X-ray analysis device

FIELD: physics.

SUBSTANCE: apparatus for carrying out both x-ray diffraction (XRD) and x-ray fluorescence (XRF) analysis of a crystalline sample, comprising an evacuable chamber; a sample holder located in the evacuable chamber, for mounting the crystalline sample so that it can be analysed; an XRF tube mounted in the evacuable chamber, for illuminating the crystalline sample with x-rays; an XRF detection arrangement for detecting secondary x-rays emitted from the surface of the crystalline sample as a result of illumination by x-rays from the XRF tube; an XRD tube, also mounted in the evacuable chamber but separate from the XRF tube, for illuminating the crystalline sample with x-rays; an XRD detection arrangement for detecting x-rays of a characteristic wavelength which have been diffracted by the crystalline sample; and a moveable XRD support assembly, comprising a first part configured to mount the XRD tube for movement of the XRD tube relative the sample holder, and a second part configured to mount the XRD detection arrangement for movement of the XRD detection arrangement relative the sample holder.

EFFECT: possibility of more accurately carrying out both x-ray diffraction and x-ray fluorescence analysis of a crystalline sample.

13 cl, 4 dwg

The scope of the invention

The present invention relates to a device for x-ray analysis to perform elemental and crystallographic analysis on the sample.

Prior art

In the prior art there are known various methods of elemental analysis and structural characteristics of a material having a crystalline structure. For example, x-ray diffraction analysis (XRD) based on the analysis of paintings, created in the result of x-ray diffraction on a dense lattice of atoms in a crystal to detect structural composition of the analyzed material. Bragg's law allows you to get the interplanar distance in the crystal lattice of the measured path difference for diffracted x-rays.

In contrast, x-ray fluorescence (XRF) is a spectroscopic method for elemental, a sample without the use of chemical analysis. When the XRF x-ray irradiation of the sample by the beam causes the emission of secondary x-rays with characteristic wavelengths, indicating the elemental composition of the sample. To ensure multi-element analysis of the x-ray source to conduct XRF is usually polychromatic.

United devices to perform XRD/XRF existed for many years. The first type of edinennogo device XRD/XRF works with the sample at atmospheric pressure. The second type of the joint device operates in a vacuum. Each type has its own advantages and disadvantages: the devices that sample analysis is carried out in vacuum, usually provide more qualitative x-ray analysis, in particular but not only, by the XRF method, because in this case, increasing the sensitivity to elements with low atomic number. On the other hand, the size and physical installation nonvacuum device is imposed fewer restrictions, and in addition, it is possible to quickly shift samples.

To deliver high-quality XRD and more complete structural characteristics for use in Mineralogy and phase analysis it is desirable to be able to modify the measured diffraction angle at a wide range. In nonvacuum systems, it is not very difficult. However, in the vacuum chamber limited space reduces the possibility of improving characteristics of the device. It was suggested several solutions to the problem of limited space when analysis of a sample in a vacuum chamber using XRD methods.

In devices that only perform XRD, x-ray tube and detector can be rotated with a fixed sample. However, for United devices XRD/XRF only x-ray tube is fixed in a fixed position and the sample is rotated p is secured and detector, the sample is fixed by rotating the detector or, as in U.S. patents US 4263510 A, US 5369275A and US 4916720 And turn and the sample and the detector. The last option, apparently, provides the best performance in a vacuum.

However, for high-quality XRF requires that the distance between the sample and the tube was small. Unfortunately, this requirement can result in tradeoffs in device XRD/XRF, because, as noted above, high-XRD measurements require that the sample could be rotated. This, in turn, imposes a limitation on the minimum distance between the location of the x-ray tube and the sample (so they are not experienced during the XRD measurements), which degrades performance when the XRF measurements.

