Source: https://patents.google.com/patent/US10024840B2/en
Timestamp: 2018-10-20 20:36:22
Document Index: 467958645

Matched Legal Cases: ['Application No. 60', 'Application No. 61', 'Application No. 2011', 'Application No. 2010', 'Application No. 2010', 'application No. 10', 'Application No. 2011', 'Application No. 08756437']

US10024840B2 - Surfaces having particles and related methods - Google Patents
US10024840B2
US10024840B2 US14057993 US201314057993A US10024840B2 US 10024840 B2 US10024840 B2 US 10024840B2 US 14057993 US14057993 US 14057993 US 201314057993 A US201314057993 A US 201314057993A US 10024840 B2 US10024840 B2 US 10024840B2
US14057993
US20140041905A1 (en )
This application is a divisional of U.S. application Ser. No. 12/601,869, which is a National Stage Entry of PCT/US2008/065083, filed May 29, 2008, which claims the benefit of U.S. Provisional Application No. 60/932,025, filed May 29, 2007, and of U.S. Provisional Application No. 61/126,589 filed May 6, 2008, the entireties of which are incorporated by reference herein.
FIG. 15 illustrates (A) an untreated control sample (top, labeled with a “C”) and a sample treated with 2 wt % Ag, 2.25 wt % PVC in THF (bottom) as viewed from underside of agar 24 hours following inoculation with E. coli, and (B) an expanded view of the treated sample from (A), with arrows pointing to zone of inhibition maxima (˜0.88 mm);
FIG. 17 illustrates percentage bacteria coverage of LB agar plates versus time for E. coli-inoculated LB broth in contact with a 4.0 wt % Ag and 2.0 wt % PVC sample and then spread plated;
A variety of ionic solutions are used in the claimed invention. These solutions include choline chloride, urea, malonic acid, phenol, glycerol, 1-alkyl-3-methylimidazolium, 1-alkylpyridinium, N-methyl-N-alkylpyrrolidinium, 1-Butyl-3-methylimidazolium hexafluorophosphate, ammonium, choline, imidazolium, phosphonium, pyrazolium, pyridinium, pyrrolidinium, sulfonium, 1-ethyl-1-methylpiperidinium methyl carbonate, and 4-ethyl-4-methylmorpholinium methyl carbonate.
Other methylimidazolium solutions are considered suitable, including 1-Ethyl-3-methylimidazolium acetate, 1-butyl-3-methylimidazolium tetrafluoroborate, 1-n-butyl-3-methylimidazolium tetrafluoroborate, 1-butyl-3-methylimidazolium hexafluorophosphate, 1-n-butyl-3-methylimidazolium hexafluorophosphate, 1-butyl-3-methylimidazolium 1,1,1-trifluoro-N-[(trifluoromethyl)sulfonyl]methanesulfonamide, 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide, 1-butyl-3-methylimidazolium bis[(trifluoromethyesulfonyl)]amide, and 1-butyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide.
Imides and amides are also properly included in the claimed invention. A non-exclusive listing of these compounds includes ethylheptyl-di-(1-methylethyl)ammonium bis[(trifluoromethyl)sulfonyl]imide, N,N,N-tributyl-1-octanaminium trifluoromethanesulfonate; tributyloctylammonium triflate, tributyloctylammonium trifluoromethanesulfonate, N,N,N-tributyl-1-hexanaminium bis[(trifluoromethyl)sulfonyl]imide, tributylhexylammonium 1,1,1-trifluoro-N-[(trifluoromethyl)sulfonyl]methanesulfonamide, tributylhexylammonium bis(trifluoromethylsulfonyl)imide, tributylhexylammonium bis[(trifluoromethyl)sulfonyl]amide, tributylhexylammonium bis[(trifluoromethyl)sulfonyl]imide, N,N,N-tributyl-1-heptanaminium bis[(trifluoromethyl)sulfonyl]imide, tributylheptylammonium 1,1,1-trifluoro-N-[(trifluoromethyl)sulfonyl]methane sulfonamide, tributylheptylammonium bis(trifluoromethylsulfonyl)imide; tributylheptylammonium bis[(trifluoromethyl)sulfonyl]amide, tributylheptylammonium bis[(trifluoromethyl)sulfonyl]imide, N,N,N-tributyl-1-octanaminium bis[(trifluoromethyl)sulfonyl]imide, tributyloctylammonium 1,1,1-trifluoro-N-[(trifluoromethyl)sulfonyl]methanesulfonamide, tributyloctylammonium bis(trifluoromethylsulfonyl)imide, tributyloctylammonium bis[(trifluoromethyl)sulfonyl]amide, tributyloctylammonium