8) and for the flash method with an extended heating (Equation 4). e i r. r Tm2 p q” —>i 2 (t5 tp) _—’ """""" ' -------- ->- Tml —> < 2> no he <—-.---.- Figure 3.1 Schematic representation of the flash method with an extended heating. Heating occurs within the radius rp on the front face. Temperature sensors are positioned at Tm] and Tmz- 13 The results in Figure 3.2 are based on a disk-shaped sample with thickness e = 3 mm and radius r5 =10 mm. The central area (rp = 0.2r3) of the front surface is subjected to heating. The axial and radial thermal diffusivities are 1.5 x 10'7 mzs‘l and 1.0 x 10'7 mzs‘l, respectively; these are known for the forward problem. These diffusivities are representatives of elastomers and biological soft tissue, which may exhibit directional thermal response. The heat transfer coefficients ho, he and h, are assumed to be the same, yielding Biot numbers of H = H0 = He = Hrare/(zz /rs = 0.05 . Figure 3.2a shows the temperature response for an instantaneous heating. The extended heating time in Figure 3.2b is 30 s, which corresponds to a Fourier number F0 = aver/e2 = 0.5. The energy absorbed per unit area Q from the flash and the heat flux absorbed per unit area q" from the extended heating have been adjusted to make the maximum temperature rise Tmax (i.e., the temperature at the center of the front surface) the same in each sample [13]. Random noise following a Gaussian distribution with a zero mean and a standard deviation 0 = 0.0017"max has been added to the calculated value to simulate experimental noise. Although the curves in Panels a and b have similar shapes, the temperature rise recorded on the rear surface is about one order greater in Panel b than in Panel a, corresponding to the difference in the total energy added to the specimen. 3.1.2 Sensitivity Analysis Figures 3.3 through 3.6 show the dimensionless sensitivity coefficients J; , J; , J I, and J (7 (or Jé ), corresponding to the temperature rise simulated in Figure r 14 3.2. It can be observed that the sensitivity curves of J; , J; , J L and J J" (or Jé) at r 2 each point have different shapes and thus are uncorrelated. Therefore, it is possible to estimate all of the unknown parameters using one point measurement [15]. The sensitivity coefficients obtained by applying a short pulse and an extended heating have similar shapes. The sensitivities from extended heating are, however, about one order greater than those from pulse. In both cases, the magnitudes of J; , J H and J (7 (or J 5) decrease as the sensor position is changed from the center to the edge; J g , first decreases and then increases. Furthermore, J; , J; , J}; and J 3"(or J5) each 2 r have their maximum magnitudes with the sensor at the center of the rear surface. The sensitivity coefficients change dramatically at the beginning of the measurements and then reach asyrnptotes as time progresses. Therefore, the temperature recorded at the beginning contains more information than it does during other times. 15 0.03 I TI I I r I I I r 0.025 " 1' ff : ‘ m S 002 r r 1:0.225 (a) ‘ M m S E t—« 0.015- ' .. _ - )2, 1‘ 1:04.50 H "1 0.01 - =11 .. . ._ -- '1 o 1' 06 5 v I" I, . 13.005- “It' . .3 § . . "hf... Tl" 15,1, I1"... "h. LEI: ~ ‘i'_|. . ”1 --_ If“: :- .H‘,l'rfll' i1“. z-h‘jw. $511} L Di; ’:'3- 0005 I I I I l I I I l 0 05115 2 2.523 3.5 4 4.5 5 a We ) Z 03 I I I I r I I T T 0.25 02 >4 E t_—1 0.15 is "'1 0.1 4) V {—1 0.05 0 _005 I I I l I l I I I 0 05 1 1.5 2 2.523 35 4.5 5 0t t/(e ) Figure 3.2 Simulation of temperature rise at various radii for the flash method with a short heat pulse (a) and an extended heating (b). 16 16 I I I I I I I I I .1 . (a) 12 - 5 10 - 4 -— rm/rs=0 :3 8" ........ rm/rs=0.225 * L. 6~" _- r /r=0.450 :'=. m S ‘ _ r /r=0.675 4 : m S .1 ..... r /r=0.900 m S 2 .4 D -2 1 1 1 L 1 1 2 2.5 2 3 3.5 4 45 5 a L’(e ) z . 0.18 I I I ‘T l f 0.16 _ (b) 0.14 5 0.12 5 0.1 4 —— r /r =0 5N008 .mt.s_o 2‘); -1 t5 ........ lmus- . .. = '§ 0.06 _. rm/rs 0.4-0 - _ r /r =0.675 0.04 m s .