JP2759830B2 - X-ray analysis method and apparatus - Google Patents

Description

Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an X-ray structure analyzer that analyzes the structure of a sample using X-rays. In particular, the so-called EXAFUS (EXAF
The present invention relates to an X-ray structure analyzer that analyzes the fine structure of a sample based on S) or XANES.

[Prior Art] A so-called X-ray diffractometer is well known as an apparatus for analyzing the structure of a sample using X-rays. In this X-ray diffractometer, a sample is irradiated with X-rays, and the structure of the sample is analyzed based on the X-ray diffracted by the sample.

It is already known that there is a so-called Exafus measuring device as a device for analyzing the structure of a sample based on a principle different from the X-ray diffraction device.

In general, the energy of X-rays applied to a sample is gradually changed, and for each of the energies, the ratio (I) of the X-ray intensity (I ₀ ) incident on the sample and the X-ray intensity (I) transmitted through the sample is obtained. ₀ / I) and plotting on a graph, an X-ray absorption spectrum as shown in FIG. 6 is obtained. In this X-ray absorption spectrum, 50 ev
The absorption edge fine structure that appears in a narrow area is usually XANES (X-RAY Absorption Near Edge Structur).
e) is called. In addition, the intensity ratio that appears in a wide area of about 1000 ev toward the higher energy side than
The vibration structure of absorption coefficient (EXAFS: Extended)
X-RAY Absorption Fine Structure).

These Zaness and Exafus contain information on chemical bonds between the absorbing atom and the surrounding atoms, the three-dimensional structure of the molecule, the interatomic distance, the coordination, and the like.
Therefore, if an X-ray absorption spectrum as shown in FIG. 6 is obtained for an unknown sample, the structure of the unknown sample can be analyzed based on the X-ray absorption spectrum.

The above-mentioned exahus measuring apparatus performs a structural analysis of a sample based on such an exahus. In order to obtain a reliable result, it is common to measure not only the exahus but also the senes in this exahus measuring apparatus.

By the way, as described above, in obtaining the X-ray absorption spectrum of FIG. 6, it is necessary to sequentially irradiate the sample with X-rays while changing the energy amount by a predetermined step width every predetermined crystal fixing time. In the Exafus region, for example, a step width of 2 to 10 ev is taken every crystal fixation time of 2 to 10 seconds.
Each sample is irradiated with X-rays while changing the amount of energy for measurement. On the other hand, in the sorness region, for example, X-rays are irradiated while changing the amount of energy by a step width of 0.5 to 1 ev every crystal fixing time of 80 seconds. As described above, the scanning manner of the X-ray energy must be changed significantly between the Exhaust region and the Zerness region.

Further, in obtaining the X-ray absorption spectrum of FIG. 6, it is necessary to change the so-called energy resolution between the Xavihs region and the Zerness region. The energy resolution is a value determined substantially by the focal point of the X-rays, that is, the line width, when the energy amount of the irradiated X-rays is constant. Are required respectively. As described above, the energy resolution between the Exhaust region and the Zerness region must be significantly changed.

As described above, when the X-ray absorption spectrum is obtained, the scanning step width and the fixed holding time of the X-ray energy and the energy resolution must be significantly changed between the Xavis region and the Zerness region. In the conventional Exahus measurement apparatus, the measurement of the Exahus and the measurement of the senes are performed separately and independently.
For this reason, work efficiency was very bad.

The present invention has been made in view of the above points,
It is an object of the present invention to provide an X-ray structure analysis method and an X-ray structure analysis method capable of continuously measuring both the Xavis and the Zerness by one device and improving the work efficiency of the sample structure analysis. .

[Means for Solving the Problems] In order to achieve the above object, the X-ray analysis method according to claim 1 causes X-rays generated from an X-ray generator to enter a spectral crystal, and the incident X-ray of the spectral crystal The angle to the line
X-rays are diffracted by the spectroscopic crystal and irradiated onto the sample while changing stepwise by a predetermined step angle for each predetermined crystal fixed holding time, and the intensity of the X-rays incident on the sample and the X-rays transmitted through the sample In the X-ray analysis method for analyzing the sample by measuring the intensity of the X-ray, the line width of the X-rays coming out of the spectral crystal and entering the sample, the above-mentioned crystal fixed holding time and the above-mentioned step angle are determined by the incidence of the spectral crystal. It is characterized in that it is changed according to the angle with respect to the X-ray.

