GB2480347A - Coating surfaces with nanoparticles by dipping - Google Patents
Coating surfaces with nanoparticles by dipping Download PDFInfo
- Publication number
- GB2480347A GB2480347A GB1102589A GB201102589A GB2480347A GB 2480347 A GB2480347 A GB 2480347A GB 1102589 A GB1102589 A GB 1102589A GB 201102589 A GB201102589 A GB 201102589A GB 2480347 A GB2480347 A GB 2480347A
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- nanoparticles
- solution
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 102
- 238000000576 coating method Methods 0.000 title claims description 19
- 239000011248 coating agent Substances 0.000 title claims description 16
- 238000007598 dipping method Methods 0.000 title 1
- 238000000034 method Methods 0.000 claims abstract description 58
- 150000003839 salts Chemical class 0.000 claims abstract description 37
- 239000011521 glass Substances 0.000 claims abstract description 31
- 238000007654 immersion Methods 0.000 claims abstract description 29
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 15
- 239000010703 silicon Substances 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 11
- 229910004613 CdTe Inorganic materials 0.000 claims abstract description 7
- 229910052737 gold Inorganic materials 0.000 claims abstract description 7
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910001218 Gallium arsenide Inorganic materials 0.000 claims abstract description 6
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 5
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 5
- 229920000642 polymer Polymers 0.000 claims abstract description 5
- 229910052709 silver Inorganic materials 0.000 claims abstract description 5
- 239000011258 core-shell material Substances 0.000 claims abstract description 4
- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 claims abstract description 4
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 52
- 239000000203 mixture Substances 0.000 claims description 9
- 239000004065 semiconductor Substances 0.000 claims description 9
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 229910000673 Indium arsenide Inorganic materials 0.000 claims description 3
- SLCWLLVFKQHEIN-UHFFFAOYSA-N trimethyl(11-sulfanylundecyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CCCCCCCCCCCS SLCWLLVFKQHEIN-UHFFFAOYSA-N 0.000 claims description 3
- 150000001734 carboxylic acid salts Chemical group 0.000 claims description 2
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 abstract description 7
- -1 cadmium chalcogenide Chemical class 0.000 abstract description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 abstract 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 abstract 3
- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 abstract 2
- 239000005083 Zinc sulfide Substances 0.000 abstract 2
- 229910052980 cadmium sulfide Inorganic materials 0.000 abstract 2
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 abstract 1
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 abstract 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 abstract 1
- 229910052793 cadmium Inorganic materials 0.000 abstract 1
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical compound [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 abstract 1
- XCAUINMIESBTBL-UHFFFAOYSA-N lead(ii) sulfide Chemical compound [Pb]=S XCAUINMIESBTBL-UHFFFAOYSA-N 0.000 abstract 1
- 239000004332 silver Substances 0.000 abstract 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 abstract 1
- 235000002639 sodium chloride Nutrition 0.000 description 32
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 24
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 13
- 238000002835 absorbance Methods 0.000 description 13
- 230000000694 effects Effects 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000010410 layer Substances 0.000 description 5
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 5
- 235000012431 wafers Nutrition 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000003247 decreasing effect Effects 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000012044 organic layer Substances 0.000 description 3
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 description 3
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 235000017550 sodium carbonate Nutrition 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 230000000875 corresponding effect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000001632 sodium acetate Substances 0.000 description 2
- 235000017281 sodium acetate Nutrition 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 235000010344 sodium nitrate Nutrition 0.000 description 2
- 239000001476 sodium potassium tartrate Substances 0.000 description 2
- 235000011006 sodium potassium tartrate Nutrition 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 241000252506 Characiformes Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910002601 GaN Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000006117 anti-reflective coating Substances 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000021164 cell adhesion Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000007210 heterogeneous catalysis Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000013580 millipore water Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- IZMLNVKXKFSCDB-UHFFFAOYSA-N oxoindium;oxotin Chemical compound [In]=O.[Sn]=O IZMLNVKXKFSCDB-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/44—Palladium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/50—Silver
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/52—Gold
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/66—Silver or gold
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
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- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0234—Nitrogen-, phosphorus-, arsenic- or antimony-containing compounds
- B01J31/0235—Nitrogen containing compounds
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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- B01J35/02—Solids
- B01J35/10—Solids characterised by their surface properties or porosity
- B01J35/1052—Pore diameter
- B01J35/1057—Pore diameter less than 2 nm
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0215—Coating
- B01J37/0219—Coating the coating containing organic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/18—Processes for applying liquids or other fluent materials performed by dipping
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- B05D1/185—Processes for applying liquids or other fluent materials performed by dipping applying monomolecular layers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2203/00—Other substrates
- B05D2203/30—Other inorganic substrates, e.g. ceramics, silicon
Abstract
The material is immersed in a solution containing nanoparticles covered with a charged organic or polymer layer and salt. The solution contains exclusively particles with same-sign charges. The specifically mentioned coated surfaces are glass, indium tin oxide (ITO), silicon and gallium arsenide. The specifically mentioned nanoparticles are gold (Au), silver (Ag), platinum (Pt), palladium (Pd), cadmium chalcogenide (cadmium sulphide CdS, cadmium selenide CdSe, cadmium telluride CdTe), indium phosphide (InP), lead sulphide (PbS), indium arsenide (InAs) and zinc oxide (ZnO), and core shell particles with an outer layer of CdSe, zinc sulphide (ZnS) or zinc selenide (ZnSe). The immersion process may be repeated.
