JP3270829B2 - X-ray fluorescence analyzer - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention can remove at least one of a measurement error due to a variation in the distance between a sample and an X-ray source and a measurement error due to a change in the degree of vacuum during measurement with a simple structure in a short time. The present invention relates to a fluorescent X-ray analyzer.

[0002]

2. Description of the Related Art Conventionally, in fluorescent X-ray analysis, measurement errors due to variations in the distance between a sample and an X-ray source and measurement errors due to changes in the degree of vacuum during measurement have been serious problems. Regarding measurement errors due to variations in the distance between the sample and the X-ray source, for example, an optical displacement sensor that performs distance measurement using laser light is provided on the side of the X-ray source, and the sample is connected to the X-ray source. By moving horizontally from below to below the displacement sensor, measuring the distance to the X-ray source, adjusting the height of the sample so that this becomes a constant value, and moving horizontally back below the X-ray source to return , Has been removed. In addition, measurement errors due to changes in the degree of vacuum during measurement are removed, for example, by taking sufficient time for evacuation, measuring the degree of vacuum, and controlling the degree of vacuum to a constant high vacuum. ing.

[0003]

However, an apparatus for removing a measurement error due to a variation in the distance between a sample and an X-ray source using a displacement sensor requires a mechanism for strictly moving the displacement sensor and the sample horizontally. However, the configuration of the device becomes complicated.
In addition, a device that controls the degree of vacuum to be measured to a constant high vacuum and removes measurement errors due to changes in the degree of vacuum during measurement requires a high-precision vacuum gauge and control mechanism, and the configuration of the device is complicated. Until it reaches a certain high vacuum
That is, it takes time to start the measurement. In order to reduce the waiting time until the start of measurement, a so-called high vacuum pump may be used. For example, a dry pump (oilless pump) and a TMP (molecular pump) may be used continuously. There is a limit to the time reduction.

The present invention has been made in view of the above-mentioned conventional problems, and at least one of a measurement error due to a variation in the distance between a sample and an X-ray source and a measurement error due to a change in the degree of vacuum during the measurement is simplified. It is an object of the present invention to provide a fluorescent X-ray analyzer that can be removed in a short time with a configuration.

[0005]

To achieve the above object, an X-ray fluorescence spectrometer according to claim 1 comprises a sample stage on which a sample is fixed and an X-ray for irradiating the sample with primary X-rays. Source
A height adjuster for adjusting the height of the sample stage with respect to the X-ray source;
Detecting means for measuring the intensity of secondary X-rays generated from the sample. The apparatus further includes an aperture block having a slit system for passing the primary X-rays and secondary X-rays incident on the detection means, an aperture for limiting an irradiation area of the sample to the primary X-rays, and the aperture. Selection means for selectively positioning the block such that the slit system or aperture is located in front of the X-ray source.

Further, in this apparatus, the slit system is positioned in front of the X-ray source by the selecting means, the sample is irradiated with primary X-rays from the X-ray source, and the detecting means detects secondary X-rays generated from the sample. While measuring the strength, with the height adjuster,
Height adjustment means is provided for changing the height of the sample table with respect to the X-ray source and adjusting the height of the secondary X-ray to a maximum measurement intensity.

According to the first aspect of the present invention, the distance between the sample and the X-ray source is adjusted to be constant by utilizing the slit system provided in the diaphragm block used for measurement and the detecting means used for measurement. A displacement sensor and a horizontal moving mechanism are not required, and the configuration of the apparatus can be simplified. Therefore, according to this device,
Measurement errors due to variations in the distance between the sample and the X-ray source can be eliminated in a short time with a simple configuration.

According to a second aspect of the present invention, there is provided an X-ray fluorescence spectrometer comprising: a sample stage on which a sample is fixed;
The apparatus includes a radiation source, a height adjuster for adjusting the height of the sample stage with respect to the X-ray source, and a detecting means for measuring the intensity of secondary X-rays generated from the sample. In addition, the apparatus includes a slit system for passing the primary X-rays and the secondary X-rays incident on the detecting means, and a secondary X-ray measured according to the degree of vacuum during the measurement.
An aperture block having a monitor sample in which the intensity of the line changes, and an aperture for limiting an irradiation area of the sample with primary X-rays;
Selective means for selectively positioning the aperture block such that the slit system, monitor sample or aperture is located in front of the X-ray source.