bis[(trifluoromethyl)sulfonyl]imide, 1-butyl-3-methylimidazolium trifluoroacetate, 1-methyl-1-propylpyrrolidinium 1,1,1-trifluoro-N-[(trifluoromethyl)sulfonyl]methanesulfonamide, 1-methyl-1-propylpyrrolidinium bis(trifluoromethylsulfonyl)imide, 1-methyl-1-propylpyrrolidinium bis[(trifluoromethyl)sulfonyl]amide, 1-methyl-1-propylpyrrolidinium bis[(trifluoromethyl)sulfonyl]imide, 1-butyl-1-methylpyrrolidinium 1,1,1-trifluoro-N-[(trifluoromethyl)sulfonyl]methanesulfonamide, 1-butyl-1-methylpyrrolidinium bis(trifluoromethylsulfonyl)imide, 1-butyl-1-methylpyrrolidinium bis[(trifluoromethyl)sulfonyl]amide, 1-butyl-1-methylpyrrolidinium bis[(trifluoromethyl)sulfonyl]imide, 1-butylpyridinium 1,1,1-trifluoro-N-[(trifluoromethyl)sulfonyl]methanesulfonamide, 1-butylpyridinium bis(trifluoromethylsulfonyl)imide, 1-butylpyridinium bis[(trifluoromethyl)sulfonyl]amide, 1-butylpyridinium bis[(trifluoromethyl)sulfonyl]imide, 1-butyl-3-methylimidazolium bis(perfluoroethylsulfonyl)imide, butyltrimethylammonium bis(trifluoromethylsulfonyl)imide, 1-octyl-3-methylimidazolium 1,1,1-trifluoro-N-[(trifluoromethyl)sulfonyl]methanesulfonamide, 1-octyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide, 1-octyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]amide, 1-octyl-3-methylimidazolium bis[(thfluoromethyl)sulfonyl]imide, 1-ethyl-3-methylimidazolium tetrafluoroborate, N,N,N-trimethyl-1-hexanaminium bis[(trifluoromethyl)sulfonyl]imide; hexyltrimethylammonium 1,1,1-trifluoro-N-[(trifluoromethyl)sulfonyl]methanesulfonamide, hexyltrimethylammonium bis(trifluoromethylsulfonyl)imide, hexyltrimethylammonium bis[(trifluoromethyl)sulfonyl]amide, hexyltrimethylammonium bis[(trifluoromethyl)sulfonyl]imide, N,N,N-trimethyl-1-heptanaminium bis[(trifluoromethyl)sulfonyl]imide, heptyltrimethylammonium 1,1,1-trifluoro-N-[(trifluoromethyl)sulfonyl]methanesulfonamide, heptyltrimethylammonium bis(trifluoromethylsulfonyl)imide, heptyltrimethylammonium bis[(trifluoromethyl)sulfonyl]amide, heptyltrimethylammonium bis[(trifluoromethyl)sulfonyl]imide, N,N,N-trimethyl-1-octanaminium bis[(trifluoromethyl)sulfonyl]imide, trimethyloctylammonium 1,1,1-trifluoro-N-[(trifluoromethyl)sulfonyl]methanesulfonamide, trimethyloctylammonium bis(trifluoromethylsulfonyl)imide, trimethyloctylammonium bis[(trifluoromethyl)sulfonyl]amide, trimethyloctylammonium bis[(trifluoromethyl)sulfonyl]imide, 1-ethyl-3-methylimidazolium ethyl sulfate, and the like.
Particles suitable for the present methods are described in additional detail elsewhere herein, and suitably include one or more functional agents. Functional agents include antimicrobial agents, biocidal agents, insulators, conductors, semiconductors, catalysts, fluorescent agents, flavor agents, catalysts, ligands, receptors, antibodies, nucleic acids, antigens, labels or tags—which may be radioactive or magnetic, lubricants, fragrances, and the like. As an example, a particle may include silver or silver ions, which are known to have antimicrobial properties. Other functionalized particles are described elsewhere herein in additional detail.
Specifically suitable polymers include polyethylene, polypropylene, polyarylate, polyester, polysulphone, polyamide, polyurethane, polyvinvyl, fluoropolymer, polycarbonate, polylactic acid, nitrile, acrylonitrile butadiene styrene, phenoxy, phenylene ether/oxide, a plastisol, an organosol, a plastarch material, a polyacetal, aromatic polyamide, polyamide-imide, polyarylether, polyetherimide, polyarylsulfone, polybutylene, polycarbonate, polyketone, polymethylpentene, polyphenylene, polystyrene, styrene maleic anhydride, polyllyl diglycol carbonate monomer, bismaleimide, polyallyl phthalate, epoxy, melamine, silicone, urea, and the like. Other suitable polymers will be known to those of ordinary skill in the art; cellulosic polymers and other cellulose-based materials are also considered suitable.
