US3652259A - Spherical powders - Google Patents

Spherical powders Download PDF

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Publication number
US3652259A
US3652259A US728923A US3652259DA US3652259A US 3652259 A US3652259 A US 3652259A US 728923 A US728923 A US 728923A US 3652259D A US3652259D A US 3652259DA US 3652259 A US3652259 A US 3652259A
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United States
Prior art keywords
particles
present
spherical
metal
copper
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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.)
Expired - Lifetime
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US728923A
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English (en)
Inventor
Walter V Knopp
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Olin Corp
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Olin Corp
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Publication date
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Publication of US3652259A publication Critical patent/US3652259A/en
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/065—Spherical particles

Definitions

  • ABSTRACT The instant disclosure teaches an improved process for obtain- [52] 0.5. CI. ..75/0.5 B, 75/0.5 BA, 75/265633, in dense spherical meml Particles characterized by coating the starting material with a weld-preventing material and heat- [5 l Int. Cl. B221 9/00, B29C 23/00 g the oated particles in a protective atmosphere.
  • a typical art process is the production of shot where the metal flows through an orifice in a thin stream which is then dispersed with high velocity jets of air, steam, water or heated gases.
  • shot may be produced by pouring molten metal on a rotating surface and then cooling with hot water.
  • An alternative method is to cut wire of a predetermined diameter into small pieces. These particles are then partially rounded in a disc mill. This method does insure close particle size; however, the particles are not truly spherical and the material is expensive.
  • the process of the present invention comprises:
  • the foregoing process readily obtains a high yield of rounded or spherical particles of predetermined size.
  • the foregoing process is characterized by its relative simplicity and by being inexpensive.
  • the particles obtained in accordance with the present invention are solid and rounded, are obtained in the desired particle size in a high yield, and are generally not hollow and generally do not have crevices.
  • the process of the present invention makes particles of closely controlled size in very high yields.
  • the process of the present invention makes spherical particles of materials and alloys which are not normally made.
  • the spherical particles may contain metallic additives which do not alloy and also non-metallic additives as well.
  • the particles prepared in accordance with the process of the present invention will have a very low oxygen content since melting is done under a protective atmosphere.
  • copper shot made in this way can be considered as OFHC copper.
  • the present invention may be readily employed with virtually any metallic material.
  • the metallic particles utilized in the process of the present invention should have a particle size larger than mesh.
  • the process of the present invention encompasses numerous modifications which provide a variety of methods for obtaining the starting material of the present invention. These modifications greatly enlarge the commercial applicability of the process of the present invention and represent important facets of the process of the present invention. These will be discussed in greater detail herein below.
  • the pure metal or alloys may be used.
  • mixtures of metals may be also conveniently employed or their reducible oxides.
  • Others which may be used include aluminum or aluminum alloys, ferrous materials, noble metals, precious metals, titanium, magnesium, zinc, nickel, beryllium, solders, and so forth.
  • the metallic particles are then coated with any desired weld-preventing material.
  • the particular weld-preventing material is naturally dependent upon the type of metal particles employed. For example, one may readily employ talc, lime, graphite, alumina, titanium dioxide, zirconium oxide, flour, non-reducible oxides, and mixtures thereof.
  • the binder material may be any material which will readily adhere to the outer surface of the metallic particles and to which the weldpreventing material will readily adhere.
  • the binder should volatilize above- F. and should volatilize at least 200 F. below the melting point of the metal being used.
  • the particular binder which is employed is not especially critical. For example, one may readily employ brazing fluxes compatible with the base material, waxes, e.g., polyethylene glycol, metal stearates, stearic acid, organic binders, gums, etc. In general, the particular choice of the binder will be influenced by the metal particles being employed.
  • the binder material should volatilize within the foregoing temperature range.
  • the coated masses are heated in a protective atmosphere to form a plurality of solid, dense, spherical, coherent, metal spheres. It is preferred to heat the masses in two stages, with the first stage being to a temperature above the volatilized temperature of the binder in order to volatilize the binder, and the second stage being above the melting point of the metal particles in order to form the fully dense spherical particle of the present invention.
  • first heating step one should heat above the volatilization-temperature of the binder, but below the melting point of the metal and in the second heating step, one should raise the temperature to above the melting point of the metal particle.
