US20040139888A1 - Printing inks and reagents for nanoelectronics and consumer products - Google Patents
Printing inks and reagents for nanoelectronics and consumer products Download PDFInfo
- Publication number
- US20040139888A1 US20040139888A1 US10/679,611 US67961103A US2004139888A1 US 20040139888 A1 US20040139888 A1 US 20040139888A1 US 67961103 A US67961103 A US 67961103A US 2004139888 A1 US2004139888 A1 US 2004139888A1
- Authority
- US
- United States
- Prior art keywords
- powder
- fillers
- filler
- nanostructured
- matrix
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Abandoned
Links
- 239000000976 ink Substances 0.000 title abstract description 5
- 239000003153 chemical reaction reagent Substances 0.000 title 1
- 239000000203 mixture Substances 0.000 claims abstract description 55
- 238000009472 formulation Methods 0.000 claims abstract description 22
- 239000002073 nanorod Substances 0.000 claims abstract description 6
- 239000000835 fiber Substances 0.000 claims abstract description 5
- 239000000945 filler Substances 0.000 claims description 118
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 239000001301 oxygen Substances 0.000 claims description 12
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052738 indium Inorganic materials 0.000 claims description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 7
- 229910052796 boron Inorganic materials 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 229910052698 phosphorus Inorganic materials 0.000 claims description 7
- 239000011574 phosphorus Substances 0.000 claims description 7
- 229910052717 sulfur Inorganic materials 0.000 claims description 7
- 239000011593 sulfur Substances 0.000 claims description 7
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052787 antimony Inorganic materials 0.000 claims description 6
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 6
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052794 bromium Inorganic materials 0.000 claims description 6
- 239000000460 chlorine Substances 0.000 claims description 6
- 229910052801 chlorine Inorganic materials 0.000 claims description 6
- 229910052732 germanium Inorganic materials 0.000 claims description 6
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 6
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims description 5
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 5
- 229910052731 fluorine Inorganic materials 0.000 claims description 5
- 239000011737 fluorine Substances 0.000 claims description 5
- 229910052711 selenium Inorganic materials 0.000 claims description 5
- 239000011669 selenium Substances 0.000 claims description 5
- 229910052714 tellurium Inorganic materials 0.000 claims description 5
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims description 5
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 3
- 239000000843 powder Substances 0.000 abstract description 129
- 230000000694 effects Effects 0.000 abstract description 11
- 150000004767 nitrides Chemical class 0.000 abstract description 6
- 229910045601 alloy Inorganic materials 0.000 abstract description 3
- 239000000956 alloy Substances 0.000 abstract description 3
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- 150000001247 metal acetylides Chemical class 0.000 abstract description 3
- 150000004763 sulfides Chemical class 0.000 abstract description 3
- 150000004820 halides Chemical class 0.000 abstract description 2
- 230000001747 exhibiting effect Effects 0.000 abstract 1
- 239000002131 composite material Substances 0.000 description 69
- 239000011159 matrix material Substances 0.000 description 53
- 239000000463 material Substances 0.000 description 43
- 239000008188 pellet Substances 0.000 description 40
- 238000000034 method Methods 0.000 description 39
- 239000002245 particle Substances 0.000 description 38
- 229920000642 polymer Polymers 0.000 description 27
- 239000011858 nanopowder Substances 0.000 description 25
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 24
- 238000011068 loading method Methods 0.000 description 20
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 19
- 239000004926 polymethyl methacrylate Substances 0.000 description 19
- 238000000576 coating method Methods 0.000 description 18
- 239000007789 gas Substances 0.000 description 18
- 238000002156 mixing Methods 0.000 description 18
- -1 poly(methyl methacrylate) Polymers 0.000 description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 17
- 239000011248 coating agent Substances 0.000 description 17
- 239000000243 solution Substances 0.000 description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 15
- 229910052802 copper Inorganic materials 0.000 description 14
- 239000010949 copper Substances 0.000 description 14
- 239000002243 precursor Substances 0.000 description 14
- 239000000126 substance Substances 0.000 description 14
- 229910052786 argon Inorganic materials 0.000 description 12
- 239000000919 ceramic Substances 0.000 description 12
- 239000002904 solvent Substances 0.000 description 11
- 229910000859 α-Fe Inorganic materials 0.000 description 11
- 239000000839 emulsion Substances 0.000 description 10
- 229910052751 metal Inorganic materials 0.000 description 10
- 239000002184 metal Substances 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 9
- 239000003814 drug Substances 0.000 description 9
- 229940079593 drug Drugs 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 150000001450 anions Chemical class 0.000 description 8
- 238000009826 distribution Methods 0.000 description 8
- 239000010410 layer Substances 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 239000002114 nanocomposite Substances 0.000 description 8
- 239000002105 nanoparticle Substances 0.000 description 8
- 230000002829 reductive effect Effects 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- 239000011701 zinc Substances 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 7
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 150000002739 metals Chemical class 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 7
- 230000035699 permeability Effects 0.000 description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 229910052709 silver Inorganic materials 0.000 description 7
- 229910052718 tin Inorganic materials 0.000 description 7
- 229910052725 zinc Inorganic materials 0.000 description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000002485 combustion reaction Methods 0.000 description 6
- 230000006870 function Effects 0.000 description 6
- 230000000737 periodic effect Effects 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 239000004332 silver Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 5
- WHJFNYXPKGDKBB-UHFFFAOYSA-N hafnium;methane Chemical compound C.[Hf] WHJFNYXPKGDKBB-UHFFFAOYSA-N 0.000 description 5
- 150000002431 hydrogen Chemical class 0.000 description 5
- 239000000178 monomer Substances 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 230000000704 physical effect Effects 0.000 description 5
- 230000005855 radiation Effects 0.000 description 5
- 230000035939 shock Effects 0.000 description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 5
- 241000894007 species Species 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 239000011135 tin Substances 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 125000004429 atom Chemical group 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 239000000969 carrier Substances 0.000 description 4
- 239000002019 doping agent Substances 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 230000005496 eutectics Effects 0.000 description 4
- 238000011065 in-situ storage Methods 0.000 description 4
- 229910052960 marcasite Inorganic materials 0.000 description 4
- 229910052763 palladium Inorganic materials 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 4
- 229910052683 pyrite Inorganic materials 0.000 description 4
- 230000009257 reactivity Effects 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 238000007650 screen-printing Methods 0.000 description 4
- 229910010271 silicon carbide Inorganic materials 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 4
- 239000011787 zinc oxide Substances 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 229910052684 Cerium Inorganic materials 0.000 description 3
- 229910052692 Dysprosium Inorganic materials 0.000 description 3
- 229910052691 Erbium Inorganic materials 0.000 description 3
- 229910052693 Europium Inorganic materials 0.000 description 3
- 229910052688 Gadolinium Inorganic materials 0.000 description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
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Definitions
- U.S. Pat. No. 6,228,904 is a continuation-in-part of U.S. patent application Ser. No. 08/739,257, filed Oct. 30, 1996, now U.S. Pat. No. 5,905,000, titled NANOSTRUCTURED ION CONDUCTING SOLID ELECTROLYTES, which is a continuation-in-part of U.S. Ser. No. 08/730,661, filed Oct. 11, 1996, now U.S. Pat. No. 5,952,040 titled “PASSIVE ELECTRONIC COMPONENTS FROM NANO-PRECISION ENGINEERED MATERIALS” which is a continuation-in-part of U.S. Ser. No. 08/706,819, filed Sep.
