CA1326132C - Pump liners and a method of cladding the same - Google Patents
Pump liners and a method of cladding the sameInfo
- Publication number
- CA1326132C CA1326132C CA000556982A CA556982A CA1326132C CA 1326132 C CA1326132 C CA 1326132C CA 000556982 A CA000556982 A CA 000556982A CA 556982 A CA556982 A CA 556982A CA 1326132 C CA1326132 C CA 1326132C
- Authority
- CA
- Canada
- Prior art keywords
- chamber
- layer
- grain
- metal
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- 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
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
- B22F7/08—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools with one or more parts not made from powder
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/067—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder
Abstract
PUMP LINERS AND A METHOD OF CLADDING THE SAME
ABSTRACT OF THE DISCLOSURE
A method of cladding an internal cavity surface of a metal object is disclosed. The method includes the steps:
a) applying a powder metal layer on said internal surface, the metal powder including metal oxide or oxides, borides and carbides, b) filling a pressure transmitting and flowable grain into said cavity to contact said layer, c) and pressurizing said grain to cause sufficient pressure transmission to the powder metal layer to consolidate same.
ABSTRACT OF THE DISCLOSURE
A method of cladding an internal cavity surface of a metal object is disclosed. The method includes the steps:
a) applying a powder metal layer on said internal surface, the metal powder including metal oxide or oxides, borides and carbides, b) filling a pressure transmitting and flowable grain into said cavity to contact said layer, c) and pressurizing said grain to cause sufficient pressure transmission to the powder metal layer to consolidate same.
Description
132613~
BACKGROUND OF THE INVENTION
This invention relates generally to cladding or coating cavities of metal ob; ects, and more particularly to mud pump liner cavities.
Internal cavities of metal objects frequently require a cladding, or a coating, that is more corrosion, oxidation and/or wear resistant than the metal object itself. This need may arise in some cases due to high temperatures created within the cavity, exposure to a corrosive or abrasive liquid, and/or to rubbing action of an internal machine member such as a - piston. An example of such a metal object is the liners in mud pu~ps used in oil field drilling. A mud pump is a part of the oil or gas well drilling fluid - 15 circulating system, one of five major components of a rotary drilling operation. The other components are the drill string and bit, the hoisting system, the power plant and the blowout prevention system.
Drilling fluid, usually called the "mud", in most cases consists of a mixture of water, various special chQmicals including corrosion inhibitors and solid particles to increase its density. Such fluid is continuously circulated down the inside of the drill ; pipe, through the bottom of the bit and back up the annular space between the drill pipe and the hole. The driving force is provided by a mud pump.
A mud pump liner is basically a heavy wall pipe section with one or two retaining rings at its outer diamQter. It is the wear resistance of the inner surface that determines the liner service life.
Consequently, the internal surface of - ~ . - ,. :
the liner is desirably clad with a wear resistant material.
The internal cladding layer is subjected to sli~ing wear by the rubber piston which can wear and cause metallic structure supporting the rubber to contact the liner cladding, thus accelerating the wear process. The cladding material is also subjected to corrosion from the drilling fluid, and metal fatigue caused by cyclic loading, especially at areas where the direction of the piston motion suddenly chanses, Further, micro regions of cladding may experience sudden pressurization and depressurization. These operating conditions impose stringent metallurgical reqùirements on the cladding materials.
An ideal cladding material should, therefore, possess high hardness and high resistance to corrosion, impact and metal fatiuge. Such properties are desirably achieved by a uniform, fine grained microstructure, which has been the goal of pump liner makers o~ many years.
The outer, heavy wall portions of the commercially available mud pump liners typically consist of either a carbon steel, or a low alloy steel; and the liner cladding is, in most cases, a cast sleeve of iron - 28~ chromium alloy.
The sleeve càn be centrifugally cast into the steel pipe section or cast separately as a pipe, ànd shrink fitted into the outer pipe section, then machined to a smooth finish.
These manufacturing procedures are lengthy and costly, while 2; providing only a cast metal microstructure which is known to be chemically nonuniform, since in castings the solidification process results in natural segregation of the elemental species contained in the alloy. Furthermore, the cladding thicknesses are kept undesirably large to allow casting processes to be used.
The claddings within metallic objects other than pump liners ~ 3261 32 can be similarly characterized and most likely be prone to the same deficiencies.
A cladding layer made of powder metals consolidated to near 100% density and bonded to the outer steel shell appears to provide the most desirable metallurgical microstructure, due to its chemical uniformity and high ductility emanating from its fine grain size. ~xisting methods of application of such powder metal layers, however, are grossly inadequate in that they either produce a porous, oxide contaminated layer which is only mechanically bonded to the outer shell as in sprayed coatings, or they are superficially and only mechanically bonded to the outer shell as in brazed-on coatings. For these, and other reasons, present powder metallurgy techiniques for such products have not been considered adequate.
SU~MARY OF THE INV~NTlON
` It is a major object of the invention to pro~ide a powder metal cladding method and apparatus for cladding the internal cavity surface of metal liners and objects, overcoming the above problem and deficiencies. In addition, the invention provides various material combinations for thè production of pump liners and internally clad pipe segments for use with oilfield mud pump fluids. There are many other products that can benefit from this processing technique.
Basically, the method of the invention concerns - 25 cladding of an internal cavity surface of a metal object, and includes the steps:
` a) applying a powder metal layer on said internal surface, the metal powder including metaloxides, borides and carbides, :
b) filling a pressur~ ting and flowable grain into said cavity to contact said layer, c) and pressurizing said grain to cause sufficient pressure transmission to the powder metal layer to consolidate same.
As will appear, pressurization of the grain is typically carried out by transmitting force to the grain along a primary axis, the layer extending about that axis and spaced therefrom, whereby force is transmitted by the grain away from the axis and against said layer. To this end, the method contemplates providing a die having a first c~amber receiving said object, the die having~a second chamber containing grain communi~ating with grain in the cavity, pressurizing of the grain in the cavity being carried out by pressurizing the grain in the second chamber, as for example by transmitting pressure from the grain in the second chamber to only a medial portion of the grain in the first chamber everywhere spaced from said layer. Further, the metal object is typically -` cylindrical, the layer being applied on an internal cylindrical surface of said object, the latter for example comprising a mud pump liner.
