JP5662219B2 - Sample positioning method and thermal analysis apparatus using the same - Google Patents

Description

  The present invention relates to a sample positioning method such as an analyzer and a thermal analyzer that measures changes in physical properties due to temperature changes of the sample using the sample positioning method.

  As for the thermal analysis apparatus, a dynamic viscoelasticity measuring apparatus that measures changes in viscoelasticity due to the temperature of a sample is known (for example, see Patent Document 1). Many conventional devices of this type apply an alternating stress or strain to the sample fixed on the chuck by the operator, and measure the viscoelasticity of the sample from the correlation with the generated strain or stress. It is composed.

  On the other hand, with respect to the sample positioning method in the thermal analyzer, there is an apparatus equipped with a positioning hole for placing the sample in the thermal sensor portion that can be removed from the analyzer (for example, Patent Document 2). reference).

JP 2001-99778 A JP 2005-345333 A

  In the dynamic viscoelasticity measuring apparatus described in Patent Document 1 described above, it is known that the measurement result changes depending on the installation state of the sample.

  For example, in the case of a sample having orientation, the complex elastic modulus increases as the load direction and the sample orientation direction coincide. When measuring the complex elastic modulus of such a sample, in general, in order to obtain the maximum value, it is desirable that the load direction be set in a straight line with respect to the direction of sample orientation. However, whether or not the sample is in an optimal installation state can only be determined from the results of actually performing a plurality of measurements, and there is a problem that even a person who is used to the measurement to some extent cannot reduce labor.

  On the other hand, when using a jig as in Patent Document 2, in order to place a sample with high accuracy on the load application portion, the dimensions of the jig itself, the load application portion, and the sample The difference needs to be reduced. Therefore, there exists a subject that exact positioning is difficult when the dimension of a sample is not decided like the dynamic viscoelasticity measuring apparatus of patent document 1. FIG. There is also a problem that there is a risk of changing the positional relationship during removal.

  Thus, when imposing work such as applying a load to the sample, the position on the sample on which the work acts is important in combination with the direction of the work. Therefore, in the sample positioning method according to the present invention, the peripheral portion including the sample is observed before the measurement is started, and the geometric positional relationship between the sample and the apparatus is compared from the observed image to determine the installation state of the sample. The purpose is to judge the suitability and make the operator recognize it, and to perform good positioning without contact with the apparatus and the sample.

  In addition, the positioning method includes various thermal analyzers such as a differential scanning calorimeter that causes a sensitivity sensor to function on a sample, and a dynamic viscoelasticity measuring device or a thermomechanical measuring device that applies a mechanical load to the sample. By adapting to the above, it is possible to provide the thermal analysis device of the present invention with high sample positioning efficiency and high accuracy.

The sample positioning method according to the present invention includes an observation image acquisition step of acquiring an observation image of a sample and a peripheral portion of the sample of the analyzer, and image processing for dividing the sample and the peripheral portion of the sample of the analyzer from the observation image by the observation device process and, from the image of the sample and the sample peripheral portion of the observation image which is a region divided by the image processing step by indexing their geometrical positions, the respective relative positions at any site of the sample and the sample peripheral portion A comparison step for determining a comparison criterion and comparing the relationship between two position references as the comparison criterion, a sample state determination step for determining the suitability of the sample installation state based on the comparison, and causing the operator to recognize the determination result A determination result output step.

  The thermal analysis apparatus of the present invention also includes a viscoelasticity measuring apparatus, a differential scanning calorimeter, and a thermomechanical measuring apparatus that include a temperature control mechanism capable of arbitrarily changing the temperature of the sample and uses the sample positioning method according to the present invention. It is applicable to either.

  According to the thermal analysis apparatus according to the present invention, it is possible to measure and quantify the determination of the sample installation state in a non-contact manner. As a result, it is possible to reduce the time required for the measurement, reduce the load on the operator associated with optimizing the installation state of the sample, and improve the measurement accuracy.

It is a flowchart of the sample positioning method of the thermal analyzer concerning this invention. It is a conceptual diagram of the sample mounting state of the viscoelasticity measuring apparatus (DMA) concerning this invention. It is a conceptual diagram of the wide-area observation image of DMA concerning this invention. It is a flowchart of the sample positioning method of Example 1 concerning this invention. It is a conceptual diagram of the sample mounting state of the suggestion scanning calorimeter (DSC) concerning this invention. It is a conceptual diagram of the wide range observation image of DSC concerning this invention. It is a flowchart of the sample positioning method of Example 2 concerning this invention.

An outline of the sample positioning method according to the present invention will be described with reference to the flowchart of FIG.
In step 1, the sample is placed in a predetermined position on the thermal analysis device, and in this state, as an observation image acquisition step, a wide area image is acquired so as to include the sample and the peripheral device portion by a CCD or the like.

  In step 2, in the acquired wide area image, the sample portion and the device portion are divided into regions by image processing using a computer. In this step, it is more preferable to add an additional step for confirming whether the area division processing itself is appropriate.

