US20130309495A1 - Process of dry milling particulate materials - Google Patents
Process of dry milling particulate materials Download PDFInfo
- Publication number
- US20130309495A1 US20130309495A1 US13/474,860 US201213474860A US2013309495A1 US 20130309495 A1 US20130309495 A1 US 20130309495A1 US 201213474860 A US201213474860 A US 201213474860A US 2013309495 A1 US2013309495 A1 US 2013309495A1
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- US
- United States
- Prior art keywords
- composition
- graphene
- metal
- matter
- particulate
- 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
- 238000000034 method Methods 0.000 title claims description 26
- 239000011236 particulate material Substances 0.000 title claims description 19
- 238000009837 dry grinding Methods 0.000 title claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 44
- 239000002245 particle Substances 0.000 claims abstract description 28
- 229910052751 metal Inorganic materials 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims abstract description 19
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 18
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 18
- 239000002114 nanocomposite Substances 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims abstract description 7
- 239000011248 coating agent Substances 0.000 claims abstract description 5
- 150000002739 metals Chemical class 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 40
- 239000000203 mixture Substances 0.000 claims description 21
- 238000003801 milling Methods 0.000 claims description 18
- 229910002804 graphite Inorganic materials 0.000 claims description 11
- 239000010439 graphite Substances 0.000 claims description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- -1 polypropylene Polymers 0.000 claims description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- 239000000956 alloy Substances 0.000 claims description 6
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- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 239000011777 magnesium Substances 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
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- 239000010949 copper Substances 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 4
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- 239000010931 gold Substances 0.000 claims description 4
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 4
- 239000002923 metal particle Substances 0.000 claims description 4
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- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052707 ruthenium Inorganic materials 0.000 claims description 4
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- 239000004332 silver Substances 0.000 claims description 4
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- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- 239000003990 capacitor Substances 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 150000001247 metal acetylides Chemical class 0.000 claims description 2
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 239000003054 catalyst Substances 0.000 claims 1
- 229910000428 cobalt oxide Inorganic materials 0.000 claims 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims 1
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- 239000000395 magnesium oxide Substances 0.000 claims 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 239000002356 single layer Substances 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 5
- 238000000498 ball milling Methods 0.000 abstract description 2
- 239000002103 nanocoating Substances 0.000 abstract description 2
- PYTMYKVIJXPNBD-UHFFFAOYSA-N clomiphene citrate Chemical compound [H+].[H+].[H+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.C1=CC(OCCN(CC)CC)=CC=C1C(C=1C=CC=CC=1)=C(Cl)C1=CC=CC=C1 PYTMYKVIJXPNBD-UHFFFAOYSA-N 0.000 description 6
- 238000000227 grinding Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
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- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000011135 tin Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 239000004962 Polyamide-imide Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000010316 high energy milling Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910000473 manganese(VI) oxide Inorganic materials 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
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- 229910002076 stabilized zirconia Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
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- 239000010937 tungsten Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/18—Details
- B02C17/20—Disintegrating members
-
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- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/16—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer formed of particles, e.g. chips, powder or granules
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
Definitions
- This invention deals with graphene platelet nano composites with metal or metal oxide, and graphene platelet nano coated with metal or metal oxide.
- the coated and composited particles are useful as electrodes and for electrical applications.
- Graphite is formed by many layers of carbon in highly structured platelets. These platelets, when separated from the graphite superstructure, are collectively called graphene. Graphene has interesting chemical, physical, and electrical properties. These properties make graphene a highly valued product. The quality of the graphene, as defined by particle diameter, particle width, and surface area, determine its industrial utility. It is advantageous to coat or composite graphene with metal particles for electrical applications.
- Graphene produced by media ball milling has very small particle size with a relatively high surface area. It is uniquely suited to make nano-composites or coatings by coating or admixing other particles. Metals or metal oxides can be coated or formed into composites with the high surface area, relatively low aspect ratio graphene. It is believed by the inventors herein that the materials of this invention have unique aspect ratios. Ground graphite admixed with silicon has an aspect ratio fairly close to 1, graphene from a GO process, epitaxially grown graphene, or graphene from an intercalated—heating process has a very high aspect ratio. The moderate aspect ratio graphene of this invention better coats 1 to 4 micron particles and better mixes with even small nano-particles.
