JP2010286346A - Spectroscope - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a spectrometer of wavelength dispersion type that has a simple structure, able to have a small work region, and has a wide wavelength scanning range. <P>SOLUTION: This spectroscope includes: a spectral element 52 for diffracting electromagnetic wave, showing the characteristics of a sample 43 released from the sample 43; spectral element rotating mechanisms (61-1 and 62-1) making the spectral element 52 rotate about the surface of the spectral element 52 as the axis; a plurality of detectors 53-1, 53-2, ..., and 53-n for detecting the electromagnetic waves diffracted by the spectral element 52 in respective different regions; and detector-rotating mechanisms (61-2 and 62-2) that share a rotating shaft with the spectral element rotating mechanisms (61-1 and 62-1) and make the plurality of detectors move around the spectral element 52. The plurality of detectors can be switched by changing the offset angle of the detector-rotating mechanisms (61-2 and 62-2). <P>COPYRIGHT: (C)2011,JPO&INPIT

Description

  The present invention relates to a wavelength dispersion type spectrometer such as an electronic probe microanalyzer (EPMA).

  In the Johansson type spectrometer, as shown in FIG. 16, the crystal lattice plane of the spectroscopic element 12e is curved to a radius of curvature 2R which is twice the radius R of the Roland circle Q, and the surface shape of the spectroscopic element 12e is It is ground to have a curvature equal to the radius R. From the theorem where the circumference angle is constant, if the excitation beam irradiation site 10e of the sample 11e is one focal point, the excitation beam irradiation site 10e, the spectroscopic surface of the spectroscopic element 12e, and the detection point by the detector 13e are If positioned above, the diffracted X-ray from the spectroscopic element 12e is focused at a detection point by the detector 13e. The Johansson type spectroscope needs to be designed so that three points including the excitation beam irradiation site 10e can always be arranged on the Roland circle Q, and the radius of the Roland circle Q is determined by the spectroscopic element 12e. The distance between the sample 11e and the spectroscopic element 12e cannot be selected freely. For this reason, it is necessary to design a spectrometer including the position of the excitation beam irradiation site 10e, and it is difficult to newly install a Johansson type spectrometer in an existing analyzer. Further, since it is necessary to control the positions of the spectroscopic element 12e and the detector 13e, the apparatus becomes complicated and the size increases.

  On the other hand, as shown in FIG. 17, the characteristic X-rays emitted from the excitation beam irradiation site 10f of the sample 11f are converted into parallel beams by using a polycapillary lens 15f, and are spectrally separated by a flat plate type spectroscopic element 12f. A method has been devised in which analysis is performed by making it incident on (see Patent Document 1). In this method, it is not necessary to focus on the detection point of the detector 13f, the spectroscopic element 12f is rotated around the X-ray irradiation site 120f on the spectroscopic element 12f, and the detector 13f is interlocked with the rotation of the spectroscopic element 12f. Therefore, the structure of the apparatus can be reduced in size. Further, the distance from the polycapillary lens 15f to the spectroscopic element 12f can be arbitrarily set, and it is relatively easy to newly install a spectroscope of the type shown in FIG. 17 in an existing analyzer.

  In the case of the wavelength dispersion type X-ray spectrometer as described above, a plurality of spectral crystals having different wavelength ranges that can be dispersed are mounted on one spectrometer, and the wavelength range that can be dispersed is widened by switching them. However, in order to analyze a wider wavelength range with a single spectroscope, it is necessary to mount a plurality of detectors having different detectable wavelength ranges and switch them to use.

JP 2004-294168 A JP 2008-026251 A

  However, since a complicated structure is required for switching the detector, a practically usable spectrometer configuration that can be reduced in size has not been proposed yet.

  An object of the present invention is to provide a wavelength-dispersion spectroscope that can reduce the work area with a simple structure and has a wide wavelength scanning range.

  In order to achieve the above object, the first aspect of the present invention includes (a) a spectroscopic element that diffracts an electromagnetic wave exhibiting characteristics of a sample emitted from the sample, and (b) the spectroscopic element on the surface of the spectroscopic element. (C) a plurality of detectors that detect electromagnetic waves diffracted by the spectroscopic element in different wavelength regions, and (d) a spectroscopic element rotation mechanism that shares a rotation axis, And a detector rotating mechanism that moves the detector around the spectroscopic element, and the gist is that the plurality of detectors can be switched by changing the offset angle of the detector rotating mechanism.

  The second aspect of the present invention includes (a) a spectroscopic element that diffracts an electromagnetic wave exhibiting characteristics of a sample emitted from the sample, and (b) a spectroscopic element rotation that rotates the spectroscopic element around the surface of the spectroscopic element. A mechanism, (c) a plurality of detectors that detect electromagnetic waves diffracted by the spectroscopic elements in different wavelength regions, and (d) a spectroscopic element rotation mechanism that shares a rotation axis and is equipped with any of the plurality of detectors And a plurality of detector rotation mechanisms that move around the spectroscopic element, and a plurality of detector rotation mechanisms can be switched to switch the plurality of detectors.

  According to the present invention, a work area can be reduced with a simple structure, and a wavelength dispersion type spectrometer having a wide wavelength scanning range can be provided.

