JPH063301A - Sample temperature detector for thermal analyzer - Google Patents

Abstract

PURPOSE:To prevent the occurrence of noise and, at the same time, to easily exchange a thermocouple being used as a sample temperature detecting means with another thermocouple. CONSTITUTION:The detector is provided with a column 40 which supports a sample holder section 31, thermocouple 50 the front end of which is fitted to the section 31 in a removable state, insulator tubes 70 which separately lead two kinds of thermocouple element wires constituting the thermocouple 50, and weight members 80 which give tension to the element wires on the exit sides of the tubes 70. In addition, the thermocouple 50 is set in such a state that it can he pulled up from the section 31 and thermal insulation plates 94 are put around the tubers 70.

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 analysis device, and more particularly to a device that can be used as a sample temperature detecting device for a thermal analysis device for examining thermal characteristics in an ultrahigh temperature range.

[0002]

2. Description of the Related Art As a thermal analysis device, a differential thermal analysis device (DTA; Differential Thermal Analysis) which measures the temperature difference between a sample and a standard sample by raising and lowering the temperature at the same time.
sis) and differential scanning calorimeter (DSC)
ing Calorimeter) or a thermogravimetric measuring device (T) for measuring the weight change of the sample when the sample is heated or cooled.
G; Thermogravimetry) and the like are known.

By the way, since these thermal analyzers are for investigating the temperature dependence of the thermal change of the sample, they are each 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, etc. of the sample mounting portion that holds the sample are selected.

For example, when a thermocouple is used as the temperature detecting means, a platinum pin 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 material around the sample holder on which the sample is placed are limited, which significantly narrows the degree of freedom in design.

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

The temperature range to be measured is 2000-2400 ° C.
As a sample temperature detection device that becomes the ultra-high temperature region of
A method has been proposed in which the sample holder part is made of tungsten and the sample holder part is supported only by a rhenium tungsten thermocouple.

By the way, it is preferable that the wire diameter of the thermocouple wire constituting the thermocouple is smaller because the amount of heat escaped from the thermocouple wire is minimized to improve the measurement accuracy. The maximum diameter is required to be 0.5 mm or less.

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

Therefore, conventionally, according to the present inventor, FIG.
A sample temperature detecting device having the structure shown in Fig. 1 has been proposed. Figure 2
In FIG. 1, reference numeral 1 is a heat-sensitive mounting portion for mounting the sample 2, 3 is a thermocouple for detecting the temperature of the sample 2, 4
Is an insulator member and 5 is a reinforcing pipe.

The heat-sensitive mounting part 1 is composed of a sample holder part 7 in the shape of a saucer, and a cylindrical sample container 8 with a bottom, which accommodates the sample 2 and is installed on the sample holder part 7. There is. The sample holder part 7 has a shape in which a tubular part 7a for inserting the thermocouple 3 is projectingly provided in the center part of the lower surface thereof. The sample holder portion 7 is made of tungsten, and the sample container 8 is made of alumina, molybdenum, boron nitride, or the like.

The thermocouple 3 is composed of a pair of thermocouple wires 10 and 11 using tungsten rhenium.
Since the load of the heat-sensitive mounting part 1 is supported by the thermocouple 3, among the wires 10 and 11 forming the thermocouple 3,
One of the thermocouple wires 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
At the tip of the wire, the pair of strands 10 and 11 are joined by welding 12.

The insulator member 4 controls the pair of thermocouple wires 10 and 11 of the thermocouple 3 to be a control section (the thermocouple wires 1 and 2).
When the temperature difference between 0 and 11 is detected and the detection result is processed), the wires 10 and 11 are held in a predetermined positional relationship with each other.
And a wire guide tube 15 joined to the main body portion 14. Here, both the main body portion 14 and the wire guide tube 15 are made of alumina or the like. Further, the main body portion 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 the tip 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 structure having 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 forming the thermocouple 3, the thick thermocouple wire 10 is the guide hole 15
It is deployed by inserting a. On the other hand, a thin thermocouple wire 11
Is wound around the thick thermocouple wire 10 several times from the joint portion by the spot welding 12, and then inserted into the guide hole 14a and wound around the main body portion 14 of the insulator member 4 so that the thick thermocouple wire is wound. 10 and then the guide hole 1
It is inserted into 5b and guided to a control unit (not shown).

