Fluorescence X-ray analysis device
By using a transparent window frame retainer and a thin film support in the fluorescence X-ray analysis device to support the septum membrane, and by using a gas flow path system to stabilize the septum membrane, the problems of measurement difficulties caused by pressure difference and septum membrane replacement difficulties are solved, and a stable and convenient measurement process is achieved.
Patent Information
- Application Number
- CN202480010379.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Priority Date
- 2023-09-01
- Filing Date
- 2024-08-30
- Publication Date
- 2026-01-30
- Estimated Expiration
- 2044-08-30
AI Technical Summary
Existing fluorescence X-ray analysis devices cannot perform measurements when there is a pressure difference in the space separated by the septum membrane, and the septum membrane is difficult to replace and is prone to bending or wrinkling.
A fluorescence X-ray analysis device was designed, wherein the window frame holding component and the thin film support component are formed of transparent material, the septum membrane is supported by multiple through holes, and the X-ray source is configured in a vacuum environment. The septum membrane is stabilized by a gas flow path system to prevent deflection and wrinkling, and the sample chamber is configured in an atmospheric pressure environment.
It enables measurements to be taken even when there is a pressure difference in the space separated by the diaphragm membrane, and the diaphragm membrane can be easily replaced without bending or wrinkling, thus improving the stability and ease of maintenance of the device.
Smart Images

Figure CN120641743B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to a fluorescence X-ray analysis device. Background Technology
[0002] As an apparatus for analyzing the elements contained in a sample, a fluorescence X-ray analysis apparatus is known (see Patent Document 1). The fluorescence X-ray analysis apparatus irradiates the sample with X-rays once and analyzes it based on the intensity and energy of the fluorescence X-rays emitted from the sample. To facilitate easy sample replacement, a simplified fluorescence X-ray analysis apparatus with a structure that separates the sample chamber from the irradiation chamber using a septum membrane is also known (see Patent Document 2). Furthermore, a fluorescence X-ray analysis apparatus with a sample cell stage comprising an X-ray transmission plate sandwiched between an outer stage frame and an inner stage frame, sealing one end of the inner stage frame (see Patent Document 3).
[0003] Existing technical documents
[0004] Patent documents
[0005] Patent Document 1: International Publication No. 2005-024407
[0006] Patent Document 2: International Publication No. 2004-088296
[0007] Patent Document 3: Japanese Patent Application Publication No. 9-127028 Summary of the Invention
[0008] The problem that the invention aims to solve
[0009] In the fluorescence X-ray analysis apparatus of Patent Document 1, there are a sample chamber for storing the sample, an irradiation chamber for storing an X-ray source that irradiates the sample with primary X-rays and is connected to the sample chamber, an irradiation chamber for storing a detection mechanism that disperses and detects secondary X-rays generated from the sample, and a partition configured to separate the irradiation chambers and allow X-rays to pass through. The partition membrane is made of polyimide or the like and deteriorates due to X-ray irradiation. Therefore, the partition membrane needs to be replaced at regular intervals. However, in the fluorescence X-ray analysis apparatus of Patent Document 1, the partition membrane cannot be easily replaced due to the structure of the apparatus.
[0010] In the fluorescence X-ray analysis apparatus of Patent Document 2, the sample chamber and the irradiation chamber are separated by a first frame and a second frame that hold the septum membrane between them. The septum membrane can be easily replaced by forming the first frame with a permanent magnet and the second frame with a material attracted by the permanent magnet. However, the septum membrane is only clamped by the magnet and is not fixed in place. Therefore, measurements cannot be performed in an environment with a pressure difference between the sample chamber and the irradiation chamber. Furthermore, when the septum membrane is clamped by the first frame and the second frame, deflection or wrinkles may occur on the septum membrane.
[0011] In the fluorescence X-ray analysis apparatus of Patent Document 3, it is not envisioned that the X-ray tube be placed in a vacuum environment and the sample be placed in an atmospheric pressure environment. Therefore, it is impossible to perform measurements in an environment where there is a pressure difference between the area where the sample is placed and the area where the X-ray tube is placed.
