GB1585583A - Container for hot consolidating powder - Google Patents

Abstract

In the process a hot-press mould is filled with powder of a metallic or non-metallic composition for the production of a sintered body and is hermetically sealed. The hot-press mould and the powder are heated to a temperature at which the hot-press moulding material flows in a plastic manner and the powder fuses by sintering. Then an external pressure is exerted on the entire outer surface of the hot-press mould in order to exert a hydrostatic pressure on the powder in the mould cavity and to compact said powder to form a sintered body. The volume of the mould cavity must not be larger than the total volume of the hot-press moulding material, in order to form around the mould cavity walls of such thickness that the outer surface of the walls does not closely follow the contour of the mould cavity. A high precision of the press moulding is thus obtained and the finishing is less complicated than in sintered bodies produced by known processes. <IMAGE>

Description

(54) CONTAINER FOR HOT CONSOLIDATING POWDER (71) We, KELSEY-HAYES COM PANY, a corporation of the State of Delaware, United States of America, of 38481 Huron River Drive, Romulus, Michigan 48174, United States of America, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement: This invention relates to the field of powder metallurgy and specifically to a container for hot consolidating powder of metallic and non-metallic composition and combinations thereof and a method for using the same.

Hot consolidation of metallic, intermetallic, and non-metallic powders and combinations thereof has become an industry standard. The advantages of hot consolidation over other techniques for consolidating powders are well known. In some cases, hot consolidation is the only practical powder metallurgical technique for consolidating certain high temperature material. For example, hot consolidation is employed extensively for high temperature - high stress materials, such as nickel-base superalloys (e.g. IN-iO0).

Hot consolidation can be accomplished by filling a container with a powder to be consolidated. The container is usually evacuated prior to filling and then hermetically sealed. Heat and pressure are applied to the filled and sealed container. This can be accomplished by using an autoclave.

The gas pressure produced in the autoclave applies an equal pressure over the surface of the container and cuases the container to shrink, or collapse, against the powder. As the container shrinks, or collapses, the powder is densified. In other words, at elevated temperatures, the container functions as a pressure transmitting medium to subject the powder to the pressure applied to the container. Simultaneously, the heat causes the powder to fuse by sintering. This process for densifying powder is generally referred to as hot isostatic pressing. In short, the combination of heat and pressure causes consolidation of the powder into a substantially fully densified and fused mass in which the individual powder particles have lost their identity.

After consolidation, the container is removed from the densified powder compact.

The compact is then further processed through one or more steps, such as forging, machining, and/or heat treating, to form a finished part.

An extremely critical element of the hot consolidation process is the nature and characteristics of the container. The material of which the container is made must be capable of performing as a pressure transmitting medium at temperatures high enough to cause sintering of the powder, that is, the container must be flexible or deformable yet maintain structural integrity at elevated temperatures. The container must be non-reactive, or only slightly reactive, with respect to the powder contained therein, or steps must be taken to shield the container from the powder. Since the container must be hermetically sealed, and in some cases vacuum evacuated, the container must be capable of withstanding heating and pressing without cracking. The type of container employed will also determine, to a large extent, the degree of precision with which the compact can be made.In other words. some types of containers are only capable of producing simple billet stock shapes and rough preforms which require extensive subsequent forging and machining to produce a finished part.

Due to the high cost of raw material and the cost of forging, recent efforts have been made to develop containers capable of producing compacts of greater precision to thereby reduce material and forming costs.

Such high precision compacts are generally referred to as "near-net shapes". Such precision compacts would only require machining or, at most, a simple forging operation, to produce a final shape, thus eliminating extensive intermediate forging steps. This invention is preferably, directed to a hot isostatic pressing container which meets the foregoing requirements as well as demonstrating the capability of producing near-net shapes.

The prior art includes many examples of containers for hot consolidating powder.

These containers are made of various materials, such as metal, glass and ceramics. The earliest containers used for hot consolidating powder, and the ones most commonly encountered in current industrial practice, are made of metal. The particular type of metal employed for the container is usually selected in view of the composition of the powder to be consolidated. That is, the requisite temperatures and pressures of consolidation and the reactivity of the powder are taken into consideration when determining the container material. Metal containers for hot consolidating nickel-base superalloys are commonly made of stainless steel. Other metals, however, are used for powders of different composition.

Examples of typical metal containers are shown in U.S. Patents 3,340,053 and 3,356,496. It is noted that these metal containers are relatively thin-walled and of simple shape. The reason that thin-walled containers have been used is that an effort was made to duplicate, as near as possible, the behaviour of a flexible rubber bag of the type which had been used to isostatically press powders at near room temperature.

Of course, rubber bags could not be used at the elevated temperatures required for hot consolidation. The theory was, however, that a thin-walled metal container would behave, at elevated temperatures, much like a rubber bag at near room temperature. It was learned that this was not the case. The walls of a thin-walled metal container do not transmit pressure evenly to the powder due to variations in the structural strength of the container. Consequently, thin-walled metal containers tend to buckle or wrinkle in weaker sections. When simple shapes, such as billet stock or forging preforms, are being produced, surface defects caused by buckling and wrinkling of the thin-walled metal container can sometimes be tolerated since these defects can be removed by machining.

It is very difficult, if not impossible. however, to produce more complicated precision shapes using thin-walled metal containers.

One of the greatest difficulties in producing precision shapes using thin-walled metal containers is that the resulting compact is greatly distorted due to non-uniform reduction in the size of the container. In other words, the shape of the resulting compact after compaction is far different from the shape of the cavity initially defined by the thin-walled container. Although such distortions, in most cases, can be accomodated for by making a greatly over-sized compact, this is done at the expense of excessive forging and/or machining and material waste.