The thermosensitive mounting portion 1 is held by the strength of the thick thermocouple wire 10 by fitting the tubular portion 7a provided on the sample holder portion 7 into the tip portion of the thermocouple 3. However, it is expected that the strength will be insufficient only with the thick thermocouple wire 10. Therefore, in the case of this conventional example, a structure in which the circumference of the thick thermocouple wire 10 is covered with the reinforcing pipe 5 joined to the upper portion of the insulator member 4 up to the vicinity of the cylindrical portion 7a, the strength of the reinforcing pipe 5 is increased. , Thick thermocouple wire 1
It prevents the deformation of 0.

[0016]

However, the above-mentioned FIG.
The conventional sample temperature detecting device shown in (1) has a problem that noise is generated when the measurement is performed in an ultrahigh temperature region. The cause of this noise may be contact due to thermal expansion of the thermocouple wires 10 and 11 forming the thermocouple 3, 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 radiant heat from the heating means for raising the temperature of the sample 2 causes the insulator member 4 and the like made of alumina to melt. .

Further, in general, a thermocouple used in a sample temperature detecting device is repeatedly heated at a high temperature, so that the thermocouple wire is easily fatigued and easily cut. Therefore, it is also strongly desired that the thermocouple wire can be easily replaced when it is cut.

The present invention has been made in view of the above circumstances, and does not cause inconvenience such as melting of constituent members during measurement in an ultrahigh temperature region, and does not generate noise, so that the temperature of a sample can be smoothly measured. It is an object of the present invention to provide a sample temperature detecting device of a thermal analysis device which can be carried out and can easily replace a thermocouple which is a means for detecting the temperature of a sample.

[0020]

A sample temperature detecting device of a thermal analysis device according to claim 1 raises and lowers the temperature of the sample while observing the temperature of the sample to observe a thermal change of the sample. In order to investigate the thermal characteristics of a sample, a sample holder part for mounting the sample, a column for supporting the sample holder part at a predetermined position inside a substantially cylindrical heating means, and a tip part of the sample A thermocouple removably attached to the holder part, and an electrode part provided on the lower side of the sample holder part for connecting the end side of the thermocouple to a control part for processing a detection signal by the thermocouple, An insulator tube that guides the two types of thermocouple wires forming the thermocouple to the electrode portion side while separating them from each other.

Further, it is detachably attached to the thermocouple wire at the outlet side of the insulator tube and is guided from the sample holder part to the outlet side of the insulator tube by applying tension to the thermocouple wire. And a weight member that prevents the slack from occurring in the thermocouple element.

A sample temperature detecting device for a thermal analyzer according to a second aspect is an improvement of the sample temperature detecting device for a thermal analyzer according to the first aspect, wherein a pair of thermocouples are provided in the sample holder portion. An element wire insertion hole for inserting an element wire and a counterbore part having a larger diameter on the sample mounting side of the element wire insertion hole are provided.

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

In the thermocouple, a pair of thermocouple wires are inserted from the upper surface side of the sample holder into the wire insertion holes, and the lumpy tip of the thermocouple is seated on the counterbore. By doing so, the tip of the thermocouple is locked to the sample holder.

The sample temperature detecting device of the thermal analysis device described in claim 3 is an improvement of the sample temperature detecting device of the thermal analysis device according to claim 1 or 2, wherein the sample temperature detecting device is provided around the insulator tube. A heat shield plate for suppressing heat transfer from the heating means to the insulator tube is provided.

