CN102507040B - Thin film temperature measurement method based on ellipsometer - Google Patents
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Abstract
The invention belongs to the technical field of temperature measurement, and in particular relates to a thin film temperature measurement method based on an ellipsometer. The thin film temperature measurement method comprises the following steps of: measuring a refractive index spectrum line and a standard refractive index spectrum line of a measured thin film by using the ellipsometer, comparing the refractive index spectrum line with the standard refractive index spectrum line, obtaining an optimal match curve by using a least square method, and consequentially obtaining the temperature value of the measured thin film according to the temperature value corresponding to the standard spectrum line. According to the thin film temperature measurement method provided by the invention, real-time or non-real-time temperature of a solid thin film can be measured indirectly and losslessly. The thin film material is not damaged in the measurement process; and when the experimental condition is not changed obviously, the thin film temperature measurement method has a higher confidence coefficient. When the temperature interval of the standard refractive index spectrum line is set to be smaller, the thin film temperature measurement method has a higher precision.
Description
Technical field
The invention belongs to the temperature measurement technology field, be specifically related to a kind of method of utilizing the ellipsometer measurement film temperature.
Background technology
Accurately the temperature of MEASUREMENTS OF THIN is the important technology of research membraneous material.For example: in thin-film process such as molecular beam epitaxy, chemical vapor deposition, ion etching, rapid thermal treatment and sputter, the measurement of underlayer temperature is particularly important to the control of membrane quality.Traditional thermometric mode mainly contains: thermocouple sensor is measured, thermal resistance sensor measurement etc.But the two maximum shortcoming is contact and destruction to film, and is unfavorable for the local temperature control in quick, the steady growth of film.
[[i]]At present, photothermal technique, interfere temperature measurement technology and heat reflectivity technology MEASUREMENTS OF THIN underlayer temperature and characterize optics and the thermophysical property of film non-contactly.These optical technologies have the advantage of noncontact and remote recording, and have higher room and time resolution.
[[ii]]Typical high temperature thermo detector and infrared thermometer are widely used in the productive life.These two kinds of thermo detectors are to utilize energy that testee gives off under different temperatures different and obtain the intrinsic temperature of object.But what their were measured is the real time temperature of object, then seems helpless for the non real-time temperature of object.
Summary of the invention
The object of the present invention is to provide and a kind ofly can measure real time temperature, can measure the film temperature measuring method of non real-time temperature again.
The present invention utilize optical technology fast, noncontact and nondestructive characteristics, the spectrum of refractive index of considering film has inseparable relation (temperature can influence the compactness extent of film etc.) with its temperature, proposes a kind of indirectly measurement method of the film temperature based on ellipsometer.This method is mainly utilized refractive index spectral line and the standard refraction rate spectral line of the tested film of ellipsometer measurement, with both relatively, adopt least square method to obtain the optimum matching curve, thereby obtain the temperature value of tested film according to the corresponding temperature value of standard spectral line, concrete measuring process is as follows:
(1) at first, utilize the refractive index spectral line of film under several groups of different temperatures of reflective ellipsometer measurement, as the standard refraction rate spectrum N of this film
T(λ);
(2) then, utilize the refractive index spectral line N of a certain tested film of reflective ellipsometer measurement temperature the unknown under same experimental conditions
x(λ);
(3) adopt least square method, calculate the refractive index spectral line N of tested film
x(λ) with every group of standard refraction rate spectral line N
TThe refractive index difference of each wavelength points of correspondence (λ) square, and summation respectively, it is poor to obtain a prescription
:
（1）
(4) compare this prescription extent, the corresponding standard refraction rate of the variance of numerical value minimum spectral line is exactly the optimum matching spectral line of tested film, thereby the corresponding temperature of this standard spectral line is exactly the temperature of tested film.
