JP3593412B2 - X-ray analyzer and attachment for X-ray fluorescence analysis - Google Patents

Description

[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to an X-ray analyzer for analyzing a crystal structure or the like of a sample using X-rays, and a fluorescent X-ray analyzer attached to an X-ray diffractometer so that X-ray fluorescence analysis can be easily performed. Regarding attachments.
[0002]
[Prior art]
2. Description of the Related Art Conventionally, an X-ray diffractometer and a fluorescent X-ray analyzer have been known as X-ray analyzers for analyzing a crystal structure or the like of a sample using X-rays.
Among them, the X-ray diffractometer irradiates the sample S with the X-rays emitted from the X-ray source 1 and detects the diffracted X-ray diffracted by the sample S by the X-ray detector 21 as shown in FIG. It has an optical system. Here, assuming that the incident angle of the X-ray with respect to the sample S is θ, the diffraction angle of the X-ray with respect to the incident X-ray has a relationship of 2θ (twice θ) (Bragg diffraction condition), and the peak of the diffracted X-ray 2θ at which the intensity appears is a unique angle according to the crystal structure of the sample S.
[0003]
Therefore, in the X-ray diffraction apparatus, the sample S is mounted on the θ rotation table 4 of a goniometer 6 called a goniometer 6, the sample S is rotated θ with respect to the X-ray from the X-ray source 1, and the 2θ rotation of the goniometer 6 is performed. An X-ray detector 21 is provided on the arm 5, and the diffraction angle 2θ when the X-ray detector 21 detects the peak intensity of the diffracted X-ray diffracted by the sample S is measured by the goniometer 6.
[0004]
On the other hand, the X-ray fluorescence analyzer irradiates the sample S with the X-rays emitted from the X-ray source 1 as shown in FIG. The optical system has an optical system that restricts the divergence of the separated fluorescent X-rays by the solar slit 11 and then guides the divergence to the X-ray detector 21.
Here, the spectral crystal 10 is provided on the θ-rotation table 4 of the goniometer 6, and the solar slit 11 and the X-ray detector 21 are provided on the 2θ-rotation arm 5 of the goniometer 6. The structure is such that the spectral angle 2θ ′ of the fluorescent X-ray is measured by the goniometer 6.
[0005]
[Problems to be solved by the invention]
By the way, if the X-ray diffraction measurement and the X-ray fluorescence analysis can be performed together on a sample, it is possible to expect a more accurate analysis result than the analysis result of the sample obtained in either one. .
[0006]
However, the conventional X-ray diffractometer and X-ray fluorescence analyzer are each configured as a dedicated analyzer, and none of them can perform X-ray diffraction measurement and X-ray fluorescence analysis with one analyzer. .
Therefore, when the X-ray diffraction measurement and the X-ray fluorescence analysis are to be performed simultaneously, both the X-ray diffraction apparatus and the X-ray fluorescence analysis apparatus must be provided, which requires a large amount of equipment cost and is economical. There was a problem that the burden was large.
[0007]
The present invention has been made in order to solve such a problem, and an object of the present invention is to enable a single analyzer to easily perform X-ray diffraction measurement and X-ray fluorescence analysis.
[0008]
[Means for Solving the Problems]
In order to achieve the above object, first, an attachment for X-ray fluorescence analysis of the present invention irradiates a goniometer provided with a θ rotation unit and a 2θ rotation unit and a sample provided in the θ rotation unit of the goniometer with X-rays. The following configuration is provided to be mounted on an X-ray diffraction apparatus including an X-ray source and an X-ray detector installed in a 2θ rotating section of a goniometer.