[0026]

In the sample temperature detecting device of the thermal analysis apparatus according to the first aspect, since the sample holder 31 is supported by the dedicated column, the thermocouple wire of the thermocouple which is the temperature detecting means has a small diameter. By using tungsten rhenium wire,
It is possible to prevent heat diffusion from the thermocouple wire and improve the measurement accuracy. Moreover, the thermocouple used has a structure in which the tip end is locked to the sample holder part and the lower end side is pulled by the weight member to prevent slack in the thermocouple wire due to thermal expansion during the measurement process. There is.

Therefore, it is possible to avoid the inconvenience that adjacent thermocouple wires come into contact with each other due to the occurrence of slack due to thermal expansion and noise is generated, and smooth temperature measurement without noise can be performed. .

Further, in the sample temperature detecting device of the thermal analyzer according to the second aspect, each thermocouple can be easily pulled out above the sample holder part by removing the weight member connected to the lower end part thereof. In addition to the effect obtained in the first aspect, the effect that the thermocouple replacement work becomes extremely easy can be obtained.

Further, in the sample temperature detecting device of the thermal analyzer according to the third aspect, heat transfer to the insulator tube can be suppressed by the heat shield plate, and the thermocouple wire having a small diameter is used. Synergistically with the reduction of heat diffusion from the thermocouple element, it is possible to prevent the occurrence of inconveniences such as melting of the insulator tube even when alumina, which has low heat resistance, is used as the insulator tube. .

[0030]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS 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 analysis apparatus according to one embodiment of the present invention is an ultrahigh temperature DTA apparatus, and the temperature of the sample is raised and lowered while observing the thermal change of the sample. To investigate the thermal characteristics of. The thermal analyzer shown in FIG. 1 uses a thermocouple to detect the temperature of the sample A and the standard sample B, and a head-shaped cylindrical molybdenum molybdenum surrounding the sample temperature detector 20. From the heating means 22, a soaking tube 21 made of metal, a heating means 22 for enclosing the circumference of the soaking tube 21 in a substantially cylindrical shape and heating the samples A and B located in the soaking tube 21 to a predetermined temperature. A partition wall 23 in which the outer circumference of the heating means 22 is multi-layered (in the case of this embodiment, four layers) to prevent the heat of the above from diffusing to the outside,
A water cooling jacket 24 for cooling that covers the outer periphery of the partition wall 23.
And these soaking cylinder 21, partition wall 23 and water cooling jacket 2
The first block 25 serving as a base for supporting the 4 and the first block 25
A predetermined calculation process is performed on the detection signal of the sample temperature detecting device 20 and the basic block 26 to which the block 25 is fixed to calculate the temperature data on the samples A and B, and the heating operation by the heating means 22. Water cooling jacket 24
The control unit 27 controls the cooling operation by the control unit 27, and the recording / display unit 28 that records and displays the temperature data calculated by the control unit 27.

The sample temperature detecting device 20 according to an embodiment of the present invention will be described in detail later.
Regarding other configurations in the ultra-high temperature DTA device,
I will supplement.

The soaking cylinder 21 is designed so that the samples A and B mounted on the heat-sensitive mounting part of the sample temperature detecting device 20 are heated uniformly when heated by the heating means 22. The portion (wall portion) covering the vicinity of the samples A and B is formed thick. Further, the soaking 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 soaking cylinder 21 is as described above. The first block 25 is fitted and supported.

The heating means 22 is, as shown in FIG.
A pair of semi-arcuate plate-shaped tungsten mesh heaters 22a, 22b having a substantially cylindrical shape by facing each other with a predetermined separation distance, and the lower ends of the pair of tungsten mesh heaters 22a, 22b. A ring 22c made of tungsten electrically and physically connected to each other, a half ring body 22d made of tungsten joined to the upper end of one tungsten mesh heater 22a, and a half ring body 22d joined to this half ring body 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. A predetermined amount of heat is obtained by energizing the tungsten electrodes 22e and 22g of No. The heating means 22 is set concentrically with the heat equalizing cylinder 21 from the upper side of the partition wall 23 in a state where the upper lid portions 23a, 23b, 23c and 23d of the partition wall 23 are opened.

