WO2021119518A1 - Ceramic surface modification materials - Google Patents

Ceramic surface modification materials Download PDF

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Publication number
WO2021119518A1
WO2021119518A1 PCT/US2020/064655 US2020064655W WO2021119518A1 WO 2021119518 A1 WO2021119518 A1 WO 2021119518A1 US 2020064655 W US2020064655 W US 2020064655W WO 2021119518 A1 WO2021119518 A1 WO 2021119518A1
Authority
WO
WIPO (PCT)
Prior art keywords
ceramic
metal
substrate
ceramic material
composition according
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.)
Ceased
Application number
PCT/US2020/064655
Other languages
English (en)
French (fr)
Inventor
Josh RAFSHOON
Lance R. BROCKWAY
David C. Walther
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nelumbo Inc
Original Assignee
Nelumbo 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.)
Filing date
Publication date
Priority claimed from PCT/US2019/065978 external-priority patent/WO2020123804A1/en
Application filed by Nelumbo Inc filed Critical Nelumbo Inc
Priority to EP20898315.5A priority Critical patent/EP4073020A4/en
Priority to US17/784,486 priority patent/US20230032108A1/en
Priority to JP2022535819A priority patent/JP2023506020A/ja
Priority to CN202080096082.8A priority patent/CN115279717A/zh
Publication of WO2021119518A1 publication Critical patent/WO2021119518A1/en
Anticipated expiration legal-status Critical
Priority to US18/505,950 priority patent/US20240149557A1/en
Ceased legal-status Critical Current

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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32—Polyesters
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/34—Polyamides
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10—Repellency against liquids
    • D06M2200/12—Hydrophobic properties
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
    • F28F2245/00—Coatings; Surface treatments
    • F28F2245/04—Coatings; Surface treatments hydrophobic

