JP3234731B2 - Method for determining mask diameter in X-ray analysis - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for judging a hole diameter (mask diameter) of a mask used for X-ray analysis of a sample.

[0002]

2. Description of the Related Art In general, when performing X-ray analysis of a sample, a plurality of types of masks having different hole diameters are prepared, and one of these masks corresponding to the sample size is selected and coated on the sample. Primary X-rays are irradiated on the measurement surface exposed from the mask hole of the sample, and secondary X-rays generated from this measurement surface are detected. The above X-ray analysis is automatically performed by inputting various measurement conditions to an X-ray analyzer. At this time, as one of the measurement conditions, the hole diameter of the mask (mask size) selected according to the sample size is used. Diameter) is input to the X-ray analyzer.

[0003] When selecting a mask diameter according to the sample size, conventionally, a bar code corresponding to the mask diameter is provided on the sample holder, or the mask diameter is checked visually or measured manually. Then, the mask diameter is determined.

[0004]

However, as described above, when a bar code is provided on a sample holder and a mask is determined by the bar code, only one mask can be attached to one holder. Therefore, many holders corresponding to each mask are required. In addition, a special device such as a reading device for reading the barcode is separately required.

[0005] Further, when the mask diameter is visually checked or measured manually, an error is likely to occur. Therefore, an incorrect measurement condition may be input to the X-ray analyzer. In addition, it is conceivable that a barcode is directly attached to the surface of each of the masks to determine the mask diameter. In this case, however, a barcode reading device is additionally required, and the X-ray analysis requires a separate barcode reader. Cannot be adopted because barcodes may be destroyed.

SUMMARY OF THE INVENTION The present invention provides a method of determining a mask diameter which can accurately determine a mask diameter without requiring a special device and can eliminate measurement errors at the time of X-ray analysis. The purpose is.

[0007]

In order to achieve the above object, according to the first aspect of the present invention, at least the surface of the mask has a trace or zero content in a sample, and
The mask diameter is determined by forming a material composed of different kinds of specific elements according to the size of the mask diameter and measuring the intensity of secondary X-rays from the specific element.

According to a second aspect of the present invention, at least the surface of the mask is formed of a material made of a specific element whose content in a sample is minute or zero.
The mask diameter is determined by measuring the intensity of secondary X-rays from a specific element passing through the viewing-restriction slit while changing the hole diameter of the viewing-restriction slit while providing a viewing-restriction slit through which the line passes.

[0009]

According to the first aspect of the present invention,
By measuring the intensity of secondary X-rays generated from different specific elements provided on each mask having a different hole diameter, the mask diameter can be reliably determined without error, and the measurement conditions according to the mask diameter can be determined. Input to X-ray analyzer for accurate X
Line analysis can be performed.

According to the second aspect of the present invention, the change in the secondary X-ray intensity from a specific element passing through the field limiting slit is measured while changing the hole diameter of the field limiting slit, so that the mask diameter can be reduced. The discrimination can be performed without error and accurate analysis by the X-ray analyzer can be performed.
In this case, as in the first invention, different masks having different diameters are not provided with different specific elements.
By providing different kinds of specific elements on each mask and measuring the intensity of the secondary X-ray intensity, the diameter of each mask can be determined.

Further, in the first and second inventions described above, unlike the case of using a conventional bar code, the bar code is used for analyzing a sample without requiring a special device for reading the bar code. The mask diameter can be accurately determined using an X-ray analyzer. Also, this holder is shared by each mask without requiring many holders corresponding to each mask. That is, it can be shared by various samples.

[0012]

An embodiment of the first invention will be described below with reference to the drawings. FIG. 1 shows a schematic configuration diagram of a fluorescent X-ray analyzer. In the drawing, a sample 2 is held by a holder 1, a mask 3 having a hole diameter corresponding to the size of the sample 2 is selected and mounted on the sample 2, and the sample 2 is measured by a hole 31 provided in the mask 3. The surface is exposed.

An X-ray tube 4 is provided on the measurement surface of the sample 2.
Irradiates primary X-rays B1 from the sample, and the primary X-rays B1 excite the atoms of the sample 2 to produce fluorescent secondary X-rays B unique to the element.
2 is generated. This secondary X-ray B2 is incident on the spectral crystal 5 and has a predetermined wavelength that satisfies the Bragg equation.
Only 2 is diffracted by the spectral crystal 5 and detected by the fluorescent X-ray detector 6.

