US20160107415A1 - Colored biocidal multi-layer structure - Google Patents
Colored biocidal multi-layer structure Download PDFInfo
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- US20160107415A1 US20160107415A1 US14/519,425 US201414519425A US2016107415A1 US 20160107415 A1 US20160107415 A1 US 20160107415A1 US 201414519425 A US201414519425 A US 201414519425A US 2016107415 A1 US2016107415 A1 US 2016107415A1
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- layer
- biocidal
- colored
- particles
- layer structure
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Definitions
- the present invention relates to biocidal layers having antimicrobial efficacy on a surface.
- Anthrax is an acute infectious disease caused by the spore-forming bacterium bacillus anthracis. Allergic reactions to molds and yeasts are a major concern to many consumers and insurance companies alike.
- MRSA methicillin-resistant Staphylococcus aureus
- VRE vancomycin-resistant Enterococcus
- Noble metal ions such as silver and gold ions are known for their antimicrobial properties and have been used in medical care for many years to prevent and treat infection. In recent years, this technology has been applied to consumer products to prevent the transmission of infectious disease and to kill harmful bacteria such as Staphylococcus aureus and Salmonella.
- noble metals, metal ions, metal salts, or compounds containing metal ions having antimicrobial properties can be applied to surfaces to impart an antimicrobial property to the surface. If, or when, the surface is inoculated with harmful microbes, the antimicrobial metal ions or metal complexes, if present in effective concentrations, will slow or even prevent altogether the growth of those microbes.
- silver sulfate, Ag 2 SO 4 described in U.S.
- Antimicrobial activity is not limited to noble metals but is also observed in other metals such as copper and organic materials such as triclosan, and some polymeric materials.
- the antimicrobial active element, molecule, or compound be present on the surface of the article at a concentration sufficient to inhibit microbial growth.
- concentration for a particular antimicrobial agent and bacterium, is often referred to as the minimum inhibitory concentration (MIC).
- MIC minimum inhibitory concentration
- the antimicrobial agent be present on the surface of the article at a concentration significantly below that which can be harmful to the user of the article. This prevents harmful side effects of the article and decreases the risk to the user, while providing the benefit of reducing microbial contamination.
- the rate of release of antimicrobial ions from antimicrobial films can be too facile, such that the antimicrobial article can quickly be depleted of antimicrobial active materials and become inert or non-functional.
- Depletion results from rapid diffusion of the active materials into the biological environment with which they are in contact, for example, water soluble biocides exposed to aqueous or humid environments. It is desirable that the rate of release of the antimicrobial ions or molecules be controlled such that the concentration of antimicrobials remains above the MIC. The concentration should remain there over the duration of use of the antimicrobial article.
- the desired rate of exchange of the antimicrobial can depend upon a number of factors including the identity of the antimicrobial metal ion, the specific microbe to be targeted, and the intended use and duration of use of the antimicrobial article.
- Antimicrobial coatings are known in the prior art, for example as described in U.S. Patent Application Publication No. 2010/0034900. This disclosure teaches a method of coating a substrate with biocide particles dispersed into a coating so that the particles are in contact with the environment. Non-planar coatings are also known to provide surface topographies for non-toxic bio-adhesion control, for example as disclosed in U.S. Pat. No. 7,143,709.
- U.S. Pat. No. 5,662,991 describes a biocidal fabric with a pattern of biocidal beads.
- U.S. Pat. No. 5,980,620 discloses a means of inhibiting bacterial growth on a coated substrate comprising a substantially dry powder coating containing a biocide.
- U.S. Pat. No. 6,437,021 teaches a water-insoluble polymeric support containing a biocide. Methods for depositing thin silver-comprising films on non-conducting substrates are taught in U.S. Patent Application Publication No. 2014/0170298.
- the antimicrobial coatings and materials lose their efficacy over time. Due to the variety of environmental circumstances and usage patterns of such anti-microbial coatings and materials, it is difficult to know when they are no longer efficacious.
- a colored biocidal multi-layer structure includes:
- biocidal second layer on or over the first layer, the biocidal second layer of a second color different from the first color.
- the present invention provides a colored biocidal multi-layer structure that provides antimicrobial properties and is readily refreshed or replaced in response to a simply observed indication.
- FIG. 1 is a cross section illustrating an embodiment of the present invention
- FIG. 2 is a cross section of a multi-layer structure in another embodiment of the present invention.
- FIGS. 3 and 4 are plan views of a layer useful in embodiments of the present invention.
- FIG. 5 is a cross section of a non-planar embodiment of the present invention.
- FIGS. 6-8 are flow diagrams illustrating methods of the present invention.
- the present invention provides an antimicrobial article such as a bi-layer biocidal structure 5 shown in FIG. 1 of the present invention that includes a simply observed indication to replace the article.
- the indication is related, either directly or indirectly, to the antimicrobial efficacy of the article or is otherwise associated with the antimicrobial efficacy of the article.
- the indication is provided by apparent changes in color of at least portions of the article. The changes are, for example, patterns, text, or graphic elements formed in an underlying layer that are exposed as overlying layers exposed to the environment are degraded over time.
- the antimicrobial article is repeatedly washed and the repeated washing removes portions of the article to expose the indication and indicate that the article should be replaced.
- the biocidal multi-layer structure 5 includes a first layer 10 of a first color and a biocidal second layer 20 on or over the first layer 10 .
- the biocidal second layer 20 has a second color different from the first color.
- Any layers, for example adhesive or environmental protection layers, located between the first layer 10 and the second layer 20 are sufficiently transparent that the color of the first layer 10 is perceived by an observer through the second layer 10 .
- the first or second layers 10 , 20 are polymer or contain polymers, for example polymers coated as a liquid or laminated and then cured with heat, drying, or radiation.
- the first layer 10 is located on or over a support 30 , for example a substrate such as glass or plastic.
- the support 30 is adhered, for example with an adhesive layer 50 such as a pressure-sensitive adhesive or glue such as wall-paper glue, to a surface 8 .
- the surface 8 is any surface 8 , planar or non-planar that is desired to resist the growth of biologically undesirable organisms, including microbes, bacteria, or fungi.
- the surface 8 is a surface of a structure 40 , such as a wall, floor, table top, door, handle, cover, device surface, or any surface likely to come into contact with a human.
- the support 30 is any layer that is capable of supporting the first and second layers 10 , 20 and in different embodiments is rigid, flexible, or transparent and is made of a plastic, paper, or vinyl or combinations of materials.