- the invention comprises a nanostructured filler, intimately mixed with a matrix to form a nanostructured composite. At least one of the nanostructured filler and the nanostructured composite has a desired material property which differs by at least 20% from the same material property for a micron-scale filler or a micron-scale composite, respectively.
- the desired material property is selected from the group consisting of refractive index, transparency to light, reflection characteristics, resistivity, permittivity, permeability, coercivity, B-H product, magnetic hysteresis, breakdown voltage, skin depth, curie temperature, dissipation factor, work function, band gap, electromagnetic shielding effectiveness, radiation hardness, chemical reactivity, thermal conductivity, temperature coefficient of an electrical property, voltage coefficient of an electrical property, thermal shock resistance, biocompatibility and wear rate.
- the nanostructured filler may comprise one or more elements selected from the s, p, d, and f groups of the periodic table, or it may comprise a compound of one or more such elements with one or more suitable anions, such as aluminum, antimony, boron, bromine, carbon, chlorine, fluorine, germanium, hydrogen, indium, iodine, nickel, nitrogen, oxygen, phosphorus, selenium, silicon, sulfur, or tellurium.
- suitable anions such as aluminum, antimony, boron, bromine, carbon, chlorine, fluorine, germanium, hydrogen, indium, iodine, nickel, nitrogen, oxygen, phosphorus, selenium, silicon, sulfur, or tellurium.
- the desired material property is selected from the group consisting of refractive index, transparency to light, reflection characteristics, resistivity, permittivity, permeability, coercivity, B-H product, magnetic hysteresis, breakdown voltage, skin depth, curie temperature, dissipation factor, work function, band gap, electromagnetic shielding effectiveness, radiation hardness, chemical reactivity, thermal conductivity, temperature coefficient of an electrical property, voltage coefficient of an electrical property, thermal shock resistance, biocompatibility, and wear rate.
- the loading of the filler does not exceed 95 volume percent, and loadings of 80 volume percent or less are preferred.
- Domain size refers to the minimum dimension of a particular material morphology. In the case of powders, the domain size is the grain size. In the case of whiskers and fibers, the domain size is the diameter. In the case of plates and films, the domain size is the thickness.
- a “nanostructured powder” is one having a domain size of less than 100 nm, or alternatively, having a domain size sufficiently small that a selected material property is substantially different from that of a micron-scale powder, due to size confinement effects (e.g., the property may differ by 20% or more from the analogous property of the micron-scale material). Nanostructured powders often advantageously have sizes as small as 50 nm, 30 nm, or even smaller. Nanostructured powders may also be referred to as “nanopowders” or “nanofillers.”
- a nanostructured composite is a composite comprising a nanostructured phase dispersed in a matrix.
- the term “agglomerated” describes a powder in which at least some individual particles of the powder adhere to neighboring particles, primarily by electrostatic forces, and “aggregated” describes a powder in which at least some individual particles are chemically bonded to neighboring particles.
- the present invention is directed to inks based on novel nanofillers that enhance a wide range of properties.
- the present invention is directed to methods for preparing nanocomposites that enable nanotechnology applications offering superior functional performance.
- nanofillers and a substance having a polymer are mixed. Both low-loaded and highly-loaded nanocomposites are contemplated.
- Nanoscale coated and un-coated fillers may be used.
- Nanocomposite films may be coated on substrates.
- the matrix may be a polymer (e.g., poly(methyl methacrylate), poly(vinyl alcohol), polycarbonate, polyalkene, or polyaryl), a ceramic (e.g., zinc oxide, indium-tin oxide, hafnium carbide, or ferrite), or a metal (e.g., copper, tin, zinc, or iron).
- Loadings of the nanofiller may be as high as 95%, although loadings of 80% or less are preferred.
- the invention also comprises devices which incorporate the nanofiller (e.g., electrical, magnetic, optical, biomedical, and electrochemical devices).
- Another aspect of the invention comprises a method of producing a composite, comprising blending a nanoscale filler with a matrix to form a nanostructured composite.
- a nanostructured composite comprising blending a nanoscale filler with a matrix to form a nanostructured composite.
- the nanostructured filler or the composite itself differs substantially in a desired material property from a micron-scale filler or composite, respectively.
- the composite may be formed by mixing a precursor of the matrix material with the nanofiller, and then processing the precursor to form a desired matrix material.
- the nanofiller may be mixed with a monomer, which is then polymerized to form a polymer matrix composite.
- the nanofiller may be mixed with a matrix powder composition and compacted to form a solid composite.
- the matrix composition may be dissolved in a solvent and mixed with the nanofiller, and then the solvent may be removed to form a solid composite.
- the matrix may be a liquid or have liquid like properties.
