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Rock IsIhod Arseo&j' j Laboratory

TECHNICAL REPORT

WTEAR AND CORROSION TENDENCIES OFMOLYBDENUM DISULFIDE CONTAINING GREASES

S. Fred Calhoun

Departinent of the Army Project No. 593-21-060

Ordnance Management Structure Code No. 5010.11.801

Report No. 62-2752 Copy- No_

IEL 1-8-107-2 Dat6 15 August 1962

DISTRIBUTED BY TIHE T11I1 REPORT MAY BE DESTROYED WHENOFFICE OF TECHNICAL SERVICES NO LONGER REQUIRED FOR REFERENCEU. S. DEPARTUME.NT OF COMMiERCEWASHINGTON 25, D, C.

Report No. 62-2752

Copy No.

WEAR AND CORROSION TENDENCIES OFMOLYBDENUM DISULFIDE CONTAINING GREASES

,/

By

S. Fred Calhoun

Approved by:

A. C. HANSONLaboratoiy Director

15 August 1962

Department of the Army ProjectNo. 593-21-060Ordnance Management Structure CodeNo. 5010.11.801

Rock Island ArsenalRock Island, Illinois

ASTIA Availability Notice;

Qualified requesters may obtaincopies of this report from ASTIA.

ABSTRACT

The tendency of molybdenum disulfide to increase the wearof greases is shown by results of laboratory tests made atRock Island Arsenal. The extreme pressure properties ofgreases were iLereased by the additiou of the rnolybdenuta di-sulfide. Both statements are supported by the literature.

Molybdenum disulfide was shown to promote rusting offerrous metals when added to grease. Literature referencesshow that it also promotes corrosion of other metals.

Laboratory d!at - ;h: A tconclusions which were made.

1 62-2752

RECOIDONDAT IONS

It is recommended that molybdenum disulfide not be usedin greases designed for automotive and artillery use by theArmed Forces. If an extreme pressure grease is needed, it isrecomm~ended that extreme pressure agents other than molyb-denum disulfide be specified.

CONCLUSIONS

Holybdenun disulfide, when incorporated into a grease,is detrimental to the weag preventive properties of thegrease. This was true for all types of greases tested orreferred to in the literature. The compound does contributeto the extreme pressure properties of most greases when usedunder conditions of high pressure and temperature. It isprobable that the extreme pressure properties of molybdenumdisulfide became apparent under conditions approachingboundary lubrication when the grease or oil is forced frombetween the rubbing surfaces by the pressure exerted. It isdoubtful if such conditions are prevalent for any appreciabletime during normal automotive or artillery use.

Molybdenum disulfide, when incorporated into greases,increases the corrosive tendencies of the grease. This wastrue for all greases investigated by this-Laboratory. Thisis caused by the formation of corrosive products throughhydrolysis and by galvanic action between the molybdenumdisulfide and metals. Extreme conditions of moisture acceler-ate this corrosive action which has been observed with manymetals, Certain additives incorporated into the molybdenumdisulfide grease will reduce or even eliminate the corrosion.

In view of the above mentioned tendencies, it isdoubtful if the extra cost of molybdenum disulfide greasescan be Justified. A good grease is able to meet all theextreme pressure needs of normal automotive and artilleryuse without being fortified with molybdenum disulfide. Ifextreme pressure conditions exist, there are many compoundswhich will enable a grease to meet them and at the sametime not reduce its ability to protect against rust andcorrosion.

The quality of the MoS 2 is an important factor in itsultimate performance. When it is to be added to greases,careful and strict control of its purity, particle size, andpH is imperative.

ii 62-2752

WEAR AND CORROSION TENDENCIES OFMOLYBDENUM DISULFIDE CONTAINING GREASES

CONTENTS

Page No.

Object 1

Introdu.ction 1

Procedure and Observations 4

Discussion 10

Literature References 16

Distribution 18

iii 62-2752

WEAR AND CORROSION TENDENCIES OFMOLYBDEINUM DISULFIDE CONTAINING GREASES

OBJECT

To study the effects of the addition of molybdenum di-sulfide upon the wear, extreme pressure properties, andcorrosion resistance of greases.

