QUARTERLY PROGRESS REPORT ON

TRIBOPOLYMERlZATlON AS AN ANTI-WEAR MECHANISM

for the

Energy-Related Inventions Program

Recommendation Number 584 Grant No. DE-FGO1-95-EE-15584

U.S. Department of Energy Washing ton

Washing, DC 20585

submitted by

Dr. Michael J. Furey Principal Investigator

Department of Mechanical Engineering Virginia Polytechnic Institute and State University

Blacksburg, Virginia 24061 -0238

for the period

July, August, September 1996

October 9, 1996

TER

DISCLAIMER

This repon was prepared as an accaunt of work qmsorcd by an agency of the United States Government Ndthcr the Unitai Statrs Gmrrnmcnt nor aoy agency thereof. nor m y of their cmpioyecs. makes any warranty, expresr or impiied or rrtuma any legal liability or rcspoatibiiity for the accuracy. compictcncrr or w- fulam of any information, apparatus, produa, or prooar d i r d d or rrprrsenu that its use would not infringe privatdy owaed righu Referrncc h a m to any sp- cific c o m m d produn. procc~s or service by trade nunc. mdanark tnanufac- turn. or otherwise doer not n-iy d u n e or imply its eadorwment rrcom- mendation. or favoring by the United States Govanment or my agency thereof. The views and Opinions of authors cxprcwd hat in do not n d y ~ t c or reflect thox of the United States G0vem-t or any agency thereof.

DISCLAIMER

Portions of this document may be illegible in electronic image products. Images are produced from the best available original document.

SITE VISIT

On August 23, 1996, a site visit to Virginia Tech was made by Ms. Amy Manheim and Mr. Fred Hart, Invention Coordinators of the Department of Energy’s Energy- Related Inventions Program. A presentation was made by Dr. Michael Furey, Principal Investigator. Others present consisted of Dr. Czeslaw Kajdas, Co- Investigator, Mr. Jeff Valentino, Graduate Student, and Mr. Karl Kaltenbach of Triad Investors, Inc. Comprehensive handout material in bound form was provided. Since this site visit included progress made during the first half of the July-August-September quarter, a copy of the major conclusions presented is attached . SUBSEQUENT PROGRESS

During the second half of that quarterly period, we have made progress in a number of areas -- many of which were discussed under future plans during the site visit. These are summarized below.

1.

2.

3.

4.

5.

We have continued to evaluate potential candidates for high load/high speed antiwear action using the approach of generating tribopolyrners capable of withstanding high temperatures. Results are promising for ceramics as well as steel.

The construction of a new instrument for high temperature studies of both liquid and vapor phase lubrication is almost complete. This will permit studies up to 350°C bulk temperature and considerably higher surface temperatures in controlled vapor-phase and liquid-phase studies. The new device will be equipped with a microprocessor unit for controlling speed, temperature, etc. and for data acquisition.

Selected monomers and monomer combinations found to be effective in hexadecane as a carrier fluid have also been tested in other fluids, including synthetic ester lubricant carriers. This is continuing.

Additional studies using FTIRM for surface analysis of wear tracks have been made and are continuing.

Further industrial contacts have been made to arrange for field testing of selected compounds as antiwear additives. The applications include the lubrication of 2-stroke and 4stroke engines, machining and cutting, and fuel injector wear, particularly in gas (e.g., natural gas) engines.

J e n

' REQUEST FOR EXTENSION

As discussed with both Ms. Manheim and Mr. Hart during the site visit, a request for a no-cost time extension of 8 months -- extending the end date from October 24, 1996 to June 24, 1997 was made by e-mail on August 23, 1996.

Such an extension would permit us to complete the items listed under the Future Plans part of our handout and maximize the benefits of this research at no additional cost the DOE.

MAJOR CONCLUSIONS

0

0

0

0

0

A high loadlhigh speed, pin-on-disk machine has been developed and used for studies of tribopoly-merization at high levels of frictional energy.

Systems investigated included ceramic-on- ceramic and steel-on-steel.

Six monomers developed previously are very effective in reducing ceramic wear at moderate levels of frictional heat generation but are ineffective at higher speeds. Most of these are vinyl-type addition monomers (e.g., diallyl phthalate, lauryl methacrylate).

However, new classes of monomers designed for higher temperature applications were found to be effective at high loads and speeds. These consisted of condensation-type monomers containing aromatic ring structures or polyamide-formers

An outstanding example of the latter is E-

caprolactam - found to reduce wear at low concentrations by over 98% for both steel and alumina systems.

t

MAJOR CONCLUSIONS (Cont.)

Examination of the worn surfaces by SEM and FTIRM shows evidence of complex film formation, including surface reactions and polymerization.

Exploratory tests in another pin-on-disk system demonstrate that vinyl-type addition monomers are effective in reducing ceramic wear in the vapor phase (Le., nitrogen carrier gas), with increased wear protection at higher temperatures.

One patent on ceramic lubrication was issued in 3995. Three patent applications based on the concept of tribopolymeriration were filed in early 1996.

An agreement was made among Virgina Tech Intellectual Properties, the Office of Sponsored Research, and Triad Investors Corporation to fund additional projects aimed at getting advances in this technology into the market place.

Three Triad-sponsored projects were initiated in early 1996 - projects dealing with (I) lubrication of two-stroke engines, (2) machining and cutting applications, and (3) vapor-phase lubrication.

4

MAJOR CONCLUSIONS (Cont.)

Together with Triad, industrial connections have been and are being explored. These include Tecumseh Engines in Michigan and Wisconsin, and Siemens Automotive in Newport News, Virginia. Other companies - including engine manufacturers and lubricantladditive companies - are being contacted.

The use of Or. Brian Vick’s surface temperature calculation approach has been helpful in examining the role of temperature on the process of tribopolymerization and other thermal effects (e.g., polymer degradation).

Exploratory work on the use of chemical modeling software (CHEM-X) to predict the orientation of monomer molecules on solid substrates (e.g., ceramics) shows promise.

As a result of this research, we have expanded our knowledge of the potential uses of tri bopolymerization under more severe conditions of high loads and speeds. This information will be helpful in selecting compounds for specific industrial applications.

MAJOR CONCLUSIONS (Cont.)

However, we need the capability of carrying out tribological tests in a controlled liquid or vapor environment and at higher temperatures. Such a device has been designed and is now being constructed. It will be a valuable and critical tool for all our present and future studies of tribopolymerization as an effective anti-wear mechanism for ceramics as well as metals.