JPH10123073A - Thermomechanical analyzer - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a thermomechanical analyzer(TMA) by which a sample is replaced automatically and by which a researcher is liberated from a complicated sample replacement operation. SOLUTION: An analyzer is constituted so as to be provided with a sample stage 32 on which many required samples S can be arranged, with a gripping means 40 which groups every sample S and with a conveyance means 30 by which the gripping means 40 is conveyed between a sample arrangement part 5 and the sample stage 32. In this case, every sample S on the sample stage 32 is gripped by the gripping means 40, and the gripping means 40 is arranged automatically to the sample arrangement part 5 in the analyzer.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a thermomechanical analysis (TMA) that can be used to determine how the mechanical properties of a substance change with temperature.
More particularly, it relates to a thermomechanical analyzer capable of automatically changing a sample to be measured.

[0002]

2. Description of the Related Art In a thermomechanical analyzer, a sample disposed in a sample placement section is brought into contact with a displacement transmission means called a detection rod, and deformation of the sample caused by heating is detected by a differential transformer or the like via the detection rod. It is provided with a structure that transmits to the detector (main detector) and measures physical changes such as expansion and compression with respect to the temperature of the sample.

The analysis process using a thermomechanical analyzer can be roughly divided into mounting a sample on a sample mounting portion, collecting and analyzing measurement data, and taking out a sample. Of these, measurement data collection and analysis are performed automatically by computer control, but mounting and removal of a sample (that is, sample replacement work) is generally performed manually and is cumbersome. Was.

Japanese Utility Model Laid-Open Publication No. 64-5153 discloses a device for automatic exchange of samples for a differential thermal analyzer (DTA) which is one of thermal analyzers. As shown in FIG. 9, the automatic sample changing apparatus disclosed in the publication has a hook-shaped exchanger (1) at the tip of a rod (100) that moves up and down.
01), the exchanger (101) rises, holds the sample container (103) disposed at the upper end (102a) of the detection rod (102), and further rises.

[0005] Then, the sample container (103) is placed in the heating furnace (1).
04) at a position above the upper end opening of the exchanger (10).
The rise in 1) stops. Then, by rotating in the direction of arrow A, the bottom of the sample container (103) projecting downward from the exchanger (101) hits the drop plate (105), and the sample container (103) comes off the exchanger (101). And fall.

Next, when the exchanger (101) rotates in the direction of arrow B and stands by at a predetermined sample exchange position, the turntable (106) rises and rotates in the direction of arrow C, and
A new sample container (103) is held in the exchanger (101). Subsequently, the turntable (106) descends,
Further, after the exchanger (101) rotates in the direction of arrow D and places the sample container (103) above the detection rod (102),
The sample container (1) held by the exchanger (101) being lowered.
03) is arranged at the upper end (102a) of the detection rod (102). With the above operation, the sample container is automatically replaced.

[0007]

Problems to be Solved by the Invention
The automatic sample exchange device disclosed in Japanese Patent No. 5153 is intended to be applied to a differential thermal analyzer (DTA) to realize automatic sample exchange. Therefore, it is essentially impossible to apply the automatic sample exchange device disclosed in the publication to a thermomechanical analyzer (TMA) having completely different device structures, sample shapes, sample placement parts, and peripheral structures.

SUMMARY OF THE INVENTION The present invention has been made in view of the above-mentioned circumstances, and realizes automatic exchange of a sample by applying to a thermomechanical analyzer (TMA) to relieve a researcher from complicated sample exchange work. Aim.

[0009]

SUMMARY OF THE INVENTION In order to achieve the above object, the present invention relates to a method for arranging a required sample in a sample arranging portion formed at a distal end portion of a support tube and heating the sample to a predetermined temperature. Stage in which a large number of required samples can be arranged, gripping means for gripping the sample, and transport means for transporting the gripping means between the sample placement unit and the sample stage It is characterized by having.

According to the present invention having such a configuration, the sample on the sample stage can be gripped by the gripping means, and the gripping means can be automatically arranged on the sample placement portion in the thermomechanical analyzer by the transporting means. It becomes possible.

Further, the sample placed on the sample mounting portion of the thermomechanical analyzer after the measurement can be grasped by the grasping means and automatically taken out by the operation of the transport means. Here, the gripping means includes a main body, a plurality of open / close claws which are provided on the main body so as to be openable and closable and cooperate to hold the sample, a driving means for driving these open / close claws to open and close, and any of the above open / close claws. A gripping detection member that moves integrally and a gripping sensor provided at a predetermined position on the main body are provided. When the opening / closing claw moves to a position where the sample is gripped, the gripping detection sensor detects the gripping. It can be configured to detect a member.