Description
Method of coating material surfaces with nanoparticles The subject matter of the invention is a method for coating the surfaces of materials with nanoparticles. The method is used to coat, i.a., such materials as glass, indium tin dioxide (ITO), silicon and other semiconductors.
Nanoparticles -particles composed of elements and chemical compounds, one dimension of which is conventionally not greater than 100 nm -are characterized by chemical and physical properties that are different from the properties of these substances in a less comminuted form. Due to their high surface energy, nanoparticles must be protected against aggregation by means of a monolayer of organic molecules or polymers. The molecules forming such protective layers may contain in their structures functional groups introduced to assure that nanoparticles coated with such molecules have appropriate physical or biotogical properties, or such properties that allow one to conduct chemical reactions on their surfaces.
In line with the development of methods for production of nanoparticles and the better understanding of their properties one tries to make use of their properties for practical purposes, including such areas as medicine, catalysis, detector design or gaining energy from renewable sources.
To make it possible, in some cases it is necessary to order nanoparticles in two-or three-dimensional structures.
Flat two-dimensional structures composed of or containing metallic (Au, Ag, Pd, Pt, Cu) or semiconductor (CdS, CdSe) nanoparticles attract attention because of their practical importance for solar cells, LSPR-or SERS-based detectors, electronics, corrosion protection, heterogeneous catalysis, anti-reflective coatings, displays and substrates for cell adhesion.
At present, such coatings can be prepared by several known methods including electrodeposition, Langmuir-Blodgett, spin-coating (casting) and sol-gel techniques.
All these methods have one or a number of drawbacks such as they require expensive equipment, they are confined to a limited set of surfaces or they can be used to flat or small size areas Therefore, it is important to search for methods allowing one to coat quickly and cheaply large areas and/or areas with developed morphology.
The subject matter of the present invention is a method for coating the surfaces of materials with nanoparticles. The coating is prepared by immersing the surface being coated in a mixture of nanoparticles covered with a positively charged organic layer, for example trimethyl(11-mercaptoundecyl)-ammonium chloride (TMA), and a salt. Then, the surface is washed in water, optionally in organic solvents, e.g., in methanol, and subsequently dried.
Similar method of surface covering with nanoparticles has been described in a recently published patent application no. US 2OO9j098366 Al and in an article [Smoukov S.K., Bishop K.J.M., Kowatczyk B, Kalsin A.M., Grzybowski B.A.; Journal of the American Chemical Society, 50 (129), 15623- 15630]. This method, however, requires using an appropriately prepared mixture composed of two types of nanoparticles, thosecovered with TMA that gives them positive charge and those covered with li-mercaptoundecanoic acid (MUA) that at high pH gives the nanoparticles a negative charge.
The method according to the invention differs in that it uses solutions of exclusively positively charged nanoparticles.
According to the invention, the method of coating the surface of a material with nanoparticles, comprising of immersing said surface in a solution containing a mixture of nanoparticles covered with charged organic or polymer layer and a salt, is characterised in that said solution contains exclusively particles with same-sign charges.
In one of the embodiments, said surface is charged positively and said solution contains only negatively charged particles.
According to the invention, said solution is an aqueous solution.
