JPH0763709A - Method and apparatus for measuring depth-wise assembly organization - Google Patents

Abstract

PURPOSE:To measure a distribution of a depth-wise crystal orientation of various polycrystalline materials at the same position under high reliability simply in a short time without working of the material. CONSTITUTION:A lattice surface (hkl) to be measured is specified a specified angle theta of incidence is inputted into an arithmetic device 16 to irradiate a sample S supported by a goniometer 10 with X rays at the angle theta of incidence from an X-ray generator 12 and a mobile type photodetecting slit 22 with a fixed angle of photodetecting is moved parallel sequentially to positions A1-n corresponding to depths t1-tn from the surface of the sample S to measure the intensity of diffraction X rays at each position with a semiconductor detector 14. Then, the diffraction X rays are measured under the same conditions for a random oriented sample the same in composition as the sample S. A random intensity ratio is determined at a specified depth of the sample S based on the results of the measurements at photodetecting slit positions obtained from both the samples. An orientation distribution of the lattice surface is determined in the depth from the intensity ratio.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and an apparatus for measuring a texture in the depth direction, and more particularly to an energy method capable of nondestructively and rapidly measuring the texture in the depth direction of a polycrystalline material such as a metal. The present invention relates to a method and apparatus for measuring a texture in the depth direction by a dispersion method.

[0002]

2. Description of the Related Art Since the texture of a polycrystalline material, particularly a metal, has a great influence on the processing characteristics and magnetic properties, controlling the texture is an effective means for improving the quality of products.

For example, the improvement of the degree of integration of secondary recrystallized grains in the (110) [001] orientation, which brings about the improvement of the magnetic properties of the unidirectional silicon steel sheet, is improved from the steel sheet surface to 1/10 to 1/1 of the sheet thickness.
It is necessary to develop the primary recrystallization texture of (110) [001] orientation at 5 depth positions.

Further, in order to improve the plastic strain ratio (r value) of the low carbon steel sheet, the texture of {111} orientation must be uniformly generated in the depth direction.

Further, in order to prevent ridging of a ferritic stainless cold rolled steel sheet, a recrystallization texture of {110} <001> orientation is developed deep into the surface of the steel sheet, and {1
It is important to suppress the formation of rolling texture in the {00} <011> orientation.

Needless to say, it is necessary to measure the texture of the material surface in order to highly control the texture as described above, and in particular, it is necessary to measure the distribution of the texture in the depth direction. It is essential.

The texture is an evaluation of the crystal orientation of the material, and its measurement is most commonly made by preparing an inverse pole figure or a positive pole figure from the X-ray diffraction measurement of the sample surface. .

When irradiating the sample surface with X-rays, the X-rays interact with the sample and penetrate to the inside of the sample of several μm to several hundreds of μm depending on the energy thereof. The pole figure obtained includes information from the sample surface to the penetration depth of the diffracted X-rays.

By the way, in order to obtain the distribution of texture in the depth direction, it is necessary to measure the crystal orientation at a specific depth position. Therefore, conventionally, at each depth position for measurement,
The sample was processed by polishing, etc., and a thin test piece with a thickness of several tens of μm was prepared and measured. However, the method of creating a test piece from the material at each measurement depth position by polishing or the like as described above requires a great deal of labor to create the test piece, and in this method, from the same position on the material surface. Since a measurement sample cannot be collected, there is a problem in that the measurement result includes variations due to locations within the material surface.

Further, as another means for easily evaluating the texture in the depth direction, there is a method of estimating from the etch pits of the sample cross section. In this method, the etch pits are dislocations in a sample having a processing strain. It is hard to appear in areas other than
Further, since the size of the etch pit sensitively changes depending on the material composition, the corrosive solution composition, the immersion time, etc., it is difficult to control the size according to the material structure. Also, with this method,
There is also a problem that the crystal orientation cannot be quantitatively evaluated.