[0012] With this configuration of the gripping means, the opening / closing claw is driven by the driving means in the closing direction from the open position,
The opening and closing claws cooperate to grip the sample. When the opening / closing claw moves to a position where the sample is gripped, the gripping confirmation sensor detects the gripping confirmation detecting member, but if the opening / closing claw is not gripping the sample, the opening / closing claw is more than the gripping position. Further, since it moves in the closing direction, the gripping confirmation sensor does not detect the gripping confirmation detecting member.

As described above, it is possible to confirm whether or not the opening / closing claw has grasped the sample based on the detection and non-detection operations of the grasping confirmation detecting member by the grasping confirmation sensor.
The transport of the sample can be realized with high reliability by preventing the transport error.

Since the position where the opening and closing claw grips the sample differs depending on the size of the sample to be transported, the fixed position on the main body of the gripping confirmation sensor corresponds to the gripping position of the sample. It is preferable to be able to adjust arbitrarily.

Further, according to the present invention, when the opening / closing claw or the main body receives pressure from the outside, the holding means is provided with a damper member for buffering the pressure by an expansion / contraction operation, and a predetermined amount of the damper member is acted on by an external force. It is good also as composition provided with the sensor for contact monitoring which detects contraction. The transport destination of the sample in the thermomechanical analyzer, that is, the sample disposition portion is generally a narrow space, and various obstacles exist around the narrow space. Moreover, the sample placement part and the obstacles around it may be formed of a brittle, impact-sensitive material such as a glass material.

When the tip of the opening / closing claw comes into contact with such a sample placement portion or an obstacle around the sample placement portion, the damper member shrinks to buffer the pressure. Alternatively, damage to the opening / closing claw can be avoided. At this time, the damper member contracts when pressure is applied from the outside, but by detecting the contraction by the contact monitoring sensor, it can be determined that the opening / closing claw or the main body has contacted an obstacle, It is possible to appropriately take measures such as stopping the operation of the transport means.

[0017]

Embodiments of the present invention will be described below in detail with reference to the drawings. 1 to 8 show an embodiment in which the present invention is applied to a horizontal differential thermomechanical analyzer, FIG. 1 is a schematic view showing the principle of the apparatus, FIG. 2 is a side view showing the appearance of the apparatus, FIG. 3 is a plan view of the same. FIG. 4 is an enlarged plan sectional view showing the structure inside and around the support tube.

As shown in these drawings, the thermomechanical analyzer according to this embodiment includes an apparatus main body 1, an electric furnace 2, and an automatic sample exchange unit 3. A support tube 4 extends from a side wall of the apparatus main body 1, and a sample S is placed in a sample placement section 5 formed at the tip of the support tube 4, and an electric furnace 2 is provided.
In addition to heating the sample S, the amount of deformation of the sample S is measured by a differential transformer 10 as main detection means built in the apparatus main body 1.

The support tube 4 is formed of a material having a small thermal deformation such as quartz glass or ceramic and has a cylindrical shape, and extends substantially horizontally from the side wall of the apparatus main body 1 as shown in FIG. In the vicinity of the tip of the support tube 4, a sample exchange window 4a is formed by notching the peripheral wall in the upper half, and the tip surface of the support tube 4 is closed by a partition wall 4b. The inside of the support tube 4 in the vicinity of the distal end is a sample placement section 5, and the sample S is placed in the sample placement section 5 in such a manner that one end thereof comes into contact with the partition wall 4b.

Inside the support tube 4, a detection rod 11 and a reference detection rod 12 extend in the axial direction and are arranged in parallel with each other. As shown in FIG. 4, the tip of the detection rod 11 is brought into contact with the end of the sample S placed in the sample placement section 5, while the tip of the reference detection rod 12 is placed on a support tube that supports one end of the sample S. 4 is brought into contact with the partition wall 4b. In this embodiment, the detection rod 11 and the reference detection rod 12 are formed of the same material having small thermal deformation such as quartz glass.

The detection rod 11 and the reference detection rod 1
The base end of 2 is connected to a differential transformer 10 built in the apparatus main body 1 (see FIG. 1). That is, the differential transformer 1
The base end of the detection rod 11 is connected to the 0 core 10a,
On the other hand, the base end of the reference detection rod 12 is connected to the coil 10b of the differential transformer 10. Core 1 of differential transformer 10
The coil 0a and the coil 10b are each movable in the axial direction, and are displaced in the same direction integrally with the axial movement of the detection rod 11 and the reference detection rod 12. Core 1 of differential transformer 10
When the relative position between 0a and the coil 10b changes, the current flowing through the coil 10b changes correspondingly. By detecting the change in the current value, the relative displacement between the detection rod 11 and the reference detection rod 12 can be obtained.