In the case of this embodiment, the partition wall 23 has a quadruple structure as described above, and the heating means 22.
Cylindrical bodies 23e, 23f, 23 concentrically surrounding the circumference of
g, 23h and an upper lid portion 2 for 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 portion 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 materials (for example, tungsten or molybdenum) capable of withstanding an ultrahigh temperature region (2000 to 2400 ° C).
Is formed by.

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 part 30 for mounting the samples A and B, and the heat-sensitive mounting part 30 inside the heating means 22 having a substantially cylindrical shape. A column 40 that supports a predetermined position of the inside of the heat tube 21 and a thermoelectric element whose tip portion is detachably attached to the sample holder portion (the portion indicated by reference numeral 31 in FIGS. 4 to 6) of the heat-sensitive mounting portion 30. Pair 50 and this thermocouple 50
Two types of thermocouple wires (FIG. 5 and FIG. 5) that constitute the thermocouple 50, and an electrode section 60 provided below the thermosensitive mounting section 30 to connect the terminal side of the thermocouple to the control section 27. 7 are denoted by reference numerals 51 and 52) and four insulator tubes 70 which are separated from each other and are guided to the electrode portion 60 side, and detachably attached to the thermocouple wires on the outlet side of these insulator tubes 70. By applying tension to these thermocouple wires, it is possible to prevent the slack from occurring in each thermocouple wire guided from the sample holder part of the heat-sensitive mounting part 30 to the outlet side of the insulator tube 70. And a member 80.

As shown in FIGS. 4 and 5, the heat-sensitive mounting section 30 has a saucer-shaped sample holder section 31.
And a bottomed cylindrical sample container 32 that accommodates a sample and is placed on the sample holder portion 31, and a flat plate-shaped mounting plate 33 for connecting the sample holder portion 31 to a support column 40. It has been configured. The sample holder part 31
The sample container 32 is provided for each of the samples A and B. The mounting plate 33 supports the pair of sample holder portions 31 from the lower side of the sample holder portions 31 via the connecting posts 34.

As shown in FIGS. 6 and 7, the sample holder portion 31 has a wire insertion hole 31a through which a pair of thermocouple wires 51 and 52 forming the thermocouple 50 are inserted.
And a counterbore portion 31b in which the hole diameter of the wire insertion hole 31a on the sample mounting side (that is, the side on which the sample container 32 is mounted) is expanded. Although not shown, each sample holder unit 31 includes three connecting columns 34 and a mounting plate 33.
Are linked to. Each connection pillar 34 and sample holder 31
As shown in FIG. 6, the upper end portion (a slightly reduced diameter) of the connection column 34 is inserted into the connection column insertion hole 31c formed in the sample holder portion 31, and the connection column insertion hole is further connected. This is done by welding the tip end of the connecting column 34 protruding from 31c. In this case, the tip of the connecting column 34 or the weld beading 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 welded portion of the sample holder portion 31 (the upper surface of the portion through which the connecting column 34 is inserted) is also formed one step lower than the mounting surface position described above. Moreover, in order to reduce the heat capacity, the sample holder portion 31 is appropriately provided with a void portion 31d in which unnecessary meat is shaved off.

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

The above-mentioned connecting columns 34 are used for the sample holder 3
In order to prevent the heat from escaping from 1 to the mounting plate 33, those having a diameter as small as possible are designed.