- :' ..... rm/rs=0.900 0 0.02 I I I I I L J I I 0 0.5 1 15 2 2.5 2 3 . . azt/(e ) Figure 3.3 Normalized sensitivity coefficients of axial thermal diffusivity (az) for the flash method with a short heat pulse (a) and an extended heating (b). 17 t3” __ r /r =0 m S _5 _ ........ r /r =0.225 : m S -....- r it =O.450 m, S -3 _ ..... rm/rs=0.675 _ r /r =0.900 m S 40 1 1 1 1 L 1 1 1 1 [J 0.5 1 1‘5 2 t2:52 3 3.5 4 4.5 5 (122(6 ) 01 I I I I I I I I I (b) 0.05 - ‘ U -------------------------------------------- -D.D5 L6 -U.1 __ r [1' :0 m S ........ rmfrs=0.225 015" ..... r /r=o.450 ‘ m S ..... 1‘ III. =O.675 02 _ m S _ _ r lr=0.900 m 5 _D25 1 J l l l I l l L 0 0.5 1 1.5 2 2.5 2 3 3.5 4 4.5 5 alt/(c ) Figure 3.4 Normalized sensitivity coefficients of radial thermal diffusivity ((1,) for the flash method with a short heat pulse (a) and an extended heating (b). 18 x 1D- 2 I I I I I I I I I — fr =0 m S ........ 1' /1' =0.225 m S ..... r /1' =0.450 U m S _ ..... r fr =0.675 m S 1' fr =0.900 m S LP -2 ~ _4 .. u.o...-......".u.-.:“ -6 l l l l l 1 l l l D 0.5 1 1.5 2 2.5 2‘ 3 3.5 4 4.5 5 0. Me ) z x 10'3 2 I I r I I r I I I __ r fr =0 0‘ m s _ \ “x“ ..... lm/rs=0.225 ‘. ~ — — 1’ ' = .' 5 .. ,2 _ 1 \ 5‘“ rm Is 0 4 0 ~. \ xx ---- rm/i's=0.675 -4 " ' ‘ -1 . \ ‘~\ _ rmlrs=0.900 -8 ¥ 1 \ \“~‘ .1 ti“ ' \ \ ‘\ (b) -8 .- \ 5“ _ x!“ ~~ x x s...” -10 _ ‘1‘ K M “-5 - ‘ ------------------------------------------- :“THE -12 - ': 44 l" T 45 1 1 1 1 1 1 1 1 1 D 0.5 1 1.5 2 3.5 4.5 5 2.5 2 3 aZt/(e ) Figure 3.5 Normalized sensitivity coefficients of Biot number (H ) for the flash method with a short heat pulse (a) and an extended heating (b). 19 0.03 I If fl I I I fir I I __ r if =0 m s _ 00000000 - . = c 25 "' 0.025 im/iS 0 2 ..-o- I III. =0-450 m S 002- ..... r /1'=0.675 - m S __ 1' 1'1' =O.9OO m S 0.015 - LO ' _0005 1 l 1 1 1 l 1 l l 0 0.5 1 15 2 2.52 3 35 4 45 5 0.. (43(6 ) 03 I I I I I I I I I — fr =0 m S . ........ ' ."-= . 2.5 _ 0.25 lmis OZ -.-.- r ,’1'=0.450 m S 0.2— ..... r /1'=0.675 — m S _ r ;‘1'=0.9OO m S 0.15 150* 0.1 0.05 U. -005 1 1 l 1 l 1 l 1 1 0 0.5 1 15 2 2.5 2 3 35 4 45 5 aztx'(e ) Figure 3.6 Normalized sensitivity coefficients of flash (Q) for the flash method with a short heat pulse (a) and of heat flux ( q") for the flash method with an extended heating (b)- 20 3.1.3 Optimization Experiments can be optimally designed by maximizing the ratio of determinants of sensitivity matrices of all unknown parameters and of the nuisance parameters A12 (Equation 22), calculation of which requires assuming values for the unknown parameters being sought. Some of the independent parameters, such as sample size, heating area and heating time are fixed for a given experiment. Other parameters, however, such as measurement time, number of temperature sensors and sensor positions, can be optimized and adjusted after the test by recording the temperature field with the use of an infrared camera. Figure 3.7 shows A12 obtained by measuring the temperature rise at the center of the rear surface during different measurement time intervals for the flash and long duration heating. The curves in each figure represent measurements starting at different times to. Observe that each curve first increases and then decreases with the increasing of final measurement time t f. The optimal measurement time can be obtained at the highest point, which represents the maximum ratio of determinants A12. Although the temperature rise measured during heating contains more information than after heating, it is not necessary to start measuring temperature at the beginning of heating. For the temperature history of the flash method with an instantaneous heat pulse in Figure 3.7a, the optimal time to start measurement is approximately 3 s after the start of heating and the corresponding optimal final time is 300 s. The optimal measurement time for the flash method with an extended heating of 30 s is between 8 and 320 s (Figure 3.7b). The maximum Asz obtained by using the flash method with an extended heating is about five 21 orders greater than