It is a block diagram which shows the fundamental structure of the analyzer which used the spectrometer which concerns on the 1st Embodiment of this invention. It is a schematic diagram explaining an example of a structure of a lens part used for the analyzer which used the spectrometer which concerns on the 1st Embodiment of this invention. It is a schematic diagram explaining the structure of the polycapillary lens which concerns on the 1st Embodiment of this invention. It is a schematic diagram explaining an example of a structure of the rotary body drive part which concerns on the 1st Embodiment of this invention. It is a schematic diagram explaining the viewing angle and diffraction angle in the spectrometer which concerns on the 1st Embodiment of this invention. It is a block diagram which shows the outline of a logic structure of the detector switching means based on the 1st Embodiment of this invention. It is a flowchart explaining the analysis method which concerns on the 1st Embodiment of this invention. It is a schematic diagram explaining the offset angle between two detectors used for the analysis method which concerns on the 1st Embodiment of this invention. In the analysis method which concerns on the 1st Embodiment of this invention, it is a schematic diagram explaining a mode that X-ray | X_line is detected with the 1st detector before switching. In the analysis method which concerns on the 1st Embodiment of this invention, it is a schematic diagram explaining a mode that a 2nd detector after switching detects an X-ray. It is a block diagram which shows the basic structure of the analyzer which used the spectrometer which concerns on the 2nd Embodiment of this invention. It is a block diagram which shows the basic structure of the analyzer which used the spectrometer which concerns on the 3rd Embodiment of this invention. It is a schematic diagram explaining the basic structure of the spectrometer which concerns on the 3rd Embodiment of this invention. It is a block diagram which shows the outline of a logic structure of the detector switching means based on the 3rd Embodiment of this invention. It is a schematic diagram which shows an example of the excitation ray source and lens part of the analyzer which used the spectrometer which concerns on other embodiment of this invention. It is a basic schematic diagram for explaining a conventional Johansson type spectroscope. It is a schematic diagram explaining the spectrometer using a polycapillary lens.

  Next, first to third embodiments of the present invention will be described with reference to the drawings. In the following description of the drawings, the same or similar parts are denoted by the same or similar reference numerals. However, it should be noted that the drawings are schematic, and the relationship between thickness and planar dimensions, the configuration of the apparatus, and the like are different from the actual ones. Therefore, specific thicknesses and dimensions should be determined in consideration of the following description. Moreover, it is a matter of course that portions having different dimensional relationships and ratios are included between the drawings. The first to third embodiments shown below exemplify apparatuses and methods for embodying the technical idea of the present invention, and the technical idea of the present invention is The material, shape, structure, arrangement, etc. are not specified below. The technical idea of the present invention can be variously modified within the technical scope described in the claims.

(First embodiment)
As an analysis apparatus using the spectroscope according to the first embodiment of the present invention, as shown in FIG. 1, an analysis unit 4 for analyzing X-rays emitted from a sample 43 and various operations of the analysis unit 4 An electronic probe microanalyzer (EPMA) provided with a control analysis device 2 that controls and analyzes and manages data obtained from the analysis unit 4 will be described as an example.

  As shown in FIG. 1, the analysis unit 4 is located between an excitation beam source (electron gun) 41 that emits an excitation beam (electron beam) E toward the sample 43, and between the excitation beam source 41 and the sample 43. A lens unit 42 that focuses and scans the excitation line E on the sample 43, a stage unit 44 that holds and moves the sample 43, and X-rays emitted from the sample 43 irradiated with the excitation line E are spectroscopically detected. The spectroscope 5 is provided. For example, as shown in FIG. 2, the lens unit 42 includes electronic lenses such as a focusing lens 421, a deflection coil 422, and an objective lens 423. The focusing lens 421 and the objective lens 423 focus the excitation line E on the sample 43, and the deflection coil 422 bends the irradiation direction of the excitation line E and scans the excitation line E on the sample 43.

  The excitation line E passes through the magnetic field formed by the lens unit 42, converges to a minute diameter, and irradiates the excitation line irradiation site 430 of the sample 43 placed on the stage unit 44. Since X-rays indicating the characteristics of the sample 43 are emitted from the excitation beam irradiation site 430 of the sample 43 to the surroundings, the sample 43 is emitted from the excitation beam irradiation site 430 above the vicinity of the sample 43 as shown in FIG. A spectrometer 5 that disperses X-rays is installed. The stage unit 44 is moved in the horizontal direction by a driving mechanism (not shown) so that the irradiation position of the excitation beam E can be scanned at the excitation beam irradiation site 430 on the sample 43.

  The spectroscope 5 according to the first embodiment includes a spectroscopic element 52 that diffracts an electromagnetic wave indicating the characteristics of the sample 43 emitted from the sample 43, and rotates the spectroscopic element 52 around the surface of the spectroscopic element 52 as an axis. A spectroscopic element rotating mechanism (61-1, 62-1) and a plurality of detectors 53-1, 53-2,..., 53-n that detect electromagnetic waves diffracted by the spectroscopic element 52 in different wavelength regions, respectively. , Detectors that share the rotation axis with the spectroscopic element rotating mechanism (61-1, 62-1) and move the plurality of detectors 53-1, 53-2,..., 53-n around the spectroscopic element 52 And a plurality of detectors 53-1, 53-2,... By changing the offset angle of the detector rotation mechanism (61-2, 62-2). 53-n can be switched. As shown in FIG. 1, the spectroscopic element rotating mechanism (61-1, 62-1) includes a disk-shaped first rotating body 61-1 and a first rotation for rotating the first rotating body 61-1. A body drive mechanism 62-1. The detector rotating mechanism (61-2, 62-2) includes a second rotating body 61-2 and a second rotating body driving mechanism 62-2 that rotates the second rotating body 61-2. The first rotating body 61-1 and the second rotating body 61-2 share a rotating shaft 60 that passes through the center of the goniometer circle formed by the first rotating body 61-1 and is perpendicular to the paper surface. Rotate.