INTRODUCTION

The recent trend to extended lubrication periods in auto-mobiles, and the insistance of the manufacturers tnat onlytheir specification greases be used, has created a problemfor the Armed Forces. For the past several years, greasesmeeting Specification MIL-G-10924 have been in general use byall branches of the Armed Services-for lubrication of automo-tive and'artillery equipment. Such greases have been gener-ally satisfactory and have greatly reduced logistic problems.If the Armed Services are to use the manufacturers specifiedgreases, a minimum of six different greases would have to bestocked in order to lubricate the various makes of automobilesfound in the services. Since different grease fittings areused for each grease, a separate grease gun equipped with aspecial fitting is practically necessary for each type ofgrease. The immensity of the supply problem is thus apparent.

Another factor in the problem is the increasing tendencyto specify greases containing molybdenum disulfide for use inthe automobiles. This is no doubt largely due to the vigor-ous manner in which the suppliers of MoS2 have pushed theirproduct. They have carried out a research and advertisingprogram designed to show their product in its best light.The relatively meager literature on work done by unbiased re-searchers does not substantiate the findings of the producers.Work done at this Laboratory also indicates that MoS 2 fallssomewhat short of the claims made for it.

Some of the properties stressed in the advertising andother sales promotional literature is the ability of MOS 2 toprevent galling and seizure, and to reduce friction and wearwhen added to greases or other lubricants, Kullman used aspecially purified MoS 2 in a lithium base grease and obtainedthe following results, Under high pressure (heavy duty)conditions the MoS 2 apparently plates out on the metal surfaceand provides "safety" lubrication for short intervals duringwhich the grease may fail to function. At low operating loads,the same effect could not be obtained either by prolongedrunning times or by increasing the operating temperatures.

1 62-2752

A Russian team(2), in determining the coefficients offriction, durability of the film, and antiseize properties ofMOS2 , concluded that as a lubricant it was "not as effectiveas some literature data would indicate?.

Halter and associates( 3 ) made a study of MOS 2 sliding onMoS 2 in a nitrogen atmosphere containing various amounts ofwater vapor and certain hydrocarbon gas vapors. In testswith water vapor they observed an increase in coefficient offriction as the humidity increased° In dry nitrogen the co-eficienet of friction wao 0.115. In an atmosphere nontaining8-16 mm partial pressure of water vapor it rose to 0.21L Itrose .u i auaixtnu of 0,24 at 20 mm partlnl! pressure of watervapor, They also report that when the partial pressure ofwater vapor exceeded 10 mm, hydrogen sulfide was detected inthe test chamber exit gas.

Peterson and Johnson(4) studied the coefficients offriction and wear characteristics of 27 crystalline solids.They observed that the lubricative effect of McS 2 was im-paibed by moisture, They alsc stated that the ability of asolid to form an adherent film on a metal was more importantthan,•jystal structure in determining lubricating ability°They. obtained galling and seizure type failures when theyattempted to determine the coefficients of friction oftitanium surfaces coated with MoS 2 0

Horth and asscciates(6', in a study of greases for balljoint suspensions; fcund that the bes• one was a soft greasemade from a low viscosity oil. They found that the additionof MoS 2 to a lithium-calcium soap grease was detrimentalboth from the standpoint of friction, as observed in steeringtorque, and wear,

Smith(7), in his paper, lists a large amount of datawhich in the main indicates MoS 2 to be a good extremepressure agent and to produce good film life. There aresome cases, especially with high viscosity oils and w+thhigh soap content, where the MCS2 was detrimental, He usedthe Timken and Falex machines in what are primarily boundaryand extreme pressure conditions,

Kay(B;9) studied the frictional pioperties of MoS2 andmade the following observations:

1. The values of the ccefficients of friction of MOS 2films rubbed onto various metals is very dependent upontemperature and humidity,

2 62-2752

2. In an investigation of a series of greases using theNavy Gear Wear Tester with various gear combinations, it wasobserved that for all metal combinations used the greasescontaining 10% MoS 2 gave greater wear than the base greaseitself.