that with an instantaneous heat pulse, again with the constraint of the same T max . Therefore, it is better to apply an extended heating to the sample instead of a short pulse. An advantage of measuring temperature with an infrared camera is that the temperature history on the entire surface can be recorded, which means that the transient temperature history at all positions is available. Figure 3.8 presents A12 obtained at different points on the rear surface with measurements starting at to 2105. The maximum A12 clearly decreases as the location of the temperature history is moved from the center to the edge on the rear surface. The best position is then at the center of the surface, if only one temperature sensor is used. 22 l 0 L l 1 1 L l 50 100 150 200 250 300 350 400 450 t. 1.8 1.6 1,4 A12 1.2 [18 . 'u I 0'6 1 l l 1 l 1 200 250 300 350 400 450 500 550 tf (S) Figure 3.7 Optimization of measurement time (to, If) for the flash method with a short heat pulse (a) and an extended heating (b). The heating time ( t p = 30 s) and heating area (rp 2 2mm) are fixed. 23 x10-9 20 r I I f I — r fr: m S __ — r fr =02 15 _ m S A ..... r fr =04 m S __ r /r =06 m S 10 e + fl «<1 5 .. 0L -------------------------------------------- _5 1 1 1 1 L 0 1 00 200 300 400 500 600 t. Figure 3.8 Optimization of sensor position (rm) and final measurement time (if) for the extended flash method, with initial measurement time to =10 s . The heating time (IP = 30 s) and heating area (rp = 2 mm) are fixed. In the work of Maillet et al. [3], two sensors were used to measure temperature, one at the center and the other outside of the heating area. Figure 3.9 shows A12 obtained by placing one sensor at the center and the second sensor at different positions on the rear surface. If the second sensor is also at the center, it is identical to the case with one sensor placed at the center. With the second sensor moved from the center to the edge, the maximum A12 first increases and then decreases. The maximum A12 is obtained with the second sensor at rm, 2 /rS = 0.4 and is about 30 times greater than the maximum A12 with one sensor at the center. 24 1 1 l 1 1 0 1 00 200 300 400 500 500 t. (s) Figure 3.9 Optimization of the second sensor position (rm,2) for the extended flash method, with the first sensor at the center on the rear surface and initial measurement time to = 10 s . The heating time (t p = 30 s) and heating area (rp = 2 mm) are fixed. Figure 3.10 shows the maximum A12 obtained with both sensors movable. If the sensors are placed at the same place, it represents the case in which one sensor is used. The A12 of each point is obtained with optimized measurement time interval. The results demonstrate that it is better to measure the transient temperature at two points than at one. The optimal choice is to place one sensor at the center and the second one outside of the heating area. 25 rm, 2/rS 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 rum/rS Cl 0.00E+00-1.50E—07 l.50E—07-3.00E-07 I 3.00E—07-4.50E—07 I 4.50E—07—6.00E-07 Figure 3.10 Optimization of positions of both sensors (rm,1, rm, 2) for the extended flash method. The A112 of each point is obtained with optimized measurement time interval. The heating time (t p = 30 s) and heating area ( rp = 2 mm) are fixed. Figure 3.11 shows the maximum A12 obtained by measuring the transient temperature at three points during optimized measurement time, with the same heating time and heating radius in Figure 3.9. One sensor is placed at the center of rear surface and the other two sensors are moved from the center to the edge. It can be observed that the A12 reaches a maximum with both sensors placed at r/rs :0.4 and thus the maximum A12 obtained with three sensors (Figure 3.11) is smaller than the maximum A12 with two sensors (Figure 3.9). 