Attempts have been made to solve the problems associated with thin-walled containers and to provide a container capable of producing near net shapes. For example, in the U.K. Patent 1,339,669 a method of consolidating metallic powder is disclosed in which a relatively thick-walled container is formed by joining two mold halves which are made of sintered metal powder and by encasing the mold halves in an outer metal sheath. The mold halves are made of sintered metal powder so that the porosity, or density, of the walls of the mold halves are approximately equal to the tap density of the powder contained in the cavity formed by the mold halves. Upon the application of heat and pressure, it is intended that the density of the container and the powder contained therein both increase substantially simultaneously to uniformly compact the powder without distortion.Another deviation from the traditional thin-walled metal container is disclosed in U.S. Patent 3,230,286. The container disclosed in this Patent is made of a metal, such as cerium, bismuth. cesium, or alloys thereof, which undergoes an abrupt densification, or reduction in volume, at a predetermined pressure. The abrupt densification, or reduction in volume, is due to a rearrangement of the crystal lattice structure of the material caused by the applied pressure. The reduction in volume is relied upon to apply pressure to the powder contained within the container.

In summary, in the development of containers and methods for hot isostatic pressing powder, the first efforts were to simulate a flexible rubber bag. Hence, thin-walled metal containers were employed. As the art advanced, various attempts were made using thicker walled containers; however, in the case of metal containers, the containers were made porous or an exotic alloy was employed which is capable of an abrupt densification under the influence of extreme pressures. These rather complicated measures were taken because it was generally believed that a thick-walled container would not effectively transmit pressure to the powder. When materials other than metals were employed, such as glass or ceramics, the container walls were also made relatively thin. If not thin, then the material was in particulate form.This required additional steps to contain the particulate material, such as the use of the inner and outer containers shown in U.S. Patent 3,700,435.

Notwithstanding all the development effort thus far expended, there is no commercially acceptable container available which is capable of producing precision compacts or near-net shapes.

According to the invention there is provided a method for hot compacting powder of metallic and non-metallic composition to form a densified compact comprising encapsulating a quantity of powder in a cavity in a thick-walled container as herein defined, having walls entirely surrounding the cavity and of sufficient thickness so as not to closely follow the contour of the cavity and of a material which is substantially fully dense and incompressible and capable of plastic flow at elevated temperatures, heating the container and powder to a temperature at which the powder will densify and applying external pressure to the entire exterior surface of the container thereby causing plastic flow of the container walls to subject the powder to a hydrostatic pressure which causes it to densify into the compact.

Further according to the invention there is provided a container when used in a method according to the invention for producing a compact of a metallic and/or non-metallic composition powder by applying a hot compacting temperature and pressure of the powder to the powder, the container being formed of a substantially fully dense and incompressible material having such a tensile strength that plastic flow of a portion of the material is produced at the hot compacting temperature and pressure of the powder. the container comprising a cavity for receiving a quantity of powder. surrounded by a wall or walls of sufficient thickness that. on application of the hot compacting temperature and pressure of the powder to the container the container material becomes plastic to provide a hvdrostatic pressure to be applied to the powder in the cavity.

This invention is based upon a recognition by the inventor that a superior container for hot consolidating powder can be made from a substantially fully dense and incompressible material if the material is capable of plastic flow at pressing temperatures and that. if the container walls are thick enough.

the container material will act like a fluid upon the application of heat and pressure to apply hydrostatic pressure to the powder. In other words. it is not necessary to use a porous material as described in U.K. Patent 1.399.669 and U.S. Patent 3.7()().453 or a material which undergoes an abrupt densification as described in U.S. Patent 3,230,286. It has been determined by the inventor that the container walls are thick enough to function in the intended manner even when the exterior surface of the container walls does not closely follow the contour of the container cavity. In other words, the exterior surface of the walls of the container do not need to follow the contour of the container cavity as, for example, do the walls of the container described in U.S. Patent 3,841,870.It is noted that the exterior surface of the walls of the container described in this Patent define a shape which is substantially identicalto the shape of the container cavity. This is typical of what is referred to as a "thin-walled" container.

The container of the present invention constitutes a radical departure from the generally accepted principles relating to containers for hot consolidating powder.

The term "thick-walled" is defined herein as meaning that the walls of the container are sufficiently thick for a part to become plastic to produce a hydrostatic pressure on the powder when the compacting temperature and pressure is applied to the outer walls of the container. This facilitates uniform shrinkage, permits a closer prediction of final dimensions, and reduces distortion.

Hence. it is possible to produce near-net shapes. In order to achieve these results, however. a container is used which is made of a substantially full dense and incompressible material. The walls of the container surrounding the powder-receiving cavity are thicker than the prior art suggests would be capable of transmitting pressure. Any heretofore known containers having walls of any significant thickness have been made of a compressible or particulate material. It has been discovered by the inventor that the thickness of the container walls does not hinder compaction. but to the contrary. is desirable and essential to produce a hydrostatic-like pressure at the interface between the container material and the powder in the cavity.In other words. a thick-walled container of the type described herein produces better results than thin-walled containers because of its ability to apply hvdrostatic pressure to the powder.

