EP3124634B1 - Prealloyed iron-based powder, a method for the manufacturing and use thereof and a sintered component - Google Patents

Prealloyed iron-based powder, a method for the manufacturing and use thereof and a sintered component Download PDF

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Publication number
EP3124634B1
EP3124634B1 EP15183275.5A EP15183275A EP3124634B1 EP 3124634 B1 EP3124634 B1 EP 3124634B1 EP 15183275 A EP15183275 A EP 15183275A EP 3124634 B1 EP3124634 B1 EP 3124634B1
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EP
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Prior art keywords
powder
weight
based powder
sintered
easily sinterable
Prior art date
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EP15183275.5A
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German (de)
English (en)
French (fr)
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EP3124634A1 (en
Inventor
Janusz KONSTANTY
Andrzej Romanski
Krystyna WIECZOREK-CIUROWA
Teodora SIKORA
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Akademia Gomiczo Hutnicza
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Akademia Gomiczo Hutnicza
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    • 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
    • C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/008—Ferrous alloys, e.g. steel alloys containing tin
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes

Definitions

  • the invention relates to an easily sinterable prealloyed iron-based powder, a method for the manufacturing and use thereof and the sintered product.
  • micro sinterable powder refers to a powder that after cold forming at pressure of 100-400 MPa and free sintering (at atmospheric pressure) in a reducing atmosphere for a time no longer than 60 minutes at a temperature not higher than 950° C allows to obtain sintered parts of the total porosity of less than 5% by volume.
  • Low-alloy iron powders containing at least 90% Fe by weight and sintered without the liquid phase allow obtaining sintered parts of the total porosity of less than 5% by volume, while maintaining the fine-grained microstructure of the material.
  • the two-phase microstructure of the material at the sintering temperature, composed of ferrite and austenite, is assured by the chemical composition of the alloy.
  • Ferrite stabilizers, e.g.: P, W, Mo, Co, and austenite stabilizers, e.g.: Cu, Ni are used in quantities and proportions assessed by means of experimental techniques (e.g. the high temperature X-ray diffraction phase analysis) or analytical techniques (e.g.
  • ThermoCalc software ® in order to obtain the ferrite-to-austenite volume ratio in the range from 2/5 to 3/5 within the possibly widest sintering temperature range. Furthermore, the increase in the phosphorus content of the powder contributes to the increase in the as-sintered hardness due to a strong solid solution strengthening effect.
  • the liquid phase sintered materials are characterized by a higher content of alloying elements such as Cu and Sn, which have to assure sufficient amount of persistent liquid phase at the sintering temperature in order to reach as-sintered porosity of less than 5% by volume.
  • alloying elements such as Cu and Sn
  • Cobalite CNF ® powder is described in the publication by BJ. Kamphuis, B. Serneels: "Cobalt and nickel free bond powder for diamond tools: Cobalite CNF "Industrial Diamond Review, No. 1, 2004, pp. 26-32 .
  • These raw materials due to the high content of expensive alloying elements and the use of chemical production methods, are expensive to manufacture. They cause a serious health hazards to the persons vulnerable to prolonged exposure to fine powders containing cobalt and/or nickel, involving the frequent occurrence of cobalt lung, giant cell interstitial pneumonia, allergic and cancerous skin diseases.
  • Document US 4518563 discloses a powder comprising Cr, from 2,5 to 7,5 wt.%; Mn, from 2,5 to 7,5 wt.%; P from 0.2 to 0.8 wt.%; Cu, from 1.0 to 5.0 wt.%; Si, from 0.5 to 2.0 wt.%; Mo, from 0 to 3 wt.%; C, from 1.5 to 3.5 wt.%; and the balance being Fe with less than 2 wt.% of impurities.
  • the powder is used in a method for manufacturing an anti-wear slide member having improved anti-pitting and initial stage fit of its slide surface.
  • the object of the invention is to provide easily sinterable prealloyed iron-based powders that do not demonstrate the prior art disadvantages resulting from the high content of alloying elements. They are therefore more environmentally friendly, cheaper and easier to manufacture, while maintaining very good properties, both technological as well as functional.
  • the object of the invention is also to propose a method for manufacturing easily sinterable prealloyed iron-based powders, which method eliminates the disadvantages occurring in the prior art, namely it is environmentally friendly, less expensive to implement and demonstrates flexibility allowing the better adjustment of the properties of the resulting powder to a particular application.
  • the easily sinterable prealloyed iron-based powder obtained by subjecting a reducible material, successively to milling, annealing and cooling thereof and grinding the cooled material to the powder, wherein the reducible material comprising oxides, carbonates, nitrates, metals and metal alloys and mixtures thereof, reducible by a technical purity hydrogen at a temperature not higher than 750°C, wherein the powder consists of:
  • the average particle size of the powder determined by the Fisher apparatus is not more than 10 ⁇ m.
  • the powder comprises polycrystalline particles constituted of grains having average size not greater than 2 ⁇ m.
  • a method for producing the easily sinterable prealloyed iron-based powder according to claims 1 to 3 is determined in claims 4-7.
  • the annealing is carried out at a temperature of 550-750°C, for a time of 1-8 hours, in a reducing atmosphere, which is hydrogen or a gas mixture containing hydrogen.
