JP2018179817A - Sample heating furnace and heat analyzer - Google Patents

Abstract

PROBLEM TO BE SOLVED: To clearly observe an observation object existing in a hollow portion 23 in a sample heating furnace 20.SOLUTION: A heating furnace body 21 includes opening observation windows 22a, 25a, and 26a for observing a sample S in a hollow portion 23 from the outside. The outside of the heating furnace body 21 includes a visual field adjustment member. A visual field adjustment component 30 includes a visual field adjustment window 32, and uses the visual field adjustment window 32 to restrict the range within the hollow portion 23 that can be observed from the outside through the observation windows 22a, 25a, and 26a. Even when the observation windows 22a, 25a, and 26a are formed in relatively large sizes, the visual field adjustment member allows clear observation of the original observation object at a narrowed visual field.SELECTED DRAWING: Figure 2

Description

  The present invention relates to a sample heating furnace for heating a sample, and a thermal analysis apparatus in which the sample heating furnace is incorporated.

  Thermal analysis devices include TG (thermogravimetry) devices, DTA (differential thermal analysis) devices, DSC (differential scanning calorimetry) devices, and various other types. The TG apparatus is an apparatus that measures the weight change of a sample with respect to temperature change or passage of time. The DTA device simultaneously heats the thermally stable standard sample and the sample to be measured, measures the temperature difference that appears between the two when the sample responds to heat, and It is a device that knows the thermal change that has occurred. And the thermal analysis device which combines the function of these TG apparatus and DTA apparatus is TG-DTA apparatus. In addition, the DSC apparatus is an apparatus for measuring the amount of heat when a sample under heating, cooling or constant temperature undergoes an endothermic reaction or an exothermic reaction. Furthermore, as an apparatus which analyzes the evolved gas by heating, there are TG-MS (thermogravimetry & mass spectrometry) apparatus, TPD (temperature programmed desorption analysis) apparatus, and the like.

These thermal analyzers incorporate a sample heating furnace for heating the sample.
Patent Document 1 discloses a sample heating furnace and a thermal analyzer of this type. The sample heating furnace disclosed in Patent Document 1 includes an opening (observation window) for observing the sample disposed inside from the outside, and heating the sample through the opening using an imaging device such as a camera. It is configured to be able to photograph a sample heated inside the furnace.

  Now, the observation window provided in the sample heating furnace may be formed larger. For example, the opening 24 (observation window) depicted in FIG. 8 of Patent Document 1 has a first measurement position 14 for disposing a sample to be measured set inside a sample heating furnace and a standard sample. Both of the two measurement positions 15 are formed in a size that can be visually recognized from the outside. Although the purpose of forming the observation window larger depends on the developer, for example, the relative position of the sample heating furnace relative to the sample may be moved to finely adjust the heating condition of the sample, in which case the opening 24 also moves Since the range in which the sample can be observed from the outside fluctuates, the opening 24 may be formed larger in consideration of this positional fluctuation.

  On the other hand, when the observation window is formed large, scattered light from the outside enters the hollow portion of the sample heating furnace from the observation window, and subtle changes including the color tone of the sample can not be accurately observed, or an imaging device In addition to the sample to be measured, light rays from the surroundings may be incident, which may have adverse effects such as being unable to clearly observe the contour and color of the sample to be originally observed and their changes. .

International Publication No. 2017/033526

  The present invention has been made in view of the above-described circumstances, and it is an object of the present invention to clearly observe an observation target in a hollow portion of a sample heating furnace.

In order to achieve the above object, the present invention relating to a sample heating furnace is a sample heating furnace having a function of placing a sample in a hollow portion of a heating furnace main body and heating the sample,
In the heating furnace main body, an observation window for observing the sample in the hollow portion from the outside is opened and provided, and a visual field adjustment means is provided outside the heating furnace main body,
The visual field adjusting means is characterized by having a function of adjusting the range in the hollow portion that can be observed from the outside through the observation window.

  By providing the visual field adjusting means in this way, even if the observation window is formed to be large, it is possible to narrow the visual field to the original observation object and to observe clearly.