The container of the invention was specificallv designed for consolidating superalloy powder. such as. IN-10(). which is a wellknown nickel-base alloy which includes alloving elements of aluminium. titanium.

tantalum. columbium. molybdenum. tungsten. chromium and cobalt. IN-IO(). and other superalloys. are employed in turbine engine components. for example. because of their high strength characteristics at elevated temperatures. These high strength characteristics. however. make these alloys difficult to work. Conventional casting tech niques cannot easily be used since the many alloying elements produce segregation problems in the cast object. Additionally, the inherent strength of these alloys at high temperatures make forging difficult and expensive. Accordingly, it has become necessary to employ powder metallurgy techniques to produce superalloy parts having optimum physical characteristics. Even present day powder metallurgy techniques often require multiple forging and machining operations to produce a final shape.

Efforts have therefore been made to produce precision powder metal compacts, or near-net shapes, to reduce, or eliminate, forging and to reduce the amount of material which must be removed by machining to produce a finished shape. The container constructed in accordance with the instant invention offers this advantage.

Embodiments of the invention will now be described by way of Example only with reference to the accompanying illustrative drawings in which: Figure 1 is a cross-sectional elevational view of a container for hot consolidating powder constructed in accordance with the present invention showing the container before hot consolidation and, in phantom, after hot consolidation; Figure 2 is a broken-away view of Figure 1 illustrating probable force distribution when pressure is applied to the container; Figure 3 is a cross-sectional elevational view of another embodiment of a container for hot consolidating powder constructed in accordance with the instant invention; Figure 4 is a cross-sectional elevational view of a densified compact subsequent to hot consolidation in the container of Figure 3;; Figure 5 is a cross-sectional elevational view of a finished part machined from the densified compact of Figure 4; Figure 6 is a cross-sectional elevational view of an embodiment of a container for hot consolidating powder designed particularly for hot consolidation in a press; and Figure 7 is a cross-sectional elevational view of suitable upper and lower press dies for use with the container of Figure 6.

A container for hot consolidating powder constructed in accordance with the invention is generally shown at 10 in Figure 1.

The container 10 includes an upper die section 12 and a lower die section 14. In the embodiment shown, the upper and lower die sections 12 and 14 are made from a standard billet stock of low carbon steel, such as an SAE 1008 to 1015 steel. Low carbon steel is a particularly desirable material for the container 10 since it is relatively inexpensive and easy to machine. It is noted, however, that other metals can be employed and, in fact, other materials, such as glass or ceramic, as long as the materials behave in the manner set forth herein.

In order to make the container 10 shown in Figure 1, two pieces of low carbon steel were machined using standard metal cutting techniques to form the upper and lower die sections 12 and 14. When the die sections 12 and 14 are joined along their mating surfaces, the upper and lower die sections form a cavity 16 having a predetermined desired configuration. The container 10, shown in Figure 1, is specially adapted to form a type of turbine disc for a jet engine. For this particular turbine disc, the cavity 16 is provided with a main section 18, which is generally disc-shaped, for forming the body of the turbine disc and a ring portion 20 which extends generally laterally from each side of the disc-shaped main section 18.

The size and shape of the cavity is determined in view of the final shape of the part to be produced. Since IN-100 powder has a tap density which is less than its theoretical density, typically 65% of theoretical density, the cavity is made large enough to accomodate a reduction in size sufficient to reach approximate theoretical density in the densified compact. Additionally, the container is designed so that the size of the densified compact after consolidation is somewhat larger than the final part. This extra material is removed by machining to form the final part.

Before the upper and lower die sections are assembled, a hole 22 is drilled in one of the die sections 12 and a fill tube 24 is inserted. The fill tube 24 for the container 10 is a piece of cold-drawn seamless steel tubing. The fill tube 24 is attached to the upper die section 12 by welding. Care is taken to insure that the welds do not leak since the fully assembled container must be evacuated to a level of about 5 - 10 microns prior to filling.

After the fill tube 24 has been attached, the two die sections 12 and 14 are placed in mating relationship and welded together. In order to facilitate welding. the outer edges of the die sections 12 and 14 are chamfered at approximately a 45" angle. When the two die sections 12 and 14 are properly assembled, the chamfered edges form a welding trough 26 for receiving weld material 28.

Again, care is taken during welding to ensure that a hermetic seal is produced to permit evacuation.

It is noted that the starting pieces of billet stock, out of which the upper and lower die sections 12 and 14 were made, are of sufficient size so that, after machining, relatively thick walls remain. That the container includes thick walls is evidenced by the fact that the external shape of the container 10 has no relation to the complex shape of the cavity 16 therein. A character istic of the thick-walled containers tested is that the volume of the cavity is not greater than the total volume of the container walls.

As will be further described, the use of thick walls reduces the distortion problems associated with thin-walled containers and permits the production of near-net shapes.

While low carbon steel was used to make the container 10, other materials can be employed. Suitable container material is characterized by certain physical characteristics. Using low carbon steel as an example, in billet stock form, the starting material for the container 10 described herein, the material is substantially fully dense. In other words, ignoring production defects, such as random porosity, the steel is as close to its theoretical density as can be obtained by standard production methods. Low carbon steel is also substantially incompressible in that its volume cannot be significantly reduced by the application of pressure. The container material may also be gas impervious, as is low carbon steel, to permit hermetic sealing of the container.These characteristics and physical properties distinguish the container material of the present invention from many of the materials heretofore employed. Further distinguishing characteristics are that the container walls are substantially uniform in composition across a cross-section from the exterior surface to the cavity and that the container walls are of substantially uniform density.

In addition to the foregoing, the container material may function as a pressure transmitting medium at the temperature and pressure necessary to compact the powder.

In order to achieve this result, the container material must be capable of plastic flow at suitable pressing temperatures. Specific pressing temperatures are determined, in great part, by the composition of the particular type of powder being compacted.

