X-ray diffraction apparatus and x-ray diffraction method
Method for structural inspection of semiconductor multilayer structure (variants) / 2442145
FIELD: structural diagnostics.
SUBSTANCE: sample is scanned in the context of the Bragg reflection with the use of Ω-method in the roentgen diffractometry single-step mode, furthermore, for multilayer structures with heterogeneous composition AlGaN/GaN with nanometric layers the roentgen single-crystal diffractometry is used with the power of 5-15 W and heterochromatic quasiparallel X-ray beam and a position-sensitive detector with an angular width of 10°-15°. At first the X-ray tube is fixed in the position of Bragg reflection for the crystallographic plane (0002) of the layer GaNm the samples are scanned via inclining the X-ray tube in the angular range lying on the left and on the right from the main diffraction maximum (0002) of the GaN layer and including all diffraction maximums of AlxGa(1-x)N/GaN structures, where x ranges from 0,1 to 0,9, and the single-step scanning is carried out by setting the X-ray tube consequently in several angular positions which correspond to the maximum reflection of each minor peak point, while recording the diffractogram with the same exposition for all minor peak points, and the exposition time ranges from 30 to 100 seconds.
EFFECT: resolution of interference peaks corresponding to separate nanometric layers of semiconductor structures; use of low-capacity devices becomes possible.
3 cl, 3 tbl, 6 dwg
Adjustable device for irradiation and detecting radiation / 2403560
Method of determining local concentration of residual microstress in metals and alloys / 2390763
Sheet of steel 01x18h9t / 2356992
Sheet of steel 01x18h9t / 2356992
Method of determining local concentration of residual microstress in metals and alloys / 2390763
Adjustable device for irradiation and detecting radiation / 2403560
Method for structural inspection of semiconductor multilayer structure (variants) / 2442145
FIELD: structural diagnostics.
SUBSTANCE: sample is scanned in the context of the Bragg reflection with the use of Ω-method in the roentgen diffractometry single-step mode, furthermore, for multilayer structures with heterogeneous composition AlGaN/GaN with nanometric layers the roentgen single-crystal diffractometry is used with the power of 5-15 W and heterochromatic quasiparallel X-ray beam and a position-sensitive detector with an angular width of 10°-15°. At first the X-ray tube is fixed in the position of Bragg reflection for the crystallographic plane (0002) of the layer GaNm the samples are scanned via inclining the X-ray tube in the angular range lying on the left and on the right from the main diffraction maximum (0002) of the GaN layer and including all diffraction maximums of AlxGa(1-x)N/GaN structures, where x ranges from 0,1 to 0,9, and the single-step scanning is carried out by setting the X-ray tube consequently in several angular positions which correspond to the maximum reflection of each minor peak point, while recording the diffractogram with the same exposition for all minor peak points, and the exposition time ranges from 30 to 100 seconds.
EFFECT: resolution of interference peaks corresponding to separate nanometric layers of semiconductor structures; use of low-capacity devices becomes possible.
3 cl, 3 tbl, 6 dwg
X-ray diffraction apparatus and x-ray diffraction method / 2449262
Method of quantitative determination of portland cement clinker phase composition / 2461817
Method and device for performance of x-ray analysis of sample / 2506570
FIELD: physics.
SUBSTANCE: X-ray diffraction apparatus has a mirror (18), having a reflecting surface (19) which is formed such that the angle in the plane parallel to the diffraction plane between the tangential line (38) of the reflecting surface (19), at any point on the reflecting surface (19), and the linear section (36) which connects any point and a sample (26) becomes constant and the crystal lattice plane which causes reflection is parallel to the reflection surface (19) at any point on the reflection surface (19); the X-ray detector (20) is one-dimensional, position-sensitive in the plane parallel to the diffraction plane; and the relative position of the mirror (18) and the X-ray detector (20) is defined in the plane parallel to the diffraction plane such that reflected X-ray beams (40) from different points on the reflecting surface (19) of the mirror (18) reach different points on the X-ray detector (20), respectively.
EFFECT: improved angular resolution, negligible reduction in X-ray intensity and simple design.
13 cl, 14 dwg
The level of technology
The present invention relates to the installation of x-ray diffraction and x-ray diffraction method of analysis or x-ray diffraction using a parallel beam.
In the method of powder x-ray diffraction of powder samples, thin-film samples or polycrystalline samples, the analyzer should be placed in the optical system from the diffracted beam (i.e. the receiving side of the optical system)to improve the angular resolution for the parallel beam. One of the famous analyzers - long parallel slit having a small angle of aperture of x-rays, and another type of analyzer crystals. How long parallel slit slightly reduces the intensity of x-rays, but bad on the angular resolution. Conversely, with crystal-analyzer better angular resolution, but poor by reducing the intensity of x-ray radiation. So in a way parallel beam it is desirable to have a suitable analyzer, which would be good and on the angular resolution and slightly reduce the intensity of x-ray radiation.
Improvement in the use of the crystal-analyzer prevention and reduction of the radiation intensity in General raskrytb Journal of Synchrotron Radiation (1996), 3, 75-83 (which is referred to hereinafter as the first publication), and Journal of Research of the Natuional Institute od Standards and Technology, 109, 133-142 (2004) (referred to hereinafter as the second publication).
The first publication discloses that a number of (e.g. six) of x-ray detectors are scintillation counters) have around the sample in the way powder diffraction using synchrotron orbital radiation. The crystal-analyzer, made of plates of Ge (111), is placed between the sample and each of the x-ray detectors. The use of multiple x-ray detectors allows short-term measurement of the diffraction pattern with a predefined angular range compared with the case of using a single x-ray detector. Accordingly, the decrease in the intensity of x-rays caused by the use of crystals analyzers, is prevented in the unit as a whole.
The second publication, as well as the first, reveals that many (e.g., nine) crystal analyzers and the same number of x-ray detectors (scintillation counters) in the way powder diffraction positioned around the sample.