  In step 3, a determination criterion for the position of each of the sample and the device is determined on the image so that the relative positional relationship between the sample portion and the device portion can be understood in the image processed in the above step. As a determination criterion for the position, consideration is given to an aspect in which a comparative determination can be made on an image such as a series of straight lines or an overlap of concentricity.

  Step 4 compares the sample determined in the above step with the determination criteria of the apparatus and makes a pass / fail determination. Pass / fail can be determined by using a computer and geometrically analyzing the relative position according to the comparison target on the image according to the comparison method. In that case, automatic determination is possible by providing a threshold value within a numerical allowable range.

Step 5 outputs a determination result to be recognized by the operator when the position of the sample is not within the allowable range in the above step. The actual output is preferably displayed visually using a monitor.
Below, positioning of the sample of a viscoelasticity measuring apparatus and a differential scanning calorimeter is explained in full detail as an Example.

Example 1
A viscoelasticity measuring apparatus will be given as an example of the thermal analysis apparatus according to the present invention and will be described with reference to FIG.
FIG. 2 shows a schematic diagram of the chamber in a state where a sample is placed in the viscoelasticity measuring apparatus.

  The sample 1 is held at both ends by a chuck 2, one of which is fixed to the housing of the apparatus and the other is fixed to the probe 3. The probe 3 is elastically held in the housing, and the chuck 2 is fixed to one end thereof. An AC force generator 5 is installed on the other end side, and an AC force can be applied to the sample 1 via the probe 3 and the chuck 2. A displacement detector 6 is installed around the probe 3 so that relative displacement can be detected.

The temperature control mechanism 4 is controlled based on a set temperature program by a measurement control function provided integrally therewith.
The observation device 8 is installed outside the temperature control mechanism 4 and images the sample 1, the chuck 2, and the probe 3 in the temperature control mechanism 4 through the observation window 7.
The obtained image is output to the image processing device 9. In the image processing apparatus 9, the areas of the sample 1, the chuck 2, and the probe 3 are extracted by image processing.

  The sample state determination unit 10 calculates the geometric relationship between the sample 1, the chuck 2, and the probe 3 based on the information on the region of the sample 1, the chuck 2, and the probe 3 of the image obtained by the image processing device 9, It is determined whether or not it is within a predetermined allowable range, and if it is within the allowable range, a pass determination is made, and if it is out of the allowable range, a failure determination is made. The result of the pass / fail is displayed on the determination result output unit 11 and notified to the operator.

  Next, the steps of the sample positioning method of the present invention will be described with reference to the flowchart shown in FIG. The operator places the sample 1 on the chuck 2 in advance and inputs the dimensions of the placed sample 1 and the measurement mode, that is, the type of the chuck 2.

  Step 1) A wide area image including the sample 1, the chuck 2, and the probe 3 is acquired by the observation device 8 using a CCD or the like.

  Step 2) The image processing device 9 performs image processing of the wide area image acquired in the above step (S21 to 22), and the sample 1, the chuck 2, and the probe in the image based on the dimensions of the sample 1 and the type of the chuck 2 input in advance by the operator. An area corresponding to 3 is extracted (S23 to 24). Here, it is once determined whether or not the region extraction has been successfully performed. By doing so, errors in image processing can be eliminated.

  Step 3) The geometric relationship among the areas of the sample 1, chuck 2 and probe 3 in the image is calculated by the sample state determination machine 10 using the dimensions of the sample 1 and the type of the chuck 2 inputted in advance. . In the configuration shown in FIG. 2, the sample center line L1 and the probe center line L2 in FIG. 3 are determined on the image as position determination criteria. Then, it is determined whether or not there is a problem in the relative position based on the degree of connection between the two straight lines. The comparison of the degree of series is performed by calculating the angle formed by the two straight lines L1 and L2.

Step 4) If the calculated angle is equal to or less than the threshold value representing the allowable range, the evaluation of the installation state is determined to be acceptable, and the positioning ends. Otherwise, it will be rejected.
Step 5) When the sample installation state calculated by the sample state determination device 10 is unacceptable, the result is output to the determination result output unit 11.
Step 6) If the test fails, re-install the sample and return to Step 1 to make the same determination.

(Example 2)
Next, a differential scanning calorimeter is given as an example of the thermal analyzer according to the present invention and will be described with reference to FIG.
FIG. 5 is a schematic diagram showing a state in which a sample is installed in a measuring apparatus in a differential scanning calorimeter.

  The sample 21 is installed on the sensor unit 22. The sensor unit 22 includes a sensor for detecting the temperature change of the sample 21, and the temperature is changed by the temperature control mechanism 23, and the temperature of the sample unit 21 is changed as the temperature of the sensor unit 22 is changed. Configured to do.

The temperature control mechanism 23 is controlled based on a set temperature program by a measurement control function provided integrally therewith.
The observation device 24 is installed outside the temperature control mechanism 23 so as to take an image of the sample 21 and the sensor unit 22 inside the temperature control mechanism 23.

  The obtained observation image is subjected to image processing by the image processing device in the same manner as the viscoelasticity measuring device configured in FIG. 2, and the geometric relationship between the sample 21 and the sensor unit 22 is determined by the sample state determination device. Calculate and notify the operator of the pass / fail result.