In another embodiment of the invention, said solution is a non-aqueous solution, preferably methanolic solution.
According to the invention, said salt is an inorganic salt.
Alternatively, said salt is an organic salt, preferably a carboxylic acid salt.
Preferably, said nanoparticles are from 1 nm to 100 nm in size.
Preferably, the concentration of said salt in said solution ranges from 0.01 mol/l to 2.0 mol/l.
In another embodiment of the invention, said surface is negatively charged, whereas said solution contains exclusively positively charged particles.
According to the invention, said nanoparticles are metallic nanoparticles, preferably selected from the group consisting of Au, Ag, Pt, Pd.
* Alternatively, said nanoparticles are semiconductor nanoparticles, preferably selected from the group consisting of CdS, CdSe, CdTe, lnP, PbS, InAs, ZnO.
In another one preferable embodiment of the invention, said nanoparticles are two-or many-component core-shell nanoparticles, with an upper layer preferably comprising of CdSe, ZnS, ZnSe.
In particular, according to the invention, said nanoparticles can be CdTe/CdSe, CdSe/ZnS or CdSe/ZnSe nanoparticles.
Preferably, said nanoparticles are covered with a positively charged layer of trimethyl(11-mercaptoundecyl)-ammonjum chloride, TMA.
Preferably, the surface to be coated is a surface selected from among glass, ITO, silicon, gallium arsenide or other semiconductors.
Preferably, the duration of a single immersion is from 10 seconds to 60 minutes, preferably from 15 seconds to 10 minutes.
According to the invention, said immersion stage is repeated.
Preferably the number of re-immersions is from 2 to 10.
Below, the invention is presented in a more detail in preferable embodiments, with reference to attached Figures, where: Fig. 1 shows a picture of glass slides immersed singly (1), twice (2), triply (3) and quintuply (4) for a period of one minute in a solution of nanoparticles with concentration of 0.15 mgAu/ml and NaCI 2 mol/l, Fig. 2 illustrates measured absorbances of glass slides immersed in solutions of nanoparticles with concentration of 0.15 mgAu/ml and NaCI concentration of 0, 0.001, 0.01, 0.1, 0.5, 2, 4 or 6 mol/I, as a function of the number of immersions. The duration of each immersion was 1 minute. After each immersion the slides were washed in water, methanol, dried and subsequently their absorbances were measured, Fig. 3 illustrates measured absorbances of glass slides immersed in solutions of nanoparticles with concentration of 0.15 mgAu/ml, as a function of salt concentration. The slides were immersed five times for 1 minute (a) or eight times for 1 minute (b). After each immersion the slides were washed in water, methanol and dried. At salt concentration close to 1 mol/l the nanoparticles precipitate from solution, which makes the measurement impossible, Fig. 4 illustrates measured absorbances of glass slides immersed in solutions of nanoparticles with concentration of 0.15 mgAu/ml and a salt: KSCN (a), Na2CO3 (b), NaCI (c), sodium acetate (d), NaNO3 (e) or sodium-potassium tartrate (f) with concentration of 2 mol/l. The duration of a single immersion was 1 minute. After each immersion the slides were washed in water, methanol and dried, Fig. 5 shows plots of surface coverage as a function of total duration of immersion in a solution of nanoparticles for three different concentrations of nanoparticles: 0.15 (a), 0.075 (b), 0.015 mgAu/ml (c) and NaCI concentration 2 mol/l, Fig. 6 shows a picture of an ITO slide immersed one time for 5 minutes in a solution of nanoparticles with concentration of 0.15 mgAu/mI and NaCI 2 mol/l, Fig. 7 shows a picture of a silicon wafer immersed five times for 5 minutes in a solution of nanoparticles with concentration of 0.15 mgAu/ml and NaCI 2 mol/l, Fig. 8 shows a picture of a silicon wafer immersed five times for 5 minutes in a solution of nanoparticles with concentration of 0.15 mgAu/ml and NaCI 2 mol/l, and subsequently kept in an oxygen plasma for 4 minutes.
The method is designed for coating materials with negatively charged surfaces, in particular glass, ITO, silicon, gallium arsenide and other semiconductors. ITO is a commonly used abbreviation for English term indium tin oxide.
