Ultra-low level standard for concentration measurements

• US 5,841,016 A
• Filed: 09/12/1996
• Issued: 11/24/1998
• Est. Priority Date: 09/12/1996
• Status: Expired due to Fees

• Current Assignee: Advanced Micro Devices, Inc.
• Original Assignee: Advanced Micro Devices, Inc.
• Inventors: Lowell, John, Hossain, Tim Z.
• Primary Examiner(s): Biegel, Ronald L.
• Assistant Examiner(s): AMROZOWICZ, PAUL DOUGLAS
• Application Number:
  US08/712,715
• Time in Patent Office: 803 Days
• Field of Search: 73/1.01, 250/252.1, 378/207
• US Class Current: 73/1.01
• CPC Class Codes: G01N 23/2251 using incident electron beams, e.g. scanning electron microscopy [SEM]

Abstract

Concentration measurement equipment is calibrated by performing a concentration measurement on a reference standard sample which includes a radioactive marker element. Because a count of decay products can be correlated with the number of atoms of the radioactive marker element, a precise count of decay products of the radioactive marker element is used to calculate an otherwise unknown number of atoms of the radioactive marker element on the reference standard sample. The calculated number of atoms of radioactive marker element is then used to calibrate a concentration measurement of the radioactive marker element by the concentration measurement device. Suitable radioactive marker elements for use in calibrating concentration measurement equipment include Pm-147 and Tc-99. Materials, methods and systems in accordance with the teachings of the invention are useful for calibrating concentration measurements and measurement equipment, including Total X-ray Fluorescence (TXRF) and Time Of Flight-Secondary Ion Mass Spectroscopy (TOF-SIMS) measurements and measurement equipment.

Claims

1. A reference standard material for calibrating a concentration measurement apparatus, the reference standard material comprising:

a substrate; and

a radioactive marker element detectable by the concentration measurement apparatus for calibration thereof, the radioactive marker element being on the substrate, having a known half-life, and in an amount sufficient for reliable detection of radioactive decay products thereof.

2. A reference standard material, as recited in claim 1, wherein a flux of decay products of the radioactive marker element provides a precise indication of a number of atoms of the radioactive marker element on the substrate.

3. A reference standard material, as recited in claim 1, wherein the radioactive marker element is a non-naturally occurring element.

4. A reference standard material, as recited in claim 1, wherein the radioactive marker element is Pm-147.

5. A reference standard material, as recited in claim 1, wherein the radioactive marker element is Tc-99.

6. A reference standard material, as recited in claim 1, wherein the radioactive marker element is a naturally occurring element.

7. A reference standard material, as recited in claim 1, wherein the radioactive marker element is Fe-55.

8. A reference standard material, as recited in claim 1, wherein the radioactive decay products are substantially limited to radioactive decay products of a type and flux for which for which shielding is substantially unnecessary for personnel safety.

9. A reference standard material, as recited in claim 1, wherein the radioactive decay products are substantially limited to β

-particles.

10. A reference standard material, as recited in claim 1, wherein the radioactive decay products are substantially limited to X-rays.

11. A reference standard material, as recited in claim 1, wherein the half-life of the radioactive marker element and amount thereof are such that a flux of decay products impinging on a detector therefor is reliably measurable to a precision of one part in one hundred.

12. A reference standard material, as recited in claim 1,

wherein decay products of the radioactive marker element include β

-particles; and

wherein the radioactive marker element has a half-life longer than a week and shorter than ten years.

13. A reference standard material, as recited in claim 1,

wherein decay products of the radioactive marker element include β

-particles; and

wherein the radioactive marker element has a half-life longer than one year and shorter than five years.

14. A reference standard material, as recited in claim 1,

wherein decay products of the radioactive marker element include β

-particles; and

wherein the radioactive marker element has a half-life longer than two years and shorter than three years.

15. A reference standard material, as recited in claim 1, supplied in association with a calculated concentration of t he radioactive marker element and an indication of a time at which the concentration of the radioactive marker element is baselined.

16. A method for calibrating a concentration measurement apparatus, the method comprising the steps of:

providing a reference standard sample including a radioactive marker element having a known half-life;

measuring a flux of radioactive decay products from the reference standard sample;

measuring a concentration of the radioactive marker element using the concentration measurement apparatus; and

calculating a calibration adjustment to the concentration measured in the concentration measuring step using the known half-life of the radioactive marker element and the radioactive decay product flux measured in the flux measuring step.

