JP2018115859A - X-ray analysis cell, X-ray analysis container, X-ray analysis apparatus and X-ray analysis method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an X-ray analysis technique that can be practically used by a more simple method such as being capable of performing X-ray analysis by on-the-spot measurement under the same atmosphere as an actual process while heating a sample at a high temperature of 800°C or higher.SOLUTION: An X-ray analysis container includes an X-ray analysis cell, a tubular body unit, and sealing members. The X-ray analysis cell includes at least one infrared heat generating unit that absorbs infrared light radiated from the outside and generates heat, and an X-ray irradiating unit that holds the sample. The infrared heat generating unit has a light receiving surface for receiving infrared rays. The X-ray irradiating unit is provided in a part of the infrared heat generating unit so as to be heated by heat conduction from the infrared heat generating unit. The tubular body unit contains the X-ray analysis cell therein and has an infrared window through which infrared rays can transmit. The sealing member is disposed at either end portion of the cylindrical body unit and holds an X-ray window.SELECTED DRAWING: Figure 10

Description

  The present invention relates to an X-ray analysis cell, an X-ray analysis container, an X-ray analysis apparatus, and an X-ray analysis method for X-ray analysis of a sample state while heating the sample at a high temperature.

  X-ray analysis is widely used as a means for non-destructive analysis of materials, and technology is improved from various viewpoints in order to meet various needs of users.

  An example of such an X-ray analysis technique is X-ray analysis in molten salt plating (for example, Non-Patent Documents 1 and 2 and Patent Document 1). Specifically, in recent years, structures using plating have been commercialized, and the use of Ti, Ta, W, etc. as higher-strength materials is expected, and as an important technology for using these materials Molten salt plating has been proposed, in which X-ray analysis is used.

Iihara, Koji Nitta, Shigeaki Uemura, Yoshihiro Saito, Koji Yamaguchi, Toshiyuki Nohira, “In-situ Analysis of Tungsten Ions in Molten Salt Bath for Tungsten Plating”, Sunbeam Annual Report / Results, vol. 1 2011, issued March 2012 Hirozo Shinoda, Shun Fujieda, Shuaki Sato, Tsubasa Ishii, “Analysis of Molten Salt Structure by XAFS Aiming at Recovery of Rare Metals from Waste by Molten Salt Electrolysis”, FY2014 SPring-8 Industrial New Field Support Issues / General Issues (Industry field) Implementation report (2014A), issued on February 27, 2015

Japanese Utility Model Publication No. 2-150555

  In X-ray analysis in industrial processes that require heating as well as normal temperature, such as the molten salt plating described above, in recent years, so-called “in-situ measurement”, that is, actual processes at higher temperatures such as 800 ° C. or higher. X-ray analysis under the same atmosphere as that described above has been required, and further improvement in analysis technology is required.

  However, in Non-Patent Document 1, about 250 ° C. is the upper limit of the heating temperature, which is far from 800 ° C. or higher. In addition, although plating can be performed by energizing the sample, the sample is sealed, so even if moisture or gas is generated from the sample during plating, these cannot be removed and the actual process It is not possible to analyze the gas flow along the line.

  And in the nonpatent literature 2, heating temperature is 500 degreeC and does not reach the said 800 degreeC or more. Further, since the sample is sealed in the measurement graphite cell, it is impossible to energize the sample, and even if moisture or gas is generated from the sample, these cannot be removed.

Further, in Patent Document 1, since the sample is directly irradiated with infrared rays and heated, a sample that does not absorb infrared rays such as WO ₃ and Na ₂ WO ₄ is unlikely to generate heat and can obtain a sufficiently high temperature. Can not.

  Therefore, we offer X-ray analysis technology that can be put into practical use with a simpler method, such as in-situ measurement and X-ray analysis in the same atmosphere as the actual process while heating the sample at a high temperature of 800 ° C or higher. It is requested to do.

An X-ray analysis cell according to one embodiment of the present invention is provided.
Comprising at least one infrared heat generating part that absorbs infrared rays irradiated from the outside and generates heat; and an X-ray irradiation part that holds a sample;
The infrared heat generating portion has a light receiving surface that receives the infrared light,
The X-ray irradiation unit is an X-ray analysis cell provided in a part of the infrared heating unit so as to be heated by heat conduction from the infrared heating unit.

The container for X-ray analysis according to one embodiment of the present invention is
An X-ray analysis container comprising an X-ray analysis cell, a cylindrical body part, and a sealing member,
The X-ray analysis cell includes at least one infrared heat generating unit that generates heat by absorbing infrared rays irradiated from the outside, and an X-ray irradiation unit that holds a sample,
The infrared heat generating portion has a light receiving surface that receives the infrared light,
The X-ray irradiation unit is provided in a part of the infrared heating unit so as to be heated by heat conduction from the infrared heating unit,
The cylindrical body portion houses the X-ray analysis cell therein, and has an infrared window portion through which the infrared rays can pass.
The sealing member is an X-ray analysis container having an X-ray window provided at each end of the cylindrical body.

An apparatus for X-ray analysis according to one embodiment of the present invention includes:
An X-ray analysis apparatus comprising an X-ray analysis container and an infrared irradiation device,
The X-ray analysis container is an X-ray analysis container comprising an X-ray analysis cell, a cylindrical body part, and a sealing member,
The X-ray analysis cell includes at least one infrared heat generating unit that generates heat by absorbing infrared rays irradiated from the outside, and an X-ray irradiation unit that holds a sample,
The infrared heat generating portion has a light receiving surface that receives the infrared light,
The X-ray irradiation unit is provided in a part of the infrared heating unit so as to be heated by heat conduction from the infrared heating unit,
The cylindrical body portion houses the X-ray analysis cell therein, and has an infrared window portion through which the infrared rays can pass.
The sealing member is provided at both ends of the cylindrical body part, and has an X-ray window part,
The infrared irradiation apparatus is an X-ray analysis apparatus that irradiates infrared rays from the outside of the X-ray analysis container toward a light receiving surface of the infrared heat generating portion of the X-ray analysis cell.

