US3914178A - Wear reducing coating - Google Patents

Wear reducing coating Download PDF

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Publication number
US3914178A
US3914178A US435889A US43588974A US3914178A US 3914178 A US3914178 A US 3914178A US 435889 A US435889 A US 435889A US 43588974 A US43588974 A US 43588974A US 3914178 A US3914178 A US 3914178A
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Prior art keywords
layer
fastener assembly
metal
lubricant
group
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US435889A
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Inventor
Charles A Fineran
Steven S Silwones
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Harvard Industries Inc
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Amerace Corp
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Priority to US435889A priority Critical patent/US3914178A/en
Priority to GB1380/75A priority patent/GB1480433A/en
Priority to CA218,189A priority patent/CA1020783A/en
Priority to DE19752502011 priority patent/DE2502011A1/de
Priority to SE7500620A priority patent/SE7500620L/xx
Priority to IT47790/75A priority patent/IT1026422B/it
Priority to BE1006415A priority patent/BE824637A/xx
Priority to FR7502059A priority patent/FR2258557B1/fr
Priority to JP50010120A priority patent/JPS50107375A/ja
Application granted granted Critical
Publication of US3914178A publication Critical patent/US3914178A/en
Priority to CA273,862A priority patent/CA1050362A/en
Priority to SE7907002A priority patent/SE7907002L/sv
Assigned to HARVARD INDUSTRIES, INC., A CORP OF DE reassignment HARVARD INDUSTRIES, INC., A CORP OF DE ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: AMERACE CORPORATION A DE CORP
Assigned to CITIBANK, N.A. reassignment CITIBANK, N.A. SECURITY INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HARMAN AUTOMOTIVE, INC., A MI CORP., HARVARD INDUSTRIES, INC., A DE CORP.
Assigned to HARVARD INDUSTRIES, INC., A CORP. OF DE., HARMAN AUTOMOTIVE, INC., A CORP. OF MICHIGAN reassignment HARVARD INDUSTRIES, INC., A CORP. OF DE. RELEASED BY SECURED PARTY (SEE DOCUMENT FOR DETAILS). Assignors: CITIBANK, N.A.
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16B—DEVICES FOR FASTENING OR SECURING CONSTRUCTIONAL ELEMENTS OR MACHINE PARTS TOGETHER, e.g. NAILS, BOLTS, CIRCLIPS, CLAMPS, CLIPS OR WEDGES; JOINTS OR JOINTING
    • F16B33/00—Features common to bolt and nut
    • F16B33/06—Surface treatment of parts furnished with screw-thread, e.g. for preventing seizure or fretting
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16B—DEVICES FOR FASTENING OR SECURING CONSTRUCTIONAL ELEMENTS OR MACHINE PARTS TOGETHER, e.g. NAILS, BOLTS, CIRCLIPS, CLAMPS, CLIPS OR WEDGES; JOINTS OR JOINTING
    • F16B37/00—Nuts or like thread-engaging members
    • F16B37/04—Devices for fastening nuts to surfaces, e.g. sheets, plates
    • F16B37/044—Nut cages
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16B—DEVICES FOR FASTENING OR SECURING CONSTRUCTIONAL ELEMENTS OR MACHINE PARTS TOGETHER, e.g. NAILS, BOLTS, CIRCLIPS, CLAMPS, CLIPS OR WEDGES; JOINTS OR JOINTING
    • F16B39/00—Locking of screws, bolts or nuts
    • F16B39/22—Locking of screws, bolts or nuts in which the locking takes place during screwing down or tightening
    • F16B39/28—Locking of screws, bolts or nuts in which the locking takes place during screwing down or tightening by special members on, or shape of, the nut or bolt
    • F16B39/284—Locking by means of elastic deformation
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16B—DEVICES FOR FASTENING OR SECURING CONSTRUCTIONAL ELEMENTS OR MACHINE PARTS TOGETHER, e.g. NAILS, BOLTS, CIRCLIPS, CLAMPS, CLIPS OR WEDGES; JOINTS OR JOINTING
    • F16B39/00—Locking of screws, bolts or nuts
    • F16B39/22—Locking of screws, bolts or nuts in which the locking takes place during screwing down or tightening
    • F16B39/28—Locking of screws, bolts or nuts in which the locking takes place during screwing down or tightening by special members on, or shape of, the nut or bolt
    • F16B39/34—Locking by deformable inserts or like parts
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S411/00—Expanded, threaded, driven, headed, tool-deformed, or locked-threaded fastener
    • Y10S411/914—Coated bolt
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S411/00—Expanded, threaded, driven, headed, tool-deformed, or locked-threaded fastener
    • Y10S411/924—Coupled nut and bolt
    • Y10S411/929—Thread lock
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S411/00—Expanded, threaded, driven, headed, tool-deformed, or locked-threaded fastener
    • Y10S411/924—Coupled nut and bolt
    • Y10S411/929—Thread lock
    • Y10S411/93—Flowing metal or settable material
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S411/00—Expanded, threaded, driven, headed, tool-deformed, or locked-threaded fastener
    • Y10S411/924—Coupled nut and bolt
    • Y10S411/947—Elastic-gripping action
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12535—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.] with additional, spatially distinct nonmetal component
    • Y10T428/12542—More than one such component
    • Y10T428/12549—Adjacent to each other
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12535—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.] with additional, spatially distinct nonmetal component
    • Y10T428/12556—Organic component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12861—Group VIII or IB metal-base component
    • Y10T428/12903—Cu-base component
    • Y10T428/12917—Next to Fe-base component
    • Y10T428/12924—Fe-base has 0.01-1.7% carbon [i.e., steel]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12861—Group VIII or IB metal-base component
    • Y10T428/12937—Co- or Ni-base component next to Fe-base component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12861—Group VIII or IB metal-base component
    • Y10T428/12951—Fe-base component
    • Y10T428/12972—Containing 0.01-1.7% carbon [i.e., steel]
    • Y10T428/12979—Containing more than 10% nonferrous elements [e.g., high alloy, stainless]

