JPH08327564A - Sample holder for x-ray diffraction apparatus - Google Patents

Abstract

PURPOSE: To provide a sample holder for an X-ray diffraction apparatus, which can easily set the interval between a sample surface and a knife edge with accuracy and has the function of determining the interval with high position reproducibility. CONSTITUTION: This sample holder for an X-ray diffraction apparatus includes a support member 1, having a sample support face 1b on which a sample 6 is mounted and a grooved part 1a provided omits surface 1c perpendicular to the sample support face 1b, and a knife edge 2 slidably secured to the grooved part 1a of the support member 1 and movable in the perpendicular direction to the sample surface 6a, and has a jig 5 mounted on the sample support face 1b of the support member 1 prior to mounting of the sample 6 and used to position the interval between the knife edge 2 and the sample surface. During positioning of the knife edge 2, the jig 5 is mounted on the sample support face 1b of the support member 1, and the knife edge 2 is slid along the grooved part 1a of the support member 1 and put into contact with the projecting part 5a of the jig 5 so as to determine the interval A between the knife edge 2 and the sample surface 6a.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sample holder for an X-ray diffractometer, and more particularly to a sample holder for an X-ray diffractometer used when measuring X-rays at a low angle incident on a sample.

[0002]

2. Description of the Related Art FIG. 3A is a diagram showing an example of the construction of an X-ray diffractometer. In this example, X-rays from an X-ray source 10 are dispersed by a dispersive crystal 11, and a spectroscopically specified light is obtained. The X-ray having a wavelength is incident on the sample 6 supported by the sample holder 12, and the X-ray reflected (diffracted) by the sample 6 is detected by the detector 14. Although not shown, the sample holder 12
The relationship between the detector and the detector 14 has a known deflectometer structure. The sample holder 12 is placed on the rotary table of the goniometer and can rotate about the central axis O as shown in FIG. 3 (b). It is like this. Further, the detector 14 is also supported by a mechanism capable of rotating around the sample about the central axis O, and the sample and the detector are driven around the central axis O by a motor or manually at a speed ratio of 1: 2, so-called. θ-2θ
It is designed to rotate due to.

By the way, when an X-ray diffractometer having a structure as shown in FIG. 3 is used to measure by an X-ray reflectance measuring method or a small angle scattering method, that is, when the rotation of the sample 6 is in a low angle region (θ Scan range of 0 to 1 deg.), X-ray sample 6
Since the incident angle on the sample is small, X reflected by the sample (diffracted)
In addition to the X-ray, there is a problem that the X-ray from the dispersive crystal 11 directly enters the detector 14. Therefore, in the measurement when the incident angle of the X-ray on the sample is small, the sample holder 12 provided with the knife edge 13 for blocking the direct beam at the low-angle incidence is used.

[0004]

As described above, the knife edge in X-ray diffraction is originally provided to block the direct beam at low angle incidence, and the distance between the sample surface and the knife edge is small. Although it is usually fixed, it is generally adjusted by a micrometer or the like when initializing the interval or changing the set value. However, when a micrometer was used, the position reproducibility was poor, and the accuracy could not be determined when the spacing was adjusted in the micro order.

The present invention has been made in view of the above circumstances, and the distance between the sample surface and the knife edge can be set easily and accurately without using a special adjusting mechanism, and the position can be determined with high position reproducibility. An object of the present invention is to provide a sample holder for an X-ray diffractometer having a function capable of performing the above.

[0006]

In order to achieve the above object, a sample holder for an X-ray diffraction apparatus according to the present invention has a sample support surface on which a sample is mounted and a groove portion provided on a surface orthogonal to the sample support surface. The knife is provided with a support member and a knife edge slidably fixed in a groove of the support member and movable in a direction perpendicular to the sample surface, and the knife is attached to the sample support surface of the support member before mounting the sample. Has a jig for positioning the gap between the edge and the sample surface,
At the time of positioning the knife edge, the jig is attached to the sample support surface of the support member, the knife edge is slid along the groove of the support member, and the knife edge is brought into contact with the jig to thereby separate the knife edge from the sample surface. It is characterized in that the interval is determined (Claim 1).

