JP5117017B2 - X-ray analyzer - Google Patents

Description

  The present invention relates to an X-ray analyzer used for examining, for example, an element contained in a sample, its amount, and its distribution state, and particularly to an X-ray analyzer extremely excellent in workability.

  As an X-ray analyzer of this type, for example, as shown in Patent Document 1, a sample chamber in which a sample is placed and primary X-rays irradiated to the sample pass, and the primary X-ray is applied to the sample. The X-ray irradiation chamber in which an X-ray detector for detecting secondary X-rays generated when irradiated is divided by a diaphragm made of an X-ray transparent material, and the X-ray irradiation chamber is evacuated. There is something.

  The X-ray analyzer includes a main body block that forms an X-ray irradiation chamber, and a diaphragm attachment member that is attached to the main body block and separates the sample chamber and the X-ray irradiation chamber by a diaphragm. The diaphragm attaching member has an X-ray passage hole that allows X-rays to pass therethrough, and is an integral member that fixes the diaphragm to the X-ray passage hole, and is fixed to the main body block. The X-ray detector is fixed as close to the X-ray passage hole as possible in order to detect secondary X-rays from the sample.

  However, due to the structure of the device, the diaphragm needs to be replaced through the sample chamber, so the working space is small and the diaphragm mounting member is mounted above the sample chamber and is not visible. It is difficult to perform necessary screw tightening work and screw removal work, which is a heavy burden. In addition, the work time is also delayed.

Further, when the membrane attachment member is attached, the membrane attachment member may hit the X-ray detector and the X-ray detector may be damaged.
JP 2000-329713 A

  Therefore, the present invention has been made to solve the above-mentioned problems all at once, the diaphragm replacement operation is very simple, and there is little risk of damage to the X-ray detector when replacing the diaphragm. Therefore, the main objective of the present invention is to provide an X-ray analysis apparatus with extremely excellent properties.

That is, the X-ray analyzer according to the present invention, a sample chamber for storing a sample, and secondary X-rays generated by passing the primary X-ray irradiated to the sample and irradiating the sample with the primary X-ray. An X-ray irradiation chamber in which an X-ray detector is detected, and the sample chamber and the X-ray irradiation chamber are separated by a diaphragm having X-ray permeability, and the sample chamber is in an atmospheric pressure state, An X-ray analyzer for making an X-ray irradiation chamber in a vacuum state, the main body block forming the X-ray irradiation chamber, and a sample side end of the main body block, the primary X-ray and the secondary X-ray A passage hole member having an X-ray passage hole for allowing the X-ray to pass therethrough, and the X-ray passage hole member, the X-ray passage hole member being attached to the passage hole member so A membrane anchor that fixes the diaphragm to the sample side of the wire passage hole Comprising a member, it said in a state where the passage hole member is provided in the main body block, the passage hole member and is detachably constituted by the membrane fixing member and the elastic fixing member, wherein the passage hole member side or An engagement concave portion provided on one side of the membrane fixing member side, and an engagement convex portion provided corresponding to the engagement concave portion on the other side of the passage hole member side or the membrane fixing member side, The elastic fixing member is provided on the inner peripheral surface of the engaging recess or the outer peripheral surface of the engaging convex portion, and the elastic deformation is caused by the engagement of the engaging concave portion and the engaging convex portion. When the member is elastically deformed, an elastic return force of the elastic deformation member acts between the inner peripheral surface of the engagement concave portion and the outer peripheral surface of the engagement convex portion, and the membrane is fixed to the passage hole member. The member is fixed .

  If it is such, a diaphragm can be replaced | exchanged, isolate | separating a passage hole member and a membrane fixing member, and fixing the passage hole member to a main body block. Therefore, since there is little fear that the passage hole member will hit the X-ray detector when the diaphragm is replaced, the X-ray detector will not be damaged. Further, since the passage hole member and the membrane fixing member are configured to be detachable by the elastic fixing member, the diaphragm can be fixed very easily without using a screw.

  In addition, it is desirable to further include an attachment restriction mechanism for restricting a rotation angle for attaching the membrane fixing member to the passage hole member from the ease and certainty when attaching the membrane fixing member to the passage hole member.