- the support 30 has a support thickness 36 measured from a first support side 32 to an opposing second support side 34 that can, for example be adhered to the surface 8 .
- the biocidal multi-layer structure 5 can form a wall paper.
- the first layer 10 has a first-layer thickness 16 measured from a first-layer first side 12 to an opposing first-layer second side 14 that is, for example, adhered to the first support side 32 .
- the biocidal second layer 20 has a second-layer thickness 26 measured from a second-layer first side 22 to an opposing second-layer second side 24 that is, for example, adhered or cross linked to the first-layer first side 12 .
- an adhesion layer such as a binder primer layer 52 ( FIG. 2 ) is located between the first and second layers 10 , 20 to adhere the first and second layers 10 , 20 together.
- the biocidal second layer 20 is a biocidal layer.
- biocidal layer is meant herein any layer that resists the growth of undesirable biological organisms, including microbes, bacteria, or fungi or more generally, eukaryotes, prokaryotes, or viruses.
- the biocidal second layer 20 resists the growth, reproduction, or life of infectious micro-organisms that cause illness or death in humans and especially antibiotic-resistant strains of bacteria.
- the biocidal second layer 20 is rendered biocidal by including chemicals such as drugs in the biocidal second layer 20 or by including particles 60 such as ionic metals or metal salts in the biocidal second layer 20 .
- the particles 60 reside in the biocidal second layer 20 .
- the particles 60 in the biocidal second layer 20 are exposed particles 62 that extend from the second-layer first side 22 into the environment and can interact with any environmental contaminants or biological organisms in the environment. Exposed particles 62 are thus more likely to be efficacious in destroying microbes.
- the particles 60 are silver or copper, are a metal sulfate, have a silver component, are a salt, have a sulfur component, have a copper component, are a silver sulfate salt, or include phosphors.
- the biocidal second layer 20 is thinner than the first layer 10 so that the second-layer thickness 26 is less than the first-layer thickness 16 , thus reducing the quantity of particles 60 or drugs that are required in the biocidal second layer 20 .
- the second-layer thickness 26 is greater than the first-layer thickness 16 .
- the particles 60 of the bi-layer biocidal structure 5 in the biocidal second layer 20 have a variety of sizes, for example some particles are large particles 64 , others are smaller particles 60 , and some of either are exposed particles 62 .
- the particles 60 include both the large particles 64 and any exposed particles 62 .
- the biocidal second layer 20 has a second-layer thickness 26 that is less than at least one diameter of one or more of the particles 60 , has a second-layer thickness 26 that is less than a mean diameter of the particles 60 , or has a second-layer thickness 26 that is less than the median diameter of the particles 60 .
- the particles 62 have at least one diameter between 0.05 and 25 microns.
- the biocidal second layer 20 is greater than or equal to 0.5 microns thick and the biocidal second layer 20 is less than or equal to 20 microns thick.
- the second-layer thickness 26 is less than the diameter of a substantial number of particles 60 , some of the particles 60 are not necessarily exposed particles 62 .
- the first layer 10 includes particles 60 .
- both the first layer 10 and the biocidal second layer 20 include particles 60 and the particles 60 in the first layer 10 are the same kind of particles 60 as the particles 60 in the biocidal second layer 20 .
- the first layer 10 is patterned or has an indicator 70 .
- the indicator 70 or pattern can be text (for example the word “Replace”), graphic elements, pictograms, or pictures.
- the patterning or indicator 70 is a patterning having the first color.
- the first layer 10 simply has a different first color from the second color and the different color indicates that the biocidal second layer 20 should be replaced. Since the biocidal second layer 20 can, over time, become ineffective and need to be replaced, the first color, the pattern or the indicator 70 indicates that the biocidal second layer 20 should be replaced.
- the first color is red (a color of alarm or emergency in many cultures), is darker than the second color (since darker colors are associated with dirt in medical environments), or is black or gray.
- the second color is lighter than the first color or is a color associated in some cultures with cleanliness or purity, such as white, blue, or green.
- the biocidal second layer 20 is non-planar.
- Such non-planar layers are made in curable polymer layers with a stamp using imprinting methods known in the art.
- the first and second layers 10 , 20 are formed on the support 30 .
- the non-planar second layer includes the particles 60 and the exposed particles 62 and has indentations 80 .
- the indentations 80 form a topographical non-planar layer in the biocidal second layer 20 that is inhospitable to the growth and reproduction of microbes.
- the first or second layers 10 , 20 have a hydrophobic surface, for example by providing a roughened surface either by imprinting or by a treatment such as sandblasting or exposure to energetic gases or plasmas.
- the first layer 10 , the biocidal second layer 20 , or the support 30 is or includes a heat-shrink film, for example polyolefin, polyvinylchloride, polyethylene, or polypropylene.
- a heat-shrink film for example polyolefin, polyvinylchloride, polyethylene, or polypropylene.
- Any of the first layer 10 , the biocidal second layer 20 , or the support 30 can include cross linking materials that are cross linked for example by radiation or heat to provide strength.
- FIG. 6 is a flow chart illustrating various methods of the present invention.
- a method of making a colored biocidal multi-layer structure 5 includes providing the support 30 in step 100 and forming the first layer 10 on the support 30 in step 105 .
- the support 30 and first layer 10 are the same structure provided as a single element.
- the first layer 10 has a first color.
- the first color is patterned in the first layer 10 in step 110 , for example forming text, graphics, graphic elements, pictures, or pictograms.
- the support 30 is paper or plastic and the first layer 10 is plastic, for example a polymer or a cross linkable polymer that is curable.
- the first layer 10 is patterned in any of a variety of ways known in the art, for example by printing with ink transfer from a patterned surface or by inkjet patterning.
- the first layer 10 is formed in various ways, including extrusion or coating, for example spin coating, curtain coating, or hopper coating, or other methods known in the art.
- the first layer 10 is cured, if necessary, for example by heat or radiation in step 115 .
- the biocidal second layer 20 is also formed in various methods known in the art and is a biocidal layer that includes biocidal materials such as drugs, biocides, or particles 60 .
- the biocidal second layer 20 has a second color different from the first color.
- a dispersion of particles 60 is formed in a carrier such as a liquid in step 140 and located on the cured first layer 10 in step 120 , for example by coating, to form the biocidal second layer 20 . Making and coating liquids with dispersed particles is known in the art.