- Native graphite has a very high G/D ratio.
- Graphite ground to amorphous powder has the G/D ratio.
- the material of the instant invention starts high and tends toward 2 the more the material is processed.
- Amorphous graphite also has a G peak red shift to 2000 cm ⁇ 1 .
- the material of the instant invention may have a small red shift, but from the quality of the data it is hard to determine.
- the very high surface area and aspect ratio confirms it is largely graphene nano-platelets.
- Mechanically exfoliated graphene is distinct from ground graphite, in that, it maintains the strong crystalline sp2 structure. As graphite is ground to amorphous, the ratio of G to D Raman lines tends to 2 and the G line red shifts from 1560 cm ⁇ 1 to 2000 cm ⁇ 1 .
- the G peak is referred to as the graphene peak.
- the D peak referred to as the Disorder peak. The more graphite is ground, the more the G peak is reduced and the D peak is increased.
- the added particles are larger than the graphene, they are coated with graphene, and if they are about the same approximate size, a nano-composite forms.
- the nanocomposites are useful for producing electrodes, especially for battery and capacitor applications.
- FIG. 1 is a graph of battery performance of a Si/graphene (200-250 m 2 /g, 100 minutes processing time).
- the exfoliated material has a particle size of 10 microns by 5 nm thick, or less.
- the dry milling is controlled by controlling the surface energy of the milling media in addition to controlling the hardness of the milling media.
- a second embodiment that is a process of dry milling particulate materials, wherein at least one of the particulate materials is a layered material, in the presence of a particulate material selected from the group consisting of i. ceramic, ii. glass, and iii. quartz, to obtain a composition wherein the layered material is exfoliated and wherein the particulate material is coated with the exfoliated material.
- the exfoliated material has a particle size of 500 nanometers or less.
- the dry milling is controlled by controlling the surface energy of the milling media in addition to controlling the hardness of the milling media.
- a fourth embodiment there is a composited product obtained by the first embodiment and a coated product obtained by the second embodiment.
- the graphene produced by the methods of this invention has a relatively narrow aspect ratio, greater than graphite.
- aspect ratios above 5 and below 200 are preferred and more preferred are aspect ratios above 10 and below 25.
- the small that is, 1 to 5 nanometers thick, and 50 to 100 nanometers diameter, high surface area (above 500 BET), medium aspect ratio graphene, is a unique size for coating with small metal or metal oxide particles.
- the metals useful in this invention are the metalloid silicon, and the metals tin, iron, magnesium, manganese, aluminum, lead, gold, silver, titanium, platinum, palladium, ruthenium, copper, nickel, rhodium, and alloys of any of the above.
- the plastic milling media useful in this invention has a hardness on the Brinell Scale in the range of 3 to 100.
- the plastic milling media is selected from the group consisting essentially of polyacetals, polyacrylates, such as, for example, methylmethacrylate, polycarbonate, polystyrene, poly-propylene, polyethylene, polytetrafluoroethylene, polyethylene-imide, polyvinylchloride, polyamine-imide, phenolics and formaldehyde-based thermosetting resins, and alloys of any of the plastics named.
- the particulate metal oxides useful in this invention are metal oxides selected from silicon, tin, iron, magnesium, manganese, aluminum, lead, gold, silver, titanium, platinum, palladium, ruthenium, copper, nickel, rhodium, tungsten, cobalt, molybdenum, and alloys of any the above named metal oxides, wherein the metal and metal oxide particles have a size of 100 microns or less. Preferred are particle sizes of 10 microns or less, and most preferred are particle sizes of 5 microns or less.
- Metal carbides, metal nitrides are useful in this invention, as well as non-layered materials.
- Graphene useful in this invention is preferred to have a thickness of 5 nm or less.
