METHOD OF MANUFACTURING POWDER COMPACTS

Abstract: A method of making high density powdered metal com­ pacts and also a method for making high density powder metal sintered products is disclosed. With respect to the com­ pacts, iron powder of coarse or fine configuration is mixed or coated with a low-melting metal additive selected from the group consisting of tin, copper-tin, copper-lead, or lead in a percentage by weight of 2-5% of the admixture. The admix­ ture is subjected simultaneously to both heat (at a tempera­ ture level such that the low-melting alloy is in a liquid phase) and pressure which is in the range of 10-30 tsi. Upon relief of heat and pressure, the agglomerated or compacted product will possess an increased density in excess of 80% and an improved hardness and strength level. With respect to a sintered product, the powder metal is selected to have a fine particle size (average range of about 4-5 microns) and the powder is dry impact coated by ball milling with a low-melting additive such as tin, copper-tin, copper-­ lead or lead; the coated particles are warm briquetted and subjected to a sintering operaton whereby the resulting pro­ duct has a minimum density of 97% or more.

Description: CRIPTION This invention relates to a method of making powder compacts. Powdered metal compacts have been used in some industrial applications, but have not generally found fuli acceptance because the extra method steps and the added cost required to obtain a reasonable strength level and density in the powdered metal compact have been excessive, particularly when compared to similar parts obtained by melt formation. The conventional commercial mode of processing powdered metal to form compacts typically comprise (a) blending and milling together selected powder elements in the presence of a lubricant, (b) compacting the mechanicall i blended charge (c) heating the compact under a reduncing atmosphere for a period of 30 min. at 810 C to volatilize the lubricant, and (d) sintering the compact at an appropriate temperature. This has resulted at best in a green density prior to sintering of about 79-86% and a sintered density of 80-89% of theoretical. A higher density level would require additional hot forging to increase the strength level any reduce porosity. In order to increase the strength ana density of the parts without seconÅary corsole-ation (hot forging), it bas been proposed to effect cold briquetting or celd compacting with a low melting matrix element effective to close pores; this processing is then followed by conventional sintering (U.S. Patents Nos. 1,922,548 and 1,793,757 disclose such proposals). Another method is to raise the temperature of the blended powders to a liquid-solid condition and then sinter such powders in such multiphase condition while under pressure. This is exemplified in U.S. Patent 3,393,630. rnhe principal difficulty that is experi enced ':it} cOlL briquetting is th'.t it promotes a negative effect on density even when low melting filler agents are employed. The principal difficulty of sintering under pressure while in the liquide-solid condition without any pre-compaction is that the equipment is severely pressed and subjected to considerable wear resulting in increased cost of processing. According to the present invention, there is provided a method of producing a metal powder compact which comprises compacting metal powder in the presence of from 1 to 5% by weight of a low-melting point metal at a temperature sufficient to melt the lovi-melting point metal. In the preferred embodiment of the invention, 1-5%, preferably 2-4g of a low melting metal ingredient (preferably selected from copper-tin, copperlead, and lead) is added to a coarse or fine iron powder and the mixture is subsequently warm- briquetted (preferably at a temperature of 450-6500F) to form a liquid phase of said addition agent while consolidating the powder. The particle size of the base iron powder is preferably relatively fine (4-5 microns) and about 2.5% of a liquid phase promoting ingredient, particularly tin, is preferably added thereto, the blended mixture has warm briquetted at a temperature of from 450 to 650 F. The compact may then be sintered. Desirably a cryogenically-produced fine powder is used as the source of the powdered metal. The present invention includes two preferred embodiments:- (I) the addition of 1-5% of a low-melting metal, such as which results, after warm briquetting, in a compact having 25% less porosity and increased strength compared with a conventional cold briquetted compact; and (II) the adaition of 1-5 < of a low melting metal, such as tin or lead, to a fine particle size iron powder, which results, after warm briquetting and sintering, in a product having only 3% porosity compared with 2Q.1 porosity when tin or lead is not used. The unprecedented strength and density level of the warm briquetted compact makes it possible to produce certain powder metal parts without sintering, resulting in significant energy