[0012] This disclosure is made in view of the above-mentioned problems, and its object is to provide a fluorescence X-ray analysis device that can perform measurements even when there is a pressure difference in the space separated by the septum membrane, and that the septum membrane can be easily installed without bending or wrinkling.
[0013] Technical solutions for solving the problem
[0014] (1) A fluorescence X-ray analysis apparatus according to one aspect of the present disclosure comprises: an irradiation chamber, which is in a vacuum environment and is provided with an X-ray source emitting X-rays; and a sample chamber, which is in an atmospheric pressure environment and is provided with a sample cell, characterized in that it comprises: a window frame retaining member, which forms part of a partition between the irradiation chamber and the sample chamber, and has an opening for the X-rays to pass from the irradiation chamber to the sample chamber; and a window frame member, which is formed of a material that allows the X-rays to pass through, retains a partition membrane forming another part of the partition, and is disposed within the opening of the window frame retaining member, the window frame retaining member having a plurality of... The window frame component has a through-hole through which X-rays pass and a thin film support member disposed adjacent to and supporting the septum membrane on the irradiation chamber side. The window frame component has: an annular inner thin film holding member having a peripheral wall extending from a base end disposed on the sample chamber side toward a front end disposed on the irradiation chamber side, the front end forming an opening closed by a portion of the septum membrane; and an annular outer thin film holding member that fixes the periphery of the portion of the septum membrane to the inner thin film holding member by being inserted from the front end of the inner thin film holding member and mounted on the base end of the inner thin film holding member.
[0015] (2) The inner film retaining member has a flange on the base end that fixes the positional relationship between the inner film retaining member and the window frame retaining member.
[0016] (3) Another aspect of the fluorescence X-ray analysis apparatus of the present disclosure is characterized in that the flange portion has: a first flange portion disposed on the front end side, which clamps the septum membrane together with the outer film holding member; and a second flange portion disposed on the base end side, having an outer diameter greater than the first flange portion, and fixed to the window frame holding member.
[0017] (4) Another aspect of the fluorescence X-ray analysis apparatus of this disclosure is characterized in that the first flange portion and the second flange portion are integrally formed.
[0018] (5) Another aspect of the fluorescence X-ray analysis apparatus of the present disclosure is characterized in that the peripheral wall has a vertical portion extending vertically from the flange toward the front end and a curved portion bending from the vertical portion toward the front end.
[0019] (6) Another aspect of the fluorescence X-ray analysis apparatus of this disclosure is characterized in that the peripheral wall has a vertical portion extending vertically from the flange toward the front end and an inclined portion extending from the vertical portion toward the front end.
[0020] (7) Another aspect of the fluorescence X-ray analysis apparatus of this disclosure is characterized in that the peripheral wall has a flat portion at the front end, the flat portion being parallel to the plane formed by the opening closed by a portion of the septum membrane.
[0021] (8) Another aspect of the fluorescence X-ray analysis apparatus of this disclosure is characterized in that the outer film holding member and / or the film support member are formed of resin.
[0022] (9) Another aspect of the fluorescence X-ray analysis apparatus of this disclosure is characterized in that the inner film holding member and / or the window frame holding member are formed of metal.
[0023] (10) Another aspect of the fluorescence X-ray analysis apparatus of the present disclosure is characterized in that the window frame retaining member has a first gas inflow hole extending from the outer side to the inner side opposite to the window frame member, and the flange has a second gas inflow hole extending through the upper surface and the lower surface.
[0024] (11) Another aspect of the fluorescence X-ray analysis apparatus of this disclosure is characterized in that the window frame retaining member has a gas supply port outside the first gas inlet hole, which supplies flowing gas between the sample cell and the diaphragm membrane via the first gas inlet hole and the second gas inlet hole.
