X-ray diffractometer having co-exiting stages optimized for single crystal and bulk diffraction

• US 7,848,489 B1
• Filed: 04/02/2009
• Issued: 12/07/2010
• Est. Priority Date: 04/02/2009
• Status: Active Grant

• Current Assignee: Bruker AXS Incorporated (Bruker Corporation)
• Original Assignee: Broker AXS Incorporated
• Inventors: Schwarz, Gerald T., He, Bob B.
• Primary Examiner(s): Glick; Edward J
• Assistant Examiner(s): Midkiff; Anastasia
• Application Number:
  US12/417,032
• Time in Patent Office: 614 Days
• Field of Search: 378 70- 81
• US Class Current: 378/79
• CPC Class Codes: G01N 23/207 Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions

Abstract

A diffractometer for X-ray diffraction measurements has two co-exiting sample stages which are mounted on the goniometer base simultaneously. A rotation stage is used for single crystal X-ray diffraction and an XYZ stage is used for general X-ray diffraction with bulky samples. The driving bases of both stages are located away from the instrument center so the measuring space in the vicinity of the instrument center is available to either of the two sample stages. With this arrangement, the rotation axis of the rotation stage stays aligned to the instrument center even when the XYZ stage is used for data collection. Therefore, realigning of the rotation stage to the instrument center is not necessary when switching the applications between the two stages.

Claims

1. An X-ray diffractometer comprising:

a base;

a first stage that is attached to the base and rotates around an ω

axis;

a rotation stage that holds a crystal in a position suitable for a diffraction measurement and is mounted on the first stage at a first predetermined distance from the ω

axis; and

an XYZ stage that holds large and multiple samples in a position suitable for a diffraction measurement and is mounted on the first stage at a position diametrically opposed to the rotation stage and at a second predetermined distance from the ω

axis, both the rotation stage and the XYZ stage being mounted on the first stage during an X-ray diffraction measurement.

2. The diffractometer of claim 1 having an instrument center located along the ω

axis and wherein the first and second predetermined distances are sufficiently large to allow a crystal mounted on the rotation stage to be positioned at the instrument center without interference from the XYZ stage and to allow a sample mounted on the XYZ stage to be positioned at the instrument center without interference from the rotation stage.

3. The diffractometer of claim 1 wherein the rotation stage comprises a base mounted on the first stage and a goniometer head removably attached to the base in a manner that the goniometer head can be removed and reattached to the base without re-aligning the diffractometer.

4. The diffractometer of claim 3 wherein the base is mounted on the first stage in a position where the goniometer head can be removed and a diffraction measurement can be made with the XYZ stage without removing the base from the first stage.

5. The diffractometer of claim 1 wherein the XYZ stage can be moved into a position where the rotation stage can be used to perform a measurement without removing the XYZ stage from the first stage.

6. An X-ray diffractometer comprising:

a base;

an X-ray source attached to the base;

a first stage that is attached to the base and rotates around an ω

axis;

a second stage that is attached to the base and rotates around a 2θ

axis;

an X-ray detector attached to the second stage;

a rotation stage that holds a crystal in a position suitable for a diffraction measurement and is mounted on the first stage at a first predetermined distance from the ω

axis; and

an XYZ stage that holds large and multiple samples in a position suitable for a diffraction measurement and is mounted on the first stage at a position diametrically opposed to the rotation stage and at a second predetermined distance from the ω

axis, both the rotation stage and the XYZ stage being mounted on the first stage during an X-ray diffraction measurement.

7. The diffractometer of claim 6 having an instrument center located along the ω

axis and wherein the first and second predetermined distances are sufficiently large to allow a crystal mounted on the rotation stage to be positioned at the instrument center without interference from the XYZ stage and to allow a sample mounted on the XYZ stage to be positioned at the instrument center without interference from the rotation stage.

8. The diffractometer of claim 6 wherein the rotation stage comprises a base mounted on the first stage and a goniometer head rotating around a φ

axis and removably attached to the base in a manner that the goniometer head can be removed and reattached to the base without re-aligning the diffractometer.

9. The diffractometer of claim 8 wherein the base is mounted on the first stage in a position where the goniometer head can be removed and a diffraction measurement can be made with the XYZ stage without removing the base from the first stage.

10. The diffractometer of claim 6 wherein the XYZ stage can be moved into a position where the rotation stage can be used to perform a measurement without removing the XYZ stage from the first stage.

11. A method for making X-ray diffraction measurements on an X-ray diffractometer having a rotation stage that holds a crystal in a position suitable for a diffraction measurement and an XYZ stage that holds large and multiple samples in a position suitable for a diffraction measurement both stages being mounted on a stage that rotates around an ω

axis, the method comprising;

(a) moving the XYZ stage away from the ω

axis without removing the XYZ stage from the stage that rotates around the ω

axis;

(b) mounting a goniometer head that rotates around a φ

axis on the rotation stage;

(c) mounting the crystal sample on the goniometer head and aligning the sample to an instrument center; and

(d) performing a single crystal X-ray diffraction measurement.

12. The method of claim 11 further comprising:

(e) removing the goniometer head from the rotation stage, leaving the rotation stage mounted on the stage that rotates around the ω

axis;

(f) moving the XYZ stage towards the ω

axis;

(g) mounting a sample on the XYZ stage and aligning the sample to the instrument center; and

(h) performing an X-ray diffraction measurement on the sample.