EP1575726A1 - Weichmagnetische pulverzusammensetzung mit isolierten teilchen und schmiermittel, ausgewählt aus organosilanen, -titanaten, -aluminaten und zirkonaten und verfahren für ihre herstellung - Google Patents
Weichmagnetische pulverzusammensetzung mit isolierten teilchen und schmiermittel, ausgewählt aus organosilanen, -titanaten, -aluminaten und zirkonaten und verfahren für ihre herstellungInfo
- Publication number
- EP1575726A1 EP1575726A1 EP03781264A EP03781264A EP1575726A1 EP 1575726 A1 EP1575726 A1 EP 1575726A1 EP 03781264 A EP03781264 A EP 03781264A EP 03781264 A EP03781264 A EP 03781264A EP 1575726 A1 EP1575726 A1 EP 1575726A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- composition according
- group
- iron
- powder
- compound
- 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
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 18
- 230000008569 process Effects 0.000 title claims abstract description 7
- 238000002360 preparation method Methods 0.000 title claims abstract description 5
- 239000002245 particle Substances 0.000 title claims description 43
- 239000000314 lubricant Substances 0.000 title claims description 31
- 239000006247 magnetic powder Substances 0.000 title claims description 4
- 150000001282 organosilanes Chemical class 0.000 title description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 78
- 239000000843 powder Substances 0.000 claims abstract description 69
- 229910052742 iron Inorganic materials 0.000 claims abstract description 34
- 230000005291 magnetic effect Effects 0.000 claims abstract description 22
- 230000001050 lubricating effect Effects 0.000 claims abstract description 21
- 150000001875 compounds Chemical class 0.000 claims abstract description 17
- 238000000576 coating method Methods 0.000 claims abstract description 14
- -1 titanates Chemical class 0.000 claims abstract description 11
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 239000007771 core particle Substances 0.000 claims abstract description 9
- 239000002131 composite material Substances 0.000 claims abstract description 7
- 150000004645 aluminates Chemical class 0.000 claims abstract description 5
- 150000004756 silanes Chemical class 0.000 claims abstract description 5
- 230000005294 ferromagnetic effect Effects 0.000 claims abstract description 4
- 238000005056 compaction Methods 0.000 claims description 26
- 125000004429 atom Chemical group 0.000 claims description 11
- RSKGMYDENCAJEN-UHFFFAOYSA-N hexadecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCCCCCC[Si](OC)(OC)OC RSKGMYDENCAJEN-UHFFFAOYSA-N 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 6
- 125000004432 carbon atom Chemical group C* 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 125000000217 alkyl group Chemical group 0.000 claims description 5
- PYGSKMBEVAICCR-UHFFFAOYSA-N hexa-1,5-diene Chemical group C=CCCC=C PYGSKMBEVAICCR-UHFFFAOYSA-N 0.000 claims description 5
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 4
- 125000003545 alkoxy group Chemical group 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical group [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 claims description 4
- 239000013522 chelant Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- UZGKAASZIMOAMU-UHFFFAOYSA-N 124177-85-1 Chemical compound NP(=O)=O UZGKAASZIMOAMU-UHFFFAOYSA-N 0.000 claims description 2
- 125000003118 aryl group Chemical group 0.000 claims description 2
- 125000004122 cyclic group Chemical group 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 229960004275 glycolic acid Drugs 0.000 claims description 2
- 125000005842 heteroatom Chemical group 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 125000000962 organic group Chemical group 0.000 claims description 2
- 229940067631 phospholipid Drugs 0.000 claims description 2
- 150000003904 phospholipids Chemical class 0.000 claims description 2
- NMEPHPOFYLLFTK-UHFFFAOYSA-N trimethoxy(octyl)silane Chemical compound CCCCCCCC[Si](OC)(OC)OC NMEPHPOFYLLFTK-UHFFFAOYSA-N 0.000 claims description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims 1
- 239000000306 component Substances 0.000 description 26
- 238000009826 distribution Methods 0.000 description 10
- 239000011162 core material Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 238000005461 lubrication Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 150000002902 organometallic compounds Chemical class 0.000 description 6
- 239000010419 fine particle Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 230000035699 permeability Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000008358 core component Substances 0.000 description 4
- 230000004907 flux Effects 0.000 description 4
- 230000033001 locomotion Effects 0.000 description 4
- 239000005022 packaging material Substances 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000001965 increasing effect Effects 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- 239000000696 magnetic material Substances 0.000 description 3