Definitions

  • Molybdenum dlsulfide or graphlte may be used as the inorganic lubricant and lauric acid or cetyl alcohol may be used as the organic lubricant. 3:099: 3 9 3 De 252/12
  • the organic lubricant is optional where the first metal 3,224,967 12/1965 Battista 252/12.2 layer is on one metallic surface and the second metal 3,244,625 4/1966 Silwones 252/28 layer is on the other metallic surface.
  • the coating is applied to lock-nut and 1;; f" bolt fasteners to prevent wear or galling over multiple onsa 1 3,729,292 4/1973 Heck 2521122 re cycles 3,791,970 2/ 1974 Tubb 252/ 12 23 Claims, 6 Drawing Figures WEAR REDUCING COATING BRIEF SUMMARY OF THE INVENTION
  • the present invention relates to a coating for reducing the wear of two opposable stainless steel surfaces which are in a sliding relationship with one another comprising: a first metal layer; a second metal layer; an inorganic lubricant; and, an organic lubricant.
  • the first metal layer is a hard metal layer, i.e., a metal layer having an elastic modulus of about 20,000,000 p.s.i. or higher such as nickel and the alloys thereof, whereas the second metal layer is a soft metal layer, i.e., a metal layer having an elastic modulus of about 17,000,000 p.s.i. or lower such as copper and the alloys thereof.
  • the inorganic lubricant comprises molybdenum disulfide, graphite or combinations thereof.
  • the organic lubricant may be any organic lubricant known in the art such as high molecular weight aliphatic alcohols and aliphatic acids or the glycerides of such acids; waxes derived from petroleum or other natural sources or blends of such waxes with polyolefins such as polyethylene, polypropylene and the like. Automotive lubricants such as motor oils and greases may also be used as well as the art known silicone oils and silicone greases.
  • the use of the organic lubricant is optional where the first metal layer is applied to one metallic surface and the second metal layer is applied to the second metallic surface.
  • coatings in accordance with the invention reduce wear between metallic surfaces and have been found to be effective to reduce wear or galling in locknut and bolt fasteners in which the bolt is used under high bolt tension.
  • nut and bolt fasteners made from A-286 stainless steel or other stainless steels have a tendency to gall after continued assemblies and reassemblies even when these operations are performed at room temperatures.
  • fasteners have a limited reuse, i.e., generally less than 20 on-off cycles.
  • such fasteners can be assembled and reassembled without galling for 50 or more reuse cycles.
  • FIG. 1 illustrates a lock-nut and bolt each having a coating in accordance with the present invention
  • FIG. 2 illustrates a bolt for use in combination with an uncoated lock-nut wherein said bolt has a coating in accordance with the present invention
  • FIG. 3 illustrates a frontal elevation in section of an off-set lock-nut having a coating thereon in accordance with the present invention
  • FIG. 3A is a plan view of the lock-nut of FIG. 3;
  • FIG. 4 illustrates two opposed metallic surfaces one of which is coated in accordance with the present invention.
  • FIG. 5 illustrates two opposed metallic surfaces both of which are coated in accordance with the present invention.
  • a self-locking threaded fastener e.g., a lock-nut, comprises a device having means built into a threaded nut to prevent the nut from unloosening during use in an environment where a high degree of vibration is en countered such as in internal combustion engines, aircraft or automotive assemblies.
  • locknut is used in applications where constant re-use is required since with prior art lock-nuts and bolts employed in fastening operations and made of high strength materials like A-286 stainless steel only about 10 to 20 reuse or off-on cycles are possible before excessive wear and/or thread damage renders them unsuitable for use, particularly in application where an automatic torque wrench is used to apply a high torque to the nut or bolt to intentionally leave a high residual stress on the bolt and obtain optimum fastening. Examples of such applications are the fastening of access panels for electronic components in aircraft or access panels in turbojet engine assemblies where ordinary maintenance requires regular removal of the panels for replacement or overhaul of components. As can be readily appreciated there would be a considerable advantage in being able to extend the reuse life of locknut and bolt fasteners in such applications.
  • the means built in to the lock-nut to prevent the nut from unloosening comprises a friction device that permits the nut to be turned on a bolt with a moderate amount of torque which provides frictional resistance to unloosening when the threaded connection is subject to vibration, and which permits assembly without undue tightening.
  • the friction on the nut before it is screwed into a fastening position is generally reflected in the torque values required to screw the nut down into such fastening position and is sufficiently high to keep the lock-nut from unloosening due to vibration when in place.
  • the friction means in the lock-nut generally comprises a polymeric washer sealed into the nut such as a polyamide or nylon compound or a polyimide such as Vespel (a trademarked compound produced and sold by E. I.
  • Friction means are also provided by crimping or offsetting one end of a nut so that when looking down into the threaded portion of the nut at least one end is in an oval, elliptical, oblate or prolate configuration instead of being ordinarily round.
  • Offsetting a nut is generally the method employed for manufacturing locknuts that are to be used in high temperature applications since polymeric materials tend to decompose upon prolongedexposure to temperatures in excess of 500F.
  • Either of these friction means i.e., offsetting or the provision of a polymeric washer
  • one embodiment comprises providing a coating on the threads of a lock-nut and/or bolt for reducing the wear and maintaining desired friction between the threads of the lock-nut and the threads of the bolt.
