JPH08240547A - Method for measuring sample length and thermal expansion in thermomechanical analyzer - Google Patents
Method for measuring sample length and thermal expansion in thermomechanical analyzerInfo
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- JPH08240547A JPH08240547A JP4406495A JP4406495A JPH08240547A JP H08240547 A JPH08240547 A JP H08240547A JP 4406495 A JP4406495 A JP 4406495A JP 4406495 A JP4406495 A JP 4406495A JP H08240547 A JPH08240547 A JP H08240547A
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- length
- measurement
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- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は、測定試料の基準温度
での長さと任意の温度下での長さに基づいて、該測定試
料の膨張率を算出する熱機械分析装置（ＴＭＡ）におい
て、測定試料の基準温度下での長さを自動的に求めるた
めの試料測長方法、およびこの試料測長方法を一部に利
用した熱膨張測定方法に関する。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 the length of a measurement sample at a reference temperature, and a thermal expansion measuring method partially using this sample length measuring method.
【０００２】[0002]
【従来の技術】図１は、示差型熱機械分析装置の一般的
な構成を示している。この示差型熱機械分析装置は、耐
熱性を有する支持管１の内部に基準試料Ｒおよび測定試
料Ｓを配置し、任意の温度下での基準試料Ｒに対する測
定試料Ｓの相対的な伸びを測定できるようになってい
る。2. Description of the Related Art FIG. 1 shows a general structure of a differential thermomechanical analyzer. This differential thermomechanical analyzer arranges a reference sample R and a measurement sample S inside a support tube 1 having heat resistance, and measures a relative elongation of the measurement sample S with respect to the reference sample R at an arbitrary temperature. You can do it.
【０００３】すなわち、支持管１の内部に配置した基準
試料Ｒおよび測定試料Ｓの上端にそれぞれ検出棒２，３
の下端を固定するとともに、各検出棒２，３に任意の測
定荷重を付加する。ここで、基準側の検出棒（以下、基
準側検出棒という）２への加圧には、分銅４等の加圧手
段を使用しており、一方、測定試料側の検出棒（以下、
測定側検出棒という）３への加圧には、電磁荷重コイル
５を使用している。また、基準試料側検出棒２には、差
動トランス６のコイル６ａが固定してあり、一方、測定
側検出棒３には、同トランスの磁石６ｂが固定してあ
る。That is, the detection rods 2 and 3 are respectively provided on the upper ends of the reference sample R and the measurement sample S arranged inside the support tube 1.
The lower end of 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 to pressurize the reference side detection rod (hereinafter referred to as the reference side detection rod) 2, while the measurement sample side detection rod (hereinafter referred to as
An electromagnetic load coil 5 is used to pressurize the measuring 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 same transformer is fixed to the measurement side detection rod 3.
【０００４】支持管１の周囲に加熱炉７を移動配置し、
任意の測定温度に基準試料Ｒおよび測定試料Ｓを加熱す
ると、熱膨張による基準試料Ｒの伸びに応じて基準側検
出棒２が上昇し、差動トランス６のコイル６ａを変位さ
せる。一方、測定側検出棒３も熱膨張による測定試料Ｓ
の伸びに応じて上昇し、差動トランス６の磁石６ｂを変
位させる。このとき、差動トランス６のコイル６ａおよ
び磁石６ｂの変位には、支持管１や各検出棒２，３の膨
張等の誤差成分が含まれているが、これら誤差成分はコ
イル６ａと磁石６ｂの相対変位により相殺される。A heating furnace 7 is movably 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 according to the expansion of the reference sample R due to thermal expansion, and the coil 6a of the differential transformer 6 is displaced. On the other hand, the measurement side detection rod 3 also has a measurement sample S due to thermal expansion.
And the magnet 6b of the differential transformer 6 is displaced. At this time, the displacements of the coil 6a and the magnet 6b of the differential transformer 6 include error components such as expansion of the support tube 1 and the detection rods 2 and 3. These error components are included in the coil 6a and the magnet 6b. Offset by the relative displacement of.
【０００５】このようにして差動トランス６のコイル６
ａと磁石６ｂの間に相対的な変位が生じると、コイル６
ａに流れる電流値が変化する。この電流の変化量を検出
することによって基準試料Ｒと測定試料Ｓとの間の伸び
の差（すなわち、基準試料Ｒに対する測定試料Ｓの相対
的な伸び）を求めることができる。なお、基準試料Ｒや
測定試料Ｓまたはそれら試料の周辺近傍の温度は、支持
管１の内底部に設置した熱電対８によって検出してい
る。In this way, the coil 6 of the differential transformer 6
When a relative displacement occurs between a and the magnet 6b, the coil 6
The value of the current flowing in a changes. By detecting this amount of change in 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. The temperature of the reference sample R, the measurement sample S, or the vicinity of the periphery of these samples is detected by the thermocouple 8 installed on the inner bottom of the support tube 1.
【０００６】[0006]
【発明が解決しようとする課題】測定試料Ｓの膨張率α
は、基準試料Ｒの基準温度Ｔ0 における長さＬ、測定温
度Ｔと基準温度Ｔ0との間の基準試料Ｒの平均膨張係数
Ｃ、測定試料Ｓの基準温度Ｔ0 における長さＬ1、およ
び測定温度Ｔでの基準試料Ｒに対する測定試料Ｓの相対
的な長さの差ΔＬ2 がわかれば、次式によって算出する
ことができる（図４参照）。The coefficient of expansion α of the measurement sample S
Is 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 relative difference .DELTA.L2 of the 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).
【０００７】ΔＬ＝ΔＬ2 ＋ΔＬ3 ΔＬ：温度変化に伴う測定試料Ｓの伸び ΔＬ3：温度変化に伴う基準試料Ｒの伸び ΔＬ3＝Ｃ×（Ｔ−Ｔ0）×Ｌ ∴ ΔＬ＝ΔＬ2 ＋Ｃ×（Ｔ−Ｔ0）×Ｌ ・・・(i) α＝（ΔＬ／Ｌ1）×１００ ［％］ ・・・(ii)ΔL = ΔL2 + ΔL3 ΔL: elongation of the measurement sample S with temperature change ΔL3: elongation of the reference sample R with temperature change ΔL3 = C × (T−T0) × L∴ΔL = ΔL2 + C × (T−T0 ) × L ・ ・ ・ (i) α = (ΔL / L1) × 100 [%] ・ ・ ・ (ii)
【０００８】さらに、測定試料Ｓの膨張率αが求まれ
ば、次式により任意の設定温度Ｔｘにおける同試料Ｓの
膨張係数Ｃｘを算出することができる。 Ｃｘ＝ΔＬ／｛Ｌ1 ×（Ｔ−Ｔｘ）｝ ・・・(iii)Further, if the expansion coefficient α of the sample S to be measured 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)
【０００９】熱機械分析装置は、図２に示すようなデー
タ処理システムを備えており、同システムのインタフェ
ース回路１０を介して入力した差動トランス６からの検
出信号に基づいて、演算部１１が上式の計算を行ない、
測定試料Ｓの膨張率α，膨張係数Ｃｘ等を自動的に算出
し、記憶部１２に記憶するかまたは出力部１３を介して
出力する。The thermomechanical analyzer is equipped with a data processing system as shown in FIG. 2. Based on the detection signal from the differential transformer 6 input via the interface circuit 10 of the system, the arithmetic unit 11 operates. Calculate the above formula,
The expansion coefficient α and the expansion coefficient Cx of the measurement sample S are automatically calculated and stored in the storage unit 12 or output via the output unit 13.
