JP3135983B2 - Sample temperature detector for thermal analyzer - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sample temperature detecting device for a thermal analyzer, and more particularly to a device which can be used as a sample temperature detecting device for a thermal analyzer for examining thermal characteristics in an ultra-high temperature range.

[0002]

2. Description of the Related Art As a thermal analyzer, a differential thermal analyzer (DTA) for simultaneously raising and lowering the temperature of a sample and a standard sample and measuring a temperature difference between the two is measured.
sis) and Differential Scanning Calorimeter (DSC)
ing Calorimeter) or a thermogravimeter (T) that measures the weight change of a sample when the sample is heated or cooled.
G; Thermogravimetry) and the like.

[0003] Incidentally, since these thermal analyzers are for examining the temperature dependence of the thermal change of a sample, all of them are equipped with a sample temperature detecting device for detecting the temperature of the sample.

In this sample temperature detecting device, the method and material of the temperature detecting means are selected according to the temperature range to be measured.
In addition, the structure, material, and the like of the sample mounting portion that holds the sample are selected.

For example, when a thermocouple is used as a temperature detecting means, a platinum thermocouple is usually used up to about 900 ° C., and a platinum rhodium thermocouple is used when the temperature exceeds 1000 ° C. As the temperature range to be measured increases, the usable thermocouple materials are limited, and further,
The structure and the material around the sample holder on which the sample is placed are limited, thereby significantly reducing the degree of freedom in design.

In particular, the temperature range to be measured is from 2000 to 24.
In the ultra-high temperature range of as high as 00 ° C., usable and available thermocouples are actually limited to tungsten rhenium thermocouples. In this temperature range, it is necessary to use an ultra-high temperature heat-resistant member such as tungsten for the structure around the sample holder on which the sample is placed.

The temperature range to be measured is 2000 to 2400 ° C.
Conventionally, as a sample temperature detector that is in the ultra-high temperature region,
There has been proposed a method in which a sample holder is made of tungsten and the sample holder is supported only by a tungsten-rhenium thermocouple.

By the way, the diameter of the thermocouple wire constituting the thermocouple is preferably smaller in order to minimize the amount of heat escaping from the thermocouple wire and improve the measurement accuracy. It is required that the diameter be at most 0.5 mm or less.

However, with a thermocouple wire having a diameter of 0.5 mm or less, sufficient strength to support the sample holder cannot be obtained.

Therefore, conventionally, the inventor of the present application has shown FIG.
A sample temperature detecting device having the structure shown in FIG. FIG.
In the figure, reference numeral 1 denotes a thermosensitive mounting portion for mounting the sample 2, 3 denotes a thermocouple for detecting the temperature of the sample 2,
Is an insulator member, and 5 is a reinforcing pipe.

The heat-sensitive mounting section 1 is composed of a sample holder section 7 in the shape of a saucer, and a cylindrical sample container 8 with a bottom which accommodates the sample 2 and is set on the sample holder section 7. I have. The sample holder 7 has a cylindrical portion 7a through which the thermocouple 3 is inserted so as to protrude at the center of the lower surface. The sample holder 7 is made of tungsten, and the sample container 8 is made of alumina, molybdenum, boron nitride, or the like.

The thermocouple 3 comprises a pair of thermocouple wires 10 and 11 using tungsten rhenium.
Since the load of the thermosensitive mounting portion 1 is supported by the thermocouple 3, of the wires 10 and 11 constituting the thermocouple 3,
One thermocouple wire 10 is a thick wire having a maximum diameter of 0.5 mm, and the other thermocouple wire 11 is a thin wire having a small diameter of 0.1 mm. Thermocouple 3
The pair of strands 10 and 11 are joined to each other by welding 12 at the tip of the wire.