[0009]
{Circle around (1)} A spectral crystal that is installed in the θ rotating part of the goniometer and disperses fluorescent X-rays emitted from the sample in response to X-ray irradiation. Solar slit to limit line direction and divergence
By attaching this attachment to the X-ray diffraction apparatus, the following optical system for X-ray fluorescence analysis can be easily formed on the apparatus. That is, when the sample is irradiated with X-rays generated by the X-ray source, the sample is excited and fluorescent X-rays having a wavelength λ peculiar to the sample are emitted. The fluorescent X-rays are irradiated on the spectral crystal to separate them. The fluorescent X-rays thus dispersed are passed through a solar slit provided in a 2θ rotating section of a goniometer, and then guided to an X-ray detector. Here, the solar slit has a function of limiting the direction and divergence of the fluorescent X-ray.
Then, the X-ray fluorescence analysis of the sample can be performed by measuring the spectral angle when the X-ray detector detects the peak intensity of the fluorescent X-ray with a goniometer.
[0011]
In the attachment for X-ray fluorescence analysis described above, it is preferable that the crystal plane of the spectral crystal be positioned with respect to the sample as follows. That is, the crystal plane of the spectral crystal is arranged in parallel with an arbitrary virtual plane passing through the sample surface of the sample, and an arbitrary interval is provided between the crystal plane and the virtual plane. With such a positional relationship, the fluorescent X-rays emitted from the sample can be reliably incident on the crystal plane of the spectral crystal.
[0012]
In addition, a second X-ray detector installed on the 2θ rotation unit of the goniometer is added to the components of the attachment for X-ray fluorescence analysis, and X-rays that have passed through the solar slit during X-ray fluorescence analysis are converted to the second X-ray. You may make it detect with an X-ray detector. In this case, the X-ray detector originally provided in the X-ray diffraction apparatus is an X-ray detector dedicated to X-ray diffraction measurement, and for example, it is possible to simultaneously perform X-ray diffraction measurement and X-ray fluorescence analysis. .
[0013]
Further, a slit means which is fixed to the main body of the goniometer and restricts the direction and divergence of the fluorescent X-ray radiated from the sample and guides the X-ray to the spectral crystal may be added to the constituent elements of the present invention. By adding such a slit means, the scattered X-rays can be shielded, and the S / N ratio (peak intensity / background intensity ratio) of the fluorescent X-rays guided to the spectral crystal can be improved, and the measurement accuracy can be improved. Can be raised.
[0014]
Next, the X-ray analyzer according to the present invention includes a goniometer having a θ rotation unit and a 2θ rotation unit, a mounting portion for a sample installed in the θ rotation unit of the goniometer, and an X-ray for irradiating the sample with X-rays. A source and a spectral crystal installed on the θ-rotating part of the goniometer and dispersing fluorescent X-rays emitted from the sample in response to X-ray irradiation, and a fluorescent X-ray placed on the 2θ rotating part of the goniometer and spectrally separated by the spectral crystal And a X-ray detector installed at the 2θ rotating part of the goniometer to detect diffracted X-rays from the sample or fluorescent X-rays passing through the solar slit.
[0015]
When performing X-ray diffraction measurement with this X-ray analyzer, a sample is mounted on a mounting portion of the sample, and the sample is irradiated with X-rays generated by an X-ray source, and diffracted X-rays diffracted from the sample are analyzed. Detect with an X-ray detector. Then, the diffraction angle 2θ when the X-ray detector detects the peak intensity of the diffracted X-ray is measured by a goniometer.
[0016]
On the other hand, when performing X-ray fluorescence analysis using this X-ray analyzer, a sample is mounted on a mounting portion of the sample, and the sample is irradiated with X-rays generated by an X-ray source, and the fluorescent X-ray emitted from the sample is irradiated. A line is irradiated on the dispersive crystal. The fluorescent X-rays separated by the spectral crystal are guided to an X-ray detector after limiting the direction and divergence by a solar slit. Then, the spectral angle 2θ ′ when the peak intensity of the fluorescent X-ray is detected by the X-ray detector is measured by a goniometer.
[0017]
In the above-mentioned X-ray analyzer, the X-ray detector is separately provided for the first and second X-ray detectors, and the X-ray diffracted by the sample during the X-ray diffraction measurement is converted to the first X-ray detector. , And the fluorescent X-rays that have passed through the solar slit during the fluorescent X-ray analysis may be detected by the second X-ray detector.