  That is, the spectroscope 5 according to the first embodiment includes a polycapillary lens 51 that converts the X-rays emitted from the excitation beam irradiation region 430 into a parallel beam, the first rotating body 61-1, and the first rotation. A goniometer device 6 having a second rotating body 61-2 having a radius larger than that of the body 61-1, a spectroscopic element 52 mounted at the center of the first rotating body 61-1, and a second rotating body 61-. 2 detectors 53-1, 53-2,..., 53-n provided on the circumference side of 2 and having different wavelength ranges of X-rays that can be detected (n is an integer of 2 or more). With.

  As shown in FIG. 3, the polycapillary lens 51 bundles about 100 to 1 million glass capillaries (capillaries) having an inner diameter of about 1 to 100 μm, and each capillary is directed to the focal point F on one end side. The other end side is an optical element configured such that individual capillaries are parallel to each other. X-rays emitted from the excitation beam irradiation site 430 of the sample 43 pass through the individual capillaries of the polycapillary lens 51 installed so that the excitation beam irradiation site 430 coincides with the focal point F, and pass through in parallel. And forms a parallel beam of X-rays on the other end side.

    For example, as shown in FIG. 4, the first rotating body drive mechanism 62-1 meshes with an actuator 621 such as a stepping motor and a servo motor, a worm (screw gear) 622 rotated by the actuator 621, and a worm 622. A worm wheel (helical gear) 623 provided in a ring shape around the first rotating body 61-1 can be used. The same applies to the second rotating body driving mechanism 62-2, and the first rotating body driving mechanism 62-1 and the second rotating body driving mechanism 62-2 can be driven independently. The power transmission mechanism of the first rotating body driving mechanism 62-1 and the second rotating body driving mechanism 62-2 is not limited to the worm gear, but the first rotating body 61-1 and the second rotating body 61. Other gear sets, belts, pulleys, chains, sprockets, etc. may be used as long as the -2 can be controlled with high precision, and a direct drive system that does not use a power transmission mechanism is used. It doesn't matter.

  The goniometer device 6 incorporates an angle detector such as a rotary encoder (not shown), and can detect the rotation angle from the reference point of the first rotating body 61-1 and the second rotating body 61-2. The angle information detected by the angle detector of the goniometer device 6 is converted into a signal and input to the control analysis device 2.

  The spectroscopic element 52 used for the spectroscope 5 according to the first embodiment is a flat plate type, and the surface of the spectroscopic element 52 includes the rotation shaft 60 with respect to the rotation surface of the first rotating body 61-1. It is mounted with the surface vertical. The spectroscopic element 52 includes lithium fluoride (LiF), lithium tantalate (LiTaO3), rubidium phthalate (RAP), thallium phthalate (TAP), pentaerythritol (PET), artificial superlattice spectroscopic element (LDE), phosphoric acid 2 It can be switched by appropriately selecting from various known crystals such as ammonium hydrogen (ADP),. For example, the spectroscopic element 52 may be configured such that a crystal is attached to each side surface of a quadrangular prism or a hexagonal prism, a mechanism that rotates with respect to the central axis of the prism is provided, and a crystal used for spectroscopy is switched by rotating the prism. Good. The direction of the axis of the prism may be perpendicular to or parallel to the first rotating body 61-1 as long as the surface of the crystal used for spectroscopy can be mounted so as to include the rotating shaft 60. X-rays converted into parallel beams by the polycapillary lens 51 are emitted from the polycapillary lens 51 toward the surface of the spectroscopic element 52. The viewing angle θ, which is the remainder of the incident angle on the spectroscopic element 52, is changed by controlling the angle of the surface of the spectroscopic element 52 with respect to the axial direction of the polycapillary lens 51 by the rotation of the first rotating body 61-1.

  The plurality of detectors 53-1 to 53-n have their respective detection directions directed to the rotation shaft 60, have a predetermined offset angle between them, and do not interfere with each other with the second rotating body 61-2. Has been placed. As long as the detectors 53-1 to 53-n do not interfere with each other, the number of the detectors 53-1 to 53-n may be any number. The X-rays converted into parallel beams by the polycapillary lens 51 are diffracted by the spectroscopic element 52, pass through a light receiving slit (not shown), and detected by any one of a plurality of detectors 53-1 to 53-n. Therefore, it goes without saying that the polycapillary lens 51, the spectroscopic element 52, and the detectors 53-1 to 53-n are located on the same plane with the direction of the rotation shaft 60 as the normal direction.

  For example, in the case of performing wavelength scanning using the spectroscopic element 52, the detector 53-1, as shown in FIG. 5, when the angle of incidence on the spectroscopic element 52 is θ, It is moved by the rotation of the second rotating body 61-2 so that the angle between the direction and the direction of the diffracted wave (hereinafter referred to as the diffraction angle) becomes 2θ. That is, the rotation of the spectroscopic element 52 installed in the first rotating body 61-1 for setting the viewing angle θ and the detector 53-1 installed in the second rotating body 61-2 linked to this rotation. By controlling the diffraction angle 2θ and maintaining the double angle relationship, the Bragg diffraction condition is satisfied.

  The detectors 53-1 to 53-n are, for example, scintillation counters, gas flow proportional counters (FPC), igzatron detectors, semiconductor detectors such as Ge and CdZnTe, etc., depending on the wavelength of the X-rays to be measured. May be used.

