GB2622117A - Electroforming method and system - Google Patents

Electroforming method and system Download PDF

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Publication number
GB2622117A
GB2622117A GB2217298.5A GB202217298A GB2622117A GB 2622117 A GB2622117 A GB 2622117A GB 202217298 A GB202217298 A GB 202217298A GB 2622117 A GB2622117 A GB 2622117A
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United Kingdom
Prior art keywords
powder particles
metallic powder
mixture solution
heat treatment
composite
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GB2217298.5A
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GB202217298D0 (en
Inventor
Oruganti Ramkumar
Gourishankar Karthick
Adharapurapu Raghavendra
Nalawade Sachin
Kumar Sondhi Sanjay
T Vishwanath
Krishnan Lakshmi
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Unison Industries LLC
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Unison Industries LLC
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Publication of GB202217298D0 publication Critical patent/GB202217298D0/en
Publication of GB2622117A publication Critical patent/GB2622117A/en
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00Electroforming
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26Methods of annealing
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00Electroforming
    • C25D1/0033D structures, e.g. superposed patterned layers
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D15/00Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C25D17/02Tanks; Installations therefor
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/08Electroplating with moving electrolyte e.g. jet electroplating
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/20Electroplating using ultrasonics, vibrations
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48After-treatment of electroplated surfaces
    • C25D5/50After-treatment of electroplated surfaces by heat-treatment

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Moulds For Moulding Plastics Or The Like (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

An electroforming system 101 and method as defined where the method includes the co-deposition of both metallic ions 125 and powder 130 from a solution 112/113 on the surface of the cathode 116. Through the application of a voltage to the electrodes 114,116 a layer with the particles 130 incorporated in a metal matrix is deposited. The metallic powder has an average particle size of 0.1-100 micrometers. The electroformed component is then heat treated in a temperature range of 600-100oC. A composite layer may thus be formed through electroforming. The powder may be metallic or comprise fibres such as carbon nanotubes, graphene, silica, titanium.

Description

ELECTROFORMING METHOD AND SYSTEM
CROSS-REFERENCE TO RELATED APPLICATION(S)
[0001] This application claims priority to Indian Provisional Patent Application No. 202211050572, filed September 5,2022, which is incorporated herein by reference in its entirety.
TECHNICAL FIELD
[0002] The present subject matter relates generally to an electroforming method and system, and more specifically to electroforming of composite materials.
BACKGROUND
[0003] An electroforming process can create, generate, or otherwise form a metallic layer of a desired component. In one example, a mold or base for the desired component can be submerged in an electrolytic liquid and electrically charged. The electric charge of the mold can attract an oppositely-charged electroforming material through the electrolytic solution. The electrical attraction of the electroforming material to the mold ultimately deposits the electroforming material onto exposed surfaces of the mold, creating an external metallic layer.
BRIEF DESCRIPTION OF THE DRAWINGS
[000 1] A full and enabling disclosure of the present disclosure, including the best mode thereof, directed to one of ordinary skill in the art, is set forth in the specification, which makes reference to the appended figures, in which: [0004] FIG. 1 is a schematic perspective view of a prior art electrodeposition tank for forming a component.
[0005] FIG. 2 is a schematic perspective view of a system for electroforming a component in accordance with various aspects described herein.
[0006] FIG. 3 is a schematic cross-sectional view of an electroformed component formed in the system of FIG. 2.
[0007] FIG. 4 is a schematic cross-sectional view of a portion of the electroformed component of FIG. 3.
[0008] FIG. 5 is a schematic cross-sectional view of the portion of FIG. 4 illustrating one exemplary first heat treatment.
[0009] FIG. 6 is a schematic cross-sectional view of the portion of FIG. 4 after one exemplary aging heat treatment subsequent to the exemplary first heat treatment of FIG 5. [0010] FIG. 7 is a schematic cross-sectional view of the portion of FIG. 4 illustrating another exemplary first heat treatment.
[0011] FIG. 8 is a schematic cross-sectional view of the portion of FIG. 4 after another exemplary aging heat treatment subsequent to the exemplary first heat treatment of FIG. 7. [0012] FIG. 9 is a schematic view of another system for electroforming a component in accordance with various aspects described herein.
[0013] FIG. 10 is a flowchart diagram illustrating a method of electroforming a component in accordance with various aspects described herein.
DETAILED DESCRIPTION
[0014] Aspects of the present disclosure are directed to a system and method for electroforming a component. It will be understood that the disclosure can have general applicability in a variety of applications, including that the electroformed component can be utilized in any suitable mobile and non-mobile industrial, commercial, and residential applications.
[0015] Electroforming is an additive manufacturing process where metal parts are formed through electrolytic reduction of metal ions on the surface of a mandrel or cathode. In a typical electroforming process a mandrel (cathode) and an anode are immersed in an electrolyte solution. A metal layer forming a part thickness builds upon the mandrel surface over time as current is passed between the electrodes. Once the desired part thickness is reached, the mandrel can be removed by mechanical, chemical, or thermal treatment, yielding a free-standing metal part. In one example, the mandrel can be a low melting point material (also referred to as a "fusible alloy") which can be cast into the mandrel shape and subsequently melted out for re-use following electroforming. Other mandrel options include conductive waxes and metallized plastic which can be formed by injection molding, additive manufacturing, or the like. In some cases, a reusable mandrel can also be utilized.
[0016] Electrofonning is used to manufacture products across a range of industries including healthcare, electronics, and aerospace. Electrofonning manufacturing process offers several advantages, including that such processes are efficient, precise, scalable, and low-cost. However, challenges due to limited material options may limit broader application of this technology for advanced structural components. Accordingly, there remains a need for improved methods of manufacturing electrofonned components, particularly high-performance structural components.
