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Basic 14Basic 14Micro-Nano TribologyMicro Nano Tribology
- Ultra low friction of Carbon Nitride (CNx) andand
Low adhesion and friction of rubber -
Prof N UmeharaProf. N. UmeharaDept. of Mechanical Science and Engineering,
N U i itNagoya University
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
-
Outline
1.Ultra low friction of Carbon Nitride (CNx)・ Mechanism
・ Effect of carbon overcoat on frictionEffect of carbon overcoat on friction
2 Low adhesion and friction of rubber2.Low adhesion and friction of rubber・ High dense plasma irradiation to CllR
UV i di ti t TPE ith PFPE・ UV ray irradiation to TPE with PFPE
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
-
1. Ultra low friction of Carbon Nitride(CNx)
A.Y.Liu, M.L.Cohen, Prediction of new lowcompressibility solids, Science, 245 (1989) 841 842841-842.
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
-
Introduction
(K.J.Wahl, Naval Research Laboratory)
0.1nt
PTFE (=0.04) Lubrication with
transfer film
0.01oeffi
cien
MoS2DLC
Lubrication with tribochemical film?Lubrication with
rictio
n co
MoS2(UHV)
Lubrication with absorbed gas?
After the annual
0.001
Fr H:DLC(N2)a-CNx(N2)
meetingof STLE, 2001
Period1980 1990 2000
MoS2; W.E.Jamison (1986)2; ( )DLC; A.Erdemir (1991), J.Franks, K.Enke and A.Richardt (1990)H:DLC; A.Erdemir (1999), C.Donnet(1998)a CNx; N Umehara K Kato(1998)
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
a-CNx; N.Umehara, K.Kato(1998)
-
Introduction
C b it id ( CN ) tiCarbon nitride(a-CNx) coatingHigh hardnessHigh wear resistanceHigh wear resistanceLow friction
Excellent tribological properties
Hardness: Ha-CNx/Ha-C=1.31Low friction coefficient(against Al O /TiC slider )Low friction coefficient(against Al2O3/TiC slider )
B.Wei et al. (1998)
Durability: Da-CNx/Da-C=3~4 (against Al2O3/TiC pin) E.C.Cutiongco et al. (1996)
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
-
Ion Beam Assisted DepositionSputtering:
Ar ion beam 1kV 100mAAr ion beam 1kV, 100mA
Mixing:
N ion beam 0.5keV,
30A/cm2
Coating time:90min
Thickness of coating:100nm
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
-
TEM photo of CNx by IBAD and Hardness
・Hardness 21GPaA h t t・Amorphous structure
・N=C bonds38) Micro-wear Mechnaisms of Thin Hard Coatings Sliding against Diamond Tip of AFM,
ASME, Advances in Information Storage Systems, 9 (1998)289-302.K. Kato, H. Koide, and N. Umehara
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
, ,
-
Effect of ambient gas on friction coefficient0.5
Pin: Si3N4 ball (r=4.0mm)
0.3
0.4
effic
ient
Disk: CNx (t=100nm)Normal load:100mNFriction cycles:240cycles
0.36
0 1
0.2
ctio
n co
e
0 05
0.16
0
0.1
in Air in high vacuum
in N2 in CO2 in O2
Fric 0.030.0090.05
(N Umehara and K Kato 1998)
vacuum(2x10-4Pa) (7x104 Pa)
(N. Umehara and K. Kato , 1998)
Running-in is important for ultra low friction of CNx.g pSomething changed during running-in.
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
-
Raman spectroscopy after running-in
0.16
0 10
0.12
0.14 in N2
in vacuumic
ient
0.06
0.08
0.10tio
n co
eff
0.02
0.04Fric
t
02.0 2.2 2.4 2.6 2.8 3.0
ID / I
G
Large ID/IG provides small friction coefficientIncrease in the number or size of small graphitic domain
N. Umehara, M. Tatsuno, K. Kato, Proc. Int. Trib. Conf. Nagasaki(2000)1007.
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
-
XPS before and after running-in
C=N C-NC=N
N-O N-O
C-N
N-O N-O
(b) wear track after 240 cycles in N2 gas
(a) a-CNx coating2 g
After running-in in N2 gasAfter running in in N2 gas, C=N increases larger than C-N.