- the biocidal second layer 20 is made separately and laminated on or over the first layer 10 .
- the biocidal second layer 20 is imprinted in step 125 and cured in step 130 to form the non-planar biocidal second layer 20 including biocidal particles 60 .
- Imprinting methods are known in the art and employ a stamp pressed against an uncured layer that is then cured and the stamp removed.
- a portion of the biocidal second layer 20 is removed in step 135 , for example to expose the particles 60 to form exposed particles 62 or increase the surface area of the exposed particles 62 that is exposed.
- Removal of portions of the biocidal second layer 20 is accomplished in step 135 , for example, by exposing the biocidal second layer 20 and particles 60 to energetic particles such as gases or plasma, for example using processes such as etching, plasma etching, reactive plasma etching, ion etching, or sandblasting. Such removal methods are known in the art.
- the biocidal second layer 20 is formed, imprinted, and treated before it is located on or over the first layer 10 , for example by lamination.
- a surface 8 is identified.
- the surface 8 is a surface which it is desired to keep free of microbes, for example a wall, floor, table top, door, handle, knob, cover, or device surface, especially any surface found in a any type of medical institution.
- the surface 8 is planar; in another embodiment, the surface 8 is non-planar.
- an adhesive is located, for example on the surface 8 or on the second support side 34 of the support 30 opposite the surface 8 , to form an adhesive layer 50 .
- the support 30 is adhered to the surface 8 in step 160 .
- the support 30 , first layer 10 , and biocidal second layer 20 are heated to shrink the layers on the surface 8 if the surface 8 is non-planar.
- the heating step (not shown separately) is also the adhesion step 160 and a separate adhesive layer 50 is not necessary or used.
- the biocidal second layer 20 is thinner than the first layer 10 .
- the biocidal second layer 20 is formed to have a thickness such that the particles 60 extend from a surface (e.g. second-layer first side 22 ) of the biocidal second layer 20 and a portion of the particle's surface area is exposed.
- the biocidal second layer 20 is formed with a thickness that is less than at least one diameter of one or more of the particles 60 , has a thickness that is less than a mean diameter of the particles 60 , or has a thickness that is less than the median diameter of the particles 60 .
- the first layer 10 is a biocidal first layer 10 and includes drugs or anti-microbial particles 60 .
- the first layer 10 is formed as a dispersion with particles or a liquid with multiple components that are coated over the support 30 or formed into a layer that is laminated to the support 30 or formed into a free-standing layer on which the biocidal second layer 20 is located.
- the biocidal second layer 20 includes one or more particles 60 in a liquid and the particles 60 self-segregate in the liquid before the liquid is cured.
- the particles 60 self-segregate after the liquid is coated, for example over or on first layer 10 , and before the liquid is cured to form the biocidal second layer 20 .
- the self-segregating particles aggregate at the second-layer first side 22 of the biocidal second layer 20 .
- the first layer 10 includes one or more particles 60
- a method of the present invention further includes forming the first layer 10 so that the particles 60 extend from a portion of the surface of the first layer 10 and are exposed and optionally further including removing a portion of the first layer surface and increasing the exposed surface area of the particles 60 , for example by etching, plasma etching, reactive plasma etching, ion etching, or sandblasting.
- the colored biocidal multi-layer structure 5 is used by first locating the structure in step 200 , for example on the surface 8 on which it is desired to inhibit the presence of microbes.
- the colored biocidal multi-layer structure 5 is observed over time in step 205 , especially with respect to the structure's color or appearance and the visibility of the patterns described above (e.g. as shown in FIGS. 3 and 4 ).
- the colored biocidal multi-layer structure 5 and especially the biocidal second layer 20 is periodically cleaned in step 210 to remove dirt and any microbes, alive or dead, on the surface (e.g. second-layer first side 22 ) of the biocidal second layer 20 .
- the cleaning process of step 210 gradually abrades or dissolves the biocidal second layer 20 so that over time the biocidal second layer 20 is at least partially removed and the first color or patterning of the first layer 10 is revealed. As long as the biocidal second layer 20 remains sufficiently in place, no color or pattern change is observed in step 215 and the periodic cleaning continues. Eventually, the color change is observed in step 215 and the biocidal layer 20 is replaced in step 220 .
- the colored biocidal multi-layer structure 5 or portions of the colored biocidal multi-layer structure 5 are replaced when the first color of the first layer 10 becomes apparent.
- another colored biocidal multi-layer structure 5 is simply located over the colored biocidal multi-layer structure 5 .
- the colored biocidal multi-layer structure 5 becomes the structure 40 and another colored biocidal multi-layer structure 5 is applied to the structure 40 , for example with an adhesive layer 50 ( FIG. 1 ).
- the colored biocidal multi-layer structure 5 is removed and another colored biocidal multi-layer structure 5 put in its place. As shown in FIG.
- the support 30 is adhered to the structure 40 with an adhesive layer 50 .
- Chemical or heat treatments are applied to the colored biocidal multi-layer structure 5 to loosen, dissolve, or remove the adhesive layer 50 so the colored biocidal multi-layer structure 5 can be removed and another adhesive layer 50 is applied to the structure 40 .
- the colored biocidal multi-layer structure 5 is peeled from the structure 40 and another colored biocidal multi-layer structure 5 having an adhesive layer 50 on the third-layer second support side 34 adhered to the structure 40 .
- portions of the colored biocidal multi-layer structure 5 are removed, for example at least a portion of the biocidal second layer 20 is mechanically separated from the first layer 10 .
- the biocidal second layer 20 is peeled from the first layer 10 .
- the biocidal second layer 20 is abraded and removed by abrasion from the first layer 10 .
- the biocidal second layer 20 is chemically separable from the first layer 10 or chemically dissolvable in a substance that does not dissolve the first layer 10 .
- a substance that chemically separates the biocidal second layer 20 from the first layer 10 or that chemically dissolves the biocidal second layer 20 is a cleaning agent.
- the biocidal second layer 20 is repeatedly cleaned, for example by spraying the biocidal second layer 20 with a cleaning agent and then rubbing or wiping the biocidal second layer 20 , and at each cleaning a portion of the biocidal second layer 20 is removed to gradually expose the first layer 10 , the first color of the first layer 10 , and the indicator 70 .
- fluorescent or phosphorescent materials are included in the biocidal second layer 20 and are illuminated in step 212 .