Apparatus for cladding an internal cavity surface of a metal object involves use of a cladding consisting essentially of a powder metal layer on said internal surface, the metal powder including metal oxide or oxides, borides and bides, the apparatus comprisin~
a) a pressure transmitting and flowable grain filled into said cavity to contact said layer, and - ` t 326 1 32 b) means for pressurizing said grain to cause sufficient pressure transmission to the powder metal layer to consolidate same, said means transmitting force to the grain along a primary axis, said layer extending about said axis and spaced therefrom, whereby force is transmitted by the grain away from said axis and against said layer.
According to one aspect, the invention relates to an apparatus for cladding an internal cavity surface of a metal object, the cladding consisting essentially o$ a powder metal layer on said internal surface, the metal powder including metal oxide or oxides, borides and carbides, said apparatus comprising (a~ a pressure transmitting and flowable grain filled into said cavity to contact said layer, (b) means for pressurising said grain to cause sufficient pressure transmission to the powder metal layer to consolidate same, said means transmitting force to the grain along a primary axis, said layer extending about said axis and spaced therefrom, whereby force is transmitted by the grain away from said axis and against said layer, (c) and including a step die having a first chamber receiving said object, the die having a second chamber containing said grain communicating with said grain in the cavity which is in the first chamber, said pressurizing of the grain in the cavity being effected by grain pressurized in the second chamber, (d) and wherein the second chamber is in axial alignment with the first chamber, the second chamber having a cross section less than the cross section of the first chamber, and said powder metal layer to be pressurized being everywhere outside the projection into said cavity of a throat defined by the second chamber, whereby : 30 pressure is transmitted from the grain in the second chamber which is everywhere spaced from said layer, (e) the first chamber filled by the grain, radially inwardly of said layer.
. -6-' A
` 1326132 ~ hese and other objects and advantages of the invention, as well as the details of an illustrative embodiment, will be more fully understood from the following specification and drawings, in which:
DRAWING DESCRIPTION
Fig. 1 is a vertical section showing a mud pump liner;
Fig. 2 is a vertical section showing a "green"
coated mud pump liner placed in a double chamber die;
Fig. 3 is similar to Fig. 2, but shows hot grain filled into the die and liner cavity, and~pressurized,.and Figs~ 4-6 are magnified section taken throùgh the ~ walls of steel tubes clad in accordance with the invention.
:
DETAILED DES~RIPTION
Referring first to Fig. 1, and alloy steel mud pump liner 10 comprises an elongated tube`ll having an outer flange 12 on one end portion. The tube axis appears at 13, and the tube inner cylindrical sùrface at 14. Tube 11 may be considered to represent other metal objects ha~ing interior surfaces (as at 14) facing internal cavities 15.
-6a-..
.~
~; A
,:
` t326132 Internal surfaces of the tube or metal object to - be clad are first cleaned to remove any oxide layers, grease or dirt; then, using a slurry of the cladding metal powder and a suitable fugitive binder, these surfaces are coated with the slurry, the coating appearing at 16. As shown, the "green" coating is generally cylindrical, and has an outer surface 16a contacting the tube surface 14. The coating process can be accomplishedby spraying, dipping in the slurry, brush, or spatula painting, or if the internal cavity is cylindrical, as is the ~ase for pipes, the slurry may be centrifugally spread onto the internal surface by high speed spinnlng of the part.
The thickness of the "green'`, weakly held together, powder metal-binder mixture can be controlled to some degree by controlling the total weight of the slurry used. Localized surfaces where cladding is not desired can be masked using adhesive tapes ~see tape 17) which are removed after slurry coating is applied.
The green coating is then dried at or near room temperature and heated to a temperature (between 1600 F and 2300 F) where the coated metal powders are easily deformable under , .
pressure. For ~ost`materials the furnace atmosphere should be either inert or reducing to prevent oxidation of the powder.
Such a furnace is indicated at 18, and it may contain inert gas such as argon or nitrogen.
Referring to Figure 2, the next step in the process is to place the liner containing the green now lightly sintered layer lla within a step die 19 where the liner fits into the large cavity (i.e.
first chamberl9)in the die as shown in the figure, and having , .
...:
- inner cylindrical walls l9a and l9b. The die second chamber 20 throat diameter Dl should be equal to or smaller than the "green" internal diameter D2 f the mud pump liner lla. This .
~ 1326132 assures relatively shearless pressing of the gre2~ ~owder metal cladding lla under largely lateral pressure durin~ the pressurizing step. Chamber 20 has a bore 20a.
As seen in Fig. 3, pressurization takes place in a press 21 after filling both the die and the pump liner cavities with a refractory powder 22 already at a temperature near or above the consolidation temperature of the clad~ing powder.
.~pressure from ram 23 is transmitted to the liner by the horizontal forces created within the refractory ?owder grain~.
In this regard, the second chamber 20 is in axial alignment with the first chamber 19, the seco~d chamber having a cross section less than the cross section o~ the first chamber, whereby pressure is transmitted from the grain 22a in the second chamber to only a medial portion of the gra~n 22b in the first chamber which is everywhere spaced from layer lla.
Therefore, lateral pressurizing of the grain in the cavity 19 is affected by grain pressurized longitudinally in the second chamber, and no destructive shear is transmitted to layer lla.
Consolidation o~ powder metal into substantially solid objects throug~ the use of refractory particles ~rain) has been disclosed in previous U.S. patents No. 3,356,496 and No. 3,689,259 by R.W. Hailey. This invention, therefore, can be regarded as an improvement over those of the two patents, the invention providing a novel die design and a unique provision for horizontal pressurization transformed from a vertically applied load. The critical factor which prevents the powder cladding layer from being stripped (due to shear forces created when a vertically applied force is directly -; 30 transmitted by a refractory bed of grain) is the die shape .
;.
., .
which moves the "shear" region away from the cladding.
EXAMPLES
A number of experiments using steel tube segments measuring 1.5 inches long having 2 or 3,25 inches O.D.'s `~ 5 and 0.25 inch wall thicXness were conducted to establish and verify the above described process. The objective was to - clad the tubes with several selected wear powder metal alloys without distoring the tubes in any way. This was accomplished utilizing the die configuration shown in Figures 2 and 3.
