WO2020255447A1 - 熱物性値測定装置及び熱物性値測定方法 - Google Patents
熱物性値測定装置及び熱物性値測定方法 Download PDFInfo
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- WO2020255447A1 WO2020255447A1 PCT/JP2019/047422 JP2019047422W WO2020255447A1 WO 2020255447 A1 WO2020255447 A1 WO 2020255447A1 JP 2019047422 W JP2019047422 W JP 2019047422W WO 2020255447 A1 WO2020255447 A1 WO 2020255447A1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K11/00—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00
- G01K11/12—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00 using changes in colour, translucency or reflectance
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K11/00—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00
- G01K11/12—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00 using changes in colour, translucency or reflectance
- G01K11/125—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00 using changes in colour, translucency or reflectance using changes in reflectance
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/18—Investigating or analyzing materials by the use of thermal means by investigating thermal conductivity
Definitions
- the present invention relates to a thermophysical property value measuring device for measuring a thermophysical property value and a thermophysical property value measuring method.
- thermoreflectance method for example, Patent Document 1
- thermoreflectance method in order to measure the temperature change on the front surface or the back surface of the thin film, the thin film is irradiated with a laser beam for temperature measurement, and the change in reflectance is detected.
- the temperature change of the thin film is as small as several ° C. or less, the amount of temperature increase is considered to be proportional to the amount of change in reflectance, so that the temperature change on the sample surface can be detected based on the change in reflectance.
- thermophysical property values including the thermal diffusivity and the interfacial thermal resistance of the sample (for example, Patent Document 2).
- the drive signals of the heating laser and the temperature measuring laser are electrically controlled by a signal generator to reduce the arrival time of the heating light and the temperature measuring light on the sample. It is explained that it can be controlled, it is possible to measure a wider range of time, and the measurement target range can be expanded.
- Patent Document 1 assumes a heat flow that is one-dimensionally transmitted in a direction perpendicular to the surface of the thin film, constructs an analysis model, and obtains a thermophysical property value. It is explained that this makes it possible to accurately analyze the thermal response of the multilayer thin film and the functionally graded material in the film thickness direction.
- thermoreflectance method for example, Patent Document 3
- the thermophysical property value measuring device described in Patent Document 3 scans the irradiation position of the temperature-measured light with respect to the sample surface by moving the XY stage on which the sample is fixed while fixing the irradiation position of the heating light with respect to the sample surface. ing. It is explained that this makes it possible to obtain the thermal diffusivity in the creeping direction and to obtain an image of heat diffusion centered on the heating position.
- the measurement position When the temperature rise is slight, it is necessary to set the measurement position to irradiate the temperature measurement light to a position slightly displaced from the irradiation area of the heating light.
- the heating light has a spatial intensity distribution. Therefore, it was difficult to strictly distinguish between the irradiated region of the heating light and the non-irradiated region. Further, in order to accurately measure the amount of displacement of the temperature measuring light with respect to the heating light, a complicated mechanism is required and it is difficult to measure easily.
- the present invention has been made in view of the above circumstances, and an object of the present invention is to provide a thermophysical property value measuring device and a thermophysical property value measuring method capable of accurately and easily measuring the thermophysical property value in the creepage direction of a thin film. And.
- thermophysical property value measuring device is A light-shielding body that is provided facing the front or back surface of the sample thin film and shields light except for openings.
- a heating laser that repeatedly irradiates the sample thin film with pulsed heating light through the light-shielding body. Measurement that irradiates temperature measurement light to a measurement position separated by a predetermined distance in the creeping direction along the extending direction of the surface from the heating light irradiation position on the sample thin film that has been irradiated with the heating light through the opening.
- thermophysical property value calculation unit that calculates a thermophysical property value in the creepage direction of the sample thin film based on the reflected light intensity of the reflected light detected by the photodetector. It is characterized by having.
- the diameter of the spot of the heating light irradiating the light-shielding body is larger than the diameter of the spot of the temperature-measured light on the sample thin film.
- the center of the heating light spot and the center of the temperature measuring light spot are at the same position in the creepage direction.
- the light-shielding body is formed by forming a light-shielding thin film having a light-shielding property on a transparent substrate made of a material through which the heating light is transmitted, excluding the opening.
- the light-shielding thin film on the transparent substrate is opposed to the surface of the sample thin film.
- the heating laser may irradiate the heating light from the transparent substrate side.
- the sample thin film is a thin film formed on a sample substrate.
- the light-shielding body is formed by forming a light-shielding thin film having a light-shielding property on a transparent substrate excluding the opening.
- the light-shielding thin film on the transparent substrate is opposed to the surface of the sample substrate opposite to the sample thin film.
- the heating laser may irradiate the heating light from the transparent substrate side.
- the light-shielding body is formed by forming a light-shielding thin film having a light-shielding property on the surface of the sample thin film.
- the heating laser may irradiate the heating light from above the light-shielding body on the surface of the sample thin film.
- the sample thin film is a thin film formed on a sample substrate.
- the light-shielding body is formed by forming a light-shielding thin film having a light-shielding property on the back surface of the sample substrate opposite to the sample thin film.
- the heating laser may irradiate the heating light from above the light-shielding body on the back surface of the sample substrate.
- the thermophysical property value calculation unit calculates the thermal diffusivity of the sample thin film from the heated light irradiation position to the measurement position based on the reflected light intensity, and includes the thermal diffusivity based on the thermal diffusivity.
- the thermophysical property value may be calculated.
- the temperature measurement light may be condensed and irradiated to the measurement position existing on the surface of the sample thin film opposite to the light-shielding body.
- the light shield has two or more openings separated from each other. Both the heating light and the temperature measuring light are applied to the sample thin film through the light-shielding body. The heating light is applied to a region including at least one of the openings. The temperature measurement light may be focused and applied to the measurement position at the same position in the creepage direction as the other 1 opening.
- the stage on which the sample thin film provided with the light-shielding body is fixed is moved in a two-dimensional direction parallel to the creepage direction to change the measurement position.
- the thermophysical property value calculation unit may calculate the thermophysical property value in the creepage direction based on the reflected light intensity reflected at the measurement position.