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
-
Depth profile of N after running-in in various environment
0 30
0.35 Beam energy: 5 kV, Beam current: 10 nASputtering energy: 3 kV, Sputtering current: 25 mA
0.25
0.30ns
ityp g gy p g
nsity CNx
Si(100)
d
Si(100) Si(100)
0.20
B in
ten
k in
te as-deposit CNx
0.10
0.15
1s P
/B
in N2approximate curve
Pea
k
< 0 01
0.05
0.10N in N2
i A
in O2N1s
< 0.01
≒ 0 030.00
0 10 20 30 40 50
in Ar ≒ 0.03
0 10 20 30 40 50Sputtering depth d, nm
T k U h IIP S i A l ti f JSME S t 11 2007Basic 14 Micro-Nano Tribology Prof. N. Umehara
- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
Tokoroyama, Umehara,IIP Session, Annual meeting of JSME,Sept. 11,2007
-
Self surface modification in the running-in process
In N2 gas
Low shearing strength layerlayer
100nm 10~20 nm
CNxCNx
Si substrateBasic 14 Micro-Nano Tribology Prof. N. Umehara
- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
Si substrate
-
Outline & Summary1.Ultra low friction of Carbon Nitride (CNx)・Mechanism Self modification in nm thickness・Mechanism Self modification in nm thickness ・Effect of carbon overcoat on friction
・Effect of Ultraviolet (UV) ray irradiation on friction
2. Low adhesion and friction of rubber・High dense plasma irradiation to CIIRHigh dense plasma irradiation to CIIR
・UV ray irradiation to TPE with PFPE・UV ray irradiation to TPE with PFPE
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
-
Enhancement of running-in of CNxith thi k b twith nm thickness carbon overcoat
Carbon layer without Nwithout N
C N
CNx on Si(100)
Si(100)( )
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
-
Effect of 3nm thickness carbon overcoat on friction of CNx
0.25
0.30
020
CNx (150nm) + C coat ing (0 nm) on Si (100) Sliding speed V: 0 .13m/s, Surface pressure: 33 MP a Si3N4 ball in N2
Only CNx0.15
0.20on
coe
ffici
ent μ
0.00
0.05
0.10
0.15
0.20
μ
C
CNx
Only CNx
0 00
0.05
0.10
Fric
tio 0 50 100 150 200 250N
0.30
0.000 4000 8000 12000 16000 20000
Number of cycles N, cycles
0.20
0.25
0.30
ent μ
0.20
C
CNx (150nm) + C coating (3 nm) on Si (100) Sliding speed V:0.13m/s, Surface pressure: 33 MPa Si3N4 ball in N2
3nm C + CNx
0.10
0.15
rictio
n co
effic
ie
0 00
0.05
0.10
0.15
μ
C
CNx
Proc ICMDT
0.00
0.05
0 4000 8000 12000 16000 20000
F 0.000 50 100 150 200 250
N
Proc. ICMDT Sapporo,2007,Tokoroyama, Wang, Umehara Fuwa
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
0 4000 8000 12000 16000 20000Number of cycles N, cycles
Umehara, Fuwa
-
Outline & Summary
1.Ultra low friction of Carbon Nitride (CNx)M h i S lf difi ti i thi k・Mechanism Self modification in nm thickness
・Effect of carbon overcoat on frictionnot need running-in
・Effect of Ultraviolet (UV) ray irradiation ( ) yon friction
2. Low adhesion and friction of rubber・High dense plasma irradiation to CIIR・High dense plasma irradiation to CIIR
UV i di ti t TPE ith PFPE・UV ray irradiation to TPE with PFPE
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
-
The expectation of ultraviolet ray irradiation to CNx
The light energy UVExpected resultC-N bond: 305 kJ/mol
h: Planck’s constant, ν: frequency, chhE Energy of photon The light energy
Wavelength<390 nm
C
c: light velocity, λ: wavelength hhE
Braking ofh: Planck’s constant, ν: frequency,c: light velocity λ: wavelength
N
CC
N NCC C
CN
C
CN
C
NC C C
CC
N
CC CC C
C
CC
C
C C C
CC
CCC C
CEnergy of photon per mol
ANchE
C-N bondc: light velocity, λ: wavelength
NC CC N CC C C
CC
CC
N
NC CC
CN
CC C C
CC
CC
N
C
NA: Avogadro’s constant Nitrogen desorption ⇒ Structural change
We assumed that the variable UV wavelength to obtain superlow friction
We focused on Nitrogen content in CNx.J. Wei et al. Surf Interface Anal. 28(1999) 208-211
g pchanged with the Nitrogen content in CNx coating because of its structure.
Nitrogen content ratio 0 9 12 19% was prepared CN ( content)e.g.
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
Nitrogen content ratio 0,9,12,19% was prepared CN0.09(x=content)
-
Background –Effect of UV irradiation
C N bond: 305 kJ/molC – C bond: 348 kJ/mol
C-N bond: 305 kJ/mol
365 nm 254 nm312 nm
329 kJ/mol
382 kJ/mol
469 kJ/mol
C – H bond for CH4 : 416 kJ/mol
Energy of photonh Pl k’ t t f
chhE
gy ph: Planck’s constant, ν: frequency,c: light velocity, λ: wavelength
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
-
Experimental – Ultraviolet ray irradiation to CNx coating
Table 2 UV irradiation condition
Did Nitrogen atoms desorb from CNx coating with UV irradiation?Table 1 The energy of each wavelength
Wavelength , nm Energy, kJ/mol Test pieces Irradiation time
Table 2 UV irradiation conditionTable 1 The energy of each wavelength
365 312
326382
•CN0 •CN0.09
•60 min•120 min
254 4690.09
•CN0.12•CN0 19
•180 min•240 min
u.)