[0017] As used herein, "electrodeposition" will include any process for building, forming, growing, or otherwise creating a metal layer over another substrate or base. Non-limiting examples of electrodeposition can include electroforming, electroless forming, electroplating, or a combination thereof While an electroforming process is generally described herein, it will be understood that aspects of the disclosure are applicable to any and all electrodeposition processes.
[0018] As used herein, "non-sacrificial anode" will refer to an inert or insoluble anode that does not dissolve in electrolytic fluid when supplied with current from a power source, while "sacrificial anode" will refer to an active or soluble anode that can dissolve in electrolytic fluid when supplied with current from a power source. Non-limiting examples of non-sacrificial anode materials can include titanium, gold, silver, platinum, and rhodium. Non-limiting examples of sacrificial anode materials can include nickel, cobalt, copper, iron, tungsten, zinc, and lead. It will be understood that various alloys of the metals listed above may be utilized as sacrificial or non-sacrificial anodes.
[0019] All directional references (e.g., radial, axial, proximal, distal, upper, lower, upward, downward, left, right, lateral, front, back, top, bottom, above, below, vertical, horizontal, clockwise, counterclockwise, upstream, downstream, aft, etc.) are only used for identification purposes to aid the reader's understanding of the present disclosure, and do not create limitations, particularly as to the position, orientation, or use of the disclosure. Connection references (e.g., attached, coupled, connected, and joined) are to be construed broadly and can include intermediate members between a collection of elements and relative movement between elements unless otherwise indicated. As such, connection references do not necessarily infer that two elements are directly connected and in fixed relation to one another. In addition, as used herein "a set" can include any number of the respectively described elements, including only one element.
[0020] The exemplary drawings are for purposes of illustration only and the dimensions, positions, order, and relative sizes reflected in the drawings attached hereto can vary. [0021] FIG. I is a schematic illustration of a prior art electroforming system I. A prior art electrodeposition tank 10 (or "tank 10") can carry a single metal constituent solution or electrolytic solution 12 having alloying metal ions. At least one electrode can be provided in the tank. The at least one electrode can include an anode 14 and a cathode 16. A component to be electroformed can form the cathode 16.
[0022] A power source 18, which can include a controller or controller module, can electrically couple to the anode 14 and the cathode 16 by electrical conduits 20 to form a circuit via the conductive electrolytic solution 12. Optionally, a switch 22 or sub-controller can be included along the electrical conduits 20 between the power source 18, anode 14, and cathode 16. During operation, a current can be supplied from the anode 14 to the cathode 16 to electroform a body at the cathode 16. Supply of the current can cause metal ions from the single metal constituent solution 12 to form a metallic layer over the component at the cathode 16.
[0023] Electroforming material options have typically included nickel, copper, or a nickel-cobalt alloy. Such materials have traditionally allowed for a suitably high deposition rate (e.g. greater than 0.001 inthr or 0.025 mm/hr), high current efficiency (e.g. the proportion of current used to convert metal ions to solid metal, instead of other side reactions), and low residual stresses in the finished component. Such material options for structural applications are typically limited to maximum usage temperatures of approximately 500°F (260°C), with strength and temperature capability limited to approximately 100 ksi (690 MPa) ultimate tensile strength at 500°F (260°C). In addition, electrodeposition of high-strength multi-component alloys can present challenges for incorporation of all of the various alloying elements in the electrolyte bath.
[0024] Aspects of the present disclosure provide for an electroforming process that can be used to manufacture high-strength parts capable of operating at higher temperatures than traditional electroforming processes, including greater than 500°F (260°C), or even up to or greater than 1200°F (650°C), including between 650-870°C (1200-1600°F) in a non-limiting example.
[0025] Aspects of the disclosure herein also provide for a thick, standalone electrofonn having an overall thickness of 1-5 mm or greater and improved material strength by way of direct incorporation of a pre-alloyed superalloy powder or other alloy powder into an electrolyte solution. The electroformed metal layer forms a composite electroformed component having the dispersed powder particles incorporated into a metal matrix. The described aspects also provide for a first heat treatment process performed at a high temperature to improve metallurgical bonding between the particles and the metal matrix, or to dissolve the particles into the metal matrix to form a homogeneous single-phase matrix. The described aspects further provide for a second heat treatment process in the form of an aging heat treatment, following the first heat treatment, to induce precipitation within the powder particles or the homogeneous single-phase matrix for additional strengthening. In this manner, problems are addressed relating to strength and high temperature capability of electroformed components by employing composite materials and heat treatments.
[0026] In this approach, metallic powder particulates (e.g. metallic superalloy particulates) are suspended in the electrolyte and incorporated in the growing metal matrix during electroforming. Subsequent heat treatment of the electroformed component at selected temperature ranges can provide for incorporation and reprecipitation of particulates in the component, resulting in optimum mechanical properties regarding material strength, tensile strength, hardness, ductility, or the like.
[0027] Referring now to FIG. 2, a system 101 for electroforming a component is illustrated in accordance with various aspects described herein. The system 101 is similar to the system 1; therefore, like parts of the system 101 will be identified with like numerals increased by 100, with it being understood that the description of the like parts of the system 1 applies to the system 101, except where noted.
[0028] The system 101 includes an electrodeposition tank 110 (or "tank 110"), an anode 114, a cathode 116, a power source 118, electrical conduits 120, and a switch 122. An electrolytic solution 112 containing metal ions 125 can be provided in the tank 110. One difference compared to the system 1 is that metallic powder particles 130 (also referred to herein as "metallic powder 130" or "powder 130") can be suspended in the electrolytic solution 112 to fonn a mixture solution 113 within the tank 110. The mixture solution 113 contains the metal ions 125 and the metallic powder 130. The powder 130 can include prealloyed superalloys or high strength alloys, including a nickel-cobalt-phosphorus alloy, a nickel-molybdenum alloy, nickel aluminide, Inconel, Ni3A1, Ni3Ta, Ni3Ti, Ni3Nb, Ni3Mo, NiAl, R108, or R718, in some non-limiting examples. Additionally or alternatively, the powder 130 can also include yttria particles, alumina particles, alumina fibers, cerium oxide particles, silica particles, silicon carbide particles, titanium particles, titanium oxide particles, titanium carbide particles, titanium nitride particles, zirconium carbide particles, carbon nanotubes, graphene, or precursors thereof, or combinations thereof, in non-limiting examples.