26 0.1 0.3 0.5 0.7 0.9 ' rm, z/rs E 0.00E+00—1.70E—07 I 1.7OE-07-3.40E-O7 I 3.40E—O7—5.10E—07 Figure 3.11 Optimization of positions of the second and third sensors (rm, 2 , rm, 3) for the extended flash method, with the first sensor at the center on the rear surface. The A12 of each point is obtained with optimized measurement time interval. The heating time (tp = 30 s) and heat area ( rp = 2 mm) are fixed. Figure 3.12 illustrates the relative utility of using more sensors. The temperature sensors are evenly positioned between the center (r = 0 mm) and the edge (r = 9 mm). For example, if three sensors are used, they are place radially at 0, 4.5 and 9 mm. It can be observed that the maximum ratio of determinants A12 decreases if more sensors are used. 27 0 50 100 150 200 250 300 350 400 450 500 550 500 tf Figure 3.12 Ratio of determinants with increasing numbers of sensors (M ) evenly positioned between the center and the edge on the rear surface for the extended flash method. The measurements start at to = 10 s. The heating time (t p = 30 s) and heat area (rp = 2 mm) are fixed. The analysis above shows that the optimal number of temperature sensors is two for the case of radial symmetry, and the optimized sensor positions are at rm,1 = 0 mm and rm“? =4mm when the heated region is rp =2mm with the sample size of rs =10 mm and e=3 mm. This is based on the material with az = 1.5 x10—7 mzs’l and a, = 1.0x10’7 "123—1. For materials with different values of thermal diffusivities, Table 3.1 lists the optimal position for the second sensor corresponding to the change of thermal diffusivities while the first sensor is placed at the center. It can be observed that 28 the optimal point for the second sensor moves to the edge with the increasing of radial thermal diffusivity and towards the heating radius, here rp /rS = 0.2 , with the increasing of axial thermal diffusivity. Table 3.1 Optimal position of the second sensor, rm,2 /rs , for changing thermal diffusivity, with rm] n», = 0. (a0 =1.0x10‘7 mzs‘l) a2 /a0 0.5 1.0 1.5 2.0 2.5 0.5 0.4 0.3 0.3 0.3 0.3 1.0 0.5 0.4 0.4 0.3 0.3 “r / a0 1.5 0.85 0.5 0.4 0.4 0.4 2.0 0.9 0.7 0.5 0.4 0.4 2.5 0.9 0.8 0.6 0.5 0.4 For materials with a priori information about the unknown parameters, it is also possible to optimize other parameters, such as heating time, heating area and sample size. In Figure 3.13, each curve traces A12 for different heating times while the other parameters are given as the same as above. The temperature is recorded at rm] = 0 mm and rm,2 =4mm , the optimal positions obtained above. The optimal heating time corresponds to the curve with the highest point, which is obtained with a heating time of 200 s and a final measurement time of approximately 300 s. 29 12 _2 J 1 1 1 1 1 1 0 50 100 150 200 250 300 350 400 tf Figure 3.13 Optimization of heating time (t p) and final measurement time (t f) for the extended flash method, based on a priori information about unknown parameters. The heat area (rp = 2 mm) is given. The maximum A12 obtained with optimized heating time and measurement time for different heating radii and sensor positions are compared in Figure 3.14. The optimal heating radius is 7 mm with the first sensor fixed at the center and the second sensor placed at r = 9 mm. The corresponding heating time for this case is 40 s and the final measurement time is 160 s. 30 0.9 0.8 0.7 0.6 0.5 I'm, 2/1'5 0.4 0.3 0.2 0.1 El 0.00E+00-2.50E—06 El 2.50E—06-5.00E—06 I 5.00E—06-7.50E-06 I 7.50E—06-1.00E-05 I 1.00E-05-1.25E—05 Figure 3.14 Optimization of heating area (rp) and second sensor position (rm, 2) for the extended flash method, based on a priori information about unknown parameters, with one sensor at the center on the rear surface. The A12 of each point is obtained with optimized heating time (t p) and measurement interval (to , t f ). Finally, the maximum A12 obtained with samples of different sizes are shown in Table 3.2. For samples with thickness 3 mm, 4 mm and 5 mm, the Optimal specimen radius is 5 mm, 10 mm and 10 mm, respectively. The maximum ratio of determinants 13sz for the extended flash method is about 10'5 if the axial thermal diffusivity is 1.5 x 10'7 mzs'land the radial thermal diffusivity is 