[0025] The effects of the invention
[0026] According to this disclosure, pressure differences can be measured even in spaces separated by diaphragm membranes, and the diaphragm membranes can be easily stretched without bending or wrinkling. Attached Figure Description
[0027] Figure 1 This is a schematic diagram showing a fluorescence X-ray analysis apparatus.
[0028] Figure 2 This is a top-down view of the sample stage.
[0029] Figure 3 This is a top-down view of the sample stage.
[0030] Figure 4 These are the top, side, and bottom views of the window frame retaining components.
[0031] Figure 5 These are the top, side, and bottom views of the membrane support component.
[0032] Figure 6 These are top, side, and bottom views of the inner film retaining component.
[0033] Figure 7 These are top, side, and bottom views of the outer film retaining component.
[0034] Figure 8 This is a diagram showing the cross-section of the sample stage.
[0035] Figure 9 This diagram shows the state of a partition film installed on a window frame component.
[0036] Figure 10 This is a diagram showing the cross-section of a modified window frame component. Detailed Implementation
[0037] Hereinafter, preferred embodiments (hereinafter referred to as embodiments) for carrying out the present invention will be described with reference to the accompanying drawings. Figure 1 This is a schematic diagram showing the fluorescence X-ray analysis apparatus 100. (See diagram below.) Figure 1 As shown, the fluorescence X-ray analysis apparatus 100 has a sample chamber 102 under atmospheric pressure and an irradiation chamber 106 under vacuum. The sample chamber 102 and the irradiation chamber 106 are separated by a partition including a partition wall 108, which prevents the gases from moving relative to each other. An opening is provided in the partition wall 108 to allow X-rays to pass from the irradiation chamber 106 to the sample chamber 102.
[0038] The irradiation chamber 106 is equipped with an X-ray source 110 that emits X-rays, a spectrometer 111 that disperses fluorescent X-rays, and a detector 112 that detects fluorescent X-rays. The X-ray source 110 irradiates the sample cell 116 with X-rays through the aforementioned opening. Fluorescent X-rays are emitted from the X-ray-irradiated sample. The spectrometer 111 disperses the fluorescent X-rays of a predetermined wavelength emitted from the sample. The detector 112 is positioned at the point of incidence of the fluorescent X-rays dispersed by the spectrometer 111. The detector 112 is, for example, a proportional counter tube. The detector 112 measures the fluorescent X-rays and outputs a pulse signal. A counter (not shown) obtains the intensity of the fluorescent X-rays by counting the pulse signals output from the detector 112. The sample is analyzed based on the intensity of the fluorescent X-rays.
[0039] Furthermore, the spectroscopic element 111 and detector 112 can be arranged for each element being analyzed, or they can be a single set of spectroscopic elements 111 and detector 112 that rotates and moves. In the case where the single set of spectroscopic elements 111 and detector 112 rotates and moves, a mechanism (goniometer) for rotating and moving the spectroscopic elements 111 and detector 112 is arranged in the illumination chamber 106. For example... Figure 1 As shown, this disclosure is particularly effective for analyzing light elements in a wavelength dispersive fluorescence X-ray analysis apparatus 100 where the distance from the sample to the detector 112 is relatively long. However, the fluorescence X-ray analysis apparatus 100 can also be an energy dispersive apparatus without the spectroscopic element 111.
[0040] A sample stage 104 is provided in the sample chamber 102, and a sample cell 116 is disposed on the sample stage 104. The interior of the sample chamber 102 can be filled with helium or filled with atmosphere. According to this disclosure, the sample can be measured regardless of whether it is in a helium environment or an atmospheric environment. Hereinafter, the case where the measurement can be performed at low cost without the need for helium supply, i.e., when the sample is placed in an atmospheric environment, will be described. Furthermore, the sample can be liquid or solid (including powder), and the case where the sample is liquid will be described below. The liquid sample is disposed in the sample cell 116. The sample cell 116 is cylindrical in shape, and the bottom surface is covered with a sample holding film. The liquid sample is disposed on the sample holding film. In addition, the upper surface of the sample cell 116 is sealed with another film to prevent the sample from overflowing. The sample stage 104 includes a window frame component 300, a window frame holding component 400, and a cover component 118. (Refer to...) Figures 2 to 8 The specific structure of the sample stage 104 is described.