- nanofiller compositions are encompassed within the scope of the invention, including nanofillers comprising one or more elements selected from the group consisting of actinium, aluminum, arsenic, barium, beryllium, bismuth, cadmium, calcium, cerium, cesium, cobalt, copper, dysprosium, erbium, europium, gadolinium, gallium, gold, hafnium, hydrogen, indium, iridium, iron, lanthanum, lithium, magnesium, manganese, mendelevium, mercury, molybdenum, neodymium, neptunium, nickel, niobium, osmium, palladium, platinum, potassium, praseodymium, promethium, protactinium, rhenium, rubidium, scandium, silver, sodium, strontium, tantalum, terbium, thallium, thorium, tin, titanium, tungsten, vanadium, y
- Domain size refers to the minimum dimension of a particular material morphology. In the case of powders, the domain size is the grain size. In the case of whiskers and fibers, the domain size is the diameter. In the case of plates and films, the domain size is the thickness.
- a “nanostructured powder” is one having a domain size of less than 100 nm, or alternatively, having a domain size sufficiently small that a selected material property is substantially different from that of a micron-scale powder, due to size confinement effects (e.g., the property may differ by 20% or more from the analogous property of the micron-scale material). Nanostructured powders often advantageously have sizes as small as 50 nm, 30 nm, or even smaller. Nanostructured powders may also be referred to as “nanopowders” or “nanofillers.”
- a nanostructured composite is a composite comprising a nanostructured phase dispersed in a matrix.
- the term “agglomerated” describes a powder in which at least some individual particles of the powder adhere to neighboring particles, primarily by electrostatic forces, and “aggregated” describes a powder in which at least some individual particles are chemically bonded to neighboring particles.
- FIG. 1 is a diagram of a nanostructured filler coated with a polymer
- FIG. 3 is a scanning electron microscope (SEM) micrograph of the stoichiometric indium tin oxide powder of Example 1;
- FIG. 4 is a diagram of the nanostructured varistor of Example 5.
- the number of atoms in the filler particles of the invention (hereinafter called “nanostructured filler” or “nanofiller”) is on the order of or significantly less than the number of atoms in the polymer molecules, e.g., 10 2 -10 10 .
- the filler particles are comparable in size or smaller than the polymer molecules, and therefore can be dispersed with orders of magnitude higher number density.
- the fillers may have a dimension less than or equal to the critical domain sizes that determine the characteristic properties of the bulk composition; thus, the fillers may have significantly different physical properties from larger particles of the same composition. This in turn may yield markedly different properties in composites using nanofillers as compared to the typical properties of conventional polymer composites.
- nanostructured filler materials may also have utility in the manufacture of other types of composites, such as ceramic- or metal-matrix composites. Again, the changes in the physical properties of the filler particles due to their increased surface area and constrained domain sizes can yield changes in the achievable properties of composites.
- the nanofillers of the invention can be inorganic, organic, or metallic, and may be in the form of powders, whiskers, fibers, plates or films.
- the fillers represent an additive to the overall composite composition, and may be used at loadings of up to 95% by volume.
- the fillers may have connectivity in 0, 1, 2, or 3 dimensions.
- Fillers may be produced by a variety of methods, such as those described in U.S. Pat. Nos. 5,486,675; 5,447,708; 5,407,458; 5,219,804; 5,194,128; and U.S. Pat. No. 5,064,464. Particularly preferred methods of making nanostructured fillers are described in U.S. patent application Ser. No.
- Solutions or suspensions may be prepared, for example, by mixing solutions containing each of the constituent elements of the desired powder.
- powders comprising larger numbers of dopants, metals, and anions can also be produced by the same methods.
- polymetallic materials comprising at least three metals and at least one anion can be produced. These materials are useful in the manufacture of capacitors, inductors, varistors, resistors, piezo-devices, thermistors, thermoelectric devices, filters, connectors, magnets, ion-conducting devices, sensors, fuel cells, catalysts, optics, photonic devices, lasers, tooling bits, armor, superconductors, inks, and pigments, for example.
- Prior art polymetallic powders are limited to sizes in excess of 300 nm, and mostly to sizes in excess of 1 micrometer.
- solid or porous polymetallic nanopowders can be made, with sizes less than 250 nm, and preferably less than 100 nm.
- nano-whiskers and nano-rods can be produced with aspect ratios of 25 or less, having a minimum dimension of less than 250 nm, and preferably less than 100 nm. At this scale, size confinement effects can come into play for many polymetallic powders.
- the final products are not limited to ionic materials, and include covalent and mixed ionic-covalent materials such as carbides, borides, nitrides, sulfides, oxycarbides, oxynitrides, oxyborides and oxysulfides.
- the invention comprises a method of continuously producing fine powders of complex inorganic compositions, including, but not limited to, carbides, nitrides, oxides, chalcogenides, halides, phosphides, borides, and combinations thereof by combustion of emulsions.
- carbides, nitrides, oxides, chalcogenides, halides, phosphides, borides, and combinations thereof by combustion of emulsions.
- the product chemistry may be varied to obtain non-stoichiometric, reduced oxide, or mixed anion materials.
- examples of this embodiment include the use of non-stoichiometric flames or reducing gases such as hydrogen, forming gas, or ammonia.
- the method can use low cost, safe, readily available and environmentally benign precursors to produce fine powders.
- the method ensures high yield and high selectivity, including harvesting 95% or more of the fine powder produced.
- the method prevents the damage of the fine powders during and after their synthesis.
- the invention includes multimetallic powders having a median particle size of less than 5 micrometers and a standard deviation of particle size of less than 100 nm.
- the median particle size is less than 100 nm and the standard deviation of particle size is less than 25 nm, and in further preferred embodiments, the median particle size is less than 30 nm and the standard deviation of particle size is less than 10 nm.