[0018]
Further, in the above-mentioned X-ray analyzer, a slit means for restricting the direction and divergence of the fluorescent X-ray emitted from the sample and guiding the X-ray to the spectral crystal may be fixed to the main body of the goniometer. By adding such a slit means, the scattered X-rays can be shielded, and the S / N ratio (peak intensity / background intensity ratio) of the fluorescent X-rays guided to the spectral crystal can be improved, and the measurement accuracy can be improved. Can be raised.
[0019]
Further, the X-ray analyzer according to the present invention may be configured such that the spectral crystal can be mounted on the mounting portion of the sample and the second sample mounting portion is provided at a position different from the mounting portion of the sample. In this case, at the time of X-ray diffraction measurement, the sample is mounted on the mounting part of the sample, and the solar slit is removed from the 2θ rotating part of the goniometer. Then, the sample is irradiated with X-rays generated by the X-ray source, diffracted X-rays diffracted from the sample are detected by the X-ray detector, and the detector detects the peak intensity of the diffracted X-rays. The diffraction angle 2θ is measured with a goniometer.
[0020]
On the other hand, at the time of X-ray fluorescence analysis, the spectroscopic crystal is mounted on the mounting portion of the sample, the sample is mounted on the second sample mounting portion, and the solar slit is installed on the 2θ rotating portion of the goniometer. Then, the sample is irradiated with X-rays generated by the X-ray source, and fluorescent X-rays emitted from the sample are irradiated on the spectral crystal. The fluorescent X-rays separated by the spectral crystal are converted into a parallel beam by limiting the direction and divergence by a solar slit, and then guided to an X-ray detector. When the X-ray detector detects the peak intensity of the fluorescent X-ray, Measure the spectral angle with a goniometer.
[0021]
Also in the above-mentioned X-ray analyzer, it is preferable that the crystal plane of the spectral crystal is arranged in parallel with an arbitrary virtual plane passing through the sample surface of the sample, and an arbitrary space is provided between the plane and the virtual plane. With such a positional relationship between the spectral crystal and the sample, the fluorescent X-rays emitted from the sample can be reliably incident on the crystal plane of the spectral crystal.
[0022]
BEST MODE FOR CARRYING OUT THE INVENTION
Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.
FIG. 1 is a configuration diagram of an X-ray analyzer according to an embodiment of the present invention.
This X-ray analyzer has a basic structure for X-ray diffraction measurement. That is, the basic structure is almost the same as that of the X-ray diffractometer shown in FIG. 10 and includes an X-ray source 1, a sample table 2 as a sample mounting section, and a first X-ray detector 3, and the X-ray source 1 Irradiates the surface (sample surface) of the sample S mounted on the sample stage with the first X-ray detector 3 to detect the diffracted X-ray diffracted on the sample surface.
[0023]
In the X-ray diffraction measurement, it is necessary to measure the incident angle θ of the X-ray with respect to the sample S and the X-ray diffraction angle 2θ from the sample with respect to the incident X-ray. For this reason, a goniometer 6 having a θ rotation table 4 as a θ rotation unit and a 2θ rotation arm 5 as a 2θ rotation unit is used. As described above, the goniometer 6 is a kind of goniometer, and has a structure in which the 2θ rotating arm 5 can rotate exactly twice θ, that is, 2θ rotation with respect to θ rotation of the θ rotation table 4. In the present invention, in some cases, the θ rotation unit (θ rotation table 4) of the goniometer 6 is fixed, and only the 2θ rotation unit (2θ rotation arm 5) is drive-controlled.
[0024]
The sample table 2 is mounted on the θ rotation table 4 of the goniometer 6, and has a structure in which the sample S can be mounted with the sample surface positioned at the rotation center of the table 4. Therefore, the sample S mounted on the sample stage 2 rotates θ together with the θ rotation table 4.
