GB2546284A - Powder formation - Google Patents

Powder formation Download PDF

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Publication number
GB2546284A
GB2546284A GB1600630.6A GB201600630A GB2546284A GB 2546284 A GB2546284 A GB 2546284A GB 201600630 A GB201600630 A GB 201600630A GB 2546284 A GB2546284 A GB 2546284A
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GB
United Kingdom
Prior art keywords
cooling tower
droplets
cooling
powder particles
coated region
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.)
Withdrawn
Application number
GB1600630.6A
Other versions
GB201600630D0 (en
Inventor
John Sutcliffe Christopher
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.)
Renishaw PLC
Original Assignee
Renishaw PLC
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
Application filed by Renishaw PLC filed Critical Renishaw PLC
Priority to GB1600630.6A priority Critical patent/GB2546284A/en
Publication of GB201600630D0 publication Critical patent/GB201600630D0/en
Publication of GB2546284A publication Critical patent/GB2546284A/en
Withdrawn legal-status Critical Current

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/16Metallic particles coated with a non-metal
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/17Metallic particles coated with metal
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/06Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/4417Methods specially adapted for coating powder
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523Pulsed gas flow or change of composition over time
    • C23C16/45525Atomic layer deposition [ALD]
    • C23C16/45555Atomic layer deposition [ALD] applied in non-semiconductor technology
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/084Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid combination of methods
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/086Cooling after atomisation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0892Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid casting nozzle; controlling metal stream in or after the casting nozzle
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00Aspects linked to processes or compositions used in powder metallurgy

Abstract

A method for producing powder particles having an outer coated region comprising atomising a first material, cooling droplets of the atomised material 5 in a cooling tower 3, and introducing a second material into the cooling tower to create a fluid volume containing the second material through which the cooled droplets pass such that powder particles are produced, coated by the second material or a material derived therefrom. Preferably the first, core material is a metal or alloy and the second, coating material is a rare earth metal. Droplets of the core material may be produced by introducing molten metal or alloy from a crucible 2 through a nozzle 4 into the tower under the influence of a gas stream (7, fig. 1b). The coating material is preferably introduced via injection nozzles 9 in the form of a liquid precursor which comes into contact with the heated substrate and reacts or decomposes to form a solid phase deposited thereon. Further materials may be introduced into the cooling tower at different temperature locations therein, to create powder particles with a series of discrete coating layers, either continuous or partial. An apparatus for producing coated powder particles is also claimed.

