JP2006118941A - Electronic probe x-ray analyzer for displaying surface analyzing data - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To obtain an element distribution image reduced in the effect due to a change in the surface shape or state of a sample in an electronic probe X-ray analyzer for performing X-ray analysis by irradiating the sample with an electron beam. <P>SOLUTION: The sample or the electron beam is scanned to two-dimensionally collect characteristic X-ray intensity data of a plurality of elements and, with respect to all of the coordinated positions of two-dimensional data, the characteristic X-ray intensity data of the respective elements are-converted to relative densities. Quantitative correction calculation is applied to these relative densities to obtain the mass concentrations of the respective elements. The sum total value of the relative intensities or mass concentrations of all of the elements at every coordinates position is used to standardize the relative intensities or mass concentrations of the respective elements and the values thereof are classified by a level to be displayed as the element distribution image. If necessary, the mass concentrations are used to calculate the concentrations of atoms, the concentrations of compounds, the number of atoms on the like at every coordinates position and these values are standardized to be displayed. Accordingly, the element distribution image reduced in the effect due to a change in the surface shape or state of the sample can be obtained. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

The present invention includes an electron probe microanalyzer (EPMA) for performing elemental analysis using characteristic X-rays detected by irradiating a sample with an electron beam, a scanning electron microscope equipped with a wavelength dispersive X-ray spectrometer (WDS), etc. In particular, the present invention relates to display of surface analysis data.

In surface analyzers using electron beams such as EPMA, the surface of the sample is irradiated with a finely focused electron beam, and characteristic X-rays generated from the sample are dispersed / detected to perform qualitative analysis, quantitative analysis, surface analysis, state analysis, etc. It can be performed.
In these analyzers, an electron beam generated from an electron gun is finely focused by a focusing lens and an objective lens and irradiated to an analysis sample. The electron beam is deflected by an electron beam deflector and can be scanned two-dimensionally on the analysis sample. It is also possible to scan the sample two-dimensionally with a sample mounting table having a mechanism that moves in X, Y, and Z directions. The X-ray signal dispersed / detected by the X-ray spectrometer is sent to the control arithmetic processing device, and analysis data is created.

When performing surface analysis in EPMA, the position of the sample is fixed and the electron beam is scanned when analyzing a relatively narrow region, while the sample stage is not deflected when analyzing a relatively large region. It is made to scan. FIG. 4 shows a concept of dividing an analysis region into a lattice by scanning an electron beam or a sample two-dimensionally. In FIG. 4, when the electron beam 41 or the sample 42 is scanned two-dimensionally, the analysis region 46 is divided into small grids. The size of one grid is determined according to the size of the analysis region and the number of divisions. The electron beam diameter may be increased according to the size of one lattice. Each grid position (x, y) 47 divided into small parts corresponds to a relative coordinate position in the analysis region. X-rays emitted from the sample 42 are dispersed by the spectroscopic element 43 and detected by the X-ray detector 44. Secondary electrons, reflected electrons, etc. are detected by the electron detector 45. The detected X-rays, secondary electrons, reflected electrons, and the like are displayed as a signal intensity distribution image by classifying the signal intensity for each of the lattice positions that are divided into small parts, corresponding to each level with an appropriate color. X-ray signal intensity may be displayed as it is divided into levels as it is, but converted to mass concentration based on a calibration curve representing the relationship between mass concentration and X-ray intensity determined in advance for each element. In some cases, values are displayed in levels. The X-ray intensity signal collected at this time is normally used as data for displaying a distribution image without being subjected to dead time correction (Dead Time) of the detector.

In addition, when performing quantitative analysis using WDS in EPMA, first, the spectroscopic element is adjusted to the peak wavelength at which the maximum intensity of the characteristic X-ray of the analysis target element A can be detected, and the X-ray intensity Ips is measured on the standard sample. Next, the background intensity Ibs is measured by shifting the diffraction wavelength of the spectroscopic element. The characteristic X-ray intensity Ns of the standard sample is obtained from Ns = Ips−Ibs. Similarly, the X-ray intensities Ipu and Ibu at the peak wavelength position and the background position are measured on the unknown sample, and the characteristic X-ray intensity Nu = Ipu−Ibu is obtained.
If K _A = Nu / Ns, K _A is called the relative intensity of element A. Since K _A is approximately proportional to the mass concentration C _A of the element A, the element A can be quantified. To determine an accurate C _A physically it is necessary to correct the difference of the X-ray generation due to difference in composition between the standard sample and unknown sample (called matrix effects). This correction means is called quantitative correction calculation, and normal EPMA has this function.

