JP2759770B2 - Sample length measuring method and thermal expansion measuring method in thermomechanical 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 thermomechanical analyzer (TMA) for calculating the expansion coefficient of a measurement sample based on the length of the measurement sample at a reference temperature and the length at an arbitrary temperature. The present invention relates to a sample length measuring method for automatically obtaining a length of a measurement sample at a reference temperature, and a thermal expansion measuring method partially utilizing the sample length measuring method.

[0002]

2. Description of the Related Art FIG. 1 shows a general configuration of a differential thermomechanical analyzer. In this differential thermomechanical analyzer, a reference sample R and a measurement sample S are arranged inside a support tube 1 having heat resistance, and the relative elongation of the measurement sample S with respect to the reference sample R at an arbitrary temperature is measured. I can do it.

That is, detection rods 2 and 3 are provided at the upper ends of a reference sample R and a measurement sample S disposed inside the support tube 1, respectively.
Is fixed, and an arbitrary measuring load is applied to each of the detection rods 2 and 3. Here, a pressurizing means such as a weight 4 is used for pressurizing the detection rod 2 on the reference side (hereinafter, referred to as a reference detection rod).
An electromagnetic load coil 5 is used for pressurizing the measurement side detection rod 3). The coil 6a of the differential transformer 6 is fixed to the reference sample side detection rod 2, while the magnet 6b of the transformer is fixed to the measurement side detection rod 3.

[0004] A heating furnace 7 is moved and arranged around the support tube 1,
When the reference sample R and the measurement sample S are heated to an arbitrary measurement temperature, the reference side detection rod 2 rises in accordance with the elongation of the reference sample R due to thermal expansion, and displaces the coil 6a of the differential transformer 6. On the other hand, the measurement side detection rod 3 is also used for the measurement sample S due to thermal expansion.
And the magnet 6b of the differential transformer 6 is displaced. At this time, the displacement of the coil 6a and the magnet 6b of the differential transformer 6 includes error components such as expansion of the support tube 1 and the detection rods 2 and 3, and these error components are the coil 6a and the magnet 6b. Offset by the relative displacement of

Thus, the coil 6 of the differential transformer 6
When a relative displacement occurs between the coil 6a and the magnet 6b, the coil 6
The value of the current flowing through a changes. By detecting the amount of change in the current, the difference in elongation between the reference sample R and the measurement sample S (that is, the relative elongation of the measurement sample S with respect to the reference sample R) can be obtained. In addition, the temperature of the reference sample R, the measurement sample S, or the vicinity of those samples is detected by a thermocouple 8 installed at the inner bottom of the support tube 1.

[0006]

The expansion coefficient α of the measurement sample S
Are the length L of the reference sample R at the reference temperature T0, the average expansion coefficient C of the reference sample R between the measurement temperature T and the reference temperature T0, the length L1 of the measurement sample S at the reference temperature T0, and the measurement temperature T If the difference .DELTA.L2 in the relative length of the measurement sample S with respect to the reference sample R is known, it can be calculated by the following equation (see FIG. 4).

ΔL = ΔL2 + ΔL3 ΔL: Elongation of measurement sample S with temperature change ΔL3: Elongation of reference sample R with temperature change ΔL3 = C × (T−T0) × L ∴ ΔL = ΔL2 + C × (T−T0) ) × L (i) α = (ΔL / L1) × 100 [%] (ii)

Further, if the expansion coefficient α of the sample S is obtained, the expansion coefficient Cx of the sample S at an arbitrary set temperature Tx can be calculated by the following equation. Cx = ΔL / {L1 × (T−Tx)} (iii)

The thermomechanical analyzer is provided with a data processing system as shown in FIG. 2, and an arithmetic unit 11 operates on the basis of a detection signal from a differential transformer 6 input via an interface circuit 10 of the system. Calculate the above formula,
The expansion coefficient α, expansion coefficient Cx, and the like of the measurement sample S are automatically calculated and stored in the storage unit 12 or output via the output unit 13.