3. In tests made on the Four Ball machine using ballsof ball bearing steel it was observed that at the lowest load(20 Kg.) the addition of MoS2 to a grease resulted in de-terioration of performance. With loads of 40 Kg. there wasno appreciable difference in performance while at higherloads tho prosence of MoS 2 results in improved performancte

Another import&aut £actoi, in the use of molybdenum di-sulfide containing greases is the tendency of the compound topromote rusting or corrosion of various metal surfaces. Thiswas first noticed by this Laboratory during the developmentof dry lubricants. Tý1 pyrlem has been partially solved bysurface pretreatments 1 . Further improvement in rustpreventive properties have been obtained by use of acidacceptors incorporated into the dry lubricant formulation.

The manufacturers of commercial dry lubricant formu-lations are rather quiet concerning the corrosion preventiveproperties of their products. Some typical statements takenfrom the brochures of various companies include, "no acceler-ation of corrosion of 2024 aluminum alloy anodized as perMIL-A-8625, Type I"; "noncorrosive to any bearing metal";and "Resistant to water". In some cases they are mon frankabout it. A news item concerning one such lubricanto2states; " , does not give corrosion protection".Weisman (13), in speaking before the Air Force-Navy-IndustryConference in San Antonio, Texas in 195%, states bluntly,"In my opinion, dry film lubricants have no rust preventiveproper ties".

Picatinny Arsenal( 1 4 ) conducted a study to evaluate theuse of molybdenum disulfide in munitions parts and came tothe following conclusions.

1. Molybdenum disulfide accelerates galvanic corrosionwhen placed in contact with various metals in moist atmos-pheres,

2. The quality of the molybdenum disulfide contributessignificantly to the extent and rapidity of this deteri-oration.

3. Molybdenum disulfide will accelerate the deteri-oration of cadmium at high humidities.

3 62-2752

4. The use of existing Specification, MIL-M,-7866, doesnot insure the application of material capable of long termopen storage without deleterious effects.

5. Molybdenum disulfide, in the presence of moisture,will act as the cathode to several metals to ±or=a a galvaniccell generating potential differences of as much as 0.5 volt.This is sufficient to cause severe and rapid corrosion.

In view of these observations it is evident that MoS 2would contribute nothing to the rust preventive properties ofa grease but might in fact accelerate corrosion.

Erb(15), in a studfy ofZantis& formulations, list-,the properties of sixty-one different resin or elastomerbased mixtures. His results show that in thirty-nine caseswhere MoS2 was included in the formulation all except thosecontaining a corrosion inhibitor allowed the panel to showdeep pitting or a badly rusted surface at the conclusion ofthe 200 hour salt spray test, Addition of a corrosion in-hibitor merely reduced the severity of the rust and in nocase eliminated it. In the 100 hour humidity cabinet testthe only formulations allowing rust to form were, with buttwo exceptions, those containing MoS 2 ,

PROCEDURE AND OBSERVATIONS

This Laboratory has on several occasions observed theshort comings of molybdenum disulfide as an additive forgreases. The following data from Table 5 of a publishedreport(16) is illustrative of the usual observations. Theadditive #21 is molybdenum disulfide. The Four Ball Wearscars for both the 3% and 5% molybdenum disulfide concen-trations are larger than for the base grease except forcondition #3. This is a high load, high temperature condi-tion that could well be termed an expreme pressure condition.The Mean Hertz load and welding loads are improved by theMoS 2 , but the Falex and Timken results are not significantlybettered. Based on these, and similar results, this Arsenalhas concluded that a minimum of 5% MoS 2 must be used toachieve any significant improvement in extreme pressure pro-perties. Table I contains the pertinent data from thereferenced report to support the observations made.

4 62-2752

I-c-

E-41--

00

o to

&0

10 z

100

a.C

5 62- 2752

The data in Table II and Ta•i III is taken from an un-published report of this Arsenal ). Table I1 contains FourBall Wear test results on three greases. They are: aqualified MIL-G-10924A grease both before and after additionof 5% of microsize MoS2 and a comnercial lithium soap greasewhich analyzed 3% molybdenum disulfide. Table II containsthe wear results under the stated conditions.