[0025]
Further, the first X-ray detector 3 is installed on the 2θ rotation arm 5 of the goniometer 6. Here, the rotation center of the 2θ rotation arm 5 coincides with the θ rotation table 4. Therefore, the first X-ray detector 3 rotates 2θ around the sample S together with the 2θ rotation arm 5.
[0026]
The X-ray source 1 is fixedly provided around the goniometer 6. A divergence slit (DS) 7 is provided in front of the X-ray source 1, and the divergence slit 7 limits the area of X-rays hitting the sample. In addition, a light receiving slit (RS) 8 and a scattering prevention slit (SS) 9 are provided in front of the first X-ray detector 3. 9 prevents the incidence of scattered X-rays.
Each of the above-described components is provided in a conventional X-ray diffractometer, and since the configuration is already well known, detailed description will be omitted.
[0027]
The X-ray analyzer according to this embodiment includes the following components necessary for performing X-ray fluorescence analysis in addition to the components for X-ray diffraction measurement described above. That is, the spectral crystal 10 is provided on the θ rotation table 4 of the goniometer 6, and the solar slit 11 and the second X-ray detector 12 are provided on the 2θ rotation arm 5.
[0028]
When a sample (substance) is irradiated with X-rays, atoms forming the sample are excited to emit X-rays (fluorescent X-rays). Since this fluorescent X-ray has a unique wavelength λ corresponding to the atomic structure of the sample (this is referred to as Mosley's relationship), the wavelength λ of the fluorescent X-ray is detected, and the elemental analysis of the sample is performed based on the detection result. Etc. can be performed. This is the basic principle of X-ray fluorescence analysis.
[0029]
The spectral crystal 10 is required to detect the wavelength λ of the fluorescent X-ray. That is, as shown in FIG. 9, when fluorescent X-rays are made incident on the spectral crystal 10 at the plane distance d at an incident angle θ ′, the X-rays are diffracted at an angle of 2θ ′ with respect to the incident X-rays. If the wavelength of the fluorescent X-ray is λ,
2d sin θ '= nλ (n is the reflection order)
X-rays diffracted only when the angle θ ′ satisfies the expression (Bragg's expression) cause interference. Therefore, the peak intensity of the fluorescent X-ray diffracted from the spectral crystal 10 is detected by the second X-ray detector 12, and 2θ ′ (spectral angle) at that time is detected by the goniometer 6, whereby the above equation is obtained. The wavelength λ can be determined.
[0030]
The spectral crystal 10 has a function of diffracting the fluorescent X-ray emitted from the sample in each crystal plane to cause interference. As the spectral crystal 10, it is preferable to use a single crystal flat plate having a known plane distance d.
[0031]
In this embodiment, the crystal plane of the spectral crystal 10 is positioned as follows with respect to the sample surface of the sample S mounted on the sample stage 2 (see FIG. 2).
That is, a virtual plane H passing through the center of the sample surface is assumed, and the crystal plane of the spectral crystal 10 is arranged in parallel with the virtual plane H, and an arbitrary plane is disposed between the virtual plane H and the crystal plane of the spectral crystal 10. An interval a is provided. If the virtual plane H is coincident with the crystal plane of the spectral crystal 10, fluorescent X-rays emitted from the sample surface cannot be incident on the crystal plane of the spectral crystal 10. Therefore, by providing the interval a as described above, the fluorescent X-rays emitted from the sample surface can be surely incident on the crystal plane of the spectral crystal 10.
[0032]
Further, by disposing the one end 10a of the spectral crystal 10 near the sample surface, the fluorescent X-rays emitted from the sample surface can be incident on the crystal surface of the spectral crystal 10 with a wide divergence angle.
