WO2005119231A1 - Characteristic measuring apparatus and characteristic measuring method - Google Patents

Abstract

A characteristic measuring apparatus provided with a first member having an energy applying means and a second member arranged to face the first member is provided. An accurate matching mechanism for an accurate waveform generation and input/output is provided by a high-speed waveform integrating circuit using a gate array and by reading out of digital data (numerical table). A sample can be held between the first and the second members, and a characteristic measuring means is arranged at least on one of the members. At the time of measuring a desired characteristic, the characteristic measuring means and the energy applying means are closely arranged. Thus, the characteristic measuring apparatus and the characteristic measuring method which permit simple and quick characteristic measurement are provided.

Description

Characteristic measuring instrument and characteristic measuring method

Technical field

 The present invention relates to a characteristic measuring instrument capable of easily measuring various characteristics of various samples including substances, materials, and systems, and the characteristic measuring instrument.

Signal and Z or signal processor that can be used particularly preferably in combination with various properties of various samples including substances, materials, and systems (eg, heat transfer, heat insulation, etc.) The present invention relates to a characteristic measuring method capable of easily measuring the thermal characteristic of the material.

Background art

 From the viewpoint of the development of materials and materials that can exhibit the desired physical properties, various materials, materials, and systems-related fields (eg, polymers, biotechnology, semiconductor materials, ceramic materials, and f-heat materials) In a wide range of technical fields including metal and composite materials-related fields, there is an increasing demand for easy measurement of various properties (for example, thermal conductivity or thermal diffusivity as thermal properties). ing. Examples of materials to be measured include, for example, insulating paper, foamed polymer materials, highly molecularly oriented polymer films, multilayer films, spin-coated thin films, cast films, vapor-deposited films, Fabrics, vacuum insulating materials, building materials, wall materials, refrigerator heat insulating materials, automobile roofing materials, and the like can be mentioned.

Of course, to develop materials that exhibit desired physical properties, it is, of course, necessary to precisely control these physical properties and to ensure sufficient quality control. Furthermore, structures that should exhibit such desired physical properties (particularly, microstructures) In order to develop materials with the above characteristics, analytical techniques that accurately and easily evaluate the properties of the materials are indispensable.

 The instrument for property measurement, the property measurement method, and the signal generator of the present invention can be suitably used for measurement of various properties such as physical properties. Here, for convenience of explanation, thermal properties (for example, First, the prior art that evaluates the heat transfer properties) will be described.

 As a method for evaluating the heat transfer properties of a material, a laser flash method, a hot wire method, a probe method, and the like have been widely used. In these, the sample to be measured is molded according to the measurement, but it is often impossible to sample actual materials.

 As a method of measuring the thermal diffusivity of a sample using a temperature wave,

There is 3-1 8 9 5 4 7 gazette. According to this method, it is possible to measure the thermal diffusivity of a thin electrical insulator of a film having a film thickness of 1 μm or more, but the simplicity of the measurement (for example, ease and speed) is not always sufficient. There was no. For example, such measurements could not be performed on portable (ie, easily brought into production) equipment.

 [Patent Document 1] Japanese Patent Application Laid-Open No. 3-1899547 Disclosure of the Invention

 An object of the present invention is to provide a characteristic measuring instrument or a characteristic measuring method capable of solving the above-mentioned disadvantages of the prior art.

 It is another object of the present invention to provide a characteristic measuring instrument and a characteristic measuring method that enable simple and quick characteristic measurement.

As a result of earnest research, the inventor has found that at least one of the first and second members is movable, and at least the characteristic applying means and the characteristic measuring means are arranged close to each other at the time of characteristic measurement. like It has been found that configuring a characteristic measuring instrument is extremely effective in achieving the above object.

 The characteristic measuring instrument of the present invention is based on the above findings, and more specifically, a first member having at least a part thereof having energy applying means, and a first member having an energy applying means disposed at least partially facing the first member. A characteristic measuring instrument comprising at least a first member and a second member; at least one of the first and second members so as to be able to hold a sample between the first and second members. One of the first and second members is movable, and at least one of the first and second members is provided with a characteristic measuring unit. At least at the time of measuring the characteristic, the characteristic measuring unit and the energy applying unit are arranged close to each other. In response to the application of energy from the energy applying means to a sample arranged between the first and second members, the characteristic change in the sample is measured by the characteristic measurement. Can be measured by means It is characterized in that the the.

 According to the present invention, further, energy is applied to the sample from the energy applying means,

 A characteristic measuring method is provided, wherein a characteristic change based on the energy application is measured by characteristic measuring means arranged close to or in contact with the sample and close to the energy applying means. Is done.

 According to the present invention, further, a CPU, a memory connected to the CPU,

A signal generation Z analyzer including at least a DZA converter connected to the CPU and an A / D converter connected to the CPU; digital data previously written in the memory, A signal which can be A-converted into an AC voltage having a frequency and supplied to external energy applying means connected to the A-converter. A file generator / analyzer is provided.

 When the characteristic measuring device or the characteristic measuring method of the present invention having the above-described configuration is used, various characteristics of various samples including various substances, materials, and systems can be easily measured.

 In addition, when such a characteristic measurement is used in combination with the signal generator / analyzer of the present invention, more rapid measurement of the characteristic is possible.

 In the present invention, for example, in a mode of measuring thermal characteristics, for example, quality control of a heat insulating material, a building material, a biomaterial including a human body, and a performance evaluation of a material used for the purpose of heat transfer or heat insulation are performed at a manufacturing site It can be measured easily.

 Examples of the main preferred embodiments of the present invention are as follows.

 (1) Select a flat part of the sample (or specimen) to be measured and sandwich it between the sensor and the heater. At this time, grease or the like may be applied to improve the contact. In principle, an insulation coating can be applied to one side of the heater and pressed against the sample. Measure the phase change and amplitude decrease of the temperature wave that reaches the position of the attached sensor.

 (2) In addition, if a calibration curve is obtained between the temperature of the temperature wave that has passed through the probe and a sample whose thermophysical properties are known as the measurement sample, the measurement of the unknown sample can be accelerated. In addition, the so-called distribution measurement at several places of the sample becomes extremely easy.

 (3) As a temperature sensor (probe), a thin metal film, semiconductor thin film, thermistor, etc., with a small heat capacity is used as a resistance temperature sensor.

(4) The device to be used in the present invention changes the temperature of the surface of the material to be measured by heating, and reaches the rear surface via the sandwiched sample. An embodiment that includes at least a device for amplifying a signal of a heated temperature wave and performing Lockin amplification or Fourier transform. According to this aspect, for example, as a material to be measured, a material having a known thermal conductivity is used to determine a change in amplitude, and by comparing with this, it is possible to convert to an apparent thermal conductivity.