An X-ray analysis method according to one embodiment of the present invention includes:
An X-ray analysis method for X-ray analysis of a sample using an X-ray analysis apparatus,
The X-ray analysis apparatus is an X-ray analysis apparatus including an X-ray analysis container and an infrared irradiation device,
The X-ray analysis container is an X-ray analysis container comprising an X-ray analysis cell, a cylindrical body part, and a sealing member,
The X-ray analysis cell includes at least one infrared heat generating unit that generates heat by absorbing infrared rays irradiated from the outside, and an X-ray irradiation unit that holds a sample,
The infrared heat generating portion has a light receiving surface that receives the infrared light,
The X-ray irradiation unit is provided in a part of the infrared heating unit so as to be heated by heat conduction from the infrared heating unit,
The cylindrical body portion houses the X-ray analysis cell therein, and has an infrared window portion through which the infrared rays can pass.
The sealing member is provided at both ends of the cylindrical body part, and has an X-ray window part,
The infrared irradiation device irradiates infrared rays from the outside of the X-ray analysis container toward the light-receiving surface of the infrared heating portion of the X-ray analysis cell;
The X-ray analysis method includes a sample holding step for holding a sample to be analyzed in the X-ray irradiation unit of the X-ray analysis cell;
A sample heating step of heating the sample held by the X-ray irradiation unit by irradiating infrared rays from the infrared irradiation device toward the light receiving surface of the X-ray analysis cell;
An X-ray irradiation step of irradiating X-rays from the outside of one of the X-ray windows toward the heated sample;
An X-ray analysis method comprising: a sample analysis step of analyzing the sample by analyzing the X-ray transmitted through the sample and emitted from the other X-ray window to the outside of the X-ray analysis container is there.

  It is possible to provide an X-ray analysis cell, an X-ray analysis container, an X-ray analysis apparatus, and an X-ray analysis method that enable in-situ measurement at a high temperature by a simple method.

It is a perspective view which shows the cell for X-ray analysis which concerns on one Embodiment of this invention. It is a top view which shows the cell for X-ray analysis shown in FIG. It is a figure explaining the temperature fall of the X-ray irradiation part in the cell for X-ray analysis shown in FIG. It is a figure which shows the relationship between the temperature of the infrared rays heat generating part in the cell for X-ray analysis shown in FIG. 1, and the temperature of an X-ray irradiation position. It is a perspective view which shows another example of the cell for X-ray analysis which concerns on one Embodiment of this invention. It is a figure explaining the temperature fall of the X-ray irradiation part in the cell for X-ray analysis shown in FIG. It is a perspective view which shows a part of container for X-ray analysis which concerns on one Embodiment of this invention. It is a perspective view of the base which mounts the cell for X-ray analysis which concerns on one Embodiment of this invention. It is a perspective view which shows the method of mounting the cell for X-ray analysis on a base. It is a perspective view of the whole container for X-ray analysis concerning one embodiment of the present invention. It is sectional drawing which shows typically the structure of the apparatus for X-ray analysis which concerns on one Embodiment of this invention. In one Embodiment of this invention, it is a schematic diagram which shows a mode that the cylindrical side surface of a cylindrical trunk | drum is covered with the heat resistant cloth. It is a perspective view which shows a part of X-ray analysis apparatus in which the cell for X-ray analysis shown in FIG. 5 was accommodated. It is a figure explaining X-ray diffraction (XRD) analysis. It is a figure which shows an example of the XANES spectrum in a X-ray absorption spectroscopy (XAFS) analysis. It is a figure which shows an example of the EXAFS spectrum in a X-ray absorption spectroscopy (XAFS) analysis.

[Description of Embodiment of the Present Invention]
First, embodiments of the present invention will be listed and described.

(1) An X-ray analysis cell according to an aspect of the present invention includes at least one infrared heat generating unit that generates heat by absorbing infrared rays irradiated from the outside, and an X-ray irradiation unit that holds a sample.
The infrared heat generating portion has a light receiving surface that receives the infrared light,
The X-ray irradiation unit is an X-ray analysis cell provided in a part of the infrared heating unit so as to be heated by heat conduction from the infrared heating unit.

  In the cell for X-ray analysis according to this aspect, an infrared heat generating portion is provided that generates heat by receiving and absorbing infrared light irradiated from the outside on the light receiving surface. And the X-ray irradiation part is provided in connection with the infrared heat generating part. For this reason, heat can be efficiently transmitted from the infrared heating unit to the X-ray irradiation unit, and the X-ray irradiation unit can be heated to an extremely high temperature in a short time.

(2) In the X-ray analysis cell, it is preferable that the infrared heat generating portion and the X-ray irradiation portion are integrated with the same material.

  When the infrared heat generating part and the X-ray irradiation part are integrated with the same material, excellent thermal shock resistance can be exhibited, and heating is performed during X-ray analysis performed by irradiating the sample with X-rays. Even if cooling is repeated, there is no possibility of breakage such as cracks, and excellent durability can be exhibited. Here, the term “integrated” means that it is configured as a continuous object without interposing other members, and is cut out from the same material and processed, or the same material is put into a mold and molded. It is preferable from the viewpoint of strength.

(3) In the cell for X-ray analysis, the infrared heat generating part and the X-ray irradiation part are preferably made of a carbon-based inorganic material or black ceramics.

  As a material of the cell for X-ray analysis, a material excellent in thermal conductivity is preferable in addition to a high absorption rate of irradiated infrared rays and a high X-ray transmittance. As such a material, a carbon-based inorganic material or black ceramics is preferable. Graphite (C) and silicon carbide (SiC) are preferable as the carbon-based inorganic material, and black diamond is preferable as the black ceramic. Among these materials, graphite (C) and silicon carbide (SiC) are excellent in durability and workability, and an X-ray analysis cell in which an infrared heating part and an X-ray irradiation part are easily integrated. Is particularly preferable.

(4) In the cell for X-ray analysis, the X-ray irradiation unit may be provided so as to protrude in a direction intersecting with the light receiving surface on a side opposite to the light receiving surface of the infrared heat generating unit. preferable.

  When the X-ray irradiating part is provided so as to protrude in the direction intersecting the light receiving surface on the side opposite to the light receiving surface of the infrared heat generating part, the infrared emitting end of the infrared irradiating device is brought close to the light receiving surface of the infrared heat generating part. Since it becomes possible to irradiate infrared rays, the infrared heating portion can be more efficiently heated, and heat conduction to the X-ray irradiation portion can be more efficiently performed. Further, since the X-ray irradiation direction to the X-ray irradiation unit does not coincide with the infrared irradiation direction, the configuration and arrangement of the apparatus are relatively easy.

(5) An X-ray analysis container according to an aspect of the present invention is an X-ray analysis container including an X-ray analysis cell, a cylindrical body part, and a sealing member,
The X-ray analysis cell includes at least one infrared heat generating unit that generates heat by absorbing infrared rays irradiated from the outside, and an X-ray irradiation unit that holds a sample,
The infrared heat generating portion has a light receiving surface that receives the infrared light,
The X-ray irradiation unit is provided in a part of the infrared heating unit so as to be heated by heat conduction from the infrared heating unit,
The cylindrical body portion houses the X-ray analysis cell therein, and has an infrared window portion through which the infrared rays can pass.
The sealing member is an X-ray analysis container having an X-ray window provided at each end of the cylindrical body.

  In the X-ray analysis container according to this aspect, the X-ray analysis cell is accommodated in the cylindrical body portion, and the X-ray analysis cell can efficiently heat the sample. Further, the sample is not affected by the external environment. For this reason, samples, such as molten salt heated to the temperature of the molten salt bath, can be analyzed with high accuracy.

