IP Library › Granted Patent US 12,654,197
Granted Patent B2
US 12,654,197 · App. 17/523,721 · Granted Jun 16, 2026

Quality control method for sensor and sensor array production

Inventors: Nicholas R. Glavin (Springboro, OH); Christopher Muratore (Kettering, OH); Melani K. Muratore (Kettering, OH)
Assignee: United States of America as represented by the Secretary of the Air Force
B05D1/28B05D3/06G01N27/125H10D62/80
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Quick Facts
Patent No.
US 12,654,197
App. No.
17/523,721
Granted
Jun 16, 2026
Kind
B2
Abstract

A process of making sensors and sensor arrays that provided real time notification of any centerline deviation. Such production process can be adjusted in real time. Thus, large numbers of units can be made—even in millions of per day—with few if any out of specification units being produced. Such process does not require large-scale clean rooms and is easily configurable.

Claims (61)

1 . A process of making a sensor or sensor array comprising:

a) applying one or more coatings of electrically conductive material to a substrate having a first side and a second side, said one or more coatings of electrically conductive material being applied to at least the first side of said substrate;

b) removing a portion of said electrically conductive material to form a pattern of electrically conductive material electrodes on said substrate;

c) applying one or more chemical coatings in the form of a continuous film over said patterned electrical conductive material to form a coated substrate, wherein said patterned electrical conductive material comprises a material selected from the group consisting of poly(3,4-ethylenedioxythiophene), poly(3,4-ethylenedioxythiophene) polystyrene sulfonate, poly(pyrrole), polycarbazoles, polyindoles, polyazepines, Cr, Mo, Ti, Sc, Ni, V, Hf, W, Nb, Au, Ag, Cu, and Pt and mixtures thereof; and said one or more chemical coatings each independently comprising a transition metal and an element selected from the group consisting of hydrogen, carbon, nitrogen, oxygen, sulfur, selenium, phosphorous and mixtures thereof, said one or more chemical coatings each independently comprising at least one of an amorphous, nanocrystalline, microcrystalline or crystalline region; and

d) pattern illumination-based annealing said coated substrate, said pattern illumination-based anneal comprising using one or more lasers and/or lamps to achieve at least one of a chemical change or change in crystallization in at least a portion of at least one of said one or more chemical coatings on said substrate,

wherein said process is a roll process wherein said coated substrate is a rolled coated substrate that comprises a chemically coated portion that is unrolled at least in part, said unrolled chemically coated portion of said coated substrate being at least in part pattern illumination-based annealed, said process comprising a quality control unit comprising one or more diagnostic detectors, said one or more diagnostic detectors positioned to collect light that has interacted with said one or more chemical coatings at the point of and/or after said pattern illumination-based annealing has occurred.

2 . A process of making a sensor or sensor array according to claim 1 wherein said one or more diagnostic detectors are each independently an optical camera, an optical detector, or Raman spectrometer.

3 . A process of making a sensor or sensor array according to claim 1 wherein said quality control unit comprises at least two diagnostic detectors, at least one of said diagnostic detectors positioned to collect light that has interacted with said one or more chemical coatings at the point of said pattern illumination-based annealing, and at least one of said diagnostic detectors positioned to collect light that has interacted with said one or more chemical coatings after said pattern illumination-based annealing has occurred.

4 . A process of making a sensor or sensor array according to claim 1 wherein said collected light that has interacted with said one or more chemical coatings at the point of and/or after said pattern illumination-based annealing has occurred is supplied prior to said interaction by a laser, an LED or a broadband light source.

5 . A process of making a sensor or sensor array according to claim 1 wherein at least a portion of said collected light that has interacted with said one or more chemical coatings at the point of and/or after said pattern illumination-based annealing has occurred is supplied by said one or more lasers and/or lamps used to achieve at least one of a chemical change or change in crystallization in at least a portion of at least one of said one or more chemical coatings on at least one side of said substrate.

6 . A process of making a sensor or sensor array according to claim 1 further comprising attaching one or more types of functional molecules and/or one or more complexes comprising one or more types of functional molecules and one or more target molecules to at least a portion of said pattern illumination-based anneal coated substrate, wherein said one or more functional molecules are biomaterials that are selected from the group consisting of: peptides, nanozymes, proteins, lipids, carbohydrates and lectins, nucleic acids and mixtures thereof.

