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Radom, 29 maja 2008
TRIBOCHEMIATRIBOCHEMIA - warsztaty - warsztaty tribologicznetribologiczne
INSTYTUT TECHNOLOGII EKSPLOATACJI INSTYTUT TECHNOLOGII EKSPLOATACJI - PAŃSTWOWY INSTYTUT BADAWCZY- PAŃSTWOWY INSTYTUT BADAWCZY
Monika MAKOWSKA
Marian GRĄDKOWSKI
Institute for Sustainable Technologies
- National Research InstitutePulaskiego 6/10
26-600 Radom
TRANSFORMATIONSTRANSFORMATIONS
OF HYDROCARBONS UNDER OF HYDROCARBONS UNDER
MIXED FRICTION CONDITIONSMIXED FRICTION CONDITIONS
lubricant
Background of the study
Dry frictionDry frictionMixed frictionMixed frictionBoundary frictionBoundary friction
Boundary layers
Experimental procedure
2. Hydraulic oil HL-46
1. n-Hexadecane – model lubricant
CC1616HH3434
LubricantsLubricants
CH3
CH2
CH2
CH2
CH2
CH2
CH2
CH2
CH2
CH2
CH2
CH2
CH2
CH2
CH2
CH3
Experimental procedure
T-11 ball-on-disk machine
pp
v
Ball
Disk-holding cup
Lubricant
DiskHeater
T-11 ball-on-disk machine which allows to run testsT-11 ball-on-disk machine which allows to run tests at elevated temperatures: at elevated temperatures:
material of the friction pair: bearing steel equivalent to AISI 52100,material of the friction pair: bearing steel equivalent to AISI 52100, ball: ball: 6,35 mm6,35 mm ( (1/4”)1/4”), R, Raa = 0,3 = 0,3 m, 58-63 HRC,m, 58-63 HRC,
disk: disk: 25,4 mm25,4 mm ( (1”)1”), R, Raa = 0,25 = 0,25 m, 58-63 HRC.m, 58-63 HRC.
Rubbing tests conditions (mixed friction):Rubbing tests conditions (mixed friction): radius of radius of ball movement on the disk surfaceball movement on the disk surface: ~10 mm,: ~10 mm, load: 9,81 or 49,05 N,load: 9,81 or 49,05 N, sliding velocity: 0,25 m/s,sliding velocity: 0,25 m/s, sliding distance: 500 m, 3000 m, 18000 m,sliding distance: 500 m, 3000 m, 18000 m, temperature: 20temperature: 20170±5°C.170±5°C.
Tribological tests conditionsTribological tests conditions
p
v
13 5
4
2
Experimental procedure
SEM/EDSSEM/EDSScanning Electron Microscopy
Energy Dispersion SpectroscopyIdentification of the elements in external layer of rubbing surface
Investigation of the wear scar surfaceInvestigation of the wear scar surface
FTIRMFTIRMFourier Transform Infrared
MicrospectrophotometryIdentification of the organic productson a rubbing surface
XPSXPSX-Ray Photoelectron
SpectroscopyIdentification of the chemical bonds types in external layer of rubbing surface
Secondary Ion Mass Spectrometry
Determination of the molecular weight of products present on the rubbing surface
SIMSSIMS
R2 = 0,8746
R2 = 0,8968
0,55
0,65
0,75
0,85
0,95
1,05
1,15
1,25
1,35
0 20 40 60 80 100 120 140 160 180
Temperature, [oC]
Wea
r sc
ar d
iam
eter
, [m
m];
Fri
ctio
n fo
rce,
[N
] Friction force and wear scar diameter – CFriction force and wear scar diameter – C16HH34
Tribological tests results
Dependence of the friction force and wear scar diameteron the temperature of friction pair lubricated with C16H34
(load of 10 N, sliding distance of 500 m)
80-90°C
Dependence of the wear scar diameter on the temperature of friction pair (load of 10 or 50 N, friction distance of 3000 or 18000 m)
Wear scar diameter – HL-46Wear scar diameter – HL-46
