Lecture 15 Tribological Characterization

Tribology
The science and technology of interacting surfaces in relative motion: The study of lubrication, adhesion, friction, and wear between contacting surfaces

It impacts national economy of all nations and lifestyles of most people

New materials and coatings Can lower friction and reduce wear, and thus can have a positive impact on future tribological systems

Economic Impact of Tribology

Economic Losses in U.S. due to inadequate control of friction and wear Worldwide, it is estimated that 1/3 to 1/2 of worlds energy production is used to combat friction and wear (A. Z. Szeri,
Tribology: Friction, Lubrication, and Wear; Hemisphere Publishing, 1980, p.2)

Loss Material Wear Friction

Cost(b$) 100 100 70

When lost-labor, down-time, cost of replacement parts added, these figures may double. Latest Overall Estimates: $500B
P. Cummins/ORNL

Therefore, even very small improvements in energy efficiency (friction) and durability (wear) can save billions of dollars. Friction has a direct impact on environmental cleanliness as well.

Tribological Characterization: Scale of Test Methods

Mostly Simulations AFM, FFM Microtribology Machines Pin-on-disk

Atomic Scale Contacts

Molecular Debris

single asperity or nano-contact

microsystem domain engineering surfaces

cm-m
FR
M. Dugger

J. Che, et al., CalTech

fd

ATOMIC/NANOSCALE TEST METHODS

Examples of Atomic Scale Studies/Simulations

Atomic Scale Studies
Molecular Debris

single asperity or nanotribology

Multiple-asperity contact: microsystem domain

engineering surfaces

Work by Motohisa Hirano and others both theoretically simulated and experimentally demonstrated superlubricity (or frictionless sliding) between sliding pairs of Si(001) and a W (011) tip in ultra-high vacuum, (PRL, 78(1997)1448)). Also see, Socoliuc, et al., Entering a new Regime of Ultralow Friction, PRL, 92(2004)134301.
Commensurate STM of one layer of graphite Incommensurate Dry N2

~ 0.001
Dienwiebel et.al.,

2D/2D

Tribolever

PRL, 92(2004)126101

Tribological Characterization at Nanoscales

AFM Tips

Surface Characterization of Diamond Films by AFM vs SEM

AFM SEM

AFM

SEM

AFM/FFM/SFM

Position Sensitive detector

Nano Wear Tests with Carbon Overcoats

FCA N: 0 at% FCA N: 8 at% FCA N: 16 at%

Sputtering

pCVD

Load: 10 N 12 scan

FCA: Filtered Cathodic Arc

X: 0.5 m/div. Z: 20 nm/div.

Durability
Pin: Al2O3-TiC ball (2 mm) Applied load: 10 gf Sliding velocity: 0.2 m/s
Rotational pass number 10000 8000 6000 4000 2000 0 0 5 10 15 20 Carbon Thickness (nm)
pCVD Sputtering FCA

Observation of stick-slip on gold

A 5x5 nm2 atomic scale friction measurement on Au(111) at 4x10-10 Torr at room temperature. The atomic lattice of gold causes stick-slip friction to occur with the periodicity of the lattice. The inset line trace shows the clearly resolved stick-slip features for the forward and backward traces.

From R. Carpick/U. Wisconsin

Friction Force Maps

700nm x 700nm image of a few nanometer flat carbon islands on a magnetite single crystal. "Material dependend friction contrast" in the right image is due to more or less adsorbates between carbon islands (lower friction) and magnetite (higher friction). (Images taken by Stefan Mller)

Nano-to-micro Scale Test Machines

Contact Geometry

Courtesy of G. Sawyer

Nano/Macrotribology of DLC Films

0.8 0.6 0.4

friction coefficient

0.2 0

0
-0.2 -0.4 -0.6 -0.8

50

100

150

200

250

300

350

time (seconds)

Courtesy of G. Sawyer

TRIBOLOGICAL CHARACTERIZATION AT MESO/MACRO-SCALES

Tribological Characterization:
Typical contact Geometries for Macroscale Experiments

There are so many contact configurations to chose from. Each geometry is very unique and designed to simulate an application. Test conditions may vary a great deal, depending on the contact geometry. Some of them are standardized and require the certain procedures to follow.