【００１０】さて、従来の熱機械分析装置は、測定温度
Ｔでの基準試料Ｒに対する測定試料Ｓの相対的な長さの
差ΔＬ2 を自動的に検出することはできるが、測定試料
Ｓの膨張率αや膨張係数Ｃｘを算出するために必要とな
る基準試料Ｒの基準温度Ｔ0における長さＬ、任意の測
定温度Ｔと基準温度Ｔ0 との間の平均膨張係数Ｃ、およ
び測定試料Ｓの基準温度Ｔ0における長さＬ1は、別途測
定しデータ処理システムのキーボード１４を使用して記
憶部１２に記憶させておかなければならなかった。The conventional thermomechanical analyzer can automatically detect the relative length difference ΔL2 of the measurement sample S with respect to the reference sample R at the measurement temperature T, but the expansion of the measurement sample S The length L of the reference sample R at the reference temperature T0 necessary for calculating the coefficient α and the expansion coefficient Cx, the average expansion coefficient C between the arbitrary 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 separately measured and stored in the storage unit 12 using the keyboard 14 of the data processing system.
【００１１】このうち基準試料Ｒのと基準温度Ｔ0にお
ける長さＬ、および任意の測定温度Ｔと基準温度Ｔ0 と
の間の平均膨張係数Ｃは、一度測定して記憶させておけ
ば、その後の測定に繰り返し使用することができる。し
かしながら、測定試料Ｓの基準温度Ｔ0における長さＬ1
は、測定毎に同試料Ｓを交換するため、その都度マイク
ロメータ等の測定器具を使い操作員の人手をもって測定
し、キーボード１４の操作により記憶部１２へ記憶させ
なければならず、測定作業が煩雑であった。Of these, the length L of the reference sample R and the length L at the reference temperature T0, and the average expansion coefficient C between the arbitrary measurement temperature T and the reference temperature T0 are measured once and stored. It can be used repeatedly for measurements. However, the length L1 of the measurement sample S at the reference temperature T0 is
Since the same sample S is exchanged for each measurement, the operator must manually measure each time using a measuring instrument such as a micrometer, and the keyboard 14 must be used to store it in the storage unit 12. It was complicated.
【００１２】この発明は、上述した事情に鑑みてなされ
たもので、測定試料の基準温度Ｔ0における長さＬ1 を
熱機械分析装置によって自動的に求め、測定作業の容易
化を実現することを目的とする。The present invention has been made in view of the above circumstances, and it is an object of the present invention to automatically obtain a length L1 of a measurement sample at a reference temperature T0 by a thermomechanical analyzer, thereby facilitating measurement work. And
【００１３】[0013]
【課題を解決するための手段】上記目的を達成するため
に、この発明の第一の試料測長方法は、支持管内に配置
した一の試料に対する他の一の試料の相対的な長さの差
を任意の温度状態のもとで検出する手段と、該検出結果
に基づいて所定の演算処理を行なう手段とを備えたいわ
ゆる示差型熱機械分析装置において、次の工程を含む方
法としてある。In order to achieve the above object, the first method for measuring the length of a sample according to the present invention is a method for measuring the relative length of another sample with respect to one sample placed in a support tube. A so-called differential thermomechanical analyzer including means for detecting a difference under an arbitrary temperature condition and means for performing a predetermined calculation process based on the detection result is a method including the following steps.
【００１４】 総合基準試料および基準温度での全長
Ｌ0が既知である測長基準試料をそれぞれ支持管内に配
置して、基準温度下での総合基準試料に対する測長基準
試料の相対的な長さの差ΔＬ0を検出する工程 総合基準試料および測定試料を支持管内に配置し
て、基準温度での総合基準試料に対する測定試料の相対
的な長さの差ΔＬ1を検出する工程 測長基準試料の全長Ｌ0 、測長基準試料の相対的な
長さの差ΔＬ0、および測定試料の相対的な長さの差Δ
Ｌ1に基づいて測定試料の基準温度における全長Ｌ1を算
出する工程The total length reference sample and the length measurement reference sample whose total length L0 at the reference temperature are known are respectively placed in the support tubes, and the relative length of the length measurement reference sample to the total reference sample under the reference temperature is measured. Step for detecting the difference ΔL0 Step for detecting the difference ΔL1 in the relative length 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 Total length L0 of the length measurement reference sample , The relative length difference ΔL0 of the measurement reference sample, and the relative length difference Δ of the measurement sample
Step of calculating the total length L1 of the measurement sample at the reference temperature based on L1
【００１５】また、この発明の熱膨張測定方法は、支持
管内に配置した一の試料に対する他の一の試料の相対的
な長さの差を任意の温度状態のもとで検出する手段と、
該検出結果に基づいて所定の演算処理を行なう手段とを
備えたいわゆる示差型熱機械分析装置において、次の工
程を含む方法としてある。Further, the thermal expansion measuring method of the present invention comprises means for detecting a difference in relative length of one sample placed in the support tube with respect to another sample under an arbitrary temperature condition,
In a so-called differential thermomechanical analyzer provided with a means for performing a predetermined calculation process based on the detection result, the method includes the following steps.
