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2013 ELGI 25th anniversary
Call for 2013 technical papers
ELGI board nomination
ELGI working groups
UKLA annual dinner
Wear behaviour of grease lubricated gears
Industry news
2012 AGM photos
Influence of grease components on the tribological behaviour of rubber seals
Surface analysis – A powerful tool in the development and testing of new lubricants
Technical papers published in Eurogrease
Patent search
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EUROGREASE 3 july/august/september 2012 1
ChairmanGlobal Lubricants Ltd.
: Terry Dicken
Sandwell Bus.Dev. Centre Oldbury Road Smethwick West Midlands B66 1NN United Kingdom (T): +44 121 544 3638 (F): +44 121 544 6505 (M): +44 7710 754 382 [email protected] Vice-Chair
Camino de la Riera 36-44
: Leandro Muntada Brugarolas S.A.
P.I. Cova Solera; 08191 Rubi Barcelona, Spain (T): +34 93 588 3100 (F): +34 93 697 6313 [email protected] SecretaryTunap Industrie Chemie GmbH & Co
: Josef Barreto-Pohlen
Bürgermeister Seidl Strasse 2 D-82515 Wolfratshausen, Germany (T): +49 8171 1600 75 (F): +49 8171 1600 69 (M):+ 49 151 150 59 421 [email protected] Treasurer: Peter-Paul Mittertreiner Lubricant Consultant Hemonylaan 26 1074 BJ Amsterdam; The Netherlands (T): +31 88 231 1820 (M): +31 (0) 6317 56098 [email protected] Director: Eddy Stempfel Fuchs-Lubritech GmbH Werner-Heisenberg-Strasse 1 D-67661 Kaiserslautern, Germany (T): +41 34 445 3375 (F): +49 6301 3206 940 [email protected] Director: Jean Hirigoyen Petro-Canada Lubricants Europe A Suncor Business Chemin des Balmes 69290 Pollionnay, France (T): +33 4 7848 1391 (F): +33 4 7848 1794 (M): +33 60807 1079 [email protected] Director: Rolf Quermann Carl Bechem GmbH Weststrasse 120 D-58089 Hagen, Germany (T): +49 2331 935 1122 (F): +49 2331 935 1129 [email protected] Editor: Valentina Serra-Holm Nynas AB P O Box 10700 SE-121 29 Stockholm, Sweden (T): +46-8-602 12 94 (F): +46-8-81 62 02 (M): +46-70-284 89 40 [email protected] Office Manager: Carol Koopman ELGI Hemonylaan 26 1074 BJ Amsterdam; The Netherlands (T): + 31 (0) 20 6716 162 (F): + 31 (0) 20 6732 760 (M): + 31(0) 62322 6180 [email protected] [email protected] www.elgi.org
july/august/september 2012 3 Content Podium (R. Quermann) 2 2013 ELGI 25th Anniversary Amsterdam 3 Call for 2013 Technical papers 4 ELGI Board Nomination 4 ELGI Working Groups meetings 4 UKLA Annual Dinner 5 Wear behaviour of grease lubricated gears (J-P Stemplinger) 6-13 Industry news 14-16 2012 AGM photos 17-20 Influence of grease components on the
tribological behaviour of rubber seals (M. Sommer) 21-30
Surface analysis – A powerful tool in the development and testing of new lubricants (A. Orendorz) 31-34 Technical papers published in Eurogrease 35 Patent search 37-39 Forthcoming events 40 Eurogrease subscription & advertising rates www.elgi.org / publications Cover photo:
© FZG FZG – back-to-back test rig. see pages 6-13 The opinions expressed in this magazine are not necessarily those of the ELGI Board and/or the publisher. No responsibility is accepted for the accuracy of the information contained in the text or illustrations.
EUROGREASE 3 july/august/september 2012 2
Rolf Quermann Carl Bechem ELGI Board Director
Dear Members I hope you all have enjoyed a sunny summer holiday and also the fantastic Olympic Games hosted in London as much as I did! The ELGI board is continuously reviewing benefits to our membership. By now you are all aware that Constantin Madius from Axel Christiernsson has taken on the role as ELGI technical coordinator to champion the ELGI working groups. He will participate in the next WG-meetings to be held at the Holiday Inn Rai in Amsterdam which are scheduled for the following dates:
• TMWG Wednesday 28th November commencing at 10.00 h • Bio-Base WG Wednesday 28th November commencing at 14.00 h • RLWG Thursday 29th November commencing at 10.00 h
If you are not a registered member yet and would like to attend these WG-meetings, please contact Carol Koopman at our office for further information on these meetings and the venue. I would also like to announce another service to our members, namely that we will publish an overview of grease related patents in the Eurogrease magazine. Please see pages 37-39 of this issue where we have covered patent search on additives, base oils and greases. A list of past published technical papers is also available in this issue of Eurogrease. We are collating papers published prior to the electronic system and will make these papers available to our members in due course to download from our website www.elgi.org / publications. Our next AGM will be held in Amsterdam in 2013. As this will be the 25th anniversary of the ELGI in The Netherlands, the intention is to receive technical papers which focus on a key topic typical for the venue, which we believe, is “Water”. Therefore the theme of the 2013 AGM: “Water – problems solved?” If you would like to present a paper then please submit your paper topic and abstract to the ELGI latest 31st October 2012. We are looking forward to reviewing your valuable proposals for presentation and see you our forthcoming AGM. Rolf Quermann Programme Coordinator
EUROGREASE 3 july/august/september 2012 3
25th ELGI Annual General Meeting 20th – 23rd April 2013
Amsterdam - The Netherlands
“Celebrating 25 years of excellence in bridging a generation of grease specialists!!”
Hotel Okura Amsterdam Ferdinand Bolstraat 333
1072 LH Amsterdam - The Netherlands T: + 31 (0)20 678 71 11 F: +31 (0)20 671 23 44
www.okura.nl
EUROGREASE 3 july/august/september 2012 4
Call for 2013 papers
“Water” problem solved? Papers considering the effects and issues of water in relation to greases: water resistant greases & additives that enhance performance and lubrication in the presence of water and moisture will be given high priority. Other topics of interest to the grease industry are welcome & will be considered too. The cut off date for submitting your paper proposal: 31st October 2012. [email protected]
ELGI Board Vacancy There are two positions available on the ELGI Board, namely Jean Hirigoyen & Eddy Stempfel will step down by rotation and are eligible and will stand for re-election at the forthcoming postal ballot prior to the 2013 AGM in Amsterdam.
3rd Vacancy on the board: A third board position is now available, following the announcement at the 2012 AGM in Munich that “there will be structural changes to the ELGI board set up.” The ELGI board will increase to 8 members in 2013 and to 9 members in 2014. Following this transition period the board will revert back to 8 then 7 members. Constitution on board positions: "The Board of Directors will never be made up of more than one third (1/3) of its directors from one country or company” and a board member should be domiciled in Europe. If you wish to stand for election or wish to nominate anyone then please send your nominations to the ELGI by 31st December 2012 to [email protected] or Fax: #31 20 67 32 760. Else see www.elgi.org
ELGI Working Groups Meetings Friday 26th October 2012 Food Grade Lubricants Working Group
UEIL Conference - Lisbon Contact: [email protected]
Wednesday 28th November 2012 Test Methods Working Group
Holiday Inn Rai Amsterdam Commencing 10.00 hrs Contact: [email protected] / [email protected]
Wednesday 28th November 2012 Bio-base Grease Working Group
Holiday Inn Rai Amsterdam Commencing 14.00 hrs Contact: [email protected] / [email protected]
Thursday 29th November 2012 Railway Lubricants Working Group
Holiday Inn Rai Amsterdam Commencing 10.00 hrs Contact: [email protected] / [email protected]
for a nomination form.
EUROGREASE 3 july/august/september 2012 5
FOR ALL YOUR
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OVERSEAS DISTRIBUTION OPPORTUNITIES EXIST
EUROGREASE 3 july/august/september 2012 6
Wear behaviour of grease lubricated gears
Presented at the 24th ELGI Annual General Meeting 2012 Munich Germany
Author: M.Sc. Johann-Paul Stemplinger1
Co-authors: Prof. Dr.-Ing. Karsten Stahl1, Prof.i.R. Dr.-Ing. Bernd-Robert Hoehn1, Dr.-Ing. Klaus Michaelis1, Dr.-Ing. Hans-Philipp Otto1, Dr.-Ing. Michael Hochmann2
1: Technische Universitaet Muenchen TUM, Mechanical Engineering, Gear Research Center FZG, Munich, Germany
2: Klueber Lubrication Muenchen KG, Marketing and Application Engineering, Munich, Germany Johann-Paul Stemplinger is an associate to Prof. Dr.-Ing. K. Stahl, at FZG since 2009. He studied Mechanical Engineering, Technical University Munich, M.Sc. Abstract: For lubrication of open gear drives applied in rotary furnaces, often gear greases are used as well as for lubrication of gear boxes in difficult sealing conditions. The selection of the gear grease influences strongly the wear behaviour. Investigations with flow greases NLGI 00 were made in a back-to-back test rig determining the weight loss due to wear according to the standardised procedure ISO 14635 part 3. Different variables, such as base oil viscosity, thickener type and additional solid lubricant type, were analysed. Only the type and amount of solid lubricant shows a significant influence on the weight loss due to wear. Finally, a linear wear coefficient clT based on the calculation method of the wear amount according to Plewe is derived and can be used to transfer the test results to any gears in practice. Keywords: Gears, Lubricants, Greases, Wear
1. Introduction For lubrication of open gear drives applied in rotary furnaces, often gear greases are used as well as for lubrication of gear boxes in difficult sealing conditions. The selection of the gear grease influences the wear behaviour.
