WO2020044399A1 - X-ray analysis device - Google Patents

X-ray analysis device Download PDF

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Publication number
WO2020044399A1
WO2020044399A1 PCT/JP2018/031550 JP2018031550W WO2020044399A1 WO 2020044399 A1 WO2020044399 A1 WO 2020044399A1 JP 2018031550 W JP2018031550 W JP 2018031550W WO 2020044399 A1 WO2020044399 A1 WO 2020044399A1
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WO
WIPO (PCT)
Prior art keywords
sample
measurement position
ray
main surface
chamber
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Application number
PCT/JP2018/031550
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French (fr)
Japanese (ja)
Inventor
剛志 秋山
Original Assignee
株式会社島津製作所
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 株式会社島津製作所 filed Critical 株式会社島津製作所
Priority to JP2020539174A priority Critical patent/JP7136211B2/en
Priority to PCT/JP2018/031550 priority patent/WO2020044399A1/en
Priority to CN201880096596.6A priority patent/CN112601952A/en
Priority to TW108128906A priority patent/TWI725511B/en
Publication of WO2020044399A1 publication Critical patent/WO2020044399A1/en

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/2204—Specimen supports therefor; Sample conveying means therefore
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence

Definitions

  • the present invention relates to an X-ray analyzer that irradiates a sample with X-rays for analysis.
  • Patent Document 1 Japanese Patent Application Laid-Open No. 60-0000043
  • the sample When the sample is directly moved between each position (standby position) where the sample is arranged (standby position) using the transfer mechanism and the measuring instrument room, the sample is arranged at the measuring position and the transfer mechanism is retracted from the measuring instrument room.
  • the moving path of the transport mechanism becomes long. In this case, the moving time of the transport mechanism becomes longer, and when the number of samples increases, the transport time of the sample also takes a considerable amount of time.
  • a receiving section for receiving the transport mechanism is required in the measuring instrument room, and in this case, if there is no provision, there is a concern that X-rays leak from the receiving section to the outside of the measuring instrument room.
  • the present invention has been made in view of the above problems, and an object of the present invention is to suppress the leakage of X-rays during measurement, and to transport a sample between a standby position and a measurement position.
  • An object of the present invention is to provide an X-ray analyzer.
  • the X-ray analyzer has a sample support unit that supports a plurality of samples arranged at each standby position, and a grip unit that grips the sample, between the standby position and the measurement position.
  • a transport unit for moving the sample, an X-ray irradiator for irradiating the sample placed at the measurement position with primary X-rays, and a fluorescent X generated from the sample irradiated with the primary X-rays
  • a sample chamber that includes a detector that detects a line and a first portion and a second portion that are separably provided, and that accommodates the sample and the grip in a state where the sample is arranged at the measurement position. And. The first part is provided around the measurement position, and the second part is provided in the transport unit. In a state where the sample is arranged at the measurement position, the second portion comes into contact with the first portion, so that the sample chamber is formed.
  • the provision of the transport unit for transporting the sample enables transport of the sample between each standby position and the measurement position.
  • a second portion which is a part of the sample chamber provided so as to be separable, is provided in the transport unit, and the second portion is another part of the sample chamber in a state where the sample is arranged at the measurement position.
  • the sample chamber is formed.
  • the holding part for holding the sample and the sample are accommodated in the sample chamber, a part of the X-ray transmitted through the sample at the time of measurement is shielded by the sample chamber. Thereby, it is possible to suppress the X-ray from leaking out of the sample chamber.
  • the X-ray analyzer may further include a sample stage for mounting the sample at the measurement position.
  • the sample stage has a first main surface facing the X-ray irradiator and the detector side, and a second main surface located opposite to the first main surface and on which the sample is placed.
  • the grip may be provided movably in a normal direction perpendicular to the second main surface.
  • the first portion has a cylinder axis parallel to the normal direction, and is provided on the second main surface such that one end side in the cylinder axis direction is closed by the sample stage.
  • the second portion may be a lid member provided so as to be able to face the cylindrical member from the other end side of the cylindrical member in the cylinder axis direction.
  • the lid member in a state where the gripping portion moves along the normal direction to approach the second main surface and the sample is arranged at the measurement position, the lid member is formed in the cylindrical shape. It is preferable that the sample chamber is formed by closing the other end of the member.
  • the configuration of the sample chamber is simplified by forming the sample chamber with a cylindrical member having one end closed by the sample stage and a lid member provided so as to be able to close the other end of the cylindrical member. Can be. Furthermore, since the sample chamber can be formed by moving the transport section in the direction of the normal to the second main surface of the sample stage, the operation of the transport section for forming the sample chamber can be simplified.
  • the gripper may maintain a state in which the sample is gripped at the measurement position, and the X-ray irradiator is gripped by the gripper.
  • the sample may be irradiated with the primary X-ray.
  • the sample is irradiated with the primary X-ray while the sample is held by the holding unit, it is possible to omit removing the sample from the holding unit at the measurement position during analysis. Along with this, it is also possible to omit holding the sample removed at the measurement position with the holding unit again. As a result, the time for moving the sample can be reduced.
  • the grip may be provided rotatably around a rotation axis perpendicular to the analysis surface of the sample.
  • the sample can be rotated at the measurement position by the rotatably provided grip portion.
  • an X-ray analyzer capable of transporting a sample between a standby position and a measurement position while suppressing leakage of X-rays during measurement.
  • FIG. 2 is a diagram illustrating a transport unit and a sample support unit when viewed from the direction of arrow II illustrated in FIG. 1.
  • FIG. 1 is a schematic sectional view showing an X-ray analyzer according to the embodiment.
  • FIG. 2 is a diagram illustrating the transport unit and the sample support unit when viewed from the direction of arrow II illustrated in FIG. 1.
  • An X-ray analyzer 1 according to an embodiment will be described with reference to FIGS.
  • the X-ray analyzer 1 includes a housing 2, a sample support unit 10, a transport unit 20, an X-ray irradiation unit 30, a detector 40, an analysis chamber 50, and a control unit 60. .
  • the housing 2 is a member constituting an outer shell of the X-ray analyzer 1, and includes a sample support unit 10, a transport unit 20, an X-ray irradiation unit 30, a detector 40, an analysis chamber 50, and a control unit 60 therein. To accommodate.
  • the sample support 10 has, for example, a flat plate shape.
  • the sample support unit 10 supports a plurality of samples S arranged at each standby position.
  • the plurality of samples S are arranged, for example, in a matrix on the sample supporter 10. Thereby, a plurality of samples S can be efficiently arranged.
  • the transport unit 20 moves the sample S between each standby position and the measurement position.
  • the transport section 20 includes an X-axis rail 21, a Y-axis rail 22, a Z-axis rail 23, a moving body 24, an arm section 25, a grip section 26, and a rotation drive section 27.
  • the X-axis rail 21 extends in the X-axis direction.
  • the X-axis rail 21 is provided movably in the Y-axis direction by a Y-axis rail 22.
  • the X-axis rail 21 runs on the Y-axis rail 22 by a drive source such as a motor.
  • the X-axis direction is any one horizontal direction
  • the Y-axis direction is a direction orthogonal to the X-axis direction.
  • Y-axis rail 22 extends along the Y-axis direction.
  • the Y-axis rail 22 guides the movement of the X-axis rail 21 in the Y-axis direction.
  • the Y-axis rails 22 are provided at both ends of the X-axis rail 21 in the X-axis direction.
  • the Z-axis rail 23 extends along the Z-axis direction.
  • the Z-axis direction is a vertical direction, and is orthogonal to the X-axis direction and the Y-axis direction.
  • the Z-axis rail 23 is fixed to the moving body 24.
  • the Z-axis rail 23 guides the movement of the arm 25 in the Z-axis direction.
  • the moving body 24 is provided movably in the X-axis direction along the X-axis rail 21.
