JPH07294400A - Sample retention device for x-ray diffraction device - Google Patents

Abstract

PURPOSE:To automate the zero-point matching of a sample holder and to easily and rapidly detect the orientation property of a sample and the array direction of a crystal. CONSTITUTION:A sample holder fitting member 330 is attracted and fixed to a rotary member 350 installed at the inspection position of a tool body 310 by magnetic force. A plurality of magnets 342 are provided at a sample holder 340 for fitting a sample and one of the magnets is used as a reference index. The sample holder 340 is attracted and fixed to the sample holder fitting member 330 by the magnets 342 and are rotated in one piece along with the rotary member 350 and the sample holder fitting member 330. A magnetic sensor 500 is installed at the zero-point position of the rotary operation and the magnetic force of the magnet 342a which is the reference index is detected, thus performing the zero-point matching of the sample holder 340.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sample holding device which is mounted on a base of a goniometer in an X-ray diffractometer and rotatably supports a sample.

[0002]

2. Description of the Related Art An X-ray diffractometer is equipped with a goniometer, which is rotatable with respect to an X-ray source, and a sample holder is mounted on the base of this goniometer. This is an apparatus for irradiating the held sample with X-rays and detecting the X-rays diffracted from the sample (diffracted X-rays) to analyze the sample based on the detection angle and the like.

For a sample having grain orientation such as a rolled material, it may be desired to detect the orientation of the orientation. For example, when a rolled material is formed by squeezing, the strength of the product changes greatly depending on the orientation of the particles and the adjustment of the squeezing direction. Therefore, it is important to detect the orientation of particles and adjust the direction of squeezing to this in order to improve product quality. Further, in the manufacture of the crystal oscillator, since the cut surface has to be aligned with the crystal array direction, it is necessary to detect the crystal array direction in advance. Thus, in order to detect the orientation direction of particles, the orientation direction of crystals, and the like, X-ray diffraction measurement is performed while rotating the sample with respect to the sample holding device, and the rotation angle at which the peak value of the diffracted X-ray is obtained You have to measure.

FIG. 9 is a front view showing a conventional rotary sample holder which can perform this type of measurement. In the conventional rotary sample holding device shown in the figure, a sample stage 900 and a sample rotating jig 901 are integrally formed, and the device as a whole is mounted on a base 902 of a goniometer. A sample holder 903 is attracted and fixed to a sample rotating jig 901 by a magnet (not shown), and the sample holder 903 is rotationally driven about an axis by a rotating unit (not shown). As the sample holder 903 rotates, the orientation of the particles and crystals of the sample S with respect to the incident X-ray changes. When the X-ray incident direction matches the grain orientation or crystal arrangement direction, a peak value of the diffracted X-ray intensity appears, which allows the orientation of the sample or the crystal arrangement direction to be detected.

Here, the orientation of the sample, the array direction of the crystals, and the like are recognized by the rotation angle from a predetermined origin. That is, the position where the reference point 903a formed on the sample holder 903 is aligned with the origin 901a formed on the sample rotating jig 901 is set to zero, and the sample holder 9 is set.
The rotation angle of No. 03 is detected, and the orientation of the sample, the crystal arrangement direction, and the like are detected by the rotation angle when the peak value of the diffracted X-ray intensity appears.

[0006]

Conventionally, a sample rotating jig 9 has been used.
The operation of aligning the origin 901a formed at 01 with the reference point 903a formed at the sample holder 903 (hereinafter, referred to as "origin alignment") was performed manually by the operator's eyes. However, since a protector for X-ray shielding is arranged around the sample holding device, and the peripheral structure is such that it is difficult for the operator to approach the face to the position where the sample holder 903 is fixed by suction, the origin adjustment is performed. Was an unexpectedly cumbersome and time-consuming task.

Further, in recent years, a multi-sample holding device for automatically processing X-ray diffraction measurement of multi-samples has attracted attention. According to this multi-sample holding device, the plurality of sample holders are rotatably transferred, so that they can be sequentially arranged at predetermined inspection positions and X-ray diffraction measurement can be performed. However, in this multi-sample holding device, the origin is manually adjusted every time the sample holder is placed at the inspection position, so that the original feature of this device is to automate the X-ray diffraction measurement of a plurality of samples. I can't. The present invention has been made in view of the above circumstances, and provides a sample holding device for an X-ray diffractometer capable of automatically adjusting the origin of the sample holder and easily and quickly detecting the orientation of the sample, the crystal arrangement direction, and the like. The purpose is to provide.

[0008]

In order to achieve the above object, a first aspect of the present invention is to provide a sample table installed on a base of a goniometer rotatable with respect to an X-ray source, and a jig installed on the sample table. A tool main body, a rotary drive source mounted on the jig main body, a tubular rotary member rotatably provided on the jig main body via a bearing and rotating about an axis by a driving force from the rotary drive source,
It is characterized by comprising a sample holder that is attracted and fixed to one end of the rotating member by a magnetic force, and an origin aligning unit that positions a reference index provided on the sample holder at a predetermined origin.