- the polymethylmeth-acrylate balls can be replaced with polycarbonate, polystyrene, polypropylene, polyethylene, polytetrafluoroethylene, polyethyleneimide, polyvinylchloride and polyamide-imide to control milling efficiency, graphene size, porosity distribution and surface area at a fixed milling time, contact quality between Si and graphene surface.
- the surface area of the Si/graphene composite produced can be varied from 100 m 2 /g to 700 m 2 /g depending on milling time (60 to 500 min.) and Si/graphene composition and type of ball materials.
- the result for the battery performance of a Si/graphene (200 to 250 m 2 /g, 100 min. processing) sample as an anode for a lithium ion battery is plotted infra.
- the Si/graphene shows high capacity (>800 mAh/g, electrode loading) over 35 cycles at 100 mA/g, which supports the low cost, simple, time-saving, environmentally benign, flexible way to produce high performance graphene-based composite materials for energy applications. Some fluctuation of the capacity is due to the variation of temperature.
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Abstract
Graphene produced by media ball milling has very small particle size, a relatively high surface area and unique aspect ratios. It is uniquely suited to make nano-composites or coating by coating or admixing other particles. Metals or metal oxides can be coated or formed into composites with the high surface area, relatively low aspect ratio graphene. If the added particles are larger than the graphene, they are coated with graphene, and if they are about the same approximate size, a nano-composite forms. The nanocomposites are useful for producing electrodes, especially for battery and supercapacitor applications.
Description
- This invention deals with graphene platelet nano composites with metal or metal oxide, and graphene platelet nano coated with metal or metal oxide. The coated and composited particles are useful as electrodes and for electrical applications.
- Graphite is formed by many layers of carbon in highly structured platelets. These platelets, when separated from the graphite superstructure, are collectively called graphene. Graphene has interesting chemical, physical, and electrical properties. These properties make graphene a highly valued product. The quality of the graphene, as defined by particle diameter, particle width, and surface area, determine its industrial utility. It is advantageous to coat or composite graphene with metal particles for electrical applications.
- Xg Sciences, Inc. headquartered in Lansing, Mich. produces a “C” grade graphene by a high energy, plastic media, dry, mechanical milling process. Grade size characteristics make it uniquely suited to coating or mixing with nanoparticles to form useful materials for electrodes.
- The applicant is aware of U.S. Patent publication 2011/0111303 A1 that published on May 12, 2011 as showing a wet process for treating graphene with silicon.
- Also, the patentees are aware of EP2275385 in the name of Peukert, et al in which a wet process is set forth for grinding particulate materials, wherein the grinding media is yttrium stabilized zirconia.
- Graphene produced by media ball milling has very small particle size with a relatively high surface area. It is uniquely suited to make nano-composites or coatings by coating or admixing other particles. Metals or metal oxides can be coated or formed into composites with the high surface area, relatively low aspect ratio graphene. It is believed by the inventors herein that the materials of this invention have unique aspect ratios. Ground graphite admixed with silicon has an aspect ratio fairly close to 1, graphene from a GO process, epitaxially grown graphene, or graphene from an intercalated—heating process has a very high aspect ratio. The moderate aspect ratio graphene of this invention better coats 1 to 4 micron particles and better mixes with even small nano-particles.
- Based on Raman spectroscopy with the aspect ratio, particle size, and/or surface area, provides graphene in this invention that is unique.
- Based on the following table calculated from Raman Spectroscopy and measuring peak height, generated the following table.
-
m2/g G D G/D Gpeak 250 50 5 10 1580 400 19 6 3.2 500 21 7 3 600 16 6 2.7 1585 - Native graphite has a very high G/D ratio. Graphite ground to amorphous powder has the G/D ratio. the material of the instant invention starts high and tends toward 2 the more the material is processed. Amorphous graphite also has a G peak red shift to 2000 cm−1. The material of the instant invention may have a small red shift, but from the quality of the data it is hard to determine. The very high surface area and aspect ratio confirms it is largely graphene nano-platelets.