  The detection signals from the detectors 53-1 to 53-n are, for example, an X-ray spectrum corresponding to wavelength scanning is created by signal processing in the control analysis device 2, and further qualitative analysis and quantitative analysis based on this are possible. . It is also possible to create an element content distribution (mapping) image on the sample 43 in accordance with the position scanning by the excitation line E or the stage unit 44.

  As shown in FIG. 1, the control analysis device 2 includes a CPU (central processing unit) 3, a program storage device 25, a wavelength information storage device 26, an angle information storage device 27, an analysis information storage device 28, an input device 22, and an output device. 23, the display device 24, the input / output control unit 21 and the like, and the hardware configuration of the Neumann computer is formed.

  The program storage device 25 of the control analysis device 2 stores a series of programs necessary for controlling the analysis unit 4. The wavelength information storage device 26 stores a wavelength range of X-rays that can be detected by each of the detectors 53-1 to 53-n and a wavelength range in which wavelength scanning can be performed by the used spectral element 52. To do. In the angle information storage device 27, as information required when the detectors 53-1 to 53-n are switched, the visual angle θ before and after the switching, the diffraction angle 2θ, and the detectors 53-1 to 53-n are arranged. Stores the angle difference and the like. The analysis information storage device 28 stores analysis conditions, analysis conditions such as the spectroscopic element 52, detectors 53-1 to 53-n used for analysis, as well as information such as analysis results when analyzed, analysis date and time, and the like. .

  The input device 22, the output device 23, and the display device 24 perform data transmission / reception with the CPU 3 via the input / output control unit 21. In FIG. 1, the input device 22 includes a keyboard, a mouse, a light pen, and the like. The analysis practitioner sets the analysis conditions such as the element to be analyzed, the type of the spectroscopic element 52, the scanning wavelength range by the plurality of detectors 53-1 to 53-n, the step width at the time of wavelength scanning, and the like. Can be done. Furthermore, it is also possible to perform an analysis stop command, correction of each set condition, and the like from the input device 22. The output device 23 and the display device 24 can be configured by a printer device, a display device, and the like, respectively. The display device 24 can display an analysis condition setting screen, an analysis result screen, and the like.

  The CPU (central processing unit) 3 of the control analyzer 2 operates an excitation source control unit 31 that controls the operation of the excitation source 41, a lens unit control unit 32 that controls the operation of the lens unit 42, and an operation of the stage unit 44. Stage control means 33 for controlling the detection signals, detection signal processing means 34 for processing the detection signals from the detectors 53-1 to 53-n, and detector switching means 35 for controlling the switching of the detectors 53-1 to 53-n. Etc. as a logical structure. As shown in FIG. 6, details of the detector switching means 35 are goniometer device control means for controlling the driving of the first rotating body driving mechanism 62-1 and the second rotating body driving mechanism 62-2 of the goniometer device 6. 351, drive amount processing means 352 for calculating the drive amount (rotation angle) of the goniometer device 6 required when the detectors 53-1 to 53-n are switched, and drive control of the detectors 53-1 to 53-n Detector control means 353 for performing

  Note that the program storage device 25, the wavelength information storage device 26, the angle information storage device 27, and the analysis information storage device 28 in FIG. 1 are schematic representations of logical configurations. The storage contents of the storage device 25, the wavelength information storage device 26, etc. may be stored in the same hardware. For example, the storage contents of the angle information storage device 27 can be stored in a main storage device composed of a volatile storage device such as SRAM and DRAM, and the program storage device 25, the wavelength information storage device 26, and the analysis information storage device. The storage contents 28 can be stored in an auxiliary storage device including a nonvolatile storage device such as a magnetic disk such as a hard disk (HD), a magnetic tape, an optical disk, or a magneto-optical disk. In addition, as the auxiliary storage device, a RAM disk, an IC card, a flash memory card, a USB flash memory, a flash disk (SSD), or the like can be used.

  As shown in FIG. 1, according to the spectrometer 5 according to the first embodiment of the present invention, a plurality of detectors 53-1 to 53-n having different wavelength ranges are switched in the procedure described below. Can be used sequentially.

  The spectroscope 5 according to the first embodiment shown in FIG. 1 is an example, and a gear on which a plurality of detectors 53-1, 53-2,. Another configuration may be employed in which a shaft for mounting the spectroscopic element 52 is passed through the central axis and the shaft is rotated by a large gear.

-Detector switching method-
As an example of the analysis method according to the first embodiment, using the flowchart of FIG. 7, the first detector 53-1 is used for the viewing angles θ _{S to} θ ₁ and the diffraction angles 2θ _{S to} 2θ ₁ . After the analysis, the case of switching to the second detector 53-2 and performing the analysis at the viewing angles θ _{2 to} θ _E and the diffraction angles 2θ _{2 to} 2θ _E will be described as an example. As shown in FIG. 8, relative to the direction of the incident wave to the spectral element 52, the rotation angle phi ₁ of the first detector _53-1, if the rotation angle phi ₂ of the second detector 53-2 The offset angle β between the first detector 53-1 and the second detector 53-2 is φ = φ ₁ −φ ₂ . :
(A) First, in step S101, the detector used for analysis, the analysis target element of the sample 43, the type of the spectroscopic element 52, the scanning wavelength range, the wavelength step width, and the viewing angle via the input device 22 shown in FIG. Various conditions and parameters used for analysis, such as θ _S , θ ₁ , θ ₂ , θ _E , and rotation angles φ ₁ , φ _2, are set as analysis conditions. The set conditions and parameters are stored in the analysis information storage device 28, and the viewing angles θ _S , θ ₁ , θ ₂ , θ _E , and the rotation angles φ ₁ , φ ₂ are stored in the angle information storage device 27.