  • the moving body 24 is moved by a driving source such as a motor.
  • a Z-axis rail 23 is fixed to the moving body 24. As a result, when the moving body 24 moves, the Z-axis rail 23 also moves along the X-axis direction.
  • the arm 25 is provided movably in the Z-axis direction by the Z-axis rail 23.
  • the arm 25 is fixed to the Z-axis rail 23 so as to be movable in the Z-axis direction.
  • the arm 25 is provided rotatably about a rotation axis perpendicular to the analysis surface Sa of the sample S.
  • the arm unit 25 is rotated by the rotation drive unit 27.
  • the grip 26 is provided at the tip of the arm 25 (the lower end in FIG. 1).
  • the holding unit 26 is provided so as to hold the sample S.
  • the holding unit 26 holds the sample S and moves the sample S between the standby position and the measurement position.
  • the grip portion 26 is provided movably in the X-axis direction, the Y-axis direction, and the Z-axis direction.
  • the grip portion 26 moves along the X-axis direction together with the moving body 24 when the moving body 24 moves along the X-axis direction.
  • the grip portion 26 moves along the X-axis rail 21 along the Y-axis direction as the X-axis rail 21 moves along the Y-axis direction.
  • the grip portion 26 moves along the Z-axis direction together with the arm portion 25 when the arm portion 25 moves along the Z-axis direction.
  • the gripper 26 is provided rotatably about a rotation axis perpendicular to the analysis surface Sa of the sample S. Specifically, as the arm 25 rotates as described above, the grip 26 rotates integrally with the arm 25.
  • the rotation axis direction coincides with the Z axis direction and a cylinder axis C direction of the first portion 511 described later.
  • the X-ray irradiator 30 irradiates the sample X arranged at the measurement position with primary X-rays.
  • X-ray irradiator 30 is, for example, an X-ray tube.
  • a target serving as an anode and a filament serving as a cathode are arranged inside the X-ray tube.
  • thermions emitted from the filament collide with the target.
  • primary X-rays generated in the target are emitted.
  • the detector 40 detects fluorescent X-rays generated from the sample S irradiated with the primary X-rays.
  • the detector 40 includes a housing provided with an introduction window through which fluorescent X-rays are introduced, and a detection element (semiconductor element) housed inside the housing.
  • the detector 40 outputs a signal proportional to the detected energy of the fluorescent X-ray to the control unit 60.
  • the analysis chamber 50 includes a sample chamber 51, an irradiation chamber 52, and a sample stage 53.
  • the sample stage 53 is a stage for placing a sample at a measurement position.
  • the sample stage 53 has a plate shape and is provided so as to partition the sample chamber 51 from the irradiation chamber 52.
  • the sample stage 53 has a first main surface 53a facing the X-ray irradiator 30 and the detector 40, and a second main surface 53b on the opposite side to the first main surface 53a and on which the sample S is placed. Having.
  • the sample chamber 51 has a first portion 511 and a second portion 512 that are configured to be separable, and accommodates the sample S and the holding portion 26 inside in a state where the sample S is arranged at the measurement position.
  • the sample chamber 51 is provided so that the pressure can be reduced.
  • the sample chamber 51 is provided so that a desired gas can be introduced.
  • the first portion 511 is provided around the measurement position.
  • the first portion 511 is, for example, a cylindrical member having a cylindrical axis C parallel to the normal line direction of the second main surface 53b.
  • the first portion 511 is provided on the second main surface 53 b such that one end side in the cylinder axis C direction is closed by the sample stage 53.
  • the first portion 511 is configured by a member capable of shielding X-rays such as an iron plate and SUS.
  • a groove is provided at the other end (upper end) of the first portion 511 in the direction of the cylinder axis C, and a seal member 513 is arranged in the groove.
  • the seal member 513 is a member for keeping the inside of the sample chamber 51 airtight.
  • the seal member 513 is made of, for example, a rubber member having elasticity.
  • the second part 512 is provided in the transport unit 20. Specifically, the second portion 512 is provided on the arm 25. The second portion 512 is provided so as to be in contact with the first portion 511. The second part 512 contacts the first part 511 in a state where the sample S is arranged at the measurement position. As a result, the sample chamber 51 is formed.
  • the second portion 512 is provided so as to be able to face the first portion 511 from the other end of the first portion 511 in the direction of the cylinder axis C.
  • the second part 512 is a lid member provided so as to be able to close the other end of the first part 511 in the direction of the cylinder axis C.
  • the second portion 512 closes the other end of the first portion 511 in a state where the sample S is arranged at the measurement position.
  • the second portion 512 is configured by a member capable of shielding X-rays such as an iron plate and SUS.
  • the irradiation room 52 is provided with the X-ray irradiation unit 30 and the detector 40.
  • the irradiation chamber 52 is provided so as to be able to reduce the pressure.
  • the irradiation chamber 52 is provided so that a desired gas can be introduced.
  • the control unit 60 controls the operation of the X-ray analyzer 1, such as the operation of the transport unit 20, the operations of the X-ray irradiation unit 30 and the detector 40.
  • the gripper 26 is moved above the sample S located at the standby position. Specifically, the moving body 24, the X-axis rail 21, and the arm 25 are moved in the X-axis direction, the Y-axis direction, and the Z-axis direction such that the gripper 26 is positioned above the sample S.
  • the gripper 26 is moved so as to approach the sample S. Specifically, the arm 25 is moved to the sample S side along the Z-axis rail 23. The sample S is held by bringing the holding unit 26 into contact with the sample S.
  • the gripper 26 is moved above the measurement position while holding the sample S. Specifically, the moving body 24, the X-axis rail 21, and the arm 25 are moved in the X-axis direction, the Y-axis direction, and the Z-axis direction, respectively, so that the grip unit 26 is positioned above the measurement position.
  • the second portion 512 provided on the arm portion 25 is located above the first portion 511, and the second portion 512 is moved from the other end (upper end) of the first portion 511 to the first portion. 511.
  • the gripper 26 is moved along the normal direction of the second main surface 53b of the sample stage 53 so as to approach the second main surface 53b.
  • the normal direction coincides with the Z-axis direction.
  • the gripper 26 is brought closer to the second main surface 53b.
  • the arm 25 is moved along the Z-axis direction so that the sample S reaches the measurement position.
  • the sample S is preferably mounted on the second main surface 53b.
  • the second portion 512 closes the other end of the first portion 511. As a result, the sample chamber 51 is formed. In this state, the holding section 26 and the sample S are accommodated inside the sample chamber 51.
  • X X-ray analysis becomes possible by placing the sample S at the measurement position.
  • primary X-rays are emitted from the X-ray irradiator 30 to the sample S arranged at the measurement position, and the fluorescent X-rays generated from the sample S are detected by the detector 40.
  • the grip portion 26 and the sample S are covered by the first portion 511 and the second portion 512. Thereby, a part of the X-ray transmitted through the sample S during the analysis is shielded by the first portion 511 and the second portion 512. Thus, it is possible to suppress the X-ray from leaking out of the sample chamber 51.
  • the state where the gripper 26 grips the sample S at the measurement position may be maintained. In this case, removing the sample S from the grip portion 26 at the measurement position during measurement can be omitted. Along with this, it is also possible to omit again holding the sample S removed at the measurement position by the holding unit 26. As a result, the time for moving the sample S can be reduced.
  • the gripping of the sample S by the gripper 26 may be released at the measurement position. In this case, it is possible to prevent the vibration from being transmitted to the sample S from the transport unit 20 side during the measurement.
  • the gripper 26 When irradiating the sample S with primary X-rays, the gripper 26 may be rotated about a rotation axis perpendicular to the analysis surface Sa of the sample S while the sample S is gripped. In this case, since the sample S can be rotated at the measurement position, the sample S can be analyzed in the circumferential direction. Further, since the arm 25 is rotated by a driving source such as a motor, the rotation mechanism can be simplified.