The ultimate principle of the inventive method is as follows: Fig. 1 is typical reflective ellipsometer principle of work synoptic diagram:
[[iii], [iv]]The flashlight of a branch of known polarization attitude incides the film sample surface, and light beam and sample are had an effect, and makes outgoing polarization state of light change (generally becoming elliptical polarization by linear polarization).Relevant with parameters such as sample thickness, refractive indexes because of the polarization state of light variation, by measuring the variation of polarization state, can inverting obtain sample optical property parameter.The reflecting light of ellipsometer is very responsive to the physical characteristics and the physical process that influence the Film Optics constant.Utilize ellipsometer, we just can measure the spectrum of refractive index of film under the different experimental conditions.
[[v]]Because temperature can influence the energy of electronics and phonon in the film, thereby influence the interaction of photon and electronics or phonon, show as change of refractive on the macroscopic view.Be film under condition of different temperatures, its spectrum of refractive index can be had any different.
[[vi]]Therefore, we just obtain a kind of indirectly measurement method of film temperature, namely by the spectrum of refractive index of ellipsometer measurement film, then itself and standard temperature-spectrum of refractive index are compared, adopt least square fitting experiment refractive index n curve, thereby be finally inversed by the temperature of tested film.
The inventive method has fast, noncontact and nondestructive characteristics, real time temperature that not only can MEASUREMENTS OF THIN, and growth temperature (and non real-time temperature) that can MEASUREMENTS OF THIN.Compose when more accurate when the standard refraction rate, this method has higher degree of confidence; The temperature difference of the different temperatures of getting when the measurement standard spectrum of refractive index hour (for example is 20
oC-50
OC), this method has higher measuring accuracy.Growth same material film under identical experiment condition particularly, this method has embodied bigger advantage.
Description of drawings
Fig. 1 is typical reflective ellipsometer principle of work synoptic diagram.
Fig. 2 is that the refractive index of growing ZnO thin-film under the different temperatures is with the wavelength change curve.
Fig. 3 is that the refractive index n of ZnO film under the condition of different temperatures is with the change curve of wavelength X.
Fig. 4 is the refractive index n value of sample under the different temperatures.
Number in the figure: 1 is light source, and 2 is the polarizer, and 3 is sample, and 4 is analyzer, and 5 is detector.θ is the flashlight incident angle.
Embodiment
At first, measure the standard refraction rate spectrum of film under the different temperatures, and the temperature interval has determined the measuring accuracy of this method.But too little temperature interval, spectrum of refractive index can't be distinguished, and can increase the complexity of calculating.The present invention adopts the ellipsometer of wide spectrum, can guarantee the match degree of confidence of curve like this.The measurement of temperature fully can be under the condition of single wavelength in fact, and general spectral line locates to have the higher discrimination of temperature in critical point (being extreme point),
[[vii]]Pertinent literature is arranged
[[viii]]Reported that the mean square deviation of temperature can descend 30% when wavelength is changed into 4428 by 6328.But adopt wide spectrum can avoid temperature only the refractive index of specific wavelength to be worked, be the spectral line that has only under the part wavelength from spectrum and can obviously distinguish the effect of temperature, thereby increase substantially the match degree of confidence.Spectral range is more wide, the match degree of confidence is more high, but thing followed calculated amount also significantly improves, therefore spectral range must obtain suitably, generally get each 5 wavelength points suitable (if employing 10 nm are two intervals between the wavelength sampled point, then getting the spectral range of each 50 nm about extreme point) about extreme point.
After obtaining standard refraction rate spectrum, measure the spectrum of refractive index of tested film, tested film and standard film are to obtain under the experiment condition of the same race, are temperature the unknown of tested film.
Subsequently, adopt the refractive index curve of the tested film of least square fitting, get a certain initial wavelength, calculate tested film refractive index difference under this wavelength in the refractive index under this wavelength and standard spectral line square, then get next wavelength, obtain equally difference square, got the wavelength of whole spectrum, to the summation of the squared difference under the same typical curve and relatively big or small, wherein the corresponding curve of minimum value is the optimum fit curve of tested film refractive index spectrum, the corresponding temperature of this curve is the temperature of tested film, and its measuring error is the temperature interval of standard refraction rate spectrum.