In one example the cladding material consisted of Stellite alloy (98.5% by wt.) No. 1 powder (see item 2, below Table 1 for chemistry~ mixed with 1.5% by weight cellulose acetate and acetone in an amount to establish sufficient fluidity to the mixture. This mixture was spun at 500 rpm to provide a thin (approxi~ately l/lOth of an inch) green coating inside a 1.5" long X 3.25" O.D. X 0.25" wall tube.
The tubing was allowed to dry at room temperature overnight and heated to 2250F for about 14 minutes. The furnace atmosphere was substantially hydrogen. Immediately after 2C the ~tube was placed in the die cavity, the refractory grain which was heated to 2300F in a separate furnace,was poured and the press ram was allowed to pressurize the grain. After a peak pressure of 45 tons per square inch was reached for .
~ about 10 seconds, the pressurization cycle was considered `` 25 complete and pressure was released. The die was then moved `~ - to a location where its contents could be emptied. In this example the cladding of the Stellite Alloy No. 1 accomplished satisfactoril~ while the Stel~te powder was consolidated to _9_ ' ' ' ` ' 1 326~ 32 near 100% of its theoretical density. A photomi~rograph of the bonding interface is shown in Figure 4.
A second example utilized Stellite Allo~ No. 6 (item 3 in Table 1) as the cladding powder. Her~ 211 of the processing parameters of example number one abov2 were used with the exception of the type of furnace atmosp.e~e which was 100~ nitrogen instead of hydrogen. Again, (exceptinq some lateral cooling cracks in the cladding) good boncing occurred between the cladding and the steel tube, and the cladding powder consolidated satisfactorily. Tubing dimensions remained within 0.5% of initial dimensions. A typical cladding microstructure at the bonding interface appears in Fig. 5.
A third example consolidated a mixture of 40%
Deloro 60 - 60~ tungsten carbide powder (item 4 in Table 1) and bonded it to a seeel tube at a temperature of 1900F
under 45 tsi pressure. ~he same 1.5% acetate anc acetone as above was used. A typical cladding microstructure at the steel tube cladding interface is shown in Figure 6.
Other applications utilizing various cladding ` 20 materials to clad internal cavities of other metal objects such as valves, tubesj rock bits, etc. can be accomplished as well.
The process, while remaining basically the same, may have some variations. For example, there may be an insulating material positioned between the part (the pump liner in Figure 2) and the die to reduce heat loss before ; pressing.
The insulating material may be a ceramic, high density graphite or a metal which may be heated together with the part. If the insulating material is a metal, a ' ' .
, '`. ' non-bonding refractory powder parting compound may be applied on the insulating material. In addition, the die itself may be a vertically split die to ease the positioning of the part within it when the part shape is more complicated than a simple cylinder. Other minor variations of the process and the ~ie may be utilized as well.
Grains used to transmit pressure may have co~position _ dS referred to in the above tw~ patents or other o~sitions that maybeused.
Examples of wear and corrosion resistant cladding materials used in the experimental program Nominal compQsition(*)Trade Name ~ Company Cz-28.5Mtr1t.5Cr-3.4Si* Triballoy Alloy I-800 Cabot Cbrporation C~,30Cr-12.5WL2.~C* Stellite Al~loy~No. 1 Cabot a~rporation Cor28Cr-4Wo1.1C* Stellite Allcy No. 6 CakDt C~rpo~ation Ni-16Cr-4Fe-3.3B-4.2Si-0.7C* Deloro Alloy No. 60 C2bot ~w~oration DelorD Alloy Nb. 60-60% tungsten * Haystellite, O~site Cabot aD~ation c~rb;de Fowder No. 4 Fe-35Cr-12Co-10~i-5Si- C* Tristelle Alloy TS-2 Cabot O~ration 20 TS-2 - 60~ * CDP-C4 CDP, Inc.
TS-2 - 60% Cr3C2 C$P-C CDP, Inc.
Tr~loy q-800 - 60%Cr3C2 * CDP-C3 CDP, Inc.
Deloro 60 - 60~ Cr3C2 * CDP-C2 CDP, Inc.
Cu-37Mn-lONi-0.5La * Amdry 935 Alloy Metals, Inc.
Ni-19Mn-6Si-0.5B-4CU-O-03 rare earth * h~y 939 Alloy Metals, Inc.
Ni-13Cr-20Cor2.3B-4Si-4Fe* Amdry 915E Alloy Metals, Inc.
.
t*) Compositions are given in weiqht percentages, except first components, whose percentage-~ are not given, make up the remaind,er ` of the mixture;
* TRADEMARK
Preferably, the lined surface is defined by a mud pump liner having cylindrical shape, said surface at the inner side of the cylinder, the metal powder in said layer selected from the group essentially consisting of:
a) Co-Cr-W-C
b) Co-Mo-Cr-Si c) Ni-Cr-Fe-Si-B
d) Ni-Mn-Si-Cu-B
e) Ni-Co-Cr-Si-Fe-B
f ) Fe-Cr-Co-Ni-Si-C
g) Cu-Mn-Ni Further, said layer may consist essentially of a mixture of 30 to 90% by weight tungsten carbide and remaining metal alloy powder selected from the group consisting of:
a) Co-Cr-W-C
b) Ni-Cr-Fe-Si-B
c) Cu-Nn-Ni d) Ni-Co-Cr-Fe-Si-B
e) Fe-Cr-Co-Ni-Si-C --
BACKGROUND OF THE INVENTION
This invention relates generally to cladding or coating cavities of metal ob; ects, and more particularly to mud pump liner cavities.
Internal cavities of metal objects frequently require a cladding, or a coating, that is more corrosion, oxidation and/or wear resistant than the metal object itself. This need may arise in some cases due to high temperatures created within the cavity, exposure to a corrosive or abrasive liquid, and/or to rubbing action of an internal machine member such as a - piston. An example of such a metal object is the liners in mud pu~ps used in oil field drilling. A mud pump is a part of the oil or gas well drilling fluid - 15 circulating system, one of five major components of a rotary drilling operation. The other components are the drill string and bit, the hoisting system, the power plant and the blowout prevention system.