  • a reducing atmosphere which is hydrogen or a gas mixture containing hydrogen.
  • the mechanical processing of the reducible material is performed in dry or wet condition.
  • further drying is carried out after the mechanical processing in wet condition.
  • the easily sinterable prealloyed iron-based powder as described above is used for the manufacturing of sintered structural and tool components, in particular sintered metal-diamond composites.
  • the sintered product, especially the sintered metal-diamond composite, prepared from the easily sinterable prealloyed iron-based powder according to the invention is characterized in that the easily sinterable prealloyed iron-based powder is the powder as described above, wherein the total porosity of the sintered product at a temperature not higher than 950°C is lower than 5%.
  • the invention allows in a surprisingly simple and inexpensive manner to produce the easily sinterable prealloyed iron-based powder comprising at least 80% of iron by weight, copper and phosphorus, and optionally at least one from the group of alloying elements including tin, cobalt,nickel, tungsten and molybdenum, as well as impurities, mainly in the form of hardly reducible oxides such, for example SiO 2 .
  • the total content of alloying elements and impurities in the powders produced according to the invention does not exceed 20% by weight, wherein the powders in which the minimum content of alloying elements is 10% by weight are intended for applications in which it is required that permanent bonding of the sintered part to another element or elements, made of iron or its alloys, must occur during sintering, e.g. by brazing.
  • the easily sinterable prealloyed iron-based powder according to the invention while maintaining properties similar to the known powders of this kind, has in comparison to them a number of economic, environmental and technological advantages such as:
  • the method of the invention for producing the new prealloyed iron-based powders eliminates the expensive chemical method for obtaining mixtures of hydroxides, oxalates or other metal compounds hardly soluble in water, in which environmentally harmful waste (salts), that require utilization, are formed, and their later thermal decomposition to oxides occurs. It is replaced by a cheaper, mechanochemical synthesis of oxides, which, in comparison with the chemical method, gives greater freedom in selection the chemical composition of the powder. Mechanochemical synthesis consists in inducing chemical reactions preceded by grinding and mechanical activation of substrates. It enables receiving new materials characterized by a low level of chemical and structural heterogeneity, fine-grained microstructure and the most often desirable complex phase composition.
  • a reducible material is thus prepared through mechanical processing by milling, resulting in grinding, homogenization and activation of the reducible material.
  • the crushed, homogenized and activated by grinding reducible material thus obtained is annealed in a reducing atmosphere, and then cooled to a temperature which prevents self-ignition of the material. Finally, the annealed and cooled material is ground to a powder having a predetermined average particle size.
  • the powders produced by the mechanochemical method of oxides synthesis are free of drawbacks, which intrinsically characterise commercial powders, while maintaining similar to them technological properties. For this reason, the presented invention has tremendous application potential.
  • a powder mixture containing 92.86 g Fe 2 O 3 ; 3.57 g CuO and 3.57 g of prealloyed Fe-P powder containing 10% phosphorus by weight was prepared by mixing the ingredients in a Turbula type mixer for 10 minutes. The powders were placed together with grinding media in a 1.25 dm 3 roller ball mill drum. 12 mm diameter 100Cr6 bearing steel balls were used as the grinding media. The degree of filling of the mill was 50% by volume, and the ball-to-powder weight ratio was 20:1. Ethyl alcohol was poured into the drum in an amount required for the complete immersion of the grinding media together with the powder in the liquid. The drum was turned on to rotate at 65% of the critical speed.
  • a powder mixture containing 92.86 g Fe 2 O 3 ; 3.57 g CuO and 3.57 g of prealloyed Fe-P powder containing 10% phosphorus by weight was prepared by mixing the ingredients in a Turbula type mixer for 10 minutes. The powders were placed together with grinding media in a 1.25 dm 3 roller ball mill drum. 12 mm diameter 100Cr6 bearing steel balls were used as the grinding media. The degree of filling of the mill was 50% by volume, and the ball-to-powder weight ratio was 20:1. Distilled water was poured into the drum in an amount required for the complete immersion of the grinding media together with the powder in the liquid. The drum was turned on to rotate at 65% of the critical speed.
  • the charge of the mill was dried in a laboratory drier at 130°C.
  • the powder was then subjected to reducing annealing for 180 minutes at 700°C in a hydrogen atmosphere.
  • the obtained metal sponge was ground in a ceramic mortar to powder ( Figure 3 ) with a nominal content of 95.5% Fe by weight, 4% Cu by weight and 0.5% P by weight, the hydrogen loss of 1.2% by weight and Fisher sub-sieve size of 2.15 ⁇ m.
  • the powder was then subjected to reducing annealing for 180 minutes at 700°C in a hydrogen atmosphere and cooled to below 30°C in order to avoid self-ignition.
  • the metal sponge thus obtained was ground in a ceramic mortar to a powder ( Figure 4 ) with a nominal content of 90% Fe by weight, 7.5% Cu by weight, 2% Sn by weight and 0.5% P by weight, the hydrogen loss of 0.6% by weight and Fisher sub-sieve size of 8 ⁇ m.
  • the prealloyed nature of the powder was verified by X-ray diffraction phase analysis ( Figure 5 ).