  • a coating for reducing the wear of two opposable metallic surfaces comprising a first metal layer; a second metal layer; an inorganic lubricant; and, an organic lubricant.
  • the aforementioned coating layers are applied to the surfaces of the metal in such a fashion so that the first metal layer is a substrate for the second metal layer or this metal layer is applied to one metallic surface and the second metal layer to the other metallic surface.
  • first metal layer is a substrate for the second metal layer it is intended by this expression to indicate that the second metal layer is placed on the first metal layer.
  • the inorganic lubricant is placed on the second metal layer whether this second metal layer is placed on the first layer or applied directly to one metallic surface and the first layer to the other metallic surface.
  • the organic lubricant is optional when the first metal layer is applied to one metallic surface and the second metal layer is applied to the remaining metallic surface.
  • the inorganic lubricant is placed on the second metal layer.
  • the organic lubricant is then employed as a final layer by which it is meant that the final layer is placed on either the aforementioned uncoated metallic surface or coated surface or both.
  • the first metal layer is a hard metal, i.e., a metal having an elastic modulus of about 20,000,000 p.s.i. and higher (i.e. a range inclusive of and greater than about 20,000,000 p.s.i.) or an elastic modulus in the range of from about 20,000,000 p.s.i. to about 75,000,000 p.s.i.
  • the hard metal includes a member selected from the group consisting of the following metals, the elastic modulus of each in p.s.i.
  • the second metal layer is a soft metal, i.e., a metal having an elastic modulus of about 17,000,000 p.s.i. and lower (i.e. a range inclusive of and lower than about 17,000,000 p.s.i.) or an elastic modulus in the range of from about 17,000,000 p.s.i. to about 2.5 million p.s.i.
  • the soft metal includes a member selected from the group consisting of the following metals, the elastic modulus of each being in p.s.i.
  • the inorganic lubricant comprises molybdenum disulfide or graphite, however, molybdenum disulfide is preferred although mixtures of molybdenum disulfide and graphite may also be used.
  • the organic lubricant coating layer is a member selected from the group consisting of cetyl alcohol, lauric acid, normally solid paraffin wax, microcrystalline wax, carnauba wax, spermacetti wax and blends thereof or blends with polyolefins such as polyethylene, polypropylene and the like.
  • the preferred organic lubricants comprise lauric acids, cetyl alcohol, or lauric triglycerides which may be further characterized as aliphatic alcohols or aliphatic acids having about 10 to about 20 carbon atoms and the glycerides, especially the triglycerides of such acids.
  • Petroleum based lubricants may also be used such as automotive motor oils and grease.
  • Silicone lubricants known in the art may also be used such as silicone oils and silicone greases.
  • a bolt 10 is illustrated having coated threads 12 which engage coated threads 14 of a locknut 16 having a Vespel polymeric washer 18, which also engages coated threads 12, and a protective outer washer 20.
  • the nutbolt assembly provides securement for such as plates 10a and 10b.
  • the coating on threads 12 is a first layer comprising nickel whereas the coating on the threads 14 is a second layer comprising copper which is also a substrate for an inorganic lubricant layer comprising molybdenum disulfide.
  • the coated thread 12 and/or coated thread 14 may optionally have an organic lubricant as a final coat.
  • a lock-nut and bolt as described in FIG. 1 can be used in a minimum of 50 on-off reuse cycles in a fastening operation where applied torque is sufficient to generate the bolt tension desired for the assembly in question without so galling or wearing the thread surfaces as to render the nut and bolt combination unsuitable for use during such reuse cycles, i.e., exhibiting undue galling.
  • the desired friction fit between washer 18 and threads 12 is maintained throughout the 50 reuse cycles.
  • P16. 2 illustrates a high strength bolt 22 having coated threads 24 for use in combination with a mating nut, such as a lock-nut.
  • the threads 24 having a coating thereon in accord with the present invention in which a first metal layer comprising nickel is coated onto the bolt thread, a second metal layer comprising copper is coated over the first metal layer, an inorganic lubricant comprising molybdenum disulfide is coated over said second metal layer and an organic lubricant comprising cetyl alcohol is applied over the inorganic lubricant.
  • Bolts of FIG. 2 when made from such materials as A-286 or other stainless steels and assemblied on plain uncoated nuts of the same material, can be used through 50 reuse cycles without undue galling. Also, if the mating nut is a lock-nut with a nylon of Vespel insert, it continues to give adequate locking torque throughout the 50 reuses.
  • FIG. 3 illustrates a lock-nut 26 having threads 28, said lock-nut having been offset by crimping one end thereof 30 so that said offset end 30 is elliptical having one elliptical diameter shorter in length than the round diameter at uncrimped nut portion 32.
  • the lock-nut is mounted in channel 34, the sidewalls of which are slotted to receive lock-nut retaining clip 36.
  • FIG. 3A is a plan view of nut 26 showing crimped end 30.
  • the crimped nut acts as a lock-nut since the shortened elliptical diameter at the crimped end 30 enables the nut to frictionally engage a bolt.
  • Threads 28 are coated with a first metal layer com prising nickel, said first metal layer being coated in turn with a second metal layer comprising copper, said sec ond metal layer in turn being coated with an inorganic lubricant comprising molybdenum disulfide and said inorganic lubricant comprising molybdenum disulfide in turn being coated with an organic lubricant such as cetyl alcohol.