Further, regarding the measurement of the texture of the steel sheet,
As a technique for a texture such as an electromagnetic steel sheet, the incident angle is fixed to a constant angle and continuous X-rays are irradiated, and the diffracted X-rays from the sample are at a position twice the incident angle, and Detected by the semiconductor detector fixed at the position where the diffraction peak and the escape generated from the detector overlap, the detected signal is energy-analyzed by the wave height analyzer, and for each crystal lattice plane obtained by removing the influence of the escape peak. A method for obtaining a pole density distribution function from the intensity of diffracted X-rays is disclosed in Japanese Patent Laid-Open No. 2-145.
In Japanese Patent Laid-Open No. 948, as a technique mainly for measuring a surface-treated steel sheet, a fluorescent X-ray intensity of a surface layer component is detected to obtain a surface layer thickness, and then each measurement target crystal plane (hk
For each l), a set diffraction angle that gives a constant X-ray penetration depth that is less than or equal to the surface layer thickness is obtained, and the diffraction angle is set to the set diffraction angle for each crystal surface to be measured. A method of detecting the diffraction intensity by using the above method and measuring the axial density texture in the surface normal direction of the surface layer from the detected diffraction intensity is disclosed in Japanese Examined Patent Publication No. 5-10617. Since the latter is not intended for measurement, and the latter is intended for measuring the texture of the surface layer, the texture in the depth direction cannot be measured to the depth by any method.

Therefore, the applicant of the present invention has two or more types of continuous X-rays with respect to the surface of the sample to be measured, which are capable of measuring the texture in the depth direction of the sheet by measuring electromagnetic steel sheets, cold rolled steel sheets and the like. And the diffraction X-ray detected from the incident X-rays at each incident angle is subjected to energy spectroscopy to obtain the intensity of the diffracted X-rays from a specific lattice plane, and a randomly oriented sample having the same composition as the above-mentioned measurement sample. For the incident X-ray intensities from the specific lattice plane under the same conditions, the ratio of the X-ray intensities of the measurement sample to the X-ray intensities of the disordered alignment sample obtained for each of the incident angles is calculated from A technique for calculating a random intensity ratio at a specific depth position corresponding to each incident angle and obtaining a distribution of the degree of orientation of the specific lattice plane in the thickness direction from the random intensity ratio is disclosed in JP-A-5-1999.
It is proposed in the Gazette.

[0013]

However, although the technique disclosed in Japanese Patent Laid-Open No. 5-1999 is effective in itself, as a result of a detailed study by the present inventors,
It was revealed that when measuring the texture up to the deep part in the plate thickness direction, an abnormal value of the measurement may be seen in a part of the depth direction.

The present invention has been made in order to solve the above-mentioned conventional problems, and various materials made of polycrystals can be formed by the Ernergi dispersion type X-ray diffraction method using white (continuous) X-rays. A method and an apparatus for measuring a texture in the depth direction, which can accurately measure the distribution of the crystal orientation degree in the thickness direction at the same position in a short time without processing, up to the deep portion in the depth direction of the plate thickness. The task is to do.

[0015]

According to the present invention, continuous X-rays are irradiated onto a measurement sample surface at a predetermined incident angle, and diffracted X-rays are arranged at a position symmetrical to the incident X-ray with respect to the normal line of the measurement sample surface. In the method for measuring a texture in the depth direction, the continuous X-rays are irradiated onto a measurement sample surface at a predetermined incident angle, and a plurality of diffracted X-rays obtained for the incident X-rays are received at the same light receiving angle. The intensity of the diffracted X-ray from the specific lattice plane is detected by detecting the light at the light receiving position, and the intensity of the diffracted X-ray from the specific lattice plane is measured under the same conditions for the disordered orientation sample having the same composition as the measurement sample. From the ratio of the diffracted X-ray intensity of the measurement sample to the diffracted X-ray intensity of the chaotically oriented sample obtained at each of the light-receiving positions, and calculating a random intensity ratio at a specific depth position corresponding to each of the light-receiving positions. And above the random strength By obtaining the distribution of the degree of orientation of the specific lattice plane in the depth direction from the ratio is obtained by solving the above problems.

The present invention also provides a method for measuring texture in the depth direction, wherein a predetermined incident angle of continuous X-rays is set to the continuous X-ray.
The angle is set so that the diffracted X-ray based on the characteristic X-ray in the line is not received.

The present invention also provides a goniometer having a function of supporting a measurement sample and adjusting an incident angle of X-rays, and an X-ray generator for generating X-rays for irradiating the surface of the measurement sample.
An energy dispersive counter arranged at a position symmetrical to the X-ray generator with respect to a normal line of the measurement sample surface, and an arithmetic unit for performing a predetermined calculation based on the diffracted X-ray intensity measured by the energy dispersive counter. And a divergence slit for limiting the beam width of the X-ray with respect to the measurement sample surface, the divergence slit being provided in front of the energy dispersion counter. The above problem is similarly solved by adopting a configuration in which a light receiving slit having a function of moving in parallel at the same light receiving angle is provided.

