JP5942889B2 - Heat transfer mechanism and thermal analysis apparatus having the same - Google Patents

Description

  The present invention relates to a heat transfer mechanism including a heat sink in which a sample to be measured and a reference material are accommodated, and a thermal analysis apparatus including the heat transfer mechanism.

  A thermal analysis apparatus such as a differential scanning calorimeter (DSC) includes a heat sink that is heated by a heater, for example, and a sample to be measured and a reference material are accommodated in the heat sink. (For example, see Patent Documents 1 and 2 below).

  In the configuration disclosed in Patent Document 1, a cooling block (heat transfer unit) 20 is disposed below the heat sink 10. At the time of analysis, not only can the heat sink 10 be heated by the heater 12, but also the heat sink 10 can be cooled by transferring heat between the heat sink 10 and the cooling source via the cooling block 20. Yes.

  A thermal resistor 14 is disposed between the heat sink 10 and the cooling block 20. The thermal resistor 14 is formed in a cylindrical shape, and its upper end surface is brazed to the heat sink 10 and its lower end surface is brazed to the cooling block 20. In this example, the thermal resistor 14 is made of iron. In contrast, the heat sink 10 is made of silver or the like, and the cooling block 20 is made of copper or aluminum.

JP 2010-190807 A JP 2002-310965 A

  However, in the configuration disclosed in Patent Document 1 as described above, the bonding surface between the thermal resistor 14 and the heat sink 10 and the bonding surface between the thermal resistor 14 and the cooling block 20 are bonded to each other. It is a surface. Therefore, there is a problem that stress is generated in each member during heating or cooling due to a difference in linear expansion coefficient between the members. In this case, repeated heating and cooling may cause adverse effects such as peeling of the thermal resistor 14 on the joint surface.

  Further, at the time of heating, the temperature of the heat sink 10 rises to about 600 ° C., for example, whereas the temperature of the cooling block 20 is as low as about 0 ° C., for example. large. Therefore, not only the difference in linear expansion coefficient but also the influence of the temperature difference as described above causes a problem that the stress generated in each member is further increased.

  The configuration disclosed in Patent Document 2 is disclosed in Patent Document 1 in that a thermal resistor 9 is disposed between the furnace block assembly (heat sink) 1 and the cooling flange (heat transfer portion) 10. It matches the configuration. However, Patent Document 2 is different from the configuration disclosed in Patent Document 1 in that the thermal resistor 9 is not cylindrical but formed by a plurality of thin members 31.

  As described above, when the thermal resistor 9 is formed by a plurality of thin members 31, the deformation of these thin members 31 can absorb the stress generated in each member due to the difference in linear expansion coefficient. there is a possibility. However, when a plurality of thin members 31 are joined to the furnace block assembly 1 and the cooling flange 10, the joining state tends to be uneven, and there is a possibility that the temperature distribution in the furnace block assembly 1 varies.

  The present invention has been made in view of the above circumstances, a heat transfer mechanism in which stress is not easily generated in each member during heating or cooling, and temperature distribution in the heat sink is less likely to vary, and a thermal analysis apparatus including the heat transfer mechanism The purpose is to provide.

The heat transfer mechanism according to the present invention includes a heat sink in which a sample to be measured and a reference material are stored, a heater for heating the heat sink, a cooling source for cooling the heat sink, and the heat sink and the cooling source. A heat transfer part for transferring heat between them, and at least one of the heat sink and the heat transfer part is formed with an opening or a recess to partially reduce the cross-sectional area, thereby reducing the thermal resistance. And the resistance value of the thermal resistance unit is such that when the heater is energized to a predetermined value, the amount of heat supplied from the heater to the heat sink is released from the heat sink via the heat transfer unit. The heat sink is set to exceed the amount of heat, and if the heater is energized to the predetermined value, the heat sink can be heated, and the energization amount to the heater is set to the predetermined amount. Characterized in that it is possible to cool the heat sink if caused to decrease than.

