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Publication numberUS3814598 A
Publication typeGrant
Publication dateJun 4, 1974
Filing dateMar 27, 1973
Priority dateDec 29, 1970
Publication numberUS 3814598 A, US 3814598A, US-A-3814598, US3814598 A, US3814598A
InventorsJ Gabriel, W Reilly
Original AssigneeChromalloy American Corp
Export CitationBiBTeX, EndNote, RefMan
External Links: USPTO, USPTO Assignment, Espacenet
Wear resistant powder metal magnetic pole piece made from oxide coated fe-al-si powders
US 3814598 A
Abstract  available in
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Claims  available in
Description  (OCR text may contain errors)

June 4; 1974 J. M. GABRIEL E ,5 WEAR RESISTANT POWDER METAL MAGNETIC POLE PIECE MADE FROM OXIDE COATED Fe *AQ-Si POWDERS 0r1g1nal Filed Dec 29 1970 United States Patent Office Patented June 4, 1974 WEAR RESISTANT POWDER METAL MAGNETIC POLE PIECE MADE FROM OXIDE COATED Fe-Al-Si POWDERS James M. Gabriel, Monsey, N.Y., and William Reilly, Fort Lee, N.J., assignors to Chromalloy American Corporation Original application Dec. 29, 1970, Ser. No. 102,364, now Patent No. 3,739,445. Divided and this application Mar. 27, 1973, Ser. No. 345,343

Int. Cl. B2215 3/14; Gllb 5/40 US. Cl. 75-206 5 Claims ABSTRACT OF THE DISCLOSURE This application is a division of copending application Ser. No. 102,364, filed Dec. 29, 1970, now US. Pat. 3,739,445.

This invention relates to a method for producing a sintered wear resistant powder metal magnetic pole piece.

STATE OF THE ART Magnetic playback television tapes employ magnetic pole pieces as pickup heads for playing back pictures recorded thereon. In one design, four pole pieces are employed in an assembly, each pole piece being soldered every 90 within a panel guide wheel near the periphery thereof. The guide wheel rotates about a central axis and wears against a magnetic playback tape of gamma iron oxide. The pickup face of each pole piece, which is disposed at the periphery of the wheel, is the only part that contacts the tape in service. As the pole pieces wear, the gap between the tape and wheel becomes too great for proper magnetic performance (permeability, coercivity, etc.) such that the picture is generally degraded, thus requiring frequent replacement with new pole pieces at, for example, IOU-hour intervals.

The pole pieces are made of a soft magnetic material comprising an iron-base alloy containing approximately 9.4% by weight of silicon and 5.7% by weight of aluminum. conventionally, the alloy is cast into a desired shape and the individual pole pieces machined from the casting, since the alloy is too brittle to withstand conven tional working operations, such as rolling, forging, forming and the like. The casting usually has a coarse grained microstructure of less than ASTM 4 accompanied by limited wear characteristics.

It would be desirable to provide a soft magnetic alloy of the foregoing type characterized by improved wear resistance and capable of being employed for prolonged periods of time in frictional contact with magnetic playback tape containing gamma iron oxide.

OBJECTS OF THE INVENTION It is thus the object of the invention to provide a powder metallurgy method for producing magnetic pole pieces characterized by improved wear resistance when in rubbing contact with a magnetic playback tape of gamma oxide iron.

Another object is to provide a method for producing an article of manufacture from a sintered soft magnetic alloy characterized by improved wear resistance as a magnetic pole piece when employed in rubbing contact with a moving magnetic tape of gamma iron oxide.

These and other objects will more clearly appear when taken in conjunction with the following disclosure and the accompanying drawing, wherein:

FIGS. 1 and 2 illustrate magnetic pole pieces produced in accordance with the invention;

FIG. 3 depicts, schematically, one embodiment of a die assembly which is employed in producing hot pressed products in accordance with the invention; and

FIG. 4 is a reproduction of a photomicrograph taken at 500 times magnification showing a typical microstructure oxide surrounding the grains of the magnetic alloy.