Be two application examples of the present invention below:
Example 1:The growth for Thin Film temperature survey, i.e. non real-time temperature survey
[[ix]]
Be equipped with ZnO film with ALD (Atomic Layer Deposition, i.e. ald) legal system, adopt diethyl zinc (DEZn) as source metal, water is as oxygen source.Two provenances alternately feed reaction chamber, and its reaction equation is:
ZnOH*+Zn(CH
2CH
3)
2 → ZnOZn(CH
2CH
3)*+C
2H
6 （2）
Zn(CH
2CH
3)*+H
2O → ZnOH*+C
2H
6 （3）
Per step reaction all is saturated surface reaction, and two steps were a circulation.In the present invention, the feeding time of each provenance is respectively DEZn:N
2: H
2O:N
2=0.5s:2s:0.5s:2s.
Adopt the ZnO film standard temperature-spectrum of refractive index of Sopra GES-5E type ellipsometer measurement as shown in Figure 2.
As can be seen from Figure 2, different temperature refractive index is influential really, totally presents with temperature of reaction to raise, and reaches downward trend after the maximal value.And each curve has discrimination preferably near peak value.
Can draw with temperature and wavelength is X, Y coordinate for this reason, and refractive index n is the 3-D view of Z coordinate, as shown in Figure 3.As can be seen from Figure 3, as long as determined temperature T and wavelength X, then refractive index n has just been determined.Otherwise, determined refractive index n and wavelength X, temperature T is not unique.Therefore, the foregoing single wavelength of getting is not generally used by the method that refractive index n obtains temperature T.Can obviously distinguish temperature province (about 0.2 μ m among Fig. 2,0.8 μ m and 3.8 μ m) and could be suitable for said method when spectral line only.The spectrum simulation method that the present invention adopts has been avoided this defective, because the spectrum of refractive index under the different temperatures often differs greatly, even the corresponding refractive index of the single wavelength of different temperatures may be identical in other words, but can not (test and use 62 wavelength points by full spectrum, from 0.19 μ m-0.8 μ m) all consistent, this has just improved the spectrum simulation degree of confidence exponentially.
In order to mate the spectrum of refractive index of unknown temperatures, the present invention adopts least square fitting.If under the identical wavelength sampled point, the spectrum of refractive index of tested ZnO film is N
x(λ), the spectrum of refractive index of standard ZnO film is N
1(λ), N
2(λ), N
3(λ), N
4(λ), N
5(λ), N
6(λ), N
7(λ).Calculate: (the wavelength sampling number is 62)
N
x1=[N
x（λ
1）-N
1（λ
1）]
2+[N
x（λ
2）-N
1（λ
2）]
2+…+[N
x（λ
62）-N
1（λ
62）]
2
……
N
x7=[N
x（λ
1）-N
7（λ
1）]
2+[N
x（λ
2）-N
7（λ
2）]
2+…+[N
x（λ
62）-N
7（λ
62）]
2
N then
x1, N
x2, N
x3, N
x4, N
x5, N
x6, N
xThe corresponding temperature of minimum value in 7 is the temperature of the tested film of optimum matching.Because the temperature difference of this standard refraction rate spectrum is 30 ℃ to the maximum, so measuring error is about 30 ℃ in this example.(detailed matlab algorithm is seen appendix)
Example 2:The real time temperature of film is measured
[[x]]
The SiO that adopts thermal evaporation to grow
x/ SiO
2(1＜x＜2) multilayer film superlattice structure, and use The high temperature anneal, be prepared into nano-silicon crystal grain film, adopt reflective RAP type ellipsometer
[5]The spectrum of refractive index of MEASUREMENTS OF THIN.With example 1 difference be, example 2 is not the growth temperature that changes sample thin film, but changes the temperature of film in the measuring process, and this temperature can exert an influence to the physical characteristics of film equally, directly cause the spectrum of refractive index of ellipsometer measurement to change, thereby can use the inventive method.Its spectrum of refractive index with computer fitting is illustrated in fig. 4 shown below.