  According to such a configuration, a thermal resistance portion can be formed on at least one of the heat sink and the heat transfer portion by using a part thereof. As a result, unlike the case where a thermal resistor is provided as a separate member between the heat sink and the heat transfer part, due to the difference in linear expansion coefficient or temperature difference of each member, heating or cooling Sometimes stress is not easily generated in each member.

  In addition, unlike the case where a thermal resistor is provided as a separate member between the heat sink and the heat transfer unit, the bonding state of the heat resistor to the heat sink and the heat transfer unit is not uneven. The heat distribution is less likely to vary in the heat sink.

  In particular, since the structure is such that at least one of the heat sink and the heat transfer part is formed with an opening or a recess to partially reduce the cross-sectional area, it is compared with the case where a thermal resistor is provided as a separate member. Thus, the configuration is simple and the above effects can be achieved at low cost.

  It is preferable that the thermal resistance portion has an opening or a recess so as to have a thermal resistance of 0.1 to 10 K / W.

  According to such a configuration, in the heat transfer mechanism including the heat sink in which the sample to be measured and the reference material are accommodated, the heat resistance portion having an appropriate heat resistance can be formed. Can function.

  The heat sink may be provided with a measured sample placing portion on which the measured sample is placed and a reference material placing portion on which the reference material is placed symmetrically with respect to the center line. In this case, the thermal resistance portion may be formed so as to be symmetric with respect to the center line.

  According to such a configuration, since the thermal resistance portion is formed so as to be symmetric with respect to the center line between the measured sample mounting portion and the reference material mounting portion, the measured sample It is possible to effectively prevent the temperature distribution from varying between the placement portion side and the reference material placement portion side.

  The heat sink and the heat transfer part may be integrally formed.

  According to such a configuration, since there is no bonding surface between the heat sink and the heat transfer portion, unevenness in the bonding state is less likely to occur, and variation in temperature distribution in the heat sink can be more effectively prevented. it can.

  A thermal analysis apparatus according to the present invention is a thermal analysis apparatus for performing thermal analysis using a sample to be measured and a reference material, and includes the heat transfer mechanism.

  According to the present invention, since at least one of the heat sink and the heat transfer portion can be used to form a thermal resistance portion, it is caused by a difference in linear expansion coefficient or a temperature difference of each member. In addition, stress is not easily generated in each member during heating or cooling. In addition, according to the present invention, unevenness in the bonding state is unlikely to occur, and therefore, the temperature distribution is unlikely to vary in the heat sink.

It is a top view which shows the structural example of the thermal analyzer provided with the heat transfer mechanism which concerns on one Embodiment of this invention. It is sectional drawing along the centerline L1 in the heat transfer mechanism of FIG. 1A. It is a top view which shows the 1st modification of a heat transfer mechanism. It is sectional drawing in alignment with the centerline L1 in the heat transfer mechanism of FIG. 2A. It is a top view which shows the 2nd modification of a heat transfer mechanism. It is a top view which shows the structural example of the thermal analyzer provided with the heat transfer mechanism which concerns on another embodiment. It is sectional drawing along the centerline L101 in the heat transfer mechanism of FIG. 4A. It is sectional drawing which shows the structural example of the thermal analyzer provided with the heat-transfer mechanism which concerns on another embodiment.

  FIG. 1A is a plan view showing a configuration example of a thermal analysis apparatus including a heat transfer mechanism 1 according to an embodiment of the present invention. FIG. 1B is a cross-sectional view along the center line L1 in the heat transfer mechanism 1 of FIG. 1A. This thermal analyzer is, for example, a differential scanning calorimeter, and performs thermal analysis using a sample to be measured and a reference material. For example, by using a differential scanning calorimeter, the calorific difference between the sample to be measured and the reference material can be measured based on a temperature change that occurs when the sample to be measured melts.