The present invention involves using a mirror having a reflective surface in the form of an equiangular spiral (logarithmic the Skye spiral) in the installation of x-ray diffraction using the method of parallel beam. On the other hand, for the installation of x-ray diffraction with the way the focused beam using mirrors (analyzing crystal)having equiangular spiral reflective surface, as disclosed in Japanese Patent publication No. 6-82398 A (1994) (referred to hereinafter as the third publication), Japanese Patent publication No. 7-63897 A (1995) (referred to hereinafter as the fourth publication) and Japanese Patent publication No. 7-72298 A (1995) (referred to hereinafter as the fifth publication).
The third publication discloses the crystal-analyzer, which has a reflective surface in the form of a logarithmic spiral. The crystal-analyzer made of synthetic multilayer gratings, in which the farther from the x-ray source is a point on the reflective surface, the greater is the lattice period. The fourth publication discloses an x-ray spectrometer in accordance with the second variant of realization, which is composed of a combination of flat elements. Each flat element has a reflective dot on the curve, which is almost logarithmic spiral. Each flat element made of a synthetic multilayer gratings, in which the farther from the x-ray source is a point to reflect athelney surface, the greater is the lattice period. The fifth publication discloses the element x-ray spectroscopy in accordance with the fourth alternative implementation, which is composed of a combination of curved reflective surfaces with steps between them, and each reflective surface has a cross-section in the longitudinal direction close to the logarithmic spiral curve. Each reflective surface is made of a synthetic multilayer gratings, in which the farther from the x-ray source is a point on the reflective surface, the greater is the lattice period.
Design, which accommodates multiple crystals analyzers and multiple x-ray detector around the sample, as disclosed in the first and second publications, is so complex and expensive that it is hardly applicable to the method of x-ray diffraction in the laboratory system.
A mirror having a reflective surface with a variable period gratings as disclosed in the third, fourth and fifth publications may not be used as a mirror in a way parallel beam for reflecting the x-ray beam having a different angle of incidence at various locations.
The invention
The present invention is to provide an installation and a method of x-ray diffraction, which is better angular resolution, slightly reduces the intensity of x-rays and simple in construction as compared with prior art that uses a lot of crystals analyzers and the combination of x-ray detectors.
Another objective of the present invention is to provide an installation and a method of x-ray diffraction, which may limit the decrease in the intensity of x-ray radiation while maintaining good angular resolution, even when the width of the incident x-ray beam is relatively high.
To install x-ray diffraction in accordance with the first variant of realization of the present invention parallel x-ray beam falls on the sample and dragirovaniya on the sample x-rays reflected by the mirror using diffraction phenomena, and then are detected by the x-ray detector. The mirror has a reflective surface which is formed so that the angle in a plane parallel to the plane of diffraction, between the tangential line of the reflective surface at any point on the reflective surface, and a line segment connecting any point and the sample became constant, and the plane of the crystal lattice, which causes the reflection was parallel from gateley surface at any point on the reflective surface. X-ray detector is one-dimensional, position-sensitive in a plane parallel to the plane of diffraction. The relative mutual position of the mirror and the x-ray detector is defined in a plane parallel to the plane of diffraction, so that reflected from different points on the reflective surface of the mirror x-rays have reached different points on the x-ray detector, respectively. In the present invention, the shape of the cross section (the shape in a plane parallel to the plane of diffraction) of the reflective surface of the mirror takes the form of a continuously curved line, and the curved reflective surface is suitable for the case when the width of the parallel beam (beam width in the plane of diffraction is small.
The reflective surface of the mirror may preferably take the form of a conformal spiral (also called logarithmic spiral) in a plane parallel to the plane of diffraction, and the middle of the equiangular spiral is located on the surface of the sample.
In the method of x-ray diffraction in accordance with the first embodiment of the present invention, as described above, the installation of x-ray diffraction in accordance with the first embodiment of the invention, the parallel x-ray beam pada is t to the sample and dragirovaniya x-rays from the sample are reflected by the mirror, using diffraction phenomena, and then detected by the x-ray detector. Sign relative to the reflective surface of the mirror, the sign relative to the x-ray detector and the characteristic concerning the relative positional relation of the mirror and the x-ray detector are the same as in the above-described installation of x-ray diffraction in accordance with the first type according to the invention. In addition, various dragirovaniya x-rays having different angles of diffraction, reflected by the mirror and then detected, separately and simultaneously, the x-ray detector.
To install x-ray diffraction in accordance with the second embodiment of the present invention parallel x-ray beam falls on the sample and dragirovaniya x-rays from the sample are reflected by mirror using diffraction phenomena, and then detected by the x-ray detector. The mirror has a reflective surface consisting of a combination of plural flat reflective surfaces, which are arranged so that the angle in a plane parallel to the plane of diffraction, between each flat reflective surface and a line segment connecting the center of each flat reflective on top of the spine and obrazac, became a regular among all flat reflective surfaces, and the plane of the crystal lattice, which causes the reflection in each flat reflective surface is parallel to each flat reflective surface. X-ray detector is one-dimensional, position-sensitive in a plane parallel to the plane of diffraction. Relative location of the flat reflective surfaces and x-ray detector is defined in a plane parallel to the plane of diffraction so that the reflected x-rays, which are reflected various flat reflective surfaces, reached different points on the x-ray detector, respectively.
The respective centers of the flat reflective surfaces can preferably be located in a plane parallel to the plane of diffraction, equiangular spiral, having a center which is located on the surface of the sample.
In the method of x-ray diffraction in accordance with the second embodiment of the present invention, as for the above described installation of x-ray diffraction in accordance with the second embodiment of the invention, the parallel x-ray beam falls on the sample, and dragirovaniya x-rays from the OBR is SCA reflected by the mirror, using diffraction phenomena, and then detected by the x-ray detector. Sign relative to the reflective surface of the mirror, the sign relative to the x-ray detector and the characteristic concerning the relative positional relation of the mirror and the x-ray detector are the same as in the above-described installation of x-ray diffraction in accordance with a second embodiment of the invention. In addition, various dragirovaniya x-rays having different angles of diffraction, reflected by the mirror and then detected separately and simultaneously, the x-ray detector.
The first and second embodiments of the present invention have the advantage that the combination of the crystal-analyzer having a reflective surface with a predefined shape, and the only one-dimensional, position-sensitive x-ray detector gives the best angular resolution, a smaller decrease in the intensity of x-rays and simple design compared with the technique of the prior art to use multiple crystals analyzers.
