JP6075873B2 - Sample holder for X-ray analyzer, attachment for X-ray analyzer, and X-ray analyzer - Google Patents

Description

  The present invention relates to a sample holder for placing a sample at a predetermined position of an X-ray analyzer, an X-ray analyzer attachment using the sample holder, and an X-ray analyzer using the X-ray analyzer attachment About.

  An X-ray analyzer is an apparatus that irradiates a sample with X-rays and detects X-rays emitted from the sample with an X-ray detector. In a general X-ray analyzer, a sample is supported by a sample holder, and the sample holder is attached to a predetermined position of the X-ray analyzer, thereby setting the sample at a predetermined position in the X-ray analyzer.

  2. Description of the Related Art Conventionally, a sample holder is known in which a sample is supported from a side surface portion by a plurality of claw-shaped support pieces biased by a spring (see, for example, Patent Document 1). A sample holder is also known in which the outer peripheral surface of the sample is supported by a ring-shaped holder (see, for example, Patent Document 2).

  There is also known a sample holder in which a sample is pressed and supported by a fixing plate having a notch in the peripheral portion and an X-ray passage hole in the central portion (see, for example, Patent Document 3). Furthermore, there is known a sample holder that can be fixed to a sample plate by a magnetic force and supported by pressing a sample with a holding plate that is not flexible (for example, see Patent Document 4).

Japanese Utility Model Publication No. 5-028954 JP 2000-009665 A Japanese Utility Model Publication No. 6-030754 JP 2008-014958 A

  In the sample holder disclosed in Patent Document 1, a step is formed at the tip of a claw-shaped support piece, and the sample is supported in a state where the sample is placed on the step. For this reason, in the sample holder of patent document 1, there existed a problem that the external shape of the sample which can be supported will be limited to a specific thing.

  Moreover, in the sample holder disclosed in Patent Document 2, the outer periphery of the sample is received by the holder while the sample is placed on the pedestal. There was a problem of being limited.

  In addition, the sample holder disclosed in Patent Document 3 has a structure in which the fixing plate is formed of a highly rigid material and cannot be bent. For this reason, the space for supporting the sample formed between the sample stage and the solid plate is limited to a certain height or thickness, and the outer shape of the sample that can be supported is also limited to a specific one. There was a problem that.

  Furthermore, in the sample holder disclosed in Patent Document 4, since the holding plate for holding and supporting the sample is formed of a highly rigid material having no flexibility, the outer shape of the sample that can be supported is still the same. There was a problem that it was limited to a specific one. As described above, in the conventional sample holder, the outer shape of the sample that can be supported is limited to a specific one, and there is a problem that it cannot be used for samples of various shapes.

  By the way, in recent years, there is an increasing demand for evaluation of pharmaceuticals using an X-ray analyzer at the stage of pharmaceutical development. For example, pharmaceutical qualitative analysis, quantitative analysis, crystallinity analysis, crystallite size analysis, structural analysis, and the like are frequently performed using an X-ray analyzer. Pharmaceutical products are often in the form of tablets, and these tablets have various outer shapes as is well known. In addition, not only drugs but also substances that can be samples of X-ray analyzers have conventionally taken many different shapes. The above-described conventional sample holder cannot cope with samples having such various outer shapes, and therefore, a sample holder that can cope with various outer shapes has long been desired.

  The present invention has been made in view of the above-mentioned problems, and is a sample holder that can accurately place samples of various outer shapes at predetermined positions in an X-ray analyzer with a simple operation. The purpose is to provide.

The sample holder for an X-ray analyzer according to the present invention has a pair of sample clamping members that support the sample and support the sample by sandwiching the sample from both sides in the sample holder attached to and detached from the X-ray analyzer, The sample holding member is a plate-like member having a planar shape wider than the sample, thinner than the sample, and having flexibility, and at least one of the pair of sample holding members has X-rays. The sample holding member is made flexible by forming a plurality of grooves extending radially from the hole in the sample holding member. .

  According to the sample holder of the present invention, the sample can be firmly supported by the sample holder only by an extremely simple operation of simply pinching the sample between the pair of sample holding members. In addition, since the sample is sandwiched between the pair of sample clamping members, the sample can be firmly supported by the sample clamping member that is flexibly moved even if the outer shape of the sample has various shapes. For this reason, even if the sample has various shapes such as a pharmaceutical product of a tablet, the sample can be handled without difficulty.

In sample holder for X-ray analysis apparatus according to the present invention, by forming a plurality of grooves extending radially from the hole in the sample clamping member, and with flexibility in the sample clamping member. Various configurations for giving flexibility to the sample clamping member are conceivable. However, if the sample clamping member is made flexible by a plurality of grooves as described above, the outer peripheral portion of the sample clamping member is bent. It is difficult (that is, the rigidity is high), and the central portion can be easily bent (that is, the rigidity is small). As a result, the sample positioning function can be achieved by the sample clamping member.

  A sample holder for an X-ray analyzer according to the present invention supports a first support member that supports one of the pair of sample holding members so as to bend and move, and the other of the pair of sample holding members that can be bent and moved. A second support member, and the first support member and the second support member are coupled together with the pair of sample clamping members facing each other.