- 125000002524 organometallic group Chemical group 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 241000237858 Gastropoda Species 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- IEKHISJGRIEHRE-UHFFFAOYSA-N 16-methylheptadecanoic acid;propan-2-ol;titanium Chemical compound [Ti].CC(C)O.CC(C)CCCCCCCCCCCCCCC(O)=O.CC(C)CCCCCCCCCCCCCCC(O)=O.CC(C)CCCCCCCCCCCCCCC(O)=O IEKHISJGRIEHRE-UHFFFAOYSA-N 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical group C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000003677 Sheet moulding compound Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000009527 percussion Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/14708—Fe-Ni based alloys
- H01F1/14733—Fe-Ni based alloys in the form of particles
- H01F1/14741—Fe-Ni based alloys in the form of particles pressed, sintered or bonded together
- H01F1/1475—Fe-Ni based alloys in the form of particles pressed, sintered or bonded together the particles being insulated
-
- 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
- B22F1/105—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing inorganic lubricating or binding agents, e.g. metal salts
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
- H01F1/22—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
- H01F1/24—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
- H01F1/26—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated by macromolecular organic substances
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
Definitions
- the present invention relates to new metal powder compositions. More specifically, the invention concerns a new iron-based powder which is useful for the preparation of soft magnetic materials having improved properties when used both at high and low frequencies . The invention also concerns a method for the manufacturing of soft magnetic composite materials prepared therefrom.
- Soft magnetic materials are used for applications, such as core materials in inductors, stators and rotors for electrical machines, actuators, sensors and transformer cores.
- soft magnetic cores such as rotors and stators in electric machines, are made of stacked steel laminates.
- Soft Magnetic Composite, SMC materials are based on soft magnetic particles, usually iron- based, with an electrically insulating coating on each particle. By compacting the insulated particles optionally together with lubricants and/or binders using the traditionally powder metallurgy process, the SMC parts are obtained.
- the SMC material can carry a three dimensional magnetic flux and as three dimensional shapes can be obtained by the compaction process.
- Two key characteristics of an iron core component are its magnetic permeability and core loss characteristics.
- the magnetic permeability of a material is an indication of its ability to become magnetised or its ability to carry a magnetic flux. Permeability is defined as the ratio of the induced magnetic flux to the magnetising force or field intensity.
- the hysteresis loss is brought about by the necessary expenditure of energy to overcome the retained magnetic forces within the iron core component.
- the eddy current loss is brought about by the production of electric currents in the iron core component due to the changing flux caused by alternating current (AC) conditions.
- a high electrical resistivity of the component is desirable in order to minimise the eddy currents .
- Desired component properties include e.g. a high permeability through an extended frequency range, low core losses, high saturation induction, and high strength. Normally an increased density of the component enhances all of these properties provided that a sufficient electrical resistivity can be maintained.
- the desired powder properties include suitability for compression moulding techniques, which i.e. means that the powder can be easily moulded to a high density component, which can be easily ejected from the moulding equipment without damages on the component surface.
- the present invention concerns a new ferromagnetic powder composition, which is suitable of compaction to high density composite components. More specifically the present invention concerns a powder composition comprising soft magnetic iron or iron-based core particles, the surface of which are surrounded by an electrically insulating in- organic coating and which composition also includes a lubricating amount of silanes, titanates, aluminates, or zirconates .
- the present invention also includes a method of preparing high-density green, and optionally heat-treated, compacts from these compositions.
- This method comprises the steps of providing the composition, optionally mixing said composition with additives, such as conventional lubricants (i.e. particular lubricants) and binders as well as flow- enhancing agents; uniaxially compacting in a die at high pressure and ejecting the green body, which may subsequently be heat-treated.
- additives such as conventional lubricants (i.e. particular lubricants) and binders as well as flow- enhancing agents
- the ferromagnetic powders used herein are made up of iron or an alloy containing iron optionally in combination with up to 20 % by weight of one or more of element selected from the group consisting of aluminium, silicon, chromium, niobium, molybdenum, nickel and cobalt.
- the new powder is based on a base powder that consists of essentially pure iron.