Here, the above-mentioned Ips, Ibs, Ipu, and Ibu are all values subjected to correction of the dead time of the detector. As a method for obtaining the background intensity, JP-A 63-313043 discloses a method of estimating based on an average atomic number of an analytical sample in addition to a method of shifting a diffraction wavelength of a spectroscopic element.
When quantitative analysis is performed, it is a principle that the X-ray intensity is measured under exactly the same analysis conditions for the standard sample and the unknown sample. However, the irradiation current value and the counting time may be realized by converting the X-ray intensity obtained under different conditions so as to be equivalent to the data collected under the same conditions.
No. 03-22583 JP 61-62850 A JP 61-70444 A JP-A-63-313043

In the area analysis data, even when the X-ray intensity is divided into levels as it is and displayed as an image, or when the X-ray intensity is converted into a mass concentration by a calibration curve and displayed, the place where the X-ray intensity is high is simply the element whose mass concentration is high. It is interpreted on the assumption that it is a place. However, in practice, the X-ray intensity collected at each coordinate position in the analysis region may change due to various factors other than the change in mass concentration.

Factors that change the X-ray intensity other than the mass concentration of an element include, for example, the following (1) to (4).
(1) When the combination of coexisting elements varies depending on each coordinate position in the analysis region, the state of the penetration / diffusion of electron beams and the state of X-ray generation differ, so the characteristic X-ray intensity measured due to the difference in so-called matrix effect changes. To do. In addition, the background intensity derived from continuous X-rays may change.
(2) The sample surface is not always smooth, and the X-ray incident intensity to the X-ray spectrometer may change due to unevenness or inclination.
(3) When the sample surface is contaminated or an insulator is analyzed, the vapor deposition film for imparting conductivity may cover the sample surface, and X-rays may be absorbed.
(4) During measurement of surface analysis data, disturbances such as vibration and temperature change may be applied, and measurement conditions such as irradiation current may vary.

When the X-ray intensity fluctuates due to these factors, reliable data cannot be obtained even if the mass concentration converted by the X-ray intensity or the calibration curve is simply displayed as an element distribution image.

In order to solve the above problems, the present invention includes means for spectroscopic / detecting characteristic X-rays generated from the surface of a sample irradiated with an electron beam, and characteristics X collected two-dimensionally by scanning the sample or the electron beam. In an electron probe X-ray analyzer comprising a display means for displaying a two-dimensional distribution image based on line intensity data, and a quantitative correction calculation means,
Calculation means for obtaining relative intensity of each element from characteristic X-ray intensity data and standard sample data of a plurality of elements collected at the same coordinates with respect to characteristic X-ray intensity data collected two-dimensionally; A calculation means for performing a quantitative correction calculation on the relative intensity to determine a mass concentration of each element; a calculation means for determining an amount related to a composition ratio based on the mass concentration of each element; and a relative intensity of each element or A calculation means for normalizing the mass concentration of each element or the amount related to the composition ratio,
Predetermined calculation is performed for all coordinate positions of characteristic X-ray intensity data collected two-dimensionally, and the amount related to the normalized relative intensity of each element, the mass concentration of each element, or the composition ratio It is an object of the present invention to provide an electron probe X-ray analyzer characterized in that at least one of them is displayed as a two-dimensional distribution image by the display means.
The present invention also provides means for spectroscopic / detecting characteristic X-rays generated from the surface of a sample irradiated with an electron beam, and characteristic X-ray intensity data collected two-dimensionally by scanning the sample or the electron beam. In an electron probe X-ray analyzer comprising display means for displaying as an image and quantitative correction calculation means,
Calculation means for obtaining relative intensity of each element from characteristic X-ray intensity data and standard sample data of a plurality of elements collected at the same coordinates with respect to characteristic X-ray intensity data collected two-dimensionally; Computation means for performing a quantitative correction calculation on the relative intensity to obtain the mass concentration of each element and computation means for normalizing the relative intensity of each element or the mass concentration of each element,
A predetermined calculation is performed on all coordinate positions of the characteristic X-ray intensity data collected two-dimensionally, and at least one of the normalized relative intensity of each element or the mass concentration of each element is calculated as two. An object of the present invention is to provide an electron probe X-ray analysis apparatus including display means for displaying as a dimension distribution image.