[0033]
The solar slit 11 has a structure in which a large number of metal foils are arranged in parallel at predetermined intervals, and the fluorescent X-rays separated by the spectral crystal 10 are passed between the metal foils to form the fluorescent X-rays. The divergence of the rays is limited, and the angle of the fluorescent X-rays incident on the second X-ray detector 12 is selectively received. The solar slit 11 is installed before the second X-ray detector 12. At this time, it is preferable that the center axis of the solar slit 11 is positioned so as to coincide with the light receiving center axis of the second X-ray detector 12.
[0034]
Further, the solar slit 11 and the second X-ray detector 12 are arranged so that at least the center line portion of the fluorescent X-ray diffracted by the spectral crystal 10 is in the solar slit within the measurement range of the spectral angle required for the fluorescent X-ray analysis. The installation position is adjusted so that the light passes through 11 and enters the light receiving surface of the second X-ray detector 12.
[0035]
FIG. 8 is a graph showing the results of the study by the present inventors regarding the appropriate length of the dispersive crystal 10 and the appropriate position of the solar slit 11. In this study, the center of the sample surface was positioned at the rotation center of the 2θ rotation arm 5. Further, the crystal plane of the spectral crystal 10 was arranged in parallel with an arbitrary virtual plane H passing through the center of the sample plane, and the distance a from the virtual plane H was set to 5 mm (see FIG. 2).
[0036]
The dashed line in the figure indicates the distance L (the length in the longitudinal direction of the spectral crystal 10) from the center of the sample surface shown in FIG. With respect to the incident angle θ ′. From this graph, it can be seen that in order to secure the diffraction angle 2θ ′ of the fluorescent X-ray from 10 ° to 90 °, the spectral crystal 10 should be set at about L = 80 mm.
[0037]
8, the distance between the center line of the fluorescent X-ray diffracted by the spectral crystal 10 and a virtual plane H ′ passing through the center of the sample surface and parallel to the center line of the diffracted fluorescent X-ray is represented by b. The relationship between the interval b and the diffraction angle 2θ ′ of the fluorescent X-ray with respect to the spectral crystal 10 is shown. As shown in this graph, the interval b was about 10 mm in the range of the diffraction angle = 0 to 90 °. Therefore, as shown in FIG. 2, if the distance b ′ between the virtual plane H (H ′) and the central axis of the solar slit 11 is set to about 10 mm, the spectral angle required for the fluorescent X-ray analysis can be measured within the measurement range. In addition, the fluorescent X-ray diffracted by the spectral crystal 10 can be made incident on the light receiving surface of the second X-ray detector 12 through the solar slit 11.
[0038]
These results are examples of the case where the distance a is set to 5 mm. In an actual design, it is preferable to appropriately adjust the length of the spectral crystal 10 and the position of the solar slit 11.
[0039]
The X-ray analyzer having the above-described configuration can perform the X-ray diffraction measurement and the fluorescent X-ray analysis by one unit. That is, when performing the X-ray diffraction measurement, the X-ray generated by the X-ray source 1 is irradiated to the sample S mounted on the sample stage 2 and the diffracted X-ray diffracted by the sample S is converted into the first X-ray. Detector 3 detects. The X-ray incident angle θ to the sample S is adjusted by the θ rotation table 4 of the goniometer 6, and the diffraction angle 2θ of the diffracted X-ray is measured by the rotation angle of the 2θ rotation arm 5 of the goniometer 6. If the peak intensity of the diffracted X-ray and the diffraction angle 2θ at that time are measured in this way, the crystal structure and the like of the sample S can be analyzed based on the measurement results.
[0040]
Next, when performing the fluorescent X-ray analysis, the X-rays generated by the X-ray source 1 are irradiated on the sample S mounted on the sample stage 2, and the fluorescent X-rays emitted from the sample S are analyzed by the spectral crystal 10. Disperse. After the fluorescent X-rays thus dispersed pass through the solar slit 11, they are incident on the second X-ray detector 12. Then, the peak intensity of the fluorescent X-rays is detected by the second X-ray detector 12, and the spectral angle 2θ ′ at that time is detected by the goniometer 6, thereby obtaining the wavelength λ of the fluorescent X-rays. Structure and the like can be analyzed.