Here, the visual field adjustment means can be constituted by, for example, a visual field adjustment component disposed outside the heating furnace main body. The view adjustment component is configured to have a view adjustment window, and to limit the range in the hollow portion that can be observed from the outside through the observation window by the view adjustment window.
If the visual field adjustment means is configured by the visual field adjustment component, it is possible to shield the scattered light from the outside by the visual field adjustment component and to suppress the incidence of the scattered light into the hollow portion of the heating furnace main body. External light beams for illuminating the inside of the hollow portion of the furnace body are taken from the view adjustment window. That is, the visual field adjustment component also functions as an external scattered light shielding component, and the visual field adjustment window also functions as an external illumination adjustment window.

  In the sample heating furnace provided with the function of arranging the sample to be measured and the standard sample side by side in the hollow portion of the heating furnace main body and heating these samples, the view adjustment window of the view adjustment component is as follows. It is preferable to comprise. That is, the visual field adjustment window is configured to limit the range of the visual field where the hollow portion of the heating furnace main body can be observed from the observation position set outside the heating furnace main body to the range not including the standard sample including the sample to be measured. I assume.

  By thus configuring the visual field adjustment window, it is possible to clearly see only the sample to be measured and to clearly observe the sample to be measured from the observation position set on the outside of the heating furnace main body. Is possible.

Moreover, it is preferable that the sample heating furnace of this invention is equipped with the cover which covers the circumference | surroundings of a heating furnace main body. By covering the heating furnace main body with the cover, it is possible to suppress the entry of cooled air from the outside into the hollow portion through the observation window, and to keep the temperature distribution in the hollow portion uniform.
Here, the cover is preferably formed with an opening at a position facing the observation window, and the opening is closed by a light transmitting filter. Thereby, it is possible to prevent the entry of cold air from the opening while securing a visual field for observing the inside of the hollow from the outside through the filter.

Further, according to the present invention relating to the thermal analysis device, in the thermal analysis device in which a sample heating furnace for heating a sample disposed in the hollow portion of the heating furnace main body is incorporated,
The heating furnace main body is provided with an observation window for observing the sample in the hollow portion from the outside, and
A field adjustment means is provided on the outside of the furnace body,
The visual field adjusting means is characterized by having a function of adjusting the range in the hollow portion that can be observed from the outside through the observation window.

Here, the visual field adjusting means may be provided not only in the sample heating furnace but also in a portion other than the sample heating furnace of the thermal analysis device.
By providing the visual field adjusting means in this way, even if the observation window is formed to be large, it is possible to narrow the visual field to the original observation object and to observe clearly.
The visual field adjustment means can be constituted by, for example, a visual field adjustment component disposed outside the heating furnace body. The view adjustment component is configured to have a view adjustment window, and to limit the range in the hollow portion that can be observed from the outside through the observation window by the view adjustment window.
In the case where the sample heating furnace arranges the sample to be measured and the standard sample side by side in the hollow portion of the heating furnace body and heats each of these samples, the visual field adjustment window of the visual field adjustment component is as follows. It is preferable to comprise. That is, the visual field adjustment window is configured to limit the range of the visual field where the hollow portion of the heating furnace main body can be observed from the observation position set outside the heating furnace main body to the range not including the standard sample including the sample to be measured. I assume.
By thus configuring the visual field adjustment window, it is possible to clearly see only the sample to be measured and to clearly observe the sample to be measured from the observation position set on the outside of the heating furnace main body. Is possible.

  As described above, according to the present invention, by providing the visual field adjustment means, it is possible to clearly observe the observation target even if the observation window is formed to be larger.

It is an exploded perspective view showing the appearance of the thermal analysis device concerning the embodiment of the present invention. It is a side sectional view showing the sample heating furnace concerning the embodiment of the present invention. It is a perspective view showing composition of a sample heating furnace concerning an embodiment of the present invention. It is an exploded perspective view showing the composition of the sample heating furnace concerning the embodiment of the present invention. It is a perspective view showing composition of a sample heating furnace concerning an embodiment of the present invention. It is a top view showing composition of a sample heating furnace concerning an embodiment of the present invention. It is a side sectional view showing the modification of the sample heating furnace concerning the embodiment of the present invention. It is a top view showing the modification of the sample heating furnace concerning the embodiment of the present invention.

Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.
As shown in FIG. 1, in the thermal analysis apparatus according to the present embodiment, a sample heating furnace 20 is mounted and incorporated on a moving table 11 provided in an apparatus main body 10. The movable table 11 is movable back and forth in the direction of arrow AB in the figure, and the sample heating furnace 20 is opened by the movement of the movable table 11 in the direction of arrow A, and the sample S placement portion set in the apparatus main body 10 Is exposed. The sample S is exchanged in a state in which the sample S placement portion is exposed, and the sample heating furnace 20 is closed by the movement of the movable table 11 in the arrow B direction, and the sample S placement portion is inserted into the hollow portion 23 of the heating furnace main body 21. Store.

  A housing 12 is installed around the sample heating furnace 20, and an imaging device 13 is fixed to the housing 12. As the imaging device 13, a camera capable of capturing an enlarged image called a microscope, a commercially available digital camera, a video camera or the like can be applied.

As shown in FIG. 2, the sample heating furnace 20 incorporates the heater 22 having a configuration in which a heater wire is wound around a cylindrical bobbin in the heating furnace main body 21. The sample S (target to be measured) and the standard sample S0 are arranged side by side in the hollow portion 23 of the heater 22 (that is, the hollow portion of the sample heating furnace 20). The sample S and the standard sample S0 are arranged in the sample S arrangement portion set in the apparatus main body 10 as described above, and arranged in the hollow portion 23 of the sample heating furnace 20 with the closing operation of the sample heating furnace 20. It will be
The heater 22 generates heat when current flows through the heater wire, and heats the sample S and the standard sample S0 disposed in the hollow portion 23 with the radiation heat.
In the hollow portion 23 of the heater 22, there is further provided a protective tube 24 formed of a heat-resistant transparent material such as quartz glass, and the sample S and the standard sample S0 are inside the protective tube 24 (inside the hollow portion). Be placed.
A heat insulating cylinder 25 is coaxially disposed on the outer periphery of the heater 22, and the heat insulating cylinder 25 prevents the heat from the heater 22 from leaking to the outside. Further, an outer frame 26 is provided on the outer periphery of the heat insulating cylinder 25, and the heater 22, the protective pipe 24 and the heat insulating cylinder 25 are supported by the outer frame 26 to constitute the heating furnace main body 21.

The observation windows 22a, 25a, 26a are respectively opened and provided in the heater 22, the heat insulating cylinder 25 and the outer frame 26 constituting the heating furnace main body 21, and the heating furnace main body passes through the respective observation windows 22a, 25a, 26a. The inside of the hollow portion 23 of 21 is observed from the outside. In the present embodiment, these observation windows 22a, 25a, 26a are formed in such a size that both the sample S in the hollow portion 23 and the standard sample S0 can be visually recognized from the outside.
And the image incident part of the imaging apparatus 13 is arrange | positioned in the external observation position which can visually recognize the inside of the hollow part 23 of the heating furnace main body 21 through these observation windows 22a, 25a, 26a.

The sample heating furnace 20 further includes a visual field adjustment component 30. The visual field adjustment component 30 has a function as a visual field adjustment means for adjusting the range in the hollow portion 23 which can be observed from the outside through the observation windows 22a, 25a, 26a provided in the heating furnace main body 21.
As shown in FIG. 3, the visual field adjustment component 30 in the present embodiment is formed of a U-shaped metal plate, and a visual field adjustment window 32 is formed in the ceiling surface portion 31 so as to open. The visual field adjustment component 30 is configured to limit the range in the hollow portion 23 which can be observed from the outside through the respective observation windows 22 a, 25 a, 26 a of the heating furnace main body 21 by the visual field adjustment window 32.

The visual field adjustment component 30 is formed by extending the support legs 33 vertically downward from both ends of the ceiling surface portion 31, and as shown in FIG. The visual field adjustment component 30 is positioned so as to be fitted. Each support leg 33 has a spring property, and the state of being fitted to both ends of the movable table 11 can be held with the spring property.
Thereby, the position shift of the visual field adjustment window 32 can be prevented at the time of sample exchange. That is, the visual field adjustment window 32 is adjusted so that the sample S can be observed from the outside through the observation windows 22a, 25a, 26a. On the other hand, for sample exchange, sample exchange is performed in a state in which the sample placement portion provided in the apparatus main body 10 is exposed, and the sample heating furnace 20 is closed by the movement of the movable stand 11 in the arrow B direction, and the sample placement portion It is stored in the hollow portion 23 of the furnace body 21. It is possible to prevent the position of the visual field adjustment window 32 from being displaced with respect to the sample S due to the vibration at this time by holding the leg 33 on the moving table 11.

