WO2023187550A1 - Procédé consistant à revêtir des particules de poudre de fer de nanoparticules de silice - Google Patents

Procédé consistant à revêtir des particules de poudre de fer de nanoparticules de silice Download PDF

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Publication number
WO2023187550A1
WO2023187550A1 PCT/IB2023/052746 IB2023052746W WO2023187550A1 WO 2023187550 A1 WO2023187550 A1 WO 2023187550A1 IB 2023052746 W IB2023052746 W IB 2023052746W WO 2023187550 A1 WO2023187550 A1 WO 2023187550A1
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WO
WIPO (PCT)
Prior art keywords
iron powder
powder particles
coated
silica
particles
Prior art date
Application number
PCT/IB2023/052746
Other languages
English (en)
Inventor
Abhijeet Premkumar Moon
Sista Kameswara Srikar
Srinivas Dwarapudi
Gourav Ranjan Sinha
Bilal Murtuza PIRJADE
Sai Krishna Reddy ADAPA
Original Assignee
Tata Steel Limited
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 Tata Steel Limited filed Critical Tata Steel Limited
Publication of WO2023187550A1 publication Critical patent/WO2023187550A1/fr

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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
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102—Metallic powder coated with organic material
    • 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
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/108—Mixtures obtained by warm mixing
    • 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
    • B22F1/16—Metallic particles coated with a non-metal
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30—Process control
    • B22F10/34—Process control of powder characteristics, e.g. density, oxidation or flowability
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • B22F3/225—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials

Definitions

  • TITLE “A METHOD OF COATING IRON POWDER PARTICLES WITH NANO SILICA PARTICLES”
  • the present disclosure relates in general to the field of material science and metallurgy. Particularly, but not exclusively, the present disclosure relates to coating of iron powder particles. Further embodiments of the disclosure disclose a method of coating silica on iron powder particles for improving oxidation resistance and flow characteristics.
  • Powder coatings on iron (Fe) powder particles are usually performed to enhance properties of such iron powder particles including, but not limited to, corrosion resistance, electrical resistivity, microwave absorbing properties and the like.
  • powder coatings of the iron powder particles may provide environmental protection such as humidity, moisture, salts, dirt, or debris etc.
  • the powder coating may be adapted to hermetically seal the iron powder particles from moisture or other environmental conditions and protect iron powder particles from any reactions that occur due to surface reactivity.
  • insulation between iron powder particles in the final coated iron powder particles is also desired for manufacturing products including, but not limited to, magnetic core.
  • the iron powder particles are required to be coated with an insulating material.
  • the coated iron powder particles are conventionally known to have poor flowability as compared to the iron powder particles without coating.
  • the present disclosure is directed to overcome one or more limitations stated above or any other limitation associated with the prior arts.
  • the present disclosure discloses a method for coating silica particles on iron powder particles which results in improvement of oxidation resistance by attaching/bonding silica particles on surface of the iron powder particles.
  • the present disclosure also aids in quick and simpler way of coating the silica particles on the iron powder particles, which may be suitable for powder metallurgy and other related component manufacturing processes including metal injection moulding (MIM) and additive manufacturing (AM).
  • MIM metal injection moulding
  • AM additive manufacturing
  • a method for producing iron powder particles with silica coating includes steps of mixing iron powder particles and a binder for a first predetermined time to form encapsulated mixture.
  • the encapsulated mixture is then mixed with silica by mechanical mixing process at a predetermined temperature for a second predetermined time to form a coated mixture.
  • the coated mixture is cooled to form coated iron powder particles.
  • mixing of iron powder particles and binder is carried out at atmospheric temperature.
  • the first predetermined time ranges from 2 minutes to 5 minutes at atmospheric temperature for the encapsulated mixture.
  • the second predetermined time ranges from 15 minutes to 35 minutes at elevated temperature from 60°C to 180 0 C for the coated mixture.
  • the coated mixture is cooled to room temperature under open atmospheric conditions.
  • the average particle size of the iron powder particles is in a range of 5 - 100 pm.
  • the carbon content of iron powder particles in wt% ranges from 0.05-0.8, oxygen content of the iron powder is by wt% 0.3-0.8 and total iron content in the iron powder particles is at least 96%.
  • the binder in the encapsulated mixture is in the range of 0.001-0.5% (in wt%) based on the average particle size of the iron powder particles.
  • the silica is added at a proportion ranging from 0.25 - 2.0% by wt.% to the encapsulated mixture, to form the coated mixture.
  • the binder is at least one of wax consisting from a group of camuba wax, mustard oil, olive oil, and castor oil, which is added in a range of 0.01 - 0.3% by wt.%.
  • mechanical mixing process is based on at least one of coating in a double cone, V, W or Y-type blenders or cylindrical -type or Nauta mixer, or hybridizers.
  • coated iron powder particles comprising iron powder particles, comprising carbon composition in the range of 0.02 to 1.0 % (in weight %), oxygen content of the iron powder is by wt% 0.3-0.8 and total iron content to be at least 96%/.
  • the coating has a composition including, by weight percentage (wt%) of, silica 0.25 wt% to 2 wt% and binder 0.001 wt% to 0.5 wt%.
  • the coating is formed by mixing, iron powder particles and a binder for a first predetermined time to form encapsulated mixture.
  • the encapsulated mixture is mixed with silica by mechanical mixing process at a predetermined temperature for a second predetermined time to form a coated mixture, wherein the mixing results in silica being coated using wax or oil-based binders.
  • the coated mixture is cooled to form the coated iron powder particles.
  • the average size of iron powder particles ranges from 5-100 pm.
  • the total iron content in the iron powder particles is at least 96%.
  • the binder is at least one of wax consisting from a group of camuba wax, mustard oil, olive oil, and castor oil, which is added in a range of 0.01 - 0.3% by wt.%.
  • the total silica content in the silica particles is at least 99.8% and the average size of silica particles is in the range of 0.01 pm to 30 pm.
  • Figure 1 illustrates an apparatus for coating iron powder particles, according to an exemplary embodiment of the present disclosure.
  • Figure 2 is a flowchart illustrating a method for producing coated iron powder particles, according to exemplary embodiments of the present disclosure.
  • Figure 3 illustrates schematic diagram of the method of Figure 2, according to exemplary embodiments of the present disclosure.
  • Figures 4a and 4b illustrate micrographs of dense close rounded iron powder particles and porous irregular iron powder particles from a scanning electron microscope (SEM), according to exemplary embodiments of the present disclosure.