  • the lock-nut illustrated in FIG. 3 and FIG. 3A even if made from materials like A-286 or other stainless steels that tend to gall when installed in tightened rela tionship to uncoated bolts of the same material, can be used through 50 reuse cycles without undue galling or loss of friction locking torque.
  • FIG. 4 illustrates two opposable sliding metallic surfaces 38 and 40 having a first metal layer 42 comprising nickel coated on metallic surface 38, said first metal layer having a second metal layer 44 coated thereon comprising copper said second metal layer 44 having an inorganic lubricant 46 coated thereon comprising molybdenum disulfide, said inorganic lubricant 46 having an organic lubricant 48 coated thereon comprising cetyl alcohol.
  • Metallic surface 38 may be a nut thread whereas metallic surface 40 may be a bolt thread.
  • FIG. 5 illustrates a set of two opposable metallic surfaces 50 and 52 that may be placed in a sliding relationship with one another, said metallic surface 50 having a first metal layer 54 comprising nickel coated thereon, said metallic surface 52 having a second metal layer 56 comprising copper coated thereon, said second metal layer 56 having an inorganic lubricant 58 comprising molybdenum disulfide coated thereon.
  • Metallic surface 50 may be a nut thread and metallic surface 52 may be a bolt thread.
  • use of an organic lubricant on the molybdenum disulfide surface is, in this instance, optional.
  • the metallic surfaces illustrated in FIG. 4 and FIG. 5 even if the parts are made of materials that tend to gall on repeated assemblies, may be placed in a sliding relationship with one another without binding or galling and that the wear thereon will be substantially reduced, even if there is a large amount of pressure at the interface of such coated metallic surfaces and even if there are repeated assemblies and disassemblies of the parts.
  • the coatings on such metallic surfaces prevent excessive wear and galling, and when the coating is applied on the threads of lock-nut and bolt fastening devices made of such materials as A-286 or 13-8 stainless steels, the parts continue to operate satisfactorily even after 50 reuses.
  • the metal coating is applied preferably by electroplating although other coating methods may be used such as flame spraying, hot melt coating, hot dip coating, cladding, fluidized bed coating, vacuum metallizing, cathode sputtering, chemical reduction, surface alloying by coating followed by heating in vacuum and all of the art known equivalents thereof.
  • the metals that may be coated according to the present invention comprise stainless steels including Handbook, austentitic, martensitic and ferritic types as defined in Metals Handbood, Vol. I, Properties and Selection of Metals, published by the American Society for Metals, copyright 1961.
  • stainless steel such as 13-8 stainless steel containing 13% chrome, 8% nickel and minor amounts of molybdenum or A-286 stainless steel containing about 25% nickel and about 16% chromium may be used as the substrate to which the coating is applied especially in that aspect of the invention which comprises the application of the coating to lock-nuts and/or bolts.
  • Other stainless steels include inter alia 18-8 stainless and Waspaloy (tradename, Special Metals, Inc.)
  • the coating of the present invention Prior to the use of the coating of the present invention severe galling resulted from reusing lock-nut-bolt combinations subject to high bolt stress.
  • the galling usually occurred between approximately the 10th and 20th reuse cycle in stainless steel nut and bolt combinations, the galling being a deformation of the thread surfaces such as scoring and chipping and in some instances breaking and fusing of the threads.
  • the coating of the invention has extended the reuse of such nut and bolt assemblies up to a minimum of 50 cycles without rendering the nut and bolt assemblies unsuitable for use during such reuse cycles.
  • Thin coatings are desirably used in lock-nut and bolt combinations since this type of coating facilitates application to standard screw threads without having to modify the screw thread dimensions to prevent binding of the lock-nut on the bolt.
  • a first metal layer such as nickel preferably of a thickness from about 0.0001 to about 000015 inch
  • the second metal layer such as copper
  • the inorganic lubricant such as molybdenum disulfide of a thickness preferably from about 0.0001 to about 0.0004 inch
  • the inorganic lubricant may be applied in any thickness from about 0.0001 inch on up since the coating is deformable under
  • the lock-nut can be a lock-nut having a polymeric washer sealed into the nut or a nut that has been offset.
  • the coating may be subjected to elevated temperature up to 600F and still effectively function as a coating that will prevent excessive wear when applied to a lock-nut and/or bolt exposed to such temperature. Also, sufficient friction is maintained between the locking element of the lock-nut and bolt so that the nut will not loosen when exposed to conditions of extreme vibration.
  • the coating of the invention may also be used on other sliding applications such as metal to metal bearing surfaces, piston rings, piston-cylinder wall interfaces, zippers and snap-fasteners in addition to lock-nut and lock-nut and bolt combinations.
  • the molybdenum disulfide coating was Everlube 642 (registered trademark, Everlube Corporation, 6940 Farmdale Avenue, North Hollywood, Calif.), a solid film lubricant conforming to Mil- L-460l0(A) which is a formulation of molybdenum disulfide, metallic oxides and salts dispersed in a resinous binder system soluble in a solvent comprising dioxane or a mixture of 50% methyl ethyl ketone and 50% toluene.
  • the molybdenum disulfide coating is applied to the metal part by dipping and is then cured by baking at about 400F for one hour.
  • the plain metal parts are blasted with 120 mesh grit for approximately 30 minutes to produce a frosty finish.
  • the bolts or nuts are then nickel plated followed by rinsing in water and neutralizing in alkali.
