JP2012032196A - Thermal conduction measuring apparatus and thermal conduction measuring method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a thermal conduction measuring apparatus and a thermal conduction measuring method capable of detecting installation abnormality of a measuring object.SOLUTION: The measuring object is gripped by a heating side gripping member thermally connected to a heating source and having an end face and a cooling side gripping member thermally connected to a cooling source and having an end face. In the gripped state, the heating side gripping member is heated by the heating source and the cooling side gripping member is cooled by the cooling source to allow heat to flow from the heating side gripping member to the cooling side gripping member. In the state, at least either one of temperature dispersion in a face direction parallel with the end face of the heating side gripping member and temperature dispersion in a face direction parallel with the end face of the cooling side gripping member is measured, and the installation abnormality of the measuring object is detected based on the measured temperature dispersion.

Description

  The present invention relates to a heat conduction measuring device and a heat conduction measuring method.

  Conventionally, various apparatuses are known as an apparatus for measuring a thermophysical value of a measurement object such as a resin material by a steady method (see Patent Documents 1 and 2). For example, as shown in FIG. 7, the apparatus described in Patent Document 1 has a layered structure in which a measurement object 100 is sandwiched between a pair of members (clamping members) 101 and 102, and the layered structure 103 is an upper rod. It is configured to be sandwiched between 104 and the lower rod 105.

  The upper rod 104 is connected to a heat source (not shown) and configured to be able to measure temperature at a plurality of locations in the longitudinal direction. The lower rod 105 is connected to a cooling device (not shown). In addition, the temperature can be measured at a plurality of locations in the longitudinal direction. Then, heat is applied from the upper rod 104 to the lower rod 105 while a load is applied to the layered structure 103 by the upper rod 104 and the lower rod 105, and the temperature is measured at a plurality of locations of the upper rod 104 and the lower rod 105. The thermal resistance of the layered structure 103 is measured, and the thermophysical property value of the measurement object 100 is obtained based on this.

Japanese Patent No. 3858660 JP 2008-309729 A

  In the apparatus of Patent Document 1, when measuring the thermophysical value of the measurement object 100, heat is passed from the upper rod 104 to the lower rod 105 in a state where the measurement object 100 is sandwiched with the pair of clamping members 101 and 102. In order to ensure measurement accuracy, it is necessary to flow heat from the upper rod 104 to the lower rod 105 so that the heat flow is not biased. In the apparatus described above, the measuring object 100 is placed in a normal state between the upper and lower rods 104, 105, that is, the upper rod 104, the measuring object 100, and the lower rod 105 are arranged in a straight line along the direction of heat flow. (See FIG. 3 (a)), the heat flows from the upper rod 104 to the lower rod 105 without the heat flow being biased.

  Therefore, when the measuring object 100 is installed, for example, the upper rod 104 and / or the lower rod 105 are tilted (see FIGS. 3B and 3E) or the thickness of the measuring object 100 is measured. When an installation abnormality occurs such as a state in which the dimensions are not uniform (see FIG. 3C) or a state in which the measurement object 100 is displaced laterally from a predetermined installation position (see FIG. 3D), the upper rod 104 The heat flow from the first to the lower rod 105 is biased, and the thermophysical property value of the measurement object 100 cannot be measured accurately.

  In addition, since the above apparatus cannot detect this installation abnormality, for example, even when the thickness of the measurement object 100 is not uniform, the thermophysical property value cannot be measured accurately.

  On the other hand, in Patent Document 2, the thickness dimension of the measuring object 100 is measured at a plurality of locations using a plurality of sensors to obtain an average value, and this average value is simulated as the thickness dimension of the measuring object 100. An apparatus for calculating thermophysical property values is disclosed (see Patent Document 2).

  However, even this apparatus cannot deal with an installation abnormality such as a lateral displacement of the measurement object 100. In addition, the obtained thermophysical property value may include an error caused by imitating the average value as the thickness dimension of the measurement object. Therefore, even with the apparatus of Patent Document 2, the thermophysical property value may not be accurately measured.

  Therefore, it is an object to provide a heat conduction measuring device and a heat conduction measuring method capable of detecting an installation abnormality of a measurement object.

  Therefore, in order to solve the above-mentioned problem, the present invention is a heat conduction measuring device used in a one-way heat flow steady comparison method, and is thermally connected to a heating source and contacts one surface of a measurement object. A heating-side clamping member having an end surface, and a cooling-side clamping member that has an end surface that is thermally connected to a cooling source and contacts the other surface of the measurement object, and sandwiches the measurement object together with the heating-side clamping member A temperature measuring unit for measuring at least one of a temperature variation in a plane direction parallel to the end surface of the heating-side clamping member and a temperature variation in a plane direction parallel to the end surface of the cooling-side clamping member; and the temperature And an abnormality detection unit that detects an installation abnormality of the measurement object based on variations in temperature measured by the measurement unit.

  In the present invention, by detecting the deviation of the heat flow from the heating side clamping member to the cooling side clamping member based on the installation abnormality of the measurement object as a temperature variation in the plane direction parallel to the end face of each clamping member, It is possible to detect an installation error of the measurement object. Thereby, the installation abnormality can be eliminated by re-installing the measurement object, and the thermophysical property value of the measurement object can be accurately obtained. In the present invention, the abnormal installation of the measurement object refers to a state where the central axes of the heating-side clamping member, the measurement object, and the cooling-side clamping member are not located on a common straight line, for example, any clamping member Or the center axis of one of the clamping members is displaced from the center axis of the other clamping member (see FIG. 3B). 3 (d)), or the thickness dimension (dimension in the clamping direction) of the measurement object is not uniform (see FIG. 3 (c)).

  In the heat conduction measuring device according to the present invention, the temperature measuring section has a temperature measuring end, and the temperature measuring end is a surface parallel to the end face of at least one of the heating side holding member and the cooling side holding member. It is preferable to be arranged at a plurality of locations in the direction.

  In this aspect, the configuration of the temperature measurement unit can be further simplified as compared with the configuration in which the temperature variation in the entire surface direction parallel to the end surface of each clamping member is measured.

