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Uilitgd States Patent [19] [11] Patent Number: 4,647,386 Jamison [45] Date of Patent: Mar

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Uilitgd States Patent [19] [11] Patent Number: 4,647,386 Jamison [45] Date of Patent: Mar UIlItGd States Patent [19] [11] Patent Number: 4,647,386 Jamison [45] Date of Patent: Mar. 3, 1987 [54] INTERCALATED TRANSITION METAL Attorney, Agent, or Firm-—Robert E. Harris BASED SOLID LUBRICATING COMPOSITION AND METHOD OF SO [57] ABSTRACT , FORMING A solid lubricating composition and method for form ing such a composition are disclosed. The composition [76] Inventor: Warren E. Jamison, 528 Parkview Ave., Golden, Colo. 80401 is formed by intercalating a transition metal that has been chemically reacted with chalcogen to form a lay [21] App]. No.: 538,137 ered structure. The transition metal is selected from [22] Filed: Oct. 3, 1983 niobium, tantalum, tungsten and/or an alloy including one or more, and the transition metal is chemically [51] Int. Cl.4 ......................................... .. C10M 125/22 combined with chalcogen selected from sulfur, sele [52] US. Cl. ...................... .. 252/25; 423/561 R nium and/or a combination which can also include [5 8] Field of Search ..................... .. 252/25; 423/561 R tellurium to form a layered transition metal dischal [56] References Cited cogenide prior to intercalation with a metal, preferably U.S. PATENT DOCUMENTS a coinage metal. The effect of intercalation is to expand the crystal lattice to create a composition having excel 3,573,204 3/1971 Van Wyk ............................ .. 252/12 Thompson 252/12 lent lubricating characteristics the performance of 3,763,043 10/1973 which is not adversely effected by operation in a high 3,769,210 10/1973 Cais et a1. ........ .. 252/25 4,040,917 8/1977 Whittingham . .. 204/36 temperature environment. 4,094,893 6/ 1978 Dines .................................. .. 252/25 Primary Examiner——.lacqueline V. Howard 16 Claims, 5 Drawing Figures US. Patent Mar. 3, 1987 Sheet 1 of2 4,647,386 e A A ' I o '9 T7/.2. / ..._..V,/M.,/V : US. Patent _Mar.3, 1987 Sheet 20f2 4,647,386 O55 3.3I.l.2O 0 _O Z w FZEQInEOQ02.2mm A1H I I I l I I I00 I50 200 250 300 350 TEMPERATURE,(°C) Fig. i 3 N .0 aw. K6:. PZHQFEMOU202.21“ S6l2. .________O la.069 l5.0 I4. l6. l7. 15 I9. mnm‘mmmmmwm X in AX NbSez Fig. 4 Ago.33 NbSSe Agoasms 1.55605 AgasaNbsz' Flg' 5 FRICTKSN COEFFICQIENT 4,647,386 1 2 gears. Therefore, these powders are normally used in INTERCALATED TRANSITION METAL BASED combination with binders which bond them to surfaces SOLID LUBRICATING COMPOSITION AND or are used in combination with a structural material to METHOD OF SO FORMING form self-lubricating solids. While solid lubricants have heretofore been sug Government Rights gested and/or utilized, particularly where liquid lubri The Government has rights in this invention pursuant cants could not be satisfactorily utilized, such solid to Contract No. F336l5-78C-5l96 awarded by the De lubricants have nevertheless not been found to be satis partment of Air Force. factory, at least for some applications, and better solid lubricating compositions have therefore still been FIELD OF THE INVENTION needed. This invention relates to a solid lubricating composi tion and method for forming such a composition, and, SUMMARY OF THE ‘INVENTION more particularly, relates to an intercalated transition This invention provides an improved solid lubricat metal based solid lubricating composition and method ing composition that is particuarly useful in hostile envi for so forming. ronments such as is presented under high temperature BACKGROUND OF THE INVENTION conditions. The lubricating composition is formed from a transition metal that has been chemically combined Liquid lubricants are well known and such lubricants with a chalcogen to form a layered transition metal have been, and are now, successfully used for many dichalcogenide (LTMD), and then intercalated with a diverse purposes. Liquid lubricants have not, however, metal to cause expansion of the crystal lattice. proved to be satisfactory for some uses, including, for It is therefore an object of this invention to provide example, use in high temperature environments where an improved solid lubricating composition. combustion or pyrolysis of conventional liquid lubri It is another object of this invention to provide an cants would occur, at extremely low temperatures improved solid lubricating composition useful in hostile where conventional liquid lubricants would freeze or gel, and/or in highly oxidizing environments where environments such as under high temperature condi conventional liquid lubricants would present an explo tions. It is still another object of this invention to provide an sion hazard. For such uses, the powders of crystalline solids have 30 improved solid lubricating composition that is an inter long been used as lubricants, and, more speci?cally, calated transition metal based solid lubricating composi powdered graphite has long been used in industry as a tion. lubricant for use in hostile environments in which oils It is still another object of this invention