- Mechanically exfoliated graphene is distinct from ground graphite, in that, it maintains the strong crystalline sp2 structure. As graphite is ground to amorphous, the ratio of G to D Raman lines tends to 2 and the G line red shifts from 1560 cm−1 to 2000 cm−1. The G peak is referred to as the graphene peak. The D peak referred to as the Disorder peak. The more graphite is ground, the more the G peak is reduced and the D peak is increased.
- If the added particles are larger than the graphene, they are coated with graphene, and if they are about the same approximate size, a nano-composite forms. The nanocomposites are useful for producing electrodes, especially for battery and capacitor applications.
-
FIG. 1 is a graph of battery performance of a Si/graphene (200-250 m2/g, 100 minutes processing time). - Thus, in one embodiment, there is a process of dry milling particulate materials, wherein at least one of the particulate materials is a layered material, in the presence of a non-layered material, to obtain a composition wherein the layered material is exfoliated and wherein the non-layered material is composited with the exfoliated material.
- The exfoliated material has a particle size of 10 microns by 5 nm thick, or less. In addition, the dry milling is controlled by controlling the surface energy of the milling media in addition to controlling the hardness of the milling media.
- In a second embodiment, that is a process of dry milling particulate materials, wherein at least one of the particulate materials is a layered material, in the presence of a particulate material selected from the group consisting of i. ceramic, ii. glass, and iii. quartz, to obtain a composition wherein the layered material is exfoliated and wherein the particulate material is coated with the exfoliated material.
- The exfoliated material has a particle size of 500 nanometers or less. In addition, the dry milling is controlled by controlling the surface energy of the milling media in addition to controlling the hardness of the milling media.
- In, a fourth embodiment, there is a composited product obtained by the first embodiment and a coated product obtained by the second embodiment.
- The graphene produced by the methods of this invention has a relatively narrow aspect ratio, greater than graphite. For this invention aspect ratios above 5 and below 200 are preferred and more preferred are aspect ratios above 10 and below 25.
- The small, that is, 1 to 5 nanometers thick, and 50 to 100 nanometers diameter, high surface area (above 500 BET), medium aspect ratio graphene, is a unique size for coating with small metal or metal oxide particles.
- The metals useful in this invention are the metalloid silicon, and the metals tin, iron, magnesium, manganese, aluminum, lead, gold, silver, titanium, platinum, palladium, ruthenium, copper, nickel, rhodium, and alloys of any of the above.
- The plastic milling media useful in this invention has a hardness on the Brinell Scale in the range of 3 to 100. The plastic milling media is selected from the group consisting essentially of polyacetals, polyacrylates, such as, for example, methylmethacrylate, polycarbonate, polystyrene, poly-propylene, polyethylene, polytetrafluoroethylene, polyethylene-imide, polyvinylchloride, polyamine-imide, phenolics and formaldehyde-based thermosetting resins, and alloys of any of the plastics named.
- The particulate metal oxides useful in this invention are metal oxides selected from silicon, tin, iron, magnesium, manganese, aluminum, lead, gold, silver, titanium, platinum, palladium, ruthenium, copper, nickel, rhodium, tungsten, cobalt, molybdenum, and alloys of any the above named metal oxides, wherein the metal and metal oxide particles have a size of 100 microns or less. Preferred are particle sizes of 10 microns or less, and most preferred are particle sizes of 5 microns or less.
- Metal carbides, metal nitrides are useful in this invention, as well as non-layered materials.
- Graphene useful in this invention is preferred to have a thickness of 5 nm or less.
- Two grams of natural graphite and 1 g of micron sized Si (1 to 4 um) were loaded into a 65 ml stainless steel grinding container and milled in the presence of 24 g of polymethyl-methacrylate balls. The polymethylmethacrylate balls consisted of two different sizes, namely, ¼ inches and ⅜ inches in diameter. The high energy milling machine was operated at <1500 rpm and its clamp speed was 1060 cycle/min. The polymethylmeth-acrylate balls can be replaced with polycarbonate, polystyrene, polypropylene, polyethylene, polytetrafluoroethylene, polyethyleneimide, polyvinylchloride and polyamide-imide to control milling efficiency, graphene size, porosity distribution and surface area at a fixed milling time, contact quality between Si and graphene surface. The surface area of the Si/graphene composite produced can be varied from 100 m2/g to 700 m2/g depending on milling time (60 to 500 min.) and Si/graphene composition and type of ball materials.
