NL2015060B1 - Improved X-ray diffractometer. - Google Patents
Improved X-ray diffractometer. Download PDFInfo
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- NL2015060B1 NL2015060B1 NL2015060A NL2015060A NL2015060B1 NL 2015060 B1 NL2015060 B1 NL 2015060B1 NL 2015060 A NL2015060 A NL 2015060A NL 2015060 A NL2015060 A NL 2015060A NL 2015060 B1 NL2015060 B1 NL 2015060B1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
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- Crystallography & Structural Chemistry (AREA)
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- General Physics & Mathematics (AREA)
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- Analysing Materials By The Use Of Radiation (AREA)
Abstract
An X-ray diffractometer is provided comprising a first arm (8) and a second arm (9), the first arm being rotatably connected to the second arm at a first rotation point (10). A sample holder (14) is mounted onto the first arm at an outer end of the first arm away from the first rotation point (10). An X-ray source (2) is configured to emit a divergent Xray beam (50) so as to irradiate a surface of the sample (5). The second arm is rotatably connected to the X-ray source (2) at a second rotation point (11). A detector (7) is configured to detect scattered beams coming from the sample, the detector being rotatably arranged around the first rotation point. Guiding means (12, 13) are provided to guide the sample (5) along a main axis of the X-ray beam thereby varying an angle between the first and second arm. The connection between the first and second arm forces the sample holder (14) to rotate relative to the main axis of the X-ray beam so that an angle between the main axis of the X-ray beam and the surface of the sample is varied. A special shield is provided that is arranged to shield the detector from the divergent X-ray beam coming from the X-ray source but allowing the scattered beams coming from the sample (5) to reach the detector (7).
Description
Improved X-ray diffractometer FIELD OF THE INVENTION
The invention relates to an X-ray diffractometer. More particularly, it relates to a diffractometer for analyzing the structure of a material from the scattering pattern produced when an X-ray beam interacts with it.
BACKGROUND ART
An X-ray diffractometer is a measuring instrument for analyzing the structure of a material from the scattering pattern produced when an X-ray beam interacts with it. Patent application EP0497406 describes such an X-ray diffractometer device. An X-ray source emits a divergent X-ray beam that irradiates the surface of a sample under investigation. By X-ray diffraction this beam is scattered in directions obeying Braggs law. The scattered beams are subsequently detected by a detector rotatable around a first rotation point. This rotation ensures that all, or at least a large fraction of all scattered beams can be detected sequentially. To enlarge the accessible number of scattered beams the angle at which the X-ray beam hits the sample surface can be varied. To accomplish this variation the sample is fixed by means of a sample holder on a first arm, which is in turn connected to a second arm at the first rotation point. The second arm is rotatably connected to the X-ray source. The center of rotation for the detector coincides with the first rotation point. When the sample is dragged along a main axis of the X-ray beam by means of a spindle, the connections between the first and second arm force the sample to rotate as well and thereby vary the angle between incident beam and sample surface.
When scattered beams at low scattering angles need to be measured (as is often the case), the divergent X-ray beam may hit the detector directly, without first being scattered by the sample. This leads to a seriously increased background.
SUMMARY OF THE INVENTION
One of the objects of the invention is to eliminate this unwanted background which may occur using the X-ray diffractometer of the state of the art. A first aspect of the invention provides an X-ray diffractometer comprising a first arm and a second arm. The first arm is rotatably connected to the second arm at a first rotation point. The diffractometer also comprises a sample holder for holding a sample under investigation, the sample holder being mounted onto the first arm at an outer end of the first arm away from the first rotation point. An X-ray source is configured to emit a divergent X-ray beam so as to irradiate a surface of the sample, wherein the second arm is rotatably connected to the X-ray source at a second rotation point. A detector is configured to detect scattered beams coming from the sample, the detector being rotatably arranged around the first rotation point. The diffractometer also comprises guiding means configured to guide the sample holder along a main axis of the X-ray beam thereby varying an angle between the first and second arm. The connection between the first and second arm forces the sample holder to rotate relative to the main axis of the X-ray beam so that an angle between the main axis of the X-ray beam and the surface of the sample is varied.
The diffractometer is characterized in that it comprises a shield rotatably arranged around a third rotation point which rotation point is fixed relative to the detector, wherein the shield is configured and arranged to shield the detector from the divergent X-ray beam coming from the X-ray source but allowing the scattered beams to reach the detector.