- the heating light may be pulsed light having a pulse width on the order of nanoseconds, picoseconds or femtoseconds.
- the temperature measurement light may be continuous light.
- the temperature measurement light may be pulsed light having a pulse width on the order of nanoseconds, picoseconds or femtoseconds.
- a signal generator that outputs a drive signal to the heating laser and the temperature measuring laser is further provided.
- the time of irradiating the sample thin film with the heating light and the time of irradiating the sample thin film with the temperature measuring light are controlled by the drive signal of the signal generator.
- the thermophysical property value calculation unit calculates the heat diffusion time based on the time difference between the heating light irradiation time and the temperature measurement light irradiation time, and calculates the thermophysical property value including the thermal diffusivity based on the thermal diffusivity. It may be calculated.
- the light-shielding body may have a light-shielding thin film on which a metal material is formed in addition to the opening.
- thermophysical property values is A heating light irradiation step of repeatedly irradiating the sample thin film with heating light of a pulse through a light-shielding body provided facing the front surface or the back surface of the sample thin film to block light except for an opening. Measurement that irradiates the temperature measurement light to a measurement position separated by a predetermined distance in the creeping direction along the extending direction of the surface from the heating light irradiation position on the sample thin film that has been irradiated with the heating light through the opening.
- the distance from the heating light irradiation position to the temperature measurement light irradiation position can be accurately specified.
- the thermophysical property value in the creepage direction of the thin film can be measured accurately and easily.
- thermophysical property value measuring apparatus which concerns on Embodiment 1 of this invention. It is a figure showing the heating light and the temperature measuring light which irradiate a sample and a light-shielding body in Embodiment 1.
- FIG. It is a figure showing the heating light and the temperature measuring light which irradiate a sample and a light-shielding body in Embodiment 1.
- FIG. It is a figure showing the heating light and the temperature measuring light which irradiate a sample and a light-shielding body in Embodiment 1.
- FIG. It is a timing chart which showed the timing of the heating light, the temperature change, the reflected light of the temperature measurement light, and the thermoreflectance signal.
- thermoreflectance signal It is a figure which shows the thermoreflectance signal. It is a figure which shows the standardized thermo-reflectance signal. It is a figure showing the heating light and the temperature measuring light which irradiate a sample and a light-shielding body in Embodiment 2 of this invention. It is a figure showing the heating light and the temperature measuring light which irradiate a sample and a light-shielding body in Embodiment 2. It is a figure showing the heating light and the temperature measuring light which irradiate a sample and a light-shielding body in Embodiment 2. It is a figure which shows the structure of the thermophysical property value measuring apparatus which concerns on Embodiment 3 of this invention.
- thermophysical property value measuring apparatus which concerns on another example of this invention. It is a figure showing the heating light and the temperature measuring light which irradiate a sample and a light-shielding body in another example of this invention. It is a figure showing the heating light and the temperature measuring light which irradiate a sample and a light-shielding body in another example of this invention.
- FIG. 1 is a diagram showing a configuration of a thermophysical property value measuring device 1 according to an embodiment.
- the thermophysical property value measuring device 1 irradiates the front surface of the sample 10 with heating light which is pulsed light, and detects the reflected light of the temperature measuring light which is continuous light irradiated on the back surface. The temperature response is measured using the method.
- the thermophysical property value measuring device 1 includes a function generator (FG: Function Generator) 21 that outputs a signal of an arbitrary function, a heating laser 22 that outputs heating light that heats the sample 10. It includes a temperature measuring laser 23 that outputs temperature measuring light for detecting the temperature. Further, the thermophysical property value measuring device 1 detects the lens 25 that collects the temperature-measured light, the XY stage 12 that moves the sample 10 and the light-shielding body 11, and the reflected light of the collected temperature-measured light in the sample 10. The light detector 26 is provided.
- FG Function Generator
- thermophysical property value measuring device 1 is an AD converter (Analog to Digital Converter) 27 that converts the detection signal of the optical detector 26 into analog / digital, and a computer that calculates the thermophysical property value based on the output signal of the AD converter 27. 28 and.
- AD converter Analog to Digital Converter
- FIGS. 2A, 2B, and 2C are diagrams showing the sample 10 and the light-shielding body 11 arranged to face the sample 10, and the heating light and the temperature measuring light irradiating the sample 10.
- the sample 10 is composed of a sample substrate 101 and a sample thin film 102 formed on the sample substrate 101.
- the sample substrate 101 is made of a material through which heating light or temperature measuring light is transmitted.
- the sample thin film 102 is made of any material to be measured for measuring the thermophysical property value.
- the creepage directions in which the front and back surfaces of the sample 10 and the light-shielding body 11 extend are referred to as the x direction and the y direction
- the film thickness direction perpendicular to the creepage direction is referred to as the z direction. ..
- the light-shielding body 11 has a function of light-shielding except for the opening 110.
- the light-shielding body 11 is composed of a transparent substrate 111 and a light-shielding thin film 112 having an arbitrary substance having a light-shielding property formed on the transparent substrate 111, and the light-shielding thin film 112 is a thin film of a metal material such as platinum.
- the transparent substrate 111 is made of a material through which heating light and temperature measuring light are transmitted.
- the opening 110 is, for example, a slit having a predetermined width.
- the shading body 11 is generated by any conventional method.
- the light-shielding body 11 may be generated by a method in which a metal thin film is formed on the transparent substrate 111 by a metal vapor deposition method, then patterned by photolithography, and the opening 110 is etched.
- the opening 110 has a predetermined shape and size, and is sufficiently smaller than the circle of the spot of the heating light.
- the light-shielding thin film 112 may be arranged in contact with the sample thin film 102.
- the center of the spot is at the same position in the creepage direction in the heating light and the temperature measuring light that irradiate the sample 10 and the light shield 11.
- the temperature-measured light is sufficiently focused by the lens 25 and irradiated to the sample substrate 101.
- the diameter of the spot of the heating light irradiating the light-shielding body 11 is sufficiently larger than the diameter of the spot of the temperature measuring light irradiating the sample substrate 101.
- the heating light is irradiated through the opening 110.
- the irradiation position of the heating light on the sample thin film 102 does not change.