[0018]

In order to improve the analysis accuracy and quality of X-ray analysis of steel sheets such as unidirectional silicon steel sheets and ferritic stainless steel cold-rolled steel sheets, the present invention has been made by the present inventors. This has been made as a result of various studies to solve the problem that an abnormal value of measurement may be seen in a partial region in the depth direction, which exists in the technique disclosed in 1999, for example, as described below. As shown in FIG. 1, when the measurement sample S is irradiated with continuous X-rays at a constant incident angle θ and when the semiconductor detector 14 detects the diffracted X-rays at the diffraction angle 2θ, the semiconductor detector 14 has a predetermined width. The movable type light receiving slit 22 having a function of introducing the diffracted X-rays into the semiconductor detector 14 is moved in parallel while maintaining the same light receiving angle, that is, the same diffraction angle 2θ, and the diffracted X-rays are formed at two or more predetermined positions. I also divided the measurement It is.

First, the measurement principle of the present invention will be described in detail.

When a white X-ray is incident on a flat plate polycrystalline sample at an incident angle θ and is diffracted in the direction of 2θ with respect to the incident X-ray having energy E _hkl , (hk in a volume of thickness dt at depth t)
l) The diffracted X-ray intensity from the lattice plane is described by the following equation (1).

ΔI _hkl (t) = {I _ohkl (θ) So (θ) / sin θ} dt × f _hkl (t) L (θ) T (θ) P _hkl F _hkl ² × exp {-2μ (E _hkl ) T / sin θ} (1)

Here, I _ohkl (θ): Thomson's elastic scattering intensity equation S _o (θ): _Cross- sectional area of incident X-ray f _hkl (t): Crystal grain whose (hkl) plane is oriented parallel to the sample surface Volume fraction of L (θ): Lorentz factor T (θ): Debye-Waller temperature factor P _hkl : Multiplicity of (hkl) plane F _hkl : Structural factor of (hkl) plane μ (E _hkl ): Energy E _hkl Absorption coefficient of sample for X-ray

Now, let (d) be the lattice spacing of the (hkl) diffractive surface.
_{If hkl} , the following expression (2) is established in energy dispersive X-ray diffraction, and _therefore μ in the above expression (1) is expressed by a function of the incident angle θ.

E _hkl = 6.2 / (d _hkl sin θ) (2)

In the case of a sufficiently thick sample, the diffraction intensity measured without division by the light-receiving slit is given by the following expression (3) obtained by integrating the depth t of expression (1) from 0 to ∞. Corresponds to the left side.

[0026]

[Equation 1]

In the above equation (3), G (θ) is a term that does not depend on the depth t, and S (θ) is given by the following equation (4).

S (θ) = 2μ (θ) / sin θ (4)

The penetration depth x of the diffracted X-ray at this time is x
Changes depending on θ as shown in the following equation (5).

X = −ln (1−K) / S (θ) (5)

Where K is a calibration constant,
Usually, 0.632 to 0.99 is used.

Further, μ (θ) in the equation (4) is Victore
en's empirical formula (International Tables for X-ray C
rystallography III, Kynoch Press, Birmingham
, (1962), p 157) can be calculated as in the following expression (6).

Μ (θ) / ρ = C (6.2 / E _hkl ) ³ −D (6.2 / E _hkl ) ⁴ + Bσ _KN (6) where, ρ: density C, D, B: atom Of σ _KN : Klein-Nishina free electron scattering cross section

Now, as an example, the penetration depth x (11) with respect to the incident angle θ of the (110) plane and the (200) plane of α-Fe.
0) and x (200) are shown in Table 1, respectively.

[0035]

[Table 1]

By decreasing the incident angle θ in the order of 15 °, 10 °, 5 °, and 4 °, the penetration depths are 3.5 μm, 7.1 μm, 23.7 μm, and 33.7 μm on the (110) plane, respectively.
5.1 μm, which is 9.1 μm on the (200) plane.
m, 18.4 μm, 61.7 μm, 91.3 μm, and it can be seen that the depth increases as the incident angle θ decreases on any surface.