Further, the positioning jig has a protrusion having a height equal to the distance between the knife edge and the sample surface (claim 2).

Further, in the sample holder for the X-ray diffractometer of the present invention, an electrode is provided at a contact portion of the tip of the knife edge with the jig, and the electrode and the jig are connected to an electric circuit to fix the knife edge and the jig. The contact with the tool is electrically detected (Claim 3).

Further, the electrodes at the tip of the knife edge are provided at two places with a predetermined space therebetween, and the two electrodes and the jig are connected to an electric circuit so that contact between the knife edge and the jig and parallelism can be improved. It is detected electrically (claim 4).

Further, in the electric circuit, one end side is connected to each of the two electrodes and the other end side is a common terminal.
A parallel circuit composed of two resistors, a power source and an ammeter connected to a common terminal of the parallel circuit, and the ammeter detects contact between the knife edge and the jig and parallelism (claim 5).

Further, resistors having different resistance values are used for the two resistors of the parallel circuit, and the electrode on the side in contact with the jig is specified by detecting the change in the current measured by the ammeter. It was made possible (Claim 6).

[0012]

In the sample holder for the X-ray diffractometer according to the present invention, a jig that does not require a special adjusting mechanism is used, and when the knife edge is positioned, the jig is attached to the sample supporting surface of the supporting member to support the supporting member. The distance between the sample surface and the knife edge can be set only by a simple adjustment in which the knife edge is slid along the groove portion of (3) and the knife edge is brought into contact with the jig.

Further, since the positioning jig has a protrusion having a height equal to the distance between the knife edge and the sample surface, the knife edge is kept in contact with the protrusion of the jig. Is fixed, the jig is removed from the sample support surface of the sample holder, and the sample is attached to the sample support surface, whereby the interval between the sample surface and the knife edge is set with good position reproducibility. It is possible to easily change the set value of the gap by preparing various kinds of jigs having different heights of the protrusions.

By the way, when positioning the knife edge in contact with the jig as described above, if the excessive force is applied while the knife edge is pressed against the jig, the positional accuracy may be deteriorated. Therefore, in the present invention, an electrode is provided at the contact portion with the jig at the tip of the knife edge, the electrode and the jig are connected to an electric circuit, and by electrically detecting the contact between the knife edge and the jig, It becomes possible to detect even a slight contact, and it is possible to prevent deterioration of the position accuracy due to excessive pressing.

Further, when the knife edge and the jig are brought into contact with each other for positioning, if the parallelism between them is poor, the positional accuracy becomes poor. Therefore, in the present invention, electrodes at the tip of the knife edge are provided at two locations with a predetermined gap, the two electrodes and the jig are connected to an electric circuit, and the contact between the knife edge and the jig and the parallelism are electrically controlled. By electrically detecting, that is, electrically detecting the contact between the two electrodes and the jig, not only the contact between the knife edge and the jig but also the parallelism can be detected. More specifically, the electric circuit includes a parallel circuit including two resistors, one end of which is connected to the two electrodes and the other end of which is a common terminal, and a power supply connected to a common terminal of the parallel circuit. And an ammeter, the two resistors in the parallel circuit having different resistance values are used, and the change in the current measured by the ammeter is detected to detect the electrode on the side in contact with the jig. Can be specified, and the parallelism between the knife edge and the jig can be detected easily and accurately.