The conventional thermomechanical analyzer can automatically detect the difference ΔL 2 in the relative length of the measurement sample S with respect to the reference sample R at the measurement temperature T. The length L of the reference sample R at the reference temperature T0 required for calculating the ratio α and the expansion coefficient Cx, the average expansion coefficient C between any measurement temperature T and the reference temperature T0, and the reference of the measurement sample S The length L1 at the temperature T0 had to be measured separately and stored in the storage unit 12 using the keyboard 14 of the data processing system.

Of these, the length L of the reference sample R at the reference temperature T0 and the average expansion coefficient C between any measurement temperature T and the reference temperature T0 are measured once and stored. Can be used repeatedly for measurement. However, the length L1 of the measurement sample S at the reference temperature T0
Since the same sample S is exchanged for each measurement, the measurement must be performed manually by an operator using a measuring instrument such as a micrometer each time, and stored in the storage unit 12 by operating the keyboard 14. It was complicated.

SUMMARY OF THE INVENTION The present invention has been made in view of the above circumstances, and has as its object to automatically determine the length L1 of a measurement sample at a reference temperature T0 by a thermomechanical analyzer, thereby facilitating the measurement operation. And

[0013]

In order to achieve the above object, a first sample length measuring method according to the present invention provides a method for measuring a relative length of another sample relative to one sample arranged in a support tube. A so-called differential thermomechanical analyzer including a means for detecting a difference under an arbitrary temperature condition and a means for performing a predetermined arithmetic processing based on the detection result is a method including the following steps.

A total reference sample and a length measurement reference sample having a known total length L 0 at a reference temperature are respectively arranged in a support tube, and the relative length of the length measurement reference sample with respect to the total reference sample at the reference temperature is measured. Step of Detecting Difference ΔL0 Step of Placing Total Reference Sample and Measurement Sample in Support Tube and Detecting Difference ΔL1 of Relative Length of Measurement Sample to Total Reference Sample at Reference Temperature Total Length L0 of Length Measurement Reference Sample , The relative length difference ΔL 0 of the length measurement reference sample, and the relative length difference Δ of the measurement sample
Calculating the total length L1 of the measurement sample at the reference temperature based on L1

The thermal expansion measuring method according to the present invention further comprises a means for detecting a difference in a relative length of one sample relative to one sample placed in the support tube under an arbitrary temperature condition;
In a so-called differential thermomechanical analyzer provided with means for performing predetermined arithmetic processing based on the detection result, the method includes the following steps.

A total reference sample having a known total length L at a reference temperature and an average expansion coefficient C between an arbitrary measured temperature T and a reference temperature T 0, and a length measurement reference sample having a known total length L 0 at a reference temperature A step of detecting the difference ΔL0 in the relative length of the length measurement reference sample with respect to the total reference sample at the reference temperature at the reference temperature, and placing the total reference sample and the measurement sample in the support tube, Detecting the relative length difference ΔL1 of the measurement sample with respect to the total reference sample at the temperature. The total length L0 of the length measurement reference sample, the relative length difference ΔL0 of the length measurement reference sample, and the relative length of the measurement sample. Length difference Δ
Step of calculating the total length L1 of the measurement sample at the reference temperature based on L1 The total elongation difference of the measurement sample with respect to the total reference sample at an arbitrary measurement temperature by arranging the total reference sample and the measurement sample in the support tube. Step of detecting ΔL2 The total length L of the total reference sample at the reference temperature, the average expansion coefficient C between any measurement temperature T and the reference temperature T0, the total length L1 of the measurement sample at the reference temperature, and the measurement at any measurement temperature Calculating the expansion coefficient or expansion coefficient of the measurement sample based on the relative elongation difference ΔL2 of the measurement sample at step

Further, according to a second sample length measuring method of the present invention, one sample is placed in a support tube, and a difference between a relative length of one sample with respect to an arbitrary reference length and an arbitrary temperature state is determined. A so-called full-expansion thermomechanical analyzer including a detecting means for detecting the original and a calculating means for performing a predetermined calculating process based on the detection result is a method including the following steps.