  • the sample S is moved from the measurement position to the standby position. Specifically, the gripper 26 is moved along the normal direction of the second main surface 53b so as to move away from the second main surface 53b of the sample stage 53 while holding the sample S arranged at the measurement position. . Specifically, the arm 25 is moved in the Z-axis direction so as to move away from the second main surface 53b.
  • the moving body 24, the X-axis rail 21, and the arm 25 are moved in the X-axis direction, the Y-axis direction, and the Z-axis direction so that the sample S is located at the standby position.
  • the holding of the sample S by the holding unit 26 is released at the standby position.
  • the gripper 26 is moved to a predetermined position.
  • the sample stage 53 is provided and the sample S is mounted on the sample stage 53 at the time of analysis has been described as an example.
  • the present invention is not limited to this.
  • the sample stage 53 may be omitted as long as the gripper 26 can maintain the state where the sample S is gripped at the measurement position and the primary X-ray can be irradiated on the sample S in this state.
  • the sample S can be measured with high accuracy.
  • the present invention is not limited to this. As long as the sample chamber 51 is formed in a state where the second portion 512 is moved along at least one of the XYZ axis directions and is in contact with the first portion 511, the shapes of the first portion 511 and the second portion 512 are Can be appropriately selected.
  • the first portion 511 is a cylindrical member whose one end is closed by the sample stage 53, and the second portion 512 is a lid member provided so that the other end of the first portion 511 can be closed.
  • the configuration of the sample chamber 51 can be simplified.
  • the sample chamber 51 can be formed by moving the gripping section 26 in the direction of the normal to the second main surface 53b of the sample stage 53, the operation of the transfer section 20 for forming the sample chamber 51 can be simplified.
  • 1 X-ray analyzer 2 housing, 10 sample support unit, 20 transport unit, 21 ⁇ X-axis rail, 22 Y-axis rail, 23 Z-axis rail, 24 moving body, 25 arm unit, 26 grip unit, 27 rotation drive unit , 30 ° X-ray irradiation unit, 40 ° detector, 50 ° analysis chamber, 51 ° sample chamber, 52 ° irradiation chamber, 53 ° sample stage, 53a ⁇ first main surface, 53b ⁇ second main surface, 60 ° control unit, 511 first part, 512 ° first 2 parts, 513 sealing member, C cylinder shaft, S sample, Sa analysis surface.

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Abstract

This X-ray analysis device (1) comprises: a sample support unit (10) for supporting a plurality of samples (S) disposed at various standby positions; a conveyance unit (20) that has a holding unit (26) for holding a sample (S) and is for moving samples between the standby positions and a measurement position; an X-ray irradiation unit (30) for irradiating primary X-rays onto a sample disposed at the measurement position; a detector (40) for detecting fluorescence X-rays emitted from the sample irradiated with the primary X-rays; and a sample chamber (51) that includes a first part (511) and a second part (512) that are provided so as to be separable and accommodates a sample (S) and the holding unit (26) in a state in which the sample (S) has been disposed at the measurement position. The first part (511) is provided near the measurement position and the second part (512) is provided to the conveyance unit (20). In a state in which the sample (S) has been disposed at the measurement position, the sample chamber (51) is formed through the touching of the first part (511) by the second part (512).

Description

Ｘ線分析装置X-ray analyzer
　本発明は、試料にＸ線を照射して分析を行なうＸ線分析装置に関する。 The present invention relates to an X-ray analyzer that irradiates a sample with X-rays for analysis.
　従来のＸ線分析装置において、複数の試料が載置された回転テーブルを回転させ、昇降位置に移動された試料を、昇降機構を用いて計測器室に移動させる技術が開示されている（特開昭６０－００００４３号公報（特許文献１）参照）。 In a conventional X-ray analyzer, there is disclosed a technique in which a rotary table on which a plurality of samples are placed is rotated, and a sample moved to an elevating position is moved to a measuring instrument room using an elevating mechanism. Japanese Patent Application Laid-Open No. 60-0000043 (Patent Document 1).
特開昭６０－００００４３号公報JP-A-60-0000043
　しかしながら、特許文献１に開示のＸ線分析装置においては、計測器室に試料を移動させるためには、回転テーブルを回転させて各試料を順に昇降位置に移動させなければならない。このため、試料が配置された各位置と計測器室との間で直接試料を移動することができなかった。この場合には、回転テーブルの所定の移動経路上にしか試料を配置できないため、装置内のスペースを効率よく利用することが困難となる。 However, in the X-ray analyzer disclosed in Patent Literature 1, in order to move a sample to the measuring instrument room, it is necessary to rotate the rotary table and move each sample sequentially to the elevating position. For this reason, the sample could not be directly moved between each position where the sample was arranged and the measuring instrument room. In this case, since the sample can be arranged only on a predetermined moving path of the rotary table, it is difficult to efficiently use the space in the apparatus.
　搬送機構を用いて試料が配置された各位置（待機位置）と計測器室との間で直接試料を移動させる場合に、試料を測定位置に配置して計測器室から搬送機構を退避させた後にＸ線分析を行なう場合には、搬送機構の移動経路が長くなる。この場合には、搬送機構の移動時間が長くなり、試料の数が多くなった場合には、試料の搬送時間も相当程度掛かってしまう。 When the sample is directly moved between each position (standby position) where the sample is arranged (standby position) using the transfer mechanism and the measuring instrument room, the sample is arranged at the measuring position and the transfer mechanism is retracted from the measuring instrument room. When the X-ray analysis is performed later, the moving path of the transport mechanism becomes long. In this case, the moving time of the transport mechanism becomes longer, and when the number of samples increases, the transport time of the sample also takes a considerable amount of time.
　また、計測器室に搬送機構を受け入れる受入部が必要となり、この場合において、何ら手立てがない場合には、当該受入部からＸ線が計測器室外に漏れ出ることが懸念される。 Also, a receiving section for receiving the transport mechanism is required in the measuring instrument room, and in this case, if there is no provision, there is a concern that X-rays leak from the receiving section to the outside of the measuring instrument room.
　本発明は、上記のような問題に鑑みてなされたものであり、本発明の目的は、測定時のＸ線の漏れを抑制しつつ、待機位置と測定位置との間で試料を搬送可能なＸ線分析装置を提供することにある。 The present invention has been made in view of the above problems, and an object of the present invention is to suppress the leakage of X-rays during measurement, and to transport a sample between a standby position and a measurement position. An object of the present invention is to provide an X-ray analyzer.
　本発明に基づくＸ線分析装置は、各待機位置に配置された複数の試料を支持する試料支持部と、上記試料を把持する把持部を有し、上記各待機位置と測定位置との間で上記試料を移動させる搬送部と、上記測定位置に配置された上記試料に向けて１次Ｘ線を照射するＸ線照射部と、上記１次Ｘ線を照射された上記試料から発生する蛍光Ｘ線を検出する検出器と、分離可能に設けられた第１部分および第２部分を含み、上記測定位置に上記試料が配置された状態で上記試料および上記把持部を収容することとなる試料室と、を備える。上記第１部分は、上記測定位置の周辺に設けられており、上記第２部分は、上記搬送部に設けられている。上記測定位置に上記試料が配置された状態において、上記第２部分が上記第１部分に当接することにより上記試料室が形成された状態となる。 The X-ray analyzer according to the present invention has a sample support unit that supports a plurality of samples arranged at each standby position, and a grip unit that grips the sample, between the standby position and the measurement position. A transport unit for moving the sample, an X-ray irradiator for irradiating the sample placed at the measurement position with primary X-rays, and a fluorescent X generated from the sample irradiated with the primary X-rays A sample chamber that includes a detector that detects a line and a first portion and a second portion that are separably provided, and that accommodates the sample and the grip in a state where the sample is arranged at the measurement position. And. The first part is provided around the measurement position, and the second part is provided in the transport unit. In a state where the sample is arranged at the measurement position, the second portion comes into contact with the first portion, so that the sample chamber is formed.
