JPH0894549A - Longitudinal x-ray diffraction device and method and mechanism for setting angle at which x-ray is taken out - Google Patents

Abstract

PURPOSE: To allow an X-ray incident on a sample to be constantly applied to the same illuminated position of the sample by easily adjusting, by means of a simple structure, the angle at which the X-ray is taken out. CONSTITUTION: An X-ray source 36 is spaced from the end of an X-ray impinging arm 43. A setting mechanism 31 for the angle at which the X-ray is taken out includes a support member 37 provided near the X-ray source 53, a locking member 38 which rotates above the support member 37 with the X-ray source 53 as its axis of rotation; a tilt stand 34 secured to the base 38b of the locking member 38 at one end and having a longitudinal X-ray diffraction device 31 mounted thereon; and a tilt angle setting screw 34a for adjusting the tilt angle of the tilt stand 34. The tilt stand 34 is constantly rotated and tilted about a rotation axis Y-Y including the X-ray source 53 by the turning of the screw 34a, so that the angle at which the X-ray is taken out from the X-ray source is varied.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and a mechanism for setting an X-ray extraction angle of a vertical X-ray diffraction apparatus for easily and accurately setting an X-ray extraction angle from an X-ray source.

[0002]

2. Description of the Related Art As a conventional X-ray extraction angle setting method and mechanism for a vertical X-ray diffractometer, the one shown in FIG. 6 is known. The vertical X-ray diffractometer 1 shown in FIG. 6 has a structure in which a sample 4 is integrated with a central rotating shaft 3 of an apparatus main body 2 such as a vertical goniometer.
Is provided on the outer peripheral surface of the apparatus main body 2 along the central axis C1 which includes the surface of the sample 4 and intersects with the center O of the rotary shaft 3.
A line incidence arm 5 is provided. A divergence slit 7 is attached to the X-ray entrance arm 5 to limit the area of X-rays irradiated on the sample. An X-ray detection arm 8 is provided on the outer peripheral surface of the apparatus main body 2 on the opposite side of the X-ray incidence arm 5 via the rotation shaft 3, along a central axis C2 intersecting with the center O of the rotation shaft 3, The X-ray detection arm 8 is provided with a scattering slit 9, a solar slit 10, a light receiving slit 11, and a detector 12 from the inside.

A pedestal 13 is attached to the bottom of the apparatus main body 2, and both sides (left and right sides in FIG. 6) of the pedestal 13 are spaced apart from the tip surface of the X-ray incidence arm 5 and a base 15 is provided. An extraction angle setting screw 14 for adjusting the extraction angle of X-rays from the X-ray source 6 fixed on the top is attached.

In this vertical X-ray diffractometer 1, the X-rays emitted from the X-ray source 6 pass through the divergence slit 7 of the X-ray incidence angle arm 5 and are applied to the sample 4 provided at the center O of the rotary shaft 3. The diffracted X-rays from the sample 4 are scattered slits 9, solar slits 10 and light-receiving slits 1 of the X-ray detection arm 8.
It is detected by the detector 12 through 1.

As a method for setting the X-ray extraction angle in this apparatus 1, the inclination of the pedestal 13 is adjusted by adjusting the height of the adjusting screw 14 provided on the left side or the right side of the pedestal 13 in FIG. The tilt angle of the vertical X-ray diffractometer 1 is controlled by this, the extraction angle of the X-rays from the X-ray source 6 is set, and the X-ray source 6 that has passed through the divergence slit 7 on the X-ray entrance arm 5 X-ray from the rotating shaft 41
It adjusts so that it may inject on the center line O of. When the X-rays diverge from the X-ray source 6, the X-rays are limited to a predetermined area by the divergence slit 7 and enter the sample 4 at a predetermined incident angle.
In this state, the rotating shaft 3 is rotated at an angular velocity θ, and the diffracted X-rays from the rotating sample 4 are passed through the scattering slit 9, the solar slit 10 and the light receiving slit 11 of the X-ray detection arm 8 which rotates at an angular velocity 2θ. It is detected by the detector 12.