[0041] Figure 2 and Figure 3 This is a top view of the sample stage 104 (excluding the cover component 118) and the partition wall 108 between the sample chamber 102 and the irradiation chamber 106. Figure 2This indicates that the window frame retaining component 400 and window frame component 300 are installed on the adjacent 108. Figure 3 This indicates that the window frame component 300 and the membrane support component 500 have been removed. Figures 4 to 7 This shows the top view (top), side view (center), and bottom view (bottom) of each component. Figure 8 This is a cross-sectional view showing the sample stage 104 and partition wall 108 with the sample cell 116 configured.
[0042] The window frame retaining member 400 forms part of the partition between the irradiation chamber 106 and the sample chamber 102, and has an opening allowing X-rays to pass from the irradiation chamber 106 to the sample chamber 102. Specifically, the window frame retaining member 400, together with the partition wall 108, forms part of the partition separating the sample chamber 102 and the irradiation chamber 106. The window frame retaining member 400 has... Figure 4 The upper retaining member 402, the lower retaining member 404 and shown are shown. Figure 5 The thin film support member 500 is shown. The upper retaining member 402 and the lower retaining member 404 have openings that allow X-rays to pass from the irradiation chamber 106 to the sample chamber 102. Furthermore, if the opening of the partition wall 108 is closed only by the thin film support member 500 and the partition film 800, the window frame retaining member 400 may not be part of the partition.
[0043] The lower retaining member 404 is a component configured to contact the upper side of the partition wall 108. Viewed from the top and bottom surfaces, the lower retaining member 404 has a generally circular outer edge and a circular opening at a position corresponding to the opening provided on the partition wall 108. In cross-sectional view, the lower retaining member 404 is thickest at the outer periphery and thinner at the inner side. For example, when the window frame member 300 is disposed, the lower retaining member 404 has a step (first step) at the outer edge of the window frame member 300 (corresponding to the peripheral wall 606 of the inner film retaining member 600 described later). The lower retaining member 404 has an O-ring at the location where this step is provided, which contacts the curved portion 610 of the inner film retaining member 600. Thus, the irradiation chamber 106 can be maintained as a vacuum even when the sample chamber 102 is replaced with atmosphere or a gas (e.g., filled with helium). Furthermore, the lower retaining member 404 has a step (second step) inside this step (first step). With the membrane support member 500 in place, the outer edge of the membrane support member 500 is located at the step (second step).
[0044] The upper retaining member 402 is configured to contact the lower retaining member 404 from above. Viewed from its upper and lower surfaces, the upper retaining member 402 has a generally circular outer edge and a circular opening with the same central location as the opening on the lower retaining member 404 but with a larger diameter. The upper retaining member 402 has an O-ring at the point of contact with the lower retaining member 404.
[0045] Furthermore, the upper retaining member 402 has a first gas inlet hole 408 extending from the outer side to the inner side opposite to the window frame member 300. The upper retaining member 402 has a gas supply port 406, which supplies flowing gas between the sample cell 116 and the diaphragm membrane 800 via the first gas inlet hole 408 and the second gas inlet hole 614 (described later). A flexible hose or the like serving as a gas flow path is installed on the gas supply port 406, and the gas supplied from the external gas supply device flows from the outer side to the inner side.
[0046] The upper retaining member 402 and the lower retaining member 404 are preferably made of metal. Compared with resin materials, metal materials are less prone to degradation by X-rays and can therefore be reused. Furthermore, the upper retaining member 402 and the lower retaining member 404 can also be integrally formed.
