US3496425A - Art of forming powder compacts of uniform interconnected porosity - Google Patents
Art of forming powder compacts of uniform interconnected porosity Download PDFInfo
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- US3496425A US3496425A US707813A US3496425DA US3496425A US 3496425 A US3496425 A US 3496425A US 707813 A US707813 A US 707813A US 3496425D A US3496425D A US 3496425DA US 3496425 A US3496425 A US 3496425A
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- 239000000843 powder Substances 0.000 title description 52
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 29
- 239000002245 particle Substances 0.000 description 27
- 239000003990 capacitor Substances 0.000 description 23
- 239000013536 elastomeric material Substances 0.000 description 23
- 229910052715 tantalum Inorganic materials 0.000 description 17
- 239000000463 material Substances 0.000 description 16
- 239000011148 porous material Substances 0.000 description 16
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 11
- 229910052721 tungsten Inorganic materials 0.000 description 9
- 239000010937 tungsten Substances 0.000 description 9
- 238000000576 coating method Methods 0.000 description 8
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 229910052792 caesium Inorganic materials 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 229910000833 kovar Inorganic materials 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 238000007743 anodising Methods 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 229920001875 Ebonite Polymers 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000010407 anodic oxide Substances 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000005056 compaction Methods 0.000 description 2
- 230000009977 dual effect Effects 0.000 description 2
- 239000013013 elastic material Substances 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 239000000806 elastomer Substances 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 210000004907 gland Anatomy 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000002048 anodisation reaction Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000010006 flight Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 239000007779 soft material Substances 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Images
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G9/052—Sintered electrodes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
- B22F3/1103—Making porous workpieces or articles with particular physical characteristics
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/1208—Containers or coating used therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
Definitions
- Powder compacting apparatus includes an enclosure made of two parts of elastomeric material. One internal part contains the powder and is made of relatively soft, flowa'ble, clastomeric material. The other part is external to the first part and is made of relatively hard, elastomeric material. The enclosure fits in a die cavity, with the hard elastomeric part placed to form a seal between the soft elastomeric part and the interface or open junction between walls of the die cavity.
- Pressing force applied to the die is transmitted to all sides of the enclosure to exert pressure isostatically on the powder, with the hard elastomeric part pressed against the wall interface of the die cavity to prevent extrusion of the soft elastomeric part from the die cavity.
- This invention relates to the art of forming powder into shaped articles, and particularly to the art of forming powder compacts of uniform interconnected porosity.
- porous powder compacts of uniform interconnected porosity.
- Such powder compacts find use in porous tungsten ionizers, tantalum capacitors, fuel cell electrodes, precision filters, heat pipe liquid transfer bodies, controlled surface area members, flow control devices, liquid gas separation devices, and precision diffusers, to mention a few examples.
- a contact-type ion engine One type of ion engine currently being developed for long-term space flights is known as a contact-type ion engine.
- a stream of cesium vapor atoms is passed through a heated porous tungsten member which serves as an ionizer.
- the cesium vapor particles lose an electron and emerge as ions.
- the ions are then subjected to accelerating electric fields to produce a desired thrust.
- a number of the cesium vapor atoms pass through the tungsten member as neutral atoms, thereby degrading the efficiency of the porous ionizer. Since the fractional part of neutral cesium atoms is dependent upon the flow rate or current density of the total cesium flow,
- uniformity in the interconnected porous structure is a critical factor in promoting high ion yield.
- uniform interconnected porosity is meant that the many paths connecting the pores of the ionizer are of minimum and uniform width and spacing.
- the conventional methods of fabricating the tungsten ionizer involve pressing tungsten powder in a complex and expensive steel die, using long dwell times and relative high compacting pressures.
- the results obtained from such methods usually fail to produce compacts that meet the requirements for ion emitters, for a number of reasons.
- the use of a steel die results in a significant wall friction which prevents the compacting pressure from being applied uniformly across the structure, thereby causing variations in the density of the compact as well as nonuniformity of the interconnected porosity.
- the use of long dwell times at high pressure within the steel die results in deformation of the tungsten at the surface of the compact and destroys the interconnected porous structure.
- the lack of interconnected porosity produces nonuniformity of the permeable porosity.
- the construction of a capacitor having a porous, sintered tantalum anode is essentially the following. Tantalum powder is pressed into a dense but porous compact and sintered to produce one electrode, called the anode.
- the surface area of this consists of all the surfaces of the powder particles that are interconnected through the pores of the compact.
- the anode is anodized to form an oxide film on the porous tantalum, without filling the pores.