In order to obtain the distribution of the orientation degree of the crystal lattice plane (hkl) in the depth direction, the diffracted X-ray is divided by moving the light-receiving slit until it corresponds to the above penetration depth at a certain incident angle θ. This results in _obtaining f _hkl (t) from the above equation (3) using the diffraction intensity measured by

Now, with the incident angle fixed at θ and the diffraction angle fixed at 2θ,
Assuming that the light-receiving slit is located at a position where diffracted X-rays from depth 0 to t ₁ are measured, the diffraction intensity I _hkl (t ₁ ) can be expressed by the following equation (7) from equation (3). it can.

[0039]

[Equation 2]

If the volume fraction of the (hkl) plane from the sample surface to t ₁ is f _hkl (t ₁ ) (constant), then f _hkl (t
₁ ) can be calculated from the above equation (7) as the following equation (8).

F _hkl (t ₁ ) = {I _hkl (t ₁ ) S (θ)} / [G (θ) {1-exp (−S (θ) t ₁ )}] ... (8)

Next, the light receiving slit is moved to measure the diffracted X-rays from the depths t ₁ to t ₂ , and the volume fraction of the (hkl) plane between them is f _hkl (t ₂ ). I
_{Since hkl} (t ₂ ) is similarly expressed by the following equation (9), the volume fraction f _hkl (t ₂ ) is given by the following equation (10).

[0043]

[Equation 3]

F _hkl (t ₂ ) = {I _hkl (t ₂ ) S (θ)} / [G (θ) × {exp (−S (θ) t ₁ ) − exp (−S (θ) t ₂ )}]… (10)

[0045] Similarly depth t by measuring to _n, the depth t _n-1 and t _n between (hkl) plane of the volume fraction f
_hkl (t _n ) can be _calculated by the following equation (11). However, n ≧ 1 and t ₀ = 0.

F _hkl (t _n ) = {I _hkl (t _n ) S (θ)} / [G (θ) × {exp (−S (θ) t _n−1 ) − exp (−S (θ) t _n )}] (11)

The same measurements as detailed above are performed on a randomly oriented sample.

Since the distribution of the crystal orientation degree in the depth direction is constant in the disorderly oriented sample, the volume fraction f of the (hkl) plane is f.
_hkl (t) = C '(constant). Therefore, the incident angle θ,
The diffraction intensity I _Rhkl (t _n ) of the disordered orientation sample corresponding to the depths t _n-1 to t _n measured by fixing the diffraction angle 2θ and moving the light receiving slit is given by the following expression (12).

I _Rhkl (t _n ) = C′G (θ) {exp (−S (θ) t _n−1 ) −exp (−S (θ) t _n )} / S (θ) (12)

By substituting the equation (12) into the equation (11), the ratio of the volume fraction of the sample to the disorderly oriented sample between the depths t _n-1 and t _n (at a specific depth) The random intensity ratio) P _hkl (t _n ) can be determined by the following equation (13).

P _hkl (t _n ) = I _hkl (t _n ) / I _Rhkl (t _n ) ... (13)

The distribution of the specific degree of lattice plane orientation in the depth direction can be obtained by calculating the random intensity ratio at the specific depth position by the equation (13).

The relationship between the light receiving slit position A and the depth t can be obtained by the following equation (14). However, A is the distance with the origin being the position for receiving the diffracted X-rays in the 2θ direction when t = 0.

T = A / (2cos θ) (14)

Next, according to the present invention, the reason why highly reliable measured values can be obtained in the entire region in the thickness depth direction will be described.

Generally, for the purpose of measuring the texture up to the deep part in the depth direction, molybdenum (Mo
), A target such as tungsten (W) is used.

When two or more types of incident angles are used as in the conventional method disclosed in the above-mentioned Japanese Patent Laid-Open No. 5-1999, the cause of the abnormal value of measurement being observed in a partial area in the depth direction is as follows. As a result of detailed examination, it has been clarified that the cause is the influence of the characteristic X-rays existing in the continuous X-rays when the continuous X-rays with large energy are used.

That is, for example, when Mo is used as an X-ray target, the continuous X-ray is generated in the X-ray generation profile.
Along with the lines, characteristic X-rays such as Mo Kα ₁ line (wavelength 0.7093Å) are included.