Drilling fluid, usually called the "mud", in most cases consists of a mixture of water, various special chQmicals including corrosion inhibitors and solid particles to increase its density. Such fluid is continuously circulated down the inside of the drill ; pipe, through the bottom of the bit and back up the annular space between the drill pipe and the hole. The driving force is provided by a mud pump.
A mud pump liner is basically a heavy wall pipe section with one or two retaining rings at its outer diamQter. It is the wear resistance of the inner surface that determines the liner service life.
Consequently, the internal surface of - ~ . - ,. :
the liner is desirably clad with a wear resistant material.
The internal cladding layer is subjected to sli~ing wear by the rubber piston which can wear and cause metallic structure supporting the rubber to contact the liner cladding, thus accelerating the wear process. The cladding material is also subjected to corrosion from the drilling fluid, and metal fatigue caused by cyclic loading, especially at areas where the direction of the piston motion suddenly chanses, Further, micro regions of cladding may experience sudden pressurization and depressurization. These operating conditions impose stringent metallurgical reqùirements on the cladding materials.
An ideal cladding material should, therefore, possess high hardness and high resistance to corrosion, impact and metal fatiuge. Such properties are desirably achieved by a uniform, fine grained microstructure, which has been the goal of pump liner makers o~ many years.
The outer, heavy wall portions of the commercially available mud pump liners typically consist of either a carbon steel, or a low alloy steel; and the liner cladding is, in most cases, a cast sleeve of iron - 28~ chromium alloy.
The sleeve càn be centrifugally cast into the steel pipe section or cast separately as a pipe, ànd shrink fitted into the outer pipe section, then machined to a smooth finish.
These manufacturing procedures are lengthy and costly, while 2; providing only a cast metal microstructure which is known to be chemically nonuniform, since in castings the solidification process results in natural segregation of the elemental species contained in the alloy. Furthermore, the cladding thicknesses are kept undesirably large to allow casting processes to be used.
The claddings within metallic objects other than pump liners ~ 3261 32 can be similarly characterized and most likely be prone to the same deficiencies.
A cladding layer made of powder metals consolidated to near 100% density and bonded to the outer steel shell appears to provide the most desirable metallurgical microstructure, due to its chemical uniformity and high ductility emanating from its fine grain size. ~xisting methods of application of such powder metal layers, however, are grossly inadequate in that they either produce a porous, oxide contaminated layer which is only mechanically bonded to the outer shell as in sprayed coatings, or they are superficially and only mechanically bonded to the outer shell as in brazed-on coatings. For these, and other reasons, present powder metallurgy techiniques for such products have not been considered adequate.
SU~MARY OF THE INV~NTlON
` It is a major object of the invention to pro~ide a powder metal cladding method and apparatus for cladding the internal cavity surface of metal liners and objects, overcoming the above problem and deficiencies. In addition, the invention provides various material combinations for thè production of pump liners and internally clad pipe segments for use with oilfield mud pump fluids. There are many other products that can benefit from this processing technique.
Basically, the method of the invention concerns - 25 cladding of an internal cavity surface of a metal object, and includes the steps:
` a) applying a powder metal layer on said internal surface, the metal powder including metaloxides, borides and carbides, :
b) filling a pressur~ ting and flowable grain into said cavity to contact said layer, c) and pressurizing said grain to cause sufficient pressure transmission to the powder metal layer to consolidate same.
As will appear, pressurization of the grain is typically carried out by transmitting force to the grain along a primary axis, the layer extending about that axis and spaced therefrom, whereby force is transmitted by the grain away from the axis and against said layer. To this end, the method contemplates providing a die having a first c~amber receiving said object, the die having~a second chamber containing grain communi~ating with grain in the cavity, pressurizing of the grain in the cavity being carried out by pressurizing the grain in the second chamber, as for example by transmitting pressure from the grain in the second chamber to only a medial portion of the grain in the first chamber everywhere spaced from said layer. Further, the metal object is typically -` cylindrical, the layer being applied on an internal cylindrical surface of said object, the latter for example comprising a mud pump liner.
Apparatus for cladding an internal cavity surface of a metal object involves use of a cladding consisting essentially of a powder metal layer on said internal surface, the metal powder including metal oxide or oxides, borides and bides, the apparatus comprisin~
a) a pressure transmitting and flowable grain filled into said cavity to contact said layer, and - ` t 326 1 32 b) means for pressurizing said grain to cause sufficient pressure transmission to the powder metal layer to consolidate same, said means transmitting force to the grain along a primary axis, said layer extending about said axis and spaced therefrom, whereby force is transmitted by the grain away from said axis and against said layer.
According to one aspect, the invention relates to an apparatus for cladding an internal cavity surface of a metal object, the cladding consisting essentially o$ a powder metal layer on said internal surface, the metal powder including metal oxide or oxides, borides and carbides, said apparatus comprising (a~ a pressure transmitting and flowable grain filled into said cavity to contact said layer, (b) means for pressurising said grain to cause sufficient pressure transmission to the powder metal layer to consolidate same, said means transmitting force to the grain along a primary axis, said layer extending about said axis and spaced therefrom, whereby force is transmitted by the grain away from said axis and against said layer, (c) and including a step die having a first chamber receiving said object, the die having a second chamber containing said grain communicating with said grain in the cavity which is in the first chamber, said pressurizing of the grain in the cavity being effected by grain pressurized in the second chamber, (d) and wherein the second chamber is in axial alignment with the first chamber, the second chamber having a cross section less than the cross section of the first chamber, and said powder metal layer to be pressurized being everywhere outside the projection into said cavity of a throat defined by the second chamber, whereby : 30 pressure is transmitted from the grain in the second chamber which is everywhere spaced from said layer, (e) the first chamber filled by the grain, radially inwardly of said layer.
. -6-' A
` 1326132 ~ hese and other objects and advantages of the invention, as well as the details of an illustrative embodiment, will be more fully understood from the following specification and drawings, in which:
DRAWING DESCRIPTION
Fig. 1 is a vertical section showing a mud pump liner;
Fig. 2 is a vertical section showing a "green"
coated mud pump liner placed in a double chamber die;
Fig. 3 is similar to Fig. 2, but shows hot grain filled into the die and liner cavity, and~pressurized,.and Figs~ 4-6 are magnified section taken throùgh the ~ walls of steel tubes clad in accordance with the invention.