Pin-on-disk Machines

Load
Coating

Sapphire Ball

Disk
Load: 1 - 20 N Speed: 0.3 - 1 m/s Environment: Dry Nitrogen Ball Radius:3.175 - 5 mm

Contact geometry

Operating principles

Operating Principles
In most cases, friction and wear data. Friction coefficient, = Ff / Fn (where, Fn is the normal force)

Wear rate in the ball and in the flat Friction coefficient

Wear Volume on ball: Wb=d4/64r (d:wear scar diameter, r: ball radius) Wear Rate=Wb/LN (N: Normal force; L:Sliding distance)

Other Popular Machines

Four Ball Machine Block-on-ring test machine

High-temperature Foil bearing test machine

Twin-disk rolling/sliding machine

Reciprocating Test Machine

Major Test Variables Time, Speed (rpm), Track Radius Load / Stress Material Composition (Pin/Ball & Flat) Coating Composition Test Environment (Dry, Inert, RH), Lubricant (& Additive) Composition and Rheological Properties Test Output Continuous Friction & Temperature Data

Typical Contact Geometries

Courtesy of G. Fenske

Low-Amplitude Reciprocating (Fretting) Test Machine

Issue - performance of SIDI components at higher pressures with low-lubricity fuels
Injector Wear

5.E-08 5.E-08 4.E-08 4.E-08 3.E-08 3.E-08 2.E-08 2.E-08 1.E-08 5.E-09 0.E+00
D ry

Diamonex-HT Uncoated Balzers Diamonex STD NFC-6

as G

Coating

NFC-2
E8 5 ha Et l no

Wear Rate (mm^3/N-m)

85 M

in ol e

Fuel

Courtesy of J. Hershberger

Images of Rubbing Surfaces

3D-Pin Surface 3D-Disk Surface

2D Images Of Pin Surfaces

THE RANGE OF TRIBOLOGICAL PROCESSES TO CONSIDER WHILE TESTING COATED SURFACES

MATERIAL INPUT Macromechanical GEOMETRY: Micromechanical changes Macrogeometry changes Topography Loose particles Tribochemical Fluids, environment changes PROPERTIES: Chemical composite. Microstructure Shear strength Elasticity Viscosity ENERGY INPUT Velocity Temperature Normal Load Tangential force MATERIAL OUTPUT GEOMETRY: Macrogeometry Topography Loose particles Fluids, environment PROPERTIES: Chemical composition Microstructure Shear strength Elasticity Viscosity ENERGY OUTPUT Friction Wear Velocity Temperature Dynamics
Courtesy of K. Holmberg, VTT/Finland
lon9706

Material transfer

Tribo-induced failure modes

Hogmark 01

Initial state

Coating detachment

Cracking & spalling

Coating & substrate deformation

Coating & substrate deformation + fracture

Transfer from the counterface

Gradual coating wear

Initial gradual wear + premature detachment

Coating detachment + substrate wear

Premature failure

Failure due to gradual wear

Courtesy of C. Donnet

Friction and Wear Mechanisms

Macro mechanisms

Micro mechanisms Transfer

Tribochemistry

Nano mechanisms
Holmberg 01
Courtesy of C. Donnet

Macro-mechanisms
Main parameters
Mechanical properties (H, E, stress) Thickness of the coating Surface roughness Debris Principle of load-carrying capacity

TiN/Steel

Hogmark 01

Lee 98

Quantification by scratch test

Courtesy of C. Donnet

Micro-mechanisms
Material response at the m scale
Stress and strain at the asperity level Crack generation and propagation Material release & Particle formation

Electroless Ni coating / gear

Hogmark 01

TiN / HSS

Hogmark 01
Courtesy of C. Donnet

Holmberg 01

Energy accommodation modes

Micro Stress Distribution on a Coated Surface

Hogmark et al.

Ways to Improve Load Carrying Capacity of Coatings

Hogmark et al.

Summary of Wear Mechanisms FRICTION MECHANISMS in Coated Surfaces

COATED CONTACT HARDNESS OF COATING
a HARD SLIDER

SOFT HARD b c

HARD SOFT d

THICKNESS OF COATING
PLOUGHING SHEARING LOAD CARRIED BY COATING STRENGTH g h SUBSTRATE DEFORMATION

SURFACE ROUGHNESS
SCRATCHING PENETRATION REDUCED CONTACT AREA & INTERLOCKING ASPERITY FATIGUE

DEBRIS
PARTICLE EMBEDDING PARTICLE PLOUGHING PARTICLE HIDING PARTICLE CRUSHING

Courtesy of K. Holmberg/VTT-Finland

lon9708

ETM - - KGH\TCB\FRICTM97.dsf.