STATEMENT OF THE INVENTION One embodiment of the invention resides in a powder metallurgy method of producing a magnetically soft ferrous alloy containing an effective amount of silicon and aluminum ranging from about 2 to 12% silicon and from about 2 to 10% aluminum for use in the manufacture of magnetic pole pieces characterized by improved resistance to wear when in rubbing contact with a moving magnetic playback tape of gamma iron oxide. A classified powder of the alloy is first thermally oxidized in air at an elevated temperature to provide a thin oxide film at the surface of the particles and the oxidized powder is then hot consolidated to a substantially fully dense body having a fine grained metallographic structure with the oxide film encapsulating the grain boundaries thereof. The oxide film improves wear resistance without substantially adversely affecting the magnetic properties.

The invention also provides as an article of manufacture a consolidated sintered magnetic alloy containing effective amounts of silicon, aluminum, oxygen, and the balance essentially iron suitable for use in magnetic pole pieces for use with magnetic playback tapes.

The magnetic alloy is advantageously produced as a vacuum hot pressed billet from thermally oxidized alloy powder of particle size ranging from about 10 to 20 microns. This results in a fine grained fully dense pressing in which the wear performance is substantially superior to the cast alloy product. The benefit provided by the product is attributed (1) to grain refinement which offers more grain boundary area than the cast structure; and (2) to the presence of a localized oxide film in the grain boundary.

As stated hereinbefore, the powder metallurgy alloy is particularly suitable for magnetic pole pieces of the type shown in FIGS. 1 and 2, FIG. 1 showing a typical panel guide wheel 10 having four magnetic pole pieces 11, 12, 13 and 14 located at intervals around the periphery of the Wheel. The actual wear surface of each of the pole pieces, i.e. surfaces 11A, 12A, 13A and 14A, extend slightly beyond the periphery of the wheel as shown. An enlarged View of a pole piece 15 is depicted with the wear surface 15A indicated as shown.

DETAIL ASPECTS OF THE INVENTION In carrying out the more preferred aspects of the invention, the alloy composition consisting essentially of approximately 9.4% silicon (e.g. 9.4% i0.4%), approximately 5.7% aluminum (e.g. 5.7%:0.3%), and the balance essentially iron, is preferably in the vacuum cast form. The vacuum cast ingots are ground clean, remelted and then atomized using an inert gas (preferably argon) preferably jet controlled using proper processing parameters (i.e. pressure, purity, flow, etc.) to achieve maxiin a metal desiccator at 25 to 30 inches Hg with the oven temperature not exceeding 140 F. The milled product is then classified to remove the 10 to 20 micron pow der. Milling times and rotation speeds are controlled to assure that flake powder shapes are not developed, otherwise, such powder contributes to an anisotropic metallurgical structure and a non-uniform performance in the field.

The milled powder has an irregular shape and is preferably blended with the unmilled atomized spherical powder. Tests have indicated an optimum blend ratio to be 5 parts of milled powder to 1 part of atomized powder. The blend ratio may vary from about 4 to l to as high as about 7 to 1. A typical charge of powder is homogeneously mixed for one hour prior to pressing. Where intermediate handling and storage times exceed 48 hours, the powder is stored in evacuated containers under a vacuum level of 10* torr or better.

A 600 gram charge of atomized (spherical shape) and milled (irregular shape) powder is blended and the blended powder is first thermally oxidized at 600 F. for 1 hour in air. One method is to uniformly spread the powder of 10 to micron size between two fine mesh stainless steel screens confined with the side walls of a stainless steel tray with side ports to allow the powder to be pre-oxidized similar to a fluid bed system in a recirculating air environment. To assure the desired oxidation, the powder is visually inspected at ten times magnification under stereo binoculars for oxide color uniformity and to assure absence of agglomeration. An oxygen content of about 3400 p.p.m. to 4400 p.p.m. by weight has been found very advantageous, although the oxygen content may vary from about 2000 p.p.m. to 8000 p.p.m. An oxide layer around particles of 10 to 20 microns average size may range in thickness up to about 2 microns.