A length measurement reference sample having a known total length L0 at a reference temperature is placed in a support tube, and the relative length of the length measurement reference sample at the reference temperature with respect to the length measurement origin of the thermomechanical analyzer is determined. Detecting process Length of thermomechanical analyzer detected
A process for storing the relative length of a long reference sample as a reference length
The sample is placed in the support tube and the difference ΔL1 in the relative length of the sample to the reference length at the reference temperature is detected.
Overall length L0 of the step length measurement reference sample detected by means, on the basis of the measured relative length difference ΔL1 of the sample to the reference length, the step of calculating the arithmetic means the total length L1 of the reference temperature of the measurement sample

[0019]

The differential thermomechanical analyzer has a length for detecting the difference in the relative length of one sample relative to one sample placed in the support tube under an arbitrary temperature condition as described above. There is provided a detecting means and a calculating means for performing a predetermined calculating process based on the detection result. Accordingly, in the sample length measuring method of the present invention, the step of detecting the relative length difference ΔL0 of the length measurement reference sample to the total reference sample at the reference temperature, and the step of detecting the measurement sample relative to the total reference sample at the reference temperature. Regarding the step of detecting the relative length difference ΔL1,
Processing can be performed by the length detecting means. The step of calculating the total length L1 of the measurement sample at the reference temperature based on each of these detection results and the known total length L0 of the length measurement reference sample can be automatically processed by the arithmetic means.

Here, the formula for calculating the total length L1 at the reference temperature of the measurement sample is as follows (see FIG. 3). L1 = L0 + ΔL0−ΔL1 (iv)

Further, in the invention of the thermal expansion measuring method, the respective steps up to the calculation of the total length L1 of the measurement sample at the reference temperature can be performed in the same manner as in the sample length measuring method. Further, the step of detecting the difference ΔL2 in the relative elongation of the measurement sample with respect to the total reference sample at an arbitrary measurement temperature can be processed by the length detection means. Then, based on these detection results, the total length L of the total reference sample at the reference temperature, which is known in advance, and the average expansion coefficient C between the arbitrary measurement temperature T and the reference temperature T0, the expansion coefficient or the expansion coefficient of the measurement sample is calculated. The step of calculating the expansion coefficient can be automatically processed by the calculation means.

In each of the above-described methods, the work of measuring the total length L0 of the length measurement reference sample using a measuring instrument such as a micrometer is required. Can be used repeatedly for a long time. Moreover, since the difference ΔL0 in the relative length of the length measurement reference sample with respect to the total reference sample at the reference temperature can be detected once and used repeatedly for length measurement of another measurement sample, the difference ΔL0 The detection step can be omitted.

On the other hand, the full-expansion thermomechanical analyzer arranges one sample in the support tube as described above, and determines the difference in the relative length of one sample with respect to an arbitrary reference length in an arbitrary temperature state. And length calculating means for performing predetermined calculation processing based on the detection result.

Accordingly, in the second sample length measuring method of the present invention, the step of detecting the relative length (reference length) of the length measurement reference sample with respect to the length measurement origin of the thermomechanical analyzer, the reference temperature The step of detecting the difference ΔL1 in the relative length of the measurement sample with respect to the reference length in the above can be processed by the length detecting means. Then, based on this detection result and the length L0 of the length measurement reference sample that is known in advance, the length L0 of the measurement sample at the reference temperature is determined.
1 The step of calculating can be automatically processed by the arithmetic means.

Here, the formula for calculating the total length L1 at the reference temperature of the measurement sample is as follows (see FIG. 5). L1 = L0-.DELTA.L1 (v)

It is necessary to measure the total length L0 of the length measurement reference sample using a measuring instrument such as a micrometer, but once measured, it is used repeatedly for length measurement of another measurement sample. be able to. Moreover, once the reference length is detected, it can be repeatedly used for measuring the length of another measurement sample, so that the step of detecting the reference length can be omitted thereafter.

[0027]

Embodiments of the present invention will be described below in detail with reference to the drawings. First, a sample length measuring method and a thermal expansion measuring method according to a first embodiment of the present invention applied to a differential thermomechanical analyzer will be described mainly with reference to FIGS. Note that the differential thermomechanical analyzer for performing these methods is the same as that described above with reference to FIGS. 1 and 2, and thus a detailed description is omitted.

Prior to performing the sample length measuring method, an overall reference sample R, a length measurement reference sample P, and a measurement sample S are prepared. In this embodiment, each sample is formed in a columnar shape having an arbitrary length. However, it is needless to say that each sample can be formed in various shapes suitable for measurement. In addition, not only a solid sample but also a powder sample, for example, can be a target of the method of this embodiment. In this case, the powder sample is pressed into a fixed shape of an arbitrary length to obtain a sample.