A second aspect of the present invention is to provide a sample table installed on a base of a goniometer rotatable with respect to an X-ray source, a plurality of sample holders for mounting samples, and a jig body mounted on the sample table. And a rotary plate rotatably supported on the jig body, a first rotary drive source for rotationally driving the rotary plate, and a plurality of rotary plates mounted on the same diameter of the rotary plate so as to be rotatable about their respective axes. Sample holder mounting member, holder mounting means for attracting and fixing the sample holder to one end surface of the sample holder mounting member by magnetic force, and the sample holder mounting member is positioned substantially on the rotation path and rotatably supported by the jig body. And a second rotary drive source that drives the rotary member to rotate, and a member that attaches the one sample holder mounting member that has rotationally moved substantially coaxially to the rotary member by magnetic attraction to the end surface of the rotary member. Contact Characterized by comprising means, the origin alignment means for positioning the reference index provided on the sample holder to a predetermined origin.

In these first and second inventions, the origin adjusting means of the sample holder may be a sensor for detecting a reference index provided on the sample holder at the origin position.
Further, the sample holder is provided with a plurality of magnets, the sample holder is attracted and fixed by the magnets, and one of the magnets is formed so as to be closer to the sensor than the other magnets and is used as a reference index. You can In this case, the sensor that detects the reference index at the origin position may detect the magnetic force generated from the magnet that serves as the reference index.

Further, in addition to the origin adjustment of the sample holder by the sensor, the axial position of the sample holder is determined by the strength of the magnetic force emitted from the magnet serving as a reference index with reference to the sample holder suction-fixed at an appropriate position. The shift may also be detected.

[0012]

In the first aspect of the invention described above, the sample table is set on the base of the goniometer, and the jig body is mounted on the sample table. The sample holder on which the sample is mounted is attracted and fixed by magnetic force to one end of a rotating member provided on the jig body. The sample holder thus fixed by suction rotates together with the rotating member to change the direction of the sample with respect to the incident X-ray. Prior to the rotation of the sample holder, the origin of the rotation angle must be set. The origin adjustment of the sample holder is automatically performed by positioning the reference sample provided on the sample holder at a predetermined origin by the origin adjusting means.

Also in the second invention, the sample table is set on the base of the goniometer, and the jig body is mounted on the sample table. The plurality of sample holders on which the samples are mounted are fixed by suction to one end surface of the sample holder mounting member by holder mounting means utilizing magnetic force. Each sample holder mounting member to which the sample holder is sucked and fixed is rotationally driven together with the rotary plate by the first rotary drive source, and when it comes to a position where it comes into contact with or faces the end face of the rotary member, the member connecting means utilizing magnetic force It is adsorbed and fixed to the end surface of the rotating member.

Since the rotary member, the sample holder mounting member and the sample holder are integrated in this way, when the rotary member is rotationally driven by the second rotary drive source, the sample holder rotates together with the rotary member and the incident X Change the orientation of the sample with respect to the line. Prior to the rotation of the sample holder, the origin of the rotation angle must be set. This origin alignment is automatically performed by positioning the reference sample provided on the sample holder at a predetermined origin by the origin alignment means.

The origin adjustment means includes a micro switch,
Various contact and non-contact sensors such as an optical sensor and a magnetic sensor can be used. For example, a protrusion may be formed as a reference index on the sample holder, and the reference index may be detected by contacting the protrusion with the microswitch at a predetermined origin position. Further, when using the optical sensor, the protrusion may be optically detected at the origin position. If a plurality of magnets are used to attract and fix the sample holder to the rotating member or the sample holder mounting member, and if one of the magnets is formed so as to be close to the sensor as a reference index, the magnet serving as the reference index When it comes to the origin position, the magnetic force generated from the magnet is detected by the magnetic sensor provided at the origin position,
The origin can be adjusted. The origin position may be set at any position on the circumference of the sample holder.

Further, when the sample holder is not properly attracted and fixed to the rotating member or the sample holder mounting member and the position of the sample holder is displaced in the axial direction, when the magnet serving as the reference index comes to the origin position, the magnetic sensor. The strength of the magnetic force detected by will fluctuate compared to the case where it is appropriate. Therefore, by examining the strength of the magnetic force detected by the magnetic sensor, the positional displacement of the sample holder in the axial direction can be detected.

[0017]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention will be described in detail below with reference to the drawings. FIG. 1 is a vertical sectional view showing a sample holding device according to a first embodiment of the present invention. The sample holding device of this embodiment includes the sample stage 1, the sample rotating jig 2, the sample holder 3, and the X-ray shielding member 4.

The sample table 1 has a structure in which a support block 11 for supporting the sample rotating jig 2 is provided at the center of the upper surface of a bottom plate 10 formed in a disk shape. A protrusion 12 for positioning and fixing projects from the center of the bottom surface of the bottom plate 10, and the protrusion 12 is fitted into a mounting recess 51 formed in the base 5 of the goniometer in the X-ray diffractometer. It can be attached to the table 5. The fitting precision between the protrusion 12 and the mounting recess 51 is, for example, about 3/1000 mm. This fitting portion is formed coaxially with the rotation center of the base 5 of the goniometer.