 (5) A mode in which a lock-in method having a high noise removal effect is applied instead of measuring a temperature change of a sample to be measured in a DC manner. In such an embodiment, a wide range of frequencies can be selected by selecting the thickness of the probe and the kind of substance, and the thickness and depth of the target sample can be defined. In other words, at low frequencies, more internal thermal conductivity is reflected, and at higher frequencies, only the surface thermal conductivity is reflected. At the same time, a high-performance thickness gauge can be incorporated to quickly convert to thermal diffusivity. Brief Description of Drawings

 FIG. 1 is a schematic perspective view of a sample for explaining the definition of thermal conductivity and the like in the present invention.

 FIG. 2 is a schematic perspective view of a sample for explaining unsteady heat conduction in the present invention.

 Fig. 3 is a schematic graph (a) and a schematic phase difference graph (b) showing an example of temperature change measurement when an AC-like temperature change is applied to a sample.

 FIG. 4 is a schematic cross-sectional view for explaining the concepts of “thermally thick” and “thermally thin”.

 FIG. 5 is a diagram showing an example of a circuit diagram of a thin-film temperature sensor.

 Figure 6 is a schematic diagram showing examples of AC power supply voltage and measurement signals.

FIG. 7 is a schematic Daraf showing an example of the phase delay (a) and the amplitude (b). FIG. 8 is a schematic cross-sectional view showing one example of the property measuring instrument of the present invention.

FIG. 9 is a schematic perspective view showing one example of the characteristic measuring instrument of the present invention.

FIG. 10 is a block diagram showing an example of a circuit diagram suitably usable in the present invention.

 FIG. 11 is a block diagram showing an example of a circuit diagram suitably usable in the present invention.

2 is an example of a circuit diagram that can be suitably used in the present invention. FIG. ^{1 and} FIG. ¹³ are examples of a partial circuit diagram that can be suitably used in the present invention.

 FIG. 14 is an example of a partial circuit diagram that can be suitably used in the present invention.

 FIG. 15 is an example of a partial circuit diagram suitably usable in the present invention.

 FIG. 16 is an example of a partial circuit diagram suitably usable in the present invention.

 FIG. 17 is an example of a measurement method algorithm that can be suitably used in the present invention.

 FIG. 18 is a schematic diagram for explaining steps of an example of a measurement method that can be suitably used in the present invention.

 FIG. 19 is a schematic diagram for explaining steps of an example of a measurement method that can be suitably used in the present invention.

 FIG. 20 is a schematic diagram for explaining steps of an example of a measurement method that can be suitably used in the present invention.

FIG. 21 shows screen display steps that can be suitably used in the present invention. This is an example.

 FIG. 22 is an example of a screen display step suitably usable in the present invention.

 FIG. 23 is an example of a screen display step suitably usable in the present invention.

 FIG. 24 is an example of a screen display step suitably usable in the present invention.

 FIG. 25 is a graph showing an example of thermal measurement data (sample: force glass) obtained in Example 1 of the present invention.

 FIG. 26 is a graph showing an example of thermal measurement data (sample: PMMA film) obtained in Example 2 of the present invention.

 FIG. 27 is a graph showing an example of the thermal measurement data ('sample: polyimide film) obtained in Example 3 of the present invention.

 FIG. 28 is a graph showing an example of thermal measurement data (sample: PET film) obtained in Example 4 of the present invention.

 FIG. 29 is a graph showing an example of thermal measurement data (sample: Kapton-1) obtained in Example 5 of the present invention.

 FIG. 30 is a graph showing an example of thermal measurement data (sample... Kapton-2) obtained in Example 5 of the present invention.

 FIG. 31 is a graph showing an example of the thermal measurement data (sample: cover glass) obtained in Example 5 of the present invention.

 FIG. 32 is a graph showing an example of thermal measurement data (sample: PMM A) obtained in Example 5 of the present invention.

 FIG. 33 is a graph showing an example of the thermal measurement data (sample: Kapton 3) obtained in Example 5 of the present invention.

FIG. 34 is a graph showing an example of thermal measurement data (sample: Kapton 4) obtained in Example 5 of the present invention. In the figure, the following symbols have the following meanings.

 1 0

 1 1 ... base

 1 2 ... Arm

 1 3

 1 4 ... heater

 1 5

 1 6

 1 7 ... 'Differential transformer Best mode for carrying out the invention

 Hereinafter, the present invention will be described more specifically with reference to the drawings as necessary. In the following description, “parts” and “%” representing the quantitative ratios are based on mass unless otherwise specified.

 (Characteristic measuring instrument)

 The characteristic measuring instrument of the present invention has at least a first member having energy applying means at least in a part thereof, and a second member for holding a sample. At least one of the first and second members is movable, and a sample to be measured can be held between the first and second members. At least one of the first and second members is provided with a characteristic measuring means, and at least at the time of measuring the characteristic, the characteristic measuring means and the energy applying means are arranged close to each other. Is configured. Energy is applied from the energy applying means to the sample arranged between the first and second members, and in response to the energy application, a characteristic change in the sample is measured by the characteristic measuring means. Can be measured.

(One embodiment of characteristic measuring instrument) One embodiment of the characteristic measuring instrument of the present invention is shown in the schematic cross-sectional view of FIG. In the embodiment of FIG. 8, at the time of measuring the sample, the energy applying means (heater serving as thermal energy applying means) and the characteristic measuring means (thermophysical property measuring means) are arranged so as to be “close” with the sample interposed therebetween. Have been.

 Referring to FIG. 8, the characteristic measuring instrument 10 of this embodiment includes a base 11 (first member) and an arm 12 (second member) rotatably supported at one end of the base 11. ), And a sample 13 to be measured can be held between the base 11 and the arm 12. A heater 14 is arranged at the tip of the arm 12, and a sensor 15 (characteristic measuring means) is arranged at a position of the base 11 facing the heater 14. With such a characteristic measuring instrument 10, the thermal characteristics of the sample 13 can be measured.

 In FIG. 8, an iron core 16 is further arranged on the arm 12, and the iron core 16 and the differential transformer 17 on the base 11 side facing the iron core 16 form a differential transformer for the iron core 16. The degree of entry into 17 (corresponding to the thickness of sample 13) can be measured.

 (One form of data processing)

 The outputs from the sensor 15 and the differential transformer 17 are amplified by a two-channel preamplifier 18 arranged in the base 11, and the output from the preamplifier 18 is passed through an AZD converter 19. Is input to the CPU 20. On the other hand, the input to the heater 14 is input from the CPU 20 via the D / A converter 21 to the heater 14. The output from the CPU 20 is displayed on the LCD panel 22 and analyzed by an external personal computer 23.