- The result for the battery performance of a Si/graphene (200 to 250 m2/g, 100 min. processing) sample as an anode for a lithium ion battery is plotted infra. The Si/graphene shows high capacity (>800 mAh/g, electrode loading) over 35 cycles at 100 mA/g, which supports the low cost, simple, time-saving, environmentally benign, flexible way to produce high performance graphene-based composite materials for energy applications. Some fluctuation of the capacity is due to the variation of temperature.
- Two grams of natural graphite and 1 g of nano sized metal oxides (Fe2O3, NiO, CoO3, MnO3) were loaded in a 65 ml stainless steel grinding container and milled in the presence of 24 g of polymethylmethyacrylate balls. The products can be used as anode materials for lithium batteries and electrodes for supercapacitors.
Claims (41)
1. A process of dry milling particulate materials, wherein at least one of the particulate materials is a layered material, in the presence of a non-layered material, to obtain a composition wherein the layered material is exfoliated and wherein the non-layered material is composited with the exfoliated material, the exfoliated material having a particle size of 10 microns by 5 nm thick, or less, and wherein the dry milling is controlled by controlling the surface energy of the milling media in addition to controlling the hardness of the milling media.
2. The process as claimed in claim 1 wherein the non-layered material is selected from the group consisting essentially of:
i. a particulate metal and,
ii. a particulate metal oxide.
3. The process as claimed in claim 1 wherein the layered material is graphite.
4. The process as claimed in claim 1 wherein the milling media has a surface energy essentially equivalent to the surface energy of the layered material.
5. The process as claimed in claim 1 wherein the milling media has a hardness on the Brinell Scale in the range of 3 to 100.
6. The process as claimed in claim 1 wherein the exfoliated material has an aspect ratio of greater than about 25.
7. The process as claimed in claim 1 wherein the exfoliated material has an aspect ratio of from 5 to 200.
8. The process as claimed in claim 1 wherein the exfoliated material has a size in the range of from 50 nm to 10 microns.
9. The process as claimed in claim 1 wherein the exfoliated material has a thickness of from 1 nm to 5 nm.
10. The process as claimed in claim 1 wherein the milling media is plastic material.
11. The process as claimed in claim 10 wherein the plastic is selected from the group consisting essentially of:
i. polymethylmethacrylate,
ii. polycarbonate,
iii. polystyrene,
iv. polypropylene,
v. polyethylene,
vi. polytetrafluoroethylene,
vii. polyethyleneimide,
viii. polyvinylchloride,
ix. polyamine-imide, and,
x. alloys of any of i. to ix.
12. The process as claimed in claim 2 wherein the particulate metals are selected from the group consisting essentially of:
i. silicon,
ii. tin,
iii. iron,
iv. magnesium,
v. manganese,
vi. aluminum,
vii. lead,
viii. gold,
ix. silver,
x. titanium,
xi. platinum,
xii. palladium,
xiii. ruthenium,
xiv. copper,
xv. nickel,
xvi. rhodium, and,
xvii. alloys of any of i. to xvi.
13. The process as claimed in claim 2 wherein the particulate metal oxides are selected from the group consisting essentially of oxides of:
i. silicon,
ii. tin,
iii. iron,
iv. magnesium,
v. manganese,
vi. aluminum,
vii. lead,
viii. gold,
ix. silver,
x. titanium,
xi. platinum,
xii. palladium,
xiii. ruthenium,
xiv. copper,
xv. nickel,
xvi. rhodium, and,
xvii. alloys of any of i. to xvi.