(B) In step S102, an analysis is performed based on the analysis conditions specified in step S101. The goniometer device control means 351 drives the first rotating body driving mechanism 62-1 and the second rotating body driving mechanism 62-2, and as shown in FIG. 9, the viewing angle θ = θ to the spectroscopic element 52 _S , with the rotation angle φ ₁ = 2θ _S of the _first detector 53-1 as an initial value, the first rotating body 61-1 is rotated, for example, clockwise, and the first rotating body 61-1 In conjunction with the rotation, the second rotating body 61-2 is rotated in the clockwise direction, and the first detector 53-1 is used to display angles θ _{S to} θ ₁ and diffraction angles 2θ _{S to} 2θ _1. Wavelength scan in the clockwise direction. When the wavelength scanning in the clockwise direction of the first detector 53-1 is completed, in step S103, based on the analysis condition specified in step S101, whether or not the analysis is performed by switching to the second detector 53-2. To decide. When switching to the 2nd detector 53-2, it progresses to Step S104.

(C) In step S104, the drive amount of the goniometer device 6 for switching to the second detector 53-2 is acquired. The drive amount processing means 352 reads the viewing angles θ ₂ and θ _E and the rotation angles φ ₁ and φ ₂ from the angle information storage device 27, calculates a rotation angle that is a drive amount necessary for the goniometer device 6, and provides angle information. The data is stored in the storage device 27, and the goniometer device control means 351 reads the rotation angle necessary for the goniometer device 6 from the angle information storage device 27.

(D) In step S105, the goniometer device control means 351 rotates the first rotating body 61-1 and the second rotating body 61-2 in conjunction with each other to obtain θ = θ ₂ and φ ₁ = 2θ _2. Then, the second rotating body 61-2 is advanced clockwise by the offset angle β via the second rotating body driving mechanism 62-2, and the rotation angle φ ₂ = 2θ of the _second detector 53-2. ₂ . Further, the detector control means 353 stops the operation of the detector 53-1, starts the operation of the detector 53-2, and outputs the detection signal from the detector 53-2 to the control analyzer 2. Switch.

(E) Proceeding to step S106, the goniometer device control means 351 drives the first rotating body driving mechanism 62-1 and the second rotating body driving mechanism 62-2, and as shown in FIG. Using -2, wavelength scanning is performed between a viewing angle θ _{2 to} θ _E and a diffraction angle 2θ _{2 to} 2θ _E. When the wavelength scanning in the detector 53-2 is completed, in step S103, based on the analysis condition specified in step S101, it is determined whether or not to continue the analysis in the next wavelength range by switching to the next detector. . If the next wavelength range is not analyzed, the process ends.

  In the above description, the case where the first rotator 61-1 and the second rotator 61-2 are rotated clockwise to perform wavelength scanning in the clockwise direction has been described, but wavelength scanning is performed in the counterclockwise direction. In this case, the first rotating body 61-1 and the second rotating body 61-2 may be rotated counterclockwise so that the diffraction angle 2θ is obtained when the viewing angle θ.

(Second Embodiment)
The configuration of the spectroscope according to the first embodiment shown in FIG. 1 is an exemplification, and the goniometer device 6 includes a plurality of detector rotation mechanisms (61-2a, 62-2a; 61− as shown in FIG. 11). 3a, 62-3a), and a plurality of detector rotation mechanisms (61-2a, 62-2a; 61-3a, 62-3a) may be provided with detectors.

  That is, as shown in FIG. 11, the spectroscope 5a according to the second embodiment of the present invention includes a spectroscopic element 52a that diffracts an electromagnetic wave indicating the characteristics of the sample 43 emitted from the sample 43, and the spectroscopic element 52a. And a plurality of detectors (53−) for detecting electromagnetic waves diffracted by the spectroscopic element 52a in different wavelength regions, respectively. 1a to 53-na; 54-1a to 54-ma) and the spectral element rotation mechanism (61-1a, 62-1a) and the rotation axis, and a plurality of detectors (53-1a to 53-na; 54). -1a to 54-ma), and a plurality of detector rotation mechanisms (61-2a, 62-2a; 61-3a, 62-3a) that move around the spectroscopic element 52a. By switching the detector rotation mechanism (61-2a, 62-2a; 61-3a, 62-3a) The difference from the first embodiment is that the detectors (53-1a to 53-na; 54-1a to 54-ma) can be switched. As shown in FIG. 11, the spectroscopic element rotating mechanism (61-1a, 62-1a) has a first disc-shaped rotating body 61-1a and a first rotation for rotating the first rotating body 61-1a. A body drive mechanism 62-1a. The first detector rotating mechanism (61-2a, 62-2a) includes a second rotating body 61-2a, and a second rotating body driving mechanism 62-2a that rotates the second rotating body 61-2a. The second detector rotating mechanism (61-3a, 62-3a) includes a third rotating body 61-3a and a third rotating body driving mechanism 62 that rotates the third rotating body 61-3a. -3a.

  Specifically, as shown in FIG. 11, n detectors 53-1a to 53-na (n is an integer of 1 or more) are provided on the second rotating body 61-2. On the rotating body 61-3, m detectors 54-1a to 54-ma (m is an integer of 1 or more) are provided.