[0047] The thin film support member 500 has a plurality of through holes 502 for X-rays to pass through, is disposed adjacent to the diaphragm membrane 800 on the irradiation chamber 106 side, and supports the diaphragm membrane 800 from the irradiation chamber 106 side. Specifically, as Figure 5 As shown, viewed from the top and bottom surfaces, the outer edge of the film support member 500 is approximately circular. The film support member 500 is formed to be thin near the outer periphery and thicker on the inner side than near the outer periphery. The thicker portion of the film support member 500 has a shape corresponding to the opening shape of the lower retaining member 404. The film support member 500 is disposed above the lower retaining member 404 such that the thicker portion is located at the opening of the lower retaining member 404. At this time, the outer edge of the film support member 500 is located at the position of a step (second step) provided on the lower retaining member 404. A plurality of through holes 502 for X-rays to pass through are provided in the thicker portion of the film support member 500.
[0048] In this embodiment, the thin film support member 500 has five through holes 502. Each through hole 502 is elongated in shape. Each through hole 502 is formed to have the same diameter but becomes longer closer to the center. However, the shape of the through holes 502 is not limited to... Figure 5The shape shown is as described. For example, the plurality of through holes 502 can also be hexagonal and arranged in a honeycomb structure. Furthermore, the film support member 500 is preferably formed of a thermoplastic resin such as polyetheretherketone (PEEK), which is less susceptible to deterioration caused by X-rays. According to this disclosure, the septum membrane 800 is partially supported by the space between adjacent through holes 502. This prevents the septum membrane 800 from rupturing due to the pressure difference between the sample chamber 102 and the irradiation chamber 106.
[0049] The window frame component 300 is formed of a material that allows X-rays to pass through, retains the partition membrane 800, which constitutes another part of the partition, and is disposed within the opening of the window frame retaining component 400. Specifically, the window frame component 300 has Figure 6 The inner film holding member 600 shown and Figure 7 The outer film retaining member 700 is shown. The window frame member 300 is disposed within the opening of the window frame retaining member 400, with the partition film 800 sandwiched between the inner film retaining member 600 and the outer film retaining member 700. The partition film 800 located in this opening forms part of the partition.
[0050] The inner film holding member 600 has an annular shape and has a flange portion and a peripheral wall 606 extending from the base end toward the front end disposed on the sample chamber 102 side. Specifically, the flange portion is provided on the base end, with a circular outer edge and a circular opening on the inner side. The flange portion has a first flange portion 602 on the front end side and a second flange portion 604 on the base end side. The peripheral wall 606 extends from the first flange portion 602 toward the front end, and the first flange portion 602 and the peripheral wall 606 together with the outer film holding member 700 clamp the septum film 800.
[0051] The outer diameter of the second flange portion 604 is larger than that of the first flange portion 602, and it is fixed to the window frame retaining member 400. The second flange portion 604 is provided with a threaded hole 616, and is fixed to the upper retaining member 402 by a screw 200 inserted into the threaded hole 616. The window frame member 300 is disposed in the window frame retaining member 400 such that the outer edge of the peripheral wall 606 is located on the step (first step) of the lower retaining member 404. In this embodiment, the first flange portion 602 and the second flange portion 604 are formed as one piece, but the first flange portion 602 and the second flange portion 604 may also be formed to be separable. In addition, the flange portion has a second gas inflow hole 614 that penetrates the upper surface of the base end side and the lower surface of the front end side.
[0052] The peripheral wall 606 extends from the first flange 602 toward the front end, where an opening is formed by a portion of the diaphragm membrane 800. Specifically, the peripheral wall 606 has a vertical portion 608 extending perpendicularly from the flange toward the front end, a curved portion 610 curving inward from the vertical portion 608 toward the front end, and a flat portion 612 parallel to the plane formed at the front end and the opening. The peripheral wall 606 and the first flange 602 are integrally formed of metal. Alternatively, the peripheral wall 606 may be configured to have the vertical portion 608 and the curved portion 610, but not the flat portion 612.