As an example, considering the case of measuring the (200) plane of α-Fe (plane spacing d ₂₀₀ = 1.4332Å), d and λ can be calculated from the Bragg diffraction equation represented by the following equation (15). And d ₂₀₀ = 1.4332Å and Mo K respectively
Substituting the wavelength 0.7093Å of the α ₁ line, θ = 14.3 ° when n = 1, and a diffraction line occurs at 2θ = 28.6 °. Since this intensity is several to several tens of times stronger than continuous X-rays other than the characteristic X-ray, it affects the characteristic X-ray and the wavelength data in the vicinity thereof, and corresponds to this wavelength. This causes an error in the orientation measurement data of the depth to be moved and its vicinity. The depth corresponding to this wavelength can be obtained as the penetration depth from the equation (5), and in this example, 1
It becomes 0 μm.

2 dsin θ = nλ (15) d: lattice spacing θ: incident angle n: reflection order λ: incident X-ray wavelength

Therefore, in the present invention, an incident angle other than the above-mentioned incident angle that causes an error in the orientation degree measurement data, and an incident angle at which the penetration depth of X-rays up to a target depth is obtained,
It is made possible to obtain the values by calculation using the equations (5) and (15) and set them in advance. In this case, the generated diffracted X-rays can be divided by the light-receiving slit to obtain the intensity change corresponding to the depth, so that the degree of orientation that does not include the error due to the characteristic X-ray as described above can be obtained. Measurement data can be obtained.

Further, in the conventional method, the depth direction is measured by changing the incident angle, but the X-ray on the low energy side is required among the continuous X-rays to measure the shallow portion. To do. However, when an ordinary X-ray target is used, the intensity of X-rays on the low energy side of about 10 K eV or less is weak, and as shown in FIG.
In the shallow region of 0 μm, there was a portion where accurate measurement could not be performed.

On the other hand, according to the present invention, as shown in FIG. 5, which will be described later, it is possible to accurately measure from a shallow portion to a deep portion without generating an abnormal value.

[0064]

Embodiments of the present invention will now be described in detail with reference to the drawings.

In this embodiment, the X-ray target is Mo, the tube voltage is 60 kV, the tube current is 300 mA, the widths of the divergence slit and the light receiving slit are 0.05 mm, and the X-ray incident angle (θ).
Is 4 °, the X-ray diffraction angle (2θ) is 8 °, and the measurement time is 1000 seconds at each measurement depth.

FIG. 1 is a schematic block diagram showing a measuring apparatus for texture in the depth direction according to an embodiment of the present invention.

The depth direction texture measuring apparatus of the present embodiment supports the measurement sample S and has a function of adjusting the incident angle of the X-rays irradiated on the surface of the sample S.
0, a rotating anticathode type X-ray generator 12 capable of generating high-power and high-energy white X-rays, and a semiconductor detector (energy dispersion counter) 14 for measuring the diffracted X-rays from the sample S. And a calculation device 16 for performing a predetermined calculation on the diffracted X-rays detected by the semiconductor detector 14.

A goniometer control device 18 is connected to the goniometer 10, and the incident angle θ of the X-ray can be arbitrarily changed by a command from the arithmetic device 16.

Further, the semiconductor detector 14 is the measurement sample S.
Is arranged at a position symmetrical to the X-ray generator 12 with respect to the normal line of the measurement surface, and when the measurement surface is irradiated with X-rays at an incident angle θ, a diffracted X-ray with a diffraction angle 2θ is generated. Receive light,
It is possible to detect.

The X-ray generator 12 is provided with a divergence slit 20 for narrowing the beam width of the X-rays which irradiate the surface of the measurement sample S. Further, in front of the semiconductor detector 14, a light receiving beam is received. A movable light-receiving slit 22 having a predetermined slit width for the diffracted X-rays and capable of moving its position in parallel while maintaining the light-receiving angle is additionally provided. The light receiving slit 22 is appropriately controlled by the slit controller 24 based on the signal input from the arithmetic unit 16.

The signal detected by the semiconductor detector 14 is input to the arithmetic unit 16 via the preamplifier 26 and the multiple wave height analyzer 28.

In the apparatus of this embodiment described above, the light-receiving slit 22 is controlled so as to move in parallel according to the measurement depth of the measurement sample S. At that time, the movement of the light receiving slit 22 is
Using a pulse motor as a moving means, several μm to several tens of μm
It is supposed to be done at intervals. However, the moving means of the light receiving slit 22 is not limited to the pulse motor.

