# US 11,749,083 B2 · Method and apparatus for optical ice detection

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- Number: US 11,749,083 B2
- Document ID: US11749083B2
- Status: Granted
- Kind: B2
- Application number: 17/068,036
- Filed: 2020-10-12
- Published: 2021-04-15
- Granted: 2023-09-05
- Earliest claimed: 2019-10-12
- Assignees: University of Wyoming
- Applicants: University of Wyoming
- Inventors: William D. Rice
- Web page: https://patentgrep.com/patent/US11749083B2

## CPC

- G08B 19/02: Alarm responsive to formation or anticipated formation of ice
- G01L 1/24: by measuring variations of optical properties of material when it is stressed, e.g. by photoelastic stress analysis {using infrared, visible light, ultraviolet}
- G01L 1/25: using wave or particle radiation, e.g. X-rays {, microwaves}, neutrons (G01L1/24 takes precedence)
- G01N 21/65: Raman scattering
- G01S 7/499: using polarisation effects
- G01N 2021/1761: {A physical transformation being implied in the method, e.g. a phase change}
- G08B: SIGNALLING SYSTEMS, e.g. PERSONAL CALLING SYSTEMS; ORDER TELEGRAPHS; ALARM SYSTEMS
- G01L: MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE (weighing G01G)
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)
- G01S: RADIO DIRECTION-FINDING; RADIO NAVIGATION; DETERMINING DISTANCE OR VELOCITY BY USE OF RADIO WAVES; LOCATING OR PRESENCE-DETECTING BY USE OF THE REFLECTION OR RERADIATION OF RADIO WAVES; ANALOGOUS ARRANGEMENTS USING OTHER WAVES

## Abstract

In an embodiment, an optical ice detection method is provided. The method includes contacting a multilayer structure with water under conditions effective to form ice, the multilayer structure comprising an optically transparent or semi-transparent material disposed over at least a portion of a material probe. The method further includes performing Raman spectroscopy on one or more of the material probe, water, or ice to obtain Raman spectra, detecting a shift in the Raman spectra, and calculating ice-induced strain in the material probe. Apparatus for optically detecting ice are also provided.

## Claims

### Claim 1

An optical ice detection method, comprising:
contacting a multilayer structure with water under conditions effective to form ice, the multilayer structure comprising an optically transparent or semi-transparent material disposed over at least a portion of a material probe;
performing Raman spectroscopy on one or more of the material probe, the water, or the ice to obtain Raman spectra;
detecting a shift in the Raman spectra; and
calculating ice-induced strain in the material probe.

### Claim 2 (depends on 1)

The method of claim 1, further comprising:
continuously or intermittently monitoring a temperature of the water.

### Claim 3 (depends on 1)

The method of claim 1, wherein detecting the shift in the Raman spectra comprises:
obtaining a first Raman spectra of one or more of the material probe and the water at a first temperature;
fitting peaks of the first Raman spectra with a peak-fitting function;
obtaining a second Raman spectra of one or more of the material probe and the water at a second temperature, wherein the second temperature is different from the first temperature; and
fitting peaks of the second Raman spectra with a peak-fitting function.

### Claim 4 (depends on 3)

The method of claim 3, wherein the first temperature, the second temperature, or both, are below the freezing point of water.

### Claim 5 (depends on 3)

The method of claim 3, wherein the first temperature, second temperature, or both, are below the freezing point of super-cooled water and ice.

### Claim 6 (depends on 1)

The method of claim 1, wherein detecting the shift in the Raman spectra comprises monitoring a frequency of a Raman 2D peak, a full width at half maximum of a Raman 2D peak, or a combination thereof.

### Claim 7 (depends on 1)

The method of claim 1, wherein detecting the shift in the Raman spectra comprises monitoring a frequency of a Raman G peak, a full width at half maximum of the Raman G peak, or a combination thereof.

### Claim 8 (depends on 1)

The method of claim 1, further comprising detecting water droplets, a charge density of the water, or a combination thereof.