- the multimetallic powders include at least two elements selected from the s group, p group, d group, and f group of the periodic table (e.g., aluminum, antimony, barium, bismuth, boron, bromine, cadmium, calcium, carbon, cerium, cesium, chlorine, chromium, cobalt, copper, dysprosium, erbium, europium, gadolinium, gallium, germanium, gold, hafnium, holmium, indium, iodine, iridium, iron, lanthanum, lead, lithium, lutetium, magnesium, manganese, molybdenum, neodymium, nickel, niobium, nitrogen, osmium, oxygen, palladium, phosphorus, platinum, praseodymium, potassium, rhenium, rhodium, rubidium, samarium, scandium, silicon, silver, sodium, strontium, sulfur, tantalum, terbium
- Nanopowder describes a powder whose mean diameter is so small that its physical properties are substantially affected by size related confinement effects. Nanopowders usually have a mean diameter less than or equal to 250 nm, and preferably have a mean diameter less than or equal to 100 nm. More preferably, nanopowders may have a mean diameter less than 50 nm.
- the term “agglomerated” describes a powder in which at least some individual particles of the powder adhere to neighboring particles, primarily by electrostatic forces, and “aggregated” describes a powder in which at least some individual particles are chemically bonded to neighboring particles.
- the term “aspect ratio” refers to the ratio of the maximum to the minimum dimension of a particle.
- the term “whisker” refers to any elongated particle (e.g., a particle having an aspect ratio greater than one, and preferably at least two). Whiskers may be round or faceted, and may have varying diameters. “Rods” are substantially cylindrical whiskers. “Nanowhiskers” and “nanorods” refer to rods and whiskers whose smallest dimension is so small that their physical properties are substantially affected by size related confinement effects. Nanowhiskers and nanorods usually have a minimum dimension less than or equal to 250 nm, and preferably have a minimum dimension less than or equal to 100 nm. More preferably, these particles may have a minimum dimension less than 50 nm.
- the combustion can be accomplished using a laminar or turbulent flame, a premixed or diffusion flame, a co-axial or impinging flame, a low-pressure or high-pressure flame, a sub-sonic or sonic or super-sonic flame, a pulsating or continuous flame, an externally applied electromagnetic field free or externally applied electromagnetic field influenced flame, a reducing or oxidizing flame, a lean or rich flame, a secondary gas doped or undoped flame, a secondary liquid doped or undoped flame, a secondary particulate doped or undoped flame, an adiabatic or non-adiabatic flame, a one-dimensional or two-dimensional or three-dimensional flame, an obstruction-free or obstructed flame, a closed or open flame, an externally heated or externally cooled flame, a pre-cooled or pre-heated flame, a one burner or multiple burner flame, or a combination of one or more of the above.
- combustion temperatures will be in excess of 600° C., a temperature at which diffusion kinetics will be sufficiently fast that a compositionally uniform powder will be produced.
- the emulsion can also be a feed to other processes of producing nanoscale powders. Examples include the powder-formation processes described in copending and commonly assigned U.S. patent application Ser. No. 08/707,341, “Boundary Layer Joule—Thompson Nozzle for Thermal Quenching of High Temperature Vapors,” now U.S. Pat. No. 5,788,738 and Ser. No. 08/706,819, “Integrated Thermal Process and Apparatus for the Continuous Synthesis of Nanoscale Powders,” now U.S. Pat. No. 5,851,507, both of which are incorporated herein.
- nanofiller compositions include metals (e.g., Cu, Ag, Ni, Fe, Al, Pd, and Ti), oxide ceramics (e.g., TiO 2 , TiO 2-x , BaFe 2 O4, dielectric compositions, ferrites, and manganites), carbide ceramics (e.g., SiC, BC, TiC, WC, WCsub.1 ⁇ x), nitride ceramics (e.g., Si 3 N 4 , TiN, VN, AlN, and Mo 2 N), hydroxides (e.g., aluminum hydroxide, calcium hydroxide, and barium hydroxide), borides (e.g., AlB 2 and TiB 2 ), phosphides (e.g., NiP and VP), sulfides (e.g., molybdenum sulfide, titanium sulfide, and tungsten sulfide), silicides (e.g.,
- the fillers are immediately mixed with a matrix material, which is preferably polymeric, buy may also be ceramic, metallic, or a combination of the above.
- the matrix may be chosen for properties such as ease of processibility, low cost, environmental benignity, commercial availability, and compatibility with the desired filler.
- the fillers are preferably mixed homogeneously into the matrix, but may also be mixed heterogeneously if desired, for example to obtain a composite having a gradient of some property.
- Mixing techniques for incorporating powders into fluids and for mixing different powders are well known in the art, and include mechanical, thermal, electrical, magnetic, and chemical momentum transfer techniques, as well as combinations of the above.
- the viscosity, surface tension, and density of a liquid matrix material can be varied for mixing purposes, the preferred values being those that favor ease of mixing and that reduce energy needed to mix without introducing any undesirable contamination.
- One method of mixing is to dissolve the matrix in a solvent which does not adversely affect the properties of the matrix or the filler and which can be easily removed and recovered.
- Another method is to melt the matrix, incorporate the filler, and cool the mixture to yield a solid composite with the desired properties.
- Yet another method is to synthesize the matrix in-situ with the filler present.
- the nanofiller can be mixed with a liquid monomer, which can then be polymerized to form the composite.
- the filler may be used as a catalyst or co-catalyst for polymerization.
- the mixing may also be accomplished in the solid state, for example by mixing a powdered matrix composition with the filler, and then compacting the mixture to form a solid composite.
- Mixing can be assisted using various secondary species such as dispersants, binders, modifiers, detergents, and additives. Secondary species may also be added to enhance one to more of the properties of the filler-matrix composite.
- Mixing can also be assisted by pre-coating the nanofiller with a thin layer of the matrix composition or with a phase that is compatible with the matrix composition.
- a coated nanoparticle is illustrated in FIG. 1, which shows a spherical nanoparticle 6 and a coating 8 .
- pre-coating can be done by forming a ceramic layer around the nanoscale filler particle during or after the synthesis of the nanoscale filler, by methods such as partial oxidation, nitridation, carborization, or boronation.
- the nanostructured filler is exposed to a small concentration of a precursor that reacts with the surface of the filler to form a ceramic coating.