[0029] As used herein, a "prealloyed" material, e.g. a prealloyed powder material, can refer to the particles of that material having the same alloy composition as the overall material as is known in the art. Other powder metallurgy alloying methods known in the art include, but are not limited to, admixing, diffusion alloying, and hybrid alloying. In addition, as used herein, a "high strength alloy" can refer to an alloy having a material property above a predetermined threshold including, but not limited to, an ultimate tensile strength (UTS) greater than 100 ksi (690 MPs) at 1200 F (650°C), or a ductility greater than 10% at 1200 F (650 °C).
[0030] The anode 114 and cathode 116 can be located within the tank 110 and submerged in the mixture solution 113. The anode 114 can be a sacrificial or non-sacrificial anode. The cathode 116 can be spaced from the anode 114 within the mixture solution 113. The cathode 116 can include a mandrel 124, which can be removable or non-removable from the electroformed component.
[0031] The anode 114 and the cathode 116 can also be electrically coupled to the power source 118 by way of electrical conduits 120 as shown. A switch 122 can be provided between the anode 1 14 and power source 118. The power source 118 can include a controller module to control the flow of current through the electrical conduits 120. Additionally or alternatively, a separate controller can be provided and electrically coupled to the power source 118.
[0032] Another difference compared to the system 1 is that a set of flow controllers 140 can be provided for stirring, mixing, agitating, dispersing, or the like of the powder 130 in the mixture solution 113. In some examples, the set of flow controllers 140 can be electrically coupled to the power source 118. Additionally or alternatively, the set of flow controllers 140 can be controllably operated by a separate controller.
[0033] The set of flow controllers 140 can be fluidly coupled to the interior of the tank 110. In the illustrated example, the set of flow controllers 140 is shown within the tank 110. It is also contemplated that the set of flow controllers 140 can be positioned externally to the tank 110 and coupled thereto, e.g. by a fluid port, conduit, or the like.
[0034] Exemplary first, second, and third flow controllers 141, 142, 143 are shown in the set of flow controllers 140. Any number or type of flow controllers can be provided. In addition, described aspects of the first, second, and third flow controllers 141, 142, 143 can be utilized in combination. For example, a single flow controller can include multiple types of flow mechanisms agitating the mixture solution 113.
[0035] The first flow controller 141 can include a liquid pump configured to flow a liquid jet 144 through the mixture solution 113. In some examples, the first flow controller 141 can include a liquid intake port 145 providing an external liquid source to the tank 110. In some examples, the liquid intake port 145 can be located within the tank 110, drawing in surrounding mixture solution 113 to form the liquid jet 144.
[0036] The second flow controller 142 can include an air pump configured to flow an air jet 146 through the mixture solution 113. The second flow controller 142 can include an air intake port 147 fluidly coupled to a source of air for forming the air jet 146. In some examples, the air intake port 147 can be located within the tank 110 and fluidly coupled through a tank wall to a source of air. In some examples, the air intake port 147 can be located externally to the tank 110.
[0037] The third flow controller 142 can include a sonic device configured to emit pressure waves. In the illustrated example, the third flow controller 142 includes an ultrasonic device with an oscillator, transducer, and the like emitting ultrasonic pressure waves 148 into the mixture solution 113. In one example, the third flow controller 142 can be located within the tank 110 and directly emitting the ultrasonic pressure waves 148 into the mixture solution 113. In another example, the third flow controller 142 can be located externally to the tank 110 and transmitting ultrasonic pressure waves 148 through a conduit, transmitter, or the like into the tank 110 and mixture solution 113.
[0038] During operation, a current can be supplied from the anode 114 to the cathode 116 to electroform a composite metal layer 150 at the cathode 116. Supply of the current in the mixture solution 113 can cause metal ions 125 as well as the metallic powder particles 130 to move toward and accumulate onto the cathode 116 (e.g. mandrel 124). In addition, the set of flow controllers 140 can be arranged to provide mixing and dispersion of the powder 130 within the mixture solution 113. The set of flow controllers 140 can be configured or arranged to sweep powder 130 that may aggregate near the bottom or in corners of the tank 110 in an upward direction and toward the cathode 116. In some examples, the set of flow controllers 140 can produce turbulent flows, circulating currents, or other flow features within the mixture solution 113, thereby ensuring availability of unagglomerated particles near the cathode 116.
[0039] It is also appreciated that the set of flow controllers 140 can direct the metallic powder particles 130 onto the cathode 116, and the powder 130 can accumulate on a surface of the cathode 116 having any direction or surface orientation. In the example shown, a non-horizontal surface 126 of the mandrel 124 is indicated upon which the powder 130 can be directed by the set of flow controllers 140. The non-horizontal surface 126 can include a vertical surface, an inclined surface, or a bottom surface of the cathode 116, in non-limiting examples. In this manner, a composite metal layer 150 can be formed over any surface of the mandrel 124 and include the metallic powder particles 130 and metal ions 125 from the mixture solution 113, [0040] Turning to FIG. 3, a schematic cross-sectional view is shown of the mandrel 124 and composite metal layer 150 after electroforming. While the mandrel 124 is illustrated as a solid component, this need not be the case and the mandrel 124 can also include a hollow portion in some examples.