　上記構成によれば、Ｘ線分析装置において、試料を搬送する搬送部を設けたことにより、各待機位置と測定位置との間で試料を搬送することが可能となる。さらに、分離可能に設けられた試料室の一部である第２部分を搬送部に設け、試料が測定位置に配置された状態において、上記第２部分が当該試料室の他の一部である第１部分に当接することにより、試料室が形成された状態となる。この状態においては、試料を把持するための把持部および当該試料が試料室内に収容されるため、測定時に試料を透過したＸ線の一部が試料室によって遮蔽される。これにより、Ｘ線が試料室の外部に漏れ出ることを抑制することができる。 According to the above configuration, in the X-ray analyzer, the provision of the transport unit for transporting the sample enables transport of the sample between each standby position and the measurement position. Further, a second portion, which is a part of the sample chamber provided so as to be separable, is provided in the transport unit, and the second portion is another part of the sample chamber in a state where the sample is arranged at the measurement position. By coming into contact with the first portion, the sample chamber is formed. In this state, since the holding part for holding the sample and the sample are accommodated in the sample chamber, a part of the X-ray transmitted through the sample at the time of measurement is shielded by the sample chamber. Thereby, it is possible to suppress the X-ray from leaking out of the sample chamber.
　上記本発明に基づくＸ線分析装置は、上記測定位置において上記試料を載置させるための試料ステージをさらに備えていてもよい。上記試料ステージは、上記Ｘ線照射部および上記検出器側を向く第１主面と、上記第１主面の反対側に位置し、上記試料が載置される第２主面とを有していることが好ましい。上記把持部は、上記第２主面に垂直な法線方向に移動可能に設けられていてもよい。この場合には、上記第１部分は、上記法線方向に平行な筒軸を有し、上記筒軸方向における一端側が上記試料ステージによって閉塞されるように上記第２主面上に設けられた筒状部材であってもよく、上記第２部分は、上記筒軸方向における上記筒状部材の他端側から上記筒状部材に対向可能に設けられた蓋部材であってもよい。さらに、この場合には、上記把持部が上記法線方向に沿って上記第２主面に近づくように移動して上記測定位置に上記試料が配置された状態で、上記蓋部材が上記筒状部材の上記他端側を閉塞することにより、上記試料室が形成された状態となることが好ましい。 The X-ray analyzer according to the present invention may further include a sample stage for mounting the sample at the measurement position. The sample stage has a first main surface facing the X-ray irradiator and the detector side, and a second main surface located opposite to the first main surface and on which the sample is placed. Is preferred. The grip may be provided movably in a normal direction perpendicular to the second main surface. In this case, the first portion has a cylinder axis parallel to the normal direction, and is provided on the second main surface such that one end side in the cylinder axis direction is closed by the sample stage. The second portion may be a lid member provided so as to be able to face the cylindrical member from the other end side of the cylindrical member in the cylinder axis direction. Further, in this case, in a state where the gripping portion moves along the normal direction to approach the second main surface and the sample is arranged at the measurement position, the lid member is formed in the cylindrical shape. It is preferable that the sample chamber is formed by closing the other end of the member.
　上記構成によれば、試料ステージに試料を載置してＸ線分析を行なうことができるため、試料を精度よく測定することができる。また、一端側が試料ステージによって閉塞された筒状部材と、筒状部材の他端側を閉塞可能に設けられた蓋部材とによって試料室を構成することにより、試料室の構成を簡素化することができる。さらに、試料ステージの第２主面の法線方向に搬送部を移動させることにより試料室を形成することができるため、試料室を形成するための搬送部の動作をシンプルにすることができる。 According to the above configuration, since the sample can be placed on the sample stage and X-ray analysis can be performed, the sample can be accurately measured. Further, the configuration of the sample chamber is simplified by forming the sample chamber with a cylindrical member having one end closed by the sample stage and a lid member provided so as to be able to close the other end of the cylindrical member. Can be. Furthermore, since the sample chamber can be formed by moving the transport section in the direction of the normal to the second main surface of the sample stage, the operation of the transport section for forming the sample chamber can be simplified.
　上記本発明に基づくＸ線分析装置にあっては、上記把持部は、上記測定位置にて上記試料を把持した状態を維持してもよく、上記Ｘ線照射部は、上記把持部に把持された上記試料に向けて上記１次Ｘ線を照射してもよい。 In the X-ray analyzer according to the present invention, the gripper may maintain a state in which the sample is gripped at the measurement position, and the X-ray irradiator is gripped by the gripper. The sample may be irradiated with the primary X-ray.
　上記構成によれば、把持部が試料を把持した状態で１次Ｘ線を試料に照射するため、分析時に測定位置で試料を把持部から取り外すことを省略することができる。これに伴い、測定位置で取り外された試料を再度把持部で把持したりすることも省略することができる。この結果、試料を移動させるための時間を短縮することができる。 According to the above configuration, since the sample is irradiated with the primary X-ray while the sample is held by the holding unit, it is possible to omit removing the sample from the holding unit at the measurement position during analysis. Along with this, it is also possible to omit holding the sample removed at the measurement position with the holding unit again. As a result, the time for moving the sample can be reduced.
　上記本発明に基づくＸ線分析装置にあっては、上記把持部は、上記試料の分析面に垂直な回転軸まわりに回転可能に設けられていてもよい。 In the X-ray analyzer according to the present invention, the grip may be provided rotatably around a rotation axis perpendicular to the analysis surface of the sample.
　上記構成によれば、把持部が回転可能に設けられることにより、測定位置において試料を回転させることができる。 According to the above configuration, the sample can be rotated at the measurement position by the rotatably provided grip portion.
　本発明によれば、測定時のＸ線の漏れを抑制しつつ、待機位置と測定位置との間で試料を搬送可能なＸ線分析装置を提供することができる。 According to the present invention, it is possible to provide an X-ray analyzer capable of transporting a sample between a standby position and a measurement position while suppressing leakage of X-rays during measurement.
実施の形態に係るＸ線分析装置を示す概略断面図である。It is a schematic sectional view showing the X-ray analysis device concerning an embodiment. 図１に示す矢視ＩＩ方向から見た場合の搬送部および試料支持部を示す図である。FIG. 2 is a diagram illustrating a transport unit and a sample support unit when viewed from the direction of arrow II illustrated in FIG. 1.
　以下、本発明の実施の形態について、図を参照して詳細に説明する。以下に示す実施の形態においては、Ｘ線分析装置として、蛍光Ｘ線分析装置を例示して説明する。また、以下に示す実施の形態においては、同一のまたは共通する部分について図中同一の符号を付し、その説明は繰り返さない。 Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings. In the embodiment described below, a fluorescent X-ray analyzer will be described as an example of the X-ray analyzer. In the following embodiments, the same or common portions are denoted by the same reference numerals in the drawings, and description thereof will not be repeated.
　（Ｘ線分析装置の構成）
　図１は、実施の形態に係るＸ線分析装置を示す概略断面図である。図２は、図１に示す矢視ＩＩ方向から見た場合の搬送部および試料支持部を示す図である。図１および図２を参照して、実施の形態に係るＸ線分析装置１について説明する。 (Configuration of X-ray analyzer)
FIG. 1 is a schematic sectional view showing an X-ray analyzer according to the embodiment. FIG. 2 is a diagram illustrating the transport unit and the sample support unit when viewed from the direction of arrow II illustrated in FIG. 1. An X-ray analyzer 1 according to an embodiment will be described with reference to FIGS.