7 . A process of making a sensor or sensor array according to claim 6 wherein said biomaterial's attachment to said pattern illumination-based anneal coated substrate comprises at least one of a covalent bond, electrostatic bond or a covalent and electrostatic bond.

8 . A process of making a sensor or sensor array according to claim 6 wherein attaching said biomaterials to said pattern illumination-based anneal coated substrate comprises contacting said at least a portion of said pattern illumination-based anneal coated substrate and said one or more types of biomaterials.

9 . A process of making a sensor or sensor array according to claim 1 wherein:

a) at least one of said one or more chemical coatings comprises, prior to said annealing, two or more regions that are amorphous, nanocrystalline, microcrystalline or crystalline with the proviso that at least two of said regions are not identical with respect to being amorphous, nanocrystalline, microcrystalline or crystalline and said laser or lamp forms on, within or on and within said at least one of said one or more chemical coatings:

(i) at least two electronic elements selected from a conductor, semiconductor and an insulator;

(ii) two or more different conductors having at least one of the following: different electrical properties or different optical properties;

(iii) two or more different semiconductors having at least one of the following: different electrical properties or different optical properties; or

(iv) two or more different insulators having at least one of the following: different electrical properties or different optical properties;

said process being performed under one of the following conditions: vacuum of less 100 torr, air or under a fluid blanket other than air;

said pattern illumination-based annealing resulting in at least one of a chemical change or a change in crystallization, and the removal of at least a portion of at least one of said one or more chemical coatings and resulting in an electrical component, an optical component or a combined electrical and optical component being formed on, within or on and within at least a portion of said pattern illumination-based annealed one or more chemical coatings.

10 . The process of claim 9 wherein, said electrical and/or optical component is selected from the group consisting of an inductor, a capacitor, a resistor, a diode, a a trace, a battery, an optical filter, a chemical sensor, a biological sensor and a solar cell.

11 . The process of claim 1 , further comprising performing steps a) to d) on the second side of said substrate as well.

12 . The process of claim 1 wherein said transition metal is selected from the group consisting of molybdenum, tungsten, niobium, tantalum, vanadium, titanium, chromium, iron, rhodium, hafnium, rhenium and mixtures thereof.

13 . A process according to claim 1 wherein said material comprises at least one region that is amorphous or nanocrystalline.

14 . The process of claim 1 wherein said pattern illumination-based annealing in step d) further comprises removal of at least a portion of said chemical coating on at least one side of said substrate, and each of said one or more chemical coatings have an area and a thickness and said removal of said at least a portion of said one or more chemical coating occurs, said removal comprising at least one of:

a.) laser ablation removal of from about 0.1% to about 99.9% of at least one of said one or more chemical coatings' area; or

b.) laser ablation removal of at least 85% of at least one of said chemical coatings' thickness; or laser ablation removal of about 85% to about 99% of at least one of said chemical coatings' thickness.

15 . The process of claim 1 wherein said substrate of said coated substrate is selected from glass, polymer, and mixtures thereof.

16 . The process of claim 1 wherein at least a portion of said coated substrate's pattern illumination-based annealed chemical coating is further treated by at least one of the following processes:

a.) two or more pattern illumination-based annealings;

b.) plasma treatment comprising exposing said at least a portion of said coated substrate's pattern illumination-based annealed chemical coating to an ionized gas derived from the group consisting of He, Ne, Ar, Kr, Xe, H 2 , O 2 , SF 6 , CF 4 , N 2 and mixtures thereof;

c.) ion beam irradiation comprising exposing said at least a portion of said coated substrate's pattern illumination-based annealed chemical coating to an ion beam, said ion beam comprising an ionized gas derived from the group consisting of He, Ne, Ar, Kr, Xe, H 2 , O 2 , SF 6 , CF 4 , N 2 and mixtures thereof;

d.) electron beam illumination comprising exposing at least a portion of said coated substrate's pattern illumination-based annealed chemical coating to an electron dose of from about 10 2 electrons/nm 2 to about 10 25 electrons/nm 2 ;

e.) thermal annealing said at least a portion of said coated substrate's pattern illumination-based annealed chemical coating, said at least a portion of said coated substrate's pattern illumination-based annealed chemical coating's thermal annealing treatment temperature being from greater than about 250° C. to about 1,500° C.;

f.) chemically etching said at least a portion of said coated substrate's pattern illumination-based annealed chemical coating comprising contacting said at least a portion of said coated substrate's pattern illumination-based annealed chemical coating with an etching composition;

g.) electro-chemically treating said at least a portion of said coated substrate's pattern illumination-based annealed chemical coating by contacting said at least a portion of said coated substrate's pattern illumination-based annealed chemical coating with a chemical composition comprising an electrolyte and subjecting said contacted at least a portion of said coated substrate's pattern illumination-based annealed chemical coating and said chemical composition comprising an electrolyte to an electrical current;

h.) surface physical modification of at least a portion of said coated substrate's pattern illumination-based annealed chemical coating.