【００１６】 基準温度での全長Ｌ並びに任意の測定
温度Ｔと基準温度Ｔ0 との間の平均膨張係数Ｃが既知で
ある総合基準試料、および基準温度での全長Ｌ0が既知
である測長基準試料をそれぞれ支持管内に配置して、基
準温度下での総合基準試料に対する測長基準試料の相対
的な長さの差ΔＬ0を検出する工程 総合基準試料および測定試料を支持管内に配置し
て、基準温度での総合基準試料に対する測定試料の相対
的な長さの差ΔＬ1を検出する工程 測長基準試料の全長Ｌ0 、測長基準試料の相対的な
長さの差ΔＬ0、および測定試料の相対的な長さの差Δ
Ｌ1に基づいて測定試料の基準温度における全長Ｌ1を算
出する工程 総合基準試料および測定試料を支持管内に配置し
て、任意の測定温度下での総合基準試料に対する測定試
料の相対的な伸びの差ΔＬ2 を検出する工程 総合基準試料の基準温度での全長Ｌ並びに任意の測
定温度Ｔと基準温度Ｔ0との間の平均膨張係数Ｃ、測定
試料の基準温度下における全長Ｌ1、および任意の測定
温度下での測定試料の相対的な伸びの差ΔＬ2 に基づい
て測定試料の膨張率または膨張係数を算出する工程A comprehensive reference sample in which the total length L at the reference temperature and the average expansion coefficient C between any measurement temperature T and the reference temperature T0 are known, and a measurement reference sample in which the total length L0 at the reference temperature is known Detecting the relative length difference ΔL0 of the length measurement reference sample to the total reference sample under the reference temperature by placing each in the support tube. Detecting relative length difference ΔL1 of measurement sample to total reference sample at temperature Length L0 of measurement reference sample, difference ΔL0 of relative length of measurement reference sample, and relative of measurement sample Difference in length Δ
The process of calculating the total length L1 of the measurement sample at the reference temperature based on L1. The difference in the relative elongation of the measurement sample with respect to the total reference sample at any 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 comprehensive reference sample at the reference temperature, the average expansion coefficient C between the arbitrary measurement temperature T and the reference temperature T0, the total length L1 of the measurement sample under the reference temperature, and the arbitrary measurement temperature Of calculating the expansion coefficient or expansion coefficient of the measurement sample based on the relative elongation difference ΔL2 of the measurement sample in
【００１７】さらに、この発明の第二の試料測長方法
は、支持管内に一の試料を配置し、任意の基準長さに対
する一の試料の相対的な長さの差を任意の温度状態のも
とで検出する手段と、該検出結果に基づいて所定の演算
処理を行なう手段とを備えたいわゆる全膨式熱機械分析
装置において、次の工程を含む方法としてある。Further, according to the second sample length measuring method of the present invention, one sample is arranged in the support tube, and the difference in the relative length of the one sample with respect to an arbitrary reference length is measured under an arbitrary temperature condition. A so-called total expansion thermomechanical analyzer including a means for originally detecting and a means for performing a predetermined calculation process based on the detection result is a method including the following steps.
【００１８】 基準温度での全長Ｌ0 が既知である測
長基準試料を支持管内に配置し、熱機械分析装置の長さ
測定原点に対する該測長基準試料の相対的な長さを検出
する工程 測定試料を支持管内に配置し、検出した熱機械分析
装置の長さ測定原点に対する測長基準試料の相対的な長
さを基準長さとして、基準温度での該基準長さに対する
測定試料の相対的な長さの差ΔＬ1を検出する工程 測長基準試料の全長Ｌ0 、測定試料の相対的な長さ
の差ΔＬ1に基づいて測定試料の基準温度下における全
長Ｌ1を算出する工程A process of arranging a length measurement reference sample having a known total length L 0 at the reference temperature in a support tube and detecting a relative length of the length measurement reference sample with respect to a length measurement origin of a thermomechanical analyzer. The sample is placed in the support tube, and the length of the detected thermomechanical analyzer is relative to the measurement origin.The reference length is the relative length of the measurement reference sample, and the relative length of the measurement sample to the reference length at the reference temperature. Of measuring the length difference ΔL1 of the total length L0 of the measurement reference sample, and calculating the total length L1 of the measurement sample at the reference temperature based on the relative length difference ΔL1 of the measurement sample
【００１９】[0019]
【作用】示差型熱機械分析装置は、上述したように支持
管内に配置した一の試料に対する他の一の試料の相対的
な長さの差を任意の温度状態のもとで検出する長さ検出
手段と、該検出結果に基づいて所定の演算処理を行なう
演算手段とを備えている。したがって、この発明の試料
測長方法における、基準温度下での総合基準試料に対す
る測長基準試料の相対的な長さの差ΔＬ0 を検出する工
程、および基準温度での総合基準試料に対する測定試料
の相対的な長さの差ΔＬ1 を検出する工程については、
上記長さ検出手段によって処理することができる。そし
て、これら各検出結果、およびあらかじめ既知である測
長基準試料の全長Ｌ0 に基づいて、測定試料の基準温度
における全長Ｌ1 算出する工程は、上記演算手段によっ
て自動的に処理することができる。The differential thermomechanical analyzer has a length for detecting a relative length difference between one sample placed in the support tube and another sample as described above under an arbitrary temperature condition. The detection means and the calculation means for performing a predetermined calculation process based on the detection result are provided. Therefore, in the sample length measuring method of the present invention, the step of detecting the relative length difference ΔL 0 of the length measuring reference sample to the total reference sample under the reference temperature, and the step of detecting the measurement sample relative to the total reference sample at the reference temperature For the step of detecting the relative length difference ΔL1,
It can be processed by the length detecting means. Then, the step of calculating the total length L1 of the measurement sample at the reference temperature based on the respective detection results and the previously known total length L0 of the length measurement reference sample can be automatically processed by the arithmetic means.
【００２０】ここで、測定試料の基準温度における全長
Ｌ1の算出式は次のとおりである（図３参照）。 Ｌ1 ＝Ｌ0＋ΔＬ0−ΔＬ1 ・・・(iv)Here, the formula for calculating the total length L1 of the measurement sample at the reference temperature is as follows (see FIG. 3). L1 = L0 + ΔL0−ΔL1 (iv)
【００２１】また、熱膨張測定方法の発明における、測
定試料の基準温度における全長Ｌ1を算出するまでの各
工程は、上記試料測長方法と同様に処理することができ
る。さらに、任意の測定温度下での総合基準試料に対す
る測定試料の相対的な伸びの差ΔＬ2 を検出する工程も
長さ検出手段で処理することができる。そして、これら
の検出結果、およびあらかじめ既知である総合基準試料
の基準温度での全長Ｌ並びに任意の測定温度Ｔと基準温
度Ｔ0 との間の平均膨張係数Ｃに基づいて、測定試料の
膨張率または膨張係数を算出する工程は、上記演算手段
によって自動的に処理することができる。Further, in the invention of the thermal expansion measuring method, each step 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. Furthermore, the step of detecting the relative difference .DELTA.L2 in elongation of the measurement sample with respect to the total reference sample at any measurement temperature can be processed by the length detecting means. Then, based on these detection results, the total length L of the comprehensive 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 of the measurement sample or The step of calculating the expansion coefficient can be automatically processed by the calculation means.
【００２２】上述した各方法において、測長基準試料の
全長Ｌ0 については、マイクロメータなどの測定器具を
使用して測定する作業が必要となるが、一度測定してお
けば、別測定試料の測長に繰り返し使用することができ
る。しかも、基準温度下での総合基準試料に対する測長
基準試料の相対的な長さの差ΔＬ0 は、一度検出すれ
ば、別測定試料の測長に繰り返し使用することができる
ため、その後、ΔＬ0 の検出工程は省略することができ
る。In each of the above-mentioned methods, it is necessary to measure the total length L0 of the length measurement reference sample using a measuring instrument such as a micrometer. It can be used repeatedly for a long time. Moreover, since the relative length difference ΔL0 of the length measurement reference sample to the total reference sample under the reference temperature can be detected once, it can be repeatedly used for the length measurement of another measurement sample. The detection step can be omitted.