  • FIGS. 5a and 5b illustrate micrographs from a scanning electron microscope (SEM) and a transmission electron microscope (TEM) pertaining to nano-silica particles, in accordance with exemplary embodiments of the present disclosure.
  • Figures 6a and 6b illustrate images from the scanning electron microscope (SEM) of uncoated iron powder particles and the coated iron powder particles with respective energy dispersive X-ray spectroscopy (EDS) analysis locations, in accordance with exemplary embodiments of the present disclosure.
  • Figure 7 illustrates field emission scanning electron microscope (FE-SEM) image of silica coated iron powder particle surface with energy dispersive X-ray spectroscopy (EDS) mapping, according to an exemplary embodiment of the present disclosure.
  • SEM scanning electron microscope
  • EDS energy dispersive X-ray spectroscopy
  • Figure 8 illustrates graph of thermogravimetric analysis (TGA) oxidation studies on uncoated iron powder particles and silica coated iron powder particles, according to exemplary embodiments of the present disclosure.
  • Embodiments of the present disclosure discloses silica coating on surface of iron powder particles and a method for coating iron powder particles. Coating of iron powder particles improves oxidation resistance, corrosion resistance, flow characteristics, electric resistivity of such iron power particles.
  • the method of present disclosure discloses producing silica coated iron powder particles, with improved insulating and oxidation characteristics. The present disclosure is directed towards producing the silica coated iron powder particles and contaminant free iron powder particles which are widely required in powder metallurgical processing, metal injection molding (MIM) and additive manufacturing (AM) processes.
  • MIM metal injection molding
  • AM additive manufacturing
  • Figures 1 and 2 are exemplary embodiments of the present disclosure illustrating an apparatus and flowchart depicting method of producing coated iron powder particles.
  • corrosion resistance, oxidation resistance, surface characteristics and flow characteristics of the coated iron powder particles may be improved.
  • the method steps described and detailed in view of Figure 2 for producing the coated iron powder particles, and order in which such method steps are described is not intended to be construed as a limitation. Additionally, individual blocks may be deleted from the methods without departing from the scope of the subject matter described herein.
  • the method is particularly applicable to the coated iron powder particles with silica powder, and it may also be extended to other type of powder coatings of iron powder particles as well.
  • Figure 1 illustrates a mixing apparatus where the iron powder particles, the binder and the silica particles are added to a mixing container (101) of the mixing apparatus.
  • a mixing apparatus includes base plate (106), hot plate (105), mechanical mixing rod (102), mixing container (101), top cover (103), blades (104).
  • the mixing container (101) is placed on the hot plate (105) which is rested on a base plate (106).
  • Iron powder particles and binder are introduced into the mixing container (101) and mixed to get the homogeneous binder encapsulated mixture.
  • mixing can be performed by either hand or with the help of mechanical mixing rod (102).
  • the mechanical mixing rod (102) consists of blades (104) attached to the rod and the blades (104) ensures uniform mixing of the iron powder particles and the binder.
  • Mixing container consists of a top cover (103) which conceals the mixing container (101) and allows the mechanical mixing rod (102) through the top cover (103). Further, the silica particles are added to the binder encapsulated mixture and then the hot plate (105) is operated at elevated temperature and the mixing continuous for a predefined time to form the silica coated iron powder particles.
  • the mixing container (101) placed above the hot plate (105) which is unidirectional, and the uniform heating of the mixture takes place radially.
  • the block 201 includes mixing of the iron powder particles and the binder for a first predetermined time to form an encapsulated mixture.
  • the term “encapsulate” may refer to coating forming a thin cover of the binder on an outer surface of the iron powder particles, where such coating may cover substantial portion of the iron powder particles.
  • such covering of the binder on the iron powder particles may range from at least 51% of the outer surface of the iron powder particles.
  • the iron powder particles are in the form of reduced or atomized and are highly pure in nature as the total iron content is greater than 98%. Further, the iron powder particles are either dense close rounded in morphology (as shown in figure 4a) or porous irregular in nature (as shown in figure 4b).
  • the carbon content of iron powder particles ranges from 0.05 wt% - 0.8 wt% and the total oxygen content in the iron powder particles ranges from 0.3 wt% to 0.8 wt%. Further, the average size of the iron powder particles ranges from 5 - 100 pm.
  • the binder is configured to impart adhesion between the iron powder particles under wet conditions, thereby increasing binding ability, plasticity and compactibility.
  • the binder may be at least one of wax or oil-based binders, which help in binding and coating particles on the iron powder particles.
  • the binder may be camuba wax which may be used to bind the coated particles on the surface of iron powder particles.
  • the waxes are able to liquify in the range of 80°C-100°C and may be smeary and slow drying in nature.
  • binders employable for coating as per the present disclosure may extend to include plant-based binders in the form of oil such as, but not limited to, castor oil, olive oil, mustard oil, almond oil, or mineral oils including, but not limited to, silicone oil and the like.
  • the binder composition is chosen such that the binder includes properties which are able to impart durability and may be easy to apply.