[0006]

However, in the X-ray extraction angle setting method in the conventional vertical X-ray diffractometer 1 described above, since the X-ray source 6 and the X-ray incidence arm 5 are separated from each other, the X-ray source is separated. The positional relationship between the source 6 and the sample 4 is not fixed, and X
The irradiation position of the X-rays emitted from the radiation source 6 on the sample 4 is not constant, and the X-ray optical system must be readjusted every time the extraction angle of the X-rays is changed, and the operation is very complicated. There was a problem that it took time.

The present invention has been made to solve the above-mentioned problems, and the extraction angle of X-rays emitted from an X-ray source can be easily adjusted with a simple structure, and the sample It is an object of the present invention to provide an X-ray extraction angle setting method and mechanism for a vertical X-ray diffraction device that can always irradiate the same irradiation position of a sample with the incident X-rays.

[0008]

In order to solve the above-mentioned problems, the present invention according to claim 1 takes out X-rays emitted from an X-ray source at a predetermined take-out angle and forms a rotary shaft at the center of the apparatus main body. In the method of setting an X-ray extraction angle of a vertical X-ray diffraction apparatus, which irradiates an integrally rotating sample surface and detects diffracted X-rays from the sample surface with a detector that rotates around the apparatus body, said vertical X-ray It is characterized in that the diffractive device is mounted on an inclined table for setting an X-ray extraction angle from the X-ray source, and the inclined table is always rotated and inclined around a rotation center axis including the X-ray source.

According to a second aspect of the present invention, a sample irradiated with X-rays emitted from an X-ray source, an apparatus main body for rotating a rotation shaft on which the sample is fixed at an angular velocity θ, and the X-rays as the sample. X-ray of a vertical X-ray diffraction apparatus including an X-ray incidence arm that guides the X-ray and an X-ray detection arm that is rotatably provided around the apparatus main body at an angular velocity of 2θ and that detects diffracted X-rays from the sample. A radiation extraction angle setting mechanism, wherein the X-ray source is provided separately from the tip of the X-ray incidence arm, and the X-ray extraction angle setting mechanism is provided in the vicinity of the X-ray source. A locking member that rotates about the X-ray source as a rotation center axis above the support member; and a tilt table on which one end side is fixed to the lower end of the locking member to mount the vertical X-ray diffraction device. , At the end of the tilting table opposite to the fixed end of the locking member, It is characterized by being provided with a tilt angle setting screw for adjusting the tilt angle of the tilt table.

According to a third aspect of the present invention, the locking portion of the locking member is formed in a wedge shape, and the wedge-shaped locking portion is formed on the top portion of the support member so as to coincide with the rotation center axis. It is characterized by being locked in the groove.

According to a fourth aspect of the invention, a tilt angle fixing screw for fixing the tilt angle of the tilt table set by the tilt angle setting screw is provided on the fixed end side of the locking member of the tilt table. The feature is that it is provided.

According to a fifth aspect of the present invention, the lower end portion of the locking member is detachably fixed to one end of the tilt base, and the base end portion of the support member is detachably fixed to the base base. It is characterized by that.

[0013]

According to the present invention, since the central axis of rotation of the locking portion of the locking member fixed to one end of the tilt table coincides with the X-ray source, the tilt angle setting screw of the tilt table is moved up and down. By doing so, the tilt table rotates about the rotation center axis and the tilt angle changes, which changes the X-ray extraction angle from the X-ray source, and the incident X-ray flux incident on the sample is always the same irradiation of the sample. The position is illuminated. In this state,
The rotation axis is rotated at an angular velocity θ, and the X-ray detection arm is rotated around the sample at an angular velocity 2θ.