【００２３】一方、全膨式熱機械分析装置は、上述した
ように支持管内に一の試料を配置し、任意の基準長さに
対する一の試料の相対的な長さの差を任意の温度状態の
もとで検出する長さ検出手段と、該検出結果に基づいて
所定の演算処理を行なう演算手段とを備えている。On the other hand, in the full expansion thermomechanical analyzer, one sample is arranged in the support tube as described above, and the difference in the relative length of the one sample with respect to an arbitrary reference length is measured under an arbitrary temperature condition. And a length detecting means for detecting the length under the condition, and a calculating means for performing a predetermined calculation processing based on the detection result.
【００２４】したがって、この発明の第二の試料測長方
法における、熱機械分析装置の長さ測定原点に対する該
測長基準試料の相対的な長さ（基準長さ）を検出する工
程、基準温度での該基準長さに対する測定試料の相対的
な長さの差ΔＬ1を検出する工程については、上記長さ
検出手段によって処理することができる。そしてこの検
出結果、およびあらかじめ既知である測長基準試料の全
長Ｌ0 に基づいて、測定試料の基準温度における全長Ｌ
1 算出する工程は、上記演算手段によって自動的に処理
することができる。Therefore, 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 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 can be processed by the length detecting means. Then, based on this detection result and the previously known total length L0 of the length measurement reference sample, the total length L at the reference temperature of the measurement sample
1 The step of calculating can be automatically processed by the calculating means.
【００２５】ここで、測定試料の基準温度における全長
Ｌ1の算出式は次のとおりである（図５参照）。 Ｌ1 ＝Ｌ0−ΔＬ1 ・・・(v)Here, the formula for calculating the total length L1 of the measurement sample at the reference temperature is as follows (see FIG. 5). L1 = L0-ΔL1 (v)
【００２６】なお、測長基準試料の全長Ｌ0 は、マイク
ロメータなどの測定器具を使用して測定する作業が必要
となるが、一度測定しておけば、別測定試料の測長に繰
り返し使用することができる。しかも、基準長さについ
ては、一度検出すれば、別測定試料の測長に繰り返し使
用することができるため、その後、基準長さの検出工程
は省略することができる。The total length L0 of the length measurement reference sample needs to be measured by using a measuring instrument such as a micrometer, but once measured, it is repeatedly used for measuring the length 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 reference length detecting step can be omitted thereafter.
【００２７】[0027]
【実施例】以下、この発明の実施例について図面を参照
して詳細に説明する。まず、示差型熱機械分析装置に適
用するこの発明の第一実施例に係る試料測長方法および
熱膨張測定方法について、図６および図７を主に参照し
て説明する。なお、これらの方法を実施するための示差
型熱機械分析装置は、図１および図２を参照して先に説
明したものと同様であるため、詳細な説明は省略する。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 the first embodiment of the present invention applied to a differential thermomechanical analyzer will be described mainly with reference to FIGS. 6 and 7. Since the differential thermomechanical analyzer for carrying out these methods is the same as that described above with reference to FIGS. 1 and 2, detailed description thereof will be omitted.
【００２８】試料測長方法の実施に先立って、総合基準
試料Ｒ，測長基準試料Ｐ，および測定試料Ｓを用意す
る。この実施例では、各試料を任意長さの円柱状に形成
するが、その他、測定に適当な種々の形状に形成できる
ことは勿論である。また、固体試料に限らず、例えば粉
体状の試料についてもこの実施例方法の対象とすること
ができる。この場合は、粉体試料を任意長さの一定形状
に押し固めて試料とする。Prior to carrying out the sample length measuring method, a comprehensive reference sample R, a length measuring reference sample P, and a measurement sample S are prepared. In this embodiment, each sample is formed into a cylindrical shape having an arbitrary length, but it is needless to say that the sample can be formed into various shapes suitable for measurement. Further, not only solid samples but also powdery samples can be the target of the method of this embodiment. In this case, the powder sample is pressed into a fixed shape having an arbitrary length to form a sample.
【００２９】ここで、総合基準試料Ｒは、示差型熱機械
分析における各種測定の基準となる試料であり、先に説
明した従来技術における基準試料Ｒに相当する。同装置
では、この総合基準試料Ｒに対する別試料の相対的な伸
び（変形）が差動トランス６によって検出される。すな
わち、この総合基準試料Ｒは、加熱による支持管１や各
検出棒２，３の変形、支持管１内の対流などに起因する
検出結果の誤差を相殺し、測定精度を向上させる目的で
示差型熱機械分析に使用される。この総合基準試料Ｒ
は、温度変化に対する変形の小さな材料で、測定試料Ｓ
（測長基準試料Ｐを含む）とほぼ同様の形状に形成す
る。また、総合基準試料Ｒは、後述する基準温度Ｔ0 と
測定温度Ｔとの間の平均膨張係数Ｃがあらかじめ既知で
ある材料によって作成する。Here, the comprehensive reference sample R is a reference sample for various measurements in the differential thermomechanical analysis, and corresponds to the reference sample R in the prior art described above. In this device, the relative extension (deformation) of another sample with respect to this comprehensive reference sample R is detected by the differential transformer 6. That is, the comprehensive reference sample R is used for the purpose of offsetting the error in the detection result due to the deformation of the support tube 1 and the detection rods 2 and 3 due to heating, the convection in the support tube 1 and the like, and improving the measurement accuracy. Used for mold thermomechanical analysis. This comprehensive reference sample R
Is a material whose deformation with respect to temperature change is small, and is a measurement sample S
The same shape as (including the length measurement reference sample P) is formed. The comprehensive reference sample R is made of a material whose average expansion coefficient C between a reference temperature T0 and a measurement temperature T, which will be described later, is known in advance.
【００３０】測長基準試料Ｐは、この実施例に係る試料
測長方法において、基準となる試料長さＬ0（(iv)式参
照） を定めるために必要とされるものである。これら
の各試料を用意したら、まず総合基準試料Ｒについて、
基準温度Ｔ0 と測定温度Ｔとの間の平均膨張係数Ｃおよ
び全長Ｌが、図２に示したデータ処理システムの記憶部
１２に記憶されているか確認し（図６のステップ（以
下、「Ｓ」と略す）１）、記憶されていない場合には、
キーボード１４を使用してこれら膨張係数Ｃ（既知の
値）および全長Ｌのデータを入力する（Ｓ２）。この実
施例では、常温を基準温度Ｔ0 とし、総合基準試料Ｒの
常温における全長Ｌは、マイクロメータ等の測定器具を
使用して測定する。なお、すでに総合基準試料Ｒに関す
るこれらのデータが記憶部１２に記憶されている場合に
は、この工程（Ｓ２）は省略することができる。The length measurement reference sample P is required to determine the reference sample length L0 (see the equation (iv)) in the sample length measuring method according to this embodiment. After preparing each of these samples, first, regarding the comprehensive reference sample R,
It is confirmed 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, referred to as “S” in FIG. 6). 1), if it is 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 room temperature is set as the reference temperature T0, and the total length L of the comprehensive reference sample R at room temperature is measured by using a measuring instrument such as a micrometer. If these data regarding the comprehensive reference sample R are already stored in the storage unit 12, this step (S2) can be omitted.