In addition, a second variant implementation of the present invention has the advantage that even when the width of the x-ray beam, which pad is t to the sample, relatively high, the use of mirrors, having the form, based on a new mathematical equation, prevents the decrease in angular resolution, caused by the x-ray aberration, and prevents a decrease in the intensity of x-ray radiation, so that was achieved and the best angular resolution, and a greater gain in the intensity of x-ray radiation.
Brief description of figures
Figure 1 depicts a schematic perspective view of the installation of x-ray diffraction in accordance with the first embodiment of the present invention;
Figure 2 is a view in plan of the installation of x-ray diffraction, is shown in figure 1;
3 is an explanatory illustration for explaining how to obtain the shape of the reflective surface of the mirror, and the corresponding mathematical equations;
4 is an explanatory illustration of a shape of the reflective surface of the mirror and the corresponding mathematical equations;
5 is an explanatory illustration indicating the trajectory of x-rays after their reflection mirror, and the corresponding mathematical equations;
6 is an explanatory illustration indicating the positioning of the mirror and the x-ray detector, and the corresponding mathematical equations;
7 is a schematic perspective view of a modified optical is the first installation of x-ray diffraction, shown in figure 1;
Fig - schematic perspective view of another modified optical system installation x-ray diffraction, is shown in figure 1;
Fig.9 is a schematic perspective view of the installation of x-ray diffraction in accordance with the second embodiment of the present invention;
Figure 10 is a view in plan of the installation of x-ray diffraction, is shown in Fig.9;
11 is an explanatory illustration of mirrors consisting of plural flat reflective surfaces, and the corresponding mathematical equations;
Fig - modification, in which the centers of the flat reflective surfaces are shifted from the equiangular spiral;
Fig - schematic perspective view of a modified optical system installation x-ray diffraction, is shown in Fig.9; and
Fig - schematic perspective view of another modified optical system installation x-ray diffraction, is shown in Fig.9.
Detailed description of preferred embodiments of the invention
Below are detailed embodiments of the present invention in conjunction with the relevant drawings. Figure 1 shows a schematic perspective view of the installation of x-ray diffraction in accordance with the first embodiment according to the present image is the shadow. Installation of x-ray diffraction contains the x-ray source having a linear (or point) focus 10 tubes x-ray multilayer mirror 12 having a parabolic reflective surface, the monochromator 13 allocation of the channel to select the characteristic lines Kα1 x-ray radiation, the holder 14 of the sample, the slit 16 Soller to limit the vertical divergence of the diffracted x-rays, a mirror 18, is designed as a crystal analyzer, and a one-dimensional position-sensitive x-ray detector 20. Figure 1 shows the case of using a linear focus x-ray radiation. Diverging beam 22, which consists of x-rays emitted from focus 10 x-ray radiation is converted into a parallel beam 24a multilayer mirror 12 having a parabolic reflective surface. Multilayer mirror 12 is optimized for the wavelength of x-ray radiation (CuKαl in this embodiment) and has a gradient lattice period. Focus 10 x-ray radiation is placed in the position of the parabolic focus multilayer mirror 12. Assuming the linear focus x-ray tube, for example, focus 10 x-ray emission is elongated in the vertical direction approximately des is th millimeters. Parallel beam 24a passes through the monochromator 13 highlight a channel, and the resulting parallel beam 24 x-ray radiation (incident x-ray beam falls on the sample 26. The width of the parallel beam 24a and parallel beam 24 in the horizontal plane is approximately 0.84 mm. Sample 26 is powdered, and the recess of the holder 14 of the sample filled in the sample 26. Dragirovaniya x-rays 28 out of the sample 26. Dragirovaniya x-rays 28 are limited vertical divergence slit 16 Soller.
Sample 26 is not limited to powder, but may be polycrystalline substance (metal etc), thin-film sample on a substrate, and can be used filamentary sample. For the so-called reflective x-ray diffraction analysis can be used any sample holder. In addition, can be used as a sample holder for x-ray diffraction analysis on missing: for example, as shown in Fig.7, the sample can be filled capillary tube 15.
On Fig shows a modified optical system installation x-ray diffraction, is shown in figure 1. A modified version of the implementation is different from the setup shown in figure 1, so that the optical system from falling pooch is and there is no monochromator highlight a channel, and the multilayer mirror 12 is optimized for use in this embodiment, the wavelength of the x-ray radiation (CuKα in this implementation, i.e. the doublet CuKαl and CuKα2).
Returning again to figure 1, the plane which includes the incident x-rays 24 and dragirovaniya x-rays 28, usually referred to as the plane of diffraction, or Equatorial plane. In this description, the plane which includes the incident x-rays 24 and dragirovaniya x-rays 28, is defined as the plane of diffraction. The divergence of the x-ray radiation in the plane of diffraction is usually called the Equatorial divergence, or radial divergence. In this description, the divergence in the plane of diffraction is called horizontal divergence, whereas the divergence in the plane perpendicular to the plane of diffraction is vertical divergence. In the optical system shown in figure 1, the plane of diffraction is in the horizontal plane, and the focus 10 x-rays mounted vertically, and the surface of the sample 26 is also mounted vertically.
The slit 16 Soller limits the vertical divergence. The horizontal divergence in the way the parallel beam, which directly affects the resolution of the detected angle DEFRA the tion, strictly limited and mirror 18 that will be described later, and the monochromator 13 allocation of the channel described above. The mirror 18 is a key component in the present invention, which guarantees the best possible angular resolution of the diffracted x-rays 28: this topic will be discussed in detail later. The approximate size of the mirror 18 is in the range between 15 and 20 millimeters in height and between 60 and 80 mm in length. The mirror 18 is slightly curved relative to the plane. The monochromator 13 allocation of channel uses the plane (220) lattice Ge, if the x-ray target Cu is used.
One-dimensional, position-sensitive x-ray detector 20 uses silicon strip detector (SSD) in this embodiment. The detector is a one-dimensional, position-sensitive in a plane parallel to the plane of diffraction. That is, one plane of the detector in the vertical direction forms a single channel detector, and there are many adjacent channels (for example, 128 channels)arranged in the horizontal direction. The size of a single channel, for example, is 0.1 mm in width and 15 mm in length (figure 1 - height).