The insulator member 4 controls a pair of thermocouple wires 10 and 11 of the thermocouple 3 by a control unit (these thermocouple wires 1 and 11).
When the temperature difference between the wires 10 and 11 is detected and the detection result is processed, the wires 10 and 11 are held in a predetermined positional relationship.
And a wire guide tube 15 joined to the main body 14. Here, the main body 14 and the wire guide tube 15 are both formed of alumina or the like. The main body 14 has a structure including a guide hole 14a for winding the thin thermocouple wire 11 and a guide tube joining portion 14b into which a distal end portion of the wire guide tube 15 is fitted. ing. Then, the wire guide tube 15 joined to the main body portion 14
Has a guide hole 15a for inserting the thick thermocouple wire 10 and a guide hole 15b for inserting the thin thermocouple wire 11.

Of the pair of thermocouple wires 10 and 11 constituting the thermocouple 3, the thick thermocouple wire 10 is connected to the guide hole 15.
a. On the other hand, a thin thermocouple wire 11
Is wound around the thermocouple wire 10 several times from the joint by the spot welding 12, and then inserted through the guide hole 14 a and wound around the main body portion 14 of the insulator member 4. 10 and then the guide holes 1
5b and guided to a control unit (not shown).

The thermosensitive mounting part 1 is held by the strength of the thick thermocouple element wire 10 by fitting a cylindrical part 7 a provided on the sample holder part 7 to the tip of the thermocouple 3. However, with only the thick thermocouple wire 10, insufficient strength is expected. Therefore, in the case of this conventional example, a structure in which the periphery of the thick thermocouple wire 10 is covered up to the vicinity of the cylindrical portion 7a with the reinforcing pipe 5 joined to the upper part of the insulator member 4 is used. , Thick thermocouple wire 1
0 is prevented from being deformed.

[0016]

However, as shown in FIG.
The conventional sample temperature detecting device described in (1) has a problem that noise is generated when an attempt is made to measure in an ultra-high temperature range. As a cause of this noise, contact due to thermal expansion between the thermocouple wires 10 and 11 constituting the thermocouple 3 can be considered, but it has not been clarified exactly.

Further, in the conventional sample temperature detecting device shown in FIG. 2, there is a problem that the insulator member 4 made of alumina or the like is melted by the radiant heat from the heating means for raising the temperature of the sample 2. .

In general, a thermocouple used in a sample temperature detecting device is liable to break due to fatigue of a thermocouple wire due to repeated high-temperature heating. Therefore, it is strongly demanded that the thermocouple element can be easily replaced when the thermocouple element is cut off.

The present invention has been made in view of the above circumstances, and does not cause inconvenience such as melting of constituent members at the time of measurement in an ultra-high temperature range, does not generate noise, and can smoothly measure the temperature of a sample. It is an object of the present invention to provide a sample temperature detecting device of a thermal analysis device which can be performed and in which a thermocouple serving as a means for detecting a temperature of a sample can be easily replaced.

[0020]

According to a first aspect of the present invention, there is provided a sample temperature detecting apparatus for a thermal analyzer, wherein the temperature of the sample is raised and lowered while measuring the temperature of the sample to observe a thermal change of the sample. A sample holder for mounting the sample, a column for supporting the sample holder at a predetermined position inside a substantially cylindrical heating means, and a tip portion for examining the thermal characteristics of the sample. A thermocouple detachably attached to the holder portion, and an electrode portion provided on the lower side of the sample holder portion for connecting the terminal side of the thermocouple to a control portion for processing a detection signal by the thermocouple, An insulator tube for guiding two thermocouple wires constituting the thermocouple to be separated from each other and leading to the electrode portion side.

Further, the thermocouple wire is detachably attached to the thermocouple wire at the outlet side of the insulator tube, and is guided from the sample holder to the outlet side of the insulator tube by applying tension to the thermocouple wire. And a weight member for preventing the thermocouple element from sagging.

According to a second aspect of the present invention, there is provided a sample temperature detecting device for a thermal analyzer which is an improvement of the sample temperature detecting device of the thermal analyzer according to the first aspect, wherein the sample holder is provided with a pair of thermocouples. A wire insertion hole through which the wire is inserted, and a counterbore portion in which the diameter of the wire insertion hole on the sample mounting side is increased are provided.