  • nickel plated nuts are transferred to the copper plating solution and after copper coating the parts are again rinsed and dried.
  • the plain A-286 nuts are directly copper-coated after grit blasting.
  • Both the nickel and copper coatings are applied by standard electrolytic methods to a coating thickness of 0.00015 plus or minus 0.0005 in Example 1.
  • the nickel coat is applied to an A-286 bolt and the mating A-286 nut was copper-plated and given a molybdenum disulfide coat on the copper.
  • Example 2 the same combi nation is used but an additional cetyl alcohol coat is applied on the molybdenum disulfide coated surface.
  • cetyl alcohol coat about 0.6 to about 1 pound of cetyl alcohol is first dissolved in one gallon of trichloroethylene. The parts to be coated are then immersed in the lubricant solution after which the solution is allowed to drain dry before handling.
  • Example 3 all four coatings, the nickel coating, the copper coating, the inorganic lubricant and the cetyl alcohol are applied to a plain A-286 nut while the A-286 mating bolts are untreated.
  • the nuts employed in these examples are A 28 locknuts which are held in an aluminum housing for the purpose of the test. Normally 2% bolt threads extend through the top of the nut during each reuse cycle where a cycle comprises turning the bolt into the nut until the bolthead is flush with the surface of the housing and then backing the bolt off until no locking torque is developed between the nut and bolt. When the head of the bolt is screwed down into an abutting relationship with the housing surface a torque wrench is employed and the torque measured right up until the bolthead seats on the housing surface. This is defined as the maximum on torque.
  • a coating for reducing the wear of two opposed stainless steel metallic surfaces disposed in sliding relationship with one another comprising:
  • a second layer having an elastic modulus inclusive of and lower than about 17,000,000 p.s.i. and comprised of a metal selected from a member of the group consisting of palladium, copper, gold, zirconium, silver, cadmium, tin, lead and alloys thereof;
  • said first layer is applied to one of said metallic surfaces and said second layer is applied to the other metallic surface
  • said second layer is a substrate for said inorganic lubricant layer.
  • said first layer metal comprises nickel and the alloys thereof
  • said second layer metal comprises copper and the alloys thereof
  • said inorganic lubricant is selected from at least one member of the group consisting of molybdenum disulfide and graphite.
  • a coating for reducing the wear of two opposed stainless steel metallic surfaces disposed in sliding relationship with one another comprising:
  • a second layer having an elastic modulus inclusive of and lower than about 17,000,000 p.s.i. and comprised of a metal selected from a member of the group consisting of palladium, copper, gold, zirconium, silver, cadmium, tin, lead and alloys thereof;
  • a layer comprised of an organic lubricant wherein said first layer is applied to at least one of said metallic surfaces and is a substrate for said second layer, said second layer is a substrate for said inorganic lubricant layer and said organic lubricant is the final layer.
  • said inorganic lubricant is selected from at least one member of the group consisting of molybdenum disulfide and graphite.
  • organic lubricant is selected from at least one member of the group consisting of aliphatic alcohols and aliphatic acids having from about to about carbon atoms and the glycerides of such acids.
  • a fastener assembly comprising first and second slidably threadably engageable stainless steel members and lubricant structure therefor including a first layer comprised of a metal having a modulus of elasticity inclusive of and greater than about 20,000,000 p.s.i. disposed on said first member, a second layer comprised of a metal having a modulus of elasticity inclusive of and lower than about 17,000,000 p.s.i. disposed on said second member and a third layer comprised of an inorganic lubricant disposed on said second layer.
  • said first layer metal is selected from a member of the group consisting of manganese, cobalt, platinum, nickel, chromium, beryllium, rhodium, molybdenum, tungsten, ruthenium, iridium, and alloys thereof and wherein said second layer metal is selected from a member of the group consisting of palladium, copper, gold, zirconium, silver, cadmium, tin, lead and alloys thereof.
  • said inorganic lubricant is selected from at least one member of the group consisting of molybdenum disulfide and graphite.
  • a fastener assembly comprising first and second stainless steel slidably threadably engageable members and lubricant structure therefor disposed between said first and second members and including a first layer comprised of a metal having a modulus of elasticity inclusive of and greater than about 20,000,000 p.s.i., a second layer comprised of a metal having a modulus of elasticity inclusive of and lower than about 17,000,000 p.s.i. disposed on said first layer, a third layer comprised of an inorganic lubricant disposed on said second layer and a final layer comprised of an organic lubricant.
  • said first layer metal is selected from a member of the group consisting of manganese, cobalt, platinum, nickel, chromium, beryllium, rhodium, molybdenum, tungsten, ruthenium, iridium, and alloys thereof and wherein said second layer metal is selected from a member of the group consisting of palladium, copper, gold, zirconium, silver, cadmium, tin, lead and alloys thereof.
  • said inorganic lubricant is selected from at least one member of the group consisting of molybdenum disulfide and graphite.
  • organic lubricant is selected from at least one member of the group consisting of aliphatic alcohols and aliphatic acids having from about 10 to about 20 carbon atoms and the glycerides of such acids.
  • said organic lubricant is selected from at least one member of the group consisting of aliphatic alcohols and aliphatic acids having from about 10 to about 20 carbon atoms and the glycerides of such acids.