In such a state of positioning, the visual field adjustment window 32 formed in the visual field adjustment component 30 is a visual field in which the inside of the hollow portion 23 of the heating furnace main body 21 can be observed from the observation position where the image incident portion of the imaging device 13 is disposed. The range is limited to the range not including the standard sample S0 including the sample S to be measured. In the specific example shown in FIG. 2, the edge 22 b of the observation window 22 a of the heater 22 is disposed in accordance with one side edge (one side edge in the width direction) of the sample S to be measured. By arranging the edge 32a of the visual field adjustment window 32 in accordance with the other side edge (the other side edge in the width direction) of the sample S, as shown in the plan view of FIG. Is limited to the range not including the standard sample S0, including the sample S to be measured.
As a result, only the light beam from the sample S to be measured mainly enters the image incident part of the imaging device 13, so that clear image data of the sample S can be collected. Furthermore, extra scattered light from the outside is shielded by the field adjustment component 30, and it is also possible to suppress the incidence of the scattered light into the hollow portion 23 of the heating furnace main body 21.
In addition, in FIG. 2 and FIG. 7 mentioned later, as shown with a dashed-dotted line, the visual field was drawn in parallel, but according to the optical system of the imaging device 13, a visual field converges or spreads radially. There is also.

  As shown in FIG. 3, the sample heating furnace 20 covers the periphery of the heating furnace main body 21 with a cover 40. Then, the ceiling surface 31 of the view adjustment component 30 is inserted into the slits formed near the upper edge portions on both sides of the cover 40 so that the view adjustment component can not be separated from the cover 40. With such a configuration, the view adjustment part can be handled integrally with the heating furnace main body 21, which helps prevent the loss of the view adjustment part.

Further, on the ceiling surface of the cover 40, an opening 41 is formed at a position facing the observation windows 22a, 25a, 26a of the heating furnace main body 21 and the visual field adjustment window 32 of the visual field adjustment component. As shown in FIG. 4, the filter 42 is disposed in the opening 41 to prevent the external cold air from intruding into the inside of the cover 40 through the opening 41. Thereby, the heating furnace main body 21 is partitioned from the outside by the cover 40, so that the cooled air from the outside can be prevented from flowing into the hollow portion 23 of the heating furnace main body 21, and the temperature distribution in the hollow portion 23 is uniform. It is possible to
The filter 42 is formed of a heat-resistant glass plate or the like having light transparency, and the inside of the hollow portion 23 of the heating furnace main body 21 can be observed from the outside through the filter 42. The filter 42 is fixed to the ceiling surface of the cover 40 by a resilient holder 43 screwed to the periphery of the opening 41.

Furthermore, in the present embodiment, as shown in FIG. 4 and FIG. 5, the mounting plate 45 is screwed to the mounting portion 44 provided so as to protrude upward from both side edges in the longitudinal direction of the ceiling surface of the cover 40. An opening (not shown) is formed in the mounting plate 45 at a position facing the opening 41 of the cover 40, and an optical filter 47 is fixed to the opening by a holder 46 having elasticity. The optical filter 47 has a function of adjusting a light beam incident from the hollow portion 23 of the heating furnace main body 21 to the image incident portion of the imaging device 13. For example, by mounting the optical filter 47 having the property of absorbing infrared light to the mounting plate 45, the infrared light emitted from the hollow portion 23 of the heating furnace main body 21 through the observation windows 22a, 25a, 26a is absorbed by the optical filter 47 Be done. As a result, it is possible to suppress the phenomenon that the image data of the imaging device 13 becomes reddish.
The optical filter 47 can be replaced depending on the type of incident light beam.

The present invention is not limited to the embodiments described above.
For example, as shown in FIG. 7 and FIG. 8, the visual field adjustment component 30 is provided with a visual field range in which the hollow portion 23 of the heating furnace main body 21 can be observed from the observation position where the image incident portion of the imaging device 13 is disposed. The configuration may also be made such that the standard sample S0 is limited to a range that does not include the sample S to be measured by the visual field adjustment window 32 alone.
For example, in the case where the relative position of the heater 22 with respect to the sample S is moved to finely adjust the heating condition of the sample S, the observation windows 22a, 25a, 26a also move relative to the sample S. Therefore, it is preferable to limit the range of the field of view in which the inside of the hollow portion 23 of the heating furnace main body 21 can be observed only with the field of view adjustment window 32 because the limited range can be fixed according to the sample S.