  And the cylindrical body part in which the cell for X-ray analysis was accommodated has opened both ends, and the opening part is sealed with the sealing member.

  The sealing members at both ends have an X-ray window portion for irradiating the sample held in the X-ray analysis cell, and an X-ray window portion for externally irradiating the X-ray transmitted through the sample. Is provided.

  By storing the X-ray analysis cell in the cylindrical body portion and sealing it in this way, the sample can be irradiated with X-rays while being sealed, and X-rays transmitted through the sample can be emitted.

  When such an X-ray analysis container is used, a sample heated to a high temperature can be analyzed with high accuracy without being affected by the external environment.

(6) In the X-ray analysis container, at least one of the sealing members includes an intake / exhaust port capable of intake or exhaust to the inside, and an electric wiring end capable of electrically connecting the inside and the outside. It is preferable to provide.

  Since the sealing member is provided with an intake / exhaust port capable of intake or exhaust into the container, the inside of the X-ray analysis container can have a desired gas atmosphere. By evacuating while supplying atmospheric gas from the intake / exhaust port in this way, the sample is not sealed in the X-ray analysis container, and even if moisture or gas is generated from the sample during X-ray analysis at high temperatures, Can be removed.

  Further, by providing an electrical wiring end that can electrically connect the inside and outside of the container, for example, a temperature sensor, an electrode for electrochemical operation, and the like can be easily attached. As a result, in-situ measurement along the actual process can be performed more easily. In addition, the electrode for electrochemical operation here refers to various electrodes used for electrochemical operation such as an electrode for electrolytic plating.

(7) In the X-ray analysis container, the cylindrical body is preferably made of quartz glass.

  Quartz glass is excellent in infrared transmittance, so that infrared rays emitted from an infrared irradiation device disposed outside the X-ray analysis container are efficiently transferred to the light-receiving surface of the infrared heating portion of the X-ray analysis cell. It can be irradiated towards. Quartz glass is also excellent in heat resistance.

(8) In the X-ray analysis container, the infrared window portion is preferably a flat window provided on a cylindrical side surface of the cylindrical body portion.

  By providing such a flat window, the infrared emitting end of the infrared irradiation device can be brought close to a predetermined distance to the light receiving surface of the X-ray analysis cell. Such a distance is preferably a distance at which all of the emitted infrared light is irradiated onto the light receiving surface in consideration of the spread of infrared rays from the infrared emission end of the infrared irradiation device. By bringing the infrared ray emitting end closer to such a distance, it is possible to irradiate the infrared ray toward the light receiving surface without waste. Moreover, since it is not necessary to enlarge the infrared heating part, the heat radiation from the infrared heating part is suppressed.

(9) It is preferable that the X-ray analysis container further includes a heat insulating member that covers a cylindrical side surface of the cylindrical body and suppresses heat radiation to the outside.

  By covering the cylindrical side surface of the cylindrical body portion with a heat insulating member, heat radiation from the X-ray analysis cell and the surrounding heating portion to the external space can be suppressed, and more efficient heating can be performed.

(10) Moreover, it is preferable that the said X-ray analysis container is further provided with the reflection member which covers the cylindrical side surface of the said cylindrical trunk | drum, and reflects the infrared rays radiated | emitted outside toward the inside. .

  By covering the cylindrical side surface of the cylindrical body portion with the reflecting member, the infrared rays emitted toward the outside are reflected toward the inside, and the temperature of the X-ray irradiation unit can be further increased.

  Note that it is preferable that the heat insulating member also serves as the reflecting member because the temperature of the X-ray irradiation unit can be further increased. A case in which the reflective member is bonded to the inner peripheral surface of the heat insulating member to integrate them together, or a case where the material itself has both heat insulating performance and reflective performance are conceivable.

(11) The X-ray analysis apparatus according to this aspect is an X-ray analysis apparatus including an X-ray analysis container and an infrared irradiation device,
The X-ray analysis container is an X-ray analysis container comprising an X-ray analysis cell, a cylindrical body part, and a sealing member,
The X-ray analysis cell includes at least one infrared heat generating unit that generates heat by absorbing infrared rays irradiated from the outside, and an X-ray irradiation unit that holds a sample,
The infrared heat generating portion has a light receiving surface that receives the infrared light,
The X-ray irradiation unit is provided in a part of the infrared heating unit so as to be heated by heat conduction from the infrared heating unit,
The cylindrical body portion houses the X-ray analysis cell therein, and has an infrared window portion through which the infrared rays can pass.
The sealing member is provided at both ends of the cylindrical body part, and has an X-ray window part,
The infrared irradiation apparatus is an X-ray analysis apparatus that irradiates infrared rays from the outside of the X-ray analysis container toward a light receiving surface of the infrared heat generating portion of the X-ray analysis cell.

  Since the X-ray analysis apparatus according to this aspect includes an X-ray analysis container in which an X-ray analysis cell is accommodated, the sample can be efficiently heated and when X-rays are observed. In addition, it is not affected by infrared rays. As a result, the molten salt heated to the temperature of the molten salt bath can be subjected to X-ray analysis with high accuracy.

(12) An X-ray analysis method according to an aspect of the present invention is an X-ray analysis method for X-ray analysis of a sample using an X-ray analysis apparatus,
The X-ray analysis apparatus is an X-ray analysis apparatus including an X-ray analysis container and an infrared irradiation device,
The X-ray analysis container is an X-ray analysis container comprising an X-ray analysis cell, a cylindrical body part, and a sealing member,
The X-ray analysis cell includes at least one infrared heat generating unit that generates heat by absorbing infrared rays irradiated from the outside, and an X-ray irradiation unit that holds a sample,
The infrared heat generating portion has a light receiving surface that receives the infrared light,
The X-ray irradiation unit is provided in a part of the infrared heating unit so as to be heated by heat conduction from the infrared heating unit,
The cylindrical body portion houses the X-ray analysis cell therein, and has an infrared window portion through which the infrared rays can pass.
The sealing member is provided at both ends of the cylindrical body part, and has an X-ray window part,
The infrared irradiation device irradiates infrared rays from the outside of the X-ray analysis container toward the light-receiving surface of the infrared heating portion of the X-ray analysis cell;
The X-ray analysis method includes a sample holding step for holding a sample to be analyzed in the X-ray irradiation unit of the X-ray analysis cell;
A sample heating step of heating the sample held by the X-ray irradiation unit by irradiating infrared rays from the infrared irradiation device toward the light receiving surface of the X-ray analysis cell;
An X-ray irradiation step of irradiating X-rays from the outside of one of the X-ray windows toward the heated sample;
An X-ray analysis method comprising: a sample analysis step of analyzing the sample by analyzing the X-ray transmitted through the sample and emitted from the other X-ray window to the outside of the X-ray analysis container is there.