[0041]
In the X-ray fluorescence analysis, the sample S and the spectral crystal 10 are fixed (that is, the θ-rotation table 4 is fixed), and only the 2θ-rotation arm 5 is rotated to measure the X-ray fluorescence spectral angle. (See FIG. 3) and a θ rotation method (see FIG. 4) in which the 2θ rotation arm 5 measures the fluorescent X-ray spectral angle while rotating the sample S and the spectral crystal 10 together with the θ rotation table 4. You may do it.
[0042]
In the case of the fixed θ method, since the rotation angle of the 2θ rotation arm 5 becomes θ ′ as shown in FIG. 3, the spectral angle of the fluorescent X-ray is obtained by setting the reading of the 2θ rotation arm 5 to θ ′. On the other hand, in the case of the θ rotation method, the rotation angle θ ′ of the θ rotation table 4 is superimposed on the rotation angle of the 2θ rotation arm 5 as shown in FIG. The reading of the arm 5 is 2θ ′.
[0043]
Further, the spectral angle of the fluorescent X-rays in the fluorescent X-ray analysis may be measured, for example, by setting the state where the light receiving central axis of the second X-ray detector 12 is arranged in parallel with the crystal plane of the spectral crystal 10 to 0 °. . Thus if zero set the reading 2 [Theta] rotary arm 5 when it was 2 [Theta] _0, the angle obtained by subtracting the reading 2 [Theta] ₀ at zero set from 2θx readings shown is 2 [Theta] rotary arm 5 in a subsequent measurement (2 [Theta] _{0 -2θx)} is the spectral angle of the fluorescent X-ray.
For example, in reading 2 [Theta] ₀ of 2 [Theta] rotary arm 5 at zero set 90 °, when the 2 [Theta] rotary arm 5 when measuring the spectral angles showed readings 60 ° (2θx) is, 90 ° -60 ° = 30 ° Is the true spectral angle.
[0044]
The angle formed between the crystal plane of the spectral crystal 10 and the sample surface of the sample S can be set arbitrarily. That is, by arranging the surfaces in parallel or by arranging them at an angle of 45 °, 25 °, or the like, an appropriate arrangement for effectively causing the fluorescent X-rays emitted from the sample S to be incident on the spectral crystal 10 effectively. It is preferable to realize
Further, regarding the fluorescent X-ray analysis, the sample surface of the sample S does not have to be positioned at the center of the θ rotation table 4 of the goniometer 6.
[0045]
In the above-described embodiment, since the first and second X-ray detectors 12 are installed on the 2θ rotating arm 5, X-ray diffraction measurement and X-ray fluorescence analysis can be performed simultaneously. However, since only a single X-ray detector is installed on the 2θ rotating arm 5 and shared for both X-ray diffraction measurement and X-ray fluorescence analysis, it is also possible to reduce equipment costs. In this case, when performing X-ray diffraction measurement, a light receiving slit (RS) 8 and a scattering prevention slit (SS) 9 are provided in front of the X-ray detector. When performing the fluorescent X-ray analysis, a solar slit 11 is provided in front of the X-ray detector instead of the slits (RS, SS) 8 and 9.
[0046]
The spectral crystal 10 and the solar slit 11 required for the X-ray fluorescence analysis are prepared as attachments for the fluorescent X-ray analysis that can be attached to the X-ray diffraction apparatus, in addition to being previously installed as components of the X-ray analysis apparatus. You may. With such an attachment, a conventional X-ray diffraction apparatus can be provided with a function of X-ray fluorescence analysis with a slight improvement (providing an attachment mounting portion), and replacement of the apparatus is not required. The attachment for X-ray fluorescence analysis may include the second X-ray detector 12.
[0047]
FIG. 5 is a configuration diagram showing a modification in the case of performing the fluorescent X-ray analysis by the θ rotation method shown in FIG.