2. Test Lubricants The investigations of the wear behaviour were made for different flow greases NLGI 00 and one base oil. The composition of the flow greases NLGI 00 was varied with regard to the base oil viscosity, to different thickener types and to the addition of different solid lubricants. Mineral oils with an EP additive and without viscosity index improver were used as base oils. The data of the investigated lubricants are shown in Table 1.
EUROGREASE 3 july/august/september 2012 7
Table 1: Data of the investigated lubricants
3. Test equipment FZG back-to-back gear test rig The test runs for the determination of the wear behaviour of gear greases NLGI 00 were performed on a FZG back-to-back gear test rig. The schematic setup of the FZG back-to-back gear test rig is shown in Figure 1.
Figure 1: FZG back-to-back gear test rig
The FZG back-to-back gear test rig utilizes a re-circulating power loop principle, also known as a four-square configuration, in order to provide a fixed torque (load) to a pair of test gears [6]. Test gear box and drive gear box are connected through two torsion shafts. One shaft is divided into two parts and contains a load coupling used to apply the torque (load) through the use of weights hung on the loading arm.
Test gears The wear behaviour of gear greases NLGI 00 is investigated in the pairing hard-hard of case carburized pinion and wheel. For this purpose the test gears type A are used [6]. The data and manufacturing details of the test gears type A are shown in Table 2.
Cod
e
Lub
rican
t com
posi
tion
Thi
cken
er [%
]
Wor
ked
pene
tratio
n [0
.1 m
m]
DIN
ISO
213
7 at
25°
C K
in. v
isco
sity
ν40
°C
[mm
²/s]
DIN
515
62 (b
ase
oil)
Kin
. vis
cosi
ty ν
100°
C
[mm
²/s]
DIN
515
62 (b
ase
oil)
Den
sity
ρ15
°C [g
/ml]
DIN
517
57 (b
ase
oil)
R Mineral baseoil + EP - - 638.3 35.2 0.911
A R + AK 3.3 410 638.3 35.2 0.911
AV1 Mineral baseoil + EP + AK 4.4 416 72.0 8.0 0.879
AV2 Mineral baseoil + EP + AK 2.6 395 1241.0 54.4 0.920
AS A + add. R 2.6 390 638.3 35.2 0.911
L R + Li 4.7 417 638.3 35.2 0.911
AF1 R + AK + FC (4.2%, GS<35µm) 2.6 408 638.3 35.2 0.911
AF2 R + AK + FC (11.1%, GS<35µm) 2.1 407 638.3 35.2 0.911
AF3 R + AK + MD (4.2%, GS<40µm) 2.6 404 638.3 35.2 0.911Explanation:AK Aluminum complex soapLi Lithium soapEP Additive RC9505 (4 %)FC Synthetic graphiteMD Molybdenum disulfide GS Grain size for 95%
EUROGREASE 3 july/august/september 2012 8
Table 2:Test gears data
4. Test conditions Wear Test A/2,8/50 The tests to analyse the wear behaviour of different gear greases NLGI 00 were made in the wear test A/2,8/50 on the basis of ISO 14635-3 [7] and DIN ISO 14635-1 [6] on a FZG back-to-back test rig. In the wear test at dip lubrication the gear type A is used to run at a circumferential speed of vt = 2.8 m/s starting with a step-test and concluding with an endurance test of 100 h in total. In the step-test the load is raised stepwise starting with load stage 1 to load stage 12 with a starting lubricant temperature of ϑS, Start = 50 °C in every load stage and a limited lubricant temperature of ϑS = 90 °C in each load stage. The duration criterion of every load stage is 21700 load cycles of the wheel, which equals to about 45 min running time. Following the step-test, an endurance test of 100 h is conducted with a maximum lubricant temperature of ϑS, Endurance = 80 °C (A/2,8/80). Two tests were made on each lubricant for statistical reasons. Analysis Based on the results of DGMK 377-01 [3], four different wear categories were defined for the 100 h endurance test. With these wear categories a classification of the different lubricants can be made based on the wear sum of pinion and wheel, see Table 3. Run-in effects can be eliminated due to the previous step-test.
Table 3: Wear categories for endurance test 100 h (A/2,8/80)
Shaft centre distance a 91.5 mmModule m 4.5 mm
pinion z1 16 −
wheel z2 24 −
Effective tooth width b 20 mmHelix angle β 0 °
α 20 °αw 22.5 °
pinion x1 0.8532 −
wheel x2 -0.50 −
pinion da1 88.77 mmwheel da2 112.50 mm
Basic material − 20MnCr5 −
Surface hardness − 61 +/-1 HRCpinion Ra 0,35+/-0,10 µmwheel Ra 0,30+/-0,10 µm
Flank roughness
Pressure angleWorking pressure angle
Profile-shift coefficient
Tip diameter
Dimension Symbol UnitNumerical value
Number of teeth
Wear category
Wear sum (pinion+wheel)
[mg]
low < 70
medium < 280
high < 700
very high > 700
EUROGREASE 3 july/august/september 2012 9
5. Test results In total, almost all investigated lubricants, except the greases with solid lubricants (AF1,2,3), show low wear in all test parts. For detailed results see the following Figures 2 -5.
Oil vs. Grease In Figure 2 an equal wear behaviour is shown for base oil R and its base grease A with a weight loss of under 25 mg after the step-test and under 50 mg after the endurance test. No significant influence of the thickener can be stated.
Figure 2: Wear behaviour – Oil vs. Grease
Influence of base oil viscosity The influence of the baseoil viscosity on the wear behaviour of greases in NLGI 00 is shown in Figure 3. Grease A, with its ISO VG 680 mineral base oil, shows lower wear compared to grease AV1, with its ISO VG 68 mineral base oil. The grease AV2 with a base oil viscosity of ν40 = 1241 mm²/s shows unexpected high wear, probably due to its mineral base oil quality.
Figure 3: Wear behaviour – Influence of base oil viscosity
Influence of thickener type The wear behaviour of different thickener types for greases in NLGI 00 is shown in Figure 4. The influence of the concentration of thickener in the grease and the type of thickener can hardly be seen. The grease AS is based on base grease A mixed up with additional base oil R within NLGI grade 00. No
050
100150200250300350400450500550600650700
Stufentest Dauerlauf
Sum
men
vers
chle
iß R
i + R
a [m
g]
A
Wea
r sum
(pin
ion
+ w
heel
) [m
g]
low
R A RStep-test(LS 1 - LS 12)
Endurance Test(100 h in LS 10)
med
ium
high
Wea
rcat
egor
yin
end
uran
cete
st
Test gears type Avt = 2.8 m/sϑS,Start = 50 °CϑS = 90 °CϑS,Endurance = 80 °C Dip lubrication
050
100150200250300350400450500550600650700
Stufentest Dauerlauf
Sum
men
vers
chle
iß R
i + R
a [m
g]
AV1 A AV2 AV1 A AV2
Test gears type Avt = 2.8 m/sϑS,Start = 50 °CϑS = 90 °CϑS,Endurance = 80 °C Dip lubrication
Wea
r sum
(pin
ion
+ w
heel
) [m
g]
low
med
ium
high
Wea
rcat
egor
yin
end
uran
cete
st
Step-test(LS 1 - LS 12)
Endurance Test(100 h in LS 10)
EUROGREASE 3 july/august/september 2012 10
significant difference can be detected between AS and A. Grease A with aluminium complex soap shows a slightly higher wear sum compared to grease L with lithium soap.
Figure 4: Wear behaviour – Influence of thickener type
Influence of amount and type of solid lubricant The influence of the amount and type of additional solid lubricants in greases NLGI 00 on the wear sum of pinion and wheel is shown in Figure 5. Compared to the base grease A without solid lubricant, AF1 and AF2 show higher wear sums correlating with their concentration of synthetic graphite in the grease, with highest wear for AF2 with a concentration of 11.1% synthetic graphite. At the end of the step-test AF1 (4.2% synthetic graphite) shows a three times higher wear sum than the base grease A and AF2 shows a eight times higher wear sum than the base grease A. This trend is confirmed in the endurance test. The grease AF3, with a concentration 4.2% of molybdenum disulfide, shows comparable wear to grease A after the step-test and a slightly higher wear after the endurance test. In comparison to the grease AF1 with synthetic graphite, the grease AF3 with molybdenum disulfide shows clearly lower wear.
Figure 5: Wear behaviour – Influence of amount and type of solid lubricant
6. Wear calculation Based on these test results, candidate lubricants can be discriminated according to their wear characteristics. In addition, it is also interesting to evaluate the actual wear rate to be expected in a gear in practice, if it is operated with the respective lubricant. For this purpose the test results are introduced into a calculation method according to Plewe [8].