A required axial load can be applied to the core 10a and the detection rod 11 of the differential transformer 10 by a pressing means 13 such as an electromagnetic actuator. When performing measurements in a compression mode in which the sample S is subjected to a compressive load and the thermal deformation of the sample S is measured, or in a tensile mode in which a tensile load is applied to the sample S to measure the thermal deformation of the sample S. 1 and 4 on the sample S by the pressing means 13.
The required weight is applied to the left of.

Further, the core 10a and the detecting rod 11 of the differential transformer 10 are connected to a detecting rod driving means 14 comprising a motor or the like.
Thereby, it can be driven rightward in FIGS. The detection rod driving means 14 is used when the detection rod 11 is retracted from the sample placement section 5 when performing the sample exchange. On the other hand, a constant load is applied to the coil 10b of the differential transformer 10 and the reference detection rod 12 in the left direction in FIGS. 1 and 4 by an urging means 15 such as a spring. Hold the state of contact with the partition wall 4b.

The electric furnace 2 has a cylindrical shape and can reciprocate in the axial direction of the support tube 4 along a guide rail 20 formed on a base 1a of the apparatus main body 1, as shown in FIGS. This movement causes it to protrude and retract at the outer peripheral position of the support tube 4.
That is, by moving the electric furnace 2 to the right in the figure, the central part is placed at the outer peripheral position of the sample placement part 5 formed on the support tube 4. On the other hand, by moving to the left in the drawing, the sample placement unit 5 is placed at a position where the sample placement unit 5 is exposed (the position in the drawing).
The electric furnace 2 is driven by electric furnace driving means 21 such as a motor shown in FIG.

A cylindrical protective tube 22 is disposed inside the electric furnace 2. The protective tube 22 is positioned coaxially with the support tube 4 and moves integrally with the electric furnace 2 to move the support tube 4.
Is covered. The distal end of the protective tube 22 is closed, and the proximal end of the protective tube 22 is exposed from the electric furnace 2.

In the thermomechanical analysis, the thermal displacement of the sample S may be measured in a predetermined gas atmosphere or a vacuum atmosphere as required. Therefore, it is preferable that the inside of the apparatus main body 1 and the support tube 4 be shielded from the atmosphere so that the atmosphere can be formed. For this reason, the inside of the apparatus main body 1 has an airtight structure, and furthermore, a pipe communicating with a gas supply source and a vacuum pump (not shown) can be connected.

The support tube 4 communicating with the inside of the apparatus main body 1 is
Since the sample exchange window is open near the tip, it is necessary to prevent the inflow of air from the sample exchange window. In the thermomechanical analyzer of this embodiment, the support tube 4 is provided by the protection tube 22.
To prevent the inflow of air from the sample exchange window.

The base end of the protection tube 22 is in close contact with the root of the support tube 4 in the apparatus main body 1 to form an airtight structure.
In order to reliably form this airtight structure, a V-ring 23 is provided at the base of the support tube 4, while the protection tube 2 is provided.
A sealing member 24 with which the V-ring abuts is mounted on the base end portion 2.

FIG. 5 shows the sealing member 24 and the V ring 2.
3 is an enlarged plan sectional view showing the configuration of FIG. Sealing member 2
A contact surface 24a of a V-ring 23 is formed at the base end of the V-ring 4. The V-ring 23 has a flexible tongue 23a opposed to the contact surface 24a. Then, when the protective tube 22 moves together with the electric furnace 2 and the center of the electric furnace 2 is positioned on the outer periphery of the sample placement section 5, the contact surface 24 a of the sealing member 24 is in contact with the tongue piece 23 a of the V-ring 23. Abuts to form a closed state.

In the conventional thermomechanical analyzer, as shown in FIG. 10 or FIG. 11, a sealed structure is formed between the root portion of the support tube 4 and the base end portion of the protection tube 22 by using an O-ring 200. It had been. That is, in the sealed structure shown in FIG. 10, an O-ring is attached to the outer peripheral surface of the support tube 4 and the O-ring is interposed between the outer peripheral surface of the support tube 4 and the inner peripheral surface of the protection tube 22 to form a sealed state. To form In addition, the sealing structure of FIG.
An O-ring 200 is provided at the base of the support tube 4 so as to face the base surface of the protection tube 22, and the O-ring 200 is crushed between the base surface of the protection tube 22 and the base of the support tube 4. To form a closed state.

However, in the closed structure shown in FIG. 10, it is necessary to center the gap between the support tube 4 and the protection tube 22 with high precision, and also to prevent the guide rail supporting the electric furnace 2 and the protection tube 22 from swaying. However, there has been a drawback that high-precision manufacturing is required, and the manufacturing cost is high. Further, in the sealed structure of FIG. 11, the amount of crushing required for the O-ring 200 to effectively form an airtight state is smaller than that of the V-ring 23, so that it is difficult to position the protection tube 22. .