  • the binder may be employed in the range of 0.001 wt% - 0.5 wt% and amount of the binder to be used depends on various factors such as size, surface roughness, specific surface area, morphology and particle size distribution of coating particles and iron powder particles.
  • the binder is added in a range of 0.01 - 0.3% by wt.% to the iron powder particles.
  • the mechanical mixing of iron powder particles and the binder in a mixing container (shown in Figure 1) at first predetermined time forms homogenised binder encapsulated mixture.
  • mixing the iron powder particles with the binder increases glueyness characteristics of the surface of the iron powder particles.
  • the first predetermined time ranges from 2 minutes to 5 minutes and mixing of the iron powder particles and the binder takes place under atmospheric temperature.
  • the mixing process takes place in at least one of double cone, V, W or Y- type blenders or cylindrical-type blender or Nauta mixer, or hybridizers.
  • the silica particles are added to the encapsulated mixture and mixed at a predetermined temperature for second predetermined time.
  • the predetermined temperature ranges from 60°C to 180°C and the predetermined time ranges from 15 minutes to 35 minutes.
  • the silica particles are in amorphous form and are used for coating on the surface of the encapsulated mixture.
  • the average silica particle size ranging from 0.01 pm to 30 pm and the bulk density of silica particles ranges around 400 g/L or less.
  • the purity of silica particles is greater than 99.8%.
  • the mixture quantity in the mixing chamber not to be exceeded greater than one-half of the capacity of the mixing chamber. Further, size difference between the iron powders and silica particles having more than seven times to enable better surface coating properties on each powder particle.
  • the silica particles are added to the mixture depending on coating thickness and final silica composition desired in the coated iron powder particles. Further, higher percentage of silica addition results in a risk of silica segregation in the mixture and the silica particles may remain unbonded with the iron powder particles. However, with lower percentage addition of the silica particles, there may not be enough silica available to have an effective surface coating on the iron powder particles.
  • the silica particles are added in the range of 0.25- 2.0% (in wt.%) depending on the particle size, morphology, character of the host particles, and the coating process is designed based on the desired coating thickness and surface coverage requirement on the iron powder particles.
  • the silica particles are added to the encapsulated mixture and such mixture is either manually or mechanically mixed at a temperature range of 60°C to 180°C for 15 minutes to 35 minutes.
  • the silica particles are attached to the encapsulated mixture.
  • progressive hot mechanical mixing results in entire mixture being non-sticky and coated with the silica particles due to combination of shear mixing and internal shear forces between the iron powder particles and the silica particles.
  • the coated mixture is cooled to form the coated iron powder particles, where the encapsulated mixture is coated by the silica particles.
  • the coated iron powder particles are allowed to cool down to room temperature under open atmospheric conditions. Further, mixing step is performed till temperature reaches below 45°C to avoid overheating or localized heating of the iron powder particles. In an embodiment, mixing of the coated iron powder particles may be performed till temperature reaches room temperature.
  • the iron powder particles to be coated are either dense rounded or porous irregular in morphology. Further, the iron powder particles are produced by either atomization or by reduction method.
  • the SEM micrograph shows that the iron powder particles having dense close rounded morphology and in Figure 4b, the SEM micrograph shows that the iron powder particles are porous and irregular in morphology.
  • Figure 5a and 5b shows the SEM and TEM micrographs of silica particles indicating the fine sized particles which are used for coating iron powder particles.
  • Figure 6a and 6b shows the scanning electron microscope (SEM) image of uncoated iron powder particles and silica coated iron powder particles with respective energy dispersive spectroscopy (EDS) locations.
  • SEM scanning electron microscope
  • EDS energy dispersive spectroscopy
  • Table 3 shows the results of Energy dispersive spectroscopy (EDS) point analysis at locations indicated in Figure 6a and 6b. Further, EDS examination obtained on the surface of the uncoated and coated iron powder particles shows clear compositional differences as seen in Table 3.
  • EDS Energy dispersive spectroscopy
  • SEM mapping of the coated iron powder particles revealed that amorphous silica particles are in nano scale regime as shown in Figure 7.
  • thermogravimetric oxidation studies TGA reveals that the onset of oxidation of uncoated iron powder particles is close to 380°C and after silica coating, the onset of oxidation shifted to higher temperature close to 640°C. Therefore, the silica coating on iron powder particles has resulted in improvement in oxidation characteristics. Further, with relative increase in binder percentage in the coating mixture, the oxidation resistance of the silica coated iron particles has subtly improved further as seen in Figure 8.
  • TGA studies reveals that the sharp initial weight loss around 280°C on heating attributed to the decomposition temperature of the binder constituent.
  • the silica coated iron powder particles of the present disclosure may be used any application including but not limiting to powder metallurgical processing to MIM and AM manufacturing techniques and the like. Silica coated iron powder particles may be used in any other industrial manufacturing application.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