1.0 x 10'7 mzs'l. 31 Table 3.2 Maximum ratio of determinants A12 , from samples of different sizes with the flash method, for materials with az ——-1.5x10"7 mzs_l and a, = 1.0x10—7 mzs—l. A12 rS=5mm rS=IOmm rs=ISmm rs=20mm e = 3 mm 2.61110" 1.2x10‘5 7.85110“ 4.551106 e = 4 mm 3.051106 9.75110r 1.15110r 7.6x10'6 e=5mm 1.2x10'6 7.11110" 1.15110" 9.9511045 3.2 Thermal Wave and Flash-field Methods 3.2.1 Temperature Simulation Instead of measuring the transient temperature at two points in the flash method, both the thermal wave and flash-field methods record the temperature of entire surface at several discrete times (Figure 3.15). The temperature of the specimen was calculated using the same equation as for the flash method, namely Equation 4. Again, the heat flux absorbed per unit area q" from the extended heating has been adjusted to make the maximum temperature rise T max the same in each sample. The error in the temperature simulation is assumed to be random, additive, uncorrelated and normally distributed with a zero mean and a known constant standard deviation 0. Figure 3.16 presents the simulated temperature rise on the front surface for the thermal wave method (Panel a) and on the rear surface for the flash-field method (Panel b). Random noise with a standard deviation 0' = 0.001Tmax is added to the equation results. The experimental parameters, such as sample size, heating area and heating time, are the same as those in Panel b of Figure 3.2. 32 fl IR Camera \ (:21 2:) Mirror ho he a U 1.. 1r 8 1 rs ,, (b) q (t5 tp) . r,, ‘1 2 _+1 ............. _ ............ D ..., —> IRCamera (,2: :1) ho he ‘u-m-m-w- |" Figure 3.15 Schematic representations of the thermal wave method (a), with temperature measurements on the front surface, and of the flash-field method (b), with temperature measurements on the rear surface. Heating occurs within the radius rp on the front face. 33 3.2.2 Sensitivity Analysis Figure 3.17 presents the sensitivity coefficients J; , J; , J Z, and J 2;" over the " r L front and rear surfaces at 45 s, which is 15 s after heating has stopped. As may be seen, the sensitivity curves J; , J; , J2, and Jilin have different shapes and are thus Z r uncorrelated, meaning it is possible to estimate the thermal diffusivities with one measurement of the entire surface temperature [15]. 3.2.3 Optimization For the thermal wave and flash-field methods, the parameters that must be set prior to the test are sample size, heating area and heating time. Those that can be adjusted after the experiment are number of measurements and measurement times. Figure 3.18 shows A12 obtained by measuring temperature at two times. The ratio of determinants A12 with two measurements being at the same time, i.e., rm] = tm, 2 , is equal to the A12 obtained with a single measurement. For both the thermal wave method (Panel a) and the flash-field method (Panel b), the A12 based on two measurements are greater than the A12 with one measurement. For the thermal wave method, the region of optimized measurement suggests that one measurement time is between 15 and 25 s with a corresponding second measurement between 30 and 40 s. For the flash-field method, the optimized region suggests that the first measurement time should be between 25 and 35 s with the second between 40 and 65 s for the maximum A12. The maximum A12 for each 34 method is smaller than 108, which is smaller than the maximum A12 for the extended flash method (Figure 3.9). Figure 3.19 shows variation in A12 obtained by adding a third measurement at various times. For the thermal wave method (Panel a), the first two measurements are fixed at 20 and 35 s, which are the optimal measurement times in Panel a of Figure 3.18. If the third measurement is added after 150 s, the ratio of determinants A12 increases to be greater than 107. If the three measurement times are 20, 35 and 270 5, A12 is about 2x10'7. In Panel b, with the first two measurements at 30 and 40 s, the A12 increases from 10‘8 (Panel b of Figure 3.18) to about 1.8x10'7 with the third measurement at 150 s. Figure 3.20 shows the change of A12 after adding a fourth measurement. The first three measurements are fixed at 20, 35 and 270 s in Panel a and at 30, 40 and 150 s in Panel b. The maximum A12 for the thermal wave and flash-field methods are about 5x10'7 and 3x107, respectively. Continuing this analysis, Figure 3.21 then shows the change of A12 by adding a fifth measurement. It can be observed that adding a fifth measurement does not increase A12 as dramatically as does the third measurement in Figure 3.19 or the fourth measurement in Figure 3.20. 