JP2003149183A - EPMA IDENTIFICATION METHOD FOR Al-Fe-BASED COMPOUND - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an EPMA identification method for an Al-Fe-based compound allowing correct identification on an Al-Fe-based compound included in an aluminum material comprising aluminum or an aluminum alloy, without being influenced by compounds other than aluminum, nor being influenced by a matrix even in the case of micro crystallized grains. SOLUTION: This EPMA identification method for the Al-Fe-based compound existing in the aluminum material comprising aluminum or an aluminum alloy is a method for identifying a plurality of AlFe crystallized grains formed of the same constitutive elements but different in the element composition ratio, by EPMA. The AlFe crystallized grains of the sample to be identified are irradiated with accelerated electron beams, and characteristic X-rays in a region including Lα beams and Lβ beams generated from the Fe element by electron beam irradiation are measured, and the AlFe crystallized grains are identified from a spectrum pattern of the measured characteristic X-ray spectrum.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an electron probe microanalyzer for irradiating a sample with an electron beam and measuring the characteristic X-rays emitted from the sample to qualitatively or quantitatively analyze the elements in the sample. microanalys
er; hereinafter referred to as “EPMA”),
In particular, the present invention relates to an EPMA identifying method of an Al-Fe compound for identifying an Al-Fe compound present in an aluminum material made of aluminum or an aluminum alloy.

[0002]

2. Description of the Related Art Iron (Fe) is used for aluminum materials used in a wide range of fields from electronic materials to building materials.
And impurities such as silicon (Si) are included. These impurities are responsible for the recrystallization properties of aluminum, the formation of texture,
Including crystal grain size, alumite film color, luster, strength,
It is known to affect ductility and the like. In general, iron has a low solid solubility in aluminum, and therefore, it exists not only in a solid solution state in an aluminum material but also as an Al—Fe-based compound in an intermetallic compound state. However, the Al-Fe-based compound contained in the aluminum material is a serious defect in the aluminum product such as color loss, deterioration of the transparency of the coating, and generation of voids in the anodic oxidation process performed when the aluminum material is surface-treated. Cause to cause.

The reason why these Al--Fe compounds cause defects in aluminum products is considered as follows. That is, Al-Fe contained in the aluminum material
The system compounds include Al ₃ Fe and A which are AlFe crystallized particles.
There are ₁₆ Fe, Al _m Fe, etc., and AlFeSi crystallized particles such as α-AlFeSi, β-AlFeSi, etc. In many cases, a plurality of these kinds of crystallized particles are mixed in the aluminum material. However, since these crystallized particles have different chemical characteristics depending on their types, for example,
When the crystallized particles as described above are anodized in a sulfuric acid aqueous solution, Al ₃ Fe and α-AlFeSi are oxidized by anodizing treatment, but Al ₆ Fe and β-AlFeSi are not oxidized. Therefore, the color tone of the anodized film formed on the surface varies depending on the type of crystallized particles, and as a result, defects such as color loss occur on the surface of the aluminum material that has undergone the anodizing process. .

In such a situation, if the crystallized particles contained in the aluminum material can be identified, the cause of the product defect in the aluminum product can be identified, and a minute compound that has been overlooked in the past can be identified. The presence of particles can be detected, which is very useful in terms of quality control in the manufacturing process of aluminum products using aluminum materials and history management of manufacturing methods and processing methods.

However, since these crystallized particles present in the aluminum material are minute, they can be analyzed by the X-ray diffraction method (XR
It is difficult to identify crystallized grains existing in the defective portion of aluminum by methods such as D), chemical analysis, and optical microscope observation. In addition, in order to identify these crystallized particles by using EPMA which has been used for qualitative analysis such as discrimination of elemental species contained in a sample and identification of a simple metal and its oxide, carbide, nitride, etc. Commonly used for Al-K
When characteristic X-ray spectra are measured using α satellite rays and Al-Kβ rays, Al ₆ Fe, Al ₃ Fe, α-Al
The spectra measured from FeSi and β-AlFeSi are almost the same as those of pure aluminum both in terms of peak wavelength position and peak intensity, and it is difficult to identify these crystallized particles. Further, a method of identifying these crystallized particles from the relative X-ray intensity ratio of Fe / Al and Fe / Si using EPMA has been proposed (Japanese Patent Laid-Open No. 2000-180393). The aluminum material in which the particles are present can be applied in the case of pure aluminum, but when the aluminum material is made of an aluminum alloy, it is affected by compounds other than aluminum, so that the crystallized particles can be correctly identified. Can not. Furthermore, when the crystallized particles to be identified have micrometer-sized fine particles, they are affected by the matrix. Therefore, it is necessary to reduce the acceleration voltage in electron beam irradiation in EPMA measurement, but the acceleration voltage must be reduced. As a result, the brightness obtained from the radiation source is reduced, the crystallized grain image is not formed, and the X-ray intensity is insufficient, so that the crystallized grain cannot be correctly identified.