Figure 2 shows a view in plan of the installation of x-ray diffraction, is shown in figure 1. The angle between the incident x the ski rays 24 and dragirovaniya x-rays 28 is 2θ. The angle θ is the Bragg angle x-ray diffraction for the sample 26. When measuring a diffraction pattern with a predefined angular limits using this installation of x-ray diffraction sample holder 14 and the reception optical system 30 are rotated synchronously to maintain the ratio between the angle ω of the fall of the x-ray radiation 24 to the surface of the sample 26 and the angle 2θ, above, as the ratio of 1 to 2. Picture of x-ray diffraction arising from sample 26 thus detected. Reception optical system 30 consists mainly of slits 16 Soller (see figure 1, figure 2 not shown), the mirror 18 and the x-ray detector 20, and these optical components are mounted on the receiving branches (not shown) of the system. Reception optical system 30, in accordance with the designation by the arrow 34, is able to rotate around the center of the goniometer (point O). The surface of the sample 26 is located at the center of the goniometer (point O).
Because the installation of x-ray diffraction method uses a parallel beam, suitable and different way of measuring, which does not support the relationship between ω and 2θ as the ratio 1 to 2. Namely, when the diffraction pattern is measured in predetermined angular limits, the holder 14, the sample can be fixed to maintain a constant angle ω of the fall of the rent is Nevskogo radiation 24 to the surface of the sample 26. Although dragirovaniya x-rays 28 from the sample 26 extend in different directions depending on the Bragg angles, these dragirovaniya x-rays 28 can be detected using the rotation of the receiving optical system 30.
Below describes in detail the shape of the reflective surface of the mirror 18. The mirror 18 is formed slightly curved thin single-crystal plate. In this embodiment, the mirror 18 is made of single crystal Ge, so that Ge (111) plane is parallel to the surface of the mirror. The mirror reflects, through the phenomena of diffraction, dragirovaniya x-rays from the sample. The plane of the Ge (111) corresponds to the plane of the crystal lattice, which causes diffraction.
Regarding figure 3, the reflective surface 19 of the mirror has the shape of an equiangular spiral (also called logarithmic spiral) in a plane parallel to the plane of diffraction. Figure 3 shows a view in a plane parallel to the plane of diffraction. Sign equiangular spiral that the angle θ0between the tangential line 38 at any point (x, y) on the equiangular spiral and linear segment 36, which connects any point (x, y) and the center of the spiral (point O)is constant at any point on the spiral. This is the reason why the spiral is called "RA is naugolnoe" spiral. The angle θ0is set equal to the Bragg angle for Ge (111) and used for wavelength x-ray radiation. In this embodiment, the mirror is made for CuKαl and, thus, the angle θ0is 13,64 degrees. Dragirovaniya x-rays (dragirovaniya on the sample)emanating from the point O to the reflective surface, falling on the reflective surface 19 at an angle of incidence θ0to the tangential line 38 of the reflective surface 19 at any point falling on the reflective surface so that dragirovaniya x-rays always satisfy the Bragg condition. Similarly reflected by reflective surface 19 of the x-rays 40, extend at an angle θ0to the tangential line 38.
The shape of the reflective surface 19 of the mirror can be determined as described below. Regarding figure 3, the center of the goniometer (point O) is defined as the beginning of the x-y coordinate system. The sample surface is located at the point O and the center of the equiangular spiral is also located at point O. it is Assumed that the Central region of the reflective surface 19 is located at the point x=r on the x-axis. When dragirovaniya x-rays 36 extend in a direction at an angle ϕ (in counterclockwise direction) to the x-axis, dragirovaniya x-rays 36 reach t is his (x, y) on the reflective surface 19. Dragirovaniya x-rays 36 can be displayed in equation (1) in figure 3, i.e. the coordinates (x, y) of each point on the trajectory diffracted x-rays satisfy equation (1). Namely, the y-coordinate of the diffracted x-rays, that is, yDBexpressed through the angle ϕ and the x-coordinate.
The slope dy/dx of the reflective surface 19 at the point (x, y) is expressed by equation (2). Equation (2) can be transformed into equation (5) using equations (3) and (4). Equation (3) expresses the relationship between x-y coordinates at the point (x, y) and at an angle ϕ. Equation (4) determines the tangent of the Bragg angle θ0mirror as "a". Equation (5), which is the differential equation is solved to obtain equation (6), which is converted to equation (7).
The ratio shown in equation (8) in figure 4, is applied to equation (7) in figure 3, and the resulting equation is converted to obtain equation (9) figure 4. Equation (9) expresses the x-coordinate of any point (x, y) on the reflective surface 19. Thus, the x-coordinate can be calculated using the distance r, the angle ϕ and the Bragg angle θ0. The combination of equations (9) and (3) leads to equation (10), which gives the y-coordinate. The combination of equations (9) and (10) determines the shape of the reflective surface is 19 mirrors.
Regarding figure 4, how reflective surface of the mirror 19 is curved, will be calculated below. Assuming that r is 200 mm, the distance Δ in the y-direction between the tangential line 38 (which is a straight line) of the reflective surface 19 in the center (200, 0) of the reflective surface 19 and the reflective surface 19 (which is a curved line) can be calculated as described below. The equation of the tangent line 38 is expressed by equation (11) figure 4. Y-coordinate in the tangential line is defined as ytan. On the other hand, the y-coordinate of the reflective surface 19 is expressed by equation (10). Shown below table 1 above indicates the distance Δ, which is calculated using the angle ϕ as a parameter. For example, when ϕ is two degrees, the x-coordinate on the reflective surface 19 is 173,099 mm, and the y-coordinate - 6,045 millimeters. Y-coordinate in the tangential line 38 when the same x-coordinate, that is, ytanis 6,528 millimeters. Accordingly, subtracting the y-coordinates of the reflective surface 19 of the y-coordinates of the tangential line 38 gives 0,483 of a millimeter, which is the distance Δ. Similarly, the Table also shows the values of Δ for φ, which is one degree, zero degrees, and a negative one degree, and Autry is atelinae two degrees. Since the y-coordinate of the reflective surface 19 is always less than the y-coordinate of the tangent line when ϕ increases and decreases from zero degrees, it is clear that the reflective surface 19 is curved to be concave down.