【００３１】この総合基準試料Ｒを支持管１内に配置し
（Ｓ３）、同試料Ｒの先端に基準側検出棒２の基端を連
結し、分銅４等の加圧手段により一定荷重をかけて、同
試料Ｒを支持管１内に固定する（Ｓ４）。次いで、測長
基準試料Ｐについて、基準温度Ｔ0での全長Ｌ0および総
合基準試料Ｒに対する相対的な長さの差ΔＬ0 が、すで
に記憶部１２に記憶されているか確認し（Ｓ５）、記憶
されていない場合にはこれらのデータを測定し、記憶部
１２へ記憶する工程（Ｓ６〜Ｓ９）を実施する。This comprehensive 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. Then, the sample R is fixed in the support tube 1 (S4). Next, for the length measurement reference sample P, it is confirmed whether or not the total length L0 at the reference temperature T0 and the relative difference ΔL0 with respect to the total reference sample R are already stored in the storage unit 12 (S5) and stored. If not, the steps (S6 to S9) of measuring these data and storing them in the storage unit 12 are performed.
【００３２】まず、基準温度Ｔ0 での測長基準試料Ｐの
全長Ｌ0 を、マイクロメータ等の測定器具を使用して測
定し、この測定データをキーボード１４から入力して、
記憶部１２へ記憶させる（Ｓ６）。さらに、測長基準試
料Ｐを支持管１内に配置し（Ｓ７）、同試料Ｐの先端に
測定側検出棒３の基端を連結し、電磁荷重コイル５によ
り一定荷重をかけて、同試料Ｐを支持管１内に固定する
（Ｓ８）。このとき、総合基準試料Ｒに対する測長基準
試料Ｐの相対的な長さの差ΔＬ0 は、差動トランス６の
コイル６ａと磁石６ｂとの間の相対変位としてあらわ
れ、この相対変位に対応して差動トランス６のコイル６
ａに流れる電流が変化する。この電流変化は、示差検出
信号（ΔＬ0を示す）として、図２に示したデータ処理
システムのインタフェース回路１０を介し記憶部１２に
送られ、同部１２に記憶される（Ｓ９）。First, the total length L0 of the length measurement reference sample P at the reference temperature T0 is measured by using a measuring instrument such as a micrometer, and this measurement data is input from the keyboard 14,
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 measuring 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 in 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 this relative displacement. Coil 6 of the 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 in the same unit 12 (S9).
【００３３】なお、熱機械分析を行なう測定試料Ｓが複
数ある場合は、最初に測定を行なう測定試料Ｓを測長基
準試料Ｐとし、該測長基準試料Ｐに関し測定，記憶した
Ｌ0，ΔＬ0 は、その後の測定試料Ｓに対する長さの算
出にそのまま使用することができる。したがって、測長
基準試料Ｐに関するＬ0，ΔＬ0 の測定，記憶は、熱機
械分析の最初にのみ行ない、その後は省略することがで
きる。When there are a plurality of measurement samples S to be subjected to thermomechanical analysis, the measurement sample S to be measured first is the length measurement reference sample P, and the measured and stored L0 and ΔL0 of the length measurement reference sample P are , And can be directly used 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 can be performed only at the beginning of the thermomechanical analysis, and can be omitted thereafter.
【００３４】続いて、測長基準試料Ｐを支持管１から取
り出し、代わりに測定試料Ｓを支持管１内に配置して
（Ｓ１０）、基準温度Ｔ0 での総合基準試料Ｒに対する
測定試料Ｓの相対的な長さの差ΔＬ1 を検出する。すな
わち、同試料Ｓの先端に測定側検出棒３の基端を連結
し、電磁荷重コイル５により一定荷重をかけて、同試料
Ｓを支持管１内に固定する（Ｓ１１）。このとき、総合
基準試料Ｒに対する測定試料Ｓの相対的な長さの差ΔＬ
1 は、差動トランス６のコイル６ａと磁石６ｂとの間の
相対変位としてあらわれ、この相対変位に対応して差動
トランス６のコイル６ａに流れる電流が変化する。この
電流変化は、示差検出信号（ΔＬ1を示す）として、図
２に示したデータ処理システムのインタフェース回路１
０を介し記憶部１２に送られ、同部１２に記憶される
（Ｓ１２）。Subsequently, the length measurement reference sample P is taken out from the support tube 1, the measurement sample S is placed in the support tube 1 instead (S10), and the measurement sample S relative to the comprehensive reference sample R at the reference temperature T0 is measured. Detect the relative length difference .DELTA.L1. That is, the base end of the measurement side detection rod 3 is connected to the tip 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 relative length difference ΔL of the measurement sample S with respect to the comprehensive 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 in accordance with this relative displacement. This change in current is expressed as a differential detection signal (indicating ΔL1) in the interface circuit 1 of the data processing system shown in FIG.
It is sent to the storage unit 12 via 0 and stored in the storage unit 12 (S12).
【００３５】このようにして、記憶部１２にＬ，ΔＬ
0，ΔＬ1に関するデータを記憶した後、データ処理シス
テムの演算部１１が、先に示した(iv)式に基づき、基準
温度Ｔ0 での測定試料Ｓの全長Ｌ1を計算し、記憶部１
２に記憶する（Ｓ１３）。以上をもって、この実施例に
係る試料測長方法の各工程が終了する。In this way, L, ΔL is stored in the storage unit 12.
After storing the data regarding 0 and ΔL1, the calculation 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 the storage unit 1
It is stored in 2 (S13). With the above, each step of the sample length measuring method according to this embodiment is completed.
【００３６】次に、測定試料Ｓに関する熱膨張測定方法
の工程について説明する（図７参照）。なお、この実施
例では、同方法の工程を試料測長方法の工程終了に連続
して行なっている。すなわち、基準温度Ｔ0での測定試
料Ｓの全長Ｌ1を計算し、記憶部に記憶した後、支持管
１の周囲に加熱炉７を移動配置し、加熱炉７の電源を投
入して支持管１内の総合基準試料Ｒおよび測定試料Ｓを
任意の測定温度Ｔまで加熱する（Ｓ１４）。Next, the steps of the thermal expansion measuring method for the measurement sample S will be described (see FIG. 7). In this embodiment, the steps of the same method are continuously performed after the steps of the sample length measuring method are completed. That is, after the total length L1 of the measurement sample S at the reference temperature T0 is calculated and stored in the storage unit, the heating furnace 7 is moved and arranged around the supporting tube 1, and the heating furnace 7 is turned on to turn on the supporting tube 1. The total reference sample R and the measurement sample S therein are heated to an arbitrary measurement temperature T (S14).
【００３７】この加熱により、図４に示すように測定試
料Ｓは一定の伸びΔＬを示すとともに、総合基準試料Ｒ
も僅かながらではあるが一定の伸びΔＬ3を示す。そし
て、これら各試料Ｒ，Ｓの伸びの差ΔＬ2が、差動トラ
ンス６のコイル６ａと磁石６ｂとの間の相対変位として
あらわれ、この相対変位に対応して差動トランス６のコ
イル６ａに流れる電流が変化する。この電流変化は、示
差検出信号（ΔＬ2を示す）として、図２に示したデー
タ処理システムのインタフェース回路１０を介し記憶部
１２に送られ、同部１２に記憶される（Ｓ１５）。As a result of this heating, the measurement sample S shows a constant elongation ΔL as shown in FIG.