The temperature sample interval of this standard refraction rate spectrum is about 50
oC, as can be seen from Figure, each curve has been distinguished clearly behind wavelength 290 nm, has higher degree of confidence when therefore mating with least square method, yet, because the temperature sample interval in this illustration is about 50
oC, so measuring error is about 50 in this example
oC.
In sum, the present invention proposes a kind of film temperature measuring method based on ellipsometer, and with the ZnO film of ALD method growth and nanocrystalline with the Si of thermal evaporation growth be example, the feasibility of this method has been described.This method has fast, noncontact and nondestructive characteristics, real time temperature that not only can MEASUREMENTS OF THIN, and growth temperature (and non real-time temperature) that can MEASUREMENTS OF THIN.Compose when more accurate when the standard refraction rate, this method has higher degree of confidence; The temperature difference of getting when standard refraction rate spectrum hour, this method has higher measuring accuracy.Growth same material film under identical experiment condition particularly, this method has embodied bigger advantage.
With reference to selected works
[[1]] K. Postava, M. Aoyama, J. Mistrik, et al. Optical measurement of silicon wafer temperature. Appl. Surf. Sci., 254 : 416-419 (2007)
[2] A. S. Lee, P. M. Norris. A new optical method for measuring surface temperature at large incident probe angles. Rev. Sci. Instrum. 68(2): 1307-1311(1997)
[3] H. Fujiwara, Spectroscopic ellipsometry - principles and application, John Wiley & Sons Ltd, The Atrium,(2007)
[4] H. G. Tompkins, E. A. Irene. Handbook of spectroscopic ellipsometry. Norwich, New York: William Andrews Publications, (2005)
[5] L. Y. Chen, X. W. Feng, Y. Su, H. Z. Ma and Y. H. Qian, Design of a scanning ellipsometer by synchronous rotation of the polarizer and analyzer, Appl. Opt
., 33: 1299(1994)
[6]The Shen Xue plinth, semiconductor optical character, Beijing: Science Press, (2002)
[7] H. D. Yao, P. G. Snyder, J. A. Woollam, Temperature dependence of optical properties of GaAs. J. Appl. Phys., 70(6) : 3261-3267(1991)
[8] R. K. Sampson, K. A. Conrad, H. Z. Massoud. Wavelength considerations for improved silicon wafer temperature measurement by ellipsometry. J. Electrochem. Soc. 141(2): 539-542 (1994)
[9] Y. C. Liu, S. K. Tung, J. H. Hsieh. Influence of annealing on optical properties and surface structure of ZnO thin films. J. Cryst. Growth, 287:105-111(2006)
[[1]0] R. J. Zhang , Y. M. Chen, et al., Influence of nanocrystal size on dielectric functions of Si nanocrystals embedded in SiO
2 matrix,Appl. Phys. Lett., 95:161109(2009)。
Appendix: the thermometric Matlab algorithm of ZnO film of ALD growth
T=[110 120 150 180 200 220 250];