TABLE II

FOUR BALL WEAR RESULTS, SCAR DIAMET-R,

CommercialLithium Soap

MIL-G-10924A MIL-G-10924A Grease -Conditions Grease + 5% MoS2 3% MoS2

28 Kgm, 600 rpm1 10 0 0M. 0.35 0.35 0.46100OF 60 Min.'

2 28 Kgrm, 600 rpm 0.40 0.37 0.56250oF 60 Min.

Table III contains the results of the Four Ball ExtremePressure tests on the same greases.

TABLE III

FOUR BALL EXTREME PRESSURE RESULTS

CommercialLithium Soap

MIL-G-10924A MIL-G-10924A Grease -

Grease +5% MoS 2 3% MoS2

Mean Hertz Load, Kg. 23.9 48o8 42.5

Welding Load, Kg. 160 315 200

Seizure Range, Kg. 44-68 80-100 100-126

6 62-2752

The data in Table I1 indicates further what seems to bea trend. Molybdenum disulfide usually does not improve theantiwear properties of a grease but in fact quite oftenworsens it.

Table III confirms the data in Table I that the extremepressure properties are usually improved by addition of MoS2.It is also rather indicative that at least 5% of MOS2 is re-quired to produce significant results.

Table IV contains the kesults of wear and extremepressure tests on four commercial specification greases re-commended by the manufacturer for lubricating the 1961 and1962 automobiles with extended lubrication periods.

TABLE IV

WEAR AND EXTREME PRESSURE RESULTS,ON GREASES FOR USE ON NEW CARS,

Shell Four BallWear at 40 Kg.,1200 RPM, 75 0 C Welding60 minutes Mean Hertz Load,

Grease Scar Diam., MM Load, KYg. Kg.

E.P. Lithium 0.38 30 200

Moly F.P. Lithium 0.39 31.1 200

Barium 0.48 27.9 160

Barium + 10% Moly 0.66 59.0 400

It is readily apparent that the MoS 2 did not improve theextreme pressure lithium grease in either wear or extremepressure properties. It is quite possible that a grease withbuilt in extreme pressure is not helped by the MoS 2 . Theaddition of 10% MoS 2 to the barium grease was definitely de-trimental to its antiwear properties, but enhanced the ex-treme pressure qualities appreciably.

7 62-2752

The corrosive tendencies of molybdenum disulfide con-taining greases have been observed in this Laboratory in thefollowing described manner:

A qualified MIL-G-10924A grease was selected and foundto have a neutralization number of 0.78 alkaline. Five per-cent by weight of dry microfine molybdenum disulfide was thenmixed into the grease. One hour after mixing the neutrali-zation number was determined to be 0.59 alkaline, The greasewas then stored for eight days at ambient conditions oftemperature and humidity. The neutralization number was thenfound to be 0.39 alkaline, The grease we,s then placed in adesiccator over water for eight days after which the neutrali-zation number was acid, This confirms the findings ofPicatinny Arsenal , and also reported personally by otherinvestigators, that MoS 2 hydrolyzes in the presence ofmoisture to form acid products which could be quite corrosiveto metals.

To further investigate the corrosive tendencies of MoS2in greases, the following tests were performed, SpecificationMIL-G-10924A contains a requirement that the greases protecta steel panel for 100 hours in a salt spray of specifiedcomposition. Two qualified greases were each mixed with 5%MoS2 and the right hand side of a steel panel coated withthe MoS 2 containing grease. The left hand side of each panelwas coated with the grease containing no MoS2. The conditionof the panels after 24 hours in the salt spray is shown pic-torially in Figure 1A and 1B. In both cases the side coatedwith the grease containing the MoS2 had rusted severely whilethe side coated with the original MIL-G-10924A grease wasfree of rust.

In another test a similar steel panel had MOS2 powderrubbed onto the right hand side by means of clean tissuepaper. The left hand side was left bare, The condition ofthe panel after only one hour in the salt spray is shown inFigure 1C. The heavier rust on the right hand side isclearly evident.