35 12 I I j I I I fi I 1 1 =15 \ _ m t =30 s m >< 0.8 - — E [:4 (a) A *1 0.6 — ~ "'1 =45 s 8 m 4 1 =15 .. m 0.2 ~ \\ . ~42 RE;— 0 1 1 1 —— —_ ._. 0 01 02 03 0.4 0.5 0.6 07 08 09 r/r S 0.3 I I r I I j I I 1 =30 \ m 0.25 - _ . t =45 s 02- in 60 4 = s ,4 m (b) E a 0.15 ~ \ tm=>"5 S - 3 0.1 - « 1—1 / / \ 0.06 - t =90 s \- - m \ U 1 1 I L 1 1 -—-—2~ Figure 3.16 Simulation of temperature rise for the thermal wave method (a) and the flash- field method (b). 03 I I I I I If I I \ 0.2 ~ . \ ‘ (a) d \ \ 0.1 — x ‘ q \ § 0" ---/f~:‘—Ha_thrz;——z=_ "-3 1-- ..................... ./ 143‘ / 01 - / J+ d / ...... 0L / Z '02 :_’_ / — _- 1+ ‘ 0L J+r -U.3 ~ 1:! d — - — II .014 l l l 1 1 1 1 1 q 0 0.1 0.2 0.3 0.4 I 0.5 0.5 0.7 0.8 [19 171' S 025 a - 1 I I ' r r r I \ 0.2 - ‘ \ \ ...... I; q \ z 0.15 - ‘ \ _ _ J; g I 0.1” \\ 1+ \ II 005- \, q . £1 """""""""""" \. Lg ............ W'd—*:t:—:h_~ 0_ 1%""----------.2- '*-—5":_;‘: 4" / 0051 - \ E", -0.1 -0.15 - / - U2 /1 1 l L 1 I I i I 01 02 03 04 0.5 05 07 08 09 11/18 Figure 3.17 Normalized sensitivity coefficients for the thermal wave method (a) and the flash-field method (b). 37 tm. 2 (S) E] 0.00E+OO—2.50E-09 El 2.50E—09-5.00E—O9 I 5.00E-09-7.50E-09 I 7.50E—09-1.00E-08 ‘ .1112; £13“: t 1&1 Lei ..fi 1 :. 35 40 45 50 55 60 65 tm, 2 (5) D 0.00E+00-2.00E—09 2.00E—09-4.00E—09 I 4.00E—09-6.00E—09 I 6.00E—09-8.00E-09 Figure 3.18 Ratio of determinants with two measurements for the thermal wave method (a) and the flash-field method (b). The heating time (t p =30s) and heating area (rp 2 2mm) are fixed. 38 2.5- m1 ‘ m2 ' (a) 0.5 - .. 41_ 0 50 100 150 200 250 300 350 400 450 500 t (S) m, 3 A‘AA“A‘A‘A“ V'vvv7"""' 1.6- 1.4- 0.8 ~ 0.6 ~ 0.4 - 0.2b ‘ 0 ‘ 1 1 0 20 40 60 80 100 tm. 3 (s) 120 140 150 180 200 Figure 3.19 Ratio of determinants with a third measurement at various times for the thermal wave method (a) and the flash-field method (b). The heating time (t p = 30 s) and heating area (rp = 2 mm) are fixed. 39 1 1 l l l l 0 2O 40 60 80 100 120 140 150 180 t (s) m 4 35 I I I I I I I I 2.5 *- Figure 3.20 Ratio of determinants with a fourth measurement at various times for the thermal wave method (a) and the flash-field method (b). The heating time (tp = 30 s) and heating area (rp = 2 mm) are fixed. 40 x10- 5.5 ~ _ 3.5 ~ 0 20 40 60 80 100 120 140 ' 38 I I I I I I 3.6 ~ 3.4 ~ 3.2 ~ 2.8 ~ 2.6 I 2.4 ~ 0 2o 40 60 I 80 100 120 140 tm 5 (b) Figure 3.21 Ratio of determinants with a fifth measurment at various times for the termal wave method (a) and the flash-field method (b). The heating time (t p = 30 s) and heating area (rp = 2 mm) are fixed. 41 Figure 3.22 illustrates the maximum ATZ with four measurements for different heating area rp and heating time tp , based on a priori information about unknown parameters. For both the thermal wave method (Panel a) and the flash—field method (Panel b), the optimal heating radius rp / rs is between 0.5 and 0.8. The corresponding heating time for the thermal wave method lies between 60 and 150 s and the maximum AD is of the same order of the maximum Ah with the extended flash method (Figure 3.14). For the flash-field method, the corresponding heating time is between 30 and 60 s and the maximum ratio of determinants ATZ is about half of that of the thermal wave method. Finally, Tables 3.3 and 3.4 list Ab obtained with various sample sizes by measuring the surface temperature field at four times. The maximum AB is obtained by using the thermal wave method (Table 3.3), which is about one and a half times of the maximum ATZ of the extended flash method (Table 3.2) and about twice of the maximum Ah of the flash-field method (Table 3.4). It is still possible, however, to increase the maximum ratio of determinants ATZ of the thermal wave and flash-field methods by adding more measurements. 