  As shown in FIG. 11, the second rotator 61-2a has a larger radius than the first rotator 61-1 and the third rotator 61-3a is the second rotator 61-2a. Have a larger radius. The first rotating body 61-1a, the second rotating body 61-2a, and the third rotating body 61-3a pass through the center of the goniometer circle formed by the first rotating body 61-1a and are perpendicular to the paper surface. It rotates by sharing the rotating shaft 60a. The third rotating body drive mechanism 62-3a has a basic configuration similar to that of the first rotating body drive mechanism 62-1a and the second rotating body drive mechanism 62-2a, and the first rotating body drive mechanism The 62-1a, the second rotating body drive mechanism 62-2a, and the third rotating body drive mechanism 62-3a can perform highly accurate drive control independent of each other.

  In FIG. 11, the first detector rotating mechanism (61-2a, 62-2a) and the first detector rotating mechanism (61-2a, 62-2a; 61-3a, 62-3a) Although two detector rotation mechanisms of two detector rotation mechanisms (61-3a, 62-3a) are illustrated, the number of detector rotation mechanisms is not limited to two, and the detector rotation mechanism is 3 There can be more than one. That is, the goniometer device 6a according to the second embodiment may include four or more rotating bodies, and each rotating body may include a detector.

  As shown in FIG. 11, the detectors 54-1a to 54-ma, like the detectors 53-1 to 53-n, have their detection directions directed to the rotation shaft 60a when m is 2 or more. The third rotating body 61-3a is disposed with a predetermined angle difference between the rotating bodies 61-3a so as not to interfere with each other. Electromagnetic waves such as X-rays converted into parallel beams by the polycapillary lens 51a are diffracted by the spectroscopic element 52a, pass through slits (not shown), and detectors 53-1a to 53-na and 54-1a to 54-ma. The polycapillary lens 51a, the spectroscopic element 52a, and the detectors 53-1a to 53-na and 54-1a to 54-ma are located on the same plane perpendicular to the rotation axis 60a.

For example, a wavelength scan, such as for qualitative and quantitative analyzes, elevation angle theta _S through? ₁ viewed using a detector _53-1a, after until the diffraction angle 2θ _S ~2θ _1, the detector 54 - 1a to switch to glancing angle theta ₂ through? _E, when performing until the diffraction angle 2θ ₂ ~2θ _E, based on the direction of the incident wave into spectral element 52a, the detector 53-1a used before the switching If the rotation angle φ ₁ is the rotation angle φ _{2 of the} detector 54-1a used after switching, the detector 53-1a installed on the second rotating body 61-2a and the third rotating body 61-3a are installed. Since the detector 54-1a can rotate independently of each other, the detector 53-1a waits as the rotation angle φ ₂ = 2θ ₂ during the wavelength scanning by the detector 53-1a. And more rapid analysis can be performed.

(Third embodiment)
The spectroscopic element is not limited to the flat plate type described in the first and second embodiments. As shown in FIG. 12, the analysis unit 4b of the analyzer using the spectroscope according to the third embodiment of the present invention includes a Johansson spectroscope 5b that performs spectroscopic analysis using a curved spectroscopic element 52b. As described in the background art section, on the Roland circle Q having the radius R equal to the curvature radius R of the surface of the spectroscopic element 52b, the spectroscopic element having the excitation ray irradiation portion 430b of the sample 43b and the curvature radius 2R of the lattice plane. 52b and the detection point need to be located. For this reason, in the analyzer using the spectroscope according to the third embodiment, the distance from the excitation beam irradiation site 430b to the spectroscopic element 52b and the n detectors 53-1b to 53- from the spectroscopic element 52b. The distance to the detection point by nb is adjusted with reference to the Roland circle Q.

  For example, as shown in FIG. 13, the spectroscope according to the third embodiment includes an excitation beam irradiation site 430b, a curved spectroscopic element 52b, and a light receiving slit 59b arranged on the outer periphery of the Roland circle Q. One rotating body 61-1b and a plurality of detectors 53-1b to 53-nb having different detectable wavelength ranges (FIGS. 12 and 13 show only two detectors 53-1b and 53-2b. The first rotating body 61-1b has the same center of rotation as the first rotating body 61-1b and has a larger radius than the first rotating body 61-1b. And a disk-shaped second rotating body 61-2b located deeper in the drawing. The second rotating body 61-2b is provided with a second rotating body driving mechanism 62-2b that rotates the second rotating body 61-2b. With the configuration as shown in FIG. 13, one end side (the left end side in FIG. 13) of the main arm 63b has an axis passing through the excitation beam irradiation site 430b parallel to the rotation axis 60b of the Roland circle Q as the rotation axis. The other end side (the right end side in FIG. 13) supports a rotation shaft 60b that is the center of the Roland circle Q so that the Roland circle Q rotates. One end portion of the auxiliary arm 64b is fixed to the rotation shaft 60b, which is always positioned on the circumference of the Roland circle Q, and the rotational axis 60b that moves by the rotation of the main arm 63b, the excitation beam irradiation site 430b whose position is fixed, The light receiving slit 59b is installed on the Roland circle Q so that the other end side of the auxiliary arm 64b separated from the distance R by the auxiliary arm 64b is positioned on the circumference of the Roland circle Q. Since the detection point D by the detectors 53-1b to 53-nb can be approximated to the slit portion of the light receiving slit 59b, the detection point D is always located on the circumference of the Roland circle Q by the auxiliary arm 64b. .