050
100150200250300350400450500550600650700
Stufentest Dauerlauf
Sum
men
vers
chle
iß R
i + R
a [m
g]
A AS L A AS L
Test gears type Avt = 2.8 m/sϑS,Start = 50 °CϑS = 90 °CϑS,Endurance = 80 °C Dip lubrication
Wea
r sum
(pin
ion
+ w
heel
) [m
g]
low
med
ium
high
Wea
rcat
egor
yin
end
uran
cete
st
Step-test(LS 1 - LS 12)
Endurance Test(100 h in LS 10)
050
100150200250300350400450500550600650700
Stufentest Dauerlauf
Sum
men
vers
chle
iß R
i + R
a [m
g]
A AF1 AF2 AF3 A AF1 AF2 AF3
3009
mg
Test gears type Avt = 2.8 m/sϑS,Start = 50 °CϑS = 90 °CϑS,Endurance = 80 °C Dip lubrication
Wea
r sum
(pin
ion
+ w
heel
) [m
g]
low
med
ium
high
Wea
rcat
egor
yin
end
uran
cete
st
Step-test(LS 1 - LS 12)
Endurance Test(100 h in LS 10)
EUROGREASE 3 july/august/september 2012 11
Wear calculation acc. to Plewe In order to transform the results of the wear test to actual operating conditions in a gear in practice, a suitable calculation method was developed by Plewe [8]:
NcWWT
W
CT
C41
T0H
0HlTl ⋅
⋅
⋅
⋅=
ζζ
ρρ
σσ
,
with Wl [mm] linear wear amount clT [mm/rev] linear wear coefficient from test (Index T) σH0 [N/mm2] nominal contact stress ρC [mm] relative radius of curvature at pitch point ζW [-] wear relevant specific sliding N [-] number of load cycles The linear wear amount Wl represents a mean layer thickness of worn out material from the tooth flank. According to investigations of Plewe [8], the removal of material is not uniform in profile in the direction of the flank. The maximum wear is expected in the middle between pitch circle and the start of contact and end of contact respectively. The maximum wear depth is about three times the calculated linear wear amount Wl. Linear wear coefficients clT of the investigated lubricants For all candidate lubricants the linear wear coefficient clT can be calculated from the respective test results according to [8]:
ρ⋅⋅⋅=
zm2ccn
mTlT Nb
mcmT ⋅=
with clT [mm/rev] linear wear coefficient
cmT [mg/(mm⋅rev)] mass specific wear coefficient mn [mm] normal module z [-] number of teeth ρ [mg/mm³] specific gravity of gears m [mg] wear amount b [mm] face width N [-] number of cycles
To be sure that there is no influence of the run-in, the linear wear coefficient clT is calculated using the result of the endurance test. For all investigated lubricants the minimum lubricating film thickness hmin was calculated according to Dowson / Higginson [1] based on the base oil data and the values for the viscosity-pressure coefficients α according to Gold[2]. Due to different load conditions and different gear geometry at the tests of Plewe (index P) and the wear test A/2,8/80 (index T) a factor f for the linear wear coefficient has to be introduced to get a direct comparability with Plewe.
4031fWP
WT41
P0H
T0H .,
=
⋅
=
ζζ
σσ
The calculated linear wear coefficients for the investigated lubricants are introduced in the Plewe-diagram, see Figure 6. Additionally the Plewe wear curves of a straight mineral oil and a grease NLGI00 without EP-additive are shown for comparison. The linear wear coefficient clT can be taken for the investigated lubricants from Figure 6, introducing the calculated minimum film thickness for the actual transmission at operating conditions to calculate the linear wear amount Wl.
EUROGREASE 3 july/august/september 2012 12
Figure 6: Wear behaviour – linear wear coefficient clT
The wear behaviour of the investigated lubricants in ISO VG 680 without solid lubricants correlates well with the Plewe-curve for greases in NLGI 00 with only small changes due to thickener, thickener type and concentration. With additional solid lubricants, increasing wear can be detected, which correlates with the amount of synthetic graphite. With lower base oil viscosity the grease AV1 shows a lower minimum film thickness and higher wear than the base grease A with a ISO VG 680 base oil. AV2 with the highest kinematic viscosity and highest minimum film thickness shows an unexpected high linear wear coefficient, probably due to its mineral base oil quality.
7. Conclusion Investigations with flow greases NLGI 00 were made in a back-to-back test rig, determining the weight loss due to wear according to the standardised procedure ISO 14635 part 3. Different variables, such as base oil viscosity, thickener type and additional solid lubricant type, were analysed. Only the type and amount of solid lubricant shows a significant influence on the weight loss due to wear, with highest wear for AF2 with 11.1% synthetic graphite. Molybdenum disulfide in grease AF3 shows for an equal concentration of 4.2% lower wear than the synthetic graphite in grease AF1 and slightly
higher wear compared to the base grease A without solid lubricant. Finally, a linear wear coefficient clT based on the calculation method of the wear amount according to Plewe was derived, which can be used to transfer the test results to any gears in practice.
8. References [1] Dowson, D., Higginson, G. R.:
Elastohydrodynamic Lubrication, Oxford, 1966
[2] Gold, P. W., Schmidt, A., Loos, J., Assmann, C.: Viskosität-Druck-Koeffizienten von mineralischen und synthetischen Schmierölen, Tribologie & Schmierungstechnik, 48. Jahrgang, 1 / 2001, S. 40 - 48
[3] Höhn, B.-R., Michaelis, K., Bayerdörfer, I.: Untersuchungen zum Einfluss von Schmier-stoff und Betriebsbedingungen auf das Verschleißverhalten von Zahnrädern, Deutsche Wissenschaftliche Gesellschaft für Erdöl, Erdgas und Kohle e.V., DGMK Forschungsbericht 377-01, Hamburg, 1996
[4] Hochmann, M.: Zahnradtragfähigkeit bei Schmierung mit Getriebefließfetten, Diss. TU München, 2011
[5] Hochmann M.: Tragfähigkeit von Zahnradpaarungen bei Schmierung mit
0,001
0,5 E-9
1 E-9
5 E-9
10 E-9
50 E-9
100 E-9
0,1 E-9
500 E-9
0,002 0,005 0,01 0,02 0,05 0,1 0,2 0,5
ARASLAV1AV2AF1AF2AF3Plewe: GreasePlewe: Oil
σH0T = 1443 N/mm²ρCT = 8,4 mmζWT = 0,765pairing: hard-hard
Variation Thickener
Min. film thickness hmin [µm]
Line
ar w
earc
oeffi
cien
tclT
[mm
/rev] With solid
lubricant
EUROGREASE 3 july/august/september 2012 13
Getriebefetten, Deutsche Wissenschaftliche Gesellschaft für Erdöl, Erdgas und Kohle e.V., 2006
[6] ISO 14635-1: Gears – FZG test procedures – Part 1: FZG test method A/8.3/90 for relative scuffing load-carrying capacity of oils, 2000
[7] ISO 14635-3: Gears – FZG test procedures – Part 3: FZG test method
A/2,8/50 for relative scuffing load-carrying capacity and wear characteristics of semifluid gear greases, 2005
[8] Plewe H.-J.: Untersuchungen über den Abriebverschleiß von geschmierten, langsam laufenden Zahnrädern, Diss. TU München, 1980
___________________________________________________________________________________
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Industry News
New marketing director at Nynas – focuses on growth Dr. Valentina Serra Holm has been appointed Marketing Director for Nynas Naphthenics business. Valentina succeeds Jean-Marie Toullat who will take on a role as Senior Advisor at Nynas. “This is obviously a great opportunity and challenge for me personally. I see a continued focus on growth for Nynas, both in respective customer segments as well as an organic growth in different parts of the world. I will continue to reinforce the strengths that make us unique today. Our high degree of specialization, local presence and personal approach coupled with a high degree of technical knowledge. These are proven strengths that we will continue to develop. I will manage our large product offering and ensure that the added volume coming from our planned acquisition* of the Harburg refinery in Germany will come to great use worldwide.” says Dr. Serra Holm. Valentina takes on the responsibility with vast experience from the specialty oil market. With a Ph D in Chemical Reaction Engineering from Abo Akademi, Finland, and a PhD in Chemical Plants from Polytechnic of Turin, Italy she has the knowledge and the proven drive to take Nynas further. Valentina joined Nynas AB in 2001 and is most recently coming from a positions as Market Manager for Nynas business area for lubricants. As a renowned and appreciated speaker at conferences and as chairman of several industry forums i.e. ELGI AGMs, the Tribology Colloquium in Esslingen and the Icis World Base Oil and Lubricant Conference in London, Valentina is well known to the industry. * Acquisition is subject to pending EU approval For more information, contact: Dr. Valentina Serra-Holm Tel: +46-70-284 89 40 [email protected]
R.T. Vanderbilt Company, Inc. Earns USDA Certified Biobased Product Label Norwalk, CT. (July 28, 2012) - R.T. Vanderbilt Company, Inc. has earned the USDA Certified Biobased Product Label for its MOLYVAN® 855 Friction Reducer. The USDA Certified Biobased Product Label verifies that the amount of renewable biobased ingredients meets or exceeds prescribed USDA standards. Biobased products are goods composed in whole or in significant part of agricultural, forestry, or marine materials. “R. T. Vanderbilt Company, Inc.’s commitment to sustainability and to the development of products that improve sustainability is demonstrated by having a key product, MOLYVAN® 855 Friction Reducer, which is a USDA Certified Biobased Product. This product not only uses a sustainable, biobased raw material, but also provides fuel economy improvement in motor vehicles and reduces greenhouse emissions.” -Hugh B. Vanderbilt, Jr., Chairman & CEO Such biobased claims are verified by independent labs and monitored by the USDA. Consumers may rely on the accuracy of the biobased amount certification in making informed purchasing decisions. “We are pleased that R.T. Vanderbilt Company, Inc. has earned the USDA Certified Biobased Product Label,” said Ron Buckhalt, USDA BioPreferred Program Manager. "Biobased products provide opportunities to help add value to renewable commodities, create jobs in rural communities and generate investment income."