14. The process as claimed in claim 1 wherein the particulate non-layered material has a size less than 100 microns.
15. The process as claimed in claim 1 wherein the particulate are metal carbides.
16. The process as claimed in claim 1 wherein the particulate materials are metal nitrides.
17. A product when produced by the process of claim 1 .
18. An electrode produced from the product as claimed in claim 17 .
19. A catalyst produced from the product as claimed in claim 17 .
20. A coating produced from the product as claimed in claim 17 .
21. An electronic component manufactured from the product as claimed in claim 17 .
22. A thermally conductive component manufactured from the product as claimed in claim 17 .
23. A process of dry milling particulate materials, wherein at least one of the particulate materials is a layered material, in the presence of a particulate material selected from the group consisting of i. ceramic, ii. glass, and iii. quartz, to obtain a composition wherein the layered material is exfoliated and wherein the particulate material is coated with the exfoliated material, the exfoliated material having a particle size of 500 nanometers or less, and wherein the dry milling is controlled by controlling the surface energy of the milling media in addition to controlling the hardness of the milling media.
24. A process of dry milling particulate materials, wherein at least one of the particulate materials is a layered material, in the presence of a particulate material selected from the group consisting of i. ceramic, ii. glass, and iii. quartz, to obtain a composition wherein the layered material is exfoliated and wherein the particulate material is coated with the exfoliated material, the exfoliated material having a particle size of 10 microns or more, and the wherein the dry milling is controlled by controlling the surface energy of the milling media in addition to controlling the hardness of the milling media.
25. A composition of matter comprising particles composited with graphene wherein the particles are selected from the group consisting essentially of metal particles, and metal oxide particles, wherein the metal and metal oxide particles have a size of 100 microns or smaller.
26. A composition of matter as claimed in claim 25 wherein the metal and metal oxide particles have a size of 100 microns or less.
27. A composition of matter as claimed in claim 25 wherein the metal and metal oxide particles have a size of 10 microns or less.
28. A composition of matter as claimed in claim 25 wherein the metal and metal oxide particles have a size of 1 micron or less.
29. A composition of matter as claimed in claim 25 wherein the graphene is less than 5 nm thick.
30. A composition of matter as claimed in claim 25 wherein the graphene is a monolayer thick.
31. A composition of matter as claimed in claim 25 wherein the oxygen content of the graphene is ten atomic weight percent or less.
32. A composition of matter as claimed in claim 25 wherein the metal is selected from the group consisting essentially of iron, magnesium, cobalt, molybdenum, and lead.
33. A composition of matter as claimed in claim 25 wherein the metal oxide is selected from the group of oxides consisting essentially of iron oxide, magnesium oxide, cobalt oxide, molybdenum oxide, and lead oxide.
34. A composition of matter as claimed in claim 25 wherein the size of the graphene particle is less than 5 microns.
35. A composition of matter as claimed in claim 25 wherein the surface area of the graphene is greater than about 300 m2/g BET.
36. A composition of matter as claimed in claim 25 wherein the metal particles are larger than the graphene composited with them.
37. A composition of matter as claimed in claim 25 wherein the metal particle are essentially the same size as the graphene they are combined with.
38. A composition of matter as claimed in claim 25 that is a nanocomposite.
39. An electrode manufactured from the composition of claim 25 .
40. A battery comprising at least one electrode as claimed in claim 39 .
41. A capacitor comprising an electrode as claimed in claim 39 .
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JP6618800B2 (en) | 2019-12-11 |
TWI589524B (en) | 2017-07-01 |
CN104582855A (en) | 2015-04-29 |
JP2018134639A (en) | 2018-08-30 |
US20160256873A1 (en) | 2016-09-08 |
EP2849887A4 (en) | 2016-01-06 |
EP4404227A2 (en) | 2024-07-24 |
EP2849887B1 (en) | 2024-03-20 |
KR102107868B1 (en) | 2020-05-07 |
KR20150035536A (en) | 2015-04-06 |
TW201402458A (en) | 2014-01-16 |
US10232377B2 (en) | 2019-03-19 |
JP2015526264A (en) | 2015-09-10 |
EP4404227A3 (en) | 2024-08-21 |
EP2849887A1 (en) | 2015-03-25 |
WO2013173053A1 (en) | 2013-11-21 |
CN104582855B (en) | 2019-09-10 |
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