As described above, the present invention calculates the relative intensity of each element from the characteristic X-ray intensity data and standard sample data of a plurality of elements collected at the same coordinates with respect to the characteristic X-ray intensity data collected two-dimensionally. Computing means for obtaining, computing means for performing a quantitative correction calculation on the relative intensity of each element to obtain the mass concentration of each element, and computing means for obtaining an amount related to the composition ratio based on the mass concentration of each element And calculation means for normalizing the relative intensity of each element or the mass concentration of each element or the amount related to the composition ratio, and all coordinates of characteristic X-ray intensity data collected two-dimensionally A predetermined calculation is performed on the position, and at least one of the normalized relative strength of each element, the mass concentration of each element, or the amount related to the composition ratio is divided into two dimensions. Since the display means is provided with the display means as an image, the X-ray intensity changes due to factors such as the difference in the matrix effect at the analysis location, the shape of the sample surface, the contamination of the sample surface, the state of the deposited film, and the measurement conditions. Therefore, it is possible to obtain an element distribution image with reduced influence, and to improve the reliability of analysis.

Here, the concept of the present invention will be described in more detail with reference to FIG. “(A) Map data of peak intensity” is the XDS collected in the same analysis region with the WDS spectroscopic element set at the detection wavelength position where the characteristic X-ray intensity of the elements 1 to N constituting the sample is maximum. Line strength data. “(B) Map data of background intensity” is data of background intensity obtained by shifting the diffraction wavelength position of the WDS spectroscopic element from the peak position. Here, all the X-ray intensity data are data subjected to dead time correction of the detector. However, the dead time correction may be performed during the collection of the map data of each element, or may be performed after the collection of all the map data.
Further, “(b) map data of background intensity” is not necessarily an actual measurement value, for example, a value estimated from an average atomic number of an analysis place using a method disclosed in JP-A-63-313043. It may be used.

In principle, it is assumed that the map data of the peak intensity and background intensity of the elements 1 to N includes all map data of main elements included in the sample. However, the elements corresponding to the items (1) to (4) below may be excluded from the measurement, but the elements corresponding to the items (2) to (3) are corrected sequentially and approximately in the course of the quantitative correction calculation. When obtaining the coefficient, the calculation is performed in consideration of the concentration.
(1) In the case of the above-mentioned quantitative correction calculation process, the element is a trace element that does not greatly affect the calculation of the correction coefficient, and the element itself is not an analysis target.
(2) An element having a measured map data and an element that can assume a certain composition ratio, and a “binding element” described later is one example.
(3) For example, in a case of iron in steel where the correction factor can be calculated based on the assumption that the main element is iron and all other than the analysis target element is occupied by iron, such as steel.
(4) In the case of an element such as lithium, which cannot be analyzed by EPMA, but whose mass concentration is known in advance by an analysis method other than EPMA.

Below, based on the map data measured about the elements 1-N, the calculation method of the quantity concerning the relative intensity | strength of each element, mass concentration, and the normalized composition ratio is explained in full detail.
In the following description, a variable with (x, y) means a variable that changes for each coordinate position on the map. Accordingly, the calculation operation at the coordinates (x, y) is performed at all the coordinates in the analysis region, but only the calculation operation at the coordinates (x, y) is described here. The coordinates (x, y) correspond to the pixels when displaying the two-dimensional distribution image.
The X-ray intensities of the elements 1 to N at the coordinates (x, y) on “(a) peak intensity map data” are P1 (x, y), P2 (x, y),..., PN (x, y), and the X-ray intensity at coordinates (x, y) on "(b) Map data of background intensity" is B1 (x, y), B2 (x, y), ..., BN (x, y) And The characteristic X-ray intensities of the standard samples of the respective elements obtained under the same conditions as for collecting the maps are I1 (std), I2 (std),..., IN (std).
K1 (x, y) = (P1 (x, y) -B1 (x, y)) / I1 (std)
K2 (x, y) = (P2 (x, y) -B2 (x, y)) / I2 (std)
...
KN (x, y) = (PN (x, y) -BN (x, y)) / IN (std)
Then, K1 (x, y), K2 (x, y), ..., KN (x, y) are elements 1 to 1 at coordinates (x, y) on "(c) map data of relative intensity". The relative intensity of N.