It is necessary to select the materials of the respective constituent members of the heat-sensitive mounting section 30 so as to withstand the measurement in the ultrahigh temperature region. In the case of this embodiment, the sample holder section 31 and Sample container 32 and connecting column 34
Both use tungsten, and the mounting plate 33 uses tungsten or molybdenum. The support column 40 is a molybdenum rod having a mechanical strength sufficient to support the heat-sensitive mounting section 30, and the tip end (upper end) of the support column 40 is attached to the mounting plate 33 as shown in FIG. The mounting plate 3 is fitted to the support column fitting hole 33b and welded.
It is joined to 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 the support block 90 located below the opening 25a. This support block 90 is equivalent to the above-mentioned insulator tube 70.
The block main body 90a and the substrate 90b joined to the lower surface of the block main body 90a are also provided. The support block 90 is fixed to a support substrate 91 attached to the base block 26 via a connecting column (not shown). That is, the pillar 40 is the support substrate 9
1, the sample holder portion 31 is supported at a predetermined position via a mounting plate 33 and a connecting post 34.

The thermocouple 50 is a pair of thermocouple wires 5.
As 1, 52, thin tungsten rhenium wires are 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 rhenium content of 26%. Further, as shown in FIG. 7, the tip end of the thermocouple 50 to which the pair of thermocouple wires 51 and 52 are joined has a lump shape (spherical shape) having a diameter larger than that of the wire insertion hole 31 a of the sample holder 31. ) Is formed. Therefore, 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 hole 31 a from the upper surface side of the sample holder portion 31, and the thermocouple 50 is inserted. The block-shaped tip of the counterbore 31b
The tip end portion of the thermocouple 50 is locked to the sample holder portion 31 by being seated on. The thermocouple wires 51 and 52 inserted through the wire insertion holes 31a are, as shown in FIG.
The element wires are inserted into the wire insertion holes 33a of the mounting plate 33 in a state of being separated from each other, passed through the insulator tube 70 located therebelow, and connected to the electrode portion 60 arranged at the lower end side of the insulator tube 70.

As shown in FIG. 8, the electrode unit 60 electrically connects each thermocouple wire T and the corresponding lead wire R from the control unit 27 by using a set screw 62 screwed to the electrode body 61. The structure that is connected to the
A total of four electrode parts 60 are provided at a rate of each. The 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,
Equipped with one thermocouple wire for every one.
Therefore, although the sample temperature detecting device 20 is equipped with four insulator tubes 70, each insulator tube 70 is fixed to the support block 90 with its lower end penetrating the support block 90. ing.

In addition, as shown in FIG. 1, the heat from the heating means 22 surrounds the insulator tubes 70 around the insulator tubes 70.
A heat shield plate 94 is provided to suppress the transmission to zero. The heat shield plates 94 are arranged in appropriate numbers from above the upper end of the insulator tube 70 at appropriate intervals. Further, as shown in FIG. 5, each heat shield plate 94 is provided with an opening 94a for inserting the insulator tube 70 or the thermocouple wire.

In the sample temperature detecting device 20 as described above, since the heat-sensitive mounting portion 30 is supported by the dedicated support column 40, the thermocouple wires 51 and 52 of the thermocouple 50, which is the temperature detecting means, have small diameters. By using tungsten rhenium wire,
It is possible to prevent heat diffusion from the thermocouple wires 51 and 52 and improve the measurement accuracy.

The tip of the thermocouple 50 used is locked to the sample holder section 31 and the electrode section 60 is used.
The lower end side connected to is pulled by the weight member 80 to prevent slack in the thermocouple wire due to thermal expansion during the measurement process. Therefore, it is possible to avoid the inconvenience that adjacent thermocouple wires come into contact with each other due to the occurrence of slack due to thermal expansion and noise is generated.

Further, each thermocouple 50 can be easily pulled out above the sample holder portion 31 by removing the weight member 80 connected to the lower end portion thereof, and the replacement work of the thermocouple 50 is facilitated. .

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

When the present inventor actually conducted an experiment, in one example, despite the measurement in the ultrahigh temperature region,
It was possible to smoothly measure the temperature of the sample without the disadvantage that the insulator tube 70 made of alumina was melted, and without generating noise, and it was also possible to replace the thermocouple very easily.