savings. Candidate parts would be heat sinks (such as diodes) and steering column collars. With respect to the 9 7% dense sintered powder product, it can be produced with existing equipment (no forging) which represents a major potential for a new class of powder metal business. A preferred mcthod for carrying out the first aspect of this invention is as follows: (1) An iron powder is prepared preferably by water atomization which may have either a coarse or a fine particle configuration. If a coarse coniiguration is employed, the average article size should be in the range of 80-100 microns and if a fine particle size configuration is used, the average particle size should be about 4-5 microns. When the powder is produced by water atomization, the chemical content of the powder will typically consist of 99.8% Fe, 0.05% C, 0.04% Mn, and .03% Si. Since the water atomization technique will require subsequent grinding and screening, the ultinate product from this production cycle will result in a screen analysis such as 2D, coarse, 60, fine, and 20, ultrafine. The particle size of the powder to be used herein should preferably be uniform but may be a blend of coarse and fine particle configurations provided the ratio is within the range of 1/2 or less. If other powder mìng techniques are employed, such as the carbonyl process, the particle size range and chemistry will be affected. (2) The selected and sized iron powder is dry impact coated with a low-melting metal selected from the group consisting of tin, copper-tin, lead, and copper-lead. One preferred method for carrying out this dry impact coating is by use of a ball milling apparatus employing large impact or milling balls consisting solely of the low-melting metal, such as tin. The powder is placed preferably in a ball milling machine (for purposes of the trials herein, an interior chamber of 8 high x 8" in diameter was used). Tin laden milling elements, preferably in the form of solid tin balls of about .5" diameter, may be used. The powder charge was about 10 cubic inches and the milling time about 48 hours. willing time and the milling rate depend upon mill volume, mill diameter, si & of the tin balls, and the speed of rotation. The ball milling elements should have a diameter at least 50 times the largest dimension of any of the particle shapes of the powder. The function of this step is to transfer, by- impact, a portion of the tin ingredient, carried by the ball milling elements, to form a tin shell about substantially each particle of the powder. The coating is genrated by abrasion or scratching of the powder particle against the surface of the ball milling elements. This obviously is accomplished by rotating the housing of the ball mill machint to impart a predetermined abraaing force from the balls. The ball milling operation will cold work or generate defect sites in substantially all of the powder particles above 124 microns; since the majority of the particles selectee for the process will be below said size range, they will generally be free of cold work or defect sites. The ball milling operation should be carried sufficiently long so that substantially each particle will be fully coated; this requires statistically a minimum period of time so that tin coating will preferably be continuous. When this step is completed, the particles will be in a condition where they will all substantially have a continuous tin envelope (coating or shell). Although the shell should preferably be an impervious continuous envelope about each particle, it is not critical that it be absolutely impervious. (3) The dry impact coatediron particles are then subjected to a heating treatement while an agglomerating pressure is applied. Beat is applied to raise the temperature of the mass of particles to a level slightly above the melting temperature of the metal coating, which should be in the-range of 50-650 F, 419 F being necessary to melt pure tin, 4460F being necessary to melt an alloy &alpha; 99.6% tin and . J copper, a melting temperatui'e of 5940F is necessary to melt an alloy of 95% lead and 5% tin, and a melting temperature of 561 F is necessary to melt an alloy of 63% tin and 575% lead and a melting temperature of 618 F is necessary to melt pure load. The warm briquetting temperature could be mised to as much as 1350 F (720 C) if necessitated by the requirement to melt the metal coating, or to improve densification by plastic deformation 450-1358 F encoJapass warm briquetting herein. The pressure applied should be no more than 30 tsi (and preferably in the range of 10-30 tsi) so that wear on the tooling used for agglomera tion is reduced to a minimum. Agglomeration or compaction may be carried out by a conventional press to obtain the maximum desired densities herein. Compact densities herein are cinsiderably impurred to 80% or more of theoretical density. The presence o.