In the assigned to applicant's U.S. patent US 5406608 described the United analyzer XRD/XRF for analysis of samples in vacuum. The x-ray source is mounted in a fixed position relative to the vacuum chamber of the device and provides polychromatic divergent x-ray beam that irradiates the sample for both measurements, XRD and XRF measurements. Provides one or more fixed and or mobile channels fluorescence to provide a choice of x-rays of a specific wavelength and energy and registering the selected rentgenovsk the x-rays. There is also a channel of diffraction, which allows you to select a specific wavelength of x-rays in the source after diffraction on the sample. Channel diffraction also has a detector installation. Detector x-ray diffraction performed can be rotated to improve the XRD measurements. However, optimization of the parameters of XRF is the availability of multiple channels of fluorescence or install channel fluorescence (includes detector installation) on a goniometer, which can be rotated around the sample.

Although the above device is a good compromise between the characteristics of XRD and XRF, he also has several disadvantages. First, the sample is fixed relative to the x-ray tube (in other words, can be rotated detector installation XRD, and not the sample), which limits the XRD characteristics, secondly, in an attempt to prevent the deterioration of characteristics XRF installation of tubes, detectors, sample and the vacuum chamber in the patent US 5406608 And limits the angular range of the detector XRD, which in turn limits the ability to perform a wider XRD measurements.

The invention

Whereas the above-described prior art, the present invention is the creation of a more perfect instrument for the analysis of the XRD/XRF samples in HAC is the mind. According to the present invention presents a device for analysis of a crystalline sample by x-ray diffraction (XRD) and x-ray fluorescence (XRF), containing: pumped chamber; a sample holder located inside the pumping chamber, to install crystalline sample so that it can be subjected to analysis; x-ray source fluorescence mounted within the pumping chamber for irradiation of the crystalline sample with x-rays; installation check XRF for detecting secondary x-rays emitted from the surface of the crystal sample in the x-ray irradiation from the specified x-ray source fluorescence, characterized in that it contains the x-ray source diffraction, also mounted within the pumping chamber, but separately from the x-ray source fluorescence, for irradiation of the crystalline sample with x-rays; installation check XRD for registration of x-rays characteristic wavelength, which were Draginovo crystalline sample; and a movable support node XRD containing the first item, made with the possibility of installation source XRD to move the source XRD relative to the sample holder, and the second part is configured to set the Desk XRD to move the installation registration XRD relative to the sample holder. Thus, the device in accordance with the invention provides separate x-ray tube in a vacuum chamber: the first for irradiating a sample with x-rays for XRF, and the second for irradiating a sample with x-rays for XRD. Tube XRD and setting an appropriate registration XRD are with the possibility of relative movement relative to the specimen. Thus, the device can collect data for XRF chemical or elemental analysis, while the XRD data provide a complete structural and phase analysis of the same sample under the same scenarios under vacuum.

Previous integrated installation XRD and XRF or represents a compromise in terms of accuracy and / or the ability to measure elements with low atomic numbers due to the fact that samples were in the atmosphere or used one static x-ray tube in a vacuum and for XRD and XRF. For more new plants is characterized by the following trade-offs: a limited range of angles in the XRD measurements (for example, when the detector XRD mobile, how to install from patent US 5406608 And the range of available angles is in the range of about from 25 to 55 degrees) and / or limited ability to bring the x-ray source to the sample, since the need for POWERCIAT the sample is forced to move the x-ray tube from the sample (to prevent collisions), which degrades the characteristics of the XRF.