| Table 1 | ||||
| ϕ (°) | 2 | 1 | 0 | -1 | -2 |
| x (mm) | 173,099 | 186,092 | 200 | 214,882 | 230,801 |
| (mm) | 6,045 | 3,248 | 0 | -3,751 | -8,060 |
| ytan(mm) | 6,528 | 3,375 | 0 | -3,611 | -7,474 |
| Δ (mm) | 0,483 | to 0.127 | 0 | 0,140 | 0,586 |
The following describes the trajectory of x-rays that have been reflected by a reflective surface. Regarding figure 5, dragirovaniya x-rays 36, which extend from a point O in a direction with an angle ϕ, is reflected at the point (x, y) on the reflective surface 19, forming a reflected x-rays 40. On the other hand, dragirovaniya x-rays, which extend from a point On the x-axis, is reflected at the point on the reflective surface 19, and point C is the intersection point of the reflective surface 19 and the x-axis, forming the reflected x-rays 42. The reflected x-rays 42, which are reflected at the point C, called the Central beam 42. The reflected x-rays 40, which are reflected at any point (x, y), the corresponding angle ϕ, soon intersect with the Central beam 42. The intersection point is defined as the point P. the Distance between point C and point P is defined as t.
Regarding figure 5, the reflected x-rays 40, which are reflected at any point (x, y), the corresponding angle ϕ, described by equation (13). Character As in equation (13) is defined in equation (12). The Central beam 42 is described by equation (14). The intersection point P has coordinates that satisfy both equations (13) and (14) simultaneously, and p is that the x-coordinate which satisfies both equations gives x-coordinate of the point P, that is, xPwhich is expressed by equation (15). Y-coordinate of the point P, that is, yPmay be calculated, for example, by substituting the obtained value of xPin equation (14).
Shown below table 2 indicates the coordinates (xP, yP) the point P and the distance t, which is calculated using the angle ϕ as a parameter, provided that r is 200 mm and θ0- 13,64 degrees. Clearly, in accordance with Table 2 that each of the reflected x-ray beam intersects the Central beam in place, approximately 200 mm apart from the center (point C) of the reflective surface of the mirror. Accordingly, for separate detection of various reflected x-rays reflected at different points on the reflective surface with a position-sensitive x-ray detector, you want to place a position-sensitive x-ray detector somewhere between point C and point P. In this embodiment, it is preferable to place the position-sensitive x-ray detector in place, remote approximately 50-100 mm from point C.
| Table 2 | ||||
| ϕ°) | 2 | 1 | 0,5 | 0,1 | 0,01 |
| xp(mm) | 353,37 | 365,27 | 371,44 | 376,48 | 377,63 |
| yp(mm) | -79,09 | -85,23 | -88,41 | -91,01 | -91,60 |
| t (mm) | 172,56 | 185,95 | 192,89 | 198,56 | 199,86 |
| ϕ(°) | -0,01 | -0,1 | -0,5 | -1 | -2 |
| yp(mm) | 377,88 | 379,04 | 384,23 | 390,85 | 404,60 |
| xp(mm) | -91,73 | -92,33 | -95,01 | -98,42 | -105,51 |
| t (mm) | 200,14 | 201,45 | 207,29 | 214,73 | 230,20 |
Below describes the function of the angular separation between the position-sensitive x-ray detector. Regarding 6, the plane of the detection of the position-sensitive x-ray detector 20 is removed from the center (point C) of the reflective surface 19 of the mirror at a distance d. The plane of the detector is almost perpendicular to the Central beam 42. Reflected from the point (x, y) of the x-ray beam 40 having an angle ϕ, reaches the point Q on the plane of the detector. The Central beam 42 from point reaches point M in the plane of the detector. The distance between the point Q and the point M is denoted as s. Various reflected x-rays coming from multiple different points on the reflective surface of the mirror, reach multiple different points on the x-ray detector, respectively.
Coordinates (xm, ympoint M is expressed by equation (16) figure 6. The equation of the straight line 44, so the overall plane of the detector, is expressed by equation (17). Point Q is the intersection point of the straight line 44 with the reflected x-ray beam 40. Since the straight line 44 is given by equation (17) figure 6, whereas the reflected x-ray beam 40 is given by equation (13) in figure 5, the coordinates (xq, yq) the point Q can be obtained by solving these two equations, the resulting equations (18) and (19). The distance s between the points Q and M can be calculated using equation (16), expressing the coordinates of the point M, and equations (18) and (19)expressing the coordinates of the point Q, leading to equation (20).
Shown below table 3 indicates the distance s in the plane of the detector, which is calculated using the angle ϕ as a parameter, provided that r is 200 mm, θ0- 13,64 C and d - 50 mm. When ϕ is two degrees, the point Q is the distance 4,28 millimeters from the point M, and when ϕ is two negative degrees, the point Q is at a distance of 6.29 mm from the point M in the opposite direction. Accordingly, assuming that dragirovaniya x-rays captured by the mirror between positive and negative two degrees in 2θ, i.e. in the range between positive and negative two degrees in φ, the lateral size of the detector should be at least about ten mill the meters, when the detector is placed at a point on the 50 mm distance d. If the area in ten millimeters divided by one hundred channels, for example, that is 0.1 mm on one channel, dragirovaniya x-ray beam is detected with a positional resolution of about 0.04 degrees in the range of four degrees 2θ. It should be noted that since the variation of the angle ϕ (i.e. variation 2θ) is not proportional to the variation of s on the plane of the detector, the characteristic curve of variation of s depending on ϕ must be obtained from equation (20) figure 6, so that it is determined which channel detector receives x-ray radiation in this angular range φ.