  The heat conduction measuring device may further include an interval measuring unit that measures an interval between the heating-side holding member and the cooling-side holding member in a state where the measurement object is interposed.

  In this aspect, the thickness dimension of the measurement object can be obtained based on the measured interval between the clamping members. At this time, the heat conduction measuring device can detect the installation abnormality of the measurement object, and therefore the installation abnormality can be eliminated when the installation abnormality is detected. Therefore, the thickness dimension of the measurement object can be obtained with high accuracy by measuring the distance between the end faces of the heating side clamping member and the cooling side clamping member at only one point.

  Further, in order to solve the above-mentioned problem, the present invention is a method for measuring a physical property value related to the heat conduction of a measurement object, wherein the measurement object is thermally connected to a heating source and one of the measurement objects. A sandwiching step of sandwiching the measurement object by a heating-side sandwiching member having an end surface contacting the surface and a cooling-side sandwiching member thermally connected to the cooling source and having an end surface contacting the other surface of the measurement object; The heating side clamping member is heated by the heating source in a state where the measurement object is sandwiched, and the cooling side clamping member is cooled by the cooling source, whereby heat is applied from the heating side clamping member to the cooling side clamping member. In the state of flowing heat in the heat flow step and in the state of flowing heat in the heat flow step, the temperature variation in the surface direction parallel to the end face of the heating side holding portion and the end face of the cooling side holding member are parallel to the end face. Comprising a temperature measuring step of measuring the variation of at least one of the temperature variation in the direction of the temperature, based on temperature variations of said measured, a detection step of detecting an installation abnormality of the measurement object, the.

  In the present invention, by detecting the deviation of the heat flow from the heating side clamping member to the cooling side clamping member based on the installation abnormality of the measurement object as a temperature variation in the plane direction parallel to the end face of each clamping member, It is possible to detect an installation error of the measurement object. Thereby, the installation abnormality can be eliminated by re-installing the measurement object, and the thermophysical property value of the measurement object can be accurately obtained.

  As described above, according to the present invention, it is possible to provide a heat conduction measuring device and a heat conduction measuring method capable of detecting an installation abnormality of a measurement object.

It is a figure showing roughly the whole heat conduction measuring device composition concerning this embodiment. (A) (b) It is a front view when the side surface which mutually opposes a sample block is seen as a front. It is a figure for demonstrating the installation state of a measurement object, Fig.3 (a) shows a normal installation state, and FIG.3 (b)-FIG.3 (e) show an installation abnormality. It is a figure for demonstrating the procedure which detects the bias | inclination of temperature distribution, and the procedure which calculates | requires thermal conductivity. It is a figure for demonstrating the procedure which calculates | requires thermal conductivity. It is a figure for demonstrating the apparatus which measures the thickness dimension of a sample, Fig.6 (a) shows the case where a contact-type displacement sensor is used, and FIG.6 (b) shows the case where a laser displacement meter is used. FIGS. 6C and 6D show the case where an optical position sensor is used. It is a figure which shows roughly the structure of the measurement part in the conventional thermophysical property value measuring apparatus.

  Hereinafter, an embodiment of the present invention will be described with reference to the accompanying drawings.

  As shown in FIG. 1, the heat conduction measurement device 10 according to the present embodiment mainly includes a measurement device main body 12, a measurement control device 14, a recording device 16, and an installation abnormality detection device 17.

  The measurement apparatus main body 12 includes a heating block 21 that is a heating source, an upper joint block 22, an upper rod 23 that is a heating side member, a cartridge 24, a lower rod 25 that is a cooling side member, and a lower joint block 26. A cooling block 27 as a cooling source and a pressure adjusting unit 30 are mainly provided. The measurement unit of the measurement apparatus main body 12 has a configuration in which a cooling block 27, a lower joint block 26, a lower rod 25, a cartridge 24, an upper rod 23, an upper joint block 22 and a heating block 21 are arranged in order from the bottom. Yes. In the present embodiment, the upper rod 23 and the upper sample block 24a of the cartridge 24 are collectively referred to as a heating side clamping member, and the lower rod 25 and the lower sample block 24b of the cartridge 24 are collectively referred to as the cooling side clamping. Sometimes referred to as a member.

  The upper rod 23 and the lower rod 25 have the same configuration. The upper rod 23 and the lower rod 25 are formed in a columnar shape or a quadrangular prism shape. The shapes of the upper rod 23 and the lower rod 25 are not limited to this.

The material of the rods 23 and 25 is copper (JIS C1100), aluminum (JIS).
A1100), aluminum alloy (JIS A5052), nickel (JIS NW2200), stainless steel (SUS304, 306) and the like are preferable.

  The upper rod 23 is connected to the heating block 21 by an upper joint block 22 at its upper end. The upper joint block 22 connects the heating block 21 and the upper rod 23 to each other with the upper rod 23 positioned with respect to the heating block 21. The lower rod 25 is connected to a cooling block 27 by a lower joint block 26 at the lower end thereof. The lower joint block 26 connects the cooling block 27 and the lower rod 25 to each other with the lower rod 25 positioned with respect to the cooling block 27. These joint blocks 22 and 26 are joints made of a material having high thermal conductivity such as copper. That is, the upper rod 23 is thermally coupled to the heating block 21, and the lower rod 25 is thermally coupled to the cooling block 27.

  Between the upper joint block 22 and the upper rod 23, silicon grease 32 (for example, G-747 manufactured by Shin-Etsu Silicon Co., Ltd.) 32 as an intervening layer which is a thermal resistance suppressing material is applied. Also, an electrically insulating silicon grease 33 is applied between the lower joint block 26 and the lower rod 25. By connecting the upper joint block 22 (lower joint block 26) and the upper rod 23 (lower rod 25) via the grease 32 (33), the joint block 22 (26) and the rod 23 (25) are brought into close contact with each other. It can be ensured, thereby preventing a decrease in heat conduction at the interface.