According to a second aspect of the present invention, there is provided an X-ray analysis method according to the first aspect, in which the X-ray analysis apparatus exits the X-ray generation device instead of changing the line width of the X-ray incident on the sample. The line width of the X-ray incident on the crystal is changed according to the angle of the spectral crystal with respect to the incident X-ray.

The X-ray analyzer according to claim 3 is an X-ray generator that generates X-rays, a spectral crystal that diffracts X-rays emitted from the X-ray generator and impinges the X-rays on the sample, and an X-ray that impinges on the sample. Incident X-ray intensity detecting means for measuring the intensity of X-rays, transmitted X-ray intensity detecting means for measuring the intensity of X-rays transmitted through the sample, and a spectroscopic crystal variably supported so that the X-ray incident angle changes. The crystal / sample supporting means for supporting the sample so that the X-ray diffracted by the spectral crystal always enters the sample even when the angle of the spectral crystal changes, and the angle of the spectral crystal with respect to the incident X-ray is set to a predetermined value. An X-ray analysis apparatus having a crystal drive control means for changing the crystal stepwise by a predetermined step angle for each crystal fixation holding time, wherein the crystal drive control means is arranged on the X-ray optical path from the spectral crystal to the sample, and the width is adjustable. One receiving slit and one receiving slit Width, the crystal fixed hold time and step angle in crystal drive control means, characterized by providing a first measurement condition changing means for changing in accordance with the angle with respect to the incident X-ray analyzing crystal.

This X-ray analysis apparatus is an X-ray analysis apparatus suitable for carrying out the X-ray analysis method according to claim 1. By adjusting the width of the light-receiving slit, which is arranged at a width and which can be adjusted, the configuration requirements of claim 1,
"Change the line width of the X-rays coming out of the spectral crystal and entering the sample."

The X-ray analyzer according to the fourth aspect has the same configuration requirements as those of the X-ray analysis apparatus according to the third aspect.
An X-ray analyzing apparatus having an X-ray generator supporting means for supporting the X-ray generating apparatus so that the angle of the X-ray generating apparatus with respect to the spectral crystal can be changed, and an angle of the X-ray generating apparatus with respect to the spectral crystal. And a second measurement condition changing means for changing the crystal fixed holding time and the step angle in the crystal driving control means in accordance with the angle of the spectral crystal with respect to the incident X-ray.

This X-ray analysis apparatus is an X-ray analysis apparatus suitable for implementing the X-ray analysis method according to the second aspect. By changing the angle of the X-ray generator with respect to the spectral crystal, the apparent X-ray focal width is changed by changing the X-ray extraction angle with respect to the X-ray generator. By changing the apparent X-ray focal width in this way,
A main component of the X-ray analysis method according to claim 2, which is "changes the line width of the X-rays exiting the X-ray generator and entering the spectral crystal according to the angle of the spectral crystal with respect to the incident X-rays", is realized. I do.

Furthermore, the X-ray analyzer according to claim 5 has the same configuration requirements as those of the X-ray analyzer according to claim 3.
An X-ray analysis apparatus having an X-ray generator, wherein the X-ray generator is disposed along a filament that emits electrons, a target with which the electrons collide, and an electron path from the filament to the target. And a third measurement in which a bias voltage applied to the electrode, a crystal fixed holding time in the crystal driving control means, and a step angle are changed according to an angle of the spectral crystal with respect to the incident X-ray. A condition changing means is provided.

This X-ray analysis apparatus is an X-ray analysis apparatus suitable for carrying out the X-ray analysis method according to claim 2, and specifically, by changing a voltage applied to the electrode having the above-mentioned configuration requirements. The width of the X-ray focus on the target is changed by adjusting the width of the electrons from the filament to the target. By changing the width of the X-ray focal point in this way, "changing the line width of the X-ray exiting the X-ray generator and entering the spectral crystal according to the angle of the spectral crystal with respect to the incident X-ray" is claimed. The main constituent requirements of the X-ray analysis method 2 are realized.