The example label is anticipated to be on certified products and available for consumers in 2012.
Celebrate and launch STRATCO’S 85TH Birthday during ILMA annual meeting
SCOTTSDALE, AZ -- With 85 candles on its corporate cake, STRATCO, Inc. is celebrating its 85th year in business with a special event during the upcoming Independent Lubricant
EUROGREASE 3 july/august/september 2012 15
Manufacturers Association (ILMA) Annual Meeting, Oct. 13-16 in Scottsdale. Diane Graham, STRATCO CEO, will host an October reception in conjunction with the ILMA Annual Meeting. The annual meeting consists of committee and technical sessions as well as networking and social events. “As a supporter of ILMA and the members of the association, I am thrilled to host this event and to celebrate STRATCO’s 85th year in business,” said Graham. “We continue to carry out the mission we established in 1928 to provide the best technology, equipment and products for better efficiency and a better environment.” STRATCO has been involved with the National Lubricating Grease Institute (NLGI) since its inception in 1933, and the European Lubricating Grease Institute (ELGI) since its inception 25 years ago. STRATCO’S state-of-the art technology and famous STRATCO® Contactor™ reactor are recognized worldwide with a Customer base in 52 countries on six continents. The versatility of the STRATCO® Contactor™ reactor and technology allows our Customers to produce different types of lubricating greases more efficiently with operational cost savings, resulting in a faster return on investment.
STRATCO is proud to introduce its new line of Grease Kettles, designed for the changing needs of our Customers. With the evolution of specialty greases, the design of kettles must also evolve to accommodate greater sophistication and efficiencies in the process. These Grease Kettles will be customized in size to the requirements of our Customers. In addition, STRATCO has conducted research for companies interested in developing alternative fuels and developed its own biodiesel process. STRATCO’s unique reactor design is also particularly well suited for production of food additives, paints, ointments and modified asphalts for the construction and roofing industries. STRATCO, Inc. is a privately held firm headquartered in Scottsdale, Arizona. The company provides engineering and equipment manufacturing solutions to customers worldwide in the lubricating grease, modified asphalt and petrochemical industries.
Auburn University offers first minor in tribology and lubrication science Auburn University has established the nation’s first undergraduate minor intribology and lubrication science. To date, there has been no multidisciplinary, tribology‐focused program at the undergraduate level in the nation, and few such programmes in the world. The dedicated minor in Auburn’s Samuel Ginn College of Engineering provides students with an in‐depth focus in all areas of tribology and offers them unique exposure to the full breadth of the field. The course of study incorporates all elements of tribology, including chemistry and mechanics of friction and wear, as well as relevant manufacturing concepts and processes. Students gain significant knowledge of hydrocarbon processing and refining, additive functionality, and applications that require precise lubrication engineering expertise, as well as training in bio-technology and renewable lubrication with additional focus on energy conservation. This unprecedented and systematic approach offers a true interdisciplinary focus that is not available at any other major university. “Up to this point, we have not had a formal curriculum dedicated to tribology,” said Dave Millin, vice president of Additives Business and Technology at The ELCO Corporation."Lubrication technology is accelerating as rapidly as any of the other technical fields, and our industry needs a constant flow of capable talent to replenish and bolster our ranks.” Meeting industry needs With the aging baby boomer demographic and impending retirements, a vast amount of knowledge and skills will leave the lubrication work force in the next few years. This knowledge base must be replaced to maximize lubrication engineering’s role in manufacturing, transportation and industrial capacity throughout the world. Accordingly, the lubrication industry must provide a pipeline to supply talent that will meet the growing need for properly trained scientists and engineers who understand the advances in all aspects of lubricant application. Auburn’s new minor will deliver uniquely qualified engineers to meet the needs of the future. This targeted approach provides prospective employers with talented men and women who
are highly productive at the onset of employment. Companies that provide various lubrication products will now have a pipeline of well‐prepared graduates, and large manufacturing companies that utilize lubricants to protect multimillion dollar machinery investments will have access to individuals who have an extensive understanding of tribology’s role in protecting that investment. Providers of additives and components to the industry can also utilize these graduates in both their technical and marketing efforts. A distinguishing feature: It’s more than just the mechanics and the chemistry Auburn’s tribology minor is unique in that it incorporates the university’s acclaimed Business‐Engineering‐Technology (B-E-T) programme – a curriculum designed to bridge the gap between engineering and business cultures. The B‐E‐T programme teaches undergraduate students crucial business and engineering principles via shared coursework and hands‐on projects that give students a feel for the myriad ways in which these disciplines work together in the real world. A new graduate entering the lubricant field with focused instruction on both tribology and real‐world
business practices will hold a clear advantage over other entry‐level employees, and will offer significant benefit to any company, particularly those involved in the manufacture and supply of lubricants to the ultimate market. Barbara Bellanti of Battenfeld Grease & Oil and NLGI's past president notes that the lubricating industry will be well served by having new graduates from Auburn University with both the technical and business education they need to be productive. “Many of us, with second and even third generation succession planning concerns have wished there were college programmes to assist in educating our next generation,” she said.“For such a critical and important industry like lubrication, this has been a long time coming.” Dr. Robert Jackson [email protected] T: + 1 334.844.3340 Morgan Stashick [email protected] T:+1 334.844.3591 www.eng.auburn.edu/tribology
The OilDoc Conference and Exhibition offers a high quality program with three session tracks, a first class speaker line-up, a lot of international networking opportunities and a major international exhibition additional to the conference.
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2012 ELGI Annual General Meeting Munich Germany
Colin Gatward & Stephen Lewis
Lisa Tocci & Serena Dicken
Dave Como & Wolfgang Boes
Eva Ortega & Leandro Muntada
Alex Zhu Zhaoying Yu Hervé Grignou
Marcel Otte, Constantin Madius Jenny Johansson & Sandra Tunhav
Qiong Zhao, Liu Yanfei, Shan Huang & Lifang Tang
2012 ELGI Annual General Meeting Munich Germany
Stefan Limbach Claude Bercq Eric Delaye Frédéric Maysonnave
Reception at BMW
Mehdi Fathi, Cassandra Boevers, Lou Honary, Anoop Kumar Oleg & Oleksandr Makedonsky, Anoop Kumar
2012 ELGI Annual General Meeting Munich Germany
2012 ELGI Annual General Meeting Munich Germany
EUROGREASE 3 july/august/september 2012 21
Influence of grease components on the tribological behaviour of rubber seals
Presented at the 24th ELGI Annual General Meeting 2012 Munich Germany
Author: Dipl.-Ing. Max Sommer
Co-authors: Prof. Dr.-Ing. Werner Haas Institut für Maschinenelemente
Stuttgart - Germany [email protected] www.ima.uni-stuttgart.de
Max obtained a Degree in Mechanical Engineering (Dipl.-Ing.) in 2010. He is a Research Assistant since June 2010 at the University of Stuttgart (Institute of Machine Components, Sealing Technology) Abstract Rolling bearings are more and more lifetime lubricated with grease instead of with oil. Therefore a reliable sealing of greases is essential. However, the tribological behaviour in the grease lubricated sealing gap is mostly unknown. Nevertheless, the knowledge of this behaviour is essential for an optimized design of seals. The aim of these investigations is to evaluate the influence of grease components on the temperature and friction torque of the tribological system. The complex tribological system of a rubber seal is reduced to an experimental model and tested on a ring-on-disc tribometer. This model will be shown and the results of investigations will be presented. Introduction Dynamic shaft applications as in gears are often sealed with elastomeric radial lip seals. These sealing systems have existed for more than 40 years and are optimized for the sealing of oil. The sealing mechanism of these sealing systems is known if oil is sealed and different hypotheses exist /1/. The geometry of a radial lip seal is shown in Figure 7. The seal ring with the sealing lip is made of elastomer such as NBR (Nitril-Butadien-Rubber). The elastomer seal ring is bonded to the rigid steel case and the sealing lip is pressed on the shaft counter face. On the one
hand the contact pressure between the sealing lip and the counter face is caused by the elastomer sealing lip itself, which is stretched during installation on the shaft counter face. On the other hand, the pressure arises from a garter spring mounted near the sealing lip. The sealing mechanism can be explained by the micro asperities on the sealing lip, which are developed during run in. These micro asperities are undistorted at standstill. But in the case of a rotating shaft, the micro asperities are distorted asymmetrically. This asymmetry comes from the asymmetric distribution of the contact pressure and tangential shear stress. The reason for this purpose is the geometry of the sealing lip. The contact angle on the oil side is bigger than the one on the air side. This leads to an asymmetric deformation of the sealing lip. A rotation of the shafts causes hydrodynamic conditions between the sealing lip and the shaft counter face. The lubricant in this area is deflected by the distorted micro asperities. Because of this, the seal pumps lubricant in both directions. But due to the asymmetric distortion of the micro asperities, the pumping rate towards the oil side is bigger than the one toward the air side. The result is a net pumping rate of lubricant from the air towards the oil side. In the case of sealing grease, no confirmed results about the sealing mechanism exist. Nevertheless radial lip seals are used for the
EUROGREASE 3 july/august/september 2012 22
sealing of greases in many cases, such as the sealing of bearings or gears. But the sealing of grease leads to totally different operating
conditions and problems in the application. The results are heavily reduced limitations of use or even leakage.