- a particle may be exposed to oxygen in order to create an oxide coating, to ammonia in order to create a nitride coating, to borane to create a boride coating, or to methane to create a carbide coating. It is important that the amount of precursor be small, to prevent thermal runaway and consequent conversion of the nanostructured filler into a ceramic particle.
- the filler can be coated with a polymer or a monomer by numerous methods, for example, surface coating in-situ, spray drying a dispersion of filler and polymer solution, co-polymerization on the filler surface, and melt spinning followed by milling.
- a preferred method is surface coating in-situ.
- the filler is first suspended in demineralized water (or another solvent) and the suspension's pH is measured. The pH is then adjusted and stabilized with small addition of acid (e.g., acetic acid or dilute nitric acid) or base (e.g., ammonium hydroxide or dilute sodium hydroxide). The pH adjustment produces a charged state on the surface of the filler.
- acid e.g., acetic acid or dilute nitric acid
- base e.g., ammonium hydroxide or dilute sodium hydroxide
- a coating material for example, a polymer or other appropriate precursor
- opposite charge is introduced into the solvent. This step results in coupling of the coating material around the nanoscale filler and formation of a coating layer around the nanoscale filler.
- the filler is removed from the solvent by drying, filtration, centrifugation, or any other method appropriate for solid-liquid separation. This technique of coating a filler with another material using surface charge can be used for a variety of organic and inorganic compositions.
- the matrix may also be dissolved in the solvent before or during coating, and the final composite formed by removing the solvent.
- a very wide range of material properties can be engineered by the practice of the invention.
- electrical, magnetic, optical, electrochemical, chemical, thermal, biomedical, and tribological properties can be varied over a wider range than is possible using prior art micron-scale composites.
- Nanostructured fillers can be used to lower or raise the effective resistivity, effective permittivity, and effective permeability of a polymer or ceramic matrix. While these effects are present at lower loadings, they are expected to be most pronounced for filler loadings at or above the percolation limit of the filler in the matrix (i.e., at loadings sufficiently high that electrical continuity exists between the filler particles).
- Other electrical properties which may be engineered include breakdown voltage, skin depth, curie temperature, temperature coefficient of electrical property, voltage coefficient of electrical property, dissipation factor, work function, band gap, electromagnetic shielding effectiveness and degree of radiation hardness. Nanostructured fillers can also be used to engineer magnetic properties such as the coercivity, B-H product, hysteresis, and shape of the B-H curve of a matrix.
- Nanostructured fillers may be used to produce composites with refractive index engineered for a particular application. Gradient lenses may be produced using nanostructured materials. Gradient lenses produced from nanostructured composites may reduce or eliminate the need for polishing lenses. The use of nanostructured fillers may also help filter specific wavelengths. Furthermore, a key advantage of nanostructured fillers in optical applications is expected to be their enhanced transparency because the domain size of nanostructured fillers ranges from about the same as to more than an order of magnitude less than visible wavelengths of light.
- Nanostructured fillers are also expected to modify the chemical properties of composites. These fillers are catalytically more active, and provide more interface area for interacting with diffusive species. Such fillers may, for example, modify chemical stability and mobility of diffusing gases. Furthermore, nanostructured fillers may enhance the chemical properties of propellants and fuels.
- nanostructured fillers have a domain size comparable to the typical mean free path of phonons at moderate temperatures. It is thus anticipated that these fillers may have dramatic effects on the thermal conductivity and thermal shock resistance of matrices into which they are incorporated.
- Nanostructured fillers in coated and uncoated form—and nanofilled composites are also expected to have significant value in biomedical applications for both humans and animals.
- the small size of nanostructured fillers may make them readily transportable through pores and capillaries. This suggests that the fillers may be of use in developing novel time-release drugs and methods of administration and delivery of drugs, markers, and medical materials.
- a polymer coating can be utilized either to make water-insoluble fillers into a form that is water soluble, or to make water-soluble fillers into a form that is water insoluble.
- a polymer coating on the filler may also be utilized as a means to time drug-release from a nanoparticle.
- a polymer coating may further be used to enable selective filtering, transfer, capture, and removal of species and molecules from blood into the nanoparticle.
- a nanoparticulate filler for biomedical operations might be a carrier or support for a drug of interest, participate in the drug's functioning, or might even be the drug itself.
- Possible administration routes include oral, topical, and injection routes.
- Nanoparticulates and nanocomposites may also have utility as markers or as carriers for markers. Their unique properties, including high mobility and unusual physical properties, make them particularly well-adapted for such tasks.
- magnetic nanoparticles such as ferrites may be utilized to carry drugs to a region of interest, where the particles may then be concentrated using a magnetic field.
- Photocatalytic nanoparticles can be utilized to carry drugs to region of interest and then photoactivated.
- Thermally sensitive nanoparticles can similarly be utilized to transport drugs or markers or species of interest and then thermally activated in the region of interest.
- Radioactive nanoparticulate fillers may have utility for chemotherapy.
- Nanoparticles suitably doped with genetic and culture material may be utilized in similar way to deliver therapy in target areas. Nanocomposites may be used to assist in concentrating the particle and then providing the therapeutic action.
- nanoparticulate fillers may be used for diagnosis of medical conditions.
- fillers may be concentrated in a region of the body where they may be viewed by magnetic resonance imaging or other techniques.
- nanoparticulates can be released into the body in a controlled fashion over a long time period, by implanting a nanocomposite material having a bioabsorbable matrix, which slowly dissolves in the body and releases its embedded filler.
- Nanostructured fillers and composites are expected to lower wear rate and thereby enhance patient acceptance of surgical procedures.
- Nanostructured fillers may also be more desirable than micron-scale fillers, because the possibility exists that their domain size may be reduced to low enough levels that they can easily be removed by normal kidney action without the development of stones or other adverse side effects.
- nanoparticulates may be removed naturally through kidney and other organs, they may also be filtered or removed externally through membranes or otherwise removed directly from blood or tissue.
- Carrier nanoparticulates may be reactivated externally through membranes and reused; for example, nutrient carriers may be removed from the bloodstream, reloaded with more nutrients, and returned to carry the nutrients to tissue. The reverse process may also be feasible, wherein carriers accumulate waste products in the body, which are removed externally, returning the carriers to the bloodstream to accumulate more waste products.
