Process for performing automated mineralogy

• US 9,194,829 B2
• Filed: 12/28/2012
• Issued: 11/24/2015
• Est. Priority Date: 12/28/2012
• Status: Active Grant

• Current Assignee: FEI Company (Thermo Fisher Scientific Incorporated)
• Original Assignee: FEI Company (Thermo Fisher Scientific Incorporated)
• Inventors: Smith, Michael D., Moeller, Kurt
• Primary Examiner(s): Ippolito, Nicole
• Assistant Examiner(s): CHOI, JAMES J
• Application Number:
  US13/730,358
• Publication Number:
  US 20140183357A1
• Time in Patent Office: 1,061 Days
• US Class Current: 1/1
• CPC Class Codes: G01N 2223/072 combination of measurements, 2 kinds of secondary emission
• CPC Class Codes: G01N 2223/076 X-ray fluorescence
• CPC Class Codes: G01N 2223/079 incident electron beam and measuring excited X-rays
• CPC Class Codes: G01N 2223/305 computer simulations
• CPC Class Codes: G01N 2223/32 adjustments of elements during operation
• CPC Class Codes: G01N 2223/418 electron microscope
• CPC Class Codes: G01N 2223/616 earth materials
• CPC Class Codes: G01N 23/203 Measuring back scattering
• CPC Class Codes: G01N 23/2251 using incident electron beams, e.g. scanning electron microscopy [SEM]
• CPC Class Codes: G01N 23/2252 Measuring emitted X-rays, e.g. electron probe microanalysis [EPMA]
• CPC Class Codes: H01J 37/20 Means for supporting or positioning the objects or the material; Means for adjusting diaphragms or lenses associated with the support introducing the objects H01J37/18
• CPC Class Codes: H01J 37/21 Means for adjusting the focus adjusting the focus while observing the image by photographic or optical means H01J37/22; means for observing the object or the point of impact on the object in tubes for the localised treatment of materials H01J37/3005

Abstract

A method and system for determining the mineral content of a sample using an electron microscope. The method includes directing an electron beam toward an area of interest of a sample, the area of interest comprising an unknown composition of minerals. The working distance between the backscattered electron detector of the microscope and the area of interest of the sample is determined. Compensation is made for the difference between the working distance and a predetermined working distance in which the predetermined working distance being the working distance that provides desired grayscale values for detected backscattered electrons. One way of compensating for working distance variation is to used an autofocus feature of the microscope to adjust the working distance. Backscattered electrons from the area of interest of the sample are then detected.

Claims

1. A method for determining mineral contents of samples using an electron microscope, said method comprising:

directing an electron beam toward a surface of a first sample comprising an unknown composition of minerals;

determining a first working distance, the first working distance being the distance between a backscattered electron detector of the electron microscope and the surface of the first sample, by determining a focal distance of the surface of the first sample using an auto-focus feature of the electron microscope;

compensating for the difference between the first working distance and a predetermined working distance, the predetermined working distance being the working distance that provides desired grayscale values for detected backscattered electrons; and

detecting backscattered electrons from the surface of the first sample.

2. The method of claim 1, further comprising:

directing an electron beam toward a surface of a second sample comprising an unknown composition of minerals;

determining a second working distance, the second working distance being the distance between the backscattered electron detector and surface of the second sample;

compensating for the difference between the second working distance and the first working distance; and

detecting backscattered electrons from the surface of the second sample.

3. The method of claim 2, in which determining the second working distance further comprises determining a focal distance of the surface of the second sample, the focal distance being determined using an auto-focus feature of the electron microscope.

4. The method of claim 1, in which compensating for the difference between the first working distance and a predetermined working distance further comprises adjusting a z-axis position of a sample stage and/or the backscattered electron detector so that there is substantially no difference between the first working distance and the predetermined working distance.

5. The method of claim 1, in which compensating for the difference between the first working distance and a predetermined working distance further comprises:

modeling an effect of a plurality of working distance variations on detected backscattered electron grayscale levels;

calculating a backscattered electron grayscale level adjustment based on the difference between the first working distance and the predetermined working distance; and

adjusting one or more of the detected backscattered electron grayscale levels based on the calculated backscattered electron grayscale level adjustment.

6. The method of claim 2, in which compensating for the difference between the second working distance and the first working distance further comprises:

modeling an effect of a plurality of working distance variations on detected backscattered electron grayscale levels;

calculating a backscattered electron grayscale level adjustment based on the difference between the second working distance and the first working distance; and

adjusting one or more of the detected backscattered electron grayscale levels based on the calculated backscattered electron grayscale level adjustment.

7. The method of claim 1, further comprising determining the mineral composition of the first sample where the electron beam irradiates the surface of the first sample based on detected backscattered electron grayscale levels.