Further, the tip of the thermocouple to which the pair of thermocouple wires is joined is formed in a lump having a diameter larger than that of the wire insertion hole.

In the thermocouple, a pair of thermocouple wires are inserted into the wire insertion hole from the upper surface side of the sample holder portion, and the massive tip of the thermocouple is seated on the counterbore portion. Then, the tip of the thermocouple is locked to the sample holder.

According to a third aspect of the present invention, there is provided a sample temperature detecting device for a thermal analyzer which is an improvement of the sample temperature detecting device of the thermal analyzer according to the first or second aspect. And a heat shield plate for suppressing heat transfer from the heating means to the insulator tube.

[0026]

In the sample temperature detecting device of the thermal analyzer according to the first aspect, since the sample holder 31 is supported by a dedicated column, the thermocouple element of the thermocouple serving as the temperature detecting means has a small diameter. By using tungsten rhenium wire,
The measurement accuracy can be improved by preventing heat diffusion from the thermocouple wire. In addition, the thermocouple used has a structure in which the tip is locked to the sample holder and the lower end is pulled by a weight member to prevent the thermocouple element from sagging due to thermal expansion during the measurement process. I have.

Therefore, it is possible to avoid such a disadvantage that adjacent thermocouple wires come into contact with each other due to the occurrence of sag due to thermal expansion to generate noise, thereby enabling smooth temperature measurement without noise. .

Further, in the sample temperature detecting device of the thermal analyzer according to the present invention, each thermocouple can be easily pulled out above the sample holder portion by removing a weight member connected to a lower end portion thereof. In addition to the effects obtained in the first aspect, there is also obtained an effect that the replacement work of the thermocouple becomes extremely easy.

Further, in the sample temperature detecting device of the thermal analyzer according to the third aspect, the heat transfer to the insulator tube can be suppressed by the heat shield plate, and the thermocouple wire having a small diameter is used. Synergistic with the reduction of heat diffusion from the thermocouple wires, it is also possible to prevent inconvenience such as melting of the insulator tube even when using alumina or the like with low heat resistance as the insulator tube .

[0030]

FIG. 1 shows an embodiment of a sample temperature detecting device of a thermal analyzer according to the present invention. In this case, the thermal analyzer according to one embodiment of the present invention is an ultra-high temperature DTA device, and the temperature of the sample is measured while raising and lowering the temperature while observing a thermal change of the sample. The purpose of this study is to examine the thermal characteristics of. The thermal analyzer shown in FIG. 1 includes a sample temperature detecting device 20 for detecting the temperatures of a sample A and a standard sample B using a thermocouple, and a headed cylindrical molybdenum surrounding the sample temperature detecting device 20. And a heating means 22 for heating the specimens A and B located in the heat equalizing cylinder 21 to a predetermined temperature by surrounding the heat equalizing cylinder 21 in a substantially cylindrical shape. A plurality of (in the case of this embodiment, quadruple) walls 23 covering the outer periphery of the heating means 22 in order to prevent the heat of the
A cooling water cooling jacket 24 covering the outer periphery of the partition 23
And these heat equalizing cylinders 21, partition walls 23 and water cooling jackets 2.
And a first block 25 serving as a base for supporting
A predetermined arithmetic process is performed on the basic block 26 to which the block 25 is fixed and the detection signal of the sample temperature detecting device 20 to calculate temperature data on the samples A and B, Water cooling jacket 24
And a recording / display unit 28 for recording and displaying the temperature data and the like calculated by the control unit 27.

The sample temperature detecting device 20 according to one embodiment of the present invention will be described in detail later.
Other configurations in the ultra-high temperature DTA device,
I will add it.