  The heat transfer mechanism 1 includes a heat sink 2, a heater 3, a cooling source 4, a heat transfer unit 5, and the like. The sample to be measured and the reference material are accommodated in the heat sink 2. The sample to be measured and the reference material in the heat sink 2 can be heated by the heater 3 and can be cooled by the cooling source 4.

  The heat sink 2 includes a mounting table 21 that extends in the horizontal direction, a cylindrical peripheral wall 22 that surrounds the outer periphery of the mounting table 21, and an annular flange portion 23 that projects radially from the lower end of the peripheral wall 22. It is formed in a circular shape when viewed. In this example, as shown in FIG. 1B, the lower plate 24 is configured such that the lower portion of the flange portion 23 is separable, and when the mounting table 21 becomes dirty, the heat sink 2 is located above the lower plate 24. The part can be removed and cleaned or replaced.

  The heat sink 2 is made of, for example, copper. However, the material of the heat sink 2 is not limited to copper, and the heat sink 2 can be formed of other materials such as silver as long as the material has high thermal conductivity. Further, the heat sink 2 is not limited to the configuration divided into a plurality of (for example, two) components as described above, and may be configured by one component.

  The mounting table 21 is provided with a measured sample mounting part 211 and a reference material mounting part 212 symmetrically on both sides of the center line L1. The measurement sample mounting unit 211 and the reference material mounting unit 212 are formed by, for example, a circular flat surface, and are arranged side by side on a horizontal plane so as to be close to each other.

  A sample to be measured (measurement sample) is placed on the measurement sample mounting unit 211. On the other hand, a reference material (reference material) such as alumina is placed on the reference material placement unit 212. At the time of analysis, as shown in FIG. 1B, the upper end portion of the peripheral wall 22 of the heat sink 2 is covered with the lid 6 so that the sample to be measured and the reference substance are not easily affected by the outside air.

  The thermocouple 7 is connected to the back side (lower surface) of the measured sample mounting part 211 and the reference material mounting part 212 in the heat sink 2. Each thermocouple 7 extends in the vertical direction so as to protrude from the lower portion of the heat sink 2. By detecting the temperature of the measured sample mounting portion 211 and the reference material mounting portion 212 via these thermocouples 7, the difference in calorie between the measured sample and the reference material can be measured based on the temperature change. it can.

  The heater 3 is composed of a sheathed heater, for example, and is configured by housing a heating element such as a nichrome wire with an insulating material sandwiched in a metal tube. The heater 3 is sandwiched between the heat sink 2 and the heat transfer unit 5 in a state of being wound in a horizontal plane. Thereby, the heat sink 2 can be heated by the heater 3, and the sample to be measured and the reference material in the heat sink 2 can be heated. During heating by the heater 3, the temperature of the heat sink 2 rises to a high temperature of about 600 ° C., for example.

  The cooling source 4 is for cooling the heat sink 2 and contains a refrigerant such as liquid nitrogen, for example. However, the cooling source 4 is not limited to using liquid nitrogen, but may be based on other configurations such as an electronic cooler. The heat transfer unit 5 has one end connected to the cooling source 4 and the other end connected to the heat sink 2 via the heater 3, thereby transferring heat between the heat sink 2 and the cooling source 4. Can be done. As a result, the heat sink 2 is cooled by the cooling source 4 and the heat transfer section 5, and the sample to be measured and the reference material in the heat sink 2 can be cooled. The temperature of the heat transfer unit 5 is as low as about 0 ° C., for example.

  The heat transfer unit 5 is made of, for example, copper. However, the material of the heat transfer unit 5 is not limited to copper, and the heat transfer unit 5 can be formed of other materials such as silver as long as the material has high thermal conductivity. Moreover, the heat sink 2 and the heat transfer part 5 are not limited to the structure formed of the same material, and may be formed of different materials. In this example, the heat transfer section 5 is formed by a rectangular plate-like member extending in the horizontal direction, but the present invention is not limited to this, and the heat transfer section 5 may be formed by another shape.