Figure 7: Geometry and Sealing Mechanism of Radial Lip Seals Figure 8 shows the different operating behaviour of grease lubricated radial lip seals compared to an oil lubricated one. The oil lubricated radial lip seal features a smooth characteristic of the measured friction torque. The friction torque reaches static conditions. The operating behaviour of the grease lubricated seals is much more complex. The measured friction torques are scattering heavily and are showing considerable changes of the measured values. Due to this behaviour, it is much harder to evaluate the behaviour of grease lubricated radial lip seals than oil lubricated ones.
Figure 8: Friction Torque of Oil and Grease Lubricated Radial Lip Seals
Nevertheless, it is necessary to understand the operating behaviour of grease lubricated radial lip seals to be able to optimize these machine components. Former investigations are showing that there is an enormous potential to increase the limit of use or reduce friction losses and wear. /2/ In this regard, each
garter spring
sealing lip
EUROGREASE 3 july/august/september 2012 23
component of the sealing systems (seal ring, shaft counter face, lubricant) plays an important role. As a consequence of the interactions between these components it is hard to make the essential investigations using the real sealing system. Because of this problem the experiments in this paper were made using a simplified model, cf. Figure 9. The radial lip seal is replaced by an elastomer ring. This ring faces the counter face, a plane steel disc. Using this ring-on-disc model it is much easier to investigate the tribological behaviour of the grease lubricated elastomer-steel-contact.
Figure 9: Real System and Simplified Model Experimental Set-Up The aim of the investigations with the ring-on-disc model is to distinguish the influences of the grease components on the tribological behaviour of the elastomer-steel friction contact. For these investigations a rotary tribometer was used. Figure 10 shows the experimental set-up. The elastomer ring is fixed to a rotating spindle. It is running on the counter face, a plane steel disc which is pressed against the elastomer ring. This counter face is hardened (55 HRC) and grinded with a roughness of about Rz = 2 µm. These specifications are according to DIN 3760 /3/, the technical standard for radial lip seals. The patterns on the surface of the disc are concentric. Thereby the elastomer ring is running in the direction of these patterns. This is equal to a radial lip seal used with a grinded shaft. The sealing lip also runs in the direction of the patterns. The internal space of the elastomer ring is filled with 0.6 g of grease before the test run.
Figure 10: Experimental Set-Up
Figure 11 shows a steel disc which is used as counter face. A microscopic image of the counter face can be seen on the right hand side. The counter face shows the typical patterns of the grinding process.
EUROGREASE 3 july/august/september 2012 24
Figure 11: Counter Face
Figure 12 shows an elastomer ring fixed with two-component adhesive on the adapter. The elastomer rings are cut out of elastomer panels by a water jet. Before the test run, a running in procedure is done. This is necessary to get a comparable surface topography of each elastomer ring. Such a typical worn elastomer surface can be seen on the right hand side.
Figure 12: Elastomer Ring
Test Rig The used rotary tribometer is shown in Figure 13. The spindle is driven by the motor via a belt transmission. The counter surface is pressed against the elastomer ring using air bellows. The counter surface is supported by a radial and an axial aerostatic bearing. Due to these non-friction bearings the friction torque can be measured during the test run using a force transducer.
Figure 13: Rotary Tribometer
EUROGREASE 3 july/august/september 2012 25
Used Greases Two series of test were done with greases consisting of different thickeners and base oils. Each grease is a laboratory specimen with a known formulation. All greases are free of additives. Test Series 1 – Thickener Type This series of test includes ten greases. Each grease contains the same mineral oil as base oil but a different type of thickener, cf. Table 4. About 90 % of the world grease production includes one of these types of thickener. /4/
Table 4: Greases of Test Series 1 Type of Thickener Percentage of
Thickener [%] Worked Penetration DIN ISO 2137 [mm/10]
NLGI Grade DIN 51818
Li-12-hydroxystrearate Li-12-HS 6 342 0-1
Ca-12-hydroxystearate Ca-12-HS 13 337 1
Li-complex soap type 1 LiX 1 14 338 1
Li-complex soap type 2 LiX 2 10 335 1
Ca-complex soap CaX 21 342 0-1
Al-stearate Al-S 10 341 0-1
Al-Complex Soap AlX 13 322 1
Polyurea PU 9 310 1
Silicic Acid 9 327 1
Organophilic Clay Clay 12 319 1
Base Oil: mineral oil, ν (40°C) = 100 mm2/s, ν (100°C) = 10 mm2/s All greases have nearly the same worked penetration and according to that the same NLGI grade. Therefore the percentage of thickener varies in the range between 6 to 21 %. The tests with the rotary tribometer were done with circumferential speeds of 0.5 and 1.6 m/s and a contact pressure of 1 MPa. This contact pressure is a typical value for the pressure in the contact between radial lip seals and the shaft counter face.
Test Series 2 – Percentage of thickener and type of base oil The greases of the second series of test are shown in Table 5. This series of test includes greases with three different types of thickener. These thickeners are combined with three types of base oil, a mineral oil, a polyalphaolefin and a polyglycol having comparable but not exactly the same viscosities. Each of these greases was manufactured with three different percentages of thickener. The base grease with 15 % thickener was diluted with base oil and homogenized using a three roll mill. All greases are free of additives.
Table 5: Greases of Test Series 2 Type of Thickener
Type of Base Oil
5 % Thickener 10 % Thickener 15 % Thickener
Worked Penetration [mm/10] / NLGI Grade
Li-12-HS mineral oil 354 / 0-1 294 / 2 238 / 3
Li-12-HS POA 345 / 0-1 374 / 0-1 279 / 2
Li-12-HS polyglycol 335 / 1 234 / 0-1 197 / 4
Ca-12-HS mineral oil 373 / 0 279 / 2 223 / 3
Ca-12-HS POA 347 / 0-1 279 / 2 234 / 3
Ca-12-HS polyglycol 395 / 00-0 283 / 2 223 / 3
EUROGREASE 3 july/august/september 2012 26
Silicic acid mineral oil - 339 / 1 212 / 3-4
Silicic acid POA 422 / 000-00 320 / 1 208 / 3-4
Silicic acid polyglycol - 392 / 00-0 324 / 1
Base Oil: mineral oil, ν (40°C) = 108 mm2/s, ν (100°C) = 10 mm2/s
Base Oil: PAO, ν (40°C) = 100 mm2/s, ν (100°C) = 14 mm2/s
Base Oil: polyglycol, ν (40°C) = 100 mm2/s, ν (100°C) = 16 mm2/s The second series of tests included 25 different greases. No tests were run with the greases made of mineral oil and polyglycol and 5 % silicic acid, as the consistency of these two greases was too low to measure the worked penetration. The tests were done running the rotary tribometer with a circumferential speed of 1.6 m/s and a contact pressure of 1 MPa. Test results The following section includes the results of the done tests. The influence of the grease formulation on the friction behaviour is discussed. Operational behaviour during tests The duration of the test was two hours. Figure 14 shows three of the measured friction torques. Every grease in both series of tests showed one of these characteristic friction behaviours during test. In the Type behaviour 1 the friction torque is comparably smooth, sinks to a low level and stays there. In the Type 2 behaviour at the beginning the friction torque shows the same behaviour as in Type 1. But later it starts scattering and jumps between a higher level and the low level. In the Type 3 behaviour, the friction torque jumps quite early to a high level and stays there till the end of the test. Only the second half of the test run was included in evaluation, as the first hour of the test run is a running-in period. During this period, the operational conditions vary because the test rig heats up due to the friction between elastomer ring and counter face.