to provide an and greases are forbidden. improved solid lubricating composition formed by In its natural state, graphite absorbs moisture from 35 chemically reacting a transition based metal with a the atmosphere and this moisture is essential to the chalcogen to form a layered transition metal dichal graphite functioning as a lubricant. If graphite is ex cogenide, and then intercalating the layered transition posed to a vacuum for extended periods however, the metal dichalcogenide with a metal to cause expansion of moisture is lost and the graphite becomes abrasive. To the crystal lattice. overcome this problem, graphite lubricating composi It is still another object of this invention to provide an tions, including iodine and other moisture substitutes, improved method for forming a solid lubricating com have heretofore been developed for speci?c applica position. tions. It is yet another object of this invention to provide an Molybdenum disul?de (M052), a natural material, has improved method for forming a solid lubricating com properties similar to those of graphite but does not 45 position by reacting a transition metal with chalcogen require moisture for good lubricating performance. For to form a dichalcogenide and then intercalating the this reason, molybdenum disul?de has more recently dichalcogenide. been used in the aerospace industry as a lubricant for With these and other objects in view, which will satellites and space vehicles and in other areas where become apparent to one skilled in the art as the descrip oils and greases are forbidden or dif?cult to employ, 50 tion proceeds, this invention resides in the novel con such as, for example, in self-lubricating bearings and struction, combination, arrangement of parts and food processing machinery. In addition, molybdenum method substantially as hereinafter described and more disul?de has also been utilized as an additive to oils and particularly de?ned by the appended claims, it being greases to improve their performance at extremely high understood that changes in the precise embodiment of loads. 55 In attempting to improve the lubricating effectiveness the herein disclosed invention are meant to be included of solid lubricants for space applications, it was empiri as come within the scope of the claims. » cally found that mixtures of silver, antimony oxide and BRIEF DESCRIPTION OF THE DRAWINGS molybdenum disul?de exhibited superior lubricating performance to molybdenum disul?de alone. Subse The accompanying drawings, together with the spec quently, it was found that other metal disul?des and i?cation, illustrate a complete embodiment of the inven diselenides, including tungsten disul?de (W52), molyb tion according to the best mode so far devised for the denum diselenide (M0862), and tungsten diselenide practical application of the principles thereof, and in_ (W Seg) are good solid lubricants. _ which: These materials are usually found in the form of pow 65 FIG. 1 is a representation of a stacked layered con ders, however, which are dif?cult to use as lubricants struction of graphite; for at least some applications, including, for example, FIG. 2 is a representation of a stacked layered con rolling bearings and mechanical components such as struction of molybdenum sul?de; 4,647,386 3 4 FIG. 3 is a graph showing friction coef?cient versus tent should not exceed ?fty atomic percent of the total temperature for selected solid lubricants; chalcogen content. FIG. 4 is a plot of friction coef?cients versus silver The transition metals (T) and chalcogens (X) are concentration in AXNbSeZ; and chemically reacted to produce a dichalcogenide (TXZ) FIG. 5 is a bar graph showing room temperature with a layered structure similar to that shown in FIG. 2 friction coef?cients for AgXNbSySeZ.y and related mate for molybdenum disul?de. This is effected by mixing rials. powders of the elements and sealing them in evacuated DESCRIPTION OF THE INVENTION vials, which are heated to temperatures above 850° C. for at least 24 hours and then slowly cooled to room Graphite is composed exclusively of carbon atoms temperature. Alternate preparation procedures include which are bonded together in two dimensional hexago passing hydrogen disul?de gas over powders of the nal arrays. Layers consisting of planar arrays of carbon metals at high temperatures and other procedures atoms are stacked, as shown in FIG. 1. The chemical known to persons skilled in the art. bonds within the layers are strong, while the bonds The transition metal dichalcogenides (TX2) are fur which hold the layers together are weak, allowing one ther reacted with a metal which can intercalate the layer to easily slide over another and this enables graph structure of the TX; compound to cause an expansion of ite to be effectively used as a lubricant. the crystal lattice. Metals that can be utilized are cop Molybdenum disul?de has a similar layered structure, per, silver, gold, germanium, bismuth, lead, indium and as shown in FIG. 2, in which hexagonal arrays of mo gallium with the coinage metals copper, silver and gold lybdenum atoms are sandwiched between hexagonal being preferred.
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