  In the X-ray analysis method according to this aspect, the X-ray analysis is performed using an X-ray analysis apparatus provided with an X-ray analysis cell, whereby the molten salt heated to the temperature of the molten salt bath is analyzed with high accuracy. be able to.

(13) In the X-ray analysis method, a desired gas is supplied into the X-ray analysis container between the sample holding process and the sample heating process, and the gas atmosphere in the X-ray analysis container is changed. It is preferable to provide a gas atmosphere adjusting step for making a desired gas atmosphere.

  By providing such a gas atmosphere adjustment step, high-precision X-ray analysis can be performed by in-situ measurement under the same gas atmosphere as in the actual process. Specific examples of X-ray analysis methods include X-ray analysis by X-ray absorption spectroscopy and X-ray analysis by X-ray diffraction.

[Details of the embodiment of the present invention]
Hereinafter, the present invention will be described based on embodiments with reference to the drawings. In addition, this invention is not limited to these illustrations, is shown by the claim, and intends that all the changes within the meaning and range equivalent to a claim are included.

[1] X-ray analysis cell Configuration of X-ray Analysis Cell The X-ray analysis cell includes an infrared heat generation unit and an X-ray irradiation unit, and is provided so that the X-ray irradiation unit is connected to a part of the infrared heat generation unit. In the following description, an X-ray analysis cell is described by taking an X-ray analysis cell provided as an example to protrude in a direction crossing the light receiving surface on the side opposite to the light receiving surface of the infrared heat generating portion. . Examples of such an X-ray analysis cell include a T-shaped X-ray analysis cell in a plan view shown in FIGS.

  FIG. 1 is a perspective view of an X-ray analysis cell according to the present embodiment, and FIG. 2 is a plan view. As shown in FIGS. 1 and 2, the X-ray analysis cell 1 of this embodiment includes an infrared heating unit 1 a and an X-ray irradiation unit 1 b. The X-ray irradiation unit 1b is provided so as to protrude from the center of the opposite surface of the infrared heating unit 1a so as to be orthogonal to the infrared heating unit 1a, and is formed in a T shape in plan view as a whole. In this example, the X-ray irradiation part 1b and the infrared heat generating part 1a are integrated by being continuously formed of the same material.

  The infrared heat generating portion 1a generates heat by receiving and absorbing infrared light irradiated from the arrow direction on the light receiving surface. And the X-ray irradiation part 1b is provided in connection with the infrared heat generating part 1a. For this reason, heat can be efficiently transmitted from the infrared heating unit 1a to the X-ray irradiation unit 1b, and the X-ray irradiation unit 1b can be heated to an extremely high temperature of 800 ° C. or more in a short time.

  By configuring the X-ray analysis cell 1 as described above, the X-ray irradiation unit 1b can be irradiated with X-rays vertically without being interrupted by the infrared heat generation unit 1a. Further, the X-ray analysis cell 1 having such a shape has a high degree of design freedom and is easy to process.

  As a material of the infrared heating part 1a, a material that has high absorbability of irradiated infrared rays, becomes high temperature in a short time, and has good thermal conductivity is preferable.

  In the present embodiment, since the sample is not directly irradiated with infrared rays, but is generated by the infrared heating unit 1a and the heat is transmitted to the X-ray irradiation unit 1b, the size of the X-ray irradiation unit 1b can be reduced. Therefore, the size of the X-ray analysis cell 1 can be reduced. Specifically, the infrared heat generating part 1a and the X-ray irradiating part 1b can be miniaturized to a rectangular size with a side of about 20 mm. The shape of the infrared heat generating portion 1a is most preferably a shape capable of receiving all of the irradiated infrared rays, and in FIGS. 1 and 2, a rectangular flat plate is used. It may be circular. On the other hand, if the infrared heat generating portion 1a is too wide, the infrared heat generating portion 1a contributes to heat dissipation.

  In the case of this embodiment, a concave groove 1c for holding a sample for analysis is provided in the upper part of the X-ray irradiation part 1b, and the sample filled and held in this concave groove 1c is transferred from the infrared heat generating part 1a. By being heated by the transmitted heat, it is possible to heat to a high temperature of 800 ° C. or higher while having a simple structure, and it is possible to reproduce the state of the molten salt, the molten state of the metal, etc. in the concave groove 1c. it can. Such groove processing is easy and does not cause an increase in cost.

  The holding of the sample is not limited to the provision of the groove 1c in the X-ray irradiation unit 1b described above. The sample is accommodated in a quartz glass or diamond member and placed on the X-ray irradiation unit 1b. It may be placed directly. Even with such a configuration, the sample accommodated in the member can be heated to an extremely high temperature.

  Then, X-ray analysis can be performed with high accuracy by irradiating the sample in which the state such as molten salt is reproduced with X-rays from the thickness direction of the X-ray irradiation unit and analyzing the transmitted X-rays. At this time, if the upper side of the groove 1c or the member in which the sample is accommodated is opened, even if moisture or gas is generated from the sample, these can be excluded from the system, and the periphery of the cell for X-ray analysis Can be filled with the desired atmospheric gas. As a result, the state of the molten salt, the molten state of the metal, etc. can be easily reproduced in the groove 1c or in the member containing the sample, and X-ray analysis is performed while measuring in situ in a gas atmosphere in accordance with the actual process. can do.

  In this embodiment, as shown in FIG. 1 and FIG. 2, the infrared heat generating part 1a and the X-ray irradiating part 1b are arranged in directions orthogonal to each other so that infrared rays and X-rays are irradiated from the respective front surfaces. It has become. However, the X-rays transmitted through the sample can be converted into X-rays even if the infrared heat generating part 1a and the X-ray irradiating part 1b intersect at an angle other than a right angle due to the arrangement position of the infrared ray source, the X-ray source and the X-ray light receiving device. There is no problem as long as the line light receiving device can receive light accurately.

  The size of the groove 1c is based on the optical path length (optical distance of X-rays passing through the analysis sample) l necessary for obtaining sufficient analysis sensitivity, the size of the irradiation area of X-rays, and the like. It is determined appropriately. The thickness t of the X-ray irradiation unit 1b is appropriately determined in consideration of the transmission X-ray detection sensitivity (X-ray attenuation), the permeability and thermal conductivity of the X-ray irradiation unit 1b. For example, when the thickness of the X-ray irradiation unit 1b is reduced, the attenuation of X-rays is suppressed and the detection sensitivity is improved. On the other hand, the amount of heat transferred to the X-ray irradiation unit 1b is reduced due to the lack of thickness. . Moreover, it becomes impossible to secure a sufficient volume of the concave groove 1c for holding the sample.

  As a specific example, when the optical path length l of the X-ray is about 1 mm, the size of the X-ray irradiation surface is generally about 1 mm square, so the size of the groove is slightly larger than this. The thickness of the X-ray irradiator 1b is set to about 2 mm.