Figure 14: Measured Characteristics of Friction Torques
Results of Test Series 1 – Type of Thickener Figure 15 shows the measured friction torques of the first test series. The error bars indicate the relative error, which was determined in three repeat experiments using a reference system. The polyurea thickened grease is the only grease with a friction torque showing a Type 3 behaviour. This behaviour was observed at both circumferential speeds. All other greases behave like Type 1 or 2. At the lower circumferential speed of 0.5 m/s they showed all a Type 1 behaviour. The greases with the following types of thickener showed an operational Type 2 behaviour at a circumferential speed of 1.6 m/s: al-stearate, Ca-12-hydroxystearate, lithium complex soap type 1, calcium complex soap and Li-12-hydroxystearate. This causes high friction torques.
EUROGREASE 3 july/august/september 2012 27
Figure 15: Results of Test Series 1
On the contrary, for the greases with the thickener type silicid acid, organiphilic clay, aluminium complex soap and lithium complex soap type 2, an operational Type 1 behaviour of was observed at a circumferential speed of 1.6 m/s. The test runs including these greases were repeated and a longer test time was used. The intention was an evaluation of the point of time of the first jump of the friction torque onto a clearly higher value. As a result of these test runs, a point of time at which the friction torque increase to clearly higher values could be observed for each grease. This result can be seen in Figure 16. As mentioned above, the inner space of the elastomer ring is filled up with grease once before the test run. During the test run, the grease enters the contact zone between the elastomer ring and the counter face and lubricates it. But then the lubricating grease escapes again, cf. Figure 17. At this point of time the friction torque increases, since the grease is no longer able to supply the contact zone with enough lubricant.
Figure 16: Start Time of Increased Friction Torques Figure 17: Emergence of Grease Results of Test Series 2 – Percentage of Thickener and Type of Base Oil The results of the second series of tests are shown in the following section. Influence of the Percentage of Thickener Figure 18 shows all measured friction torques of the second test series. A clear correlation with the worked penetration can be observed. The greases with a higher percentage of thickener, and therefore a lower worked penetration cause higher friction torques. Furthermore an influence of the percentage of thickener on the operational behaviour could be observed. Greases with a high worked penetration showed Type 1 friction torques, those with a low worked penetration showed Type 2 friction torques. An exception was given by the grease with mineral oil as base oil and 15 % silicic acid as thickener.
EUROGREASE 3 july/august/september 2012 28
Figure 18: Influence of the Worked Penetration on the Friction Torque
Influence of the Type of Base Oil The measured frictions torques of test series 2 are itemized by the type of base oil in Figure 19.
Figure 19: Influence of the Type of Base Oil on the Friction Torque
A linear trend line is observed for each type of base oil. The influence of the base oil is evident. The greases with polyclycol as base oil showed the highest friction torques of all greases. The lowest friction torques were measured during the test runs with the greases with mineral oil as base oil. Polyalphaolefine as base oil causes friction torques at a medium level. The approximate parallel trend lines mean that the influence of the base oil is independent from the worked penetration. Depending on the high of the friction torque the test rig heated up to temperatures between 60 and 136°C during the tests. The viscosity of the mineral oil is the lowest and the viscosity of the polyclycol is the highest at these temperatures, cf. Table 2. This means that the height of the friction torque depends on the viscosity of the base oil. Influence of the Type of Thickener Figure 20 shows the measured frictions torques of test series 2 itemized by the type of thickener.
EUROGREASE 3 july/august/september 2012 29
Figure 20: Influence of the Type of Thickener on the Friction Torque
The highest measured friction torques were noted for the greases with Li-12-hydroxystearate as thickener. The greases thickened with Ca-12-hydroxystearate showed friction torques of a medium level. The lowest friction torques could be observed in the test runs with the greases with a silicic acid thickener. The linear trend lines tend to the same values in the area at high worked penetrations. These greases contain a low percentage of thickener, and therefore the thickener’s influence on the operational behaviour is small. With growing percentage of thickener and NLGI grade the trend lines move away from each other. This indicates a growing influence of the type of thickener if more thickener is included in the grease. Summary The investigations performed demonstrate a clear influence of the grease formulation on the operating behaviour of a grease lubricated elastomer-steel contact. Several factors, such as base oil nature, type and percentage of thickener, play an important role on the value and characteristic of the friction torque. Greases with a high amount of thickener showed high values of the friction torque compared to greases with less thickener. The influence of the type of base oil on the value of the friction torque is independent from the worked penetration. In the tests greases based on polyglycol showed the highest friction torques. The friction torques of greases with polyalphaolefine and especially mineral oil as base oil were conspicuously lower.
The influence of the type of thickener depends on the amount of thickener. Greases with a high worked penetration showed no measurable influence of the type of thickener. However, this influence grows with decreasing worked penetration. This effect is best visible for greases with a Li-12-hydroxystearate thickener. For greases with a Ca-12-hydroxystearate thickener, or especially silicid acid, this effect is less pronounced. The influence of the grease formulation is most noticeable in the friction torque measured for greases with 15 % of thickener. The measured values reach from 0,24 Nm (mineral oil + silicid acid) to 0,76 Nm (polyglycol + Li-12-hydroxystearate). This represents an increase of the friction torque of about 300 %, caused by a change of the grease formulation, at a comparable worked penetration. Outlook At this time, rheological measurements of the greases are in progress. The measured rheological parameters will be integrated with the presented tribological tests, with the aim of establishing a correlation between rheological parameters and the tribological behaviour of an elastomer-steel contact. Such a correlation will be helpful in evaluating the influence of grease on the operational behaviour of radial lip seals. Acknowledgments This research project (IGF-Nr. 16090 N/1) was funded by the German Federal Ministry of Economics and Technology (BMWi) by means of the research association ”Arbeitsgemeinschaft industrieller Gemeinschaftsforschung (AiF)”.
EUROGREASE 3 july/august/september 2012 30
References /1/ Müller, H. K.: Abdichtung bewegter
Maschinenteile, Medienverlag Müller, Waiblingen 1990.
/2/ Dürnegger, W.: Fette mittels Radial-Wellendichtungen zuverlässig abdichten, FKM-Forschungsheft 302, Frankfurt a. M., 2009.
/3/ Deutsches Institut für Normung: DIN 3760 Radial-Wellendichtringe, 1996.
/4/ NLGI: Grease Production Survey Report, Kansas City, 2007.
/5/ Deutsches Institut für Normung: DIN ISO 2137 Schmierfett und Petrolatum – Bestimmung der Konuspenetration, 1997.
/6/ Deutsches Institut für Normung: DIN 51818 Konsistenz-Einteilung für Schmierfette, 1981.
______________________________________________________
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EUROGREASE 3 july/august/september 2012 31
Surface analysis – A powerful tool in the development and testing of new lubricants
Presented at the 24th ELGI Annual General Meeting 2012 Munich Germany
Dr. Adam Orendorz
[email protected] Co-authors: Dr.-Ing. Marius Kuhn, Dipl.-Ing. (FH) Philipp Staub, Dr. Michael Rankl
Klüber Lubrication München KG, Munich – Germany 2003 Diploma in Physics, University of Kaiserslautern, Germany 2008 Doctoral Degree in Surface Physics, Technical University of Kaiserslautern, Germany 2008 – 2010: Research Trainee at Freudenberg Forschungsdienste KG, Weinheim, Germany Since 2010: Specialist for material and surface analysis at Klüber Lubrication München KG, Munich, Germany 1. Introduction High performance lubricants are designed for concrete applications by choosing convenient base oils, thickeners, additives and solid lubricants. While the choice of base oils and thickener is very often determined by applications e.g. compatibility with elastomers, H1 classification, thermal stability, regarding additives the choice is rather complex. On the one hand there are synergistic and antagonistic interactions between different additives, on the other hand the effectiveness of additives is determined by types of friction and base oils itself. Hence there is a strong demand for
innovations supporting the development process of lubricants in the lubricant industry. Because EP /AW additives are interacting with surfaces of the friction partners, surface analysis is suitable for detailed investigations of additive performance and reaction products. 2. Tribological reaction layers In the boundary and mixed friction regime, the surfaces of the friction components are in partial contact (figure 1).To avoid welding and wear under such frictional conditions, metal surfaces have to be passivated by extreme pressure (EP) / anti-wear (AW) additives.
Figure 1: Left side: Boundary friction – the surfaces of the friction components are in severe contact; right side: Mixed friction – the surfaces of the friction components are in partial contact, i.e. not completely separated by
lubricating film. Both types of additives react physico-chemically on metal surfaces [1-3]. First, either the additives or their decompositions adsorb on the surface. After adsorption a chemical reaction takes places due to the
EUROGREASE 3 july/august/september 2012 32
energy which is put into this tribologocal system. At mixed friction very often a polymer or glass-like protection film, e.g. polyphosphates is developed by the additives themselves. In the boundary friction regime, a decomposition of the additives and chemical reaction with the solid material beneath take places, thus forming an inorganic layer containing elements from the lubricant as well as from the material, e.g. iron sulphides [1-3]. According to the results discussed later in this paper and in agreement with literature [4,5] a natural tribological layer contains regions with chemical changes as well as adsorption (figure 2).