Further, in this apparatus, the slit system is positioned in front of the X-ray source by the selection means, the sample is irradiated with primary X-rays from the X-ray source, and the detection means detects secondary X-rays generated from the sample. While measuring the strength, with the height adjuster,
Height adjustment means is provided for changing the height of the sample table with respect to the X-ray source and adjusting the height of the secondary X-ray to a maximum measurement intensity. Furthermore, in this apparatus, the diaphragm is positioned in front of the X-ray source by the selection means, the sample is irradiated with primary X-rays from the X-ray source, and the intensity of the secondary X-rays generated from the sample is measured by the detection means. Measurement means for measuring the temperature. Furthermore, the apparatus arranges the monitor sample in front of the X-ray source by the selection device before and after the operation of the measurement device, irradiates the monitor sample with the primary X-ray from the X-ray source, and monitors the detection device. The measurement intensity of the sample is corrected by measuring the intensity of the secondary X-rays generated from the sample and estimating the degree of vacuum during the measurement of the measurement intensity of the sample by the measuring means based on the measurement intensity of the monitor sample. A correction means is provided.

According to the second aspect of the present invention, the distance between the sample and the X-ray source is adjusted to be constant by utilizing the slit system provided in the aperture block used for measurement and the detection means used for measurement. A displacement sensor and a horizontal moving mechanism are not required, and the configuration of the apparatus can be simplified. In addition, using the monitor sample provided in the aperture block used for measurement and the detecting means used for measurement, the degree of vacuum during the measurement of the measured intensity of the sample to be analyzed is estimated and corrected based on the measured intensity of the monitor sample. Therefore, a high-precision vacuum gauge and a control mechanism are not required, the configuration of the apparatus is simple, and the measurement can be started before a certain high vacuum is reached, so that the entire measurement work can be completed in a short time. Therefore, according to this apparatus, both a measurement error due to a variation in the distance between the sample and the X-ray source and a measurement error due to a change in the degree of vacuum during the measurement can be removed with a simple configuration in a short time.

[0011]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An apparatus according to a first embodiment of the present invention will be described below with reference to the drawings. First, the configuration of this device will be described. As shown in FIG. 1, this apparatus includes a sample stage 2 on which a sample 1 is fixed, an X-ray tube 4 which is an X-ray source for irradiating the sample 1 with primary X-rays 3, and an X-ray A height adjuster 5 for adjusting the height of the tube 4 is provided, and a detecting means 7 for measuring the intensity of secondary X-rays 6 such as fluorescent X-rays and scattered rays generated from the sample 1. Here, the detecting means 7 includes a divergent slit 8, a spectral element 9, a light receiving slit 10, and a detector 11. Further, the detecting means 7 is arranged around the X-ray tube 4 in accordance with the number of elements to be analyzed contained in the sample 1.
A plurality may be provided.

Further, the apparatus comprises a slit system 14 for passing the primary X-ray 3 and the secondary X-ray 6 incident on the detecting means 7, and a fluorescent X-ray measured according to the degree of vacuum during the measurement.
An aperture block 15 having a monitor sample 12 (FIG. 2) in which the intensity of the line 6 changes, an aperture 13 (FIG. 3) for limiting an irradiation area of the sample 1 with the primary X-ray 3, and the aperture block 15 , The slit system 14, the monitor sample 12
There is provided a selection means 17 for moving the diaphragm 13 (FIG. 3) in the direction perpendicular to the paper surface and selectively positioning the diaphragm 13 (FIG. 3) in front of the X-ray tube 4. 1 to 3, the stop block 15, the divergent slit 8, and the light receiving slit 10 are shown in cross sections.