  As a specific embodiment of the attachment restriction mechanism, the attachment restriction mechanism includes a guide surface provided on the passage hole member and a guided surface provided on the membrane fixing member. It is conceivable that the membrane fixing member can be attached to the passage hole member only when the rotation angle is adjusted so that the guide surfaces face each other.

  Furthermore, in order to prevent the membrane fixing member from being arbitrarily removed from the passage hole member due to a decrease in the fixing force of the elastic fixing member, and to further fix the membrane fixing member to the passage hole member, the passage hole It is desirable to further include a detachment prevention mechanism that prevents the membrane fixing member from detaching from the member.

  As a specific embodiment of the disengagement prevention mechanism, it comprises a hooking portion provided on one of the passage hole member or the membrane fixing member and a receiving portion provided on the other side. In a state where the membrane fixing member is attached by an elastic fixing member, the membrane fixing member is prevented from coming off by rotating the membrane fixing member in the axial direction so that the hooking portion is hooked on the receiving portion. It is done.

  It is desirable that the passage hole member has an air hole on a surface that comes into contact with the membrane fixing member when the membrane fixing member is attached.

  According to the present invention configured as described above, an X-ray analyzer that excels in workability and safety is very easy to replace the diaphragm, and less likely to damage the X-ray detector when the diaphragm is replaced. Can be provided.

  An embodiment of the present invention will be described below with reference to the drawings.

  As shown in FIGS. 1 and 2, the X-ray analyzer 1 according to the present embodiment converts primary X-rays emitted by an X-ray tube 9 of an X-ray generator into, for example, an X-ray guide (X-Ray Guide made of glass). Tube, hereinafter simply referred to as XGT) 10 is led to the X-ray irradiation chamber 31 in a vacuum state, and primary X-rays are applied to the sample W in the sample chamber 21 in the atmospheric pressure state provided below the X-ray irradiation chamber 31. The X-ray detector 11 detects secondary X-rays (fluorescence X-rays) generated at that time, and the sample chamber 21 and the X-ray irradiation chamber 31 are made of, for example, polyethylene resin or the like It is partitioned by a diaphragm F having X-ray permeability.

  This X-ray analysis apparatus 1 can make the beam diameter of primary X-rays as extremely thin as several tens to several hundreds of μm by using the XGT 10, and has a sufficiently large power at the minute region X-ray irradiation site of the sample W. Can be reliably irradiated.

  Specifically, the X-ray analyzer 1 includes a casing 2 that forms a sample chamber 21 and a main body block 3 that forms an X-ray irradiation chamber 31.

  As shown in FIGS. 1 and 2, the casing 2 is maintained in an atmospheric pressure state, and is provided with a sample stage 22 on which a sample W to be measured is placed. As shown in FIG. 2, the sample chamber 21 is provided with an open / close door 23 for inserting and removing the sample W. Further, the diaphragm F is exchanged by opening the door 23. The sample stage 22 is provided so as to be linearly movable in each of the X, Y, and Z directions by a driving mechanism (not shown). Note that the sample stage 22 is not shown in FIG.

  As shown in FIGS. 1 and 3, the main body block 3 has a substantially cubic shape continuously provided in the casing 2, and has an insertion hole 32 through which the XGT 10 is inserted, and is inserted into the inside. An X-ray irradiation chamber 31 connected to the hole 32 is provided. Further, the side wall has an attachment hole 33 for the X-ray detector 11 and the optical microscope 12 to be inserted and installed, and the bottom wall has an opening 34 to which a later-described passage hole member 4 is attached. Have.

  The inside of the X-ray irradiation chamber 31 is maintained in an appropriate vacuum state together with the insertion hole 32, and particularly when the lower end of the XGT 10 and the primary X-ray are irradiated to the sample W as shown in FIG. Are provided with an X-ray detector 11 comprising a semiconductor detector for detecting secondary X-rays (fluorescent X-rays) generated in the optical microscope and an objective lens of an optical microscope for confirming the irradiation position of the sample W. In FIG. 1, reference numeral 13 denotes a tank containing a medium for cooling the X-ray detector 11, and reference numeral 14 denotes a signal amplifier.