| Table 3 | ||||
| ϕ (°) | 2 | 1 | 0,5 | 0,1 | 0,05 |
| s (mm) | 4,28 | 2,37 | 1,25 | 0,259 | 0,130 |
| ϕ (°) | 0,04 | 0,03 | 0,02/td> | 0,01 |
| s (mm) | 0.104 g | 0,078 | 0,052 | 0,026 |
| ϕ (°) | -0,01 | -0,02 | -0,03 | -0,04 | to-0.05 |
| s (mm) | 0,026 | 0,053 | 0,079 | 0,105 | 0,132 |
| ϕ (°) | -0,1 | -0,5 | -1 | -2 |
| s (mm) | 0,264 | 1,37 | 2,88 | 6,29 |
As can be seen from Fig.6, in accordance with the present invention, multiple different dragirovaniya x-rays having different angles of diffraction can be yourself separately and simultaneously through the mirror when stationary one-dimensional position-sensitive x-ray the portion of the detector 20. Thus, since different dragirovaniya x-rays having different angles of diffraction can be yourself at the same time, the detected intensity of x-ray radiation can be increased compared with the case where only dragirovaniya x-rays with a single diffraction angle detected immediately using conventional crystal analyzer. Therefore, the present invention allows relatively rapid measurement of the diffraction pattern, even with the use of crystal-analyzer. It should be noted, however, that when the x-ray detector remains stationary during the measurement, the angle of coverage is limited to within approximately four degrees 2θ, for example. So to get a picture of powder diffraction in a wider angular range, the reception optical system 30 must be rotated, as shown in figure 2.
Below describes how to install x-ray diffraction in accordance with the second embodiment of the present invention. Figure 9 shows a schematic perspective view of the installation of x-ray diffraction in accordance with the second embodiment of the present invention. Installation of x-ray diffraction of the second variant implementation, shown in Fig.9, differs in the form of mirror 60 from the mouth of the unit x-ray diffraction of the first variant implementation, shown in figure 1. The configuration of the second variant of implementation, except for the mirrors, the same as the configuration of the first variant implementation, shown in figure 1. Figure 10 shows in plan the installation of x-ray diffraction, is shown in Fig.9.
The shape of the reflective surface of the mirror 60 is described in detail below. The mirror 60 is configured to combine the plural flat reflective surfaces 62. In this embodiment, the selective mirror that is each flat reflective surface 62, is made of single crystal Ge, and formed so that the plane of the Ge (111) was parallel planar reflective surface 62 selective mirrors. Each of the selective mirror is used to reflect through the phenomena of diffraction, and dragirovaniya x-rays coming from the sample. The plane of the Ge (111) corresponds to the plane of the crystal lattice, which causes diffraction.
Many flat reflective surfaces 62 are improving one curved reflective surface. The main curve of the reflective surface has the shape of an equiangular spiral in a plane parallel to the plane of diffraction, i.e. the form considered in connection with the above 3 and 4.
The following describes the procedure for creating plural is i.i.d. flat reflective surfaces by dividing one curve of the reflective surface. Figure 11 shows only three flat reflective surfaces 62a, 62b and 62c mirror, which consists of a combination of plural flat reflective surfaces 62. The centers of the flat reflective surfaces are located on the above equiangular spiral. Tangential line equiangular spiral in the supposed center of each flat reflective surface itself becomes flat reflective surface. Considering the i-th planar reflective surface 62b, for example the center (point Ci) is a flat reflective surface 62b is at an angle φito the x-axis. Length of the flat reflective surface 62b is designated as Li. The angular range of the diffracted x-rays covered flat reflective surface 62b is δϕi. The angle between diregiovani x-rays propagating towards the center (point Ci) is a flat reflective surface 62b, and diregiovani x-rays propagating towards the center (point Ci+1) adjacent planar reflective surface 62a is Δϕi. Detected width, which reflected a flat reflective surface 62b of x-rays fall on the plane of the detector 20 of x-ray radiation, denoted as Wi.
The equation of the straight line i-the flat reflective surface 62b is expressed by equation (21) figure 11. Symbol Andiis determined by equation (22).
The method for dividing the equiangular spiral can use a variety of installation conditions. Shown below table 4 indicates three conditions. The first condition is that the captured angular limits δϕ respective flat reflective surfaces are equal. In this case, the length L of the mirrors are different from each other, and also detected width W that is mapped to a respective flat reflective surfaces different from each other. The second condition is that the length L of the mirrors of the respective flat reflective surfaces are equal. In this case, the captured angular limits δϕ respective flat reflective surfaces are different from each other, and also detected width W that is mapped to a respective flat reflective surfaces different from each other. The third condition is that the detected width W that is mapped to a respective flat reflective surfaces are equal. In this case, the captured angular limits δϕ respective flat reflective surfaces are different from each other, and also the length L of the mirrors are different from each other.
| Table 4 | ||
| The angular limits | The length mirrors | Detected width |
| The first condition | δϕ1=δϕ2=...=δϕN=δϕ | L1>L2>...>LN | W1>W2>...>WN |
| The second condition | δϕ1<δϕ2<...<δϕN | L1=L2=...=LN=L | W1>W2>...>WN |
| The third condition | δϕ1<δϕ2<...<δϕN | L1<L2<...<LN | W1=W2=...=WN=W |
Shown below table 5 shows a specific example of the mirror, consisting of a combination of eleven flat reflective surfaces in the above-mentioned third condition, in which the detected width W in the plane of the detector are equal. These calculated values are based on the condition that the size of a single channel x-ray detector is 0.1 mm, and the detector has 128 channels. The table indicates that h is detected on the width W (s in Table 5), corresponding one flat reflective surface is 1,1636 mm. Real device, based on a specific example is described below. Assuming that W is 1.1 mm, the width of one channel of the x-ray detector is 0.1 mm, and the detector has 121 channel, one channel group, consisting of eleven channels must be mapped to a single flat reflective surface. The reflected x-rays that have been reflected in the center of each flat reflective surface, reaching the point Q (see Fig.6) in the plane of the detector, and the coordinates of point Q are (xp, yp). The angle (x-axis) diffracted x-rays, extending to the center of each flat reflective surface is φ. The distance between the point Q and the center M of the plane of the detector is indicated as s (see Fig.6). The numerical values in figure 5 are calculated under the condition that r is 200 mm, θ0- 13,64 C and d - 50 millimeters.