- the irradiation position of the temperature measurement light changes by the moving distance. Therefore, by moving the sample 10 and the light-shielding body 11, the distance between the irradiation position of the heating light and the irradiation position of the temperature measuring light can be changed.
- the diameter of the spot of the temperature measuring light needs to be sufficiently small so that the change in the distance between the irradiation position of the heating light and the irradiation position of the temperature measuring light can be discriminated.
- the spots on the sample thin film 102 of the temperature measuring light are focused by the lens 25 to a size smaller than a circle having a diameter of 3 ⁇ m.
- the function generator 21 of the thermophysical property value measuring device 1 outputs an electric signal for outputting pulsed light on the order of nanoseconds to the heating laser 22.
- the pulse width of the pulsed light output by the heating laser 22 is about 1 ns, and the repetition period is 20 ⁇ s.
- the signal output by the function generator 21 has a frequency of 50 kHz corresponding to the repetition period.
- the electric signal input from the function generator 21 to the heating laser 22 can be controlled in the time interval of one cycle, and can be set by the setting panel of the function generator 21 or the externally connected computer 28. Is.
- the timing of generation of the electric signal input to the heating laser 22 is output to the AD converter 27 and used for timing control of AD (Analog to Digital) conversion.
- the heating laser 22 is a fiber laser that outputs pulsed light having a pulse width of 1 ns by an electric signal input from the function generator 21.
- the heating light output from the heating laser 22 is applied to the surface of the transparent substrate 111 opposite to the light-shielding thin film 112.
- the temperature measurement light output from the temperature measurement laser 23 is focused by the lens 25 and radiates to the surface of the sample thin film 102 opposite to the light shield 11.
- the sample 10 and the light-shielding body 11 are integrally fixed to the XY stage 12.
- the irradiation position of the temperature measuring light on the sample 10 and the light shielding body 11 is changed.
- the irradiation position of the temperature measurement light is accurately set by observing with a CCD microscope or the like.
- the photodetector 26 is a detector that receives the reflected light of the temperature measurement light and converts it into an electric signal, for example, a photodiode.
- the AD converter 27 performs analog / digital conversion of the detection signal photoelectrically converted by the photodetector 26.
- the computer 28 analyzes the digital signal output from the AD converter 27 and executes a process of calculating the thermophysical property value. That is, the computer 28 functions as a thermophysical property value calculation unit.
- thermophysical property value measuring device 1 configured as described above will be described. As shown in FIGS. 2A-C, the thermophysical property value measuring device 1 according to the present embodiment irradiates the surface of the sample thin film 102 of the sample 10 with heating light via the light-shielding body 11 to irradiate the surface of the sample thin film 102 of the sample 10 with heating light. Measurement is performed with a front heating / rear detection (FR) arrangement that irradiates the back surface with temperature measurement light.
- FR front heating / rear detection
- An electric signal having a repetition period of 20 ⁇ s is output from each of the terminals of output A and output B of the function generator 21.
- the output signal of the output B has a certain delay with respect to the output signal of the output A, and is output to the AD converter 27.
- the heating laser 22 outputs heating light having a pulse width of 1 ns and a repetition period of 20 ⁇ s based on the electric signal output from the output A of the function generator 21.
- the heating light output from the heating laser 22 passes through the transparent substrate 111 and irradiates the light-shielding thin film 112. Then, only the heating light that has passed through the opening 110 of the light-shielding thin film 112 irradiates the surface of the sample thin film 102. That is, the center of the irradiation area of the heating light is the center of the opening 110.
- the irradiation region of the sample thin film 102 becomes smaller. The temperature of the area irradiated with the heating light in the sample thin film 102 rises momentarily, and then the heat diffuses into the sample thin film 102.
- the temperature measuring laser 23 outputs temperature measuring light which is continuous light. After being focused by the lens 25, the temperature-measured light passes through the sample substrate 101 and irradiates the back surface of the sample thin film 102. Since the reflectance of the temperature-measured light is proportional to the temperature change, the thermophysical property value measuring device 1 observes the change in the back surface temperature of the sample thin film 102 from the change in the reflectance of the temperature-measured light.
- the temperature change due to one pulse of the heating light is about 0.1 ° C.
- the center of the heating light spot that irradiates the light-shielding thin film 112 and the center of the temperature measuring light spot that irradiates the sample thin film 102 are at the same position in the creepage direction. It is in.
- the sample 10 and the light shield 11 are moved by driving the XY stage 12 while keeping the centers of the spots of the heating light and the temperature measuring light at the same positions in the creepage direction.
- the XY stage is driven only in the x direction will be described.
- the heat propagation direction to be observed is the synthesis direction in which the component in the film thickness direction and the component in the creepage direction are combined.
- the heat propagation direction to be observed is the synthesis direction in which the component in the film thickness direction and the component in the creepage direction are combined.
- the component in the film thickness direction is obtained by the measurement when the temperature measurement position in FIG. 2A is x1
- the component in the creepage direction can be obtained from the measurement in the synthesis direction.
- the temperature measurement position can be changed to x1, x2, x3.
- the case where the XY stage 12 is used to move only in the x direction will be described, but a stage that can move in the three-dimensional direction may be used. The same applies to the second and third embodiments.
- the reflected light of the temperature measurement light is incident on the photodetector 26 and converted into an electric signal.
- the detection signal output by the photodetector 26 is input to the AD converter 27.
- the thermoreflectance signal output by the AD converter 27 is transmitted to the computer 28 as a temperature response signal.
- the computer 28 can calculate the thermophysical property value of the sample thin film 102 by analyzing the received thermoreflectance signal.
- FIG. 3 is a timing chart showing the timing of the heating light, the temperature change, the reflected light of the temperature measurement light, and the thermoreflectance signal.
- thermoreflectance signal which is the temperature response signal obtained in this way, is transmitted from the AD converter 27 to the computer 28.
- the computer 28 can calculate the thermophysical property value of the sample thin film 102 by analyzing using the received thermoreflectance signal.
- thermoreflectance method The signal observed by the thermoreflectance method is a time response signal.
- FIG. 4 shows a thermoreflection signal at a position where the coordinates in the x direction shown in FIGS. 2A, 2B, and 2C are x1, x2, and x3.