  The heating block 21 and the cooling block 27 are for applying heat transmitted in one direction from the heating block 21 toward the cooling block 27, and each include a Peltier element (not shown). The heating block 21 generates heat by the heat generated by the heat generating part of the Peltier element, and the cooling block 27 is cooled by the heat absorption of the heat absorbing part of the Peltier element.

  The measuring device body 12 is provided with a radiator 35 for absorbing heat from the Peltier elements in the heating block 21 and the cooling block 27. The heat radiator 35 prevents a thermal influence on a load cell 30d described later by the heat absorption side of the Peltier element of the heating block 21 by using it together with a heat insulating material 37 described later.

  The measuring device main body 12 is provided with a pressing force adjusting unit 30 for adjusting the pressing force between the cartridge 24 and the upper and lower rods 23 and 25 and the pressing force applied to the sample W. The pressure adjusting unit 30 includes a support base 30a, a pressing member 30b movable in the vertical direction with respect to the support base 30a, a pressure adjusting screw 30c for pressing the pressing member 30b, and a pressure detecting unit. Load cell 30d and an expansion allowable spring 30f made of a coil spring. The pressing member 30b is disposed so as to be able to press the load cell 30d, and is displaced downward according to the screwing amount of the pressure adjusting screw 30c to press the load cell 30d. Thereby, the pressing force between the cartridge 24 and the upper and lower rods 23 and 25 and the pressing force applied to the sample W are adjusted. The expansion allowing spring 30f is disposed between the pressure adjusting screw 30c and the pressing member 30b, and allows the sample W to expand during measurement by contracting.

  The load cell 30d is disposed on the heating block 21 via a heat insulating material 37. A load corresponding to the screwing amount of the pressure adjusting screw 30c is applied to the load cell 30d, and the load cell 30d outputs a signal corresponding to the load. The signal output from the load cell 30d is input to the measurement control device 14. The load display unit 53 of the measurement control device 14 displays the detection value of the load cell 30d.

  The cartridge 24 is a holding portion that holds a sample W that is a measurement object, and is formed separately from the upper rod 23 and the lower rod 25. The cartridge 24 is sandwiched between the upper rod 23 and the lower rod 25 at the time of measurement, and can be removed therefrom after the measurement. That is, the cartridge 24 can be attached to and detached from the upper rod 23 and the lower rod 25.

  The cartridge 24 includes a pair of upper and lower sample blocks 24a and 24b, and has a configuration in which the sample W is sandwiched between an upper sample block 24a that is a heating-side clamping unit and a lower sample block 24b that is a cooling-side clamping unit. . The total thickness (vertical thickness) of the cartridge 24 is 50 mm or less, more specifically about 2 to 20 mm, and the thickness of the sample W is preferably 0.1 mm to 10 mm. If the thickness of the sample W is within this range, almost all of the heat of the sample blocks 24a and 24b can be transmitted. Therefore, physical property values relating to heat conduction can be obtained without using means such as insulating the periphery of the measuring device main body 12. Can be measured.

  Each sample block 24a, 24b is formed in a cylindrical shape or a quadrangular prism shape. The contact surface with the sample W is adjusted to flatness, surface roughness, and parallelism of 0.01 mm or less.

  The upper sample block 24a and the lower sample block 24b may be fixed by the adhesive force or adhesive force of the sample W itself, or may be fixed by auxiliary means such as an adhesive tape.

  The material of the sample blocks 24a and 24b is preferably copper (JIS C1100), aluminum (JIS A1100), aluminum alloy (JIS A5052), nickel (JIS NW2200) or the like. Furthermore, the surface of the sample blocks 24a and 24b may be subjected to surface treatment close to actual use by electrolytic plating or electroless plating. When the measuring device 10 is configured to measure electrical characteristics, the material of the sample blocks 24a and 24b is preferably copper.

  The cartridge 24 is connected to the upper rod 23 and the lower rod 25 through intervening layers 39 and 40. That is, the intervening layer 39 exists between the upper rod 23 and the upper sample block 24a, and the intervening layer 40 exists between the lower sample block 24b and the lower rod 25. The intervening layers 39 and 40 are a contact thermal resistance reducing material and are made of silicon grease having electrical insulation.

  The sample W is adjusted to a prescribed thickness by dispenser or screen printing and applied to the sample blocks 24a and 24b. That is, in one sample block 24a (24b), the sample W is applied to the inner side surface that is a contact surface with the sample W. Then, the other sample block 24b (24a) is overlaid on the one sample block 24a (24b), whereby the cartridge 24 is produced.

  In the case where the sample W is, for example, a curable resin material, the sample W is hardened by performing a heat treatment in a state adjusted to a specified thickness. In this case, the thickness of the sample W may be adjusted by screen printing or the like, but it is also possible to adjust the gap width between the sample blocks 24a and 24b using a spacer. The spacer may be any spacer as long as the thickness is known and the contact surface with the sample blocks 24a and 24b is minimal.

  The thickness of the sample W is obtained by subtracting the thickness of each sample block 24a, 24b from the total thickness of the sample W cartridge 24. For measuring the thickness, a micrometer having a minimum reading accuracy of 0.001 mm or a measuring instrument having a measurement accuracy equal to or higher than this is used. The sample W is not limited to an irregular shape, and may be a regular shape. In the case of the fixed sample W having a certain shape, the thickness may be measured in advance and then placed on the sample blocks 24a and 24b.

  The upper rod 23, the lower rod 25 and the sample blocks 24a and 24b are provided with temperature measurement holes 23a, 25a, 24c and 24d, respectively. In the upper rod 23 and the lower rod 25, a plurality (four in the illustrated example) of holes 23a and 25a are provided so as to be arranged at equal intervals in the longitudinal direction of the rod. The longitudinal direction here is a direction in which heat is transmitted in the upper rod 23 and the lower rod 25, and is a direction (vertical direction) in which the heating block 21 and the cooling block 27 are arranged.

