Title of Invention

" METHOD FOR METALLIZING POLYETHER FOAM TO PRODUCE AN ANTI- MICROBIAL AND FILTRATION MATERIAL"

Abstract There is disclosed a method for metallizing a polyether foam comprising the steps of premetallizing a polyether foam substrate to prepare the foam substrate for application of a metal by using a mixture of stannous chloride and an acid, such as herein described, and immersing the foam substrate in the mixture; and metallizing the foam substrate to apply the metal to the foam; without requirement of an etching step or any additional step.
Full Text CROSS REFERENCE TO RELATED APPLICATIONS
The present application claims priority to U.S. Provisional Patent Application No,
60/603,610, which was filed August 23,2004 and which is hereby incorporated by
reference in its entirety.
FIELD OF THE INVENTION
This invention is directed generally to forming anti-microbial materials, and more
particularly to forming foam materials having anti-microbial activity and/or filtration
properties,
BACKGROUND
There are several prior art methods that describe metallizing of foam substrates
(e.g., Patent Nos: 6,395,402; 5,151,222; 3,661,597). Different methods have bee4 used to
metallize foam for various applications such as EMI shielding etc. Patent No: 6,3195,402
discuss the metallization of copper/nickel for EMI applications. While the adhesion of
the metal to the foam may he good, the process cannot produce a good silver coating due
to the difference in deposition rates of copper versus silver. In addition, these materials

do not provide any-mierobial activity as copper/nickel do not provide anti-microbial
properties. The other patents listed produce rigid foam that cannot be used in a .
medical anti-microbial applications) or as a flexible filter.
Accordingly, what is needed is a method of metallizing foam that is capable of
using silver .Also what is needed is a method of forming a foam material that has! anti-
microbial activity. Additionally what is needed is a method of forming a foam material
that may be used as a filter and having anti-microbial activity.

SUMMARY OF THE INVENTION
The present invention provides a method of metallizing a foam material. The
method may be used to form a foam material having anti-microbial activity by
metallizing the foam with a metal, such as silver. The resulting foam may be used in a
variety of different applications such as a filter' material. The methods of the present
invention are simpler than prior art methods since the foam materials may be metallized
without the need for an activation/seeding step. The resulting foam may also be designed
such that the product has a low resistance and/or an optimal metal ion release. The
method of the present invention uses one or more of the steps of etching the foam, pre-
metallizing the foam and metallizing the foam with silver. Depending on the selected
properties of the final foam, the method may use some or all of these steps.
These and other embodiments are described in more detail below.
DETAILED DESCRIPTION OF THE INVENTION
The present invention is more particularly described in the following description
and examples that are intended to be illustrative only since numerous modifications and
variations therin will be apparent to those skilled in the art As used in the specification
and in the claims, the singular form "a," "an," and "the" may include plural referents
unless the context clearly dictates otherwise. Also, as used in the specification and in the
claims, the term "comprising" may include the embodiments "consisting of and "consisting essentially of"
The present invention provides a method of metallizing a foam material. The
method may be used to form a foam material having anti-microbial activity by
metallizing the foam with a metal that provides anti-microbial activity to a material. The
resulting foam may be used in a variety of different applications that may benefit from a
material having anti-microbial activity including, but not limited to, the use of the
metallized foam as a filter material. The methods of the present invention are simpler
than prior art methods because the foam materials may be metallized without an
activation/seeding step commonly associated with prior art methods. The resulting
metallized foam materials are formed such that the metal adheres well to the foam. The

resulting foam may be designed such that the product has a low resistance and/or an
optimized silver ion release.
The methods of the present invention are designed to metallize foam without the
need for an activator. As such, the methods of the present invention are capable of
metallizing the film through one or more of the steps of etching the foam, pre-metallizing
the foam and/or metallizing the foam with the selected metal Depending on the selected
properties of the final foam, one or more of these steps may be omitted while still
achieving a metallized foam product. As used herein, an "etchant" is a material capable
of etching or removing portions of the foam material to permit better adhesion of the
metal to the foam substrate to be metallized.
Accordingly, in a first aspect, the methods of the present invention etch the foam
to increase the surface area of the foam. To etch the foam, the foam substrate is first
quenched using an etchant and then rinsed. The etchant may be, in one embodiment, a
base solution. The type of base solution may be any base solution capable of removing or
etching portions of the foam substrate. The type of base solution that may be used may
vary depending on one or more factors including, but not limited to, the foam substrate to
be etched, the metal to be applied, the degree of etching desired, and/or the final
characteristics of the metallized foam. Examples of base solutions that may be used for
the etchant include, but are not limited to, alkaline hydroxides, such as lithium hydroxide,
sodium hydroxide, potassium hydroxide, rubidium hydroxide, cesium hydroxide,
francium hydroxide, beryllium hydroxide, magnesium hydroxide, calcium hydroxide,
strontium hydroxide, barium hydroxide, or a combination thereof. In one embodiment,
the base solution is sodium hydroxide.
The foam may be etched by immersing the foam substrate in a solution containing
the etchant As used herein, "immersed" is meant to include any method by which a
solution may be contacted with at least a portion of a surface area of a foam substrate
including, but not limited to, dipping, spraying, immersing, quenching, and/or any other
method capable of applying a liquid to at least a portion of a substrate.
In one embodiment, the first step in the process may be performed either
immediately prior to the second step or may be performed as a preparation step with
subsequent steps taking place at a future time. As such, thicker foams and/or extended