- a stoichiometric (90 wt % ln203 in SnO 2 ) indium tin oxide (ITO) nanopowder was produced using the methods of copending patent application Ser. No. 09/046,465.
- 50 g of indium shot was placed in 300 ml of glacial acetic acid and 10 ml of nitric acid.
- the combination in a 1000 ml Erlenmeyer flask, was heated to reflux while stirring for 24 hours.
- 50 ml of HNO 3 was added, and the mixture was heated and stirred overnight.
- the solution so produced was clear, with all of the indium metal dissolved into the solution, and had a total final volume of 318 ml.
- FIG. 2 shows the measured X-ray diffraction (XRD) spectrum for the powder
- FIG. 3 shows a scanning electron microscope (SEM image of the powder. These data show that the powder was of nanometer scale.
- the nanostructured powder was then mixed with poly(methyl methacrylate) (PMMA) in a ratio of 20 vol % powder to 80 vol % PMMA.
- PMMA poly(methyl methacrylate)
- the powder and the polymer were mixed using a mortar and pestle, and then separated into three parts, each of which was pressed into a pellet.
- the pellets were pressed by using a Carver hydraulic press, pressing the mixture into a 1 ⁇ 4 inch diameter die using a 1500 pound load for one minute.
- ⁇ volume resistivity in ohm-cm
- R represents the measured resistance in ohms
- A represents the area of the electroded surface of the pellet in cm 2
- t represents the thickness of the pellet in cm.
- the average volume resistivity of the stoichiometric ITO composite pellets was found to be 1.75 ⁇ 10 4 ohm-cm.
- ITO nanopowder Another quantity of ITO nanopowder was produced as described above, and was reduced by passing 2 SCFM of forming gas (5% hydrogen in nitrogen) over the powder while ramping temperature from 25° C. to 250° C. at 5° C./min. The powder was held at 250° C. for 3 hours, and then cooled back to room temperature. The XRD spectrum of the resulting powder indicated that the stoichiometry of the reduced powder was In 18 SnO 29-x , with x greater than 0 and less than 29.
- the reduced ITO nanopowder was combined with PMMA in a 20:80 volume ratio and formed into pellets as described above.
- the pellets were electroded as described, and their resistivity was measured.
- the average resistivity for the reduced ITO composite pellets was found to be 1.09 ⁇ 10 4 ohm-cm.
- micron scale ITO was purchased from Alfa Aesar (catalog number 36348), and was formed into pellets with PMMA and electroded as described above. Again, the volume fraction of ITO was 20%.
- the average measured resistivity of the micron scale ITO composite pellets was found to be 8.26 ⁇ 10 8 ohm-cm, representing a difference of more than four orders of magnitude from the nanoscale composite pellets. It was thus established that composites incorporating nanoscale fillers can have unique properties not achievable by prior art techniques.
- Nanoscale hafnium carbide fillers were prepared as described in copending U.S. patent application Ser. No. 08/706,819 and Ser. No. 08/707,341.
- the nanopowder surface area was 53.5 m 2 /gm, and mean grain size was 16 nm.
- Micron scale hafnium carbide powder was purchased from Cerac (catalog number H-1004) for comparison.
- Composite pellets were produced as described in Example 1, by mixing filler and polymer with a mortar and pestle and pressing in a hydraulic press. Pellets were produced containing either nanoscale or micron scale powder at three loadings: 20 vol % powder, 50 vol % powder, and 80 vol % powder. The pellets were electroded as described above, and their resistivities were measured. (Because of the high resistances at the 20% loading, these pellets' resistivities were measured at 100V. The other pellets were measured at IV, as described in Example 1).
- the nanoscale and micron scale copper powders were each mixed at a loading of 20 vol % copper to 80 vol % PMMA and formed into pellets as described above.
- pellets having a loading of 15 vol % copper in poly(vinyl alcohol) (PVA) were produced by the same method.
- the pellets were electroded and resistivities measured at 1 volt as described in Example 1. Results are shown in Table 2.
- Example 1 The stoichiometric (90 wt % In 2 O 3 in SnO 2 ) indium tin oxide (ITO) nanopowder of Example 1 was coated with a polymer as follows.
- a complex oxide nanoscale filler having the following composition was prepared: Bi 2 O 3 (48.8 wt %), NiO (24.4 wt %), CoO (12.2 wt %), Cr 2 O 3 (2.4 wt %), MnO (12.2 wt %), and Al 2 O 3 ( ⁇ 0.02 wt %).
- the complex oxide filler was prepared from the corresponding nitrates of the same cation. The nitrates of each constituent were added to 200 mL of deionized water while constantly stirring. Hydroxides were precipitated with the addition of 50 drops of 28-30% NH 4 OH.
- the solution was filtered in a large buchner funnel and washed with deionized water and then with ethyl alcohol.
- the powder was dried in an oven at 80° C. for 30 minutes.
- the dried powder was ground using a mortar and pestle.
- a heat treatment schedule consisting of a 15° C./min ramp to 350° C. with a 30 minute dwell was used to calcine the ground powder.
- the nanofiller was then incorporated at a loading of 4% into a zinc oxide ceramic matrix.
- the composite was prepared by mechanically mixing the doped oxide nanofiller powder with zinc oxide powder, incorporating the mixture into a slurry, and screen printing the slurry (further described below).
- devices were made using both a nanoscale matrix powder produced by the methods of copending and commonly assigned U.S. application Ser. No. 08/706,819, and using a micron scale matrix powder purchased from Chemcorp. The fillers and the matrix powders were mixed mechanically using a mortar and pestle.
- a paste was prepared by mixing 4.0 g of powder with 2.1 g of a commercial screen printing vehicle purchased from Electro Science Laboratories (ESL vehicle 400).
- the doped nanoscale powder paste was made using 3.5 g powder and 3.0 g ESL vehicle 400.
- Each paste was mixed using a glass stir rod.
- Silver-palladium was used as a conducting electrode material.
- a screen with a rectangular array pattern was used to print each paste on an alumina substrate.