[0006]

Therefore, the present inventors have found that the Al--Fe compound present in the aluminum material is not affected by the compounds other than aluminum contained in the aluminum material, and the crystal is not affected. As a result of diligent study on an identification method that is not affected by the matrix even when the emitted particles are minute,
The present invention has been completed by finding that characteristic X-ray spectra in a region including α-rays and Lβ-rays are measured, and that these Al—Fe-based compounds can be identified from the spectrum pattern of the measured spectra.

Therefore, an object of the present invention is to provide an Al--Fe compound contained in an aluminum material made of aluminum or an aluminum alloy without being affected by a compound other than aluminum and when the crystallized particles are minute. EPM of Al-Fe compounds that can be correctly identified without being affected by the matrix
A method of identification.

[0008]

That is, the present invention is an Al-Fe compound present in an aluminum material made of aluminum or an aluminum alloy, which is formed of the same constituent elements and has different elemental composition ratios. EP of a plurality of AlFe crystallized particles, or a plurality of AlFeSi crystallized particles formed from the same constituent element and having different phases
In this method, the AlFe crystallized particles of the identified sample are irradiated with an accelerated electron beam and Fe is irradiated by the electron beam.
Characteristic X-rays in a region containing Lα rays and Lβ rays generated from an element are measured, and these AlFe crystallized particles are identified from the spectrum pattern of the measured characteristic X-ray spectrum. It is an EPMA identification method for system compounds.

Further, according to the present invention, Al-present in an aluminum material composed of aluminum or an aluminum alloy is used.
This is a method for identifying a Fe-based compound by EPMA, in which the Al-Fe-based compound of the identified sample is irradiated with an accelerated electron beam,
The characteristic X-ray intensity generated from Fe element and Si element by electron beam irradiation is measured, and the relative X-ray intensity of these Fe element and Si element is determined from the measured characteristic X-ray intensity, and the obtained relative X-ray intensity is obtained. By calculating the relative X-ray intensity ratio between the Fe element and the Si element, the Al—Fe based compound is determined to be separated into AlFe crystallized particles and AlFeSi crystallized particles, and the separated AlFe crystallized particles The particles are irradiated with an accelerated electron beam, and Fe is irradiated by the electron beam.
Characteristic X-rays in a region containing Lα rays and Lβ rays generated from the element are measured, the AlFe crystallized particles are identified from the spectrum pattern of the measured characteristic X-ray spectrum, and the separated AlFeSi crystals are also identified. The emitted particles are irradiated with an accelerated electron beam, and Fe is irradiated by the electron beam.
Characteristic X-rays in a region containing Lα rays and Lβ rays generated from elements are measured, and these AlFeSi crystallized particles are identified from the spectrum pattern of the measured characteristic X-ray spectrum. Compounds EPM
A identification method.

In the present invention, the Al--Fe compound means iron (Fe) contained as an impurity in an aluminum material made of aluminum or an aluminum alloy.
Which is present in the form of an intermetallic compound in which an Al element and an Fe element are bonded,
Further, an intermetallic compound containing silicon (Si) together with iron as an impurity is also included. Specific examples of the Al-Fe compound include AlFe crystallized particles whose constituent elements are two kinds of elements Al and Fe, and AlFeSi crystallized particles whose constituent elements are Al, Fe and Si. , AlFe crystallized particles have the same constituent elements but different composition ratios, Al ₆ Fe, Al ₃ Fe, Al _m
Further, Fe or the like, and as AlFeSi crystallized particles, α-AlFeS having the same constituent elements but different phases
Examples include i and β-AlFeSi.

EP used in carrying out the identification method of the present invention
As the MA, a wavelength dispersion type (Wavelength Dispersive X-
ray Analysis) is preferred. As for the electron beam irradiation source, a tungsten filament electron gun, LaB ₆ (6
- lanthanum boride) cathode equipped with an electron gun, and CeBi _x
(US FEI trade name: Sebikkusu) either of the cathode mounting electron gun may be used but, LaB ₆ cathode mounting electron gun and CEBI _x cathode mounting electron gun has a high brightness, high analysis spatial resolution Therefore, even crystallized particles having a diameter of 1 μm or less can be identified.