- the oxide film serves as the dielectric and its thickness is directly proportional to the forming voltage or voltage applied during the anodization process.
- the pores are then filled with conductive material which serves as the other electrode and is called the counterelectrode.
- any pores that are isolated from, and not connected with, the remaining pores of the sintered anode are not reached either by the dielectric film or by the counterelectrode material. These isolated pores are completely inefiectual in the capacitor.
- the more interconnected pores there are the greater the capacitance that can be obtained, since the capacitance value is directly proportional to the electrode surface area, which in turn is determined by the interconnected pore area.
- V was an abbreviation for voltage. More precisely, the V refers to the formation voltage applied during the anodizing process. The higher the formation voltage V, the thicker the dielectric film, and, thus, the higher the breakdown voltage. Conversely, the thicker the dielectric film, the lower the capacitance C. This results from the well-known relationships that the capacitance is inversely proportional to the electrode spacing, the breakdown voltage is directl proportional to the electrode spacing, and the thickness of the dielectric film determines the electrode spacing.
- a primary object of this invention is to produce powder compacts of uniform and greater interconnected porosity.
- a further object of this invention is to provide means by which substantially isostatic pressure will be applied to a powder during its formation into a compact.
- the hard elastomeric part In the die cavity, the hard elastomeric part is in such a position at to provide a seal between the soft elastomeric part and the crevices in the die, such as the junction that is located between a die wall and a die punch. Due to its fiowability, the inner, relatively soft, elastomeric material transmits substantially isostatic pressure to the powder. The outer relatively hard elastomeric material prevents the soft material from extruding out of the die, and thereby allows the pressure equilibrium on the compact to be maintained.
- FIGURE 1 is a perspective 'view, partly in section and with portions removed, of one form of apparatus for fabricating powder compacts in accordance with the invention
- FIGURE 2 is a sectional view of the apparatus of FIG URE 1;
- FIGURE 3 is an exploded view showing one .means of assembling dual elastic containers for a powder compact in accordance with the invention
- FIGURES 4 and 5 are sectional views showing alternative'forms of apparatus according to the invention.
- FIGURE 6 is a sectional view of apparatus for forming tantalum anodes for use in slug capacitors
- FIGURE 7 is a greatly enlarged, fragmentary, sectional view showing some of the component parts of a tantalum slug capacitor
- FIGURE 8 is a sectional view of a complete tantalum slug capacitor.
- FIGURE 9 is a greatly enlarged sectional view of an elemental capacitor associated with a single tantalum powder particle.
- FIGURE 1 there is shown a cylindrical die member 10 provided with a longitudinal cylindrical bore 12. Within the cylindrical bore 12 and extending along the length thereof are a pair of oppositely disposed die shoes 14 and 16. The die shoes 14 and 16 are curved on their outer surfaces to mate with the inner surface of the cylindrical bore 12. The die shoes 14 and 16 have inner surfaces 18 and 20 which are flat, and are arranged so that the flat surfaces 18 and 20 are parallel to each other. Thus, there is formed within the die member 10 a die cavity 22, which is bounded by the flat surfaces 18 and 20 of the die shoes 14 and 16, respectively, and by the exposed inner surface portions of the cylindrical bore 12.
- a bottom punch 24 Fitted within the die cavity 22 is a bottom punch 24. Shown above the die cavity 22 is a top punch 26, which is similar to the bottom punch 24. In operation, the top punch 26 may be lowered into the die cavity 22 to compress an assembly nested between the punches 24 and 26 and containing a compactable powder, as will be explained.
- the die member 12, the die shoes 14 and 16, and the two punches 24 and 26 are all mad of hard, nondeformable material such as steel. While the die cavity 22 is shown as having a generally rectangular configuration, it should be understood that other configurations may be used to suit manufacturing needs.
- .means are provided for enclosing a compactable powder within an assembly forming dual elastic containers.
- a compactable powder 28, made of metal or non-metal, is enclosed within a first container 30 made of relatively soft, fiowable, elastomeric material.
- the first container 30 is snugly enclosed within a second container 32 made of relatively hard, nonflowable, elastomeric material, with the second container shaped to fit rather loosely within the walls of the die cavity 22.
- the interior of the first container 30 is shaped to conform to the configuration desired of the final powder compact, which in this example is illustrated as being a thin, fiat, rectangular plate.
- the horizontal surfaces of the two elastomeric containers 30 and 32 are parallel to the horizontal hearing surfaces of the two punches 24 and 26.