The method according to the invention uses metallic nanoparticles, including Au, Ag, Pt, Pd and/or semiconductor nanoparticles, including CdS, CdSe, CdTe, InP, PbS, InAs, ZnO, two-and many-component core-shell nanoparticles with upper layer composed of, e.g., CdSe, ZnS, ZnSe such as for instance CdTe/CdSe, CdSe/ZnS, CdSe/ZnSe coated with a positively charged organic or polymer layer, or mixtures of nanoparticles of such type.
The method uses nanoparticles from 1 nm to 100 nm in size.
In the method according to the invention, it is preferable to clean by washing the surface being coated in order to reach larger surface coverage. This variant is illustrated with the embodiment 2.
The method according to the invention uses solution of organic and inorganic salts in arbitrary * concentrations, while in order to reach maximal coverage it is preferable to use concentrations ranging from 0.01 to 2 mol/l. It follows from Fig. 2 and 3 that maximal absorbance, corresponding to the maximal coverage, has been reached for a salt concentration 0.1 mol/I after eight one-minute immersions. Under these conditions, further immersions did not lead to an increased surface coverage. Depending on the type of salt and the concentration of nanoparticles, under certain conditions nanoparticles can aggregate and/or precipitate from the mixture. Such a phenomenon occurred in the embodiment 4 for NaCI concentration of approximately 1 mol/l, and therefore the absorbance for that concentration has not been measured, Fig. 3. In such a case is not possible to coat a surface. As follows from the embodiment 4, in such a case salt concentration must be decreased or increased.
The type of salt used in experiment shows an effect on the reached coverage. Among the salts tested, the densest surface coverage was obtained while using salts of carboxylic acids -Fig. 4.
In the method according to the invention, the rate of surface coating with nanoparticles increases in line with nanoparticle concentration, as shown in Fig. 5.
In the method according to the invention, any surface concentrations lower than the maximal one can be reached by decreasing concentrations of nanoparticles, by decreasing salt concentration, and by decreasing the number of immersions of the surface being coated in the solution of nanoparticles.
The change of surface coverage in time, in the course of immersion, is described satisfactorily with the following equation: dP(t)/dt (Dmax -cD)Kc, where t(t) is the surface coverage, Pmax is the maximal surface coverage, K -proportionality factor, c -concentration of nanoparticles. In the above equation the adsorption of nanoparticles on the substrate surface is irreversible. The irreversibility of adsorption is concluded from the observation that the slide coverage -as measured by the slide's absorbance -does not change after the slide has been washed.
After completion of coating the surface, the organic layer on the surface of nanoparticles can be removed with chemical methods or with oxygen plasma, which can lead to local aggregation of nanoparticles -embodiment 8.
Prepared coatings are mechanically stable enough to be transported, stored, covered with liquids and heated above room temperature. The method according to the invention yields always a coating with a single layer of nanoparticles. No formation of two and multilayer structures on coated materials has been found.
In addition, according to the conclusion published by the authors [Tretiakov K.V., Bishop K.J.M., Kowalczyk B., iaiswal A., Poggi M.A., Grzybowski B.A.; Journal of Physical Chemistry A, 16 (113), 3799- 3803] cooperative contributions of positively and negatively charged particles lead to an inhomogeneous coating on a nano level -formation on the surface of structures containing a few nanoparticles each, as the negatively and positively charged particles attract to each other electrostatically. Lack of such a cooperative effect in the method described here allows for obtaining surfaces coated with single nanoparticles.
Materials and equipment Glass slides were purchased at Roth, silicon wafers were obtained from the Institute of Electronic Materials Technology in Warsaw. The surfaces were cut manually to designed dimensions, on the spot. In tests 10.5 mm wide glass strips were used, which allowed to place them vertically in a spectrophotometer cell. The chemicals were purchased at Sigma-Aldrich, the solvents at Chempur. In all the experiments 15 MO Millipore water was used. The UV-Vis spectra were recorded with Shimadzu spectrophotometer. The deposition was performed in 15 ml polypropylene test tubes (Sarstedt). The pictures of nanoparticles-coated semiconductor surfaces were taken with a Zeiss scanning electron microscope (SEM) at the Institute of Physics of the Polish Academy of Sciences and the Institute of High Pressure Physics of the Polish Academy of Sciences.
Experimental Silicon, gallium arsenide, gallium nitride and ITO were washed with 20 % nitric acid, water, acetone and methanol directly before use. The glass was washed with piranha solution (a mixture of concentrated sulphuric acid and 30% hydrogen peroxide in proportion 3:1), acetone and methanol.