Next, the method of this embodiment performed by using the above measuring apparatus will be described with reference to the flow charts of FIGS.

First, in order to determine the measurement conditions, the lattice plane (hkl) to be measured is specified, and the constant C,
D, B, the density ρ, and the incident angle θ are input to the arithmetic unit 16 (steps 110 to 114).

Next, the linear absorption coefficient μ (θ) of the sample at the incident angle θ is calculated from the equation (6), and the penetration depth x is calculated from the equations (4) and (5) (step 11
6) The positions A _{1 to} A _n of the light receiving slit 22 are input (step 118), and the measurement depths t ₁ to t _n corresponding to the light receiving slit positions A _{1 to} A _n are calculated from the equation (14). (Step 120). It is judged whether or not the condition of the calculated depth t is appropriate, and if it is inappropriate, the process returns to step 118, the light receiving slit position A is input again, and the measurement depth t is calculated again (step 122, 12
4).

If the condition of the depth t is appropriate, the incident angle θ is set as the measurement condition, and the light receiving slit position A ₁
The X-ray diffraction measurement is started from. At that time, first, A ₁ <A
Confirm that ₂ <... <A _n (step 12)
6).

Next, the goniometer 10 is set to a predetermined incident angle θ (step 128), the position of the light-receiving slit 22 is set (step 130), and then the diffraction X-ray intensity is counted (measured) (step 132). ).

Thereafter, it is judged whether or not the light receiving slit position A is the maximum light receiving slit position A _n (step 13).
4, 136), and if A = A _n is not satisfied, the above step 13 is performed.
Returning to 0, the light receiving slit 22 is set to the next light receiving slit position, and the same operation is executed.

When A = A _n , that is, when the measurement of the X-ray diffraction from the minimum A ₁ of the light receiving slit position to the maximum A _n of the sample S is completed, the disordered orientation having the same composition as the measurement sample S is obtained. Replace with sample (steps 138, 14
0), X-ray diffraction measurement is performed on the sample under the same conditions as the measurement sample S according to steps 130 to 136.

As described above, the diffraction intensity measured at each of the light-receiving slit positions A _{1 to} A _n of the measurement sample S and the disordered orientation sample has the (hkl) plane specified by the multiple wave height analyzer 28. The integrated intensity (peak area) or peak height is read and the result is stored in the arithmetic unit 16.

After all the X-ray diffraction measurement is completed (step 142), the random intensity P _hkl (t at the depth t ₁ -t _n position in the arithmetic unit 16 is calculated from the equation (13).
₁ ) to P _hkl (t _n ) are calculated and predetermined (hkl)
By outputting the orientation distribution in the depth direction of the surface, the measurement of the texture in the depth direction is completed (steps 144, 14).
6).

The measurement conditions and the results when this embodiment was applied to the decarburized / primary recrystallization annealed samples of unidirectional silicon steel sheet are shown in Table 2 for the (110) plane and for the (200) plane. 3 respectively.

[0083]

[Table 2]

[0084]

[Table 3]

Further, FIG. 4 shows the output results of the orientation degree distributions in the depth direction of the (110) plane and the (200) plane when Mo is used as an X-ray target.

From this FIG. 4, it can be seen that according to the present embodiment, even when Mo is used as the X-ray target, no abnormal value is observed in the depth direction.

Further, in FIGS. 5 and 6, using Mo as an X-ray target and using the method of the present invention (slit scan method) and the conventional method (incident angle changing method), α-Fe ( The results of measuring the (200) plane are shown.

As shown in FIG. 6, the conventional method has a depth of 10 μm.
Although abnormal values based on the characteristic X-rays due to the Mo target are seen in the front and rear portions, in the present invention, abnormal values do not occur accurately from the shallow portion (surface) in the depth direction of the steel sheet to the deep portion, and are accurate. It turns out that it is possible to measure.

As described in detail above, according to the present embodiment, the polycrystalline material can be formed in the depth direction at the same position without special processing, that is, nondestructively, in a short time and simply. The degree of crystal orientation of any lattice plane can be obtained with high accuracy.

The present invention has been specifically described above, but the present invention is not limited to the above-mentioned embodiments, and various modifications can be made without departing from the scope of the invention.