  For example, temperature sensors 44 and 47 such as thermocouples can be inserted into the holes 23a and 25a. That is, the hole 23a of the upper rod 23 can be attached with a detection unit as a temperature measurement end of the temperature sensor 44 which is a heating side member temperature measurement unit, and the hole 25a of the lower rod 25 is provided with a cooling side member temperature measurement unit. It is possible to attach a detection unit as a temperature measurement end of the temperature sensor 47. Thus, since temperature can be detected at a plurality of locations in the longitudinal direction, temperature gradients at the upper rod 23 and the lower rod 25 can be derived based on the temperature difference between the locations. The holes 23a and 25a are filled with grease (not shown) in order to ensure close contact between the peripheral surfaces of the holes 23a and 25a and the temperature sensors 44 and 47.

  As shown in FIG. 2A, a plurality (three in the illustrated example) of holes 24c and 24d of the sample blocks 24a and 24b are also provided. The holes 24c and 24d are arranged on one side surface of the sample blocks 24a and 24b so as to be arranged at equal intervals in the width direction of the blocks 24a and 24b. That is, the plurality of holes 24c and 24d are equally spaced so as to be aligned in a direction parallel to the contact surfaces of the sample blocks 24a and 24b with the sample W (that is, the end surface of the heating side clamping member and the end surface of the cooling side clamping member). It is arranged. For example, temperature sensors 45 and 46 such as thermocouples can be inserted into the holes 24c and 24d. That is, the holes 24c and 24d of the sample blocks 24a and 24b are respectively attached with detection units as temperature measurement ends of temperature sensors 45 and 46 (also serving as a temperature measurement unit of the installation abnormality detection device 17) which are clamping unit temperature measurement units. It is possible. Three holes 24c (holes 24d) are provided, and a detection unit for the temperature sensor 45 (46) is provided in each of the holes 24c (24d). Therefore, the detection parts of the temperature sensors 45 and 46 are arranged at a plurality of positions in the width direction of the sample blocks 24a and 24b. The holes 24c and 24d are filled with grease (not shown) in order to ensure close contact between the peripheral surfaces of the holes 24c and 24d and the temperature sensors 45 and 46.

  The temperature sensors 44 to 47 are configured by, for example, thermocouples. It is also possible to use a temperature sensor having equivalent performance. Detection signals from the temperature sensors 44 to 47 are input to the calculation unit of the recording device 16. Further, the detection signals of the temperature sensors 45 and 46 are also input to the installation abnormality detection unit 73 of the installation abnormality detection device 17.

  As shown in FIG. 2B, when the electrical characteristics of the sample are measured simultaneously, the sample blocks 24a and 24b are provided with holes 24e and 24f for measuring electrical resistance. The electrical resistance measurement holes 24e and 24f are disposed on the side surface opposite to the temperature measurement holes 24c and 24d. Two holes 24e and 24f for measuring electrical resistance are provided, both of which are screw holes. One hole 24e, 24f is for applying a constant current, and the other hole 24e, 24f is for voltage measurement. Since the silicon grease 39 (40) between the sample block 24a (24b) and the upper rod 23 (lower rod 25) is insulative and the sample block 24a (24b) is made of a conductive material, the upper and lower sample blocks 24a , 24b can be connected to a terminal for electrical resistance measurement (not shown) to measure the electrical resistance of the sample W.

  As shown in FIG. 1, the measurement control device 14 includes a condition setting unit 51 for setting measurement conditions and various alarms, and a temperature control unit 52 for controlling the heating amount of the heating block 21 and the cooling amount of the cooling block 27. And a load display portion 53.

  The condition setting unit 51 has an unillustrated input unit such as a touch panel. The input unit can input measurement conditions. Examples of the measurement conditions set in the condition setting unit 51 include a sample temperature, a sample temperature width, a sample temperature upper limit value, and the like. The sample temperature upper limit value is used as a reference for performing alarm determination.

  The temperature control unit 52 controls the heating amount of the heating block 21 and the endothermic amount of the cooling block 27 according to the conditions set in the condition setting unit 51. That is, the signal output from the temperature sensors 44 to 47 is input to the temperature control unit 52, and the temperature control unit 52 sets the temperature of the sample W by the condition setting unit 51 based on the received signal. The Peltier element of the heating block 21 and the Peltier element of the cooling block 27 are controlled so as to reach the sample temperature.

  The temperature control unit 52 controls the Peltier elements of the heating block 21 and the cooling block 27 so that the temperatures of the heating block 21, the sample blocks 24a and 24b, and the cooling block 27 are stabilized at the set temperature. The temperature fluctuation range is controlled to ± 0.5K or less, for example.

  The load display unit 53 receives the signal output from the load cell 30d and displays the detected pressure of the load cell 30d.

  The recording device 16 includes an input unit 61, a calculation unit 62, a recording unit 63, and a display unit 64. The input unit 61 is used to input data related to specifications for calculating a temperature gradient, such as the overall thickness of the cartridge 24 and temperature measurement positions (positions of the holes 24c and 24d). The data input here is actually measured data.

  The calculation unit 62 includes a CPU, a ROM, a RAM, and the like, and exhibits a predetermined function by executing a program stored in the ROM. This function includes a temperature calculation unit 66, a physical property value deriving unit 67, and an electrical characteristic measuring unit 68.

  The temperature calculation unit 66 includes a signal from the temperature sensor 44 attached to the temperature measurement hole 23a of the upper rod 23, a signal from the temperature sensor 45 attached to the temperature measurement hole 24c of the upper sample block 24a, A signal from the temperature sensor 46 attached to the temperature measurement hole 24d of the lower sample block 24b and a signal from the temperature sensor 47 attached to the temperature measurement hole 25a of the lower rod 25 are input.

  The temperature calculation unit 66 derives a temperature difference between the sample blocks 24a and 24b. That is, the temperature calculation unit 66 derives an average temperature difference between the upper sample block 24a and the lower sample block 24b as a temperature difference between the blocks 24a and 24b. Specifically, the temperature calculation unit 66 averages temperature data at a plurality of locations for each of the sample blocks 24a and 24b, and derives a difference between the average values as a temperature difference between the sample blocks 24a and 24b. The temperature calculation unit 66 sets each detection end (holes 24c, 24d) in the upper and lower pairs of the upper sample block 24a and the lower sample block 24b as one set, and calculates a temperature difference for each set. The average value of the difference may be derived as a temperature difference between the sample blocks 24a and 24b.