[Function] According to the first aspect of the invention, the diffracted X-ray diffracted by the dispersive crystal (9) and incident on the sample (11) according to the angle (θ) of the dispersive crystal (9) with respect to the incident X-ray (A). The line width of (B) is changed. As a result, an energy resolution suitable for each of the Xavihs and the Zerness can be selected.

At the same time, the crystal fixed holding time, which is the time for keeping the dispersive crystal (9) at one angle (θ), and the step width, which is the change width of the angle of the dispersive crystal (9), are changed. . As a result, an energy scanning mode suitable for each of the Xavis and the Zurness can be selected. The angle (θ) of the dispersive crystal (9) is changed by changing the wavelength of the diffracted X-rays.
This is to change the amount of energy of X-rays incident on.

According to the second aspect of the present invention, instead of changing the line width of the diffracted X-ray (B), the line width of the X-ray (A) incident on the spectral crystal (9) is changed by the angle (θ) of the spectral crystal (9). ),
Thereby, the energy resolution suitable for each of the Zaness and the Exafus is selected.

According to the invention of claim 3, X-rays emitted from the X-ray generator (5)
The line is diffracted by the dispersive crystal (9) and is incident on the sample (11).
X-ray intensity (I ₀ ) incident on the sample and X-ray transmitted through the sample
The line intensity (I) is detected by X-ray intensity detecting means (incident X-ray intensity detecting means 13a, transmitted X-ray intensity detecting means 13b). Based on the detected intensities, a target X-ray absorption spectrum is obtained.

The crystal / sample supporting means is usually called a goniometer, and includes an angle (θ) of the dispersive crystal (9) with respect to the incident X-ray and an angle (2θ) of the sample (11) with respect to the incident X-ray. Are moved little by little while keeping the relationship constant. The crystal drive control means drives the above-mentioned crystal / sample support means and gradually changes the angle (θ) of the spectral crystal (9).
By the action of the crystal / sample support means and the crystal drive control means, the energy amount of the X-ray incident on the sample (11) is gradually changed. That is, the coordinate position of the horizontal axis in the graph of FIG. 6 is determined.

First measurement condition changing means (control device 24, operating device 25)
Describes at least three measurement condition items such as the slit width (18) of the light receiving slit (12), the crystal fixed holding time, and the angular step width of the spectral crystal (that is, the energy step width). (The amount of energy of X-rays incident on the laser beam 11). This makes it possible to automatically adapt the measurement conditions to each of the Zaness area and the Exahus area.

According to the fourth aspect of the present invention, the angle of the X-ray generator (5) with respect to the spectral crystal (9), the crystal fixed holding time, and the angular step of the spectral crystal are controlled by the second measurement condition changing means (control device 24, operating device 25). At least three measurement condition items of the width are changed and set in accordance with the angle (θ) of the spectral crystal.
By changing the angle of the X-ray generator (5), the angle of extraction of X-rays (A) from the X-ray generator toward the dispersive crystal (9) is changed to change the apparent focal width.
The energy resolution for obtaining the X-ray absorption spectrum (FIG. 6) is adapted to the Exahus region or the Zaness region.

According to the fifth aspect of the present invention, the focal length of the electron beam irradiated onto the target (7), the crystal fixed holding time, and the angular step width of the spectral crystal are measured by the third measurement condition changing means (control device 24, operating device 25). Are changed and set in accordance with the angle (θ) of the spectral crystal.
By changing the focal width of the electron flux, the spectral crystal (9)
The energy resolution for obtaining the X-ray absorption spectrum is adjusted to the Xavihs region or the Zaness region by changing the focal width of the X-ray (A) toward the X-ray.

Embodiment FIG. 1 schematically shows an entire embodiment of an X-ray structure analyzing apparatus according to the present invention.