According to the first aspect of the present invention, when determining the mask 3 according to the size of the sample 2, the specific element which is generally not contained in the analysis sample at all or has a very small content, For example, elements such as lanthanum, cerium, platinum, and gold are used, and each of the masks 3 having a different pore size is formed by each of these different specific elements.
To form As an example, a mask with a hole diameter of 5 mm (5φ) is lantern, 10φ is cerium, 20φ is platinum, 30
φ is formed of gold.

Further, the surface of each of the masks 3 may be separately coated with a film made of each of the above specific elements.

Then, each of the masks 3 is determined by measuring a unique secondary X-ray intensity generated from each of the specific elements.

That is, on the output side of the X-ray detector 6, a detection circuit 7 for detecting the intensity of secondary X-rays generated from each of the specific elements by peak value analysis, and the secondary circuit detected by the detection circuit 7 A mask diameter judging means 8 for judging each of the masks 3 based on the X-ray intensity is connected. Further, a memory 9 is connected to the input side of the determination means 8, and the memory 9 stores the hole diameter of each mask 3 and each specific element provided in each mask 3.

The primary X-ray B1 from the X-ray tube 4
Is irradiated on the specific element of the mask 3, and a specific secondary X-ray B 2 generated from the specific element is diffracted by the spectral crystal 5 and detected by the detector 6. The detection result is sent from the detection circuit 7 to the mask diameter determination means 8,
The detection result from the detection circuit 7 is compared with the contents stored in the memory 9 by the determination means 8.

In this way, the hole diameter of the mask 3 is judged by the judging means 8, and a setting signal a corresponding to the hole diameter is inputted from the judging means 8 to the X-ray analyzer as one of the measurement conditions. X-ray analysis of the sample 2 is automatically performed. At this time, the power of the X-ray tube 4 and the types of the dispersive crystal 5 and the detector 6 are changed based on various measurement conditions including the setting signal a, thereby obtaining the sample 2.
Is automatically analyzed.

Next, the second invention will be described with reference to FIG. In the second invention, the mask 3 is formed using at least one of the above-described specific elements, or the surface of the mask 3 is coated as a film with the specific element. Then, a disk-shaped slit member 10 is provided on the path of the secondary X-ray B2 generated from the specific element of the mask 3 and reaching the spectral crystal 5.

The slit member 10 has a rotating shaft 11 at its center.
The slit member 10 rotates around the rotation shaft 11 by driving a pinion 12 meshing with a gear provided around the outer periphery thereof by a motor 13. Then, as shown in FIG. 3, the outer peripheral portion of the slit member 10 has different hole diameters corresponding to the respective mask diameters, for example, 6 mm.
A plurality of circular field limiting slits 14 are formed. The hole diameter of the slit 14 is, for example, 5, 10, 20, 25, 30, 35φ corresponding to each mask diameter.

As in the case of the first invention, the detection circuit 7 and the mask diameter judging means 8 are connected to the output side of the detector 6, and the input side of the mask diameter judging means 8 is The memory 9 storing the hole diameter and number of each slit 14 is connected.

A mark indicating the hole diameter number of the slit 14, for example, a disk 15 in which a number of through holes or projections corresponding to the number are arranged on the circumference of the rotation shaft of the motor 13, is attached. Opposite to 15 is a sensor 16 for optically or magnetically detecting the mark. Further, a driving circuit 17 for driving the motor 13 to rotate the slit member 10 by a predetermined angle is connected to the motor 13.

When the mask diameter is determined according to the second aspect of the present invention, the slit member 10 is rotated by the driving of the motor 13 so that one of the slits 14 of the secondary X-ray B2 generated from the specific element of the mask 3 is used. When the secondary X-ray B2 is located on the path and passes through the slit 14, the intensity is detected by the detector 6, and the detection result is sent from the detection circuit 7 to the judgment means 8. When the slit 14 is located on the path of the secondary X-ray B2, a signal from the disk 15 is sent to the sensor 16, and the number of the slit 14 is input from the sensor 16 to the determination means 8. You.

The determination means 8 compares the secondary X-ray intensity detected by the detection circuit 7 with the number of the sensor 16 and the contents stored in the memory 9.