2. X-ray analysis cell material As described above, the material of the infrared heat generating portion 1a is preferably a material that has high absorption of irradiated infrared rays and can heat the light-receiving surface to a predetermined temperature in a short time. The material of the irradiation unit 1b is excellent in thermal conductivity from the heated infrared heating unit 1a, can heat the sample to a predetermined temperature in a short time, and is excellent in transmission of irradiated X-rays. Material is preferred.

  The following is known about heating by infrared irradiation. That is, as compared with white ceramics, black ceramics absorb infrared rays well and rise in temperature quickly, and the ultimate temperature is also high. On the other hand, transparent quartz glass has a slow temperature rise and a low reached temperature. In addition, when comparing black ceramics with a material in which transparent quartz glass is placed in front of black ceramics, the material in which transparent quartz glass is placed in front of black ceramics has a slower temperature rise and a lower reaching temperature. The difference is small, when the distance from the emitting end (rod) of the infrared irradiation device is 10 mm or less, even if it is a material in which transparent quartz glass is placed in front of black ceramics, the ultimate temperature exceeds 900 ° C., It has been found that a sufficiently high temperature can be obtained even when irradiated with infrared rays through transparent quartz glass.

  In addition to the black ceramics exhibiting excellent temperature rise as described above, carbon-based inorganic materials also have excellent temperature rise.

  Graphite (C) and silicon carbide (SiC) are preferable as the carbon-based inorganic material, and black diamond is preferable as the black ceramic.

  Among these, graphite (C) and silicon carbide (SiC) are excellent in durability and workability. Therefore, by using these substances in both the infrared heating part 1a and the X-ray irradiation part 1b, infrared heating The cell 1 for X-ray analysis in which the part 1a and the X-ray irradiation part 1b are integrated can be easily manufactured.

  A material in which the surface of diamond is covered with graphite can also be used. Such a material is preferable because it has both elevated temperature and thermal conductivity.

3. In the above, the X-ray analysis cell 1 is formed in a T-shape and only one infrared heating unit 1a is provided, but the infrared heating unit 1a When there is only one, the heat transfer to the X-ray irradiation unit 1b is performed only from the infrared heating unit 1a side, and therefore the temperature tends to decrease as it goes to the tip of the X-ray irradiation unit 1b. There is a possibility that a problem may occur in the thermal uniformity of the entire portion 1b.

  Therefore, how much heat from the infrared heat generating portion 1a is transmitted to the sample filled in the concave groove 1c of the X-ray irradiation portion 1b was measured.

  FIG. 3 shows, as an image, the device configuration (upper stage) and the temperature distribution in the X-ray irradiation part 1b when measuring the temperature drop of the X-ray irradiation part 1b in the T-shaped X-ray analysis cell 1 (lower stage). ).

  In FIG. 3, the control thermocouple 12 is screwed to the X-ray analysis cell 1. For the screw 13, a screw made of the same material as that of the X-ray analysis cell is used in order to prevent occurrence of distortion and cracking due to loosening and tightening due to thermal expansion with the X-ray analysis cell 1.

  As described above, when there is only one infrared heating unit 1a, heat transfer to the X-ray irradiation unit 1b is performed only from the infrared heating unit 1a side. As the distance increases, a temperature gradient is formed that decreases.

  Next, an experiment was conducted to check how much the temperature of the X-ray irradiation unit 1b (specifically, the concave groove 1c) is lowered with respect to the infrared heating unit 1a. Specifically, the control thermocouple 12 is installed on the back surface of the light receiving surface of the infrared heating unit 1a, and the temperature measuring thermocouple is installed at the X-ray irradiation position. While controlling the heat generation of the part 1a, the temperature of the back surface of the infrared heat generating part 1a (control temperature) and the temperature of the X-ray irradiation position were measured and compared.

  The measurement results are shown in FIG. In FIG. 4, the horizontal axis represents the control temperature, and the vertical axis represents the measured X-ray irradiation position temperature. As shown in FIG. 4, the difference between the control temperature and the X-ray irradiation position temperature increases as the temperature increases.

  On the other hand, when a plurality of infrared heating units are provided and each infrared heating unit is irradiated with infrared rays, heating of the X-ray irradiation unit is promoted and soaking is improved. In this case, it is preferable to arrange these infrared heat generating portions on the left and right and top and bottom, for example, with the X-ray irradiation portion interposed therebetween so as not to disturb the X-ray path.

  As an example, there is an H-shaped X-ray analysis cell 1 in which infrared heating portions 1a are provided on both sides of an X-ray irradiation unit 1b shown in FIG. As shown in FIG. 6, the X-ray analysis cell 1 is irradiated with infrared rays on the infrared irradiation units 1 a on both sides, and the X-ray irradiation unit 1 b is heated from both sides. By using such a cell 1 for X-ray analysis, the temperature difference generated between the infrared heat generating portion 1a and the X-ray irradiating portion 1b can be further reduced, and heating can be performed more quickly.

  That is, the temperature gradients from the respective sides indicated by the broken lines in the lower part of FIG. 6 are added to form a temperature gradient with a small temperature drop as indicated by the solid line. As a result, the groove 1c can be heated more uniformly. Moreover, heating is accelerated.

[2] X-ray analysis apparatus X-ray Analysis Container FIG. 7 shows a part of the X-ray analysis container according to this embodiment, specifically, the vicinity of the X-ray analysis cell housed in the cylindrical body of the X-ray analysis container. It is a perspective view. FIG. 8A is a perspective view of a pedestal on which the X-ray analysis cell according to the present embodiment is placed, and FIG. 8B is a perspective view showing a method of placing the X-ray analysis cell on the pedestal. FIG. 9 is a perspective view of the entire X-ray analysis container.

  7 to 9, 1 is an X-ray analysis cell, 15 is an X-ray analysis container, 1a is an infrared heating unit, 1b is an X-ray irradiation unit, 1c is a concave groove, and 2 is an X-ray analysis cell 1. The cylindrical body part 3 of the X-ray analysis container 15 to be stored is a pedestal on which the X-ray analysis cell 1 stored in the cylindrical body part 2 is placed. Reference numeral 2a denotes an infrared window provided on the cylindrical side surface of the cylindrical body 2 so as to face the infrared heating part 1a of the cell 1 for X-ray analysis. 7 and 8 are X-ray window portions, 7 is an entrance window, and 8 is an exit window. Reference numerals 9a and 9b denote lids (flanges) as sealing members for sealing both end portions of the cylindrical body portion 2. 7 to 9, the X-ray analysis cell 1 which is a characteristic part is illustrated in a larger size.