A mounting portion 13 for the sample rotating jig 2 is formed on the upper end of the support block 11 of the sample table 1. The mounting portion 13 has a jig body 2 of a sample rotating jig 2 to be described later.
A plane portion 14 on which 0 is mounted and a reference surface 15 which is a reference position of the sample are formed. The reference surface 15 is provided with, for example, a fastening hole 15a as a fastening portion of the sample rotating jig 2, and the sample rotating jig 2 can be fixed by a fastener such as a bolt 201. In addition, the reference surface 15 is the protrusion 12
It is formed on the same plane as the center of. As will be described later, the surface of the sample S mounted on the sample holder 3 is the reference surface 1
It is positioned so as to be flush with the surface of the sample table 5, and is thereby placed on the center axis of rotation of the sample table 1.

As shown in FIGS. 2 and 3, the sample rotating jig 2 has a rotary driving source 21 such as an electric motor mounted on the bottom of the jig body 20 and a rotating member 23 rotated via a bearing 22. Supports freely. Side wall 2 of jig body 20
0a is provided with, for example, a screw hole 20b as a fixing means to the fastening portion (fastening hole 15a) provided on the reference surface 15 of the sample table 1 described above. That is, in this embodiment, the fastening hole 15a and the screw hole 20b are opposed to each other with the side wall 20a of the jig body 20 in contact with the reference surface 15 of the sample table 1.
The bolt 201 is passed through the fastening hole 15a to form the screw hole 20b.
The sample rotating jig 2 is fixed to the sample table 1 by screwing the sample rotating jig 2 onto the sample table 1.

A drive gear 24 is attached to the drive shaft 21a of the rotary drive source 21, while a driven gear 25 is provided on the peripheral wall of the rotary member 23. The drive gear 24 and the driven gear 25 mesh with each other to rotate. The driving force from the driving source 21 is transmitted to the rotating member 23.

The rotating member 23 is formed in a cylindrical shape, and the hollow portion forms an X-ray transmitting hole 26. This X-ray transmission hole 26 is necessary when performing a measurement method (transmission method) of irradiating the sample S with X-rays from the back side and detecting the X-rays that have transmitted through the sample S. The inner diameter of the X-ray transmission hole 26 is preferably set to be larger than at least the entire width of the X-ray guided from the X-ray source through the divergence slit. By setting the inner diameter of the X-ray transmission hole 26 in this way, X-rays from the X-ray source can be transmitted without interruption.

In the X-ray diffractometer currently on the market, X
The irradiation width of X-rays irradiated from the radiation source to the sample on the sample holding device through the divergence slit is about 24 mm.
When the apparatus of this embodiment is applied to this type of X-ray diffraction apparatus, the inner diameter of the X-ray transmission hole 26 may be set to about 24 mm. Further, at one end of the rotating member 23, the sample holder mounting portion 27 is formed of a magnetic material such as a steel material. Since it is complicated to form the sample holder mounting portion 27 only with a different type member (magnetic material), it is preferable to form the entire rotary member 23 including the sample holder mounting portion 27 with a magnetic material.

As shown in FIG. 4, the sample holder 3 is formed in a stepped ring shape, and the hollow portion serves as the sample mounting portion 30. The inner diameter of the sample mounting portion 30 is substantially the same as that of the X-ray transmission hole 26 formed in the rotating member 23. The sample holder 3 is made of a material such as aluminum alloy or plastic that has a small reflection of X-rays, and is formed to have a thickness of about 3 mm. In addition, the stepped portion narrows the surface area near the sample surface and suppresses the reflection of X-rays. Magnets 31 are embedded in the sample holder 3 at a plurality of locations (two locations in the figure) with their end surfaces exposed. The sample holder 3 can be attracted and fixed to the sample holder mounting portion 27 made of a magnetic material by the magnetic force of these magnets 31.

Also, one of these magnets 31a
Is a reference index for origin alignment regarding the rotation operation of the sample holder 3. A magnetic sensor 16 is installed on the sample table 1. The magnetic sensor 16 is arranged so as to face the peripheral surface of the sample holder 3 which is suction-fixed to the sample holder mounting portion 27 at an arbitrary position. This magnetic sensor 1
The position facing 6 is the origin for the rotation operation of the sample holder 3.

The thickness of the magnet 31a used as a reference index is adjusted so as to pass through the proximity position facing the magnetic sensor 16 as the rotating member 23 rotates, and the sample holder 3
It is arranged so as to project from the peripheral surface of the. On the other hand, the magnet 31 not serving as a reference index is formed shorter than the magnet 31a, and is adjusted so as to pass a position that deviates from the detection area of the magnetic sensor 16. In this embodiment, the magnet 31a, which serves as the reference index, and the magnetic sensor 16 constitute an origin aligning unit for the rotation operation of the sample holder 3.

The X-ray shielding member 4 is formed in a cylindrical shape with a lid as shown in FIG.
The lower end opening is fitted to the peripheral surface of 0, and a fastener 41 such as a screw is attached.
The structure is fixed by. Sample rotation jig 2
Are stored inside the X-ray shielding member 4. The X-ray shielding member 4 is made of a material capable of shielding X-rays, for example, a non-ferrous material such as brass or copper alloy. Lead is generally used as the material of the X-ray shielding member 4, but brass can sufficiently achieve the purpose for shielding the weak X-rays emitted from the sample during the X-ray diffraction measurement. . Needless to say, the X-ray shielding member 4 may be made of lead or lead alloy. The wall pressure of the X-ray shielding member 4 is appropriately determined according to the intensity of X-rays emitted from the sample S.