[0014]

The present invention will be described in detail with reference to the drawings.
1 to 4 show an X-ray extraction angle setting mechanism of a vertical X-ray diffractometer according to an embodiment of the present invention, which is designated by reference numeral 31.
Is an X-ray extraction angle setting mechanism of the vertical X-ray diffractometer (hereinafter simply referred to as "X-ray extraction angle setting mechanism"). This X-ray extraction angle setting mechanism 31 is used for the pedestal 3 of the vertical X-ray diffraction device 32.
3 is mounted on the tilt table 34, and this tilt table 34 is further mounted on the base 35. On the base 35, the side of the vertical X-ray diffraction device 32 mounted on the tilt table 34 ( An X-ray generator 36 is provided on the right side in FIG. 1, and two support members 37 are provided on both sides of the X-ray generator 36 in parallel with the center line O of the rotation axis of the vertical X-ray diffraction device 32. A locking member 38 that rotates the tilt table 34 about the upper surface of the support member 37 is provided between the support member 37 and the tilt table 34.

A rotary shaft 41 is provided at the center of a vertical goniometer, which is the main body 32a of the vertical X-ray diffractometer 32, and a projecting end of the rotary shaft 41 has a sample holder 41a which rotates integrally with the rotary shaft 41. Is provided. More specifically, the projecting end of the rotary shaft 41 has a lower half formed in a semicircular cross section by notching the upper half horizontally, and the X-ray analysis is performed on the horizontal portion of the rotary shaft 41 having the semicircular cross section. A sample holder 41a for accommodating the sample 42 is attached. Then, by rotating the rotating shaft 41, the sample 42 in the sample holder 41a is rotated around the center line O at an angular velocity θ. Further, on the outer peripheral surface of the vertical X-ray diffraction device 32, an X-ray incidence arm 43 for guiding the X-rays emitted from the X-ray generation device 36 to the sample 42, and an X-ray detection for detecting the diffracted X-rays from the sample 42. The arm 44 for the rotary shaft 4
It is provided so as to be rotatable around 1.

The X-ray incidence arm 43 is provided with a divergence slit 45 for limiting the area of the X-ray to irradiate the sample by limiting the divergence angle of the X-ray in the horizontal direction.
In the ray arm 44, a scattering slit 47 for removing scattered X-rays from other than the sample such as air scattering, and a solar slit 48 for limiting the vertical divergence of the diffracted X-rays and extracting only the central part of the Debye ring. A light-receiving slit 49 for adjusting the resolution of diffracted X-rays, a detector 50 for detecting X-rays, and the like are provided.

In the X-ray generator 36, a vertical X-ray source 53 is composed of an electron gun 51 that emits thermoelectrons upward from a filament and a drum-shaped target 52 that receives the thermoelectrons while rotating at high speed. The vertical X-ray source 53 is covered with a tube shield 54. The tube shield 54 has a window (not shown) in the horizontal direction.
It is formed on the surface, and X-rays are radiated to the surroundings from this window.

In the pedestal 33, one is provided at the center of the X-ray detection arm 44 side (left side in FIG. 1) and the X-ray incidence arm 43 is provided.
Two position adjusting screws 33a on both sides of the side (right side in FIG. 1)
Are provided, and the height and horizontal position of the surface of the sample 42 are adjusted by adjusting these position adjusting screws 33a. Further, the tilt table 34 has an X-ray detection arm 44.
One tilt angle setting screw 34a is attached to the center of the side, and two tilt angle fixing screws 34b are attached to both side parts on the X-ray incidence arm 43 side. By adjusting the tilt angle fixing screw 34b, the tilt angle of the tilt table 34 with respect to the X-ray source 53 is adjusted and held. Further, the tip ends of the tilt angle setting screw 34a and the tilt angle fixing screw 34b are, for example, as shown in FIG.
Formed on the upper surface of the screw pedestal 35a fixed on
By being supported inside the groove 35b, it can be moved horizontally according to the tilt angle of the tilt table 34. The V groove 35
A ball screw may be attached to the inclined table 34 instead of b.