In the figure, sample link 2, crystal link 3 and X
Three links of the line link 4 are connected to the rotation center 1. The X-ray link 4 is fixed and does not move, but the crystal link 3 and the sample link 2 rotate around the rotation center.

An X-ray generator 5 is fixed to the tip of the X-ray link 4, and a filament 6 and a target 7 that rotates at an appropriate speed are provided in the X-ray generator.
An appropriate voltage is applied to the filament 6, and electrons are emitted from the filament 6 by this voltage application. The emitted electrons impinge on the target 7 and X-rays are extracted as shown by a broken line A at an appropriate extraction angle, for example, 12 °.

At the tip of the crystal link 3, a base 8 is fixed.
On the base, a spectral crystal, for example, germanium (440) 9
Has been fixed. The X-rays extracted from the target 7 are radiated to the spectral crystal 9, and are diffracted by the spectral crystal as indicated by a broken line B.

A base 10 is fixed to the tip of the sample link 2,
On the base, receiving slit 12, in the order of X-ray irradiation direction B,
An incident X-ray intensity detecting means 13a, a sample 11 to be measured, and a transmitted X-ray intensity detecting means 13b are provided. Both X-ray intensity detecting means 13a and 13b are, for example, a semiconductor detector (SSD) 1
Consists of three.

As shown in FIG. 2, the light receiving slit 12 includes a base member 15 having a rectangular hole 14 formed therein and two shielding plates 16 provided on both sides of the base member and movable as indicated by an arrow E. And These shielding plates 16 are driven by driving means 17 such as a solenoid and a pulse motor, and move between a solid line position and a chain line position. At the position of the solid line, the slit gap 18 is wide (W), and at the position of the chain line, the slit gap 18 is narrow (N).

In FIG. 1, the intensity (I ₀ ) of the X-ray diffracted by the spectral crystal 9 and incident on the sample 11 is detected by the incident X-ray intensity detecting means 13a. I) is detected by the transmitted X-ray intensity detecting means 13b. The detection output of each of these detection means 13a and 13b is
26, the intensity ratio (I ₀ / I) is calculated by this measuring instrument.

A feed screw 19 is attached between the X-ray generator 5 and the spectral crystal base 8, and an X-ray is attached to the right end of the feed screw 19.
The axis pulse motor 20 is connected. A feed screw 21 is also provided between the spectral crystal base 8 and the sample base 10, and a Y-axis pulse motor 22 is mounted on the upper end of the feed screw 21.
Is connected. By the rotation of the X-axis pulse motor 20,
The base 8 moves along the virtual circle 23, and at this time,
Changes with respect to the incident X-ray. If the angle θ changes, the wavelength of the X-ray diffracted by the dispersive crystal 9 changes, whereby the energy amount of the X-ray incident on the sample 11 can be changed.

Y-axis pulse motor according to rotation of X-ray pulse motor 20
22 also rotates by an appropriate angle, and the sample 11 with respect to the
Is always maintained at 2θ. Thus, the X-ray can be always guided to the sample 11 even when the angle θ of the spectral crystal 9 changes.

The mechanical configuration of the X-ray structural analysis apparatus according to the present invention is roughly as described above. Hereinafter, a measurement procedure performed by the control device 24 will be described. The control device 24 incorporates a microcomputer, and the operation control described below is automatically executed according to a predetermined program.

First, measurement conditions are instructed to the control device 24 via the operation device 25 such as a keyboard. As the measurement conditions to be indicated,
As shown in the attached Table 1, there are a measurement section, an energy step width, and a light receiving slit width. The crystal fixed holding time in the table can be instructed in advance at the same time as each of the above elements, but in the present embodiment, as described later, the length of the length is controlled by the control device 24 in relation to the light receiving slit width. The settings are changed automatically.

What is being obtained now is the X-ray absorption spectrum shown in FIG. The measurer sets some approximate measurement intervals in advance with a rough idea of the X-ray absorption spectrum. In the embodiment, four measurement sections are set: a section which is an area before the Zerness, a b section which is an area including the Zerness, a c section which includes an initial area of Exahus, and a d section which includes a late area of the Exahus. I have.