Once the pressing temperature is determined, a suitable container material can be selected which is capable of plastic flow at such temperature. Most metals are capable of plastic flow even at room temperature, therefore, consideration must also be given to the amount of pressure required to cause plastic flow in the container material at the suitable pressing temperature. As the temperature increases the tensile strength of metal decreases so that lower pressures are required to cause significant plastic flow. In other words, in order to compact any given powder, the temperature. as well as the pressure, must be determined. Once these two parameters are determined then a container material is selected which is plastic, i.e. has a low enough tensile strength, at the particular temperature so that it will deform plastically with relative ease at the particular pressure employed.In the case of IN-100, pressing temperatures of between 1850O and 2200"F are common. As is wellknown, low carbon steel is capable of plastic flow under stress, and this capability increases with increasing temperature. At temperatures of 1850O to 22000F, significant plastic flow can be induced by the application of pressures of 10,000 to 15,000 psi.

While these pressures are commonly used in practice, lower or higher pressures may be used. In all cases, the extent of plastic flow depends upon the tensile strength of the material at the pressing temperature.

Another significant consideration is that the structural integrity of the container must be maintained during hot consolidation.

Structural integrity of a metal container is maintained as long as the temperature of consolidation does not exceed the melting temperature of the container material.

More precisely, the temperature should not exceed the melting temperature of any major solid phase of the container material.

If the melting point is exceeded, the container material will lose its strength in shear.

This would lead to the destruction of the container. Since other potential container materials, e.g., glass, consist of a supercooled liquid, it cannot reach the liquid state. A glass container formed in accordance with the invention would retain sufficient strength until its viscosity becomes so low that the glass is fluid.

Therefore, as a rule, the container material must retain sufficient strength at pressing temperatures to maintain the structural integrity of the container.

Another physical property of the container material which must be taken into consideration is the material's rate of expansion and contraction with temperature. When complex shapes are being produced, such as those which include undercuts, it is believed that the thermal expansivity of the container must be reasonably close to that of the material being compacted. If the thermal characteristics of the two materials are widely different, stresses will be built up in the compact during cooling which could cause fracture. While a critical difference has not been precisely determined, it is at least known that the difference in thermal expansivity between an SAE 1010 steel and IN-100 is not deleterious.In order to determine the best container material for consolidating other types of powder it may be necessary to conduct preliminary tests to insure that the thermal characteristics of the respective materials are compatible.

IN-100 powder and other superalloys are normally compacted at temperatures of between 18500 and 2200"F and pressures from 10,000 to 15,000 psi. Such pressures can easily be attained in commercially available autoclaves. At temperatures of be tween 185 to 0 and 2200"F and pressures of 10,000 to 15,000 psi, the walls of a thickwalled low carbon steel container act very much like a fluid. That is, the metal can flow under stress. Due to the fluid-like behavior of the container walls at these temperatures and pressures, a hydrostatic pressure is applied to the powder contained in the cavity. As used herein, a hydrostatic pressure is one in which the direction of the force acting on any surface of the powder is normal to the surface.A major problem with thin-walled containers is that, while a hydrostatic pressure may be applied to the external surface of the container, the container is not capable of transmitting a hydrostatic pressure to the powder. The application of a hydrostatic pressure will insure that near uniform shrinkage will occur.

It has been determined that the walls of a container are thick enough to accomplish the intended result, i.e. a hydrostatic pressure, if the exterior surface of the walls does not closely follow the contour of the cavity.

This definition is, at best, an approximation of what is referred herein to as a "thickwalled" container. In terms of a desired result, a thick-walled container is one which has walls that are thick enough to produce a hydrostatic pressure on the powder upon the application of heat and pressure. By way of example, one of the greatest problems associated with thin-walled containers arise when the part to be produced includes an annular portion, such as the ring-shaped extensions of the part shown in Figure 1. A typical thin-walled container surrounds three sides of the extension. as viewed in cross section, leaving the interior volume vacant. This arrangement causes serious distortion problems during hot compaction.

As a minimum in this case, the thickness of the container in the region of the annular portion must be sufficient to substantially fill the interior volume of the cavity in the region of the annular portion. When this is accomplished it can no longer be said that the exterior surface of the container follows the contour of walls that define the cavity of the container. The result is that the outer walls of the container solidly support the interior walls of the ring portion so that practically uniform and undistorted shrink age will occur.

The container 10 was processed in the following manner. Once the die sections 12 and 14 were welded together, a vacuum pump was connected to the fill tube 24 and the cavity 16 was evacuated. This procedure was followed in the case of IN-100 powder to prevent contamination by atmospheric gases which would produce undesirable oxides and nitrides and to eliminate a potential source of porosity in the resulting compact. Additionally, a vacuum within the container increases the difference in pressure between the external and internal surfaces to facilitate pressing. It is noted, however, that these precautions may not be necessary for other types of powder. Once evacuated, the container 10 was filled with atomized IN-100 powder. During the filling stage it was necessary to fill all portions of the cavity 16 and to achieve the highest tap density.This- was accomplished by rotating the container and by striking the sides of the container with a mallet. It is noted that this procedure, although highly successful in ensuring complete filling and maximum tap density, is difficult to perform on a thinwalled metal container without bending the walls and changing the shape of the cavity.

After the container 10 was filled, the fill tube 24 was hermetically sealed by pinching it closed and welding it. The filled and sealed container 10 was then placed in an argon gas autoclave. The autoclave was cycled to subject the container 10 to a temperature of approximately 19500F and a pressure ranging up to 10,000 to 15,000 psi over a period of approximately two hours.