  In the sample holder for an X-ray analyzer according to the present invention, a magnet may be provided on one of the first support member and the second support member, and the first support member and the second support member may be provided. The other of the members can have a property of being attracted to the magnet.

  In the sample holder for an X-ray analyzer according to the present invention, a positioning member for positioning the sample can be provided between the pair of sample clamping members.

  In the sample holder for an X-ray analyzer according to the present invention, the positioning member is a plate-like member that is thinner than the sample, and may have a sample storage hole having a slightly larger diameter than the sample.

  Next, the attachment according to the present invention is characterized by including a sample holder having the above-described configuration. This attachment is a sample changer used in, for example, an X-ray analyzer.

  Next, an X-ray analysis apparatus according to the present invention includes a sample holder having the above-described configuration. This X-ray analyzer is, for example, an X-ray diffractometer or a fluorescent X-ray apparatus.

  According to the sample holder, the attachment, and the X-ray analyzer of the present invention, the sample can be firmly supported by the sample holder by an extremely simple operation of simply sandwiching the sample with the pair of sample clamping members. In addition, since the sample is sandwiched between the pair of sample clamping members, the sample can be firmly supported by the sample clamping member that is flexibly moved even if the outer shape of the sample has various shapes. For this reason, even if the sample has various shapes such as a pharmaceutical product of a tablet, the sample can be handled without difficulty.

It is a disassembled perspective view of one Embodiment of the sample holder for X-ray analyzers which concerns on this invention. FIG. 2 is an exploded cross-sectional view of the sample holder for the X-ray analyzer in FIG. 1. It is sectional drawing which shows the state which assembled the sample holder for X-ray analyzers of FIG. It is a perspective view which shows the sample changer which is one Embodiment of the attachment which concerns on this invention. It is a figure which shows the structure of the back side of the sample changer of FIG. It is a disassembled perspective view of other embodiment of the sample holder for X-ray analyzers which concerns on this invention. It is sectional drawing which shows the state which assembled the sample holder for X-ray analyzers of FIG. It is a figure which shows the state which rotated the sample holder for X-ray analyzers of FIG. 7 180 degrees, and reversed the upper surface and the lower surface. It is a perspective view which shows other embodiment of the sample changer which is one Embodiment of the attachment which concerns on this invention. It is a figure which shows the state which reversed the turntable of the sample changer shown in FIG. It is a figure which expands and shows the sample changer of FIG.

  Hereinafter, a sample holder for an X-ray analyzer, an attachment for an X-ray analyzer, and an X-ray analyzer according to the present invention will be described based on embodiments. Of course, the present invention is not limited to this embodiment. In addition, in the drawings attached to the present specification, components may be shown in different ratios from actual ones in order to show characteristic parts in an easy-to-understand manner.

(Embodiment of sample holder for X-ray analyzer)
FIG. 1 is an exploded perspective view showing an embodiment of a sample holder for an X-ray analyzer according to the present invention. FIG. 2 shows an exploded view of the cross-sectional structure of the sample holder. FIG. 3 shows a cross-sectional structure of the sample holder in an assembled state.

  The sample holder 1 of this embodiment is an instrument for supporting the sample S. The sample S is, for example, a pharmaceutical tablet. This sample S is formed in a flat disk shape with a thick central portion and a thin peripheral portion. In addition, the sample applicable to the sample holder 1 of this embodiment is not limited to the sample S of the above shape, It can apply also to the sample of other various shapes. For example, it is possible to support a sample having the same thickness in the peripheral portion and the central portion, and it is also possible to support samples of various shapes such as an oval shape, a square shape, and the like.

  The sample holder 1 has a first support member 2 and a second support member 3. The first support member 2 is formed in a substantially circular ring shape, and has a stepped portion 4 therein. A recess 2 a is formed by the stepped portion 4. The 2nd support member 3 is also formed in the substantially circular ring shape, and has the level | step-difference part 5 in the inside. The step portion 5 forms a recess 3a.

  A plurality of (four in this embodiment) magnets 6 are provided inside the ring-shaped peripheral portion of the first support member 2. These magnets 6 are provided at appropriate intervals in the circumferential direction. These magnets 6 are provided so that they cannot be easily removed from the first support member 2 by adhesion, fitting, or the like. The second support member 3 is made of a material that is attracted to the magnet.

  The sample holder 1 has a pair of sample clamping members 8a and 8b. The sample sandwiching members 8a and 8b have a substantially circular planar shape when viewed from the direction of the arrow A, and are plate shapes having a uniform thickness. Further, the sample clamping members 8 a and 8 b have a planar shape wider than that of the sample S when viewed from the direction of the arrow A, and a thickness smaller than that of the sample S. Holes 9a and 9b for transmitting X-rays are provided in the central portions of the sample clamping members 8a and 8b. The diameters of these holes 9a and 9b are smaller than the diameter of the sample S. As shown in FIG. 3, the second support member 3 can be coupled to the first support member 2 by the magnetic force of the magnet 6.