Another panel was coated with a commercial MoS 2 grease.The rusted condition of this panel after 24 hours in the saltspray is shown in Figure ID,

Another rust preventive test which has risen in favorrecently and is included in Specificaticn MIL-G-10924B isFederal Standard No. 4012. This test involves coating abearing with the grease under specified conditions and thenkeeping it in a moist atmosphere in a sealed jar for fourteendays. A good grease will prevent any rust forming on either

8 62-2752

S....i A,

-lid

r~'C

j i

A B

C D

CONDITION OF PANELS AFTER SALT SPRAY TEST

FIGURE 1 9 62-2752

the race or the rollers of the bearing. Figure 2 shows theresults when an acceptable MIL-G-10924B grease was testedwithout and also with 5% of MoS2 mixed into it. The rustingdue to the MoS 2 is clearly evident.

Figure 3 shows the results obtained when the same testwas made on two commercial MOS2 greases. An acceptable MIL-G-10924B grease is included for contrast. The two MoS2greases included in this test displayed an extreme amount ofrusting which is evident from the photograph.

The results of the test on two commercial MoS 2 greasesare shown in Figure 4. These are products specified by carmanufacturers for use in late model cars with the extendedlubrication periods.

Again we see an amount of rusting which is far beyondthat which would be sanctioned by the Military.

SIn an attempt to determine if the corrosive tendenciesof MoS2 could be reduced the fQllowing investigation wasmade. One of the commercial MoS 2 greases was treated by in-corporating into it 1% of nonyl phenosyacetic acid (NPA).This compound has been found to be one of the better antirustagents in another investigationcarried out by this Laboratory.The results are shown in Figure 5. It is thus evident that aMoS 2 grease can be treated to prevent rusting. The effectsof NPA on other properties of the grease have not been fullydetermined at this time and the results obtained here are notto be construed as an unqualified recommendation for its use.

DISCUSSION

A possible explanation Of why MoS2 added to greases isineffective or harmful as a lubricant 4s found in theNational Engineering Laboratory report 1 8 ). They state:"It is known that molybdenum disulfide is effective as alubricant only if it can be bonded to the surface, and re-sults show that the presence of surface active agents suchas oleic acid is detrimental; they form their own mono layeron the surface and repel the molybdenum disulfide." Petroleumoils, and greases made from them, usually contain polar ma-terials, either natural or added, and thus would negate anyadvantage of the molybdenum disulfide.

Jost(19) mentions three catagories of application ofmolybdenum disulfide in antifriction bearings. First, whereit is harmful, second, where it gave inconclusive or con-troversial results, and third, where positive evidenceshowed some benefit. Applications where molybdenum disulfide

10 62-2752

QUALIFIED MIL-G-10924B GREASE

SAYE GREASE PLUS 5% MOLYBDENuM DISLVLFIDE

RESULTS OF FEDERAL STANDARD 4012 RUSTPREVENTIVE TEST OF GREASES

Neg.No. 3785FIGUPL5 2• ii 62-2752

C> Q

F-i

0H

r-in

Ne.o 363F IGUR 3 12 2-275

10% MOLY BARIUM

MOLY E. P. LITHIUM

RESULTS OF FEDERAL STANDARD 4012 TEST ON AUTOMOTIVE GREASES

"FIGU•RE 4 13 62-2752

CC

02o

xi0

W4+

0e .o.37

FIGURE5 14 2-275

is harmful were usually those where too great an amount ofsolid matter was introduced into the bearing. In general,the addition of more than 10% of molybdenum disulfide to agrease may lead to operating difficulties.

Applications where the use of molybdenum disulfide isinconclusive include instances where antifriction bearingsare operating under conditions where temperature and pressureare not severe and where a first class lubricant is used.The general maxim,, that, wherever conventional oils andgreases can be used, molybdenum disulfide should not be con-sidered, is true for ball and roller bearings as well as thesleeve type. The author further states that to use any molyb-denum disulfide without strict control of its purity, particlesize, pH value, carrier or bonding medium and operatingconditions is to invite failure.