[0041] At least the composite metal layer 150 can define a composite electroformed component 160. In some examples, the mandrel 124 can be removed from the composite metal layer 150, e.g. a sacrificial mandrel, to form the composite electroformed component 160. In some examples, the mandrel 124 can remain in place and at least partially define the composite electroformed component 160 with the composite metal layer 150.
[0042] In addition, a layer thickness 152 is illustrated for the composite metal layer 150. The layer thickness 152 can be between 0.5-10 mm, including between 0.5-5 mm, or between 1-5 mm, in non-limiting examples. The layer thickness 152 can also be constant or varied over portions of the composite metal layer 150. It is contemplated that the composite metal layer 150 can form a standalone, thick electrofonn, such as may be used for structural applications.
[0043] An enlarged portion 162 of the composite electroformed component 160 is schematically illustrated in FIG. 4. The powder 130 is shown dispersed in a metal matrix 154 within the composite electroformed layer 150. The metal matrix 154 can be formed from the metal ions 125 (FIG. 2) as described above. The metal matrix can include nickel, a nickel alloy (e.g. nickel-cobalt, nickel-tungsten or nickel-molybdenum alloy), copper, cobalt, or combinations thereof, in some non-limiting examples.
[0044] The powder 130 can have an average particle size in a range between 1-1000 pm. In some non-limiting examples, the powder 130 can have an average particle size in a range between 1-1000 pm, including between 50-500 pm, or between 10-50 pm, or between 1-20 pm, or between 1-10 pm, or between 5-10 pm, or between 1-5 pm, or between 0.1-1 pm. It is also contemplated that the powder 130 can include varying particle sizes for improved packing of the powder 130 within the composite metal layer 150. In one non-limiting example, a first subset of the powder 130 can have an average particle size in a range between 500-1000 pm, a second subset of the powder 130 can have an average particle size in a range between 50-500 pm, and a third subset of the powder 130 can have an average particle size in a range between 1-10 gm.
[0045] While the powder 130 is illustrated with generally spherical or rounded particles, the powder 130 can include any suitable geometric profile including fibers, tubes, flakes, sheets, or the like, or combinations thereof. In addition, in some examples, a volume fraction of the powder 130 in the composite metal layer 150 can be in a range between 30-70 vol%. In some examples, a mass fraction of the powder 130 in the composite metal layer 150 can be in a range between 30-70%.
[0046] Another difference compared to the electroforming system 1 is that the metallic powder particles 130 can include a coating 170. The coating 170 can include ceramic powder in a non-limiting example. A coating thickness 172 is illustrated for one of the metallic powder particles 130. The coating thickness 172 can be in a range between 1-100 nm in some examples. The coating 170 can be separately or physically applied to the powder 130 in some examples. The coating 170 can also include a native oxide of controlled thickness grown on the powder particles 130 in accordance with a predetermined temperature or time schedule. In a non-limiting example, the powder 130 can be heat treated in a range between 500-600°C for 5-10 hours, thereby growing an oxide layer onto the powder 130 to form the coating 170. [0047] It is contemplated that the coating 170 can limit or prevent an undesired reaction of the metallic powder 130 with the electrolytic solution 112 (FIG. 2). For example, many high-strength alloys typically include metals such as aluminum or titanium, which can be highly reactive in aqueous electrolytic solutions. It is appreciated that direct incorporation of aluminum, titanium, or the like into the electrolytic solution 112, e.g. as the powder 130, can generate undesired ion production within the solution and the resulting electroformed component. Use of the coating 170 in the powder 130 can provide for inclusion of traditional metals in aqueous solution for high-strength alloys while preventing undesired reaction of the metal in solution.
[0048] Additionally or alternatively, at least some of the powder 130 can be provided without any coating 170. In such a case, the powder 130 can include non-reactive or less reactive metals in aqueous electrolyte environments, including alloys or pre-formed precipitates with low activity of the active element e.g. aluminum or titanium, such as Ni3A1 or Ni3Ti in some non-limiting examples. For example, if' using Ni3A1 for the powder 130, it is understood that Ni3A1 is a compound and therefore less chemically reactive with electrolytic solutions compared to other superalloy powders such as MCrAIY.
[0049] In addition, at least one heat treatment can be performed on the composite electroformed component 160. The at least one heat treatment can include stress equalizing, stress relieving, annealing, solution annealing, tempering, age hardening, precipitation hardening, or diffusion, in some non-limiting examples.
[0050] It is contemplated that the at least one heat treatment can include a first heat treatment performed in a first temperature range and a second, aging heat treatment performed in a second, aging temperature range. The aging heat treatment can be performed subsequently to the first heat treatment. In some examples, the first temperature range can be between 600-I 200°C. In some examples, the second, aging temperature range can be between 500-800°C.
[0051] Turning to FIG. 5, the enlarged portion 162 of the composite electroformed component 160 is illustrated in one non-limiting example of operation after completion of the first treatment. The first heat treatment can be performed in a temperature range between 600-850°C. The first heat treatment can also be performed over a time duration of between 12 hours. In the example shown, the powder 130 remains distributed throughout the metal matrix 154, and the first heat treatment enhances or improves metallurgical bonding between incorporated powder 130 and the metal matrix 154. It is also contemplated that the first, high temperature heat treatment can remove or dissolve the coating 170 (see FIG. 4) into the metal matrix 154. Additionally or alternatively, a separate coating diffusion heat treatment can be performed on the composite electroformed component 160 for incorporation into the metal matrix 154. In an example where the coating 170 includes ceramic, the incorporation of ceramic into the composite metal layer 150 can provide for additional strengthening of the composite electroformed component 160.
[0052] It is understood that, in some examples, the metallic powder particles 130 can have a uniform or non-uniform size, shape, arrangement, distribution, or the like after performing a heat treatment on the composite electroformed component 160.