  • the protective atmosphere which is employed may be neutral on the reducing side.
  • a lean gas or a strongly reducing gas For example, one may employ hydrogen, carbon monoxide, dissociated ammonia, nitrogen, argon, helium and so forth.
  • a vacuum or partial vacuum may be used as a protective atmosphere.
  • the particles are cooled and the weld-preventing material removed. Frequently, it is only necessary to screen the particles in order to remove the weldpreventing material. If desired, one may wash and etch the materials.
  • the process of the present invention contemplates a variety of ways to obtain the starting material, i.e., a variety of ways for providing the starting metallic particles having a particle size larger than 100 mesh. Some of these methods will be discussed hereinbelow.
  • either a fine metallic powder or a coarse metallic powder may be sintered together to form a cake.
  • the sintering process may also be conveniently utilized to reduce the oxygen content of the metal powder.
  • either copper oxide or a fine copper powder may be furnaced to reduce the oxygen content and to sinter them together to form a coarser particle or cake and to increase the density.
  • the sintered cake may then be mechanically broken up to produce a material having a particle size larger than 100 mesh.
  • the material may then be processed in accordance with the present invention.
  • a fine metallic powder can be agglomerated, but not necessarily sintered, using a plastic material which will readily volatilize during subsequent processing.
  • the agglomerated cake would then be broken up to desired size in the manner described above with respect to the sintered cake.
  • An alternate modification in the process of the present invention utilizes material obtained by disintegrating a stream of molten metal by the use of a fluid.
  • a molten stream of copper can be disintegrated by impingement with water or air.
  • the shot material obtained will contain some oxygen; therefore, when the material is heated up in an atmosphere with hydrogen, the shot will crack because of the pressure of the water vapor formed, i.e., hydrogen embrittlement. If one were to attempt to braze this material, the attempt would be unsuccessful, since the brazing material will flow into the crevices.
  • the shot material may be corrected by treating it in accordance with the process of the present invention. The shot which is treated thereby will contain no cracks and will contain substantially no oxygen. Hence, during brazing, the brazing material will remain on the surface.
  • EXAMPLE I there was provided 2,000 grams of copper powder having a particle size below 100 mesh.
  • the copper powder was furnaced at a temperature of about l,400 F. to sinter it together to form a cake and to reduce the oxygen content.
  • the sintered cake was broken up to produce a coarse, substantially oxygen-free, copper powder having a mesh size above 100 mesh.
  • the material which had a particle size in the range of -50+80 mesh was separated from the remainder of the material by screening and comprised approximately 75 percent of the total.
  • the 50+80 mesh material was moistened with polyethylene glycol and coated with tale. The coated masses were heated in dissociated ammonia at about 800 F. for minutes, thereby volatilizing the polyethylene glycol.
  • the masses were then heated at l,200 F. for 15 minutes to form the uniform, dense, spherical, solid particles of the present invention. Approximately 75 percent of the particles obtained were in the desired 50+80 size range. The size distribution of the resulting particles is given in Table 1 below.
  • Example II TABLE 1 Particle Size Yield, Percent EXAMPLE ll Example I was repeated with the exception that the desired ultimate product was in the size range of 40+60 mesh and the starting material was in this size range. The ultimate yield of product in the -40+60 range was approximately 70 percent. The product size distribution is shown in Table II below. The resulting material was spherical, fully dense and free of oxygen.
  • the starting material was obtained by impinging air on a molten stream of copper.
  • Starting material in the size range of 30+80 mesh was wetted with polyethylene glycol and coated with tale in a manner after Example l.
  • the coated material was then heated in a manner after Example I to yield spherical, fully dense shot having no cracks and having substantially no oxygen therein.
  • the resultant shot was brazed effectively.
  • untreated material could not be brazed in view of the cracks appearing on the surface.
  • a process for obtaining dense, spherical metal powders which comprises:
  • step (A) A process according to claim 1 wherein the starting material metallic particles in step (A) are obtained by sintering a plurality of metal particles to form a cake and mechanically breaking up said cake.
  • a process according to claim 3 wherein the particles which are sintered have a particle size smaller than 100 mesh.
  • step (A) is obtained by disintegrating a stream of molten metal by impinging said stream with a fluid.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
US728923A 1968-05-14 1968-05-14 Spherical powders Expired - Lifetime US3652259A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US72892368A 1968-05-14 1968-05-14

Publications (1)

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US3652259A true US3652259A (en) 1972-03-28

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US728923A Expired - Lifetime US3652259A (en) 1968-05-14 1968-05-14 Spherical powders

Country Status (4)

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US (1) US3652259A (fr)
DE (1) DE1801829B2 (fr)
FR (1) FR96445E (fr)
GB (1) GB1176275A (fr)