The pressure in the autoclave produced an isostatic pressure over the surface of the container. At the pressing temperature of 19500F, the low carbon steel had softened to the point where it could no longer support the pressure applied (10,000 - 15,000 psi) and plastic flow occured. The applied pressure provided the driving force for reducing the size of the cavity. It is possible to reduce the size of the cavity because the cavity is filled with a compressible material, i.e., the less than fully dense powder. The size of the cavity continues to shrink until the powder reaches approximately full density. As the powder densifies it also fuses by sintering so that the compact produced was a fully dense and solid mass.

After consolidation, the container 10 was removed from the autoclave and cooled.

The container was then removed from the densified compact by pickling in a nitric acid solution.

Since IN-100 is corrosion resistant, the nitric acid solution preferentially attacked the low carbon steel container. The container dissolved leaving the densified IN-100 compact. While a nitric acid solution was employed, other types of solutions can be used. Alternatively, the container could have been removed by machining or a combination of rough machining followed by pickling.

Before the container 10 was removed from the densified compact, the external shape of the container was measured and recorded. After the container 10 was removed, the dimensions of the densified compact were measured. By comparing the size and shape of the densified compact with the original cavity, the amount and manner of shrinkage could be determined. The dimensions of the container after compaction and of the densified compact are shown in phantom in Figure 1. Specifically, phantom line 30 outlines the shape of the densified compact while phantom line 32 outlines the exterior shape of the container 10.

It is noted that surprisingly uniform shrinkage occurred. Moreover, wall thickness of the container increased. The fact that areas such as 34 and 36 increased in thickness, or size, during hot compaction indicates that the direction of force applied to the powder was hydrostatic and unrelated to the direction of the force acting upon the surface of the container. This is shown schematically in Figure 2 which illustrates the probable directions of the forces acting upon the powder and the container. The direction of the force acting upon the surface of the container, which is indicated by arrows 38, is perpendicular to the container surface. The direction of the force's action upon the powder, which is indicated by arrows 40, is generally perpendicular to the surface of the cavity.The direction of forces acting on the powder, however, is not necessarily parallel to the direction of the force action on the container surface. This is characteristic of a hydrostatic pressure. This indicates that the container walls actually act like a fluid to apply a hydrostatic pressure to the powder. The result is a more uniform reduction in the size of the cavity.

For a number of reasons low carbon steel appears to be the most commercially attractive material from both economic and processing standpoints for making containers to hot consolidate IN-100 and other superalloy powders. Low carbon steel is relatively inexpensive (as compared to the cost per pound of the powder to be consolidated) and is easy to obtain. Low carbon steel is very machinable, it can be welded easily, and the finished container can withstand significant abuse. It is pointed out, however, that thick-walled containers in accordance with the instant invention may be made of other metals and other materials. Glass and ceramics are examples of such materials.

The important result is that plastic flow coupled with sufficiently thick container walls will produce a hydrostatic pressure upon the powder.

It is also noted that the invention is not limited to producing a cavity by machining.

Other well-known metalworking techniques, such as, casting or forging may be employed to produce the container. For example, a cast container can be produced by using an expendable core having the shape of the desired cavity. After the metal is cast around the expandable core, the core is removed, such as by leaching. A two-part container could also be produced by a forging process. The only drawback with forging is that undercuts could not be produced such as are possible with machining or casting.

A unique method for assembling a container for producing a part of extremely complex shape is shown in Figures 3 through 5. The desired part is shown generally at 42 in Figure 5. It is noted that this is a rather complex turbine disc which includes a number of undercuts. In order to produce a densified compact which can be machined to produce the part 42 shown in Figure 5, a cavity, generally indicated at 44, is formed in a thick-walled container having the shape shown in Figure 3. It should be apparent, that it would be difficult, if not impossible, to machine a cavity of such complex shape in a two-section container, such as the one previously described and shown in Figure 1.

In order to produce the part shown in Figure 5, the cavity 44 includes a generally discshaped portion 46 and a generally ringshaped portion 48 extending substantially laterally from the disc-shaped portion 46. In addition, the ring-shaped portion 48 angles inwardly in such a manner that it would be difficult to machine. Hence, the container is made in three sections. Specifically, the container includes a first main section 50, a second main section 52, and an intermediate section 54. The first main section 50 and the intermediate section 54 includes surfaces 56 and 58 which generally define the discshaped portion 46 of the cavity 44. The second main section 52 and the intermediate section 54 include surfaces 60 and 62 which define the ring-shaped portion 48. These three sections are machined separately and then fitted together to form the complex cavity 46.

As in the first embodiment of the container, the first and second main section 50 and 52 include joinable mating surfaces. The outer edges of these surfaces are chamfered to form a weld trough 64 for receiving weld material 66. A hole 68 is drilled in one of the main sections, in this case, the first main section 50 for receiving a fill tube 70 which is attachcd by welding. As shown in Figure 3, the intermediate section 54 is supported between the first and second main section 50 and 52 by co-operating the interfitting means which locate and support the intermediate section 54.The co-operating interfitting means includes an extension 72 of the cylindrical portion of the intermediate section 54 which fits into a cylindrical bore 74 in the second main section 52 and also an extension 76 of the cylindrical portion of the first main section 5O which seats in a cylindrical bore 78 in the intermediate sec tion 54.

This container was processed in generally the same manner as the first container.