FIG. 8B is a schematic sectional view showing details of the heater 14 and the sensor 15 (sample portion). Each of these elements has a thin film resistor or a thermistor arranged on a substrate. In the embodiment of FIG. If necessary, the heater 14 may be placed on a very small ball (not shown) so that the sample to be measured is sandwiched in parallel with the measurement surface of the sensor 15. In such an embodiment, the measurement accuracy can be further improved.

 In the embodiment of FIG. 8, the thickness of the sample 13 can be measured simultaneously with the thermal characteristics of the sample 13 by detecting the displacement in the transformer coil 17. In this case, it is preferable to calibrate the zero thickness of the sample 13 (without the sample) in advance.

 FIG. 9 is a schematic perspective view of the characteristic measuring device corresponding to FIG. In the embodiment shown in FIG. 9, the lever 30 can press the sample sandwiched between the base 11 and the arm 12. This pressurization can be performed by a separately provided motor (not shown). In the above-described embodiment of FIG. 8, the operation speed can be further improved by combining a signal generation analyzer as described later. · (One mode of measurement method)

In the embodiment of FIG. 8, the optimum heat application condition can be determined for one sample by trial and error within a certain range. In this case, for example, the measurement data is stored in real time (along with the calibration probe) on the LCD panel 22 or a laptop personal computer (for example, connected to the CPU 20 if necessary). Optimal heat application conditions (conditions where the graph becomes linear) For example, conditions where the relationship between the square root of the frequency of the applied temperature wave and the phase measured by the sensor 15 becomes linear Can be checked. By the calculation in the personal computer, the thermal diffusivity α (and the thermal conductivity) can be automatically calculated. In the embodiment shown in FIG. 8, the display color on the liquid crystal panel 22 can be changed for different measurements as necessary. In addition, the characteristic measuring instrument of the present invention can be widely used not only for thermophysical properties (for example, viscosity), but also for elastic modulus, dielectric constant, conductivity, and humidity, as described later.

 (Measurable characteristics)

 When the measuring instrument of the present invention is used, the following characteristics can be measured. (1) Physical properties (i) Mechanical properties, such as viscosity, dynamic elastic modulus (ii) Thermal properties, such as thermal diffusivity, thermal conductivity, thermal resistivity (iii) Electrical properties, such as dielectric Rate, conductivity (2) Other characteristics, such as humidity

 (Energy application means)

 In the present invention, the type, mechanism, shape, size, and the like of the energy applying means are not particularly limited, as long as useful properties of the sample can be measured based on the energy application from the means. It can be appropriately selected and used. As such energy applying means, for example, those listed below can be used.

 A. C Joule heating to thin film resistors, flash irradiation, modulation laser irradiation, and joule heating of chip resistors.

 (Characteristic measuring means)

 In the present invention, the type, mechanism, shape, size, and the like of the characteristic measuring means are not particularly limited as long as useful properties of the sample corresponding to the energy application from the energy applying means can be measured. It can be appropriately selected and used from the characteristic measuring means. As such a characteristic measuring means, for example, those listed below can be used.

Thin film resistors, chip resistors, thermistors, thermocouples, RTDs, strain gauges Page, Peltier element, infrared detecting element, etc.

 (Preferred combination of energy applying means and measuring means)

 In the present invention, the following combinations of energy applying means and characteristic measuring means can be suitably used in connection with various characteristic measurements as described below.

 <Characteristics to be measured> <Energy applying means> <Characteristic measuring means> Thermal properties Heater Temperature sensor Viscosity solenoid diaphragm Accelerometer, strain gauge, etc.

 Dielectric constant, conductivity Metal electrode Metal electrode Dynamic elastic modulus Solenoid diaphragm Strain gauge

 (First and second members)

 In the present invention, the first and second members constituting the characteristic measuring instrument can hold a sample to be measured (at least for a time required for characteristic measurement) between them. The shape, material, size, and the like of the first and second members are not particularly limited as long as possible.

 At least one of the first and second members is movable. Such a movable mode (for example, rotational movement, parallel movement), a mechanism (for example, manual operation, motor use), and the like are not particularly limited as long as the above-described sample holding is possible. However, in the present invention, at least at the time of measuring the property, the property measuring means and the energy applying means are arranged in close proximity to each other and the sample is arranged between the first and second members. On the other hand, it is necessary that the property change in the sample can be measured by the property measuring means in response to the energy application from the energy applying means.

In view of being simple and easy to carry, the characteristic measuring instrument of the present invention is a stapler (so-called stapler) type as shown in FIGS. It is preferable that

 (Position relationship with sample)

 In the present invention, at least at the time of measuring the characteristic, the characteristic measuring means is disposed in contact with or close to the sample. At the time of “contact”, the sample may be appropriately pressurized. Further, the degree of “proximity” of the characteristic measuring means to the sample is not particularly limited as long as a desired characteristic can be measured.

 (Position relation between energy applying means and characteristic measuring means)

 In the present invention, the energy applying means is arranged on the first member, but the characteristic measuring means may be arranged on the first member, or may be arranged on the second member. . Furthermore, when a plurality of characteristic measuring means are used, a part of them may be arranged on the first member, and the remaining characteristic measuring means may be arranged on the second member.

 In the present invention, at least at the time of measuring characteristics, the energy applying means and the characteristic measuring means are arranged close to each other. The degree of the “close proximity” is not particularly limited as long as a desired property can be measured. However, in a mode in which a fine region of a sample can be measured or in a mode in which a characteristic measuring instrument is miniaturized, the degree of “proximity” is preferably as follows.

 (1) An aspect in which the characteristic measuring means is arranged on the second member In this aspect, at the time of measuring the desired characteristic, the sample is sandwiched between the energy applying means and the characteristic measuring means. . That is, in this embodiment, the degree of “proximity” between the energy applying unit and the characteristic measuring unit corresponds to the thickness of the sample (or the desired thickness at the time of pressurization).

(2) Embodiment in which the characteristic measuring means is arranged on the first member In this embodiment, at the time of desired characteristic measurement, the energy applying means and the characteristic measuring means are arranged on the same side with respect to the sample. The Rukoto. sand In other words, in this aspect, the energy applying means and the characteristic measuring means

The degree of "proximity" may be less than lcm, or even between 0.1 and 10 mm (particularly between 0.01 and 0.5 mm), as the distance between the "centers" of these means. preferable.

 (Signal generation / analyzer)

 The signal generation / analyzer of the present invention includes at least a CPU, a memory connected to the CPU, a DZA converter connected to the CPU, and an AZD converter connected to the CPU. In such a signal generator / analyzer, for example, digital data written in advance in the memory is D / A converted to an AC voltage having a predetermined frequency, and the digital data is converted to an A / D converter. A signal obtained by AZD converting an output from an external sensor (for example, as shown in FIG. 8) supplied to the connected external energy applying means and connected to the AZD converter; By multiplying by a periodic function such as a sine wave, a cosine wave, or a rectangular wave having the same or twice the frequency, the output, the in-phase component, and the 90 ° component can be calculated.