[0053] FIG. 6 illustrates the enlarged portion 162 of the composite electroformed component 160 resulting from a second, aging heat treatment following the first heat treatment of FIG. 5. The aging heat treatment can be performed in a second, aging temperature range between 500-800°C. The aging heat treatment can also be performed over a time duration of between 5-20 hours.
[0054] It is understood that the aging heat treatment can form precipitates 180 within the composite electroformed component 160. In the illustrated example, formation of the precipitates 180 can be limited to within the powder particles 130 and not within the metal matrix 154. It is appreciated that, in some examples, the metal matrix 154 can dilute the overall chemistry and reduce the driving force for precipitation therein. Limiting the formation of precipitates 180 to the powder particles 130 can preserve the overall material strength while bypassing barriers to precipitation within the metal matrix 154 itself. [0055] It is further contemplated that the precipitates 180 can include fine, second-phase particles having an average particle size in a range between 10-1000 nm in a non-limiting example. In addition, in some examples, the aging heat treatment can be performed once, forming a single-step aging heat treatment, or performed twice to form a two-step aging heat treatment.
[0056] Turning to FIG. 7, the enlarged portion 162 of the composite electroformed component 160 is illustrated in another example of operation after completion of the first treatment. In this example, the first heat treatment can be performed in a temperature range between 850-1200°C. The first heat treatment can also be performed over a time duration of between 1-2 hours. In the example shown, the powder 130 and coating 170 are dissolved and fully incorporated into the metal matrix 154 (FIG. 4), thereby defining a matrix 156 in the form of a single-phase, homogeneous, solid-solutioned matrix. It is understood that in another example where the metallic powder particles 130 are not coated, the first heat treatment can dissolve the powder 130 alone into the metal matrix 154 to define the matrix 156.
[0057] FIG. 8 illustrates the enlarged portion 162 of the composite electroformed component 160 resulting from a second, aging heat treatment following the first heat treatment of FIG. 7. The aging heat treatment can be performed in a temperature range between 500-800°C. The aging heat treatment can also be performed over a time duration of between 5-20 hours.
[0058] It is understood that the aging heat treatment can form precipitates 182 within the composite electroformed component 160. In the illustrated example, the precipitates 182 are distributed throughout the matrix 156. The precipitates 182 can be the same as, or different from, the precipitates 180 (FIG. 6). The precipitates 182 can include fine, second-phase particles having an average particle size in a range between 10-1000 nm in a non-limiting example. In addition, in some examples, the aging heat treatment can be performed once to define a single-step aging heat treatment, or performed twice to define a two-step aging heat treatment.
[0059] Referring generally to FIGS. 5-8, regardless of the temperature range for the first heat treatment or aging heat treatment, it is contemplated that a mean free path (X) within the composite metal layer 150 after completion of heat treatment(s) can be in a range between 10-350 rim including between 10-200 nm, or between 10-100 rim in some non-limiting examples. In one example, for homogenously dispersed particles with substantially no agglomeration, the mean free path X can be determined by Expression 1 below: 4(1-nr [0060] Expression 1: A = 3f [0061] where r = particle size, and f = the volume fraction of the particles.
[0062] For effective strengthening in structural applications, it can be desirable that the metal layer 150 can include layer particles dispersed with an appropriate size, volume fraction, and spacing. In one non-limiting example, the metal layer 150 can have a post-heat treatment microstructure such that a mean free path within the metal layer 150 conforms closely to that of a perfectly uniform distribution, with no agglomeration.
[0063] Furthermore, in one example where the precipitates 180, 182 have a particle size of 0.1-0.5 micrometers, the precipitates 180, 182 can self-distribute to fonn a desired interparticle spacing range, e.g. 10-350 nm. In such a case, post-processing of the composite electroformed component 160 can be minimized because the spacing range is suitable for high strength applications.
[0064] Still further, it is appreciated that direct incorporation of the powder 130, which contains strengthening particles, into the mixture solution 113 can increase resulting precipitation rates during aging heat treatments. Introduction of powder 130 in concentrations forming the above-described 30-70% volume fraction or 30-70% mass fraction in the composite metal layer 150 can provide for increased precipitation locations or increase in driving force for precipitation in the composite metal component 160.
[0065] Turning now to FIG. 9, another system 201 for electroforming a component is illustrated in accordance with various aspects described herein. The system 201 is similar to the system I, 101; therefore, like parts of the system 201 will be identified with like numerals further increased by 100, with it being understood that the description of the like parts of the system 1, 101 applies to the system 201, except where noted.
[0066] The system 201 includes an electrodeposition tank 210 (or "tank 210"), an anode 214, a cathode 216 including a mandrel 224, a power source 218, electrical conduits 220, and a switch 222. An electrolytic solution 212 can be provided in the tank 210. One difference compared to the system 1, 101 is that the system 201 can include a separate dissolution reservoir 205 (or "reservoir 205"). The anode 214 can be located in the dissolution reservoir 205, and the cathode 216 can be located in the tank 210. Metallic powder particles 230 can also be suspended in the electrolytic solution 212 to form a mixture solution 213 within the tank 210.
[0067] At least one conduit can fluidly couple the reservoir 205 and the tank 210. In the illustrated example, a first conduit 207 can provide a first fluid path between the reservoir 205 and the tank 210, and a second conduit 209 can provide a second fluid path between the reservoir 205 and the tank 210, though this need not be the case. It is contemplated that a recirculation circuit can be provided wherein electrolytic fluid can circulate between the reservoir 205 and the tank 210 by way of the first and second conduits 207, 209. In another example, fluid can flow in one direction from the reservoir 205 to the tank 210, and the tank 210 can include a drain or the like for removal of fluid therein. Fluid can be supplied continuously, or with discrete portions at regular or irregular time intervals, from the reservoir 205 to the tank 210.