amounts of foam may be treated in a mass processing step. This would; enable a
manufacturer to quench thick foam {1' thick) and 12 feet or more of length at a time.
Alternatively, flame-treated non-etched foam may be etched in-house using a stronger
solution of sodium hydroxide.
The first etching step may be performed under a range of operating temperatures
and/or dwell or etch times, depending on the type of foam to be etched, the etcnant used,
and/or the selected characteristics of the finished product Various embodiments for the
methods of the present invention are set forth below, although it is to be understood that
other embodiments are also included within the scope of the present invention. For the
percentage of the foam that is etched:

For the temperature at which the process is to be operated:

For the etch time of the process:

The temperature and time of etch may be dependent on the concentration of the
etchant solution.
After the foam has been etched, the foam may be conditioned with a non-ionic
surfactant or other suitable material to enable the surface to be wet out and/or to clean the

surface of any debris/dirt. A good rinsing process using de-ionized water with
temperature under 70o C follows may be used with the following embodiments;

Some polyether foams may not be etched since the chemistry as described below
is sufficient to activate the surface of the foam material. As a result, for the methods of
the present invention, when a polyether foam is used as the foam substrate, the foams
may be metallized without the need for an activation/seeding step or an etching step for
preparing the foam for metallization.
After the step of etching the foam, then the methods of the present invention may
include a pre-metallization step. The pre-metallization step is utilized to prepare the foam
for the application of the metal and to help facilitate attachment of the metal to the foam
substrate. In one embodiment, the pre-metallization step may be accomplished by
dipping the etched foam in an acid solution. An acid dip, such as with HC1, may then be
used. The acid dip acts as a pre-metallizing step utilizing the acid as the solvent. Other
acids, such as sulfuric acid or nitric acid, may be used for the pre-metallization step. A
rinsing step may then be used upon completion of the pre-metallizing step.
For the dwell times of the pre-metallizing step, various embodiments are set forth
below:

For the concentration of the acid in the pre-metallizing step, various embodiments
include:



For the concentration of the stannous chloride, various embodiments are set forth below:
The pre-inetailization step may, in one embodiment, provide a mixture of stannous
chloride and muriatic acid. The amount of stannous chloride may be, in one embodiment,
selected to be between about 60 gm/1 up to about 140 gm/1 and the concentration of the
muriatic acid may be between about 6 to about 15%. The dwell time may be selected to
be between about 3 and 15 minutes. Once the pre-metallization step is completed, the
process may be followed by a special counter flow rinsing with controlled water flow.
This step enables the acid to remove any excess salts and acids from the substrates yet
leave an optimum amount of activators on the surface. For the concentration of the
muriatic acid, various embodiments are set forth below:


For the dwell time, various embodiments for the present invention may include:

It is to be understood that embodiments for the concentration of the acid, the
concentration of the stannous chloride and/or the dwell time are not required to be used in
the order listed above in the respective tables, but may be used in any order or
combination thereof Accordingly, in one embodiment, the concentration of the acid
may be from about 5 to about 20%, the concentration of the stannous chloride may be
about 10%, and the dwell time may be from about 5 to about 60 minutes. Alternatively,
in another embodiment, the concentration of the acid may be from about 8 to about 18%,
the concentration of the stannous chloride may be from about 5 to about 40%, and the
dwell time may be from about 10 to about 50 minutes.
Once the foam has been prepared, the methods of the present invention then
include a final step of applying the metal to the foam. The step may be referred to as a
metallization step. The metallization step may be performed using blown metallization
technologies such as those described in patent number 3,877,965 or Patent Application
No. 10/666.568, which are hereby incorporated by reference.
The metallized foam may then be placed in an oven at 60-70' C for about 30
minutes to produce a semi-quenching effect to help attach the metal to the foam.
The methods of the present invention may be used with a variety of different
metals that may be desired to be attached to a foam substrate. In one embodiment, the
metal is silver. Silver provides anti-microbial, conductive and/or anti-static properties to
the foam substrate. In. alternative embodiments, the metal may be selected from copper,
gold, aluminum, or any other metal capable of being attached to a foam substrate.