　図１および図２に示すように、Ｘ線分析装置１は、筐体２、試料支持部１０、搬送部２０、Ｘ線照射部３０、検出器４０、分析チャンバ５０、および制御部６０を備える。 As shown in FIGS. 1 and 2, the X-ray analyzer 1 includes a housing 2, a sample support unit 10, a transport unit 20, an X-ray irradiation unit 30, a detector 40, an analysis chamber 50, and a control unit 60. .
　筐体２は、Ｘ線分析装置１の外殻を構成する部材であり、試料支持部１０、搬送部２０、Ｘ線照射部３０、検出器４０、分析チャンバ５０、および制御部６０を内部に収容する。 The housing 2 is a member constituting an outer shell of the X-ray analyzer 1, and includes a sample support unit 10, a transport unit 20, an X-ray irradiation unit 30, a detector 40, an analysis chamber 50, and a control unit 60 therein. To accommodate.
　試料支持部１０は、たとえば平板形状を有する。試料支持部１０は、各待機位置に配置された複数の試料Ｓを支持する。複数の試料Ｓは、たとえば、試料支持部１０に行列状に配置されている。これにより、複数の試料Ｓを効率よく配置することができる。 The sample support 10 has, for example, a flat plate shape. The sample support unit 10 supports a plurality of samples S arranged at each standby position. The plurality of samples S are arranged, for example, in a matrix on the sample supporter 10. Thereby, a plurality of samples S can be efficiently arranged.
　搬送部２０は、各待機位置と測定位置との間で試料Ｓを移動させる。搬送部２０は、Ｘ軸レール２１、Ｙ軸レール２２、Ｚ軸レール２３、移動体２４、アーム部２５、把持部２６、および回転駆動部２７を含む。 (4) The transport unit 20 moves the sample S between each standby position and the measurement position. The transport section 20 includes an X-axis rail 21, a Y-axis rail 22, a Z-axis rail 23, a moving body 24, an arm section 25, a grip section 26, and a rotation drive section 27.
　Ｘ軸レール２１は、Ｘ軸方向に延在する。Ｘ軸レール２１は、Ｙ軸レール２２によってＹ軸方向に移動可能に設けられている。Ｘ軸レール２１は、たとえばモータ等の駆動源によってＹ軸レール２２上を走行する。 The X-axis rail 21 extends in the X-axis direction. The X-axis rail 21 is provided movably in the Y-axis direction by a Y-axis rail 22. The X-axis rail 21 runs on the Y-axis rail 22 by a drive source such as a motor.
　なお、Ｘ軸方向とは、水平方向における任意の１方向であり、Ｙ軸方向とは、Ｘ軸方向に直交する方向である。 Note that the X-axis direction is any one horizontal direction, and the Y-axis direction is a direction orthogonal to the X-axis direction.
　Ｙ軸レール２２は、Ｙ軸方向に沿って延在する。Ｙ軸レール２２は、Ｘ軸レール２１のＹ軸方向の移動を案内する。Ｙ軸レール２２は、Ｘ軸方向におけるＸ軸レール２１の両端に設けられている。 Y-axis rail 22 extends along the Y-axis direction. The Y-axis rail 22 guides the movement of the X-axis rail 21 in the Y-axis direction. The Y-axis rails 22 are provided at both ends of the X-axis rail 21 in the X-axis direction.
　Ｚ軸レール２３は、Ｚ軸方向に沿って延在する。Ｚ軸方向は、上下方向であり、Ｘ軸方向およびＹ軸方向に直交する。Ｚ軸レール２３は、移動体２４に固定されている。Ｚ軸レール２３は、アーム部２５のＺ軸方向の移動を案内する。 The Z-axis rail 23 extends along the Z-axis direction. The Z-axis direction is a vertical direction, and is orthogonal to the X-axis direction and the Y-axis direction. The Z-axis rail 23 is fixed to the moving body 24. The Z-axis rail 23 guides the movement of the arm 25 in the Z-axis direction.
　移動体２４は、Ｘ軸レール２１に沿ってＸ軸方向に移動可能に設けられている。移動体２４は、モータ等の駆動源によって移動する。移動体２４には、Ｚ軸レール２３が固定されている。これにより、移動体２４が移動することにより、Ｚ軸レール２３もＸ軸方向に沿って移動する。 The moving body 24 is provided movably in the X-axis direction along the X-axis rail 21. The moving body 24 is moved by a driving source such as a motor. A Z-axis rail 23 is fixed to the moving body 24. As a result, when the moving body 24 moves, the Z-axis rail 23 also moves along the X-axis direction.
　アーム部２５は、Ｚ軸レール２３によってＺ軸方向に移動可能に設けられている。アーム部２５は、Ｚ軸方向に移動可能にＺ軸レール２３に固定されている。また、アーム部２５は、試料Ｓの分析面Ｓａに垂直な回転軸まわりに回転可能に設けられている。アーム部２５は、回転駆動部２７によって回転する。 The arm 25 is provided movably in the Z-axis direction by the Z-axis rail 23. The arm 25 is fixed to the Z-axis rail 23 so as to be movable in the Z-axis direction. The arm 25 is provided rotatably about a rotation axis perpendicular to the analysis surface Sa of the sample S. The arm unit 25 is rotated by the rotation drive unit 27.
　把持部２６は、アーム部２５の先端（図１中下端）に設けられている。把持部２６は、試料Ｓを把持可能に設けられている。把持部２６は、試料Ｓを把持し、待機位置と測定位置との間で試料Ｓを移動させる。 The grip 26 is provided at the tip of the arm 25 (the lower end in FIG. 1). The holding unit 26 is provided so as to hold the sample S. The holding unit 26 holds the sample S and moves the sample S between the standby position and the measurement position.
　把持部２６は、Ｘ軸方向、Ｙ軸方向、およびＺ軸方向に移動可能に設けられている。把持部２６は、移動体２４がＸ軸方向に沿って移動することにより、移動体２４とともにＸ軸方向に沿って移動する。把持部２６は、Ｘ軸レール２１がＹ軸方向に沿って移動することにより、Ｘ軸レール２１とともにＹ軸方向に沿って移動する。把持部２６は、アーム部２５がＺ軸方向に沿って移動することにより、アーム部２５とともにＺ軸方向に沿って移動する。 The grip portion 26 is provided movably in the X-axis direction, the Y-axis direction, and the Z-axis direction. The grip portion 26 moves along the X-axis direction together with the moving body 24 when the moving body 24 moves along the X-axis direction. The grip portion 26 moves along the X-axis rail 21 along the Y-axis direction as the X-axis rail 21 moves along the Y-axis direction. The grip portion 26 moves along the Z-axis direction together with the arm portion 25 when the arm portion 25 moves along the Z-axis direction.
　把持部２６は、試料Ｓの分析面Ｓａに垂直な回転軸まわりに回転可能に設けられている。具体的には、上記のようにアーム部２５が回転することにより、アーム部２５と一体となって把持部２６が回転する。なお、上記回転軸方向は、Ｚ軸方向および後述する第１部分５１１の筒軸Ｃ方向と一致する。 The gripper 26 is provided rotatably about a rotation axis perpendicular to the analysis surface Sa of the sample S. Specifically, as the arm 25 rotates as described above, the grip 26 rotates integrally with the arm 25. The rotation axis direction coincides with the Z axis direction and a cylinder axis C direction of the first portion 511 described later.
　Ｘ線照射部３０は、測定位置に配置された試料Ｓに向けて１次Ｘ線を照射する。Ｘ線照射部３０は、たとえばＸ線管である。Ｘ線管の内部には陽極であるターゲットと陰極であるフィラメントとが配置されている。ターゲットとフィラメントとの間に高電圧を印加することにより、フィラメントから放射された熱電子をターゲットに衝突させる。これにより、ターゲットで発生した１次Ｘ線が出射される。 (4) The X-ray irradiator 30 irradiates the sample X arranged at the measurement position with primary X-rays. X-ray irradiator 30 is, for example, an X-ray tube. A target serving as an anode and a filament serving as a cathode are arranged inside the X-ray tube. By applying a high voltage between the target and the filament, thermions emitted from the filament collide with the target. Thereby, primary X-rays generated in the target are emitted.