  And the X-ray analyzer 1 of this embodiment is provided in the sample W side edge part (opening 34) of the main body block 3, as shown in FIG.1 and FIG.4, and a primary X-ray and a secondary X-ray are obtained. A passage hole member 4 having an X-ray passage hole 412 to be passed through, and a membrane that holds the diaphragm F and is attached to the passage hole member 4 to fix the diaphragm F to the sample W side of the X-ray passage hole 412 When the fixing member 5 and the membrane fixing member 5 are attached to the passage hole member 4, they are interposed between the membrane fixing member 5 and the passage hole member 4 and exert an elastic return force on them. And an elastic fixing member 6 such as an O-ring to be fixed. Each member 4, 5, 6 will be described below.

  The passage hole member 4 narrows the opening 34 of the main body block 3 to a hole having a predetermined size. As shown in FIGS. 5, 6, and 7, the passage hole member 4 fits into the opening 34 and the outer periphery thereof is a seal member. A cylindrical portion 41 that is in close contact with the inner periphery of the opening 34 via the O-ring 15 without any gap, and a collar portion 42 provided at the lower end of the cylindrical portion 41.

  The cylindrical part 41 has substantially the same diameter as the opening part 34 of the main body block 3, and an accommodation recessed part 411 for arranging the X-ray detector 11 from an oblique direction in the center part, and a bottom part of the accommodation recessed part 411 And an X-ray passage hole 412 for allowing primary X-rays and secondary X-rays to pass therethrough. The X-ray passage hole 412 is formed to have a tongue shape toward the X-ray detector 11 side. Further, a concave groove 414 into which the O-ring 15 is fitted is provided on the outer peripheral surface 41 a of the cylindrical portion 41.

  Further, the cylindrical portion 41 has an engagement recess 413 formed on the end surface where the X-ray passage hole 412 is provided. The engagement recess 413 is provided in an annular shape so as to surround the X-ray passage hole 412. The inner peripheral surface 413c is a tapered surface having a cross-sectional diameter that decreases toward the tip. An air hole A is provided in a part of the bottom of the engagement recess 413. As described above, since the air passage A is formed by providing the air hole A in the bottom portion of the engaging recess 413, the attachment and detachment between the passage hole member 4 and the membrane fixing member 5 can be facilitated. It is possible to prevent the damage caused by the suction of the diaphragm F.

  The collar portion 42 has a so-called roughly oval shape in which the left and right end portions of the disc are cut out in plan view (see FIG. 6).

  Then, as shown in FIG. 6, it protrudes from the one end 421a of one notch 421 to the upper surface 42a of the collar 42 so as not to reach the one end 422a of the other notch 422 along the outer edge. A strip 423 is provided. Similarly, the protrusion 423 is provided from the other end 422b of the other notch 422 to the extent that it does not reach the other end 421b of the notch 421 along the outer edge. The upper surface of the protrusion 423 comes into contact with the lower surface of the main body block 3 when the passage hole member 4 is attached to the main body block 3. The flange portion 42 has a plurality of screw holes (for example, four) for screwing the passage hole member 4 to the main body block 3 and is fixed to the main body block 3 with screws.

  As shown in the exploded perspective view of FIG. 8, the membrane fixing member 5 includes a fixing member main body 51 and a membrane pressing plate 52 for attaching the diaphragm F to the fixing member main body 51 via the O-ring 15. .

  As shown in FIGS. 8, 9, and 10, the fixing member main body 51 includes a main body portion 512, an annular member 513 attached to the outer peripheral edge of one surface 512 b of the main body portion 512, and an upper surface of the annular member 513. Two locking pieces 514 attached to the.

  The main body 512 has a disc shape having an opening 512a at the center, and an engagement convex portion 511 that engages with the engagement concave portion 413 of the passage hole member 4 is provided on the inner side of the one surface 512b. .