By combining the signal generation analyzer of the present invention with the above-described characteristic measuring instrument of the present invention, the operation speed can be further improved. That is, in this case, in the signal generation / analyzer, the numerical data corresponding to the sine curve is held in the memory 1 in advance, the signal corresponding to the numerical data is A-converted, and the heater 14 (for example, FIG. ) Can be applied. In this case, the detection signal from the sensor 15 can be A / D converted, converted to digital data, and compared by the CPU. In this case, the operation speed can be significantly increased by using a gate array connected to the CPU. Further, in this embodiment, when a sine curve is generated, a cosine signal is also generated, so that calculation speed is increased. Can be further improved.

 (Measurement principle in one mode of thermal measurement)

 Hereinafter, the measurement principle of the thermal measurement and the apparatus for the measurement that can be suitably used in the present invention will be described in detail (for such a measurement principle of the thermal measurement, see, for example, Japanese Patent No. 205959). (Please refer to No. 841)

 (Definition of thermal conductivity and thermal diffusivity)

Area A as shown in FIG. 1, the plate-like sample having a thickness d, one side of the sample temperature I \, temperature opposite surface _{Τ 2 (Τ 1> Τ 2} ) steady-state near Rutoki, thickness When the heat quantity Q flows only by one-dimensional heat conduction inside the sample in the direction, this heat quantity Q is expressed by the following equation.

 [Number 1]

Q = λ ■ (Τ, -Τ ₂ ) ■ = λ ■ A ■ The proportionality constant I at this time is defined as thermal conductivity.

 Considering the case where the concentration in the sample is unsteady, if the density of the sample is ρ and the specific heat at constant pressure is C p between the temperature distribution in the sample and the temporal change of temperature, the following heat diffusion equation expressed.

 [Number 2]

The proportional constant at this time is defined as the thermal diffusivity.

 The thermal diffusivity α and the thermal conductivity; L have the relationship shown in the following equation.

[Number 3] (Measurement theory for AC-like thermal change)

 In the present invention, a description will be given of a measurement theory when applying an AC-like thermal change to a sample.

 In other words, when the unsteady heat conduction of the sample is considered in one dimension only in the thickness direction (X-axis direction), the above-mentioned thermal diffusion equation (2) is as follows.

 [Number 4]

 T is τ

 = · (4)

 a t d x, Equation (4) above is solved under the following conditions as shown in FIG.

 (i) The sample temperature changes in alternating current on one side of the sample to be measured.

 X = 0, T = T. -c o s (ω t)

 (i i) Temperature waves diffuse infinitely.

 (ii) The sample to be measured is thermally thick as shown in the following formula.

[Number 5]

2 or

d>

 At this time, the solution is expressed by the following equation.

 [Number 6]

 ω ω

T (x, t) = Τ ₀ ■ e X ρ ■ xcos ω · t-one. ■ x (5)

2 ■ a 2 ■ a where ω is the angular velocity of the modulation frequency, and if the modulation frequency is f, it is expressed as ω = 2 · π.f. In equation (5), the term of exp is the temperature amplification at distance X, and the term of cos is the phase at X. Therefore, the change of the temperature with time in the sample thickness d is expressed by the following equation. [Number 7]

 ω

T (d, t) = T ₀ ■ e χ ρ dcos ω d (6)

 2-2 ■ Focusing only on the temperature phase difference, the phase difference Δ 0 is the phase difference between the x = 0 plane and the X = d plane.

 [Equation 8] ω

 Δ Θ = (7)

 2 ■ 4

 [Number 9]

7Γ

 Δ Θ = (8)

 a 4 is represented. Figures 3 (a) and (b) show schematic diagrams of the data. From the above equation (8), for a sample with a known thickness d, one surface is heated in an alternating current by changing the modulation frequency f, and the phase delay Δ ø of the temperature change on the back surface at that time is measured. And the thermal diffusivity α can be determined. As described above, in the measurement in which an AC-like temperature change is applied to the sample, the thermal diffusivity is obtained from the phase difference of the temperature change between the heated surface and the back surface of the sample. High-precision measurement is possible.

 (Thermal diffusion length)

 Under the condition of "thermally thick"

 [Number 1 0]

Is called thermal diffusion length because it has a dimension of length, and is one of the important parameters in this measurement method. The relationship between the sample thickness d and the thermal diffusion length μ is as shown in Figs. 4 (a) and (b). d> μ: Thermally thick

 dgu μ: Defined as thermally thin. Since the thermal diffusion length is the wavelength of the temperature change, if it is larger than the thickness of the sample, that is, if it is thermally thin, the entire sample will undergo temperature fluctuations in the same cycle. In this case, the phase difference of the temperature fluctuation between the front surface and the back surface of the sample approaches 0, and the thermal diffusivity cannot be obtained from the equation (8). Therefore, the “thermally thick” condition required for Eq. (8) to be satisfied means that a temperature wave of at least one wavelength must be present in the sample.

(Method of heating the sample surface)

 In the present invention, a preferred embodiment in which a heat source is provided on a sample surface will be described.

 In such an embodiment, it is preferable that a metal thin film is prepared by sputtering a metal such as gold (Au) on a sample, and the thin metal film is used as an AC heater. In such an AC heater, for example, an AC current modulated by a function / synthesizer is supplied, and an AC-like temperature wave is generated in the sample by Joule heat at that time. Since the Joule heat is maximum at the peak value of the current regardless of whether the current is positive or negative, the cycle of the temperature change at this time is twice the alternating current as shown in equation (10).

 [Number 1 1]

V = V. 'c os cy' t): l = l. -c o s (co 't) (9)

P = I ² · R

= 1 ₀ ² ■ R ■ cos ² (cu 't)

= (l ₀ ² ■ R / 2) ■ (1 + cos (2 ■ ω ■ t)) (1 0) where V is voltage, I is current, and P is heat generation. Therefore, the actual heating frequency is twice as high as the applied modulation frequency. this According to the method, the heat capacity of the AC heater is negligibly small compared to the probe and the measurement sample, and the response can follow the AC quickly.

 The method of measuring the temperature change on the back surface of the sample depends on the change in resistance of the thin film resistance due to the temperature wave, the change in resistance of the thermistor, and the like.

 The temperature sensor circuit incorporates a bridge circuit and a preamplifier, so that only the AC component of the probe resistance can be extracted as a voltage change. This signal is A / D converted to allow for further computer processing.

 The amplitude of the temperature wave depends on the sputtering conditions, the temperature dependence of the resistance value of the temperature sensor, the amount of electricity, etc., but it should be deducted as the device constant by previously measuring the blank and measuring with a standard material. Can be done.