L=[0.19 0.2 0.21 0.22 0.23 0.24 0.25 0.26 0.27 0.28 0.29 0.3 0.31 0.32 0.33 0.34 0.35 0.36 0.37 0.38 0.39 0.4 0.41 0.42 0.43 0.44 0.45 0.46 0.47 0.48 0.49 0.5 0.51 0.52 0.53 0.54 0.55 0.56 0.57 0.58 0.59 0.6 0.61 0.62 0.63 0.64 0.65 0.66 0.67 0.68 0.69 0.7 0.71 0.72 0.73 0.74 0.75 0.76 0.77 0.78 0.79 0.8];
n1=[1.86245 1.84982 1.84294 1.84097 1.84324 1.84906 1.85777 1.86874 1.88138 1.895 1.90886 1.92195 1.93293 1.94062 1.95081 1.99702 2.01622 2.07034 2.27083 2.22837 2.1483 2.09328 2.05392 2.02536 2.00284 1.98445 1.96903 1.95586 1.94443 1.9344 1.9255 1.91755 1.91038 1.90389 1.89798 1.89258 1.88761 1.88303 1.8788 1.87487 1.87121 1.8678 1.86462 1.86163 1.85883 1.8562 1.85372 1.85138 1.84917 1.84708 1.8451 1.84323 1.84144 1.83975 1.83814 1.8366 1.83514 1.83374 1.83241 1.83113 1.82991 1.82874];
n2=[1.89053 1.87782 1.87002 1.86695 1.86826 1.87341 1.88178 1.89274 1.90564 1.91977 1.93437 1.94848 1.96099 1.9711 1.98257 2.01819 2.06722 2.08649 2.32338 2.30634 2.22125 2.15629 2.11139 2.07725 2.05133 2.03027 2.01268 1.9977 1.98474 1.97338 1.96333 1.95436 1.94629 1.939 1.93236 1.92629 1.92073 1.9156 1.91086 1.90647 1.90239 1.89859 1.89503 1.89171 1.88859 1.88566 1.8829 1.8803 1.87785 1.87553 1.87333 1.87125 1.86927 1.8674 1.86561 1.86391 1.86229 1.86075 1.85927 1.85786 1.85651 1.85522];
n3=[1.9062 1.89598 1.89078 1.89002 1.89322 1.89983 1.9093 1.92105 1.93449 1.94897 1.96378 1.97809 1.99103 2.00247 2.01658 2.05031 2.10255 2.13917 2.37713 2.36236 2.27467 2.20596 2.15792 2.12115 2.09296 2.06992 2.0506 2.03406 2.0197 2.00708 1.99587 1.98583 1.97678 1.96858 1.9611 1.95424 1.94794 1.94212 1.93673 1.93173 1.92707 1.92273 1.91866 1.91485 1.91126 1.90789 1.90472 1.90172 1.89889 1.8962 1.89366 1.89125 1.88896 1.88678 1.8847 1.88272 1.88084 1.87903 1.87731 1.87567 1.87409 1.87258];
n4=[1.92913 1.91228 1.90233 1.8982 1.89905 1.90405 1.91244 1.92347 1.93643 1.95053 1.96492 1.97858 1.99039 1.99994 2.01248 2.05353 2.12125 2.17736 2.39668 2.35892 2.26715 2.20013 2.15184 2.11633 2.08815 2.06501 2.04555 2.02886 2.01434 2.00156 1.99019 1.98001 1.97083 1.96249 1.95489 1.94793 1.94152 1.9356 1.93012 1.92503 1.9203 1.91587 1.91173 1.90785 1.90421 1.90078 1.89755 1.8945 1.89161 1.88888 1.8863 1.88384 1.88151 1.87929 1.87718 1.87517 1.87325 1.87141 1.86966 1.86799 1.86638 1.86485];
n5=[1.92311 1.91658 1.90966 1.90431 1.90202 1.90364 1.90944 1.9193 1.93273 1.94898 1.96709 1.98577 2.00337 2.01794 2.03024 2.06553 2.14533 2.20697 2.41266 2.36513 2.2675 2.19816 2.14862 2.11252 2.08426 2.06142 2.04254 2.02666 2.01311 2.00143 1.99127 1.98237 1.97452 1.96756 1.96135 1.95579 1.9508 1.94629 1.94222 1.93852 1.93515 1.93208 1.92927 1.92669 1.92432 1.92215 1.92014 1.91828 1.91656 1.91497 1.91349 1.91211 1.91083 1.90963 1.90852 1.90747 1.90649 1.90558 1.90472 1.90391 1.90315 1.90243];