The X-ray shielding member 4 is provided with an X-ray transmission window 42. The X-rays from the X-ray source are guided to the sample S through the X-ray transmission window 42, and the diffracted X-rays emitted from the sample S are transmitted. It is designed to lead to an X-ray detector.

Next, the operation of the sample holding device according to the first embodiment described above will be described. To mount the apparatus of this embodiment on the base 5 of the goniometer in the X-ray diffraction apparatus, the sample table 1
The protrusion 12 provided on the bottom plate 10 may be fitted into the mounting recess 51 formed on the base 5 of the goniometer. Once this mounting is performed, even if it becomes necessary to remove the sample rotating jig 2 for maintenance or the like thereafter, the sample stage 1 can be left as it is and only the sample rotating fixture 2 can be removed from the sample stage 1. The attachment / detachment work becomes easy.

That is, the sample table 1 and the goniometer base 5
Since, as described above, there is a high degree of fitting accuracy, it is necessary to perform a high degree of alignment during mounting. On the other hand, since a simple attachment / detachment structure such as fastening with a bolt 60 may be provided between the sample table 1 and the sample rotating jig 2,
Easy to install. By the way, in order to detect the incident angle of X-rays on the sample S and the output angle of the diffracted X-rays with the goniometer, the surface of the sample S must be placed on the rotation center of the pedestal 5 of the goniometer. In this embodiment, since the reference surface 15 of the sample base 1 is formed so as to be flush with the rotation center of the base 5 of the goniometer, the surface 3a of the sample holder 3 positioned on the reference surface 15, that is, The surface Sa of the sample S is inevitably arranged on the central axis of rotation of the goniometer.

Further, in the sample holder of this embodiment, the X-ray shielding member 4 can be mounted on the sample table 1, so that the X-rays scattered from the sample S are efficiently distributed around the sample rotating jig 2. It can be shielded against radiation and the safety against X-ray exposure is improved. The following procedure is performed to detect the orientation of the sample S, the crystal orientation direction, and the like. First, after mounting the sample on the sample holder 3, the sample holder 3 is mounted on the sample holder mounting portion 27. At this time, the sample holder 3 includes the magnets 31 and 31a.
Since it is adsorbed and fixed to the sample holder mounting portion 27 by the magnetic force of 1, the troublesome work such as screwing is unnecessary.

Next, the rotary member 23 is rotated by the driving force of the rotary drive source 21. Then, the sample holder 3 rotates together with the rotating member 23. When the magnet 31a serving as the reference index reaches the position (origin) facing the magnetic sensor 16, the magnetic sensor 16 causes the magnet 31a to move.
The magnetic force generated by a is detected. The attitude of the sample holder 3 at the time of this detection is set to zero, and the rotation angle of the sample holder 3 is measured and X-ray diffraction measurement is performed. Then, if the rotation angle when the peak value of the diffracted X-ray is detected is calculated, from the relationship between this rotation angle and the incident angle of the X-ray,
It is possible to detect the orientation of the sample S, the crystal arrangement direction, and the like.

Next, a second embodiment of the present invention will be described. FIG. 5 is a vertical sectional view showing a sample holding device according to the second embodiment of the present invention. The sample holding device of this embodiment is
The sample stage 200, the sample rotating jig 300, and the X-ray shielding member 400 are provided as constituent elements, and a plurality of sample holders 340 can be mounted as described later.

The sample table 200 has a disk-shaped bottom plate 2
A support block 202 for supporting the sample rotating jig 300 is provided at the center of the upper surface of 01. A protrusion 203 for positioning and fixing projects from the center of the bottom surface of the bottom plate 201, and the base 100 of the goniometer in the X-ray diffractometer is used.
By fitting the projection 203 into the mounting recess 100a formed in the above, the mounting base 100 can be mounted. The fitting precision between the protrusion 203 and the mounting recess 100a is, for example, about 3/1000 mm. This fitting portion is formed coaxially with the rotation center of the base 100 of the goniometer.

At the upper end of the support block of the sample table 200,
A mounting portion 204 for mounting the sample rotating jig 300 is formed. A flat surface portion 205 and a reference surface 206 are formed on the mounting portion 204, and a jig body 310 of a sample rotating jig 300, which will be described later, is mounted on the flat surface portion 205. The reference surface 206 serves as a positioning reference for the mounted sample rotating jig 300. Further, on the reference surface 206, the sample rotating jig 300
As a fixing means of, for example, a fastening hole 207 is provided,
The sample rotating jig 300 can be fixed by a fastener 208 such as a bolt. The reference surface 206 is formed on the same plane as the above-mentioned protrusion 203.

The sample rotating jig 300 comprises a jig body 310,
The rotary plate 320, the sample holder mounting member 330, the sample holder 340, and the rotating member 350 are provided. The lower side surface of the jig body 310 forms a positioning surface 310 a that comes into contact with the reference surface 206 of the sample table 200.
A screw hole 318 into which the fastener 208 is screwed is formed on the positioning surface 310a.