[0068] In some examples, a filter can be provided in the at least one conduit, e.g. the first conduit 207 or the second conduit 209, for retaining the metallic powder particles 230 within the electrolyte solution 212 in the tank 210. In such a case, the mixture solution 213 can be contained within the tank 210, and the electrolytic solution 212 can be contained within the reservoir 205.
[0069] A set of flow controllers 240 can be provided in the system 201. In the illustrated example, the set of flow controllers 240 includes first, second, and third flow controllers 241, 242, 243 are illustrated in the system 201. Another difference is that the set of flow controllers 240 can be fluidly coupled to either or both of the reservoir 205 or the tank 210. In the illustrated example, the first flow controller 241 is located in the reservoir 205, and the second and third flow controllers 242, 243 are located in the tank 210. In one non-limiting example, the first flow controller 241 can include a liquid pump configured to flow a liquid jet 244 through the electrolyte solution 212. The second flow controller 242 can include an air pump configured to flow an air jet 246 through the mixture solution 213. The third flow controller 243 can include a sonic device configured to emit pressure waves 248 through the mixture solution 213. Additionally or alternatively, a flow controller having a liquid pump forming a liquid jet can also be provided in the tank 210.
[0070] In one non-limiting example of operation, a current can be supplied from the anode 214 in the dissolution reservoir 205 to the cathode 216 in the electrodeposition tank 210. The current can cause dissolution of alloying metal ions 225 into the electrolyte solution 212. The electrolyte solution 212 can flow into the tank 210, where the metallic powder particles 230 can be dispersed therein to form the mixture solution 213. A composite metal layer 250 can be deposited onto the cathode 216. Supply of the current in the mixture solution 213 can cause metal ions 225 as well as the metallic powder particles 230 to move toward and accumulate onto the cathode 216. The set of flow controllers 240 can be arranged to provide mixing, agitation, dispersion, or the like for the electrolyte solution 212 and the mixture solution 213. For example, the first flow controller 241 can provide for uniform dispersion of alloying metal ions 225 within the electrolyte solution 212 upstream of the electrodeposition tank 210. The second and third flow controllers 242, 243 can provide for mixing and dispersion of the metallic powder particles 230 within the mixture solution 213, providing unagglomerated particles in the region of the cathode 216. For example, the second or third flow controllers 242, 243 can be configured or arranged to sweep metallic powder particles 230 that may aggregate near the bottom or in corners of the tank 210 in an upward direction and toward the cathode 216 In this manner, the composite metal layer 250 at least partially defining a composite electroformed component can be formed at the cathode 216 as described above.
[0071] FIG. 10 is a flowchart illustrating a method 300 of electroforming a component, such as the composite electroformed component 160, 260, in accordance with various aspects described herein. At 302, the method 300 includes electroforming a composite metal layer, such as the composite metal layer 150, 250, onto a mandrel, such as the mandrel I 24, 224, from a mixture solution, such as the mixture solution 113, 213. The mixture solution 113, 213 can include the electrolytic solution 112, 212 with dispersed metallic powder particles, such as the powder 130, 230, therein. The powder 130, 230 can have an average particle size between 0.1-1000 i.tm as described above. The method 300 at 302 can further include applying a voltage to an electrode, such as the cathode 116, 216, in the mixture solution to form the composite metal layer. The composite metal layer can have the metallic powder particles incorporated within a metal matrix, such as the metal matrix 154, and defining a composite electroformed component, such as the composite electroformed component 160, 260.
[0072] The method 300 can include at 304 performing at least a first heat treatment on the composite electroformed component within a first temperature range of 600-1200°C. Optionally, the method can include at 306 performing an aging heat treatment on the composite electroformed component. The aging heat treatment can be performed in a temperature range of 500-800°C.
[0073] The method 300 can further include wherein a coating is provided on the metallic powder particles in the mixture solution. Optionally, the first heat treatment can strengthen a metallurgical bond between the powder 130, 230 and the metal matrix 154 in the composite electroformed component 160, 260. Optionally, the first heat treatment can dissolve the powder 130, 230 into the metal matrix 154 to form a second matrix 156 in the form of a single-phase, homogeneous, solid-solutioned matrix. Optionally, the aging heat treatment can form precipitates 180, 182 in the metallic powder particles 130, 230. Optionally, the aging heat treatment can form precipitates 180, 182 in the metal matrix 154 or the second matrix 156.
[0074] Aspects of the present disclosure provide for a variety of benefits. Suspension of powdered or particulate alloys or superalloys within the electrolyte can provide for deposition of a composite material onto the cathode, preserving the needed alloy material within the composite material without need of providing the various alloying elements dissolved within the electrofonning bath. In this manner, direct incorporation of the particles, e.g. highly pre-alloyed powders or ex-situ created precipitates, is enabled in the composite electroformed layer.
[0075] In addition, the use of flow controllers can provide for a more uniform alloy particle incorporation at sufficient concentrations within the electroformed layer. Ultrasound devices and flow jets can enable availability of an abundance of unagglomerated particles at the cathode surface. Furthermore, coating the alloy particles with ceramic powders can prevent undesired reaction with the surrounding electrolyte and also provide additional strengthening of the finished component. The one or more heat treatments of the composite electroformed component can provide for dissolving and reprec p tation of the strengthening particles therein.
[0076] To the extent not already described, the different features and structures of the various embodiments can be used in combination with each other as desired. That one feature cannot be illustrated in all of the embodiments is not meant to be construed that it cannot be, but is done for brevity of description. Thus, the various features of the different embodiments can be mixed and matched as desired to form new embodiments, whether or not the new embodiments are expressly described. All combinations or permutations of features
described herein are covered by this disclosure.