Tribological tests results
R2 = 0,9849
R2 = 1
0,2
0,3
0,4
0,5
0,6
0,7
0,8
0,9
10 30 50 70 90 110 130
Temperature, [0C]
Wea
r sca
r dia
met
er, [
mm
] load = 50 N, s = 18 000 m
load = 10 N, s = 3 000 m
Profilograms of the disk surfaces after rubbing at different temperatures (load of 10 N, sliding distance of 3000 m)
ProfilogramsProfilograms –– CC16HH34
Rubbing surface analysis
Rubbing surface analysis
SEM images of the wear scar formed at different temperatures
20oC 100oC 170oC
SEM imagesSEM images –– CC16HH34
Rubbing surface analysis
Products layered on the steel surface at 100C (sliding distance of 3000 m)
SEM imagesSEM images –– CC16HH34
Relative content of carbon, iron and oxygen on the disk rubbing surface (load of 10 N, distance of 3000 m) along the marked lines: at 100°C (H-100) and 170°C (H-170)
(a and b mark the inner and the outer boundary of the friction track)
Rubbing surface analysis
SEM/EDS analysisSEM/EDS analysis –– CC16HH34
NoContent [% (m/m)]
Iron Carbon Oxygen Oxygen/carbon
1 90,82±2,38 7,15±1,50 0,00 -
2 86,24±2,23 11,80±1,39 0,00 -
3 30,52±1,07 62,05±1,40 6,98±1,14 0,11
4 98,45±2,53 0,00 0,00 -
5 88,59±2,32 8,94±1,64 0,24±1,18 0,03
6 42,74±1,31 50,99±1,64 5,10±0,55 0,10
7 22,88±0,96 68,72±1,35 7,47±1,11 0,11
8 84,25±2,20 13,75±1,56 0,48±1,20 0,035
9 70,34±1,86 27,72±2,13 0,68±1,34 0,025
10 69,86±1,83 27,37±1,31 1,04±1,07 0,038
11 16,11±0,84 75,68±1,32 7,77±1,32 0,10
12 6,59±0,34 76,58±0,82 16,32±0,88 0,21
13 8,40±0,47 80,50±0,97 10,52±0,45 0,13
Rubbing surface analysis
Elemental composition of the products layered on the steel surface at 100oC (blue cells contain data concerning points within the wear scar)
Presence of the elements on rubbing surface – SEM/EDSPresence of the elements on rubbing surface – SEM/EDS
IR spectra of the IR spectra of the tribotribochemichal products layered on the steel surface after chemichal products layered on the steel surface after static and rubbing testsstatic and rubbing tests
4000,0 3000 2000 1500 1000 700,0
0,0
10
20
30
40
50
60
70
80
90
100,0
cm-1
%T
2958,92
2934,522856,25
1467,10
1378,10
721,45
4000,0 3000 2000 1500 1000 700,0
0,0
10
20
30
40
50
60
70
80
90
100,0
cm-1
%T
2958,92
2934,522856,25
1467,10
1378,10
721,45
3993,0 3000 2000 1500 1000 707,0
-10,0
0
10
20
30
40
50
60
70
80
90
100
110
120,0
cm-1
%T
3607,54
2939,882861,47
2731,792674,73
2024,68
1468,85
1378,17
1303,31
1132,34
1077,71 890,97
722,08
3993,0 3000 2000 1500 1000 707,0
-10,0
0
10
20
30
40
50
60
70
80
90
100
110
120,0
cm-1
%T
3607,54
2939,882861,47
2731,792674,73
2024,68
1468,85
1378,17
1303,31
1132,34
1077,71 890,97
722,08
4000,0 3000 2000 1500 1000 600,0
0,0
10
20
30
40
50
60
70
80,0
cm-1
%T
3509,12
2925,232855,82
1730,97
1594,89
1460,311377,73
1252,631179,23
723,53
n-hexadecane after static test
after rubbing test
Investigation of the boundary layer structure
IdentificationIdentification ofof thethe organicorganic products on rubbing surfaceproducts on rubbing surface - - FTIRMFTIRM
4000,03000200015001000600,0
0,0
10
20
30
40
50
60
70
80,0
cm-1
%T
3509,12
2925,232855,82
1730,97
1594,89
1460,311377,73
1252,631179,23
723,53