  The connection between the members separated from each other in the heat transfer mechanism 1 can be performed using a fixing tool such as a fixing screw. For example, the heat sink 2 and the heat transfer unit 5 can be connected by screwing a fixing screw from one side of the heat sink 2 side or the heat transfer unit 5 side to the other side with the heater 3 sandwiched therebetween. . Also, the lower plate 24 of the heat sink 2 can be fixed by, for example, screwing a fixing screw from the upper side of the heat sink 2 and connecting to the lower plate 24.

  However, the members separated from each other in the heat transfer mechanism 1 are not limited to fixing screws, and may be connected by any other means such as brazing or welding. Further, other members or materials such as a brazing material (not shown) may be interposed between the members separated from each other.

  In the present embodiment, the opening 51 is formed in the heat transfer portion 5 and the cross-sectional area in the direction orthogonal to the center line L1 is partially reduced, so that both sides of the opening 51 in the direction orthogonal to the center line L1 In addition, thermal resistance parts 52 are respectively formed. In this example, a rectangular opening 51 is formed at the center of the heat transfer section 5 so that the two thermal resistance sections 52 are formed so as to be symmetric with respect to the center line L1. .

  Each thermal resistance part 52 is formed in, for example, an elongated bar shape parallel to the center line L1. The cross section in the direction orthogonal to the center line L1 in each thermal resistance part 52 is, for example, rectangular. The thermal resistance of each thermal resistance portion 52 can be defined by the cross-sectional area and length of each thermal resistance portion 52. In this example, the opening 51 is formed so that the thermal resistance of about 3 K / W is generated by the two thermal resistance parts 52.

  However, the shape of the opening 51 is not limited to a rectangular shape. Further, the shape of each thermal resistance portion 52 is not limited to an elongated rod shape whose cross section is a rectangular shape. Further, the shape is not limited to the shape that penetrates the heat transfer part 5 as in the opening 51, for example, a recess that does not penetrate the heat transfer part 5 is formed, and the cross-sectional area of the heat transfer part 5 is partially reduced. Thus, a configuration in which the thermal resistance portion is formed may be employed.

  The thermal resistance of the thermal resistance portion 52 is not limited to the above value, but the opening 51 is preferably formed so as to have a thermal resistance of 0.1 to 10 K / W as a whole. Thereby, in the heat transfer mechanism 1 including the heat sink 2 in which the sample to be measured and the reference material are accommodated, the heat resistance portion 52 having an appropriate heat resistance can be formed. Can function.

  The thermal resistance of the thermal resistance unit 52 as described above can be set based on the relationship between the amount of heat supplied from the heater 3 to the heat sink 2 and the amount of heat released from the heat sink 2 via the heat transfer unit 5. Specifically, when the heater 3 is energized to a predetermined value, the amount of heat supplied from the heater 3 to the heat sink 2 exceeds the amount of heat released from the heat sink 2 via the heat transfer unit 5. Thermal resistance is set.

  Thus, the heat sink 2 can be heated if the heater 3 is energized to a predetermined value, and the heat sink 2 can be cooled if the energization amount to the heater 3 is reduced below the predetermined value. Therefore, it is possible to adjust the temperature to an arbitrary temperature by heating or cooling the heat sink 2 only by controlling the energization amount to the heater 3.

  As described above, in the present embodiment, the thermal resistance portion 52 can be formed using a part of the heat transfer portion 5. As a result, unlike the case where a thermal resistor is provided as a separate member between the heat sink 2 and the heat transfer portion 5, due to the difference in linear expansion coefficient or temperature difference of each member, In addition, stress is not easily generated in each member during cooling.

  In addition, unlike the case where a thermal resistor is provided as a separate member between the heat sink 2 and the heat transfer unit 5, the joining state of the heat resistor to the heat sink 2 and the heat transfer unit 5 becomes uneven. Therefore, the temperature distribution in the heat sink 2 is less likely to vary.