If the relative intensities of the elements 1 to N constituting the sample are obtained, the mass concentrations C1 (x, y), C2 (x, y), ..., CN (x, y) of the elements 1 to N at the coordinates (x, y) are obtained. The operation for obtaining y) can be performed using a normal quantitative correction calculation means. Examples of the quantitative correction calculation method include a so-called ZAF method, a filetette method, and a simple correction method based on these methods, but are not particularly limited in the present invention.
That is, if the correction coefficients of the elements 1 to N obtained by the quantitative correction calculation at the coordinates (x, y) are G1 (x, y), G2 (x, y), ..., GN (x, y),
C1 (x, y) = G1 (x, y) x K1 (x, y)
C2 (x, y) = G2 (x, y) x K2 (x, y)
...
CN (x, y) = GN (x, y) x KN (x, y)
As a result, “(d) mass concentration map data” is obtained.
This map data is data obtained by correcting the matrix effect at the same coordinate position, unlike the mass concentration map obtained using the conventional calibration curve. However, when there is an element that has not been measured but should be considered when obtaining the correction coefficient, the calculation is performed in consideration of the mass concentration of the element.

Next, normalization of mass concentration will be described.
When the analysis sample consists only of elements 1 to N,
SC (x, y) = Σ (C1 (x, y) + C2 (x, y) + ... + CN (x, y))
, Normalized mass concentration of elements 1-N at coordinates (x, y)
C1 ^* (x, y), C2 ^* (x, y), ..., CN ^* (x, y) is
C1 ^* (x, y) = C1 (x, y) / SC (x, y)
C2 ^* (x, y) = C2 (x, y) / SC (x, y)
...
CN ^* (x, y) = CN (x, y) / SC (x, y)
Thus, “(e) normalized mass concentration map data” is obtained.
Here, when there is an element that has not been measured but is considered when calculating the correction coefficient, it is obvious that normalization may be performed by adding the concentration to SC (x, y).

The normalization performed on the mass concentration can be similarly performed on the relative intensity before the correction calculation. That is,
SK (x, y) = Σ (K1 (x, y) + K2 (x, y) + ... + KN (x, y))
If so, normalized relative intensities of elements 1 to N at coordinates (x, y)
K1 ^* (x, y), K2 ^* (x, y), ..., KN ^* (x, y) is
K1 ^* (x, y) = K1 (x, y) / SK (x, y)
K2 ^* (x, y) = K2 (x, y) / SK (x, y)
...
KN ^* (x, y) = KN (x, y) / SK (x, y)
Thus, normalized relative intensity map data (not shown) of the elements 1 to N is obtained.
As a case where the relative intensity is normalized and displayed, the analysis sample may be composed of only elements 1 to N, and the correction coefficient of each constituent element may be small or similar. Data with normalized relative intensity is less accurate than data with normalized mass concentration, but the time required for correction calculation can be reduced.

Next, a case where the normalized atomic concentration is obtained based on the mass concentration will be described. The atomic weights of the elements 1 to N are A1, A2,..., AN, and the atomic concentrations of the elements 1 to N in the coordinates (x, y) are Ca1 (x, y), Ca2 (x, y),. y).
SCa (x, y) = C1 (x, y) / A1 + C2 (x, y) / A2 + ... + CN (x, y) / AN
After all,
Ca1 (x, y) = (C1 (x, y) / A1) / SCa (x, y)
Ca2 (x, y) = (C2 (x, y) / A2) / SCa (x, y)
...
CaN (x, y) = (CN (x, y) / AN) / SCa (x, y)
Thus, map data (not shown) of atomic concentrations normalized to 1 is obtained.