The solution of gold nanoparticles with radii 3.06 ± 0.55 nm was obtained according to a literature procedure [Jana N.R., Peng G.X., Journal of the American Chemical Society, 47 (125), 14280- 14281]. The nanoparticles contained in 10 g of the solution were coated with N,N,N-trimethyl(11-mercaptoundecyl)-ammonium chloride (TMA) [Kalsin A.M., Fialkowski M., Paszewski M., Smoukov * S.K., Bishop K.J.M., Grzybowski B.A., Science, 5772 (312), 420-424J, that positively charged nanoparticles and subsequently dissolved in 50 ml water yielding a 0.6 mg/g gold solution, in the following referred to as the stock solution.
The mixtures of nanoparticles and salts with appropriate component concentrations were prepared from stock solutions of nanoparticles, salts or their concentrated standard solutions with water, whereas the solution of nanoparticles was always added as the last one.
A slide of material to be coated was immersed in a vertical position for a specific time period in 4 ml of a mixture of nanoparticles and salt in a 15 ml test tube. Then, the slide was washed in a beaker containing 300 ml water and dried by placing it in a vertical position on a filter paper so that the surface under study contacted the substrate with the bottom edge only. Additional washing in organic solvent such as methanol, acetone or tetrahydrofuran speeds up drying with no effect on the coating density. The drying method has an effect on the pattern that is sometimes formed by nanoparticles on the surface, this, however, has not been studied systematically. Coated surfaces were studied with a spectrophotometric method (glass) or with a scanning electron microscope SEM (ITO, gallium arsenide and silicon).
The effect the environment conditions have on the material coverage has been studied on glass, assuming that the surface concentration of nanoparticles is proportional to the measured absorbance of glass slides. In addition, it has been assumed that the observed bathochromic shift of absorption maximum (from 525 nm to 550 nm) has no effect on the extinction coefficient value.
Embodiments of the invention Embodiment 1. Visual presentation of the invention.
Using the method according to the invention, glass slides were immersed in a solution of nanoparticles with concentration of 0.15 mgAu/ml and NaCI 2 mol/l. Fig. 1 presents a picture of the surfaces of these glass slides immersed singly (1), twice (2), triply (3) and quintuply (4) for a time period of one minute. It can be seen from the picture that the intensity of the red tint coming from nanoparticles increases in line with growing coverage of the glass surface that increases with the number of immersions.
Embodiment 2. Effect of surface cleaning on the surface coverage.
Using the method according to the invention, four glass slides were immersed in four solutions of nanoparticles with concentration of 015 mgAu/ml and NaCI 2 mol/l. The first glass slide was immersed four times for a time period of 60 minutes, and the other glass slides for time periods 15, 5 and 1 minute, respectively. The absorbances of covered glass slides were 0.12, 0.26, 0.2 and 0.19, respectively. The embodiment shows that in order to reach high surface coverage the surfaces should be immersed preferably for an appropriate period of time, from 1 to 15 minutes, but also cleaned by washing between subsequent re-immersions. When no washing is applied, even the longer duration of the immersion does not lead to a possibly maximal coverage.
Embodiment 3. Salt concentration effect on the surface coverage.
Using the method according to the invention the glass slides were immersed in solutions of nanoparticles with concentration of 0.15 mgAu/ml and various NaCI concentrations. The duration of a single immersion was 1 minute. Fig. 2 shows variations in absorbance of glass slides in line with increasing number of immersions in solutions with salt concentration varying from zero to 6 mol/l. The data indicates that there is an optimal salt concentration of about 0.1 mol/l, at which a high surface coverage is reached in the shortest time. At lower or higher salt concentrations, the process occurs slower or does not occur at all, which is shown in the next embodiment.
Embodiment 4. Salt concentration effect on the surface coverage.
Using the method according to the invention the glass slides were immersed in solutions of nanoparticles with concentration of 0.15 mgAu/ml and various NaCI concentrations. The duration of a single immersion was 1 minute. Fig. 3 shows variations in absorbance of glass slides immersed 5 times (a) or 8 times (b) as a function of NaCI concentration in solution. The data indicates that the salt concentration has a key effect on the coating process. It proceeds with the highest rate at the concentration of about 0.1 mol/l. Under these conditions, with NaCl concentration close to 1 mol/l, nanoparticles aggregate or precipitate from solution, which prevents covering of the surface.