The sealing structure of this embodiment, in which the V-ring 23 is brought into contact with the contact surface 24a of the facing sealing member 24, is different from the conventional sealing structure using the O-ring 200 as described above. There is an advantage that the allowable range of centering and positioning at the time of abutment and contact between the protective tube 22 and the protective tube 22 is wide, and therefore, manufacture is easy.

As shown in FIG. 1, a sample temperature detector 16 for detecting the temperature of the sample S is provided near the sample placement section 5 in the support tube 4 described above. Also, the electric furnace 2 has an electric furnace temperature detector 17 for detecting the heat generation temperature.
Is provided. In this embodiment, thermocouples are used as the sample temperature detector 16 and the electric furnace temperature detector 17. Further, in the thermomechanical analyzer according to this embodiment, as shown in FIGS. 2 and 3, a cooling fan 6 is disposed near an opening of one end of the electric furnace 2. This cooling fan 6
Has a function of sending cool air into the electric furnace 2 and forcibly cooling the electric furnace 2.

In the electric furnace 2, a metal soaking tube (not shown) is provided.
By radiating heat from the sample to the sample, the sample can be uniformly heated. A cover 25 is provided on the outer periphery of the electric furnace 2.

The above-mentioned electric furnace 2, the coil 10b of the differential transformer 10, the pressurizing means 13 of the detecting rod 11, the detecting rod driving means 14, the electric furnace driving means 21, the sample temperature detector 16, and the electric furnace temperature detector 17 are controlled by the control device 7 as shown in FIG. 1 so that thermomechanical analysis can be automatically performed. That is, when a required sample is placed on the sample placement unit 5 by the sample automatic exchange unit 3 described later, the detection rod 11 is moved in the axial direction by the detection rod driving means 14, and its tip is separated from the sample placement unit 5. .

Subsequently, after the required sample S is placed on the sample placement unit 5 by the automatic sample exchange unit 3, the driving force of the detection rod driving means 14 on the detection rod 11 is released, and the detection force is detected by the pressure means 13. A predetermined load is applied to the rod 11. Due to this load, the state where the tip of the detection rod 11 is in contact with one end of the sample S is maintained.

Next, the electric furnace driving means 21 is operated,
The central part of the electric furnace 2 is arranged at the outer peripheral position of the sample placing part 5. At this time, the sealing member 2 attached to the base end of the protection tube 22
4 comes into contact with a V-ring 23 provided at the base of the support tube 4 in the apparatus main body 1 to form a sealed structure from inside the protective tube 22 to inside the apparatus main body 1. Here, if necessary, the inside of the apparatus main body 1 can be vacuum-sucked from the inside of the sealed protective tube 22 or filled with an inert gas or the like to form a required measurement atmosphere.

Thereafter, the electric furnace 2 is operated to operate the sample placing section 5.
Heats the sample S placed in the
By detecting a change in the current flowing through the zero coil 10b, the deformation of the sample S in the axial direction is measured. That is, when the sample S is deformed by heating, the amount of deformation is transmitted to the detection rod 11, and the detection rod 11 moves in the axial direction. At this time, if the support tube 4 that supports the sample S is deformed by heat, the deformation is transmitted to the reference detection rod 12 that comes into contact with the support tube 4, and the reference detection rod 12 moves in the axial direction.

As a result, the relative displacement between the core 10a of the differential transformer 10 to which the detection rod 11 is connected and the coil 10b of the differential transformer 10 to which the reference detection rod 12 is connected, causes the deformation component of the support tube 4 to be reduced. This corresponds to only the deformation of the subtracted sample S. Then, based on the relative displacement, the value of the current flowing through the coil 10b of the differential transformer 10 changes. This is detected by the control device 7, and the thermomechanical analysis of the sample S is executed through a predetermined calculation process. The control device 7
The calculation process for the thermomechanical analysis by the method is the same as that of a conventionally known thermomechanical analyzer, and the description thereof is omitted here.

The temperature of the sample S is detected by a sample temperature detector 16, and the controller 7 controls the electric furnace 2 based on the temperature information from the sample temperature detector 16. At this time, the heating temperature of the electric furnace 2 is also changed by the electric furnace temperature detector 17.
, And the temperature condition of the electric furnace 2 is also input to the control device 7.

When the thermomechanical analysis of the sample S is completed in this way, the differential of the electric furnace 2 is stopped, and the temperature in the electric furnace 2 is naturally lowered to a predetermined temperature. Then, when the temperature in the electric furnace 2 drops to a temperature at which it is not damaged even if it is rapidly cooled, the cooling fan 6 is driven to perform forced cooling. Thereby, the cooling of the electric furnace 2 can be accelerated, and the cycle time of the thermomechanical analysis measurement for the next sample S can be shortened.