After the measurement sections are set, the energy step width in each measurement section is determined. In the apparatus according to this embodiment, in FIG. 1, the angle θ of the dispersive crystal 9 is fixed at a certain angle (θ1) for a predetermined short time, and the incident X-ray intensity (I ₀ ) And the transmitted X-ray intensity (I) are detected, and the intensity ratio (I ₀ / I) is calculated by the measuring instrument 26. Then, the result is plotted on FIG. When one plot is completed, the angle θ of the spectral crystal 9 is rotated to the next angular position (θ2), and the intensity ratio (I ₀ / I) at that position is obtained and plotted on the drawing. Such an operation is repeated many times to obtain an X-ray absorption spectrum as shown in FIG. The energy step width is a change width (θ2−θ1) of the angle θ of the dispersive crystal 9. Note that the crystal fixed holding time means that the spectral crystal 9 is rotated by one angle (θ1 or θ2) while one plot point is obtained.
It is the time to keep it fixed.

In the embodiment, in the section b in which it is predicted that the X-ray absorption spectrum suddenly rises and the surge region is included,
The energy step width is very short, for example, set to about 0.5ev. In other words, in this section, the angle of the spectral crystal 9 is very finely changed.

The light receiving slit width is the width of the slit gap 18 as described with reference to FIG. In this embodiment, the slit width in section b is narrow, for example, 0.1 mm
It is set to the degree. This is because, as described above, the required resolution differs between the Exhaust region and the Zerness region, and the measurement conditions are adapted to it.

With the above, the instruction of the measurement condition to the control device 24 is completed. Thereafter, when a start button (not shown) provided on the operating device 25 is pressed, the device operates according to the set measurement conditions in Table 1. In this case, the energy step width and the like are automatically changed according to the measurement sections a, b, c, and d, that is, according to the angle θ of the spectral crystal 9 with respect to the incident X-ray. X-ray absorption spectra are continuously and automatically determined.

In this case, since the slit width is reduced in the section b, the incident X-ray intensity (I ₀ ) tends to decrease in this section. This decrease in X-ray intensity is detected by the incident X-ray intensity detection means 13a. Then, in response to the decrease in the X-ray intensity, the control device 24 automatically extends the crystal fixed holding time in the section b, for example, to 80 seconds so that the incident X-ray intensity (I ₀ ) becomes constant. Thus, even when the width of the light receiving slit is changed, it is possible to always obtain incident X-rays having a constant intensity, and to obtain accurate measurement results.

In the related art, the sections a to b and the sections c to d in FIG. 1 must be measured separately and compared with each other later. You don't have to do extra work.

 FIG. 3 shows a second embodiment.

This embodiment is different from the previous embodiment shown in FIG. 1 in that the X-ray generator 5 has an X-ray link 4 as shown in FIG.
Is rotatable with respect to. By rotating the X-ray generator 5, the angle at which the X-ray is extracted from the target 7 can be converted between 6 ° and 12 °. The rotation of the X-ray generator 5, that is, the change of the X-ray take-out angle is changed according to the measurement sections a, b, c, and d, for example, as shown in Table 2. The reason why the take-out angle is reduced in the sections a and b is that the apparent focus of the X-rays incident on the spectral crystal 9, that is, the X-ray width is narrowed to obtain an energy resolution suitable for the Zaness region. That's why.

Also in the second embodiment, an X-ray absorption spectrum as shown in FIG. 6 is continuously and automatically obtained.

In this embodiment, the light receiving slit 12 is not a slit slit variable type as shown in FIG.
A slit having a fixed gap can be used.

 FIG. 5 shows a main part of the third embodiment.

The mechanical configuration of this embodiment can be the same as that shown in FIG. 1 and FIG. What is different is the internal structure of the X-ray generator 5. FIG. 5 shows a main part inside the X-ray generator 5. Although the target 7 is shown linearly, it is actually cylindrical as shown in FIG.