  FIG. 10 is a cross-sectional view schematically showing the configuration of the X-ray analysis apparatus according to this embodiment. Note that, here, the X-ray analysis apparatus is an X-ray analysis apparatus applied to X-ray analysis (XAFS) by X-ray absorption spectroscopy. In FIG. 10, reference numeral 4 denotes a rod (light source) of the infrared irradiation device, and the tip thereof is an infrared ray emitting end for emitting infrared rays. Reference numeral 5 denotes an X-ray emission unit of the X-ray irradiation apparatus, and 6 denotes an X-ray light receiving unit.

  The cylindrical body portion 2 is a cylindrical member made of a material having excellent infrared transmittance such as quartz glass, and a space for accommodating the X-ray analysis cell 1 is provided on the inner side. The sealing members 9a and 9b are made of stainless steel (SUS), and are attached to both ends of the cylindrical body part 2 via O-rings (not shown) to seal the cylindrical body part 2. it can. Since the O-ring is located sufficiently away from the infrared heat generating portion 1a of the X-ray analysis cell 1, there is no possibility of melting or breaking even when the infrared heat generating portion 1a becomes high temperature.

  Then, an X-ray is obtained by fixing a polyimide film, specifically, a Kapton (registered trademark) film manufactured by DuPont using a heat-resistant adhesive, in the opening provided in the central portion of the sealing member 9a. A window (incident window) 7 is provided. Similarly, an X-ray window (outgoing window) 8 is provided in the opening provided in the center of the sealing member 9b. Since the heat-resistant adhesive is located sufficiently away from the infrared heat generating portion 1a of the cell 1 for X-ray analysis, there is no possibility of deterioration or melting even when the infrared heat generating portion 1a becomes high temperature.

  In the present embodiment, the upper sealing member 9a has an air supply port so that gas can be supplied into the X-ray analysis container 15 from the direction of the arrow 10a, while the lower sealing member 9b has Is provided with an exhaust port so that gas can be exhausted from the X-ray analysis container 15 in the direction of the arrow 10b, and an air supply pipe and an exhaust pipe are bonded to each other with a heat-resistant adhesive. Two air supply ports and two air discharge ports may be provided on one of the sealing members 9a and 9b.

  Thus, by providing the air supply port and the exhaust port, and supplying and exhausting the gas into the X-ray analysis container 15 as necessary, the gas atmosphere in accordance with the actual process with the gas flow can be changed to X. Since it can be arbitrarily set in the line analysis container 15, in-situ measurement along an actual process is possible.

  The upper sealing member 9a is provided with an insertion hole through which a temperature sensor such as a thermocouple is inserted in order to control the temperature in the X-ray irradiation unit 1b of the X-ray analysis cell 1 from the direction of the arrow 11. ing. The insertion hole after the temperature sensor is inserted is sealed with a heat resistant adhesive.

  In this way, the temperature in the X-ray irradiation unit 1b of the X-ray analysis cell 1 can be controlled by adjusting the intensity of infrared rays irradiated from the outside based on the temperature measured by the temperature sensor.

  As shown in FIG. 7, the X-ray analysis cell 1 is inserted into the cylindrical body 2 after being set on the pedestal 3. By setting the X-ray analysis cell 1 on the pedestal 3 in this manner, the position of the light receiving surface of the infrared heat generating part 1a in the cylindrical body part 2 is positioned at a position suitable for infrared irradiation and X-ray irradiation. The position of the part 1b is adjusted to the X-ray irradiation position.

  Specifically, as shown in FIG. 8A, a T-shaped recess having the same shape and size as the cross-sectional shape of the T-shaped X-ray analysis cell 1 is provided on the upper surface of the pedestal 3. As shown in FIG. 8B, the lower end portion of the T-shaped X-ray analysis cell 1 is fitted and fixed. The X-ray analysis cell 1 fixed to the pedestal 3 is then placed at a predetermined position by inserting the pedestal 3 into the cylindrical body 2.

  At this time, the light receiving surface of the infrared heat generating portion 1a of the X-ray analysis cell 1 is accommodated so as to face the infrared window portion 2a. The X-ray incident surface and the transmitted X-ray radiation surface of the concave groove 1c are accommodated so as to face the X-ray window portion (incident window) 7 and the X-ray window portion (exit window) 8, respectively. Thereby, infrared rays can be irradiated to the light receiving surface from the front, and X-rays can be reliably irradiated to the sample, and transmitted X-rays can be emitted.

  The infrared window portion 2a is provided on the cylindrical side surface of the cylindrical body portion 2 at a location facing the infrared heating portion 1a of the cell 1 for X-ray analysis. For this reason, the tip of the rod 4 of the infrared irradiation apparatus can be brought close to the infrared heat generating portion 1 a of the X-ray analysis cell 1 accommodated in the cylindrical body portion 2. In addition, since there is no diffusion of infrared rays due to the cylindrical shape of the cylindrical body portion 2, the infrared rays emitted from the rod 4 of the infrared irradiation device are efficiently emitted toward the infrared heating portion 1a of the cell 1 for X-ray analysis without waste. can do.

  As a specific example of the cylindrical body portion 2, a cylinder having an inner diameter of 40 mmφ and a length of 250 mm is used. The infrared heat generating portion 1a and the X-ray irradiating portion 1b are miniaturized to a rectangular size of 20 mm on a side, and the pedestal 3 has a length of 85 mm, a width of 27 mm, and a height of 10 mm.

  Using such an apparatus for X-ray analysis, it was confirmed that the temperature in the vicinity of the groove 1c of the X-ray irradiation part 1b could be raised to 800 ° C. or higher under an argon (Ar) flow.

  In the present embodiment, in order to more efficiently raise the temperature of the X-ray irradiation unit 1b, a heat-resistant cloth 14 containing alumina, silica, or the like is wound around the outside of the cylindrical body part 2 as shown in FIG. It is preferable. In particular, at least the inner surface side is preferably made of a material that easily reflects infrared rays such as white. Such a heat-resistant cloth 14 is a heat insulating member that suppresses heat radiation from the X-ray analysis cell 1 and the surrounding heating portion to the external space, and also reflects the infrared rays reflected from the infrared heat generating portion 1 a in the cylindrical body portion 2. Since it is also a reflecting member that reflects the light, the ultimate temperature in the X-ray irradiation unit 1b can be further increased by 50 to 100 ° C., and the temperature can be increased to 900 ° C. or higher. The heat-resistant cloth may be provided not only on the outer side of the cylindrical body part 2, but also on the inner wall surface of the cylindrical body part 2 excluding the infrared window part 2a, and may be provided on both wall surfaces. Further, a film-like infrared reflecting material or metal foil may be used instead of the heat resistant cloth.

  In this embodiment, in order to reproduce the environment of the molten salt plating in the actual process in the X-ray analysis container 15, not only the gas atmosphere described above but also an electrode for electrochemical operation as necessary. May be attached so that the electrochemical operation can be performed in the X-ray analysis apparatus.