[0077] This written description uses examples to disclose the disclosure, including the best mode, and also to enable any person skilled in the art to practice the disclosure, including making and using any devices or systems and performing any incorporated methods. The patentable scope of the disclosure is defined by the claims, and may include other examples that occur to those skilled in the art. Such other examples are intended to be within the scope of the claims if they have structural elements that do not differ from the literal language of the claims, or if they include equivalent structural elements with insubstantial differences from the literal languages of the claims.
[0078] Further aspects of the disclosure are defined by the following clauses: [0079] A method of forming a component, the method comprising electroforming a composite metal layer onto a mandrel from a mixture solution, the mixture solution comprising an electrolytic solution with dispersed metallic powder particles therein having an average particle size between 0. I -1000 micrometers, and with the composite metal layer having the metallic powder particles incorporated within a metal matrix and defining a composite electroformed component, and performing at least a first heat treatment on the composite electroformed component within a first temperature range of 600-1200°C. [0080] A method of forming a component, the method comprising disposing an electrode defining a mandrel within a mixture solution comprising an electrolytic solution with dispersed metallic powder particles therein having an average particle size between 0.1-1000 micrometers, applying a voltage to the electrode in the mixture solution to form a composite metal layer on the electrode, the composite metal layer having the metallic powder particles incorporated within a metal matrix and defining a composite electroformed component, and performing a first heat treatment on the composite electroformed component within a first temperature range of 600-1200°C.
[0081] The method of any preceding clause, wherein the metallic powder particles comprise at least one of a superalloy, a high strength alloy, nickel, aluminum, titanium, tantalum, niobium, cobalt, phosphorus, molybdenum, or steel.
[0082] The method of any preceding clause, further comprising performing an aging heat treatment on the composite electroformed component, subsequent to the first heat treatment, within a second temperature range of 500-800°C to form precipitates in the composite electroformed component.
[0083] The method of any preceding clause, wherein the precipitates are formed within the metallic powder particles.
[0084] The method of any preceding clause, wherein the first heat treatment dissolves the metallic powder particles into the metal matrix to define a second matrix, and wherein the precipitates are formed within the second matrix.
[0085] The method of any preceding clause, wherein the precipitates comprise at least one of Ni3A1, Ni3Ta, Ni3Ti, Ni3Nb, Ni3Mo, NiAl, or Ni3Ti.
[0086] The method of any preceding clause, wherein the metallic powder particles in the mixture solution have a coating comprising at least one of ceramic or a native oxide of the metallic powder particles.
[0087] The method of any preceding clause, further comprising forming a coating on the metallic powder particles in the mixture solution.
[0088] The method of any preceding clause, further comprising growing a native oxide onto the metallic powder particles to form the coating [0089] The method of any preceding clause, further comprising heat treating the metallic powder particles in a range between 500-600°C for 5-10 hours to grow the native oxide layer. [0090] [0091] The method of any preceding clause, wherein the coating comprises at least one of ceramic or the native oxide.
[0092] The method of any preceding clause, wherein the first heat treatment removes the coating from the metallic powder particles and incorporates the coating into the metal matrix. [0093] The method of any preceding clause, further comprising dispersing the metallic powder particles within the mixture solution by at least one of: applying pressure waves to the mixture solution, flowing a liquid jet through the mixture solution, or flowing an air jet through the mixture solution.
[0094] The method of any preceding clause, wherein the mandrel includes a non-horizontal surface [0095] The method of any preceding clause, wherein the dispersing further comprises directing the metallic powder particles within the mixture solution toward the non-horizontal surface.
[0096] The method of any preceding clause, wherein an average particle size of the metallic powder particles in the mixture solution is between 0.1-20 micrometers.
[0097] The method of any preceding clause, wherein the metallic powder particles comprise a mass fraction of between 30-70% for the composite electroformed component. [0098] The method of any preceding clause, wherein the metallic powder particles comprise a volume fraction of between 30-70 vol% for the composite electroformed component.
[0099] The method of any preceding clause, wherein the metallic powder particles have an average particle size is between 0.1-1 micrometers.
[0100] The method of any preceding clause, wherein the average particle size is between 1-10 micrometers.
[0101] The method of any preceding clause, wherein the composite electroformed component comprises a thickness between 0.5-10 mm.
[0102] The method of any preceding clause, wherein the composite electroformed component comprises a thickness between 0.5-5 mm.
[0103] The method of any preceding clause, wherein the composite electroformed component comprises a thickness between 1-5 mm.
[0104] A system for electroforming a component, comprising: an electroforming tank; a cathode located within the electroforming tank, a power source electrically coupled to the cathode, and a mixture solution within the electroforming tank comprising an electrolytic solution with dispersed metallic powder particles therein, the metallic powder particles having an average particle size between 1-1000 micrometers.
[0105] The system of any preceding clause, further comprising a coating over at least some of the dispersed metallic powder particles.
[0106] The system of any preceding clause, wherein the coating comprises at least one of ceramic or a native oxide of the metallic powder particles.
[0107] The system of any preceding clause, wherein the metallic powder particles comprise at least one of a superalloy, a high strength alloy, nickel, aluminum, titanium, tantalum, niobium, cobalt, phosphorus, molybdenum, or steel.
[0108] The system of any preceding clause, further comprising a set of flow controllers located within the electroforming tank and configured to agitate the mixture solution. [0109] The system of any preceding clause, wherein the set of flow controllers comprises an ultrasonic device emitting ultrasonic pressure waves into the mixture solution.
[0110] The system of any preceding clause, wherein the set of flow controllers comprises a liquid pump emitting a liquid jet into the mixture solution.
[0111] The system of any preceding clause, wherein the liquid pump comprises a liquid intake port fluidly coupled to at least one of the mixture solution or an external liquid source. [0112] The system of any preceding clause, wherein the set of flow controllers comprises an air pump emitting an air jet into the mixture solution.