Here, the slit system 14 includes a slit 14a formed on the aperture block 15 for passing the primary X-ray 3 and a slit 14b for passing the secondary X-ray 6 incident on the detecting means 7. Further, as shown in FIG. 2, for example, when an attached matter on a silicon wafer is to be analyzed, among the elements expected to be contained, the absorption of the generated fluorescent X-ray 6 is sensitive to the degree of vacuum. What is necessary is just to make the monitor sample 12 a material such as boron adhered to a silicon wafer. Above the monitor sample 12,
A monitor sample aperture 16 is formed. Note that FIG.
May be provided in the direction perpendicular to the plane of the paper according to the size of the irradiation area of the primary X-ray 3. Also, primary X
The line 3 and the secondary X-ray 6 are not limited to a so-called needle-shaped one, but may be a band-shaped one having a width in a direction perpendicular to the paper surface. In this case, the slit system 14, the monitor sample aperture 16, the aperture 13, Divergence slit 8 and light receiving slit 1
0 and the like also have a shape extending in a direction perpendicular to the paper of the drawing.

[0014] The aperture block may be a disc-shaped one having a slit system, a monitor sample, and an aperture around the disc, in which case the selection means may move the disc-shaped aperture block around the central axis. It may be rotated to selectively position the slit system, the monitor sample or the aperture in front of the X-ray tube. Note that an aperture block having a plurality of apertures and a selecting means for selectively positioning the aperture block so that one of the apertures is located in front of the X-ray tube are usually provided in a fluorescent X-ray apparatus, In the aperture block, the slit system 14
And a monitor sample 12 (FIG. 2).

The apparatus further comprises a control means 21 including the following height adjusting means 18, measuring means 19 and correcting means 20. As shown in FIG.
Reference numeral 8 designates a slit system 14 positioned in front of the X-ray tube 4 by the selection means 17, irradiates the sample 1 from the X-ray tube 4 with primary X-rays 3, and causes the detection means 7 to emit secondary X-rays generated from the sample 1.
The height of the sample table 2 with respect to the X-ray tube 4 is changed by the height adjuster 5 while measuring the intensity of the
Adjust the height to the maximum measurement intensity.

Further, as shown in FIG.
Reference numeral 9 designates a diaphragm 13 located in front of the X-ray tube 4 by the selection means 17, irradiates the sample 1 with the primary X-rays 3 from the X-ray tube 4, and causes the detection means 7 to emit fluorescent X-rays 6 Is measured. Further, as shown in FIG. 2, before and after the operation of the measuring means 19, the correcting means 20 positions the monitor sample 12 in front of the X-ray tube 4 by the selecting means 17. 12 is irradiated with the primary X-rays 3, the detecting means 7 measures the intensity of the fluorescent X-rays 6 generated from the monitor sample 12, and the measurement of the sample 1 by the measuring means 19 based on the measured intensities of the monitor samples 12. The measurement intensity of the sample 1 is corrected by estimating the degree of vacuum during the measurement of the intensity.

Next, the operation of this device will be described.
First, as shown in FIG. 1, for example, when a blank wafer on which nothing is attached is fixed to the sample table 2 as a reference sample 1 in advance, and it is input to the control unit 21 that distance characteristics should be obtained, The height adjusting means 18 positions the slit system 14 in front of (below) the X-ray tube 4 by the selecting means 17, irradiates the blank wafer 1 with the primary X-rays 3 from the X-ray tube 4, The height adjuster 5 measures the height of the sample table 2 with respect to the X-ray tube 4 while measuring the intensity of the characteristic X-rays of silicon (silicon) generated from the blank wafer 1 and the fluorescent X-rays 6 as Si-Kα rays. The characteristics of the measured intensity I of the fluorescent X-ray 6 with respect to the distance d _T between the sample 1 and the X-ray tube 4 (strictly, the target of the X-ray tube 4) as shown in FIG. Store in graph, table or formula form.

The height adjusting means 18 stores, as the reference height, the height of the sample table 2 at which the measured intensity I of the fluorescent X-ray 6 at this distance characteristic becomes the maximum _IMAX . Here, as described above, the slit system 14 includes the slit 14a that allows the primary X-ray 3 to pass therethrough and the fluorescent X-ray 6 that enters the detection unit 7 to pass therethrough. When the measured intensity I of the fluorescent X-rays 6 reaches the maximum _IMAX , the surface of the sample 1 moves relative to the X-ray tube 4 as shown in FIG. As shown, the generated fluorescent X-rays 6 are at a height at which the fluorescent X-rays 6 pass through the slit 14b at the maximum intensity and enter the detecting means 7. In other words, the distance between the surface of the sample 1 and the X-ray tube 4 (strictly, the target of the X-ray tube 4) is the optimum distance d _TG . Blank wafer,
That is, such a sample stage 2 in the sample 1 serving as a reference
The optimum height is set as the reference height.