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
EP15183275.5A 2015-07-27 2015-09-01 Prealloyed iron-based powder, a method for the manufacturing and use thereof and a sintered component Active EP3124634B1 (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PL413283A PL232405B1 (pl) 2015-07-27 2015-07-27 Proszek stopowy na bazie żelaza, sposób jego wytwarzania i zastosowanie

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EP3124634A1 EP3124634A1 (en) 2017-02-01
EP3124634B1 true EP3124634B1 (en) 2024-10-23

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CN107030584A (zh) * 2017-04-27 2017-08-11 安庆瑞钼特金属新材料有限公司 钨铜、钼铜合金薄板、箔材零件的表面处理方法
CN109702188B (zh) * 2019-03-01 2021-03-26 河南工程学院 一种金刚石工具用铜基预合金粉添加剂及其制备方法
CN114466719B (zh) * 2019-10-03 2024-07-05 尤米科尔公司 制备用于金刚石工具的预合金粉的方法和由此获得的粉末
CN113523266A (zh) * 2020-04-14 2021-10-22 江苏友和工具有限公司 一种陶瓷片及其加工工艺
CN111822715B (zh) * 2020-06-15 2021-09-14 中国地质大学（武汉） 高耐磨性孕镶金刚石钻头胎体材料及利用其制造金刚石钻头的方法
CN112223129B (zh) * 2020-09-11 2021-09-21 泉州众志金刚石工具有限公司 一种混凝土研磨用金属基地坪磨块材料
CN112676562A (zh) * 2020-12-17 2021-04-20 安徽奥微新材料有限公司 一种添加稀土的高性能金属预制粉制备方法

Citations (1)

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Publication number Priority date Publication date Assignee Title
US6596224B1 (en) * 1996-05-24 2003-07-22 Massachusetts Institute Of Technology Jetting layers of powder and the formation of fine powder beds thereby

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SE414191B (sv) * 1978-05-03 1980-07-14 Hoeganaes Ab Sett att enligt patentet 7612217-5 framstella jernbaserat pulver
JPS583901A (ja) * 1981-07-01 1983-01-10 Toyota Motor Corp 摺動部材の製法
JPS59145756A (ja) * 1983-02-08 1984-08-21 Hitachi Powdered Metals Co Ltd 内燃機関の動弁機構部材用焼結合金の製造方法
BE1009811A3 (fr) 1995-12-08 1997-08-05 Union Miniere Sa Poudre prealliee et son utilisation dans la fabrication d'outils diamantes.
JP4174689B2 (ja) 1997-04-29 2008-11-05 エヌ ヴェ ユミコア ソシエテ アノニム 予備合金化された、銅含有粉末およびダイヤモンド工具の製造におけるその使用
DE19822663A1 (de) 1998-05-20 1999-12-02 Starck H C Gmbh Co Kg Sinteraktive Metall- und Legierungspulver für pulvermetallurgische Anwendungen und Verfahren zu deren Herstellung und deren Verwendung
FR2784691B1 (fr) 1998-10-16 2000-12-29 Eurotungstene Poudres Poudre metallique prealliee micronique a base de metaux de transition 3d
WO2003083150A1 (en) 2002-03-29 2003-10-09 Umicore Pre-alloyed bond powders

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US6596224B1 (en) * 1996-05-24 2003-07-22 Massachusetts Institute Of Technology Jetting layers of powder and the formation of fine powder beds thereby

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PL413283A1 (pl) 2017-01-30
PL232405B1 (pl) 2019-06-28
EP3124634A1 (en) 2017-02-01

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