 (Basic system configuration)

 An example of a basic system configuration (the measuring apparatus of the present invention) that can be suitably used for the measuring method of the present invention is shown in the block diagram of FIG. Circuits as shown in the block diagram of FIG. 11 are connected to the ports a to g in FIG. 10, respectively.

 This system consists of a heat source having a DA conversion function and an amplification function for heating the sample with AC, a bypass circuit for detecting the temperature change on the back surface of the sample, and a pre-conditioner for converting the resistance change to voltage. , A preamplifier, an AD converter, software with a Fourier function to extract a specific frequency component of temperature change on the back of the sample, an IC for calculation, a CPU for generating functions, It consists of a sample holder for crimping or holding a sample, a sample thickness measurement system, and a display element. It can be connected to a personal computer via USB if necessary.

(Circuit configuration) FIG. 12 shows an example of a circuit diagram that can be suitably used in the present invention. The circuit diagrams of FIGS. 13 to 16 are enlarged views of each part of the circuit diagram of FIG. Tables 1 to 6 below show examples of circuits, components, and elements that can be used for the circuits shown in Figs. For example, the following a-i

Corresponds to 1.

 a Basic sine wave or square wave waveform output wave height data table, plus or minus waveform data, output wave height data shifted by 90 ° phase About 200,000 points

 b Specifying the interval for reading the waveform data from Table a, frequency control c Specifying the value to multiply the waveform data read from Table a, and controlling the waveform amplitude

 d Performs the sum of products of the sensor signal acquired via the AZD converter and the sine component waveform data of twice the frequency of the waveform memory (after inversion and non-inversion depending on whether the DZA output is positive or negative). Integration is performed every 100 000 times at intervals of 100 ms for 0.1 s, and is used as the basic integrated value of the signature.

 e The product sum of the sensor signal acquired via the AZD converter and the cosine component waveform data of 1 or 2 times the frequency of the waveform memory (after inversion and non-inversion depending on whether the D / A output is positive or negative) Do. The integration is performed every 100 000 times at intervals of 100 ms for 0.1 s, and is used as the basic integration value of cosine.

 f The AZD conversion value of the sample thickness data obtained from the thickness measurement unit g Gives the integration time (number of integrations) to obtain the basic integrated value. Usually 0.1 seconds or 1 wave longer.

 h Measurement section heater output (analog value)

i Measurement section Sensor signal (analog value) [table 1 ]

1 A / D converter for thickness gauge

 2 A / D converter for sensor

3 D / A converter not used

 4 D / A converter 1 Heater signal 5 Flash memory for reference storage

6 CPU

 7 FPGA

 8 To LCD panel

 9 amplifier

 10 amplifier

 ® Waveform memory

 ① Thickness gauge input

 ® Heater output

①Sensor input

part No. Date Code Manf No order numb destination LOT Code

7802 48 025F

 7803

 7804 48M04F

 7805

 7805

 7905 79L05 / A 617 / JRC

 BUZZ

 C1 CAP 18PF 50V CERM 018PF PCC180CNCT-ND ECJ-2VC1H180J MR-1728 39040038

C2 CAP 18PF 50V CERM 018PF PCC180CNCT-ND ECJ-2VC1H180J R-1728 39040038

C3 1 .F

 C4 10 F Large capacity layer ceramic capacitor

 C5 1 JULF

 C6 I OJ F Large capacitance ceramic capacitor

 C7 10 F Large capacity layer ceramic capacitor

 C9 10jUF Large capacitance ceramic capacitor

 C10 10 F Large capacity layer ceramic capacitor

 C11 10 / zF Large capacitance ceramic capacitor

 C13 CAP CERAMIC 1000PF 100PF 311-1122-1-ND 0305CG102J9B200 MX-7433

C14 1 F

C19 1 F

C20

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 C38 10 F Large capacitance ceramic capacitor

 C39 10 F Large capacitance ceramic capacitor

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 C43 CY55Y5UIE CY55Y5U1017-100 zF Super large capacitance ceramic capacitor

 C44 CY55Y5U1E CY55Y5U1W7-100; uF ultra large capacity layer ceramic capacitor

 C45 10 zF Large capacitance ceramic capacitor

 C46 1 / F

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R18 RES 100 OHM 1/1 OW 1 1000 P100CCT-N100Q ERJ-6ENF1000V MQ-160 3092556706

R19 RES 100 OHM 1/1 OW 1 1000 P100CCT-N100Q ERJ-6ENF1000V MQ-160 3092556706

R20 RES 10.0KOHM 1 / 8W 1002 311-10.0K 10ΚΩ 9C08052A1002FKHFTMP-1930

 R21 220

 R22 RES 10.0KOHM 1 / 8W 1002 311-10.0K 10ΚΩ 9C08052A1002FKHFTMP-1930

 R23 RES 10.0KOHM 1 / 8W 1002 31 -10.0Κ 10ΚΩ 9C08052A1002FKHFT P-1930

 R24 RES 10.0KOHM 1 / 8W 1002 311-10.0K 10ΚΩ 9C08052A1002FKHFTMP-1930

 R25 RES 10.0KOH 1 / 8W 1002 311-10.0K 10ΚΩ 9C08052A1002FKHFTMP-1930

 R26 RES 10.0KOHM 1 / 8W 1002 311-10.0K 10ΚΩ 9C08052A1002FKHFTMP-1930

 R27 RES 10.0KOHM 1 / 8W 1002 311-10.0K 10ΚΩ 9C08052A1002FKHFTMP-1930

 R28 RES 82 OHM 1 / 10W5 ° / c82R 311-82GCT82Q 9C06031A82R0JLHFT MS-2423

 R29 RES 82 OHM 1/1 OW 5% 82R 311-82GCT82Q 9C06031A82R0J and HFT MS-2423

 R30 RES 82 OHM 1 门 0W5 ° / c82R 311-82GCT82Q 9C06031A82R0JLHFT MS-2423

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 R33 RES 82 OHM 1 / 10W5 ° / d32R 311-82GCT82Q 9C06031A82R0J HFT MS-2423

 R34 RES 82 OHM 1 / 10W5% 82R 311-82GCT82Q 9C06031A82R0J HFT MS-2423

 R35 RES 82 OHM 1/1 OW 5% 32R 311-82GCT82Q 9C06031A82R0J HFT MS-2423

 R36 RES 82 OHM 1 / 10W5 ° / cS2R 311-82GCT82Q 9C06031A82R0J HFT MS-2423

 R37 RES 82 OHM 1 / 10W5 ° / c82R 311-82GCT82Q 9C06031A82R0JLHFT MS-2423

 R38 RES 82 OHM 1 / 10W5% 82R 311-82GCT82D 9C06031A82R0JLHFT MS-2423

 R39 RES 82 OHM 1/1 OW 5% B2R 311-82GCT82D 9C06031A82R0JLHFT MS-2423

 SW1 Switch tact spst 12mm mom extend EG1024-ND Dec.02 TL1100FF160Q

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 U7 OP177 / G 0 Analog devices