The heat equalizing cylinder 21 is designed such that the samples A and B mounted on the heat-sensitive mounting portion of the sample temperature detecting device 20 are uniformly heated when the heating means 22 heats the sample. The portion (wall) covering the vicinity of the samples A and B is formed thick. The heat equalizing cylinder 21 covers the periphery of the sample temperature detecting device 20 so that the central axis thereof coincides with the central axis of the sample temperature detecting device 20, and the lower end portion of the heat equalizing cylinder 21 is as described above. The first block 25 is fitted and supported.

The heating means 22, as shown in FIG.
A pair of semi-circular plate-shaped tungsten mesh heaters 22a and 22b each having a substantially cylindrical shape by facing each other at a predetermined separation distance, and lower ends of the pair of tungsten mesh heaters 22a and 22b A tungsten ring 22c electrically and physically connected to each other, a tungsten half-ring 22d joined to the upper end of one tungsten mesh heater 22a, and a tungsten ring 22d joined to the half-ring 22d. A tungsten electrode 22e, a tungsten half-ring body 22f joined to the upper end of the other tungsten mesh heater 22b, and a tungsten electrode 22g joined to the half-ring body 22f. By applying a current to the tungsten electrodes 22e and 22g, a predetermined heat is obtained. The heating means 22 is set concentrically with respect to the heat equalizing cylinder 21 from above the partition 23 with the upper lids 23a, 23b, 23c, 23d of the partition 23 open.

In the case of this embodiment, the partition wall 23 has a quadruple structure as described above.
23e, 23f, 23 surrounding concentrically the periphery of
g, 23h, and an upper lid 2 covering the upper part of each of these cylinders
3a, 23b, 23c, and 23d, and bottom plate portions 23i, 23j, 23k, and 23l that cover the lower part of each cylindrical body. The constituent members of the partition wall 23 have high heat resistance, and at least the upper lid portion 23a, the cylindrical body 23e, the bottom plate portion 23i, and the like are made of a material (for example, tungsten, molybdenum, or the like) that can withstand an extremely high temperature region (2000 to 2400 ° C.).
It is formed with.

Next, the sample temperature detecting device 2 according to one embodiment
0 will be described in detail. The sample temperature detecting device 20 includes a heat-sensitive mounting portion 30 for mounting the samples A and B, and the heat-sensitive mounting portion 30 inside the substantially cylindrical heating means 22 (more precisely, the heat equalizing portion). A column 40 that is supported at a predetermined position inside the thermal cylinder 21), and a thermoelectric that is detachably attached to the sample holder portion (the portion indicated by reference numeral 31 in FIGS. Pair 50 and this thermocouple 50
An electrode part 60 provided below the thermosensitive mounting part 30 to connect the end side of the thermocouple to the control part 27, and two kinds of thermocouple wires constituting the thermocouple 50 (FIGS. 7 are indicated by reference numerals 51 and 52). The four insulator tubes 70 are guided to the electrode portion 60 side apart from each other, and are detachably attached to the thermocouple wires at the outlet side of the insulator tubes 70. A weight for preventing the slack of each thermocouple wire led from the sample holder portion of the thermosensitive mounting portion 30 to the outlet side of the insulator tube 70 by applying tension to these thermocouple wires. And a member 80.

Here, as shown in FIGS. 4 and 5, the heat-sensitive mounting section 30 is provided with a sample holder 31 having a tray shape.
A sample container 32 having a bottomed cylindrical shape that accommodates a sample and is placed on the sample holder unit 31, and a flat mounting plate 33 for connecting the sample holder unit 31 to a column 40. The configuration is as follows. The sample holder section 31
The sample container 32 is provided for each of the samples A and B. The mounting plate 33 supports the pair of sample holders 31 from below the sample holders 31 via connecting columns 34.