Next, a method for determining the mass concentration of a compound from the mass concentration of each element when the compounds 1 to N are combined with a certain binding element at a certain ratio to form a compound will be described. Let AD be the atomic weight of the binding element that binds to the elements 1 to N at a constant ratio, and R1, R2,. There is usually no need to measure the map data of the binding elements.
M1 (x, y), M2 (x, y), ..., MN (x, y) at mass coordinates (x, y) of a compound made from the elements 1 to N and the binding element,
M1 (x, y) = C1 (x, y) x (A1 + R1 x AD) / A1
M2 (x, y) = C2 (x, y) × (A2 + R2 × AD) / A2
...
MN (x, y) = CN (x, y) x (AN + RN x AD) / AN
It is. Here, the mass concentrations C1 (x, y), C2 (x, y),..., CN (x, y) of the elements 1 to N are obtained from the quantitative correction calculation considering the concentration of the binding element. is there.
SM (x, y) = M1 (x, y) + M2 (x, y) + ... + MN (x, y)
Then, the mass concentration M1 ^* (x, y), M2 ^* (x, y), ..., MN ^* (x, y) of the standardized compounds of elements 1 to N at coordinates (x, y) is ,
M1 ^* (x, y) = M1 (x, y) / SM (x, y)
M2 ^* (x, y) = M2 (x, y) / SM (x, y)
...
MN ^* (x, y) = MN (x, y) / SM (x, y)
Thus, map data (not shown) of the mass concentration of the normalized compounds of elements 1 to N is obtained.

Next, a method for obtaining the normalized number of atoms of each element when a binding element is present will be described.
Since the bond element atomic weight is AD, and the bond ratio between the bond element and elements 1 to N is R1, R2,..., RN, and the mass concentration of the bond element is CD (x, y),
CD (x, y) = (C1 (x, y) x R1 / A1 + C2 (x, y) x R2 / A2 + ... + CN (x, y) x RN / AN) x AD
As required.
SX (x, y) = C1 (x, y) / A1 + C2 (x, y) / A2 + ... + CN (x, y) / AN + CD (x, y) / AD, elements 1 to N And the atomic concentration of the binding element
X1 (x, y), X2 (x, y), ..., XN (x, y), XD (x, y)
X1 (x, y) = (C1 (x, y) / A1) / SX (x, y)
X2 (x, y) = (C2 (x, y) / A2) / SX (x, y)
...
XN (x, y) = (CN (x, y) / AN) / SX (x, y)
XD (x, y) = (CD (x, y) / AD) / SX (x, y)
It becomes. The normalized number of atoms of each element can be obtained based on this atomic concentration.

When obtaining the normalized number of atoms of each element, the number of atoms of all elements including the binding element may be specified, or only the number of atoms of the binding element may be specified. Alternatively, the number of atoms of a specific element of interest may be specified, or the total number of atoms of a specific plurality of elements of interest may be specified.
Here, for example, a case where the number of atoms of the binding element is designated as T and normalized by T will be described.
The numbers of elements 1 to N and the number of atoms of the bonding element when normalized by the number of atoms T of the bonding element are X1 ^* (x, y), X2 ^* (x, y), ..., XN ^* (x, y), XD ^* (x, y)
X1 ^* (x, y) = X1 (x, y) x (T / XD (x, y))
X2 ^* (x, y) = X2 (x, y) x (T / XD (x, y))
...
XN ^* (x, y) = XN (x, y) x (T / XD (x, y))
XD ^* (x, y) = XD (x, y) × (T / XD (x, y)) = T
Thus, map data (not shown) representing the number of atoms of each element normalized by T is obtained. The method of displaying the standardized number of atoms is, for example, a semiconductor compound such as (Ga _x , Al _1-x ) As, a mineral such as (Na, K) ₁ Al ₁ Si ₃ O ₈ , etc. This is extremely useful when displaying analysis results of known samples.

Next, a method for obtaining the average atomic number using the normalized mass concentration will be described.
If the atomic numbers of elements 1 to N are Z1, Z2,..., ZN, and the average atomic number in the coordinates (x, y) of the analysis region is Zp (x, y), Zp (x, y) is elements 1 to N. Is obtained by summing the amounts obtained by apportioning the atomic number of each element at the normalized mass concentration. That is,
Zp (x, y) = C1 ^* (x, y) x Z1 + C2 ^* (x, y) x Z2 + ... + CN ^* (x, y) x Z2
As a result, map data (not shown) of the average atomic number is obtained.
The average atomic number is an important parameter for quantitative correction calculation, and has a certain relationship with the contrast of the reflected electron image, and thus provides useful information that complements the interpretation of the quantitative analysis result.