Thereafter, when the sample 1 is fixed, the sample table 2 is assumed to be at this reference height first. The distance characteristic and the reference height are unique to the apparatus, and need only be obtained at regular intervals (for example, 24 hours) even when time-dependent changes are considered.
May be stored.

As shown in FIG. 2, when the control means 21 is previously instructed to determine the degree of vacuum characteristic, the evacuation of the measurement atmosphere of the apparatus is started, and the correction means 20 selects the selection means 17. The monitor sample is placed in front of the X-ray tube 4 by, for example, the silicon wafer 12 to which, for example, boron is attached, as described above.
2 is irradiated with primary X-rays 3 and the detecting means 7 measures the intensity of the characteristic X-rays of boron generated from the monitor sample 12 and the intensity of the fluorescent X-rays 6 as B-Kα rays, as shown in FIG. , The time characteristic of the measured intensity ^MI of the fluorescent X-ray 6 with respect to the time t is obtained and stored in the form of a graph, a table or an equation. The subscript ^M
Indicates a numerical value related to the monitor sample 12.

[0021] Here, the relationship with respect to the fluorescence measured intensity of X-ray 6 ^M I and the atmosphere of the density [rho _x (related to the degree of vacuum) is, as shown in the following equation (1), using a numerical value may be a known table This is also remembered. However, in actuality, the absorption from the X-ray tube 4 to the sample 1 is extremely small compared to the absorption from the sample 1 to the detector 11, so that the second term exp ｛ − (Μ / ρ) _S・ ρ _x・
^M d _S } may be set to 1. Note that these time characteristics and equation (1) are specific to the apparatus and need only be obtained at regular intervals (for example, 24 hours) even if changes over time are taken into account. It may be stored.

[0022]

(Equation 1)

For the sake of simplicity, the height adjusting means 1 described above is used.
8 and the operation of the correction means 20 have been described using the same detection means 7 shown in FIG. 1 or FIG. 2, respectively.
Actually, the two detecting means 7 are not the same because the wavelengths of the fluorescent X-rays 6 to be measured are different, and at least one of them is not on the paper. In the following, the same applies to the description of the operation of the measuring means 19.

As described above, the preparation in advance is completed. As shown in FIG. 1, a sample 1 to be analyzed, for example, a silicon wafer 1 having boron as an adhering substance is fixed to a sample table 2. At this time, as described above, the sample stage 2 is at the reference height, but due to variations in the thickness and warpage of the sample 1, as shown in FIG. The distance d _T1 may have a deviation d _C within the range of, for example, about ± 30 μm from the optimum distance d _TG . Therefore, the control means 2
When the sample 1 is input to the effect that the measurement is to be performed on the sample 1, first, the height adjusting means 18 of FIG. 4 irradiates the sample 1 with primary X-rays 3, and adjusts the height of the sample stage 2 with respect to the X-ray tube 4 by the height adjuster 5.
At least two height, for example, by 0.3mm changed vertically from the reference height, strength I _A of the fluorescent X-rays 6 generated from the sample 1 to the detecting means 7, thereby measuring the I _B.

The height adjusting means 18, the measurement result I _A of the two points, the I _B, by applying the distance characteristic of FIG stored,
The difference d _C is obtained as d _TG −d _T1 on FIG. 4, and the height of the sample stage 2 is raised from the reference height by d _C by the height adjuster 5. Is adjusted to the optimum height of the sample stage 2 at which the strength of the sample table 2 is maximized. Thereby, regarding the sample 1, the fluorescent X-rays 6 generated as shown in FIG.
At the maximum intensity, the light passes through the slit 14b and enters the detection means 7 at an optimum height. Instead of such an operation, a distance characteristic as shown in FIG. 4 is obtained for each sample 1 to be analyzed, and the height of the sample X The height of 2 may be adjusted.