Further, the jig body 310 has a bearing 311 on the top.
The bearing 311 rotatably supports the rotating shaft 312. The rotary plate 32 is attached to the tip of the rotary shaft 312.
0 is fixed, and a wheel gear 313 is attached to the base end. The wheel gear 313 meshes with a worm gear 315 attached to the drive shaft of a first drive motor (first rotary drive source) 314. The rotational drive force from the first drive motor 314 is applied to the worm gear 31.
5 and the wheel gear 313 to be transmitted to the rotary shaft 312 to rotate the rotary plate 320.

The first drive motor 314 is provided with a rotation speed detection sensor 316 such as an encoder, and a control circuit (not shown) calculates the rotation angle of the rotary plate 320 based on the detection signal from the sensor 316. It has become. Reference numeral 317 is a date sensor that detects one rotation of the rotating plate to detect that a predetermined reference sample holder mounting member is fixed to a rotating member described later.

As shown in FIGS. 5 and 6, a plurality of (four in the figure) sample holder mounting members 330 are rotatably attached to the rotary plate 320 with an arbitrary amount of play. That is, as shown in an enlarged manner in FIG. 4, the rotary plate 320 is provided with a plurality of member mounting holes 321 on the same diameter. On the other hand, the sample holder mounting member 330 is formed in a cylindrical shape having a short axial length, and an engaging groove 331 for engaging the rotating plate 320 is formed in the circumferential direction on the outer periphery thereof.

Here, the diameter up to the upper edge of the engagement groove 331 formed in the sample holder mounting member 330 is longer than the inner diameter of the member mounting hole 321 formed in the rotary plate 320 by an arbitrary dimension. The diameter up to the bottom surface of the engaging groove 331 is shorter than the inner diameter of the member mounting hole 321 by an arbitrary dimension. Therefore, the sample holder mounting member 330 is mounted with play and is rotatable within the member mounting hole 321.

Around each sample holder mounting member 330,
A plurality (three in FIG. 6) of holder support protrusions 322 are projected from the rotary plate 320. This holder support protrusion 32
2 is a mounting surface 33 of a sample holder mounting member 330, which will be described later.
The purpose of this is to prevent the sample holder 340 attached to 0a from being detached from the sample holder 340 and to reduce the eccentricity deviation when rotating. Further, the sample holder mounting member 33
The width of the engaging groove 331 formed in 0 is wider than the thickness of the rotary plate 320 by an arbitrary dimension, and the sample holder mounting member 330 is movable in the axial direction within the member mounting hole 321 by this dimension difference. (See Figure 8).

The hollow portion of the sample holder mounting member 330 is an X-ray transmission hole 332 penetrating from one end in the axial direction to the other end. The X-ray transmission hole 332 enables the above-mentioned transmission method measurement, and is formed to have a diameter capable of transmitting the X-ray emitted from the X-ray source over almost the entire width. In the X-ray diffractometer currently on the market, the irradiation width of the X-ray irradiated from the X-ray source to the sample S on the sample holding device through the divergence slit is about 24 mm. Therefore, this kind of X
When the apparatus of this embodiment is applied to the line diffraction apparatus, the inner diameter of the X-ray transmission hole 332 may be set to about 24 mm.

The sample holder mounting member 330 is made of a magnetic material attracted by a magnet, and is highly accurately chamfered so that both axial end surfaces are parallel to each other. further,
Each sample holder mounting member 3 mounted on the rotary plate 320
The 30 are mutually faced so as to have a thickness with no dimensional difference. Then, one of the chamfered end faces is a mounting face 330a of the sample holder 340, and the other end face is a fixed face 330b to the rotating member 350 described later (see FIG. 8).

The sample holder 340 is formed in a stepped ring shape as shown in FIG. 7, the outer diameter of which is approximately the same as the outer diameter of the sample holder mounting member 330, and the inner diameter is the same mounting member 330. The size is almost the same as the inner diameter of the X-ray transmission hole 332. The hollow portion of the sample holder penetrating in the axial direction serves as a sample mounting portion 341 for mounting the sample S. The sample holder 340 is made of a material such as aluminum alloy or plastic that has a small X-ray reflection, and is formed to have a thickness of about 3 mm. In addition, the stepped portion narrows the surface area near the sample surface and suppresses the reflection of X-rays. Magnets 342 are embedded in the sample holder 340 at a plurality of locations (two locations in this embodiment) with their end faces exposed.
The sample holder 340 can be attracted and fixed to the sample holder mounting member 330 made of a magnetic material by the magnetic force of these magnets 342.

Also, one of these magnets 342a
Is a reference index for origin alignment regarding the rotation operation of the sample holder 340. A magnetic sensor 500 is installed on the sample table 200. The magnetic sensor 500 includes a sample holder 3 attached to a sample holder mounting member 330 by suction.
It is arranged so as to face the peripheral surface of 40 at an arbitrary position. The position facing the magnetic sensor 500 is the origin for the rotation operation of the sample holder 340.