　検出器４０は、１次Ｘ線を照射された試料Ｓから発生する蛍光Ｘ線を検出する。検出器４０は、蛍光Ｘ線が導入される導入窓が設けられた筐体と、筐体内部に収容された検出素子（半導体素子）によって構成されている。検出器４０は、検出した蛍光Ｘ線のエネルギーに比例した信号を制御部６０に出力する。 The detector 40 detects fluorescent X-rays generated from the sample S irradiated with the primary X-rays. The detector 40 includes a housing provided with an introduction window through which fluorescent X-rays are introduced, and a detection element (semiconductor element) housed inside the housing. The detector 40 outputs a signal proportional to the detected energy of the fluorescent X-ray to the control unit 60.
　分析チャンバ５０は、試料室５１、照射室５２、および試料ステージ５３によって構成される。 The analysis chamber 50 includes a sample chamber 51, an irradiation chamber 52, and a sample stage 53.
　試料ステージ５３は、測定位置に試料を載置させるためのステージである。試料ステージ５３は、板状形状を有し、試料室５１と照射室５２とを仕切るように設けられている。試料ステージ５３は、Ｘ線照射部３０および検出器４０側を向く第１主面５３ａと、当該第１主面５３ａと反対側に位置し、試料Ｓが載置される第２主面５３ｂとを有する。 The sample stage 53 is a stage for placing a sample at a measurement position. The sample stage 53 has a plate shape and is provided so as to partition the sample chamber 51 from the irradiation chamber 52. The sample stage 53 has a first main surface 53a facing the X-ray irradiator 30 and the detector 40, and a second main surface 53b on the opposite side to the first main surface 53a and on which the sample S is placed. Having.
　試料室５１は、分離可能に構成された第１部分５１１および第２部分５１２を有し、測定位置に試料Ｓが配置された状態で、試料Ｓおよび把持部２６を内部に収容する。試料室５１は、減圧可能に設けられている。また、試料室５１は、所望のガスを導入可能に設けられている。 The sample chamber 51 has a first portion 511 and a second portion 512 that are configured to be separable, and accommodates the sample S and the holding portion 26 inside in a state where the sample S is arranged at the measurement position. The sample chamber 51 is provided so that the pressure can be reduced. The sample chamber 51 is provided so that a desired gas can be introduced.
　第１部分５１１は、測定位置の周辺に設けられている。第１部分５１１は、たとえば、上記第２主面５３ｂの法線方向に平行な筒軸Ｃを有する筒状部材である。第１部分５１１は、筒軸Ｃ方向の一端側が試料ステージ５３に閉塞されるように第２主面５３ｂ上に設けられている。第１部分５１１は、鉄板およびＳＵＳ等のＸ線を遮蔽可能な部材によって構成されている。 The first portion 511 is provided around the measurement position. The first portion 511 is, for example, a cylindrical member having a cylindrical axis C parallel to the normal line direction of the second main surface 53b. The first portion 511 is provided on the second main surface 53 b such that one end side in the cylinder axis C direction is closed by the sample stage 53. The first portion 511 is configured by a member capable of shielding X-rays such as an iron plate and SUS.
　筒軸Ｃ方向の第１部分５１１の他端（上端）には、溝部が設けられており、当該溝部内にシール部材５１３が配置されている。シール部材５１３は、試料室５１内を気密に維持するための部材である。シール部材５１３は、たとえば、弾性を有するゴム部材によって構成されている。 溝 A groove is provided at the other end (upper end) of the first portion 511 in the direction of the cylinder axis C, and a seal member 513 is arranged in the groove. The seal member 513 is a member for keeping the inside of the sample chamber 51 airtight. The seal member 513 is made of, for example, a rubber member having elasticity.
　第２部分５１２は、搬送部２０に設けられている。具体的には、第２部分５１２は、アーム部２５に設けられている。第２部分５１２は、第１部分５１１に当接可能に設けられている。第２部分５１２は、測定位置に試料Ｓが配置された状態で第１部分５１１に当接する。これにより、試料室５１が形成された状態となる。 The second part 512 is provided in the transport unit 20. Specifically, the second portion 512 is provided on the arm 25. The second portion 512 is provided so as to be in contact with the first portion 511. The second part 512 contacts the first part 511 in a state where the sample S is arranged at the measurement position. As a result, the sample chamber 51 is formed.
　第２部分５１２は、上記筒軸Ｃ方向における第１部分５１１の他端側から第１部分５１１に対向可能に設けられている。第２部分５１２は、筒軸Ｃ方向における第１部分５１１の他端側を閉塞可能に設けられた蓋部材である。第２部分５１２は、測定位置に試料Ｓが配置された状態で第１部分５１１の他端側を閉塞する。第２部分５１２は、鉄板およびＳＵＳ等のＸ線を遮蔽可能な部材によって構成されている。 The second portion 512 is provided so as to be able to face the first portion 511 from the other end of the first portion 511 in the direction of the cylinder axis C. The second part 512 is a lid member provided so as to be able to close the other end of the first part 511 in the direction of the cylinder axis C. The second portion 512 closes the other end of the first portion 511 in a state where the sample S is arranged at the measurement position. The second portion 512 is configured by a member capable of shielding X-rays such as an iron plate and SUS.
　照射室５２には、Ｘ線照射部３０および検出器４０が設けられている。照射室５２は、減圧可能に設けられている。また、照射室５２は、所望のガスを導入可能に設けられている。 The irradiation room 52 is provided with the X-ray irradiation unit 30 and the detector 40. The irradiation chamber 52 is provided so as to be able to reduce the pressure. The irradiation chamber 52 is provided so that a desired gas can be introduced.
　制御部６０は、搬送部２０の動作、Ｘ線照射部３０および検出器４０の動作等のＸ線分析装置１の動作を制御する。 The control unit 60 controls the operation of the X-ray analyzer 1, such as the operation of the transport unit 20, the operations of the X-ray irradiation unit 30 and the detector 40.
　（搬送部の搬送動作およびＸ線分析）
　待機位置に位置する試料Ｓを測定位置に移動させる場合には、まず、待機位置に位置する試料Ｓの上方に把持部２６を移動させる。具体的には、試料Ｓの上方に把持部２６が位置するように、移動体２４、Ｘ軸レール２１およびアーム部２５をそれぞれ、Ｘ軸方向、Ｙ軸方向およびＺ軸方向に移動させる。 (Transport operation of transport unit and X-ray analysis)
When moving the sample S located at the standby position to the measurement position, first, the gripper 26 is moved above the sample S located at the standby position. Specifically, the moving body 24, the X-axis rail 21, and the arm 25 are moved in the X-axis direction, the Y-axis direction, and the Z-axis direction such that the gripper 26 is positioned above the sample S.
　続いて、試料Ｓに近づけるように把持部２６を移動させる。具体的には、Ｚ軸レール２３に沿ってアーム部２５を試料Ｓ側に移動させる。試料Ｓに把持部２６を当接させて、試料Ｓを把持する。 Next, the gripper 26 is moved so as to approach the sample S. Specifically, the arm 25 is moved to the sample S side along the Z-axis rail 23. The sample S is held by bringing the holding unit 26 into contact with the sample S.
　次に、試料Ｓを把持した状態で測定位置の上方に把持部２６を移動させる。具体的には、測定位置の上方に把持部２６が位置するように、移動体２４、Ｘ軸レール２１およびアーム部２５をそれぞれ、Ｘ軸方向、Ｙ軸方向、およびＺ軸方向に移動させる。これにより、アーム部２５に設けられた第２部分５１２が、第１部分５１１の上方に位置することとなり、第２部分５１２が、第１部分５１１の他端側（上端側）から第１部分５１１に対向する。 Next, the gripper 26 is moved above the measurement position while holding the sample S. Specifically, the moving body 24, the X-axis rail 21, and the arm 25 are moved in the X-axis direction, the Y-axis direction, and the Z-axis direction, respectively, so that the grip unit 26 is positioned above the measurement position. Thus, the second portion 512 provided on the arm portion 25 is located above the first portion 511, and the second portion 512 is moved from the other end (upper end) of the first portion 511 to the first portion. 511.