Embodiment 5. Salt type effect on the surface coverage.
Using the method according to the invention the glass slides were immersed in solutions of nanoparticles with concentration of 0.15 mgAu/ml and that of tested salts 2 mol/l. The duration of a single immersion was 1 minute. Fig. 4 shows variations in absorbance of glass slides in line with increasing number of immersions in solutions containing nanoparticles in concentration of 0.15 mgAu/ml and salts: KSCN, Na2CO3, NaCl, sodium acetate, NaNO3, KNaC4H4O6 (sodium-potassium tartrate) in concentration of 2 mol/l. The data indicates that the type of salt can have an effect on the surface coverage. The use of KSCN or Na2CO3 is unfavourable.
Embodiment 6. Effect of nanoparticles concentration on the surface coverage.
Using the method according to the invention the glass slides were immersed in solutions with concentrations of 0.15 (a), 0.075 (b) and 0.015 mgAu/ml (c), and NaCI of 2 mol/l. The results are shown in Fig. 5. The embodiment shows that the rate of surface coverage, a, is proportional to the concentration of nanoparticles in solution. The experiment has been performed so that an appropriate number of solution samples were prepared for each concentration of nanoparticles. A glass slide was immersed for a time period from 1 to 5 minutes, washed, dried, then absorbance was measured, and subsequently the glass slide was immersed in a new sample of corresponding solution. The measurements were repeated triply for each concentration of nanoparticles. The plot presents averaged data. The experimental data are fitted with a function D(t) = Dmax -exp[-at], where P(t) is the surface coverage after time t, Dmax -the maximal surface coverage, a -is a constant indicating the adsorption rate of nanoparticles on the surface. The horizontal axis represents the total time over which the samples were kept in solutions. It turned out that the constant a is proportional to the concentration of nanoparticles in solution, a = Kc, where K is a constant, and c denotes the concentration of nanoparticles.
Embodiment 7. Coating ITO.
Using the method according to the invention an ITO slide was immersed for 5 minutes in a solution of nanoparticles with concentration of 0.15 mgAufml and NaCI 2 mol/l. Fig. 6 shows a picture of so prepared surface obtained with a scanning electron microscope. The embodiment shows that ITO can be covered with nanoparticles using the method according to the invention. Lower coverage density as compared with the embodiment 8 is primarily related to a smaller number of immersions.
Embodiment 8. Coating silicon.
Using the method according to the invention a silicon wafer was immersed five times in a solution of nanoparticles with concentration of 0.15 mgAu/ml and NaCI 2 mol/l. The duration of a single immersion was 5 minutes. Fig. 7 shows a picture of so prepared surface obtained with a scanning electron microscope. The embodiment shows that silicon can be covered with nanoparticles using the method according to the invention.
Embodiment 9. Coating silicon. Oxygen plasma effect on coated surfaces.
Using the method according to the invention a silicon wafer was immersed five times in a solution of nanoparticles with concentration of 0.15 mgAu/ml and NaCI 2 mol/l. The duration of a single immersion was 5 minutes. After the surfaces have been coated with nanoparticles, they were cleaned in oxygen plasma for 4 minutes and subsequently washed in water and in methanol. Fig. 8 shows a scanning electron microscope picture of the surface obtained in such a procedure. Better contrast of the picture as compared with the embodiment 8 indicates that the non-conductive organic layer has been removed from the nanoparticles which resulted in a partial local aggregation of nanoparticles.
Claims (20)
- Patent claims 1. A method for coating the surfaces of materials with nanoparticles, comprising of immersing the said surface in a solution containing a mixture of nanoparticles covered with a charged organic or polymer layer and salt, characterised in that the said solution contains exclusively particles with same-sign charges.
- 2. The method of claim 1, characterised in that the said surface is positively charged, whereas the said solution contains exclusively negatively charged particles.
- 3. The method of claim 1 or 2, characterised in that the said solution is an aqueous solution.
- 4. The method of claim 1 or 2, characterised in that the said solution is a non-aqueous solution.
- 5. The method of claim 4, characterised in that the said solution is a methanolic solution.
- 6. The method of any of the foregoing claims, characterised in that the said salt is an inorganic salt.