Next, the automatic sample exchange unit 3 will be described. FIG. 6 is an enlarged front view showing the entire structure of the automatic sample exchange unit 3. As shown in FIG. 2 and FIG. 2 and FIG. 3, the automatic sample exchange unit 3 includes a transport unit 30 including a base 31, a sample stage 32, an elevating mechanism 33, a horizontal transport rail 34, and a support arm 35, and a gripping unit. 40
And

The base 31 is the main body 1 of the thermomechanical analyzer.
The sample stage 32 is provided on the upper flat surface of the base 31. This sample stage 3
2, a large number of samples S can be arranged in a matrix in the X and Y directions in FIG. Here, the X direction is a direction parallel to the axis of the support tube 4, and the prism or columnar sample S is disposed in the sample disposition section 5 with its long side extending in the X direction. Similarly, also on the sample stage 32, the sample S is disposed with its long side extending in the X direction.

The sample stage 32 can be moved in the X direction in FIG. 3 by a back and forth moving mechanism (not shown) built in the base 31. The sample stage 32
The arrangement surface of the sample S is adjusted to be substantially the same height as the sample arrangement portion 5 formed on the support tube 4 in the thermomechanical analyzer.

The elevating mechanism 33 is provided at the rear of the base 31, and receives power from an elevating drive source (not shown) such as a motor built in the base 31 to move the support 33a in the vertical direction (see FIG. 2). (Z direction). At the upper end of the column 33a, a horizontal transport rail 34 is provided extending in the Y direction in FIG. The horizontal transfer rail 34 has an X in FIG.
The base end of the support arm 35 extending in the direction is mounted,
The support arm 35 is reciprocated in the Y direction by a horizontal drive source (not shown) such as a built-in motor.

The holding means 40 is provided with the support arm 35 described above.
And is moved between the sample stage 32 and the sample placement unit 5 by the vertical movement by the elevating mechanism 33 and the movement in the Y direction by the horizontal transfer rail 34. The gripping means 40 has a pair of open / close claws 43 and 44 projecting downward from the bottom surface of the grip body 41 as described later, and these open / close claws 43 and 44 cooperate to grip the sample S.

The mechanism for moving the sample stage 32 back and forth, an elevation drive source, and a horizontal drive source (all not shown)
Are controlled by the controller 8. That is,
At the time of sample exchange, the controller 8 operates the forward / backward movement mechanism to move the sample stage 32 in the X direction, and arranges a required sample S on the movement path of the gripping means 40.

Next, the horizontal drive source is operated to move the gripping means 40 in the Y direction along the horizontal transport rail 34,
The open / close claws 43 and 44 of the gripping means 40 are positioned above the selected sample S on the sample stage 32. When entering this operation, if the support 33a of the elevating mechanism 33 is in a lowered state, the elevating drive source is activated in advance,
The gripping means 40 is arranged at a raised position.

Subsequently, the lifting drive source is operated to operate the gripper 4.
0 is lowered, and the open / close claws 43 and 44 of the gripping means 40 are positioned to a position where the selected sample S on the sample stage 32 can be gripped. Then, after the opening and closing claws 43 and 44 grip the sample S at this position, the lifting drive source is operated again to raise the gripping means 40, and the horizontal drive source is operated to move the gripping means 40 in the Y direction. Then, the gripped sample S is positioned at a position above the sample placement unit 5.

The lifting drive source is actuated from the upper position to lower the gripping means 40 toward the sample placement unit 5, and the held sample S is placed in the sample placement unit 5. Thereafter, the open / close claws 43 and 44 are opened to release the gripping of the sample S, and the gripping means 40 is raised by the elevation drive source to complete the operation of arranging the sample S on the sample mounting unit 5.

In order to remove the measured sample S from the sample placement unit 5, after opening the electric furnace 2, the horizontal drive source and the elevation drive source are operated to move the gripping means 40 to the sample placement unit 5. Then, the sample S on the sample placement unit 5 is gripped by the opening / closing claws 43 and 44, and the lifting drive source and the horizontal drive source are operated again to transport the gripped sample S to the sample stage 32. It should be noted that operation information of the apparatus main body 1 and the electric furnace 2 side is output from the control device 7 to the controller 8, and the sample S
Start and end of measurement, opening and closing of electric furnace 2, detection rod driving means 1
The operation of exchanging the sample S is executed in cooperation with the operation of Step S4.