- This powder could be e.g. commercially available water-atomised or gas- atomised iron powders or reduced iron powders, such as sponge iron powders.
- the powder particle shape could be round, irregular or flat.
- Preferred electrically insulating coatings which may be used according to the invention, are thin phosphorous containing coatings of the type described in the US patent 6348265 which is hereby incorporated by reference. Also other, preferably inorganic coatings may be used, for example coatings based on Cr, Mg, Mo, Zn, Ni, or Co.
- the lubricating agent used according to the invention is a type of organo-silanes, organo-titanates, organo- aluminates or organo-zirconates .
- This class of substances is often referred to as surface modifying agents, coupling agents, or cross-linking agents depending on the chemical functionality of their linked groups.
- the specific type of organo-silanes, organo- titanates, or ' gano-aluminates or organo-zirconates which are used according to the present invention and which may be referred to as organo-metallic compounds are distinguished by the presence of at least one hydrolysable group and at least one lubricating organic moiety. This type of compounds can be defined by the following general formula:
- M is a central atom selected from Si, Ti, Al, and Zr; Ri is a hydrolysable group; R 2 is a group consisting of a lubricating organic moiety; wherein the sum of m+n must equal the coordination number of the central atom and where n is an integer >1 and m is an integer >1.
- Ri is an alkoxy group having less than 12 C atoms. Preferred are those alkoxy groups, which have less than 6, and most preferred are alkoxy groups having 1-3 C atoms.
- R may also be a chelate group, such as a residue of hydroxyacetic acid (-0C (0) ) -CH 2 0-) or a residue of ethylene glycol (-OCH 2 CH 2 0-) .
- R 2 is an organic group including between 6-30, preferably 10-24 carbon atoms optionally including one or more hetero atoms selected from the group consisting of N, 0, S and P.
- R 2 is a group consisting of an organic moiety, which is not easily hydrolysed and often lipophilic and can be a chain of an alkyl, ether, ester, phospho-alkyl, phospho-alkyl, phospho-lipid, or phospho-amine .
- the phosphorous may be present as phosphato, pyrophosphato, or phosphito groups.
- R 2 may be linear, branched, cyclic, or aromatic.
- a preferred group of lubricating silanes according to the present invention are alkyl-alkoxy silanes and polyether- alkoxy silanes. Furthermore, promising results have been obtained with hexadecyl-trimethoxy silane, isopropyl- triisostearyl titanate, isopropyl-tri (dioctyl) phosphato titanate, neopentyl (diallyl) oxy-tri (dioctyl) hosphato zirconate, neopentyl (diallyl) oxy-trineodecanoyl zirconate, and diisobutyl-acetoacetyl aluminate .
- the amount of the compound is preferably present in amounts above 0.05%, such as in amounts of 0.05-0.5%, preferably 0.07-0.45%, and most preferably 0.08-0.4% by weight of the composition.
- a too low amount of lubricating agent gives high density but results in poor ejection behaviour and may thus result in poor surface condition of the tool and/or SMC parts.
- a too high amount may give excellent ejection behaviour but could render in low component densities.
- the compound is present as a lubricating layer on the insulated particles . It should, however, be noted that the geometry of the component as well as the material and quality of the tool, have great impact on the surface condition of the SMC parts after ejection.
- organo-silanes organo-titanates, or organo-aluminates
- US patents 4820338 and 6537389 silanes, titanates or aluminates are used in order to accelerate a coupling between the magnetic powder particles and an electrically insulating organic binder polymer.
- the powder particles do not have an inorganic coating.
- the US patent 6537389 discloses a wide range of silicon-, aluminium-, or boron-containing compounds as molecular precursors for producing electrically insulating ceramics on soft magnetic powders.
- the precursor compounds are converted by thermal treatments into ceramic, metallic or intermetallic end products to enhance temperature and solvent resistance.
- the US patent 6537389 distinguishes from the present invention i.a. in that the organo- metallic compounds are used as precursors for producing chemically and thermally resistant coatings, and not as the key component that facilitates production of high density parts.
- the precursor compounds described in the examples of US patent 6537389 do not include a lubricating moiety.
- the lubricating compound (s) used according to the present invention can be used in such a way that it is dissolved or dispersed in a suitable solvent, e.g. an organic sol- vent, such as acetone or ethanol .