  The temperature calculation unit 66 derives the temperature gradient at the upper rod 23 based on the data regarding the temperature measurement position on the upper rod 23 and the detection value of the temperature sensor 44. Further, the temperature calculation unit 66 derives the temperature gradient at the lower rod 25 based on the data regarding the temperature measurement position at the lower rod 25 and the detection value of the temperature sensor 47.

  The physical property value deriving unit 67 derives a physical property value related to the heat conduction of the sample W based on the measurement result of the temperature calculating unit 66. Here, it is assumed that the thermal conductivity is derived. The physical property value deriving unit 67 derives the distance between the temperature measurement positions of the sample blocks 24 a and 24 b stored in advance and the sample W by using the input data relating to the entire thickness of the cartridge 24 and the sample W. The thickness is derived, the temperatures of the upper and lower surfaces of the sample W are calculated based on the detected values of the temperature sensor 45 and the temperature sensor 46, and the temperature of the sample W is calculated based on the calculated temperature data and the thickness of the sample W. Deriving the gradient. Then, the thermal conductivity of the sample W is derived from this temperature gradient.

  The electrical characteristic measuring unit 68 derives the electrical resistance of the sample W based on the inter-terminal voltage and current value of the terminals attached to both the sample blocks 24a and 24b.

  The recording unit 63 records the temperature measured by each of the temperature sensors 44 to 47, the derived thermal conductivity, the measured conduction resistance value of the sample W, and the like. The display unit 64 displays the temperature measured by each of the temperature sensors 44 to 47, the derived thermal conductivity, the conduction resistance value, and the like.

  The installation abnormality detection device 17 is a device for detecting an installation abnormality of the sample W in the measurement unit of the measurement apparatus main body 12, and includes a calculation unit 71 and a display unit 72. The calculation unit 71 includes a CPU, a ROM, a RAM, and the like, and exhibits a predetermined function by executing a program stored in the ROM. This function includes an installation abnormality detection unit 73.

  The installation abnormality detection unit 73 detects an installation abnormality of the sample W (an abnormality in the pinching state). The installation abnormality detection unit 73 includes a signal from the temperature sensor 45 attached to the temperature measurement hole 24c of the upper sample block 24a and a temperature sensor 46 attached to the temperature measurement hole 24d of the lower sample block 24b. Signal.

  Here, in this embodiment, the normal installation state of the sample W means that the heating side clamping member (the upper rod 23 and the upper sample block 24a), the sample W, and the cooling side clamping, as shown in FIG. In this state, the central axes of the members (lower sample block 24b and lower rod 25) are located on a common straight line. On the other hand, the abnormal installation of the sample W means a state where the central axes of the heating side clamping members 23 and 24a, the sample W, and the cooling side clamping members 25 and 24b are not located on a common straight line, for example, any member The central axis is inclined with respect to the central axis of the other member (see FIGS. 3B and 3E), or the central axis of one of the members is on the side of the central axis of the other member Or a state where the thickness dimension of the measurement object (dimension in the clamping direction) is not uniform (see FIG. 3C).

  The installation abnormality detection unit 73 detects an installation abnormality based on temperature variations in the width direction of the upper sample block 24a and the lower sample block 24b. That is, the installation abnormality detection unit 73 detects the deviation of the heat flow from the upper rod 23 to the lower rod 25 based on the installation abnormality of the sample W in the plane direction parallel to the contact surface with the sample W in each of the sample blocks 24a and 24b. By detecting this as a variation in temperature, the installation abnormality of the sample W is detected. Specifically, the installation abnormality detection unit 73 determines that there is an installation abnormality when the temperature variation in the width direction is larger than a predetermined range, and determines that there is no installation abnormality when the variation is within a predetermined range. Specifically, the installation abnormality detection unit 73 obtains a difference between the maximum value and the minimum value among the temperature data at a plurality of locations (three locations in the present embodiment) in the width direction of the upper sample block 24a, A predetermined value stored in advance is compared. Further, the installation abnormality detection unit 73 obtains a difference between the maximum value and the minimum value among the temperature data at a plurality of locations (three locations in the present embodiment) in the width direction of the lower sample block 24b, The predetermined specified value is compared. Then, the installation abnormality detection unit 73 determines that an installation abnormality has occurred in at least one of the upper sample block 24a and the lower sample block 24b when the value of the difference is larger than a specified value. If the value is less than the specified value, it is determined that no installation abnormality has occurred.

  The display unit 72 displays the temperatures measured by the temperature sensors 45 and 46, the difference value, whether or not an installation abnormality has occurred, and the like.

  Next, a procedure for measuring the thermal conductivity using the measuring apparatus 10 will be described.

  First, the cartridge 24 is prepared. In the production process of the cartridge 24, the sample W is applied to one sample block 24a (24b) so as to be adjusted to a specified thickness. Then, if necessary, a spacer is installed, and the other sample block 24b (24a) is polymerized so that the coated surface of the sample W is sandwiched. Thereby, the cartridge 24 is completed. Then, the thickness of the entire cartridge 24 is measured with a micrometer. This measured value is input to the recording device 16 by the input unit 61. In order to regulate the thickness of the sample W, it is desirable to use a spacer.

  Next, the cartridge 24 is set between the upper rod 23 and the lower rod 25, temperature sensors 45 and 46 are attached to the sample blocks 24a and 24b, and terminals for measuring electrical characteristics are attached. At this time, temperature sensors 44 and 47 are already attached to the upper rod 23 and the lower rod 25. At this time, silicon grease 39, 40 is applied to the contact surface between the upper rod 23 and the cartridge 24 and the contact surface between the cartridge 24 and the lower rod 25. Thereby, contact thermal resistance can be reduced.

  Next, the pressure adjusting screw 30c of the pressure adjusting unit 30 is screwed in to adjust the pressing force between the cartridge 24 and the upper and lower rods 23 and 25 and the pressing force applied to the sample W. Since the detected load of the load cell 30d is displayed on the load display unit 53 of the measurement control device 14, the pressing force may be adjusted while referring to this display.

