# US 9,752,988 B2 · In-situ identification and control of microstructures produced by phase transformation of a material

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- Number: US 9,752,988 B2
- Document ID: US9752988B2
- Status: Granted
- Kind: B2
- Application number: 13/159,955
- Filed: 2011-06-14
- Published: 2012-07-12
- Granted: 2017-09-05
- Earliest claimed: 2010-06-14
- Assignees: The Regents of the University of Michigan
- Applicants: Jyotirmoy Mazumder; Lijun Song; Cunshan Wang
- Inventors: Jyotirmoy Mazumder; Lijun Song; Cunshan Wang
- Web page: https://patentgrep.com/patent/US9752988B2

## CPC

- G01N 21/718: {Laser microanalysis, i.e. with formation of sample plasma}
- 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)

## Abstract

A microstructure detector and in-situ method for real-time determination of the microstructure of a material undergoing alloying or other phase transformation. The method carried out by the detector includes the steps of: (a) detecting light emitted from a plasma plume created during phase transformation of a material; (b) determining at least some of the spectral content of the detected light; and (c) determining an expected microstructure of the transformed material from the determined spectral content. Closed loop control of the phase transformation process can be carried out using feedback from the detector to achieve a desired microstructure.

## Claims

### Claim 1

A method of determining a microstructure of a material during phase transformation of the material, comprising the steps of:
(a) detecting light emitted from a plasma plume created during phase transformation of a material;
(b) determining at least some of the spectral content of the detected light; and
(c) determining, from the determined spectral content, spectral data representing one or more spectral parameters; and
(d) determining an expected microstructure including a crystal structure of the transformed material from the determined spectral data.

### Claim 2 (depends on 1)

The method of claim 1, wherein the phase transformation of a material in step (a) comprises an alloying of at least two different materials, and wherein step (c) further comprises, for each of at least two of the different materials, determining from the spectral content at least one spectral line associated with that material, and thereafter determining the microstructure based at least in part on the relative line intensities of the determined spectral lines.

### Claim 3 (depends on 2)

The method of claim 2, wherein step (c) further comprises determining the relative amount of the different materials based on the determined spectral lines.

### Claim 4 (depends on 1)

The method of claim 1, wherein step (c) further comprises determining electron temperature from the determined spectral content and determining the microstructure based at least in part on the electron temperature.

### Claim 5 (depends on 1)

The method of claim 1, wherein step (c) further comprises determining electron density from the determined spectral content and determining the microstructure based at least in part on the electron density.

### Claim 6 (depends on 5)

The method of claim 5, wherein the electron density is determined based on line broadening of one or more spectral lines contained in the determined spectral content.

### Claim 7 (depends on 6)

The method of claim 6, wherein the electron density is determined based at least in part on Stark broadening of the one or more spectral lines.

### Claim 8 (depends on 1)

The method of claim 1, wherein step (c) further comprises determining a plurality of parameters from the determined spectral content, and thereafter determining the microstructure based on the parameters.

### Claim 9 (depends on 8)

The method of claim 8, wherein the parameters include electron temperature, electron density, and spectral line intensities.

### Claim 10 (depends on 1)

The method of claim 1, wherein step (a) further comprises detecting light emitted from a plasma plume created by phase transformation of the material.

### Claim 11 (depends on 10)

The method of claim 10, wherein step (a) further comprises detecting light emitted from a plasma plume created by a laser cladding or laser alloying process.

### Claim 12 (depends on 1)

The method of claim 1, wherein step (a) further comprises detecting light emitted from a plasma plume created by interaction of injected energy with the material.

### Claim 13

A microstructure detector for use during phase transformation of a material, comprising:
a light collector oriented to receive light emitted from a plasma plume created during phase transformation of a material;
a sensor that receives the light from said light collector, said sensor including a photo-detector operable to output spectral data indicative of at least some of the spectral content of the received light; and
a computing device that receives the spectral data from said sensor, said computing device operating to determine an expected microstructure including a crystal structure of the transformed material from the received spectral data.

### Claim 14 (depends on 13)

A microstructure detector as set forth in claim 13, wherein said computing device operates to determine one or more spectral parameters from the spectral data and determine the microstructure based on the one or more spectral parameters.

### Claim 15 (depends on 14)

A microstructure detector as set forth in claim 14, wherein the one or more spectral parameters include one or more of the following: electron temperature, electron density, and spectral line intensities.

### Claim 16 (depends on 14)

A microstructure detector as set forth in claim 14, wherein the one or more spectral parameters comprise electron temperature, electron density, and spectral line intensities, and wherein said computing device operates to determine the microstructure based at least in part on all three spectral parameters.

### Claim 17 (depends on 13)

A computer-controlled phase transformation system comprising a phase transformation controller and the microstructure detector of claim 13, wherein said computing device provides feedback that is inputted to said phase transformation controller, and wherein said phase transformation controller operates to carry out the phase transformation of the material and operates to adjust one or more of process parameters during the phase transformation based on the feedback received from said microstructure detector.
