EP1387730B1 - Iron powder composition including an amide type lubricant and a method to prepare it - Google Patents

Iron powder composition including an amide type lubricant and a method to prepare it Download PDF

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Publication number
EP1387730B1
EP1387730B1 EP02724846A EP02724846A EP1387730B1 EP 1387730 B1 EP1387730 B1 EP 1387730B1 EP 02724846 A EP02724846 A EP 02724846A EP 02724846 A EP02724846 A EP 02724846A EP 1387730 B1 EP1387730 B1 EP 1387730B1
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EP
European Patent Office
Prior art keywords
lubricant
fatty acid
composition according
atoms
iron
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.)
Expired - Lifetime
Application number
EP02724846A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP1387730A1 (en
Inventor
Björn Johansson
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.)
Hoganas AB
Original Assignee
Hoganas AB
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Filing date
Publication date
Application filed by Hoganas AB filed Critical Hoganas AB
Publication of EP1387730A1 publication Critical patent/EP1387730A1/en
Application granted granted Critical
Publication of EP1387730B1 publication Critical patent/EP1387730B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M105/00Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/56Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing nitrogen
    • C10M105/68Amides; Imides
    • 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
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • 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
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/108Mixtures obtained by warm mixing
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M171/00Lubricating compositions characterised by purely physical criteria, e.g. containing as base-material, thickener or additive, ingredients which are characterised exclusively by their numerically specified physical properties, i.e. containing ingredients which are physically well-defined but for which the chemical nature is either unspecified or only very vaguely indicated
    • C10M171/06Particles of special shape or size
    • 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
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02Compacting only
    • B22F2003/023Lubricant mixed with the metal powder
    • 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
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy

Definitions

  • the present invention relates to metal powder compositions and a method of preparing such compositions.
  • the invention relates to iron-based compositions having consistent apparent density and flowability at different temperatures.
  • the powder metallurgy art generally uses different standard temperature regimes for the compaction of a metal powder to form a metal component. These include chill-pressing (pressing below ambient temperatures), cold-pressing (pressing at ambient temperatures), hot-pressing (pressing at temperatures above those at which the metal powder is capable of retaining work-hardening), and warm-pressing (pressing at temperatures between cold-pressing and hot-pressing).
  • the US patents 5,744, 433 (Storstrom et al) and 5,154,881 (Rutz) disclose metal powder compositions including amide lubricants which are especially developed for warm compaction.
  • the US patent 5,744, 433 discloses a lubricant for metallurgical powder compositions contains an oligomer of amide type, which has a weight-average molecular weight M w of 30,000 at the most.
  • the amide lubricant consists of the reaction product of a monocarboxylic acid, a dicarboxylic acid and a diamine.
  • ADVAWAX.®. 450 which is an ethylenebisstearamitle product.
  • An object of the present invention is to reduce or eliminate current problems associated with large scale production.
  • Another object is to provide a new type of lubricant useful in metal compositions intended for compaction at elevated temperatures.
  • Still another problem is to provide an iron-based powder composition distinguished by excellent flow rate and apparent density.
  • a further object is to provide a powder composition, which generates a minimum of dust and the preparation of which does not require the use of organic solvents.
  • Another object is to provide a method for warm compaction such a metal powder composition.
  • iron-based powder encompasses powder essentially made up of pure iron; iron powder that has been prealloyed with other substances improving the strength, the hardening properties, the electromagnetic properties or other desirable properties of the end products; and particles of iron mixed with particles of such alloying elements (diffusion annealed mixture or purely mechanical mixture).
  • alloying elements are nickel, copper, molybdenum, chromium, manganese, phosphorus, carbon in the form of graphite, and tungsten, which are used either separately or in combination, e.g. in the form of compounds (Fe 3 P and FeMo).
  • the lubricants according to the invention are used in combination with iron-based powders having high compressability.
  • such powders have a low carbon content, preferably below 0.04% by weight.
  • Such powders include e.g. Distaloy AE, Astaloy Mo and ASC in the form of graphite, and tungsten, which are used either separately or in combination, e.g. in the form of compounds (Fe 3 P and FeMo).
  • the lubricants according to the invention are used in combination with iron-based powders having high compressability.
  • such powders have a low carbon content, preferably below 0.04% by weight.
  • Such powders include e.g. Distaloy AE, Astaloy Mo and ASC 100.29, all of which are commercially available from Hoganas AB, Sweden.
  • the lubricant used according to the present invention is new and may be represented by the following formula: D-C ma -B-A-B-C mb -D wherein
  • the lubricant has the chemical structure wherein D is COR, wherein R is an aliphatic group 16 - 20 C atoms, C is -NH (CH 2 ) n CO- wherein n is 5 or 11; B is amino; A is alkylen having 6-14 C atoms optionally including up to 3 O atoms, and ma and mb, which may be the same or different is an integer 2-5.
  • lubricants may be selected from the group consisting of
  • the oligomer amide type lubricant which is added to the iron-based powder is preferably in the form of a solid powder, can make up 0.1-1% by weight of the metal-powder composition, preferably 0.2-0.8% by weight, based on the total amount of the metal-powder composition.
  • the possibility of using the lubricant according to the present invention in low amounts is an especially advantageous feature of the invention, since it enables high densities to be achieved
  • the fatty acid used according to the present inventions is preferably a fatty acid having 10-22 C atoms.
  • examples of such acids are oleic acid, stearic acid and palmitic acid.
  • the amount of the fatty acid is normally 0.005-0.15, preferably 0.010-0.08 and most preferably 0.015-0.07 % calculated on the total weight of the powder composition. Fatty acid contents below 0.005 make it difficult to achieve an even distribution of the fatty acid. If the content is higher than 0.15 there is a considerable risk that the flow will deteriorate.
  • the melting point of the fatty acid should be lower than that of the amide oligomer lubricant.
  • the new powder composition may contain one or more additives selected from the group consisting of processing aids and hard phases.
  • the processing aids used in the metal-powder composition may consist of talc, forsterite, manganese sulphide, sulphur, molybdenum disulphide, boron nitride, tellurium, selenium, barium difluoride and calcium difluoride, which are used either separately or in combination.
  • the hard phases used in the metal-powder composition may consist of carbides of tungsten, vanadium, titanium, niobium, chromium, molybdenum, tantalum and zirconium, nitrides of aluminium, titanium, vanadium, molybdenum and chromium, Al 2 O 3 , and various ceramic materials.
  • the flow agent which is preferably a silicon dioxide
  • the flow agent is used in an amount from about 0.005 to about 2 percent by weight, preferably from about 0.01 to about 1 percent by weight, and more preferably from about 0.025 to about 0.5 percent by weight, based on the total weight of the metallurgical composition.
  • the flow agent should have an average particle size below about 40 nanometers.
  • Preferred silicon oxides are the silicon dioxide materials, both hydrophilic and hydrophobic forms, commercially available as the Aerosil line of silicon dioxides, such as the Aerosil 200 and R812 products, from Degussa Corporation.
  • the iron-based powder, at least one oligomer amide type lubricant, at least one fatty acid and optionally one or more additives, such as processing aids and hard phases, are heated to a temperature above the melting point of the lubricant; the obtained mixture is subsequently cooled to a temperature below the melting point of the lubricant and above the melting point of the fatty acid ; and a pulverulent flow agent is added to the obtained mixture, which is then mixed and cooled.
  • the powder mixture tested was prepared by dry mixing Distaloy AE (an iron-based powder available from Höganäs AB, Sweden) with 0.6 % by weight of organic material which consisted of the oligomer amide type lubricant defined above and 0.03 or 0.05 % by weight of stearic acid. 0.3 % by weight of graphite was aslo added and the obtained mixture was heated to 165°C. The mixture was cooled to 110°C and 0.06 % by weight of Aerosil® was added at this temperature. Essentially the same results are obtained when the Aerosil is added at ambient temperature.
  • the above mixture which included 0.03% by weight of stearic acid was also tested with regard to the dust reduction in comparison with a mixture prepared according to the US patent 5 368 630.
  • the known mixture also included 0.6% by weight of organic material but in this case the organic material consisted of 0.55% by weight of lubricant and 0.15% by weight of an organic binder (cellulose butyrate).
  • the iron-based powder was Distaloy AE in both mixtures.
  • the preparation of the known mixture involves dry mixing of the iron-based powder, the lubricant according to the US patent and 0.3% by weight of graphite.
  • the organic binder was dissolved in acetone and added to the dry mixture and after thorough mixing. The acetone was removed and 0.06% by weight of Aerosil® was added to the dried mixture.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)
  • Powder Metallurgy (AREA)
EP02724846A 2001-04-17 2002-04-17 Iron powder composition including an amide type lubricant and a method to prepare it Expired - Lifetime EP1387730B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
SE0101343A SE0101343D0 (sv) 2001-04-17 2001-04-17 Ikon powder composition
SE0101343 2001-04-17
PCT/SE2002/000763 WO2002083346A1 (en) 2001-04-17 2002-04-17 Iron powder composition including an amide type lubricant and a method to prepare it