The support member 37 is formed in a cylindrical shape, and the base end portion 37a is detachably fixed to the base 35 by bolts or the like.
Moreover, the center line O of the rotation axis of the vertical X-ray diffractometer 32 is provided on the upper surface.
A V groove 37b is formed in parallel with the. A locking member 38 is attached between the support member 37 and the inclined table 34. The upper locking portion 38a of the locking member 38 is formed in a wedge shape, and the wedge-shaped locking portion 38a is locked in the V groove 37b of the support member 37. The rotation center axis YY formed by the V groove 37b of the support member 37 and the locking portion 38a of the locking member 38 provided on both sides of the X-ray source is the X-ray source divergent X-ray source. It is provided to match the position. Further, the lower end portion 38b of the locking member 38 is provided on the inclined table 34.
Is removably fixed to one end of the tilt base 34 by the screw 55, whereby the tilting base 34 is rotatable about the rotation center axis Y-Y.

Next, an X-ray extraction angle setting method of this embodiment will be described.

First, as shown in FIG. 2, an inclined table 34 is placed on a base 35 to which an X-ray generator 53 is attached, and a pedestal 33 to which a vertical X-ray diffraction device 32 is attached is mounted on the inclined table 34. To place. Further, a pair of supporting members 37 are provided on both sides of the X-ray generator 53, and a locking portion 38a of a locking member 38 in which one end of the inclined table 34 is fixed to a V groove 37b formed at the top of the supporting member 37. Lock.

In this state, the X-ray from the X-ray source 53 passes through the divergence slit 44 and is incident on the center line O of the rotating shaft 41 of the vertical X-ray diffracting device 32, and the position adjusting screw 33a of the pedestal 33 is used. And adjust the height position of 33b. The tilt angle fixing screw 34b of the tilt table 34 is floated from the base 35 so that the tilt table 34 is supported in a horizontal state by the tilt angle setting screw 34a and the tip portion 38a of the locking member 38.

Next, turn the tilt angle setting screw 34a to
The tilt table 3 on the side provided with the tilt angle setting screw 34a
4 is moved up and down, the tilting table 34 is locked by the locking member 3
The rotation center axis Y-Y formed by the locking portion 38a of No. 8 and the V groove on the upper surface of the support member 37 is inclined. In this embodiment, the rotation center axis Y-Y of the locking member 38 coincides with the X-ray source 53, and by changing the tilt angle of the tilt table 35, the X-ray extraction angle from the X-ray source 53 changes. .

For example, as shown in FIG. 4, the tilt table 34 rotates about the rotation center axis Y--Y to allow the sample 42 to rotate.
When the position of is changed from the position of (a) to the position of (b), the extraction angle of the X-ray from the X-ray source 53 is changed from the position of (a) to the position of (b), and the sample 42 The angle of incidence of X-rays on α1 changes from α1 to α2 (usually in the range of 3 to 12 °), and the incident X-ray flux is always the same irradiation position of the sample 42,
For example, it is incident on the center line O of the rotation shaft 41. Sample 4
The diffracted X-ray from 2 is detected by the detector 50 via the scattering slit 47, the solar slit 48, and the light receiving slit 49 provided in the X-ray detecting arm 44.

As described above, by changing the extraction angle of the X-rays from the X-ray source 53, the effective focal width of the extracted X-ray lines changes, and the intensity and resolution of the X-rays differ. Note that X
It is also possible to extract point-like X-rays by changing the direction of the radiation source.

Further, when the incident angle is set by the above method and the optimum effective focal width of the X-ray is determined, the rotary shaft 41 is rotated at the set take-out angle to rotate the sample 42 around the center line O. By rotating the X-ray detection arm 44 at the angular velocity 2θ around the center line O while rotating the X-ray detection arm 44 at the angular velocity θ, the 2θ of the diffracted X-ray from the sample can be measured.