Cited By (34)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3909241A (en) * 1973-12-17 1975-09-30 Gte Sylvania Inc Process for producing free flowing powder and product
US4174211A (en) * 1977-04-23 1979-11-13 Mitsubishi Kinzoku Kabushiki Kaisha Process for manufacturing composite powder for powder metallurgy
US4202686A (en) * 1976-12-27 1980-05-13 Mitsubishi Kinzoku Kabushiki Kaisha Process for manufacturing fine powder of metal
US4606869A (en) * 1984-08-27 1986-08-19 The New Jersey Zinc Company Method of making air atomized spherical zinc powder
US4731111A (en) * 1987-03-16 1988-03-15 Gte Products Corporation Hydrometallurical process for producing finely divided spherical refractory metal based powders
US4772315A (en) * 1988-01-04 1988-09-20 Gte Products Corporation Hydrometallurgical process for producing finely divided spherical maraging steel powders containing readily oxidizable alloying elements
US4778517A (en) * 1987-05-27 1988-10-18 Gte Products Corporation Hydrometallurgical process for producing finely divided copper and copper alloy powders
US4781753A (en) * 1987-01-29 1988-11-01 Gte Products Corporation Process for producing fine spherical particles from non-flowing powders
US4787934A (en) * 1988-01-04 1988-11-29 Gte Products Corporation Hydrometallurgical process for producing spherical maraging steel powders utilizing spherical powder and elemental oxidizable species
US4802915A (en) * 1988-04-25 1989-02-07 Gte Products Corporation Process for producing finely divided spherical metal powders containing an iron group metal and a readily oxidizable metal
US4816067A (en) * 1988-06-20 1989-03-28 Gte Products Corporation Process for producing fine spherical particles
US4859237A (en) * 1988-01-04 1989-08-22 Gte Products Corporation Hydrometallurgical process for producing spherical maraging steel powders with readily oxidizable alloying elements
US4927456A (en) * 1987-05-27 1990-05-22 Gte Products Corporation Hydrometallurgical process for producing finely divided iron based powders
US5102454A (en) * 1988-01-04 1992-04-07 Gte Products Corporation Hydrometallurgical process for producing irregular shaped powders with readily oxidizable alloying elements
US5114471A (en) * 1988-01-04 1992-05-19 Gte Products Corporation Hydrometallurgical process for producing finely divided spherical maraging steel powders
US6290746B1 (en) * 1998-11-26 2001-09-18 Sumitomo Special Metals Co., Ltd. Method of producing metal ball and semiconductor package
US6514846B2 (en) * 2000-12-08 2003-02-04 Tao-Kuang Chang Method of fabricating soldering balls for semiconductor encapsulation
US10639712B2 (en) 2018-06-19 2020-05-05 Amastan Technologies Inc. Process for producing spheroidized powder from feedstock materials
US20200266170A1 (en) * 2016-01-19 2020-08-20 Namics Corporation Resin composition, conductive copper paste, and semiconductor device
US10987735B2 (en) 2015-12-16 2021-04-27 6K Inc. Spheroidal titanium metallic powders with custom microstructures
US11148202B2 (en) 2015-12-16 2021-10-19 6K Inc. Spheroidal dehydrogenated metals and metal alloy particles
US11311938B2 (en) 2019-04-30 2022-04-26 6K Inc. Mechanically alloyed powder feedstock
US11590568B2 (en) 2019-12-19 2023-02-28 6K Inc. Process for producing spheroidized powder from feedstock materials
US11611130B2 (en) 2019-04-30 2023-03-21 6K Inc. Lithium lanthanum zirconium oxide (LLZO) powder
US11717886B2 (en) 2019-11-18 2023-08-08 6K Inc. Unique feedstocks for spherical powders and methods of manufacturing
US11855278B2 (en) 2020-06-25 2023-12-26 6K, Inc. Microcomposite alloy structure
US11919071B2 (en) 2020-10-30 2024-03-05 6K Inc. Systems and methods for synthesis of spheroidized metal powders
US11963287B2 (en) 2020-09-24 2024-04-16 6K Inc. Systems, devices, and methods for starting plasma
US12040162B2 (en) 2022-06-09 2024-07-16 6K Inc. Plasma apparatus and methods for processing feed material utilizing an upstream swirl module and composite gas flows
US12042861B2 (en) 2021-03-31 2024-07-23 6K Inc. Systems and methods for additive manufacturing of metal nitride ceramics
US12094688B2 (en) 2022-08-25 2024-09-17 6K Inc. Plasma apparatus and methods for processing feed material utilizing a powder ingress preventor (PIP)
US12195338B2 (en) 2022-12-15 2025-01-14 6K Inc. Systems, methods, and device for pyrolysis of methane in a microwave plasma for hydrogen and structured carbon powder production
US12261023B2 (en) 2022-05-23 2025-03-25 6K Inc. Microwave plasma apparatus and methods for processing materials using an interior liner
US12406829B2 (en) 2021-01-11 2025-09-02 6K Inc. Methods and systems for reclamation of Li-ion cathode materials using microwave plasma processing