  A plurality (eight in this embodiment) of grooves 10 extending radially from the holes 9a and 9b are provided radially around the holes 9a and 9b of the sample clamping members 8a and 8b. Thus, by providing the plurality of grooves 10 extending radially from the central portion in the sample holding members 8a and 8b, the sample holding members 8a and 8b have flexibility. Specifically, with the peripheral portions of the sample clamping members 8a and 8b fixed, the central portions of the sample clamping members 8a and 8b (that is, the portions where the holes 9a and 9b are provided) are shown in FIGS. Can be bent in the vertical direction (arrow BB ′ direction).

  One sample clamping member 8 a is inserted into the recess 2 a of the first support member 2 and supported by the first support member 2 while being received by the stepped portion 4. The outer dimensions of the sample clamping member 8a are as follows with respect to the diameter of the recess 2a, that is, the outer dimensions such that when the first supporting member 2 is turned upside down, it falls from the first supporting member 2 by its own weight. It is also possible to set the outer dimensions such that the weight can be removed from the concave portion 2a of the first support member 2 by applying a slight force although it does not fall by its own weight.

  The other sample clamping member 8 b is inserted into the recess 3 a of the second support member 3 and supported by the second support member 3 while being received by the stepped portion 5. The external dimensions of the sample clamping member 8b can be set as follows with respect to the diameter of the concave portion 3a, that is, the external dimensions of dropping from the second support member 2 by its own weight. It is also possible to set the outer dimensions so that the second support member 3 can be removed from the concave portion 3a by applying the above force.

  A positioning member 11 is provided between the pair of sample clamping members 8a and 8b. The positioning member 11 is formed as a ring-shaped member having a uniform thickness and having a hole 12 in the central portion. The positioning member 11 is formed in a substantially circular shape. The diameter of the positioning member 11 is smaller than the diameter of the recess 2 a of the first support member 2 and the diameter of the recess 3 a of the second support member 3. For this reason, the positioning member 11 is accommodated in the internal space of the first support member 2 and the second support member 3 that are coupled to each other.

  The diameter of the hole 12 in the central portion of the positioning member 11 is slightly larger than the outer diameter of the sample S. For this reason, the sample S can be accommodated in the hole 12 of the positioning member 11, and the position of the sample S is determined in this state.

  The first support member 2, the sample clamping members 8a and 8b, the positioning member 11, and the second support member 3 can be formed of any material, for example, metal, resin, or the like. Note that the second support member 3 used in the present embodiment is formed of a material that can be attracted to the magnet because of being coupled to the first support member 2 by magnetic force.

  Since the sample holder 1 of the present embodiment is configured as described above, the following operation is performed when the sample S is supported by the sample holder 1 as shown in FIG. That is, in FIG. 1 and FIG. 2, one sample clamping member 8a is mounted in the recess 2a of the first support member 2, and the sample S is placed on the sample clamping member 8a. Next, the positioning member 11 is arranged on the sample clamping member 8 a around the sample S so that the sample S is accommodated in the hole 12 of the positioning member 11.

  Next, the other sample holding member 8b is mounted in the recess 3a of the second support member 3, and the second support member 3 thus mounted with the sample holding member 8b is attached to the surface of the first support member 2. The magnet 6 is fixed, that is, coupled by the magnetic force of the magnet 6. As described above, the sample S can be supported by the sample holder 1 as shown in FIG. In this state, the lower sample clamping member 8a is pushed by the sample S and bent downward (B direction) in FIG. 3, and the upper sample clamping member 8b is pushed by the sample S and moved upward (B Deflection in the 'direction). The sample S is firmly supported under an appropriate pressing force by the sample clamping members 8a and 8b which are bent and moved in this manner. Further, the sample S is positioned at a predetermined position by the positioning member 11.

  As described above, according to the sample holder 1 of the present embodiment, the sample S can be firmly supported by the sample holder 1 by an extremely simple operation of simply sandwiching the sample S between the pair of sample clamping members 8a and 8b. . Further, since the sample S is sandwiched between the pair of sample clamping members 8a and 8b, the sample S is firmly supported by the sample clamping members 8a and 8b which are flexibly moved even if the outer shape of the sample S is various. it can. For this reason, even if the sample S has various shapes like a tablet medicine, the sample S can be handled without difficulty.

  In the present embodiment, the sample holding members 8a and 8b are made flexible by the plurality of grooves 10 arranged radially in FIG. In this case, the outer peripheral portions of the sample clamping members 8a and 8b are not easily bent (that is, the rigidity is high), and the central portion is easily bent (that is, the rigidity is small). For this reason, the sample S tends to be pushed to the central part of the sample clamping members 8a and 8b according to the difference in the bending force of the sample clamping members 8a and 8b. That is, the sample clamping members 8a and 8b have a function of pushing the sample S to the central portion. This function is a positioning function for placing the sample S at a fixed position. If the positioning function by the sample clamping members 8a and 8b is sufficient, the positioning member 11 in FIG. 1 can be removed.