Specialists in the art know that it is difficult to increase the number of x-ray tubes in the chamber due to the additional cooling requirements. For exact measurements, XRD recommended the x-ray source with a power of 1 kW or more; the preferred option is the source power of 1.8 kW, operating at a voltage of 45 kV and current of 40 mA. Install a powerful source of x-rays in vacuum complicates the task of cooling the source, reducing the available surface through which can be transmitted heat. It is therefore desirable to establish as much of the x-ray tube outside the vacuum chamber to provide heat removal from the tube. However, in the case of the combined device XRD-XRF XRD detector must be installed on the same side of the sample, and the tube, and should be removed from the sample. This is necessary in order dragirovaniya x-rays went before into the detector, in order to improve the angular resolution of the detector. The gap between the sample and the detector must be in a vacuum, and therefore the sample must be deeply in a vacuum chamber. This means that the fixed x-ray tube should also include deep inside the vacuum chamber, and only one, to whom NZW x-ray tube has access from the outside of the vacuum chamber, what complicates the problem of heat dissipation. This problem is compounded if the x-ray tube should be rotated in a vacuum, since in this case no part of the tube can protrude out of the housing, and the tube is placed in the vacuum. Previous United devices XRD-XRF were limited to either the use of one fixed x-ray tube and for XRD and XRF, or the use of two fixed x-ray tube and rotation of the sample and the detector when performing XRD XRD analysis.

In addition, the increase in the number of x-ray sources requires more space inside the vacuum chamber. Space is expensive given in a vacuum chamber, because the increase in the size of the vacuum chamber increases the cost of production and requires a more productive, more expensive vacuum pumps. In addition, as confirmed by the US patent 5406608 and other documents, known from the prior art, one x-ray source to minimize expenses.

However, the authors of the present invention realize that if you have a second tube for XRD, which can move relative to the sample, and if there is also a mobile recording XRD, it is possible to measure a wider range of angles of diffraction. Preferred embodiments of the permit measurement range from some of the degrees (for example, 7 degrees to about 80 degrees. At the same time, a separate tube and registering installation for XRD allows you to do without compromise with XRF, so in preferred versions of the separate tube XRF can be mounted in a fixed position in the vicinity of the sample in the sample holder (which may be, however, secured in such a way as to rotate around a vertical axis).

Placing the device XRD in a vacuum, it is possible to isolate the sample, for example, from moisture. This in turn contributes to the analysis of certain industrial compounds, such as cement and its components (e.g., unbound lime), which is very hygroscopic and therefore quickly degrade its properties in the presence of water available in the damp air.

Fixing the sample in a horizontal position, you can place powdered samples, not fearing them to scatter. Known from the prior art configuration with a rotating sample holder or limited in the types of samples that can be analyzed or must limit the angular rotation of the sample, thereby limiting characteristics of performing XRD measurements. Powdered samples are often subjected to analysis, for example, in the cement industry.

Tube XRD and installation for recording XRD is predpochtitelno are each on different arms of the goniometer. Alternatively, you can use two separate goniometer so that it was possible to independently control the motion of the source XRD and XRD detector, although it is preferable that both movements were controlled by a single control device, such as a computer. The XRD tube preferably entirely situated inside the vacuum chamber, so that its angular movement is no limited, and in this case can be provided with the appropriate power and cooling using inputs with deep vacuum coming from the outside of the vacuum chamber inside the vacuum chamber together with the optional flexible tubing inside the chamber, so that the tube XRD was able to move relative to the camera.

A significant advantage of this fully integrated device XRD and XRF is the combination of the data of chemical analysis for the interpretation of XRD data for mineralogical analysis with XRF data, which is an additional input to the system processing XRD to confirm and quantify the relevant minerals or phases in the same sample. The data obtained in the modes of XRF and XRD, collects preferably one operating system, and then these data are processed to obtain a complete chemical and mineralogical characteristics of the polycrystalline material.

Brief description the drawings

The invention can be practically implemented in many different ways, and below, purely as an example the description of the private option, with reference to the accompanying drawings, on which:

Figure 1 provides a top view of the joint device XRD/XRF embodying the present invention and which includes a tube and detectors XRD and XRF;

Figure 2 contains a view in section along the line a-a' in figure 1, further illustrating the location of the tube and detector XRD;

Figure 3 contains a view in section along the line B-In' figure 1, further illustrating the location of the tube and detector XRF;

Figa contains a view in section along the line C-C' figure 1 is a detail illustrating the XRD tube and method of connection to the vacuum enclosure and passing through the vacuum housing; and

Fig.4b contains a side view of the installation shown in figa.