As shown in FIGS. 6 and 7, the sample holder portion 31 has a wire insertion hole 31a for inserting a pair of thermocouple wires 51 and 52 constituting the thermocouple 50.
And a counterbore 31b having an increased diameter on the sample mounting side (that is, the side on which the sample container 32 is mounted) of the wire insertion hole 31a. Further, although not shown, each sample holder 31 is attached to the mounting plate 33 by three connecting columns 34.
It is connected to. Each connecting column 34 and the sample holder 31
As shown in FIG. 6, the upper end portion (slightly reduced in diameter) of the connecting column 34 is inserted into the connecting column insertion hole 31 c formed in the sample holder portion 31, and further, the connection column insertion hole is formed. The welding is performed by welding the distal end of the connecting column 34 protruding from 31c. In this case, the connecting column 34 is connected so that the distal end portion of the connecting column 34 or the welding wall does not protrude above the mounting surface position of the sample container 32 (the surface position indicated by the arrow (a) in FIG. 6). The size of the upper end portion is selected, and the welding position of the sample holder 31 (the upper surface of the portion where the connecting column 34 is inserted) is formed one step lower than the mounting surface position. Further, the sample holder portion 31 is appropriately provided with a void portion 31d from which unnecessary meat is cut off in order to reduce the heat capacity.

The mounting plate 33 has a substantially disk shape as a whole. As shown in FIG. 6, the two sample holders 31 are supported by three connecting columns 34, respectively. At a position directly below the center of the portion 31, a large diameter wire insertion hole 33a for inserting the thermocouple 50 is provided, and a central portion of the plate (that is, the two wire insertion holes 33a are formed). In the middle), a pillar fitting hole 33b for fitting the tip (upper end) of the pillar 40 is formed. The connection between each connecting column 34 and the mounting plate 33 is performed as shown in FIG.
As shown in FIG.
The lower end of the connecting post 34 (slightly reduced in diameter) is inserted through the connecting post 34c, and the distal end of the connecting post 34 projecting downward from the connecting post insertion hole 33c is welded.

Each of the connecting columns 34 is provided with the sample holder 3.
In order to prevent heat from escaping from 1 to the mounting plate 33, the one having a diameter as small as possible is designed.

It is necessary to select a material for each component of the heat-sensitive mounting section 30 so as to withstand measurement in an ultra-high temperature range. In this embodiment, the sample holder section 31 and the Sample container 32 and connecting column 34
Are all made of tungsten, and the mounting plate 33 is made of tungsten or molybdenum. The strut 40 is a bar made of molybdenum having sufficient mechanical strength to support the heat-sensitive mounting portion 30. As shown in FIG. 1, the tip end (upper end) of the strut 40 is formed of the mounting plate 33. The mounting plate 3 fits into the support hole 33b and is welded.
3. The lower end of the column 40 is inserted through the opening 25a at the center of the first block 25, and is connected to a support block 90 located below the first block 25. The support block 90 is provided with the insulator tube 70 described above.
And has a block body 90a and a substrate 90b joined to the lower surface of the block body 90a. The support block 90 is fixed to a support board 91 attached to the base block 26 via a connecting column (not shown). That is, the column 40 is supported by the support substrate 9.
1 and supports the sample holder 31 at a predetermined position via a mounting plate 33 and a connecting column 34.

The thermocouple 50 includes a pair of thermocouple wires 5.
1, 52, a tungsten rhenium wire having a small diameter is used. Each of the pair of thermocouple wires 51 and 52 has a diameter of 0.2 mm, but one thermocouple wire 51 has a rhenium content of 5% and the other thermocouple wire 52 has a content of 5%.
Has a rhenium content of 26%. As shown in FIG. 7, the distal end of the thermocouple 50 to which the pair of thermocouple wires 51 and 52 is joined has a massive (spherical) shape having a diameter larger than the wire insertion hole 31 a of the sample holder 31. ) Is formed. Accordingly, as shown in FIGS. 6 and 7, the pair of thermocouple wires 51 and 52 of the thermocouple 50 are inserted into the wire insertion holes 31 a from the upper surface side of the sample holder portion 31, and the thermocouple 50 is inserted. Of the lump-shaped tip of the counterbore 31b
, The tip of the thermocouple 50 is locked to the sample holder 31. The thermocouple wires 51, 52 inserted through the wire insertion holes 31a are, as shown in FIG.
In a state where they are separated from each other, the wire is inserted through the wire insertion hole 33a of the mounting plate 33, is passed through the insulator tube 70 located below the wire, and is connected to the electrode portion 60 provided at the lower end side of the insulator tube 70.