The powder (e.g. 600 to 800 grams) may be directly hot pressed to the desired shape, or the powder charge may be first cold pressed to a cylindrical shape under 300 p.s.i. pressure and thereafter hot pressed to form the desired product. The hot pressing is carried out under vacuum (e.g. 5 10= torr) at a pressure (18,000 p.s.i.) sufiicient to provide a substantially fully dense sintered body. The hot pressing is preferably carried out at a temperature of about 1050 C., the temperature being reached in 3 hours, held for one hour at temperature and then cooled to black heat in 2 hours. The die and punch assembly is shown schematically in FIG. 3 comprising a stress relieved die 16 of a molybdenum alloy containing by weight about 0.5% Ti, about 0.5 Zr, about 0.06% C and the balance essentially molybdenum. The die has a center opening or cavity 17 of about 2 inches in diameter running therethrough having fitted into it at opposite ends thereof punches 18 and 19 of the same alloy material. The assembly with the powder charge is placed in a vacuum chamber and heated to temperature by a conventional resistance heat susceptor.

In loading the die and punch assembly, a graphite foil disc 19A (0.005 inch thick) is placed on the inner end face of punch 19 within cavity 17 as shown; the cavity is lined with graphite foil to provide a sleeve thereof; and the powder material 22 then charged therein from the opposite end. Another graphite foil disc 18A is placed on top of the powder and punch 18 then inserted into the cavity in compression relationship to the powder charge. Pressure is applied to both punches in the direction of arrows 20 and 21 using a 30-ton capacity press. The graphite foil (discs and sleeve) help to eliminate contamination during the hot pressing cycle and also avoids fusion of the powder to the die and punches.

In applying the pressure after positioning of the die assembly with the vacuum heating chamber, a minimum pressure of lbs. (dial reading) is applied from room temperature to 1050 C., at which time the 18,000 p.s.i. load is applied and held for 1 hour. Thereafter, the power is shut 0E and the pressure released. As the pressed part reaches black heat, an argon back fill is employed to obtain rapid cooling under inert conditions.

The density obtained is substantially equal to full density (for example, at least 99.9% of theoretical). The cylindrical product is cleaned by grinding or machining and the opposite faces are finished parallel for subsequent cutting into magnetic pole pieces. The final hardness on the Rockwell C scale is generally at least about 50 R The preferred primary grain size of the final product lies within the ASTM 8 to 11 range as measured in accordance with ASTM E112 at 100 times magnification.

In order to assure optimum magnetic properties, it is desirable that voids and inclusions not exceed a singular defect size greater than 10 microns. In addition, the distribution of defects should be such that the average distance between defects is at least 10 times greater than the maximum defect diameter.

A fully dense, hot consolidated product produced in accordance with the invention comprises approximately by weight 9.4% silicon, approximately 5.7% aluminum and the balance essentially iron. In addition, the alloy contains oxygen within the preferred range of 3400 p.p.m. to 4400 p.p.m., which provides a metallographic structure having the desired grain boundary oxide film exhibiting optimum wear resistance for magnetic pole pieces produced from the product. FIG. 4 illustrates such a microstructure. In determining the wear resistance of this povwder metallurgy product, actual field testing was employed. Wear rates versus time data have disclosed that the powder metallurgy product exhibits at least a three to one improvement in pole piece life as compared to the same alloy in the conventionally cast form but without oxygen.

Summarizing the invention, a powder metallurgy method is provided of producing a hot consolidated magnetically soft ferrous alloy suitable for use in the manufacture of magnetic pole pieces. The ferrous alloy powlder contains an effective amount of silicon and aluminum ranging from about 2 to 12% silicon, from about 2 to 10% aluminum, about 2000 p.p.m. to 8000 p.p.m. oxygen, and the balance essentially iron. The oxygen is added to the powder by pre-oxidation to provide a thin oxide film thereon and then hot consolidated at an elevated temperature sutficient to provide a substantially fully ldense sintered body.