- a suitable solvent e.g. an organic sol- vent, such as acetone or ethanol .
- the obtained solution or dispersion is subsequently added to the iron based powder during mixing and optionally heating.
- the solvent is finally evaporated optionally in vacuum.
- the powder used has coarse particles i.e. the powder is essentially without fine particles.
- the term "essentially without fine particles" is intended to mean that less than about 5 % of the iron or iron-based powder particles have size below 45 ⁇ m as measured by the method described in SS-EN
- the term "essentially consisting” is intended to mean that at least 40 %, preferably at least 60 % of the particles have a particle size above 106 and 212 ⁇ m, respectively. So far the best results have been obtained with powders having an average particle size about 250 ⁇ m and only less than 3 % below 106 ⁇ m. The maximum particle size may be about 5 mm.
- the particle size distribution for iron-based powders used at PM manufacturing is normally distributed with a Gaussian distribution with an average particle diameter in the region of 30 to 100 ⁇ m and about 10-30% less than 45 ⁇ m. Iron based powders essentially free from fine particles may be obtained by removing the finer fractions of the powder or by manufacturing a powder having the desired particle size distribution .
- the iron or iron-based powder must not be mixed with a separate (particular) lubricant before it is transferred to the die.
- external lubrication die wall lubrication
- the invention does not exclude the possibility of, when it is of interest, to utilise conventional internal lubrication (in an amount up to 0.5% by weight), external lubrication or a combination of both.
- the powder to be compacted may also include additives selected from the group consisting of binders, lubricants, and flow- enhancing agents.
- additives selected from the group consisting of binders, lubricants, and flow- enhancing agents.
- inorganic lubricants which may be used in addition to organic PM lubricants, are hexagonal boron nitride, and MoS 2 .
- soft magnetic composite materials having a density of at least 7.45 g/cm 3 can be prepared by uniaxially compacting the new powder cor ⁇ - positions in a die at high compaction pressures and without die wall lubrication.
- the green body When the green body has been ejected from the compaction tool it can be heat treated up to temperatures of about 700°C.
- At high compaction pressure is intended to mean at pressures of about at least 800 MPa. More interesting results are obtained with higher pressures such as pressures above 900, more preferably above 1000, and most preferably above 1100 MPa.
- Conventional compaction at high pressures, i.e. pressures above about 800 MPa, with conventionally used powders including finer particles are generally considered unsuitable due to the high forces required in order to eject the compacts from the die, the accompanying high wear of the die, and the fact that the surfaces of the components tend to be less shiny or dete- riorated. High electrical resistance can be obtained even though high compaction pressures are used to achieve the high density.
- the ejection force is reduced at high pressures of about 1000 MPa, and that components having acceptable or even perfect surfaces may be obtained.
- the compaction may be performed with standard equipment, which means that the new method may be performed without expensive investments.
- the compaction is performed uni- axially and preferably in a single step at ambient or elevated temperature.
- the compaction may be performed with the aid of a percussion machine (Model HYP 35-4 from Hydropulsor) as described in patent publication WO 02/38315.
- the heat treatment may be performed at the temperatures normally used, e.g. up to temperatures of about 700°C in different types of atmospheres or at reduced pressure and optionally in the presence of steam. Prior to the heat treatment the pressed components may optionally be green machined and/or cleaned.
- a main object of the present invention is to achieve high density products and to this end it is preferred to use coarse powders as described above. It has, however, also been found that these lubricating effects can also be obtained in combination with powders including higher amounts of fine particles i.e. the type of powders which are conventionally used in the PM industry today.
- Example 3 and 5 below illustrates the lubricating effect of the organo-metallic compounds according to the present invention on both conventional powders and coarse powders . As can be observed high densities are obtained also with a conventional powder including higher amounts of fine particles.
- Compositions including iron or iron- based powders with the particle size distributions which are normally used today and the lubricating agents according to the present invention may be of special interest for certain applications and are therefore also within the scope of the invention.
- high density is intended to mean compacts having a density of about at least 7.45 g/cm 3 .
- “High density” is not an absolute value.
- a typical achievable density according to the state of the art for single heat-treated, single pressed components is about 7.2 g/cm 3 .