After hot consolidation the densified compact recovered had the shape shown generally at 80 in Figure 4. This densified compact was then machined to the final shape shown in Figure 5. It is particularly pointed out that the final part 42 was produced without a forging operation and with minimal scrap.

The containers described above were subjected to heat and pressure by using an argon gas autoclave. It is noted, however, that other means may be employed to apply heat and pressure. One procedure which has been developed by the inventor herein includes pressing the container between the dies of a press.

In order to consolidate the powder using a press, a standard mechanical or hydraulic press is fitted with upper and lower dies similar to the upper and lower dies 82 and 84 shown in Figure 7. The lower die 84 includes a cavity for receiving a preheated, powderfilled container. The upper die 82 which is mounted on the ram of the press includes an extension 88 which enters the recess 86 to engage and apply pressure to the container.

Since the container material has been preheated to a temperature at which plastic flow will occur relatively easily and since the lower die 86 restrains the container, the container material will act like a fluid to subject the powder to a hydrostatic pressure. Since the powder in the container is at less than full density, the pressure of the container material will cause the powder to densify. Densification will proceed until the powder achieves full density. At this point, the entire mass, that is, the container material and the powder, is at full density.

The container is then removed from the lower die 84 by a suitable stripping opera tion and the container material is removed from the densified powder compact.

It is noted that the side walls 90 of the recess 86 in the lower die 84 are tapered and that the sides of the container 96 as shown in Figure 6 are provided with a corresponding draft angle to facilitate ejection of the container from the lower die 84 after press ing. The upper die 82 is also tapered to correspond to the taper of the lower die 84.

In the event that a mechanical press is employed, damage to the press could be caused if the powder reaches full density before the ram reaches the end of its downward stroke because the ram would be working against a fully dense and incom pressible mass. This could cause breakage of the press crank or at least jamming of the press. Obviously. this problem is not pre sented in a hydraulic press since its stroke terminates upon reaching a predetermined pressure.

In order to prevent damage to a mechanical press, the upper and lower dies 82 and 84 are designed to permit controlled escape of container material from between the dies when the pressure exceeds a desired maximum. In other words, a gap is provided between the sides 90 of the recess 86 in the lower die 84 and the sides 92 of the extension 88 of the upper die 82 to permit formation of a flash under conditions of excessive pressure. In order to ensure that the pressure experienced by the container is sufficiently high to achieve full densification of the powder, it may be necessary to force the escaping container metal to follow a tortuous path. For example, the sides 92 of the upper die 82 may be continued to form a curved surface 94 which would resist the flow of container metal by forcing it to reverse its direction of flow thus extending the path of the material.The additional surface also increases the total frictional resistance experienced by the material. In any event, the upper and lower dies are designed to relieve excess pressure by the controlled escape of container material.

A container designed particularly for consolidating the powder using a press is shown generally at 96 in Figure 6. The internal cavity of the container illustrates the rather complicated shapes which can be produced by this method. It should be apparent, therefore, that near net shapes can easily be produced. The container 96 includes an upper section 98 and a lower section 100 which have been machined from a low carbon steel. A core 102 is also machined from the same material and fitted between the upper and lower sections 98 and 100. As with the containers described above, the upper and lower sections 98 and 100 are welded together at their mating surfaces as indicated by the weldment 105.

In order to fill the cavity defined by the walls of the container 96 with powder, the upper section 98 is provided with one or more passageways 104 which communicate with the cavity. The passageways 104 extend through a conical-shaped portion 106 formed in the upper section 98 of the container and merge in a single opening 108.

A fill tube 110 is welded to the upper section 98 of the container at the opening 108 for conducting powder into the passageways 104. The fill tube 110 is also used to connect a vacuum pump to the container 96 for evacuating the cavity prior to filling with powder.

After the container 96 has been evacuated and filled with powder the fill tube 110 is closed by crimping the end of the fill tube as at 111.

When the powder is to be consolidated by pressing in a press. it is necessary to protect the fill tube 110 from damage. Since the contents of the container 96 are under a vacuum, damage to the fill tube 110 could result in a leak which would cause contamination of the powder. In order to prevent damage to the fill tube 110 a protective shield, generally indicated at 112, is welded to the container and surrounds the fill tube 110. The protective shield 112 comprises a sleeve 114 which is placed over the fill tube 110 and is welded to the container 96. In order to provide additional support the vacant space within the sleeve 114 may be filled with powder. A plug 116 is then welded across the entrance to the sleeve 114.

The upper die 82 includes a special configuration which corresponds to the exterior shape of the upper portion of the container 96. Specifically, it includes a tapered recess 118 which corresponds in size and shape to the conical portion 106 of the container 96. An extension 120 of the tapered recess is also formed to receive the protective shield 112 which is located on top of the container 96. It is noted that the extension 120 is also tapered and that the protective shield 112 is provided with a suitable draft angle for facilitating separation of the upper die 82 from container 96.

It is not essential that the container 96 include a domed portion 106. As an alternative the container 96 could have the shape indicated by the dotted line 121. The container shape shown, however, obviously requires less material than the alternative and, for this reason, is more desirable.

A typical procedure for compacting powder using a press includes the following steps. After the container 96 is fabricated a vacuum pump is connected to the fill tube 110 and the cavity of the container is evacuated to shrink the cavity about 10 microns. After evacuation the container is filled with powder while maintaining the cavity under vacuum. This can be accomplished by using a tee-type connection at the fill tube 110 wherein one branch of the tee is connected to the vacuum pump while the other branch is connected to a supply of powder. After filling, the fill tube 110 is closed. This may be accomplished by crimping the fill tube 110 and welding the crimped end.