- the top punch 26 is lowered into the die cavity 22, as shown in FIGURE 2, and suitable force is applied to the two punches 24 and 26 to compress the assembly comprising the two containers 30 and 32 and powder 28.
- the compressing force is transmitted through the second container 32 to the first container 30.
- the first container 30 acts like a liquid under pressure, and absorbs any pressure gradients exerted upon it by the second container 32. Consequently, the first container 30 distributes the pressure uniformly over all surfaces of the powder 28.
- the first container 30 can be said to exert pressure substantially isostatically over the powder 28.
- the pressure is uniformly distributed over the powder 28, there is less tendency of the pores between the powder particles to close during compaction. As a result, the powder particles can be compacted to a higher density, corresponding to the most efficient packing of spherical particles, while still retaining the desired uniform interconnected porosity.
- the second container 32 confines the softer, more fiowable material of the first container 30 so that neither the powder 28 nor the material of the first container 30 are extruded from the die cavity 22.
- the second container 32 forms a seal at the crevices or junctions 33 and 35 between the side walls of the die cavity 22 and the vertical surfaces of the die punches 24 and 26, respectively.
- extrusion of powder material along the walls of the die cavity has resulted in scoring of the walls of the steel die. Such an occurrence is practically eliminated by the isolation afforded by the second container 32.
- the hardness or toughness of the material of the second container 32 prevents the material of the second container 32 from extruding from the walls of the die cavity 22 under the high pressure required for compacting the powder 28.
- both containers 30 and 32 Due to the elasticity of the materials of both containers 30 and 32, they return to their original size when the compacting pressure is relieved, thereby releasing the powder compact. This prevents any mechanical damage of the powder compact during its removal from the die cavity 22.
- FIGURE 3 is an exploded view of one means by which the powder 28 can be assembled within the containers 30 and 32.
- the container assembly shown consists of five flat layers of elastic material, all of which conform to the contours of the walls of the die cavity 22.
- the first layer 34 which is placed upon the bottom punch 24, is a solid layer of the hard elastomeric material.
- the second layer 36, which is placed upon the first layer 34, is formed of a rim 38 of a hard elastomeric material which surrounds a rectangular insert 40 made of the soft elastomeric material.
- the third layer 42 which is placed upon the second layer 36, consists of a rim 44 of a hard elastomeric material provided with a liner 46 of the soft elastomeric material.
- the space within the liner 46 forms a cavity which will be filled with the powder 28.
- the fourth layer 48 is identical to the second layer 36 and is placed upon the third layer 42, thereby enclosing the powder 28 within a container of soft elastomeric material.
- the fifth layer 50 is identical to the first layer 34 and is placed upon the fourth layer 48 to enclose the first container within a second container of hard elastomeric material.
- spherical powder particles provide the most uniform porous structure combined with the optimum density both of solid material and of interconnected porosity.
- tungsten compacts have been successfully made and operated, using tungsten spheroids falling within two size ranges. In the smaller size range the tungsten particles ranged in diameter from 2 to 5 microns, While in a larger size range they'.ranged in diameter from 7 to 9 microns.
- One material that has been successfully used for the soft elastomeric material is a silicone rubber having a Shore A hardness less than about 40. This material is known in the trade as Dow Corning DC-6510.
- An example of a-material that has been successfully used for the hard elastomeric material is a polyurethane elastic material known in the trade as American Latex Daycollan 80. This material has a Shore A hardness of about 80. It is apparent that other suitable materials may be used for both the soft and hard elastomeric materials.
- the hard elastomeric material has been shown as a container 32 completely enclosing the inner container 30, it will be understood that such construction may be generally used to seal in the soft elastomeric material no matter where the crevices are located in the die cavity walls. However, it may be preferred to utilize a more simplified construction by employing a simple insert or a thin slab of the hard elastomeric material at the locations where such wall crevices or junctions occur.
- FIGURE 4 shows an alternative arrangement in which a slab 52 of hard elastomeric material is placed between a top die punch 26 and the soft elastomeric container 30 that is placed in a die 54 where side wall 56 and base 58 are formed of a single piece of metal.
- the slab 52 forms a seal between the top die punch and the internal surface of the wall 56.
- a slab 60 placed between the top die punch 26 and the soft elastomeric container 30 has an inner portion 62 of soft elastomeric material and a rim 64 of hard elastomeric material.
- the rim 64 provides a seal between the top die punch and the internal surface of the die wall 56 in much the same fashion as the slab 52 of FIGURE 4 and container 32 of FIG- URES 1-3.