EP of Al-Fe compound in the present invention
Regarding the MA identification method, first, Al which is a sample to be identified
An -Fe compound is irradiated with an electron beam accelerated by an electron gun, and the characteristic X-ray intensity generated from the Fe element and the Si element by the electron beam irradiation is measured. As electron beam irradiation conditions at this time, the acceleration voltage is usually 10 to 20 kV, preferably about 15 kV, and the sample absorption current is 10 nA or more,
It is preferably about 15 nA and the electron beam diameter is 1 μm.
It is preferably mφ or less. Further, as the measurement condition of the specific X-ray, the measurement time is 5 seconds or more, preferably about 10 seconds. The relative X-ray intensities of the Fe element and the Si element are calculated by using the measured characteristic X-ray intensities, and the relative X-ray intensities of the Fe-element and the Si-element of the Al-Fe compound, which is the sample to be identified, are calculated. Calculate the X-ray intensity ratio.

When the relative X-ray intensity ratio calculated by the above method is 20 or less, the measured Al--Fe compound is Al ₆ Fe, Al ₃ Fe, or Al _m Fe.
It can be determined as Fe crystallized particles, and when the relative X-ray intensity ratio is 20 or more, α-AlFeSi, β-AlFeS
It can be determined that the AlFeSi crystallized particles are any of i, and thus the Al-Fe compound to be identified is
It is possible to perform a classification determination as to whether the particles are AlFe crystallized particles or AlFeSi crystallized particles.

Next, the separated AlFe crystallized particles are irradiated with an electron beam accelerated by an electron gun. As the electron beam irradiation conditions at this time, the acceleration voltage is 3 to 15 k.
V, preferably 5 to 10 kV. Acceleration voltage is lower as the difference was observed in the peak wavelength position of the measured characteristic X-ray spectrum, but it is convenient to determine the difference between the spectrum, below the 3 kV, LaB ₆ cathode mounting electron gun or CEBI _x cathode Even when the on-board electron gun is used, the obtained brightness is lowered, so that it is difficult to determine the spectrum when the AlFe crystallized particles are fine particles. On the contrary, when the accelerating voltage becomes higher than 15 kV, F
Since the higher-order line of e-Kα becomes large, the measured characteristic X
The position of the peak wavelength of the line spectrum becomes unclear,
It becomes difficult to identify the Fe crystallized particles. The sample absorption current is preferably 50 nA or more,
The electron beam diameter is preferably 1 μmφ or less. As the characteristic X-ray measurement condition, the characteristic X-ray spectrum to be measured is L generated from Fe element by electron beam irradiation.
The wavelength region may be 17.0 to 18.0Å, and the measurement time may be 10 seconds or more / step, as long as the region includes α rays and Lβ rays.

Generated from the Fe element measured by the above method
Of the characteristic X-ray spectrum including Lα and Lβ
According to the cuttle pattern, the measured AlFe crystallized particles
Al ₆Fe or Al₃To identify if it is Fe
You can That is, in this measurement spectrum, Fe
Due to the Lα line-derived peak and Lβ line generated from the element
If another peak appears between the incoming peaks, Al
₆Fe and Al if no peak appears at this position₃Fe
Can be identified as For this reason
Obviously, depending on the bonding state of Al and Fe, these
Differences in spectral patterns are likely to occur.

The AlFeSi crystallized particles can also be identified by performing the EPMA measurement on the AlFeSi crystallized particles determined to be separated by the same method as described above. That is, as the electron beam irradiation condition, the acceleration voltage is 3 to 15
kV, preferably 5-10 kV. Acceleration voltage is lower as the difference was observed in the peak wavelength position of the measured characteristic X-ray spectrum, but it is convenient to determine the difference between the spectrum, below the 3 kV, LaB ₆ cathode mounting electron gun or CEBI _x cathode Even when using the on-board electron gun,
When the AlFeSi crystallized particles are fine particles, it is difficult to determine the spectrum because the obtained brightness is lowered. On the other hand, when the accelerating voltage is higher than 15 kV, the higher-order line of Fe-Kα becomes large, so that the position of the peak wavelength of the characteristic X-ray spectrum to be measured becomes unclear, which makes it difficult to identify AlFeSi crystallized particles. Become. Also,
The sample absorption current is preferably 50 nA or more, and the electron beam diameter is preferably 1 μmφ or less. As the measurement condition of the characteristic X-ray, the characteristic X-ray spectrum to be measured may be a region containing Lα rays and Lβ rays generated from Fe element by electron beam irradiation,
The wavelength range is preferably 17.0 to 18.0Å,
The measurement time is preferably 10 seconds or more / step.