Here, the comprehensive reference sample R is a sample serving as a reference for various measurements in differential thermomechanical analysis, and corresponds to the reference sample R in the prior art described above. In the same device, the relative elongation (deformation) of another sample with respect to the general reference sample R is detected by the differential transformer 6. That is, the comprehensive reference sample R is used for the purpose of canceling the error of the detection result caused by deformation of the support tube 1 and the detection rods 2 and 3 due to heating, convection in the support tube 1 and the like, and improving the measurement accuracy. Used for mold thermomechanical analysis. This general reference sample R
Is a material having a small deformation with respect to a temperature change.
(Including a length measurement reference sample P). The total reference sample R is made of a material whose average expansion coefficient C between a reference temperature T0 and a measured temperature T, which will be described later, is known in advance.

The length measurement reference sample P is required for determining the reference sample length L0 (see equation (iv)) in the sample length measurement method according to this embodiment. After preparing each of these samples, first, for the general reference sample R,
It is checked whether the average expansion coefficient C and the total length L between the reference temperature T0 and the measured temperature T are stored in the storage unit 12 of the data processing system shown in FIG. 2 (step (hereinafter, "S" in FIG. 6). 1) If not stored,
The data of the expansion coefficient C (known value) and the total length L are input using the keyboard 14 (S2). In this embodiment, the normal temperature is set as the reference temperature T0, and the total length L of the general reference sample R at the normal temperature is measured using a measuring instrument such as a micrometer. If these data relating to the general reference sample R have already been stored in the storage unit 12, this step (S2) can be omitted.

This general reference sample R is placed in the support tube 1 (S3), the base end of the reference side detection rod 2 is connected to the tip of the sample R, and a constant load is applied by a pressing means such as a weight 4 or the like. Then, the sample R is fixed in the support tube 1 (S4). Next, for the length measurement reference sample P, it is confirmed whether the total length L0 at the reference temperature T0 and the relative length difference ΔL0 with respect to the total reference sample R are already stored in the storage unit 12 (S5), and are stored. When there is no such data, a process (S6 to S9) of measuring these data and storing the data in the storage unit 12 is performed.

First, the total length L0 of the length measurement reference sample P at the reference temperature T0 is measured using a measuring instrument such as a micrometer.
It is stored in the storage unit 12 (S6). Further, the length measurement reference sample P is placed in the support tube 1 (S7), the base end of the measurement side detection rod 3 is connected to the tip of the sample P, and a constant load is applied by the electromagnetic load coil 5 to the sample. P is fixed in the support tube 1 (S8). At this time, the difference ΔL0 of the relative length of the length measurement reference sample P with respect to the total reference sample R appears as a relative displacement between the coil 6a and the magnet 6b of the differential transformer 6, and corresponds to the relative displacement. Coil 6 of differential transformer 6
The current flowing through a changes. This current change is sent as a differential detection signal (indicating ΔL0) to the storage unit 12 via the interface circuit 10 of the data processing system shown in FIG. 2 and stored therein (S9).

When there are a plurality of measurement samples S to be subjected to thermomechanical analysis, the measurement sample S to be measured first is defined as a length measurement reference sample P, and L0 and ΔL0 measured and stored with respect to the length measurement reference sample P are: Can be used as it is for the subsequent calculation of the length of the measurement sample S. Therefore, the measurement and storage of L0 and ΔL0 for the length measurement reference sample P are performed only at the beginning of the thermomechanical analysis and can be omitted thereafter.

Subsequently, the length measurement reference sample P is taken out of the support tube 1, and the measurement sample S is placed in the support tube 1 instead (S10), and the measurement sample S with respect to the total reference sample R at the reference temperature T0 is obtained. The relative length difference ΔL1 is detected. That is, the base end of the measurement side detection rod 3 is connected to the distal end of the sample S, and a constant load is applied by the electromagnetic load coil 5 to fix the sample S in the support tube 1 (S11). At this time, the difference ΔL between the relative length of the measurement sample S and the total reference sample R
1 appears as a relative displacement between the coil 6a of the differential transformer 6 and the magnet 6b, and the current flowing through the coil 6a of the differential transformer 6 changes according to the relative displacement. This current change is converted into a differential detection signal (indicating ΔL1) by the interface circuit 1 of the data processing system shown in FIG.
0, and is sent to the storage unit 12 and stored therein (S12).