  The engaging convex portion 511 has an annular shape, and a concave groove 511b into which an O-ring 6 that is an elastic fixing member is fitted is provided on the outer peripheral surface 511a. The inner peripheral surface 511c of the engaging convex portion 511 forms an inner wall of the opening 512a and is a tapered surface corresponding to the inner peripheral surface 413c of the engaging concave portion 413. The inner peripheral surface 413 c of the engaging recess 413 and the inner peripheral surface 511 c of the engaging convex portion 511 constitute a slide guide mechanism when the membrane fixing member 5 is attached to the passage hole member 4.

  Further, when the membrane pressing plate 52 is attached to the other surface (lower surface) 512c of the main body portion 512, the lower surface 512c of the main body portion 512 and the lower end surface 52a of the membrane pressing plate 52 are substantially on the same plane. In addition, a stepped portion 5121 is provided which is recessed about the thickness of the film pressing plate 52 (see FIG. 11). The step portion 5121 is provided with an annular groove 5122 having a smaller diameter than the diaphragm F into which the O-ring 15 is fitted.

  The outer contour of the annular member 513 substantially coincides with the outer contour of the main body 512, and the inner contour is circular. The thickness thereof is substantially the same as or slightly larger than that of the flange portion 42.

  The lock piece 514 constitutes an attachment limiting mechanism 7 and a detachment preventing mechanism 8 which will be described later, has a rectangular plate shape, and the thickness thereof is the same as the height of the protrusion 423. The lock piece 514 is attached to the notch 5131 of the annular member 513. Thus, in a state where the lock piece 514 is attached to the annular member 513, the inner contour thereof is similar to the outer diameter contour of the flange portion 42 of the passage member and is slightly larger in size.

  The membrane pressing plate 52 is for attaching the diaphragm F to the main body portion 512 and is an annular flat plate whose outer contour is substantially the same as the contour of the main body portion 512. And it attaches to the step part 5121 of the main-body part 512 with the screw | thread which is not shown in figure. Thereby, when the diaphragm F is attached to the main body part 512, the lower end surface 52a of the film pressing plate 52 and the diaphragm F facing the sample chamber 21 are substantially on the same plane (see FIG. 11).

  Furthermore, when the membrane fixing member 5 is attached and fixed to the passage hole member 4, the diaphragm F contacts the sample side opening (the sample side end surface of the cylindrical portion 41) of the X-ray passage hole 412 (see FIG. 12). Thus, since the lower end surface 52a of the membrane pressing plate 52 and the surface of the diaphragm F facing the sample chamber 21 are substantially flush with each other, the position adjustment of the sample W can be performed safely and easily. .

  As shown in FIGS. 11 and 12, the elastic fixing member 6 is an O-ring that is fitted into a concave groove 511 b provided on the outer peripheral surface 511 a of the engaging convex portion 511. Then, in a state where the passage hole member 4 is attached to the main body block 3 with screws (see FIG. 4), the membrane fixing member 5 is fixed to the passage hole member 4. Specifically, the O-ring 6 is elastic when the engagement concave portion 413 provided on the lower surface of the passage hole member 4 and the engagement convex portion 511 provided on the main body portion 512 of the membrane fixing member 5 are fitted together. By deforming, an elastic restoring force is applied to the outer peripheral surface 413b of the engaging recess 413 and the bottom surface of the recessed groove 511b. Thereby, the membrane fixing member 5 is fixed to the passage hole member 4.

  In such a case, since it can be attached / detached by the O-ring 6 which is an elastic fixing member, one-touch attachment without screw fastening is possible, and attachment / detachment of the membrane fixing member 5 becomes extremely easy. Moreover, since it is attached with a snap by the O-ring 6, it can be easily determined whether it is attached properly. Furthermore, the elastic peripheral force of the O-ring 6 after attachment causes the inner peripheral surface 413c of the engagement concave portion 413 and the inner peripheral surface 511c of the engagement convex portion 511 to be pressed and adhered, so that the membrane fixing member 5 is passed through the passage hole member 4. Can be attached without rattling.