Definitions

  • the porous ceramic material is primarily crystalline. In some embodiments, the porous ceramic material comprises a surface area of about 10 m 2 to 1500 m 2 per square meter of projected substrate area. In some embodiment, the porous ceramic material includes a surface area of about 15 m 2 to 1500 m 2 per gram of ceramic material. In some embodiments, the porous ceramic material includes a mean pore diameter of about 2 nm to about 20 nm. In some embodiments, the pore size distribution.
  • the invention also provides methods of application of non-oxide ceramic coatings on a substrate.
  • a ceramic metal oxide (e.g., magnesium oxide) film or layer deposited onto a metal substrate (e.g., aluminum) may be converted into a metal compound (e.g., metal phosphate or metal carbonate) film or layer.
  • the converted film or layer may retain structural artifacts of the base structure of the original ceramic metal oxide film or layer.
  • Binderless refers to absence of a binder that may be exogenously added to a primary material to improve structural integrity, particularly with regard to an organic binder or resin (e.g., polymers, glues, adhesives, asphalt) or inorganic binder (e.g., lime, cement glass, gypsum, etc.).
  • organic binder or resin e.g., polymers, glues, adhesives, asphalt
  • inorganic binder e.g., lime, cement glass, gypsum, etc.
  • First quartile pore diameter refers to the value of the pore diameter at which the cumulative pore surface area determined in the direction of increasing pore size is equivalent to 25% of the total cumulative pore surface area as determined by BJH gas adsorption/desorption measurements.
  • a “functional material layer” refers to a layer of material which may serve as the uppermost surface layer interacting with the surrounding environment or may serve as an interfacial layer for subsequent materials (intermediate layer between two other layers of material).
  • a functional material layer imparts one or more desirable functional properties to the underlying substrate and/or the material on which it is deposited.
  • the interconnected network of ceramic material has an open cell porous structure, for example, characterized by one or more of: ability to effect capillary rise of a liquid having a low surface tension (e.g., less than about 25 mN/m, such as isopropanol) at greater than about 5mm up a surface against gravity in a closed container in 1 hour; surface area of about 0.1 m 2 /g to about 10,000 m 2 /g; mean pore size of about 10 nm to about 1000 nm or about 1 nm to about 1000 nm; pore volume as measured by mercury (Hg) intrusion porosimetry of about 0 to about 1 cc/g; and tortuosity of about 1 to about 1000 as defined by the length of a fluid path to the shortest distance, the “arc-chord ratio”; and/or permeability of about 1 to about 10,000 millidarcy.
  • a low surface tension e.g., less than about 25 mN/m, such as isopropan
  • At least one metal in the interconnected network of ceramic material is in the 2 + oxidation state.
  • the ceramic material consists of one or more oxide ceramics, one or more non-oxide ceramics, or a combination thereof. In some embodiments, the ceramic material consists of one or more oxide ceramics. In some embodiments, the ceramic material consists of one or more non-oxide ceramics. In some embodiments, the ceramic material comprises an oxide ceramic. In some embodiments, the oxide ceramic is an oxide, a hydroxide, a mixed oxide/hydroxide, an aluminate, a silicate, a titanate, a zirconate, a tungstate, or mixtures thereof.
  • the formed ceramic material is in the form of a sphere. In some embodiments, the formed ceramic material is in the form of a ring. In some embodiments, the formed ceramic material is in the form of a cylinder. In some embodiments, the formed ceramic material is in the form of a honeycomb. In some embodiments, the formed ceramic material is in the form of a trilobe. In some embodiments, the formed ceramic material is in the form of a quadrilobe. In some embodiments, the formed ceramic material is an extrudate.
  • the conversion provides a reduced substrate susceptibility to corrosion.
  • the substrate is protected by an inert metal phosphate or metal carbonate barrier from corrosive environments and/or chemicals.
  • This protective layer may act in two main ways to prevent corrosion and/or reduction of electrical conductivity of the substrate.
  • the primary protection is physical, with the inert barrier preventing corrosive species from attacking the substrate and reducing electrical conductivity.
  • the secondary function of the metal phosphate layer is to act as a sacrificial element to react with corrosive species instead of the substrate.
  • sintering e.g., laser sintering, uniaxial hot pressing, hot isostatic pressing
  • melt casting or injection molding of modified particles, power, extrudate, pellets, or flakes results in a ceramic monolith.
  • this ceramic monolith has a theoretical density of greater than about 80%, greater than about 90%, or greater than about 95%.
  • this ceramic monolith comprises magnesium-aluminum spinel, aluminum titanate, zinc-aluminum spinel, or comprises silicon, aluminum, magnesium, zirconium, titanium, or calcium.
  • a hydroxyapatite, octacalcium phosphate, tricalcium phosphate corrosion protection layer is created by depositing an interconnected ceramic comprising calcium phosphate directly onto a substrate.