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  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Lubricants (AREA)
  • Laminated Bodies (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
US435889A 1974-01-23 1974-01-23 Wear reducing coating Expired - Lifetime US3914178A (en)

Priority Applications (11)

Application Number Priority Date Filing Date Title
US435889A US3914178A (en) 1974-01-23 1974-01-23 Wear reducing coating
GB1380/75A GB1480433A (en) 1974-01-23 1975-01-13 Coatings interposed between two slidably engageable stainless steel surfaces
CA218,189A CA1020783A (en) 1974-01-23 1975-01-20 Coating
DE19752502011 DE2502011A1 (de) 1974-01-23 1975-01-20 Ueberzug
SE7500620A SE7500620L (de) 1974-01-23 1975-01-21
BE1006415A BE824637A (fr) 1974-01-23 1975-01-22 Revetement anti-usure
IT47790/75A IT1026422B (it) 1974-01-23 1975-01-22 Rivestimento di superfici contrap poste di acciaio inossidabile in relazione di scorrimento per ridurne l usura
FR7502059A FR2258557B1 (de) 1974-01-23 1975-01-23
JP50010120A JPS50107375A (de) 1974-01-23 1975-01-23
CA273,862A CA1050362A (en) 1974-01-23 1977-03-14 Coating
SE7907002A SE7907002L (sv) 1974-01-23 1979-08-22 Notningsreducerande beleggning

Applications Claiming Priority (1)

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US435889A US3914178A (en) 1974-01-23 1974-01-23 Wear reducing coating

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US3914178A true US3914178A (en) 1975-10-21

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US435889A Expired - Lifetime US3914178A (en) 1974-01-23 1974-01-23 Wear reducing coating

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US (1) US3914178A (de)
JP (1) JPS50107375A (de)
BE (1) BE824637A (de)
CA (1) CA1020783A (de)
DE (1) DE2502011A1 (de)
FR (1) FR2258557B1 (de)
GB (1) GB1480433A (de)
IT (1) IT1026422B (de)
SE (2) SE7500620L (de)

Cited By (31)

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US4023224A (en) * 1974-04-05 1977-05-17 Eaton Corporation Method for producing self-locking fasteners
US4060116A (en) * 1974-11-11 1977-11-29 Eaton Corporation Method for producing self-locking fasteners
DE2923579A1 (de) * 1979-06-11 1980-12-18 Mitrofanova Geb Zaprudskaja Antifriktionspaste
US4389462A (en) * 1981-07-08 1983-06-21 Cabot Corporation Process for enclosing a pin shank within an enclosing member and article produced thereby which is substantially devoid of a gap between the enclosing member and the head of the pin
US4634545A (en) * 1985-03-07 1987-01-06 Superior Graphite Co. Railroad track lubricant
US4746248A (en) * 1987-02-19 1988-05-24 E. I. Du Pont De Nemours And Company Anchor bolt assembly
US4825527A (en) * 1988-01-25 1989-05-02 Multifastener Corporation Method of attaching an element to a panel
US4896391A (en) * 1984-07-09 1990-01-30 Long-Lok Fasteners Corporation Method of forming a self-locking fastener
US4984938A (en) * 1988-08-25 1991-01-15 H&S Machine & Supply Company, Inc. Coated washer for an anchor bolt system
US5125686A (en) * 1989-11-16 1992-06-30 Takata Corporation Position adjusting device for a shoulder belt of a seat assembly
WO1992014939A1 (en) * 1991-02-15 1992-09-03 Paul Edward Ewing Locking fastener
US5193958A (en) * 1989-08-08 1993-03-16 Itw Ltd. Coating of screws
US5217814A (en) * 1991-02-09 1993-06-08 Taiho Kogyo Co., Ltd. Sintered sliding material
US5260100A (en) * 1989-08-08 1993-11-09 Itw. Ltd. Coating screws wtih sealant
US5328618A (en) * 1992-08-03 1994-07-12 410261 B.C. Ltd. Magnetic lubricants
US5363821A (en) * 1993-07-06 1994-11-15 Ford Motor Company Thermoset polymer/solid lubricant coating system
US20040042868A1 (en) * 2001-10-30 2004-03-04 Yake Donald L. Coated, weldable fastener, a method of preventing adherence of a second coating to a fastener portion, and a method fastening
US20060171795A1 (en) * 2005-01-28 2006-08-03 Cromwell Stephen D Substantial embedment of metallic debris
US20070140853A1 (en) * 2005-12-21 2007-06-21 General Electric Company Dovetail surface enhancement for durability
US20070243044A1 (en) * 2006-03-29 2007-10-18 Chin-Chiu Chen Wear resistant nut
US20080024909A1 (en) * 2006-07-25 2008-01-31 Kor Seng Ang Application of pfpes for hdd screw lubricant
US20090095044A1 (en) * 2001-05-22 2009-04-16 Peter Schule Method for prolonging service life of a machine for bending tubes
US20110081220A1 (en) * 2009-10-02 2011-04-07 Illinois Tool Works Inc. Fastener and method of prolonging use of a driver blade in a fastening tool
US20130183119A1 (en) * 2012-01-12 2013-07-18 Kamax Holding Gmbh & Co. Kg Screw having an underhead bearing surface including lubricant pockets
US8636124B2 (en) 2010-09-23 2014-01-28 Caterpillar Inc. Coated power rail
US20140169911A1 (en) * 2012-12-17 2014-06-19 Fuji Engineering Co., Ltd. Sealer, fastener, bolt and method of fabricating bolt
US8905335B1 (en) * 2009-06-10 2014-12-09 The United States Of America, As Represented By The Secretary Of The Navy Casting nozzle with dimensional repeatability for viscous liquid dispensing
WO2016004332A1 (en) * 2014-07-02 2016-01-07 Thermal Metal Treating, Inc. Molybdenum disulfide coated non-ferrous and ferrous materials and methods for coating the non-ferrous and ferrous materials with molybdenum disulfide
US10221880B2 (en) * 2014-08-14 2019-03-05 Sfs Intec Holding Ag Drilling screw
US20200056506A1 (en) * 2018-08-17 2020-02-20 United Technologies Corporation Gas turbine engine seal ring assembly
US10876580B2 (en) 2016-11-30 2020-12-29 Saint-Gobain Performance Plastics Pampus Gmbh Torque control system