- the fastest rise time of the signal strength is x1, and the signal strength at the maximum is also the largest.
- the minimum value of the signal intensity is set in the time range corresponding to one cycle (20 ⁇ s) of the heating light. It is a figure which shows the standardized value by subtracting from the signal strength in time and then dividing by the maximum value.
- thermoreflectance signal at the measurement point of x3 has a peak intensity of about 130 ns, which is relatively reduced, while a peak intensity of about 3000 ns is reached at a relatively late time.
- Each signal indicates a temperature change due to thermal diffusion in the creepage direction of the sample thin film 102.
- the computer 28 obtains the heat diffusion time from the heating light irradiation position to each measurement position by analyzing these thermoreflectance signals using a theoretical formula based on the thermal diffusion equation, and heat diffusion based on the thermal diffusion time.
- the thermophysical property value including the rate can be calculated.
- the thermophysical property value measuring device 1 irradiates the sample 10 with heating light, which is pulsed light output from the heating laser 22, and outputs the sample 10 from the temperature measuring laser 23.
- the sample 10 is irradiated with temperature-measured light which is continuous light.
- the computer 28 analyzes the thermoreflectance signal obtained by AD-converting the detection signal of the reflected light in the sample thin film 102 of the temperature-measured light.
- a light-shielding thin film 112 having an opening 110 is provided so as to face the surface of the sample thin film 102 opposite to the sample substrate 101.
- the sample 10 and the light-shielding body 11 move in the creepage direction in a state where the center of the spot of the heating light and the center of the spot of the reflected light are at the same position in the creepage direction.
- the heating light is emitted through the opening 110 of the light-shielding thin film 112, and the temperature measurement light is emitted to a measurement position separated from the irradiation position of the heating light by a predetermined distance.
- the temperature change can be acquired based on the detection signal of the reflected light at each measurement position, so that the thermophysical property value in the creepage direction of the sample thin film 102 can be accurately and easily measured.
- thermophysical property value measuring device 1 The configuration and operation of the thermophysical property value measuring device 1 are the same as those in the first embodiment. In the present embodiment, the configurations of the sample 10 and the light-shielding body 11 are different.
- FIGS. 6A, 6B, and 6C are diagrams showing the sample 10 according to the present embodiment, the light-shielding body 11 arranged to face the sample 10, and the heating light and the temperature measuring light irradiating the sample 10.
- the configurations of the sample 10 and the light-shielding body 11 are the same as those in the first embodiment, but the light-shielding thin film 112 of the light-shielding body 11 faces the back surface of the sample substrate 101 of the sample 10 opposite to the sample thin film 102. The point is different from the first embodiment.
- the back surface of the sample substrate 101 and the surface of the light-shielding thin film 112 opposite to the transparent substrate 111 face each other.
- the sample substrate 101 and the light-shielding thin film 112 may be arranged in contact with each other.
- the heating light output from the heating laser 22 is irradiated toward the surface of the transparent substrate 111 opposite to the light-shielding thin film 112.
- the center of the heating light spot is at the same position as the center of the temperature measuring light spot in the creepage direction.
- the heating light passes through the opening 110 of the light-shielding thin film 112 to reduce the irradiation diameter, and then passes through the sample substrate 101 to irradiate the back surface of the sample thin film 102.
- the temperature of the irradiation region of the sample thin film 102 rises momentarily, and then the heat diffuses into the inside of the sample thin film 102.
- heat propagates in the direction of the white arrow.
- the temperature measurement light output from the temperature measurement laser 23 is sufficiently focused by the lens 25, and then, as shown in FIGS. 6A, 6B, and 6C, the surface of the sample thin film 102 opposite to the sample substrate 101. Irradiate. Since the reflectance of the temperature-measured light is proportional to the temperature change, the thermophysical property value measuring device 1 observes the change in the surface temperature of the sample thin film 102 from the change in the reflectance of the temperature-measured light. The temperature change due to one pulse of the heating light is about 0.1 ° C.
- the diameter of the heating light spot irradiating the light-shielding thin film 112 is sufficiently larger than the diameter of the temperature measuring light spot irradiating the sample thin film 102.
- the positions of the sample 10 and the light shield 11 move in the x direction or the y direction by driving the XY stage in a state where the center of the spot is at the same position in the creepage direction in the heating light and the temperature measuring light. 6A, 6B, and 6C show the case of moving in the x direction.
- the heating light is irradiated through the opening 110.
- the irradiation position of the heating light on the sample thin film 102 does not change.
- the irradiation position of the temperature measurement light changes only by the moving distance. In FIGS. 6A, 6B, and 6C, the irradiation positions of the temperature measurement light are changed to x1, x2, and x3.
- the distance between the irradiation position of the heating light and the irradiation position of the temperature measuring light can be changed.
- the diameter of the spot of the temperature measuring light needs to be sufficiently small so that the change in the distance between the irradiation position of the heating light and the irradiation position of the temperature measuring light can be discriminated.
- the spots on the sample thin film 102 of the temperature measuring light are focused by the lens 25 to a size smaller than a circle having a diameter of 3 ⁇ m.
- the reflected light of the temperature measurement light is incident on the photodetector 26 and converted into an electric signal, and is converted into a digital signal by the AD converter 27.
- the thermoreflectance signal output from the AD converter 27 is transmitted to the computer 28 as a temperature response signal.
- the computer 28 calculates the thermophysical property value of the sample thin film 102 by analyzing the received thermoreflectance signal.
- the light-shielding thin film 112 having the opening 110 is provided so as to face the surface of the sample substrate 101 of the sample 10 opposite to the sample thin film 102, and the heating light is shielded from light. It is irradiated through the opening 110 of the thin film 112.
- the sample 10 and the light-shielding body 11 move in the creepage direction in a state where the center of the spot of the heating light and the center of the spot of the reflected light are at the same position in the creepage direction.
- the heating light is emitted through the opening 110 of the light-shielding thin film 112, and the temperature measurement light is emitted to a measurement position separated from the irradiation position of the heating light by a predetermined distance.
- the temperature measurement light can be directly irradiated to each measurement position on the sample thin film 102, and the temperature change can be acquired based on the detection signal of the reflected light of the measurement light. Therefore, the thermophysical properties of the sample thin film 102 in the creeping direction. The value can be measured accurately and easily.