Although it is slight, it shows a constant elongation ΔL3. Then, the difference ΔL2 in elongation between 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 corresponding to this 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 stored in the storage unit 12 (S15).
【００３８】これにより、記憶部１２には総合基準試料
Ｒの基準温度Ｔ0 での全長Ｌ並びに任意の測定温度Ｔと
基準温度Ｔ0 との間の平均膨張係数Ｃ、測定試料Ｓの基
準温度Ｔ0での全長Ｌ1、および測定温度Ｔでの測定試料
Ｓの総合基準試料Ｒに対する相対的な伸びの差ΔＬ2 の
各データが記憶される。その後、データ処理システムの
演算部１１が、先に示した(i)式によって、測定温度Ｔ
における総合基準試料Ｒと測定試料Ｓとの伸びの差ΔＬ
を算出し、記憶部１２に記憶する（Ｓ１６）。As a result, the storage unit 12 stores the total length L of the comprehensive reference sample R at the reference temperature T0, the average expansion coefficient C between the arbitrary measurement temperature T and the reference temperature T0, and the reference temperature T0 of the measurement sample S. And the relative difference ΔL2 in elongation of the measurement sample S at the measurement temperature T with respect to the total reference sample R are stored. After that, the calculation unit 11 of the data processing system calculates the measured temperature T by the formula (i) shown above.
Difference ΔL between the total reference sample R and the measurement sample S in
Is calculated and stored in the storage unit 12 (S16).
【００３９】続いて、演算部１１は、先に示した(ii)式
によって、測定試料Ｓの膨張率αを算出し、記憶部１２
に記憶する（Ｓ１７）。さらに、所定の設定温度Ｔｘに
おける測定試料Ｓの膨張係数Ｃｘを求める場合には、そ
の設定温度Ｔｘの値をキーボード１４から記憶部１２へ
入力する（Ｓ１８）。演算部１１は、先に示した(iii)
式に基づいて、設定温度Ｔｘにおける膨張係数Ｃｘを計
算し、記憶部１２に記憶する（Ｓ１９）。Subsequently, the arithmetic unit 11 calculates the expansion coefficient α of the measurement sample S by the equation (ii) shown above, and the storage unit 12
(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 has the above-mentioned (iii)
The expansion coefficient Cx at the set temperature Tx is calculated based on the equation and stored in the storage unit 12 (S19).
【００４０】以上をもって、この実施例に係る熱膨張測
定の各工程が終了する。これら算出したデータは、必要
に応じ出力部１３を介して出力することができる。な
お、別の測定試料について、続いて試料の測長および熱
膨張測定を実施する場合には、上述したＳ３，Ｓ４の工
程に続いて、Ｓ１０〜Ｓ１３の工程を実施し、さらにＳ
１４以降の熱膨張測定の各工程を行なう（Ｓ２０）。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. In addition, in the case where the length measurement and the thermal expansion measurement of the sample are subsequently performed on another measurement sample, the steps S10 to S13 are performed subsequent to the steps S3 and S4 described above, and further S
Each step of thermal expansion measurement after 14 is performed (S20).
【００４１】次に、全膨式熱機械分析装置に適用するこ
の発明の第二実施例に係る試料測長方法について、図８
を主に参照して説明する。なお、同方法を実施するため
の全膨式熱機械分析装置は、図１および図２に示した示
差型熱機械分析装置の、基準側検出棒２およびそれに付
随する構成部分が省略された構造となっており、差動ト
ランス６のコイル６ａは、装置本体に固定されている。Next, the sample length measuring method according to the second embodiment of the present invention applied to the full expansion thermomechanical analyzer will be described with reference to FIG.
Will be mainly described. The full expansion thermomechanical analyzer for carrying out the method has a structure in which the reference-side detection rod 2 and its accompanying components of the differential thermomechanical analyzer shown in FIGS. 1 and 2 are omitted. The coil 6a of the differential transformer 6 is fixed to the apparatus body.
【００４２】試料測長方法の実施に先立って、測長基準
試料Ｐ，および測定試料Ｓを用意し、まず、基準温度Ｔ
0での測長基準試料Ｐの全長Ｌ0（実測値）がすでに記憶
部１２に記憶されているか確認し（Ｓ３１）、記憶され
ていない場合には、マイクロメータ等の測定器具を使用
して測定し、その測定データをキーボード１４から入力
して記憶部１２に記憶する（Ｓ３２）。この実施例にお
いても、常温を基準温度Ｔ0 としている。なお、すでに
記憶されている場合には、この工程（Ｓ３２）は省略で
きる。Prior to carrying out the sample length measuring method, a length measuring reference sample P and a measuring sample S are prepared, and first, a reference temperature T
It is confirmed whether the total length L0 (measured value) of the length measurement reference sample P at 0 is already stored in the storage unit 12 (S31), and if not stored, 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 the reference temperature T0. Note that this step (S32) can be omitted if it is already stored.
【００４３】次に、測長基準試料Ｐについて、基準温度
Ｔ0 での熱機械分析装置の長さ測定原点に対する相対的
な全長（基準長さ）がすでに記憶部１２に記憶されてい
るか確認し（Ｓ３３）、記憶されていない場合には、支
持管１内に測長基準試料Ｐを配置し（Ｓ３４）、同試料
Ｐの先端に測定側検出棒３の基端を連結し、電磁荷重コ
イル５により一定荷重をかけて、同試料Ｐを支持管１内
に固定する（Ｓ３５）。Next, for the length measurement reference sample P, it is confirmed whether the total length (reference length) relative to the length measurement origin of the thermomechanical analyzer at the reference temperature T0 is already stored in the storage unit 12 ( S33), if 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 Then, a constant load is applied to fix the sample P in the support tube 1 (S35).
【００４４】この実施例では、熱機械分析装置の長さ測
定原点を、測長基準試料Ｐを配置した支持管１の内底面
とし、この内底面から測長基準試料Ｐの先端までの全長
（基準長さ）が、差動トランス６のコイル６ａと磁石６
ｂとの間の相対変位としてあらわれ、この相対変位に対
応して差動トランス６のコイル６ａに流れる電流が変化
する。この電流変化は、検出信号（基準長さを示す）と
して、図２に示したデータ処理システムのインタフェー
ス回路１０を介し記憶部１２に送られ、同部１２に記憶
される（Ｓ３６）。In this embodiment, the length measurement origin of the thermomechanical analyzer is the inner bottom surface of the support tube 1 in which the length measurement reference sample P is arranged, and the total length from this inner bottom surface to the tip of the length measurement reference sample P ( (Reference length) is the coil 6a and the magnet 6 of the differential transformer 6.
It appears as a relative displacement with respect to b, and the current flowing through the coil 6a of the differential transformer 6 changes corresponding to this relative displacement. This change in current is sent as a detection signal (indicating a reference length) to the storage unit 12 via the interface circuit 10 of the data processing system shown in FIG. 2 and stored in the storage unit 12 (S36).