That is, an incident-side solar slit 31 as slit means is provided between the sample S and the dispersive crystal 10, and the incident-side solar slit 31 restricts the direction and divergence of the fluorescent X-rays emitted from the sample, and May be led. The incident-side solar slit 31 is fixed to a non-rotating portion of the main body of the goniometer, and is positioned so as to always guide the fluorescent X-ray in a fixed direction regardless of the θ rotation and the 2θ rotation of the goniometer.
[0048]
The incident side solar slit 31 shields the scattered X-rays and improves the S / N ratio (peak intensity / background intensity ratio) of the fluorescent X-rays guided to the spectral crystal, thereby increasing the measurement accuracy. Becomes possible.
In addition, as this slit means, a slit used in an ordinary X-ray apparatus can be applied. The slit means may be provided as an attachment for X-ray fluorescence analysis that can be mounted on an X-ray diffraction apparatus.
[0049]
6 and 7 are configuration diagrams showing another embodiment of the present invention.
The X-ray analyzer shown in the figure has a configuration in which the sample stage 2 (sample mounting unit) provided in the θ rotation unit of the goniometer 6 can mount the spectral crystal 10 instead of the sample. Further, a second sample mounting section 20 is provided at an arbitrary place different from the sample table 2. In addition, a single X-ray detector 21 is installed on the 2θ rotating arm 5, and the light receiving slit (RS) 8 and the scattering prevention slit (SS) 9 and the solar slit 11 are exchanged in front of the single X-ray detector 21. A slit mounting portion 22 that can be provided is provided.
[0050]
In this X-ray analyzer, when the sample S is mounted on the sample table 2 and the light receiving slit (RS) 8 and the scattering prevention slit (SS) 9 are mounted on the slit mounting section 22, an optical system for X-ray diffraction measurement is provided. Can be formed. On the other hand, if the spectral crystal 10 is mounted on the sample stage 2, the sample S is mounted on the second sample mounting section 20, and the solar slit 11 is mounted on the slit mounting section 22, an optical system for X-ray fluorescence analysis can be obtained. Can be formed.
[0051]
Here, it is preferable that the crystal surface of the spectral crystal 10 mounted on the sample stage 2 and the sample surface of the sample S mounted on the second sample mounting unit 20 have the same arrangement relationship as in the previous embodiment. Note that the second sample mounting section 20 may be installed at a location other than the goniometer 6.
[0052]
【The invention's effect】
As described above, according to the present invention, the X-ray diffraction measurement and the fluorescent X-ray analysis can be easily performed by one apparatus, so that the sample analysis can be performed with high accuracy at low equipment cost. be able to.
[Brief description of the drawings]
FIG. 1 is a plan configuration diagram of an X-ray analyzer according to an embodiment of the present invention.
FIG. 2 is a schematic plan view showing an arrangement relationship between a sample, a spectral crystal, and a solar slit in the same apparatus.
FIG. 3 is a schematic plan view showing an operation when X-ray fluorescence analysis is performed in a θ-fixed manner by the apparatus.
FIG. 4 is a schematic plan view showing an operation when X-ray fluorescence analysis is performed by a θ rotation method using the same apparatus.
FIG. 5 is a configuration diagram showing a modified example when performing X-ray fluorescence analysis by a θ rotation method using the same apparatus.
FIG. 6 is a plan view showing a state in which an optical system for X-ray diffraction measurement is formed by an X-ray analyzer according to another embodiment of the present invention.
FIG. 7 is a plan view showing a state where an optical system for X-ray fluorescence analysis is formed by the same apparatus.
FIG. 8 is a graph showing examination data on the arrangement relationship of a sample, a spectral crystal, and a solar slit of the X-ray analyzer shown in FIG.
FIG. 9 is a diagram for explaining a principle of spectral X-ray fluorescence by a spectral crystal.
FIG. 10 is a plan view showing a conventional X-ray diffraction apparatus.
FIG. 11 is a plan view showing a conventional X-ray fluorescence analyzer.