  The curved spectroscopic element 52b is a circle of the first rotating body 61-1b which is the Roland circle Q via the spectroscopic element holder 65b so that the normal direction of the spectroscopic element 52b is directed to the rotation axis 60b of the Roland circle Q. It is installed so that it can rotate on the circumference and slide on the circumference. The spectroscopic element 52b slides on the circumference of the Roland circle Q by being linearly driven along the spectroscopic element guide 56b by the spectroscopic element driving mechanism 55b. The spectroscopic element guide 56b maintains a constant angle with respect to the surface of the sample 43b irradiated with the excitation ray E, and the spectroscopic element 52b moves linearly, so that the excitation beam irradiation part 430b and the surface of the spectroscopic element 52b are moved. When the distance of the spectroscopic element central axis 520b passing therethrough changes, the rotation axis 60b, which is the center of the Roland circle Q, rotates about the excitation beam irradiation site 430b.

  As shown in FIG. 13, the spectroscopic element driving mechanism 55b rotates around the spectroscopic element central axis 520b so that the spectroscopic element 52b held by the spectroscopic element holder 65b slides on the circumference of the Roland circle Q.

  The light receiving slit 59b is linearly moved along the light receiving slit guide 58b while being fixed so that the rotation center of the light receiving slit 59b slides on the circumference of the Roland circle Q by the light receiving slit driving mechanism 57b. The light receiving slit guide 58b is a guide for linear movement when driving the light receiving slit 59b, and is set so that the optical axis passing through the light receiving slit 59b always faces the direction of the spectral element central axis 520b. The light receiving slit guide 58b has a spectral element central axis 520b and a light receiving slit so that the diffracted X-rays from the spectroscopic element 52b pass through the light receiving slit 59b and are detected by any of the detectors 53-1b to 53-nb. 59b and any of detectors 53-1b to 53-nb are held in a straight line.

  The plurality of detectors 53-1b to 53-nb are respectively held by the detector holders 66-1b to 66-nb, and have a predetermined angle difference between them so as not to interfere with each other, and the spectroscopic element guide 56b, It is disposed on the circumferential side of the second rotating body 61-2b that rotates deeper in the drawing than the light receiving slit guide 58b. Each of the detector holders 66-1b to 66-nb can be rotated (rotated) on a plane parallel to the second rotating body 61-2b, and along with the rotation (revolution) of the second rotating body 61-2b, Control is performed so that the detection directions of the detectors 53-1b to 53-nb used for detection are directed to the light receiving slit 59b.

  Each of the detector holders 66-1b to 66-nb sequentially attaches or detaches any of the detectors 53-1b to 53-nb to the light receiving slit guide 58b. It is possible to move. The light receiving slit guide 58b has an opening on the lower surface of the position of the detector, and when any of the detectors 53-1b to 53-nb is selected and attached to the light receiving slit guide 58b sequentially through the opening, The alignment of any of the selected detectors 53-1b to 53-nb and the opening of the light receiving slit guide 58b is performed by rotating the second rotating body 61-2b by the second rotating body driving mechanism 62-2b. Is done by.

  In FIG. 13, the second rotating body 61-2b is located at the back of the paper surface. At the time of measurement (during analysis), X-rays are diffracted by the spectroscopic element 52b, focused by the light receiving slit 59b, and the detection point D is set. The excitation-ray irradiation site 430b, the spectroscopic element 52b, and the detection point D are respectively arranged on the circumference of the Roland circle Q that forms the same plane so that any of the detectors 53-1b to 53-nb can sequentially detect them. To position.

  As shown in FIG. 14, the detector switching means 35b that the CPU 3 of the control analysis device 2 according to the third embodiment has as a logical structure is used to control the drive of the second rotating body drive mechanism 62-2b of the goniometer device 6b. Of the goniometer device control means 351b for performing the above, the drive amount processing means 352b for calculating the drive amount of the spectroscope 5b required when switching the detectors 53-1b to 53-nb, and the detectors 53-1b to 53-nb Detector control means 353b that performs drive control, and spectroscopic control means 355b that drives and controls the spectroscopic element drive mechanism 55b and the light receiving slit drive mechanism 57b are provided. The excitation beam irradiation part 430b of the sample 43b, the spectroscopic surface of the spectroscopic element 52b, and the detection point D of the light receiving slit 59b by the detectors 53-1b to 53-nb are a main arm 63b, an auxiliary arm 64b, and a spectroscopic element driving mechanism. 55b, the light receiving slit driving mechanism 57b, and the second rotating body driving mechanism 62-2b, and the distance from the sample 43b to the spectroscopic element 52b and the spectroscopic element 52b are detected so that they are always located on the circumference of the Roland circle Q. The distance to the point D is controlled to be equal, and the Bragg diffraction condition is satisfied with the double angle of the viewing angle θ and the diffraction angle 2θ, so that X-ray wavelength scanning is achieved.

  For example, the first detector 53-1b and the second detector 53-2b are arranged with an offset angle β with respect to the rotation shaft 60b, and are analyzed using the first detector 53-1b. In the case where the analysis is performed after switching to the second detector 53-2b, when the detection by the first detector 53-1b is completed, the first detector 53-1b moves the light receiving slit guide 58b. Is removed from the light-receiving slit guide 58b. By rotating the second rotating body 61-2b by the offset angle β by the second rotating body driving mechanism 62-2b, the second detector 53-2b and the opening of the light receiving slit guide 58b are aligned. Done. The second detector 53-2b is mounted on the light receiving slit guide 58b by being raised from the back of the paper and inserted into the light receiving slit guide 58b through the opening, and is detected by the second detector 53-2b. Is possible.