- FIGURE 6 illustrates apparatus for fabricating porous tantalum anodes for use in tantalum slug capacitors.
- An elastomericenclosure 66 is disposed in a die cavity between die shoes 14 and 16 and die punches 24 and 26.
- the elastomeric enclosure 66 includes a bottom slab 68 of soft elastomer having a number of cavities 70 formed in its upper surface for containing tantalum powder 72.
- An insert 74 of hard elastomer rims the outer periphery of the lower side of the slab 68.
- On top of the bottom slab 68 is placed a top slab 76 of soft elastomer, the upper side of which is rimmed with an insert 78 of hard elastomer.
- a tantalum wire 80 is inserted in each mass of powder 72, with the wires 80 6 held vertically in place in long, narrow holes '81 in the top slab 76.
- the enclosure 66 When the enclosure 66 is compressed, the powder masses are squeezed into compacts having the wires embedded therein. When the pressure is released from the die, the two slabs 68 and 76 can be separated and the powder compacts may be lifted out of the cavities 70 by the wires 80.
- Tantalum powder particles having an average size of 4 microns have been compacted at pressure of 2,000 to 8,000 pounds per square inch sustained for approximately 15 seconds to form compacts of about 50% density; that is, 50% powder volume and 50% pore volume. These compacts have been formed without the use of binders or lubricants.
- the powder compacts are then sintered in vacuum for approximately 10 to 30 minutes at temperatures from about 1,600 to 2,000 degrees centigrade to achieve the required densification.
- the sintered powder'compact will hereinafter be referred to as the anode.
- the sintered anode is first anodized in a water solution of phosphoric acid to produce a film of tantalum pentoxide, which is the dielectric film.
- the dielectric film 82 covers the exposed surfaces of the tantalum powder 72 and the embedded portion of the tantalum wire 80.
- the dielectric film 82 forms at a thick- 'ness of about 15 angstroms per volt of anodizing or formation voltage.
- the anode After anodizing, the anode is dipped in a solution of manganese nitrate to fill the pore space. The anode is then baked to decompose the manganese nitrate and produce a conductive film of manganese dioxide over the dielectric film 82. The process of dipping and baking is repeated several times until the entire pore space is filled with the conductive film 84 of manganese dioxide. The internal pore fillings of manganese dioxide are interconnected with the surface coatings of manganese dioxide to seal the dielectric film 82.
- the external surface of the conductive film 84 is next coated with a graphite solution, known in the trade as Aquadag, to form a graphite conductive coating 86.
- the graphite coating 86 not penetrate the already filled pore space.
- the assembly is next dipped in a silver solution to coat the graphite with silver coating 87.
- the assembly is placed in a metal can 88 that has been pretinned on the inside, and the space between the can 88 and the silver is filled with solder 90.
- a cathode lead 92 is secured to the can 88 by welding.
- the remaining constructional elements consist of an insulating washer 94 for centering the tantalum wire 80; an anode lead 96 butt welded to the tantalum wire; a Kovar gland 98 soldered to the anode lead 96; a glass bead 100 sealed to the Kovar gland 98; and a Kovar ring 102 sealed to the glass bead 100 and soldered to the can 88.
- Kovar is the trade name for a metal having a composition of 54% iron, 28% nickel, and 18% cobalt.
- FIGURE 9 A highly magnified section of one of the elemental capacitors associated with a single tantalum powder particle is shown schematically in FIGURE 9.
- the elemental capacitor is essentially comprised of a powder particle 72, the dielectric coating 82 and the conductive coating 84.
- the total capacitance is the sum of all the elemental capacitors connected in parallel.
- Tantalum anodes have been made with the apparatus of the invention which has a sintered density of about 50% to 80% and an interconnected porosity of over By 90% interconnected porosity is meant that over 90% of the total pore volume is fully interconnected.
- capacitors have been fabricated which have CVs of above 6,000 microfarad-volts per gram as compared with CVs of 2,000 to 2,200 microfarad-volts per gram for conventional tantalum capacitors.
- CVs of about 2,500 have been obtained as compared with CVs of 1,500 in conventional tantalum capacitors.
- An anode for an electrical capacitor comprising:
- said particles having an average diameter within an order of magnitude of 8 microns
- An electrical capacitor having an anode with a dielectric film on the surface thereof and a cathode overlying the dielectric film;
- said anode comprising a unitary porous mass of filmforming metal particles sintered together in spaced areas on their surface forming a body having cavities and holes therein;
- said particles having an average diameter within an order of magnitude of 8 microns
- said dielectric member is an anodic oxide coating on said powder particles, and said capacitor has a capacitnce and voltage product above 6,000 microfarad-volts per gram of said mass of powder particles.