- FIG. 7 is a diagram showing the configuration of the thermophysical property value measuring device 3 according to the third embodiment.
- the thermophysical property value measuring device 3 irradiates the surface of the sample 10 with heating light which is pulsed light, and detects the reflected light of the temperature measuring light which is continuous light irradiating the surface. The temperature response is measured using the method.
- the thermophysical property value measuring device 3 includes a function generator 21, a heating laser 22, a temperature measuring laser 23, a lens 25, an XY stage 12, and the same as in the first embodiment. It includes a photodetector 26, an AD converter 27, and a computer 28. In this embodiment, as shown in FIG. 7, the irradiation direction of the temperature measuring light irradiating the sample 10 is different from that in the first embodiment.
- FIG. 8 is a diagram showing the sample 10 and the light-shielding body 11 arranged to face the sample 10, and the heating light and the temperature measuring light irradiating the sample 10.
- the sample 10 has the same configuration as that of the first embodiment, and is composed of the sample substrate 101 and the sample thin film 102.
- the sample substrate 101 is made of a material that transmits heating light or temperature measuring light, but in the present embodiment, it may be made of a material that does not transmit heating light or temperature measuring light.
- the light-shielding body 11 has two or more openings, and has a function of light-shielding except for the openings. In the present embodiment, the case where the two openings 108 and 109 are provided will be described.
- the light-shielding body 11 is composed of a light-shielding thin film 112 in which an arbitrary substance having a light-shielding property is formed on a transparent substrate 111, and the light-shielding thin film 112 is a metal thin film such as platinum.
- the transparent substrate 111 is made of a material through which heating light and temperature measuring light are transmitted. The method of manufacturing the light-shielding body 11 is the same as that of the first embodiment.
- Each of the openings 108, 109 has a predetermined shape and size.
- the x-coordinates of the centers of the openings 108 and 109 are x1 and x2, respectively.
- the light-shielding thin film 112 may be arranged in contact with the sample thin film 102.
- the heating laser 22 is a fiber laser that outputs pulsed light having a pulse width of 1 ns by an electric signal input from the function generator 21.
- the heating light output from the heating laser 22 is applied to the surface of the transparent substrate 111 opposite to the light-shielding thin film 112.
- the temperature measurement light output from the temperature measurement laser 23 is focused by the lens 25 and irradiates the surface of the transparent substrate 111 opposite to the light-shielding thin film 112. That is, the irradiation directions of the heating light and the temperature measuring light are the same.
- the lens 25 collects the temperature-measured light to a size smaller than a circle having a diameter of 3 ⁇ m.
- the diameter of the heating light spot that irradiates the light-shielding thin film 112 is sufficiently larger than the diameter of the temperature-measuring light spot that irradiates the light-shielding thin film 112.
- the heating light can pass through both of the two openings 108, 109.
- the center of the heating light spot and the center of the temperature measuring light spot may be at the same position in the creepage direction.
- thermophysical property value measuring device 3 configured as described above will be described.
- both the heating light and the temperature measuring light are applied to the surface of the sample thin film 102 of the sample 10 via the light shield 11 for surface heating / surface temperature measurement (FF). : Front heating / Front detection) Measure with the arrangement.
- An electric signal having a repetition period of 20 ⁇ s is output from the output A terminal of the function generator 21.
- the output signal of the output B has a certain delay with respect to the output signal of the output A, and is output to the AD converter 27.
- the heating laser 22 outputs heating light having a pulse width of 1 ns and a repetition period of 20 ⁇ s by the electric signal output from the output A of the function generator 21.
- the heating light output from the heating laser 22 is emitted toward the surface of the transparent substrate 111 opposite to the light-shielding thin film 112.
- the center of the spot for irradiating the light-shielding thin film 112 of the heating light is the center of the opening 108. Since the spot diameter is sufficiently large, the heating light passes through the openings 108 and 109 and irradiates the surface of the sample thin film 102. That is, in FIG. 8, the irradiation region of the sample thin film 102 of the heating light is a region centered on the positions where the x-coordinates are x1 and x2. The temperature of the irradiation region of the sample thin film 102 rises momentarily, and then the heat diffuses into the inside of the sample thin film 102.
- the temperature measurement light output from the temperature measurement laser since it passes only through the opening 108 and irradiates the surface of the sample thin film 102.
- the time change of the reflected light intensity of the temperature measurement light in the sample thin film 102 is indicated by a white arrow after the temperature change of the position x2 due to the heating light passing through the opening 108 and the temperature rise due to the heating light passing through the opening 109. It is expressed as the sum of the temperature changes at the position x2 due to the diffusion of heat as shown in.
- the temperature change at the position x2 due to the heating light passing through the opening 108 is the temperature change on the sample surface due to heat diffusion in the film thickness direction of the sample thin film 102, and the sample thin film 102 is directly heated without installing the light-shielding body 11. It can be obtained by the measurement when it is done. Therefore, after the temperature rises due to the heating light passing through the opening 109, the temperature change at the position x2 due to the diffusion of heat is the change in the reflectance of the temperature-measured light due to the configuration provided with the light-shielding body 11 shown in FIG. It can be calculated from the difference between the above and the change in the reflectance of the temperature-measured light measured without installing the light-shielding body 11.
- thermoreflectance signal in the present embodiment.
- the computer 28 can calculate the thermophysical property value including the thermal diffusivity in the creepage direction of the sample thin film 102.
- one or more openings may be provided apart from each other in the creepage direction.
- the XY stage 12 to which the sample 10 and the light shielding body 11 are fixed is moved, and the centers of the spots of the heating light and the temperature measuring light are set to another.
- the thermoreflectance signal at another position can be acquired. Based on the obtained thermoreflectance signal, the thermophysical property value in the creepage direction can be known in more detail.
- the heating light can also pass through the opening 108 at the position of x2. That is, the center of the spot of the heating light may be x1 or x2.
- the light-shielding thin film 112 has two or more openings, the heating light is applied to the region including at least one opening 109, and the temperature measurement light is focused, and the like.
- the measurement position at the same position as the opening 108 of 1 in the creepage direction is irradiated.