As shown in FIG. 8, the electrode section 60 electrically connects each thermocouple wire T and the corresponding lead wire R from the control section 27 by using a set screw 62 screwed to the electrode main body 61. Connected to a single thermocouple wire
In total, four electrode units 60 are provided. Further, these four electrode portions 60 are mounted on the weight member 80 having a substantially ring shape.

The insulator tube 70 is a straight tube made of alumina.
One thermocouple wire is provided for one wire.
Therefore, the sample temperature detecting device 20 is provided with four insulator tubes 70, and each insulator tube 70 is fixed to the support block 90 with its lower end portion penetrating the support block 90. ing.

As shown in FIG. 1, heat from the heating means 22 surrounds these insulator tubes 70.
A heat shield 94 is provided to suppress transmission to zero. The heat shield plates 94 are provided at appropriate intervals from above the upper end of the insulator tube 70 at appropriate intervals. As shown in FIG. 5, each heat shield plate 94 is provided with an opening 94a through which the insulator tube 70 or the thermocouple wire is inserted.

In the sample temperature detecting device 20 as described above, since the thermosensitive mounting portion 30 is supported by the dedicated support 40, the thermocouple wires 51 and 52 of the thermocouple 50 serving as temperature detecting means have small diameters. By using tungsten rhenium wire,
The measurement accuracy can be improved by preventing heat diffusion from the thermocouple wires 51 and 52.

The thermocouple 50 used has its tip locked to the sample holder 31 and the electrode 60
The lower end connected to the thermocouple is pulled by the weight member 80 to prevent the thermocouple wire from sagging due to thermal expansion during the measurement process. Therefore, it is possible to avoid a disadvantage that adjacent thermocouple wires come into contact with each other due to the occurrence of sag due to thermal expansion to generate noise.

Further, if the weight member 80 connected to the lower end of the thermocouple 50 is removed, the thermocouple 50 can be easily pulled out above the sample holder 31 and the replacement work of the thermocouple 50 becomes easy. .

Further, as in the above-described embodiment, the insulator tube 7
0, a heat shield plate 94 is provided around the heat shield plate 94, heat transfer to the insulator tube 70 can be suppressed by the heat shield plate 94, and a thermocouple element having a small diameter is used as a thermocouple element wire. In synergy with the reduction of heat diffusion from the strand, the insulator tube 70
Even when alumina or the like having low heat resistance is used, it is expected that problems such as melting of the insulator tube 70 can be prevented.

When the present inventor actually conducted an experiment, it was found that, in one embodiment, despite the measurement in an ultra-high temperature region,
There was no inconvenience such as melting of the alumina insulator tube 70, and the temperature of the sample could be smoothly measured without generating noise. Further, the thermocouple could be replaced very easily.

In one embodiment, the lump of the tip of the thermocouple 50 is seated on the counterbore 31b of the sample holder 31 so that the tip of the thermocouple 50 is connected to the sample holder 3.
1, but it is only necessary that the attachment / detachment can be easily performed. The specific structure for locking the tip of the thermocouple 50 to the sample holder 31 is not limited to the above-described embodiment. . For example, a structure in which a hook or the like that locks the distal end of the thermocouple 50 protrudes from the bottom of the sample holder 31 can be used.

[0051]

According to the sample temperature detecting device of the thermal analyzer according to the present invention, since the sample holder 31 is supported by a dedicated support, the thermocouple wire of the thermocouple serving as the temperature detecting means is thin. By using a tungsten rhenium wire having a diameter, heat diffusion from a thermocouple wire can be prevented, and measurement accuracy can be improved. In addition, the thermocouple used has a structure in which the tip is locked to the sample holder and the lower end is pulled by a weight member to prevent the thermocouple element from sagging due to thermal expansion during the measurement process. I have.