[0016]

Embodiments of the present invention will be described below with reference to the drawings. FIG. 1 is an explanatory view of a sample holder for an X-ray diffraction apparatus showing an embodiment of the present invention, (a) is a perspective view of the sample holder showing a state in which a jig is attached to a sample supporting surface of a supporting member,
FIG. 9B is a perspective view of the sample holder showing a state in which the jig is removed from the sample supporting surface of the supporting member and the sample is attached after the position of the knife edge is set. In FIG. 1, a support member 1 formed in the shape of a rectangular block includes a sample support surface 1b on which a sample 6 is attached by a fixing method (not shown) such as clip fastening or screw fastening, and a surface 1c orthogonal to the sample support surface 1b. The groove portion 1a of the supporting member 1
A knife edge 2 is slidably fixed to the sample surface 6
It is movable in the direction perpendicular to a. Further, in this sample holder, the knife edge 2 and the sample surface 6 are attached to the sample supporting surface 1b of the supporting member 1 before the mounting of the sample 6.
A jig 5 for positioning the gap with a is provided, and at the time of positioning the knife edge 2, as shown in FIG. 1A, the sample supporting surface 1b of the supporting member 1 is clipped or screwed. The jig 5 is attached by a fixing method (not shown), the knife edge 2 is slid along the groove 1a of the support member 1, and the knife edge 2 is brought into contact with the jig 5 so that the knife edge 2 and the sample surface The interval can be determined.

The jig 5 is provided with a protrusion 5a having a height equal to the distance A between the knife edge 2 and the sample surface, and the knife edge 2 is brought into contact with the protrusion 5a of the jig 5. After positioning, the jig 5 is attached to the sample support surface 1b of the support member 1.
If the sample 6 is attached to the sample support surface 1b of the support member 1 as shown in FIG. 1B, the distance A between the sample surface 6a and the knife edge 2 is automatically set with high accuracy.

In the above-mentioned prior art, a micrometer or the like has generally been used to set the distance between the knife edge and the sample surface. In this case, the accuracy of the distance is the mechanical accuracy of the micrometer. However, if the sample holder of the present invention as shown in FIG. 1 is used, the distance between the knife edge 2 and the sample surface is the protrusion of the jig 5. It is determined by the height A of 5a, and as long as the knife edge 2 is not pressed against the protrusion 5a of the jig 5 with an excessive force, the interval can be set with higher accuracy than the conventional method, and the position reproducibility is also high.

By the way, when the knife edge 2 is brought into contact with the protrusion 5a of the jig 5 and positioned, a method of not applying an excessive force is to provide an electrode on the knife edge so that the knife edge and the jig are electrically connected. By connecting to the circuit and detecting the conduction between the knife-edge electrode and the jig, even a slight contact can be detected. That is, when the spacing is set on the micro order, it is difficult to perform the visual inspection, but the spacing can be set with high accuracy by electrically detecting the contact between the knife edge and the jig. Further, as in the embodiment shown in FIG. 1, the electrodes 3 and 4 are provided at the upper portion and the lower portion of the tip of the knife edge 2,
By electrically detecting the contact between the three electrodes 3 and 4 and the projection 5a of the jig 5, the parallelism between the knife edge 2 and the jig 5 can be ensured, and the jig 5 can be removed to support the support member 1. The parallelism between the knife edge 2 and the sample 6 when the sample 6 is attached can be ensured. Specific examples will be described below with reference to FIGS.

The jig 5 and the electrodes 3 and 4 provided at the upper and lower portions of the knife edge 2 in FIG. 1A are connected to an electric circuit as shown in FIG. In this case,
The jig 5 (or the protrusion 5a of the jig 5) is made of a conductor such as metal. As mentioned above, knife edge 2
Slides along the groove 1a provided in the support member 1,
The jig 5 is fixed to a surface (sample support surface) 1b perpendicular to the moving direction of the knife edge 2 of the support member 1, and the sample surface set by the height A of the projection 5a provided on the jig 5 is set. Corresponds to the distance between the knife edge 2 and the knife edge 2.

As shown in FIG. 2, the electric circuit is a parallel circuit composed of two resistors R1 and R2, one ends of which are connected to the two electrodes 3 and 4 of the knife edge 2 and the other end of which is a common terminal. , A DC power source 8 connected to a common terminal of the parallel circuit, and an ammeter 7 connected between the DC power source 8 and the jig 5. Further, the two resistors in the parallel circuit have different resistance values (for example, R1 = 1.5 kΩ, R2 = 3.
0 kΩ) is used.