The present invention may be used with any type of foam. Examples of foams
that may be used include, but are not limited to, poiyurethane, polyester, polyether, or a
combination thereof. The resulting foams have enhanced resistance (ohms/square), anti-
microbial activity, ion release, or a combination thereof, as compared to prior art foams.
The metallized foam products made according to the methods of the present
invention may be used in any application wherein the advantages offered by the metal
may be utilized. For example, due to the anti-microbial benefits, if the metal is silver, the
metallized foam may be used as a filter material for the filtration of liquids. In addition,
the foam may be in the form of a thin layer, such that the resulting metallized foam may
be used as a wrap for wounds to assist in healing of the wounds.
The present invention will now be further described through examples. It is to be
understood that these examples are non-limiting and are presented to provide a better
understanding of various embodiments of the present invention.
EXAMPLES
Example 1
A bath was prepared by dissolving 4.2 gm of silver nitrate in de-ionized water. It
was then complexed with 3,3 nil of 27% aqua ammonia. A quenched foam sample
weighing 24.0 gm. was cleaned with non-ionic surfactant such as Triton X-100 and rinsed
thoroughly. Foam was etched with 15% HC1 for 20 minutes. The foam was then pre-
metallized with solution having 10% HC1 and 10 gm/1 of anhydrous tin chloride for 20
minutes. The foam was then rinsed in counter flow de-ionized water. 0,63gm of terra
sodium EDTA was dissolved in 2 liters of de-ionized water. 6.5ml of NBI/AEM
surfactant was also added to the bath. The foam was placed in the reactor and solution
was agitated. Silver complex was added and then 1.8ml of formaldehyde was added.
After three hours the sample was removed and subjected to hot water rinse. Then a 0.2%
NaOH solution was (50mL volume) was made up and at 60* C, The metallized foam was
then dipped into the solution, The color changed to a gold tone.

Example 2
The sample obtained from example 1 cut to produce a 1,5gm sample. This was
then placed in a beater with 5% sodium chloride solution for 24-hour period at 37°C.
The solution after 1-hour period was then tested for silver ions using a Perkin Elmer
Analyst 300. The ion. release was 0.5ppm
Example 3
The sample obtained from example 1 was cut to weight 0.75 gm and was
subjected to Dow Coming Corporate Test Method 0923 and/or ASTM-E2149 Test
method. The organism used was Staphylococcus aureus ATCC 6538. The reduction of
organism growth was over 99.9%.
Example 4
The Sample obtained from example 1 was subject to process similar to the one
described in U.S. Patent Application No. 10/836,530, the disclosure of which is hereby
incorporated by reference in its entirety. This sample was then subjected to the ion
release protocol as described in example 2. The ion release was at 6.2ppm in one hour
Example 5
The sample obtained from example 1 was subject to ASTM E-2149 test for
antimicrobial efficacy. The organism used was Staphylococcus aureus ATCC 6538, The
reduction of organism growth was over 99.9%.
The foregoing is provided for purposes of illustrating, explaining, and describing
embodiments of this invention. Modifications and adaptations to these embodiments will
be apparent to those skilled in the art and may be made without departing from the scope
or spirit of this invention.

WE CLAIM:
1. A method for metallizing a polyether foam comprising the steps of:
pre-metallizing a polyether foam substrate to prepare the foam substrate for application
of a metal by using a mixture of stannous chloride and an acid, such as herein described, and
immersing the foam substrate in the mixture; and
metallizing the foam substrate to apply the metal to the foam;
without requirement of an etching step or any additional step.
2. The method as claimed in claim 1, wherein the foam substrate is immersed in the
mixture for a period of time from 5 to 60 minutes.
3. The method as claimed in claim 1, wherein the mixture contains from 5 to 40% of
stannous chloride and from 4 to 25% of the acid.
4. The method as claimed in claim 1, wherein the metal is selected from silver, gold,
aluminum, copper, or a combination thereof.
5. The method as claimed in claim 4, wherein the metal comprises silver.


ABSTRACT

"METHOD FOR METALLIZING POLYETHER FOAM TO PRODUCE AN
ANTI-MICROBIAL AND FILTRATION MATERIAL"
There is disclosed a method for metallizing a polyether foam comprising the steps of premetallizing a polyether foam substrate to prepare the foam substrate for application of a metal by using
a mixture of stannous chloride and an acid, such as herein described, and immersing the foam substrate
in the mixture; and metallizing the foam substrate to apply the metal to the foam; without requirement
of an etching step or any additional step.