- warm compaction an increase of about 0.2 g/cm 3 may be reached.
- high density is intended to mean compacts having a density of about 7.45-7.65 g/cm 3 and above, depending on type and amount of additives used, and type of iron-based powder used. Components having lower densities can of course also be produced but are believed to be of less interest.
- the advantage obtained by using the powder and method according to the present invention is that high- density SMC parts can be cost-efficiently produced. SMC parts with remarkably high magnetic induction levels together with low core losses can be obtained.
- Other advantages are that the mechanical strength after heat treatment is increased and that, in spite of very high densities, compacted parts with high electrical resistance can be successfully ejected from the dies without negatively influence the finish of the die walls and/or on the surfaces of the compacted SMC parts. It is thus possible to obtain parts having excellent surface finish. These results can be obtained with a single compaction step. Examples of products of special interest for the new powder compacts are inductors, stators and rotors for electrical machines, actuators, sensors and transformer cores.
- An iron-based water atomised powder (Somaloy 550TM, available from Hoganas AB, Sweden) was used as starting material. This powder has an average particle size between 212 and 425 ⁇ m and less than 5% of the particles have a particle size below 45 ⁇ m.
- This powder which is a pure iron powder, the particles of which are electrically insulated by a thin phosphorus containing barrier, was treated with 0.2% by weight of a hexadecyl-trimethoxy silane as a lubricating agent.
- the addition of the lubricating agent was performed as follows : hexadecyl- trimethoxy silane was diluted in ethanol to a 20% solution by weight and the solution was stirred during 60 minutes.
- Rings with an inner diameter of 47 mm and an outer diameter of 55 mm and a height of 4 mm were uniaxially compacted in a single step at different compaction pressures 800, 1000 and 1200 MPa, respectively.
- compaction pressures 800, 1000 and 1200 MPa respectively.
- the green density is significantly higher for the powder according to the invention and magnetic properties are, hence, improved compared with the materials used in the comparative examples.
- the comparative example also demonstrates that no or only minor improvements of the magnetic properties can be obtained by increasing the compaction pressure to 1000 MPa and 1200 MPa.
- a very high purity water atomised iron-based powder the particles of which were provided with a thin insulating coating and which had a mean particle size above 212 ⁇ m was treated with 0.1% and 0.2% of hexadecyl- trimethoxysilane, respectively, according to the procedure in Example 1.
- the same iron-based powder without any lubricating agent was used as a reference.
- Cylindrical samples with a diameter of 25 mm and a height of 4 mm were compacted in an uniaxially press movement at a compaction pressure of 1000 MPa.
- Table 2 shows the ejection energy needed for ejecting the components and the green density obtained.
- the ejection energy is expressed as percentage of the ejection energy for the sample without lubricating agent.
- the S-powder has about 14 % of the particles less than 45 ⁇ m and a weight average particle size of about 100 ⁇ m.
- the C-powder has a significantly coarser particle size distribution with a weight average size of about 250 ⁇ m and less than 3% below 106 ⁇ m.
- A-E Five different kinds of organo-silanes were used (A-E) : A Methyl-trimethoxy silane B Propyl-trimethoxy silane C Octyl-trimethoxy silane D Hexadecyl-trimethoxy silane E Polyethyleneether-trimethoxy silane with 10 ethylene ether groups
- lubricant agent optionally mixed with conventionally used i.e. particular lubricants, can be of interest for some applications .
- This example demonstrates the lubrication effect of organo-metallic compounds with different central atoms.
- the lubrication effect of four different agents have been examined i.e. silane, titanate, zirconate and aluminate, having Si, Ti, Zr and Al as the central atom, respectively.
- the various central atoms have different coordination numbers and chemical properties.
- the chemical structure of the organo-metallic compound was selected so that the chain length of the lubricating group or groups (R 2 ) would 'show comparable properties which can be compared with those obtained with hexadecyl-trimethoxy silane (D) .
- a high purity water atomised iron-based powder with a thin insulating coating were treated with 0.2% by weight of each organo-metallic compound as lubricating agent.
- the obtained mixtures were compacted at 1100 MPa in a uniaxial press movement into slugs with a diameter of 25 mm and a height of 12 mm.
- the dynamic ejection force per unit sliding area was measured and after ejection green surface finish was evaluated and density was measured as is shown below in table 4.