In this way, the storage unit 12 stores L, ΔL
After storing the data relating to 0 and ΔL1, the arithmetic unit 11 of the data processing system calculates the total length L1 of the measurement sample S at the reference temperature T0 based on the equation (iv) shown above, and
2 (S13). With the above, each step of the sample length measuring method according to this embodiment is completed.

Next, the steps of the thermal expansion measurement method for the measurement sample S will be described (see FIG. 7). In this embodiment, the steps of the same method are performed continuously to the end of the steps of the sample length measuring method. That is, after calculating the total length L1 of the measurement sample S at the reference temperature T0 and storing it in the storage unit, the heating furnace 7 is moved and arranged around the support tube 1 and the heating furnace 7 is turned on to turn on the support tube 1 Is heated to an arbitrary measurement temperature T (S14).

Due to this heating, as shown in FIG. 4, the measurement sample S exhibits a constant elongation ΔL,
It also shows a slight but constant elongation ΔL3. The difference ΔL2 between the elongation of each of the samples R and S appears as a relative displacement between the coil 6a of the differential transformer 6 and the magnet 6b, and flows into the coil 6a of the differential transformer 6 in accordance with the relative displacement. The current changes. This current change is sent as a differential detection signal (indicating ΔL2) to the storage unit 12 via the interface circuit 10 of the data processing system shown in FIG. 2, and is stored in the storage unit 12 (S15).

Thus, the storage section 12 stores the total length L of the total reference sample R at the reference temperature T0, the average expansion coefficient C between an arbitrary measurement temperature T and the reference temperature T0, and the reference temperature T0 of the measurement sample S. And the data ΔL2 of the relative elongation of the measurement sample S at the measurement temperature T with respect to the total reference sample R are stored. After that, the arithmetic unit 11 of the data processing system calculates the measured temperature T by the equation (i) shown above.
Difference ΔL between the total reference sample R and the measurement sample S at
Is calculated and stored in the storage unit 12 (S16).

Subsequently, the calculation unit 11 calculates the expansion coefficient α of the measurement sample S according to the equation (ii) shown above, and
(S17). Further, when obtaining the expansion coefficient Cx of the measurement sample S at the predetermined set temperature Tx, the value of the set temperature Tx is input from the keyboard 14 to the storage unit 12 (S18). The calculation unit 11 performs the operation (iii) described above.
Based on the equation, the expansion coefficient Cx at the set temperature Tx is calculated and stored in the storage unit 12 (S19).

With the above, each step of the thermal expansion measurement according to this embodiment is completed. These calculated data can be output via the output unit 13 as needed. When the measurement of the length of the sample and the measurement of the thermal expansion are performed on another measurement sample, the steps S10 to S13 are performed following the steps S3 and S4.
The respective steps of the thermal expansion measurement after 14 are performed (S20).

Next, a sample length measuring method according to a second embodiment of the present invention applied to a full expansion thermomechanical analyzer will be described with reference to FIG.
This will be mainly described. The full-expansion thermomechanical analyzer for carrying out the method has the same structure as that of the differential thermomechanical analyzer shown in FIGS. 1 and 2 except that the reference-side detection rod 2 and its accompanying components are omitted. The coil 6a of the differential transformer 6 is fixed to the apparatus main body.

Prior to carrying out the sample length measuring method, a length measuring reference sample P and a measuring sample S are prepared.
It is checked whether the total length L0 (actually measured value) of the length measurement reference sample P at 0 has already been stored in the storage unit 12 (S31). If not, measurement is performed using a measuring instrument such as a micrometer. Then, the measurement data is input from the keyboard 14 and stored in the storage unit 12 (S32). Also in this embodiment, the normal temperature is set as the reference temperature T0. If the information has already been stored, this step (S32) can be omitted.

