High frequency deflection measurement of IR absorption with a modulated IR source

• US 8,680,467 B2
• Filed: 09/19/2011
• Issued: 03/25/2014
• Est. Priority Date: 05/15/2007
• Status: Active Grant

• Current Assignee: Bruker Nano, Inc. (Bruker Corporation)
• Original Assignee: Anasys Instruments Corp. (Bruker Corporation)
• Inventors: Prater, Craig, Kjoller, Kevin
• Primary Examiner(s): Porta, David
• Assistant Examiner(s): FEIN, ABRA S
• Application Number:
  US13/236,115
• Publication Number:
  US 20130036521A1
• Time in Patent Office: 918 Days
• Field of Search: 250/338.1, 850/56, 737/05
• US Class Current: 250/338.1
• CPC Class Codes: B82Y 35/00 Methods or apparatus for measurement or analysis of nanostructures
• CPC Class Codes: G01N 21/35 using infrared light G01N21/39 takes precedence
• CPC Class Codes: G01Q 30/02 Non-SPM analysing devices, e.g. SEM [Scanning Electron Microscope], spectrometer or optical microscope
• CPC Class Codes: G01Q 60/32 AC mode

Abstract

A method of obtaining submicron resolution IR absorption data from a sample surface. A probe microscope probe interacts with the sample surface while a tunable source of IR radiation illuminates the sample-tip interaction region. The source is modulated at a frequency substantially overlapping the resonant frequency of the probe and may be modulated at the contact resonance frequency of the probe when the probe is in contact with the sample surface. The modulation frequency is continually adjusted to account for shifts in the probe resonant frequency due to sample or other variations. A variety of techniques are used to observe such shifts and accomplish the adjustments in a rapid manner.

Claims

1. A method of obtaining measurements of infrared absorption of sub-micron regions of a sample with a probe microscope employing a cantilever probe with a tip, the method comprising:

a) illuminating a region of a sample with a tunable source of infrared radiation;

b) interacting the probe tip with a surface of the sample;

c) adjusting repeatedly a modulation frequency of the source of infrared radiation such that the modulation frequency substantially overlaps a resonant frequency of the cantilever probe and remains substantially overlapped as the cantilever resonant frequency shifts;

d) measuring a probe response resulting from absorption of infrared radiation by the sample.

2. The method of claim 1 wherein the resonant frequency corresponds to a contact resonance of the cantilever probe in contact with the sample surface.

3. The method of claim 2 wherein the contact resonant frequency of the cantilever probe is selected by performing a thermal tune of the cantilever probe.

4. The method of claim 3 wherein the thermal tune is performed in less than 1 second.

5. The method of claim 3 wherein the thermal tune is performed in less than 0.1 seconds.

6. The method of claim 3 wherein the thermal tune is performed by:

a. recording data indicative of a deflection of the cantilever over a period of time;

b. performing a fast Fourier transform on the data;

c. repeating steps a) and b);

d. averaging the fast Fourier transforms using root mean square averaging;

e. identifying a resonant frequency of the cantilever probe from a peak in the averaged fast Fourier transform.

7. The method of claim 1 wherein the tunable source of infrared radiation is at least one of a quantum cascade laser and an optical parametric oscillator.

8. The method of claim 1 wherein step d) is repeated at a plurality of wavelengths of the tunable source of infrared radiation to create an absorption spectrum of the submicron region of the sample.

9. The method of claim 1 wherein step d) is repeated at a plurality of positions on the sample surface to create an absorption map of the sample surface.

10. The method of claim 1 comprising covering the surface of the sample in fluid so that the tip-sample interaction is within fluid.

11. A method of obtaining measurements of infrared absorption of sub-micron regions of a sample with a probe microscope employing a cantilever probe with a tip, the method comprising:

a. illuminating a region of a sample with a quantum cascade laser;

b. interacting the probe tip with a surface of the sample;

c. measuring a thermal tune of the cantilever probe to determine a contact resonant frequency of the cantilever probe;

d. adjusting a pulse frequency of the quantum cascade laser such that the pulse frequency substantially overlaps a resonant frequency of the cantilever probe;

e. measuring a probe response resulting from absorption of infrared radiation by the sample.

12. The method of claim 11 further comprising the step of repeating steps a-e so as to account for contact resonant frequency shifts of the cantilever probe.

13. The method of claim 12 wherein the contact frequency shifts are due to variations in at least one of:

sample elastic modulus, tip-sample contact area, normal tip-sample force, or lateral tip-sample force.

14. The method of claim 11 comprising covering the surface of the sample in fluid so that the tip-sample interaction is within fluid.