Embodiments are defined in the dependent claims.
BRIEF DESCRIPTION OF THE DRAWINGS
These and other aspects of the invention are apparent from and will be elucidated with reference to the embodiments described hereinafter. In the drawings,
Figure 1 shows a top view of the X-ray diffractometer 1 according to an embodiment of the invention;
Figure 2 shows a top view of the X-ray diffractometer according to the embodiment of Figure 1 but in a different state;
Figure 3 is a perspective view of an embodiment of the X-ray diffractometer;
Figure 4 is a perspective view of the embodiment of the X-ray diffractometer of Figure 3 seen from a different perspective;
Figure 5 shows the divergent X-ray beam coming from the source and hitting the sample;
Figure 6a schematically shows a top view of the shield and the bar;
Figure 6b schematically shows a top view of the shield and the cable;
Figure 7 shows a top view of the embodiment of Figures 3 and 4 in which the pin abuts against the bar, and
Figure 8 shows a perspective view of the situation of Figure 7.
It should be noted that items which have the same reference numbers in different Figures, have the same structural features and the same functions, or are the same signals. Where the function and/or structure of such an item has been explained, there is no necessity for repeated explanation thereof in the detailed description.
DETAILED DESCRIPTION OF EMBODIMENTS
Figure 1 shows a top view of the X-ray diffractometer 1 according to an embodiment of the invention. The diffractometer comprises an X-ray source 2 which emits a divergent X-ray beam (not visible in Figure 1) that irradiates the surface of a sample 5 under investigation. In Figure 1 a main axis 3 of the divergent X-ray beam is indicated by a line 3. In the following the divergent X-ray beam is also referred to as the direct beam 50, see also Figure 5. A diaphragm 4 is positioned close to the X-ray source 2 to limit the beam divergence to ensure that only the sample surface is irradiated. However, because the direct beam 50 is also scattered by air the edges of the direct beam are rather diffuse. This results in a significant part of the direct beam hitting the detector without interacting with the sample.
Due to X-ray diffraction the direct beam 50 is scattered in directions obeying Braggs law. In Figure 1, an arrow 6 indicated a main axis of one of the scattered beams. The scattered beams are subsequently detected by a rotating detector 7. This rotation ensures that all, or at least a large fraction of all scattered beams can be detected sequentially. In an embodiment the detector 7 comprises an array of sensors. By using an array of sensors rather than a single detector the sensitivity and the speed of the measurements is improved.
To enlarge the accessible number of scattered beams an angle a (hereafter: angle of incidence a) at which the direct beam 50 hits the sample surface can be varied. To accomplish this variation the sample 5 is fixed on a first arm 8 (also referred to as sample arm), which is in turn connected to a second arm 9 (also referred to as tube arm) at rotation point 10. The tube arm 9 is rotatably connected to the X-ray source 2 at a rotation point 11. So both connections of tube arm 9 are rotation points. The center of rotation for a detection surface of the detector 7 coincides with the rotation point 10.
As shown in the top view of Figure 1, the X-ray diffractometer 1 also comprises a spindle 12 and a coupling body 13 slidably arranged onto the spindle 12.
The coupling body 13 is arranged to rotatably couple the sample arm 8 to the spindle 12. The coupling body 13 is moved along the spindle 12 by means of a motor (not shown). In this way the sample 5 being positioned in a sample holder at the outer end of the sample arm 8, can be dragged along the main axis 3 of the direct beam 50 by means of the spindle 12, the coupling body 13 and the motor. The spindle 12, the coupling body 13 and the motor are further referred to as the guiding means for guiding the sample 5.
When the sample 5 is dragged along a straight line parallel to the spindle 12, the connections between the sample arm 8, the tube arm 9 and the coupling body 13 force the sample 5 to rotate as well and thereby vary the angle a between the incident beam (i.e. main axis 3) and sample surface. As can be seen from Figure 1, an angle between the sample arm 8 and the tube arm 9 is two times a.
The diffractometer 1 further comprises a detector arm 15 which is rotatably coupled to the tube arm 9 at the rotation point 10. An angle between the main axis of the tube arm 9 and the detector arm 15 is referred to as angle β.