8. The method of claim 2, further comprising:

determining the mineral composition of the first sample where the electron beam irradiates the surface of the first sample based on detected backscattered electron grayscale levels from the first sample; and

determining the mineral composition of the second sample where the electron beam irradiates the surface of the second sample based on detected backscattered electron grayscale levels from second sample.

9. The method of claim 1, further comprising:

detecting energies of x-rays emitted in response to the electron beam; and

determining the mineral composition of the first sample where the electron beam irradiates the surface of the first sample based on detected backscattered electron grayscale levels and the detected x-ray energies.

10. A method for determining mineral contents of samples using an electron microscope, said method comprising:

directing an electron beam toward a surface of a first sample comprising an unknown composition of minerals;

determining a first focal distance of the surface of the first sample, the first focal distance being determined using an auto-focus feature of the electron microscope;

determining a first working distance based on the first focal distance, the first working distance being the distance between a backscattered electron detector of the electron microscope and the surface of the first sample;

detecting backscattered electrons from the surface of the first sample;

directing an electron beam toward a surface of a second sample comprising an unknown composition of minerals;

determining a second focal distance of the surface of the second sample, the second focal distance being determined using the auto-focus feature of the electron microscope;

determining a second working distance based on the second focal distance, the second working distance being the distance between the backscattered electron detector of the electron microscope and the surface of the second sample;

adjusting a z-axis position of a sample stage and/or the backscattered electron detector so that there is substantially no difference between the second working distance and the first working distance; and

detecting backscattered electrons from the surface of the second sample.

11. A system for determining mineral contents of samples using a scanning electron microscope, said system comprising:

a scanning electron microscope;

one or more energy dispersive x-ray detectors;

a backscattered electron detector of the scanning electron microscope;

a system controller, the system controller comprising a computer processor and a non-transitory computer-readable medium, the non-transitory computer-readable medium being encoded with computer instructions that, when executed by the computer processor, cause the system controller to perform the steps of;

directing an electron beam toward a surface of a first sample comprising an unknown composition of minerals;

determining a first working distance, the first working distance being the distance between a backscattered electron detector and the surface of the first sample, by determining a focal distance of the surface of the first sample using an auto-focus feature of the scanning electron microscope;

compensating for the difference between the first working distance and a predetermined working distance, the predetermined working distance being the working distance that provides desired grayscale values for detected backscattered electrons; and

detecting backscattered electrons from a region of the surface of the first sample.

12. The system of claim 11, further comprising computer instructions for:

directing an electron beam toward a surface of a second sample comprising an unknown composition of minerals;

determining a second working distance, the second working distance being the distance between the backscattered electron detector and the surface of the second sample;

compensating for the difference between the second working distance and the first working distance; and

detecting backscattered electrons from a region of the surface of the second sample.

13. The system of claim 12, in which the computer instructions for determining the second working distance further comprise computer instructions for determining a focal distance of the surface of the second sample, the focal distance being determined using an auto-focus feature of the scanning electron microscope.

14. The system of claim 11, in which the computer instructions for compensating for the difference between the first working distance and a predetermined working distance further comprise computer instructions for adjusting a z-axis position of a sample stage and/or the backscattered electron detector so that there is substantially no difference between the first working distance and the predetermined working distance.

15. The system of claim 11, in which the computer instructions for compensating for the difference between the first working distance and a predetermined working distance further comprises computer instructions for:

modeling an effect of a plurality of working distance variations on detected backscattered electron grayscale levels;

calculating a backscattered electron grayscale level adjustment based on the difference between the first working distance and the predetermined working distance; and

adjusting one or more of the detected backscattered electron grayscale levels based on the calculated backscattered electron grayscale level adjustment.

16. The system of claim 12, in which the computer instructions for compensating for the difference between the second working distance and the first working distance further comprises computer instructions for:

modeling an effect of a plurality of working distance variations on detected backscattered electron grayscale levels;

calculating a backscattered electron grayscale level adjustment based on the difference between the second working distance and the first working distance; and

adjusting one or more of the detected backscattered electron grayscale levels based on the calculated backscattered electron grayscale level adjustment.

17. The system of claim 11, further comprising computer instructions for determining the mineral composition of the first sample at the region of the surface of the first sample based on the detected backscattered electrons.

18. The system of claim 12, further comprising computer instructions for:

determining a mineral composition of the first sample at the region of the surface of the first sample based on the detected backscattered electrons from the first area of interest; and

determining a mineral composition of the second sample at the region of the surface of the second sample based on the detected backscattered electrons from second area of interest.

19. The system of claim 11, further comprising computer instructions for:

detecting energies of x-rays emitted in response to the electron beam; and

determining the mineral composition of the first sample at the region of the surface of the first sample based on detected backscattered electron grayscale levels and the detected x-ray energies.