A detailed description of the preferred variant of the invention

Figure 1 shows a schematic top view of the joint device 10 XRD/XRF. The device 10 includes a vacuum chamber 15 containing components XRD indicated in General position 20 and described in more detail below with reference to figure 2, and the individual components of the XRF indicated in General position 30 and described below with reference to figure 3.

More components 20 XRD contain the tube 40 XRD and detector 50 XRD, each of to who which is mounted on the corresponding arm of the goniometer 60 XRD. The goniometer 60 and installed the tube 40 XRD and detector 50 XRD configured to move relative to the vertical axis And passing through the plane of the paper as shown in figure 1) as described below. The axis specifies the center of the holder 100 of the sample, which is in the process of applying holds analyzed crystalline sample (not shown).

With the goniometer 60 XRD associated drive pulleys 70 goniometer, which may, for example, be operated manually or by a computer to move the goniometer 60 XRD in the selected angular position. Finally, figure 1 also schematically shows the location of cooling and feeding tubes 80 to summarize the cooling and power supply to the tube 40 XRD. As you can see in the top view shown in figure 1, the tube 40 XRD physically isolated from the walls of the vacuum chamber 15, so that its movement can occur unimpeded. The pumping of the vacuum chamber 15 in the application process is carried out using standard pumping equipment, which must be known to experts in the art and which is not shown in figure 1.

In General, the individual components 30 XRF contain the tube 80 XRF, which is fixed relative to the holder 100 of the sample and the vacuum chamber 15 and is located on the same axis with the axis of the holder 100 of the sample. Components 0 XRF also include a detector 110 XRF, mounted on the goniometer 120 XRF. Instead of a single detector XRF 110 mounted on the goniometer 120 XRF so that the detector could be moved, may be placed in the set of the xed channels XRF in spatially separated locations inside the vacuum chamber 15 to provide simultaneous selection and measuring fluorescent x-rays from a sample of different energies. However, these particular characteristics of the detector XRF are not part of the present invention and can be used any known method of installation of the detector, for example, described in U.S. patent US 5406608 And assigned to the applicant of the present invention, the content of which is fully incorporated into the present application by reference.

Figure 2 shows a view in section along the line a-a' in figure 1, illustrating in more detail the placement of the components 20 XRD. As described above in connection with figure 1, the vertical axis defines the longitudinal axis of the tube 90 XRF, which has an anode 130, rhodium tip located near the holder 100 of the sample. The use of rhodium as a material of the anode target for x-ray radiation is, of course, only one of the possible materials for the target, such as copper, tungsten, molybdenum and gold; the specific material of the anode target for x-ray radiation determines the energy distribution of x is from radiation, emitted from the tube 90 XRF. As you can clearly see in figure 2, the axis of the holder 100 of the sample coincides with the axis of the tube 909 XRF.

As shown in figure 2, the tube 40 XRD installed on the right shoulder of the goniometer 60 XRD. Tube 40 XRD preferably represents a source of monochromatic x-rays, which allows to obtain the diraction pattern with good resolution, as described below. Tube 40 XRD also preferably has a relatively high power output to ensure the lowest possible thresholds registration. In a preferred embodiment of the power output tube 40 XRD is 1800 watts at a voltage of 45 kV and current of 40 mA.

The XRD tube 40 has a window 220 of the tube (see also figa), which is connected with divergent optics 45 output XRD to create divergent monochromatic x-ray beam that irradiates the sample in the holder 100 of the sample.