In one embodiment, the tip end of the thermocouple 50 is seated on the counterbore 31b of the sample holder 31 so that the tip of the thermocouple 50 is held by the sample holder 3.
However, the specific structure for locking the tip of the thermocouple 50 to the sample holder part 31 is not limited to the one embodiment described above. . For example, a structure in which a hook for locking the tip of the thermocouple 50 is provided on the bottom of the sample holder 31 in a protruding manner can be used.

[0051]

In the sample temperature detecting device of the thermal analyzer according to the first aspect of the invention, since the sample holder 31 is supported by the dedicated prop, the thermocouple wire of the thermocouple which is the temperature detecting means is thin. By using a tungsten rhenium wire having a diameter, it is possible to prevent heat diffusion from the thermocouple wire and improve the measurement accuracy. Moreover, the thermocouple used has a structure in which the tip end is locked to the sample holder part and the lower end side is pulled by the weight member to prevent slack in the thermocouple wire due to thermal expansion during the measurement process. There is.

Therefore, it is possible to avoid the inconvenience that the adjacent thermocouple wires come into contact with each other due to the occurrence of the slack due to the thermal expansion and the noise is generated, and the smooth temperature measurement without noise can be performed. .

Further, in the sample temperature detecting device of the thermal analysis device according to the second aspect, each thermocouple can be easily pulled out above the sample holder part by removing the weight member connected to the lower end part thereof. In addition to the effect obtained in the first aspect, the effect that the thermocouple replacement work becomes extremely easy can be obtained.

Further, in the sample temperature detecting device of the thermal analyzer according to the third aspect, heat transfer to the insulator tube can be suppressed by the heat shield plate, and the thermocouple wire having a small diameter is used. Synergistically with the reduction of heat diffusion from the thermocouple element, it is possible to prevent the occurrence of inconveniences such as melting of the insulator tube even when alumina, which has low heat resistance, is used as the insulator tube. .

[Brief description of 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 heating means in a conventional thermal analysis device.

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

5 is a cross-sectional view taken along line I-I of FIG.

FIG. 6 is a detailed view of a sample holder unit in one embodiment of the present invention.

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

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

[Explanation of symbols]

 Reference Signs List 21 heat equalizing tube 22 heating means 30 heat-sensitive mounting section 31 sample holder section 31a element wire insertion hole 31b counterbore section 32 sample container 33 mounting plate 34 connecting column 40 column 50 thermocouple 51, 52 thermocouple element 60 electrode section 70 Insulator tube 80 Weight member 94 Heat shield

Claims (3)

[Claims] 1. Raising the sample while measuring the temperature of the sample
A sample temperature detecting device of a thermal analysis device for examining the thermal characteristics of a sample by observing a thermal change of the sample by lowering the temperature, and a sample holder part for mounting the sample, and the sample holder part. A column that supports a predetermined position inside the substantially cylindrical heating unit, a thermocouple whose tip is detachably attached to the sample holder unit, and a control unit that processes a detection signal from the thermocouple. An electrode portion provided on the lower side of the sample holder portion for connecting the terminal side, and an insulator tube that guides the two types of thermocouple wires forming the thermocouple to the electrode portion side while separating them from each other, Attached to the thermocouple wire detachably on the outlet side of the insulator tube, and applying a tension to the thermocouple wire, to the thermocouple wire guided from the sample holder part to the outlet side of the insulator tube. Sagging may occur Sample temperature detector thermal analysis apparatus characterized by comprising a weight member for preventing. 2. The sample holder part is provided with a wire insertion hole for inserting a pair of thermocouple wires, and a spot facing part in which the diameter of the wire insertion hole on the sample mounting side is expanded. Provided, on the other hand, the tip of the thermocouple to which the pair of thermocouple wires are joined is formed in a lump having a diameter larger than the wire insertion hole, and the thermocouple is a pair of thermocouple wires. The tip end of the thermocouple is locked to the sample holder part by inserting it from the upper surface side of the holder part into the wire insertion hole and seating the block-shaped tip part of the thermocouple on the counterbore part. The sample temperature detecting device of the thermal analysis device 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. Instrument sample temperature detector.