- the fluorescent or phosphorescent materials respond to ultra-violet, visible, or infrared illumination and emit light that can be seen or detected in step 213 and compared to a threshold emission value in step 214 .
- a threshold emission value in step 214 .
- the cleaning step 215 refreshes the biocidal second layer 20 so that the exposed particles 60 in the biocidal second layer 20 are more efficacious. This can be done, for example, by ionizing the particles 70 , by removing oxidation layers on the particles 60 , or by removing extraneous materials such as dust from the particles 70 .
- Useful cleaners include hydrogen peroxide, for example 2% hydrogen peroxide, water, soap in water, or a citrus-based cleaner.
- the 2% hydrogen peroxide solution is reactive to make oxygen radicals that improve the efficacy of particles 60 .
- cleaning is accomplished by spraying the second-layer first side 22 of the biocidal second layer 20 with a cleaner and then wiping or rubbing the second-layer first side 22 .
- the cleaner can dissolve the biocidal second layer 20 material and the wiping or rubbing can remove dissolved material or abrade the second-layer first side 22 of the biocidal second layer 20 to expose other particles 60 or increase the exposed surface area of exposed particles 62 .
- the present invention is useful in a wide variety of environments and on a wide variety of surfaces 8 , particularly surfaces 8 that are frequently handled by humans.
- the present invention can reduce the microbial load in an environment and is especially useful in medical facilities.
Abstract
Description
- Reference is made to commonly-assigned co-pending U.S. patent application Ser. No. ______ (Attorney Docket No. K001887) filed concurrently herewith, entitled Making Colored Biocidal Multi-Layer Structure, by Scheible et al, to commonly-assigned co-pending U.S. patent application Ser. No. ______ (Attorney Docket No. K001888) filed concurrently herewith, entitled Using Colored Biocidal Multi-Layer Structure, by Scheible et al, to commonly-assigned co-pending U.S. patent application Ser. No. 13/235,789, filed Sep. 19, 2011, entitled Antibacterial and Antifungal Protection for Toner Image, by Blanton et al, and to commonly-assigned co-pending U.S. patent application Ser. No. 13/357,082, filed Jan. 24, 2012, entitled Ink Having Antibacterial and Antifungal Protection, by Blanton et al, the disclosures of which are incorporated herein.
- The present invention relates to biocidal layers having antimicrobial efficacy on a surface.
- Widespread attention has been focused in recent years on the consequences of bacterial and fungal contamination contracted by contact with common surfaces and objects. Some noteworthy examples include the sometimes fatal outcome from food poisoning due to the presence of particular strains of Escherichia coli in undercooked beef; Salmonella contamination in undercooked and unwashed poultry food products; as well as illnesses and skin irritations due to Staphylococcus aureus and other micro-organisms. Anthrax is an acute infectious disease caused by the spore-forming bacterium bacillus anthracis. Allergic reactions to molds and yeasts are a major concern to many consumers and insurance companies alike. In addition, significant fear has arisen in regard to the development of antibiotic-resistant strains of bacteria, such as methicillin-resistant Staphylococcus aureus (MRSA) and vancomycin-resistant Enterococcus (VRE). The U.S. Centers for Disease Control and Prevention estimates that 10% of patients contract additional diseases during their hospital stay and that the total deaths resulting from these nosocomially-contracted illnesses exceeds those suffered from vehicular traffic accidents and homicides. In response to these concerns, manufacturers have begun incorporating antimicrobial agents into materials used to produce objects for commercial, institutional, residential, and personal use.
- Noble metal ions such as silver and gold ions are known for their antimicrobial properties and have been used in medical care for many years to prevent and treat infection. In recent years, this technology has been applied to consumer products to prevent the transmission of infectious disease and to kill harmful bacteria such as Staphylococcus aureus and Salmonella. In common practice, noble metals, metal ions, metal salts, or compounds containing metal ions having antimicrobial properties can be applied to surfaces to impart an antimicrobial property to the surface. If, or when, the surface is inoculated with harmful microbes, the antimicrobial metal ions or metal complexes, if present in effective concentrations, will slow or even prevent altogether the growth of those microbes. Recently, silver sulfate, Ag2SO4, described in U.S. Pat. No. 7,579,396, U.S. Patent Application Publication 2008/0242794, U.S. Patent Application Publication 2009/0291147, U.S. Patent Application Publication 2010/0093851, and U.S. Patent Application Publication 2010/0160486 has been shown to have efficacy in providing antimicrobial protection in polymer composites. The United States Environmental Protection Agency (EPA) evaluated silver sulfate as a biocide and registered its use as part of EPA Reg. No, 59441-8 EPA EST. NO. 59441-NY-001. In granting that registration, the EPA determined that silver sulfate was safe and effective in providing antibacterial and antifungal protection.
- Antimicrobial activity is not limited to noble metals but is also observed in other metals such as copper and organic materials such as triclosan, and some polymeric materials.
- It is important that the antimicrobial active element, molecule, or compound be present on the surface of the article at a concentration sufficient to inhibit microbial growth. This concentration, for a particular antimicrobial agent and bacterium, is often referred to as the minimum inhibitory concentration (MIC). It is also important that the antimicrobial agent be present on the surface of the article at a concentration significantly below that which can be harmful to the user of the article. This prevents harmful side effects of the article and decreases the risk to the user, while providing the benefit of reducing microbial contamination. There is a problem in that the rate of release of antimicrobial ions from antimicrobial films can be too facile, such that the antimicrobial article can quickly be depleted of antimicrobial active materials and become inert or non-functional. Depletion results from rapid diffusion of the active materials into the biological environment with which they are in contact, for example, water soluble biocides exposed to aqueous or humid environments. It is desirable that the rate of release of the antimicrobial ions or molecules be controlled such that the concentration of antimicrobials remains above the MIC. The concentration should remain there over the duration of use of the antimicrobial article. The desired rate of exchange of the antimicrobial can depend upon a number of factors including the identity of the antimicrobial metal ion, the specific microbe to be targeted, and the intended use and duration of use of the antimicrobial article.
- Antimicrobial coatings are known in the prior art, for example as described in U.S. Patent Application Publication No. 2010/0034900. This disclosure teaches a method of coating a substrate with biocide particles dispersed into a coating so that the particles are in contact with the environment. Non-planar coatings are also known to provide surface topographies for non-toxic bio-adhesion control, for example as disclosed in U.S. Pat. No. 7,143,709.