:
DETAILED DES~RIPTION
Referring first to Fig. 1, and alloy steel mud pump liner 10 comprises an elongated tube`ll having an outer flange 12 on one end portion. The tube axis appears at 13, and the tube inner cylindrical sùrface at 14. Tube 11 may be considered to represent other metal objects ha~ing interior surfaces (as at 14) facing internal cavities 15.
-6a-..
.~
~; A
,:
` t326132 Internal surfaces of the tube or metal object to - be clad are first cleaned to remove any oxide layers, grease or dirt; then, using a slurry of the cladding metal powder and a suitable fugitive binder, these surfaces are coated with the slurry, the coating appearing at 16. As shown, the "green" coating is generally cylindrical, and has an outer surface 16a contacting the tube surface 14. The coating process can be accomplishedby spraying, dipping in the slurry, brush, or spatula painting, or if the internal cavity is cylindrical, as is the ~ase for pipes, the slurry may be centrifugally spread onto the internal surface by high speed spinnlng of the part.
The thickness of the "green'`, weakly held together, powder metal-binder mixture can be controlled to some degree by controlling the total weight of the slurry used. Localized surfaces where cladding is not desired can be masked using adhesive tapes ~see tape 17) which are removed after slurry coating is applied.
The green coating is then dried at or near room temperature and heated to a temperature (between 1600 F and 2300 F) where the coated metal powders are easily deformable under , .
pressure. For ~ost`materials the furnace atmosphere should be either inert or reducing to prevent oxidation of the powder.
Such a furnace is indicated at 18, and it may contain inert gas such as argon or nitrogen.
Referring to Figure 2, the next step in the process is to place the liner containing the green now lightly sintered layer lla within a step die 19 where the liner fits into the large cavity (i.e.
first chamberl9)in the die as shown in the figure, and having , .
...:
- inner cylindrical walls l9a and l9b. The die second chamber 20 throat diameter Dl should be equal to or smaller than the "green" internal diameter D2 f the mud pump liner lla. This .
~ 1326132 assures relatively shearless pressing of the gre2~ ~owder metal cladding lla under largely lateral pressure durin~ the pressurizing step. Chamber 20 has a bore 20a.
As seen in Fig. 3, pressurization takes place in a press 21 after filling both the die and the pump liner cavities with a refractory powder 22 already at a temperature near or above the consolidation temperature of the clad~ing powder.
.~pressure from ram 23 is transmitted to the liner by the horizontal forces created within the refractory ?owder grain~.
In this regard, the second chamber 20 is in axial alignment with the first chamber 19, the seco~d chamber having a cross section less than the cross section o~ the first chamber, whereby pressure is transmitted from the grain 22a in the second chamber to only a medial portion of the gra~n 22b in the first chamber which is everywhere spaced from layer lla.
Therefore, lateral pressurizing of the grain in the cavity 19 is affected by grain pressurized longitudinally in the second chamber, and no destructive shear is transmitted to layer lla.
Consolidation o~ powder metal into substantially solid objects throug~ the use of refractory particles ~rain) has been disclosed in previous U.S. patents No. 3,356,496 and No. 3,689,259 by R.W. Hailey. This invention, therefore, can be regarded as an improvement over those of the two patents, the invention providing a novel die design and a unique provision for horizontal pressurization transformed from a vertically applied load. The critical factor which prevents the powder cladding layer from being stripped (due to shear forces created when a vertically applied force is directly -; 30 transmitted by a refractory bed of grain) is the die shape .
;.
., .
which moves the "shear" region away from the cladding.
EXAMPLES
A number of experiments using steel tube segments measuring 1.5 inches long having 2 or 3,25 inches O.D.'s `~ 5 and 0.25 inch wall thicXness were conducted to establish and verify the above described process. The objective was to - clad the tubes with several selected wear powder metal alloys without distoring the tubes in any way. This was accomplished utilizing the die configuration shown in Figures 2 and 3.
In one example the cladding material consisted of Stellite alloy (98.5% by wt.) No. 1 powder (see item 2, below Table 1 for chemistry~ mixed with 1.5% by weight cellulose acetate and acetone in an amount to establish sufficient fluidity to the mixture. This mixture was spun at 500 rpm to provide a thin (approxi~ately l/lOth of an inch) green coating inside a 1.5" long X 3.25" O.D. X 0.25" wall tube.
The tubing was allowed to dry at room temperature overnight and heated to 2250F for about 14 minutes. The furnace atmosphere was substantially hydrogen. Immediately after 2C the ~tube was placed in the die cavity, the refractory grain which was heated to 2300F in a separate furnace,was poured and the press ram was allowed to pressurize the grain. After a peak pressure of 45 tons per square inch was reached for .
~ about 10 seconds, the pressurization cycle was considered `` 25 complete and pressure was released. The die was then moved `~ - to a location where its contents could be emptied. In this example the cladding of the Stellite Alloy No. 1 accomplished satisfactoril~ while the Stel~te powder was consolidated to _9_ ' ' ' ` ' 1 326~ 32 near 100% of its theoretical density. A photomi~rograph of the bonding interface is shown in Figure 4.
A second example utilized Stellite Allo~ No. 6 (item 3 in Table 1) as the cladding powder. Her~ 211 of the processing parameters of example number one abov2 were used with the exception of the type of furnace atmosp.e~e which was 100~ nitrogen instead of hydrogen. Again, (exceptinq some lateral cooling cracks in the cladding) good boncing occurred between the cladding and the steel tube, and the cladding powder consolidated satisfactorily. Tubing dimensions remained within 0.5% of initial dimensions. A typical cladding microstructure at the bonding interface appears in Fig. 5.
A third example consolidated a mixture of 40%
Deloro 60 - 60~ tungsten carbide powder (item 4 in Table 1) and bonded it to a seeel tube at a temperature of 1900F
under 45 tsi pressure. ~he same 1.5% acetate anc acetone as above was used. A typical cladding microstructure at the steel tube cladding interface is shown in Figure 6.