It is advantageous to employ milled and/or unmilled atomized powder (substantially flake-free) produced from vacuum cast alloy having a particle size range of about 325 mesh +5 microns and, more advantageously, from about 10 to 20 microns, the preferred alloy composition ranging by weight from about 9% to 9.8% silicon, about 5.4% to 6% aluminum, about 3300 to 4400 p.p.m. oxygen, and the balance essentially iron. A particular composition is one containing approximately 9.4% silicon, approximately 5.7% aluminum, and the balance essentially iron. The sintered body is generally characterized metallographically by a grain size within the ASTM 8 to 11 range.

The preferred range of 3300 to 4400 p.p.m. of oxygen is directly related to the improved Wear resistance and magnetic performance of the alloy. However, as stated above, this range can be broadened for less stringent applications.

In vacuum hot pressing the alloy powder, the temperature may range from about 1000 C. to 1100 C. with the preferred temperature being about 1050 C.

In hot pressing the thermally oxidized powder under vacuum, the pressure to achieve substantially full density may range from about 12,000 to 20,000 p.s.i. (e.g. 18,000 psi). As stated hereinbefore for a pressure of 18,000 p.s.i., the preferred temperature of 1050 C. is reached in about 3 hours, the compressed powder being held at temperature for one hour and thereafter cooled to black heat in 2 hours. At the lower temperature range, a longer time of pressing is employed, while at the higher temperature range, a lower time intent} is used.

In thermally oxidizing the powder in air, the temperature may range from about 450 F. to 650 F. and, more preferably, from about 500 F. to 600 F.

Although the present invention has been described in conjunction with preferred embodiments, it is to be understood that modifications and variations may be resorted to without departing from the spirit and scope of the invention as those skilled in the art will readily understand. Such modifications and variations are considered to be within the purview and scope of the invention and the appended claims.

What is claimed is: 1. A powder metallurgy method of producing a magnetically soft ferrous alloy suitable for use in the manufacture of magnetic pole pieces characterized by improved resistance to wear when in rubbing contact with a moving magnetic playback tape of gamma iron oxide which comprises,

providing a ferrous alloy powder composition of said magnetic alloy containing an elfective amount of silicon and aluminum in amounts ranging from about 2% to 12% silicon, from about 2% to aluminum, and the balance essentially iron, in which particles thereof of size falling within the range of 325 mesh to 5 microns are characterized by a thin encapsulating film of oxide formed by thermal oxidation at an elevated temperature, the amount of oxygen ranging from about 2000 to 8000 p.p.m.,

and then hot consolidating said powder in vacuum at an elevated temperature suificiently to provide a substantially fully dense sintered body. 2. A powder metallurgy method of producing a magnetically soft ferrous alloy suitable for use in the manufacture of magnetic pole pieces characterized by improved resistance to wear when in rubbing contact with a moving magnetic playback tape of gamma iron oxide which comprises,

providing an alloy powder composition of said magnetic alloy of average particle size ranging from about 10 microns to 20 microns consisting essentially of about 9%, to 9.8% silicon, about 5.4% to 6% aluminum, and the balance essentially iron,

thermally oxidizing said powder at an elevated temperature whereby to produce a thin oxide film thereon, the amount of oxygen ranging from about 2000 to 8000 p.p.m.,

and then hot vacuum pressing said powder at an elevated temperature ranging from about 1000 C. to 1100 C. to form a substantially fully dense body thereof,

the average grain size of the hot pressed body corresponding to a size within the range of about ASTM 8 to 11.

3. The method of claim 2, wherein the powder is thermally oxidized in air at a temperature of about 450 F. to 650 F.

4. The method of claim 3, wherein the alloy composition consists essentially of approximately 9.4% silicon, approximately 5.7% aluminum, and the balance essentially iron.

5. A powder metallurgy method of producing a magnetically soft ferrous alloy suitable for use in the manufacture of magnetic pole pieces characterized by improved resistance to wear when in rubbing contact with a moving magnetic playback tape of gamma iron oxide which comprises,

providing an atomized alloy powder composition of said magnetic alloy of average particle size ranging from about 10 microns to 20 microns consisting essentially of about 9% to 9.8% silicon, about 5.4% to 6% aluminum and the balance essentially iron, thermally oxidizing said powder in air at a temperature of about 450 F. to 650 F. to produce a thin oxide film on the particles thereof corresponding to a total oxygen content of about 3300 p.p.m. to 4400 p.p.m., forming a compact of said powder, and then hot vacuum pressing said powder at an elevated temperature of about 1000 C. to 1100 C. to form a substantially fully dense body thereof,

the average grain size of the hot pressed body corresponding to a size within the range of about ASTM 8 to 11.