In FIG. 1A, the protrusion 5a of the jig 5 is formed.
And the tip of knife edge 2 are parallel, electrodes 3 and 4
Touch at the same time. In that case, the ammeter 7 of FIG.
A current value of 5 mA is displayed. Next, when the jig 5 and the tip of the knife edge 2 are not parallel to each other and the upper portion of the knife edge 2 is wider than the lower portion of the knife edge 2, only the lower electrode 4 contacts the protrusion 5 a of the jig 5. At that time, the ammeter 7 shows 0.
A current value of 5 mA is displayed. Similarly, knife edge 2
When the lower part is wider than the upper part, only the upper electrode 3 comes into contact with the protrusion 5a of the jig 5, and the ammeter 7 displays a current value of 1.0 mA.

In this way, the two electrodes 3 and 4 are provided above and below the tip of the knife edge 2 and the resistors R1 and R2 having different resistance values are respectively connected as shown in FIG. 2 to form a parallel circuit. Allows the knife edge 2 and the protrusion 5 of the jig 5 to
The parallelism with a can be detected from the change in the current value of one ammeter 7, and the contact and parallelism between the knife edge 2 and the protrusion 5a of the jig 5 can be easily detected. Therefore, FIG.
In the example, if the current value of the ammeter 7 is adjusted to be 1.5 mA, the interval and parallelism between the knife edge 2 and the jig 5 can be secured, and the jig 5 is fixed after the knife edge 2 is fixed. If the sample 6 is removed and attached as shown in FIG. 1B, the distance A between the knife edge 2 and the sample surface 6a and the parallelism can be set accurately.

In FIG. 1, when adjusting (changing) the distance between the sample surface 6a and the knife edge 2, the projection 5
The jig 5 is replaced with a jig 5 having a different height A. That is, if the distance between the sample surface 6a and the knife edge 2 is set to, for example, 10 μm, a jig having a height A of the projection 5a of 10 μm is used, and if set to 15 μm, the height A of the projection 5a is set to A.
= 15 μm jig is used. Therefore, if many kinds of jigs having different heights of the protrusions 5a are prepared, the sample surface 6
The distance between a and the knife edge 2 can be set variously.

[0025]

As described above, the sample holder for the X-ray diffractometer according to the present invention comprises the jig which does not require a special adjusting mechanism, and supports the sample of the supporting member when positioning the knife edge. Since the jig is attached to the surface, the knife edge is slid along the groove portion of the supporting member, and the knife edge is brought into contact with the jig, the distance between the sample surface and the knife edge can be set by only simple adjustment. The distance between the sample surface and the knife edge can be easily determined with high position reproducibility.

In the sample holder for the X-ray diffraction apparatus according to the present invention, since the positioning jig has a protrusion having a height equal to the distance between the knife edge and the sample surface, the jig is provided with a knife. With the simple operation of fixing the knife edge with the edge in contact, removing the jig from the sample support surface of the sample holder and mounting the sample on the sample support surface, the sample surface and the knife edge can be accurately repositioned. You can set the interval. Furthermore, it is possible to set an arbitrary interval by preparing many kinds of jigs in which the heights of the protrusions are changed in advance.

In the sample holder for the X-ray diffractometer according to claim 3, an electrode is provided at a contact portion of the tip of the knife edge with the jig, the electrode and the jig are connected to an electric circuit, and the knife edge and the jig are connected. By electrically detecting the contact with, even a slight contact can be detected, and it is possible to prevent the deterioration of the position accuracy due to excessive pressing.

In the sample holder for the X-ray diffractometer according to claim 4, electrodes at the tip of the knife edge are provided at two positions with a predetermined interval, and the two electrodes and the jig are connected to an electric circuit, and a knife is provided. By electrically detecting the contact and parallelism between the edge and the jig, that is, by electrically detecting the contact between the two electrodes and the jig, not only the contact between the knife edge and the jig but also the parallelism Can be detected.

