WO2015119716A1 - Compositions de nano-tribologie et procédés associés comprenant des nano-feuilles moléculaires - Google Patents

Compositions de nano-tribologie et procédés associés comprenant des nano-feuilles moléculaires Download PDF

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Publication number
WO2015119716A1
WO2015119716A1 PCT/US2014/071886 US2014071886W WO2015119716A1 WO 2015119716 A1 WO2015119716 A1 WO 2015119716A1 US 2014071886 W US2014071886 W US 2014071886W WO 2015119716 A1 WO2015119716 A1 WO 2015119716A1
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Prior art keywords
oil
nano
sheets
composition
nanoparticles
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PCT/US2014/071886
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English (en)
Inventor
Ajay P. Malshe
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Nanomech, Inc.
Priority date (The priority date 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 date listed.)
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Publication date
Priority claimed from US14/173,369 external-priority patent/US9718967B2/en
Application filed by Nanomech, Inc. filed Critical Nanomech, Inc.
Priority to CA2936897A priority Critical patent/CA2936897C/fr
Priority to EP14881721.6A priority patent/EP3102339A4/fr
Priority to BR112016017584A priority patent/BR112016017584A2/pt
Priority to MX2016009943A priority patent/MX2016009943A/es
Publication of WO2015119716A1 publication Critical patent/WO2015119716A1/fr
Priority to IL246518A priority patent/IL246518A0/en

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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/12—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by mechanical means
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
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    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C08K2003/382—Boron-containing compounds and nitrogen
    • C08K2003/385—Binary compounds of nitrogen with boron
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    • C08K3/042—Graphene or derivatives, e.g. graphene oxides
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    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
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    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/102—Aliphatic fractions
    • C10M2203/1025—Aliphatic fractions used as base material
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    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
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    • C10M2205/16—Paraffin waxes; Petrolatum, e.g. slack wax
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02—Hydroxy compounds
    • C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
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    • C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
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    • C10M2219/062—Thio-acids; Thiocyanates; Derivatives thereof having carbon-to-sulfur double bonds
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    • C10M2227/06—Organic compounds derived from inorganic acids or metal salts
    • C10M2227/061—Esters derived from boron

Definitions

  • This specification also relates to compositions and methods in the sub-field of nano-tribology and associated solid surface nano-engineering, nano- lubrication, and nano-wear.
  • Tribology refers to the science and engineering of solid surfaces. Tribology includes the study and application of surface chemistry and structure, friction, lubrication, corrosion, and wear. The tribological interactions of a solid surface with interfacing materials and the surrounding environment may result in the loss of material from the surface in processes generally referred to as "wear.” Major types of wear include abrasion, friction (adhesion and cohesion), erosion, and corrosion. Wear may be reduced by the use of lubricants and/or other anti-wear agents. Wear may also be reduced by modifying the surface properties of solids using one or more "surface engineering" processes (i.e., modifying the chemical and/or structural properties of solid surfaces).
  • a composition comprises a plurality of nanoparticles having open architecture, a plurality of multifunctional nano-sheets, and an organic medium intercalating the nanoparticles.
  • a method comprises contacting a surface with a composition.
  • the composition comprises a plurality of nanoparticles having open architecture and an organic medium intercalated in the nanoparticles.
  • the surface and the contacting composition are subjected to a frictional force.
  • Constituent layers of the nanoparticles are delaminated to form a plurality of multifunctional nano-sheets.
  • the nano- sheets deposit on the surface in a tribo-film.
  • Figure 1 is a diagram illustrating a method of producing nanoparticles
  • Figure 2 is a diagram illustrating one method of preparing nanoparticle based lubricants
  • Figure 3 shows transmission electron microscopy (TEM) micrographs of molybdenum disulfide particles;
  • Figure 3(A) shows molybdenum disulfide as it is available, typically from about a few microns to submicron size;
  • Figure 3(B) shows molybdenum disulfide that has been ball milled in air for 48 hours;
  • Figure 3(C) is a high resolution electron microscopy image that shows molybdenum disulfide that has been ball milled in air for 48 hours;
  • Figure 3(D) is a high-resolution transmission electron microscopy (HRTEM) image that shows molybdenum disulfide that has been ball milled in air for 48 hours followed by ball milling in oil for 48 hours;
  • HRTEM transmission electron microscopy
  • Figure 4 is a graph showing XRD spectra of molybdenum disulfide particles;
  • Figure 4(A) is the XRD spectra for molybdenum disulfide that has been ball milled in air for 48 hours followed by ball milling in oil for 48 hours;
  • Figure 4(B) is the XRD spectra for molybdenum disulfide that has been ball milled in air for 48 hours;
  • Figure 4(C) is the XRD spectra for molybdenum disulfide that has not been ball milled;
  • Figure 5 is a graph showing XPS spectra of molybdenum disulfide particles in which the carbon peak for molybdenum disulfide that has not been ball milled is shown, as well as the carbon peak for molybdenum disulfide that has been ball milled in air for 48 hours, followed by ball milling in oil for 48 hours;
  • Figure 6 shows graphs and bar charts depicting tribological test data for different additives in paraffin oil
  • Figure 6(A) shows the average wear scar diameter for a base oil (paraffin oil), paraffin oil with micron sized MoS 2 , paraffin oil with MoS 2 that was milled in air for 48 hours, and paraffin oil with MoS 2 that was milled in air for 48 hours followed by milling in canola oil for 48 hours
  • Figure 6(B) shows the load wear index for paraffin oil without a nanoparticle additive, paraffin oil with micron sized M0S2, paraffin oil with MoS 2 that was milled in air for 48 hours, and paraffin oil with M0S2 that was milled in air for 48 hours followed by milling in canola oil for 48 hours
  • Figure 6(C) shows the coefficient of friction for paraffin oil without a nanoparticle additive, paraffin oil with micron sized MoS 2 (c-MoS 2 ), paraffin oil with MoS 2 that was milled in air for 48 hours
  • Figure 7 is a TEM image showing the architecture of molybdenum disulfide nanoparticles (15-70 nm average size);
  • Figure 7(A) shows the close caged dense oval shaped architecture of molybdenum disulfide nanoparticles that have been ball milled in air for 48 hours;
  • Figure 7(B) shows the open ended oval shaped architecture of molybdenum disulfide nanoparticles that have been ball milled in air for 48 hours followed by ball milling in canola oil for 48 hours;
  • Figure 8 is a graph depicting a comparison of wear scar diameters for different additives in paraffin oil; one additive is crystalline molybdenum disulfide (c-MoS2); another is molybdenum disulfide nanoparticles that were ball milled in air (n-MoS2); another additive is molybdenum disulfide nanoparticles that were ball milled in air followed by ball milling in canola oil and to which a phospholipid emulsifier was added (n-MoS2+Emulsifier); and
  • c-MoS2 crystalline molybdenum disulfide
  • n-MoS2 molybdenum disulfide nanoparticles that were ball milled in air
  • n-MoS2+Emulsifier molybdenum disulfide nanoparticles that were ball milled in air followed by ball milling in canola oil and to which a phospholipid emulsifier was added
  • Figure 9 shows photographs and graphs produced using energy dispersive x-ray analysis (EDS) depicting the chemical analysis of wear scar diameters in four-ball tribological testing for nanoparticle based lubricants;
  • EDS energy dispersive x-ray analysis
  • Figure 9(A) shows paraffin oil without any nanoparticle composition additive;
  • Figure 9(B) shows paraffin oil with molybdenum disulfide nanoparticles that have been ball milled in air for 48 hours followed by ball milling in oil for 48 hours and treated with a phospholipid emulsifier.