Other applications utilizing various cladding ` 20 materials to clad internal cavities of other metal objects such as valves, tubesj rock bits, etc. can be accomplished as well.
The process, while remaining basically the same, may have some variations. For example, there may be an insulating material positioned between the part (the pump liner in Figure 2) and the die to reduce heat loss before ; pressing.
The insulating material may be a ceramic, high density graphite or a metal which may be heated together with the part. If the insulating material is a metal, a ' ' .
, '`. ' non-bonding refractory powder parting compound may be applied on the insulating material. In addition, the die itself may be a vertically split die to ease the positioning of the part within it when the part shape is more complicated than a simple cylinder. Other minor variations of the process and the ~ie may be utilized as well.
Grains used to transmit pressure may have co~position _ dS referred to in the above tw~ patents or other o~sitions that maybeused.
Examples of wear and corrosion resistant cladding materials used in the experimental program Nominal compQsition(*)Trade Name ~ Company Cz-28.5Mtr1t.5Cr-3.4Si* Triballoy Alloy I-800 Cabot Cbrporation C~,30Cr-12.5WL2.~C* Stellite Al~loy~No. 1 Cabot a~rporation Cor28Cr-4Wo1.1C* Stellite Allcy No. 6 CakDt C~rpo~ation Ni-16Cr-4Fe-3.3B-4.2Si-0.7C* Deloro Alloy No. 60 C2bot ~w~oration DelorD Alloy Nb. 60-60% tungsten * Haystellite, O~site Cabot aD~ation c~rb;de Fowder No. 4 Fe-35Cr-12Co-10~i-5Si- C* Tristelle Alloy TS-2 Cabot O~ration 20 TS-2 - 60~ * CDP-C4 CDP, Inc.
TS-2 - 60% Cr3C2 C$P-C CDP, Inc.
Tr~loy q-800 - 60%Cr3C2 * CDP-C3 CDP, Inc.
Deloro 60 - 60~ Cr3C2 * CDP-C2 CDP, Inc.
Cu-37Mn-lONi-0.5La * Amdry 935 Alloy Metals, Inc.
Ni-19Mn-6Si-0.5B-4CU-O-03 rare earth * h~y 939 Alloy Metals, Inc.
Ni-13Cr-20Cor2.3B-4Si-4Fe* Amdry 915E Alloy Metals, Inc.
.
t*) Compositions are given in weiqht percentages, except first components, whose percentage-~ are not given, make up the remaind,er ` of the mixture;
* TRADEMARK
Preferably, the lined surface is defined by a mud pump liner having cylindrical shape, said surface at the inner side of the cylinder, the metal powder in said layer selected from the group essentially consisting of:
a) Co-Cr-W-C
b) Co-Mo-Cr-Si c) Ni-Cr-Fe-Si-B
d) Ni-Mn-Si-Cu-B
e) Ni-Co-Cr-Si-Fe-B
f ) Fe-Cr-Co-Ni-Si-C
g) Cu-Mn-Ni Further, said layer may consist essentially of a mixture of 30 to 90% by weight tungsten carbide and remaining metal alloy powder selected from the group consisting of:
a) Co-Cr-W-C
b) Ni-Cr-Fe-Si-B
c) Cu-Nn-Ni d) Ni-Co-Cr-Fe-Si-B
e) Fe-Cr-Co-Ni-Si-C --
Claims
The embodiments of the invention in which an exclusive property or privilege is claimed are defined as follows:
1. Apparatus for cladding an internal cavity surface of a metal object, the cladding consisting essentially of a powder metal layer on said internal surface, the metal powder including metal oxide or oxides, borides and carbides, said apparatus comprising:
(a) a pressure transmitting and flowable grain filled into said cavity to contact said layer, (b) means for pressurizing said grain to cause sufficient pressure transmission to the powder metal layer to consolidate same, said means transmitting force to the grain along a primary axis, said layer extending about said axis and spaced therefrom, whereby force is transmitted by the grain away from said axis and against said layer, (c) and including a step die having a first chamber receiving said object, the die having a second chamber containing said grain communicating with said grain in the cavity which is in the first chamber, said pressurizing of the grain in the cavity being effected by grain pressurized in the second chamber, (d) and wherein the second chamber is in axial alignment with the first chamber, the second chamber having a cross section less than the cross section of the first chamber, and said powder metal layer to be pressurized being everywhere outside the projection into said cavity of a throat defined by the second chamber, whereby pressure is transmitted from the grain in the second chamber which is everywhere spaced from said layer, (e) the first chamber filled by the grain, radially inwardly of said layer.
2. The apparatus of claim 1 wherein said object is cylindrical and said layer is affixed to an internal cylindrical surface of said object, the throat having a diameter D1, the powder metal layer having an inner diameter of D2, D1 being less than D2, the first chamber having one inner diameter greater than D2.
3. The apparatus of claim 2 wherein said object comprises a mud pump liner, the first chamber also having another inner diameter larger than the one inner diameter, and at the end of the first chamber remote from the second chamber.
4. The apparatus of claim 1, wherein said surface is defined by a mud pump having a cylindrical shape, said surface at the inner side of the cylinder, the metal powder in said layer selected from the group consisting:
(a) Co-Cr-W-C
(b) Co-Mo-Cr-Si-(c) Ni-Cr-Fe-Si-B
(d) Ni-Mn-Si-Cu-B
(e) Ni-Co-Cr-Si-Fe-B
(f) Fe-Cr-Co-Ni-Si-C
(g) Cu-Mn-Ni and containing admixed powders of hard compounds such as oxides, borides and carbides.
5. The apparatus of claim 1 wherein said layer consists of a mixture of about 97% by weight of metal powder, and at least about 1.0% by weight of cellulose acetate and hydrocarbon solvent.
6. The invention of claim 1 wherein said layer consists essentially of a mixture of 30 to 92% by weight tungsten carbide and remaining metal alloy powder selected from the group consisting of:
(a) Co-Cr-W-C
(b) Ni-Cr-Fe-Si-B
(c) Cu-Mn-Ni (d) Ni-Co-Cr-Fe-Si-B
(e) Fe-Cr-Co-Ni-Si-C
7. The apparatus of claim 1 wherein said means includes a plunger transmitting force to the grain along a primary axis.
8. The apparatus of claim 1 wherein said object is generally cylindrical and said layer is affixed to an internal cylindrical surface of said object.