(Modification)
In FIG. 1, by changing the diameters of the holes 9a and 9b provided in the sample clamping members 8a and 8b, it is possible to deal with samples S having different sizes. Therefore, a plurality of sample clamping members 8a and 8b having holes 9a and 9b having different diameters are prepared in advance, and they are exchanged as appropriate to each of the first support member 2 and the second support member 3. By mounting and using, it can respond to various samples S having different sizes.

  Further, by changing the shape and number of the grooves 10 provided in the sample holding members 8a and 8b, the bending force (force required for bending) of the center portion of the sample holding members 8a and 8b can be changed. Samples S having different sheath shapes can be handled. Accordingly, a plurality of sample holding members 8a and 8b having different shapes and numbers of the grooves 10 are prepared in advance, and are exchanged as appropriate to each of the first support member 2 and the second support member 3. By mounting and using, various samples S having different shapes can be handled.

  In the above embodiment, the first support member 2 and the second support member 3 are coupled by the magnet 6. However, the configuration for coupling the first support member 2 and the second support member 3 may be any other configuration.

(Embodiment of X-ray analyzer)
In FIG. 3, an embodiment of the X-ray analysis apparatus according to the present invention includes an X-ray source 15, an X-ray detector 16, and a goniometer that individually rotates and moves the X-ray source 15 and the X-ray detector 16. That is, it has a goniometer / not shown. The goniometer individually rotates and moves the X-ray source 15 and the X-ray detector 16 about the axis line X1 extending in the direction perpendicular to the plane of the drawing in FIG. be able to.

  The X-ray source 15 includes, for example, a filament (cathode) that generates thermoelectrons when energized and a target (countercathode) that collides with thermoelectrons emitted from the filament. The X-ray detector 16 is, for example, a 0 (zero) -dimensional X-ray detector having no position resolution, a one-dimensional X-ray detector having a linear position resolution, or 2 having a planar position resolution. A dimensional X-ray detector or the like is used.

  In general, the X-ray source 15 is one element constituting the incident optical system. In addition to the X-ray source, the incident optical system includes other optical elements such as a slit, a solar slit, a monochromator, and a collimator. The goniometer described above can rotate the entire incident optical system as indicated by the arrow C-C ′ around the incident position P1 of the X-ray with respect to the sample S.

  The X-ray detector 16 is one element constituting the light receiving optical system. In addition to the X-ray detector, the light receiving optical system includes other optical elements such as a slit, a solar slit, a monochromator, an attenuator, and the like. The light receiving optical system can rotate and move as indicated by an arrow D-D ′ with the X-ray incident position P <b> 1 with respect to the sample S as the center.

  When performing measurement using X-rays on the sample S supported by the sample holder 1, an X-ray source 15 is arranged on one side of the sample holder 1, for example, as indicated by E in FIG. The X-ray detector 16 is arranged on the other side of the sample holder 1, the X-ray R0 emitted from the X-ray source 15 is incident on the sample S, and is diffracted by the sample S and emitted to the opposite side of the incident side. X-ray R1 can be detected by the X-ray detector 16. X-ray measurement according to this method is called transmission-type X-ray measurement.

  In the present embodiment, by operating the goniometer, both the X-ray source 15 and the X-ray detector 16 can be arranged on one same side of the sample holder 1 as indicated by the symbol F. In this state, the X-ray R00 emitted from the X-ray source 15 is incident on the sample S, and the diffracted X-ray R11 diffracted by the sample S and exiting to the same side as the incident side can be detected by the X-ray detector 16. X-ray measurement according to this method is called reflection-type X-ray measurement.

  In the X-ray analyzer according to the present embodiment, since the X-ray passing holes 9a and 9b are provided in both the sample clamping members 8a and 8b, the transmission X-ray measurement and the reflection X-ray measurement can be freely performed. Can be selected and executed.

(Embodiment of attachment for X-ray analyzer)
In general, the X-ray analysis apparatus includes various attachments, that is, replacement accessories. FIG. 4 shows a sample changer which is one of the attachments. The sample changer 20 is built in the base 21, a main body 22 protruding from the base 21, a guide member 23 for mounting the base 21 at a predetermined position of the X-ray analyzer, and the base 21. A locking handle 24 extending from the locking device and a turntable 25 rotatably attached to the main body 22 are provided.

  A rotation drive device for rotating the turntable 25 is incorporated in the main body 22. This rotary drive device is configured to include a motor capable of controlling the rotation angle, such as a servo motor or a pulse motor. The turntable 25 is driven by the rotation driving device and rotates at a desired angle around the center line X0.

  A plurality (ten in this embodiment) of holder mounting portions 28 are provided in the peripheral portion of the turntable 25. In the present embodiment, the holder mounting portion 28 is configured by a circular opening 29 opened in the turntable 25 and a holder support portion 30 formed in a ring shape by a material adsorbed on the magnet. By inserting the sample holder 1 shown in FIG. 3 into the opening 29 in FIG. 4, the sample holder 1 can be fixed to the holder support portion 30 by the action of the magnet 6 in FIG. 3.