The magnet 342a used as a reference index has its thickness adjusted so as to pass through the proximity position facing the magnetic sensor 500 as the rotary plate 320 rotates, and is arranged so as to project from the peripheral surface of the sample holder 3. There is. On the other hand, the magnet 342 that is not the reference index is
It is formed shorter than 2a, and is adjusted so as to pass a position deviating from the detection region of the magnetic sensor 500. In this embodiment, the magnet 342a, which serves as the reference index, and the magnetic sensor 500 constitute the origin aligning means for the rotation operation of the sample holder 340.

The sample holder 340 is highly accurately chamfered so that at least one end surface (preferably both end surfaces) in the axial direction is orthogonal to the axis, and the chamfered one end surface is the sample holder mounting member 330. It is a surface 340a to be mounted on the (see FIG. 8). Then, on the peripheral wall of the sample holder 340, the magnets 3 as holder mounting means are provided at a plurality of places.
42 is buried with the end surface exposed, and has a structure in which the mounted surface 340a is attracted and fixed to the mounting surface 330a of the sample holder mounting member 330 by magnetic force.

The rotary member 350 is formed in a tubular shape as shown in FIG. 5, and is rotatably supported at the bottom of the jig body 310 via a bearing 351. One end surface of the rotating member is a fixed surface 350a of the sample holder mounting member 330, and this fixed surface 350a is precisely faced so as to be orthogonal to the axis (see FIG. 8). The outer diameter of the fixed surface 350 a is the same as the fixed surface 33 formed on the sample holder mounting member 330.
The size is set to be almost the same as the outer diameter of 0b. Further, the fixed surface 350a is positioned substantially on the rotation path of the fixed surface 330b formed on the sample holder mounting member 330.

At the end of the peripheral wall of the rotating member 350, the protrusion 35
2 is formed, and one side surface of the protrusion 352 is an inclined surface 352a continuous with the fixed surface 350a (see FIG. 8). The inclined surface 352a is the fixed surface 33 of the sample holder mounting member 330 that has been rotationally moved as described later.
0b is guided in the direction of contact with the fixed surface 350a. Further, magnets 353 as member connecting means are buried in a plurality of positions on the fixed surface 350a with their end faces exposed, and the sample holder mounting member 33 is magnetized by magnetic force.
The structure is such that the fixed surface 330b of 0 is fixed by suction.

The hollow portion of the rotary member 350 is an X-ray transmission hole 354 that penetrates from one end to the other end in the axial direction. The X-ray transmission hole 354 is formed to have a diameter capable of transmitting the X-ray emitted from the X-ray source by the transmission method over almost the entire width. When the apparatus of this embodiment is applied to the X-ray diffractometer currently on the market, the sample holder mounting member 330 is used.
Similarly, the inner diameter of the X-ray transmission hole 354 may be set to about 24 mm.

The protrusion 35 formed on the peripheral wall of the rotating member 350.
A driven gear 355 is formed at the tip portion of 2. A second drive motor (second rotary drive source) 356 is fixed to the lower part of the jig body 310.
The drive gear 357 attached to the drive shaft of the
It meshes with 5. The rotary member 350 transmits the rotary drive force from the second drive motor 356 via the drive gear 357 and the driven gear 355, and rotates about the axis.

As shown in FIG. 5, an X-ray shielding member 400 can be attached to the bottom plate of the sample table 200. The X-ray shielding member 400 is formed in a cylindrical shape with a lid, and the lower end opening is fitted into the peripheral surface of the bottom plate 201 of the sample table 200 and fixed by a fastener 401 such as a screw. The sample rotating jig 300 is housed inside the X-ray shielding member 400. The X-ray shielding member 400 is made of a material capable of shielding X-rays, for example, a non-ferrous material such as brass or copper alloy.
Lead is generally used as the X-ray shielding material, but brass can be sufficiently used to shield the weak X-rays emitted from the sample S during X-ray diffraction measurement. However, X-ray shielding member 400 made of lead or lead alloy
Needless to say, it may be formed. The wall pressure of the X-ray shielding member 400 is appropriately determined according to the intensity of X-rays emitted from the sample S.

Further, the X-ray shielding member 400 is provided with an X-ray transmission window 402, and the X-ray transmission window 402 allows X-ray transmission.
The X-rays from the radiation source are guided to the sample S, and the diffracted X-rays emitted from the sample S are guided to the X-ray detector.

Next, the operation of the apparatus of this embodiment described above will be described. Goniometer base 100 for X-ray diffractometer
To mount the apparatus of this embodiment, the bottom plate 2 of the sample table 200
The projection portion 203 provided on 01 is used for the goniometer base 100.
It suffices to fit the mounting recess 100a formed in 1. Once this mounting is performed, even if it becomes necessary to remove the sample rotating jig 300 for maintenance or the like thereafter, the sample stage 200 can be left as it is and only the sample rotating fixture 300 can be removed from the sample stage 200. Therefore, the attachment / detachment work becomes easy. That is, the goniometer base 100 and the sample table 20
Since a high fitting precision is provided between 0 and 0, a high degree of alignment is required for mounting. On the other hand, since a simple attachment / detachment structure such as fastening with a fastener (bolt) 208 may be provided between the sample table 200 and the sample rotating jig 300, the mounting work is easy.

To mount the sample rotating jig 300 on the sample table 200, the bottom surface of the jig body 310 is placed on the flat surface 2 of the sample table 200.
05, and the jig body 31 on the reference plane 206.
The positioning surface 310a of 0 is brought into contact, the fastener 208 is passed through the fastening hole 207 and screwed into the screw hole 318.