  In particular, since the opening 51 is formed in the heat transfer part 5 and the sectional area is partially reduced, the structure is simple compared to the case where a thermal resistor is provided as a separate member. Yes, the above effects can be achieved at low cost.

  Further, in the present embodiment, since the thermal resistance portion 52 is formed in a symmetric arrangement with respect to the center line L1 between the measured sample placement portion 211 and the reference material placement portion 212, It is possible to effectively prevent a variation in temperature distribution between the measured sample placement unit 211 side and the reference material placement unit 212 side.

  FIG. 2A is a plan view showing a first modification of the heat transfer mechanism 1. 2B is a cross-sectional view taken along the center line L1 in the heat transfer mechanism 1 of FIG. 2A. This heat transfer mechanism 1 differs from the case of FIG. 1A and FIG. 1B only in the shape of the heat transfer part 5, and has the same structure about another part. About the structure similar to the case of FIG. 1A and 1B, the same code | symbol is attached | subjected to a figure and detailed description is abbreviate | omitted.

  In this heat transfer mechanism 1, recesses 53 are formed from the side surfaces on both sides of the center line L <b> 1 in the heat transfer unit 5 toward the center line L <b> 1 side. These recesses 53 are formed in the heat transfer portion 5, and one thermal resistance portion 54 is formed along the center line L1 by partially reducing the cross-sectional area in the direction orthogonal to the center line L1. . In this example, the concave portions 53 are formed in the same shape (for example, a rectangular shape), so that the thermal resistance portion 54 is formed so as to be symmetric with respect to the center line L1.

  The thermal resistance portion 54 is formed in, for example, an elongated rod shape parallel to the center line L1. The cross section of the heat resistance portion 54 in the direction perpendicular to the center line L1 has a cross shape, and has a higher strength than that of a simple rectangular cross section. The thermal resistance of the thermal resistance portion 54 can be defined by the cross-sectional area and length of the thermal resistance portion 54.

  In this example, each concave portion 53 is formed so that the thermal resistance portion 54 generates a thermal resistance of 0.1 to 10 K / W, more preferably about 3 K / W. However, the shape of each recess 53 is not limited to a rectangular shape. Further, the shape of the heat resistance portion 54 is not limited to a slender bar shape whose cross section is a cross shape.

  FIG. 3 is a plan view showing a second modification of the heat transfer mechanism 1. This heat transfer mechanism 1 differs from the case of FIG. 1A and FIG. 1B only in the shape of the heat transfer part 5, and has the same structure about another part. About the structure similar to the case of FIG. 1A and 1B, the same code | symbol is attached | subjected to a figure and detailed description is abbreviate | omitted.

  In this heat transfer mechanism 1, a rectangular recess 55 is formed from one side surface across the center line L1 in the heat transfer portion 5 to the vicinity of the other side surface beyond the center line L1. The recess 55 is formed in the heat transfer portion 5 and the cross-sectional area in the direction orthogonal to the center line L1 is partially reduced, so that one heat resistance portion is formed along the other side surface of the heat transfer portion 5. 56 is formed. Thus, the thermal resistance portion may not be formed in an arrangement that is symmetric with respect to the center line L1.

  The thermal resistance portion 56 is formed in, for example, an elongated rod shape parallel to the center line L1. The cross section of the thermal resistance portion 56 in the direction orthogonal to the center line L1 is, for example, rectangular. The thermal resistance of the thermal resistance unit 56 can be defined by the cross-sectional area and length of the thermal resistance unit 56.

  In this example, the concave portion 55 is formed so that the thermal resistance portion 56 generates a thermal resistance of 0.1 to 10 K / W, more preferably about 3 K / W. However, the shape of the recess 55 is not limited to a rectangular shape. Further, the shape of the thermal resistance portion 56 is not limited to a long and narrow bar shape having a rectangular cross section, and the cross section may have another shape such as a cross shape as in the example of FIGS. 2A and 2B. .