Molybdenum disulfide is of value where conditions areso severe that seizure and galling are eminent. Under theseconditions a grease or an oil would be squeezed from betweenthe contacting surfaces. The presence of MOS2 thus preventsmetal to metal contact and provides lubrication during thecritical period. It should be pointed out at this point thatthere are several polar type compounds which have exhibitedextreme pressure properties equal to or superior to MoS2 andwhich are noncorrosive or to some extent corrosion preventive.

15 62-2752

LITERATURE REFERENCES

1. Kullman, Werner, G., "Effect of Molybdenum Disulfide As AHigh Pressure Additive To Bearing Grease", Erdol U. Kohl,9:380-82, June 1956.

2. Alihits, I. Ya., and Sushkima, L. N., "Molybdenum D isul-fide As A Lubricant", Issledovan Podshipnikov Skol'zheniyai Smazochn Oberud., Moscow, Sbornik, 1958, 124-45.

3. Halter, A. J., and Oliver, C. S., "Chemical AtmosphereEffects on the Frictional Behavior of Molybdenum Disul-fide", (General Electric Co., Schenectady, N.Y.),American Chemical Society, Discussion of Pet. Chem.,Preprint 3, No. 4A, 77-84 (1958).

4. Peterson, M. B., and Johnson R. L., "Factors InfluencingFriction and Wear With Solid Lubricants", Lub. Eng.11, 355-40 (1955).

5. Peterson, M. B., and Johnson, R. L., "Solid Lubricantsfor Titanium", Lub, Eng. 11,297-99 (1955).

6. Horth, A. C., Pattenden, W. C., Keller, G. F., andPanjer, L., 'Best Ball Joint Grease is Soft and Not TooViscous", SAE Journal, Page 96, September 1961.

7. Smith, E. E., "Molybdenum Disulfide As A Grease Additive",NLGI Spokesman No, 9, 20-36 (1956).

8. Kay, E., "An Investigation of the Lubricating Propertiesof Molybdenum Disulfide", Technical Note Chem. 1387.Royal Aircraft Establishment, November 1961.

9. Kay, E., "An Evaluation of Greases Using a Gear WearTester", Tech. Note Chem. 1311, Royal Aircraft Establish-ment, July 1957.

10. Meade, F. S., Murphy, G. P., "Corrosion Preventive andWear Life Properties of Phosphatized Cadmium Plated Steeland Phosphatized Zinc Plated Steni As Substrates forRIA Compound 9A"', RIA Report No. 61-710.

16 62-2752

LITERATURE REFERENCES (Cont.)

11, Meade, F. S., Murphy, G. P., "Effect on Wear Life andCorrosion Preventive Properties of Various Surface Pre-treatments Followed By Application of RIA Compound 9A",RIA Report No. 60-3179.

12. 'Sonded Lubricant Coating", Product Design and Develop-ment, Dec., 1960, page 20.

13. Weisman, M. H., "Proceedings of the Air Force-Navy-Industry Conference on Aircraft Lubricants", page 402,(1956).

14. Perna, C., '"valuation of the Use of Molybdenum Disul-fide in Contact With Cadmium in the M525AI (T336E10)PD Fuse Head Assembly", Picatinny Arsenal TechnicalReport No. DC 3-1, January 1961.

15. Erb, Robert A., "Development of An Antiseize Compound",Report No. F-A2040, Table 4, 1958, The Franklin Insti-tute, Philadelphia, Pa.

16. Calhoun, S. F., "Antiwear and E.P. Additives for Greases"ASLE Transactions, Vol. 3, No. 2, 208-214, October 1960.

17. Calhoun, S. F., "Comments on Letter and Report fromHeadquarters U. S. Continental Army Command", October 4,1961.

18. Scientific Lubrication, Vol. 13, No. 10, October 1961,page 12.

19. Jost, H. Peter, "Some Notes on the Application of Molyb-denum Disulfide to Antifriction Bearings", ScientificLubrication, Special Extra Issue, November 1958, page48-54.

17 62-2752

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