  • Figures 10(A) and 10(B) show schematic diagrams of the crystal structure of molybdenum disulfide.
  • Figure 11 shows a schematic diagram of the crystal structure of hexagonal boron nitride.
  • any numerical range recited in this specification is intended to include all subranges of the same numerical precision subsumed within the recited range.
  • a range of "1.0 to 10.0" is intended to include all sub-ranges between (and including) the recited minimum value of 1.0 and the recited maximum value of 10.0, that is, having a minimum value equal to or greater than 1.0 and a maximum value equal to or less than 10.0, such as, for example, 2.4 to 7.6.
  • Any maximum numerical limitation recited in this specification is intended to include all lower numerical limitations subsumed therein and any minimum numerical limitation recited in this specification is intended to include all higher numerical limitations subsumed therein.
  • compositions and methods described in this specification may comprise, among other components, nanoparticles and/or nano-sheets.
  • the nanoparticles may comprise a transition metal chalcogenide compound, including sulfides, selenides, and tellurides or one or more element such as, for example, titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, molybdenum, or tungsten.
  • a transition metal chalcogenide compound including sulfides, selenides, and tellurides or one or more element such as, for example, titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, molybdenum, or tungsten.
  • the nanoparticles may comprise a chalcogenide material such as, for example, molybdenum disulfide, tungsten disulfide, niobium diselenide, and/or other materials such as, for example, hexagonal boron nitride, graphite, metals such as copper or silver, inorganic compounds such as calcium carbonate, polymers such as polytetrafluoroethylene (PTFE), or dithiophosphate compounds.
  • a chalcogenide material such as, for example, molybdenum disulfide, tungsten disulfide, niobium diselenide, and/or other materials such as, for example, hexagonal boron nitride, graphite, metals such as copper or silver, inorganic compounds such as calcium carbonate, polymers such as polytetrafluoroethylene (PTFE), or dithiophosphate compounds.
  • a chalcogenide material such as, for example, molybdenum disulfide
  • compositions described in this specification may therefore comprise, among others, molybdenum disulfide nanoparticles, tungsten disulfide nanoparticles, niobium diselenide nanoparticles, hexagonal boron nitride nanoparticles, graphite nanoparticles, copper nanoparticles, silver nanoparticles, calcium carbonate nanoparticles, PTFE nanoparticles, nanoparticles of dithiophosphate compounds, or combinations of any thereof .
  • the nanoparticles may have an open architecture.
  • open architecture or “open-ended architecture” refers to the morphology of particles comprising fissures, separations, or other discontinuities in the particles' outer surfaces which provide openings to the internal portions of the individual particles.
  • open architecture or “open-ended architecture” refer to the morphology of the layered particles comprising inter- layer defects (e.g., shearing, buckling, folding, curling, and dislocating of constituent molecular layers) at the surface of the particles, which increase the inter-planar spacing between groupings of molecular layers, thereby providing fissures, separations, or other discontinuities in the particles' outer surfaces and openings to the internal portions of the particles.
  • inter- layer defects e.g., shearing, buckling, folding, curling, and dislocating of constituent molecular layers
  • layered particles refers to particles comprising generally parallel stacked molecular layers, wherein the inter-layer bonding comprises relatively weak bonding such van der Waals bonding, and wherein the intra-layer bonding comprises relatively strong bonding such as covalent bonding.
  • layered particles include, but are not limited to, graphite particles, molybdenum disulfide particles, tungsten disulfide particles, niobium diselenide particles, and hexagonal boron nitride particles. It is understood that the terms “open architecture” and “open-ended architecture” exclude particle morphologies such as nano- tubes and fullerenes, which are characterized by closed particle surfaces lacking fissures, separations, or other discontinuities in the particles' outer surfaces.
  • compositions described in this specification may also comprise an organic medium encapsulating/coatmg the nanoparticles and/or intercalated in the nanoparticles.
  • an organic medium may be integrated into the internal portions of individual nanoparticles by intercalating into the spaces formed by the fissures, separations, or other discontinuities in the outer surfaces of nanoparticles having an open architecture.
  • the nanoparticles may be intercalated and encapsulated/coated with an organic medium.
  • the nanoparticles may have an average primary particle size of less than or equal to 1000 nanometers, and in some embodiments, less than or equal to 500 nanometers, less than or equal to 400 nanometers, less than or equal to 300 nanometers, less than or equal to 200 nanometers, less than or equal to 100 nanometers, less than or equal to 75 nanometers, less than or equal to 50 nanometers, or less than or equal to 25 nanometers.
  • the term "average primary particle size” refers to a particle size as determined by visually examining a microscopy image of a sample of particles, measuring the largest length dimension of the individual particles in the image ⁇ i.e., the diameters of the smallest spheres that completely surround the individual particles in the image), and calculating the average of the length dimensions (diameters) based on the magnification of the image.
  • a microscopy image e.g., light microscopy, transmission electron microscopy, and the like
  • the average primary particle size of constituent particles or a subset of the constituent particles based on like particle composition
  • the term "average primary particle size” refers the size of individual particles as opposed to agglomerations of two or more individual particles.
  • compositions and methods described in this specification may comprise, among other components, nanoparticles and/or nano-sheets.
  • nano-sheets refers to planar-shaped particles having a thickness dimension of less than 500 nanometers and an aspect ratio (defined as the ratio of the largest length/width dimension to the thickness dimension) of at least 2.
  • nano-sheets may have a thickness dimension of less than 100 nanometers and an aspect ratio of at least 10.
  • Nano-sheets may have a thickness dimension of less than 50 nanometers and an aspect ratio of at least 20.
  • Nano-sheets may have a thickness dimension of less than 25 nanometers and an aspect ratio of at least 40.
  • Nano- sheets may have a thickness dimension of less than 10 nanometers and an aspect ratio of at least 100. Nano-sheets may have a thickness dimension corresponding to approximately one unit cell dimension and such nano-sheets may be referred to as molecular nano-sheets. Nano- sheets may have length and width dimensions of less than 1000 nanometers. [0030] Molecular nano-sheets are a sub-genus of nano-sheets in which the thickness dimensions of the nano-sheets correspond to approximately one unit cell dimension. Molecular nano-sheets may be, but are not necessarily, crystalline molecular structures. In some embodiments, molecular nano-sheets may have length and width dimensions of less than or equal to 1000 nanometers, 500 nanometers, or 100 nanometers.
  • molecular nano-sheets may have a thickness dimension corresponding to approximately one unit cell dimension.