- the sample thin film 102 may simultaneously have a region where both the heating light and the temperature measuring light are irradiated and a region where either the heating light or the temperature measuring light is irradiated.
- the light-shielding thin film 112 faces the sample thin film 102 of the sample 10, but as in the second embodiment, the surface of the sample substrate 101 opposite to the sample thin film 102 is light-shielded.
- the thin films 112 may face each other. In this case, the heating light and the temperature measuring light pass through the opening 110 of the light-shielding thin film 112, pass through the sample substrate 101, and irradiate the sample thin film 102.
- the thermophysical property value measuring device 3 irradiates the surface of the light-shielding thin film 112 opposite to the sample thin film 102 with heating light and temperature measuring light.
- the light-shielding thin film 112 has two or more openings including openings 108 and 109.
- the heating light passes through both the openings 108 and 109 to heat the sample thin film 102, and the temperature measurement light passes only through the openings 108 and is reflected by the sample thin film 102.
- the computer 28 analyzes the thermo-reflectance signal obtained based on the reflected light of the obtained temperature measurement light. As a result, even in the front heating front temperature measurement configuration, the thermophysical property value in the creepage direction of the sample thin film 102 can be accurately measured.
- thermoreflectance signal obtained by irradiating the sample 10 in which the sample thin film 102 of titanium nitride is formed on the sample substrate 101 with heating light and temperature measuring light. was acquired and analyzed by the computer 28.
- the light-shielding body 11 has a wire structure in which platinum (Pt) light-shielding thin films 112 are formed on the transparent substrate 111 with slits at intervals of 15 ⁇ m.
- the diameter of the spot of the heating light was set to about 30 ⁇ m, which is about twice the period of 15 ⁇ m of the wire structure.
- the heating light is applied to the sample thin film 102 through two linear openings adjacent to one light-shielding thin film.
- the thermal diffusivity of the sample substrate 101 is smaller than that of the sample thin film 102, the approximation of one-dimensional heat conduction to the creepage method is well established.
- the temperature drops more slowly due to the increase in the distance between the heating position and the temperature measurement position, as compared with the three-dimensional heat diffusion when heating in dots. It has the feature that it becomes easy to detect.
- FIG. 10 shows the results of measurement by changing the position of irradiating the temperature measurement light between one section of 15 ⁇ m.
- the displacement amount on the horizontal axis is a value with the center of the slit, which is the opening 110, being 0 ⁇ m.
- the vertical axis is the time when the signal strength of the normalized thermoreflectance signal as shown in FIG. 5 is maximized. As shown in FIG. 9, the time at which the signal strength is maximized when the displacement amount is changed is symmetrical with respect to the measurement point having the displacement amount of 8 ⁇ m, which corresponds to half of the period of the wire structure.
- the temperature rise due to heat transfer derived from the heating light passing through the opening 110 closest to the temperature measurement light irradiation position is detected.
- the actual maximum signal strength at the measurement point having a displacement of 8 ⁇ m, which maximizes the time for which the signal strength is maximized, is the minimum.
- the time for which the signal intensity is maximized is the maximum and the maximum signal intensity is the minimum. Therefore, the heating light and the temperature measuring light are predetermined for the light shielding body 11. It is guaranteed that the light is emitted at a distance of a certain distance.
- the light-shielding body 11 includes three or more openings 110 and the heating light passes through each of the openings 110, the influence of the third and subsequent openings 110 is the film thickness direction that has been conventionally performed. It can be handled by the same analysis method as the one-dimensional thermal diffusion of.
- the creepage direction of the sample thin film 102 You can get the knowledge about the heat diffusion of. For example, when the sample thin film 102 has in-plane anisotropy, when the light-shielding body 11 having the slit-shaped opening 110 is installed with respect to the sample thin film 102, it is possible to measure by rotating the direction of installation. The thermal diffusivity in the direction of can be easily measured.
- the magnitude relationship between the thermal diffusivity time in the creepage direction of the sample thin film 102 to be measured and the thermal diffusivity time in the creepage direction of the standard sample is clarified. Can be done. In addition, theoretical calculations can be performed based on the time change of the thermoreflectance signal at each measurement point, and the thermophysical property values including the thermal diffusivity can be obtained.
- the sample thin film provided with the light-shielding body excluding the opening is repeatedly irradiated with the heating light of the pulse through the opening of the light-shielding body, and from the heating light irradiation position on the sample.
- the temperature measurement light is irradiated to the measurement position separated by a predetermined distance in the creepage direction along the extending direction of the surface, and the creepage direction of the sample thin film is based on the reflected light intensity of the reflected light of the sample thin film of the temperature measurement light. It was decided to calculate the thermophysical property value of. This makes it possible to accurately and easily measure the thermophysical property values in the creepage direction of the sample thin film.
- the temperature measuring light is continuous light, but it may be pulsed light.
- FIG. 11 shows the configuration of the thermophysical property value measuring device 4 in which the temperature measuring light is pulsed light.
- the heating laser 22 and the temperature measuring laser 23 are pulse-driven by the electric signal generated by the signal generator A (SG: Signal Generator) 41, and output pulsed light on the order of nanoseconds.
- the heating light of the pulsed light is intensity-modulated by the light modulator 45 based on the electric signal generated by the signal generator B (SG) 44, and is applied to the sample 11.
- the temperature-measured light of the pulsed light is condensed by the lens 25 and irradiated to the sample 11.
- thermophysical property value measuring device 4 can measure the thermophysical property value more accurately based on the thermoreflectance signal with reduced noise.
- the heating light is set to be pulsed light on the order of nanoseconds, but pulsed light on the order of picoseconds or femtoseconds may be used.
- the temperature-measured light is also picosecond-order pulsed light.
- the temperature measurement light is also pulsed light on the order of femtoseconds.
- the light-shielding body 11 is formed by forming a light-shielding thin film 112 on the transparent substrate 111, but as shown in FIG. 12, the surface of the sample thin film 102 of the sample 10 has a light-shielding property.
- the material may be directly deposited to form the light-shielding thin film 112.
- a light-shielding material may be directly formed on the surface of the sample substrate 101 of the sample 10 opposite to the sample thin film 102 to form the light-shielding thin film 112.