Next, the form for implementing this invention is demonstrated based on FIGS. 1-3. FIG. 1 shows a schematic configuration of an electronic probe microanalyzer according to the present invention. In FIG. 1, the electron beam emitted from the electron gun 1 is narrowed down by the focusing lens 2 and the objective lens 3 and irradiated to the analysis sample 6. The electron gun 1, the focusing lens 2, the objective lens 3, and the electron beam deflector 4 are connected to the interface 14 via the electron optical system controller 8. The spectroscopic element 9 is connected to the interface 14 via the spectroscopic element control device 11, and the sample mounting table 7 is connected to the interface 14 via the sample mounting table control device 13. In addition to controlling each part of the apparatus through the interface 14, the control arithmetic processing unit 15 takes in the X-ray signal detected by the X-ray detector 10 through the X-ray signal processing unit 13 and performs data processing. The database 16 stores physical constants used for quantitative analysis, apparatus parameters, data on standard samples and backgrounds, and the like. The display device 17 is a monitor such as a cathode ray tube or a liquid crystal display, and the input device is a mouse or a keyboard. The optical microscope 5 is used to set the analysis point at a predetermined position.

FIG. 3 is a flowchart showing an implementation procedure.
Procedure 1: An analysis condition such as an analysis element, a characteristic X-ray type, and an acceleration voltage is input by the input device 18. Specify the acquisition method, such as whether to measure the background intensity on the analysis sample or use the estimated value based on the average atomic number.
Procedure 2: Specify whether to scan an electron beam or a sample as a method of collecting data two-dimensionally. Based on this, an analysis region on the analysis sample 6 is designated using an electron beam scanning image such as secondary electrons and reflected electrons, and the optical microscope 5. At this time, the number of analysis areas to be divided into grids and the X-ray measurement time per grid are also specified.
Procedure 3: An apparatus state such as an electron beam and an analysis position is set according to the designated analysis condition. The WDS spectroscopic element 9 is set at the peak position of the characteristic X-ray of the analytical element by the spectroscopic element control device 11, and map data of the peak intensity is acquired. Measure for all elements to be measured. The dead time correction may be performed at any time before the calculation of the relative intensity, but may be performed immediately after acquisition of the map data.

Procedure 4: In accordance with the background intensity acquisition method specified in Procedure 1, proceed to Procedure 5 when measuring, or proceed to Procedure 6 when using an estimated value based on the average atomic number.
Procedure 5: The WDS spectroscopic element 9 is set to the background measurement position, and background intensity map data is acquired. Measure for all elements to be measured. The dead time correction may be performed at any time before the calculation of the relative intensity, but may be performed immediately after acquisition of the map data.
Procedure 6: “Data representing the relationship between the average atomic number and the background intensity” prepared in advance is read from the database 16.

Step 7: If it is necessary to measure the peak intensity and background intensity of the standard sample, proceed to step 8. If there is already acquired standard sample data and use it, proceed to step 9.
Procedure 8: The peak intensity and background intensity of the standard sample are measured for all the elements to be measured. The dead time correction of peak intensity and background intensity is performed immediately after measurement. The standard sample measurement in steps 7 and 8 may be performed between the end of step 1 and the relative intensity calculation in step 11, and does not necessarily have to be performed in the order shown here.
Procedure 9: Read standard sample data measured under the same conditions as when the map data of the analysis sample was acquired from the data measured in advance and stored in the database 16.
Step 10: Proceed to step 11 when using “(b) background intensity map data”, and proceed to step 13 when using an estimated value from the average atomic number.
Step 11: “(c) Map data of relative intensity” is created from “(a) peak intensity map data” and “(b) background intensity map data”.
Step 12: “(c) Relative intensity map data” is subjected to a quantitative correction calculation to create “(d) mass concentration map data”.

Step 13: Calculate the temporary relative intensity of each element from only “(a) map data of peak intensity” and the standard sample data, without taking the background intensity into consideration.
Step 14: Normalize the provisional relative strength of each element with the sum of the provisional relative strengths of all elements, and calculate the average atomic number by using that value as the normalized provisional mass concentration.
Step 15: Using the average atomic number calculated from the temporary relative intensity, estimate the background intensity based on the “data representing the relationship between the average atomic number and the background intensity” called in step 6.
Step 16: Calculate the relative intensity from the estimated background intensity and “(a) map data of peak intensity” to create “(c) map data of relative intensity”.
Step 17: Perform a quantitative correction calculation on “(c) Map data of relative intensity” to create “(d) Map data of mass concentration”. In the second and subsequent iterations, the average atomic number of the procedure 14 is obtained using a value obtained by standardizing the mass concentration obtained by this procedure.
Step 18: Repeat Steps 14 to 17 until a predetermined convergence condition is satisfied.