MAJOR SOURCES OF FRICTION

Physisorption/chemisorption

Roughness

H2O

OH

Major Causes of Friction

Adhesion

Capillary Forces

Elastic/plastic Deformation
Real Contact Areas

Deformation

Adhesion Mechanisms of Friction

The Case of Carbon Films - Covalent sigma (the strongest) - Ionic - Metallic Not applicable to carbon - Magnetic N --* Attraction (in F the case of graphite) - van der Waals -Electrostatic -Capillary A2 A
1

van der Waals

Capillary

Ar = A1 + A2 + . . . Ff = .Ar
Electrostatic

Transfer Films vs Friction

Transfer formation : run-in phenomena + COF fluctuations Transfer film (0.01 - 50 m) Repartition of the lubricant reservoir Interfilm sliding : general condition of steady-state Wear not linear versus duration Accommodation modes Transfer formation Interfilm sliding

Donnet 01

Singer 92

PTFE & Polyimide TiN, CrN, (Ti,Al)N MoS2 DLC

Yamada 90 Huang 94, Wilson 98 Fayeulle 90, Wahl 95 Ronkainen 93, Donnet 95, Grill 97

Effect of Transfer Film Forming Tendency on Friction

DLC-coated Steel Disk Against Various Counterface Balls

0.25

Dry N2

Friction Coefficient

0.2

Zirconia Steel Sapphire DLC-Coated Steel

Sapphire

0.15

Zirconia

Transfer Film

0.1

0.05

DLC Coated Steel Ball

0
Uncoated Steel Ball

100

200

300

400

500

600

Coated Steel Ball

Distance (m)

Tribochemistry vs Friction
Friction-induced fresh surfaces Temperature increase Effect of the surrounding environment

Tribo-reactions at the nm scale

Metal Jahanmir 89, Kuwano 90, Erdemir 91 TiN, CrN, TiC, HBN Mkel 85, Gardos 89, Singer 91, Martin 92, Lin 96 Oxides Blomberg 93, Gee 95, Erdemir 95, Prasad 97 Various (Ti, Al, Zr, Si)N, Rebouta 95 DLC Miyoshi 90, Ronkainen 90, Donnet 95, Erdemir 95, Voevodin 96, Grill 97, Fontaine 01 Diamond, Graphite Gardos 90, Hayward 90, Langlade 94, Blanchet 94 MoS2 Spalvins 80, Fleischauer 87, Singer 90, Martin 93, Wahl 95, Role of H2O on B2O3 Role of gaseous H2 on a-C:H films
1

(H=34at%)

0.1 0.01 0.001

10 hPa H2 =0.003
0 100 200 300 400 Number of cycles 500

0.1 0.01 0.001

=0.7 =0.007
0

UHV or Ar

Formation of lamellar boric acid

Erdemir 90-98

Donnet 01

100 200 300 400 Number of cycles

500

Tribochemical film Formation in Lubricated Contacts

300 m 300 m

Sture Hogmark

Steel/DLC EP

Stee/DLC EP

S W

30 m

Fe O S W

30 m

Fe O C

After 8000 cycles

at 700 N

Ni O W

Roughness vs Friction

F1 = W1 tan

W = W1 + W2 + . . . F = W tan

Tribology of Diamond Films

Roughness Effect

Erdemir, et al., Surface and Coatings Technology, 121(1999) 565-572

Roughness Effect on Friction

Diamond Films
MCD

Rough

Polished MCD

NCD

B. K. Gupta et al., J. Tribol., 116(1994)445.

Environment vs Friction
Physisorption/chemisorption

H2O

OH

0.8 0.7 Friction coefficient 0.6 0.5 0.4 0.3 0.2 0.1 0 0 50 100 150 200
Courtesy of J. Andersson Due to higher degree of covalent bond interactions Diamond Coated Ball

In water In air In argon

Initial friction is 0.1-0.2

Diamond Coated Disk

# Revolutions

Effect of Water Partial Pressure on Frictional Behavior of DLC Film

0.14

At 2000 Pa At 460 Pa At 0.4 Pa

Vacuum Experiments

0.12

0.1

Friction coefficient

?
0.08 0.06

0.04

Smoother and lower friction at lower water vapor pressures

0.02

0 0 20 40 60 80 100 120

Time (s)

J. Anderson and R. Erck/ANL

Environmental Sensitivity of MoS2 Type Solid Lubricant Coating

Work the best in dry, inert, or vacuum type environments

Base MoS2

Ti-Doped

Multiarc, Inc. data

The performance and durability of these solids are strongly affected by the presence of moisture and oxygen in the environment. Aging may also pose a major problem. Doping with Ti, Ni, Au, and Pb may reduce environmental sensitivity.

Friction Mechanisms of Soft Metals

Mainly because of their low shear strengths and rapid recovery as well as recrystallization, certain pure metals (e.g., In, Pb, Ag, Au, Pt, Sn, etc.) can provide low friction when present on sliding surfaces.

Most desired case

After Bowden and Tabor

Thickness of the film is very important

Selected References
K. Holmberg and A. Matthews, Coatings Tribology: Properties, Techniques, and Applications in Surface Engineering, Elsevier, 1994. B. Bhushan and B. K. Gupta, Handbook of Tribology: Materials, Coatings and Surface Treatments, McGraw-Hill, 1991. B. Bhushan, Modern Tribology Handbook, Volumes I & II, CRC Press, 2000.