Next, it is confirmed whether the total length (reference length) of the length measurement reference sample P relative to the origin of the length measurement of the thermomechanical analyzer at the reference temperature T 0 is already stored in the storage unit 12 ( S33) If it is not stored, the length measurement reference sample P is placed in the support tube 1 (S34), the base end of the measurement side detection rod 3 is connected to the tip of the sample P, and the electromagnetic load coil 5 is connected. The sample P is fixed in the support tube 1 by applying a constant load (S35).

In this embodiment, the origin of the length measurement of the thermomechanical analyzer is the inner bottom surface of the support tube 1 on which the length-measuring reference sample P is arranged, and the total length from this inner bottom surface to the tip of the length-measuring reference sample P ( The reference length) is equal to the coil 6a of the differential transformer 6 and the magnet 6
b, and the current flowing through the coil 6a of the differential transformer 6 changes in accordance with the relative displacement. This current change is sent as a detection signal (indicating the reference length) to the storage unit 12 via the interface circuit 10 of the data processing system shown in FIG. 2, and is stored in the storage unit 12 (S36).

When there are a plurality of measurement samples to be subjected to thermomechanical analysis, the reference length detected and stored at the beginning of the measurement can be used as it is for calculating the length for the subsequent measurement samples. Therefore, the detection and storage (S34 to S36) of the reference length for the length measurement reference sample P are performed only at the beginning of the thermomechanical analysis, and can be omitted thereafter.

Subsequently, the measurement reference sample P is taken out of the support tube 1, and the measurement sample S is placed in the support tube 1 instead (S37), and the base end of the measurement side detection rod 3 is attached to the tip of the sample S. Are connected, and a fixed load is applied by the electromagnetic load coil 5 to fix the sample S in the support tube 1 (S38). Thus, the total length at the reference temperature T0 from the inner bottom surface of the support tube 1 which is the origin of the length measurement of the thermomechanical analyzer to the tip of the measurement sample S is the relative length between the coil 6a and the magnet 6b of the differential transformer 6. It appears as displacement, and the current flowing through the coil 6a of the differential transformer 6 changes in accordance with this relative displacement. This current change is detected as a detection signal via the interface circuit 10 of the data processing system shown in FIG.
And stored in the same section 12 (S39).

In this manner, the relative length from the inner bottom surface of the support tube 1, which is the origin of the length measurement of the thermomechanical analyzer at the reference temperature T0, is defined as the reference length of the length measurement reference sample P and the measurement length of the measurement sample S. The total length is stored in the storage unit 12. After that, the calculation unit 11 calculates the difference ΔL1 between the stored reference length of the length measurement reference sample P and the detected value of the full length of the measurement sample, and stores the difference in the storage unit 12 (S40). Further, the calculation unit 11
Using ΔL1 and the total length (actually measured value) L0 of the length measurement reference sample P, the total length L1 of the measurement sample S is calculated and stored based on the equation (v) shown above (S41). With the above, each step of the sample length measuring method according to this embodiment is completed. Thereafter, the thermal expansion measurement by the full expansion type thermomechanical analyzer is continuously performed, and the expansion coefficient and the expansion coefficient of the sample S can be calculated using the total length L1 of the measurement sample S already stored.

The present invention is not limited to the above embodiment. For example, the sample length measuring method and the thermal expansion measuring method according to the first and second aspects of the present invention are based on the principle that a relative difference between one sample and another sample is detected under an arbitrary temperature state. The present invention can be applied to various employed differential thermomechanical analyzers to facilitate the work.
In addition, the sample length measuring method according to the third aspect of the present invention is a method for measuring the length of one sample relative to an arbitrary reference length under an arbitrary temperature condition. The present invention can be applied to a full expansion type thermomechanical analyzer to facilitate the operation.

[0049]

As described above, according to the present invention, the length L1 at the reference temperature T0 is automatically obtained by the thermomechanical analyzer, thereby facilitating the measurement operation.

[Brief description of the drawings]

FIG. 1 is a front sectional view showing a configuration of a general differential thermomechanical analyzer.

FIG. 2 is a block diagram showing a data processing system of the apparatus.

FIG. 3 is a schematic diagram for explaining a sample length measuring method applied to a differential thermomechanical analyzer.

FIG. 4 is a schematic diagram for explaining a thermal expansion measurement method applied to a differential thermomechanical analyzer.