Next, the steps of the sample positioning method of the present invention will be described with reference to the flowchart shown in FIG. As in the first embodiment, the operator places the sample 21 on the sensor unit 22 and inputs the dimensions of the placed sample 21 in advance.
Step 1) A wide area image including the sample 21 and the sensor unit 22 is acquired by the observation device 24 using a CCD or the like.

  Step 2) Similar to the dynamic viscoelasticity measuring apparatus having the configuration shown in FIG. 2, the image processing apparatus performs image processing of the wide area image in the previous step (S21 to 22), the dimensions of the sample 21 input by the operator in advance, the known sensor A region corresponding to the sample 21 and the sensor unit 22 in the image is extracted from the size and shape of the unit 22 (S23 to 24). In addition, the region extraction result confirms its quality (S25).

  Step 3) The geometrical relationship between the region of the sample 21 and the sensor unit 22 in the image is calculated using the dimension of the sample 21 inputted in advance and the known dimension and shape of the sensor unit 22. In this case, since it is ideal that the sensor and the sample are concentric, in the configuration illustrated in FIG. 5, the closer the distance between the sample center point C1 and the sensor unit center point C2 in FIG. Therefore, the distance between C1 and C2 is measured.

Step 4) If the calculated distance is equal to or less than the threshold, the evaluation of the installation state is determined to be acceptable, and the positioning ends. Otherwise, fail and go to the next step.
Step 5) If the above step fails, notify the operator of the evaluation result of the calculated installation state of the sample.
Step 6) Reinstall the sample and return to Step 1 again to make the same determination.

  In this way, the positioning of the sample can be determined by measuring and quantifying the sample installation state in a non-contact manner by comparing the relative position criteria by using the surrounding apparatus part. It becomes possible.

  In the above-described embodiment, when the position pass / fail judgment at step 4 fails, the position correction is made and then the process returns to step 1 again. However, the positional deviation amount is recorded. You can then proceed to the target measurement as is. The problem can be eliminated if correction of data for the later target measurement is possible based on the amount of misalignment.

  Moreover, although the case of the viscoelasticity measuring apparatus and the differential scanning calorimeter was shown in the Example, if this positioning method is applicable, this invention is not limited to them. The technical idea of the present invention is particularly significant when applied to a thermal analyzer.

DESCRIPTION OF SYMBOLS 1 ... Sample 2 ... Chuck 3 ... Probe 4 ... Temperature control mechanism 5 ... AC force generator 6 ... Displacement detector 7 ... Observation window 8 ... Observation device 9 ... Image processing device 10 ... Sample state determination device 11 ... Determination result display part L1 ... sample center line L2 ... probe center line 21 ... sample 22 ... sensor unit 23 ... temperature control mechanism 24 ... observation device L1 ... sample center line C1 ... sample center point L2 ... sensor unit center line C2 ... sensor unit center point

Claims (5)

An observation image acquisition step (S1) for acquiring an observation image of the sample and the peripheral portion of the sample of the analyzer;
An image processing step (S2) for dividing the sample and a peripheral portion of the sample of the analyzer from the observation image;
The geometric position is calculated from the sample of the observation image divided into regions in the image processing step and the image of the peripheral portion of the sample, and the relative position of each of the sample and the peripheral portion of the sample is determined at an arbitrary position. A comparison step (S3) for determining the comparison criteria of the two and comparing the relationship between the two location criteria as the comparison criteria ;
A sample state determination step (S4) for determining the suitability of the sample installation state based on the comparison;
A determination result output step (S5) for allowing an operator to recognize the determination result, and a sample positioning method. The comparison step (S3)
In the observation image which is a region divided by the image image processing step, the position reference of any site of the sample peripheral portion, and any position reference of a portion the analyzer side of a portion corresponding to said analysis device Is ,
The sample positioning method according to claim 1 , wherein the position reference of the sample compares a position where the work is applied to the sample and a position reference of the sample determined from the work direction. The thermal analyzer is a thermal analyzer that performs the sample positioning method according to claim 1, wherein the thermal analyzer includes:
A temperature control mechanism that can arbitrarily change the temperature of the sample ;
A sample placement unit for placing the sample;
A detector for detecting displacement or thermal change of the sample;
An imaging device for obtaining an observation image of the sample and its peripheral portion;
An image processing device that performs image processing acquired by the imaging device. The position reference on the analyzer side is a center line in the longitudinal direction passing through the center in the cross section of the probe weighting the sample at the time of dynamic viscoelasticity measurement ,
Position reference of the sample is a center line passing through a section center of the sample to be parallel to the load application direction of the probe, a method of positioning a sample according to claim 2. The analyzer is a differential scanning calorimeter,
In the comparison step (S3),
Positional reference any site of the sample peripheral portion, a central point of the thermal sensor in the differential scanning calorimetry meter,
Position reference for any portion of the sample, Ri sectional center point der of the sample,
The sample positioning method according to claim 1 , wherein in the sample state determination step (S4), the suitability of the installation state of the sample is determined based on the distance between the center point of the thermal sensor and the center point of the cross section of the sample.

Images