9. The apparatus of claim 8 wherein said object comprises a mud pump liner.
10. The apparatus of claim 2 wherein the metal powder in said layer is selected from the group consisting of:
(a) Co-Cr-W-C
(b) Co-Mo-Cr-Si (c) Ni-Cr-Fe-Si-B
(d) Ni-Mn-Si-Cu-B
(e) Ni-Co-Cr-Si-Fe-B
(f) Fe-Cr-Co-Ni-Si-C
and contains admixed powders of hard compounds selected from the group consisting of oxides, borides and carbides.
1. Apparatus for cladding an internal cavity surface of a metal object, the cladding consisting essentially of a powder metal layer on said internal surface, the metal powder including metal oxide or oxides, borides and carbides, said apparatus comprising:
(a) a pressure transmitting and flowable grain filled into said cavity to contact said layer, (b) means for pressurizing said grain to cause sufficient pressure transmission to the powder metal layer to consolidate same, said means transmitting force to the grain along a primary axis, said layer extending about said axis and spaced therefrom, whereby force is transmitted by the grain away from said axis and against said layer, (c) and including a step die having a first chamber receiving said object, the die having a second chamber containing said grain communicating with said grain in the cavity which is in the first chamber, said pressurizing of the grain in the cavity being effected by grain pressurized in the second chamber, (d) and wherein the second chamber is in axial alignment with the first chamber, the second chamber having a cross section less than the cross section of the first chamber, and said powder metal layer to be pressurized being everywhere outside the projection into said cavity of a throat defined by the second chamber, whereby pressure is transmitted from the grain in the second chamber which is everywhere spaced from said layer, (e) the first chamber filled by the grain, radially inwardly of said layer.
2. The apparatus of claim 1 wherein said object is cylindrical and said layer is affixed to an internal cylindrical surface of said object, the throat having a diameter D1, the powder metal layer having an inner diameter of D2, D1 being less than D2, the first chamber having one inner diameter greater than D2.
3. The apparatus of claim 2 wherein said object comprises a mud pump liner, the first chamber also having another inner diameter larger than the one inner diameter, and at the end of the first chamber remote from the second chamber.
4. The apparatus of claim 1, wherein said surface is defined by a mud pump having a cylindrical shape, said surface at the inner side of the cylinder, the metal powder in said layer selected from the group consisting:
(a) Co-Cr-W-C
(b) Co-Mo-Cr-Si-(c) Ni-Cr-Fe-Si-B
(d) Ni-Mn-Si-Cu-B
(e) Ni-Co-Cr-Si-Fe-B
(f) Fe-Cr-Co-Ni-Si-C
(g) Cu-Mn-Ni and containing admixed powders of hard compounds such as oxides, borides and carbides.
5. The apparatus of claim 1 wherein said layer consists of a mixture of about 97% by weight of metal powder, and at least about 1.0% by weight of cellulose acetate and hydrocarbon solvent.
6. The invention of claim 1 wherein said layer consists essentially of a mixture of 30 to 92% by weight tungsten carbide and remaining metal alloy powder selected from the group consisting of:
(a) Co-Cr-W-C
(b) Ni-Cr-Fe-Si-B
(c) Cu-Mn-Ni (d) Ni-Co-Cr-Fe-Si-B
(e) Fe-Cr-Co-Ni-Si-C
7. The apparatus of claim 1 wherein said means includes a plunger transmitting force to the grain along a primary axis.
8. The apparatus of claim 1 wherein said object is generally cylindrical and said layer is affixed to an internal cylindrical surface of said object.
9. The apparatus of claim 8 wherein said object comprises a mud pump liner.
10. The apparatus of claim 2 wherein the metal powder in said layer is selected from the group consisting of:
(a) Co-Cr-W-C
(b) Co-Mo-Cr-Si (c) Ni-Cr-Fe-Si-B
(d) Ni-Mn-Si-Cu-B
(e) Ni-Co-Cr-Si-Fe-B
(f) Fe-Cr-Co-Ni-Si-C
and contains admixed powders of hard compounds selected from the group consisting of oxides, borides and carbides.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA000556982A CA1326132C (en) | 1985-01-07 | 1988-01-20 | Pump liners and a method of cladding the same |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US06/689,312 US4603062A (en) | 1985-01-07 | 1985-01-07 | Pump liners and a method of cladding the same |
| CA000510057A CA1235026A (en) | 1985-01-07 | 1986-05-27 | Pump liners and a method of cladding the same |
| CA000556982A CA1326132C (en) | 1985-01-07 | 1988-01-20 | Pump liners and a method of cladding the same |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000510057A Division CA1235026A (en) | 1985-01-07 | 1986-05-27 | Pump liners and a method of cladding the same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1326132C true CA1326132C (en) | 1994-01-18 |
Family
ID=24767910
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000510057A Expired CA1235026A (en) | 1985-01-07 | 1986-05-27 | Pump liners and a method of cladding the same |
| CA000556982A Expired - Fee Related CA1326132C (en) | 1985-01-07 | 1988-01-20 | Pump liners and a method of cladding the same |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000510057A Expired CA1235026A (en) | 1985-01-07 | 1986-05-27 | Pump liners and a method of cladding the same |
Country Status (7)
| Country | Link |
|---|---|
| US (3) | US4603062A (en) |
| EP (1) | EP0247255B1 (en) |
| JP (1) | JPS62294105A (en) |
| AT (1) | ATE70475T1 (en) |
| AU (1) | AU590884B2 (en) |