The sample S is mounted in the sample mounting hole 341 of the sample holder 340, and its surface is the surface 34 of the sample holder 340.
It is in the same plane as 0b. The sample holder 340, on which the sample S is mounted, attracts the mounted surface 340a to the mounting surface 330a of the sample holder mounting member 330 by the magnetic force of the magnet 342 (see FIG. 8).

Here, the surface 340b (sample surface) of the sample holder 340 on the sample holder mounting member 330 fixed to the rotating member 350 is positioned on the same plane as the positioning surface 310a of the jig body 310. This positioning is performed by adjusting the position of the rotating member 350 in the axial direction, but the adjusting work may be performed only when the sample rotating jig 300 is started up. The surface 340b (sample surface) of the sample holder 340 thus positioned is inevitably on the rotation center of the goniometer because the reference surface 206 of the sample table 200 that contacts the positioning surface 310a is on the rotation center of the goniometer. Will be placed. Further, in the sample holding device of this embodiment, the X-ray shielding member 40 is attached to the sample table 200.
Since 0 can be attached, X scattered from the sample S
The rays can be efficiently shielded around the sample rotating jig 300, and the safety against X-ray exposure is improved.

In the sample rotating jig 300 of this embodiment, since a plurality of (four in this embodiment) sample holder mounting members 330 are mounted on the rotating plate 320, the rotating plate 320 is rotated by the first drive motor. Thus, the arbitrary sample holder mounting member 330 can be fixed to the rotating member 350. Therefore, after the measurement for one sample S is completed, the rotating member 350 is rotated and the next sample holder mounting member 330 is rotated.
A plurality of samples S can be automatically measured by repeating the operation of fixing the to the rotating member 350.

Here, the fixing operation of the sample holder mounting member 330 to the rotating member 350 will be described with reference to FIG. The first drive motor 314 is operated to rotate the rotary plate 320.
Is rotated, one of the plurality of sample holder mounting members 330 attached to the rotary plate 320 is rotated by the rotary member 350.
And the fixed surface 330b of the sample holder mounting member 330 comes into contact with the fixed surface 350a of the rotating member 350.
When the first drive motor 314 is stopped when the sample holder mounting member 330 is substantially coaxial with the rotating member 350, the sample holder mounting member 330 causes the magnet 3 to move.
The magnetic force of 53 attracts and fixes the rotary member 350.

At this time, when the fixed surface 330b of the sample holder mounting member 330 comes into contact with the fixed surface 350a of the rotating member 350, these surfaces are not on the same plane. For example, the fixed surface 330b is more than the fixed surface 350a. When it is located on the slightly left side (FIG. 8), the edge of the fixed surface 330b first contacts the inclined surface 352a of the rotating member 350, is guided by the inclined surface 352a, and is guided to the fixed surface 350a.
On the other hand, when the fixed surface 330b is located slightly to the right of the fixed surface 350a (FIG. 8), the fixed surface 330b is attracted to the fixed surface 350a by the magnetic force of the magnet 353.

After that, when the second drive motor 356 is operated, the sample holder mounting member 330 together with the fixing member 350.
Rotate together. Then, when the magnet 342a serving as the reference index reaches a position (origin) facing the magnetic sensor 500, the magnetic sensor 500 detects the magnetic force generated by the magnet 342a. The posture of the sample holder 330 at the time of this detection is set to zero, and the rotation angle of the sample holder 330 is measured and X-ray diffraction measurement is performed. In this way, if the rotation angle when the peak value of the diffracted X-ray is detected is obtained, the orientation of the sample S, the crystal arrangement direction, and the like are detected from the relationship between the rotation angle and the incident angle of the X-ray. be able to.

Further, since X-ray transmission holes 332 and 354 are formed on the back surface of the sample S as shown in FIG. 5, X-rays are emitted from the back surface of the sample and diffracted X-rays are detected on the front side. Transmission method measurement is also possible. Moreover, in the apparatus of this embodiment, the X-ray transmission holes 332 and 354 are each formed to have a size that allows transmission of X-rays over substantially the entire width, so that the sample S can be irradiated with X-rays without loss. It is also possible to arrange the collimator 600 inside the X-ray transmission hole 354 and irradiate the X-ray from the close position of the sample S, as shown in FIG.

The present invention is not limited to the above embodiment. For example, the magnetic sensor 16 or 500
Is the magnet 31a or 34 which is the reference index
By detecting the strength of the magnetic force detected by the magnetic sensor 16 or 500 when the magnetic force generated by 2a is detected at the origin position, it is possible to detect the positional deviation of the sample holder 3 or 340 in the axial direction.

That is, in the case where the magnetic force detected by the magnetic sensor 16 or 500 is weak on the basis of the strength of the magnetic force when the sample holder 3 or 340 is adsorbed and fixed at the proper position, FIG. It can be seen that the sample holder 3 or 340 is displaced to the left. on the other hand,
When the magnetic force detected by the magnetic sensor 16 or 500 is strong, the sample holder 3 or 3 is moved to the right in FIG. 1 or 5.
It can be seen that a positional shift of 40 has occurred.