  • a molecular nano-sheet may comprise a single layer of any layered nanoparticle (e.g., a graphite/graphene molecular nano-sheet, a molybdenum disulfide molecular nano-sheet, a tungsten disulfide molecular nano-sheet, a niobium diselenide molecular nano-sheet, or a hexagonal boron nitride molecular nano- sheet).
  • any layered nanoparticle e.g., a graphite/graphene molecular nano-sheet, a molybdenum disulfide molecular nano-sheet, a tungsten disulfide molecular nano-sheet, a niobium diselenide molecular nano-sheet, or a hexagonal boron nitride molecular nano- sheet.
  • a unit cell is the smallest molecular unit that a crystal can be divided into using crystallographic symmetry operations.
  • a unit cell is the simplest repeating unit in a crystalline material.
  • Unit cells stacked in three- dimensional space describe the bulk arrangement of atoms of a crystalline material.
  • molybdenum disulfide predominantly exists in a hexagonal crystal form characterized by MoS 2 layers in which the molybdenum atoms have trigonal prismatic coordination of six sulfur atoms with two molecules per unit cell.
  • the molybdenum disulfide crystal structure comprises a tri-layer having one planar hexagonal layer of molybdenum atoms interspersed between two planar layers of sulfur atoms forming an intra-molecular covalently bonded S-Mo-S molecular layer.
  • Bulk molybdenum disulfide comprises relatively weak inter-molecular van der Waals bonds between the adjacent sulfur atoms of stacked S-Mo-S molecular layers.
  • FIG. 10(A) two intra-molecular covalently bonded S-Mo-S molecular layers 10 are shown with inter-molecular van der Waals bonds 17 between the adjacent sulfur atoms 1 1 of the two stacked S-Mo-S molecular layers 10.
  • the molybdenum atoms 13 and the sulfur atoms 1 1 form the tri-layer comprising one planar hexagonal layer of molybdenum atoms 13 interspersed between two planar layers of sulfur atoms 11 and forming covalent bonds 15.
  • a molybdenum disulfide molecular nano-sheet may comprise a molybdenum disulfide crystal having a thickness dimension corresponding to the thickness of the covalently bonded S-Mo-S molecular layer (without adjoining inter-molecular van der Waals bonded layers, i.e., approximately 3.241 angstroms) and, in some embodiments, length and width dimensions of less than or equal to 1000 nanometers.
  • a tungsten disulfide molecular nano-sheet may comprise a tungsten disulfide crystal having a thickness dimension corresponding to the thickness of the covalently bonded S-W-S molecular layer (without adjoining inter-molecular van der Waals bonded layers) and, in some embodiments, length and width dimensions of less than or equal to 1000 nanometers.
  • the crystal structure of hexagonal boron nitride is characterized by hexagonal coordination between three nitrogen atoms and three boron atoms forming adjacent six-sided rings that form intra-molecular covalently-bonded mono-layers that are atomically thin (i.e., having a thickness dimension of a single atom).
  • three intra-molecular covalently bonded B-N molecular layers 20 are shown with inter-molecular van der Waals bonds 27 between the adjacent B-N molecular layers 20.
  • the boron atoms 23 and the nitrogen atoms 21 form the mono-layer comprising the hexagonal atomic orientation within a single plane and forming the covalent bonds 25.
  • the hexagonal boron nitride crystal structure comprises B-N molecular mono-layers
  • bulk hexagonal boron nitride comprises relatively weak inter-molecular van der Waals bonds between the adjacent B-N molecular mono-layers. Therefore, a hexagonal boron nitride molecular nano-sheet may comprise a hexagonal boron nitride crystal having a single atomic thickness dimension and, in some embodiments, length and width dimensions of less than or equal to 1000 nanometers.
  • a graphite molecular nano-sheet may comprise a graphene crystal having a single atomic thickness dimension and, in some embodiments, length and width dimensions of less than or equal to 1000 nanometers.
  • nano-sheets may comprise a material such as, for example, molybdenum disulfide, tungsten disulfide, niobium diselenide, hexagonal boron nitride, graphite/graphene, metals such as copper or silver, inorganic compounds such as calcium carbonate, polymers such as PTFE, or dithiophosphate compounds.
  • the nano-sheets may comprise molecular nano-sheets comprising a material such as, for example, molybdenum disulfide, tungsten disulfide, niobium diselenide, hexagonal boron nitride, or graphene.
  • compositions described in this specification may comprise molybdenum disulfide nano-sheets, tungsten disulfide nano-sheets, niobium diselenide nano- sheets, hexagonal boron nitride nano-sheets, graphite nano-sheets, graphene molecular nano- sheets, metal (e.g., copper) nano-sheets, inorganic compound (e.g., calcium carbonate) nano- sheets, polymer (e.g., PTFE) nano-sheets, nano-sheets comprising dithiophosphate compounds, or combinations of any thereof.
  • metal e.g., copper
  • inorganic compound e.g., calcium carbonate
  • polymer e.g., PTFE
  • layered materials such as, for example, molybdenum disulfide, tungsten disulfide, niobium diselenide, hexagonal boron nitride, and graphite, may form nano-sheets (e.g., planar-shaped particles having a thickness dimension of less than 500 nanometers and an aspect ratio of at least 2) or molecular nano-sheets (e.g., crystalline molecular structures comprising a thickness dimension corresponding to approximately one unit cell dimension).
  • nano-sheets e.g., planar-shaped particles having a thickness dimension of less than 500 nanometers and an aspect ratio of at least 2
  • molecular nano-sheets e.g., crystalline molecular structures comprising a thickness dimension corresponding to approximately one unit cell dimension.
  • molecular nano-sheets are a subgenus of nano-sheets.
  • the nano-sheets may be functionalized.
  • the nano-sheets may be functionalized with organic molecules or functional groups, inorganic molecules or functional groups, or both organic and inorganic molecules or functional groups, forming functionalized nano-sheets.
  • the nano-sheets may be functionalized with catalysts, antioxidants, anti-corrosion agents, biocidal agents, or combinations of any thereof.
  • antioxidants examples include, but are not limited to, antioxidants selected from the group consisting of hindered phenols, alkylated phenols, alkyl amines, aryl amines, 2,6-di-tert-butyl-4-methylphenol, 4,4'-di-tert- octyldiphenylamine, tert-butyl hydroquinone, tris(2,4-di-tert-butylphenyl)phosphate, phosphites, thioesters, or combinations of any thereof; anticorrosion agents selected from the group consisting of alkaline earth metal bisalkylphenolsulphonates, dithiophosphates, alkenylsuccinic acid half-amides, or combinations thereof; and biocidal agents material selected from the group consisting of alkyl benzothiazole, hydroxylamine benzothiazole, an amine salt of an alkyl succinic acid, an amine salt of an
  • the nano-sheets may be functionalized with a dispersant agent.
  • Suitable dispersant agents may comprise at least one material selected from the group consisting of amide compounds, borate compounds, and boride compounds.
  • a dispersant agent may comprise at least one of succinimide and disodium octaborate tetrahydrate.
  • the nano-sheets may be coated and/or encapsulated with an organic medium.