It is noted that the X-ray diffractometer 1 in Figure 1 is in a position wherein the diffracted beams 6 do not reach the detector 7. Once the angle β is increased, as will be shown in Figure 2, the diffracted beams 6 will reach the detector 7. But when scattered beams at low scattering angles need to be measured, the direct beam 50 might hit the detector 7 directly, without first being scattered by the sample 5 (as will explained in detail with reference to Figure 5, 6a and 6b). This leads to a seriously increased background.
To eliminate this unwanted background, a shield 16 is moved between the X-ray source 2 and the detector 7. This shield 16 is positioned to block radiation coming directly from the source 2, while radiation travelling via the sample 5 (i.e. the diffracted beams 6) can enter the detector 7 freely. The shield 16 is rotatable around a rotation point 17 near the detector 7. In the embodiment of Figure 1, the rotation point 17 is arranged on the detector arm 15. The shield 16 may have a tapered outer end as can be seen from the top view shown in Figure 1.
When the detector 7 is rotated away from the sample 5, the shield 16 will be rotated to prevent it to block radiation scattered from the sample surface. This is realized by mounting the shield 16 on a ruler or guidance 18. The guidance 18 is arranged between the detector arm 15 and the outer end of the sample arm 8 where the sample 5 is held. In an embodiment, the guidance 18 ensures that the shield 16 is directed towards the edge of the sample nearest to the X-ray source. The shield 16 is sharp, because it rotates with the angle of incidence and it must function in the same way for all angles of incidence.
Figure 2 shows a top view of the X-ray diffractometer 1 according to the embodiment of Figure 1 but in a different state. As compared to the situation of Figure 1, the angle of incidence a is decreased. The angle β is set so as to be able to detect the diffracted beams. In Figure 2, the angle β is set to about 90°.
Figure 3 is a perspective view of an embodiment of the X-ray diffractometer 1. The diffractometer 1 comprises a bottom plate 30 on which an X-ray source 2 is mounted. A spindle 12 is also arranged on the bottom plate 30. A coupling body 13 is slidably arranged on the spindle 12. A motor 31 is arranged on the bottom plate 30 and configured to displace the coupling body 13 along the spindle 12. A sample holder 14 is arranged on the coupling body 13. The sample holder 14 holds the sample 5. Next to the bottom plate 30 a slider 32 is arranged which interacts with the coupling body so as to eliminate mechanical play thus ensuring an exact linear movement of the sample holder 14.
Figure 3 further shows a detector 7 arranged on the detector arm 15, and a shield 16 rotatably arranged next to the detector 7. The shield 16 is rotatable around a rotation point 17. The shield 16 comprises a main blocking part extending in a direction parallel to the bottom plate 30 and an upright extension extending in a direction perpendicular to the bottom plate. On top of the upright extension, a pin 33 is arranged. A cable 34 is arranged between the rotation point 17 and a connection point 35 near the sample holder 14. In this embodiment the cable 34 functions as guidance 18.
Figure 3 further shows a bar 36 which is connected to the X-ray source 2 and extends along the X-ray beam (not shown) coming from the X-ray source 2. Finally, Figure 3 also shows a motor 38 arranged and configured to determine the angle β of the detector arm 15.
Figure 4 is a perspective view of the embodiment of the X-ray diffractometer of Figure 3 seen from a different perspective. In Figure 4 the tube arm 9 is visible. Furthermore, the diaphragm 4 is visible through which the divergent X-ray beam leaves the X-ray source 2. It is noted that the X-ray source 2 can be a point source or a line source.
Figure 5 shows a top view of the detector 7, the sample 5 and the shield 16 according to an embodiment. Figure 5 also shows the divergent X-ray beam 50 (i.e. the direct beam) coming from the source 2 and hitting the sample 5. The shield 16 is configured to prevent the direct beam 50 from directly hitting the detector 7. Due to the dimensions and the positioning of the shield 16, the direct beam 50 will not hit the detector 7 and only diffracted beams 6 will reach the detector 7. This means that due to the shield 16, so-called background is prevented. Please note that the dimensions of the sample 5 relative to the detector 7 are exaggerated in Figure 5.
In the embodiment shown in Figure 5, the shield 16 comprises a tapered outer end away from the rotation point 17. The diffractometer comprises an orientation mechanism arranged to orientate the tapered outer end of the shield 16 so that the tapered outer end points to a side edge of the sample 5 which is nearest to the X-ray source 2. Due to the combination of the tapered outer end (i.e. edge) of the shield 16 and the pointing to the side edge, an optimal part of the X-ray beam can be used to radiate the sample also in these situations with large a and β.