- First a layer of silver-palladium powder (the lower electrode) was screen printed on the substrate and dried on a hot plate. Then the ceramic filled powder was deposited, also by screen printing. Four print-dry cycles were used to minimize the possibility of pinhole defects in the varistor. Finally, the upper electrode was deposited.
- the electrode/composite/electrode varistor was formed as three diagonally offset overlapping squares, as illustrated in FIG. 4.
- the effective nanostructured-filler based composite area in the device due to the offset of the electrodes was 0.036 in 2 (0.2315 cm 2 ).
- the green thick films were co-fired at 900° C. for 60 minutes.
- the screen printed specimen is shown in FIG. 4, where light squares 10 represent the silver-palladium electrodes, and dark square 12 represents the composite layer.
- Silver leads were attached to the electrodes using silver epoxy.
- the epoxy was cured by heating at a 50° C./min ramp rate to 600° C. and then cooling to room temperature at a rate of 50° C./min.
- the TestPoint computer software in conjunction with a Keithley® current source, was used to obtain a current-voltage curve for each of the varistors.
- Testpoint and Keithley are trademarks or registered trademark of Keithley Scientific Instruments, Inc.
- the electrode/micron scale matrix composite/electrode based varistor device had a total thickness of 29-33 microns and a composite layer thickness of 19 microns.
- the electrode/nanoscale matrix composite/electrode based varistor device had a total thickness of 28-29 microns and a composite layer thickness of 16 microns.
- Examination of current-voltage response curves for both varistors showed that the nanostructured matrix varistor had an inflection voltage of about 2 volts, while the inflection voltage of the micron scale matrix varistor had an inflection voltage of about 36 volts. Fitting the current-voltage response curves to the standard varistor power-law equation
- Thermal batteries are primary batteries ideally suited for military ordinance, projectiles, mines, decoys, torpedoes, and space exploration systems, where they are used as highly reliable energy sources with high power density and extremely long shelf life. Thermal batteries have previously been manufactured using techniques that place inherent limits on the minimum thickness obtainable while ensuring adequate mechanical strength. This in turn has slowed miniaturization efforts and has limited achievable power densities, activation characteristics, safety, and other important performance characteristics. Nanocomposites help overcome this problem, as shown in the following example.
- the pellets of anode electrodes were prepared by a cold press process. A hard steel die with a 20 mm internal diameter was used to make the thin disk pellets. 0.314 grams of Li 44%-Si 56% alloy powder (with 76-422 mesh particle size) was pressed under 6000 psi static pressure to form a pellet. The thickness and density of the pellets so obtained was determined to be 0.84 mm and 1.25 g/cm 2 , respectively. Electrolyte pellets were produced using 0.55 grams of blended electrolyte powder under 4000 psi static pressure. The thickness and density of the pellets obtained were 0.84 mm and 2.08 g/cm 2 respectively.
- Ferrite inductors were prepared using nanostructured and micron-scale powders as follows. One-tenth of a mole (27.3 grams) of iron chloride hexahydrate (FeCl 3 ⁇ 6H 2 O) was dissolved in 500 ml of distilled water along with 0.025 moles (3.24 grams) of nickel chloride (NiCl 2 ) and 0.025 moles (3.41 grams) of zinc chloride (ZnCl 2 ). In another large beaker, 25 grams of NaOH was dissolved in 500 ml of distilled water. While stirring the NaOH solution rapidly, the metal chloride solution was slowly added, forming a precipitate instantaneously.
- the precipitate solution was vacuum filtered while frequently rinsing with distilled water. After the precipitate had dried enough to cake and crack, it was transferred to a glass dish and allowed to dry for 1 hour in an 80° C. drying oven. At this point, the precipitate was ground with a mortar and pestle and calcined in air at 400° C. for 1 hour to remove any remaining moisture and organics.
- BET analysis of the produced powder yielded a surface area of 112 m 2 /g, confirming the presence of nanometer-sized individual particles with an estimated BET particle size of 11 nm.
- XRD analyses of all nanoscale powders showed the formation of a single (Ni, Zn)Fe 2 O 4 ferrite phase with peak shapes characteristic of nanoscale powders.
- XRD peak broadening calculations reported an average crystallite size of 20 nm of the thermally quenched powders and 8 nm for the chemically derived powders.
- Nanoscale ferrite filler powders were uniaxially pressed at 5000 pounds in a quarter-inch diameter die set into green pellets.
- the powders were mixed with 2 weight percent Duramax® binder for improved sinterability.
- the amount of powder used for pressing varied from 1.5 to 1.7 grams, typically resulting in cylinders having a post-sintered height of approximately 1.5 cm.
- a multi-level heating profile was employed. The pellets were fired at a rate of 5° C./min to 300° C., 10° C./min to 600° C., and 20° C./min to the final sintering temperature, where it was held for four hours.
- Resistivity measurements were made with a Keithley® 2400 SourceMeter using a four-wire probe attachment and TestPointTM data acquisition software. Voltage was ramped from 0.1 to 20 volts while simultaneously measuring current. The results were plotted as field (voltage divided by pellet thickness) versus current density (current divided by electrode cross sectional area). The slope of this graph gives material resistivity (p).
- Table 3 summarizes electrical properties of inductors prepared from micron-sized powder or from nanopowder. In most cases there is an advantage to using nanoscale precursor powder instead of micron-sized powder. It is important to keep in mind that all measurements were taken from cylindrical devices, which have inherently inefficient magnetic properties. Solenoids of this shape were used in this study because of the ease of production and excellent reproducibility. All measured properties would be expected to improve with the use of higher magnetic efficiency shapes such as cores or toroids, or by improving the aspect ratio (length divided by diameter) of the cylindrical samples.
- the inductors made from ferrite nanopowders exhibited significantly higher Q-factor, critical resonance frequency, and resistivity. They also exhibited more than 20% lower loss factor as is desired in commercial applications.