(Other embodiments)
As described above, the present invention has been described according to the first to third embodiments. However, it should not be understood that the description and drawings constituting a part of this disclosure limit the present invention. From this disclosure, various alternative embodiments, examples and operational techniques will be apparent to those skilled in the art.

  For example, in the description of the first and second embodiments, the shapes of the plurality of rotating bodies included in the goniometer devices 6 and 6a are not limited to the disk shape. As long as the surface of the spectroscopic element 52 includes the rotation shaft 60 and a plurality of detectors can be arranged so that the detection direction faces the rotation shaft 60, a ring shape, a rod shape, or the like may be used. For example, a rod-shaped rotating body may be installed so as to coincide with the rotating shaft 60, and the spectroscopic element 52 may be mounted at the tip.

  In the third embodiment, the number of rotating bodies included in the goniometer device 6b is not limited to two. As shown in the second embodiment, three or more rotating bodies are provided. And a detector may be included in each rotating body.

  Further, in the description of the first to third embodiments, by providing a CCD detector, a photodiode, a photomultiplier tube, etc. as a detector, wavelengths other than X-rays, that is, wavelengths of 0.1 to 0 are used. It can detect electromagnetic waves with a wavelength of .01 nm or less or ultraviolet rays with a wavelength of 10 nm or more. As a spectroscopic element, the spectroscopic element holder is equipped with various spectroscopic crystals, diffraction gratings, reflectors, etc. And by making it changeable, more analyzes can be performed for a wide range of analysis objects. For example, the spectroscopic element 52 may be a diffraction grating and the cathode luminescence may be detected by a CCD detector.

  In the description of the first to third embodiments, the excitation ray source 41 and the lens unit 42 are not limited to the electron gun and the electron lens, but as shown in FIG. Even with a fluorescent X-ray analysis (XRF) apparatus that employs a polycapillary lens 42d focused on the 43d excitation beam irradiation site 430d, a similar system can be constructed and a similar method can be implemented. Furthermore, it will be clear from the above description that similar effects can be obtained.

  In the description of the first to third embodiments, other analysis apparatuses using wavelength dispersion type spectrometers such as a particle beam excitation X-ray analysis (PIXE) apparatus using an ion beam as an excitation line are used. However, it will be apparent from the above description that a similar system can be constructed, a similar method can be implemented, and a similar effect can be obtained.

  As described above, the present invention naturally includes various embodiments not described herein. Therefore, the technical scope of the present invention is defined only by the invention specifying matters according to the scope of claims reasonable from the above description.

Q ... Roland circle 2 ... Control analysis device 3 ... CPU
4, 4b ... Analysis unit 5,5a, 5b ... Spectroscope 6,6a, 6b ... Goniometer device 10e, 10f, 430, 430b, 430d ... Excitation beam irradiation site 11e, 11f, 43, 43b, 43d ... Sample 12e, 12f , 52, 52a, 52b ... spectral elements 13e, 13f, 53-1-53-n, 54-1-54-m ... detectors 15f, 42d, 51, 51a ... polycapillary lens 21 ... input / output control unit 22 ... Input device 23 ... Output device 24 ... Display device 25 ... Program storage device 26 ... Wavelength information storage device 27 ... Angle information storage device 28 ... Analysis information storage device 31 ... Excitation source control means 32 ... Lens part control means 33 ... Stage part Control means 34 ... detection signal processing means 35, 35b ... detector switching means 41 ... excitation source 41d ... X-ray source 42 ... lens section 44 ... stay Section 55b ... Spectroscopic element driving mechanism 56b ... Spectral element guide 57b ... Light receiving slit driving mechanism 58b ... Light receiving slit guide 59b ... Light receiving slit 60, 60a, 60b ... Rotating shaft 61-1 ... First rotating body 61-2 ... Second Rotating body 61-3 ... Third rotating body 62-1 ... First rotating body driving mechanism 62-2 ... Second rotating body driving mechanism 62-3 ... Third rotating body driving mechanism 63b ... Main arm 64b Auxiliary arm 65b Spectroscopic element holder 66-1b to 66-nb Detector holder 351, 351b Goniometer device control means 352, 352b Drive amount processing means 353, 353b Detector control means 355b Spectroscope control means 421 ... Converging lens 422 ... Deflection coil 423 ... Objective lens 520b ... Spectral element central axis 621 ... Actuator 622 ... Worm 623 ... Worm wheel

Claims (2)

A spectroscopic element that diffracts an electromagnetic wave indicating the characteristics of the sample emitted from the sample;
A spectroscopic element rotating mechanism for rotating the spectroscopic element around the surface of the spectroscopic element;
A plurality of detectors for detecting the electromagnetic waves diffracted by the spectroscopic element in different wavelength regions;
A detector rotating mechanism that shares a rotation axis with the spectroscopic element rotating mechanism and moves the plurality of detectors around the spectroscopic element, and changing the offset angle of the detector rotating mechanism, A spectrometer characterized in that the detector can be switched. A spectroscopic element that diffracts an electromagnetic wave indicating the characteristics of the sample emitted from the sample;
A spectroscopic element rotating mechanism for rotating the spectroscopic element around the surface of the spectroscopic element;
A plurality of detectors for detecting the electromagnetic waves diffracted by the spectroscopic element in different wavelength regions;
A plurality of detector rotation mechanisms that share a rotation axis with the spectroscopic element rotation mechanism, mount any of the plurality of detectors, and move around the spectroscopic element, and the plurality of detector rotation mechanisms. A spectroscope characterized in that the plurality of detectors can be switched by switching.

Images