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DE3220749C2 (de) * 1982-06-02 1984-12-06 Rommel, Erwin, 4320 Hattingen Verfahren zum Herstellen eines mit einer galvanischen Oberflächenschicht versehenen Verbindungselementes
US4468309A (en) * 1983-04-22 1984-08-28 White Engineering Corporation Method for resisting galling
GB8313646D0 (en) * 1983-05-17 1983-06-22 Boc Nowsco Ltd Screw-thread protection
US4692988A (en) * 1986-08-19 1987-09-15 Nowsco Well Service (U.K.) Limited Screw thread protection
GB2402401A (en) * 2003-06-05 2004-12-08 Halco Drilling Internat Ltd Coated pistons
DE102010021976A1 (de) 2010-05-28 2011-12-01 Schaeffler Technologies Gmbh & Co. Kg Verfahren zur Herstellung eines Lagerteils
DE202017103484U1 (de) * 2017-06-09 2018-09-13 Gea Mechanical Equipment Gmbh Schraubverbindung an einer Zentrifuge
DE202023100657U1 (de) 2023-02-10 2024-05-14 Ti Automotive (Heidelberg) Gmbh Schraubelement mit Korrosionsschutzbeschichtung

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US2122915A (en) * 1936-11-12 1938-07-05 Illinois Tool Works Thread forming fastener
US3099083A (en) * 1958-02-27 1963-07-30 Dow Chemical Co Method of suppressing bimetallic couple corrosion of magnesium metal articles
US3079338A (en) * 1959-01-26 1963-02-26 Caubet Jacques Jean Anti-friction material
US3224967A (en) * 1962-08-03 1965-12-21 Fmc Corp Bearing
US3244625A (en) * 1963-10-15 1966-04-05 Elastic Stop Nut Corp Solid film lubricant
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Cited By (44)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4023224A (en) * 1974-04-05 1977-05-17 Eaton Corporation Method for producing self-locking fasteners
US4060116A (en) * 1974-11-11 1977-11-29 Eaton Corporation Method for producing self-locking fasteners
DE2923579A1 (de) * 1979-06-11 1980-12-18 Mitrofanova Geb Zaprudskaja Antifriktionspaste
US4389462A (en) * 1981-07-08 1983-06-21 Cabot Corporation Process for enclosing a pin shank within an enclosing member and article produced thereby which is substantially devoid of a gap between the enclosing member and the head of the pin
US4896391A (en) * 1984-07-09 1990-01-30 Long-Lok Fasteners Corporation Method of forming a self-locking fastener
US4634545A (en) * 1985-03-07 1987-01-06 Superior Graphite Co. Railroad track lubricant
US4746248A (en) * 1987-02-19 1988-05-24 E. I. Du Pont De Nemours And Company Anchor bolt assembly
US4825527A (en) * 1988-01-25 1989-05-02 Multifastener Corporation Method of attaching an element to a panel
US4984938A (en) * 1988-08-25 1991-01-15 H&S Machine & Supply Company, Inc. Coated washer for an anchor bolt system
US5193958A (en) * 1989-08-08 1993-03-16 Itw Ltd. Coating of screws
US5260100A (en) * 1989-08-08 1993-11-09 Itw. Ltd. Coating screws wtih sealant
US5125686A (en) * 1989-11-16 1992-06-30 Takata Corporation Position adjusting device for a shoulder belt of a seat assembly
US5217814A (en) * 1991-02-09 1993-06-08 Taiho Kogyo Co., Ltd. Sintered sliding material
WO1992014939A1 (en) * 1991-02-15 1992-09-03 Paul Edward Ewing Locking fastener
US5190423A (en) * 1991-02-15 1993-03-02 Ewing Paul E Locking fastener
US5314279A (en) * 1991-02-15 1994-05-24 Ewing Paul E Locking fastener
US5328618A (en) * 1992-08-03 1994-07-12 410261 B.C. Ltd. Magnetic lubricants
US5363821A (en) * 1993-07-06 1994-11-15 Ford Motor Company Thermoset polymer/solid lubricant coating system
US20090095044A1 (en) * 2001-05-22 2009-04-16 Peter Schule Method for prolonging service life of a machine for bending tubes
US20040042868A1 (en) * 2001-10-30 2004-03-04 Yake Donald L. Coated, weldable fastener, a method of preventing adherence of a second coating to a fastener portion, and a method fastening