  • an organic medium may be chemically or physically adsorbed onto nano-sheets or otherwise chemically or physically bonded to nano-sheets.
  • nanoparticles may be encapsulated and/or intercalated with an organic medium.
  • organic medium refers to hydrophobic/oleophilic substances and carbon-based compounds.
  • the organic medium may comprise at least one material selected from the group consisting of oil media, grease media, alcohol media, composite oils, mineral oils, synthetic oils, canola oil, vegetable oil, soybean oil, corn oil, rapeseed oil, ethyl and methyl esters of rapeseed oil, monoglycerides, distilled monoglycerides, diglycerides, acetic acid esters of monoglycerides, organic acid esters of monoglycerides, sorbitan, sorbitan esters of fatty acids, propylene glycol esters of fatty acids, polyglycerol esters of fatty acids, hydrocarbon oils, n-hexadecane, phospholipids, lecithins, amide compounds, boron-containing compounds, dithiophosphate compounds, and combinations of any thereof.
  • suitable dithiophosphate compounds that may comprise an organic medium include, but are not limited to, zinc dialkyl dithiophosphate (ZDDP) and molybdenum dithiophosphate (MoDTP), which may be used alone or in combination with any other organic medium such as an oil medium.
  • the organic medium may comprise an oil medium such as, for example, a composite oil, a mineral oil, a synthetic oil, canola oil, a vegetable oil, soybean oil, corn oil, a hydrocarbon oil, a mineral oil, or combinations of any thereof.
  • compositions described in this specification may also comprise a secondary or tertiary particulate material such as, for example, polytetrafluoroethylene; soft metals such as gold, platinum, silver, lead, nickel, copper; cerium fluoride; zinc oxide; silver sulfate; cadmium iodide; lead iodide; barium fluoride; tin sulfide; zinc phosphate; zinc sulfide; mica; boron nitrate; borax; fluorinated carbon; zinc phosphide; boron; or combinations of any thereof.
  • the secondary or tertiary particulate material may comprise nanoparticles.
  • the secondary or tertiary nanoparticles may have an average primary particle size of less than or equal to 1000 nanometers, and in some embodiments, less than or equal to 500 nanometers, less than or equal to 400 nanometers, less than or equal to 300 nanometers, less than or equal to 200 nanometers, less than or equal to 100 nanometers, less than or equal to 75 nanometers, less than or equal to 50 nanometers, or less than or equal to 25 nanometers.
  • compositions described in this specification may also comprise a base lubricant material, which may be different than the organic medium described above.
  • the nanoparticles and/or nano-sheets may be dispersed in the base lubricant material.
  • the base lubricant material may comprise a material such as, for example, an oil, a grease, a polymer, a plastic, a gel, a wax, a silicone, a hydrocarbon oil, a vegetable oil, corn oil, peanut oil, canola oil, soybean oil, a mineral oil, a paraffin oil, a synthetic oil, a petroleum gel, a petroleum grease, a hydrocarbon gel, a hydrocarbon grease, a lithium based grease, a fluoroether based grease, ethylenebistearamide, or combinations of any thereof.
  • a material such as, for example, an oil, a grease, a polymer, a plastic, a gel, a wax, a silicone, a hydrocarbon oil, a vegetable oil, corn oil, peanut oil, canola oil, soybean oil, a mineral oil, a paraffin oil, a synthetic oil, a petroleum gel, a petroleum grease, a hydrocarbon gel, a hydrocarbon grease, a lithium based grease, a fluoroether
  • the base lubricant material may comprise at least one material selected from the group consisting of an oil, a grease, a plastic, a gel, a wax, a silicone, and combinations of any thereof.
  • the base lubricant material may comprise an oil or a grease.
  • the base lubricant material may comprise at least one material selected from the group consisting of a mineral oil, a paraffin oil, a synthetic oil, a petroleum grease, a hydrocarbon grease, a lithium based grease, or combinations of any thereof.
  • the compositions described in this specification may also comprise an emulsifier.
  • the emulsifier may comprise at least one material selected from the group consisting of lecithins, phospholipids, soy lecithins, detergents, distilled monoglycerides, monoglycerides, diglycerides, acetic acid esters of monoglycerides, organic acid esters of monoglycerides, sorbitan esters of fatty acids, propylene glycol esters of fatty acids, polyglycerol esters of fatty acids, compounds containing phosphorous, compounds containing sulfur, compounds containing nitrogen, or combinations of any thereof.
  • the emulsifier may comprise a compound containing phosphorous.
  • the emulsifier may comprise a phospholipid. In various embodiments, the emulsifier may comprise a lecithin. [0046] In various embodiments, the compositions described in this specification may also comprise one or more of an antioxidant, an anticorrosion agent, or a biocidal that is not bonded to or adsorbed to the surfaces of nano-sheets.
  • compositions may comprise at least one antioxidant material selected from the group consisting of hindered phenols, alkylated phenols, alkyl amines, aryl amines, 2,6-di-tert-butyl-4-methylphenol, 4,4'- di-tert-octyldiphenylamine, tert-butyl hydroquinone, tris(2,4-di-tert-butylphenyl)phosphate, phosphites, thioesters, or combinations of any thereof.
  • antioxidant material selected from the group consisting of hindered phenols, alkylated phenols, alkyl amines, aryl amines, 2,6-di-tert-butyl-4-methylphenol, 4,4'- di-tert-octyldiphenylamine, tert-butyl hydroquinone, tris(2,4-di-tert-butylphenyl)phosphate, phosphites, thio
  • compositions may comprise at least one anticorrosion agent selected from the group consisting of alkaline earth metal bisalkylphenolsulphonates, dithiophosphates, alkenylsuccinic acid half-amides, or combinations thereof.
  • the compositions may comprise at least one biocidal material selected from the group consisting of alkyl benzothiazole, hydroxylamine benzothiazole, an amine salt of an alkyl succinic acid, an amine salt of an alkenyl succinic acid, a partial alkyl ester of an alkyl succinic acid, a partial alkyl ester of an alkenyl succinic acid, or combinations of any thereof.
  • compositions described in this specification may be used to formulate a lubricant.
  • compositions comprising nanoparticles and/or nano-sheets may be used as performance-enhancing additives to off-the-shelf liquid based lubricants.
  • lubricant compositions may comprise nanoparticles and/or nano-sheets dispersed in a lubricant base material as described above, wherein a separate organic medium is intercalated in the nanoparticles, encapsulates the nanoparticles, and/or encapsulates the nano-sheets.
  • Lubricant compositions comprising nanoparticles and/or nano-sheets, with or without an intercalating and/or encapsulating organic medium, in accordance with the embodiments described in this specification, will provide a synergistically enhanced combination of lubrication in mechanical systems.
  • compositions described in this specification may be used to formulate a coating or solid film on a substrate or surface.
  • compositions comprising nanoparticles and/or nano-sheets, with or without an intercalating and/or encapsulating organic medium may be physically rubbed onto substrates and surfaces to form burnished films and coatings.
