# US 9,750,833 B2 · Generation of microbiocide inside a package utilizing a controlled gas composition

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- Number: US 9,750,833 B2
- Document ID: US9750833B2
- Status: Granted
- Kind: B2
- Application number: 15/227,658
- Filed: 2016-08-03
- Published: 2016-11-24
- Granted: 2017-09-05
- Earliest claimed: 2009-03-24
- Assignees: Purdue Research Foundation
- Applicants: Purdue Research Foundation
- Inventors: Kevin M. Keener; Jeanette L. Jensen
- Web page: https://patentgrep.com/patent/US9750833B2

## CPC

- A61L 2/14: Plasma, i.e. ionised gases
- B65B 55/02: Sterilising, e.g. of complete packages
- B65B 55/18: by liquids or gases (B65B55/14 takes precedence)
- H01J 37/32348: {Dielectric barrier discharge}
- H01J 37/32825: {Working under atmospheric pressure or higher}
- A61L 2103/23: {Containers other than laboratory or medical, e.g. bottles or mail}
- A61L: METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES (preservation of bodies or disinfecting characterised by the agents employed A01N; preserving, e.g. sterilising, food or foodstuffs A23; preparations for medical, dental or toiletry purposes A61K)
- B65B: MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING (bundling and pressing devices for cigars A24C1/44; devices for tensioning and securing binders adapted to be supported by the article or articles to be bound B25B25/00; applying closure members to bottles, jars or similar containers B67B1/00-B67B6/00; concurrent cleaning, filling and closing of bottles B67C7/00; emptying bottles, jars, cans, casks, barrels or similar containers B67C9/00)
- H01J: ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS (spark-gaps H01T; electric arc lamps H05B31/00; particle accelerators H05H)

## Abstract

An apparatus and method of producing an atmospheric non-equilibrium plasma (ANEP) in a sealed container having a selected working gas and an object to be treated is described. A variety of working gas mixtures including air, O2, N2, CO2, He and Ar, in combination with a range of ionization gradients, voltages and ANEP column lengths was investigated so as to establish effective ranges of the variables using the sterilization of a sample as a measure of effectiveness. Certain combinations of working gas, voltage gradient, voltage or ANEP column length were found to have greater effectiveness. The approach may be used for food products, medical equipment, or other objects where treatment with reactive gas atmospheres is effective.

## Claims

### Claim 1

A method of sterilizing or decontaminating an object, comprising:
providing a dielectric barrier discharge (DBD) device having electrodes spaced apart and including a dielectric layer extending beyond ends of a conductive portion of at least one of the electrodes;
providing a container suitable for substantially completely enclosing the object;
inserting the object into the container;
filling the container with a working gas at substantially atmospheric pressure;
disposing a portion of the container with respect to the DBD device such that reactive species are produced in the container by the DBD device; and,
activating the DBD device for a first period of time by applying a voltage gradient,
wherein the voltage gradient applied to the DBD device is greater than approximately 1.4 times an ionization voltage gradient of the working gas.

### Claim 2 (depends on 1)

The method of claim 1, wherein the first period of time is about 15 seconds or less.

### Claim 3 (depends on 1)

The method of claim 1, wherein the first period of time is about 60 seconds or less.

### Claim 4 (depends on 1)

The method of claim 1, wherein the working gas is air.

### Claim 5 (depends on 1)

The method of claim 1, wherein the working gas is comprised of at least two gasses selected from air, N2, O2, CO2, and at least a noble gas.

### Claim 6 (depends on 1)

The method of claim 1, wherein the object remains within the container for a second period of time commencing after a completion of the first period of time.

### Claim 7 (depends on 6)

The method of claim 6, wherein a sum of the first period of time and the second period of time is selected to result in decontamination of the object.

### Claim 8 (depends on 1)

The method of claim 1, wherein a sum of the first period of time and a second period of time is selected to result in sterilization of the object.

### Claim 9 (depends on 1)

The method of claim 1, where an ANEP (Atmospheric Non-Equilibrium Plasma) is created in a region where the object in the container is disposed between electrodes of the DBD.

### Claim 10 (depends on 1)

The method of claim 1, wherein the ANEP is created in a region where the object in the container is not disposed between electrodes of the DBD.

### Claim 11 (depends on 1)

The method of claim 1, wherein the DBD device comprises a pair of electrodes, spaced apart and adjusting a spacing between the electrodes to captivate t portion of the container between the electrodes.

### Claim 12 (depends on 11)

The method of claim 11, wherein the electrodes are shaped to be conformal with the captivated portion.

### Claim 13 (depends on 1)

The method of claim 1, wherein the container is held against the electrodes by an internal pressure of the working gas.

### Claim 14 (depends on 1)

The method of claim 1, wherein a voltage applied to the DBD to produce the voltage gradient is at least about 50 kV RMS and less than 130 kV RMS.

### Claim 15

A method of sterilizing or decontaminating an object, comprising:
packaging the object to be treated in a substantially dielectric closed container, a volume of the container not containing the object being filled with a working gas at substantially atmospheric pressure;
placing the packaged object in an apparatus for generating an atmospheric non-equilibrium plasma (ANEP);
compressing the substantially dielectric closed container to result in a predetermined spacing between opposing electrodes of the apparatus;
activating the apparatus so as to generate the ANEP inside at least a portion of the container for a time period; and
removing the container from the apparatus;
wherein a voltage gradient applied to the working gas is at least about 1.4 times an ionization voltage gradient of the working gas.

### Claim 16 (depends on 15)

The method of claim 15, wherein a voltage applied to the apparatus to produce the voltage gradient is at least about 50 kV RMS and less than 130 kV RMS.

### Claim 17 (depends on 16)

The method of claim 16, wherein a voltage applied to the apparatus to produce the voltage gradient is less than 80 kV RMS.

### Claim 18 (depends on 15)

The method of claim 15, wherein the ANEP is produced only within the container.

### Claim 19 (depends on 15)

The method of claim 15, wherein the working gas is comprised of at least two gasses selected from air, N2, O2, CO2, and a noble gas.

### Claim 20 (depends on 15)

The method of claim 15, wherein the substantially dielectric closed container comprises at least two layers and a first layer is high density polyethylene fibers and a second layer is a polyethylene film.