FIG. 7 is a perspective view showing the internal structure of the holding means 40, and FIG. 8 is a front view of the same. As shown in these figures, a guide rail 42 is provided on the lower surface of the plate-shaped grip body 41.
A pair of open / close claws 43, 44 that are movable in the lateral direction along are supported. The pair of opening / closing claws 43 and 44 cooperate with each other to grip the sample S at an intermediate portion thereof.

At the center of the upper surface of the grip body 41, a drive motor 45 is provided. The rotating shaft 4 of the drive motor 45
5a penetrates the grip body 41 and is exposed on the lower surface side of the grip body 41. An elliptical cam 46 is attached to the rotating shaft 45a, and the driving motor 45 and the cam 46 constitute driving means for the opening and closing claws 43 and 44.

That is, the pair of opening / closing pawls 43 and 44 are constantly urged by a biasing means 47 such as a coil spring in a direction (close direction) to reduce the distance between them.
3 and 44, the peripheral surface of the cam 46 is
3 and 44. The cam 46 rotates with the rotation of the drive motor 45, and the opening and closing claws 43 and 44 perform symmetrical opening and closing operations according to the shape of the cam 46. The gripping force of the sample S by the opening and closing claws 43 and 44 is defined by the urging force applied from the urging means 47. Therefore, it is preferable that the urging means 47 can adjust the urging force applied to the opening and closing claws 43 and 44 according to the hardness of the sample S.

A first shutter 48 is attached to the upper end of one opening / closing claw 43 as a gripping detection member, and the upper end of the other opening / closing claw 44 is a detection member for opening position confirmation. Is mounted. These shutters 48 and 49 are exposed on the upper surface side of the grip main body 41 via long holes 41a and 41b formed in the grip main body 41.

Further, on the upper surface of the grip body 41, a grip confirmation sensor 50 and an origin sensor 51 are provided. In this embodiment, these sensors 50 and 51 are constituted by optical sensors. That is, the gripping confirmation sensor 50 includes a light emitting unit 50a and a light receiving unit 50b.
Reference numeral 50b is provided to face the moving path of the first shutter 48 in accordance with the movement of the opening / closing claw 43, and oppose each other. This installation position is
When the opening and closing claws 43 and 44 cooperate to grip the sample S, the first shutter 48 is adjusted to a position where the light beam from the light projecting unit 50a is blocked.

Incidentally, the positions where the open / close claws 43 and 44 grip the sample S differ depending on the size of the sample S to be transported. Therefore, the position where the first shutter 48 stops when the open / close claws 43 and 44 cooperate to grip the sample S also differs. Thus, the sample S to be transported is
In accordance with the stop position of the first shutter 48 that changes depending on the size of the
The shutter 48 can be arbitrarily adjusted along the movement path.

As the adjusting mechanism, various known position adjusting mechanisms can be adopted. For example, guide rails are provided on both sides in the front-rear direction along the long hole 41a, and the light projecting unit 50a and the light receiving unit 50b can slide on these guide rails. What is necessary is just to set it as the structure which can fix the light projection part 50a and the light receiving part 50b with a fastener.

The origin sensor 51 also includes a light projecting unit 51a and a light receiving unit 5
1b, and the respective parts 51a, 51b
Are provided opposite to each other with the movement path of the second shutter 49 accompanying the movement of. In this embodiment, the fully opened position of the opening / closing claw 44 is set as the origin, and when the opening / closing claw 44 comes to this fully opened position, the light projecting portion 51a and the light receiving portion 51a are located at positions where the light rays from the light projecting portion 51a are blocked by the second shutter 49. A portion 51b is provided.

The grip body 41 is mounted on the distal end 35a of the support arm 35 via two damper members 52,52. In this embodiment, the damper members 52, 52
A hydraulic damper is used, and the piston rod 52b is axially expandable and contractable while receiving hydraulic pressure with respect to the outer cylinder 52a. The outer cylinder 52a and the piston rod 5
One (outer cylinder 52a in the figure) of 2b is mounted on the distal end 35a of the support arm 35, and the other (piston rod 52b in the figure) is mounted on the upper surface of the grip body 41, respectively.

When the open / close claws 43, 44 provided on the lower surface of the grip body 41 receive an external force from below, the damper members 52, 52 contract the piston rod 52b so as to buffer the impact of the external force. I have. This piston rod 52
b is constantly urged downward by a hydraulic pressure, and projects by a predetermined length by the hydraulic pressure when no external force is applied.

One of the tip 35a of the support arm 35 and the grip body 41 (the grip body 41 in the figure) is provided with a contact monitoring sensor 54, and the other (the tip 35a of the support arm 35 in the figure). 3) is provided with a third shutter 55 as a contact monitoring detecting member.