As described above, the protective shield 112 is then attached to the container 96 so that it surrounds the fill tube 110.

The container 96 is then heated in a furnace to a temperature at which the powder will densify. The container material is selected so that at the appropriate densification temperature the container material will be capable of plastic flow when subjected to a pressure sufficient to cause densification of the powder. It has been found that for most applications, the container and powder are heated to a temperature of between 1,700"F and 2,300 F. The specific temperature is selected in view of the alloy composition of the powder being compacted. Suitable densification temperatures are well known for common alloys.

Within this range of temperatures a low carbon steel container will maintain structural integrity, but is capable of plastic flow at pressures exceeding about 5,000 psi. The heated container is then transferred to a press for consolidation of the powder.

A test part was made from titanium powder using a container having the configuration of container 96 by preheating to a temperature of about 1,750"F and applying a pressure of about 15,000 psi by means of a standard mechanical press outfitted with tools similar to those shown in Figure 6.

After heating in the furnace for a time sufficient to obtain a uniform temperature throughout, the container was conveyed to a press fitted with dies having the configuration of the upper and lower dies 82 and 84.

The press was then cycled through a single stroke. As described above, because the container is restrained by the lower die 82, the heated container material flows plastically and subjects the powder to a hydrostatic pressure which causes it to densify. Thereafter, the container 96 was ejected from the lower die 82 and cooled. The container was then removed from the densified powder compact.

Consolidating the powder using a press rather than an autoclave is advantagous since cycle time at maximum temperature can be reduced significantly. The typical cycle time in an autoclave can easily exceed four hours from loading to unloading while the cycle time for a press is measured in minutes. Moreover, autoclaves which operate in the 15,000 psi range are sophisticated pieces of equipment and are quite expensive. Therefore, the use of mechanical and hydraulic presses significantly simplify the consolidation process.

WHAT WE CLAIM IS: 1. A method for hot compacting powder of metallic and non-metallic composition to form a densified compact comprising encapsulating a quantity of powder in a cavity in a thick-walled container as herein defined, having walls entirely surrounding the cavity and of sufficient thickness so as not to closely follow the contour of the cavity and of a material which is substantially fully dense and incompressible and capable of plastic flow at elevated temperatures, heating the container and powder to a temperature at which the powder will densify and applying external pressure to the entire exterior surface of the container thereby

**WARNING** end of DESC field may overlap start of CLMS **.

Claims (25)

**WARNING** start of CLMS field may overlap end of DESC **. contents of the container 96 are under a vacuum, damage to the fill tube 110 could result in a leak which would cause contamination of the powder. In order to prevent damage to the fill tube 110 a protective shield, generally indicated at 112, is welded to the container and surrounds the fill tube 110. The protective shield 112 comprises a sleeve 114 which is placed over the fill tube 110 and is welded to the container 96. In order to provide additional support the vacant space within the sleeve 114 may be filled with powder. A plug 116 is then welded across the entrance to the sleeve 114. The upper die 82 includes a special configuration which corresponds to the exterior shape of the upper portion of the container 96. Specifically, it includes a tapered recess 118 which corresponds in size and shape to the conical portion 106 of the container 96. An extension 120 of the tapered recess is also formed to receive the protective shield 112 which is located on top of the container 96. It is noted that the extension 120 is also tapered and that the protective shield 112 is provided with a suitable draft angle for facilitating separation of the upper die 82 from container 96. It is not essential that the container 96 include a domed portion 106. As an alternative the container 96 could have the shape indicated by the dotted line 121. The container shape shown, however, obviously requires less material than the alternative and, for this reason, is more desirable. A typical procedure for compacting powder using a press includes the following steps. After the container 96 is fabricated a vacuum pump is connected to the fill tube 110 and the cavity of the container is evacuated to shrink the cavity about 10 microns. After evacuation the container is filled with powder while maintaining the cavity under vacuum. This can be accomplished by using a tee-type connection at the fill tube 110 wherein one branch of the tee is connected to the vacuum pump while the other branch is connected to a supply of powder. After filling, the fill tube 110 is closed. This may be accomplished by crimping the fill tube 110 and welding the crimped end. As described above, the protective shield 112 is then attached to the container 96 so that it surrounds the fill tube 110. The container 96 is then heated in a furnace to a temperature at which the powder will densify. The container material is selected so that at the appropriate densification temperature the container material will be capable of plastic flow when subjected to a pressure sufficient to cause densification of the powder. It has been found that for most applications, the container and powder are heated to a temperature of between 1,700"F and 2,300 F. The specific temperature is selected in view of the alloy composition of the powder being compacted. Suitable densification temperatures are well known for common alloys. Within this range of temperatures a low carbon steel container will maintain structural integrity, but is capable of plastic flow at pressures exceeding about 5,000 psi. The heated container is then transferred to a press for consolidation of the powder. A test part was made from titanium powder using a container having the configuration of container 96 by preheating to a temperature of about 1,750"F and applying a pressure of about 15,000 psi by means of a standard mechanical press outfitted with tools similar to those shown in Figure 6. After heating in the furnace for a time sufficient to obtain a uniform temperature throughout, the container was conveyed to a press fitted with dies having the configuration of the upper and lower dies 82 and 84. The press was then cycled through a single stroke. As described above, because the container is restrained by the lower die 82, the heated container material flows plastically and subjects the powder to a hydrostatic pressure which causes it to densify. Thereafter, the container 96 was ejected from the lower die 82 and cooled. The container was then removed from the densified powder compact. Consolidating the powder using a press rather than an autoclave is advantagous since cycle time at maximum temperature can be reduced significantly. The typical cycle time in an autoclave can easily exceed four hours from loading to unloading while the cycle time for a press is measured in minutes. Moreover, autoclaves which operate in the 15,000 psi range are sophisticated pieces of equipment and are quite expensive. Therefore, the use of mechanical and hydraulic presses significantly simplify the consolidation process. WHAT WE CLAIM IS:

1. A method for hot compacting powder of metallic and non-metallic composition to form a densified compact comprising encapsulating a quantity of powder in a cavity in a thick-walled container as herein defined, having walls entirely surrounding the cavity and of sufficient thickness so as not to closely follow the contour of the cavity and of a material which is substantially fully dense and incompressible and capable of plastic flow at elevated temperatures, heating the container and powder to a temperature at which the powder will densify and applying external pressure to the entire exterior surface of the container thereby

causing plastic flow of the container walls to subject the powder to a hydrostatic pressure which causes it to densify into the compact.

2. A method as claimed in Claim 1, in which the step of encapsulating the powder in the cavity includes hermetically sealing the container.

3. A method as claimed in Claim 1 or Claim 2, including cooling the container and compact and removing the compact from the container.

4. A method as claimed in any one of the preceding claims in which the step of applying external pressure to the entire exterior surface of the container includes applying gas pressure in an autoclave.

5. A method as claimed in any one of the preceding claims, in which the step of applying external pressure to the entire exterior surface of the container includes pressing the container between the dies of a press while restraining the container to cause plastic flow of the container walls.

6. A method as claimed in Claim 5, in which the powder is encapsulated in a metal container and including the step of permitting the controlled escape of container metal from between the press dies when the pressure exceeds a desired maximum to prevent damage to the press.

7. A method as claimed in Claim 5 or Claim 6, in which the powder is encapsulated in a low carbon steel container capable of plastic flow at temperatures above 1000"F and a pressure exceeding 5000 psi and including a further step of preheating the container and powder to a temperature above 1000"F and applying a pressure above 5000 psi to the entire exterior surface.

8. A method substantially as herein described with reference to the accompanying illustrative drawings.

9. A container when used in a method as claimed in any one of the preceding claims for producing a compact of a metallic and/or non-metallic composition powder, being formed of a substantially fully dense and incompressible material having such a tensile strength that plastic flow of a portion of the material is produced at the hot compacting temperature and pressure of the powder and comprising a cavity for receiving a quantity of powder. surrounded by a wall or walls of sufficient thickness that. on application of the hot compacting temperature and pressure of the powder to the container the container material becomes plastic to provide a hydrostatic pressure to be applied to the powder in the cavity.

10. A container as claimed in Claim 9.

in which the container material is gas impervious.

11. A container as claimed in Claim 9 or Claim 10. in which the container material is a metal-base material.

12. A container as claimed in any one of Claims 9 to 11, in which the container material is capable of plastic flow at temperatures exceeding 500"F without loss of structural integrity of the container.

13. A container as claimed in Claim 11 or Claim 12 when appendant to Claim 11, in which the metal-base material is a low carbon steel.

14. A container as claimed in any one of Claims 9 to 13, in which the container walls are substantially uniform in composition across a cross section from the exterior suface to the cavity.

15. A container as claimed in Claim 14, in which the container walls are substantially uniform in density.

16. A container as claimed in any one of Claims 9 to 15, including a multiple of sections, each of the sections defining a portion of the cavity.

17. A container as claimed in Claim 16, in which the cavity is of complex shape and includes a generally disc-shaped portion and a generally ring-shaped portion extending substantially laterally from the disc-shaped portion the container comprising a first section, a second section, and a third section located between the first and second sections, the first section and the third section including surfaces defining the disc-shaped portion and the second section and the third section including surfaces defining the ringshaped portion.

18. A container as claimed in Claim 17, in which the first and second sections include joinable mating surfaces.

19. A container as claimed in Claim 17, or Claim 18, in which the sections include co-operating interfitting means for locating and supporting the third section between the first and second sections.

20. A container as claimed in any one of Claims 9 to 19 including an opening communicating with the cavity for filling the cavity with powder.

21. A container as claimed in any one of Claims 9 to 20, in which the external surface of the walls of the container do not follow the contour of the cavity defining internal surface.

22. A container when used in a method as claimed in any one of Claims 1 to 9 for producing a compact of a metallic and/or non-metallic composition powder comprising a plurality of walls of non-uniform thickness having an external surface and an internal surface, the internal surface defining a cavity for receiving the powder. the walls being formed of a container material which is substantially fully dense and incompressible and is capable of plastic flow at temperatures of 500"F and above without losing structural integrity and having sufficient thickness so that said external surface does not follow the contour of the cavitydefining internal surface whereby, upon application of the compacting temperature and pressure of the powder to the container, a part of the container material becomes plastic to provide a hydrostatic pressure to the powder contained in the cavity.

23. A container as claimed in any one of Claims 9 to 22, in which the volume of the cavity is not greater than the total volume of the walls.

24. A container as claimed in Claim 10 and any one of Claims 11 to 23 when appendant to Claim 10, comprising: a plurality of walls defining a cavity within the container, at least one passageway communicating with the cavity for filling the cavity with powder, a fill tube joined to the container at the passageway for conducting a vacuum pump to the container for evacuating the cavity, and a protective shield surrounding the full tube to prevent damage to the fill tube during pressing.

25. A container when used in a method as claimed in any of Claims 1 to 9 substantially as herein described with reference to the accompanying illustrative drawings.