 U9 TI1C / A E IC SERIAL AOC LP CMO TLC4545IDGK 296-12746-5-ND NF-2721

 U 10 TI G / AME IC SERIAL AOC LP CMO TLC4545IDGK 296-12746-5-ND NF-2721

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 U12 D01 / 3827 IC D / A CONV LP 16-BITDAC8501 E / 250 12867229 Z-5655

 U13 D 01/3827 IC D / A CONV LP 16-B1TDAC8501 E / 250 12867229 LZ-5655

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 U16 93C46B / I / SN0343 / 38E

U17 1 Α ^Λ F Transistor GP NPN AMP MBT3904FSCT-ND BT390412867229 LQ-2022

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 U20 CY7C1049 IC SRAM 512KX83.3V CY7C1049CV33-20VC 428-1488-5-ND LF-3172

 U21 XC18V01 IC PROM SERIAL CONRG C18V01 S020C 122-1237-12867229 JN-1964

 VR CW-2

 XC2S-144 XC2S50T IC FPGA 2.5V 384 CLB 122-1225-N D XC2S50-5TNJ-975

 XTAL BB99 / 16.000M Crystal 16.000 MHZSMD 18PF 12867229 JA-1930 796268

06 (Example of measurement conditions)

 In the system configuration of the present invention (for example, the one shown in FIG. 8), examples of conditions that can be suitably used are as follows.

 (i) Sample size: 1 mm square or more with no limit

 , Ι 1) Thickness: 1 μ πι ~ 10 mm

 In the embodiment of the present invention for measuring thermal conductivity, the conductive material that can be suitably used for the AC heat source is not particularly limited as long as it generates heat by Joule heat when an electric current flows. Examples of such conductive materials include, for example, gold, silver, platinum, copper, iron, zinc, antimony, iridium, chromenole, constantan, nickel, aluminum, chrome, nickel , Carbon, thermistor, thermocouple, etc. (sample)

 There is no particular limitation as long as the measurement of its properties (eg, thermal properties) is a useful sample. Examples of such samples include, for example, polymer compounds, rubber, organic dyes, ores, glass, ceramics, metal plates, aqueous solutions, greases, oils, gases, plant cells, animal cells, and various types of Industrial products, thermal insulation paper, foamed polymer materials, highly molecularly oriented polymer films, multilayer films, spin-coated thin films, cast films, vapor-deposited films, fabrics, composite materials, as well as banknotes, telephone cards, and plant materials Leaves.

The sample to be measured suitable in the thermal measurement mode of the present invention may be of any size as long as the measurement of its thermal characteristics is useful, but it is as flat as a temperature sensor (temperature probe). It is desirable to have a part. Even a conductive or liquid substance such as a metal plate can be measured by attaching a thin insulating film to the tip of the probe. The measurement area depends on the size of the temperature probe used, etc. Usually, the size of the region to be formed is preferably about 5 mm × 5 mm, more preferably about 1 mm × 1 mm. There is no limit on the temperature probe size, as long as measurement is possible.

 In the present invention, the magnitude and waveform of the temperature change to be given to at least a part of the sample to be measured are not particularly limited. That is, the input amplitude may be such that the sample is not damaged, and the waveform may be a sine wave or at least a temporal change that can be given to the sample.

 (Example of data processing means)

 A signal amplification and calculation device is built in the device, and the signal received by the sensor on the probe is received by the bridge circuit, and after AD conversion, it can be digitally subjected to Fourier transformation or mouth-in amplification. Is desirable. The analysis needs to know the signal amplification, noise rejection, phase lag and amplitude attenuation from the surface, and its relationship to the frequency of the given temperature wave.

 (One aspect of the measurement method)

 An example of a measurement method (algorithm) usable in the present invention is shown in the flowchart of FIG. In Fig. 17, a ~! ! The operation indicated by is the operation corresponding to the circuits a to h shown in FIGS. 10 and 11.

 Detailed examples of the calculation of the slope and intercept in FIG. 17 are shown in FIGS. Figures 21 to 24 are examples of displays at each stage of the actual measurement.

 (Details of device configuration)

 Details of the configuration in FIG. 8 are described below.

(1) Heater section 14 The tip of the arm is the sensor section.To prevent rattling when the sample is sandwiched, when a constant load is applied, the sensor surface It adopts a method to ensure its behavior. It is desirable that the change width of the temperature wave be about 1 ° C. or less, preferably 1 ° C. or less, and more preferably 0.5 ° C. or less.

 (2) Temperature wave sensor 15 A sensor with the same lmm square size is attached to the opposite electrode of the heater. Temperature waves that have diffused through the sample are significantly attenuated, which requires a highly sensitive temperature sensor. In this device, it is desirable to use a thin film resistance sensor or thermistor sputtered with nickel. A special resin coat is applied to the surface for insulation and protection of the electrodes.

 (3) Contact of sample When applying pressure, it is preferable to consider the thermal contact between the sample and the sensor when measuring the thermal diffusivity and thermal conductivity. The system in Fig. 8 employs a method in which the contact area is reduced and an appropriate pressure is applied by the load of the arm in order to ensure contact between the sample and the electrode. A special soft resin is coated on the surface to improve adhesion even with hard samples. The contribution of the insulation can be deducted by strict checks (eg, based on Figures 18-20).

 (One mode of analysis device)

 As shown in FIGS. 10 and 11, such an analyzer includes a frequency amplifier section and an analysis software section. Such analyzers are located in the center of the Field Processor Gate Array (Xilinx, etc.) in the waveform processor and the CPU that performs calculations. Main memory, external AC output circuit DA converter, signal input circuit AD converter, thickness gauge analysis Circuit.

This analyzer can be connected to an external personal computer via an interface such as USB, and can control the captured data and save the captured data. The block diagrams are shown in Figures 10 and 11. The basic sine waveform and cosine wave delayed by 90 ° are written in the memory as table data in advance. This signal is then received from the output amplitude control register to generate a continuous digital signal waveform with a constant frequency and amplitude. This is an output to the sample section for AC heating through a DZA converter and an analog amplifier.The data from the temperature sensor returned from the sample section is prepared by the preamplifier, then A / D converted, and the waveform Compare with internal output from memory. Since the temperature change is twice the frequency of the heater, sine and cosine waves of twice the frequency of the output to the heater are multiplied for a certain period of time and integrated to obtain a time average.