  In FIG. 4, the position indicated by the arrow M, that is, the position closest to the base 21 among the rotational movement trajectories of the plurality of holder mounting portions 28 provided on the turntable 25 is the position for measuring the sample. . Hereinafter, this position is referred to as a measurement position M. FIG. 5 shows a configuration when the sample changer 20 of FIG. 4 is viewed from the back side. As shown in FIGS. 4 and 5, a through hole 30 penetrating the main body 22 back and forth is provided in the main body 22 corresponding to the measurement position M.

  The X-ray analyzer to which the sample changer 20 as an attachment is attached includes an X-ray source 15, an X-ray detector 16, and a goniometer (that is, a measurement) that individually rotates and moves the X-ray source 15 and the X-ray detector 16. Square tool / not shown). The goniometer is centered on an axis X1 extending in the vertical direction in FIG. 4 (corresponding to the X1 direction in FIG. 3) through the X-ray incident position P1 with respect to the sample S (see FIG. 3) set in the holder mounting portion 28. The radiation source 15 and the X-ray detector 16 can be individually rotated.

  When the measurement using the X-ray is performed on the sample S supported by the sample holder 1 (see FIG. 3) mounted on the holder mounting portion 28 at the measurement position M, for example, it is indicated by a symbol E in FIG. As described above, the X-ray source 15 is disposed on one side (the back side in FIG. 4) of the sample changer 20, and the X-ray detector 16 is disposed on the other side (the front side in FIG. 4) of the sample changer 20. The X-ray R0 emitted from the source 15 is incident on the sample S (see FIG. 3) through the through-hole 30, and the diffracted X-ray R1 diffracted by the sample S and exiting to the opposite side of the incident side is detected by the X-ray detector 16. it can. This X-ray measurement method is a transmission-type X-ray measurement.

  By operating the goniometer and rotating the X-ray source 15 and the X-ray detector 16 about the axis X1, both the X-ray source 15 and the X-ray detector 16 are sampled as indicated by the symbol F. It can be arranged on one same side of the changer 20 (the front side of the sample changer 20 in FIG. 4). In this state, the X-ray R00 emitted from the X-ray source 15 is incident on the sample S (see FIG. 3), and the diffracted X-ray R11 diffracted by the sample S and emitted to the same side as the incident side is detected by the X-ray detector 16. Can be detected. This X-ray measurement is a reflection type X-ray measurement.

(Second embodiment of sample holder for X-ray analyzer)
FIG. 6 is an exploded perspective view showing another embodiment of the sample holder for an X-ray analyzer according to the present invention. FIG. 7 shows a cross-sectional structure of the sample holder in a state where the sample holder is assembled. In the embodiment of FIG. 6, the same members as those of the previous embodiment shown in FIG.

  This embodiment is different from the embodiment shown in FIG. 1 in that a protruding edge 33 as a protruding portion is provided on the outer peripheral surface of the first support member 2. As shown in FIG. 7, when the second support member 3 is attracted to the first support member 2 by the magnet 6, the outer peripheral side surface of the second support member 3 is a protruding edge of the outer peripheral portion of the first support member 2. It is surrounded by 33 inner peripheral surfaces. Accordingly, the protruding edge 33 can prevent the second support member 3 from being displaced on the surface of the first support member 2. By preventing the displacement of the second support member 3 relative to the first support member 2, the sample S can be stably placed at a certain position. Note that the protruding edge 33 can be provided on the second support member 3 instead of being provided on the first support member 2.

  When the second support member 3 is accommodated in the protruding edge 33 of the first support member 2 as in the present embodiment, the second support member 3 is removed from the first support member 2. May be difficult. In order to solve this problem, in the present embodiment, a removal jig 34 that is a jig for removing the second support member 3 from the first support member 2 is prepared.

  The removal jig 34 includes a knob 35 that is a member that an operator picks with a finger, and a magnet 36 that is fixed to the tip of the knob 35. The knob portion 35 can be formed in a shape that is easy for an operator to pick, such as a prismatic shape or a cylindrical shape. The magnet 36 can be formed in a shape that is easily attracted to the surface of the second support member 3, for example, a prismatic shape or a cylindrical shape.

  The operator picks the knob 35 with his / her finger, attracts the magnet 36 to an appropriate position of the second support member 3, and then moves the knob 35 in a direction away from the first support member 2. Accordingly, the operator can easily remove the second support member 3 from the first support member 2 by the magnetic force of the magnet 36. In order to realize this operation, the magnetic force of the magnet 36 is desirably larger than the magnetic force of the magnet 6 in the first support member 2.

(Second embodiment of X-ray analyzer and attachment for X-ray analyzer)
FIG. 9 shows a second embodiment of the X-ray analyzer and the X-ray analyzer attachment according to the present invention. The X-ray analyzer 40 shown here has a goniometer 50 and a sample changer 100 as an attachment.

  The goniometer 50 has an incident side arm 51 and a light receiving side arm 52. These arms are actually formed by mechanical parts having high rigidity, but are shown by one line for convenience in FIG. The incident side arm 51 supports the X-ray tube 53. An X-ray source 54 is provided inside the X-ray tube 53. The light receiving side arm 52 supports the X-ray detector 55. The goniometer 50 can individually rotate and move the X-ray source 54 and the X-ray detector 55 around an axis X1 passing through a sample S placed at a measurement position M described later.