  • compositions comprising nanoparticles and/or nano-sheets, with or without an intercalating and/or encapsulating organic medium may also be deposited as solid films and coatings using pneumatic methods analogous to sandblasting.
  • compositions comprising nanoparticles and/or nano-sheets, with or without an intercalating and/or encapsulating organic medium, may also be added to thermoplastic or thermosetting resinous binders to make film-forming coating compositions (e.g., binders based on epoxy, urethane, urea, acrylic, phenolic, amide- imide, polyimide, azole, and like chemical systems).
  • thermoplastic or thermosetting resinous binders e.g., binders based on epoxy, urethane, urea, acrylic, phenolic, amide- imide, polyimide, azole, and like chemical systems).
  • compositions comprising nanoparticles and/or nano-sheets, with or without an intercalating and/or encapsulating organic medium, may be used in a method to lubricate a surface and/or deliver active materials and agents to the surface, including catalysts, anti-corrosion agents, antioxidants, biocidal agents, and other functional groups and molecules.
  • the method may comprise applying the compositions described in this specification to the surface or otherwise contacting the surface with the compositions.
  • the surface and the applied/contacting composition are subjected to a frictional force, pressure, or other mechanical stress, which causes constituent layers of the nanoparticles to delaminate and form a plurality of nano-sheets.
  • nano-sheets may be formed in situ on a surface as the force/pressure exfoliates the constituent molecular layers of nanoparticles having an open architecture.
  • the compositions may comprise an organic medium and the organic medium coats or encapsulates the nano-sheets formed in situ.
  • the coated or encapsulated nano-sheets formed in situ may deposit on the surface in a tribo-film.
  • compositions described in this specification may be made from solid lubricant starting or feed materials.
  • solid lubricants may include, but are not limited to, layered materials such as, for example, hexagonal boron nitride and chalcogenides, like molybdenum disulfide, tungsten disulfide, niobium diselenide, or a combination thereof.
  • layered materials such as, for example, hexagonal boron nitride and chalcogenides, like molybdenum disulfide, tungsten disulfide, niobium diselenide, or a combination thereof.
  • Other suitable layered materials include graphite.
  • solid lubricant starting or feed materials that may be used alone or in combination with the layered materials include, but are not limited to polytetrafluoroethylene, soft metals (such as, for example, silver, lead, nickel, copper), cerium fluoride, zinc oxide, silver sulfate, cadmium iodide, lead iodide, barium fluoride, tin sulfide, zinc phosphate, zinc sulfide, mica, boron nitrate, borax, fiuorinated carbon, zinc phosphide, boron, or a combination thereof.
  • Fiuorinated carbons may be, without limitation, carbon-based materials such as graphite which has been fiuorinated to improve its aesthetic characteristics.
  • Such materials may include, for example, a material such as CF X wherein x ranges from about 0.05 to about 1.2. Such a material is produced, for example, by Allied Chemical under the trade name Accufluor.
  • the methods of making the nanoparticles encapsulated and/or intercalated with the organic medium, and the nano-sheets may include, for example, the milling of a solid lubricant feed material.
  • the solid lubricant feed material may be capable of being milled to particles comprising an average primary particle size of about 1000 nanometers or less (submicron size), for example, from about 500 nanometers to about 10 nanometers.
  • the particles may have an average primary particle size of less than or equal to about 500 nanometers, less than or equal to about 100 nanometers, less than or equal to about 75 nanometers, and less than or equal to about 50 nanometers.
  • the milling may result in milled lubricant particles comprising a mixture, the mixture comprising particles having an average primary particle size of less than or equal to about 500 nanometers, plus larger particles. Additionally, the milling may result in milled nano-sheets in combination with nanoparticles.
  • the milling may include, among other techniques, ball milling and chemo- mechanical milling.
  • ball milling may include dry ball milling, wet ball milling, and combinations thereof.
  • Ball milling may refer to an impaction process that may include two interacting objects where one object may be a ball, a rod, 4 pointed pins (jack shape), or other shapes.
  • Chemo-mechanical milling may refer to an impaction process that may form an integrated complex between the organic medium and the nanoparticles, and between the organic medium and the nano-sheets.
  • the organic medium may coat, encapsulate, and/or intercalate the nanoparticles, and coat and/or encapsulate the nano-sheets.
  • chemo-mechanical milling may be performed using a ball milling technique.
  • the solid lubricant feed material may be dry milled and then wet milled.
  • An emulsifier may be mixed with a lubricant base material and added to the wet milled particles.
  • Diy milling may refer to particles that have been milled in the presence of a vacuum, a gas, or a combination thereof.
  • Wet milling may refer to particles that have been milled in the presence of a liquid.
  • the lubricant nanoparticle composition may further comprise an organic medium.
  • organic media include, but are not limited to, oil media, grease media, alcohol media, or combinations thereof.
  • Specific examples of organic media include, but are not limited to, composite oil, canola oil, vegetable oils, soybean oil, corn oil, ethyl and methyl esters of rapeseed oil, distilled monoglycerides, monoglycerides, diglycendes, acetic acid esters of monoglycerides, organic acid esters of monoglycerides, sorbitan, sorbitan esters of fatty acids, propylene glycol esters of fatty acids, polyglycerol esters of fatty acids, n-hexadecane, hydrocarbon oils, phospholipids, or a combination thereof. Many of these organic media may be environmentally acceptable.
  • compositions described in this specification may contain emulsifiers, surfactants, or dispersants.
  • emulsifiers may include, but are not limited to, emulsifiers having a hydrophilic-lipophilic balance (HLB) from about 2 to about 7; a HLB from about 3 to about 5; or a HLB of about 4.
  • HLB hydrophilic-lipophilic balance
  • emulsifiers may include, but are not limited to, lecithins, soy lecithins, phospholipid lecithins, detergents, distilled monoglycerides, monoglycerides, diglycerides, acetic acid esters of monoglycerides, organic acid esters of monoglycerides, sorbitan esters of fatty acids, propylene glycol esters of fatty acids, polyglycerol esters of fatty acids, compounds containing phosphorous, compounds containing sulfur, compounds containing nitrogen, or a combination thereof.
  • surfactants examples include, but are not limited to, 2-alkyl-succinic acid 1 -propyl ester, canola oil, dialkyl hydrogen phosphite, glycerol mono oleate, lecithin, octadecylamine, oleic acid, oleylamide, oleylamine, poly(methyl methacrylate), sodium stearate, Span 80, stearic acid, thiocarbamates (molybdenum dithiocarbamate or MoDTC), thiophosphates (molybdenum dithiophosphate or MoDTP, zinc dialkyl dithiophosphate or ZDDP), trioctylphosphine oxide, Tween 20, or combinations of any thereof.
  • dispersants examples include, but are not limited to, polyisobutylene succinimides (PIBS), succinic anhydrides, PIBS anhydrides, succiniate esters, metal sulfonates, polymeric detergents, polymeric dispersants, polyoxyethylene alkyl ethers, polyoxyethylene dialkylphenol ethers, polyalphaolefins (PAO), alkylglycoside, polyoxyethylene fatty acid esters, sucrose fatty acid esters, sorbitan fatty acid esters, polyoxyethylene sorbitan fatty acid esters, borate esters, phosphate esters, phosphate amines, fatty acid alkanolamide, and combinations thereof.