As another non-limiting example, a polymeric particle may include multiple ligands bound to its surface so as to enable specific binding between that particle and a particular target. As another non-limiting example, a silver particle—having biocidal properties—might also include a fragrant agent so as to impart a pleasing smell to a composite material that has biocidal properties.
Separate particles may be separated by distances of from about 0.1 nm to about 1 mm. Particles may be separated by uniform or non-uniform distances depending on the needs of the user and the method in which the composite material was formed. In some embodiments, two or more particles are in contact with one another.
Structures may be chosen, constructed, or placed singly or multiply so as to maximize fluid-particle contact. As one example, a series of filter-type structures—having the same or different active particles—may be arrayed so as to provide a multi-stage fluid treatment system.
The high-contrast agents can be particles as described above but will typically contain elements that have high atomic numbers. Some examples of these particles are: gold particles and nanoparticles, silver particles, copper particles, platinum particles, titanium particles, iodine containing particles or compounds, barium-containing particles or compounds, diatrizoate, metizoate, ioxaglatc, iopamidol, iohexyl, ioxilan, iopromide, iodixanol, and the like. Gadolinium-containing particles or compounds can also be used as a component of MRI contrast.
Following introduction of a solution, e.g., blood, enzyme digested blood, other biofluid, to a plastic surface enhanced in this way, the target DNA, proteins, etc will bind to the nanoparticles. The presence of the target molecules can be detected via a change in voltage, light intensity, mass, or other discernible change, which change may be amplified or otherwise enhanced through the binding of additional particles or markers, e.g. fluorescing molecules, at the location of the binding. Such a device may effect a visible change upon the binding of target compounds, making a separate reader unnecessary for the result of the test. Because the target molecules are bound to the particles embedded in a surface, the bound molecule will likely resist being displaced by moderate rinsing. If stronger methods—such as vigorous rinsing, heating, or the introduction of bond-cleaving agents—are used, the target molecules may be displaced, thus permitting re-use of the biosensor.
Polymer surfaces that interface with water, such as bottles, vessels, tanks, pipes, hydration bladders, valves and tubes of hydration packs, filters, valves, and spouts, may be treated by the process described with antimicrobial particles that will protect the surfaces, and also treat the water and deactivate microbial contaminants. Examples of such particles include ion-exchanged zeolites, silver-loaded insoluble phosphates, silver-loaded calcium phosphate, silver-ion-modified glass, silver-ion-exchanged potassium titanate fiber, silver-loaded inorganic colloid, silver nano or micro particles, and the same using copper, zinc, or other metallic ions, metallic nanoparticles, ion-loaded glass, ion-exchanged zirconium phosphate-based ceramics and other ceramics, zinc pyrithione particles, copper pyrithione particles, and the like.
Common objects may also be embedded with antimicrobial-acting particles. A non-exclusive listing of such objects includes keyboards; computer mouse; clear film with pressure sensitive adhesive backing; food containers; water containers and bottles; eating and cooking utensils; shower curtains; water and beverage dispensers; shopping cart handles and shopping carts; hydration packs, bladders, valves, tubing, and bags; water pipes; sewage pipes, gas pipes, footwear, cell phones; video game controllers and buttons; laptop and ultraportable computers, mouse pads and pointing pads; vehicle steering wheels; vehicle plastic surfaces, vehicle buttons, vehicle vents, train and subway supports and handrails; airplane and train tray tables, armrests, windowshades, cutting boards; trash cans; dish drying rack and pan; fish tank tubing; fish tank filters, lobster traps; fish nets and tanks; boat hulls; refrigerator sealing gaskets; refrigerator surfaces; biometric readers such as finger and palm print readers; boat and other water-based propellers; humidifier and dehumidifier tanks and surfaces; shower mat; gym and yoga mat; gym equipment; catheters; intubation tubes; implantable devices and materials; newborn baby holders used at hospitals; premature infant holders; bathroom and shower soap and shampoo dispensers; plastic handles and knobs for doors, cabinets, sinks, showers and similar; ATM keypads; ATM screens and screen protectors; credit cards and other plastic cards; salt, pepper, and similar shakers; athletic helmet straps and interior helmet padding; litter boxes; pet bowls for food and water; pet carriers; subway, train, car, restaurant, or other scats having polymer coverings; table surfaces and counter top surfaces and refinishings; placemats; colanders; tanks; medical tool trays; plastic medical tools, orthodontic devices, table tops, faceplates for consumer electronics; remote controls; tiles, shower surfaces; toilet surfaces; trash bins and lids and handles. Other applications will be apparent to those of ordinary skill in the art.