  The X-ray source 54 includes, for example, a filament (cathode) that generates thermoelectrons when energized and a target (countercathode) that collides with thermoelectrons emitted from the filament. The X-ray detector 55 is, for example, a 0 (zero) -dimensional X-ray detector having no position resolution, a one-dimensional X-ray detector having a linear position resolution, or 2 having a planar position resolution. A dimensional X-ray detector or the like is used.

  In general, the X-ray source 54 is one element constituting the incident optical system. In addition to the X-ray source, the incident optical system includes other optical elements such as a slit, a solar slit, a monochromator, and a collimator. The goniometer 50 described above can rotate the entire incident optical system as indicated by the arrow C-C 'about the axis X1.

  The X-ray detector 55 is one element constituting the light receiving optical system. In addition to the X-ray detector, the light receiving optical system includes other optical elements such as a slit, a solar slit, a monochromator, an attenuator, and the like. The light receiving optical system can be rotated about the axis X1 as indicated by an arrow D-D '.

  The sample changer 100 has a disk-shaped base 101. The base 101 includes a disk-shaped fixing base 102 and a disk-shaped rotating base 103 that is rotatably attached to the fixing base 102. A rotation support mechanism for rotatably supporting the rotation table 103 and a lock mechanism for prohibiting rotation of the rotation table 103 are provided between the fixing table 102 and the rotation table 103. A handle 104 extending from the locking mechanism is exposed to the outside of the fixing base 102. The lock mechanism can be turned on (ie, locked) by turning the handle 104 in either the forward or counterclockwise direction when viewed from the direction of the arrow H, and the handle 104 can be turned in the opposite direction. The lock mechanism can be turned off (ie, unlocked).

  A table support 105 is fixed to the surface of the turntable 103 of the base 101. The table support 105 extends forward of the turntable 103. A guided member 106 is fixed to the outer peripheral side surface of the fixing base 102 of the base 101. The guided member 106 extends to the side of the fixing base 102. The sample changer 100 is disposed at a predetermined position with respect to the goniometer 50 by inserting the guided member 106 into a guide member 57 provided on the surface of the face plate 56 integral with the goniometer 50.

  A part of the peripheral surface of the table support 105 is a flat surface, and a disk-shaped turntable 107 is provided on the flat surface. The turntable 107 is attached to the table support 105 so as to be rotatable about a center line X2 extending outward from the table support 105. Inside the table support 105, a rotation drive device for rotating the turntable 107 in-plane is incorporated. This rotary drive device is configured to include a motor capable of controlling the rotation angle, such as a servo motor or a pulse motor. The turntable 107 is driven by the rotation driving device and rotates at a desired angle around the center line X2. In addition, a rotation driving device for rotating the sample holder 1 in the plane is provided inside the table support 105. Thus, the sample holder 1 revolves by the rotation of the turntable 107 and rotates by the in-plane rotation.

  FIG. 9 shows a state in which the turntable 107 is leveled upward. The turntable 103 is fixed in this state by the handle 104, that is, locked. The locked state can be released by turning the handle 104 in the clockwise direction or the counterclockwise direction when viewed from the arrow H direction. After releasing the locked state, the operator can change the angle of the turntable 107 with respect to the horizontal by holding the table support 105 with his hand and rotating it in the direction of arrow J or arrow K.

  Then, after changing the angle, the turntable 107 can be fixed at the angular position by turning the handle 104 to lock the turntable 103. FIG. 10 shows a state in which the table support 105 is rotated in such a manner and the turntable 107 is leveled downward in the figure. In this state, by turning the handle 104 (see FIG. 9) to place the turntable 103 in a locked state, the turntable 107 can be placed in a horizontal state facing downward.

  FIG. 11A shows the turntable 107 viewed from the front. FIG.11 (b) is a side view according to the GG line in Fig.11 (a). In FIG. 11A, a plurality (six in this embodiment) of holder mounting portions 108 are provided on the peripheral portion of the surface of the turntable 107. In the present embodiment, the holder mounting portion 108 is configured by a circular opening 109 opened in the turntable 107 and a holder support portion 110 formed in a ring shape by a material adsorbed on the magnet. 9, the sample holder 1 is placed on the ring-shaped holder support portion 110 of the holder mounting portion 108 as indicated by an arrow L, so that the sample holder 1 is moved to the holder support portion by the action of the magnet 6 in FIGS. 110 can be fixed.

  In FIG. 11A, a plurality (four in the present embodiment) of positioning protrusions 111 are provided around the holder mounting portion 108. These positioning protrusions 111 are formed by a large diameter portion 112 fixed to the surface of the turntable 107 and a small diameter portion 113 provided on the large diameter portion 112. The twelve positioning protrusions 111a existing on the outside are provided two for each holder mounting part 108. On the other hand, the six positioning projections 111b existing inside are provided two by one with respect to one holder mounting portion 108, and each projection 111b is shared by two adjacent holder mounting portions 108. Is done.