Description

POWDER FORMATION
The present invention relates to the production of coated powder particles, more specifically the invention relates to the production of coated metal particles produced by an atomisation process.
It is known to produce powdered material, through techniques such as crushing, grinding, electrolytic deposition and atomisation.
In recent times the advent of additive manufacturing that may involve selective laser melting (SLM) or selective laser sintering (SLS) of a metal powder as well as other techniques has made it desirable to closely control the properties of metal powders such as particle size which can be achieved using known atomisation based techniques. It also may be desirable to impart specific properties to powders and one method of doing this is introduce particular substances to the powders.
Introduction of substances to metal powders produced by atomisation can be achieved before atomisation by incorporation of the substance into a metal or an alloy however this method may still not give the powder the desired properties. A first aspect of the invention provides a method for producing powder particles having an outer coated region comprising atomising a first material, cooling droplets of the atomised material in a cooling tower, and introducing a second material into the cooling tower to create a fluid volume containing the second material through which the cooling droplets pass such that powder particles are produced comprising a coated region of the second material, or material derived from the second material.
Preferably, the outer coated region is a continuous layer forming the entire surface of the particle and may be the second material or a material derived from the second material. Alternatively, the outer coated region may only partially cover a core made up of the first material.
Preferably introduction of a second material comprises injection of the second material into the cooling tower, for example through an injection nozzle.
The second material may be a precursor.
The second material may be a liquid.
The method may comprise introduction of one or more further materials into the cooling tower, the or each additional further material may be the same or a different material to the second material. The further material or further materials may be introduced at different temperatures in the cooling tower to the temperature stage at which the second material is introduced. Introduction of the further material or further materials may comprise injection of the further material or further materials into the cooling tower, for example through an injection nozzle.
The second and/or each further material may be introduced at a specific temperature location into the cooling tower.
The outer coated region may comprise a series of discrete layers of different materials or a series of discrete layers where at least one layer of material is the same material as at least one other layer of material. At least one of the series of discrete layers may be a continuous layer encapsulating the particle and/or previously applied layer or layers, and/or at least one of the discrete layers may only partially cover the particle and/or previously applied layer or layers, or any variation of continuous and partial layers.
The second and/or each further material may comprise a rare earth metal.
The first material may comprise a metal or alloy.
The method may comprise chemical vapour deposition.
The method may comprise atomic layer deposition. A second aspect the invention provides an apparatus comprising a cooling tower, a device for producing droplets of a first material, the droplets passing through the cooling tower to form powder particles and further comprising a device for the introduction of a second material into a path of the cooling droplets as the cooling droplets pass through the cooling tower such that the powder particles are formed with an outer coated region of the second material or a material derived from a second material. A third aspect the invention provides a powder produced by the method of the first aspect of the invention and/or by the apparatus of the second aspect of the invention.
In order that the invention be better understood, it will now be described, by way of example only, with reference to the accompanying drawings, in which:
Figure la shows schematic representation of an atomisation tower according to an embodiment of the invention.
Figure lb shows a close up of the injection nozzle of the crucible.
In an embodiment of the invention an atomising tower 1 comprising a crucible 2 mounted on top of a cooling tower 3 and having a nozzle 4 in the bottom of the crucible 2. Atomised droplets of metal are formed by forcing molten metal or alloy through the nozzle of the crucible and a gas source 6 introduces a gas stream 7 into the resulting metal stream. The introduction of the gas serves to create turbulence in the metal stream as the gas expands due to heating and creates the atomised metal particles as is well known in the art. The invention is not limited to this method of producing atomised particles and other methods such as water atomisation, plasma atomisation, electrode induction gas atomisation (EIGA), centrifugal atomisation, vacuum atomisation, inert gas atomisation or any other method of producing atomised particles can be used.
As the metal particles pass through the cooling tower 3 they solidify and cool and can be collected in a collection chamber 8 as a powder from the bottom of the atomisation tower.
In the current embodiment chemical vapour deposition (CVD) is used to produce a coated powder however the invention is not limited to CVD and other embodiments of the invention may use other coating techniques such as atomic layer deposition (ALD). In CVD a precursor containing gas comes into contact with a heated substrate and the precursor reacts or decomposes to form a solid phase deposited on the substrate.
At locations along the tower 3 injectors 9 which may be in the form of nozzles are located, it may be the case that a single injector 9 or multiple injectors 9 are provided. These injectors 9 are provided to inject material into the cooling tower 3 and thus into the path of the atomised particles as they pass through the cooling tower 3.
The material injected in the current embodiment is a liquid precursor. Injection of the liquid precursor creates a volume of gas in the tower 1 through which the falling metal particles must travel and forms a coating on the particle. More than one injector 9 may be provided along the length of the tower and in one embodiment of the invention at each injector stage a different precursor may be injected while in another embodiment the same precursor may be used throughout the process and in yet a further embodiment at least one injection stage injects a precursor which has already been injected in a previous stage. The invention can therefore produce metal particles having a single coating or more than one coating as desired. The precursors used may comprise rare earth elements, organometallic compounds, halides, hydrides or any other suitable precursor.
The location of the material injection nozzles along the tower is crucial and depends on the temperature of the metal particles as the temperature of the metal particles influences the reactions which the precursors undergo and hence can provide different coatings even when the same precursor is injected by injection at different locations along the cooling tower. The nature of the precursor also influences the location of the injector nozzle as different precursors will need different metal particle temperatures to achieve the desired reactions and therefore produce a desired coating. In the current embodiment the nozzles are located at a position after the metal particles have solidified but while they are still above ambient temperature although in other embodiments of the invention this need not be the case.
In the above described embodiments an apparatus and method for producing coated metal or metal alloy powders, the invention is not limited to such applications and the scope of the invention is defined in the claims.

