Combinatorial screening system and X-ray diffraction and Raman spectroscopy

• US 7,269,245 B2
• Filed: 07/21/2005
• Issued: 09/11/2007
• 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, Burgäzy, Frank W., Frampton, Christopher S.
• Primary Examiner(s): Ho; Allen C.
• Application Number:
  US11/186,390
• Publication Number:
  US 20060023837A1
• Time in Patent Office: 782 Days
• Field of Search: 378/71, 378/73, 378/76, 378/79, 378/80, 378/81, 378/70, 356/301
• US Class Current: 378/71
• 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 samples in a library of samples mounted in a sample holder, the system comprising:

a movable sample support that moves the sample holder to position a sample in the library at a test location;

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;

an optical source that directs photon energy toward the sample to produce a Raman excitation of the sample;

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

a mounting system for the X-ray detector and the Raman probe that movably positions at least one of the X-ray detector and the Raman probe relative to the test location; and

a controller that, for each sample in the sample library, controls the movable sample support, the X-ray source, the X-ray detector, the Raman probe and the mounting system to move the at least one of the X-ray detector and the Raman probe into position to make an X-ray diffraction measurement and perform the X-ray diffraction measurement on that sample and to move the at least one of the X-ray detector and the Raman probe into position to make a Raman measurement and perform the Raman measurement on that sample without reloading and realigning the sample holder in the analysis system.

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 wherein the sample support is movable in at least two perpendicular directions.

7. An analysis system according to claim 1 wherein the sample support 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 the test location.

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

9. 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 move in unison.

10. An analysis system for examining the structure of samples in a library of samples 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 a sample;

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

an optical source that directs photon enemy toward the sample to produce a Raman excitation of 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 detector and the Raman probe are connected and which movably positions at least one of the X-ray detector and the Raman probe relative to the sample locations;

a movable sample support that supports the 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; and

a controller that, for each sample in the sample library, controls the movable sample support, the X-ray source, the X-ray detector, the Raman probe and the goniometer to move that sample to the predetermined sample location and to move the at least one of the X-ray detector and the Raman probe into position to make an X-ray diffraction measurement and perform the X-ray diffraction measurement on that sample and to move the at least one of the X-ray detector and the Raman probe into position to make a Raman measurement and perform the Raman measurement on that sample so that measurements are made with both the X-ray detector and the Raman probe without reloading and realigning the sample holder in the analysis system.

11. A method of examining the structure of samples in a library of samples mounted in a sample holder, the method comprising:

supporting the sample holder with a movable sample support;

moving the sample support to position a sample in the library at a test location;

movably positioning at least one of an X-ray detector and a Raman probe relative to the test location to perform an X-ray diffraction measurement;

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

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

movably positioning at least one of the X-ray detector and the Raman probe relative to the test location to perform a Raman spectroscopy measurement;

inducing a Raman excitation in the sample by directing photon energy from an optical source toward the sample and detecting photon energy scattered from the sample as a result of the Raman excitation with the Raman probe; and

repeating the preceding steps for each sample in the sample library so that measurements of each sample in the sample library are made with both the X-ray detector and the Raman probe without reloading and realigning the sample holder.

12. A method according to claim 11 further comprising locating the X-ray source and X-ray detector on a goniometer.

13. A method according to claim 12 wherein the X-ray source and X-ray detector are mounted to two different circles of the goniometer.

14. A method according to claim 13 wherein the X-ray source and the Raman probe are mounted to the same circle of the goniometer.

15. A method according to claim 11 further comprising optically examining the sample with a video apparatus.

16. A method according to claim 11 wherein the sample support is movable in at least two perpendicular directions.

17. A method according to claim 11 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 the test location.

18. A method according to claim 17 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.

19. A method according to claim 11 further comprising locating a knife edge adjacent to the sample to block X-ray energy from reaching adjacent regions of the sample holder.

20. A method according to claim 11 wherein the Raman probe and the knife edge are both mounted to a common movement stage such that they move in unison.