Figure 2: Schematic diagram of a reaction layer and the surface near reagion of a steel material after tribological
contact. 3. Surface analysis methodology 3.1. General approach In principle, there are two approaches to analyse a tribological system. Either, you can try to analyse it “in-situ” running the test rig or you can take your sample out of the test rig after the measurement for further analysis (“ex-situ”). Both approaches have advantages and disadvantages. In in-situ measurements you can observe the behaviour of the lubricant in the lubrication gap while a system is running. But an in-situ analysis is usually restricted in the choice of instruments or tribological conditions. For ex-situ investigations there is a broad variety of analytical tools, but you can only do measurements after stopping the tribological test. Furthermore, by taking the sample out of the tribological system and due to a likely preparation, there is always the risk of contamination and modification of the sample. Although both approaches are found, ex-situ analysis methods are used more often in practice. 3.2. Types of Information Every analytical technique delivers a certain kind of information e.g. about the topography, chemical composition, and mechanical properties (figure 3). By combination of different techniques it is possible to complete this information to get an overall impression of the sample.
Figure 3: Types of information attained by surface analysis methods.
EUROGREASE 3 july/august/september 2012 33
3.3. Surface and topography The first information about the surface can be collected by visual and microscopic methods. Basic light microscopy is restricted especially at higher magnifications to its depth of sharpness. Therefore, electron microscopy, SEM is used very often to analyse pitting and scuffing in detail. Although, some electron microscopy might appear very stereoscopic, the techniques mentioned above deliver only 2D information. For further information about surface roughness or amount of wear it is necessary to use either tactile systems or optical systems, e.g. white light interferometry or confocal light microscopy. 3.4. Chemical composition The chemical composition of reaction layers can be analysed by different methods. They all have their strengths and weaknesses. Photoelectron spectroscopy, XPS (≡ electron spectroscopy for chemical analysis, ESCA) and Auger electron spectroscopy, AES, have a good lateral resolution, but they usually have detection limits of about 0,5 – 1 % for interesting elements like phosphorus and sulphur [6]. Secondary neutral mass spectrometry, SNMS, has a good depth resolution and detection limits in the ppm-range but has only a low lateral resolution of about 2 – 4 mm [7]. With these techniques it is possible to analyse the elemental composition of reaction layers in the nm-range. For molecular composition analysis of reaction layers only time of flight secondary ion mass spectrometry, ToF-SIMS, can be used. Unfortunately, this technique is not quantitative and has problems to detect molecules and molecular fragments, which are not well ionisable [7]. 3.5. Structure Microsections are very common in material analysis to understand changes in material properties e.g. hardness, ductility due to different processing or working conditions. Though, for microsections in the nm-region it is no longer possible to use preparation techniques like grinding disc and light
microscopy. An efficient way to get microsections of reaction layers is a combination of focussed ion beam together with the transmission electron microscope [8]. 3.6. Mechanical properties While the former techniques are already well established, there are only few investigations about the mechanical properties of tribological reaction layers [9-11]. Two techniques which seem to deliver that type of information about reaction layer are nanoindentation and atomic force microscopy, AFM. Nevertheless, both methods are sensible to surface roughness. Therefore, all information about hardness, ductility and friction coefficient of reaction layers collected on technical samples have to be handled with care. 4. Assisted development of lubricants In figure 4 cylindrical roller bearings have been analysed by SNMS. Both bearings ran on a FE8 test rig at similar test conditions. The Bearing with grease sample 1 failed after 470 h showing many indentations in the raceway due to strong pitting. Measurements after the test have shown that the concentration of phosphorus has been enriched only slightly at the surface compared to the amount of this element in the grease. Phosphorus was one of the fingerprint elements of the AW additives in this grease sample. Therefore, this grease was modified by exchanging the AW additive. The new grease was labelled grease sample 2 and the bearing at the FE8 test run 715 h before failure. Similar analysis using SNMS technique revealed an increase of phosphorus from 2 at-% to 6 at-% at the surface indicating a formation of an AW layer this time due to tribological strain. The corresponding macroscopic analysis of the surface revealed a strongly changed appearance due to the chemical modification and the high forces applied in the test rig but no pitting.
EUROGREASE 3 july/august/september 2012 34
Figure 4: Two SNMS measurements on cylindrical roller bearings after FE8 measurements with corresponding macroscopic images from the racetrack. Grease sample 2 has an adjusted EP/AW additive formulation after grease
sample 1 didn’t show enough EP/AW performance in the tribological testing. 5. Summary Several analytical techniques can be used to understand how modern lubricants perform at the friction point. Furthermore, as shown in chapter 4, surface analysis can assist in the development of lubricants. Through better understanding of processes in the friction point testing time, can be significantly reduced. Bibliography [1] Z. Pawlak – Tribochemistry of Lubricating Oils, Elsevier (2003) [2] L.R. Rudnick (Ed.), W.D. Phillips – Lubricant Additives – Chemistry and Applications, p. 45 – 111,
Marcel Dekker Inc. (2003) [3] Q. Xue, W. Liu – Lubrication Science 7 (1), p. 81 – 92 (1994) [4] Czichos, H. / Habig, K.-H. – TribologieHandbuch,Vieweg+TeubnerVerlag (2010) [5] FVA Research Project 289 I & II – Triboschutzcharakterisierung (2000) [6] FVV Research Project 616 – Tribomutation / Zylinderzwickel (1997) [7] Bubert, H. / Jenett H. – Surface and Thin Film Analysis, Wiley-VCH Verlag GmbH (2002) [8] FVA Research Project 289 Ib&IIb – Triboschutzschichten II (2004) [9] Bec, S. et al. – Proceedings of the Royal Society A 455,p. 4181–4203 (1999) [10] Pereira, G. et al. – Tribology 1 (1),p. 4 – 17 (2007) [11] Naveira Suarez, A. et al. – Tribology International 43 (12), p. 2268 – 2278 (2010)
EUROGREASE 3 july/august/september 2012 35
ELGI Technical Papers published in Eurogrease 1991-2012 The complete list of technical papers published from 1991 to 2012 is available on the website www.elgi.org / publications. All past papers published are being collated electronically and will be available to our members to download in due course. Herewith, an example of the titles of the technical papers published in 2011 Eurogrease magazine. Date Eurogrease Publication Author(s) Title Technical Paper
2011 04 October/November/December
P. M. Lugt, A. van den Kommer, H. Lindgren, C. Roth
The ROF+ methodology for grease life testing
2011 04 October/November/December
S. Rovinetti, M. Avataneo, M. Beltramin, G. Boccaletti, V. Carsetti, G. Marchionni, F. Riganti, A. Russo
The new frontier of fluorinated lubricants
2011 03 July/August/September
M. Jungk
Comparison testing of solid lubricants as dispersion, grease, paste and powder
2011 03 July/August/September
A Medzhibovskiy
Specifics of energetic effect of anti-wear additives (friction modifiers) in lubricants
2011 03 July/August/September
L. Honary
A status update on manufacturing biobased grease with microwaves
2011 02 April/May/June
D. Devore, S. Wang
A Study of polymer additives in mineral oil and vegetable oil-based
2011 02 April/May/June
P. Bessette
The advantages and disadvantages of attenuated total reflectance, ATR, infrared spectroscopy
2011 02 April/May/June
S. Hausmann
Grease Thickeners - REACh registration progress (ERGTECF)
2011 02 April/May/June
P. Boogaard
Toxicity of lithium salts - how bad are they? (ERGTCEF)
2011 02 April/May/June
E. Rushton
Classification and labelling of products (CLP ERGTECF)
2011 01 January/February/March
M. Fiedler
Complexity of trilbological characterizations illustrated with poly-alpha-olefin grease
2011 01 January/February/March
B. Koch, T. Litters, N. Zaki
Influence of base oil polarity and thickener type on visco-elastic properties. Investigations with strain sweep rheometry at +25 ̊ C and +80 ˚C
EUROGREASE 3 july/august/september 2012 36
Patech Fine Chemicals Co. Ltd.No. 41, Alley 1, Lane 420, Kuang-Fu S. Rd.,Taipei 10695, TaiwanWebsite : www.patechfc.com.twE-mail: [email protected]
PATECH FINE CHEMICALS Co. has been manufacturing a wide variety of high quality ester type oleo-chemical derivatives and proved ourselves as a valuable partner in the European, US, Japan, China, South East Asia and Taiwanese markets.
Patech’s business policy was based on developing long-term strategic partnership with our customers.
Our esters are used in many special applications such as: LUBRICANTS(Industrial and Automotive application), REFRIGERATION and AIR-CONDITIONING OILS, PLASTICS (Plasticizers, Internal & External Lubricants for PVC and Engineering Plastics) and COSMETIC (Skin Care, Hair Care, Sunscreen, Make Up....).
Apart from standard list of esters, we produce custom made esters as well. Our R&D department is readily involved in design of special esters for certain customer's application/projects, and working very often with end user’s R&D department.
For European customers we deliver esters from our storage in Rotterdam where all currently supplied esters are stocked. Delivery could be in IBC, Drums and in Road Tanks.