  When the pressing force is adjusted, a check is started as to whether or not a sample W installation abnormality has occurred. That is, the heating block 21 is heated and the cooling block 27 is cooled. The temperature difference between the heating block 21 and the cooling block 27 due to the heating and cooling is for detecting an installation abnormality of the sample W, so that if a heat flow from the upper rod 23 to the lower rod 25 occurs. Well, it may be smaller than when the physical property value relating to the heat conduction of the sample W is measured.

  With this heating and cooling, heat is transferred from the heating block 21 to the upper rod 23, the cartridge 24, and the lower rod 25, and the measurement data of each temperature sensor 45, 46 is output every predetermined time. It is transmitted to the installation abnormality detection unit 73.

The installation abnormality detection unit 73 of the installation abnormality detection device 17 derives the absolute value of the difference between the maximum value and the minimum value of the temperature data sent from the temperature sensors 45 and 46 for each of the sample blocks 24a and 24b. Specifically, the installation abnormality detection unit 73, as the determination 1, based on the temperature data (T _1a , T _1b , T _1c ) sent from the temperature sensor 45 of the upper sample block 24a (see FIG. 4),
(Maximum value of T _1a , T _1b , T _1c ) − (Minimum value of T _1a , T _1b , T _1c )
Perform the operation. Then, the installation abnormality detection unit 73 compares the value of the calculation result with a predetermined value stored in advance (for example, 0.5K in the present embodiment).

Together with this determination 1, the installation abnormality detection unit 73, as determination 2, is based on the temperature data (T _2a , T _2b , T _2c ) sent from the temperature sensor 46 of the lower sample block 24b (see FIG. 4),
(Maximum value of T _2a , T _2b , T _2c ) − (minimum value of T _2a , T _2b , T _2c )
Perform the operation. Then, the installation abnormality detection unit 73 compares the value of the calculation result with the specified value (in this embodiment, for example, 0.5K).

The installation abnormality detection unit 73
(Maximum value of T _1a , T _1b , T _1c ) − (minimum value of T _1a , T _1b , T _1c ) ≦ specified value (maximum value of T _2a , T _2b , T _2c ) − (T _2a , T _2b , T _2c minimum value) ≦ specified value, it is determined that no installation abnormality has occurred,
(Maximum value of T _1a , T _1b , T _1c ) − (minimum value of T _1a , T _1b , T _1c )> specified value (maximum value of T _2a , T _2b , T _2c ) − (T _2a , T _2b , T _2c minimum value) ≦ specified value or
(Maximum value of T _1a , T _1b , T _1c ) − (minimum value of T _1a , T _1b , T _1c ) ≦ specified value (maximum value of T _2a , T _2b , T _2c ) − (T _2a , T _2b , T _2c minimum value)> specified value or
(Maximum value of T _1a , T _1b , T _1c ) − (minimum value of T _1a , T _1b , T _1c )> specified value (maximum value of T _2a , T _2b , T _2c ) − (T _2a , T _2b , T _2c (minimum value)> predetermined value, it is determined that an installation error has occurred.

  When an installation abnormality is detected, the display unit 72 of the installation abnormality detection device 17 displays that effect. When this display is made, the operator of the device 10 loosens the pressure adjusting screw 30c of the pressure adjusting unit 30. Then, the cartridge 24 is removed from between the upper rod 23 and the lower rod 25, and this cartridge 24 is installed again, or another cartridge 24 is newly installed.

  The cartridge 24 is re-installed or a new cartridge 24 is installed in the same manner as described above, and when this is completed, the installation abnormality is checked again. In this check, if an installation abnormality is not detected, measurement of a physical property value related to the heat conduction of the sample W is started, and if an installation abnormality is detected, the cartridge 24 is installed again.

  On the other hand, if the installation abnormality is not detected at the time of the first installation abnormality check, the measurement of the physical property value relating to the heat conduction of the sample W is started as it is.

  Subsequently, the heating block 21 is heated and the cooling block 27 is cooled in order to measure the physical property values relating to the heat conduction of the sample W. Accordingly, heat is transferred from the heating block 21 to the upper rod 23, the cartridge 24, and the lower rod 25, and measurement data of the temperature sensors 44 to 47 are output at predetermined time intervals. Each temperature is displayed on the display unit 64 of the recording device 16 and recorded in the recording unit 63, while the temperature measured by the temperature sensors 45 and 46 is also transmitted to the installation abnormality detection device 17.

  The installation abnormality detection device 17 moves from the upper rod 23 to the lower rod 25 until the measurement unit of the measurement device main body 12 is in a steady state during the measurement operation of the physical property value related to the heat conduction of the sample W in the device 10. Using the heat flow, the installation abnormality that occurred during the measurement is also detected.

  Specifically, in the installation abnormality detection unit 73 of the installation abnormality detection device 17, the absolute value of the difference between the maximum value and the minimum value of the temperature data sent from the temperature sensors 45 and 46 is used as the sample blocks 24a and 24b. Derived every time. Then, similarly to the above, the installation abnormality detection unit 73 compares the temperature difference value obtained for each of the sample blocks 24a and 24b with the specified value to determine whether or not an installation abnormality has occurred.

  If the installation abnormality is not detected, the measurement is continued as it is. If the installation abnormality is detected, the measurement of the physical property value relating to the heat conduction of the sample W is stopped, the cartridge 24 is re-installed, and the measurement is performed again.

  Control is performed until the amount of change in the sample temperature becomes 0.2 K or less per minute, and after the amount of change in temperature becomes 0.2 K or less, the state is regarded as a steady state, and the temperature in this steady state is recorded.