- thermophysical property value measuring devices 1, 3 and 4 measure the sample 10 having the sample thin film 102 formed on the sample substrate 101, but are self-supporting without the sample substrate 101. It is also possible to measure the sample thin film 102, which is a film.
- the sample thin film 102 is irradiated with heating light directly or through the sample substrate 101, but the front surface or the back surface of the sample thin film 102 is for enhancing the absorption or reflection of light.
- a thin film may be further provided.
- the thin film here is a thin film different from the light-shielding thin film 112.
- Thermophysical property value measuring device 10 ... Sample 11 ... Shading body 12 ... XY stage 21 ... Function generator 22 ... Heating laser 23 ... Temperature measuring laser 24 ... Optical modulator 25 ... Lens 26 ... Light detection Instrument 27 ... AD converter 28 ... Computer 41 ... Signal generator A 44 ... Signal generator B 45 ... Optical modulator 47 ... Lock-in amplifier 101 ... Sample substrate 102 ... Sample thin film 108, 109, 110 ... Opening 111 ... Transparent substrate 112 ... Light-shielding thin film
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Abstract
Description
試料薄膜の表面または裏面に対向して備えられ、開口部を除いて遮光する遮光体と、
前記遮光体を介して前記試料薄膜に繰り返しパルスの加熱光を照射する加熱用レーザと、
前記開口部を通って前記加熱光が照射された前記試料薄膜上の加熱光照射位置から表面の延在方向に沿った沿面方向に予め定めた距離離れた測定位置に測温光を照射する測温用レーザと、
前記測温光の前記試料薄膜での反射光を検出する光検出器と、
前記光検出器で検出した前記反射光の反射光強度に基づいて、前記試料薄膜の前記沿面方向の熱物性値を算出する熱物性値算出部と、
を備えることを特徴とする。
前記加熱光のスポットの中心と、前記測温光のスポットの中心と、は沿面方向において同じ位置にあり、
前記遮光体の前記開口部を、前記加熱光及び前記測温光のスポットの中心からずらすことにより、前記測温位置を前記加熱光照射位置から予め定めた距離離すようにしてもよい。
前記透明基板上の前記遮光薄膜を前記試料薄膜の表面に対向させ、
前記加熱用レーザは、前記加熱光を前記透明基板側から照射してもよい。
前記遮光体は、透明基板に前記開口部を除いて、遮光性を有する遮光薄膜を成膜して形成したものであって、
前記透明基板上の前記遮光薄膜を、前記試料基板の前記試料薄膜と反対の面に対向させ、
前記加熱用レーザは、前記加熱光を前記透明基板側から照射してもよい。
前記加熱用レーザは、前記加熱光を前記試料薄膜の表面上の前記遮光体の上から照射してもよい。
前記遮光体は、前記試料基板の前記試料薄膜と反対側の裏面に遮光性を有する遮光薄膜を成膜して形成したものであって、
前記加熱用レーザは、前記加熱光を前記試料基板の前記裏面上の前記遮光体の上から照射してもよい。
前記加熱光及び測温光はいずれも前記遮光体を介して前記試料薄膜に照射され、
前記加熱光は、少なくとも1の前記開口部を含む領域に照射され、
前記測温光は、集光されて、他の1の前記開口部と沿面方向において同じ位置にある前記測定位置に照射されてもよい。
前記熱物性値算出部は、前記測定位置で反射した前記反射光強度に基づいて、前記沿面方向の前記熱物性値を算出してもよい。
前記加熱光の前記試料薄膜への加熱光照射時刻と、前記測温光の前記試料薄膜への測温光照射時刻を、前記信号発生器の駆動信号により制御し、
前記熱物性値算出部は、前記加熱光照射時刻及び前記測温光照射時刻の時間差に基づいて、熱拡散時間を算出し、前記熱拡散時間に基づいて熱拡散率を含む前記熱物性値を算出してもよい。
試料薄膜の表面又は裏面に対向して備えられ開口部を除いて遮光する遮光体を介して、前記試料薄膜に対して、繰り返しパルスの加熱光を照射する加熱光照射ステップと、
前記開口部を通って前記加熱光が照射された前記試料薄膜上の加熱光照射位置から表面の延在方向に沿った沿面方向に予め定めた距離離れた測定位置に測温光を照射する測温光照射ステップと、
前記測温光の前記試料薄膜での反射光を検出する光検出ステップと、
前記光検出ステップで検出した前記反射光の反射光強度に基づいて、前記試料薄膜の前記沿面方向の熱物性値を算出する熱物性値算出ステップと、
を有することを特徴とする。
本発明の実施の形態について図面を参照して詳細に説明する。図1は、実施の形態に係る熱物性値測定装置1の構成を示す図である。本実施の形態では、熱物性値測定装置1は、試料10の表面にパルス光である加熱光を照射して、裏面に照射した連続光である測温光の反射光を検出するサーモリフレクタンス法を用いて、温度応答の測定をする。
本発明の実施の形態2について図面を参照して詳細に説明する。熱物性値測定装置1の構成及び動作は、実施の形態1と同様である。本実施の形態では、試料10と遮光体11の構成が異なる。