Claims (19)

Claims
1. A method for producing powder particles having an outer coated region comprising atomising a first material, cooling droplets of the atomised material in a cooling tower, and introducing a second material into the cooling tower to create a fluid volume containing the second material through which the cooling droplets pass such that powder particles are produced comprising a coated region of the second material, or material derived from the second material.
2. A method according to claim 1 wherein the outer coated region is a continuous layer forming the entire surface of the particle.
3. A method according to claim 1 wherein the outer coated region only partially covers a core made of the first material.
4. A method according to any preceding claim wherein introduction of a second material is injected through an injection nozzle.
5. A method according to any preceding claim wherein the second material is a precursor.
6. A method according to any preceding claims wherein the second material is a liquid.
7. A method according to any preceding claims comprising introduction of one or more further materials into the cooling tower.
8. A method according to claim 7 where the introduction of one or more further materials is the introduction of at least one material that is the same or a different material to the second material.
9. A method according to claims 7 or 8 wherein the or each further material is introduced at different temperature stage in the cooling tower to a temperature stage at which the second material is introduced.
10. A method according to any of claims 7 to 9 wherein the or each further material is introduced at a specific temperature location into the cooling tower.
11. A method according to any of claims 7 to 10 wherein the outer coated region comprises a series of discrete layers of different materials.
12. A method according to claim 11 wherein at least one layer of the series of discrete layers is continuous layer encapsulating the particle and/or previously applied layer or layers.
13. A method according to claims 11 or 12 wherein at least one of the discrete layers only partially covers the particle and/or previously applied layer or layers.
14. A method according to claim 13 when dependent on claim 12 wherein the discrete layers are any variation of continuous and partial layers.
15. A method according to any of claims 7 to 14 wherein the or each further material comprises a rare earth metal.
16. A method according to any preceding claim wherein the second material comprises a rare earth metal.
17. A method according to any preceding claim where the first material comprises a metal or alloy.
18. An apparatus comprising a cooling tower, a device for producing droplets of a first material, the droplets passing through the cooling tower and further comprising a device for the introduction of a second material into a path of the cooling droplets as the cooling droplets pass through the cooling tower such that the powder particles are formed with an outer coated region of the second material or a material derived from a second material.
19. A powder produced according to the method of claims 1 to 17 and/or the apparatus of claim 18.
GB1600630.6A 2016-01-13 2016-01-13 Powder formation Withdrawn GB2546284A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
GB1600630.6A GB2546284A (en) 2016-01-13 2016-01-13 Powder formation

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Application Number Priority Date Filing Date Title
GB1600630.6A GB2546284A (en) 2016-01-13 2016-01-13 Powder formation

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GB2546284A true GB2546284A (en) 2017-07-19

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR3051699A1 (en) * 2016-12-12 2017-12-01 Commissariat Energie Atomique ATOMIZATION AND CHEMICAL VAPOR DEPOSITION DEVICE
CN110931198A (en) * 2019-10-30 2020-03-27 宁波市普盛磁电科技有限公司 Preparation method of gas atomized iron-silicon-aluminum magnetic powder

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110382440A (en) * 2016-11-07 2019-10-25 科罗拉多大学董事会 The performance of improved technology grade ceramics

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1992005902A1 (en) * 1990-10-09 1992-04-16 Iowa State University Research Foundation, Inc. Environmentally stable reactive alloy powders and method of making same
EP0682578A1 (en) * 1993-02-06 1995-11-22 Osprey Metals Limited Production of powder
US20140373679A1 (en) * 2013-06-20 2014-12-25 Iowa State University Research Foundation, Inc. Passivation and alloying element retention in gas atomized powders

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1992005902A1 (en) * 1990-10-09 1992-04-16 Iowa State University Research Foundation, Inc. Environmentally stable reactive alloy powders and method of making same
EP0682578A1 (en) * 1993-02-06 1995-11-22 Osprey Metals Limited Production of powder
US20140373679A1 (en) * 2013-06-20 2014-12-25 Iowa State University Research Foundation, Inc. Passivation and alloying element retention in gas atomized powders

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR3051699A1 (en) * 2016-12-12 2017-12-01 Commissariat Energie Atomique ATOMIZATION AND CHEMICAL VAPOR DEPOSITION DEVICE
CN110931198A (en) * 2019-10-30 2020-03-27 宁波市普盛磁电科技有限公司 Preparation method of gas atomized iron-silicon-aluminum magnetic powder

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Publication number Publication date
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