Publications (2)

Publication Number Publication Date
EP1387730A1 EP1387730A1 (en) 2004-02-11
EP1387730B1 true EP1387730B1 (en) 2005-08-17

Family

ID=20283794

Family Applications (1)

Application Number Title Priority Date Filing Date
EP02724846A Expired - Lifetime EP1387730B1 (en) 2001-04-17 2002-04-17 Iron powder composition including an amide type lubricant and a method to prepare it

Country Status (10)

Country Link
US (1) US20020178863A1 (es)
EP (1) EP1387730B1 (es)
JP (1) JP4126230B2 (es)
CN (1) CN1250684C (es)
AT (1) ATE302081T1 (es)
DE (1) DE60205610T2 (es)
ES (1) ES2248547T3 (es)
SE (1) SE0101343D0 (es)
TW (1) TWI235183B (es)
WO (1) WO2002083346A1 (es)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6872235B2 (en) 2001-04-17 2005-03-29 Höganäs Ab Iron powder composition
SE0401644D0 (sv) * 2004-06-23 2004-06-23 Hoeganaes Ab Lubricants for insulated soft magnetic iron-based powder compositions
DE102005023420A1 (de) 2005-05-20 2006-11-23 Ems-Chemie Ag Polyamidformmassen mit verbesserter Fliessfähigkeit, deren Herstellung sowie deren Verwendung
DE102005023419B4 (de) 2005-05-20 2007-02-22 Ems-Chemie Ag Polyamid-Oligomere und deren Verwendung
JP2010285633A (ja) * 2009-06-09 2010-12-24 Kobe Steel Ltd 粉末冶金用混合粉末の製造方法、及び焼結体の製造方法
WO2011029759A1 (en) * 2009-09-08 2011-03-17 Höganäs Ab Metal powder composition
WO2015035515A1 (en) 2013-09-12 2015-03-19 National Research Council Of Canada Lubricant for powder metallurgy and metal powder compositions containing said lubricant

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999059753A1 (en) * 1998-05-15 1999-11-25 Höganäs Ab Iron-based metallurgical compositions containing flow agents and methods for using same

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2733868B2 (ja) * 1990-09-25 1998-03-30 日立粉末冶金株式会社 粉末冶金用成形潤滑剤
US5279640A (en) * 1992-09-22 1994-01-18 Kawasaki Steel Corporation Method of making iron-based powder mixture
US5368630A (en) * 1993-04-13 1994-11-29 Hoeganaes Corporation Metal powder compositions containing binding agents for elevated temperature compaction
SE9401922D0 (sv) * 1994-06-02 1994-06-02 Hoeganaes Ab Lubricant for metal powder compositions, metal powder composition containing th lubricant, method for making sintered products by using the lubricant, and the use of same
US5976215A (en) * 1997-08-29 1999-11-02 Kawasaki Steel Corporation Iron-based powder mixture for powder metallurgy and process for preparing the same

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999059753A1 (en) * 1998-05-15 1999-11-25 Höganäs Ab Iron-based metallurgical compositions containing flow agents and methods for using same

Also Published As

Publication number Publication date
ES2248547T3 (es) 2006-03-16
EP1387730A1 (en) 2004-02-11
ATE302081T1 (de) 2005-09-15
JP4126230B2 (ja) 2008-07-30
JP2004524450A (ja) 2004-08-12
DE60205610D1 (de) 2005-09-22
DE60205610T2 (de) 2006-02-09
CN1250684C (zh) 2006-04-12
CN1503707A (zh) 2004-06-09
WO2002083346A1 (en) 2002-10-24
TWI235183B (en) 2005-07-01
US20020178863A1 (en) 2002-12-05
SE0101343D0 (sv) 2001-04-17

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