While using the right drive pulley 70 goniometer gives effect to the right shoulder, so that the tube 40 XRD describes arcuate movement around the holder 100 of the sample, in which you installed the sample. The General direction of movement of the tube XRD on the arm of the goniometer denoted θ_D. The angle between the sample (strictly speaking, between the crystal planes within the sample) and the XRD tube determines the diffraction according to Bragg law: nλ=2d _hklsinθ₁where n is an integer number of wavelengths λ, θ₁is the diffraction angle, and d_hkl- interplanar distance, depending on the Miller indices h, k and l of the crystal. The requirement of the law Bragg to θ and λ correspond to each other, makes necessary the existence of a range of wavelengths or angles. The wider available range of angles θ, the more you can get information about the crystal.

On the left shoulder (as shown in figure 2) goniometer 60 installed detector 50 XRD. As in the case of tube 40 XRD drive pulley 70 goniometer allows the left arm of the goniometer XRD lead detector 50 XRD in arcuate movement θ_Daround the holder 100 of the sample. These particular characteristics of the detector 50 XRD are not as such part of the present invention, and the specialist should be clear that it is possible to use any suitable registering installation XRD. However, in General the XRD detector contains optics 55 receiving XRD, which includes the crystal-monochromator collimator (not shown) and a matrix detector 65. The crystal-monochromator is set at a certain angle to the sample and dragirovaniya beam, so that was out, and fell into the detector a certain characteristic wavelength from the source 40 XRD, When the device 10 embodying the present invention, is running in integrated mode XRD/XRF (that is, when both osushestvlyaetsya XRD, and XRF analysis), this crystal isolates creates the fluorescence x-rays coming from the tube 90 XRF (which can create a strong background in the analysis XRD), as well as unwanted diffraction peaks, so that the diffraction pattern of the sample can be obtained by scanning tube 40 XRD and detector 50 XRD. Must be, however, it is clear that the monochromator is not an essential characteristic of the detector. For example, the primary radiation from the tube 40 XRD can be filtered in such a way as to obtain a beam with a single wavelength (K-alpha line of copper). In this case, the monochromator can be excluded from the secondary beam, especially when the tube 90 XRF works asynchronously (and therefore there is no problem associated with the fluorescence of the sample, creating the background when analyzing XRD).

In one embodiment, the tube 40 XRD and detector 50 XRD can move independently under the action of drive pulleys 70 goniometer, but in the preferred embodiment, the Central controller controls the arcuate movement of the two devices, so you can cover a large range of angles between the x-ray source from the tube 40 and the channel register in the detector 50. It is important to note that since the components 20, 30 XRD and XRF are in different planes (on different axes - see figure 1) and has a separate x-ray the felling for each part of the system, there is much more space to move the tube 40 XRD and detector 50 XRD, which reduces the minimum total angle between the x-ray source from the tube 40 XRD and detector 50 XRD to about 7 degrees (approximately 3.5 degrees to the horizontal on each side of the sample) and increase the maximum angle of 80 degrees (40 degrees to the horizontal, respectively, for tube 40 XRD and detector 50 XRD).

Photons registered by the detector 50 XRD, counted and processed by electronic means not shown to obtain the diffraction pattern.

Figure 3 shows a section along the line B-In' figure 1. And on this drawing tube 90 XRF depicted along the longitudinal axis And with the anode 130, pictured next to the sample in the holder 100 of the sample.

In the process, the x-ray emission from the tube 90 XRF falls on the sample holder 100 of the sample, and this leads to the emission of secondary x-ray radiation. The holder 100 of the sample made with the possibility of rotation that allows you to change the orientation of the sample during the study. The characteristic energy of the fluorescent x-rays emitted from the sample, are separated from the continuous spectrum of x-ray energy, for example by Bragg reflection from the surface of the crystal. On the left side of figure 3 shows the static to the cash register fluorescence, acting on this basis. Static registration channel fluorescence contains monochromator 140 XRF 140, scintillation detector 150 XRF, hermetic or gas detector 160 XRF, such as gas-filled counter, and crystal 170 XRF Bragg.