[0053] The outer film retaining member 700 is an annular component that, together with the inner film retaining member 600, retains the septum membrane 800. Specifically, the outer film retaining member 700 is an annular component inserted from the front end of the inner film retaining member 600. The inner diameter of the outer film retaining member 700 corresponds to the outer diameter of the peripheral wall 606. By mounting the outer film retaining member 700 onto the base end of the inner film retaining member 600, a portion of the septum membrane 800 (the portion closing the opening of the peripheral wall 606) is secured to the periphery of the inner film retaining member 600. Figure 7 and Figure 8 In this design, the outer diameter of the base end of the outer film retaining member 700 is larger than the outer diameter of the front end, but the outer film retaining member 700 only needs to be able to maintain the shape of the septum film 800 together with the inner film retaining member 600. In addition, the outer film retaining member 700 is preferably formed of a thermoplastic resin such as polyetheretherketone, which is less susceptible to deterioration caused by X-rays, so as to facilitate installation on the peripheral wall 606.
[0054] The cover component 118 encloses the space where the sample cell 116 is located. Specifically, as follows: Figure 8 As shown, the cover member 118 has a shape that covers the space where the sample pool 116 is disposed, and is disposed in contact with the upper retaining member 402 of the window frame retaining member 400. The cover member 118 has an O-ring at the position where it contacts the upper retaining member 402, which divides the space between the inner and outer sides of the cover member 118, except for the paths of the first gas inlet hole 408 and the second gas inlet hole 614, so that the gas does not move.
[0055] According to this disclosure, the partition membrane 800, which needs to be replaced periodically, can be easily installed on the window frame component 300 without causing flexing or wrinkling. Figure 9 This diagram shows the state in which the partition film 800 is installed on the window frame component 300. First, the inner film retaining component 600 is placed on a flat surface with its base end facing down (front end facing up). The partition film 800, whose size is much larger than the opening, is then placed over the front opening. In this state, the outer film retaining component 700 is fitted from the front end of the peripheral wall 606 toward its base end. At this time, the... Figure 9The stretching force in the direction of the arrow acts on the diaphragm membrane 800. Therefore, the diaphragm membrane 800 can be easily stretched without bending or wrinkling. Furthermore, since the peripheral wall 606 has a curved portion 610 and a flat portion 612, the force applied to the diaphragm membrane 800 in the stretched state can be distributed. Therefore, since the force is not applied to any one point of the diaphragm membrane 800, the possibility of breakage when the diaphragm membrane 800 is clamped can be reduced.
[0056] Furthermore, according to this disclosure, sample replacement or gas replacement of the sample chamber 102 can be performed while the irradiation chamber 106 is maintained as a vacuum. Specifically, the lower holding member 404 has an O-ring at a position where a step (first step) is provided. When the window frame member 300 is disposed on the lower holding member 404, the O-ring contacts both the curved portion 610 of the inner film holding member 600 and the lower holding member 404. Thus, an airtight seal can be achieved between the window frame member 300 and the window frame holding member 400. In addition, the opening of the window frame holding member 400 is closed by the partition film 800 held by the window frame member 300. Therefore, even when the sample cell 116 is removed (see reference...), the sample chamber 102 can be replaced or the sample chamber 102 can be purged. Figure 2 The sample chamber 102 and the irradiation chamber 106 are also isolated. Therefore, sample replacement or gas replacement of the sample chamber 102 can be performed while maintaining the irradiation chamber 106 under vacuum. Furthermore, the sample can be easily replaced without the use of tools simply by opening the cover part 118 and replacing the sample cell 116.
[0057] Furthermore, the film support member 500 is made of a material less susceptible to X-ray degradation, but it is preferable to replace it at regular intervals. According to this disclosure, the film support member 500 is disposed on the window frame retaining member 400 and is not fixed by screws or the like. Therefore, as described above, the film support member 500 can be easily replaced simply by disposing the window frame member 300, on which the partition film 800 is mounted, within the opening of the window frame retaining member 400. Furthermore, according to this disclosure, a threaded hole 616 is provided on the second flange portion 604, and the window frame member 300 is fixed to the upper retaining member 402 by inserting a screw 200 into the threaded hole 616. Since this screw fixing operation can be performed from the easily accessible upper side, the user can easily fix the window frame member 300 to the upper retaining member 402.