  • PIBS polyisobutylene succinimides
  • succinic anhydrides examples include, but are not limited to, succinic anhydrides, PIBS anhydrides, succiniate esters, metal sulfonates, polymeric detergents, polymeric dispersants, polyoxyethylene alkyl
  • amine-containing dispersants such as, for example, phosphate amines
  • a method of making a composition such as, for example, a lubricant additive or a primary lubricant formulation, is described. The composition may be used as an additive dispersed in a lubricant base material or as a component of a primary lubricant formulation.
  • lubricant base materials may include, but are not limited to, oils, greases, plastics, gels, sprays, or a combination thereof.
  • bases may include, but are not limited to, hydrocarbon oils, vegetable oils, corn oil, peanut oil, canola oil, soybean oil, mineral oil, paraffin oils, synthetic oils, petroleum gels, petroleum greases, hydrocarbon gels, hydrocarbon greases, lithium based greases, fluoroether based greases, ethylenebistearamide, waxes, silicones, or a combination thereof.
  • Described in this specification is a method of lubricating or coating an object that is part of an end application with a composition comprising nanoparticles and/or nano-sheets, with or without an intercalating and/or encapsulating organic medium. Further described is a method of lubricating an object by employing nanoparticles and/or nano-sheets, with or without an intercalating and/or encapsulating organic medium, as a delivery mechanism.
  • Figure 1 illustrates a method of preparing nanoparticle based lubricants or compositions.
  • a solid lubricant feed is introduced via line 210 to a ball milling processor 215. Ball milling is carried out in the processor 215 and the solid lubricant feed is milled to comprise particles having an average primary particle size of less than or equal to about 1000 nanometers, less than or equal to about 500 nanometers, less than or equal to about 100 nanometers, less than or equal to about 80 nanometers, or less than or equal to about 50 nanometers.
  • the ball milling may result in milled lubricant particles comprising a mixture, the mixture comprising particles having an average particle dimension of less than or equal to about 1000 nanometers or less than or equal to about 500 nanometers, plus larger particles.
  • the ball milling may be high energy ball milling, medium energy ball milling, or combinations thereof. Additionally, in various embodiments the ball milling may be carried out in a vacuum, in the presence of a gas, in the presence of a liquid, in the presence of a second solid, or combinations thereof.
  • the nanoparticle composition may be removed from the processor via line 220.
  • the nanoparticle composition may be a nanoparticle based lubricant.
  • the ball milling may comprise a first ball milling and at least one more subsequent ball millings, or ball milling and/or other processing as appropriate.
  • the ball milling may comprise dry milling followed by wet milling.
  • Figure 2 illustrates a further method 100 of preparing nanoparticle based lubricants and other compositions where dry milling is followed by wet milling.
  • Feed 110 introduces a solid lubricant feed into a ball milling processor 115 where dry ball milling, such as in a vacuum or in air, reduces the solid lubricant feed to particles having an average dimension of the size described above.
  • Line 120 carries the dry milled particles to a wet milling processor 125.
  • the dry milled particles are combined with a composite oil or an organic medium prior to entering the wet milling processor 125.
  • the organic medium and dry milled particles may be combined in the wet milling processor 125.
  • the dry milling and wet milling may be carried out in a single processor where the organic medium is supplied to the single processor for wet milling after initially carrying out dry milling.
  • the balls in the ball milling apparatus may be coated with the organic medium to incorporate the organic medium in the nanoparticles and/or onto the nano-sheets.
  • line 130 carries the wet milled particles to a container 135, which may be a sonication device.
  • line 130 may carry a mixture comprising nanoparticles and/or nano-sheets, organic medium, and a complex comprising nanoparticles combined with an organic medium and/or nano-sheets combined with an organic medium.
  • a lubricant base material may be fed to the container 135 via line 150.
  • the base may be supplied to the wet milling processor 125 and the mixing, which may include sonicating, may be carried out in the wet milling processor 125.
  • the lubricant nanoparticle and/or nano-sheet composition may be employed as an additive and dispersed in the lubricant base material.
  • a lubricant base material may be paired with a lubricant nanoparticle and/or nano-sheet composition according to the ability of the base material and the lubricant nanoparticle and/or nano-sheet composition to blend appropriately. In such cases the lubricant nanoparticle and/or nano-sheet composition may enhance the performance characteristics of the base.
  • an emulsifier may be mixed with the lubricant base material. Emulsifiers may further enhance dispersion of the lubricant nanoparticle and/or nano-sheet composition in the lubricant base material. The emulsifier may be selected to enhance the dispersion stability of a nanoparticle or nano-sheet composition in a base. An emulsifier may also be supplied to the container 135 via line 140. In some embodiments, the emulsifier and base are combined in the container 135 prior to introduction of the wet milled particles.
  • Prior mixing of the emulsifier with the base material may enhance dispersion upon addition of nanoparticles, nano-sheets, and/or complexes thereof with an organic medium, by homogeneously dispersing the nanoparticles/nano-sheets/ complexes.
  • the mixing of the emulsifier and base may comprise sonicating.
  • the emulsifier may be supplied to the wet milling processor 125 and the mixing, which may include sonicating, may be carried out in the wet milling processor 125.
  • the lubricant removed from the container 135 via line 120 may be a blend comprising the wet milled particles, organic medium, and base.
  • the blend may further comprise an emulsifier.
  • antioxidants or anticorrosion agents may be milled with the nanoparticles and/or nano-sheets or added to prior-milled nanoparticles and/or nano- sheets.
  • antioxidants include, but are not limited to, hindered phenols, alkylated phenols, alkyl amines, aryl amines, 2,6-di-tert-butyl-4-methylphenol, 4,4'-di-tert- octyldiphenylamine, tert-Butyl hydroquinone, tris(2,4-di-tert-butylphenyl)phosphate, phosphites, thioesters, or combinations of any thereof.
  • anticorrosion agents include, but are not limited to, alkaline-earth metal bisalkylphenolsulphonates, dithiophosphates, alkenylsuccinic acid half-amides, or combinations of any thereof.
  • biocidals may be milled with the nanoparticles and/or nano-sheets or added to prior-milled nanoparticles and/or nano-sheets.
  • biocidals may include, but are not limited to, alkyl or hydroxylamine benzotriazole, an amine salt of a partial alkyl ester of an alkyl, alkenyl succinic acid, or a combination thereof.
  • further processing of wet milled nanoparticles and/or nano-sheets may comprise removal of oils that are not a part of a complex with the lubricant particles or nano-sheets.
  • Such methods may be suitable for applications that benefit from use of dry particles and sheets of lubricant, such as coating applications.
  • Oil and/or other liquids can be removed from wet milled nanoparticles and/or nano-sheets to produce substantially dry lubricant particles, sheets, and complexes having intercalated and/or encapsulated organic media.
  • Such wet milling followed by drying may produce a lubricant with reduced tendency to agglomerate.