The fact that the filament 6 is provided to fly electrons toward the target 7 is the same as in the previous two embodiments. The difference is that an electrode 27 is provided around the electron path from the filament 6 to the target 7. Two different voltages are applied to the electrode 27 from a voltage application circuit 28. When a different voltage is applied to the electrode 27, the degree of attraction of the electrons moving from the filament 6 to the target 7 by the electrode 27 is different, so that the focal width of the electrons on the target 7 changes.

In the embodiment, as shown in Table 3, the focal width is narrowed to 0.1 mm corresponding to the section b including the zerness region, and is increased to 0.5 mm in other sections. It is.

As described above, if the electron focal width on the target 7 is changed, the line width of the generated X-rays A also changes, so that the energy resolution can be appropriately switched to suit the respective values of Xerness and Exahus.

Also in the cases shown in Tables 2 and 3, the crystal fixed holding time is automatically changed and set by the control device 24 according to the fluctuation of the incident X-ray intensity (I ₀ ).

Although the present invention has been described with reference to the three embodiments, the present invention is not limited to these embodiments and can be variously modified.

For example, as the measurement conditions to be changed corresponding to the measurement sections a, b, c, and d, in addition to the combinations in Tables 1 to 3, an energy step width, a crystal fixed holding time, a light receiving slit width, and X-ray extraction The four corner items can be changed. In addition, energy step width, crystal fixed holding time,
It is also possible to set so as to change four items of the light receiving slit width and the X-ray focus.

In FIG. 2, the slit gap of the light receiving slit 12 is changed between two positions of a solid line position and a chain line position. However, the present invention is not limited to this, and the slit gap is steplessly changed according to the measurement sections a to d. It can also be adjustable. By doing so, more accurate measurement results can be obtained.

The measurement section is not limited to the four sections a and b, and can be further finely divided. In addition, the position to be divided can be arbitrarily set according to the property of the sample to be measured.

The links 2, 3, and 4 shown in FIG. 1 and FIG.
The crystal / sample supporting means including the 21 and the pulse motors 20 and 22 is generally called a goniometer,
The intended effect is that the angle (θ) of the dispersive crystal 9 and the sample
With the eleven angles (2θ) being kept constant at all times, they are changed little by little. As long as this action is achieved, it goes without saying that a goniometer having a configuration other than the goniometer shown in FIGS. 1 and 3 can be used in the present invention.

The numerical values of the respective measurement items listed in Tables 1 to 3 are merely examples, and in actual analysis work, depending on the sample to be measured, the type of spectral crystal, the specific configuration of the analyzer, and the like, A more appropriate numerical value is selected.

[Effects of the Invention] According to the invention of claims 1 to 5, the energy resolution, the crystal fixed holding time, and the energy step width for obtaining the X-ray absorption spectrum are changed according to the angle of the spectral crystal.
That is, since it can be changed in accordance with the amount of energy of the X-rays incident on the sample, the measurement of the Xavis and the Xerness can be continuously performed by one device, and the analysis work becomes very easy.

[Brief description of the drawings]

FIG. 1 is a schematic diagram showing an embodiment of an X-ray analysis apparatus according to the present invention, FIG. 2 is a schematic diagram showing an example of a light receiving slit used in the embodiment, and FIG. 3 is an X-ray analysis according to the present invention. FIG. 4 is a schematic view showing another embodiment of the apparatus, FIG. 4 is a plan view showing an example of an X-ray generator used in the embodiment, FIG. 5 is a schematic diagram showing an example of the internal structure of the X-ray generator, FIG. FIG. 6 is a graph showing an example of the X-ray absorption spectrum of the sample. 5 X-ray generator, 9 Spectral crystal, 13 X-ray intensity detecting means, 2, 3, 4 Link, 24 Control device 20, 22
... Pulse motor, 12 ... Slit, 25 ... Operation device, 6 ... Filament, 7 ... Target, 27 ... Electrode

Claims (5)