In this embodiment, the contact monitoring sensor 54
Is constituted by an optical sensor including a light projecting unit 54a and a light receiving unit 54b, and the light projecting unit 54a and the light receiving unit 54b are arranged to face each other. Then, when the piston rod 52b contracts by a predetermined amount due to the action of the external force, the third shutter 55 is interposed at an intermediate position between the light projecting portion 54a and the light receiving portion 54b so as to block the light beam emitted from the light projecting portion 54a. It has been adjusted.

Next, the operation of the gripping means 40 having the above configuration will be described. The operation of the gripping means 40 is also controlled by the controller 8 shown in FIG. That is, when a drive command is sent from the controller 8 to the drive motor 45,
The drive motor 45 operates to rotate the cam 46.
With the rotation of the cam 46, the opening and closing claws 43 and 44 perform opening and closing operations. When the opening / closing claw 44 is opened to the fully open position which is the origin, the second shutter 49 is interposed between the light projecting unit 51a and the light receiving unit 51b constituting the origin sensor 51, and the light emitted from the light projecting unit 51a is emitted. Block out. Then, a detection signal of the second shutter 49 is transmitted from the origin sensor 51 to the controller 8.
Output to When a detection signal is input from the origin sensor 51, the controller 8 issues a stop command to the drive motor 45, and holds the open / close claws 43, 44 in the fully open state.

When the tips of the open / close claws 43, 44 are too low and come into contact with the sample stage, the support tube 4, or the like due to malfunction of the transfer means 30, the piston rods 52b of the damper members 52, 52 are contracted and the impact is caused. Absorbs the opening and closing claw 43,
Damage such as 44 is avoided. Further, the piston rod 52
The contact monitoring sensor 54 and the third shutter 5
5 moves relative to each other, and a third shutter 55 is interposed between the light projecting part 54a and the light receiving part 54b constituting the sensor 54. Then, the contact monitoring sensor 54 outputs the third shutter 5.
5 is output to the controller 8. The controller 8 confirms the occurrence of the operation abnormality by inputting the detection signal from the contact monitoring sensor 54, and immediately stops the operation of the support arm 35.

Next, when the sample S is gripped by the open / close claws 43, 44, the controller 8 issues a drive command to the drive motor 45, and the drive motor 45 is driven based on the drive command.
Operates to rotationally drive the cam 46. With the rotation of the cam 46, the open / close claws 43, 44 gradually close from the fully opened state, which is the origin position. At this time, the first shutter 48 also moves integrally with the opening / closing claws 43 and 44. Then, when the first shutter 48 moves between the light emitting unit 50a and the light receiving unit 50b that constitute the gripping confirmation sensor 50, the light emitted from the light emitting unit 50a is blocked by the first shutter 48.
Then, a detection signal of the first shutter 48 is output from the gripping confirmation sensor 50 to the controller 8.

As described above, the grip confirmation sensor 50 is
When the opening / closing claws 43 and 44 hold a sample of a predetermined size, the first shutter 48 is adjusted to a position where the light beam from the light projecting unit 50a is blocked. Therefore, when the detection signal of the first shutter 48 is input from the gripping confirmation sensor 50, the sample S is gripped by the open / close claws 43 and 44. In this embodiment, after the detection signal of the first shutter 48 is input from the gripping confirmation sensor 50,
The cam 46 is continuously rotated for a predetermined time without stopping.

Even when the cam 46 is rotated in this way, if the sample S is gripped by the opening / closing claws 43, 44 at the time when the controller inputs the detection signal of the first shutter 48, the opening / closing claw 43, 44 44 does not close, and therefore the first shutter 48 also includes the light projecting unit 50a and the light receiving unit 50.
The signal remains stopped during the period b, and the detection signal of the first shutter 48 continues to be output. The controller 8 determines that the opening / closing claws 43 and 44 properly grip the sample S by confirming that the detection signal of the first shutter 48 is continuously output.

On the other hand, when the opening and closing claws 43 and 44 do not grip the sample S, the opening and closing
3 and 44 are further closed, and the first shutter 48 is integrated therewith.
Also moves out of the space between the light projecting unit 50a and the light receiving unit 50b. Then, the light receiving unit 50b enters a state of receiving the light beam from the light projecting unit 50a, and the gripping confirmation sensor 50 stops outputting the detection signal of the first shutter 48. First shutter 4
When the detection signal of No. 8 is no longer input at such a timing, the controller sets the open / close claws 43 and 44 to the sample S.
It is determined that could not be held, and the sample transport operation in the cycle is stopped.

The present invention is not limited to the above embodiment. For example, in the above-described embodiment, the differential method in which the relative displacement between the reference detection rod 12 and the detection rod 11 is detected by the differential transformer 10 is employed, but the deformation amount of the sample is measured using only the detection rod. The present invention can also be applied to a so-called total expansion type thermomechanical analyzer.