In the sample holder for an X-ray diffraction apparatus according to claim 5, the electric circuit includes a parallel circuit including two resistors, one end of which is connected to the two electrodes and the other end of which is a common terminal. Since the power source and the ammeter are connected to the common terminal of the parallel circuit, the contact state of the two electrodes can be simultaneously detected with a simple circuit configuration and one ammeter.

In the sample holder for the X-ray diffractometer according to claim 6, resistors having different resistance values are used for the two resistors of the parallel circuit, and the change in the current measured by the ammeter is detected. The electrode on the side in contact with the jig can be specified, the parallelism between the knife edge and the jig can be easily and accurately detected, and the parallelism can be easily adjusted.

[Brief description of drawings]

FIG. 1 is an explanatory view of a sample holder for an X-ray diffraction apparatus showing an embodiment of the present invention, (a) is a perspective view of the sample holder showing a state in which a jig is attached to a sample supporting surface of a supporting member,
FIG. 9B is a perspective view of the sample holder showing a state in which the jig is removed from the sample supporting surface of the supporting member and the sample is attached after the position of the knife edge is set.

FIG. 2 is a diagram showing an embodiment of the present invention and is a circuit diagram showing a configuration example of an electric circuit for detecting contact between two electrodes provided on a knife edge and a jig.

FIG. 3 is an explanatory diagram of an X-ray diffractometer in which the sample holder of the present invention is used.

[Explanation of symbols]

 1: Support member 1a: Groove 1b: Sample support surface 1c: Surface orthogonal to sample support surface 2: Knife edge 3,4: Electrode 5: Jig 5a: Projection 6: Sample 6a: Sample surface 7: Ammeter 8 : DC power supply 10: X-ray source 11: Spectroscopic crystal 12: Sample holder 13: Knife edge 14: Detector

Claims (6)

[Claims] 1. A sample holder for an X-ray diffractometer in which X-rays are incident on a sample surface at a low angle and diffracted (reflected) on the sample surface is detected by a detector. A support member having a groove portion provided on a surface orthogonal to the sample support surface; and a knife edge slidably fixed to the groove portion of the support member and movable in a direction perpendicular to the sample surface. Before the attachment, the jig is attached to the sample support surface of the support member and has a jig for positioning the gap between the knife edge and the sample surface. When positioning the knife edge, the jig is attached to the sample support surface of the support member. A sample ho for an X-ray diffractometer, characterized in that the interval between the knife edge and the sample surface is determined by sliding the knife edge along the groove of the mounting and supporting member and bringing the knife edge into contact with the jig. Ruda. 2. The sample holder for an X-ray diffraction apparatus according to claim 1, wherein the positioning jig has a protrusion having a height equal to the distance between the knife edge and the sample surface. Sample holder for X-ray diffractometer. 3. The sample holder for an X-ray diffractometer according to claim 2, wherein an electrode is provided at a contact portion of the tip of the knife edge with the jig, and the electrode and the jig are connected to an electric circuit to form a knife edge. A sample holder for an X-ray diffractometer, which is characterized by electrically detecting a contact with a jig. 4. The sample holder for an X-ray diffractometer according to claim 3, wherein the electrodes at the tip of the knife edge are provided at two positions with a predetermined interval, and the two electrodes and the jig are connected to an electric circuit. A sample holder for an X-ray diffractometer, which electrically detects the contact between the knife edge and the jig and the parallelism. 5. The sample holder for an X-ray diffractometer according to claim 4, wherein the electric circuit is a parallel circuit including two resistors, one end of which is connected to each of the two electrodes and the other end of which is a common terminal. And a power source and an ammeter connected to a common terminal of the parallel circuit, wherein the ammeter detects the contact between the knife edge and the jig and the parallelism, and a sample holder for an X-ray diffractometer. 6. The sample holder for an X-ray diffractometer according to claim 5, wherein resistors having different resistance values are used as the two resistors of the parallel circuit, and a change in current measured by the ammeter is detected. A sample holder for an X-ray diffraction device, characterized in that the electrode on the side in contact with the jig can be specified.