Documents:

00728-kolnp-2007-correspondence-1.1.pdf

00728-kolnp-2007-form-3-1.1.pdf

00728-kolnp-2007-priority document.pdf

0728-kolnp-2007 abstract.pdf

0728-kolnp-2007 claims.pdf

0728-kolnp-2007 correspondence others.pdf

0728-kolnp-2007 description(complete).pdf

0728-kolnp-2007 form-1.pdf

0728-kolnp-2007 form-3.pdf

0728-kolnp-2007 form-5.pdf

0728-kolnp-2007 international publication.pdf

0728-kolnp-2007 international search authority report.pdf

728-KOLNP-2007-(21-11-2011)-ABSTRACT.pdf

728-KOLNP-2007-(21-11-2011)-CERTIFIED COPIES(OTHER COUNTRIES).pdf

728-KOLNP-2007-(21-11-2011)-CLAIMS.pdf

728-KOLNP-2007-(21-11-2011)-DESCRIPTION (COMPLETE).pdf

728-KOLNP-2007-(21-11-2011)-EXAMINATION REPORT REPLY RECEIVED.pdf

728-KOLNP-2007-(21-11-2011)-FORM-1.pdf

728-KOLNP-2007-(21-11-2011)-FORM-2.pdf

728-KOLNP-2007-(21-11-2011)-FORM-3.pdf

728-KOLNP-2007-(21-11-2011)-OTHER PATENT DOCUMENT-1.pdf

728-KOLNP-2007-(21-11-2011)-OTHER PATENT DOCUMENT.pdf

728-KOLNP-2007-(21-11-2011)-OTHERS.pdf

728-KOLNP-2007-ABSTRACT.pdf

728-KOLNP-2007-ASSIGNMENT 1.1.pdf

728-KOLNP-2007-ASSIGNMENT.pdf

728-KOLNP-2007-CLAIMS.pdf

728-KOLNP-2007-CORRESPONDENCE 1.1.pdf

728-KOLNP-2007-CORRESPONDENCE 1.3.pdf

728-KOLNP-2007-CORRESPONDENCE 1.4.pdf

728-KOLNP-2007-CORRESPONDENCE.pdf

728-KOLNP-2007-DESCRIPTION (COMPLETE).pdf

728-KOLNP-2007-EXAMINATION REPORT 1.1.pdf

728-KOLNP-2007-EXAMINATION REPORT.pdf

728-KOLNP-2007-FORM 1.pdf

728-KOLNP-2007-FORM 18 1.1.pdf

728-KOLNP-2007-FORM 18 1.2.pdf

728-kolnp-2007-form 18.pdf

728-KOLNP-2007-FORM 2.pdf

728-KOLNP-2007-FORM 3 1.1.pdf

728-KOLNP-2007-FORM 3.pdf

728-KOLNP-2007-FORM 5 1.1.pdf

728-KOLNP-2007-FORM 5.pdf

728-KOLNP-2007-GPA 1.1.pdf

728-KOLNP-2007-GPA.pdf

728-KOLNP-2007-GRANTED-ABSTRACT.pdf

728-KOLNP-2007-GRANTED-CLAIMS.pdf

728-KOLNP-2007-GRANTED-DESCRIPTION (COMPLETE).pdf

728-KOLNP-2007-GRANTED-FORM 1.pdf

728-KOLNP-2007-GRANTED-FORM 2.pdf

728-KOLNP-2007-GRANTED-SPECIFICATION.pdf

728-KOLNP-2007-INTERNATIONAL PUBLICATION.pdf

728-KOLNP-2007-OTHERS 1.1.pdf

728-KOLNP-2007-OTHERS.pdf

728-KOLNP-2007-PA.pdf

728-KOLNP-2007-REPLY TO EXAMINATION REPORT 1.1.pdf

728-KOLNP-2007-REPLY TO EXAMINATION REPORT.pdf

728-KOLNP-2007-SPECIFICATION.pdf


Patent Number 254524
Indian Patent Application Number 728/KOLNP/2007
PG Journal Number 46/2012
Publication Date 16-Nov-2012
Grant Date 12-Nov-2012
Date of Filing 27-Feb-2007
Name of Patentee NOBLE FIBER TECHNOLOGIES, LLC
Applicant Address 300 PALM STREET SCRANTON, PA 18505
Inventors:
# Inventor's Name Inventor's Address
1 CHANDRA, N, SATISH 202 BARRINGTON PLACE, LANSDALE, PA 19446
2 MCNALLY, WILLIAM, F. 210 GRANDVIEW STREET, CLARKS SUMMIT PA 184111,
3 FUREY,JOEL, M 300 NORTH HOLLOW ROAD, STOWE, VT 05672,
PCT International Classification Number B32B 3/26 , B05D 3/10
PCT International Application Number PCT/US2005/029956
PCT International Filing date 2005-08-23
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 60/603,610 2004-08-23 Uganda