For example, when the diffraction intensity is measured by the multiple wave height analyzer 28, the energy window width of the multiple wave height analyzer 28 is set to a necessary minimum so as not to count the fluorescent X-rays from the sample. The semiconductor detector 14
It goes without saying that the detection efficiency of can be improved and the count value reading time can be shortened.

When the fluorescent X-rays from the sample overlap the measured diffracted X-rays, immediately before or after the light-receiving slit 22, and when the characteristic X-rays from the X-ray tube overlap, the divergence slit. A suitable filter may be installed immediately before or after 20.

[0093]

As described above, according to the present invention, the distribution of the degree of crystal orientation of an arbitrary lattice plane in the thickness direction at the same position can be easily obtained in a short time without processing a polycrystalline material. The excellent effect that it can be measured with high reliability is obtained.

[Brief description of drawings]

FIG. 1 is a schematic configuration diagram showing a texture measuring apparatus according to an embodiment of the present invention.

FIG. 2 is a flowchart showing a front part of an embodiment method according to the present invention.

FIG. 3 is a flowchart showing a latter part of the method of the above embodiment.

FIG. 4 is a diagram showing the measurement results of the orientation degree distribution in the depth direction according to the above example.

FIG. 5 is a diagram showing the relationship between the measurement result and the depth by the method of the present invention.

FIG. 6 is a diagram showing a relationship between a measurement result and a depth by a conventional method.

[Explanation of symbols]

 10 ... Goniometer 12 ... X-ray generator 14 ... Semiconductor detector 16 ... Arithmetic device 18 ... Goniometer controller 20 ... Divergence slit 22 ... Movable type light receiving slit 24 ... Movable type light receiving slit controller 26 ... Preamplifier 28 ... Multiplex type Wave height analyzer

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Michio Katayama 1 Kawasaki-cho, Chuo-ku, Chiba-shi, Chiba Kawasaki Steel Corporation Technical Research Division (72) Inventor Yuji Kobayashi 3-9-12 Matsubara-cho, Akishima-shi, Tokyo No. Rigaku Denki Co., Ltd. Haijima Factory (72) Inventor Yoshio Iwasaki 3-9-12 Matsubara-cho, Akishima-shi, Tokyo Rigaku Denki Co., Ltd. Haijima Factory

Claims (3)

[Claims] 1. A texture in the depth direction for irradiating a measurement sample surface with continuous X-rays at a predetermined incident angle and detecting diffracted X-rays at a position symmetrical to the incident X-rays with respect to the normal line of the measurement sample surface. In the above measuring method, the continuous X-rays are irradiated onto the surface of the measurement sample at a predetermined incident angle, and the diffracted X-rays obtained from the incident X-rays are detected at a plurality of light receiving positions at the same light receiving angle, and the energy spectrum Then, the intensity of the diffracted X-ray from the specific lattice plane is determined, and the intensity of the diffracted X-ray from the specific lattice plane is determined under the same conditions for the disordered orientation sample having the same composition as the measurement sample. From the obtained ratio of the diffraction X-ray intensity of the measurement sample to the diffraction X-ray intensity of the disordered sample, a random intensity ratio at a specific depth position corresponding to each of these light receiving positions is calculated. In the direction Method of measuring the depth direction texture and obtains the degree of orientation of the distribution of the specific lattice plane. 2. The method according to claim 1, wherein a predetermined incident angle of the continuous X-ray is set to a characteristic X in the continuous X-ray.
A method for measuring a texture in the depth direction, which is characterized by setting an angle at which a diffracted X-ray based on a line is not received. 3. A goniometer having a function of supporting a measurement sample and adjusting an incident angle of X-rays, an X-ray generator for generating X-rays for irradiating the measurement sample surface, and a normal line of the measurement sample surface. Regarding the above-mentioned X-ray generator, an energy dispersive counter arranged at a position symmetrical to the X-ray generator, and a calculator in the depth direction including a calculator for performing a predetermined calculation based on the diffracted X-ray intensity measured by the energy dispersive counter. A tissue measuring apparatus, wherein the X-ray generator is provided with a divergence slit that limits the beam width of the X-ray with respect to the measurement sample surface, and is parallel to the front of the energy dispersion counter at the same light-receiving angle. A depth direction texture measuring device characterized in that a light receiving slit having a function of moving is provided.