As the angle of incidence a increases the shield 16 may block the direct X-ray travelling to the sample surface. To prevent this, the shield 16 according to an embodiment is turned away with increasing angle of incidence. This is achieved by arranging a pin 33 (see also Figure 8) on the shield 16 which pin 33 will eventually meet a side of the bar 36. Such a situation is depicted in Figure 6b. Figure 6b schematically shows a top view of the shield 16 and the bar 36. An arrow 60 indicates in which direction the shield 16 is turned in order to avoid intercepting the direct beam 50 before it hits the sample 5. The shield 16 is guided by the flexible cable 34. When pin 33 abuts with bar 36 the cable 34 will be bent at the guidance point 42. The spring loaded roll 41 prevents the cable from hanging loose at all times so that the shield 16 will automatically turn back in case the pin 33 leaves the bar 36 again. In this way the shield 16 will return to its position determined by the cable 34 which tends to orientate the sharp side of the shield towards the side edge 51 of the sample 5, see Figure 5, through connection point 35. Because pin 33 is connected to the shield 16, the shield 16 is pushed out of the direct beam 50. This ensures the whole sample is illuminated at all times.
In the embodiment with the stiff guidance 18 shown in Figure 1 and 2, the flexible cable 34 is replaced by the stiff guidance 18. In this embodiment, the shield 16 is pushed along the stiff guidance 18 in its correct position by a spring 61 as shown in Figure 6a. As the sample 5 is moved away from the X-ray source 2, the bar 36 prevents the shield 16 to intercept the beam traveling to the sample surface by blocking pin 33. Because the pin 33 is connected to the shield 16, the shield 16 is pushed back along the stiff guidance 18 by the bar 36, thus ensuring the sample 5 is completely illuminated at all times. This translation is indicated by double sided arrow 70 in Figure 6a. At the same time spring 61 is loaded.
When the sample 5 is moved towards the X-ray source 2, or when the detector 7 is rotated away from the sample 5, the spring 61 will relax and push back the shield 16 in its original position. This ensures the shield 16 is functioning optimally at all times. The embodiment with the flexible cable is easier to realize as compared to the other embodiment.
Figure 7 shows a top view of the embodiment of Figures 3 and 4 in which the pin 33 abuts against the bar 36 in order to turn the shield 16 out of the direct beam 50 so as to avoid the shield 16 from blocking the sample under investigation.
Figure 8 shows a perspective view of the situation of Figure 7. As can be seen from Figure 8, the bar 36 forces the shield 16 to rotate around rotation point 17 in the direction of arrow 60 thus preventing it from intercepting the direct beam before it hits the sample.
It should be noted that the above-mentioned embodiments illustrate rather than limit the invention, and that those skilled in the art will be able to design many alternative embodiments. In the claims, any reference signs placed between parentheses shall not be construed as limiting the claim. Use of the verb "comprise" and its conjugations does not exclude the presence of elements or steps other than those stated in a claim. The article "a" or "an" preceding an element does not exclude the presence of a plurality of such elements. In the device claim enumerating several means, several of these means may be embodied by one and the same item of hardware. The mere fact that certain measures are recited in mutually different dependent claims does not indicate that a combination of these measures cannot be used to advantage.
CLAUSES
The above description relate to the following embodiments: 1. An X-ray diffractometer comprising: - a first arm (8) and a second arm (9), the first arm being rotatably connected to the second arm at a first rotation point (10); - a sample holder (14) for holding a sample (5) under investigation, the sample holder (14) being mounted onto the first arm at an outer end of the first arm away from the first rotation point (10); - an X-ray source (2) configured to emit a divergent X-ray beam (50) so as to irradiate a surface of the sample (5), wherein the second arm is rotatably connected to the X-ray source (2) at a second rotation point (11); - a detector (7) configured to detect scattered beams coming from the sample, the detector being rotatably arranged around the first rotation point; - guiding means (12,13) configured to guide the sample (5) along a main axis of the X-ray beam thereby varying an angle between the first and second arm, wherein the connection between the first and second arm forces the sample holder (14) to rotate relative to the main axis of the X-ray beam so that an angle between the main axis of the X-ray beam and the surface of the sample is varied, characterized in that the diffractometer comprises a shield rotatably arranged around a third rotation point which rotation point is fixed relative to the detector, wherein the shield is configured and arranged to shield the detector from the divergent X-ray beam coming from the X-ray source but allowing the scattered beams coming from the sample (5) to reach the detector (7). 2. An X-ray diffractometer according to embodiment 1, wherein the detector is coupled to the first rotation point by way of a detector arm, wherein the third rotation point is located on the detector arm next to the detector. 3. An X-ray diffractometer according to any one of the preceding embodiments, wherein the shield comprises a tapered outer end away from the third rotation point, wherein the diffractometer further comprises an orientation mechanism arranged to orientate the tapered outer end of the shield so that the tapered outer end points to a side edge of the sample which is nearest to the X-ray source. 4. An X-ray diffractometer according to embodiment 3, wherein the orientation mechanism comprises a rod coupled between the detector arm near the detector and the first arm at the outer end of the first arm away from the first rotation point. 5. An X-ray diffractometer according to embodiment 3, wherein the orientation mechanism comprises a cable coupled between the detector arm near the detector and the first arm at the outer end of the first arm away from the first rotation point. 6. An X-ray diffractometer according to any one of the preceding embodiments, wherein the shield is spring biased and wherein the diffractometer comprises blocking means which forces the shield to rotate around the third rotation point in a situation wherein the shield tends to prevent the X-ray beam from reaching the sample under investigation. 7. An X-ray diffractometer according to embodiment 6, wherein the shield comprises an extension extending in a direction perpendicular to a plane in which the first and second arm are able to rotate, the blocking means comprising a bar extending from the X-ray source towards the sample holder and being slightly angled relative to the main axis of the X-ray beam, wherein if the extension of the shield is forced against a side of the bar, the shield will rotate out of the X-ray beam.
Claims (7)
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
NL2015060A NL2015060B1 (en) | 2015-06-30 | 2015-06-30 | Improved X-ray diffractometer. |
US15/740,706 US10539519B2 (en) | 2015-06-30 | 2016-06-09 | X-ray diffractometer |
CA2989369A CA2989369A1 (en) | 2015-06-30 | 2016-06-09 | Improved x-ray diffractometer |
EP16731538.1A EP3317653B1 (en) | 2015-06-30 | 2016-06-09 | X-ray diffractometer |
AU2016287001A AU2016287001A1 (en) | 2015-06-30 | 2016-06-09 | Improved X-ray diffractometer |
PCT/EP2016/063199 WO2017001165A1 (en) | 2015-06-30 | 2016-06-09 | Improved x-ray diffractometer |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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NL2015060A NL2015060B1 (en) | 2015-06-30 | 2015-06-30 | Improved X-ray diffractometer. |
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NL2015060B1 true NL2015060B1 (en) | 2017-01-24 |
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NL2015060A NL2015060B1 (en) | 2015-06-30 | 2015-06-30 | Improved X-ray diffractometer. |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0118965A1 (en) * | 1983-03-15 | 1984-09-19 | Technische Hogeschool Eindhoven | Kinematic X-ray analysis apparatus |
EP0497406A1 (en) * | 1991-01-31 | 1992-08-05 | Philips Patentverwaltung GmbH | Radiographic device for measuring stress |
US20110268251A1 (en) * | 2010-04-29 | 2011-11-03 | Bruker Axs, Inc. | Method and apparatus for using an area x-ray detector as a point detector in an x-ray diffractometer |
US20120195406A1 (en) * | 2011-01-31 | 2012-08-02 | Rigaku Corporation | X-ray diffraction apparatus |
-
2015
- 2015-06-30 NL NL2015060A patent/NL2015060B1/en not_active IP Right Cessation
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0118965A1 (en) * | 1983-03-15 | 1984-09-19 | Technische Hogeschool Eindhoven | Kinematic X-ray analysis apparatus |
EP0497406A1 (en) * | 1991-01-31 | 1992-08-05 | Philips Patentverwaltung GmbH | Radiographic device for measuring stress |
US20110268251A1 (en) * | 2010-04-29 | 2011-11-03 | Bruker Axs, Inc. | Method and apparatus for using an area x-ray detector as a point detector in an x-ray diffractometer |
US20120195406A1 (en) * | 2011-01-31 | 2012-08-02 | Rigaku Corporation | X-ray diffraction apparatus |
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