  FIG. 4A is a plan view illustrating a configuration example of a thermal analysis apparatus including a heat transfer mechanism 101 according to another embodiment. 4B is a cross-sectional view taken along the center line L101 in the heat transfer mechanism 101 of FIG. 4A.

  The heat transfer mechanism 101 includes a heat transfer member 100 in which a heat sink 102 and a heat transfer portion 105 are integrally formed. Specifically, a cylindrical portion constituting the heat sink 102 is formed so as to protrude upward at an end portion of the flat plate portion constituting the heat transfer portion 105. The heat transfer member 100 is made of, for example, copper. However, the material of the heat transfer member 100 is not limited to copper, and the heat transfer member 100 can be formed of other materials such as silver as long as the material has high thermal conductivity.

  The sample to be measured and the reference material are accommodated in the heat sink 102. A mounting table 121 extending in the horizontal direction is formed in the heat sink 102, and the measurement sample mounting unit 122 and the reference material mounting unit 123 are provided on both sides of the mounting table 121 across the center line L 101. It is provided symmetrically. The measurement sample mounting unit 122 and the reference material mounting unit 123 are formed by, for example, a circular flat surface, and are arranged side by side on a horizontal plane so as to be close to each other.

  In addition to the heat transfer member 100, the heat transfer mechanism 101 includes a heater 103, a cooling source 104, a holding plate 108, and the like. The heater 103 is composed of a sheathed heater, for example, and is configured by housing a heating element such as a nichrome wire with an insulating material sandwiched in a metal tube.

  The heater 103 is provided below the heat transfer member 100 while being wound in a horizontal plane. For example, a holding plate 108 is attached to the heat transfer member 100 from below using a fixing tool such as a fixing screw, and the heater 103 is held between the holding plate 108 and the heat transfer member 100. . As a result, the heat transfer member 100 is heated by the heater 103 so that the sample to be measured and the reference material in the heat sink 102 can be heated. However, the manner in which the heater 103 is attached to the heat transfer member 100 is not limited to the manner in which the holding plate 108 is used, and any other manner can be employed, for example, fixing using a fixing material such as cement. .

  The cooling source 104 is for cooling the heat sink 102 and contains, for example, a refrigerant such as liquid nitrogen. The heat transfer unit 105 of the heat transfer member 100 is connected to the cooling source 104 at one end and integrally formed with the heat sink 102 at the other end, so that heat is transferred between the heat sink 102 and the cooling source 104. Can be communicated. Thus, the heat transfer member 100 is cooled by the cooling source 104, and the sample to be measured and the reference material in the heat sink 102 can be cooled.

  At the time of analysis, as shown in FIG. 4B, the upper end portion of the heat sink 102 is covered with a lid 106. Thermocouples 107 are respectively connected to the back side (lower surface) of the measured sample mounting part 122 and the reference material mounting part 123 in the heat sink 102. Each thermocouple 107 extends in the vertical direction so as to protrude from the lower portion of the heat transfer member 100. By detecting the temperature of the measured sample mounting part 122 and the reference material mounting part 123 via these thermocouples 107, it is possible to measure the calorific difference between the measured sample and the reference material based on the temperature change. it can.

  In the present embodiment, the opening 151 is formed in the heat transfer unit 105, and the cross-sectional area in the direction orthogonal to the center line L101 is partially reduced, so that both sides of the opening 151 in the direction orthogonal to the center line L101. In addition, thermal resistance portions 152 are respectively formed. In this example, a rectangular opening 151 is formed at the center of the heat transfer section 105, so that the two thermal resistance sections 152 are formed so as to be symmetric with respect to the center line L101. .

  The structure of each thermal resistance part 152 is the same as that of the case of FIG. 1A and FIG. 1B, and there can exist an effect similar to this case. In particular, in the present embodiment, since the heat sink 102 and the heat transfer unit 105 are integrally formed, there is no bonding surface between the heat sink 102 and the heat transfer unit 105. For this reason, unevenness in the bonding state is unlikely to occur, and variations in temperature distribution in the heat sink 102 can be more effectively prevented.