【００４５】なお、熱機械分析を行なう測定試料が複数
ある場合は、測定開始当初に検出，記憶した基準長さ
が、その後の測定試料に対する長さの算出にそのまま使
用することができる。したがって、測長基準試料Ｐに関
する基準長さの検出，記憶（Ｓ３４〜Ｓ３６）は、熱機
械分析の最初にのみ行ない、その後は省略することがで
きる。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 sample. Therefore, the detection and storage (S34 to S36) of the reference length for the length measurement reference sample P can be performed only at the beginning of the thermomechanical analysis, and can be omitted thereafter.
【００４６】続いて、測長基準試料Ｐを支持管１から取
り出し、代わりに測定試料Ｓを支持管１内に配置して
（Ｓ３７）、同試料Ｓの先端に測定側検出棒３の基端を
連結し、電磁荷重コイル５により一定荷重をかけて、同
試料Ｓを支持管１内に固定する（Ｓ３８）。これによ
り、熱機械分析装置の長さ測定原点である支持管１の内
底面から測定試料Ｓの先端までの基準温度Ｔ0 における
全長が、差動トランス６のコイル６ａと磁石６ｂとの間
の相対変位としてあらわれ、この相対変位に対応して差
動トランス６のコイル６ａに流れる電流が変化する。こ
の電流変化は、検出信号として、図２に示したデータ処
理システムのインタフェース回路１０を介し記憶部１２
に送られ、同部１２に記憶される（Ｓ３９）。Subsequently, the length measurement reference sample P is taken out from the support tube 1, 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. And the sample S is fixed in the support tube 1 by applying a constant load by the electromagnetic load coil 5 (S38). As a result, the total length at the reference temperature T0 from the inner bottom surface of the support tube 1 which is the length measurement origin of the thermomechanical analyzer to the tip of the measurement sample S is the relative distance between the coil 6a of the differential transformer 6 and the magnet 6b. It appears as a 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 is stored in the same section 12 (S39).
【００４７】このようにして、基準温度Ｔ0での熱機械
分析装置の長さ測定原点である支持管１の内底面からの
相対寸法として、測長基準試料Ｐの基準長さおよび測定
試料Ｓの全長が記憶部１２に記憶される。その後、演算
部１１がこれら記憶された測長基準試料Ｐの基準長さお
よび測定試料の全長の検出値の差ΔＬ1を計算し、記憶
部１２に記憶する（Ｓ４０）。さらに、演算部１１は、
このΔＬ1および測長基準試料Ｐの全長（実測値）Ｌ0を
使い、先に示した(v)式に基づいて、測定試料Ｓの全長
Ｌ1を算出し記憶する（Ｓ４１）。以上をもって、この
実施例に係る試料測長方法の各工程が終了する。その後
は、全膨式熱機械分析装置による熱膨張測定を引き続き
行ない、すでに記憶してある測定試料Ｓの全長Ｌ1を使
用して同試料Ｓの膨張率や膨張係数を算出することがで
きる。In this way, as the relative dimension from the inner bottom surface of the support tube 1 which is the length measurement origin of the thermomechanical analyzer at the reference temperature T0, the reference length of the measurement reference sample P and the measurement sample S are measured. 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 total length of the measurement sample, and stores it in the storage unit 12 (S40). Further, the calculation unit 11
Using this ΔL1 and the total length (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. After that, the thermal expansion measurement by the total expansion thermomechanical analyzer is continuously performed, and the expansion coefficient and expansion coefficient of the sample S can be calculated using the already stored total length L1 of the sample S.
【００４８】なお、この発明は上述した実施例に限定さ
れるものではない。例えば、請求項１，２の発明に係る
試料測長方法および熱膨張測定方法は、一の試料に対す
る他の一の試料の相対的な差を任意の温度状態のもとで
検出するという原理を採用している各種示差型熱機械分
析装置に適用して、作業の容易化を図ることができる。
また、請求項３の発明に係る試料測長方法は、任意の基
準長さに対する一の試料の相対的な長さの差を任意の温
度状態のもとで検出する原理を採用している各種全膨式
熱機械分析装置に適用して、作業の容易化を図ることが
できる。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 inventions of claims 1 and 2 are based on the principle that a relative difference between one sample and another sample is detected under an arbitrary temperature condition. It can be applied to various adopted differential thermomechanical analyzers to facilitate work.
Further, the sample length measuring method according to the invention of claim 3 adopts the principle of detecting a difference in relative length of one sample with respect to an arbitrary reference length under an arbitrary temperature condition. It can be applied to a full expansion thermomechanical analyzer to facilitate work.
【００４９】[0049]
【発明の効果】以上説明したように、この発明によれ
ば、基準温度Ｔ0 における長さＬ1 を熱機械分析装置に
よって自動的に求め、測定作業の容易化を図ることがで
きる。As described above, according to the present invention, the length L1 at the reference temperature T0 can be automatically obtained by the thermomechanical analyzer, and the measurement work can be facilitated.
【図１】一般的な示差型熱機械分析装置の構成を示す正
面断面図である。FIG. 1 is a front cross-sectional view showing the configuration of a general differential thermomechanical analyzer.
【図２】同装置のデータ処理システムを示すブロック図
である。FIG. 2 is a block diagram showing a data processing system of the same apparatus.
【図３】示差型熱機械分析装置に適用する試料測長方法
を説明するための模式図である。FIG. 3 is a schematic diagram for explaining a sample length measuring method applied to a differential thermomechanical analyzer.
【図４】示差型熱機械分析装置に適用する熱膨張測定方
法を説明するための模式図である。FIG. 4 is a schematic diagram for explaining a thermal expansion measurement method applied to a differential thermomechanical analyzer.
【図５】全膨式熱機械分析装置に適用する試料測長方法
を説明するための模式図である。FIG. 5 is a schematic diagram for explaining a sample length measuring method applied to the full expansion thermomechanical analyzer.
【図６】この発明の第一実施例に係る試料測長方法の工
程を説明するためのフローチャートである。FIG. 6 is a flowchart for explaining steps of the sample length measuring method according to the first embodiment of the present invention.
【図７】この発明の第一実施例に係る熱膨張測定方法の
工程を説明するためのフローチャートである。FIG. 7 is a flow chart for explaining steps of the thermal expansion measuring method according to the first embodiment of the present invention.
【図８】この発明の第二実施例に係る試料測長方法の工
程を説明するためのフローチャートである。FIG. 8 is a flow chart for explaining steps of a sample length measuring method according to a second embodiment of the present invention.