- Fabrics or materials incorporating biocidal elements are known in the art and commercially available. U.S. Pat. No. 5,662,991 describes a biocidal fabric with a pattern of biocidal beads. U.S. Pat. No. 5,980,620 discloses a means of inhibiting bacterial growth on a coated substrate comprising a substantially dry powder coating containing a biocide. U.S. Pat. No. 6,437,021 teaches a water-insoluble polymeric support containing a biocide. Methods for depositing thin silver-comprising films on non-conducting substrates are taught in U.S. Patent Application Publication No. 2014/0170298.
- However, as noted above, the antimicrobial coatings and materials lose their efficacy over time. Due to the variety of environmental circumstances and usage patterns of such anti-microbial coatings and materials, it is difficult to know when they are no longer efficacious.
- There is a need, therefore, for an anti-microbial article that is readily replaced or refreshed in response to a simply observed indication incorporated into the anti-microbial article.
- In accordance with the present invention, a colored biocidal multi-layer structure includes:
- a first layer of a first color; and
- a biocidal second layer on or over the first layer, the biocidal second layer of a second color different from the first color.
- The present invention provides a colored biocidal multi-layer structure that provides antimicrobial properties and is readily refreshed or replaced in response to a simply observed indication.
- The above and other features and advantages of the present invention will become more apparent when taken in conjunction with the following description and drawings wherein identical reference numerals have been used to designate identical features that are common to the figures, and wherein:
-
FIG. 1 is a cross section illustrating an embodiment of the present invention; -
FIG. 2 is a cross section of a multi-layer structure in another embodiment of the present invention; -
FIGS. 3 and 4 are plan views of a layer useful in embodiments of the present invention; -
FIG. 5 is a cross section of a non-planar embodiment of the present invention; and -
FIGS. 6-8 are flow diagrams illustrating methods of the present invention. - The Figures are not drawn to scale since the variation in size of various elements in the Figures is too great to permit depiction to scale.
- The present invention provides an antimicrobial article such as a bi-layer
biocidal structure 5 shown inFIG. 1 of the present invention that includes a simply observed indication to replace the article. In an embodiment, the indication is related, either directly or indirectly, to the antimicrobial efficacy of the article or is otherwise associated with the antimicrobial efficacy of the article. The indication is provided by apparent changes in color of at least portions of the article. The changes are, for example, patterns, text, or graphic elements formed in an underlying layer that are exposed as overlying layers exposed to the environment are degraded over time. In one method of the present invention, the antimicrobial article is repeatedly washed and the repeated washing removes portions of the article to expose the indication and indicate that the article should be replaced. - Referring to
FIG. 1 , in an embodiment of the present invention, the biocidalmulti-layer structure 5 includes afirst layer 10 of a first color and a biocidalsecond layer 20 on or over thefirst layer 10. The biocidalsecond layer 20 has a second color different from the first color. Any layers, for example adhesive or environmental protection layers, located between thefirst layer 10 and thesecond layer 20 are sufficiently transparent that the color of thefirst layer 10 is perceived by an observer through thesecond layer 10. In an embodiment, the first orsecond layers - In an embodiment, the
first layer 10 is located on or over asupport 30, for example a substrate such as glass or plastic. In a useful arrangement, thesupport 30 is adhered, for example with anadhesive layer 50 such as a pressure-sensitive adhesive or glue such as wall-paper glue, to asurface 8. Thesurface 8 is anysurface 8, planar or non-planar that is desired to resist the growth of biologically undesirable organisms, including microbes, bacteria, or fungi. In various applications, thesurface 8 is a surface of astructure 40, such as a wall, floor, table top, door, handle, cover, device surface, or any surface likely to come into contact with a human. - The
support 30 is any layer that is capable of supporting the first andsecond layers support 30 has asupport thickness 36 measured from afirst support side 32 to an opposingsecond support side 34 that can, for example be adhered to thesurface 8. The biocidalmulti-layer structure 5 can form a wall paper. - The
first layer 10 has a first-layer thickness 16 measured from a first-layerfirst side 12 to an opposing first-layersecond side 14 that is, for example, adhered to thefirst support side 32. The biocidalsecond layer 20 has a second-layer thickness 26 measured from a second-layerfirst side 22 to an opposing second-layer second side 24 that is, for example, adhered or cross linked to the first-layerfirst side 12. Alternatively, an adhesion layer such as a binder primer layer 52 (FIG. 2 ) is located between the first andsecond layers second layers - The biocidal
second layer 20 is a biocidal layer. By biocidal layer is meant herein any layer that resists the growth of undesirable biological organisms, including microbes, bacteria, or fungi or more generally, eukaryotes, prokaryotes, or viruses. In particular, the biocidalsecond layer 20 resists the growth, reproduction, or life of infectious micro-organisms that cause illness or death in humans and especially antibiotic-resistant strains of bacteria. In various embodiments, the biocidalsecond layer 20 is rendered biocidal by including chemicals such as drugs in the biocidalsecond layer 20 or by includingparticles 60 such as ionic metals or metal salts in the biocidalsecond layer 20. Theparticles 60 reside in the biocidalsecond layer 20. In an embodiment, some of theparticles 60 in the biocidalsecond layer 20 are exposedparticles 62 that extend from the second-layerfirst side 22 into the environment and can interact with any environmental contaminants or biological organisms in the environment.Exposed particles 62 are thus more likely to be efficacious in destroying microbes. In various embodiments, theparticles 60 are silver or copper, are a metal sulfate, have a silver component, are a salt, have a sulfur component, have a copper component, are a silver sulfate salt, or include phosphors. In an embodiment, the biocidalsecond layer 20 is thinner than thefirst layer 10 so that the second-layer thickness 26 is less than the first-layer thickness 16, thus reducing the quantity ofparticles 60 or drugs that are required in the biocidalsecond layer 20. In an alternative embodiment, the second-layer thickness 26 is greater than the first-layer thickness 16. - Referring further to
FIG. 2 , theparticles 60 of the bi-layerbiocidal structure 5 in the biocidalsecond layer 20 have a variety of sizes, for example some particles arelarge particles 64, others aresmaller particles 60, and some of either are exposedparticles 62. Theparticles 60 include both thelarge particles 64 and any exposedparticles 62. In an embodiment, the biocidalsecond layer 20 has a second-layer thickness 26 that is less than at least one diameter of one or more of theparticles 60, has a second-layer thickness 26 that is less than a mean diameter of theparticles 60, or has a second-layer thickness 26 that is less than the median diameter of theparticles 60. In another embodiment, theparticles 62 have at least one diameter between 0.05 and 25 microns. Suitable particles with such a size range have been made. Alternatively, the biocidalsecond layer 20 is greater than or equal to 0.5 microns thick and the biocidalsecond layer 20 is less than or equal to 20 microns thick. When the second-layer thickness 26 is less than the diameter of a substantial number ofparticles 60, some of theparticles 60 are not necessarily exposedparticles 62. - In another embodiment and as shown in
FIG. 2 , thefirst layer 10 includesparticles 60. Alternatively, both thefirst layer 10 and the biocidalsecond layer 20 includeparticles 60 and theparticles 60 in thefirst layer 10 are the same kind ofparticles 60 as theparticles 60 in the biocidalsecond layer 20. - Referring to
FIGS. 3 and 4 , according to embodiments of the present invention, thefirst layer 10 is patterned or has anindicator 70. Theindicator 70 or pattern can be text (for example the word “Replace”), graphic elements, pictograms, or pictures. In an embodiment, the patterning orindicator 70 is a patterning having the first color. Alternatively, thefirst layer 10 simply has a different first color from the second color and the different color indicates that the biocidalsecond layer 20 should be replaced. Since the biocidalsecond layer 20 can, over time, become ineffective and need to be replaced, the first color, the pattern or theindicator 70 indicates that the biocidalsecond layer 20 should be replaced. - In various embodiments, the first color is red (a color of alarm or emergency in many cultures), is darker than the second color (since darker colors are associated with dirt in medical environments), or is black or gray. Alternatively or in addition, for similar reasons in some embodiments the second color is lighter than the first color or is a color associated in some cultures with cleanliness or purity, such as white, blue, or green.