n6=[1.92683 1.91873 1.9113 1.90649 1.90553 1.90891 1.91661 1.9282 1.94301 1.96019 1.97869 1.99717 2.01386 2.02659 2.03647 2.07807 2.16772 2.22864 2.42133 2.36985 2.27453 2.20762 2.15957 2.12436 2.09662 2.07404 2.05521 2.03924 2.02549 2.01353 2.00301 1.9937 1.98539 1.97794 1.97122 1.96514 1.9596 1.95455 1.94992 1.94567 1.94175 1.93813 1.93478 1.93166 1.92877 1.92607 1.92355 1.92119 1.91898 1.9169 1.91495 1.91311 1.91138 1.90975 1.9082 1.90674 1.90535 1.90404 1.90279 1.90161 1.90048 1.89941];
n7=[1.90264 1.88635 1.87827 1.87666 1.88026 1.888 1.89899 1.9124 1.92748 1.94342 1.95932 1.974 1.98596 1.99397 2.00383 2.05762 2.12752 2.20376 2.37815 2.32362 2.23637 2.17629 2.13286 2.10089 2.07552 2.0547 2.0372 2.02221 2.00919 1.99774 1.98758 1.97849 1.9703 1.96287 1.95611 1.94992 1.94424 1.93899 1.93414 1.92964 1.92546 1.92155 1.9179 1.91449 1.91128 1.90827 1.90543 1.90275 1.90022 1.89782 1.89556 1.89341 1.89137 1.88943 1.88758 1.88583 1.88415 1.88255 1.88102 1.87956 1.87817 1.87683];
n=[n1 n2 n3 n4 n5 n6 n7];
T1=zeros(1,62);
T2=zeros(1,62);
T3=zeros(1,62);
T4=zeros(1,62);
T5=zeros(1,62);
T6=zeros(1,62);
T7=zeros(1,62);
for i=1:62
T1(i)=T(1);
T2(i)=T(2);
T3(i)=T(3);
T4(i)=T(4);
T5(i)=T(5);
T6(i)=T(6);
T7(i)=T(7);
end
plot3(T1,L,n1,T2,L,n2,T3,L,n3,T4,L,n4,T5,L,n5,T6,L,n6,T7,L,n7,'LineWidth',4);
grid on;
Xlabel (' temperature T '); Ylabel (' wavelength X '); Zlabel (' refractive index n ');
Nx=zeros (1,62); %nx is the spectrum of refractive index of tested film
t1=sum((nx-n1).^2);
t2=sum((nx-n2).^2);
t3=sum((nx-n3).^2);
t4=sum((nx-n4).^2);
t5=sum((nx-n5).^2);
t6=sum((nx-n6).^2);
t7=sum((nx-n7).^2);
[M,I]=min(t1,t2,t3,t4,t5,t6,t7);
Tmatch=T(I)。
Claims (2)
1. film temperature measuring method based on ellipsometer is characterized in that concrete steps are:
(1) at first, utilize the refractive index spectral line of film under several groups of different temperatures of reflective ellipsometer measurement, as the standard refraction rate spectrum N of this film
T(λ);
(2) then, utilize the refractive index spectral line N of a certain tested film of reflective ellipsometer measurement temperature the unknown under same experimental conditions
x(λ);
(3) adopt least square method, calculate the refractive index spectral line N of tested film
x(λ) with every group of standard refraction rate spectral line N
TThe refractive index difference of each wavelength points of correspondence (λ) square, and summation respectively, it is poor to obtain a prescription
(4) compare this prescription extent, the corresponding standard refraction rate of the variance of numerical value minimum spectral line is exactly the optimum matching spectral line of tested film, and the corresponding temperature of this standard refraction rate spectral line is exactly the temperature of tested film.
2. the film temperature measuring method based on ellipsometer according to claim 1 is characterized in that in the step (1), and during the standard refraction rate of MEASUREMENTS OF THIN spectrum, the error of described different temperatures is 20
oC-50
oC.
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