17 . The process of claim 1 wherein step b) comprises removing a portion of said electrically conductive material to form a pattern of electrically conductive material electrodes on said substrate using a laser.

18 . A roll-to-roll process for making a sensor or sensor array on a flexible substrate that has a first side and a second side, said process comprising utilizing an apparatus comprising:

a) three rolls comprising a first roll, a second roll that comprises a main roll, and a third roll, wherein said rolls contact at least portions of a flexible substrate, and said main roll is positioned along said flexible substrate between said first and third rolls;

b) a chemical coating sputtering target positioned along said flexible substrate;

c) a laser positioned along said flexible substrate; and

d) a metal sputtering target positioned along said flexible substrate,

wherein said process comprises four unit operations, said unit operations comprising:

1) a first unit operation where the rolls rotate so that the flexible substrate is moved past said metal sputtering target, and said metal sputtering target deposits metal onto the first side of said flexible substrate to form an electrically conductive material coated substrate on a portion of said substrate;

2) a second unit operation where the electrically conductive material coated substrate is moved past said laser, and said laser patterns said electrical conductive material on said portion of said substrate to form patterned electrically conductive material on said substrate;

3) a third unit operation where the patterned electrically conductive material on said substrate is moved past the chemical coating sputtering target, and said chemical coating sputtering target applies a chemical coating on top of said patterned electrical conductive material on said substrate to form a chemically coated substrate;

4) a fourth unit operation, wherein the chemically coated substrate from the third unit operation is moved past said laser, wherein said laser anneals said chemically coated substrate.

19 . The roll-to-roll process of claim 18 wherein the rolls rotate in a first direction during said first unit operation, and the rolls rotate in the opposite direction during said second unit operation.

20 . The roll-to-roll process of claim 18 wherein said process forms a flexible substrate with a plurality of sensors thereon.

21 . The roll-to-roll process of claim 20 wherein the flexible substrate has a centerline, and the process further comprises a quality control unit comprising one or more diagnostic detectors positioned along said flexible substrate to provide real-time notification of any centerline deviation.

22 . An all-laser roll-to-roll process for making a sensor, said process comprising:

a) providing a spool of flexible substrate material;

b) depositing a layer of metal over said substrate;

c) using a laser to ablate said layer of metal to form a pattern of electrically conductive material out of said metal on said substrate, wherein said pattern of electrically conductive material comprises metal contacts and an area connecting said metal contacts;

d) coating said substrate with said patterned electrically conductive material thereon with a coating of amorphous MoS 2 to form a coated substrate with patterned electrically conductive material beneath said coating;

e) using a laser at a laser energy condition to laser ablate said coated substrate to remove some or all of the amorphous MoS 2 , except an area connecting the metal contacts;

f) laser annealing the coated substrate formed in step e) at a different energy condition than used for laser ablating in step e), wherein said laser annealing induces crystallization in the MoS 2 that remains after the laser ablating in step e); and

g) monitoring the success of the laser annealing to induce crystallization in the MoS 2 using a camera and a Raman spectrometer mounted to monitor the process at the location of the laser in step f).

23 . The process of claim 22 further comprising mounting an optical light source and a detector downstream of the process in step g) to evaluate broadband light transmission and absorption through the coated substrate.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 10, 2021
From: GLAVIN, NICHOLAS R, DR; MURATORE, CHRISTOPHER, DR; MURATORE, MELANI K
To: GOVERNMENT OF THE UNITED STATES, AS REPRESENTED BY THE SECRETARY OF THE AIR FORCE
Reel/Frame 058078/0013 →
Continuity (5)
Continuation In Part 17336799 · Jun 2, 2021
Continuation In Part 17216729 · Mar 30, 2021
Provisional Application 63001604 · Mar 30, 2020
Related Publication 20220062948A1 · Mar 3, 2022
Related Publication 20230148461A9 · May 11, 2023
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