  Further, the visual field adjustment component is not limited to the U-shaped configuration as shown in the drawings. Furthermore, the visual field adjustment component can be provided at a site other than the sample heating furnace 20, such as the housing 12 of the thermal analysis device, if necessary.

  The range and the outline of the visual field limited by the visual field adjustment window of the visual field adjustment component can be set arbitrarily. Similarly, the position and opening area of the observation window formed in the heating furnace main body can be set arbitrarily.

The view adjustment component may be adjustable in movement with respect to the furnace body, and may be configured to change the relative position of the view adjustment window with respect to the observation window of the furnace body. Further, the visual field adjustment window is not limited to the rectangular opening as shown in FIG. 6 or FIG. 8 and can be opened in an arbitrary shape as needed.
Furthermore, in the above embodiment, it is also possible to mount the optical filter 47 fixed to the mounting plate 45 to the visual field adjustment window.

  It goes without saying that the thermal analysis apparatus and the sample heating furnace to which the present invention is applied are not limited to those having the structure described in the above-described embodiment.

S: sample (to be measured), S0: standard sample,
10: device main body, 11: moving base, 12: housing, 13: imaging device,
20: sample heating furnace, 21: heating furnace main body, 22: heater, 23: hollow portion, 24: protective tube, 25: heat insulating cylinder, 26: outer frame, 22a, 25a, 26a: observation window,
30: Field of view adjustment parts, 31: Ceiling surface, 32: Field of view adjustment window, 33: Support legs,
40: Cover, 40a: Slit, 41: Opening, 42: Filter, 43: Holder, 44: Mounting portion, 45: Mounting plate, 46: Holder, 47: Optical filter

Claims (7)

A sample heating furnace having a function of placing a sample in a hollow portion of a heating furnace body and heating the sample,
The heating furnace main body is provided with an observation window for observing the sample in the hollow portion from the outside, and a visual field adjustment means is provided outside the heating furnace main body,
The sample heating furnace, wherein the visual field adjusting means has a function of adjusting a range in the hollow portion which can be observed from the outside through the observation window. The field of view adjustment means is composed of a field of view adjustment component disposed outside the heating furnace main body,
The sample heating furnace according to claim 1, wherein the visual field adjustment component has a visual field adjustment window, and a range in the hollow portion that can be observed from the outside through the observation window is limited by the visual field adjustment window. In a sample heating furnace provided with a function of arranging a sample to be measured and a standard sample side by side in the hollow portion of the heating furnace main body and heating each sample,
The visual field adjustment window is a range that does not include the standard sample, including the sample to be measured, from the observation position set on the outside of the heating furnace body to the range of the visual field where the hollow portion of the heating furnace body can be observed. The sample heating furnace according to claim 2, characterized in that it has a configuration to limit. A cover that covers the periphery of the heating furnace body;
4. The cover according to any one of claims 1 to 3, wherein the cover has an opening at a position facing the observation window, and the opening is closed by a light transmitting filter. The sample heating furnace as described in one term. In a thermal analysis apparatus incorporating a sample heating furnace for heating a sample disposed in a hollow portion of a heating furnace main body,
While providing the observation window for observing the sample in the said hollow part from the exterior in the said heating furnace main body,
Field of view adjusting means is provided outside the heating furnace main body,
The thermal analyzer according to claim 1, wherein the visual field adjusting means has a function of adjusting a range in the hollow portion which can be observed from the outside through the observation window. The field of view adjustment means is composed of a field of view adjustment component disposed outside the heating furnace main body,
The thermal analyzer according to claim 5, wherein the visual field adjustment component has a visual field adjustment window, and a range in the hollow portion that can be observed from the outside through the observation window is limited by the visual field adjustment window. The sample heating furnace has a function of arranging a sample to be measured and a standard sample side by side in the hollow portion of the heating furnace main body and heating each sample.
The visual field adjustment window is a range that does not include the standard sample, including the sample to be measured, from the observation position set on the outside of the heating furnace body to the range of the visual field where the hollow portion of the heating furnace body can be observed. The thermal analysis system according to claim 6, characterized in that it has a configuration to limit.

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