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4731110A (en) * 1987-03-16 1988-03-15 Gte Products Corp. Hydrometallurigcal process for producing finely divided spherical precious metal based powders
US4723993A (en) * 1987-03-23 1988-02-09 Gte Products Corporation Hydrometallurgical process for producing finely divided spherical low melting temperature metal based powders
CN107282919A (zh) * 2017-06-14 2017-10-24 南京师范大学 一种纳米铝粉/石蜡含能复合粒子及其制备方法和应用

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2969281A (en) * 1958-01-17 1961-01-24 American Metal Climax Inc Process for making spherical metal particles
US3036938A (en) * 1958-06-10 1962-05-29 Percy W Hudson Method of purifying and spherifying copper powder
US3214262A (en) * 1961-11-24 1965-10-26 Huettenwerk Oberhausen Ag Process for producing dense iron powders from sponge iron
US3214264A (en) * 1959-10-23 1965-10-26 Huettenwerk Oberhausen Ag Treatment of metal oxides
US3434831A (en) * 1966-09-08 1969-03-25 Olin Mathieson Fabrication of spherical powders

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2969281A (en) * 1958-01-17 1961-01-24 American Metal Climax Inc Process for making spherical metal particles
US3036938A (en) * 1958-06-10 1962-05-29 Percy W Hudson Method of purifying and spherifying copper powder
US3214264A (en) * 1959-10-23 1965-10-26 Huettenwerk Oberhausen Ag Treatment of metal oxides
US3214262A (en) * 1961-11-24 1965-10-26 Huettenwerk Oberhausen Ag Process for producing dense iron powders from sponge iron
US3434831A (en) * 1966-09-08 1969-03-25 Olin Mathieson Fabrication of spherical powders