[Explanation of symbols]
1: X-ray source 2: Sample table 3: First X-ray detector 4: θ rotation table 5: 2θ rotation arm 6: Goniometer 10: Crystalline crystal 11: Solar slit 12: Second X-ray detector 20: Second sample mounting section 21: X-ray detector 22: slit mounting section 31: incident side solar slit S: sample

Claims (9)

A goniometer having a θ rotation unit and a 2θ rotation unit in the main body, an X-ray source for irradiating a sample provided in the θ rotation unit of the goniometer with X-rays, and an X-ray detector installed in the 2θ rotation unit of the goniometer An attachment for X-ray fluorescence analysis attached to an X-ray diffraction apparatus comprising:
A dispersive crystal that is installed on the θ-rotation part of the goniometer and that disperses fluorescent X-rays emitted from the sample with X-ray irradiation;
An attachment for X-ray fluorescence analysis, comprising: a solar slit installed on a 2θ rotating section of the goniometer and for limiting the direction and divergence of X-ray fluorescence separated by the spectral crystal. The fluorescence X-ray analysis attachment according to claim 1,
An attachment for X-ray fluorescence analysis, wherein the crystal plane of the spectral crystal is positioned so as to be parallel to an arbitrary virtual plane passing through the sample surface of the sample and at an arbitrary distance from the virtual plane. The attachment for fluorescent X-ray analysis according to claim 1 or 2,
An attachment for X-ray fluorescence analysis, comprising: a second X-ray detector installed on a 2θ rotating section of the goniometer and detecting X-ray fluorescence passing through the solar slit. The fluorescence X-ray analysis attachment according to any one of claims 1 to 3,
An attachment for X-ray fluorescence analysis, wherein the attachment is provided fixed to the main body of the goniometer, and slit means for restricting the direction and divergence of X-rays emitted from the sample and guiding the X-rays to the spectral crystal. a goniometer having a θ rotation unit and a 2θ rotation unit;
A mounting part for the sample installed on the θ rotating part of the goniometer,
An X-ray source for irradiating the sample with X-rays,
A dispersive crystal that is installed on the θ-rotation part of the goniometer and that disperses fluorescent X-rays emitted from the sample with X-ray irradiation;
A solar slit installed on the 2θ rotating part of the goniometer, for limiting the direction and divergence of the fluorescent X-rays separated by the spectral crystal,
An X-ray analyzer, comprising: an X-ray detector installed at a 2θ rotating section of the goniometer and detecting a diffracted X-ray from a sample or a fluorescent X-ray passed through the solar slit. The X-ray analyzer according to claim 5,
The X-ray detector includes a first X-ray detector that detects diffracted X-rays from a sample and a second X-ray detector that detects fluorescent X-rays that have passed through the solar slit. Characteristic X-ray analyzer. The X-ray analyzer according to claim 5 or 6,
An X-ray analyzer, which is provided fixed to the main body of the goniometer and has slit means for restricting the direction and divergence of fluorescent X-rays emitted from the sample and leading the X-ray to the spectral crystal. The X-ray analyzer according to claim 5, wherein the spectroscopic crystal can be mounted on the mounting portion of the sample, and a second sample mounting portion is provided at a position different from the mounting portion of the sample,
At the time of X-ray diffraction measurement, the sample was mounted on the mounting part of the sample, and the solar slit was removed from the 2θ rotating part of the goniometer,
At the time of X-ray fluorescence analysis, the spectroscopic crystal is mounted on the mounting portion of the sample, the sample is mounted on the second sample mounting portion, and the solar slit is installed on the 2θ rotating portion of the goniometer. Characteristic X-ray analyzer. The X-ray analyzer according to any one of claims 5 to 8,
An X-ray analyzer, wherein a crystal plane of the spectral crystal is positioned so as to be parallel to an arbitrary virtual plane passing through the sample surface of the sample and at an arbitrary interval between the virtual plane and the virtual plane.

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