本発明の実施の形態3について図面を参照して詳細に説明する。図7は、実施の形態3に係る熱物性値測定装置3の構成を示す図である。本実施の形態では、熱物性値測定装置3は、試料10の表面にパルス光である加熱光を照射して、表面に照射した連続光である測温光の反射光を検出するサーモリフレクタンス法を用いて、温度応答の測定をする。
実施の形態1に示した構成の熱物性値測定装置1において、試料基板101に窒素チタンの試料薄膜102を形成した試料10に加熱光と測温光を照射して得られたサーモリフレクタンス信号を、コンピュータ28が取得し解析した。ここで、遮光体11は、図9に示すように、透明基板111に白金(Pt)の遮光薄膜112が15μmの間隔でスリットを挟んで形成されたワイヤ構造を有している。加熱光のスポットの直径は、ワイヤ構造の周期である15μmの約2倍である約30μmとした。
10…試料
11…遮光体
12…XYステージ
21…関数発生器
22…加熱用レーザ
23…測温用レーザ
24…光変調器
25…レンズ
26…光検出器
27…ADコンバータ
28…コンピュータ
41…信号発生器A
44…信号発生器B
45…光変調器
47…ロックインアンプ
101…試料基板
102…試料薄膜
108,109,110…開口部
111…透明基板
112…遮光薄膜
Claims (16)
- 試料薄膜の表面または裏面に対向して備えられ、開口部を除いて遮光する遮光体と、
前記遮光体を介して前記試料薄膜に繰り返しパルスの加熱光を照射する加熱用レーザと、
前記開口部を通って前記加熱光が照射された前記試料薄膜上の加熱光照射位置から表面の延在方向に沿った沿面方向に予め定めた距離離れた測定位置に測温光を照射する測温用レーザと、
前記測温光の前記試料薄膜での反射光を検出する光検出器と、
前記光検出器で検出した前記反射光の反射光強度に基づいて、前記試料薄膜の前記沿面方向の熱物性値を算出する熱物性値算出部と、
を備える熱物性値測定装置。 - 前記遮光体に照射する前記加熱光のスポットの直径は、前記試料薄膜上の前記測温光のスポットの直径より大きく、
前記加熱光のスポットの中心と、前記測温光のスポットの中心と、は沿面方向において同じ位置にあり、
前記遮光体の前記開口部を、前記加熱光及び前記測温光のスポットの中心からずらすことにより、前記測温位置を前記加熱光照射位置から予め定めた距離離す、
請求項1に記載の熱物性値測定装置。 - 前記遮光体は、前記加熱光が透過する材料で構成された透明基板に、前記開口部を除いて遮光性を有する遮光薄膜を成膜して形成したものであって、
前記透明基板上の前記遮光薄膜を前記試料薄膜の表面に対向させ、
前記加熱用レーザは、前記加熱光を前記透明基板側から照射する、
請求項1又は2に記載の熱物性値測定装置。 - 前記試料薄膜は、試料基板上に成膜された薄膜であって、
前記遮光体は、透明基板に前記開口部を除いて、遮光性を有する遮光薄膜を成膜して形成したものであって、
前記透明基板上の前記遮光薄膜を、前記試料基板の前記試料薄膜と反対の面に対向させ、
前記加熱用レーザは、前記加熱光を前記透明基板側から照射する、
請求項1又は2に記載の熱物性値測定装置。 - 前記遮光体は、前記試料薄膜の表面に遮光性を有する遮光薄膜を成膜して形成したものであって、
前記加熱用レーザは、前記加熱光を前記試料薄膜の表面上の前記遮光体の上から照射する、
請求項1又は2に記載の熱物性値測定装置。 - 前記試料薄膜は、試料基板上に成膜された薄膜であって、
前記遮光体は、前記試料基板の前記試料薄膜と反対側の裏面に遮光性を有する遮光薄膜を成膜して形成したものであって、
前記加熱用レーザは、前記加熱光を前記試料基板の前記裏面上の前記遮光体の上から照射する、
請求項1又は2に記載の熱物性値測定装置。 - 前記熱物性値算出部は前記反射光強度に基づいて、前記加熱光照射位置から前記測定位置までの前記試料薄膜の熱拡散時間を算出し、前記熱拡散時間に基づいて熱拡散率を含む前記熱物性値を算出する、
請求項1から6のいずれか1項に記載の熱物性値測定装置。 - 前記測温光は、集光されて、前記試料薄膜の前記遮光体と反対側の面に存する前記測定位置に照射される、
請求項1から7のいずれか1項に記載の熱物性値測定装置。 - 前記遮光体は、互いに分離された2以上の前記開口部を有し、
前記加熱光及び測温光はいずれも前記遮光体を介して前記試料薄膜に照射され、
前記加熱光は、少なくとも1の前記開口部を含む領域に照射され、
前記測温光は、集光されて、他の1の前記開口部と沿面方向において同じ位置にある前記測定位置に照射される、
請求項1から7のいずれか1項に記載の熱物性値測定装置。 - 前記遮光体を備えた前記試料薄膜を固定したステージを前記沿面方向に平行な2次元方向に移動して、前記測定位置を変更し、
前記熱物性値算出部は、前記測定位置で反射した前記反射光強度に基づいて、前記沿面方向の前記熱物性値を算出する、
請求項1から9のいずれか1項に記載の熱物性値測定装置。 - 前記加熱光は、パルス幅がナノ秒、ピコ秒又はフェムト秒のオーダーのパルス光である、
請求項1から10のいずれか1項に記載の熱物性値測定装置。 - 前記測温光は、連続光である、
請求項11に記載の熱物性値測定装置。 - 前記測温光は、パルス幅がナノ秒、ピコ秒又はフェムト秒のオーダーのパルス光である、
請求項11に記載の熱物性値測定装置。 - 前記加熱用レーザ及び前記測温用レーザに対して駆動信号を出力する信号発生器を更に備え、
前記加熱光の前記試料薄膜への加熱光照射時刻と、前記測温光の前記試料薄膜への測温光照射時刻を、前記信号発生器の駆動信号により制御し、
前記熱物性値算出部は、前記加熱光照射時刻及び前記測温光照射時刻の時間差に基づいて、熱拡散時間を算出し、前記熱拡散時間に基づいて熱拡散率を含む前記熱物性値を算出する、
請求項13に記載の熱物性値測定装置。 - 前記遮光体は、前記開口部以外に金属材料を成膜した遮光薄膜を有する、
請求項1から14のいずれか1項に記載の熱物性値測定装置。 - 試料薄膜の表面又は裏面に対向して備えられ開口部を除いて遮光する遮光体を介して、前記試料薄膜に対して、繰り返しパルスの加熱光を照射する加熱光照射ステップと、
前記開口部を通って前記加熱光が照射された前記試料薄膜上の加熱光照射位置から表面の延在方向に沿った沿面方向に予め定めた距離離れた測定位置に測温光を照射する測温光照射ステップと、
前記測温光の前記試料薄膜での反射光を検出する光検出ステップと、
前記光検出ステップで検出した前記反射光の反射光強度に基づいて、前記試料薄膜の前記沿面方向の熱物性値を算出する熱物性値算出ステップと、
を有する熱物性値測定方法。
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