  When the sample holder 1 is placed on the holder mounting portion 108 as indicated by a symbol L in FIG. 9, the bottom surface of the first support portion 2 of the sample holder 1 is supported by the holder mounting portion 108 as shown in FIG. Surface contact is made with the upper surface of the portion 110. And the outer peripheral side surface of the 1st support part 2 is positioned by the small diameter part 113 of the four protrusions 111 for positioning. That is, the positional deviation of the sample holder 1 is regulated by the four small diameter portions 113. As a result, the sample holder 1 can always be stably placed at a fixed position on the turntable 107.

  When removing the sample holder 1 from the holder mounting portion 108, the operator puts a finger, for example, a thumb between two adjacent positioning projections 111 b adjacent to each other and places the finger on the outer peripheral side surface of the sample holder 1. . Further, the operator puts another finger, for example, the index finger or the middle finger between the two outer positioning projections 111 a facing each other and places the finger on the outer peripheral side surface of the sample holder 1. Thereby, the sample holder 1 is picked by the operator's finger. Thereafter, the operator picks up the sample holder 1 with his / her thumb and removes the sample holder 1 from the holder mounting portion 108. As described above, the operator can attach and remove the sample holder 1 with his / her finger placed between the four positioning projections 111, so that the attaching and removing operations are very easy.

  9 and 11A, the sample is measured at the position indicated by the arrow M, that is, the position closest to the base 101 among the rotational movement trajectories of the plurality of holder mounting portions 108 provided on the turntable 107. It is a position to do. Hereinafter, this position is referred to as a measurement position M. As shown in FIG. 10, a portion of the table support 105 corresponding to the measurement position M is provided with a through hole 114 that passes through the table support 105 in the vertical direction in the figure.

  In FIG. 9, when performing measurement using X-rays on the sample S supported by the sample holder 1 mounted on the holder mounting portion 108 at the measurement position M, particularly X-ray measurement of the reflection method, for example, FIG. 9, the X-ray source 54 is arranged on one side of the sample changer 100 (in FIG. 9, the upper side of the sample changer 100) as indicated by reference numeral 54 (F), and the reference to the sample changer 100 as indicated by reference numeral 55 (F). The X-ray detector 55 is arranged on the same side (the upper side of the sample changer 100 in FIG. 9). In this state, the X-ray R0 emitted from the X-ray source 54 is incident on the sample S, and the X-ray detector 55 detects the diffracted X-ray R1 that is diffracted by the sample S and travels in the direction reflected by the sample S. To do.

  On the other hand, when performing transmission type X-ray measurement, the handle 104 is operated to release the locked state of the turntable 103, and the turntable 107 is placed in a horizontal state with the turntable 107 facing downward as shown in FIG. In this state, the handle 104 (see FIG. 9) is operated to set the turntable 103 to the locked state, and the position of the turntable 107 is fixed.

  Then, the goniometer 50 is operated to rotate the X-ray tube 53 upward (in the direction of the arrow C ′), so that the X-ray source 54 is arranged at a position immediately above indicated by reference numeral (E) as shown in FIG. Further, in FIG. 9, the goniometer 50 is operated to rotate the X-ray detector 55 downward (in the direction of the arrow D ′), and as shown in FIG. 10, the X-ray detector 55 is directly below indicated by the symbol (E). Place in position. In this state, the X-ray R0 emitted from the X-ray source 54 is incident on the sample S, and the X-ray detector 55 detects the diffracted X-ray R1 that is diffracted by the sample S and travels in the direction passing through the sample S. To do. When this transmission type X-ray measurement is performed, as shown in FIG. 8, the sample holder 1 is inverted by 180 ° as compared with the case of the reflection type shown in FIG.

  When the angle of the turntable 107 with respect to the horizontal is changed between when the reflection type X-ray diffraction measurement is performed and when the transmission type X-ray diffraction measurement is performed, the angle to be changed is inverted by 180 ° as described above. It is not restricted to, It can be set as the arbitrary inclination angles as needed.

  If the X-ray detector 55 is transported from the angular position shown in FIG. 9 to a position directly below as shown in FIG. 10 with the table support 105 placed in a region below the goniometer 50 as shown in FIG. In order to prevent the X-ray detector 55 from colliding with the table support 105, it is necessary to increase the turning radius of the X-ray detector 55 by the goniometer 50. On the other hand, in the X-ray analyzer 40 of the present embodiment, the table support 105 is inverted to the upper position as shown in FIG. 10 when performing transmission X-ray measurement, as shown in FIG. Compared with the case where the table support body 105 is placed at the lower position, the space in the lower area of the goniometer 50 is greatly opened. For this reason, even when the turning radius of the X-ray detector 55 by the goniometer 50 is set to be small, the X-ray detector 55 can be disposed at a position directly below as shown in FIG.

(Other embodiments)
The present invention has been described with reference to preferred embodiments with respect to each of the sample holder, attachment, and X-ray analyzer. However, the present invention is not limited to these embodiments, and the invention described in the claims. Various modifications can be made within the range.