- 7. The method of any of the claims 1-5, characterised in that the said salt is an organic salt.
- 8. The method of claim 7, characterised in that the said salt is a carboxylic acid salt.
- 9. The method of any of the foregoing claims, characterised in that the said nanoparticles are from 1 nm to 100 nm in size.
- 10. The method of any of the foregoing claims, characterised in that the concentration of the said salt in the said solution ranges from 0.Olmol/l to 2.0 mol/l.
- 11. The method of any of the claims 1 or 3-9, characterised in that the said surface is negatively charged, whereas the said solution contains exclusively positively charged particles.
- 12. The method of claim 11, characterised in that the said nanoparticles are metallic nanoparticles, preferably selected from the group consisting of Au, Ag, Pt, Pd.
- 13. The method of claim 11, characterised in that the said nanoparticles are semiconductor nanoparticles, preferably selected from the group consisting of CdS, CdSe, CdTe, lnP, PbS, InAs, ZnO.
- 14. The method of claim 11, characterised in that the said nanoparticles are two-or many-component core-shell nanoparticles, with an upper layer preferably comprising of CdSe, ZnS, ZnSe.
- 15. The method of claim 14, characterised in that the said nanoparticles are CdTe/CdSe, CdSe/ZnS or CdSe/ZnSe nanoparticles.
- 16. The method of any of the claims 11-17, characterised in that the said nanoparticles are covered with a positively charged trimethyl(11-mercaptoundecyl)-ammonium chloride (TMA) layer.
- 17. The method of any of the claims 11-16, characterised in that the surface to be coated is a surface selected from among glass, indium tin oxide (ITO), silicon, gallium arsenide or other semiconductors.
- 18. The method of any of the foregoing claims, characterised in that the duration of a single immersion ranges from 10 seconds to 60 minutes, preferably from 15 seconds to 10 minutes.
- 19. The method of any of the foregoing claims, characterised in that the said immersion stage is repeated.
- 20. The method of claim 19, characterised in that the number of re-immersions ranges from 2 to 10.
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| WO2000013806A1 (en) * | 1998-09-04 | 2000-03-16 | Seimei Shiratori | Method and apparatus for forming film by alternate deposition, and film-coated structure |
| WO2001072878A1 (en) * | 2000-03-28 | 2001-10-04 | The Board Of Regents For Oklahoma State University | Assembly of free-standing films using a layer-by-layer process |
| WO2005063307A1 (en) * | 2003-12-23 | 2005-07-14 | Kimberly-Clark Worldwide, Inc. | Bacteria binding products |
| US20050255236A1 (en) * | 2004-05-12 | 2005-11-17 | Tao Deng | Method for forming nanoparticle films and applications thereof |
| WO2008152295A2 (en) * | 2007-05-28 | 2008-12-18 | Commissariat A L'energie Atomique | Thin films of conjugated polymers containing inorganic nanoparticles and process for the manufacture thereof |
| JP2010284603A (en) * | 2009-06-12 | 2010-12-24 | Kyushu Univ | Multilayer film substrate having multilayer formed from metal fine particles and method of manufacturing the same |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000013806A1 (en) * | 1998-09-04 | 2000-03-16 | Seimei Shiratori | Method and apparatus for forming film by alternate deposition, and film-coated structure |
| WO2001072878A1 (en) * | 2000-03-28 | 2001-10-04 | The Board Of Regents For Oklahoma State University | Assembly of free-standing films using a layer-by-layer process |
| WO2005063307A1 (en) * | 2003-12-23 | 2005-07-14 | Kimberly-Clark Worldwide, Inc. | Bacteria binding products |
| US20050255236A1 (en) * | 2004-05-12 | 2005-11-17 | Tao Deng | Method for forming nanoparticle films and applications thereof |
| WO2008152295A2 (en) * | 2007-05-28 | 2008-12-18 | Commissariat A L'energie Atomique | Thin films of conjugated polymers containing inorganic nanoparticles and process for the manufacture thereof |
| JP2010284603A (en) * | 2009-06-12 | 2010-12-24 | Kyushu Univ | Multilayer film substrate having multilayer formed from metal fine particles and method of manufacturing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023158682A1 (en) * | 2022-02-16 | 2023-08-24 | Botanisol Analytics, Inc. | Painted substrate for spectroscopy |
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