  The electrode for electrochemical operation is attached to the end portion of the electric wiring and is connected to an electrochemical operation device installed outside. As in the case of the temperature sensor, the electrical wiring is attached by providing an insertion hole in the sealing member 9a (see FIG. 10) and fixing it with a heat resistant adhesive. Moreover, you may provide a connector in a sealing member. Thereby, the electrical wiring between the inside and the outside of the X-ray analysis container 15 can be easily performed.

  By reproducing the environment of the molten salt plating in the actual process as described above, in-situ measurement along the actual process becomes possible.

  In the above description, the T-shaped X-ray analysis cell has been described as an example, but the H-shaped X-ray analysis cell shown in FIG. 5 also has a cylindrical shape as shown in FIG. It can be considered in the same manner as in the case of the T-shaped X-ray analysis cell except that infrared window portions 2a are provided on both side surfaces of the body portion 2.

2. X-ray analysis apparatus The X-ray analysis apparatus includes an infrared irradiation apparatus, an X-ray irradiation apparatus, and an X-ray light receiving apparatus in addition to the X-ray analysis container 15 described above. As shown in FIG. 10, after the sample to be analyzed is heated to a sufficiently high temperature by the irradiated infrared rays, X-rays are emitted from the X-ray emission part 5 toward the X-ray window part (incident window) 7. The state of the sample can be analyzed by receiving and analyzing the transmitted X-rays emitted from the X-ray window part (exit window) 8 by the X-ray light receiving part 6 of the light receiving device.

  The infrared irradiation apparatus is equipped with one unit (in the case of a T-shaped X-ray analysis cell) and a plurality of units, for example, two units (in the case of an H-shaped X-ray analysis cell) as necessary. Each of the irradiating rods 4 is disposed so as to be opposed to the light receiving surface of the infrared heat generating portion. As the infrared irradiation device, it is preferable to use an infrared image furnace that raises the temperature of the sample by using light energy by a combination of an infrared lamp and a reflecting surface thereof.

[3] X-ray analysis method X-ray analysis using the apparatus for X-ray analysis of the present embodiment includes a sample holding step for holding a sample to be analyzed in an X-ray irradiation part of an X-ray analysis cell, and an X-ray analysis. A sample heating step of heating the sample held by the X-ray irradiator by irradiating infrared rays with an infrared irradiator toward the light receiving surface of the cell, and from the outside of one X-ray window toward the heated sample Through an X-ray irradiation step of irradiating X-rays and a sample analysis step of analyzing the sample by analyzing the X-rays that have passed through the sample and emitted from the other X-ray window to the outside of the X-ray analysis container Done.

  By using the apparatus for X-ray analysis of this embodiment, the X-ray analysis can be performed at a high temperature of 800 ° C. or higher, which is much higher than the conventional measurement temperature, through the above steps. As a result, in the conventional analyzer, since the ultimate temperature is lower than the melting point of the sample, a high melting point material that could not be analyzed for the molten sample can be melted and analyzed.

  Specific X-ray analysis includes X-ray diffraction (XRD) by X-ray diffraction and X-ray analysis (XAFS) by X-ray absorption spectroscopy.

  Since the X-ray diffraction analysis method by X-ray diffraction is an analysis method that can obtain the crystal structure and amorphous information of the sample, it is possible to obtain information on the electronic state and local structure of the sample.

  As shown in FIG. 13, in the XRD, information on the crystal structure of the sample is obtained by measuring the dependence of the diffraction X-ray angle (diffraction angle 2θ) by fixing the energy of the irradiated X-ray and scanning the detector. As well as being obtained, information on the amorphous can be obtained.

  On the other hand, X-ray analysis by X-ray absorption spectroscopy increases the energy of X-rays while looking at the intensity of X-rays before irradiation of the sample and the intensity of transmitted light of the sample irradiated with X-rays. This is an analysis method for knowing the electronic state and local structure of a sample by measuring a spectrum, and X-ray analysis can be performed while performing in-situ measurement.

14 and 15 are diagrams showing examples of analysis results by XAFS. 14 and 15 use a sample in which Na ₂ WO ₄ and WO ₃ are mixed at a molar ratio of 3: 1, using an infrared heating apparatus GA298 manufactured by Thermo Riko Co., Ltd., which uses an infrared image furnace. 14 is a spectrum obtained when heated to 800 ° C., FIG. 14 is a XANES (X-ray Absorption Near Edge Structure) spectrum, and FIG. 15 is an EXAFS (Extended X-ray Absorption). Fine Structure (broad spectrum X-ray absorption fine structure) spectrum.

In FIG. 14, the horizontal axis represents X-ray energy (eV), and the vertical axis represents normalized absorption rate (au). In FIG. 15, the horizontal axis represents the wave number (Å ⁻¹ ), and the vertical axis represents the EXAFS vibration (au) weighted by the square of the wave number.

  As shown in FIGS. 14 and 15, according to the present embodiment, the electronic state of the sample can be captured from the XANES spectrum obtained from the XAFS measurement, and the local structure of the sample can be captured from the EXAFS spectrum with sufficient statistical accuracy. I understand that

  As described above, according to the present embodiment, an X-ray analysis technique that can be practically used with a simpler method, such as being able to measure and analyze in situ while heating a sample at a high temperature of 800 to 900 ° C. Can be provided.

(Appendix)
The present invention includes the following embodiments.

(Appendix 1)
Comprising at least one infrared heat generating part that absorbs infrared rays irradiated from the outside and generates heat; and an X-ray irradiation part that holds a sample;
The infrared heat generating portion has a light receiving surface that receives the infrared light,
The X-ray irradiation unit is an X-ray analysis cell provided in a part of the infrared heating unit so as to be heated by heat conduction from the infrared heating unit.

(Appendix 2)
The cell for X-ray analysis according to appendix 1, further comprising a groove for holding a sample to be analyzed in an upper part of the X-ray irradiation unit.

(Appendix 3)
The cell for X-ray analysis according to Supplementary Note 1 or Supplementary Note 2, which is formed in a T shape in plan view.

(Appendix 4)
The cell for X-ray analysis according to Supplementary Note 1 or Supplementary Note 2, wherein infrared light receiving parts are provided on both side surfaces of the X-ray irradiation part and formed in an H shape in a plan view.

(Appendix 5)
An X-ray analysis apparatus comprising an X-ray analysis container and an infrared irradiation device,
The X-ray analysis container is an X-ray analysis container comprising an X-ray analysis cell, a cylindrical body part, and a sealing member,
The X-ray analysis cell includes at least one infrared heat generating unit that generates heat by absorbing infrared rays irradiated from the outside, and an X-ray irradiation unit that holds a sample,
The infrared heat generating portion has a light receiving surface that receives the infrared light,
The X-ray irradiation unit is provided in a part of the infrared heating unit so as to be heated by heat conduction from the infrared heating unit,
The cylindrical body portion houses the X-ray analysis cell therein, and has an infrared window portion through which the infrared rays can pass.
The sealing member is provided at both ends of the cylindrical body part, and has an X-ray window part,
The infrared irradiation apparatus is an apparatus for X-ray analysis that irradiates infrared rays from the outside of the X-ray analysis container toward a light receiving surface of the infrared heat generating portion of the X-ray analysis cell.