Fluorescent x-rays from the sample passes into the monochromator 140 and faces the crystal 170 Bragg, which dirigeret only one wavelength related to a specific item under a certain angle Bragg. Thus, the crystal 170 Bragg provides monopropylene and focusing x-ray beam of energy required for the detectors 150, 160. To provide simultaneous selection and measuring fluorescent x-rays of different energies can be used multiple static fluorescence channels, such as shown on the left in figure 3. Such a matrix of static channels is particularly useful when the device 10 is installed to control, for example, a certain correlation between the known elements in the production process, such as steel or cement.

However, the application of static fluorescence channels are usually characterized by rigidities in other respects, since each channel is configured to measure only one specific energy (and therefore for Eden is eficacia specific item). Therefore, to overcome this drawback can be used in addition or instead, a serial channel fluorescence mounted on the goniometer 120 XRF, and this is shown to the right in figure 3. The detector 110 with XRF 1 shows in greater detail here in the form of, for example, a scintillation detector 190 and flow proportional (FPC) of the counter 200. Each device is mounted on the goniometer 120 XRF together with the collimator 210. The goniometer 120 XRF is based on the θ-2θ rotation, and fluorescence spectra containing many wavelengths, collyriums primary collimator in front of the flat crystal monochromator. Under this angle the crystal dirigeret only one wavelength related to one specific item of interest. This dragirovaniya wavelength then further collyriums front of the detector of the secondary collimator. Using the mechanism of the optical encoder crystal is located at the angle θ and the detector is located at an angle 2θ. As you rotate the crystal, that is, as the change of the angle θ, different wavelengths dirigida different angles and are identified by the detector synchronously moving the angle 2θ. Thus can be obtained a complete range. At the same time, the channel XRF is fixed and is intended for static measurement the Oia one specific wavelength. In other words, the goniometer 120 XRF acts as a coherent system in which the scanning process at a time is measured one wavelength. On the other hand, the position of the monochromator or a fixed channel XRF is set in advance relative to the fixed positions of the crystal and detector for the perception of one particular wavelength. Preferred embodiments of the present invention makes it possible to combine a flexible, incremental changes XRF using a goniometer 120 XRF with many fixed channels for XRF measurement/registration limited range of elements (and, of course, with the availability of the individual components 20 XRD).

Finally, on figa shows a section along the line C-C in figure 1, is made not to scale. On figa shows a side view in partial section of the tube 40 XRD together with its related compounds for cooling and power. As follows from figure 1 and the above description, the tube 40 XRD mechanically isolated and insulated from the vacuum chamber 15 (as opposed to tube 90 XRF, which is suspended from the top). The insulating tube 40 XRD from the vacuum chamber 15 allows the tube to move relative to the camera. The insulating tube 40 XRD from the vacuum chamber 15 also prevents the transfer of heat, i.e. does not allow a vacuum chamber 15 to act as popot the body heat of the tube 40 XRD. However, for this reason, it is desirable in some other way to cool the tube 40 XRD. You must also be submitted to the tube 40 XRD power with relatively high voltages, and the design depicted in figa, offers one version of how to achieve this. As seen on figa, and fig.4b, which is an enlarged top view of the tube 40 XRD, as it was shown in figure 1, and at the end of the tube 40 XRD has a high-vacuum connection. From this high-vacuum connection 230 moves in the transverse direction of the high-voltage cable 240, coming from the tube 40 XRD against the wall of the vacuum chamber. High-vacuum connection and cable in the place of his retreat filled electrically insulating material such as epoxy resin, which may contain impurities thermally conductive material to facilitate cooling of x-ray tube 40.

Insulating insert or flange 260 in the wall of the vacuum chamber 15 provides electrical isolation between the internal volume of the vacuum chamber 15 and the atmosphere and at the same time provides a vacuum seal. On the atmospheric side of the vacuum chamber 15 there is a second high-voltage connection to an external power source (not shown).