According to the spectrum pattern of the characteristic X-ray spectrum containing Lα and Lβ rays generated from the Fe element measured by the above method, whether the measured AlFeSi crystallized particles are α-AlFeSi or β-AlFeSi Can be identified. That is, in this measurement spectrum, if a further peak appears between the peak derived from the Lα line and the peak derived from the Lβ line generated from the Fe element, β-AlFeSi, and if no peak appears at this position, , Α-AlFeSi.

In the present invention, an aluminum material containing an Al--Fe compound is dissolved in hot phenol, then diluted with benzyl alcohol, and the resulting solution is filtered to obtain an insoluble Al--Fe compound. A well-known phenol method (Light metal Vol.35, No.1)
1, P.647 to 649, Light Metals Vol.39, No.9, P.645 to 650), the Al-Fe compound may be separated and concentrated and used as an identification sample. Al- contained in aluminum material
Since the Fe-based compound can be separated and concentrated to be used as an identification sample, in the measurement by EPMA, the characteristic X-ray intensity from the Al-Fe-based compound to be identified is easily ensured, and a clear spectrum is obtained. be able to. Also,
Since only the Al-Fe-based compound is separated and used as the identification sample, it is possible to avoid the risk of measuring characteristic X-rays from compounds other than the Al-Fe-based compound contained in the aluminum material, Accurate spectra can be collected. There are no restrictions on the electron beam irradiation condition and the characteristic X-ray measurement condition in the EPMA measurement for the identification sample separated by the above-mentioned phenol method other than those shown above.

In the EPMA identification method of the present invention, the aluminum material containing the Al--Fe compound may be measured as a so-called bulk material sample in the state of the aluminum material. Since the Al-Fe compound can be identified in the state of existing in the aluminum material, the labor for adjusting the identification sample can be saved and the measurement can be performed efficiently, and the aluminum material is processed into the aluminum product. By identifying the Al-Fe compound in the actual manufacturing process, it can be a powerful tool in product management. For bulk material samples, EP
The electron beam irradiation conditions and the characteristic X-ray measurement conditions in MA measurement are not particularly limited, as in the case of the identification sample employing the phenol method.

[0020]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, a wavelength dispersion type EPMA (electron beam microanalyzer EPMA-150 manufactured by Shimadzu Corporation) is used.
0; X-ray extraction angle δ: 52.5 °), a preferred embodiment of the present invention will be specifically described based on an example.

Example 1 [Preparation of measurement sample] Aluminum material containing Al ₃ Fe single phase material, aluminum material containing Al ₆ Fe single phase material, α
-AlFeSi-based aluminum material, and β
Regarding the aluminum material containing the -AlFeSi main material, the Al ₃ Fe single phase material, the Al ₆ Fe single phase material, the α-AlFeSi main material, and the β-AlFeSi were separated from the aluminum material by the following method. First, 300
120 ml of phenol was charged into a ml flask and heated at 180 ° C. for about 1 minute to remove water, and then Al ₃
0.1 to 1 g of the aluminum material containing the Fe single phase material was finely shredded and put into a flask, and a reflux condenser was attached to heat it for about 3 to 5 minutes to dissolve the sample aluminum material in phenol. 80 ml of benzyl alcohol was added and the mixture was cooled to room temperature, and the obtained solution was filtered through a PTFE membrane filter (pore size 0.1 μm) to separate the Al ₃ Fe single phase material, which was used as measurement sample 1.
Al ₆ F separated from aluminum material by the same method
The single phase material was used as measurement sample 2, the α-AlFeSi main material was used as measurement sample 3, and the β-AlFeSi main material was used as measurement sample 4.