  In the calculation unit 62 of the recording device 16, the temperature gradient at the upper rod 23, the temperature gradient at the lower rod 25, the temperature at the cartridge 24, based on the measurement values by the temperature sensors 44 to 47 and the data related to the temperature measurement position. Deriving the temperature gradient. For the upper rod 23 and the lower rod 25, temperature measurement positions are stored in advance. For this reason, the temperature gradient in the upper rod 23 and the lower rod 25 is derived based on the stored measurement position and the measured temperature. On the other hand, since the cartridge 24 has a different thickness for each cartridge 24, the temperature measurement positions of the sample blocks 24 a and 24 b stored in advance and the sample W are stored using the data regarding the thickness of the cartridge 24 input by the input unit 61. And the thickness of the sample W are derived. Then, the calculation unit 62 calculates the temperatures of the upper and lower surfaces of the sample W based on the detection values of the temperature sensor 45 and the temperature sensor 46, and based on the calculated temperature data and the thickness of the sample W, the temperature Deriving the gradient.

Subsequently, the calculation unit 62 derives the thermal conductivity of the sample W. Calculation of thermal conductivity is performed as follows. That is, as shown in FIGS. 4 and 5, the thermal conductivity of the sample _{W k s [W / (m} · K)], the thermal conductivity of the upper rod 23 and lower rod _{25 k r [W / (m} · K)], the thermal conductivity k _B [W / (m · K)] of the sample blocks 24a and 24b, the thickness t _s [m] of the sample W, and the position between the sensor position of the sample blocks 24a and 24b and the sample W. The distance t _SB [m], the temperature difference ΔT _B [K] between the upper and lower sample blocks 24a, 24b, the temperature difference ΔT _s [K] between the upper and lower surfaces of the sample W, the sensor of the sample blocks 24a, 24b and the surface of the sample W Difference ΔT _SB [K], heat flow rate q ₁ [W / m ² ] passing through the upper rod 23, heat flow rate q ₂ [W / m ² ] passing through the lower rod 25, and heat passing through the sample W Flow velocity q [W / m ² ], temperature gradient at upper rod 23 (dT / dx) ₁ [K / M], the temperature gradient at the lower rod _{25 (dT / dx) 2 [} K / m], when the temperature gradient of the sample _{W (dT / dx) s [} K / m], the following relationship is established.

In the above equation (3), to derive the thermal conductivity k _s of sample W, while obtaining the temperature difference [Delta] T _s between the upper and lower surface of the sample W from equation (4), the sample W thickness t _s is The thickness of the upper sample block 24a and the lower sample block 24b stored in advance is subtracted from the total thickness of the cartridge 24 input by the input unit 61. Then, the temperature gradient (dT / dx) _s of the sample W is obtained from the relational expression (6). The thermal conductivity k _s of the sample W can be obtained from this temperature gradient and the heat flow rate q obtained from the relational expressions (1) and (2).

  As described above, according to the present embodiment, the flow of heat from the upper rod 23 to the upper sample block 24a, the sample W, the lower sample block 24b, and the lower rod 25 from the upper rod 23 due to the installation abnormality of the sample W is reduced. By detecting the variation in temperature in the surface direction parallel to the contact surface with the sample W in each of the sample blocks 24a and 24b, the installation abnormality of the sample W can be detected. Thereby, the installation abnormality can be eliminated by re-installing the sample W or the like, and the thermophysical property value of the sample W (physical property value related to thermophysical conduction) can be accurately obtained.

  In the present embodiment, since the temperature distribution in the plane direction parallel to the contact surface with the sample W is measured by the three temperature sensors 45 and 46 in each sample block 24a and 24b, in each sample block 24a and 24b. The configuration of the temperature measuring units 45 and 46 can be simplified as compared with the configuration of measuring the temperature variation across the parallel plane direction.

  Further, in the present embodiment, the temperature sensors 45 and 46 used for detecting the installation abnormality are also used for deriving the thermophysical property values, so that the number of the temperature measurement ends 45 and 46 in the apparatus 10 can be reduced. Can be suppressed.

  In the present embodiment, the upper sample block 24a can be detached from the upper rod 23 and the lower sample block 24b can be detached from the lower rod 25, so that the replacement work of the sample W (cartridge 24) can be facilitated. Can be planned.

  In addition, in the present embodiment, in addition to the detection of the installation abnormality before entering the measurement operation of the thermophysical property value in the heat conduction measuring device 10, the lower part is moved from the upper rod 23 during the thermophysical property measurement operation in the heat conduction measuring device 10. The sample W generated during the measurement operation of the thermophysical property value is measured by measuring the temperature variation in the direction parallel to the contact surface with the sample W in each of the sample blocks 24a and 24b using the flow of heat flowing to the rod 25. It is also possible to detect an installation error of the.

  Note that the present invention is not limited to the above-described embodiment, and various modifications and improvements can be made without departing from the spirit of the present invention.

  In the above embodiment, the detection of the installation abnormality of the sample W is performed before and during the measurement operation of the thermophysical property value of the sample W in the heat conduction measuring device 10, but the measurement operation is not limited to this. It may be performed either before entering or during the measurement operation.

  Further, in the above embodiment, when an installation abnormality of the sample W is detected, the operator corrects the installation state, but the mechanism for correcting the installation state of the sample W is provided in the heat conduction measuring device 10. The installation state may be automatically corrected by the device.

  Moreover, in the said embodiment, although the recording device 16 and the installation abnormality detection apparatus 17 are comprised as a separate apparatus, these may be comprised as one apparatus.

  In the above embodiment, the upper rod 23 and the upper sample block 24a are formed separately from each other, and the lower rod 25 and the lower sample block 24b are formed separately from each other. Although the cartridge 24 is sandwiched by the lower rod 25, the present invention is not limited to this. For example, as shown in FIG. 6A, the heating-side clamping member 123 and the cooling-side clamping member 125 are each composed of a single member, and the heating-side clamping member 123 and the cooling-side clamping member 125 are the sample. You may comprise so that W may be inserted | pinched. That is, the heating side clamping member 123 may be configured by integrating the upper rod 23 and the upper sample block 24a, and the cooling side clamping member 125 may be configured by integrating the lower rod 25 and the lower sample block 24b. Even in this case, the installation abnormality of the sample W can be detected by measuring the temperature variation in the plane direction parallel to the contact surface (end surface) of each of the clamping members 123 and 125 with the sample W.