- Referring to
FIG. 5 , in an embodiment the biocidalsecond layer 20 is non-planar. Such non-planar layers are made in curable polymer layers with a stamp using imprinting methods known in the art. As shown inFIG. 5 , the first andsecond layers support 30. The non-planar second layer includes theparticles 60 and the exposedparticles 62 and hasindentations 80. Theindentations 80 form a topographical non-planar layer in the biocidalsecond layer 20 that is inhospitable to the growth and reproduction of microbes. In yet another embodiment, the first orsecond layers - In a further embodiment of the present invention, the
first layer 10, the biocidalsecond layer 20, or thesupport 30 is or includes a heat-shrink film, for example polyolefin, polyvinylchloride, polyethylene, or polypropylene. Any of thefirst layer 10, the biocidalsecond layer 20, or thesupport 30 can include cross linking materials that are cross linked for example by radiation or heat to provide strength. -
FIG. 6 is a flow chart illustrating various methods of the present invention. Referring toFIG. 6 , a method of making a colored biocidalmulti-layer structure 5 includes providing thesupport 30 instep 100 and forming thefirst layer 10 on thesupport 30 instep 105. In one embodiment, thesupport 30 andfirst layer 10 are the same structure provided as a single element. Thefirst layer 10 has a first color. In an optional embodiment, the first color is patterned in thefirst layer 10 instep 110, for example forming text, graphics, graphic elements, pictures, or pictograms. In various embodiments, thesupport 30 is paper or plastic and thefirst layer 10 is plastic, for example a polymer or a cross linkable polymer that is curable. Thefirst layer 10 is patterned in any of a variety of ways known in the art, for example by printing with ink transfer from a patterned surface or by inkjet patterning. Thefirst layer 10 is formed in various ways, including extrusion or coating, for example spin coating, curtain coating, or hopper coating, or other methods known in the art. Thefirst layer 10 is cured, if necessary, for example by heat or radiation instep 115. - The biocidal
second layer 20 is also formed in various methods known in the art and is a biocidal layer that includes biocidal materials such as drugs, biocides, orparticles 60. The biocidalsecond layer 20 has a second color different from the first color. In an embodiment, a dispersion ofparticles 60 is formed in a carrier such as a liquid instep 140 and located on the curedfirst layer 10 instep 120, for example by coating, to form the biocidalsecond layer 20. Making and coating liquids with dispersed particles is known in the art. In an alternative, the biocidalsecond layer 20 is made separately and laminated on or over thefirst layer 10. - Optionally, the biocidal
second layer 20 is imprinted instep 125 and cured instep 130 to form the non-planar biocidalsecond layer 20 includingbiocidal particles 60. Imprinting methods are known in the art and employ a stamp pressed against an uncured layer that is then cured and the stamp removed. Again optionally, a portion of the biocidalsecond layer 20 is removed instep 135, for example to expose theparticles 60 to form exposedparticles 62 or increase the surface area of the exposedparticles 62 that is exposed. Removal of portions of the biocidalsecond layer 20 is accomplished instep 135, for example, by exposing the biocidalsecond layer 20 andparticles 60 to energetic particles such as gases or plasma, for example using processes such as etching, plasma etching, reactive plasma etching, ion etching, or sandblasting. Such removal methods are known in the art. In other embodiments, the biocidalsecond layer 20 is formed, imprinted, and treated before it is located on or over thefirst layer 10, for example by lamination. - In
step 150, asurface 8 is identified. Thesurface 8 is a surface which it is desired to keep free of microbes, for example a wall, floor, table top, door, handle, knob, cover, or device surface, especially any surface found in a any type of medical institution. In an embodiment, thesurface 8 is planar; in another embodiment, thesurface 8 is non-planar. Instep 155, an adhesive is located, for example on thesurface 8 or on thesecond support side 34 of thesupport 30 opposite thesurface 8, to form anadhesive layer 50. Thesupport 30 is adhered to thesurface 8 instep 160. In a further embodiment, thesupport 30,first layer 10, and biocidalsecond layer 20 are heated to shrink the layers on thesurface 8 if thesurface 8 is non-planar. In an embodiment, the heating step (not shown separately) is also theadhesion step 160 and a separateadhesive layer 50 is not necessary or used. In an embodiment, the biocidalsecond layer 20 is thinner than thefirst layer 10. In another embodiment, the biocidalsecond layer 20 is formed to have a thickness such that theparticles 60 extend from a surface (e.g. second-layer first side 22) of the biocidalsecond layer 20 and a portion of the particle's surface area is exposed. For example, the biocidalsecond layer 20 is formed with a thickness that is less than at least one diameter of one or more of theparticles 60, has a thickness that is less than a mean diameter of theparticles 60, or has a thickness that is less than the median diameter of theparticles 60. - In a further embodiment, the
first layer 10 is a biocidalfirst layer 10 and includes drugs oranti-microbial particles 60. In such an embodiment, thefirst layer 10 is formed as a dispersion with particles or a liquid with multiple components that are coated over thesupport 30 or formed into a layer that is laminated to thesupport 30 or formed into a free-standing layer on which the biocidalsecond layer 20 is located. In an alternative, the biocidalsecond layer 20 includes one ormore particles 60 in a liquid and theparticles 60 self-segregate in the liquid before the liquid is cured. In an embodiment, theparticles 60 self-segregate after the liquid is coated, for example over or onfirst layer 10, and before the liquid is cured to form the biocidalsecond layer 20. In another embodiment, the self-segregating particles aggregate at the second-layerfirst side 22 of the biocidalsecond layer 20. - In another embodiment, the