### Claim 9 (depends on 8)

The method of claim 8, wherein detecting the charge density of water comprises detecting a change in a frequency of a Raman G peak.

### Claim 10 (depends on 1)

The method of claim 1, wherein:
the material probe comprises Si, SiGe, Ge, graphene, carbon nanotubes, transition-metal dichalcogenides, two-dimensional atomic layers from bulk crystals, quantum wells, pressed powders, nanoparticles, quantum dots, or a combination thereof; or
the optically transparent or semi-transparent material comprises quartz, glass, diamond, sapphire, zinc selenide, poly(methyl methacrylate) (PMMA), barium borosilicate, borosilicate, alumina, aluminum oxynitride (AlON), magnesium aluminate spinel, yttria (Y2O3), yttria alumina garnet (YAG), magnesium oxide, air, vacuum, transparent epoxies, or a combination thereof; or
a combination thereof.

### Claim 11 (depends on 10)

The method of claim 10, wherein the material probe is graphene.

### Claim 12 (depends on 10)

The method of claim 10, wherein the optically transparent or semi-transparent material is quartz.

### Claim 13 (depends on 1)

The method of claim 1, wherein:
the material probe is silicon; and
the optically transparent or semi-transparent material is silicon.

### Claim 14 (depends on 1)

The method of claim 1, further comprising determining a type and a direction of the ice-induced strain using polarization resolution, wherein the type comprises uniaxial or biaxial.

### Claim 15

A method of detecting ice, comprising:
contacting a multilayer structure with water under conditions effective to form ice, the multilayer structure comprising an optically transparent or semi-transparent material disposed over at least a portion of a material probe, the material probe comprising Si, SiGe, Ge, graphene, carbon nanotubes, transition-metal dichalcogenides, two-dimensional atomic layers from bulk crystals, quantum wells, pressed powders, nanoparticles, quantum dots, or a combination thereof;
performing Raman spectroscopy on one or more of the material probe, the water, or the ice to obtain Raman spectra;
detecting a change in the Raman spectra; and
calculating ice-induced strain in the material probe.

### Claim 16 (depends on 15)

The method of claim 15, wherein detecting the change in the Raman spectra comprises:
obtaining a first Raman spectra of one or more of the material probe and the water at a first temperature;
fitting peaks of the first Raman spectra with a peak-fitting function;
obtaining a second Raman spectra of one or more of the material probe and the water at a second temperature, wherein the second temperature is different from the first temperature; and
fitting peaks of the second Raman spectra with a peak-fitting function.

### Claim 17 (depends on 15)

The method of claim 15, wherein detecting the change in the Raman spectra comprises monitoring a frequency of a Raman 2D peak, a full width at half maximum of a Raman 2D peak, or a combination thereof.

### Claim 18

An apparatus for optically detecting ice, comprising:
a multilayer structure comprising an optically transparent layer or semi-transparent layer disposed over at least a portion of a material probe, the material probe comprising Si, SiGe, Ge, graphene, carbon nanotubes, transition-metal dichalcogenides, two-dimensional atomic layers from bulk crystals, quantum wells, pressed powders, nanoparticles, quantum dots, or a combination thereof; and
a Raman probe to detect a shift in Raman spectra, the Raman probe optically coupled to the multilayer structure.

### Claim 19 (depends on 18)

The apparatus of claim 18, wherein the optically transparent or semi-transparent material comprises quartz, glass, diamond, sapphire, zinc selenide, poly(methyl methacrylate) (PMMA), barium borosilicate, borosilicate, alumina, aluminum oxynitride (AlON), magnesium aluminate spinel, yttria (Y2O3), yttria alumina garnet (YAG), magnesium oxide, air, vacuum, transparent epoxies, or a combination thereof.

### Claim 20 (depends on 18)

The apparatus of claim 18, wherein:
the material probe is graphene; and
the optically transparent or semi-transparent material is quartz.