[0113] The system of any preceding clause, wherein the air pump comprises an air intake port fluidly coupled to a source of air.
[0114] The system of any preceding clause, further comprising a dissolution tank having an anode electrically coupled to the power source.
[0115] The system of any preceding clause, wherein the dissolution tank is fluidly coupled to the electroforming tank by at least one fluid conduit.
[0116] The system of any preceding clause, wherein the mixture solution is contained in the electroforming tank.
[0117] The system of any preceding clause, further comprising an anode located within the electroforming tank and spaced from the cathode.

Claims (20)

  1. CLAIMSWhat is claimed is A method of forming a component, the method comprising: electroforming a composite metal layer onto a mandrel from a mixture solution, the mixture solution comprising an electrolytic solution with dispersed metallic powder particles therein having an average particle size between 0.1-1000 micrometers, and with the composite metal layer having the metallic powder particles incorporated within a metal matrix and defining a composite electroformed component; and performing at least a first heat treatment on the composite electroformed component within a first temperature range of 600-1200°C.
  2. 2 The method of claim 1, wherein the metallic powder particles comprise at least one of a superalloy, a high strength alloy, nickel, aluminum, titanium, tantalum, niobium, cobalt, phosphorus, molybdenum, or steel.
  3. 3. The method of any one of claims 1-2, further comprising performing an aging heat treatment on the composite electroformed component, subsequent to the first heat treatment, within a second temperature range of 500-800°C to form precipitates in the composite electroformed component.
  4. 4. The method of claim 3, wherein the aging heat treatment forms the precipitates within the metallic powder particles.
  5. 5. The method of claim 3 or 4, wherein the first heat treatment dissolves the metallic powder particles into the metal matrix to define a second matrix, and wherein the precipitates are formed within the second matrix.
  6. 6. The method of any one of claims 3-5, wherein the precipitates comprise at least one of Ni3A1, Ni3Ta, Ni3Ti, Ni3Nb, Ni3Mo, NiAl, or Ni3Ti.
  7. 7. The method of any one of claims 1-6, wherein the metallic powder particles in the mixture solution have a coating comprising at least one of ceramic or a native oxide of the metallic powder particles.
  8. 8. The method of claim 7, further comprising growing the native oxide onto the metallic powder particles to form the coating.
  9. 9. The method of claim 7 or 8, wherein the first heat treatment removes the coating from the metallic powder particles and incorporates the coating into the metal matrix.
  10. 10. The method of any one of claims 1-9, further comprising dispersing the metallic powder particles within the mixture solution by at least one of: applying pressure waves to the mixture solution, flowing a liquid jet through the mixture solution, or flowing an air jet through the mixture solution.
  11. I I. The method of claim 10, wherein the mandrel includes a non-horizontal surface.
  12. 12. The method of claim I I, wherein the dispersing further comprises directing the metallic powder particles within the mixture solution toward the non-horizontal surface.
  13. 13. The method of any one of claims 1-12, wherein an average particle size of the metallic powder particles in the mixture solution is between 0.1-20 micrometers.
  14. 14. The method of any one of claims 1-13, wherein the metallic powder particles comprise a mass fraction of between 30-70% for the composite electroformed component.
  15. 15. The method of any one of claims 1-14, wherein the metallic powder particles comprise a volume fraction of between 30-70 vol% for the composite electroformed component.
  16. 16. The method of any one of claims 1-15, wherein the composite electroformed component comprises a thickness between 0.5-10 mm.
  17. 17. A system for electroforming a component, comprising: an electroforming tank; a cathode located within the electroforming tank; a power source electrically coupled to the cathode; and a mixture solution within the electroforming tank comprising an electrolytic solution with dispersed metallic powder particles therein, the metallic powder particles having an average particle size between 1-1000 micrometers.
  18. 18. The system of claim 17, further comprising a set of flow controllers located within the electroforming tank and configured to agitate the mixture solution.
  19. 19. The system of claim 18, wherein the set of flow controllers comprises at least one of an ultrasonic device emitting ultrasonic pressure waves into the mixture solution, a liquid pump emitting a liquid jet into the mixture solution, or an air pump emitting an air jet into the mixture solution.
  20. 20. The system of claim 19, further comprising a dissolution tank having an anode electrically coupled to the power source, wherein the dissolution tank is fluidly coupled to the electroforming tank by at least one fluid conduit.
GB2217298.5A 2022-09-05 2022-11-18 Electroforming method and system Pending GB2622117A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3061525A (en) * 1959-06-22 1962-10-30 Platecraft Of America Inc Method for electroforming and coating
US4601795A (en) * 1985-03-27 1986-07-22 The United States Of America As Represented By Secretary Of Interior Alloy coating method
WO2006063431A1 (en) * 2004-12-17 2006-06-22 Integran Technologies Inc. Strong, lightweight article containing a fine-grained metallic layer
US20170067179A1 (en) * 2015-09-03 2017-03-09 King Fahd University Of Petroleum And Minerals Alumina-coated co-deposit and an electrodeposition method for the manufacture thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3061525A (en) * 1959-06-22 1962-10-30 Platecraft Of America Inc Method for electroforming and coating
US4601795A (en) * 1985-03-27 1986-07-22 The United States Of America As Represented By Secretary Of Interior Alloy coating method
WO2006063431A1 (en) * 2004-12-17 2006-06-22 Integran Technologies Inc. Strong, lightweight article containing a fine-grained metallic layer
US20170067179A1 (en) * 2015-09-03 2017-03-09 King Fahd University Of Petroleum And Minerals Alumina-coated co-deposit and an electrodeposition method for the manufacture thereof

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US20240309534A1 (en) 2024-09-19
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CA3183104A1 (en) 2024-03-05

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