  However, the configuration of the thermal resistance unit 152 is not limited to the same configuration as in the case of FIG. 1A and FIG. 1B. For example, the configuration as in FIG. 2A and FIG. 2B or the configuration as in FIG. Various configurations can be adopted.

  FIG. 5 is a cross-sectional view illustrating a configuration example of a thermal analysis apparatus including a heat transfer mechanism 201 according to still another embodiment.

  The heat transfer mechanism 201 includes a heat transfer member 200 in which a heat sink 202 and a heat transfer unit 205 are integrally formed. Specifically, a cylindrical portion constituting the heat sink 202 is formed so as to protrude upward at an end portion of the flat plate portion constituting the heat transfer portion 205. The heat transfer member 200 is made of, for example, copper. However, the material of the heat transfer member 200 is not limited to copper, and the heat transfer member 200 can be formed of other materials such as silver as long as the material has high thermal conductivity.

  The sample to be measured and the reference material are accommodated in the heat sink 202. A mounting table 221 extending in the horizontal direction is formed in the heat sink 202, and the sample mounting unit 222 and the reference material mounting are placed on both sides of the mounting table 221 across a center line (not shown). The placement part 223 is provided symmetrically. The measured sample placing part 222 and the reference material placing part 223 are formed by, for example, circular flat surfaces, and are arranged side by side on a horizontal plane so as to be close to each other.

  In addition to the heat transfer member 200, the heat transfer mechanism 201 includes a heater 203 and a cooling source 204. The heater 203 is composed of, for example, a sheathed heater, and is configured by accommodating a heating element such as a nichrome wire with an insulating material sandwiched in a metal tube. In this example, the heater 203 is attached while being wound around the outer periphery of the heat sink 202. Thereby, the heat sink 202 can be heated by the heater 203, and the sample to be measured and the reference material in the heat sink 202 can be heated.

  The cooling source 204 is for cooling the heat sink 202 and contains, for example, a refrigerant such as liquid nitrogen. The heat transfer unit 205 of the heat transfer member 200 is connected to the cooling source 204 at one end and integrally formed with the heat sink 202 at the other end, so that heat is transferred between the heat sink 202 and the cooling source 204. Can be communicated. Thereby, the heat transfer member 200 is cooled by the cooling source 204, and the sample to be measured and the reference material in the heat sink 202 can be cooled.

  At the time of analysis, the upper end of the heat sink 202 is covered with a lid 206 as shown in FIG. Thermocouples 207 are respectively connected to the back side (lower surface) of the measurement sample mounting part 222 and the reference material mounting part 223 in the heat sink 202. Each thermocouple 207 extends in the vertical direction so as to protrude from the lower portion of the heat transfer member 200. By detecting the temperature of the measured sample mounting part 222 and the reference material mounting part 223 via these thermocouples 207, the calorific difference between the measured sample and the reference material can be measured based on the temperature change. it can.

  In the present embodiment, since the heat sink 202 is formed in a cylindrical shape, a concave portion 251 is formed upward from the bottom surface of the heat sink 202, and the cross-sectional area in the direction perpendicular to the center line L 201 of the heat sink 202 is partially reduced. Has been. As a result, the lower peripheral wall of the heat sink 202 constitutes the thermal resistance portion 252.

  As described above, even when the recess 251 is formed not on the heat transfer unit 205 side but on the heat sink 202 side, the same effects as in the above embodiment can be obtained. However, instead of forming the recess 251 on the heat sink 202 side, a configuration in which an opening is formed may be used. Moreover, the structure in which the opening part or the recessed part was formed in both the heat sink 202 side and the heat-transfer part 205 side may be sufficient.