- the oThi' tin or low melting envelope about the particles improve compressibility acting as a lubricant, and the liquified metal phase as a pore filler during the compaction operation. With prior uncoated powders, a density of about 82% of theoretical c (.4 gr. or cubic c'ntimeter is typically obtained using a compressive force of about 30 tsi; with a dry impact coated powder herein, densities of about 7.0 gm. per cubic centimeter can be obtained as the same fores level. (4) The application of heat and pressure is removed al- ..'ing the low-melting metal to solidify and form an auxiliary bend between the particles in addition to the normal compressive and mechanical interlocking bond therebetween. Test results of this kind of a warm briquetted product shows that it can be aubjected te a hardness test evidencing a Rockwell value of about RB45. Noreover, a special bend test for such a product will show that it has a strength level of at least 2000 psi, which is 400% greater than that of a product produced without the use of the low-melting metal lubricant. ':'ith respect to the second aspect of this invention, the first method is varied in either or both of two respects. First, the iron powder selected is limited to a fine particle size, averaging 4-5 microns. This can preferably be obtained by extracting the iron powder as a by-product of processing of scrap or machining chips from industrial metal work. To this end, scrap metal in the form of machine turnings are segregated or selected. Machine turnings are segments of ribbons of low carbon or alloy steel; the turnings should be selected to have a surface to volume ratio of at least 60:1. The machine turnings may be shavings cut from alloy bar, and the bar may have a chemistry which includes alloying ingredients such as manganese, silicon, chromium, nickel and molybdenum. The turnings will have a size characterized by a width of .1-1.0", thickness of .005-.03", and a length of 1-100". Machine turnings are usually not suitable for melting in an electric furnace because they prevent efficient melt down due to such surface to volume ratio. The turnings should be selected to be generally compatible in chemistry when in the final product; this is achieved optimally when the turnings are selected from a common machining operation where the saone metal stock was utilized in forming all the turnings. The selected scrap pieces are put into a suitable charg- ing passage leading to a ball milling machine (or equivalent impacting device). Within the passage means, an ingredient for freezing the metal pieces is 'introduced, such as liquid nitrogen; it is sprayed directly onto the metal pieces. Mere contact of the liquid nitrogen with the scrap pieces will freeze them instantly. The liquid nitrogen should be applied uniformly throughout its path to the point of impaction. The ball milling elements are motivated preferably by rotation of the housing to contact and impact the frozen pieces of scrap metal causing them to fracture and be comminuted. Such impaction is carried out to apply a sufficient fracturing force for a sufficient period of time and rate to reduce said scrap pieces to a powder form. The resulting powder will be layered or flake in configuration and typically have both coarse and fine powder proportions. A typical screen analysis for a cryogenic powder would be as follows (for a 100 gm. sample): Nach Wt. in Gm. After 72 hrs. Wt. in Gm. 60 60.0 31.5 100 19.5 11.0 140 5.5 7.5 200 6.5 18.0 325 4.5 22.5 +325 4.0 9.5 Secondly, the method is varied in another important aspect: the compact or briquetted product is subjected to sintering. This treatment can be carried out in a conventional sintering furnace vith heating to a temperatue preferably about 2000 F. The temperature to which the briquetted or compact is heated should be at least to the plastic region for the metal constituting the powder. h controlled or protective atmosphere may be maintained in the furnace, preferably consisting of inert or reducing gases. with sintering, a final density of about 97,' has been achieved without the necessity for secondary consolidation such as forging. This is an extremely high density for a process which is essentially two step and devoid of secondary consolidation. Since the compact does not contain a volatile lubriceting agent, such as Acromax, the delubrication step is eliminated from the process or from the zone in a sintering furnace. The resulting mechanical properties for such a sintered product would be as follows: tensile strength 115,000 psi, % elongantion 10%, and hardness RB78. Test results to support the above methods are depicted in Table I. In one test example, an iron powder specimen identified as Atomet 28 was employed which has a chemistry of 99,8%, Fe 0.05%C and an average particle size of 70-80 microns. The second powder specimen consisted of carbonyl powder, having a chemistry of 99.9% Fe 0.1% C and a particle size range of 4-5 microns. Each of the powders were subjected to a ry impact coating according to the step (2) described in the preferred method. Tin was employed in amount of 2.5% weight percentage of the powder