As described above, according to the X-ray extraction angle setting mechanism 31 of this embodiment, it is only necessary to adjust the tilt angle setting screw 34a and rotate the tilt base 34 about the rotation center axis Y--Y. X-ray optical system is not displaced, that is, incident X
The extraction angle of the X-rays from the X-ray source 53 can be set easily, quickly and surely without changing the irradiation position of the ray bundle on the sample 42.

After the small angle of incidence of the X-ray on the sample 42 is set, the tilt angle fixing screw 34b of the tilt table 34 is set.
The tilting member 34 is turned on and the tilting base 34 is supported on the base 35 by the tilting angle fixing screw 34b, so that the locking member 38 is locked.
You may make it remove from 4. As a result, the tilting table 34 includes the tilt angle setting screw 34a and the tilt angle fixing screw 3a.
4b and a predetermined inclination angle are held, and a predetermined X-ray extraction angle is obtained. Further, by removing the support members 37 on both sides of the X-ray generator 53 from the base 35, it becomes possible to use X-rays diverging from both sides of the X-ray source 53,
The line generator 53 can be effectively used and maintenance is facilitated.

FIG. 5 shows a modification of the wedge-shaped tip and the V-shaped groove which constitute the rotating mechanism for rotating the tilting table 34 of the above-described embodiment about the rotation center axis Y--Y, and the locking member 38.
On the horizontal plate at the upper end of the
The tip of the screw 61 is rotatably locked in a recess 62 formed in the upper surface of the support member 37. In addition to this, the tip end portion of the locking member 38 is formed into a spherical shape, and this spherical end portion is rotated in conformity with the rotation center axis YY, or an axis having the rotation center axis YY as the rotation center. It may be configured with a bearing and the like. Further, as shown in FIG. 5, the locking member 38 and the inclined base 34 are connected by overlapping the base end portion 38b of the locking member 38 with the lower surface of one end of the inclined base 34 and connecting them with bolts or the like. Alternatively, the tilting base 34 and the locking member 38 may be integrally formed.

In the above embodiment, the supporting members are provided on both sides of the X-ray generator, but they may be provided on either one of them, or a tube shield may be used as the supporting member instead of the supporting member. May be. Further, by controlling the driving of the tilt angle setting screw by a driving source such as a motor, it is possible to change the small angle incidence of X-rays at a constant angular velocity. Further, in the above embodiment, an example using the rotating anticathode type as the X-ray generator is given.
As the X-ray generator, other X-rays such as an enclosed X-ray generator
Of course, a line generator may be used.

[0031]

As described above, according to the method of the present invention, the angle of extraction of X-rays emitted from the X-ray source is changed by changing the inclination of the tilting table with the X-ray source as the rotation center axis. As a result, the X-ray having the optimum effective focal width can be irradiated to the sample, and even if the extraction angle is changed, the X-ray optical system is not displaced, and the incident X-ray is always irradiated to the same position on the sample. can do. Therefore, it is not necessary to readjust the X-ray optical system every time the take-out angle is changed,
The sample can be analyzed easily, quickly and accurately.

According to the mechanism of the present invention, the tilt angle of the tilt table is adjusted by rotating the tilt angle setting screw.
X-rays can be easily and quickly moved without causing a shift in the X-ray optical system.
The extraction angle of X-rays from the radiation source can be changed. In this state, the sample is rotated at the angular velocity θ and
By rotating the X-ray detection arm at an angular velocity of 2θ, it is possible to measure 2θ of the diffracted X-ray from the sample.

After the tilt angle of the tilt table is set, the tilt angle of the tilt table can be held by the tilt angle setting screw and the tilt angle fixing screw by adjusting the tilt angle fixing screw. .

Further, by removing the locking member and the support member, there are no obstacles around the X-ray source, and the X-ray source can be used in multiple ways and the maintenance is easy.