　続いて、試料ステージ５３の第２主面５３ｂの法線方向に沿って把持部２６を第２主面５３ｂに近づけるように移動させる。なお、上記法線方向は、Ｚ軸方向に一致する。把持部２６で把持された試料Ｓが測定位置に到達するまで、把持部２６を第２主面５３ｂに近づける。具他的には、試料Ｓが測定位置に到達するように、アーム部２５をＺ軸方向に沿って移動させる。この場合には、試料Ｓは、第２主面５３ｂ上に載置されることが好ましい。 Next, the gripper 26 is moved along the normal direction of the second main surface 53b of the sample stage 53 so as to approach the second main surface 53b. The normal direction coincides with the Z-axis direction. Until the sample S gripped by the gripper 26 reaches the measurement position, the gripper 26 is brought closer to the second main surface 53b. Specifically, the arm 25 is moved along the Z-axis direction so that the sample S reaches the measurement position. In this case, the sample S is preferably mounted on the second main surface 53b.
　試料Ｓが測定位置に配置された状態においては、第２部分５１２が第１部分５１１の他端側を閉塞する。これにより、試料室５１が形成された状態となる。この状態においては、試料室５１の内部に把持部２６および試料Ｓが収容される。 In the state where the sample S is placed at the measurement position, the second portion 512 closes the other end of the first portion 511. As a result, the sample chamber 51 is formed. In this state, the holding section 26 and the sample S are accommodated inside the sample chamber 51.
　試料Ｓが測定位置に配置されることにより、Ｘ線分析が可能となる。分析を行なう場合には、Ｘ線照射部３０から１次Ｘ線を測定位置に配置された試料Ｓに照射し、試料Ｓから発生した蛍光Ｘ線を検出器４０にて検出する。 Ｘ X-ray analysis becomes possible by placing the sample S at the measurement position. When performing analysis, primary X-rays are emitted from the X-ray irradiator 30 to the sample S arranged at the measurement position, and the fluorescent X-rays generated from the sample S are detected by the detector 40.
　１次Ｘ線を試料Ｓに照射する際には、把持部２６および試料Ｓが第１部分５１１および第２部分５１２によって覆われている。これにより、分析時に試料Ｓを透過したＸ線の一部が第１部分５１１および第２部分５１２によって遮蔽される。これにより、Ｘ線が試料室５１の外部に漏れ出ることを抑制することができる。 (4) When irradiating the sample S with the primary X-ray, the grip portion 26 and the sample S are covered by the first portion 511 and the second portion 512. Thereby, a part of the X-ray transmitted through the sample S during the analysis is shielded by the first portion 511 and the second portion 512. Thus, it is possible to suppress the X-ray from leaking out of the sample chamber 51.
　また、１次Ｘ線を試料Ｓに照射する際には、把持部２６が測定位置にて試料Ｓを把持した状態を維持していてもよい。この場合には、測定時に測定位置で試料Ｓを把持部２６から取り外すことを省略することができる。これに伴い、測定位置で取り外された試料Ｓを再度把持部２６で把持したりすることも省略することができる。この結果、試料Ｓを移動させるための時間を短縮することができる。 (4) When irradiating the sample S with the primary X-ray, the state where the gripper 26 grips the sample S at the measurement position may be maintained. In this case, removing the sample S from the grip portion 26 at the measurement position during measurement can be omitted. Along with this, it is also possible to omit again holding the sample S removed at the measurement position by the holding unit 26. As a result, the time for moving the sample S can be reduced.
　なお、測定位置において把持部２６による試料Ｓの把持を解除してもよい。この場合には、測定時に搬送部２０側から振動が試料Ｓに伝達されることを防止することができる。 Note that the gripping of the sample S by the gripper 26 may be released at the measurement position. In this case, it is possible to prevent the vibration from being transmitted to the sample S from the transport unit 20 side during the measurement.
　さらに、１次Ｘ線を試料Ｓに照射する際には、試料Ｓを把持した状態で、試料Ｓの分析面Ｓａに垂直な回転軸まわりに把持部２６を回転させてもよい。この場合には、測定位置にて試料Ｓを回転させることができるため、周方向に試料Ｓを分析することができる。また、モータ等の駆動源でアーム部２５を回転させるため、回転機構も簡素化することができる。 (4) When irradiating the sample S with primary X-rays, the gripper 26 may be rotated about a rotation axis perpendicular to the analysis surface Sa of the sample S while the sample S is gripped. In this case, since the sample S can be rotated at the measurement position, the sample S can be analyzed in the circumferential direction. Further, since the arm 25 is rotated by a driving source such as a motor, the rotation mechanism can be simplified.
　分析が終了すると、測定位置から待機位置に試料Ｓを移動させる。具体的には、測定位置に配置された試料Ｓを把持した状態で把持部２６を試料ステージ５３の第２主面５３ｂから遠ざかるように、第２主面５３ｂの法線方向に沿って移動させる。具体的には、第２主面５３ｂから遠ざかるように、アーム部２５をＺ軸方向に移動させる。 (5) When the analysis is completed, the sample S is moved from the measurement position to the standby position. Specifically, the gripper 26 is moved along the normal direction of the second main surface 53b so as to move away from the second main surface 53b of the sample stage 53 while holding the sample S arranged at the measurement position. . Specifically, the arm 25 is moved in the Z-axis direction so as to move away from the second main surface 53b.
　続いて、試料Ｓが待機位置に位置するように、移動体２４、およびＸ軸レール２１およびアーム部２５をそれぞれ、Ｘ軸方向、Ｙ軸方向、およびＺ軸方向に移動させる。待機位置にて把持部２６による試料Ｓの把持を解除する。次に、把持部２６を所定の位置に移動させる。 Next, the moving body 24, the X-axis rail 21, and the arm 25 are moved in the X-axis direction, the Y-axis direction, and the Z-axis direction so that the sample S is located at the standby position. The holding of the sample S by the holding unit 26 is released at the standby position. Next, the gripper 26 is moved to a predetermined position.
　上記のような搬送動作を繰り返し行うことにより、複数の試料Ｓを分析することができる。 繰 り 返 し By repeatedly performing the above-described transport operation, a plurality of samples S can be analyzed.
　（その他の変形例）
　上述の実施の形態においては、試料ステージ５３を設け、分析時に試料ステージ５３に試料Ｓを載置する場合を例示して説明したが、これに限定されない。把持部２６が試料Ｓを測定位置で把持した状態を維持でき、この状態で１次Ｘ線を試料Ｓに照射できる限り、試料ステージ５３を省略してもよい。試料ステージ５３に試料を載置してＸ線分析を行なう場合には、試料Ｓを精度よく測定することができる。 (Other modifications)
In the above-described embodiment, the case where the sample stage 53 is provided and the sample S is mounted on the sample stage 53 at the time of analysis has been described as an example. However, the present invention is not limited to this. The sample stage 53 may be omitted as long as the gripper 26 can maintain the state where the sample S is gripped at the measurement position and the primary X-ray can be irradiated on the sample S in this state. When the sample is placed on the sample stage 53 and X-ray analysis is performed, the sample S can be measured with high accuracy.