[0058] Furthermore, according to this disclosure, it is possible to prevent degradation of the diaphragm membrane 800 caused by ozone generated during measurement. Specifically, as... Figure 1 and Figure 8 As shown, there is a gap between the sample holding membrane and the septum membrane 800, which are positioned close together and block the bottom surface of the sample cell 116. Therefore, even when the sample chamber 102 is atmospheric, there is still atmospheric pressure between the sample holding membrane and the septum membrane 800. Furthermore, as... Figure 1As shown, X-rays irradiate the septum membrane 800 during the measurement. Since the atmosphere contains oxygen, when this oxygen is exposed to X-rays, ozone is produced, which promotes the degradation of the septum membrane 800. In this disclosure, gas is supplied from an external gas supply device to the gas supply port 406. Nitrogen is preferably supplied, but atmospheric gas may also be used. Figure 8 The dashed arrow indicates the path of the supplied gas flow. Gas supplied from gas supply port 406 passes through the first gas inlet hole 408 to reach the space between window frame component 300 and window frame retaining component 400. Figure 8 The space near the outer film holding member 700. This space exists in a ring shape along the outer film holding member 700. Furthermore, since this space is connected to the second gas inlet 614, the supplied gas reaches the space between the sample cell 116 and the cover member 118 through the second gas inlet 614. In addition, a portion of the supplied gas reaches the gap between the sample holding film and the septum film 800 through the space between the sample cell 116 and the inner film holding member 600. Furthermore, the spaces between the sample cell 116 and the inner film holding member 600, and between the sample holding film and the septum film 800, are actually very small, but for ease of understanding, Figure 8 The description is exaggerated. When ozone is generated between the sample holding membrane and the septum membrane 800, the ozone is discharged along with the supplied gas into the space between the sample cell 116 and the cover member 118. Then, the ozone is discharged from the gas supply port 406, which is opposite to the gas supply port 406 supplied by the gas supply device. As described above, by supplying gas from the gas supply port 406, ozone does not remain between the sample holding membrane and the septum membrane 800, thus preventing the septum membrane 800 from deteriorating due to ozone generated during measurement.
[0059] This invention is not limited to the above embodiments and various modifications are possible. The structure of the fluorescence X-ray analysis device 100 described above is an example and is not limited thereto. It can also be replaced with a structure that is substantially the same as the structure shown in the above embodiments, a structure that has the same effect, or a structure that achieves the same purpose. For example, although the outer edges of the window frame component 300 and the window frame retaining component 400 have been described as circular, they can also be polygonal or other shapes.
[0060] also, Figure 10This is a cross-sectional view of the window frame component 300 in a modified example. In the modified example, the first flange 602 and the peripheral wall 606 of the inner film retaining component 600 are formed integrally, but the first flange 602 and the second flange 604 can be separate. Furthermore, in this modified example, the peripheral wall 606 has an inclined portion 1002 that slopes inward from the vertical portion 608 to the front end, instead of the curved portion 610. This shape also allows for easy installation of the partition film 800 onto the window frame component 300. As described above, the flat portion 612 can also be omitted in the modified example.
[0061] Furthermore, the second flange portion 604 has a second peripheral wall 1004 extending vertically toward the front end. For example... Figure 10 As shown, the diaphragm membrane 800 is held not only by the outer film holding member 700 and the first flange portion 602, but also by the second peripheral wall 1004 and the outer film holding member 700. That is, viewed in cross-section, the diaphragm membrane 800 is fixed by being bent twice. Therefore, in the modified example, the diaphragm membrane 800 can be fixed more firmly.