  For example, the sample holder is not limited to the configuration shown in FIGS. 1 to 3 and the configuration shown in FIG. 6, and can be appropriately modified. For example, each member constituting the sample holder 1 in FIG. 1 or FIG. 6 can have an arbitrary planar shape other than a circular shape.

  Further, the attachment of the present invention is not limited to the sample changer having the configuration shown in FIGS. 4 and 5 and the sample changer having the configuration shown in FIGS. 9 and 10, and may be an attachment that realizes other arbitrary functions. good.

  1. 1. Sample holder, A first support member, 2a. 2. recess, A second support member, 3a. Recess, 4. Step part, 5. Step part, 6. Magnets, 8a, 8b. Sample clamping member, 9a, 9b. Hole, 10. Groove, 11. Positioning member, 12. Hole, 15. X-ray source, 16. X-ray detector, 20. 20. Sample changer (attachment) Base, 22. Body, 23. Guide member, 24. Lock handle, 25. Turntable, 28. Holder mounting portion, 29. Opening, 30. Through hole, 33. Protruding edge, 34. Removal jig, 35. Knob part, 36. Magnet, 40. X-ray analyzer, 50. Goniometer, 51. Incident side arm, 52. Light receiving side arm 53. X-ray tube, 54. X-ray source, 55. X-ray detector, 56. Face plate, 57. Guide member, 100. Sample changer (attachment), 101. Base, 102. Fixing base, 103. Turntable, 104. Handle, 105. Table support, 106. Guided member, 107. Turntable, 108. 109. holder mounting part; Opening, 110. Holder support, 111. Positioning protrusion, 112. Large diameter part, 113. Small diameter portion, 114. Through hole

Claims (11)

In the sample holder that supports the sample and is attached to and detached from the X-ray analyzer,
Having a pair of sample clamping members for supporting the sample from both sides;
The sample clamping member is a plate-like member having a planar shape wider than the sample, a thickness thinner than the sample, and having flexibility,
At least one of the pair of sample clamping members is provided with a hole for transmitting X-rays ,
The sample holder for an X-ray analyzer , wherein the sample holding member is made flexible by forming a plurality of grooves extending radially from the hole in the sample holding member . A first support member that supports one of the pair of sample clamping members so as to bend and move;
A second support member that supports the other of the pair of sample clamping members to bend and move, and
Said first support member and the second support member is X-ray analysis apparatus for sample holder of claim 1 Symbol mounting, characterized in that it is coupled in the pair of sample clamping members are opposed to each other. A magnet is provided on one of the first support member and the second support member, and the other of the first support member and the second support member has a property of adsorbing to the magnet. The sample holder for an X-ray analyzer according to claim 2 , wherein the sample holder is an X-ray analyzer. A detaching jig provided with a magnet; and the first supporting member and the first detaching jig by the detaching jig in a state where the magnet is attracted to the first supporting member or the second supporting member. The sample holder for an X-ray analyzer according to claim 2 or 3, wherein the two support members are separated from each other. The protrusion part for controlling the position shift of the other party support member was provided on the outer peripheral surface of the said 1st support member or the said 2nd support member, The any one of Claim 2 to 4 characterized by the above-mentioned. The sample holder for X-ray analyzers as described in one. The sample holder for an X-ray analyzer according to any one of claims 1 to 5 , wherein a positioning member for positioning the sample is provided between the pair of sample clamping members. . The X-ray analyzer according to claim 6 , wherein the positioning member is a plate-like member thinner than the sample, and has a hole for storing a sample having a diameter slightly larger than the sample. Sample holder. An X-ray analyzer attachment comprising the sample holder according to any one of claims 1 to 7 . A turntable having a plurality of holder mounting portions; and a plurality of positioning protrusions provided around the plurality of holder mounting portions;
The sample holder is attracted to the holder mounting portion by magnetic force, and the adsorbed sample holder is positioned by being surrounded by the positioning projections,
9. The attachment for an X-ray analyzer according to claim 8, wherein four positioning protrusions are provided for one of the holder mounting portions. The attachment according to claim 8, an X-ray source that generates X-rays for irradiating the sample, and an X-ray detection unit that detects X-rays emitted from the sample,
The attachment has a turntable with a plurality of holder mounting portions,
The attachment selectively places a sample included in one of the plurality of holder mounting portions at a position irradiated with X-rays generated by the X-ray source by rotating the turntable in-plane. X-ray analyzer. A goniometer that measures the angle of the X-ray source and the angle of the X-ray detection means about the rotation center line passing through the sample placed at the position irradiated by the X-ray;
The attachment is
A table support that supports the turntable in an in-plane rotation;
Table rotating means for rotating the table support around a line passing through the sample;
Locking means for fixing the position of the table support rotated by the table rotating means,
The table support is the table when the X-ray source and the X-ray detection means are arranged in a reflective manner and when the X-ray source and the X-ray detection means are arranged in a transmissive manner. 11. The X-ray analyzer according to claim 10, wherein the X-ray analyzer is rotated to different angular positions by the rotating means and fixed by the locking means at the rotated position.

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