17. A method, as recited in claim 16, wherein the concentration measuring step is performed using Total X-Ray Fluorescence (TXRF) and the concentration measurement apparatus so calibrated is a TXRF apparatus.

18. A method, as recited in claim 16, wherein the concentration measuring step is performed using Time of Flight-Secondary Ion Mass Spectroscopy (TOFSIMS) and the concentration measurement apparatus so calibrated is a TOF-SIMS apparatus.

19. A method, as recited in claim 16, wherein the concentration measuring step is performed using Heavy Ion Backscattering (HIBS) and the concentration measurement apparatus so calibrated is a HIBS apparatus.

20. A method, as recited in claim 16,

wherein the radioactive decay products of the radioactive marker element are substantially limited to β

-particles; and

wherein the radioactive decay product measuring step is performed using β

-particle detector.

21. A method, as recited in claim 16,

wherein the concentration measuring step is performed using Total X-Ray Fluorescence (TXRF) and the concentration measurement apparatus so calibrated is a TXRF apparatus;

wherein the radioactive decay products of the radioactive marker element are substantially limited to X-rays; and

wherein the radioactive decay product measuring step is performed using an X-ray detector of the TXRF apparatus in passive mode.

22. A method, as recited in claim 16, wherein the calibration adjustment calculating step includes the steps of:

calculating, in accordance with radioactive decay equations, the concentration of the radioactive marker element using the known half-life of the radioactive marker element, the measured radioactive decay product flux, and time elapsed between the radioactive decay product flux measurement and the concentration measurement; and

calculating an adjustment factor for future concentration measurements based on a discrepancy between the concentration calculated in accordance with the radioactive decay equations and that measured using the concentration measurement apparatus.

23. A method, as recited in claim 22, wherein the radioactive decay product flux measurement is performed before the concentration measurement.

24. A method, as recited in claim 22, wherein the radioactive decay product flux measurement is performed after the concentration measurement.

25. A method, as recited in claim 22, wherein the radioactive decay product flux measurement is performed at approximately the same time as the concentration measurement.

26. An apparatus comprising:

a surface concentration measurement apparatus having a detector for generating a first signal indicative of a surface concentration measurement of an amount of a radioactive marker element on a reference standard sample; and

a calibration subsystem coupled to receive the first signal and to supply a calibration correction to the first signal using, in accordance with radioactive decay equations, a known half-life of the radioactive marker element and a measured radioactive decay product flux.

27. An apparatus, as recited in claim 26, wherein the calibration subsystem includes:

a decay product detector for generating a second signal indicative of the radioactive decay product flux from the radioactive marker element on the reference standard sample; and

a processor coupled to receive the second signal from the decay product detector, the processor configured to calculate the calibration correction based on a discrepancy between a radioactive marker element surface concentration calculated in accordance with the radioactive decay equations and the known half-life and that indicated by the first signal.

28. An apparatus, as recited in claim 26, further comprising:

storage coupled to receive the calibration correction from the calibration subsystem and coupled to supply the calibration correction for correction of a second signal from the detector, the second signal indicative of a surface concentration measurement of a non-reference sample.

29. An apparatus, as recited in claim 27, wherein the decay product detector includes a β

-particle detector.

30. An apparatus, as recited in claim 27, wherein the decay product detector includes an X-ray detector.

31. An apparatus, as recited in claim 26, wherein the surface concentration measurement apparatus includes a Total X-Ray Fluorescence (TXRF) apparatus.

32. An apparatus, as recited in claim 26, wherein the surface concentration measurement apparatus includes a Time Of Flight Secondary Ion Mass Spectrometer (TOF-SIMS) apparatus.

33. An apparatus, as recited in claim 26, wherein the radioactive decay products of the radioactive marker element are substantially limited to β

-particles, the measured radioactive decay product flux being an β

-particle measurement.

34. An apparatus, as recited in claim 27,

wherein the surface concentration measurement apparatus includes a Total X-Ray Fluorescence (TXRF) apparatus having an X-ray detector for detecting fluorescence X-rays in a surface concentration measurement mode;

wherein the radioactive decay products of the radioactive marker element are substantially limited to X-rays; and

wherein the decay product detector is an X-ray detector of the TXRF apparatus operating in a passive measurement mode.