42 30 60 90 120 150 180' t13(5) El 0.00E+00-5.00E-O6 5.00E-06-l.00E—05 I l.00E—05-1.50E—05 I 1.50E—05-2.00E—05 $3“: ' (”1717); ‘KXA; g-Kffi: 3“" > R“ '1 7' . 1, (s) El 0.00E+00-2.00E—06 2.00E—06-4.00E—06 I 4.00E—06-6.00E—06 I 6.00E-06-8.00E—06 Figure 3.22 Optimization of heating time (tp) and heating area (rp) for the thermal wave method (a) and the flash-field method (b), based on a priori information about unknown parameters, with four optimized measurement times. 43 Table 3.3 Maximum ratio of determinants Ab , from samples of different sizes with the method based on four measurements, for materials with thermal wave a: =l.5x10’7 mzs-l and a, =l.Ox10“7 mzs’]. Ab rs=5mm rS=10mm rs=ISmm e=3nm1 lelUS 1.6x10'S 13x105 e=4nmi 8.2x10'6 1.6x10‘5 15x105 e=5nmi 4.3x10'6 1.2x10‘S 12x105 Table 3.4 Maximum ratio of determinants A72 , from samples of different sizes with the flash—field method based on four measurements, for materials with a: =l.5x10’7 mzs—l and a, ---1.Ox10’7 mzs’l. A113 rs=5mm rs=10mm rs=15mm e=3nmi 6Jx106 7.3x10'6 50x106 e=4nmi 2.6x10'6 74x106 7.1x10'6 e=5nm1 86x107 5.811106 72xlo° 44 CHAPTER 4 COMPARISON OF METHODS Consider a sample with dimensions e=3mm and rs = 10 mm and axial and radial thermal diffusivities of 1.5 x 10'7 mzs'l and 1.0 x 10‘7 mzs'l. The heat transfer coefficients on the front (ho ), rear (he) and side (hr) surfaces are assumed to be the same (H = H0 = He = Hrare/az /r5 = 0.05 ). The heat flux (1,,“ is set to produce the same maximum temperature rise, for each measurement method. Case 1 includes the optimal parameters for the extended flash method from Figure 3.14. The heating radius is 7 mm with the heating time of 60 5; one temperature sensor is at the center and the other is at r = 9 mm on the rear surface. Each sensor is sampled for 80 measurements that are evenly spaced from 10 s to 168 s. In Case 2, only the temperature at the center on the rear surface is recorded, but for 160 measurements, and other parameters are the same as those in Case 1. Case 3 represents the flash method with non-optimized parameters. The heating radius is 2 mm and the heating time is 20 3. One sensor is positioned at the center and the second sensor is at r = 4 mm. Temperature is recorded 80 times with each sensor for 5 s St S 84 5. Case 4 simulates the thermal wave method with optimized parameters from Panel a of Figure 3.22. The heating time is 60 s and the heating radius is 7 mm. The four measurements are at 30, 90, 120 and 270 s. In Case 5, only the temperatures at 30 and 905 are measured, instead of the four measurements in Case 4. Case 6 models the flash-field method with optimized parameters from Panel b of Figure 3.22, with heating time t = 30 s and heating area p rp = 7 mm. The four measurement times are 25, 30, 60 and 180 s. 45 As before, the error in temperature simulation is assumed to be random, additive, uncorrelated and normally distributed with a zero mean and a known constant standard deviation 0. Tables 4.2 and 4.3 summarize the estimated parameters for three different levels of measurement errors: a = 0.001Tmax , a = 0.01Tmflx and 0' = 002me , where Tmx is the maximum temperature rise in the sample. In each case, a total of 160 measurements were considered. The parameters were accurately estimated if no errors were considered and when the standard deviation of errors is as small as 0.001Tmax. For Cases 1 and 4, with the maximum ATZ , all of the parameters were identified with high accuracy even with measurement error as large as 0' = 0.02Tmax. In Cases 2, 3 and 6, the identification errors for thermal diffusivities were greater than those in Cases 1 and 4, but were still smaller