Step 19: Specify a standardized quantity to be displayed as a two-dimensional distribution image from among quantities related to relative intensity, mass concentration, or composition ratio.
Step 20: Necessary calculations are performed on the specified amount, and a two-dimensional distribution image is displayed on the display device 17.
By the procedure described above, the element distribution reduces the influence of changes in X-ray intensity due to factors such as differences in the matrix effect at the analysis location, sample surface shape, sample surface contamination and vapor deposition film conditions, and fluctuations in measurement conditions. An image can be obtained.

The block diagram which shows schematic structure of the electronic probe microanalyzer concerning implementation of this invention. The figure used in order to demonstrate the idea of this invention. The flowchart for demonstrating embodiment of this invention. The figure for demonstrating the concept which carries out the grid division | segmentation of the analysis area | region two-dimensionally.

Explanation of symbols

(Explanation of symbols in FIG. 1)
1: Electron gun 10: X-ray detector
2: Focusing lens 11: Spectroscopic element control device
3: Objective lens 12: X-ray signal processor
4: Electron beam deflector 13: Sample mounting table controller
5: Optical microscope 14: Interface
6: Analytical sample 15: Control processing unit
7: Sample mounting table 16: Database
8: Electro-optical system controller 17: Display device
9: WDS spectroscopic element 18: Input device

Claims (6)

A means for spectrally detecting / detecting characteristic X-rays generated from the surface of a sample irradiated with an electron beam, and displaying a two-dimensional distribution image based on characteristic X-ray intensity data collected two-dimensionally by scanning the sample or electron beam In an electron probe X-ray analyzer comprising display means for performing and quantitative correction calculation means,
Calculation means for obtaining relative intensity of each element from characteristic X-ray intensity data and standard sample data of a plurality of elements collected at the same coordinates with respect to characteristic X-ray intensity data collected two-dimensionally; A calculation means for performing a quantitative correction calculation on the relative intensity to determine a mass concentration of each element; a calculation means for determining an amount related to a composition ratio based on the mass concentration of each element; and a relative intensity of each element or A calculation means for normalizing the mass concentration of each element or the amount related to the composition ratio,
Predetermined calculation is performed for all coordinate positions of characteristic X-ray intensity data collected two-dimensionally, and the amount related to the normalized relative intensity of each element, the mass concentration of each element, or the composition ratio An electron probe X-ray analysis apparatus characterized in that at least one of them is displayed as a two-dimensional distribution image by the display means. The at least one of the amounts related to the composition ratio is an atomic concentration of each element obtained based on a mass concentration of each element and an atomic weight of each element. The electron probe X-ray analyzer according to 1. At least one of the amounts related to the composition ratio includes a mass concentration of a binding element that binds to each element at a constant binding ratio, a mass concentration of each of the elements, an atomic weight of the binding element, and a mass of each element. The electron probe X-ray analyzer according to claim 1, wherein the mass concentration of the compound is determined based on the atomic weight. At least one of the amounts related to the composition ratio includes the mass concentration of the binding element, the mass concentration of each element, the atomic mass of the binding element, the atomic mass of each element, and the number of atoms for normalization. The electron probe X-ray analyzer according to claim 1, wherein the bond element and the number of atoms of each element are determined based on At least one of the amounts related to the composition ratio is an average atomic number obtained by summing amounts obtained by apportioning atomic numbers of each element at a normalized mass concentration of each element. Item 2. The electron probe X-ray analyzer according to Item 1. Means for spectroscopic / detection of characteristic X-rays generated from the surface of a sample irradiated with an electron beam, and display for displaying characteristic X-ray intensity data collected two-dimensionally by scanning the sample or the electron beam as a two-dimensional distribution image An electronic probe X-ray analyzer comprising: means and quantitative correction calculation means;
Calculation means for obtaining relative intensity of each element from characteristic X-ray intensity data and standard sample data of a plurality of elements collected at the same coordinates with respect to characteristic X-ray intensity data collected two-dimensionally; Computation means for performing a quantitative correction calculation on the relative intensity to obtain the mass concentration of each element and computation means for normalizing the relative intensity of each element or the mass concentration of each element,
A predetermined calculation is performed on all coordinate positions of the characteristic X-ray intensity data collected two-dimensionally, and at least one of the normalized relative intensity of each element or the mass concentration of each element is calculated as two. An electron probe X-ray analyzer comprising display means for displaying as a dimension distribution image.

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