References Cited UNITED STATES PATENTS 3,661,570 5/1972 Moss -206 2,864,734 12/1958 Adams et a1 29-1825 X 3,598,925 8/ 1970 Sakai et a1. 79-1002 C 3,614,339 10/19711 Schneider 79-1002 C 2,992,474 7/ 1961 Adams et a1. 29-11825 2,988,806 6/1961 Adams et a1. 29-1825 3,720,551 3/1973 Allen 75-212 X FOREIGN PATENTS 989,500 4/ 1965 Great Britain. 445,614 4/1936 Great Britain.

BENJAMIN R. PADGETI, Primary Examiner R. E. SCHAFER, Assistant Examiner US. Cl. X.R.

Referenced by
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US4069043 *Jan 19, 1976Jan 17, 1978Carpenter Technology CorporationWear-resistant shaped magnetic article and process for making the same
US4126451 *Mar 30, 1977Nov 21, 1978Airco, Inc.Manufacture of plates by powder-metallurgy
US4336066 *May 23, 1980Jun 22, 1982Nippon Gakki Seizo Kabushiki KaishaMethod for manufacturing components for magnetic heads of increased abrasion resistance
US4532737 *Dec 16, 1982Aug 6, 1985Rca CorporationMethod for lapping diamond
US4533384 *Jun 16, 1983Aug 6, 1985Thyssen Aktiengesellschaft Vorm. August Thyssen-HutteProcess for preparing binder-free hot-briquets
US4564401 *Sep 29, 1983Jan 14, 1986Crucible Materials CorporationMethod for producing iron-silicon alloy articles
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US4693863 *Apr 9, 1986Sep 15, 1987Carpenter Technology CorporationProcess and apparatus to simultaneously consolidate and reduce metal powders
US4752344 *Dec 22, 1986Jun 21, 1988International Business Machines CorporationMagnetic layer and method of manufacture
US4801505 *Oct 20, 1987Jan 31, 1989Fuji Photo Film Co., Ltd.Magnetic recording medium
US4956220 *Mar 20, 1987Sep 11, 1990Hitachi Maxell, Ltd.Magnetic recording medium
US5238507 *Jun 8, 1990Aug 24, 1993Matsushita Electric Industrial Co., Ltd.Magnetic material
US5350628 *Nov 19, 1992Sep 27, 1994Matsushita Electric Industrial Company, Inc.Magnetic sintered composite material
US20060027950 *Aug 3, 2005Feb 9, 2006Denso CorporationMethod for manufacturing soft magnetic material
US20140352667 *Jun 4, 2014Dec 4, 2014Continental Automotive GmbhFluid Injector For a Combustion Engine
EP0088992A2 *Mar 9, 1983Sep 21, 1983Asea AbMethod for manufacturing an object of soft-magnetic material by bonding together a mass of powder grains
Classifications
U.S. Classification419/19, 419/48, 419/60, 419/23, 428/928, 419/35, 419/31, 75/232
International ClassificationC22C33/02, C22C32/00, B22F3/14
Cooperative ClassificationY10S428/928, B22F3/14, C22C33/0278, C22C32/0026
European ClassificationB22F3/14, C22C33/02F4, C22C32/00C4
Legal Events
DateCodeEventDescription
Mar 21, 1988ASAssignment
Owner name: CHROMALLOY GAS TURBINE CORPORATION, BLAISDELL ROAD
Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNOR:CHROMALLOY AMERICAN CORPORATION;REEL/FRAME:004862/0635
Effective date: 19880311
Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:CHROMALLOY AMERICAN CORPORATION;REEL/FRAME:004862/0635
Owner name: CHROMALLOY GAS TURBINE CORPORATION, A DE. CORP., N