  • an agent such as acetone or other suitable solvent, may be added that dissolves oils that are not a part of a complex with the nanoparticles or nano-sheets, followed by a drying process such as supercritical drying, to produce a substantially dry lubricant comprising particles or sheets treated by milling in an organic medium.
  • Ball milling conditions may vary and, in particular, conditions such as temperature, milling time, and size and materials of the balls and vials may be manipulated.
  • ball milling may be carried out from about 12 hours to about 50 hours, from about 36 hours to about 50 hours, from about 40 hours to about 50 hours, or for about 48 hours ( ⁇ 1 hour, + 2 hours, or ⁇ 3 hours).
  • Ball milling may be conducted at room temperature or elevated temperatures.
  • the benefits of increasing milling time may comprise at least one of increasing the time for the organic medium and nanoparticles to interact, integrate, and complex; and producing finer sizes, better yield of nanoparticles, more uniform shapes, and more passive surfaces.
  • An example of ball milling equipment suitable for carrying out the described milling includes the SPEX CertiPrep model 8000D, along with hardened stainless steel vials and hardened stainless steel grinding balls, but any type of ball milling apparatus may be used.
  • a stress of 600-650 MPa, a load of 14.9 N, and a strain of IO- O -4 per second may be used.
  • a hybrid milling process may produce a mixture of both nanoparticles encapsulated and/or intercalated with an organic medium and nano-sheets coated and/or encapsulated with an organic medium.
  • the hybrid milling process may produce combinations of nanoparticles and nano-sheets that are functionalized, for example, with catalysts, antioxidants, anti-corrosion agents, biocidals, or combinations of any thereof.
  • the proportions of the components in a nanoparticle and/or nano-sheet based lubricant or other composition may contribute to performance of the composition, such as the composition's dispersion stability and ability to resist agglomeration.
  • suitable starting ratios of solid lubricant feed particles to organic medium may be about 1 part particles to about 4 parts organic medium by weight, about 1 part particles to about 3 parts organic medium by weight, about 3 parts particles to about 8 parts organic medium by weight, about 2 parts particles to about 4 parts organic medium by weight, about 1 part particles to about 2 parts organic medium by weight, or about 1 part particles to about 1.5 parts organic medium by weight.
  • Suitable ratios of organic medium to emulsifier in a composition including nanoparticles and/or nano-sheets may be about 1 part organic medium to less than or equal to about 1 part emulsifier, about 1 part organic medium to about 0.5 parts emulsifier by weight, or from about 0.4 to about 1 part emulsifier for about 1 part organic medium by weight.
  • the amount of lubricant nanoparticle and/or nano-sheet composition (by weight) sonicated or dispersed in a lubricant base material may comprise from about 0.25% to about 5%, about 0.5% to about 3%, about 0.5% to about 2%, or about 0.75% to about 2%, based on total weight of the composition.
  • the amount of emulsifier (by weight) sonicated or dissolved in a lubricant base material may comprise from about 0.5% to about 10%, from about 4% to about 8%, from about 5% to about 6%, or from about 0.75% to about 2.25%, based on total weight of the composition.
  • compositions described in this specification may be used, without limitation, as lubricants, coatings, delivery mechanisms, or combinations of any thereof.
  • the compositions may be used, without limitation, as an additive dispersed in a base oil or other lubricant composition.
  • the compositions may also be used, without limitation, to lubricate a boundary lubrication regime.
  • a boundary lubrication regime may be a lubrication regime where the average lubricant film thickness may be less than the composite surface roughness and the surface asperities may come into contact with each other under relative motion. During the relative motion of two surfaces with lubricants in various applications, three different lubrication stages may occur, and the boundary lubrication regime may be the most severe condition in terms of temperature, pressure and speed.
  • Mating parts may be exposed to severe contact conditions of high load, low velocity, extreme pressure (for example, 1-2 GPa), and high local temperature (for example, 150-300 degrees C).
  • the boundary lubrication regime may also exist under lower pressures and low sliding velocities or high temperatures. In the boundaiy lubrication regime, the mating surfaces may be in direct physical contact.
  • compositions may further be used, without limitation, as a lubricant or coating in machinery applications, manufacturing applications, mining applications, aerospace applications, automotive applications, pharmaceutical applications, medical applications, dental applications, cosmetic applications, food product applications, nutritional applications, health related applications, bio-fuel applications or a combination thereof.
  • end applications include, without limitation, machine tools, bearings, gears, camshafts, pumps, transmissions, piston rings, engines, power generators, pin-joints, aerospace systems, mining equipment, manufacturing equipment, or a combination thereof.
  • Further specific examples of uses may be, without limitation, as an additive in lubricants, greases, gels, compounded plastic parts, pastes, powders, emulsions, dispersions, or combinations thereof.
  • compositions may also be used as a lubricant that employs the lubricant nanoparticle and/or nano-sheet composition as a delivery mechanism in pharmaceutical applications, medical applications, dental applications, cosmetic applications, food product applications, nutritional applications, health related applications, bio-fuel applications, or a combination thereof.
  • the various compositions and methods may also be used, without limitation, in hybrid inorganic-organic materials.
  • Examples of applications using inorganic-organic materials include, but are not limited to, optics, electronics, ionics, mechanics, energy, environment, biology, medicine, smart membranes, separation devices, functional smart coatings, photovoltaic and fuel cells, photocatalysts, new catalysts, sensors, small microelectronics, micro-optical and photonic components and systems for nanophotonics, innovative cosmetics, intelligent therapeutic vectors that combined targeting, imaging, therapy, and controlled release of active molecules, and nanoceramic-polymer composites.
  • the dry ball milling operations may create a close caged dense oval shaped architecture (similar to a football shape or fullerene type architecture). This may occur when solid lubricant feed materials are milled in a gas or vacuum.
  • Figure 7(A) shows the close caged dense oval shaped architecture of molybdenum disulfide nanoparticles that have been ball milled in air for 48 hours.
  • the wet ball milling operation may create an open architecture (as described above), which may be encapsulated and/or intercalated with an organic medium. This may occur when solid lubricant feed materials are milled in a gas or vacuum followed by milling in an organic medium.
  • Figure 7(B) shows the open architecture of molybdenum disulfide nanoparticles that have been ball milled in air for 48 hours followed by ball milling in canola oil for 48 hours.
  • the ball milling operations may create nano-sheets, which may be coated and/or encapsulated with an organic medium, or functionalized with catalysts, antioxidants, anti-corrosion agents, biocidals, or combinations of any thereof.
  • the tribological performance of a nanoparticle based lubricant may be improved.
  • the tribological performance may be measured by evaluating different properties.
  • An anti-wear property may be a lubricating fluid property that has been measured using the industry standard Four-Ball Wear (ASTM D4172) Test.
  • the Four-Ball Wear Test may evaluate the protection provided by a lubricant under conditions of pressure and sliding motion. Placed in a bath of the test lubricant, three fixed steel balls may be put into contact with a fourth ball of the same grade in rotating contact at preset test conditions.
  • Lubricant wear protection properties may be measured by comparing the average wear scars on the three fixed balls. The smaller the average wear scar, the better the protection.