  • the substrate is immersed in an aqueous bath containing a calcium salt such as calcium chloride or calcium nitrate, a phosphate salt, such as potassium hydrogen phosphate, and a chelating/complexing agent, such as urea, hexamethylenetetramine, or ethylenediaminetetraacetic acid. All components are at a concentration ranging from 0.025M to 1M.
  • the conversion occurs in a heated aqueous solution between 50°C and 90°C, with immersion time from 60 to 1500 minutes. Following immersion, thermal annealing occurs at temperatures from 200°C to 600°C for 60 to 1500 minutes.
  • a mixed metal ceramic surface modification was created by converting an interconnected magnesium oxide structured ceramic surface modification on an aluminum substrate to a mixed tin and magnesium oxide surface modification on an aluminum substrate.
  • the interconnected structured magnesium oxide surface modified substrate was prepared as described above. At the conclusion of this step, the surface of the interconnected magnesium oxide surface modified aluminum substrate appeared white.
  • the aqueous solution was maintained at pH 3-7 with the addition of 1M nitric acid and optionally contained a buffer, such as a citric acid system, phosphoric acid system, carbonate system, acetate system, or a common biological buffer such as tris or MOPS. After pH dosing, the solution turned a bright orange color signifying the presence of decavanadate ions. All components were at a concentration ranging from 0.01 M to 200 mM. The conversion occurred in an aqueous solution maintained between 20°C and 90°C, typically either 20°C, with immersion time from 60 to 1500 minutes, typically about 120 minutes. Following immersion, the sample was thoroughly rinsed with de-ionized water and the sample was allowed to dry.
  • a buffer such as a citric acid system, phosphoric acid system, carbonate system, acetate system, or a common biological buffer such as tris or MOPS.
  • An interconnected magnesium oxide structured ceramic surface modification is applied to aluminum particles, powder, flakes, or extrudates with a maximum dimension less than 1 cm as described above.
  • the coating thickness and particle size are selected such that the aluminum to magnesium ratio is about 2 to 1.
  • These particles, powder, flakes, or extrudates are then post processed using sintering, casting, or molding into a monolith or netshape object by melting the aluminum substrate and flowing it through the porous ceramic coatings resulting in a spinel monolith due to the reaction of the molten aluminum with a stochiometric quantity of magnesium oxide.
  • the process is repeated using a titania coating on aluminum particles to create aluminum titanate.
  • An interconnected magnesium oxide porous ceramic surface modification is applied to aluminum particles, powder, flakes, or extrudates with a maximum dimension less than 1 cm as described above.
  • the magnesium oxide layer provides electrical insulating properties relative to uncoated aluminum.
  • the modified power, flakes, particles or extrudates are then added to a resin or binder to create a thermally conductive paste with electrically insulating properties
  • An interconnected structured manganese oxide modified aluminum panel as described above is created.
  • the modified panel is then filled with another ceramic material by sputtering, ALD, or casting solutions of metal salts or suspensions of metal particulate into the pores. This results in a ceramic filled interconnected ceramic network.
  • the first and second ceramics can be the same or different ceramic materials.
  • a clean 4006 aluminum foil substrate was coated with an interconnected structured ceramic surface based on a mixture of magnesium and aluminum oxides. The surface was then functionalized using a dilute solution of hexadecylphosphonic acid in isopropanol, similar to the procedure in Example 16.
  • Nitrogen BET surface area measurements indicated that the surface area is 300 to 500 square meters per square meter of projected substrate surface area and that the mass specific surface area of the ceramic material is 150 to 200 m 2 /g.
  • Mercury porosimetry indicated that there is a bimodal pore size distribution with pore sizes concentrated at about 5 nm and about 30 nm. BJH measurements indicate the volume of pores smaller than 2.7 nm in diameter is effectively zero.
  • the aqueous solution is maintained at pH 3-7 with the addition of 1M nitric acid and may contain a buffer, such as a citric acid system, phosphoric acid system, carbonate system, acetate system, or a common biological buffer such as tris or MOPS. All components are at a concentration ranging from 0.01 M to 1M, typically about 100 mM.
  • the conversion occurs in an aqueous solution maintained between 20°C and 90°C, typically about 70C, with immersion time from 60 to 1500 minutes, typically about 90 minutes. Following the immersion step, the solution is thoroughly rinsed with de-ionized water and allowed to dry.

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US17/784,486 US20230032108A1 (en) 2019-12-12 2020-12-11 Ceramic Surface Modification Materials
JP2022535819A JP2023506020A (ja) 2019-12-12 2020-12-11 セラミック複合材料
CN202080096082.8A CN115279717A (zh) 2019-12-12 2020-12-11 陶瓷表面改性材料
US18/505,950 US20240149557A1 (en) 2019-12-12 2023-11-09 Ceramic Surface Modification Materials

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US202062989150P 2020-03-13 2020-03-13
US62/989,092 2020-03-13
US62/989,150 2020-03-13
US202063038693P 2020-06-12 2020-06-12
US202063038642P 2020-06-12 2020-06-12
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