Our European customers could contact our office in UK and talk to Mr. Ranko Pilic.Tel: 00 44 1892 615 698Mobile: 00 44 75 00 955 023E-mail: [email protected]
EUROGREASE 3 july/august/september 2012 37
Patent Search Dear Reader We are introducing an overview on grease related patents in our EUROGREASE magazine. The patents are collated into different groups based on their main focus: additive, base oil, grease, heat conductive. We hope to add more groups to this list in the future. There is a differentiation between patent applications and patent documents within each group. We hope that this new initiative will be of value to you and we welcome your comments, suggestions or contributions. Josef Barreto-Pohlen ELGI Board Secretary Tunap [email protected]
Focus Pat.-No Type Title
Additive US 2012/0108480 A1 patent application Lubricant additives
US 2012/0122743 A1 patent application Lubricant and synergistic additive formulation
US 2012/0122744 A1 patent application Imides and bis-Imides as friction modifiers in lubricants
WO 2012/048201 A2 patent application Lubricants containing nanofibres
AU 2007280548 B2 patent document Lubricant composition
EP 2078725 B1 patent document Phosphorus-molybdenum compound, method for producing the same, lubricant additive containing the compound, and lubricant composition
EP 2195404 B1 patent document Titanium compounds and complexes as additives in lubricants
EP 2260091 B1 patent document Use of a lubricating grease composition on the basis of ionic liquids
US 8207098 B2 patent document Lubricant additive, lubricant composition and grease composition
Base Oil EP 2014750 B1 patent document High viscosity lubricant copolymers
EP 2344581 B1 patent document Improved HVI-PAO bi-modal lubricant compositions
US 2012/0129746 A1 patent application Modified vegetable oil lubricants
Grease EP 2447348 A1 patent application Grease composition
EP 2457983 A1 patent application Lubricant of solid or liquid consistency, exhibiting low coefficient of friction (=US 2012/0135897 A1)
EP 2462209 A2 patent application A grease composition and methods for manufacturing the grease composition
EP 2465916 A1 patent application Grease composition and machine component
EUROGREASE 3 july/august/september 2012 38
Focus Pat.-No Type Title
EP 2467461 A1 patent application Lubricating grease compositions
US 2012/0098269 A1 patent application Grease composition
US 2012/0106881 A1 patent application Grease for slide bearing
US 2012/0122742 A1 patent application Lubricant stick formulations
US 2012/0135897 A1 patent application Lubricant of solid or liquid consistency, exhibiting low viscosity ratio (=EP 2457983 A1)
US 2012/0142566 A1 patent application Grease composition and mechanical part
US 2012/0149613 A1 patent application Grease composition and methods for manufacturing the grease composition
US 2012/0149614 A1 patent application Grease, rolling bearing, constant velocity joint, and rolling parts
US 2012/0149616 A1 patent application Water-based lubricants
US 2012/0165104 A1 patent application Grease composition
US 2012/0190602 A1 patent application Lubricating grease compositions
US 2012/0195678 A1 patent application Grease composition and constant velocity joint
US 2012/0196781 A1 patent application Grease composition for bearing of wind power generator
WO 2012/053575 A1 patent application Grease composition
WO 2012/055821 A1 patent application Lubricant thickened with oleophilic fibres
WO 2012/057181 A1 patent application Lubricating grease composition
WO 2012/064246 A1 patent application Process for rapid transesterification of a fat and a semisolid grease produced according to the process
WO 2012/076025 A1 patent application Polymer thickened grease compositions and their use
WO 2012/076638 A1 patent application Polymer thickened grease compositions with improved low friction properties
WO 2012/080939 A1 patent application Composition de graisse [Grease composition]
WO 2012/080940 A1 patent application Composition de graisse [Grease composition]
WO 2012/082890 A1 patent application Thickened grease composition
WO 2012/090722 A1 patent application Grease composition, grease pre-lubricated bearing, universal joint and linear motion device
WO 2012/090846 A1 patent application Grease composition
EUROGREASE 3 july/august/september 2012 39
Focus Pat.-No Type Title
WO 2012/091019 A1 patent application Bearing grease
WO 2012/093731 A1 patent application Imide compound, method for producing same, thickening agent for grease, and grease composition
EP 0911382 B1 patent document Grease composition for rolling bearings
EP 1831338 B1 patent document Urea-based lubricating grease composition
EP 1840195 B1 patent document Grease composition for constant velocity joint and constant velocity joint
EP 1953213 B1 patent document Grease composition for constant velocity joint and constant velocity joint
EP 2300581 B1 patent document Lubricant composition based on natural and renewable raw materials
US 8153568 B2 patent document Water-resistant grease and water-resistant-grease-enclosed rolling bearing and hub
US 8167726 B2 patent document Constant velocity joint grease cap with increased torsional compliance
US 8182155 B2 patent document Lubricating grease and lubricating grease-enclosed roller bearing
US 8183191 B2 patent document Grease composition
US 8188016 B2 patent document Lubricant composition and bearing using same
US 8193133 B2 patent document Process for preparing fine powder polyurea and greases there from
US 8211839 B2 patent document Non-corrosive EP grease composition
US 8216983 B2 patent document Grease composition for use in constant velocity joint and constant velocity joint
US 8216985 B2 patent document Grease composition and grease-enclosed bearing
US 8242063 B2 patent document Lubricating grease composition
US 8242065 B2 patent document Grease composition
Heat Conductive EP 2439241 A1 patent application Moisture-thickening heat-conductive silicone
grease composition
EP 2455339 A1 patent application
Magnesium oxide particles, method for producing same, heat dissipating filler, resin composition, heat dissipating grease, and heat dissipating coating composition
US 2012/0085964 A1 patent application Moisture-thickening heat-conductive silicone grease composition
WO 2012/067247 A1 patent application High durability thermally conductive composite and low pump-out grease
EP 1535988 B1 patent document Heat-dissipating silicone grease composition
EUROGREASE 3 july/august/september 2012 40
Forthcoming Events
ELGI Board Meeting
November 2012 ELGI Board Meeting
ELGI Working Groups
Next meeting date to be confirmed Joint Grease Cleanliness WG Meeting
26th October 2012 UEIL Conference Lisbon Joint Food Grade Lubricants WG Meeting
28th November 2012 Amsterdam Test Methods WG & Joint Bio-Based Greases WG Meetings
29th November 2012 Amsterdam Railway Lubricants WG Meeting
Other meetings
04-07 September 2012 38th Leeds-Lyon Symposium on Tribology Leeds UK [email protected]
18-20 September 2012 SAE International Powertrain, Fuels & Lubricants Conference Malmo Sweden
19-20 September 2012 ACI 4th Annual European Base Oils and Lubricants Summit Prague www.acieu.net
02-04 October 2012 SAE Commercial Vehicle Engineering Congress Rosemont USA www.sae.org
04-05 October 2012 Lubgrax Meeting Espaco Apas Sao Paulo Brazil www.lubgrax.com.br
08-10 October 2012 STLE International Joint Tribology, Conference Denver USA http://www.sae.org/events/pfl/index.htm
10-11 October 2012 9th ICIS Middle Eastern Base Oils & Lubricants Conference Dubai www.icis.com
13-16 October 2012 ILMA Annual Meeting Arizona USA www.ilma.org
23-25 October 2012 Parts2clean Trade Fair Stuttgart Exhibition Centre Germany www.parts2clean.de
24-26 October 2012 UEIL Congress Lisbon Portugal www.ueil.org
01-02 November 2012 International Lubricants & Waxes Meeting Texas USA www.npra.org
07 November 2012 UKLA Annual Dinner London UK [email protected] www.ukla.org.uk
07-08 November 2012 ICIS African Base Oils & Lubricants Conference Durban SA
www.icisconference.com/africanbaseoils
07-10 November 2012 NORA Annual Recycling Conference & Trade Show Florida, USA
www.noranews.org
13-16 November 2012 8th International Conference Lubricants Russia Moscow www.rpi-conferences.com
29-30 November 2012 8th ICIS Pan-American Base Oils & Lubricants Conference New Jersey USA
www.icis.com
02-06 December 2012 ASTM Committee D-2 on Petroleum Products & Lubricants Norfolk VA USA
www.astm.org
15-17 January 2013 Fuels: Conventional & Future Energy for Automobiles Stuttgart/Oslfildern
www.tae.de/fuels
21-24 January 2013 OilDoc Conference / Exhibition 2013 Rosenheim Bavaria Germany www.oildoc.com
21 March 2013 Argus European Base Oils Markets Istanbul [email protected]
24-26 March 2013 International Petrochemical Conference San Antonio USA
09-10 April 2013 UNITI Mineral Oil Technology Congress 2013 Stuttgart Germany www.umtf.de
20-23 April 2013 25th ELGI AGM Amsterdam The Netherlands www.elgi.org [email protected]
15-18 June 2013 80th NLGI Annual Conference Loews Ventana Canyon Tucson Arizona
www.nlgi.org / [email protected]
03-06 September 2013 Oil and Gas Conference and Exhibition Aberdeen United Kingdom www.offshore-
europe.co.uk
08-13 September 2013 5th World Tribology Congress Torino (Italy) http://www.wtc2013.it/
21-23 January 2014 19th International Colloquium Tribology “Industrial and Automotive Lubrication
Ostfildern Germany www.tae.de
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