La présente divulgation divulgue un procédé de production de particules de poudre de fer revêtues de silice possédant des propriétés physiques améliorées. Le processus débute par le mélange de particules de poudre de fer et de cire ou d'un liant à base d'huile dans des mélangeurs selon une composition définie, dans un milieu atmosphérique ouvert à température ambiante. Ensuite, des particules de silice sont ajoutées aux particules de poudre de fer encapsulées par le liant et mélangées davantage jusqu'à atteindre une plage de températures prédéfinie. En outre, le mélange est refroidi jusqu'à ce qu'il atteigne une température ambiante, ce qui permet d'obtenir des particules de poudre de fer revêtues de silice. Ce processus permet d'obtenir des particules de poudre de fer revêtues présentant des caractéristiques améliorées de résistance à la corrosion et à l'oxydation, de surface et de fluidité.
PCT/IB2023/052746 2022-03-29 2023-03-21 Procédé consistant à revêtir des particules de poudre de fer de nanoparticules de silice WO2023187550A1 (fr)

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IN202231018302 2022-03-29
IN202231018302 2022-03-29

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Citations (9)

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Publication number Priority date Publication date Assignee Title
US20010035069A1 (en) * 1999-09-09 2001-11-01 Johan Arvidsson Powder composition
US20050139039A1 (en) * 2003-12-22 2005-06-30 Hoganas Ab Metal powder composition and preparation thereof
US20060000310A1 (en) * 2004-07-02 2006-01-05 Hoganas Ab Powder additive
US20080302209A1 (en) * 2005-12-30 2008-12-11 Hoganas Ab (Publ) Metallurgical Powder Composition
CN101346203A (zh) * 2005-12-30 2009-01-14 霍加纳斯股份有限公司 冶金粉末组合物
KR20090104140A (ko) * 2004-07-02 2009-10-05 회가내스 아베 유동 강화제로서 탄소 블랙을 포함하는 분말 야금학적 조성물
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JP2011213514A (ja) 2010-03-31 2011-10-27 Admatechs Co Ltd シリカ粒子材料、シリカ粒子材料含有組成物、およびシリカ粒子の表面処理方法

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US20010035069A1 (en) * 1999-09-09 2001-11-01 Johan Arvidsson Powder composition
US20050139039A1 (en) * 2003-12-22 2005-06-30 Hoganas Ab Metal powder composition and preparation thereof
US20060000310A1 (en) * 2004-07-02 2006-01-05 Hoganas Ab Powder additive
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CN101346203A (zh) * 2005-12-30 2009-01-14 霍加纳斯股份有限公司 冶金粉末组合物
US20100224025A1 (en) * 2007-09-14 2010-09-09 Jfe Steel Corporation Iron-based powder for powder metallurgy
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JP2011213514A (ja) 2010-03-31 2011-10-27 Admatechs Co Ltd シリカ粒子材料、シリカ粒子材料含有組成物、およびシリカ粒子の表面処理方法

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Title
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J. YANG: "Dry particle coating for improving the flowability of cohesive powders", POWDER TECHNOLOGY, vol. 158, 2005, pages 21 - 33, XP025306025, DOI: 10.1016/j.powtec.2005.04.032

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