In the above embodiment, the horizontal structure in which the support tubes 4 and the electric furnace 2 are arranged horizontally is used. However, the thermomechanical analyzer of the vertical structure in which the support tubes 4 and the electric furnace 2 are arranged vertically is used. Can also be applied. In this case, the thermomechanical analyzer has a structure in which the automatic sample exchange unit 3 shown in FIGS. 2 and 3 is also vertically arranged corresponding to the electric furnace 2, the support tube 4, and the like.

Further, the shape and number of the open / close claws of the gripping means may be arbitrarily changed according to the shape and size of the sample. The damper member is not limited to a hydraulic damper, and various known dampers can be applied. Various sensors such as a proximity sensor capable of detecting a detecting member other than the optical sensor can be applied to the gripping confirmation sensor, the origin sensor, and the contact monitoring sensor.

[0073]

As described above, according to the thermomechanical analyzer of the present invention, the sample on the sample stage is grasped by the grasping means, and the grasping means is moved by the transport means to the sample placement section in the thermomechanical analyzer. 5, the sample can be automatically exchanged, and the work efficiency can be improved by relieving the researcher from complicated sample exchange work.

[Brief description of the drawings]

FIG. 1 is a schematic view showing the principle of a horizontal differential thermomechanical analyzer according to an embodiment of the present invention.

FIG. 2 is a side view showing the appearance of the apparatus.

FIG. 3 is a plan view of the same.

FIG. 4 is an enlarged plan sectional view showing the structure inside and around the support tube.

FIG. 5 is an enlarged plan sectional view showing a configuration of a sealing member and a V-ring.

FIG. 6 is an enlarged front view showing the entire structure of the automatic sample exchange unit.

FIG. 7 is a perspective view showing the internal structure of the gripping means.

FIG. 8 is a front view of the same.

FIG. 9 is a perspective view showing a conventional automatic sample exchange device applied to a differential thermal analyzer (DTA).

FIG. 10 is a cross-sectional view showing a conventional sealing structure for sealing between a base end of a protection tube and a root of a support tube using an O-ring.

FIG. 11 is a cross-sectional view showing another conventional sealing structure for sealing the space between the base end of the protection tube and the base of the support tube using an O-ring.

[Explanation of symbols]

 1: Apparatus main body 2: Electric furnace 3: Automatic sample exchange unit 4: Support tube 5: Sample placement part 6: Cooling fan 7: Control device 8: Controller 10: Differential transformer 11: Detection rod 12: Reference detection rod 13: Pressurizing means 14: detecting rod driving means 15: urging means 16: sample temperature detector 17 electric furnace temperature detector 20: guide rail 21: electric furnace driving means 22: protective tube 23: V ring 24: sealing member 25: Cover 30: transport means 31: base 32: sample stage 33: elevating mechanism 34: horizontal transport rail 35: support arm 40: gripping means 41: gripping body 42: guide rails 43, 44: opening / closing claw 45: drive motor 46: Cam 47: urging means 48: first shutter 49: second shutter 50: gripping confirmation sensor 51: origin sensor 52: damper member 54: contact monitoring cell Sensor 55: Third shutter

 ──────────────────────────────────────────────────続 き Continued on the front page (72) Inventor Yoshiumi Sugiura 3-9-12 Matsubaracho, Akishima-shi, Tokyo Rigaku Electric Co., Ltd.

Claims (4)

[Claims] 1. A thermomechanical analyzer for placing a required sample in a sample placement portion formed at the tip of a support tube and measuring physical deformation when the sample is heated to a predetermined temperature. A thermomechanical analyzer comprising: a sample stage capable of disposing a large number of samples; gripping means for gripping a sample; and transport means for transporting the gripping means between the sample placement section and the sample stage. 2. The thermomechanical analyzer according to claim 1, wherein the gripping means includes a main body, a plurality of open / close claws provided on the main body so as to be openable and closable, and cooperates to hold the sample. A driving unit for driving the opening and closing, a gripping detection member that moves integrally with one of the opening and closing claws, and a gripping sensor provided at a predetermined position of the main body, wherein the opening and closing claws grip the sample. When you move to the position where
A thermomechanical analyzer, wherein the gripping confirmation sensor detects the gripping confirmation detecting member. 3. The thermomechanical analyzer according to claim 2, wherein the gripping confirmation sensor is capable of arbitrarily adjusting a fixed position on the main body. 4. The thermomechanical analyzer according to claim 2, wherein the gripping means is provided with a damper member for buffering the pressure by an expansion / contraction operation when the opening / closing claw or the main body receives a pressure from the outside. A thermomechanical analyzer comprising a contact monitoring sensor for detecting a predetermined amount of contraction due to an external force acting on the damper member.