[0062] Explanation of icon numbers
[0063] 100 Fluorescence X-ray analysis device, 102 Sample chamber, 104 Sample stage, 106 Irradiation chamber, 108 Partition wall, 110 X-ray source, 111 Spectrometer element, 112 Detector, 116 Sample cell, 118 Cover component, 200 Screw, 300 Window frame component, 400 Window frame holding component, 402 Upper holding component, 404 Lower holding component, 406 Gas supply port, 408 First gas inlet hole, 500 Thin film support component, 502 Through hole, 600 Inner thin film holding component, 602 First flange, 604 Second flange, 606 Peripheral wall, 608 Vertical part, 610 Bending part, 612 Flat part, 614 Second gas inlet hole, 616 Threaded hole, 700 Outer thin film holding component, 800 Partition membrane, 1002 Inclined part, 1004 Second peripheral wall.
Claims
1. A fluorescent X-ray analysis device having an irradiation chamber in a vacuum environment and provided with an X-ray source that emits X-rays, and a sample chamber in an atmospheric pressure environment and provided with a sample cell, characterized in that, has: a window frame holding member that constitutes a part of a partition between the irradiation chamber and the sample chamber, and has an opening through which the X-rays pass from the irradiation chamber to the sample chamber; and a window frame member that is formed of a material that transmits the X-rays, holds a partition film that constitutes another part of the partition, and is disposed in the opening of the window frame holding member, the window frame holding member has a plurality of through-holes through which the X-rays pass, and has a film support member that is disposed in abutment with the partition film on the irradiation chamber side and supports the partition film from the irradiation chamber side, the window frame member has: an inner side film holding member that is annular, has a peripheral wall that extends from a base end disposed on the sample chamber side toward a front end disposed on the irradiation chamber side, and the front end forms an opening that is closed by a part of the partition film; and an outer side film holding member that fixes a peripheral edge of the part of the partition film on the inner side film holding member by being inserted from the front end of the inner side film holding member and mounted on the base end of the inner side film holding member.
2. The fluorescent X-ray analysis apparatus according to claim 1, wherein the inner side film holding member has a flange portion on the base end that fixes a positional relationship with the window frame holding member.
3. The fluorescent X-ray analysis apparatus according to claim 2, wherein the flange portion has: a first flange portion that is provided on the front end side, and sandwiches the partition film with the outer side film holding member; and a second flange portion that is provided on the base end side, has an outer diameter larger than the first flange portion, and is fixed to the window frame holding member.
4. The fluorescent X-ray analysis apparatus according to claim 3, wherein the first flange portion and the second flange portion are formed integrally.
5. The fluorescent X-ray analysis apparatus according to claim 2, wherein the peripheral wall has a vertical portion that vertically extends from the flange portion toward the front end, and a curved portion that curves from the vertical portion toward the front end.
6. The fluorescent X-ray analysis apparatus according to claim 2, wherein the peripheral wall has a vertical portion that vertically extends from the flange portion toward the front end, and an inclined portion that inclines from the vertical portion toward the front end.
7. The fluorescent X-ray analysis apparatus according to claim 1, wherein the peripheral wall has a flat portion at the front end that is parallel to a plane formed by the opening closed by the part of the partition film.
8. The fluorescent X-ray analysis apparatus according to claim 1, wherein the outer side film holding member and / or the film support member is formed of a resin.
9. The fluorescent X-ray analysis apparatus according to claim 1, wherein the inner side film holding member and / or the window frame holding member is formed of a metal.
10. The fluorescent X-ray analysis apparatus according to claim 2, wherein the window frame holding member has a first gas inflow hole that penetrates from an outer side surface to an inner side surface opposite the window frame member, The flange portion has a second gas inflow hole that penetrates the upper surface and the lower surface.
11. The fluorescent X-ray analysis apparatus according to claim 10, wherein The window frame holding member has a gas supply port on the outside of the first gas inflow hole, which supplies a flowing gas between the sample cell and the separator membrane via the first gas inflow hole and the second gas inflow hole.
Citation Information
Patent Citations
Fluorescent x-ray analytical apparatus
JP1997127028A
Fluorescent x-ray analyzer
WO2004088296A1
Fluorescent x-ray analyzer
WO2005024407A1
X-ray fluorescence analyzer
CN120641744A