| CA (2) | CA1235026A (en) |
| DE (1) | DE3683044D1 (en) |
Families Citing this family (28)
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| US4603062A (en) * | 1985-01-07 | 1986-07-29 | Cdp, Ltd. | Pump liners and a method of cladding the same |
| US4919013A (en) * | 1988-09-14 | 1990-04-24 | Eastman Christensen Company | Preformed elements for a rotary drill bit |
| US4853178A (en) * | 1988-11-17 | 1989-08-01 | Ceracon, Inc. | Electrical heating of graphite grain employed in consolidation of objects |
| US4933140A (en) * | 1988-11-17 | 1990-06-12 | Ceracon, Inc. | Electrical heating of graphite grain employed in consolidation of objects |
| JP2587872B2 (en) * | 1988-12-19 | 1997-03-05 | 住友金属鉱山株式会社 | Method for producing soft magnetic sintered body of Fe-Si alloy |
| US5294382A (en) * | 1988-12-20 | 1994-03-15 | Superior Graphite Co. | Method for control of resistivity in electroconsolidation of a preformed particulate workpiece |
| US4915605A (en) * | 1989-05-11 | 1990-04-10 | Ceracon, Inc. | Method of consolidation of powder aluminum and aluminum alloys |
| US5324168A (en) * | 1993-05-13 | 1994-06-28 | Eastman Kodak Company | Use of stellite to prevent silver plateout |
| EP0754847B1 (en) * | 1995-07-20 | 1999-05-26 | Spx Corporation | Method of providing a cylinder bore liner in an internal combustion engine |
| US5617773A (en) * | 1995-11-07 | 1997-04-08 | Craft; Alan | Liner for use in corrosive and abrasive fluid pump and method of making same |
| CN2256043Y (en) * | 1995-12-15 | 1997-06-11 | 王德庆 | Long service life oil sucking pump with ceramic inlaid cylinder body |
| US6230610B1 (en) | 1999-06-11 | 2001-05-15 | Utex Industries, Inc. | Pump liner |
| US6463843B2 (en) | 1999-06-11 | 2002-10-15 | Fredrick B. Pippert | Pump liner |
| US6675699B1 (en) | 2000-09-25 | 2004-01-13 | Utex Industries, Inc. | Composite components for use in pumps |
| DE10333152B3 (en) * | 2003-07-22 | 2005-01-20 | A. Raymond & Cie | Coating adhesion surfaces with a melt adhesive, comprises applying a mixed adhesive in powder form and then pressing to generate heat |
| DE202004016252U1 (en) * | 2004-08-12 | 2005-12-22 | Schmidt + Clemens Gmbh & Co. Kg | Composite pipe, for use in steam cracking of hydrocarbons or in rotary furnaces or refuse incinerators, comprises outer spun pipe and coaxial inner pipe which is made by compressing powder |
| US7767274B2 (en) * | 2005-09-22 | 2010-08-03 | Skaff Corporation of America | Plasma boriding method |
| CA2649525A1 (en) * | 2006-04-20 | 2007-11-01 | Habib Skaff | Mechanical parts having increased wear resistance |
| WO2008116159A2 (en) * | 2007-03-22 | 2008-09-25 | Skaff Corporation Of America, Inc. | Mechanical parts having increased wear-resistance |
| IT1399883B1 (en) | 2010-05-18 | 2013-05-09 | Nuova Pignone S R L | INCAMICIATA IMPELLER WITH GRADUATED FUNCTIONAL MATERIAL AND METHOD |
| US8962154B2 (en) * | 2011-06-17 | 2015-02-24 | Kennametal Inc. | Wear resistant inner coating for pipes and pipe fittings |
| CN102978581A (en) * | 2012-11-06 | 2013-03-20 | 上海宏昊企业发展有限公司 | Thermal expansion aluminum guide roller and production process thereof |
| DE102013211848A1 (en) * | 2013-06-21 | 2014-12-24 | Heraeus Precious Metals Gmbh & Co. Kg | Pump housing made of at least two different sinterable materials |
| DE102013211844A1 (en) | 2013-06-21 | 2014-12-24 | Heraeus Precious Metals Gmbh & Co. Kg | Pump housing made of a magnetic and a non-magnetic material |
| DE102013211845A1 (en) * | 2013-06-21 | 2014-12-24 | Heraeus Precious Metals Gmbh & Co. Kg | Pump housing with hard inner layer and weldable outer layer |
| DE102014004121A1 (en) | 2014-03-24 | 2015-09-24 | Heraeus Deutschland GmbH & Co. KG | Pump housing made of at least three different sinterable materials |
| CN105063499B (en) * | 2015-07-20 | 2017-04-05 | 安徽工程大学 | A kind of ball grinding machine lining board remanufactures Surface coating parts |
| TWI807812B (en) * | 2022-05-06 | 2023-07-01 | 高科晶捷自動化股份有限公司 | Glue-discharging device and glue-discharging method thereof |
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| US4603062A (en) * | 1985-01-07 | 1986-07-29 | Cdp, Ltd. | Pump liners and a method of cladding the same |
-
1985
- 1985-01-07 US US06/689,312 patent/US4603062A/en not_active Expired - Lifetime
-
1986
- 1986-05-27 AT AT86303990T patent/ATE70475T1/en not_active IP Right Cessation
- 1986-05-27 CA CA000510057A patent/CA1235026A/en not_active Expired
- 1986-05-27 EP EP86303990A patent/EP0247255B1/en not_active Expired
- 1986-05-27 DE DE8686303990T patent/DE3683044D1/en not_active Expired - Fee Related
- 1986-05-29 AU AU58057/86A patent/AU590884B2/en not_active Ceased
- 1986-05-30 US US06/868,991 patent/US4746554A/en not_active Expired - Fee Related
- 1986-06-12 JP JP61137261A patent/JPS62294105A/en active Granted
- 1986-06-16 US US06/874,607 patent/US4715313A/en not_active Expired - Fee Related
-
1988
- 1988-01-20 CA CA000556982A patent/CA1326132C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CA1235026A (en) | 1988-04-12 |
| US4603062A (en) | 1986-07-29 |
| US4715313A (en) | 1987-12-29 |
| US4746554A (en) | 1988-05-24 |
| AU5805786A (en) | 1987-12-03 |
| EP0247255B1 (en) | 1991-12-18 |
| EP0247255A1 (en) | 1987-12-02 |
| DE3683044D1 (en) | 1992-01-30 |
| JPS62294105A (en) | 1987-12-21 |
| ATE70475T1 (en) | 1992-01-15 |
| JPH0314882B2 (en) | 1991-02-27 |
| AU590884B2 (en) | 1989-11-23 |
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| MKLA | Lapsed |