  In addition, the membrane fixing member 5 can be fixed to the passage hole member 4 by the action of the elastic fixing member 6 simply by moving the membrane fixing member 5 to the passage hole member 4 in one direction, that is, in the axial direction.

  Therefore, the X-ray analyzer 1 according to the present embodiment includes the attachment limiting mechanism 7 and the detachment preventing mechanism 8. Hereinafter, the mechanisms 7 and 8 will be described with reference to FIG.

  First, the attachment restriction mechanism 7 will be described. The attachment restriction mechanism 7 restricts the direction in which the membrane fixing member 5 is attached to the passage hole member 4, and specifically determines the relative fitting angle of the membrane fixation member 5 with respect to the passage hole member 4. As shown in FIG. 12 in particular, the configuration is such that the side surfaces 421c and 422c of the notches 421 and 422 of the passage hole member 4 that is the guide surface and the lock pieces 514 of the membrane fixing member 5 that is the guided surface. It is comprised from the inner side surface 514a. The membrane is fixed to the passage hole member 4 only when the side surfaces 421c and 422c of the notches 421 and 422 and the inner side surface 514a of the lock piece 514 of the membrane fixing member 5 which is the guided surface are fitted to face each other. The member 5 can be attached and detached.

  With this attachment limiting mechanism 7, the attachment rotation angle of the membrane fixing member 5 is limited to only one direction or two directions, and the membrane fixing member 5 can be attached easily and reliably.

  Next, the detachment prevention mechanism 8 will be described. The detachment prevention mechanism 8 prevents the membrane fixing member 5 from being detached from the passage hole member 4 by one operation, and the hook provided on one of the passage hole member 4 or the membrane fixing member 5 is provided. Part 81 and a receiving part 82 provided on the other side, and when the membrane fixing member 5 is attached to the passage hole member 4 by the elastic fixing member 6, it is rotated in the axial direction to thereby pull the pulling member. The hook 81 is hooked on the receiving portion 82 to prevent the hook 81 from coming off.

  In the present embodiment, as shown in FIG. 12 in particular, the hook portion 81 is a lower side surface 514b of the lock piece 514, and the receiving portion 82 is a protrusion 423 at the outer edge of the flange portion 42 of the passage hole member 4. It is the plane part 424 in which is not provided. More specifically, the hook portion 81 includes a lower surface 514 b of the lock piece 514 and an upper surface 512 b of the main body portion 512.

  Then, as shown in FIG. 14, in the state where the membrane fixing member 5 is attached to the passage hole member 4, the lower surface 514 b of the lock piece 514 as the hook portion 81 is rotated by rotating the membrane fixing member 5 in the axial direction. The flat portion 424 that is the receiving portion 82 is inserted between the upper surface 512b of the main body portion 512. Further, when the angle is rotated by a predetermined angle or more, the end portion 4231 of the ridge portion 423 hits the inner surface 514c of the lock piece 514 so as not to rotate any more.

  By this detachment prevention mechanism 8, it is possible to prevent the membrane fixing member 5 from being arbitrarily detached. Further, since the flat portion 424 is placed between the lower surface 514b of the lock piece 514 and the upper surface 512b of the main body portion 512, the membrane fixing member 5 can be more firmly fixed.

  According to the X-ray analyzer 1 according to the present embodiment configured as described above, the diaphragm F is replaced while the passage hole member 4 and the membrane fixing member 5 are separated and the passage hole member 4 is fixed to the main body block 3. can do. Therefore, since there is little fear that the passage hole member 4 hits the X-ray detector 14 when the diaphragm F is replaced, the X-ray detector 14 is less likely to be damaged. Further, since the passage hole member 4 and the membrane fixing member 5 are configured to be detachable by the elastic fixing member 6, the diaphragm F can be fixed very easily without using screws.

  The present invention is not limited to the above embodiment.

  In the above embodiment, only the fluorescent X-ray is detected as the secondary X-ray generated in the sample when the sample W is irradiated with the primary X-ray. However, in order to detect the scattered X-ray in addition to this. X-ray detectors may be provided.

  A collimator may be used instead of XGT.

  Further, in the above-described embodiment, the engagement concave portion is provided in the passage hole member and the engagement convex portion is provided in the film holding member.