The process as described above is also applicable to creating catalytic surfaces. The process described above can be with traditional heterogeneous catalysts like vanadium oxide, nickel, alumina, platinum, rhodium, palladium, mesoporous silicates, etc. Similarly, some homogeneous catalysts can be used like: enzymes, abzymes, ribozymes, deoxyribozymes, and the like. Electro-catalysts are also suitable, including, for example, platinum nanoparticles. Organocatalysts are also substances that can suitably be embedded into a surface.
Flat industrial-grade PVC samples and freshly extruded PVC samples (fabricated using the fiber extruder, were placed between two steel plates that were heated to temperatures ranging from 150-185° C. and pressed at pressures ranging from 1,000-15,000 lbs. The PVC samples were removed at time periods ranging from 30 seconds to 30 minutes, and were examined. Silver microparticles (Powder, 2.0-3.5 μm, 99+%. Sigma-Aldrich, www.sigma-aldrich.com, Cat. No. 327085) were then aerosolized onto the resulting hot and softened PVC surfaces.
Antibacterial activity over time was assessed via growth analysis testing. The same initial procedure was used as for turbidity testing, as described elsewhere herein, but rather than perform visual observations, 200 μl of solution was removed from each test tube and plated on LB plates (1.0% Tryptone, 0.5% yeast extract, 1.0% NaCl, 1.5% agar (Teknova www.teknova.com, Cat. No. L1100) at hours 1, 2, 3, 4, 5, 6, 8, and 10. The plates were immediately refrigerated at 4° C. until 1 hour after all plates were collected. The plates were then incubated together in a lab oven at 37° C. and observed at hour 8. All samples were compared and a relative density scale was used, with 1 indicating lowest bacteria growth and 10 indicating highest bacteria growth. ImageJ was used to quantify the bacteria density for plates where a full lawn had not developed—all 4 wt % Ag 2.25 wt % plates—and that were not destroyed due to application of bad dye (hour 3, 4, 5, 6, and 8). The dye was intended to make the test results easier to analyze.
Silver particles in silver-THF solutions prepared without the addition of PVC visibly settled out faster than the silver particles in PVC-stabilized solutions, prepared with identical silver concentrations. Silver nanoparticles also agglomerated to a greater extent in silver-THF solutions not stabilized with PVC. This greater agglomeration was evident in the fact that average size of the silver particles on PVC substrates treated with unstabilized silver-THF solutions was larger (radius ˜6.3 μm for solution with 1.5 wt % silver and 0 wt % PVC) than the size of particles on substrates treated with stabilized solutions (radius ˜466.6 nm for solution with 1.5 wt % silver and 2.25 wt % PVC) (FIG. 9). As shown in FIG. 9, the average size of the silver particles on the PVC substrates also decreased with increasing PVC concentration, thus indicating that PVC retarded agglomeration and allowed for smaller particle size. However, such a trend was not always achieved for increasing PVC concentrations owing to various sources of error and possibly complex relations between the concentration of silver and PVC added to the silver-THF solutions.
Microorganisms recovered in 4 wt % Microorganisms recovered in
Ag, 2.25 wt % PVC sample after 24 Control sample after
hours (cfu/ml) 24 hours (cfu/ml)
Industrial-grade flat PVC sheets were embedded with silver particles and the antibacterial properties of the resulting surface were confirmed. Silver nanopowder was suspended in THF and PVC solution and spin-coated onto flat PVC substrates at concentrations of 0.45 wt % to 4.0 wt %. PVC powder was used as a stabilizer at concentrations from 0.0 wt % to 3.0 wt %. Raman spectroscopy confirmed the identity of the embedded particles as the organically coated silver nanoparticles. Optical microscopy and ImageJ software were used to measure area fraction of embedded surface coverage and average particle size for all samples. Embedded surface area fractions ranged from 0.1%-20% and particle-agglomerate radii from 73 ran to 400 nm. Desired area fraction of embedded surface coverage and particle size dispersion were controlled by varying the concentration of silver and PVC powder in the solution. Dissolving PVC powder in the silver solution helped stabilize the suspension, retarding agglomeration.
a substrate having at least one surface in which a population of metallic nanowires is at least partially embedded,
the population of metallic nanowires forming a conductive pathway by touching or proximity of the metallic nanowires to one another, wherein the population of metallic nanowires provides a coverage of 1% to 5% of the surface of the substrate, and
wherein the substrate is a single-layer substrate, and wherein the substrate is capable of reaction with the population of metallic nanowires, and wherein the substrate degrades the population of metallic nanowires.