According to this apparatus, the distance between the sample 1 and the X-ray tube 4 is set to a constant d _TG by using the slit system 14 provided in the diaphragm block 15 used for measurement and the detection means 7 used for measurement. Since the adjustment is performed, the displacement sensor and the horizontal moving mechanism are not required, and the configuration of the apparatus can be simplified. That is, according to this device can be removed measurement errors due to variations in the distance d _T between the sample 1 and the X-ray tube 4 with a simple structure. Further, as the fluorescent X-rays 6 to be measured in the height adjustment, among the ones generated from the sample 1 to be analyzed, those whose absorption is insensitive to the degree of vacuum, for example, Si-Kα rays in the case described above may be used. In this case, the height can be adjusted before the degree of vacuum in the apparatus reaches a high vacuum, and the entire measurement operation can be completed in a shorter time.

Next, as shown in FIG.
Before the operation of the measuring means 19 described later, the selecting means 17
To position the monitor sample 12 in front of the X-ray tube 4,
The X-ray tube 4 irradiates the monitor sample 12 with primary X-rays 3, and the detecting means 7 determines the intensity of the characteristic X-rays of boron generated from the monitor sample 12 and the intensity of the fluorescent X-rays 6 which are BKα rays. It is measured for 1 second, and stores the measured intensity ^M I _0.

Subsequently, as shown in FIG.
Is to position the aperture 13 in front of the X-ray tube 4 by the selecting means 17, irradiate the sample 1 to be analyzed from the X-ray tube 4 with primary X-rays 3, and to apply the B- the intensity of the fluorescent X-ray 6 is a Kα line, for example, by measuring one second n times ie n seconds, stores those measured intensities I ₁ ~I _n.

Following the operation of the measuring means 19,
Thus, as shown in FIG.
To position the monitor sample 12 in front of the X-ray tube 4,
The monitor sample 12 is irradiated with the primary X-ray 3 from the X-ray tube 4.
BK generated from the monitor sample 12 by the detecting means 7.
The intensity of α ray 6 is measured, for example, for one second, and the measured intensity is
^MI_{n + 1}Is stored.

Then, the correction means 20 operates as follows:
Measurement intensity of stored monitor sample 12^MI₀,^MI_{n + 1}
The measured intensity I of the stored sample 1 based on₁~ I_nMeasurement
Density of constant atmosphere ρ₁~ Ρ_n(Related to vacuum)
By estimating, the measured intensity I of sample 1₁~ I_nComplement
Correct. First, the measurement intensity of the monitor sample 12^MI₀, ^M
I_{n + 1}To the time characteristic of FIG. 5, and the corresponding time
0, n + 1. Also, from 0 to n + 1 on the horizontal axis
Is measured n times for sample 1 by dividing
The time corresponding to each of the times 1 to n is determined, and further,
The measured intensity of the monitor sample 12 that should correspond to each time (actual
Has not been measured)^MI₁~^MI_nAsk for. Soshi
And the density ρ of the atmosphere at time 0, n + 1₀, Ρ_{n + 1}
Is calculated by the following equations (2) and (3) obtained by modifying the equation (1).
Similarly, the density ρ of the atmosphere at times 1 to n₁~ Ρ
_nIs estimated and calculated by the following equation (4).

[0031]

(Equation 2)

[0032]

(Equation 3)

[0033]

(Equation 4)

Here, the measured intensity I _j (I _{1 to} I
_n ) is expressed by the following equation (5), similarly to the measured intensity ^MI of the monitor sample 12 in the equation (1).
Using the density ρ _{1 to} ρ _n of the atmosphere thus obtained, the following formula (6) is used to calculate the intensity (I _j ) of the sample 1 per one time (per second) to be measured at the highest ultimate vacuum degree in this apparatus. obtaining the average of the intensity ^C I) of.