[Measurement by EPMA] Next, a part of the obtained measurement samples 1 and 2 was sampled and mounted on an EPMA sample stage, and after Pt deposition, a tungsten filament electron gun was used to accelerate at an accelerating voltage of 5 kV. Sample absorption current 30n
A, F under electron beam irradiation condition of electron beam diameter 5 μm
A spectrum was measured in a region including e-Lα line and Fe-Lβ line. In addition, the measurement condition of the spectrum is that the used spectroscopic crystal is RAP (Rubidium acid phthalate: Rubidium aci).
d phtharate), the analysis wavelength is 17.0 to 18.0 Å, the step width is 0.002 Å, and the measurement time is 10 seconds.

The spectra of the Al ₃ Fe single phase material and the Al ₆ Fe single phase material (measurement samples 1 and 2) obtained by the above method are shown in FIGS. 1 (A) and 1 (B). For reference, FIG. 2 shows a spectrum of pure iron (99.998% Fe) measured by EPMA. The Al ₃ Fe single phase material of FIG. 1 (A) and FIG.
In the Al ₆ Fe single-phase material (B), peak 1 derived from Fe-Lα line and peak 2 derived from Fe-Lβ line can be confirmed. However, in FIG. 1 (B), peak 3 appears near the Fe—Kα higher-order line which can be confirmed in the spectrum of pure iron shown in FIG. 2. Therefore, Fe-Lα ray and Fe
-By using the difference between the peaks appearing between the Lβ lines, A
It is possible to identify the l ₃ Fe single phase material and the Al ₆ Fe single phase material.

Spectra obtained from measurement samples 3 and 4 by the same method as described above are shown in FIGS. 3 (A) and 3 (B). As in the case of the Al ₃ Fe single-phase material and the Al ₆ Fe single-phase material, in the spectrum of the β-AlFeSi main material of FIG. 3 (B), peak 3 which is considered to be derived from the satellite of Fe-Lα line was confirmed. Yes, that is, Fe-L
By utilizing the difference in this peak appearing between the α-ray and the Fe-Lβ-ray, it is possible to identify the α-AlFeSi main material and the β-AlFeSi main material.

Example 2 An aluminum material containing an Al ₃ Fe single phase material was measured Sample 5
Similarly, an aluminum material containing an Al ₆ Fe single phase material, an aluminum material containing an α-AlFeSi main material,
And the aluminum material containing the β-AlFeSi main material were used as measurement samples 6 to 8 in the bulk material sample state. Next, with respect to the measurement samples 5 and 6, Pt vapor deposition was performed after electrolytic polishing, the Pt sample was mounted on the EPMA sample table, and the acceleration voltage was 10 kV using a tungsten filament electron gun.
A spectrum was measured in a region including the Fe-Lα line and the Fe-Lβ line under electron beam irradiation conditions with a sample absorption current of 50 nA and an electron beam diameter of 1 μmφ. The measurement conditions of the spectrum are as follows: the analyzing crystal used is RAP (rubidium acid phthalate), the analysis wavelength is 17.0 to 18.0Å, the step width is 0.002Å, and the measurement time is 30 seconds.

The spectra of the Al ₃ Fe single phase material and the Al ₆ Fe single phase material (measurement samples 5 and 6) obtained by the above method are shown in FIGS. 4 (A) and 4 (B). Similar to the spectra shown in FIGS. 1A and 1B above, A in FIG.
The spectrum of the l ₆ Fe single phase material includes Fe-Lα rays and Fe.
Between -Lβ line, peak 3 which is considered to be derived from the satellite of Fe-Lα line can be confirmed. Therefore, Fe-Lα
By using the difference between the peaks appearing between the Fe-Lβ line and the Fe-Lβ line, the Al ₃ Fe single-phase material and the Al ₆ Fe ₆
The Fe single phase material can be identified.

Spectra obtained from measurement samples 7 and 8 by the same method as described above are shown in FIGS. 5 (A) and 5 (B). As in the case of the Al ₃ Fe single-phase material and the Al ₆ Fe single-phase material, in the spectrum of the β-AlFeSi main material of FIG. 5 (B), peak 3 which is considered to be derived from the satellite of Fe-Lα line was confirmed. Fe-L
By utilizing the difference in this peak appearing between the α-ray and the Fe-Lβ-ray, it is possible to identify the α-AlFeSi main material and the β-AlFeSi main material also in the bulk material sample.

[0028]

EFFECT OF THE INVENTION EPMA of Al--Fe compound of the present invention
According to the identification method, Al-F existing in the aluminum material
The e-based compound is not affected by compounds other than aluminum contained in the aluminum material, and
Even when the crystallized particles are minute, the Al—Fe compound can be identified without being affected by the matrix.