(57) [Claims] An X-ray generated from an X-ray generator is made incident on a spectral crystal, and the angle of the spectral crystal with respect to the incident X-ray is determined by:
X-rays are diffracted by the spectroscopic crystal and irradiated onto the sample while changing stepwise by a predetermined step angle for each predetermined crystal fixed holding time, and the intensity of the X-rays incident on the sample and the X-rays transmitted through the sample To analyze the sample by measuring the strength of X
In the X-ray analysis method, the line width of the X-ray coming out of the spectral crystal and entering the sample, the crystal fixed holding time and the step angle are changed according to the angle of the spectral crystal with respect to the incident X-ray. X-ray analysis method. 2. The X-rays exiting the X-ray generator and entering the spectral crystal instead of the line width of the X-rays exiting the spectral crystal and entering the sample.
2. The X-ray analysis method according to claim 1, wherein the line width of the line is changed according to an angle of the spectral crystal with respect to the incident X-ray. 3. An X-ray generator for generating X-rays, a spectral crystal for diffracting X-rays emitted from the X-ray generator and causing the X-ray to enter a sample, and an incident X-ray for measuring the intensity of the X-rays incident on the sample. X-ray intensity detection means, X-ray transmission intensity detection means for measuring the intensity of X-rays transmitted through the sample, and a spectroscopic crystal variably supported so that the X-ray incident angle changes, and the angle of the spectroscopic crystal changes The crystal / sample supporting means for supporting the sample so that the X-ray diffracted by the spectral crystal always enters the sample, and the angle of the spectral crystal with respect to the incident X-ray is set at a predetermined time for each fixed crystal holding time. An X-ray analysis apparatus having a crystal drive control means for changing the step angle stepwise by a step angle, a light receiving slit arranged on an X line from the spectral crystal to the sample and having an adjustable width, and a width of the light receiving slit. , Crystal drive control X-ray analysis apparatus, characterized in that the crystal fixed hold time and step angle in stages, provided with a first measurement condition changing means for changing in accordance with the angle with respect to the incident X-ray analyzing crystal. 4. An X-ray generator for generating X-rays, a spectral crystal for diffracting X-rays emitted from the X-ray generator and causing the X-rays to enter a sample, and an incident X-ray for measuring the intensity of the X-rays incident on the sample. X-ray intensity detection means, transmitted X-ray intensity detection means for measuring the intensity of X-rays transmitted through the sample, and a variable angle support for the spectral crystal so that the incident angle of X-rays changes, and the angle of the spectral crystal changes The crystal / sample supporting means for supporting the sample so that the X-ray diffracted by the spectral crystal always enters the sample, and the angle of the spectral crystal with respect to the incident X-ray is set at a predetermined time for each fixed crystal holding time. An X-ray analysis device having crystal drive control means for changing the step angle of the X-ray generation device stepwise, wherein the X-ray generation device supports the X-ray generation device so that the angle of the X-ray generation device with respect to the spectral crystal can be changed. Means and X-ray generation A second measuring condition changing means for changing the angle of the crystal with respect to the dispersive crystal, the crystal fixed holding time in the crystal driving control means, and the step angle in accordance with the angle of the dispersive crystal with respect to the incident X-ray. Line analyzer. 5. An X-ray generator for generating X-rays, a spectral crystal for diffracting X-rays emitted from the X-ray generator and causing the X-rays to enter a sample, and an incident X-ray for measuring the intensity of the X-rays incident on the sample. X-ray intensity detection means, transmitted X-ray intensity detection means for measuring the intensity of X-rays transmitted through the sample, and a variable angle support for the spectral crystal so that the incident angle of X-rays changes, and the angle of the spectral crystal changes The crystal / sample supporting means for supporting the sample so that the X-ray diffracted by the spectral crystal always enters the sample, and the angle of the spectral crystal with respect to the incident X-ray is set at a predetermined time for each fixed crystal holding time. An X-ray analysis apparatus comprising: a crystal drive control unit that changes the step angle by a step angle of: a filament that emits electrons, a target that the electrons collide with, and a filament to a target. And a bias voltage applied to the electrode, a crystal fixed holding time and a step angle in the crystal drive control means according to an angle of the spectral crystal with respect to an incident X-ray. An X-ray analyzer, comprising: a third measurement condition changing means for changing.