[0035]

(Equation 5)

[0036]

(Equation 6)

When an element other than boron is measured by the corresponding detecting means 7, the corresponding known numerical values (μ · ρ) _S , (μ · ρ) _D , d _D, etc. are obtained. Similarly, using the densities ρ _{1 to} ρ _{n of the} atmosphere (applicable to elements other than boron) as well, for the characteristic X-ray of the element, from the measured intensity I _j of the sample 1, Determine the average intensity ^CI to be measured in degrees.

The height adjustment means 18 adjusts the height of the sample table 2 in the sample 1 to be analyzed by the correction means 20 to adjust the intensity ^M of the fluorescent X-ray 6 of the first monitor sample 12.
The measurement of I _0, by measuring means 19 may be performed between the measurement of the intensity I ₁ ~I _n of the fluorescent X-ray 6 of the analysis sample 1.

According to this device, the diaphragm blower used for measurement is
The monitor sample 12 provided in the
Using the output means 7 to measure the intensity of the monitor sample 12^MI
₀, ^MI_{n + 1}Intensity I of sample 1 to be analyzed based on
₁~ I_nSince the degree of vacuum during measurement is estimated and corrected,
No need for a precision vacuum gauge or control mechanism, simplifies equipment configuration
Measurement can be started before reaching a certain high vacuum.
Thus, the entire measurement operation can be completed in a short time. Therefore, the high
In addition to the effect of the
For example, a measurement error due to a variation in the distance between the sample 1 and the X-ray tube 4 may occur.
Both the difference and the measurement error due to the change in the degree of vacuum during the measurement,
It can be removed in a short time with a simple configuration.

Next, the apparatus according to the second embodiment of the present invention is shown in FIG.
It is explained according to. In the device of the second embodiment, the detecting means 27 used when the height adjusting means 18 is operated, that is, the structure of the detecting means 27 corresponding to the slit system 14 is the same as the detecting means 7 (FIG. Different from 1). Specifically, the detecting means 27 does not include a spectral element, and includes a divergence slit 8, a light receiving slit 10, and X
It comprises a line shutter 22 and a detector 11. The height adjusting means 18 is operated by the reciprocating means 23 during operation.
The X-ray shutter 22 is retracted from the front of the camera (the state shown in FIG. 6).
The X-ray shutter 22 is advanced forward of.

The reason why the spectroscopic element is not used for the detecting means 27 corresponding to the slit system 14 is that if the Si-Kα ray is adopted as the fluorescent X-ray 6 to be measured in the height adjustment as described above, the sample 1 to be analyzed becomes For example, in the case of a silicon wafer 1 on which aluminum having a thickness of several μm is formed, the Si—Kα ray 6 generated from silicon as a substrate is absorbed by a thick aluminum film and becomes weak, and this is diffracted by a spectral element. If it is made weaker, the detector 11
This is because it becomes difficult to measure the strength at a time. In addition, even if the detector 11 is not an SSD without using a spectroscopic element, if the Si-Kα ray 6 is not extremely weak, the intensity can be measured by spectral separation using a pulse height analyzer usually used for the detector 11. That is sufficient for strength measurement for height adjustment.

When the sample 1 to be analyzed does not contain silicon (silicon), the height can be adjusted by measuring the intensity of the scattered radiation 6 near the Si-Kα ray at the wavelength with the detector 11. However, even in such a case, the spectral element should not be used so that the scattered radiation 6 is not weakened.

An X-ray shutter 22 is provided immediately before the detector 11 of the detecting means 27 corresponding to the slit system 14 so that when the height adjusting means 18 is not operated, the advancing / retreating means 23 advances so as to cover the detector 11. In the detection means 27, the detector 11 is oriented in the direction of looking at the sample 1, and if there is no X-ray shutter 22, the measurement means 19
During the measurement of the sample 1 to be analyzed by the method (FIG. 3) or the like, the fluorescent X-rays 6 having a strong intensity generated from the sample 1 continue to be incident on the detector 11, and the life of the detector 11 is shortened unnecessarily. Because. The configurations, operations, and effects other than those described above are the same as those of the device of the first embodiment.