than 1%. In Case 5, the radial thermal diffusivity could be estimated with an error less than 2% when the standard deviation of error is 0.02Tmax. The identification error of the axial thermal diffusivity, however, was as great as 20%. Obviously, the thermal wave method by using two measurements, with AIZ two orders smaller than when four measurements are used, is sensitive to measurement errors. For the thermal wave and flash-field methods, it is necessary to measure the temperature of entire surface more than twice for good accuracy. For the flash method, it is better to have two temperature sensors than one, if other parameters are the same. Cases with greater AI), , especially those that are two orders greater, have better accuracy in the estimation. In general, the optimized thermal wave and flash-field methods have the same accuracy as the flash method with optimized parameters. 46 Table 4.1 Estimation results with measurement errors of standard deviation 0' = 0001me . az(mzs") a,(mzs") H (I'anmax Case Aiz 1.500 x 10'7 1.000 x 10'7 5.000 x 10'2 1.000 1 1.2 x10'5 1.500 x 10'7 1.000 x 10‘7 5.008 x 10'2 1.000 2 1.0 x1045 1.499 x 10'7 1.001 x 10'7 4.991 x 10'2 1.000 3 3.2 x10'7 1.501 x 10'7 0.999 x 10'7 4.987 x 10'2 0.999 4 1.6 x10'5 1.500 x 10'7 1.000 x 10'7 4.999 x 10'2 1.000 5 7.8 1110'8 1.507 x 10'7 1.001 x 10'7 5.048 x 10'2 0.991 6 7.3 x10‘6 1.500 x 10'7 1.000 x 10'7 4.998 x 10‘2 1.000 Table 4.2 Estimation results with measurement errors of standard deviation a = 0.01Tmax. a: (mzs'l) a, (mzs'l) H (In/(Inmax Case Ah 7 1.500 x 10‘7 1.000 x 10'7 5.000 x 10'“ 1.000 1 1.2 x10'5 1.501 x 10'7 1.000 x 10'7 5.028 x 10‘2 1.000 2 1.0 x106 1.494 x 10'7 1.003 x 10'7 4.987 x 10‘2 1.001 3 3.2 x107 1.510 x 10'7 1.003 x 10‘7 5.166x10'2 1.002 4 1.6 x105 1.501 x 10'7 1.000 x 10'7 5.001 x 10'2 1.000 5 7.8 x10'8 1.590 x 10'7 1.006 x 10'7 5.551 x 10'2 1.029 6 7.3 x10'6 1.503 x 10‘7 0.999 x 10'7 4.985 x 10'2 1.000 47 Table 4.3 Estimation results with measurement errors of standard deviation o- = 0.027max. a2 (mZS-l) (1,. (“1254) H qH/qnmax Case Ab 1.500 x 10'7 1.000 x 10‘7 5.000 x 10'2 1.000 1 1.2 x10'5 1.504 x 10'7 1.002 x 10'7 5.057 x 10'2 1.003 2 1.0 x10'6 1.512 x 10'7 0.996 x 10'7 5.055 x 10'2 1.001 3 3.2 x107 1.513 x 10'7 0.993 x 10'7 4.986x 10'2 0.991 4 1.6 x105 1.502 x 10'7 1.002 x 10‘7 5.004 x 10‘2 1.002 5 7.8 x108 1.803 x 10'7 1.012 x 10'7 6.438 x 10'2 1.083 6 7.3 x106 1.498 x 10’7 1.005 x 10'7 4.996 x 10'2 1.003 48 CHAPTER 5 CONCLUSION Three methods to measure simultaneously the axial and radial thermal diffusivities of anisotropic materials have been optimized and compared based on the D- optimal criteria: the extended flash method, the thermal wave method and the flash-field method. For the extended flash method, the number of sensors and sensor positions were optimized using the D-optimization method. The parameters that must be fixed in experiments, such as heating time, heating area and sample size, were then adjusted using the information obtained about the unknown parameters. Although one temperature sensor contains enough information to determine simultaneously the axial and radial thermal diffusivities, a second temperature sensor improves the measurement accuracy. For the thermal wave and flash-field methods, the adjustable parameters are number of measurements, measurement times, heating time, heating area and sample size. It has been demonstrated that using more than two measurements improves the accuracy of estimation. Based on the D-optimal criteria, the thermal wave and flash-field methods with optimal parameters are as accurate as the flash method for materials with 0:2 =1.5x10—7 mzs‘1 and ar =1.Ox10'7 mzs—l. This work has addressed estimating the axial and radial thermal diffusivities, heat transfer coefficients and heat flux. The thermal diffusivities are the parameters of primary interest. The heating transfer coefficients and heat flux are taken as additional unknown, or nuisance, parameters. 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