US20050258045A1 (en) * 2001-10-30 2005-11-24 Yake Donald L Method of preventing adherence of a second coating to a fastener portion
US7021875B2 (en) * 2001-10-30 2006-04-04 Newfrey Llc Coated, weldable fastener, a method of preventing adherence of a second coating to a fastener portion, and a method fastening
US20060159544A1 (en) * 2001-10-30 2006-07-20 Yake Donald L Coated, weldable fastener, a method of preventing adherence of a second coating to a fastener portion, and a method fastening
US7594985B2 (en) 2001-10-30 2009-09-29 Newfrey Llc Method of preventing adherence of a second coating to a fastener portion
US7255521B2 (en) 2001-10-30 2007-08-14 Newfrey Llc Coated, weldable fastener, a method of preventing adherence of a second coating to a fastener portion, and a method fastening
US20060171795A1 (en) * 2005-01-28 2006-08-03 Cromwell Stephen D Substantial embedment of metallic debris
US7516547B2 (en) 2005-12-21 2009-04-14 General Electric Company Dovetail surface enhancement for durability
US20070140853A1 (en) * 2005-12-21 2007-06-21 General Electric Company Dovetail surface enhancement for durability
US20070243044A1 (en) * 2006-03-29 2007-10-18 Chin-Chiu Chen Wear resistant nut
US7729082B2 (en) 2006-07-25 2010-06-01 Hitachi Global Storage Technologies Netherlands B.V. Application of PFPES for HDD screw lubricant
US20080024909A1 (en) * 2006-07-25 2008-01-31 Kor Seng Ang Application of pfpes for hdd screw lubricant
US8905335B1 (en) * 2009-06-10 2014-12-09 The United States Of America, As Represented By The Secretary Of The Navy Casting nozzle with dimensional repeatability for viscous liquid dispensing
US20110081220A1 (en) * 2009-10-02 2011-04-07 Illinois Tool Works Inc. Fastener and method of prolonging use of a driver blade in a fastening tool
US8636124B2 (en) 2010-09-23 2014-01-28 Caterpillar Inc. Coated power rail
US20130183119A1 (en) * 2012-01-12 2013-07-18 Kamax Holding Gmbh & Co. Kg Screw having an underhead bearing surface including lubricant pockets
US8784030B2 (en) * 2012-01-12 2014-07-22 Kamax Holding Gmbh & Co. Kg Screw having an underhead bearing surface including lubricant pockets
US20140169911A1 (en) * 2012-12-17 2014-06-19 Fuji Engineering Co., Ltd. Sealer, fastener, bolt and method of fabricating bolt
US8944735B2 (en) * 2012-12-17 2015-02-03 Fuji Engineering Co., Ltd. Sealer, fastener, bolt and method of fabricating bolt
WO2016004332A1 (en) * 2014-07-02 2016-01-07 Thermal Metal Treating, Inc. Molybdenum disulfide coated non-ferrous and ferrous materials and methods for coating the non-ferrous and ferrous materials with molybdenum disulfide
US9828563B2 (en) 2014-07-02 2017-11-28 Thermal Metal Treating, Inc. Molybdenum disulfide coated non-ferrous and ferrous materials and methods for coating the non-ferrous and ferrous materials with molybdenum disulfide
US10221880B2 (en) * 2014-08-14 2019-03-05 Sfs Intec Holding Ag Drilling screw
US10876580B2 (en) 2016-11-30 2020-12-29 Saint-Gobain Performance Plastics Pampus Gmbh Torque control system
US20200056506A1 (en) * 2018-08-17 2020-02-20 United Technologies Corporation Gas turbine engine seal ring assembly
US10920617B2 (en) * 2018-08-17 2021-02-16 Raytheon Technologies Corporation Gas turbine engine seal ring assembly

Also Published As

Publication number Publication date
FR2258557B1 (de) 1980-06-27
JPS50107375A (de) 1975-08-23
DE2502011A1 (de) 1975-07-24
FR2258557A1 (de) 1975-08-18
CA1020783A (en) 1977-11-15
IT1026422B (it) 1978-09-20
SE7907002L (sv) 1979-08-22
SE7500620L (de) 1975-07-24
GB1480433A (en) 1977-07-20
BE824637A (fr) 1975-07-22

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