  In the present embodiment, the configuration in which the heater 203 is wound along the outer periphery of the heat sink 202 has been described. However, the configuration in FIGS. 1A and 1B, the configuration in FIGS. 2A and 2B, the configuration in FIG. In addition, the heater 203 may be wound in a horizontal plane. On the other hand, in the configuration of FIGS. 1A and 1B, the configuration of FIGS. 2A and 2B, or the configuration of FIG. 3, the heater can be wound along the outer periphery of the heat sink. Thus, any other configuration can be adopted as the configuration of the heater.

  Although the case where the heat transfer mechanism according to the present invention is applied to a differential scanning calorimeter has been described in the above embodiment, the present invention can also be applied to a thermal analyzer other than the differential scanning calorimeter. For example, the present invention is applied to various thermal analyzers for performing thermal analysis using a sample to be measured and a reference material, such as a thermal analyzer for observing the surface state of the sample to be measured and a reference material by heating or cooling. The invention can be applied.

DESCRIPTION OF SYMBOLS 1 Heat transfer mechanism 2 Heat sink 3 Heater 4 Cooling source 5 Heat transfer part 6 Cover 7 Thermocouple 21 Mounting base 22 Peripheral wall 23 Flange part 24 Lower plate 51 Opening part 52 Thermal resistance part 53 Concave part 54 Thermal resistance part 55 Concave part 56 Thermal resistance part DESCRIPTION OF SYMBOLS 100 Heat transfer member 101 Heat transfer mechanism 102 Heat sink 103 Heater 104 Cooling source 105 Heat transfer part 106 Cover 107 Thermocouple 108 Holding plate 121 Placement table 122 Measured sample placement part 123 Reference material placement part 151 Opening part 152 Thermal resistance part DESCRIPTION OF SYMBOLS 200 Heat transfer member 201 Heat transfer mechanism 202 Heat sink 203 Heater 204 Cooling source 205 Heat transfer part 206 Lid 207 Thermocouple 211 Measured sample mounting part 212 Reference material mounting part 221 Mounting base 222 Measured sample mounting part 223 Reference material Placement part 251 Concave part 252 Thermal resistance part

Claims (6)

A heat sink containing a sample to be measured and a reference material;
A heater for heating the heat sink;
A cooling source for cooling the heat sink;
A heat transfer unit for transferring heat between the heat sink and the cooling source,
At least one of the heat sink and the heat transfer part is formed with an opening or a recess, and the cross-sectional area is partially reduced to form a heat resistance part ,
The resistance value of the thermal resistance unit is set such that when the heater is energized to a predetermined value, the amount of heat supplied from the heater to the heat sink exceeds the amount of heat released from the heat sink through the heat transfer unit. And
The heat transfer can heat the heat sink by energizing the heater to the predetermined value, and can cool the heat sink by reducing the energization amount to the heater from the predetermined value. mechanism. The heat sink is provided with a measured sample mounting portion on which the measured sample is mounted and a reference material mounting portion on which the reference material is mounted symmetrically with respect to the center line,
The heat transfer mechanism according to claim 1, wherein the thermal resistance portion is formed in an arrangement that is symmetrical with respect to the center line.   The heat transfer mechanism according to claim 1 or 2, wherein the heat sink and the heat transfer portion are integrally formed. The heat transfer mechanism according to claim 1, wherein the thermal resistance portion has a thermal resistance of 0.1 to 10 K / W. A heat sink containing a sample to be measured and a reference material;
A heater for heating the heat sink;
A cooling source for cooling the heat sink;
A heat transfer unit for transferring heat between the heat sink and the cooling source,
At least one of the heat sink and the heat transfer part is formed with an opening or a recess, and the cross-sectional area is partially reduced to form a heat resistance part,
The heat resistance portion has a heat resistance of 0.1 to 10 K / W. A thermal analysis device for performing thermal analysis using a sample to be measured and a reference material,
Thermal analysis apparatus characterized by comprising a heat transfer mechanism according to any of claims 1-5.

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