Therefore, it is possible to avoid the disadvantage that adjacent thermocouple wires come into contact with each other due to the occurrence of sag due to thermal expansion to generate noise, and it is possible to perform noise-free and smooth temperature measurement. .

In the sample temperature detecting device of the thermal analyzer according to the present invention, each thermocouple can be easily pulled out above the sample holder portion by removing a weight member connected to a lower end portion thereof. In addition to the effects obtained in the first aspect, there is also obtained an effect that the replacement work of the thermocouple becomes extremely easy.

Further, in the sample temperature detecting device of the thermal analyzer according to the third aspect, the heat transfer to the insulator tube can be suppressed by the heat shield plate, and the thermocouple wire having a small diameter is used. Synergistic with the reduction of heat diffusion from the thermocouple wires, it is also possible to prevent inconvenience such as melting of the insulator tube even when using alumina or the like with low heat resistance as the insulator tube .

[Brief description of the drawings]

FIG. 1 is an overall configuration diagram of an embodiment of the present invention.

FIG. 2 is a configuration diagram of a conventional sample temperature detecting device.

FIG. 3 is a perspective view of a heating means in a conventional thermal analyzer.

FIG. 4 is an enlarged view of a main part in FIG.

FIG. 5 is a sectional view taken along line II of FIG. 4;

FIG. 6 is a detailed view of a sample holder according to one embodiment of the present invention.

FIG. 7 is an enlarged view of a sample holder section according to one embodiment of the present invention.

FIG. 8 is an enlarged view of a weight member according to one embodiment of the present invention.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 21 Heat equalizing cylinder 22 Heating means 30 Heat-sensitive mounting part 31 Sample holder part 31a Element wire insertion hole 31b Counterbore part 32 Sample container 33 Mounting plate 34 Connecting column 40 Support column 50 Thermocouple 51, 52 Thermocouple element wire 60 Electrode part 70 Insulator tube 80 Weight member 94 Heat shield plate

Claims (3)

(57) [Claims] 1. A method for measuring the temperature of a sample while raising the sample.
A sample temperature detecting device of a thermal analysis device for examining thermal characteristics of a sample by lowering the temperature and observing a thermal change of the sample, comprising: a sample holder portion for mounting the sample; and a sample holder portion. A column supported at a predetermined position inside the substantially cylindrical heating means; a thermocouple having a tip detachably attached to the sample holder; and a control unit for processing a detection signal by the thermocouple. An electrode portion provided on the lower side of the sample holder portion for connecting a terminal side, and an insulator tube for guiding two thermocouple wires constituting the thermocouple away from each other and leading to the electrode portion side, At the outlet side of the insulator tube, the thermocouple wire is detachably attached to the thermocouple wire, and tension is applied to the thermocouple wire so that the thermocouple wire is guided from the sample holder portion to the insulator tube outlet side. Sagging Sample temperature detector thermal analysis apparatus characterized by comprising a weight member for preventing. 2. The sample holder section includes a wire insertion hole through which a pair of thermocouple wires are inserted, and a counterbore portion having an increased diameter on the sample mounting side of the wire insertion hole. On the other hand, the tip of the thermocouple to which the pair of thermocouple wires is joined is formed in a lump having a diameter larger than the wire insertion hole, and the thermocouple is formed by forming the pair of thermocouple wires into the sample. The distal end of the thermocouple is locked to the sample holder by inserting the bulk end of the thermocouple into the counterbore by inserting the distal end of the thermocouple into the counterbore by inserting the strand through the strand insertion hole from the upper surface side of the holder. The sample temperature detecting device for a thermal analyzer according to claim 1, wherein: 3. The thermal analysis according to claim 1, wherein a heat shield plate for suppressing heat transfer from the heating means to the insulator tube is provided around the insulator tube. Sample temperature detector of the device.