In other words, based on the generated temperature wave (input side, heater side), the signal on the back side and the sensor side is the intensity phase delay an- ¹

(sin / cos), the amplitude A is determined by the root mean square of the sine component and the cos component.

 (One embodiment of the frequency amplifier unit)

 This frequency amplifier device portion includes a control portion and a sample portion, and includes, for example, a CPU + waveform processor (constituted by FPGA) + memory + AZD, D / A.

 The CPU is responsible for power-on waveform synthesis, switch reading, liquid crystal display, and RS232C communication. The waveform processor and sum-of-products calculation are handled by the waveform processor.

During operation, the CPU synthesizes an arbitrary waveform and writes it to flash memory or the like. After that, the memory is disconnected from the CPU and connected to a waveform processor (such as a Field Programmable Gate Array FPA: sparta n2 XC2S100 from XI inx). In the memory, for example, in addition to the peak value, a bit (Cos-bit) indicating the sign of the waveform and a bit (sin-bit) whose phase is shifted by 90 degrees are also written. The waveform processor reads the peak value data from memory at 100 k times Z second and sends it to the DZA converter, while the waveform processor, for example, reads the sensor data via the A / D converter at 100 k times / second. Capture the signal. If the sin-bit of the D / A output is positive, the signal is inverted as it is, and if negative, the acquired signal is inverted and added to the sine component integrated value. Similarly, add to the cosine component integrated value using cos_bit.

 An interrupt is issued to CPU every 100 000 times (at 100 ms intervals) for the sine and cosine components. The CPU further integrates this value an appropriate number of times, and uses it as a basic integrated value for each of the sine and cosine. The phase difference is obtained from the value obtained by further integrating this basic integrated value for one measurement frequency. In this case, the basic integration value is set to 0.1 second intervals in order to reduce the influence of power supply hum by making an integral multiple of the wave enter at either 50 Hz or 60 Hz. is there. Therefore, the minimum time required for measurement in this case is the longer of one wave of the measurement cycle or 0.1 second.

 The memory can store, for example, output crest data for 2 seconds (200,000 points). Normally, it is sufficient to insert sine wave data that is one cycle in two seconds (the waveform depends on the program).

 The measurement frequency can be changed by appropriately changing the reading interval from the memory.

 (One mode of sample measurement)

One embodiment of the measurement method using the system of FIG. 8 will be described below. First, the sample 13 is inserted into the predetermined position in FIG. 8 (between the heater 14 and the sensor 15), and the same measurement as described above is performed. First, the thickness of the sample 13 is measured with the iron core 16 and the transformer 17. In this measurement algorithm, for example, the physical property value of the standard polymer and the measurement conditions (which can be specialized for other substances) are stored in memory, and the initial application is performed based on the measured thickness. Frequency and voltage can be determined.Frequency scan before and after this, if the signal intensity is too much or less than that of the standard sample, increase or decrease the amplitude of the AC temperature wave according to the difference from the standard, and rescan the frequency Let. Calculate the correlation coefficient at three or more points, and if it deviates significantly from the straight line, change the frequency band to be measured again and perform the measurement again.

 Subtract the blank from the straight line obtained by the above frequency scan. Next, two phase points of this value (for example, 180 ° and 270 °) are determined, and the frequencies at which these values are obtained are determined. From this, the slope of the straight line is calculated to calculate the thermal diffusivity. Calculate the thermal conductivity from the amplitude.

 (One form of thermal diffusivity · thermal conductivity conversion program)

 Amplitude change can be converted to thermal conductivity by comparing it with the attenuation of a standard material whose thermal conductivity and thermal diffusivity are known. In this case, for example, standard sample data, substrate thermal data, instrument correction factors, and measurement analysis programs can be written to main memory. With these values and the values taken in, the thermal diffusivity and then the thermal conductivity are calculated.

(Connection with computer)

The above-described characteristic measuring instrument of the present invention can be used alone as an analysis lock-in system for the purpose of measuring thermal diffusivity and thermal conductivity with a small and light-weight, on-site measuring device. In other words, the function of the function generator for heat generation, amplification at the same frequency as the given frequency It has a lock-in amplifier function, a thickness measurement function, an applied pressure control function, etc., and calculates these values and converts them into thermal diffusivity and thermal conductivity while considering the thickness and thermal conductivity of the sample. And a device that can display the results or transport the results to an external personal computer.

 (1) Normal mode: Sends the measurement status, measurement frequency, calculated phase, and amplitude in text format. This can be transferred to another personal computer at the same time as it is sent to the display.

 (2) Slave mode: The slave mode is entered when a predetermined command is received via the 232C. In addition to remote operation, frequency specification, waveform selection, etc. are possible (depending on the program). If a Windows program is prepared at the connection destination, it can be driven and analyzed even with that software.

(One mode of thickness measurement)

A 16-bit A / D connected to a different CPU from the above can be prepared for signal input from the thickness gauge, and the thickness can be measured sequentially. Thickness sensors can use differential transducers, strain gauges, dielectric constant measurement elements, etc., but conversion to thickness, correction values, etc. can be written to the flash memory and called up as needed. If the conversion factor to ₀ or the thickness changes, it can be rewritten via the CPU. The data acquisition speed can be as low as 100 Q times the sample for about Z seconds. For example, if a time constant of 1 second or more is inserted to avoid power hum, it is difficult to acquire a high-speed signal.

 Hereinafter, the present invention will be described more specifically with reference to examples.

 [Example]

 Example 1

Using the apparatus shown in FIGS. 8 to 9, the thermal characteristics of borosilicate glass (Matsunami Micro Cover Glas) were measured under the following conditions. Frequency: 22 to 100 Hz, Heater input: 2 V, 1 Hz step, Heater resistance: 50 Ω, Sensor resistance: 2 kΩ, Phase and amplitude measured at integration time of 1 second (Η = 100).

Thermal diffusivity: 3. 2 2 X 1 0 - 7 m 2 /

 Standard deviation: 0.0 7 3 6 7

 X 1 0 1

: 0.0 0 7 4

 Thickness: 1 4 5.3 m

 Standard deviation: 0.2 6 3 7

 τπ Ρϊτ ^ τ: 0.0 2 6 3

 The measured data is shown in the graph of Fig. 25.

Example 2

 The thermal characteristics of the PMMA film (Sumitomo Chemical, Technology # 125) were measured under the following conditions using the equipment shown in Figs.

Frequency: 20 to 48 Hz, heater input: 2 V, frequency scan in 0.5 Hz step, heater resistance: 50 Ω, sensor resistance: 2 kΩ, integration time 1 second, It was measured phase and amplitude (n = 2 0) thermal diffusivity: 0. 9 1 1 X 1 0 - 7 m 2

 Standard deviation: 0.03 0 8

 Standard error: 0.0 0 6 7 2

 Thickness: 1 2 1.3 β m

 Standard deviation: 0.4 1 3

 Standard error: 0.09 0 2

 The measured data is shown in the graph of Figure 26.

