X-ray diffraction screening system convertible between reflection and transmission modes

• US 20060023838A1
• Filed: 07/19/2005
• Published: 02/02/2006
• Est. Priority Date: 07/29/2004
• Status: Active Grant

• Current Assignee: Bruker AXS Incorporated (Bruker Corporation)
• Original Assignee: Bruker AXS Incorporated (Bruker Corporation)
• Inventors: He, Bob Baoping, Bollig, Ryan C.
• Granted Patent: US 7,242,745 B2
• Time in Patent Office: Days
• US Class Current: 378/81
• CPC Class Codes: G01N 23/20016 Goniometers

Abstract

An X-ray diffraction apparatus provides analysis in either transmission or reflective mode and easy conversion between the two modes. An X-ray source and X-ray detector are each connected to a different circle of a goniometer. The two circles may be rotated independently to position the source and detector on the same side of a sample library for reflection mode operation, or on opposite sides of the sample library for transmission mode operation. The sample library has a horizontal orientation that allows open sample containers of the library to maintain the sample without spillage, and it connects to an XYZ stage that can move in three dimensions. The system may use a beamstop, and the goniometer and XYZ stage be motorized and controlled for automated sample analysis.

Claims

1. An X-ray diffraction apparatus for analyzing a sample on a sample holder, the apparatus comprising:

a mounting assembly that maintains the sample holder along a horizontal axis, such that one side of the sample holder is located to a first side of the axis and an opposite side of the sample holder is located to a second side of the axis;

an X-ray source that directs X-ray energy toward the sample holder;

an X-ray detector that detects X-ray energy diffracted from the sample; and

a movement assembly that allows movement of one of the source and detector along a predetermined path between a first position, in which the source and detector are on same side of the horizontal axis, and a second position, in which the source and detector are on opposite sides of the horizontal axis from each other.

2. An apparatus according to claim 1 wherein the movement assembly allows movement of the X-ray source along said predetermined path.

3. An apparatus according to claim 1 wherein the movement assembly allows movement of the X-ray detector along said predetermined path.

4. An apparatus according to claim 1 further comprising a goniometer to which the X-ray source assembly and the X-ray detector assembly are connected.

5. An apparatus according to claim 4 wherein the source assembly is connected to a first circle of the goniometer and the detector assembly is connected to a second circle of the goniometer, and wherein each of the first and second circles is rotatable independently.

6. An apparatus according to claim 5 further comprising a video assembly that is focused on the sample and that is connected to the first circle of the goniometer.

7. An apparatus according to claim 5 further comprising a counterweight attached to the first circle of the goniometer that counterbalances the source assembly.

8. An apparatus according to claim 7 wherein the counterweight is located to a side of the first circle opposite that to which the source assembly is connected.

9. An apparatus according to claim 8 wherein the counterweight is connected to the first circle via a rotary connection aligned with a central axis of the goniometer.

10. An apparatus according to claim 5 further comprising a counterweight attached to the second circle of the goniometer that counterbalances the detector assembly.

11. An apparatus according to claim 10 wherein the counterweight is located to a side of the second circle opposite that to which the detector assembly is connected.

12. An apparatus according to claim 11 wherein the counterweight is connected to the second circle via a connecting rod that extends around an outer surface of the goniometer.

13. An apparatus according to claim 1 wherein the mounting assembly is movable to allow relocation of the sample holder between a sample position and an alternate position.

14. An apparatus according to claim 13 wherein the mounting assembly is movable in at least two perpendicular directions.

15. An apparatus according to claim 13 wherein, when the sample holder is in the sample position, complete movement of at least one of the source assembly and the detector assembly is obstructed, and wherein such obstruction is removed when the sample holder is in the alternate position.

16. An apparatus according to claim 1 wherein the sample is a first sample, and wherein the sample holder comprises a plurality of sample locations for retaining a plurality of samples simultaneously.

17. An apparatus according to claim 16 wherein, at any given time, one of the plurality of samples is positioned at a sample site to which X-ray energy from the source is directed and from which diffracted X-ray energy is detected by the detector, and wherein the mounting assembly is movable to reposition the sample holder to change which of the plurality of samples is at the sample site.

18. An apparatus according to claim 1 further comprising motors that are used for moving the X-ray source assembly and the detector assembly and a controller that automatically controls the motors.

19. An apparatus according to claim 1 further comprising a beamstop located between the sample and the detector that blocks non-diffracted X-ray energy from reaching the detector.

20. An apparatus according to claim 1 further comprising a video assembly positioned to allow viewing of the sample.

21. An X-ray diffraction apparatus for analyzing a sample positioned at a sample site, the sample being located on a sample holder having a plurality of sample locations, the apparatus comprising:

a goniometer;

a mounting assembly that maintains the sample holder in a horizontal orientation and that is movable in at least two directions to reposition the sample holder to change which of the plurality of sample locations is at the sample site;

an X-ray source assembly that is connected to a first circle of the goniometer and that has an X-ray source that directs X-ray energy toward the sample holder, the source assembly being movable with movement of the first goniometer circle along a predetermined path to relocate the X-ray source from a first source position in which the X-ray energy is directed toward an upper surface of the sample holder to a second source position in which the X-ray energy is directed toward a lower surface of the sample holder; and

an X-ray detector assembly that is connected to a second goniometer circle of the goniometer and that has an X-ray detector that detects X-ray energy diffracted from an upper surface of the sample, the detector assembly being movable with the second goniometer circle.

22. An X-ray diffraction apparatus for analyzing a sample on a sample holder, the apparatus comprising:

a mounting assembly that locates the sample holder at a predetermined location;

an X-ray source that directs X-ray energy toward the sample holder;

an X-ray detector that detects X-ray energy diffracted from the sample; and

a goniometer to which the X-ray source and the X-ray detector are secured, the goniometer having at least two circles that are rotatable independently of each other and that each have a mounting side to which either the X-ray source or the X-ray detector may be secured, each of the circles also being connected to a respective counterweight that is located on a side of that circle opposite its mounting side, the counterweight for a first of the circles being connected to the first circle via a rotary connection aligned with a central axis of the goniometer, and the counterweight for a second of the circles being connected to the second circle via a connecting rod that extends around an outer surface of the goniometer.

23. An X-ray diffraction apparatus according to claim 22 wherein the X-ray source is secured to the first circle of the goniometer and the X-ray detector is secured to the second circle.

24. An X-ray diffraction apparatus according to claim 23 further comprising a video system secured to the first circle of the goniometer that captures an image of the sample.

25. An X-ray diffraction apparatus according to claim 22 wherein the first and second circles of the goniometer have a first relative position in which the X-ray source and the X-ray detector are located to the same side of the sample, thereby allowing reflection-mode operation of the system, and a second relative position in which the X-ray source and the X-ray detector are located on opposite sides of the sample, thereby allowing transmission-mode operation of the system.

26. A method of analyzing a sample on a sample holder, the method comprising:

locating the sample holder on a mounting assembly that maintains the sample holder along a horizontal axis, with one side of the sample holder being located to a first side of the axis and an opposite side of the sample holder being located to a second side of the axis;

directing X-ray energy toward the sample holder with an X-ray source;

detecting X-ray energy diffracted from the sample with an X-ray detector; and

moving one of the source and detector along a predetermined path between a first position, in which the source and detector are on the same side of the horizontal axis, and a second position, in which the source and detector are on opposite sides of the horizontal axis from each other.

27. A method according to claim 26 further comprising securing the source assembly to a first circle of a goniometer and securing the detector assembly to a second circle of the goniometer, each of the first and second circles being rotatable independently.

28. A method according to claim 27 further comprising attaching a source counterweight to the first circle of the goniometer to counterbalance the source assembly, the source counterweight being located to a side of the first circle opposite that to which the source assembly is secured.

29. A method according to claim 28 further comprising attaching a detector counterweight to the second circle of the goniometer to counterbalance the detector assembly, wherein the detector counterweight is located to a side of the second circle opposite that to which the detector assembly is secured, and wherein the source counterweight is connected to the first circle via a rotary connection that passes through the goniometer.

30. A method according to claim 26 wherein the mounting assembly is movable in at least two perpendicular directions.