Analysis of the IR spectrum of Analysis of the IR spectrum of tribochemicaltribochemical products layered products layeredon the steel rubbing surfaceon the steel rubbing surface
—C=O,>C=C<, —COO—, [R(COO)m]nMe
C—H,
—OH
=C—H—OH, —COOH, (RCOO)nMe C—O
Investigation of the boundary layer structure
IdentificationIdentification ofof thethe organicorganic products on rubbing surfaceproducts on rubbing surface - - FTIRMFTIRM
Investigation of the boundary layer structure
ESCA/XPS survey profile of the steel disk lubricated by n-ESCA/XPS survey profile of the steel disk lubricated by n-
hexadecane during rubbing testhexadecane during rubbing test
708 532 284
Fe2p
O1s C1s
Identification of the chemical bond type - XPSIdentification of the chemical bond type - XPS
Investigation of the boundary layer structure
Analysis of ESCA/XPS spectrum of Analysis of ESCA/XPS spectrum of tribotribochemichal productschemichal products
708 532 284
Fe2p
O1s C1s
6000
5000
3000
2000
1000
0
4000
c/s
740 730 720 710 700Binding energy [eV ]
1
2
0,5
1,5
0
c/s
545 540 535 530 525Binding energy [eV ]
10000
15000
5000
0
c/s
300 295 290 285 280Binding energy [eV ]
Fe2p
O1s
C1s
Fe2p
O1s C1s
Identification of the chemical bond type - XPSIdentification of the chemical bond type - XPS
Investigation of the boundary layer structure
Result of the overlapping peak separation in O1s photoelectron spectrumResult of the overlapping peak separation in O1s photoelectron spectrum
708 532 284
Fe2p
O1s C1s
6000
5000
3000
2000
1000
0
4000
c/s
740 730 720 710 700Binding energy [eV ]
1
2
0,5
1,5
0
c/s
545 540 535 530 525Binding energy [eV ]
10000
15000
5000
0
c/s
300 295 290 285 280Binding energy [eV ]
Fe2p
O1s
C1s
Fe2p
O1s C1s
Identification of the chemical bond type - XPSIdentification of the chemical bond type - XPS
0
1
2
3
4
5
6
7
8
9
10
544 542 540 538 536 534 532 528 526530
536,18 533,68
531,61
529,81
Binding Energy [eV ]
N(E
)/E
Fe2O3
C=O (org.)
C–O (org.)
O1s bond - 532 eV
Chemical structure of the products layered on the rubbing surfaceChemical structure of the products layered on the rubbing surface
R = ~3-12 carbon atoms (C3-12)
Investigation of the boundary layer structure
Identification of the Identification of the tribotribochemical products structurechemical products structure
–R–
HHCCHH
HH
284,
5828
4 ,58
CCHH
286,
4028
6 ,40
HH
Fe
711,
5071
1,50
CO
288,
2828
8,28
O
536
536 ,,
1818
531531,,6161
Conclusions
ConclusionsConclusions
Aliphatic saturated hydrocarbons Aliphatic saturated hydrocarbons undergo conversionsundergo conversions underunder the mixed friction conditions the mixed friction conditions
These products are organic salts of carboxylic acids These products are organic salts of carboxylic acids and ironand iron
They influence the friction conditions and may They influence the friction conditions and may decrease the weardecrease the wear
These phenomena may be applied in lubrication These phenomena may be applied in lubrication processes, e.g. processes, e.g. iin developing ecological lubrication n developing ecological lubrication techniquestechniques
Thank You for Your Thank You for Your attentionattention