[Brief description of drawings]

FIG. 1 is an overall perspective view of an X-ray extraction angle setting mechanism of a vertical X-ray diffractometer according to an embodiment of the present invention.

FIG. 2 is a front view of FIG.

FIG. 3 is an explanatory diagram illustrating a state in which tips of the tilt angle setting screw and the tilt angle fixing screw of FIG. 1 are provided so as to be horizontally movable inside a V groove of a pedestal.

FIG. 4 is an explanatory diagram for explaining that the extraction angle of X-rays from the X-ray source changes when the tilting table is tilted using the X-ray extraction angle setting mechanism of FIG.

FIG. 5 is an explanatory view illustrating a modified example of the rotation center shaft configured by the support member and the locking member of the present invention.

FIG. 6 is a front view of a vertical X-ray diffractometer in which a conventional X-ray source is provided separately.

[Explanation of symbols]

 31 X-ray extraction angle setting mechanism of vertical X-ray diffractometer 32 Vertical X-ray diffractometer 32a Device body (vertical goniometer) 33 Pedestal 34 Tilt table 34a Incident angle setting screw 34b Incident angle fixing screw 35 Base 36 X-ray generation Device 37 Supporting member 37b V groove, recess, 38 Locking member 38a One end (wedge, screw, spherical end) of the locking member 38b The other end of the locking member 41 Rotating shaft 41a Sample holder 42 Sample 43 X-ray incidence Arm 44 X-ray detection arm 53 X-ray source

Claims (5)

[Claims] 1. An X-ray diverged from an X-ray source is taken out at a predetermined take-out angle and irradiated onto a sample surface which rotates integrally with a rotating shaft at the center of the apparatus main body, and the diffracted X-ray from the sample surface is aforesaid. In a method for setting an X-ray extraction angle of a vertical X-ray diffraction device for detecting with a detector that rotates around an apparatus body, the vertical X-ray diffraction device is placed on an inclined table for setting an X-ray extraction angle from the X-ray source. An X-ray extraction angle setting method for a vertical X-ray diffractometer, characterized in that it is placed and the tilt table is always tilted about a rotation center axis including the X-ray source. 2. A sample irradiated with X-rays diverged from an X-ray source, a device body for rotating a rotation shaft on which the sample is fixed at an angular velocity θ, and an X-ray entrance for guiding the X-rays to the sample. An X-ray extraction angle setting mechanism of a vertical X-ray diffraction device, comprising an arm and an X-ray detection arm that is rotatably provided around the device body at an angular velocity 2θ and detects diffracted X-rays from the sample. Therefore, the X-ray source is provided apart from the tip of the X-ray incidence arm, and the X-ray extraction angle setting mechanism is provided near the X-ray source. A locking member that rotates around the X-ray source as a central axis of rotation on the upper part, a tilt table on which one end side is fixed to a lower end portion of the locking member and the vertical X-ray diffraction device is mounted, and the tilt table of the tilt table. Adjust the tilt angle of this tilting base to the end opposite to the fixed end of the locking member. X-ray extraction angle setting mechanism of a vertical X-ray diffractometer is characterized in that an inclined angle setting screws. 3. The locking portion of the locking member is formed in a wedge shape, and the wedge-shaped locking portion is locked in a V groove formed on the top of the support member so as to coincide with the rotation center axis. The X-ray extraction angle setting mechanism of the vertical X-ray diffractometer according to claim 2. 4. A tilt angle fixing screw for fixing the tilt angle of the tilt table set by the tilt angle setting screw is provided on the fixed end side of the locking member of the tilt table. The X-ray extraction angle setting mechanism of the vertical X-ray diffractometer according to claim 2 or 3. 5. The lower end portion of the locking member is detachably fixed to one end of the tilt base, and the base end portion of the support member is detachably fixed to the base base. The X-ray extraction angle setting mechanism of the vertical X-ray diffractometer according to Item 2, 3 or 4.