first layer 10 includes one ormore particles 60, and a method of the present invention further includes forming thefirst layer 10 so that theparticles 60 extend from a portion of the surface of thefirst layer 10 and are exposed and optionally further including removing a portion of the first layer surface and increasing the exposed surface area of theparticles 60, for example by etching, plasma etching, reactive plasma etching, ion etching, or sandblasting. - Referring to
FIG. 7 , in another method of the present invention, the colored biocidalmulti-layer structure 5 is used by first locating the structure instep 200, for example on thesurface 8 on which it is desired to inhibit the presence of microbes. The colored biocidalmulti-layer structure 5 is observed over time instep 205, especially with respect to the structure's color or appearance and the visibility of the patterns described above (e.g. as shown inFIGS. 3 and 4 ). The colored biocidalmulti-layer structure 5 and especially the biocidalsecond layer 20 is periodically cleaned instep 210 to remove dirt and any microbes, alive or dead, on the surface (e.g. second-layer first side 22) of the biocidalsecond layer 20. According to various embodiments of the present invention, the cleaning process ofstep 210 gradually abrades or dissolves the biocidalsecond layer 20 so that over time the biocidalsecond layer 20 is at least partially removed and the first color or patterning of thefirst layer 10 is revealed. As long as the biocidalsecond layer 20 remains sufficiently in place, no color or pattern change is observed instep 215 and the periodic cleaning continues. Eventually, the color change is observed instep 215 and thebiocidal layer 20 is replaced instep 220. - Replacement can proceed in a variety of ways. According to various embodiments of the present invention, the colored biocidal
multi-layer structure 5, or portions of the colored biocidalmulti-layer structure 5 are replaced when the first color of thefirst layer 10 becomes apparent. In one embodiment, another colored biocidalmulti-layer structure 5 is simply located over the colored biocidalmulti-layer structure 5. Thus, the colored biocidalmulti-layer structure 5 becomes thestructure 40 and another colored biocidalmulti-layer structure 5 is applied to thestructure 40, for example with an adhesive layer 50 (FIG. 1 ). In another embodiment, the colored biocidalmulti-layer structure 5 is removed and another colored biocidalmulti-layer structure 5 put in its place. As shown inFIG. 1 , thesupport 30 is adhered to thestructure 40 with anadhesive layer 50. Chemical or heat treatments are applied to the colored biocidalmulti-layer structure 5 to loosen, dissolve, or remove theadhesive layer 50 so the colored biocidalmulti-layer structure 5 can be removed and anotheradhesive layer 50 is applied to thestructure 40. In an embodiment, the colored biocidalmulti-layer structure 5 is peeled from thestructure 40 and another colored biocidalmulti-layer structure 5 having anadhesive layer 50 on the third-layersecond support side 34 adhered to thestructure 40. - Alternatively, portions of the colored biocidal
multi-layer structure 5 are removed, for example at least a portion of the biocidalsecond layer 20 is mechanically separated from thefirst layer 10. In an embodiment, the biocidalsecond layer 20 is peeled from thefirst layer 10. Alternatively, the biocidalsecond layer 20 is abraded and removed by abrasion from thefirst layer 10. As the biocidalsecond layer 20 is removed, the first color, pattern, orindicator 70 of thefirst layer 10 becomes increasingly visible. In another embodiment, the biocidalsecond layer 20 is chemically separable from thefirst layer 10 or chemically dissolvable in a substance that does not dissolve thefirst layer 10. In a useful embodiment, a substance that chemically separates the biocidalsecond layer 20 from thefirst layer 10 or that chemically dissolves the biocidalsecond layer 20 is a cleaning agent. In an embodiment, the biocidalsecond layer 20 is repeatedly cleaned, for example by spraying the biocidalsecond layer 20 with a cleaning agent and then rubbing or wiping the biocidalsecond layer 20, and at each cleaning a portion of the biocidalsecond layer 20 is removed to gradually expose thefirst layer 10, the first color of thefirst layer 10, and theindicator 70. - Referring to
FIG. 8 in another embodiment of the present invention, fluorescent or phosphorescent materials are included in the biocidalsecond layer 20 and are illuminated instep 212. The fluorescent or phosphorescent materials respond to ultra-violet, visible, or infrared illumination and emit light that can be seen or detected instep 213 and compared to a threshold emission value instep 214. Thus, the continuing presence of the biocidalsecond layer 20 is observed. When light emission in response to illumination is no longer present at a desired level, the biocidalsecond layer 20 is replaced. - According to yet another embodiment of the present invention, the cleaning
step 215 refreshes the biocidalsecond layer 20 so that the exposedparticles 60 in the biocidalsecond layer 20 are more efficacious. This can be done, for example, by ionizing theparticles 70, by removing oxidation layers on theparticles 60, or by removing extraneous materials such as dust from theparticles 70. - Useful cleaners include hydrogen peroxide, for example 2% hydrogen peroxide, water, soap in water, or a citrus-based cleaner. In an embodiment, the 2% hydrogen peroxide solution is reactive to make oxygen radicals that improve the efficacy of
particles 60. In various embodiments, cleaning is accomplished by spraying the second-layerfirst side 22 of the biocidalsecond layer 20 with a cleaner and then wiping or rubbing the second-layerfirst side 22. The cleaner can dissolve the biocidalsecond layer 20 material and the wiping or rubbing can remove dissolved material or abrade the second-layerfirst side 22 of the biocidalsecond layer 20 to exposeother particles 60 or increase the exposed surface area of exposedparticles 62. - The present invention is useful in a wide variety of environments and on a wide variety of
surfaces 8, particularly surfaces 8 that are frequently handled by humans. The present invention can reduce the microbial load in an environment and is especially useful in medical facilities. - The invention has been described in detail with particular reference to certain embodiments thereof, but it will be understood that variations and modifications can be effected within the spirit and scope of the invention.