[Brief description of drawings]

FIG. 1 shows Al ₃ by the EPMA identification method of the present invention.
Fe is a characteristic X-ray spectrum of the single-phase material and Al ₆ Fe single phase material, (A) is Al ₃ Fe single phase material, (B) is Al ₆ Fe single phase material.

FIG. 2 is a characteristic X-ray spectrum of pure iron.

FIG. 3 shows α-A according to the EPMA identification method of the present invention.
1A is a characteristic X-ray spectrum of a main material of 1FeSi and a main material of β-AlFeSi, where (A) is a main material of α-AlFeSi,
(B) is a β-AlFeSi main material.

FIG. 4 shows Al ₃ by the EPMA identification method of the present invention.
Fe is a characteristic X-ray spectrum of the single-phase material and Al ₆ Fe single phase material, (A) is Al ₃ Fe single phase material, (B) is Al ₆ Fe single phase material.

FIG. 5 shows α-A according to the EPMA identification method of the present invention.
1A is a characteristic X-ray spectrum of a main material of 1FeSi and a main material of β-AlFeSi, where (A) is a main material of α-AlFeSi,
(B) is a β-AlFeSi main material.

[Explanation of symbols]

1 ... Peak derived from Fe-Lα line, 2 ... Fe-Lβ
Line-derived peak, 3 ... Fe-Lα ray satellite-derived peak

Claims (6)

[Claims] 1. An EPMA is used to identify a plurality of AlFe crystallized particles which are Al-Fe compounds existing in an aluminum material made of aluminum or an aluminum alloy and which are composed of the same constituent elements and have different element composition ratios. In this method, the AlFe crystallized particles of the identified sample are irradiated with an accelerated electron beam, and characteristic X-rays in a region containing Lα and Lβ rays generated from the Fe element by the electron beam irradiation are measured. EPMA identification method for Al-Fe compounds, characterized in that these AlFe crystallized particles are identified from the spectrum pattern of the characteristic X-ray spectrum. 2. A method of identifying a plurality of AlFeSi crystallized particles, which are Al-Fe compounds existing in an aluminum material made of aluminum or an aluminum alloy, and which are formed of the same constituent element and have different phases by EPMA. Yes, the AlFeSi crystallized particles of the identified sample were irradiated with an accelerated electron beam, and characteristic X-rays in a region containing Lα and Lβ rays generated from the Fe element by the electron beam irradiation were measured, and the measured characteristics EPMA identification method of Al-Fe type compound characterized by identifying these AlFeSi crystallized particles from the spectrum pattern of X-ray spectrum. 3. The acceleration voltage in electron beam irradiation is 3 to 15
EPMA identification method of the Al-Fe type compound of Claim 1 or 2 which is kV. 4. The Al—Fe system according to claim 1, wherein an aluminum material containing an Al—Fe system compound is dissolved in phenol and the Al—Fe system compound is separated and concentrated to obtain an identification sample. EPMA identification method of compounds. 5. An aluminum sample containing an Al—Fe compound is used as an identification sample as a bulk material sample.
EPMA identification method of the Al-Fe type compound in any one of. 6. A method for identifying an Al—Fe compound present in an aluminum material made of aluminum or an aluminum alloy by EPMA, which is an identification sample of Al—Fe.
The compound compound is irradiated with an accelerated electron beam, the characteristic X-ray intensity generated from the Fe element and the Si element is measured by the electron beam irradiation, and the relative X of the Fe element and the Si element is measured from the measured characteristic X-ray intensity. The line intensity is obtained, and the relative X-ray intensity ratio between the Fe element and the Si element is calculated from the obtained relative X-ray intensity to separate the Al—Fe compound into AlFe crystallized particles and AlFeSi crystallized particles. Then, the separated AlFe crystallized particles are irradiated with an accelerated electron beam, and the characteristic X-rays in the region including the Lα and Lβ rays generated from the Fe element by the electron beam irradiation are measured. Then, the AlFe crystallized particles were identified from the spectrum pattern of the measured characteristic X-ray spectrum, and the fractionated AlFeSi crystallized particles were irradiated with an accelerated electron beam to obtain an electron beam. L generated from Fe element by irradiation
EPMA of an Al-Fe compound characterized by measuring characteristic X-rays in a region including α-rays and Lβ-rays, and identifying these AlFeSi crystallized particles from the spectrum pattern of the measured characteristic X-ray spectrum. Identification method.