　上述の実施の形態においては、試料室５１を構成する第１部分５１１が筒状部材であり、第２部分５１２が筒状部材の他端側を閉塞可能に設けられた蓋部材である場合を例示して説明したが、これに限定されない。第２部分５１２をＸＹＺ軸方向の少なくともいずれかに沿って移動させて第１部分５１１に当接させた状態において試料室５１が形成される限り、第１部分５１１および第２部分５１２の形状は、適宜選択することができる。 In the above-described embodiment, a case where the first portion 511 constituting the sample chamber 51 is a tubular member and the second portion 512 is a lid member provided so as to be able to close the other end of the tubular member. Although illustrated and described, the present invention is not limited to this. As long as the sample chamber 51 is formed in a state where the second portion 512 is moved along at least one of the XYZ axis directions and is in contact with the first portion 511, the shapes of the first portion 511 and the second portion 512 are Can be appropriately selected.
　なお、上記のように、第１部分５１１を、一端側が試料ステージ５３によって閉塞された筒状部材とし、第２部分５１２を、第１部分５１１の他端側を閉塞可能に設けられた蓋部材とすることにより、試料室５１の構成を簡素化することができる。さらに、試料ステージ５３の第２主面５３ｂの法線方向に把持部２６を移動させることにより試料室５１を形成することができるため、試料室５１を形成するための搬送部２０の動作をシンプルにすることができる。 As described above, the first portion 511 is a cylindrical member whose one end is closed by the sample stage 53, and the second portion 512 is a lid member provided so that the other end of the first portion 511 can be closed. By doing so, the configuration of the sample chamber 51 can be simplified. Further, since the sample chamber 51 can be formed by moving the gripping section 26 in the direction of the normal to the second main surface 53b of the sample stage 53, the operation of the transfer section 20 for forming the sample chamber 51 can be simplified. Can be
　以上、本発明の実施の形態について説明したが、今回開示された実施の形態はすべての点で例示であって制限的なものではない。本発明の範囲は請求の範囲によって示され、請求の範囲と均等の意味および範囲内でのすべての変更が含まれる。 Although the embodiments of the present invention have been described above, the embodiments disclosed herein are illustrative in all aspects and not restrictive. The scope of the present invention is defined by the appended claims, and includes all modifications within the scope and meaning equivalent to the appended claims.
　１　Ｘ線分析装置、２　筐体、１０　試料支持部、２０　搬送部、２１　Ｘ軸レール、２２　Ｙ軸レール、２３　Ｚ軸レール、２４　移動体、２５　アーム部、２６　把持部、２７　回転駆動部、３０　Ｘ線照射部、４０　検出器、５０　分析チャンバ、５１　試料室、５２　照射室、５３　試料ステージ、５３ａ　第１主面、５３ｂ　第２主面、６０　制御部、５１１　第１部分、５１２　第２部分、５１３　シール部材、Ｃ　筒軸、Ｓ　試料、Ｓａ　分析面。 1 X-ray analyzer, 2 housing, 10 sample support unit, 20 transport unit, 21 軸 X-axis rail, 22 Y-axis rail, 23 Z-axis rail, 24 moving body, 25 arm unit, 26 grip unit, 27 rotation drive unit , 30 ° X-ray irradiation unit, 40 ° detector, 50 ° analysis chamber, 51 ° sample chamber, 52 ° irradiation chamber, 53 ° sample stage, 53a {first main surface, 53b} second main surface, 60 ° control unit, 511 first part, 512 ° first 2 parts, 513 sealing member, C cylinder shaft, S sample, Sa analysis surface.

Claims (4)

  1. 　各待機位置に配置された複数の試料を支持する試料支持部と、
    　前記試料を把持する把持部を有し、前記各待機位置と測定位置との間で前記試料を移動させる搬送部と、
    　前記測定位置に配置された前記試料に向けて１次Ｘ線を照射するＸ線照射部と、
    　前記１次Ｘ線を照射された前記試料から発生する蛍光Ｘ線を検出する検出器と、
    　分離可能に設けられた第１部分および第２部分を含み、前記測定位置に前記試料が配置された状態で前記試料および前記把持部を収容することとなる試料室と、を備え、
    　前記第１部分は、前記測定位置の周辺に設けられており、
    　前記第２部分は、前記搬送部に設けられており、
    　前記測定位置に前記試料が配置された状態において、前記第２部分が前記第１部分に当接することにより前記試料室が形成された状態となる、Ｘ線分析装置。     A sample support unit that supports a plurality of samples arranged at each standby position,
    A transport unit that has a gripper that grips the sample, and that moves the sample between each of the standby positions and the measurement position,
    An X-ray irradiator that irradiates primary X-rays toward the sample disposed at the measurement position;
    A detector for detecting fluorescent X-rays generated from the sample irradiated with the primary X-rays;
    A sample chamber that includes a first part and a second part that are separably provided, and that stores the sample and the grip in a state where the sample is arranged at the measurement position,
    The first portion is provided around the measurement position,
    The second portion is provided in the transport unit,
    An X-ray analyzer, wherein the sample chamber is formed by the second portion abutting on the first portion in a state where the sample is arranged at the measurement position.
  2. 　前記測定位置において前記試料を載置させるための試料ステージをさらに備え、
    　前記試料ステージは、前記Ｘ線照射部および前記検出器側を向く第１主面と、前記第１主面の反対側に位置し、前記試料が載置される第２主面とを有し、
    　前記把持部は、前記第２主面に垂直な法線方向に移動可能に設けられ、
    　前記第１部分は、前記法線方向に平行な筒軸を有し、前記筒軸方向における一端側が前記試料ステージによって閉塞されるように前記第２主面上に設けられた筒状部材であり、
    　前記第２部分は、前記筒軸方向における前記筒状部材の他端側から前記筒状部材に対向可能に設けられた蓋部材であり、
    　前記把持部が前記法線方向に沿って前記第２主面に近づくように移動して前記測定位置に前記試料が配置された状態で、前記蓋部材が前記筒状部材の前記他端側を閉塞することにより、前記試料室が形成された状態となる、請求項１に記載のＸ線分析装置。     Further comprising a sample stage for mounting the sample at the measurement position,
    The sample stage has a first main surface facing the X-ray irradiator and the detector side, and a second main surface located opposite to the first main surface and on which the sample is placed. ,
    The grip is provided to be movable in a normal direction perpendicular to the second main surface,
    The first portion has a cylindrical axis parallel to the normal direction, and is a cylindrical member provided on the second main surface such that one end side in the cylindrical axis direction is closed by the sample stage. ,
    The second portion is a lid member provided so as to be able to face the cylindrical member from the other end side of the cylindrical member in the cylindrical axis direction,
    In a state where the gripping part moves along the normal direction to approach the second main surface and the sample is placed at the measurement position, the lid member closes the other end side of the cylindrical member. The X-ray analyzer according to claim 1, wherein the sample chamber is formed by closing the sample chamber.
  3. 　前記把持部は、前記測定位置にて前記試料を把持した状態を維持し、
    　前記Ｘ線照射部は、前記把持部に把持された前記試料に向けて前記１次Ｘ線を照射する、請求項１または２に記載のＸ線分析装置。     The gripper maintains a state where the sample is gripped at the measurement position,
    The X-ray analyzer according to claim 1, wherein the X-ray irradiator irradiates the primary X-ray toward the sample held by the holding unit.
  4. 　前記把持部は、前記試料の分析面に垂直な回転軸まわりに回転可能に設けられている、請求項１から３のいずれか１項に記載のＸ線分析装置。 4. The X-ray analyzer according to claim 1, wherein the grip is rotatably provided around a rotation axis perpendicular to an analysis surface of the sample. 5.
PCT/JP2018/031550 2018-08-27 2018-08-27 X-ray analysis device WO2020044399A1 (en)

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DE112022003111T5 (en) 2021-07-29 2024-04-11 Shimadzu Corporation ANALYSIS SYSTEM, ANALYSIS DEVICE AND CONTROL METHOD

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TWI725511B (en) 2021-04-21
TW202022364A (en) 2020-06-16

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