In the second embodiment described above, the rotary plate 3
The number of the sample holder mounting members 330 attached to the 20 can be arbitrarily set as required. Further, the movement of the sample holder mounting member 330 in the axial direction can be realized by elastically bending the rotary plate 320 and bending the rotary plate 320.

Further, the X-ray transmission window 402 provided in the X-ray shielding member 4 is closed by a member made of a material having a small X-ray absorption coefficient, such as a Be plate or an Al vapor deposition mylar foil, and the inside of the X-ray shielding member 4 is closed. If it is made airtight, the periphery of the sample S (inside the X-ray shielding member 4) can be formed in various gas atmospheres, vacuum atmospheres, humidity atmospheres, etc., and measurement under these atmospheres is also possible. Further, by providing the X-ray shielding member 4 with a heat insulating property, the inside can be made into a high temperature or low temperature atmosphere. Instead of the X-ray shielding member, a dedicated container for forming various gas atmospheres or vacuum atmospheres or a dedicated container for forming high temperature and low temperature atmospheres can be attached to the sample table.

[0067]

As described above, according to the sample holding apparatus of the present invention, the origin alignment relating to the rotation operation of the sample holder is automated, and as a result, the orientation of the sample, the crystal arrangement direction, etc. can be easily and quickly obtained. Can be detected.

[Brief description of drawings]

FIG. 1 is a longitudinal sectional view showing a sample holding device according to a first embodiment of the present invention.

FIG. 2 is a longitudinal sectional view showing a sample rotating jig and a magnetic sensor in the same apparatus.

FIG. 3 is a right side view of the same.

FIG. 4 is a front view showing a sample holder of the apparatus.

FIG. 5 is a vertical sectional view showing a sample holding device according to a second embodiment of the present invention.

FIG. 6 is a right side view showing a sample rotating jig and a magnetic sensor in the same apparatus.

FIG. 7 is a front view showing a sample holder of the apparatus.

FIG. 8 is a vertical cross-sectional view showing a mounting operation and the like of a sample holder mounting jig.

FIG. 9 is a front view showing a conventional sample holding device.

[Explanation of symbols]

 1: Sample table 2: Sample rotating jig 3: Sample holder 4: X-ray shielding member 16: Magnetic sensor 20: Jig body 23: Rotating member 27: Sample holder mounting part 31: Magnet 31a: Magnet (reference index) 200 : Sample stand 300: Sample rotating jig 310: Jig body 320: Rotating plate 330: Sample holder mounting member 340: Sample holder 342: Magnet 342a: Sample holder (reference index) 350: Rotating member 353: Magnet 400: X-ray Shielding member 500: Magnetic sensor

Claims (5)

[Claims] 1. A sample stage installed on a base of a goniometer rotatable with respect to an X-ray source, a jig body mounted on the sample stage, and a rotary drive source mounted on the jig body. A cylindrical rotating member that is rotatably provided on the jig body via a bearing and rotates about an axis by a driving force from the rotary driving source, and a sample holder that is attracted and fixed to one end of the rotating member by a magnetic force. A sample holding device for an X-ray diffractometer, comprising: and an origin adjusting means for positioning a reference index provided on the sample holder at a predetermined origin. 2. A sample stage installed on a base of a goniometer rotatable with respect to an X-ray source, a plurality of sample holders for mounting samples, and a jig main body mounted on the sample stage, A rotary plate rotatably supported by the tool body, a first rotary drive source for rotationally driving the rotary plate, and a plurality of samples mounted on the same diameter of the rotary plate so as to be rotatable about their respective axes. A holder mounting member, a holder mounting means for attracting and fixing the sample holder to one end surface of the sample holder mounting member by magnetic force, and a holder mounting member that is positioned substantially on a rotation path of the sample holder mounting member and is rotatable about the jig body. The supported rotary member, the second rotary drive source that rotationally drives the rotary member, and the one sample holder mounting member that has been rotationally moved substantially coaxially with the rotary member by magnetic force to the end surface of the rotary member. X is provided with a member connecting means for adsorbing and fixing to the sample holder, and an origin aligning means for positioning the reference index provided on the sample holder at a predetermined origin.
Sample holder for line diffraction device. 3. The sample holding device for an X-ray diffraction apparatus according to claim 1, wherein the origin aligning means for rotating the sample holder comprises:
A sample holding device for an X-ray diffractometer, which is a sensor for detecting a reference index provided on the sample holder at an origin position. 4. A sample holder for an X-ray diffraction apparatus according to claim 3, wherein the sample holder is provided with a plurality of magnets, and the sample holder is attracted and fixed by the magnets, and one of the magnets is attached. A sample of an X-ray diffraction apparatus, which is formed so as to be closer to the sensor than another magnet as the reference index, and the sensor detects a magnetic force emitted from the magnet serving as the reference index at an origin position. Holding device. 5. The sample holding device of the X-ray diffractometer according to claim 4, wherein the sensor uses a sample holder fixed at an appropriate position as a reference to determine the strength of magnetic force emitted from a magnet serving as the reference index. A sample holding device for an X-ray diffraction apparatus, which is also capable of detecting a positional deviation of the sample holder in the axial direction.