  • Extreme pressure properties may be lubricating fluid properties that have been measured using the industry standard Four-Ball Wear (ASTM D2783) Test. This test method may cover the determination of the load-carrying properties of lubricating fluids. The following two determinations may be made: 1) load-wear index (formerly Mean-Hertz load) and 2) weld load (kg).
  • the load-wear index may be the load-carrying property of a lubricant. It may be an index of the ability of a lubricant to minimize wear at applied loads.
  • the weld load may be the lowest applied load in kilograms at which the rotating ball welds to the three stationary balls, indicating the extreme pressure level that the lubricants can withstand.
  • the coefficient of friction may be a lubricating fluid property that has been measured using the industry standard Four-Ball Wear (ASTM D4172) Test.
  • COF may be a dimensionless scalar value which describes the ratio of the force of friction between two bodies and the force pressing them together.
  • the coefficient of friction may depend on the materials used. For example, ice on metal has a low COF, while rubber on pavement has a high COF.
  • a common way to reduce friction may be by using a lubricant which is placed between two surfaces.
  • compositions described in this specification may have a wear scar diameter of about 0.4 mm to about 0.5 mm.
  • the composition may have a COF of about 0.06 to about 0.08.
  • the composition may have a weld load of about 150 kg to about 350 kg.
  • the composition may have a load wear index of about 20 to about 40.
  • the values of these tribological properties may change depending on the amount of lubricant nanoparticle and/or nano-sheet composition sonicated or dissolved in the lubricant base material.
  • Figure 3 shows TEM micrographs of the as-available (700 nm), air milled, and hybrid milled (48 hrs in air medium followed by 48 hours in oil medium) MoS 2 nanoparticles.
  • Figure 3(A) represents micron-sized particle chunks of the as-available MoS 2 sample off the shelf.
  • Figure 3(B) represent agglomerates of nanoparticles when milled in the air medium.
  • Figure 3(B) clearly demonstrates size reduction in air milled MoS 2 . Higher magnification (circular regions) revealed formation of the disc shaped nanoparticles after milling in the air medium.
  • the particle size was reduced to less than 30 nm after milling in air and hybrid conditions. Regardless of the occasionally observed clusters, the average size of the clusters is less than or equal to 200 nm.
  • Hybrid milled samples were dispersed in paraffin oil (from Walmart) and remained suspended without settling. However, the dispersion was not uniform after a few weeks. To stabilize the dispersion and extend the anti-wear properties, phospholipids were added. Around 2% by weight of soy lecithin phospholipids (from American Lecithin) was added in the base oil.
  • Figures 4 and 5 show the XRD and XPS spectra of MoS 2 before and after ball milling, respectively.
  • XRD spectra revealed no phase change as well as no observable amorphization in the MoS 2 after milling. This observation is consistent with the continuous platelets observed throughout the nanoparticle matrix in TEM analysis for milled material. Broadening of peaks (FWHM) was observed in XRD spectra of MoS 2 ball milled in air and hybrid media, respectively. The peak broadening may be attributed to the reduction in particle size.
  • the estimated grain size is 6 nm. This follows the theme of ball milling where clusters consist of grains and sub-grains of the order of 10 nm.
  • XPS analysis was carried out to study the surface chemistry of the as-available and hybrid milled MoS 2 nanoparticles.
  • a carbon (C) peak observed at 285 eV in the as-available MoS 2 sample shifted to 286.7 eV.
  • Wear scar diameter (WSD, mm) of each stationary ball was quantified in both vertical and horizontal directions. The average value of WSD from 3 independent tests was reported within ⁇ 0.03 mm accuracy.
  • Figure 6(A) shows the average wear scar measurements for paraffin oil without a nanoparticle additive, paraffin oil with micron sized MoS 2 , paraffin oil with MoS 2 that was milled in air for 48 hours, and paraffin oil with MoS 2 that was milled in air for 48 hours followed by milling in canola oil for 48 hours.
  • Figure 6(B) shows the load wear index for paraffin oil without a nanoparticle additive, paraffin oil with micron sized MoS , paraffin oil with MoS 2 that was milled in air for 48 hours, and paraffin oil with MoS 2 that was milled in air for 48 hours followed by milling in canola oil for 48 hours.
  • Figure 6(C) shows the COF for paraffin oil without a nanoparticle additive, paraffin oil with micron sized MoS 2 , paraffin oil with MoS 2 that was milled in air for 48 hours, and paraffin oil with MoS 2 that was milled in air for 48 hours followed by milling in canola oil for 48 hours.
  • Figure 6(D) shows the extreme pressure data for paraffin oil with micron sized MoS 2 , paraffin oil with MoS 2 that was milled in air for 48 hours, and paraffin oil with MoS 2 that was milled in air for 48 hours followed by milling in canola oil for 48 hours.
  • the nanoparticle additive was present in the amount of 1 % by weight.
  • FIG. 9(a) depicts the base case of paraffin oil without a nanoparticle additive.
  • Figure 9(b) depicts paraffin oil with the molybdenum disulfide nanoparticles and the emulsifier. It shows the early evidences of molybdenum (Mo)-sulfur (S)-phosphorous (P) in the wear track.
  • Iron (Fe) is seen in Figures 9(a) and 9(b), as it is the material of the balls (52100 steel) in the four-ball test.
  • the molybdenum and sulfur peaks coincide and are not distinguishable because they have the same binding energy. Elemental mapping also showed similar results.

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Abstract

L'invention concerne des compositions ayant une pluralité de nanoparticules et de nano-feuilles. L'invention porte également sur des procédés de fabrication et d'utilisation desdites compositions.
PCT/US2014/071886 2014-02-05 2014-12-22 Compositions de nano-tribologie et procédés associés comprenant des nano-feuilles moléculaires WO2015119716A1 (fr)

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BR112016017584A BR112016017584A2 (pt) 2014-02-05 2014-12-22 Composições de nanotribologia e métodos relacionados incluindo nanofolhas moleculares
MX2016009943A MX2016009943A (es) 2014-02-05 2014-12-22 Composiciones de nanotribologia y metodos relacionados que incluyen nanolaminas moleculares.
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CN107418654A (zh) * 2017-06-05 2017-12-01 上海烯古能源科技有限公司 一种石墨烯润滑油组合物及其制备方法与应用
CN108130178A (zh) * 2018-01-31 2018-06-08 厦门六烯科技有限公司 一种氟化石墨烯增强润滑油及其制备方法
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CN110373259A (zh) * 2019-06-28 2019-10-25 中国矿业大学 矿井提升钢丝绳改性润滑脂的制备及其抗磨性能检测方法
CN111019735A (zh) * 2019-11-19 2020-04-17 湖南长城拉力润滑油有限公司 一种润滑油抗磨剂的制备方法和润滑油
CN111423917A (zh) * 2020-04-03 2020-07-17 广西大学 一种新型润滑油的制备方法
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CA2936897C (fr) 2020-12-15
MX2016009943A (es) 2017-01-11
BR112016017584A2 (pt) 2017-08-08
CA2936897A1 (fr) 2015-08-13

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