- Zinc Commercially available zinc powder ( ⁇ 325 mesh) was used as the precursor to produce nanosize zinc powder. Feed zinc powder was fed into the thermal reactor suspended in an argon stream (argon was used as the plasma gas; the total argon flow rate was 2.5 ft 3 /min). The reactor was inductively heated with 16 kW of RF plasma to over 5,000K in the plasma zone and about 3,000K in the extended reactor zone adjacent the converging portion of the nozzle. The vaporized stream was quenched through the converging-diverging nozzle. The preferred pressure drop across the nozzle was 250 Torr, but useful results were obtained at different pressure drops, ranging from 100 to 550 Torr.
- the powder produced was separated from the gas by means of a cooled copper-coil-based impact filter followed by a screen filter.
- the nanosize powder produced by the invention were in the 5-25 nanometer range. The size distribution was narrow, with a mean size of approximately 15 nm and a standard deviation of about 7.5 nm.
- Iron-Titanium Intermetallic 2-5 micron powders of iron and 10-25 micron powders of titanium were mixed in 1:1 molar ratio and fed into the thermal reactor suspended in an argon stream (total gas flow rate, including plasma gas, was 2.75 ft 3 /min).
- the reactor was inductively heated with 18 kW of RF plasma to over 5,000K in the plasma zone and above 3,000K in the extended reactor zone adjacent the converging portion of the nozzle.
- the vaporized stream was quenched through the converging-diverging nozzle.
- the preferred pressure drop across the nozzle was 250 Torr, but useful results were obtained at different pressure drops, ranging from 100 to 550 Torr.
- the powder produced was separated from the gas by means of a cooled copper-coil-based impact filter followed by a screen filter.
- the nanopowders produced by the invention were in the 10-45 nanometer range. The size distribution was narrow, with a mean size of approximately 32 nm and a standard deviation of about 13.3 nm.
- the powder produced was separated from the gas by means of a cooled copper-coil-based impact filter followed by a screen filter.
- the powder produced by the invention were in the 10-25 nanometer range. The size distribution was narrow, with a mean size of about 16.1 nm and a standard deviation of about 6.3 nm.
- Cerium Oxide Commercially available cerium oxide powder (5-10 micron size) was used as the precursor to produce nanosize CeO 2 .
- the cerium oxide powder was suspended in a mixture of argon and oxygen as the feed stream (at total rates of 2.25 ft 3 /min for argon and 0.25 ft 3 /min for oxygen).
- the reactor was inductively heated with 18 kW of RF plasma to over 5,000K in the plasma zone and about 3,000K in the extended reactor zone adjacent the converging portion of the nozzle.
- the vaporized stream was quenched through the converging-diverging nozzle.
- the preferred pressure drop across the nozzle was 250 Torr, but useful results were obtained at different pressure drops, ranging from 100 to 650 Torr.
- the powder produced was separated from the gas by means of a cooled copper-coil-based impact filter followed by a screen filter.
- the powder produced by the invention was in the 5-25 nanometer range.
- the size distribution was narrow, with a mean size of about 18.6 nm and a standard deviation of about 5.8 nm.
- Silicon Carbide Commercially available silicon carbide powder ( ⁇ 325 mesh size) was used as the precursor to produce nanosize SiC. The powder was suspended in argon as the feed stream (total argon flow rate of 2.5 ft 3 /min). The reactor was inductively heated with 18 kW of RF plasma to over 5,000K in the plasma zone and about 3,000K in the extended reactor zone adjacent the converging portion of the nozzle. The vaporized stream was quenched through the converging-diverging nozzle. The preferred pressure drop across the nozzle was 250 Torr, but useful results were obtained at different pressure drops, ranging from 100 to 550 Torr.
- Molybdenum Nitride Commercially available molybdenum oxide (MoO 3 ) powder ( ⁇ 325 mesh size) was used as the precursor to produce nanosize Mo 2 N. Argon was used as the plasma gas at a feed rate of 2.5 ft 3 /min. A mixture of ammonia and hydrogen was used as the reactant gases (NH 3 at 0.1 ft 3 /min; H 2 at 0.1 ft 3 /min). The reactor was inductively heated with 18 kW of RF plasma to over 5,000K in the plasma zone and about 3,000K in the extended reactor zone adjacent the converging portion of the nozzle. The vaporized stream was quenched through the converging-diverging nozzle.
- MoO 3 molybdenum oxide
- the preferred pressure drop across the nozzle was 250 Torr, but useful results were obtained at different pressure drops, ranging from 100 to 550 Torr.
- the powder produced was separated from the gas by means of a cooled copper-coil-based impact filter followed by a screen filter.
- the Mo 2 N powder produced by the invention was in the 5-30 nanometer range. The size distribution was narrow, with a mean size of about 14 nm and a standard deviation of about 4.6 nm.
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US12/768,020 US20100210450A1 (en) | 2002-12-10 | 2010-04-27 | Tungsten comprising nanomaterials and related nanotechnology |
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US08/730,661 US5952040A (en) | 1996-10-11 | 1996-10-11 | Passive electronic components from nano-precision engineered materials |
US08/739,257 US5905000A (en) | 1996-09-03 | 1996-10-30 | Nanostructured ion conducting solid electrolytes |
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Also Published As
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US20030207977A1 (en) | 2003-11-06 |
US20030212179A1 (en) | 2003-11-13 |
US20020188052A1 (en) | 2002-12-12 |
US20070032572A1 (en) | 2007-02-08 |
US6933331B2 (en) | 2005-08-23 |
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US20020014182A1 (en) | 2002-02-07 |
US20030199624A1 (en) | 2003-10-23 |
US20030207978A1 (en) | 2003-11-06 |
US7388042B2 (en) | 2008-06-17 |
US8058337B2 (en) | 2011-11-15 |
US7183337B1 (en) | 2007-02-27 |
US20080142764A1 (en) | 2008-06-19 |
US20100320417A1 (en) | 2010-12-23 |
US7238734B2 (en) | 2007-07-03 |
US7250454B2 (en) | 2007-07-31 |
US20030207976A1 (en) | 2003-11-06 |
US8389603B2 (en) | 2013-03-05 |
US7387673B2 (en) | 2008-06-17 |
US20030207975A1 (en) | 2003-11-06 |
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