Method and apparatus for resolution and sensitivity enhanced atomic force microscope based infrared spectroscopy

Patent metadata

Field	Value
Publication number	US-11714103-B2
Application number	US-202117171652-A
Country	US
Kind code	B2
Filing date	Feb 9, 2021
Priority date	Oct 29, 2016
Publication date	Aug 1, 2023
Grant date	Aug 1, 2023

Abstract

Methods and apparatus for obtaining extremely high sensitivity chemical composition maps with spatial resolution down to a few nanometers. In some embodiments these chemical composition maps are created using a combination of three techniques: (1) Illuminating the sample with IR radiation than is tuned to an absorption band in the sample; and (2) Optimizing a mechanical coupling efficiency that is tuned to a specific target material; (3) Optimizing a resonant detection that is tuned to a specific target material. With the combination of these steps it is possible to obtain (1) Chemical composition maps based on unique IR absorption; (2) spatial resolution that is enhanced by extremely short-range tip-sample interactions; and (3) resonant amplification tuned to a specific target material. In other embodiments it is possible to take advantage of any two of these steps and still achieve a substantial improvement in spatial resolution and/or sensitivity.

First claim

We claim:

1. A method of mapping a surface of a heterogeneous sample comprising the steps of:
a. Interacting a probe of a probe microscope with a region of the sample;
b. Illuminating the sample with a beam infrared radiation wherein the beam is modulated at a frequency f m ;
c. Measuring a phase of oscillation of the probe while interacting with the sample region;
d. Tuning the modulation frequency f m based on the phase measurement by maintaining the phase at a phase setpoint;
e. Measuring a probe response to infrared radiation incident on the region of the sample; and
f. Making a map of the distribution of at least one material component in the sample, wherein the map has a spatial resolution of less than 10 nm.

2. The method of claim 1 wherein the probe is oscillated at a frequency f l and the probe response is measured at a sideband frequency between f m and f l .

3. The method of claim 2 wherein the phase measurement is performed at a sideband frequency.

4. The method of claim 3 wherein the phase measurement is used to adjust the modulation frequency f m to ensure that the sideband frequency substantially corresponds to a probe resonance.

5. The method of claim 1 wherein the frequency f m substantially corresponds to a resonance of the probe.

6. The method of claim 5 wherein a phase locked loop is used to adjust the modulation frequency f m based on the phase measurement.

7. The method of claim 1 further comprising the step of measuring an amplitude of the probe response, wherein the amplitude measurement is performed either concurrently with the phase measurement or subsequent to Step e.).

8. The method of claim 1 wherein the phase measurement is performed at a mechanically excited resonance of the probe.

9. The method of claim 8 wherein the phase measurement is inferred from at least one of an amplitude and the phase measurement.

10. The method of claim 9 wherein a piezoactuator mechanically excites the resonance of the probe.

11. The method of claim 1 wherein the phase measurement is performed at at least one of the frequency f l and the sideband frequency.

12. A method of mapping a surface of a heterogeneous sample comprising the steps of:
a. Interacting a probe of a probe microscope with a region of the sample;
b. Illuminating the sample with a beam infrared radiation wherein the beam is modulated at a frequency f m ;
c. Measuring a phase of oscillation of the probe while interacting with the sample region;
d. Tuning the modulation frequency f m based on the phase measurement;
e. Measuring a probe response to infrared radiation incident on the region of the sample; and
further comprising the step of making a map of the distribution of at least one material component in the sample; and wherein the map has a spatial resolution of less than 10 nm.

13. A method of mapping a surface of a heterogeneous sample comprising the steps of:
Interacting a probe of a probe microscope with a region of the sample;
Illuminating the sample with a beam infrared radiation wherein the beam is modulated at a frequency f m ;
Measuring a phase of oscillation of the probe while interacting with the sample region;
Tuning the modulation frequency f m based on the phase measurement;
Measuring a probe response to infrared radiation incident on the region of the sample; and
wherein the probe is oscillated at a frequency f l and the probe response is measured at a sideband frequency between f m and f l .

14. The method of claim 13 wherein a phase locked loop is used to adjust the modulation frequency f m based on the phase measurement.

15. The method of claim 13 wherein the phase measurement is performed at a sideband frequency.

16. The method of claim 15 wherein the phase measurement is used to adjust the modulation frequency f m to ensure that the sideband frequency substantially corresponds to a probe resonance.

17. The method of claim 13 wherein the sideband frequency substantially corresponds to a resonance of the probe.

18. The method of claim 13 wherein the phase measurement is performed at a mechanically excited resonance of the probe.

19. The method of claim 18 , wherein the phase measurement is inferred from at least one of an amplitude and the phase measurement.

20. The method of claim 19 , wherein a piezoactuator mechanically excites the resonance of the probe.

21. The method of claim 13 wherein the phase measurement is performed at at least one of the frequency f l and the sideband frequency.

22. The method of claim 13 wherein the sample region is immersed in a liquid.

Assignees

• Bruker Nano Inc

Inventors

• Prater Craig
• Kjoller Kevin

Classifications

• G01Q30/02 Primary

  Non-SPM analysing devices, e.g. SEM [Scanning Electron Microscope], spectrometer or optical microscope · CPC title

• G01N21/35

  using infrared light (G01N21/39 takes precedence) · CPC title

• G01N21/3563

  for analysing solids; Preparation of samples therefor · CPC title

• G01Q60/34

  Tapping mode · CPC title

• G01N2201/0612

  Laser diodes · CPC title