- A-D organo-metallic agents
- Cylindrical samples with a diameter of 25 mm and a weight of 50 grams were compacted in an uniaxially press move- ment at a compaction pressure of 1000 MPa and green densities above 7.6 g/cm 3 for all the samples were obtained.
- This example illustrates the importance of the inorganic insulation.
- a high purity iron powder the particles of which are electrically insulated by a thin phosphorus-containing barrier was compared with an identical powder without the phosphorous-based inorganic insulation. Both types of powders were subsequently treated with 0.2% by weight of hexadecyl-trimethoxy silane as a lubricating agent according to the invention.
- Rings with an inner diameter of 45 mm and an outer diameter of 55 mm and a height of 5 mm were uniaxially compacted in a single step at compaction pressure 1100 MPa. After compaction the parts were heat treated at 500°C for 30 minutes in air. The electrical resistivity was measured by the four-point method.
- the following table 6 shows electrical resistivity and density of composite components prepared of powders with and without insulated particles.
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Electromagnetism (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Soft Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
- Lubricants (AREA)
- Silicon Polymers (AREA)
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SE0203851A SE0203851D0 (sv) | 2002-12-23 | 2002-12-23 | Iron-Based Powder |
SE0203851 | 2002-12-23 | ||
PCT/SE2003/002067 WO2004056508A1 (en) | 2002-12-23 | 2003-12-22 | Soft magnetic powder composition comprising insulated particles and a lubricant selected from organo-silanes, -titanates, -aluminates and zirconates and a process for their preparation |
Publications (2)
Publication Number | Publication Date |
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EP1575726A1 true EP1575726A1 (de) | 2005-09-21 |
EP1575726B1 EP1575726B1 (de) | 2010-07-07 |
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EP03781264A Expired - Lifetime EP1575726B1 (de) | 2002-12-23 | 2003-12-22 | Weichmagnetische pulverzusammensetzung mit isolierten teilchen und schmiermittel, ausgewählt aus organosilanen, -titanaten, -aluminaten und zirkonaten und verfahren für ihre herstellung |
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EP (1) | EP1575726B1 (de) |
JP (2) | JP4886987B2 (de) |
KR (1) | KR101035757B1 (de) |
CN (1) | CN100548541C (de) |
AT (1) | ATE473064T1 (de) |
AU (1) | AU2003288880B8 (de) |
BR (1) | BR0317661A (de) |
CA (1) | CA2505381C (de) |
DE (1) | DE60333309D1 (de) |
ES (1) | ES2348212T3 (de) |
MX (1) | MXPA05006847A (de) |
PL (1) | PL209529B1 (de) |
RU (1) | RU2335817C2 (de) |
SE (1) | SE0203851D0 (de) |
TW (1) | TWI229018B (de) |
WO (1) | WO2004056508A1 (de) |
ZA (1) | ZA200503597B (de) |
Families Citing this family (17)
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SE0203851D0 (sv) * | 2002-12-23 | 2002-12-23 | Hoeganaes Ab | Iron-Based Powder |
PL2139630T3 (pl) * | 2007-03-21 | 2013-10-31 | Hoeganaes Ab Publ | Kompozyty sproszkowanych metali i polimerów |
RU2510993C2 (ru) * | 2008-03-20 | 2014-04-10 | Хеганес Аб (Пабл) | Порошковая ферромагнитная композиция и способ ее получения |