mass. This required ball milling to be carried out for 2 period of 48 hours to achieve a coating thickness of about 0.1 micron. Each powder specimen was heated to a temperature level of 4730F. Density measuroments are obtained and compared with the same powder specimen but uncoated and prepared according to a conventional technique using 1% Zinc Stearate admixed lubricant. TABLE I EMI8.1 <tb> <SEP> Conventional <SEP> Tech <SEP> Liquid <SEP> Phase <tb> (Eo <SEP> Tin) <SEP> Campacting <SEP> (5%tin) <tb> <SEP> Green <SEP> 74 <SEP> (% <SEP> theoretical <SEP> 80 <SEP> (% <SEP> theoretical <tb> <SEP> Atomet <SEP> 28 <SEP> Density <SEP> density) <SEP> density) <tb> Sintered <SEP> 75 <SEP> " <SEP> " <SEP> 84 <SEP> " <SEP> " <tb> <SEP> Density <tb> <SEP> Green <SEP> 72 <SEP> " <SEP> " <SEP> 80 <SEP> " <SEP> " <tb> <SEP> Carbonyl <SEP> Density <tb> <SEP> Powder <tb> <SEP> Sintered <SEP> 80 <SEP> " <SEP> " <SEP> 97 <SEP> " <SEP> " <tb> <SEP> Density <tb> Although percentages of tin above 5% can be employed and will operably work within the system as described, it is auggested that more than 5% tin is not desirable because of economic reasons, tin being considerably more expensive than iron. Also certain physical characteristics are affected by the presence of large amounts of tin in the resulting product. It is important to point out that the use of tin by itself without the warm temperature to effect the liquid phase will create a negative effect on Density, The variation of density as a function of the percentage of tin employed is shown. It increase for those compacts which are produced with warm compaction at a temperature of about 473 F (2450C), the tin being in a liquid form during the compaction. Use of 2.5 or 5% tin in the solid state reduces the density that can be obtained from that achieve when tin is not present. It is therefor important to emphasize that the use of a low-melting temperature metal additive is only effective when compaction takes place with heat such that the additive is in liquid phase.

Claims: CLAIMS 1. A method of producing a metal powder compact which comprises compacting metal powder in the presence of from 1 to 5% by weight of a low-melting point metal at a temperature sufficient to melt the low-melting joint metal. 2. A method according to Claim I wherein the metal powder is compacted in the presence of from 2 to 4, by weight of the low-melting point metal. 3. A method according to Claim I or Claim 2 wherein the metal powder is compacted at a pressure of less than 30 tons per square inch. 4. h method according to Claim I or Claim 2 wherein the metal rowder-is compactcd at a pressure of from 10 to 30 tons per square inch. 5. A method according to any one of Claims 1 to 4 wherein the metal powder is iron. 6. A methods according to any one of Claims I to 5 wherein the low-melting point metal is tin, a cooper-tin alloy, a copper-lead alloy, or lead. 7. A method according to any one of Claims 1 to- 5 wherein the low-melting point metal is tin. 8. A method according to any one of Claims I to 7 wherein the metal powder is compected at a temperature of from 450 to 650 F. 9. A method according to any one of Claims 1 to S where- in the metal powder has a particle size of from 60 to 120 microns. 10. A method according to any one of Claims 1 to 9 wherein the metal powder particles are coated with the low-melting point metal prior to compacting. 11. A method according to Claim 10 wherein the coating is effected by dry-impact coating. 12. h method according to Claim 11 wherein the dryimpact coating is effected by ball milling with milling elements composed of or carrying the low-melting point metal 13. A method according to Claim 11 wherein metal powder compact is sintered. 14. A method of making high density powdered metal compacts comprising adding 2-4% by weight of a low-melting point metal to an iron powder supply having P uniform particle size to form a mixture, and warm briquetting the mixture at a temperature effective to melt the low-melting metal while employing a compacting pressure no greater than 30 T.s.i. 15. A method of making high density powdered metal compact, comprising: (a) preparing a 99.8 pure iron powder having a uniform particle size of 60-1 20 microns, (b) dry impact coating of the particles of prepared iron powder with a metal lubricating agent constituting 1-5% by weight of said powder, said agent being characterized by an ability to form a liwuid phase in the temperature range of 450650 F, (c) heating said coated powder to said temperature range for forming a liquid phase of said agent, while agglomerating said powder with pressure of 10-30 tsi whereby a compacted product is obtained having a theoretical density of at least 80%, a Rockwell hardness of RB45, and a bend strength of 2000 psi.

Inventors: KAUFMAN, SYDNEY MORTON, SUH, SANG-KEE
Applicants: FORD FRANCE SOCIETE ANONYME, FORD MOTOR COMPANY LIMITED, FORD-WERKE AKTIENGESELLSCHAFT
Application year: 1979
Main classification: B22F3
IPC codes: C22C33, B22F1, B22F3