When the intensity of the secondary X-rays detected by the detection circuit 7 is equal to or higher than a predetermined intensity, a large amount of the secondary X-ray passes through the slit 14, so that the diameter of the slit 14 is larger than the mask diameter. It is determined by the determination means 8 that the value is larger, and a signal is output from the determination means 8 to the drive circuit 17,
The slit member 10 is rotated by the motor 13, and the next slit 14 is rotated and positioned on the path of the secondary X-ray.

In determining the actual mask diameter, the rotation of the motor 13 causes the slit 14 to be sequentially rotated and positioned on the path of the secondary X-ray from the one having the larger hole diameter, and the intensity of the secondary X-ray passing through the slit 14 is increased. Is measured, and this secondary X
When the line intensity falls below the predetermined intensity, the slit 14
It is determined by the determination means 8 that the hole diameter matches the mask diameter. In this way, the hole diameter of the mask 3 is determined, and a setting signal corresponding to the mask diameter is input from the determination means 8 to the X-ray analyzer as one of the measurement conditions, and the X-ray analysis of the sample 2 by the X-ray analyzer is automatically performed. It is done on a regular basis. For example, when the hole diameter of the mask 3 is 20φ, and when the hole diameter of the slit 14 is 35, 30, 25φ, a large secondary X-ray intensity generated from a specific element in the periphery of the hole 31 of the mask 3 is detected. On the other hand, when the diameter is 20φ, the secondary X-ray intensity is hardly detected, and it can be determined from this that the mask diameter is 20φ.

Next, the actual test results are shown in FIG. In FIG. 4, the vertical axis represents the secondary X-ray intensity from the specific element provided on the mask 3, the horizontal axis represents the mask diameter, and when the mask diameter is 5, 10, 20, 25, 30, and 35φ, FIG. 5 shows a measurement graph when this is determined by a secondary X-ray passing through the slit 14.

As is clear from FIG.
When the hole diameter of No. 4 matches the mask diameter, the X-ray intensity is almost zero. For example, if the mask diameter is 25φ, X
The linear strength (pcs) is 95 when the hole diameter of the slit 14 is 35φ and is 20 when the hole diameter is 30φ, but is zero when the hole diameter is 25φ and is also zero when the hole diameter is 20φ, 15φ, 10φ and 5φ.

A plurality of slits 1 having a fixed hole diameter are provided.
Instead of 0, for example, a single slit with automatic iris can also be used. In this case, the hole diameter is detected by interlocking the slit hole diameter detecting means with the aperture mechanism.

[Brief description of the drawings]

FIG. 1 is a schematic configuration diagram showing an X-ray analyzer using a method of determining a mask diameter according to a first invention.

FIG. 2 is a schematic configuration diagram showing an X-ray analyzer using a determination method according to a second invention.

FIG. 3 is an enlarged front view of a field limiting slit of the device.

FIG. 4 is a characteristic diagram showing a relationship between a mask diameter and X-ray intensity when the hole diameter of the visual field limiting slit is changed.

[Explanation of symbols]

2 sample, 3 mask, 31 mask hole, 14 field-of-view limiting slit.

Continuation of front page (58) Field surveyed (Int.Cl. ⁷ , DB name) G01N 23/00-23/227 G01B 15/00-15/08

Claims (2)

(57) [Claims] 1. A sample is covered with a mask, a measurement surface of the sample is exposed by a mask hole, primary X-rays are irradiated on the measurement surface, secondary X-rays generated from the sample are detected, and the sample is analyzed. A method of determining a mask diameter at the time of X-ray analysis, wherein at least the surface of the mask has a trace or zero content in a sample, and different types of specific elements depending on the size of the mask diameter. A method for determining a mask diameter in an X-ray analysis in which the mask diameter is determined by measuring the intensity of a secondary X-ray from the specific element and formed from a material consisting of the following. 2. A sample is covered with a mask, a measurement surface of the sample is exposed through a mask hole, and the measurement surface is irradiated with primary X-rays, secondary X-rays generated from the sample are detected, and the sample is analyzed. A method of determining a mask diameter during X-ray analysis, wherein at least the surface of the mask is formed of a material made of a specific element whose content in a sample is minute or zero, and passes through the secondary X-ray. A mask in X-ray analysis for determining the mask diameter by measuring the intensity of secondary X-rays from a specific element passing through the view restriction slit while changing the hole diameter of the view restriction slit. Diameter determination method.