JP5482097B2 (ja) * | 2009-10-26 | 2014-04-23 | Tdk株式会社 | 軟磁性材料、並びに、圧粉磁芯及びその製造方法 |
CN102844824B (zh) * | 2010-02-18 | 2017-08-15 | 霍加纳斯股份有限公司 | 铁磁粉末组合物及其制造方法 |
AT12021U1 (de) * | 2010-04-14 | 2011-09-15 | Plansee Se | Beschichtungsquelle und verfahren zu deren herstellung |
CN101982856B (zh) * | 2010-09-21 | 2012-02-15 | 李延军 | 笔杆式汽车点火线圈内用软磁铁芯及其制作方法 |
CN102136330A (zh) * | 2011-04-01 | 2011-07-27 | 钢铁研究总院 | 一种复合软磁材料及其制备方法 |
EP2509081A1 (de) * | 2011-04-07 | 2012-10-10 | Höganäs AB | Neue Zusammensetzung und Verfahren |
CN102896315B (zh) * | 2012-09-15 | 2015-04-01 | 安徽省怀远县尚冠模具科技有限公司 | 一种模具上压板的制备方法 |
CN102909373A (zh) * | 2012-09-15 | 2013-02-06 | 安徽省怀远县尚冠模具科技有限公司 | 一种模具冲压顶杆的制备方法 |
JP2014196554A (ja) * | 2013-03-08 | 2014-10-16 | Ntn株式会社 | 磁心用粉末および圧粉磁心、並びに磁心用粉末および圧粉磁心の製造方法 |
CN104217834B (zh) * | 2013-06-03 | 2018-01-23 | 株式会社田村制作所 | 软磁性粉末组合物、芯、电抗器 |
CN105149601A (zh) * | 2015-09-29 | 2015-12-16 | 四川有色金源粉冶材料有限公司 | 一种高比重合金喂料的制备方法 |
CN105108166B (zh) * | 2015-09-29 | 2017-06-06 | 四川有色金源粉冶材料有限公司 | 一种注射成型用铁基合金粉末的制备方法 |
US11948714B2 (en) * | 2019-12-12 | 2024-04-02 | Murata Manufacturing Co., Ltd. | Soft magnetic material and green compact |
JP7322846B2 (ja) * | 2019-12-12 | 2023-08-08 | 株式会社村田製作所 | 軟磁性材料および圧粉成形体 |
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JPS5947301A (ja) * | 1982-09-08 | 1984-03-17 | Fuji Photo Film Co Ltd | 強磁性金属粉末 |
JPH0611008B2 (ja) * | 1983-11-16 | 1994-02-09 | 株式会社東芝 | 圧粉鉄心 |
EP0205786B1 (de) | 1985-06-26 | 1990-01-31 | Kabushiki Kaisha Toshiba | Magnetkern und Herstellungsverfahren |
US4985273A (en) * | 1988-06-07 | 1991-01-15 | Matsushita Electric Industrial Co., Ltd. | Method of producing fine inorganic particles |
US6887412B1 (en) * | 1999-09-28 | 2005-05-03 | Nec Tokin Corporation | Composite magnetic sheet and method of producing the same |
JP2002015912A (ja) * | 2000-06-30 | 2002-01-18 | Tdk Corp | 圧粉磁芯用粉末及び圧粉磁芯 |
SE0203851D0 (sv) * | 2002-12-23 | 2002-12-23 | Hoeganaes Ab | Iron-Based Powder |
US20060096406A1 (en) * | 2004-11-08 | 2006-05-11 | Yao-Huang Liu | Gear lever having a light emitting effect |
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Also Published As
Publication number | Publication date |
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JP4886987B2 (ja) | 2012-02-29 |
JP2006511711A (ja) | 2006-04-06 |
RU2335817C2 (ru) | 2008-10-10 |
TWI229018B (en) | 2005-03-11 |
EP1575726B1 (de) | 2010-07-07 |
CA2505381A1 (en) | 2004-07-08 |
JP2010251779A (ja) | 2010-11-04 |
RU2005123385A (ru) | 2006-03-27 |
PL209529B1 (pl) | 2011-09-30 |
WO2004056508A1 (en) | 2004-07-08 |
MXPA05006847A (es) | 2005-08-16 |
TW200422122A (en) | 2004-11-01 |
ZA200503597B (en) | 2006-08-30 |
ES2348212T3 (es) | 2010-12-01 |
CN100548541C (zh) | 2009-10-14 |
AU2003288880B8 (en) | 2006-11-16 |
AU2003288880A1 (en) | 2004-07-14 |
CA2505381C (en) | 2011-12-13 |
CN1732059A (zh) | 2006-02-08 |
AU2003288880B2 (en) | 2006-10-12 |
KR101035757B1 (ko) | 2011-05-20 |
ATE473064T1 (de) | 2010-07-15 |
DE60333309D1 (de) | 2010-08-19 |
SE0203851D0 (sv) | 2002-12-23 |
BR0317661A (pt) | 2005-12-06 |
PL376102A1 (en) | 2005-12-12 |
KR20050085871A (ko) | 2005-08-29 |
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