Finally, water-cooled x-ray tube through the inlet opening 280 of cooling water and the exhaust hole is ment 290 water cooling. As the inlet and outlet openings are formed by pipes and tubes, which, at least partially, are flexible to accommodate movements of the tube 40 XRD relative to the vacuum chamber 15. Although figa and 4b is not shown, in the walls of the vacuum chamber 15 is also provided sealed connectors or flanges to provide a connection with an external source of water.

Although for illustrative purposes has been described one specific embodiment of the present invention, a specialist in the art should understand that various modifications without departure from the scope of the invention defined by the attached claims.

1. Device for performing x-ray diffraction analysis (XRD)and x-ray fluorescence analysis (XRF) of the crystalline sample containing the pumped chamber;
the sample holder located in the pumping chamber for installation of the crystal sample to be analyzed;
the x-ray source fluorescence installed in the pumping chamber for irradiation of the crystalline sample x-rays;
installation registration XRF for detecting secondary x-ray radiation emitted from the surface of the crystal sample in the x-ray irradiation of the doctrine from the specified x-ray source fluorescence,
characterized in that it contains:
the x-ray source diffraction, also mounted in the pumping chamber but separated from the x-ray source fluorescence, for irradiation of the crystalline sample x-rays;
installation registration XRD for registration of x-ray radiation of a characteristic wavelength, which was diregiovani crystalline sample; and
the mobile anchor node XRD containing the first part is made with the possibility of installation source XRD, to move the source XRD relative to the sample holder, and the second part is made with the possibility of installation registration XRD to move the installation registration XRD relative to the sample holder.

2. The device according to claim 1, characterized in that the first part of the rolling bearing unit is designed with the possibility of installing the XRD tube for rotational movement through a variety of angular positions relative to the sample holder, and that the second part of the rolling bearing unit is designed with the possibility of installation of the detector XRD for rotational movement through a variety of angular positions relative to the sample holder.

3. The device according to claim 2, characterized in that the mobile reference node contains a goniometer, and the first part of the rolling support unit includes a first arm of the goniometer, and the WTO is the first part of the rolling support unit includes the second arm of the goniometer.

4. The device according to claim 3, further containing a means of bringing into action of the goniometer for actuating each of the first arm and the second arm of the goniometer in order to control the angular displacement, respectively, of the tube XRD and installation registration XRD around the sample holder between the first and second end positions.

5. The device according to claim 4, characterized in that the sample holder forms a horizontal plane within the pumping chamber, the first and second end position setting register XRD draw angles relative to this horizontal plane, respectively, equal to approximately 3° and 40°, and that the first and second end positions of the XRD tube draw angles relative to this horizontal plane of approximately 3° and 40°.

6. Device according to any one of the preceding paragraphs, characterized in that the tube XRF mounted in a fixed position relative to the sample holder and the vacuum chamber.

7. The device according to claim 6, characterized in that the XRF tube has a longitudinal axis that intersects the sample holder.

8. The device according to claim 1, characterized in that the sample holder is made with the possibility of rotation around the axis.

9. The device according to claim 1, characterized in that the installation registration XRF installed on a movable support site XRF.

10. The device according to claim 1, the tives such as those the XRD tube placed inside the vacuum chamber.

11. The device according to claim 10, further containing a cooling channel that goes from the outside of the vacuum chamber to the tube XRD for submission to it cooling, and the connection to the power source, also reaching outside the vacuum chamber to the XRD tube to feed her power.

12. The device according to claim 11, characterized in that the cooling channel, and the connection to the power source is flexible at least in its part to save power and cooling to the XRD tube during its movement relative to the vacuum chamber in use.

13. The device according to claim 1, characterized in that the tube XRD performed with the opportunity to create a monochromatic x-ray beam, and the tube XRF performed with the opportunity to create a polychromatic x-ray beam.