１：支持管 ２：基準側検出棒 ３：測定側検出棒 ６：差動トランス ７：加熱炉 ８：熱電対 １０：インタフェース回路 １１：演算部 １２：記憶部 １３：出力部 １４：キーボード 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: Calculation unit 12: Storage unit 13: Output unit 14: Keyboard
Claims (3)
の一の試料の相対的な長さの差を任意の温度状態のもと
で検出する手段と、該検出結果に基づいて所定の演算処
理を行なう手段とを備えた熱機械分析装置において、 総合基準試料および基準温度での全長Ｌ0が既知である
測長基準試料をそれぞれ前記支持管内に配置して、基準
温度下での総合基準試料に対する測長基準試料の相対的
な長さの差ΔＬ0を検出する工程と、 総合基準試料および測定試料を前記支持管内に配置し
て、基準温度での総合基準試料に対する測定試料の相対
的な長さの差ΔＬ1を検出する工程と、 測長基準試料の全長Ｌ0 、前記測長基準試料の相対的な
長さの差ΔＬ0、および前記測定試料の相対的な長さの
差ΔＬ1に基づいて測定試料の基準温度における全長Ｌ1
を算出する工程と、 を含むことを特徴とする熱機械分析装置における試料測
長方法。1. A means for detecting a difference in relative length between one sample placed in a support tube and another sample under an arbitrary temperature condition, and a predetermined calculation based on the detection result. In a thermomechanical analyzer equipped with a means for performing processing, a total reference sample and a length measurement reference sample whose total length L0 at a reference temperature are known are respectively arranged in the support tubes, and a total reference sample under the reference temperature is provided. Detecting the relative length difference ΔL0 of the measurement reference sample with respect to, and arranging the total reference sample and the measurement sample in the support tube, and the relative length of the measurement sample with respect to the total reference sample at the reference temperature. Measuring the difference ΔL1 in length, and measuring based on the total length L0 of the length measurement reference sample, the relative length difference ΔL0 of the length measurement reference sample, and the difference ΔL1 in the relative length of the measurement sample. Total length L1 of sample at reference temperature
A method of measuring a sample in a thermomechanical analyzer, comprising:
の一の試料の相対的な長さの差を任意の温度状態のもと
で検出する手段と、該検出結果に基づいて所定の演算処
理を行なう手段とを備えた熱機械分析装置において、 基準温度での全長Ｌ並びに任意の測定温度と基準温度と
の間の平均膨張係数Ｃが既知である総合基準試料、およ
び基準温度での全長Ｌ0が既知である測長基準試料をそ
れぞれ前記支持管内に配置して、基準温度下での総合基
準試料に対する測長基準試料の相対的な長さの差ΔＬ0
を検出する工程と、 総合基準試料および測定試料を前記支持管内に配置し
て、基準温度での総合基準試料に対する測定試料の相対
的な長さの差ΔＬ1を検出する工程と、 測長基準試料の全長Ｌ0 、前記測長基準試料の相対的な
長さの差ΔＬ0、および前記測定試料の相対的な長さの
差ΔＬ1に基づいて測定試料の基準温度における全長Ｌ1
を算出する工程と、 総合基準試料および測定試料を前記支持管内に配置し
て、任意の測定温度下での総合基準試料に対する測定試
料の相対的な伸びの差ΔＬ2 を検出する工程と、 前記総合基準試料の基準温度での全長Ｌ並びに任意の測
定温度と基準温度との間の平均膨張係数Ｃ、前記測定試
料の基準温度下における全長Ｌ1、および前記任意の測
定温度下での測定試料の相対的な伸びの差ΔＬ2 に基づ
いて測定試料の膨張率または膨張係数を算出する工程
と、 を含むことを特徴とする熱機械分析装置における熱膨張
測定方法。2. A means for detecting a difference in relative length of one sample with respect to another sample arranged in the support tube under an arbitrary temperature condition, and a predetermined calculation based on the detection result. In a thermomechanical analyzer equipped with a means for performing treatment, a total length L at a reference temperature and a total reference sample having a known average expansion coefficient C between an arbitrary measurement temperature and the reference temperature, and a total length at the reference temperature The length-measuring reference samples whose L0 are known are arranged in the supporting tubes, respectively, and the relative length difference ΔL0 of the length-measuring reference sample to the total reference sample under the reference temperature is increased.
And a step of detecting the relative reference sample and the measurement sample in the support tube to detect the relative length difference ΔL1 of the measurement sample to the reference sample at the reference temperature, and the measurement reference sample L0, the relative length difference ΔL0 of the measurement reference sample, and the relative length difference ΔL1 of the measurement sample based on the total length L1 of the measurement sample at the reference temperature.
And a step of arranging the total reference sample and the measurement sample in the support tube to detect a difference ΔL2 in relative elongation of the measurement sample with respect to the total reference sample under an arbitrary measurement temperature, The total length L of the reference sample at the reference temperature, the average expansion coefficient C between any measurement temperature and the reference temperature, the total length L1 of the measurement sample under the reference temperature, and the relative of the measurement sample under the arbitrary measurement temperature. Of the expansion coefficient or expansion coefficient of the measurement sample based on the difference .DELTA.L2 in elongation of the sample, and the thermal expansion measuring method in the thermomechanical analyzer.
準長さに対する前記一の試料の相対的な長さの差を任意
の温度状態のもとで検出する手段と、該検出結果に基づ
いて所定の演算処理を行なう手段とを備えた熱機械分析
装置において、 基準温度での全長Ｌ0 が既知である測長基準試料を前記
支持管内に配置し、前記熱機械分析装置の長さ測定原点
に対する該測長基準試料の相対的な長さを検出する工程
と、 測定試料を前記支持管内に配置し、前記検出した熱機械
分析装置の長さ測定原点に対する測長基準試料の相対的
な長さを基準長さとして、基準温度での該基準長さに対
する測定試料の相対的な長さの差ΔＬ1を検出する工程
と、 測長基準試料の全長Ｌ0 、前記測定試料の相対的な長さ
の差ΔＬ1に基づいて測定試料の基準温度下における全
長Ｌ1を算出する工程と、 を含むことを特徴とする熱機械分析装置における試料測
長方法。3. A means for arranging one sample in a support tube, and detecting a difference in relative length of the one sample with respect to an arbitrary reference length under an arbitrary temperature condition, and the detection result. In a thermomechanical analyzer equipped with means for performing a predetermined calculation process based on the above, a length measurement reference sample having a known total length L0 at a reference temperature is arranged in the support tube, and the length of the thermomechanical analyzer is A step of detecting a relative length of the length measurement reference sample with respect to a measurement origin, and a measurement sample arranged in the support tube, and the detected length of the thermomechanical analyzer relative to the length measurement reference sample with respect to the measurement origin. Different length as a reference length, a step of detecting a difference ΔL1 in relative length of the measurement sample with respect to the reference length at a reference temperature, a total length L0 of the length measurement reference sample, a relative length of the measurement sample. Based on the length difference ΔL1 under the reference temperature of the measurement sample Sample measurement method in the thermal mechanical analysis apparatus characterized by comprising the steps of: calculating a length L1, a.
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| JPH06201621A (en) * | 1992-12-30 | 1994-07-22 | Shimadzu Corp | Heat analyzer |
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| JP2016095196A (en) * | 2014-11-13 | 2016-05-26 | サムソン エレクトロ−メカニックス カンパニーリミテッド． | Thermal expansion coefficient measurement method and thermomechanical analysis apparatus |
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