(Appendix 6)
The apparatus for X-ray analysis according to appendix 5, wherein the infrared irradiation apparatus is an infrared image furnace.

  The present invention provides a molten sample analysis technique capable of performing X-ray analysis while performing in-situ measurement under a predetermined atmosphere in accordance with an actual process for a sample that has not been realized due to a high melting point. It can greatly contribute to the improvement and development of technology in the industrial field that handles molten materials such as molten metals and molten salts.

DESCRIPTION OF SYMBOLS 1 X-ray analysis cell 1a Infrared heat generating part 1b X-ray irradiation part 1c Concave groove 2 Cylindrical body part 2a Infrared window part 3 Base 4 Rod 5 X-ray emission part 6 X-ray light-receiving part 7 X-ray window part (incident window)
8 X-ray window (outgoing window)
9a, 9b Sealing member (lid)
DESCRIPTION OF SYMBOLS 10a Arrow which shows the position of an air inlet 10b Arrow which shows the position of an exhaust port 11 Arrow which shows the insertion position of a temperature sensor 12 Thermocouple for control 13 Screw 14 Heat-resistant cloth 15 X-ray analysis container l Optical path length t X-ray irradiation part Thickness

Claims (13)

Comprising at least one infrared heat generating part that absorbs infrared rays irradiated from the outside and generates heat; and an X-ray irradiation part that holds a sample;
The infrared heat generating portion has a light receiving surface that receives the infrared light,
The X-ray irradiation unit is an X-ray analysis cell provided in a part of the infrared heating unit so as to be heated by heat conduction from the infrared heating unit.   The cell for X-ray analysis according to claim 1, wherein the infrared heating unit and the X-ray irradiation unit are integrated with the same material.   The cell for X-ray analysis according to claim 1 or 2, wherein the infrared heat generating part and the X-ray irradiation part are made of a carbon-based inorganic material or black ceramics.   The X-ray irradiating unit is provided on the side of the infrared heat generating unit that is opposite to the light receiving surface and protrudes in a direction intersecting with the light receiving surface. The cell for X-ray analysis as described. An X-ray analysis container comprising an X-ray analysis cell, a cylindrical body part, and a sealing member,
The X-ray analysis cell includes at least one infrared heat generating unit that generates heat by absorbing infrared rays irradiated from the outside, and an X-ray irradiation unit that holds a sample,
The infrared heat generating portion has a light receiving surface that receives the infrared light,
The X-ray irradiation unit is provided in a part of the infrared heating unit so as to be heated by heat conduction from the infrared heating unit,
The cylindrical body portion houses the X-ray analysis cell therein, and has an infrared window portion through which the infrared rays can pass.
The said sealing member is an X-ray analysis container which is provided in the both ends of the said cylindrical trunk | drum, respectively, and has an X-ray window part.   6. The X according to claim 5, wherein at least one of the sealing members includes an intake / exhaust port capable of intake or exhaust to the inside, and an electric wiring end capable of electrically connecting the inside and the outside. Container for line analysis.   The container for X-ray analysis according to claim 5 or 6, wherein the cylindrical body portion is made of quartz glass.   The X-ray analysis container according to any one of claims 5 to 7, wherein the infrared window portion is a flat window provided on a cylindrical side surface of the cylindrical body portion.   Furthermore, the container for X-ray analysis of any one of Claims 5-8 provided with the heat insulation member which covers the cylindrical side surface of the said cylindrical trunk | drum, and suppresses the thermal radiation to the exterior.   Furthermore, the reflective body which covers the cylindrical side surface of the said cylindrical trunk | drum, and reflects the infrared rays radiated | emitted toward the exterior toward an inside is provided. X-ray analysis container. An X-ray analysis apparatus comprising an X-ray analysis container and an infrared irradiation device,
The X-ray analysis container is an X-ray analysis container comprising an X-ray analysis cell, a cylindrical body part, and a sealing member,
The X-ray analysis cell includes at least one infrared heat generating unit that generates heat by absorbing infrared rays irradiated from the outside, and an X-ray irradiation unit that holds a sample,
The infrared heat generating portion has a light receiving surface that receives the infrared light,
The X-ray irradiation unit is provided in a part of the infrared heating unit so as to be heated by heat conduction from the infrared heating unit,
The cylindrical body portion houses the X-ray analysis cell therein, and has an infrared window portion through which the infrared rays can pass.
The sealing member is provided at both ends of the cylindrical body part, and has an X-ray window part,
The infrared irradiation apparatus is an apparatus for X-ray analysis that irradiates infrared rays from the outside of the X-ray analysis container toward a light receiving surface of the infrared heat generating portion of the X-ray analysis cell. An X-ray analysis method for X-ray analysis of a sample using an X-ray analysis apparatus,
The X-ray analysis apparatus is an X-ray analysis apparatus including an X-ray analysis container and an infrared irradiation device,
The X-ray analysis container is an X-ray analysis container comprising an X-ray analysis cell, a cylindrical body part, and a sealing member,
The X-ray analysis cell includes at least one infrared heat generating unit that generates heat by absorbing infrared rays irradiated from the outside, and an X-ray irradiation unit that holds a sample,
The infrared heat generating portion has a light receiving surface that receives the infrared light,
The X-ray irradiation unit is provided in a part of the infrared heating unit so as to be heated by heat conduction from the infrared heating unit,
The cylindrical body portion houses the X-ray analysis cell therein, and has an infrared window portion through which the infrared rays can pass.
The sealing member is provided at both ends of the cylindrical body part, and has an X-ray window part,
The infrared irradiation device irradiates infrared rays from the outside of the X-ray analysis container toward the light-receiving surface of the infrared heating portion of the X-ray analysis cell;
The X-ray analysis method includes a sample holding step for holding a sample to be analyzed in the X-ray irradiation unit of the X-ray analysis cell;
A sample heating step of heating the sample held by the X-ray irradiation unit by irradiating infrared rays from the infrared irradiation device toward the light receiving surface of the X-ray analysis cell;
An X-ray irradiation step of irradiating X-rays from the outside of one of the X-ray windows toward the heated sample;
A sample analysis step of analyzing the sample by analyzing the X-ray transmitted through the sample and emitted from the other X-ray window to the outside of the X-ray analysis container.   A gas atmosphere adjustment step of supplying a desired gas into the X-ray analysis container between the sample holding step and the sample heating step so that the gas atmosphere in the X-ray analysis container is changed to a desired gas atmosphere. The X-ray analysis method according to claim 12, comprising:

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