Cited By (44)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3909241A (en) * 1973-12-17 1975-09-30 Gte Sylvania Inc Process for producing free flowing powder and product
US4202686A (en) * 1976-12-27 1980-05-13 Mitsubishi Kinzoku Kabushiki Kaisha Process for manufacturing fine powder of metal
US4174211A (en) * 1977-04-23 1979-11-13 Mitsubishi Kinzoku Kabushiki Kaisha Process for manufacturing composite powder for powder metallurgy
US4606869A (en) * 1984-08-27 1986-08-19 The New Jersey Zinc Company Method of making air atomized spherical zinc powder
US4781753A (en) * 1987-01-29 1988-11-01 Gte Products Corporation Process for producing fine spherical particles from non-flowing powders
US4731111A (en) * 1987-03-16 1988-03-15 Gte Products Corporation Hydrometallurical process for producing finely divided spherical refractory metal based powders
US4927456A (en) * 1987-05-27 1990-05-22 Gte Products Corporation Hydrometallurgical process for producing finely divided iron based powders
US4778517A (en) * 1987-05-27 1988-10-18 Gte Products Corporation Hydrometallurgical process for producing finely divided copper and copper alloy powders
US4787934A (en) * 1988-01-04 1988-11-29 Gte Products Corporation Hydrometallurgical process for producing spherical maraging steel powders utilizing spherical powder and elemental oxidizable species
US4859237A (en) * 1988-01-04 1989-08-22 Gte Products Corporation Hydrometallurgical process for producing spherical maraging steel powders with readily oxidizable alloying elements
US4772315A (en) * 1988-01-04 1988-09-20 Gte Products Corporation Hydrometallurgical process for producing finely divided spherical maraging steel powders containing readily oxidizable alloying elements
US5102454A (en) * 1988-01-04 1992-04-07 Gte Products Corporation Hydrometallurgical process for producing irregular shaped powders with readily oxidizable alloying elements
US5114471A (en) * 1988-01-04 1992-05-19 Gte Products Corporation Hydrometallurgical process for producing finely divided spherical maraging steel powders
US4802915A (en) * 1988-04-25 1989-02-07 Gte Products Corporation Process for producing finely divided spherical metal powders containing an iron group metal and a readily oxidizable metal
US4816067A (en) * 1988-06-20 1989-03-28 Gte Products Corporation Process for producing fine spherical particles
US6290746B1 (en) * 1998-11-26 2001-09-18 Sumitomo Special Metals Co., Ltd. Method of producing metal ball and semiconductor package
US6514846B2 (en) * 2000-12-08 2003-02-04 Tao-Kuang Chang Method of fabricating soldering balls for semiconductor encapsulation
US12214420B2 (en) 2015-12-16 2025-02-04 6K Inc. Spheroidal titanium metallic powders with custom microstructures
US10987735B2 (en) 2015-12-16 2021-04-27 6K Inc. Spheroidal titanium metallic powders with custom microstructures
US11148202B2 (en) 2015-12-16 2021-10-19 6K Inc. Spheroidal dehydrogenated metals and metal alloy particles
US11577314B2 (en) 2015-12-16 2023-02-14 6K Inc. Spheroidal titanium metallic powders with custom microstructures
US11839919B2 (en) 2015-12-16 2023-12-12 6K Inc. Spheroidal dehydrogenated metals and metal alloy particles
US20200266170A1 (en) * 2016-01-19 2020-08-20 Namics Corporation Resin composition, conductive copper paste, and semiconductor device
US10892242B2 (en) * 2016-01-19 2021-01-12 Namics Corporation Resin composition, conductive copper paste, and semiconductor device
US11273491B2 (en) 2018-06-19 2022-03-15 6K Inc. Process for producing spheroidized powder from feedstock materials
US11465201B2 (en) 2018-06-19 2022-10-11 6K Inc. Process for producing spheroidized powder from feedstock materials
US11471941B2 (en) 2018-06-19 2022-10-18 6K Inc. Process for producing spheroidized powder from feedstock materials
US12311447B2 (en) 2018-06-19 2025-05-27 6K Inc. Process for producing spheroidized powder from feedstock materials
US10639712B2 (en) 2018-06-19 2020-05-05 Amastan Technologies Inc. Process for producing spheroidized powder from feedstock materials
US11611130B2 (en) 2019-04-30 2023-03-21 6K Inc. Lithium lanthanum zirconium oxide (LLZO) powder
US11633785B2 (en) 2019-04-30 2023-04-25 6K Inc. Mechanically alloyed powder feedstock
US11311938B2 (en) 2019-04-30 2022-04-26 6K Inc. Mechanically alloyed powder feedstock
US11717886B2 (en) 2019-11-18 2023-08-08 6K Inc. Unique feedstocks for spherical powders and methods of manufacturing
US11590568B2 (en) 2019-12-19 2023-02-28 6K Inc. Process for producing spheroidized powder from feedstock materials
US12176529B2 (en) 2020-06-25 2024-12-24 6K Inc. Microcomposite alloy structure
US11855278B2 (en) 2020-06-25 2023-12-26 6K, Inc. Microcomposite alloy structure
US11963287B2 (en) 2020-09-24 2024-04-16 6K Inc. Systems, devices, and methods for starting plasma
US11919071B2 (en) 2020-10-30 2024-03-05 6K Inc. Systems and methods for synthesis of spheroidized metal powders
US12406829B2 (en) 2021-01-11 2025-09-02 6K Inc. Methods and systems for reclamation of Li-ion cathode materials using microwave plasma processing
US12042861B2 (en) 2021-03-31 2024-07-23 6K Inc. Systems and methods for additive manufacturing of metal nitride ceramics
US12261023B2 (en) 2022-05-23 2025-03-25 6K Inc. Microwave plasma apparatus and methods for processing materials using an interior liner
US12040162B2 (en) 2022-06-09 2024-07-16 6K Inc. Plasma apparatus and methods for processing feed material utilizing an upstream swirl module and composite gas flows
US12094688B2 (en) 2022-08-25 2024-09-17 6K Inc. Plasma apparatus and methods for processing feed material utilizing a powder ingress preventor (PIP)
US12195338B2 (en) 2022-12-15 2025-01-14 6K Inc. Systems, methods, and device for pyrolysis of methane in a microwave plasma for hydrogen and structured carbon powder production

Also Published As

Publication number Publication date
FR96445E (fr) 1972-06-30
DE1801829B2 (de) 1971-12-02
DE1801829A1 (de) 1971-02-25
GB1176275A (en) 1970-01-01

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