| Table 5 | |||
| No. | s (mm) | xq(mm) | yq(mm) | ϕ(°) |
| 1 | -5,8182 | 247,1055 | -17,7459 | -1,8705 |
| 2 | -4,6545 | 246,5722 | -18,7801 | -1,5411 |
| 3 | -3,4909 | 246,0389 | -19,8144 | -1,1928 |
| 4 | -2,3273 | 245,5055 | -20,8486 | -0,8227 |
| 5 | -1,1636 | 244,9722 | -21,8828 | -0,4268 |
| 6 | 0,0000 | 244,4388 | -22,9170 | 0,0000 |
| 7 | 1,1636 | 243,9055 | -23,9512 | 0,4650 |
| 8 | 2,3273 | 243,3722 | -24,9854 | 0,9786 |
| 9 | 3,4909 | 242,8388 | -26,0196 | 1,5572 |
| 10 | 4,6545 | 242,3055 | -27,0539 | 2,2291 |
| 11 | 5,8182 | 241,7721 | -28,0881 | 3,0516 |
Shown below table 6 indicates a specific example of a flat reflective surface, the mirror consists of a combination of eleven flat reflective surfaces, when the condition shown in the above figure 5. The angle φ represents the angle at the center of each flat reflective surface. Coordinates (x, y) is shown for the center and both edges of each flat reflective surface. For example, with respect to the first flat reflective surface, the x-coordinate of the center is 228,6781 mm, and the negative y-coordinate -7,4681 mm, the x-coordinate of one end is 231,3450 mm, and the negative y-coordinate - 8,2081 mm, and the x-coordinate of the other end is 226,0113 millimeters, and the negative y-coordinate - 6,7281 mm. The symbol L shows the length of each flat reflective surface is I. Symbol Δϕ displays the angle between the centers of two adjacent planar reflective surfaces. Full length eleven flat reflective surfaces is approximately 80 millimeters.
| Table 6 | ||||
| No. | ϕ(°) | Δϕ(°) | x(mm) | y(mm) | L(mm) |
| 231,3450 | -8,2081 | |||
| 1 | -1,8705 | 228,6781 | -7,4681 | 5,5352 |
| 0,3294 | 226,0113 | -6,7281 | ||
| 2 | -1,5411 | 223,3621 | -6,0091 | 5,6007 |
| 0,3483 | 220,6060 | -5,2614 | ||
| 3 | -1,1928 | 217,8684 | -4,5363 | 5,7905 |
| 0,3701 | 215,0085 | -3,7789 | ||
| 4 | -0,8227 | 212,1693 | -3,0467 | 6,0108 |
| 0,3959 | 209,1881 | -2,2778 | ||
| 5 | -0,4268 | 206,2291 | -1,5363 | 6,2748 |
| 0,4268 | 203,1015 | -0,7526 | ||
| 6 | 0,0000 | 200,0000 | 0,0000 | 6,5945 |
| 0,4650 | 196,6929 | 0,8026 | ||
| 7 | 0,4650 | 193,4158 | 1,5696 | 6,9972 |
| 0,5136 | 189,8799 | 2,3974 | ||
| 8 | 0,9786 | 186,3800 | 3,1836 | 7,5238 |
| 0,5786 | 182,5391 | 4,0466 | ||
| 9 | 1,5572 | 178,7427 | 4,8592 | 8,2571 |
| 0,6719 | 174,4649 | 5,7750 | ||
| 10 | 2,2291 | 170,2446 | 6,6267 | 9,3902 |
| 0,8225 | 165,2603 | 7,6327 | ||
| 11 | 3,0516 | 160,3596 | 8,5488 | 9,9712 |
| 155,4589 | 9,4649 | |||
| The total number of | 77,9460 | |||
Mirror consisting of a combination of flat reflective surfaces, has the following advantage compared with a curved mirror having a shape conformal spiral. Using a curved mirror, one channel can accept, in principle, not only imageavenue x-rays, having given angle 2θ, but also other dragirovaniya x-rays with different angles within a small angular range, if the channel width of the detector is not infinitely narrowed. Conversely, using a mirror, consisting of a combination of many flat reflective surfaces, a certain group of channels mapped to a flat reflective surface, takes dragirovaniya x-rays having the same angles of diffraction, so that the resulting angular resolution was increased to the angular resolution of the crystal-analyzer.
On Fig shows a modification in which the coordinates of the centers of the respective flat reflective surfaces are shifted from the equiangular spiral. It is assumed, for example, that the centers C1C2and C3three flat reflective surfaces, 62d, 62e and 62f, are located on the same equiangular spiral. When the Central flat reflective surface 62e is slightly moved in the direction of propagation of the diffracted x-rays 56, a flat reflective surface 62e is shifted while maintaining its inclination so that its center C2moved to C2a. Even with the transfer of the angle of a flat reflective surface 62e for the diffracted x-ray radiation 56 is retained as is, and therefore d is mahiravana x-ray radiation 56 is reflected by a flat reflective surface 62e. Right flat reflective surface 62f similarly moved so that the center C3 shifted to C3Aand the distance it transfer more than to the Central flat reflective surface 62e. Even if plural flat reflective surfaces are shifted sequentially, as mentioned above, the resulting combined mirror can properly reflect dragirovaniya x-rays, although the point of detection of the reflected x-rays on the plane of the detector is also shifted along with the shift of flat reflective surfaces. Accordingly, if a large plane detection, shown in Fig modification is preferred.
On Fig shows a modification using a sample holder for x-ray diffraction analysis to allow the installation of x-ray diffraction, shown in Fig.9, in accordance with the second type of the present invention, as well as for the modification shown in Fig.7. For example, the capillary tube 15 may be filled with the pattern.
On Fig shows a modified optical system installation x-ray diffraction, shown in Fig.9, in accordance with the second embodiment of the present invention, as well as for the modification shown in Fig. Modi is economony embodiment differs from the installation, shown in Fig.9, in which the monochromator allocation is not transmitted from the input side optical system, and a multilayer mirror 12 is optimized for use in this embodiment, the wavelength of the x-ray radiation (CuKα1 in this embodiment, i.e. the doublet CuKαl and CuKα2). Although the above description discusses the case when the focus of the x-ray tube is a linear focus, the present invention can be applied to a point focus.