- sai particles consist of tantalum having an average diameter of about 8 microns.
- said dielectric member is an anodic oxide coating on said powder particles
- said capacitor has a capacitance and voltage product above 2,500 microfarad-volts per gram of said mass of powder particles.
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
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Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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US70781368A | 1968-02-23 | 1968-02-23 |
Publications (1)
Publication Number | Publication Date |
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US3496425A true US3496425A (en) | 1970-02-17 |
Family
ID=24843258
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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US707813A Expired - Lifetime US3496425A (en) | 1968-02-23 | 1968-02-23 | Art of forming powder compacts of uniform interconnected porosity |
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Country | Link |
---|---|
US (1) | US3496425A (enrdf_load_stackoverflow) |
DE (1) | DE1906255B1 (enrdf_load_stackoverflow) |
FR (1) | FR2002433A1 (enrdf_load_stackoverflow) |
GB (1) | GB1266013A (enrdf_load_stackoverflow) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4059442A (en) * | 1976-08-09 | 1977-11-22 | Sprague Electric Company | Method for making a porous tantalum pellet |
US4126451A (en) * | 1977-03-30 | 1978-11-21 | Airco, Inc. | Manufacture of plates by powder-metallurgy |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS50106844A (enrdf_load_stackoverflow) * | 1974-01-31 | 1975-08-22 | ||
CA1222152A (en) * | 1982-09-20 | 1987-05-26 | Walter J. Rozmus | Method and assembly for hot consolidating materials |
IL164017A0 (en) * | 2004-09-09 | 2005-12-18 | Cerel Ceramic Technologies Ltd | Solid electrolyte capacitor with controlled properties and method for manufacturing the same |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2299228A (en) * | 1938-01-12 | 1942-10-20 | Radio Patents Corp | Electric condenser |
US2406345A (en) * | 1942-04-15 | 1946-08-27 | Joseph B Brennan | Electrode and method of making same |
US3004332A (en) * | 1958-09-02 | 1961-10-17 | Bell Telephone Labor Inc | Powder metallurgy process |
US3166693A (en) * | 1965-01-19 | Form an oxide | ||
US3302073A (en) * | 1963-10-21 | 1967-01-31 | Gen Electric | Electrical capacitors and electrode material therefor |
US3330999A (en) * | 1964-01-31 | 1967-07-11 | Int Standard Electric Corp | Electrolytic capacitor with dielectric film formed on ceramic material |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE693504C (de) * | 1935-06-27 | 1940-07-11 | Gen Motors Corp | Vorrichtung zum Formen keramischer Koerper, bei der fein gepulverter keramischer Stoff in die Hoehlung eines Formblockes eingefuellt wird |
-
1968
- 1968-02-23 US US707813A patent/US3496425A/en not_active Expired - Lifetime
-
1969
- 1969-01-24 FR FR6901444A patent/FR2002433A1/fr not_active Withdrawn
- 1969-02-07 DE DE19691906255 patent/DE1906255B1/de active Pending
- 1969-02-24 GB GB1266013D patent/GB1266013A/en not_active Expired
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3166693A (en) * | 1965-01-19 | Form an oxide | ||
US2299228A (en) * | 1938-01-12 | 1942-10-20 | Radio Patents Corp | Electric condenser |
US2406345A (en) * | 1942-04-15 | 1946-08-27 | Joseph B Brennan | Electrode and method of making same |
US3004332A (en) * | 1958-09-02 | 1961-10-17 | Bell Telephone Labor Inc | Powder metallurgy process |
US3302073A (en) * | 1963-10-21 | 1967-01-31 | Gen Electric | Electrical capacitors and electrode material therefor |
US3330999A (en) * | 1964-01-31 | 1967-07-11 | Int Standard Electric Corp | Electrolytic capacitor with dielectric film formed on ceramic material |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4059442A (en) * | 1976-08-09 | 1977-11-22 | Sprague Electric Company | Method for making a porous tantalum pellet |
US4126451A (en) * | 1977-03-30 | 1978-11-21 | Airco, Inc. | Manufacture of plates by powder-metallurgy |
Also Published As
Publication number | Publication date |
---|---|
DE1906255B1 (de) | 1971-06-24 |
FR2002433A1 (enrdf_load_stackoverflow) | 1969-10-17 |
GB1266013A (enrdf_load_stackoverflow) | 1972-03-08 |
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