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

Patent metadata

Field	Value
Publication number	US-10914755-B2
Application number	US-201916351223-A
Country	US
Kind code	B2
Filing date	Mar 12, 2019
Priority date	Oct 29, 2016
Publication date	Feb 9, 2021
Grant date	Feb 9, 2021

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 with a probe of a scanning probe microscope comprising the steps of:
a. Oscillating the probe at a first frequency f 1 ;
b. Interacting the probe with a region of the sample;
c. Measuring a phase of oscillation of the probe while interacting with the sample region;
d. Adjusting one or more probe interaction parameter based on the phase measurement;
e. Illuminating the sample with a beam infrared radiation wherein the beam is modulated at a frequency f m ;
f. Tuning the modulation frequency f m such that a sideband frequency between f 1 and f m is substantially equal to a resonance of the probe while interacting with the sample region; and
g. Measuring a probe response to infrared radiation incident on the sample region.

2. The method of claim 1 further comprising the steps of repeating steps a-g on a second region of the sample comprising a second material component.

3. The method of claim 1 wherein the measured phase is measured at frequency f 1 .

4. The method of claim 1 wherein the probe microscope is operated in an amplitude modulation mode wherein feedback loop attempts to maintain an amplitude of probe oscillation at f 1 at a given setpoint amplitude.

5. The method of claim 1 wherein the probe interaction adjusting step substantially maximizes the measured probe response at the sideband frequency.

6. The method of claim 1 wherein the probe interaction adjusting step substantially maximizes a phase contrast between two or more material components in the sample.

7. The method of claim 1 wherein the measured phase is measured at a sideband frequency between f 1 and f m .

8. The method of claim 1 wherein the phase measurement is performed at a sideband frequency between f 1 and f m and further comprising the step of tuning the radiation modulation frequency f m based on the phase measurement.

9. The method of claim 1 wherein steps d and f are performed substantially simultaneously to compensate for shifts in probe resonance due to changes in probe interaction parameters.

10. The method of claim 1 further comprising the step of tuning an emission wavelength of the radiation source to substantially overlap with an absorption band of at least one material component in the sample.

11. The method of claim 1 further comprising the step of making a map of the distribution of at least one material component in the sample.

12. The method of claim 1 wherein the map has a spatial resolution of less than 10 nm.

13. An apparatus for mapping a surface of a sample with a scanning probe microscope comprising:
a. A probe with a sharp tip:
b. A radiation source;
c. A radiation source modulator;
d. A probe response detector;
e. A processing element, the apparatus configured to:
a. Interact the sharp tip with the sample surface;
b. direct a beam from the light source at a region of the sample in the vicinity of the probe tip;
c. modulate the light beam at at least one frequency f m ;
d. measure a response of the probe to radiation incident on the sample;
e. determine at least one parameter of the probe response at at least one sideband frequency; and
f. automatically adjust at least one probe interaction parameter, wherein the probe interaction parameter is a phase of probe oscillation, and tune the modulation frequency f m .

14. The apparatus of claim 13 further comprising a probe actuator configured to oscillate the probe at frequency f 1 and wherein the lock-in amplifier is configured to determine a parameter of the probe response at a sideband frequency between f 1 and f m .

15. The apparatus of claim 13 further comprising a phase locked loop configured to adjust f m such that a sideband frequency between f 1 and f m substantially corresponds to a probe resonance.

16. The apparatus of claim 13 , further comprising a lock-in amplifier to determine the at least one parameter of the probe response.

Assignees

• Bruker Nano Inc

Inventors

• Prater Craig
• Kjoller Kevin

Classifications

• G01N2201/0612

  Laser diodes · CPC title

• G01N2201/12

  Circuits of general importance; Signal processing · CPC title

• 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

• G01Q60/34

  Tapping mode · CPC title