2. The composite material of claim 1, wherein the substrate comprises a polymer.
3. The composite material of claim 2, wherein the polymer is characterized as conductive.
4. The composite material of claim 1, wherein the population of metallic nanowires comprises silver.
5. The composite material of claim 1, wherein the substrate is harder than the population of metallic nanowires.
6. The composite material of claim 2, wherein at least one of the population of metallic nanowires is fully embedded below the surface of the substrate.
7. The composite material of claim 6, wherein at least another one of the population of metallic nanowires includes a first portion embedded below the surface of the substrate and a second portion exposed above the surface of the substrate.
8. The composite material of claim 2, wherein the population of metallic nanowires comprises metallic nanowires that are fused together.
9. The composite material of claim 2, wherein the population of metallic nanowires is localized in a surface portion of the substrate, such that a remaining portion of the substrate is devoid of any metallic nanowire.
10. The composite material of claim 2, wherein the substrate is a polymeric sheet.
11. A display device comprising the composite material of claim 2.
a substrate having at least one surface in which nanowires are at least partially embedded,
the embedded nanowires are localized in a surface portion of the substrate, such that a remaining portion of the substrate is devoid of any nanowire, wherein the embedded nanowires provides a coverage of 1% to 5% of the surface of the substrate,
the substrate, with the embedded nanowires, has a lower resistivity relative to the substrate in the absence of the embedded nanowires, and
wherein the substrate is a single-layer substrate, and wherein the substrate is capable of reaction with the embedded nanowires, and wherein the substrate degrades the embedded nanowires.
13. The composite material of claim 12, wherein the embedded nanowires comprise silver.
14. The composite material of claim 12, wherein at least one of the embedded nanowires is fully embedded below the surface of the substrate.
15. The composite material of claim 12, wherein at least one of the embedded nanowires includes a first portion embedded below the surface of the substrate and a second portion exposed above the surface of the substrate.
16. The composite material of claim 12, wherein the embedded nanowires comprise nanowires that are fused together.
17. The composite material of claim 12, wherein the embedded nanowires form a conductive pathway by touching or proximity of the embedded nanowires to one another.
18. The composite material of claim 12, wherein the substrate is an extruded polymeric substrate.
19. The composite material of claim 12, wherein the substrate is a polymeric sheet.
20. A sensor device comprising the composite material of claim 12.
a substrate having at least one surface in which a population of metallic particles is at least partially embedded,
the population of metallic particles forming a conductive pathway by touching or proximity of the metallic particles to one another, wherein the population of metallic particles provides a coverage of 1% to 5% of the surface of the substrate, and
wherein the substrate is a single-layer substrate, and wherein the substrate is capable of reaction with the population of metallic particles, wherein the substrate degrades the population of metallic particles.
22. The composite material of claim 21, wherein the population of metallic particles comprises nanowires, nanorods, or a combination thereof.
23. The composite material of claim 21, wherein the population of metallic particles comprises metallic particles of disproportionate aspect ratio.
24. The composite material of claim 21, wherein the population of metallic particles comprises silver-containing particles.
25. The composite material of claim 21, wherein at least one of the population of metallic particles is fully embedded below the surface of the substrate.
26. The composite material of claim 21, wherein at least one of the population of metallic particles is partially exposed above the surface of the substrate.
27. The composite material of claim 21, wherein the population of metallic particles comprises metallic particles that are fused together.
28. The composite material of claim 21, wherein the substrate is a polymeric sheet.
29. A display device comprising the composite material of claim 21.
30. The composite material of claim 2, wherein the substrate is porous.
31. The composite material of claim 12, wherein the substrate is porous.
32. The composite material of claim 21, wherein the substrate is porous.
US14057993 2007-05-29 2013-10-18 Surfaces having particles and related methods Active 2030-08-02 US10024840B2 (en)
US60186910 true 2010-05-28 2010-05-28
US14057993 US10024840B2 (en) 2007-05-29 2013-10-18 Surfaces having particles and related methods
PCT/US2008/065083 Division WO2008150867A3 (en) 2007-05-29 2008-05-29 Surfaces having particles and related methods
US12601869 Division US8852689B2 (en) 2007-05-29 2008-05-29 Surfaces having particles and related methods
US60186910 Division 2010-05-28 2010-05-28
US20140041905A1 true US20140041905A1 (en) 2014-02-13
US10024840B2 true US10024840B2 (en) 2018-07-17
US14057993 Active 2030-08-02 US10024840B2 (en) 2007-05-29 2013-10-18 Surfaces having particles and related methods
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