Apparatus for determining a thermal conductivity and a thermal diffusivity of a material, and related methods

Patent metadata

Field	Value
Publication number	US-10578569-B2
Application number	US-201615345330-A
Country	US
Kind code	B2
Filing date	Nov 7, 2016
Priority date	Nov 7, 2016
Publication date	Mar 3, 2020
Grant date	Mar 3, 2020

Abstract

A method of determining a thermal conductivity and a thermal diffusivity of a material comprises exposing a specimen comprising a substrate of a material and a metallic film over the substrate to an amplitude modulated pump laser beam comprising electromagnetic radiation having a first wavelength and a first modulation frequency to form a pump spot on the metallic film. The specimen is exposed to a probe laser beam comprising electromagnetic radiation having a second wavelength to form a probe spot on the metallic film. A phase shift between the pump laser beam and a reflected probe laser beam is measured while scanning the pump spot relative to the probe spot. A modulation frequency of the pump laser beam is changed to a second modulation frequency and the pump spot is scanned relative to the probe spot while detecting the phase shift. A phase profile of the material is measured and a continuum-based model is fit to the phase profile. Related microscopes and related methods are also disclosed.

First claim

What is claimed is:

1. A method of determining a thermal conductivity and a thermal diffusivity of a material, the method comprising:
exposing a specimen comprising a substrate of a material and a metallic film over the substrate to an amplitude modulated pump laser beam comprising electromagnetic radiation having a first wavelength and a first modulation frequency to form a pump spot on the metallic film;
exposing the specimen to a probe laser beam comprising electromagnetic radiation having a second wavelength to form a probe spot on the metallic film;
measuring a thermal wave phase shift between the pump laser beam and a reflected probe laser beam while scanning the pump spot relative to the probe spot;
changing a modulation frequency of the pump laser beam to a second modulation frequency and scanning the pump spot relative to the probe spot while measuring the thermal wave phase shift between the pump laser beam and the reflected probe laser beam;
determining at least one phase profile of the material, the at least one phase profile comprising a relationship between the thermal wave phase shift and a scan distance between the pump laser beam and the reflected probe laser beam at each of the first modulation frequency and the second modulation frequency;
measuring a phase offset between the pump laser beam and the probe laser beam at the first modulation frequency and the second modulation frequency after moving the probe spot; and
determining a thermal conductivity and a thermal diffusivity of the substrate based, at least in part, on the at least one phase profile of the material.

2. The method of claim 1 , further comprising scanning the pump spot relative to the probe spot at each of at least three different frequencies of the pump laser beam.

3. The method of claim 1 , further comprising selecting the first modulation frequency and the second modulation frequency to be between about 1 kHz and about 100 kHz.

4. The method of claim 1 , wherein scanning the pump spot relative to the probe spot comprises moving the pump spot while maintaining a position of the probe spot.

5. The method of claim 1 , wherein exposing the specimen to an amplitude modulated pump laser beam comprises transmitting the pump laser beam from an emitter through a confocal lens pair, the confocal lens pair comprising a first lens separated from a second lens by a distance equal to about a sum of a focal length of the first lens and the second lens.

6. The method of claim 5 , wherein scanning the pump spot relative to the probe spot comprises disposing the emitter and the first lens on a movable stage configured to move in a first direction orthogonal to a direction between the first lens and the second lens and a second direction orthogonal to the direction between the first lens and the second lens.

7. The method of claim 1 , wherein scanning the pump spot comprises transmitting the pump laser beam to an objective lens and changing an angle of incidence of the pump laser beam to change a position of the pump spot on the metallic film.

8. The method of claim 1 , further comprising selecting the substrate material to comprise a nuclear fuel and selecting the metallic film to comprise one or more of gold, aluminum, titanium, or copper.

9. The method of claim 1 , wherein scanning the pump spot relative to the probe spot comprises changing a distance between the pump spot and the probe spot on the metallic film from between about 0 μm to about 20 μm.

10. The method of claim 1 , wherein measuring a phase offset between the pump laser beam and the probe laser beam further comprises determining the phase offset of the pump laser beam due to instrumentation.

11. The method of claim 10 , further comprising determining a phase offset between the pump laser beam and the reflected probe laser beam while the pump laser beam is at a third modulation frequency greater than the first modulation frequency and the second modulation frequency.

12. The method of claim 11 , further comprising determining a contact resistance between the substrate and the metallic film based, at least in part, on the phase offset between the pump laser beam and the reflected probe laser beam at the third modulation frequency.

13. The method of claim 1 , further comprising forming the metallic film on the substrate by sputter deposition.

14. The method of claim 13 , wherein forming the metallic film on the substrate by sputter deposition comprises forming the metallic film on the substrate while the substrate is in a hot cell.

15. The method of claim 1 , further comprising determining a convolved spot size of the probe laser beam and the pump laser beam.

16. The method of claim 1 , further comprising moving the probe spot on a surface of the metallic film after determining the thermal conductivity and the thermal diffusivity of the substrate.

17. The method of claim 1 , further comprising determining a standard deviation of the determined thermal conductivity and the determined thermal diffusivity.

18. An apparatus for determining at least one of a thermal conductivity and a thermal diffusivity of a material, the apparatus comprising:
a pump laser configured to transmit a pump laser beam comprising amplitude modulated electromagnetic radiation having a first wavelength to a specimen comprising a metallic film overlying a substrate of a material;
a first lens and a second lens disposed between the pump laser and the material and positioned such that the pump laser beam passes from the first lens to the second lens prior to contacting the metallic film;
a stage operably coupled to the pump laser and the first lens and configured to move the first lens and the pump laser relative to the second lens;
a probe laser configured to transmit a probe laser beam comprising electromagnetic radiation having a second wavelength;
a detector operably coupled to a lock in amplifier configured to measure a phase offset between the pump laser beam and a reflected probe laser beam reflected from the metallic film; and
a processor operably coupled to the lock in amplifier and configured to determine a thermal conductivity and a thermal diffusivity of the substrate material based, at least in part, on at least one phase profile of the substrate material.

19. The apparatus of claim 18 , wherein a distance between the first lens and the second lens is equal to about a sum of a focal length of the first lens and the second lens.

20. The apparatus of claim 18 , further comprising a movable stage configured to move in a first direction and a second direction, each of the first direction and the second direction orthogonal to a direction between the first lens and the second lens.

21. The apparatus of claim 18 , further comprising a polarizing beam splitter between the probe laser and a sample.

22. The apparatus of claim 18 , further comprising a quarter waveplate between the pump laser and the substrate and between the probe laser and the substrate material.

23. A method of determining a thermal conductivity and a thermal diffusivity of a material, the method comprising:
exposing a specimen comprising a substrate of a material and a metallic film over the substrate to an amplitude modulated pump laser beam comprising electromagnetic radiation having a first wavelength and a first modulation frequency to form a pump spot on the metallic film;
exposing the specimen to a probe laser beam comprising electromagnetic radiation having a second wave

Assignees

• Battelle Energy Alliance Llc

Inventors

• Hurley David H
• Schley Robert S
• Khafizov Marat

Classifications

• G01N25/18 Primary

  by investigating thermal conductivity (by calorimetry G01N25/20; by measuring change of resistance of an electrically-heated body G01N27/18) · CPC title