FIG. 5 is a schematic diagram for explaining a sample length measuring method applied to a full expansion thermomechanical analyzer.

FIG. 6 is a flowchart for explaining steps of a sample length measuring method according to the first embodiment of the present invention.

FIG. 7 is a flowchart for explaining steps of a thermal expansion measuring method according to the first embodiment of the present invention.

FIG. 8 is a flowchart for explaining steps of a sample length measuring method according to a second embodiment of the present invention.

[Explanation of symbols]

 1: Support tube 2: Reference side detection rod 3: Measurement side detection rod 6: Differential transformer 7: Heating furnace 8: Thermocouple 10: Interface circuit 11: Operation unit 12: Storage unit 13: Output unit 14: Keyboard

──────────────────────────────────────────────────続 き Continued on front page (58) Field surveyed (Int.Cl. ⁶ , DB name) G01N 25/00-25/72

Claims (3)

(57) [Claims] 1. A means for detecting a relative length difference between one sample and another sample disposed in a support tube under an arbitrary temperature condition, and a predetermined calculation based on the detection result. A thermomechanical analyzer comprising means for performing a process, wherein a total reference sample and a length measurement reference sample having a known total length L0 at the reference temperature are respectively arranged in the support tube, and a total reference sample at the reference temperature is provided. Detecting the difference ΔL0 in the relative length of the length measurement reference sample with respect to, and arranging the total reference sample and the measurement sample in the support tube, and measuring the relative length of the measurement sample with respect to the total reference sample at the reference temperature. Detecting the difference ΔL1 in length, and measuring based on the total length L0 of the length measurement reference sample, the difference ΔL0 in the relative length of the length measurement reference sample, and the difference ΔL1 in the relative length of the measurement sample. Total length L1 of sample at standard temperature
Calculating the length of the sample in the thermomechanical analyzer. 2. A means for detecting a relative length difference between one sample and another sample placed in a support tube under an arbitrary temperature condition, and a predetermined calculation based on the detection result. A thermomechanical analyzer provided with means for performing processing, a total reference sample having a known total length L at a reference temperature and an average expansion coefficient C between an arbitrary measured temperature and a reference temperature, and a total length at a reference temperature. A length measurement reference sample having a known L0 is placed in each of the support tubes, and a difference ΔL0 between a relative length of the length measurement reference sample and a total length of the reference sample at a reference temperature is measured.
Detecting the relative length difference ΔL1 of the measurement sample with respect to the total reference sample at the reference temperature by arranging the total reference sample and the measurement sample in the support tube; Of the measurement sample at the reference temperature based on the total length L0 of the measurement sample, the relative length difference ΔL0 of the measurement reference sample, and the relative length difference ΔL1 of the measurement sample.
Calculating the relative elongation of the measurement sample relative to the total reference sample at an arbitrary measurement temperature by arranging the total reference sample and the measurement sample in the support tube; The total length L of the reference sample at the reference temperature and the average expansion coefficient C between any measurement temperature and the reference temperature, the total length L1 of the measurement sample at the reference temperature, and the relative value of the measurement sample at the arbitrary measurement temperature. Calculating a coefficient of expansion or a coefficient of expansion of the measurement sample based on a typical elongation difference ΔL2. 3. A detecting means for arranging one sample in a support tube and detecting a difference in a relative length of the one sample with respect to an arbitrary reference length under an arbitrary temperature condition, and the detecting means. A thermomechanical analyzer provided with arithmetic means for performing predetermined arithmetic processing based on the result, wherein a length measurement reference sample having a known overall length L0 at a reference temperature is arranged in the support tube; Detecting a relative length of the length measurement reference sample at a reference temperature with respect to the length measurement origin; and
The relative length of the reference sample at the quasi-temperature is defined as the reference length.
Before the step of storing, a measurement sample was placed on the support tube, the group <br/> relative length difference ΔL1 the measurement sample with respect to the quasi-length at the reference temperature Te
A step of detecting the serial detection means, the overall length L0 of the measurement reference sample, based on the measurement relative length difference ΔL1 of the sample to the reference length, the calculating means the total length L1 under the reference temperature of the measurement sample A method for measuring the length of a sample in a thermomechanical analyzer, comprising the steps of: