Combinatorial screening system with X-ray diffraction and Raman spectroscopy

• US 20060023837A1
• Filed: 07/21/2005
• Published: 02/02/2006
• Est. Priority Date: 07/30/2004
• Status: Active Grant

• Current Assignee: Bruker AXS Incorporated (Bruker Corporation)
• Original Assignee: Bruker AXS Incorporated (Bruker Corporation)
• Inventors: He, Bob Baoping, Frampton, Christopher S., Burgazy, Frank W.
• Granted Patent: US 7,269,245 B2
• Time in Patent Office: Days
• US Class Current: 378/70
• CPC Class Codes: B01J 2219/00707 separated from the reactor apparatus
• CPC Class Codes: G01N 23/20 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
• CPC Class Codes: G01N 23/20016 Goniometers
• CPC Class Codes: G01N 23/2206 Combination of two or more measurements, at least one measurement being that of secondary emission, e.g. combination of secondary electron [SE] measurement and back-scattered electron [BSE] measurement
• CPC Class Codes: G01N 23/227 Measuring photoelectric effect, e.g. photoelectron emission microscopy [PEEM]

Abstract

A sample analysis system makes use of both X-ray diffraction analysis and Raman spectroscopy of a sample. The sample is part of a sample library that is mounted on an XYZ stage that allows each sample to be examined in turn, as the XYZ stage is moved to position successive samples to a sample location. The system components may be mounted on a goniometer to allow their repositioning. A video system may be used for optical examination of the sample, and a knife edge may be used to prevent X-ray radiation from reaching a sample adjacent to the sample positioned at the sample location. A controller may be used to automatically control the operation of the analysis components and the movement of the sample holder to as to allow automated analysis of all of the samples in the sample holder.

Claims

1. An analysis system for examining the structure of a sample mounted in a sample holder, the system comprising:

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

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

a Raman probe that detects photon energy scattered from the sample as a result of Raman excitation of the sample.

2. An analysis system according to claim 1 further comprising a goniometer to which the X-ray source and X-ray detector are connected.

3. An analysis system according to claim 2 wherein the X-ray source and X-ray detector are mounted to two different circles of the goniometer.

4. An analysis system according to claim 2 wherein the X-ray source and the Raman probe are mounted to the same circle of the goniometer.

5. An analysis system according to claim 1 further comprising a video apparatus for optical examination of the sample.

6. An analysis system according to claim 1 further comprising a movable sample support that supports sample holder while it is mounted in the analysis system.

7. An analysis system according to claim 6 wherein the sample support is movable in at least two perpendicular directions.

8. An analysis system according to claim 6 wherein the sample holder comprises a plurality of sample locations, each of which may contain an individual sample, and wherein the sample support may be moved to change which of the samples is located at a predetermined sample location.

9. An analysis system according to claim 8 further comprising a controller that controls the movement of sample support and operation of the X-ray source, the X-ray detector and the Raman probe so as to allow automated analysis of the samples on the sample holder.

10. An analysis system according to claim 1 further comprising a knife edge that may be located adjacent to the sample to block X-ray energy from reaching adjacent regions of the sample holder.

11. An analysis system according to claim 1 wherein the Raman probe and the knife edge are both mounted to a common movement stage such that they may be moved in unison.

12. An analysis system for examining the structure of a sample mounted in a sample holder having a plurality of adjacent sample locations, the system comprising:

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

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

a Raman probe that detects photon energy scattered from the sample as a result of Raman excitation of the sample;

a goniometer to which the X-ray source and X-ray detector are connected; and

a movable sample support that supports sample holder while it is mounted in the analysis system and that is movable in at least two perpendicular directions to change which of the samples is located at a predetermined sample location.

13. A method of examining the structure of a sample mounted in a sample holder, the method comprising:

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

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

inducing a Raman excitation in the sample and detecting photon energy scattered from the sample as a result of the Raman excitation.

14. A method according to claim 13 further comprising locating the X-ray source and X-ray detector on a goniometer.

15. A method according to claim 14 wherein the X-ray source and X-ray detector are mounted to two different circles of the goniometer.

16. A method according to claim 15 wherein the X-ray source and the Raman probe are mounted to the same circle of the goniometer.

17. A method according to claim 13 further comprising optically examining the sample with a video apparatus.

18. A method according to claim 13 further comprising supporting the sample holder while it is mounted in the analysis system with a movable sample support.

19. A method according to claim 18 wherein the sample support is movable in at least two perpendicular directions.

20. A method according to claim 18 wherein the sample holder comprises a plurality of sample locations, each of which may contain an individual sample, and wherein the method further comprising moving the sample support to change which of the samples is located at a predetermined sample location.

21. A method according to claim 20 further comprising controlling the movement of sample support and operation of the X-ray source, the X-ray detector and the Raman probe with a controller so as to allow automated analysis of the samples on the sample holder.

22. A method according to claim 13 further comprising locating a knife edge adjacent to the sample to block X-ray energy from reaching adjacent regions of the sample holder.

23. A method according to claim 13 wherein the Raman probe and the knife edge are both mounted to a common movement stage such that they may be moved in unison.