10 the focus of the x-ray tube radiation
12 multilayer mirror
13 monochromator allocate channel
14 the sample holder
16 slit Soller
18 the mirror
19 reflective surface
20 the x-ray detector
22 diverging beam
24a parallel beam
24 parallel beam of incident x-rays)
26 sample
28 dragirovaniya x-rays
30 reception optical system
40 reflected x-rays
60 mirror
62 is a flat reflective surface
Equations used in the variants of implementation of the present invention:
mirror (18) has a reflective surface (19)which is formed so that the angle in a plane parallel to the plane of diffraction, between the tangential line (38) of the reflective surface (19) at any point on the reflective surface (19) and the line segment (36)connecting any point and the sample (26), became permanent, and the plane of the crystal lattice, which causes the reflection is parallel to the reflective surface (19) at any point on the reflective surface (19);
x-ray detector (20) is one-dimensional, position-sensitive in a plane parallel to the plane of diffraction; and
the relative mutual position of the mirror (18) and x-ray detector (20) is defined in a plane parallel to the plane of diffraction so that the reflected x-rays (40) from different points on the reflective surface (19) of the mirror (18) reached different points on the detector (20) x-ray radiation, respectively.
2. Installation of x-ray diffraction according to claim 1, to the second reflective surface (19) of the mirror (18) has the shape of an equiangular spiral in the plane parallel to the diffraction plane, and the Central equiangular spiral is located on the surface of the sample (26).
3. The method of x-ray diffraction, in which a parallel x-ray beam (24) onto the sample (26), and dragirovaniya x-rays (28) from a sample (26) reflected by the mirror (18)using diffraction phenomena, and then detected by a detector (20) x-ray radiation, characterized in that:
mirror (18) has a reflective surface (19)which is formed so that the angle in a plane parallel to the plane of diffraction, between the tangential line (38) of the reflective surface (19) at any point on the reflective surface (19) and the line segment (36)connecting any point and the sample (26) became constant, and the plane of the crystal lattice, which causes the reflection is parallel to the reflective surface (19) at any point on the reflective surface (19);
x-ray detector (20) is one-dimensional, position-sensitive in a plane parallel to the plane of diffraction;
the relative mutual position of the mirror (18) and a detector (20) x-ray radiation is defined in a plane parallel to the plane of diffraction, so that the reflected x-rays (40) from different points on the reflective surface (19) of the mirror (18) was achieved according to CNAE point on the detector (20) x-ray radiation, respectively; and
various dragirovaniya x-rays (28)having different angles of diffraction, reflected by the mirror (18) and then detected separately and simultaneously by the detector (20) x-ray radiation.
4. The method of x-ray diffraction according to claim 3, in which the reflective surface (19) of the mirror (18) has the shape of an equiangular spiral in a plane parallel to the plane of diffraction, and the Central equiangular spiral is located on the surface of the sample (26).
5. Installation of x-ray diffraction, in which a parallel x-ray beam (24) onto the sample (26), and dragirovaniya x-rays (56) from a sample (26) reflected by the mirror (60)using diffraction phenomena, and then detected by a detector (20) x-ray radiation, characterized in that:
mirror (60) has a reflective surface consisting of a combination of flat reflective surfaces (62), which are located so that the angle in a plane parallel to the plane of diffraction, between each flat reflective surface (62) and a line segment connecting the center of each flat reflective surface and the sample (26)becomes constant for all flat reflective surfaces (62), and the plane of the crystal lattice, which causes the reflection in each flat reflective surface (62),is parallel to each flat reflective surface (62);
x-ray detector (20) is one-dimensional, position-sensitive in a plane parallel to the plane of diffraction; and
relative location of the flat reflective surfaces (62) and a detector (20) x-ray radiation is defined in a plane parallel to the plane of diffraction, so that the reflected x-rays that have been reflected various flat reflective surfaces (62), reached different points on the detector (20) x-ray radiation, respectively.
6. Installation of x-ray diffraction according to claim 5, in which the respective centers of the flat reflective surfaces (62) are located in a plane parallel to the plane of diffraction, equiangular spiral, having a center located on the surface of the sample (26).
7. Installation of x-ray diffraction according to claim 5, in which the center of at least one of the flat reflective surfaces (62) is shifted in a plane parallel to the plane of diffraction, from the point at equiangular spiral having a center located on the surface of the sample (26).
8. Installation of x-ray diffraction according to claim 5, in which the limits of the angular coverage of the respective flat reflective surfaces (62) are equal.
9. Installation of x-ray diffraction according to claim 5, in which the mirror length L of the respective flat from artelinic surfaces (62) are equal.
10. Installation of x-ray diffraction according to claim 5, in which the width W of the detection in accordance with the relevant flat reflective surfaces (62), are equal.
11. The method of x-ray diffraction, in which a parallel x-ray beam (24) onto the sample (26) and dragirovaniya x-rays (56) from a sample (26) reflected by the mirror (60)using diffraction phenomena, and then detected by a detector (20) x-ray radiation, characterized in that:
mirror (60) has a reflective surface consisting of a combination of flat reflective surfaces (62), which are located so that the angle in a plane parallel to the plane of diffraction, between each flat reflective surface (62) and a line segment connecting the center of each flat reflective surface (62) and the sample (26), was constant for all flat reflective surfaces (62), and the plane of the crystal lattice, which causes the reflection in each flat reflective surface (62), is parallel to each flat reflective surface (62);
x-ray detector (20) is one-dimensional, position-sensitive in a plane parallel to the plane of diffraction;
relative location of the flat reflective surfaces (62) and x-ray detector is (20) defined in the plane parallel to the plane of diffraction, so that the reflected x-rays that have been reflected in various flat reflective surfaces (62), reached different points on the detector (20) x-ray radiation, respectively; and
various dragirovaniya x-rays (56)having different angles of diffraction, reflected by the mirror (60) and then detected separately and simultaneously by the detector (20) x-ray radiation.
12. The method of x-ray diffraction according to claim 11, in which the respective centers of the flat reflective surfaces (62) are located in a plane parallel to the plane of diffraction, equiangular spiral, having a center which is located on the surface of the sample (26).
13. The method of x-ray diffraction according to claim 11, in which the center of at least one of the flat reflective surfaces (62) is shifted in a plane parallel to the plane of diffraction, from the point at equiangular spiral having a center located on the surface of the sample (26).