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EP3124634A1 - Vorlegiertes auf eisen basierendes pulver, verfahren zu seiner herstellung, verwendung davon und gesintertes teil - Google Patents

Vorlegiertes auf eisen basierendes pulver, verfahren zu seiner herstellung, verwendung davon und gesintertes teil Download PDF

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Publication number
EP3124634A1
EP3124634A1 EP15183275.5A EP15183275A EP3124634A1 EP 3124634 A1 EP3124634 A1 EP 3124634A1 EP 15183275 A EP15183275 A EP 15183275A EP 3124634 A1 EP3124634 A1 EP 3124634A1
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EP
European Patent Office
Prior art keywords
based powder
easily sinterable
weight
prealloyed iron
sintered
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.)
Granted
Application number
EP15183275.5A
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English (en)
French (fr)
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EP3124634B1 (de
Inventor
Janusz KONSTANTY
Andrzej ROMA SKI
Krystyna WIECZOREK-CIUROWA
Teodora SIKORA
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.)
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.
  • the 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
  • 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 according to the invention is characterized in that it comprises at least 80% Fe by weight, Cu and P as alloying additives and inevitable impurities, particularly hardly reducible oxides.
  • the easily sinterable prealloyed iron-based powder comprises at least 90% Fe by weight, 1- 9,8% Cu by weight and 0.2-2% P by weight.
  • the easily sinterable prealloyed iron-based powder further comprises at least one alloying element selected from the group consisting of Sn, Co, Ni, W, Mo.
  • the easily sinterable prealloyed iron-based powder comprises at least 1-18% Cu by weight, 0,5-4% Sn by weight and 0.2-2% P by weight.
  • the total content of Co and/or Ni and/or W and/or Mo is not more than 5% by weight.
  • the hydrogen loss of the powder annealed in a reducing atmosphere is less than 1.5% by weight.
  • 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.
  • 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 reducible material comprises oxides, carbonates, nitrates, metals and metal alloys and mixtures thereof, reducible by technical purity hydrogen at a temperature not higher than 750°C.
  • 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 avo id 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 Vorlegiertes auf eisen basierendes pulver, verfahren zu seiner herstellung, verwendung davon und gesintertes teil Active EP3124634B1 (de)

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

Publications (2)

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

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN109702188A (zh) * 2019-03-01 2019-05-03 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
CN111822715A (zh) * 2020-06-15 2020-10-27 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
CN112223129A (zh) * 2020-09-11 2021-01-15 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
WO2021063653A1 (en) * 2019-10-03 2021-04-08 Umicore Process for the preparation of pre-alloyed powders for diamond tools, and the powders so obtained
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
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

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2023184A (en) * 1978-05-03 1979-12-28 Hoeganaes Ab An Iron Based Powder for Powder Metallurgical Manufacture of Precision Components
US4518563A (en) * 1981-07-01 1985-05-21 Toyota Jidosha Kabushiki Kaisha Method for manufacturing a slide member
US4588441A (en) * 1983-02-08 1986-05-13 Yutaka Ikenoue Process for the preparation of sintered alloys for valve mechanism parts for internal combustion engines
EP0865511B1 (de) 1995-12-08 1999-08-18 n.v. Union Miniere s.a. Vorlegiertes pulver sowie seine anwendung zur herstellung von diamantwerkzeuge
US6312497B1 (en) 1997-04-29 2001-11-06 N. V. Union Miniere S.A. Pre-alloyed, copper containing powder, and its use in the manufacture of diamond tools
US6554885B1 (en) 1998-05-20 2003-04-29 H. C. Starck Gmbh Pre-alloyed powder
US6613122B1 (en) 1998-10-16 2003-09-02 Eurotungstene Poudres Micronic pre-alloyed metal powder based on three-dimensional transition metal
EP1492897B1 (de) 2002-03-29 2005-07-20 Umicore Vorlegierte bindepulver

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Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2023184A (en) * 1978-05-03 1979-12-28 Hoeganaes Ab An Iron Based Powder for Powder Metallurgical Manufacture of Precision Components
US4518563A (en) * 1981-07-01 1985-05-21 Toyota Jidosha Kabushiki Kaisha Method for manufacturing a slide member
US4588441A (en) * 1983-02-08 1986-05-13 Yutaka Ikenoue Process for the preparation of sintered alloys for valve mechanism parts for internal combustion engines
EP0865511B1 (de) 1995-12-08 1999-08-18 n.v. Union Miniere s.a. Vorlegiertes pulver sowie seine anwendung zur herstellung von diamantwerkzeuge
US6312497B1 (en) 1997-04-29 2001-11-06 N. V. Union Miniere S.A. Pre-alloyed, copper containing powder, and its use in the manufacture of diamond tools
US6554885B1 (en) 1998-05-20 2003-04-29 H. C. Starck Gmbh Pre-alloyed powder
US6613122B1 (en) 1998-10-16 2003-09-02 Eurotungstene Poudres Micronic pre-alloyed metal powder based on three-dimensional transition metal
EP1492897B1 (de) 2002-03-29 2005-07-20 Umicore Vorlegierte bindepulver
US7077883B2 (en) 2002-03-29 2006-07-18 Umicore Pre-alloyed bond powders

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BJ. KAMPHUIS; B. SERNEELS: "Cobalt and nickel free bond powder for diamond tools: Cobalite CNF", INDUSTRIAL DIAMOND REVIEW, 2004, pages 26 - 32, XP009098907

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN109702188A (zh) * 2019-03-01 2019-05-03 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
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
WO2021063653A1 (en) * 2019-10-03 2021-04-08 Umicore Process for the preparation of pre-alloyed powders for diamond tools, and the powders so obtained
CN114466719A (zh) * 2019-10-03 2022-05-10 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
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
CN111822715A (zh) * 2020-06-15 2020-10-27 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
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
CN112223129A (zh) * 2020-09-11 2021-01-15 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

Also Published As

Publication number Publication date
EP3124634B1 (de) 2024-10-23
PL232405B1 (pl) 2019-06-28
PL413283A1 (pl) 2017-01-30

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