In the present invention, in the case of an apparatus only for removing a measurement error due to a variation in the distance between the sample and the X-ray source, the measuring means 19 is not provided, and the X-ray source is manually operated by the selecting means 17. An aperture 13 is positioned in front of the X-ray tube 4, the primary X-ray 3 is irradiated from the X-ray tube 4 to the sample 1 to be analyzed, and the detecting means 7 measures the intensity of the fluorescent X-ray 6 generated from the sample 1. You may. In the case of the same apparatus, the monitor sample 12 and the correction means 2 in the aperture block 15 are used.
It is not necessary to provide 0.

[0045]

As described above in detail, according to the present invention, at least one of the measurement error due to the variation in the distance between the sample and the X-ray source and the measurement error due to the change in the degree of vacuum during the measurement can be simplified. With a simple configuration, it can be removed in a short time.

[Brief description of the drawings]

FIG. 1 is a side view showing a state in which a height adjusting means is operating in a device according to a first embodiment of the present invention.

FIG. 2 is a side view showing a state in which a correction unit is operating in the apparatus.

FIG. 3 is a side view showing a state in which the measuring means is operating in the apparatus.

FIG. 4 is a diagram showing distance characteristics stored in advance in height adjustment means in the apparatus.

FIG. 5 is a diagram showing a time characteristic stored in advance in a correction unit in the apparatus.

FIG. 6 is a side view showing a state during operation of a height adjusting unit in the device according to the second embodiment of the present invention.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... sample, 2 ... sample stage, 3 ... primary X-ray, 4 ... X-ray source (X
5) height adjuster, 6 ... secondary X-ray, 7, 27 ... detection means, 12 ... monitor sample, 13 ... aperture, 14 ... slit system, 15 ... aperture block, 17 ... selection means,
18 height adjusting means, 19 measuring means, 20 correcting means.

──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int.Cl. ⁷ , DB name) G01N 23/00-23/227

Claims (2)

(57) [Claims] 1. A sample stage on which a sample is fixed; an X-ray source for irradiating the sample with primary X-rays; a height adjuster for adjusting the height of the sample stage relative to the X-ray source; Detecting means for measuring the intensity of secondary X-rays, a slit system for passing the primary X-rays and secondary X-rays incident on the detecting means, and a diaphragm for limiting the irradiation area of the sample with primary X-rays A diaphragm block having: a selector for selectively positioning the diaphragm block so that the slit system or the diaphragm is located in front of the X-ray source; and positioning the slit system in front of the X-ray source by the selector. While irradiating the sample with primary X-rays from the X-ray source and causing the detecting means to measure the intensity of secondary X-rays generated from the sample,
A fluorescent X-ray analysis apparatus comprising: a height adjuster that changes a height of a sample stage with respect to an X-ray source and adjusts the height of a secondary X-ray to a maximum measurement intensity. 2. A sample stage on which a sample is fixed; an X-ray source for irradiating the sample with primary X-rays; a height adjuster for adjusting the height of the sample stage relative to the X-ray source; Detecting means for measuring the intensity of the secondary X-ray; a slit system for passing the primary X-ray and the secondary X-ray incident on the detecting means; and a secondary X-ray which is measured according to the degree of vacuum during the measurement. An aperture block having a monitor sample whose intensity changes and an aperture for limiting the irradiation area of the sample with primary X-rays; and positioning the aperture block with the slit system, monitor sample or aperture in front of the X-ray source. Selecting means for selectively positioning the slit system in front of the X-ray source by the selecting means, irradiating the sample with primary X-rays from the X-ray source, and causing the detecting means to generate primary X-rays from the sample. While measuring the intensity of the next X-ray,
A height adjuster that changes the height of the sample table with respect to the X-ray source and adjusts the height of the secondary X-ray to a maximum measurement intensity; Measuring means for positioning the aperture, irradiating the sample with primary X-rays from the X-ray source, and causing detecting means to measure the intensity of secondary X-rays generated from the sample, and selecting means before and after the operation of the measuring means Position the monitor sample in front of the X-ray source by
Irradiates the next X-ray, and causes the detecting means to measure the intensity of the secondary X-ray generated from the monitor sample, and estimates the degree of vacuum during the measurement of the measured intensity of the sample by the measuring means based on the measured intensity of the monitor sample. X-ray fluorescence spectrometer provided with a correction means for correcting the measurement intensity of the sample by performing the measurement.