  In addition, with regard to the detachment prevention mechanism, in the above-described embodiment, the receiving hole is provided in the passage hole member and the hooking portion is provided in the membrane fixing member, but the reverse may be possible.

  Moreover, you may not provide an attachment restriction mechanism or a removal prevention mechanism.

  In addition, some or all of the above-described embodiments and modified embodiments may be combined as appropriate, and the present invention is not limited to the above-described embodiments, and various modifications can be made without departing from the spirit of the invention.

The schematic block diagram of the X-ray analyzer in one Embodiment of this invention. Sectional drawing which mainly shows the sample chamber of the X-ray analyzer in the embodiment. The perspective view which shows the main body block in the same embodiment. The perspective view which shows the state by which the through-hole member was attached to the main body block in the same embodiment. The perspective view of the passage hole member in the embodiment. The top view of the passage hole member in the embodiment. The sectional view on the AA line of the passage hole member in the embodiment. The disassembled perspective view of the film | membrane fixing member in the embodiment. The perspective view of the film | membrane fixing member in the embodiment. The top view of the film | membrane fixing member in the embodiment. BB sectional drawing of the film | membrane fixing member in the embodiment. Sectional drawing which shows the state by which the film | membrane fixing member was attached to the passage hole member in the embodiment. The perspective view which shows the case where the detachment prevention mechanism in the same embodiment is acting.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 ... X-ray analyzer W ... Sample a ... Primary X-ray b ... Secondary X-ray F ... Diaphragm 21 ... Sample chamber 3 ... Main body block 31 ... X Irradiation chamber 4 ... Passing hole member 412 ... X-ray passing hole 413 ... Engaging recess A ... Air hole 5 ... Membrane fixing member 511 ... Engaging protrusion 6 ... Elastic fixing member (O-ring)
7 ... Mounting restriction mechanism 8 ... Disengagement prevention mechanism 9 ... X-ray tube 10 ... X-ray conduit (XGT)
11 ... X-ray detector

Claims (3)

A sample chamber for storing a sample and an X-ray detector for detecting secondary X-rays generated by the primary X-rays irradiated to the sample passing through the sample X-rays and the sample are disposed. An X-ray irradiation chamber, wherein the sample chamber and the X-ray irradiation chamber are separated by a diaphragm having X-ray permeability, and the sample chamber is in an atmospheric pressure state and the X-ray irradiation chamber is in a vacuum state X A line analyzer,
A main body block forming the X-ray irradiation chamber;
A passage hole member provided at the sample side end of the main body block and having an X-ray passage hole through which the primary X-ray and secondary X-ray pass;
Membrane fixation for holding the diaphragm and fixing the diaphragm to the sample side of the X-ray passage hole by being attached to the passage hole member so that the diaphragm is in contact with the sample side opening of the X-ray passage hole A member, and
In the state where the passage hole member is provided in the main body block, the passage hole member and the membrane fixing member are configured to be detachable by an elastic fixing member,
An engagement recess provided on one of the passage hole member side or the membrane fixing member side and an engagement protrusion provided on the other of the passage hole member side or the membrane fixing member side corresponding to the engagement recess. And
The elastic fixing member is provided on the inner peripheral surface of the engagement concave portion or the outer peripheral surface of the engagement convex portion;
The elastic deformation member is elastically deformed by fitting the engaging concave portion and the engaging convex portion, and the inner peripheral surface of the engaging concave portion and the outer peripheral surface of the engaging convex portion are The elastic return force of the elastic deformation member works, the membrane fixing member is fixed to the passage hole member ,
The X-ray analyzer according to claim 1, wherein the passage hole member has an air hole on a surface that comes into contact with the membrane fixing member when the membrane fixing member is attached .   The X-ray analysis apparatus according to claim 1, further comprising an attachment limiting mechanism for limiting a rotation angle for attaching the membrane fixing member to the passage hole member.   The X-ray analyzer according to claim 1, further comprising a detachment preventing mechanism that prevents the membrane fixing member from being detached from the passage hole member.