Example 3

 Using the equipment shown in Figs. 8 and 9 under the following conditions,

(Toray, kapton 100H) was measured for thermal properties. Frequency: 20 to 48 Hz, one heater input: 2 V, frequency scan in 0.5 Hz step, heater resistance: 50 Ω, sensor resistance: 2 kΩ, integration time 1 second, Phase and amplitude were measured (η = 20) Thermal diffusivity: 1-0 2 X 10

 Standard deviation: 0-0 4 9 6

 Standard error: 0-0 1 1 0 9

 Thickness: 1 23.6 βm

 standard deviation :

 Standard error:

 The measured data is shown in the graph of Figure 27.

Example 4

 The thermal characteristics of the PET film (Toray, Lumilar S10) were measured using the equipment shown in Figs.

 Frequency: 20 to 48 Hz, heater input: 2 V, frequency scan in 0.5 Hz step, heater resistance: 50 Ω, sensor resistance: 2 kΩ, integration time 1 second, Phase and amplitude were measured (n = 20) Thermal diffusivity: 0.919 X

 Standard deviation: 0.0 4 5 6

 Standard error: 0.0 0 9 9

 Thickness: 1 23.7 β m

 Standard deviation: 0-5 5 5

 Standard error: 0.12 1

 The measured data is shown in the graph of Fig. 28.

Example 5

The graphs in Figs. 29 to 34 and Table 7 show measurement examples of the following samples. The measurement conditions are as follows: Fig. 29: Toray, kapton-1

 Figure 30: Function, kapton—2

 Figure 31: Cano-glass

 Figure 32: PMMA

 Figure 33: Bundle, K ap t on — 3

 Figure 34:: Toray, K ap t on — 4

[Table 7] a = DxiO " ⁷ m ² · sec

 Cover glass 3 ； ''-,, α '■

153.9 3.58

153.5 3.59

 153.5 3.35

153.2 3.47

153.1 3.51

153.1 3.55

153.0 3.83

153.0 3.61 Mean, 153.3 3.6 Standard deviation '0.3 01 Measurement conditions>

 Table 7: Thousand-yen bill, 10,000-yen bill, one-dollar bill, power par glass 1, 2, 3, JR commuter pass, passnet power card, Shinseido card, business card 1, 2, 3, 4, BicCamera receipt Thermal paper

Auto mode measurement using the algorithm shown in Fig. 17, etc. Frequency range Approx. 10 to 300 Hz, AC applied voltage 2-4 V _pp

Claims

1. a first member having energy applying means at least in part thereof;

 A characteristic measuring instrument having at least a second member disposed to face the first member;

 Blue

 At least one of the first and second members is movable between the first and second members so as to hold a sample,

 A characteristic measuring means is arranged on at least one of the first and second members, and at least at the time of measuring the characteristic, the characteristic measuring means and the energy applying means are arranged close to each other. And a characteristic change in the sample is measured by the characteristic measuring means in response to energy application from the energy applying means to the sample arranged between the first and second members. A characteristic measuring instrument characterized by being measurable.

 2. The characteristic measuring instrument according to claim 1, wherein the characteristic measuring means is arranged in at least a part of the second member.

 3. The characteristic measuring instrument according to claim 1, wherein the characteristic measuring means is arranged at least in a part of the first member.

 4. The characteristic measuring instrument according to any one of claims 1 to 3, wherein the characteristic is a physical characteristic.

 5. The property measuring instrument according to claim 4, wherein the property is a thermal property.

6. The property measuring instrument according to claim 4, wherein the physical property is a mechanical property.

7. The property is measured in a state where at least one of the energy applying means and the property measuring means is in contact with the sample. 7. The property measuring instrument according to any one of claims 6 to 6.

 8. The property measuring instrument according to any one of claims 1 to 7, wherein a thickness measuring means for measuring a thickness of the sample is arranged on at least one of the first and second members. .

 9. The property measuring instrument according to claim 5, wherein periodic joule heat is applied to the sample from the energy applying means, and a temperature wave generated in the sample is thereby measured by the property measuring means. .

 10. The characteristic measuring instrument according to any one of claims 1 to 9, wherein a displacement meter is disposed on the first and Z or second members, and the thickness of the sample can be monitored sequentially.

 11. The characteristic measuring device according to any one of claims 1 to 10, wherein an applied pressure applied to the sample disposed between the first and second members is variable.

 12. The characteristic measuring means has two or more types of sensors selected from temperature, humidity, and pressure sensors, and applies energy to the sample from the energy applying means in an alternating manner. The characteristic measuring instrument according to any one of claims 1 to 11, wherein a plurality of physical properties based on the characteristic can be measured.

 13. Energy is applied to the sample from the energy applying means, and the characteristic based on the energy application is obtained by the characteristic measuring means arranged close to or in contact with the sample and arranged close to the energy applying means. A characteristic measuring method characterized by measuring a change.

 14. The characteristic measuring method according to claim 13, wherein the energy is heat energy.

 15. The characteristic measuring method according to claim 13 or 14, wherein the thickness of the sample is also measured when the characteristic is measured.

16. Based on the data of the standard sample corresponding to the thickness of the sample, 16. The characteristic measuring method according to claim 15, wherein a frequency at which the energy is applied is determined at the time of measuring the sample.

 17. The characteristic measuring method according to claim 16, wherein a frequency at the time of applying the energy is scanned based on a comparison with the standard sample data.

 18. The characteristic measuring method according to claim 17, wherein an optimal value of the frequency at the time of applying the energy is obtained by the scanning.

 1 9. C PU and

 A memory connected to the CPU;

 A DZA converter connected to the CPU;

 A signal generating Z analyzer including at least an A / D converter connected to the CPU;

 The memory has a large-capacity digital data table corresponding to a periodic change of a sine wave, a cosine wave, a variable-duty rectangular wave, a triangular wave, or the like written in advance in the memory. A signal analyzer that has an algorithm that can arbitrarily change the frequency by changing it, and an algorithm that can change the amplitude of the A output and feed pack the measurement signal to control the output intensity.

20. By multiplying a signal obtained by AZD-converting the output from the external sensor connected to the A / D converter with a sine wave having the frequency of the applied AC voltage or twice the frequency. 10. The signal generation analyzer according to claim 19, wherein the output and the in-phase component can be calculated.

2 1. A signal obtained by AZD converting the output from an external sensor connected to the AZD converter, and a sine wave, cosine wave or square wave having a frequency twice as high as the AC voltage, and 90 °. 21. The signal generation according to claim 20, wherein the output, the in-phase component, and the 90 ° component can be calculated by multiplying each of the phase-shifted rectangular waves. 'Analyzer,