  In the one-way heat flow steady comparison method, the thickness dimension of the sample W is required when calculating the physical property value related to heat conduction. Therefore, in the above embodiment, the operator or the like inputs the value into the heat conduction measuring device 10. However, for example, a device for measuring the thickness dimension of the sample W as shown in FIGS. 6A to 6D may be provided in the heat conduction measuring device 10.

  In this aspect, the thickness dimension of the sample W can be obtained based on the measured distance between the clamping members 123 and 125 (or both sample blocks 24a and 24b). At this time, since the heat conduction measuring device can detect the installation abnormality of the sample W, it can be eliminated. Therefore, by measuring only one point between the contact surfaces of the heating side clamping member 123 (or the upper sample block 24a) and the cooling side clamping member 125 (or the lower sample block 24b) with the sample W, The thickness dimension can be obtained with high accuracy.

  As an apparatus for measuring the thickness dimension of the sample W, for example, a contact-type displacement sensor (FIG. 6A) that directly touches the contact surface of the clamping member 123 and measures based on the vertical position of the contact surface. )), A laser displacement meter (see FIG. 6 (b)) that measures the distance between the pins attached to both the holding members 123 and 125 in a non-contact manner by a laser, and slits and pins provided in both the holding members 123 and 125 There are various contact-type and non-contact-type sensors such as an optical position sensor (see FIG. 6C and FIG. 6D) that measures the distance of the light by receiving the light emitted from the irradiation unit by the light receiving unit. Used.

  In the above embodiment, the temperature variation in the surface direction parallel to the contact surface with the sample W in both the sample blocks 24a and 24b is measured, but the sample W in either one of the sample blocks 24a (or 24b) Only the temperature variation in the plane direction parallel to the contact surface may be measured. If the temperature variation in the surface direction parallel to the end surface of the lower rod 25 on the lower sample block 24b can be measured, the upper rod 23 and the cartridge 24 are integrated as shown in FIG. It is possible to detect an abnormal installation that is inclined.

  Moreover, in the said embodiment, although the temperature of several places (namely, intermittently) is measured in the surface direction parallel to the contact surface with the sample W in both sample blocks 24a and 24b, the surface direction parallel to a contact surface You may measure the temperature of the whole area | region continuously. Thereby, it is possible to detect the installation abnormality with higher accuracy.

  In addition, a specific method for detecting a temperature variation over a predetermined range is not limited. In the above embodiment, the temperature variation of a predetermined range or more is detected using the difference between the maximum value and the minimum value of the temperature in the common plane direction. For example, the positions facing each other across the sample W May be detected on the basis of the temperature difference between them, the relative ratio of the temperatures at each position, or the like, or may be detected based on whether or not the temperature difference between the opposing positions exceeds a threshold.

Specifically, for example, the temperature difference between T _1a and T _2a in FIG. 4 is ΔT _a , the temperature difference between T _1b and T _2b is ΔT _b , and the temperature difference between T _1c and T _2c is ΔT _c. When the thickness of the sample W is a predetermined value or less,
If the maximum value of the temperature differences ΔT _a , ΔT _b , ΔT _c ≦ the specified value, it is determined that no installation abnormality has occurred,
If the maximum value among the temperature differences ΔT _a , ΔT _b , ΔT _c > the specified value, it may be determined that an installation abnormality has occurred.

Also, the presence / absence of an installation abnormality is determined based on whether or not the difference between the maximum value of T _1a , T _1b , and T _1c and the minimum value of T _2a , T _2b , and T _2c is within a specified value. Also good.

10 Heat Conduction Measurement Device 17 Installation Abnormality Detection Device 21 Heating Block (Example of Heating Source)
23 Upper rod (example of heating side member)
24 cartridge (an example of a clamping part)
24a Upper sample block (an example of a heating side clamping part)
24b Lower sample block (an example of a cooling side clamping part)
24c, 24d Temperature measurement hole 25 Lower rod (an example of a cooling side member)
27 Cooling block (an example of a cooling source)
45, 46 Temperature sensor (example of temperature measurement unit)
71 Calculation unit 72 Display unit 73 Installation abnormality detection unit W Sample

Claims (4)

A heat conduction measuring device used in a one-way heat flow steady comparison method,
A heating-side clamping member having an end face that is thermally connected to a heating source and contacts one surface of the measurement object;
A cooling-side clamping member that has an end face that is thermally connected to a cooling source and that contacts the other surface of the measurement object, and sandwiches the measurement object together with the heating-side clamping member;
A temperature measuring unit that measures at least one of a temperature variation in a plane direction parallel to the end surface of the heating-side clamping member and a temperature variation in a plane direction parallel to the end surface of the cooling-side clamping member;
A heat conduction measurement device comprising: an abnormality detection unit that detects an installation abnormality of the measurement object based on variations in temperature measured by the temperature measurement unit.   The temperature measurement unit has a temperature measurement end, and the temperature measurement ends are respectively arranged at a plurality of locations in a plane direction parallel to the end face of at least one of the heating side clamping member and the cooling side clamping member. Item 2. The heat conduction measuring device according to Item 1.   The heat conduction measuring device according to claim 1 or 2, further comprising an interval measuring unit that measures an interval between the heating-side clamping member and the cooling-side clamping member in a state where the measurement object is sandwiched. A method for measuring a physical property value related to heat conduction of a measurement object,
A heating-side clamping member having an end surface that is thermally connected to the heating source and that contacts one surface of the measurement object, and an end surface that is thermally connected to the cooling source and contacts the other surface of the measurement object A clamping step of sandwiching a measurement object by a cooling side clamping member having
Heating the heating side clamping member by the heating source while the measurement object is sandwiched and cooling the cooling side clamping member by the cooling source, heat is applied from the heating side clamping member to the cooling side clamping member. A heat flow process,
With the heat flowing in the heat flow step, at least one of a temperature variation in the surface direction parallel to the end surface of the heating-side clamping portion and a temperature variation in the surface direction parallel to the end surface of the cooling-side clamping member. A temperature measurement process for measuring temperature variations;
And a detection step of detecting an installation abnormality of the measurement object based on the measured temperature variation.

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