-
- 5 bi-layer biocidal structure
- 8 surface
- 10 first layer
- 12 first-layer first side
- 14 first-layer second side
- 16 first-layer thickness
- 20 second layer
- 22 second-layer first side
- 24 second-layer second side
- 26 second-layer thickness
- 30 support
- 32 first support side
- 34 second support side
- 36 support thickness
- 40 structure
- 50 adhesive layer
- 52 binder primer
- 60 particle
- 62 exposed particle
- 64 large particle
- 70 indicator
- 80 indentations
- 100 provide support step
- 105 provide first layer step
- 110 pattern first layer step
- 115 cure first layer step
- 120 locate second layer step
- 125 imprint second layer step
- 130 cure second layer step
-
- 135 remove second layer portion step
- 140 form dispersion step
- 150 identify surface step
- 155 locate adhesive step
- 160 adhere support to surface step
- 200 locate structure step
- 205 observe structure step
- 210 clean structure step
- 212 illuminate structure step
- 213 sufficient emission comparison step
- 214 detect emission step
- 215 observe color change step
- 220 replace biocidal layer step
Claims (26)
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US14/519,425 US20160107415A1 (en) | 2011-09-19 | 2014-10-21 | Colored biocidal multi-layer structure |
US14/526,646 US9480249B2 (en) | 2014-10-21 | 2014-10-29 | Imprinted particle structure |
US14/645,762 US20160262380A1 (en) | 2012-01-24 | 2015-03-12 | Biocidal article with patterned adhesive layer |
US14/645,789 US20160263860A1 (en) | 2012-01-24 | 2015-03-12 | Biocidal device with patterned adhesive layer |
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
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US13/235,789 US20130071143A1 (en) | 2011-09-19 | 2011-09-19 | Antibacterial and antifungal protection for toner image |
US13/357,082 US20130186301A1 (en) | 2012-01-24 | 2012-01-24 | Ink having antibacterial and antifungal protection |
US14/519,425 US20160107415A1 (en) | 2011-09-19 | 2014-10-21 | Colored biocidal multi-layer structure |
Publications (1)
Publication Number | Publication Date |
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US20160107415A1 true US20160107415A1 (en) | 2016-04-21 |
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US14/519,425 Abandoned US20160107415A1 (en) | 2011-09-19 | 2014-10-21 | Colored biocidal multi-layer structure |
US14/519,451 Expired - Fee Related US9358577B2 (en) | 2011-09-19 | 2014-10-21 | Making colored biocidal multi-layer structure |
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US14/519,451 Expired - Fee Related US9358577B2 (en) | 2011-09-19 | 2014-10-21 | Making colored biocidal multi-layer structure |
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US (2) | US20160107415A1 (en) |
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US20020000041A1 (en) * | 1994-01-28 | 2002-01-03 | Siamak Doroodian-Shoja | Disposable razor wear indicator |
US20050287353A1 (en) * | 2004-06-24 | 2005-12-29 | Trogolo Jeffrey A | Antimicrobial coating for erosive environments |
US20080148512A1 (en) * | 2006-12-13 | 2008-06-26 | Jonas Beskow | Wet/Dry Floor Cleaning Device |
US20090130157A1 (en) * | 2005-12-14 | 2009-05-21 | Ylitalo Caroline M | Antimicrobial Adhesive Films |
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US5662991A (en) | 1994-12-23 | 1997-09-02 | Gentex Corporation | Laminated biocidal fabric |
BR9612636A (en) | 1996-06-05 | 1999-07-20 | Rainer Clover | Bacterial growth inhibition |
FR2786064B1 (en) | 1998-11-25 | 2000-12-29 | Eastman Kodak Co | NOVEL BIOCIDAL MATERIAL AND PROCESS FOR PREPARING SUCH MATERIAL |
US7143709B2 (en) | 2004-02-17 | 2006-12-05 | University Of Florida Research Foundation, Inc. | Surface topography for non-toxic bioadhesion control |
US7650848B2 (en) * | 2004-02-17 | 2010-01-26 | University Of Florida Research Foundation, Inc. | Surface topographies for non-toxic bioadhesion control |
US7579396B2 (en) | 2007-01-31 | 2009-08-25 | Eastman Kodak Company | Polymer composite |
US20080242794A1 (en) | 2007-03-30 | 2008-10-02 | Sandford David W | Color stabilized antimicrobial polymer composites |
JP2011530400A (en) | 2008-08-07 | 2011-12-22 | マディコ インコーポレイテッド | Manufacturing method of antibacterial coating |
US8158140B2 (en) | 2008-10-14 | 2012-04-17 | Eastman Kodak Company | Silver polyamide composite |
US8338514B2 (en) | 2008-12-19 | 2012-12-25 | Eastman Kodak Company | Polyolefin antimicrobial compositions and melt-processing methods |
CA2819030C (en) | 2010-11-26 | 2020-02-25 | C.R. Bard, Inc. | Deposition of a silver layer on a nonconducting substrate |
US20130189499A1 (en) * | 2012-01-24 | 2013-07-25 | Thomas Nelson Blanton | Antibacterial and antifungal protection for ink jet image |
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2014
- 2014-10-21 US US14/519,425 patent/US20160107415A1/en not_active Abandoned
- 2014-10-21 US US14/519,451 patent/US9358577B2/en not_active Expired - Fee Related
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US20020000041A1 (en) * | 1994-01-28 | 2002-01-03 | Siamak Doroodian-Shoja | Disposable razor wear indicator |
US20050287353A1 (en) * | 2004-06-24 | 2005-12-29 | Trogolo Jeffrey A | Antimicrobial coating for erosive environments |
US20090130157A1 (en) * | 2005-12-14 | 2009-05-21 | Ylitalo Caroline M | Antimicrobial Adhesive Films |
US20080148512A1 (en) * | 2006-12-13 | 2008-06-26 | Jonas Beskow | Wet/Dry Floor Cleaning Device |
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US20160107191A1 (en) | 2016-04-21 |
US9358577B2 (en) | 2016-06-07 |
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