C KLL
N KL
L
O KL
L
0.19
AES analysis
lized
inte
nsity
(a.
C=1
150 250 350 450 550
Nor
mal
N=x
N/C ratio: N/C=x/1Basic 14 Micro-Nano Tribology Prof. N. Umehara
- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
150 250 350 450 550Kinetic energy, eV
/C a o /C /
-
J. M. Ripalda et al. Diam. Relat. Mater. 7(1998) 402-406.XPS analysis resultsCN0.12 N1s peak
As deposit UV 365 nm 120 min irradiation
What kind of deformation did it take place?As-deposit UV-365 nm 120 min irradiation
(a.u
.)
N1s
N-C sp3N-C sp2 N1s
N-C sp2
y (a
.u.)
Inte
nsity
N C spN-N/N-O N-C sp
3
N-N/N-OInten
sity
I th f it d ti t t l d f ti t k l
390395400405410Kinetic energy, eV
390395400405410Kinetic energy, eV
In the case of no nitrogen desorption, structural deformation took place.
CN0.09,CN0.19 showed deformation.Triphenilamine
In the case of UV irradiation to CNx, the bond originated from N-C sp2
NN The bond shows like graphite was
assumed to increaseBasic 14 Micro-Nano Tribology Prof. N. Umehara
- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
increased. assumed to increase.
-
Experimental of tribological property under N2UV i di ti diti
Wavelength Irradiation time
UV irradiation conditionsUV irradiation ⇒ Friction in N2
UV In N R t ti•365 nm•312 nm
•60 min•120 min
LoadIn N2 Rotation
312 nm•254 nm
120 min•180 min•240 min
CNx•240 min
Friction test conditionsFriction test conditions
Load 0.1 NSliding speedRotation speed
4.19×10-2 m/s200 rpm
Rotation radiusAmbient
2.0 mmNitrogen
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
g
-
1 0
Friction test results under N2 environment
0 60.70.80.91.0
ffic
ient
As-deposit365 nm-60 min365 nm-120 min365 nm-180 minThe running-in period of CN0 12
Sliding speed V: 4.2×10-2 m/s,
Load W: 0.1 NCNx coating (0.1 m) on Si(100)
Si3N4(8 mm) ball
CN0.12 365 nm-UV irradiation
0 20.30.40.50.6
Fric
tion
coe 365 nm 180 min
365 nm-240 minThe running in period of CN0.12
was decreased by UV irradiation3 4
In N2
The variation of
0.91.0
As-deposit0.00.10.2
0 1000 2000 3000 4000 5000N mber of sliding c cles N C cles
Sliding speed V: 4.2×10-2 m/s,
Load W: 0 1 N
with number of cycles
0 60.70.80.9
ffic
ient
365 nm-60 min365 nm-120 min365 nm 180 min
Number of sliding cycles N, CyclesLoad W: 0.1 NCNx coating (0.1 m) on Si(100)
Si3N4(8 mm) ball
In N2
As deposit: =0 040
The average of 5000~10000 cycles
0.40.50.6
ctio
n co
ef 365 nm-180 min365 nm-240 min
As-deposit: =0.04060 min: =0.019↓120 min: =0 018↓
0 10.20.3Fr
ic 120 min: =0.018↓180 min: =0.022↓240 min: =0 015↓
0.00.1
0 5000 10000 15000
240 min: =0.015↓
decreased by UV irradiation
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
Number of sliding cycles N, Cycles irradiation.
-
The effect of UV irradiation on running-in period
Running-in As-deposit:3100 cycles
-
3.4 The effect of UV irradiation on minimum mCN0.19
As-deposit: =0.040 ⇒ 312 nm-120 min: =0.004
The minimum friction coefficient: min
0 080.090.10
cien
t av
e
365 nm312 nm
Sliding speed V: 4.2×10-2 m/s, Load W: 0.1 N
CN coating (0 1 m) on Si(100)
p
0.050.060.070.08
ctio
n co
effic
312 nm254 nm
CN0.19 coating (0.1 m) on Si(100)Si3N4(8 mm) ball
in N2
0.020.030.04
Ave
rage
fric
0.000.01
0 60 120 180 240UV i di i i T i
A
UV irradiation time T, min
CN0.09 As-deposit: =0.028 ⇒ 254 nm-120 min: =0.002Minimum friction coefficient
CN0.12 As-deposit: =0.033 ⇒ 365 nm-60 min: =0.008
The friction coefficient decreased by UV irradiationBasic 14 Micro-Nano Tribology Prof. N. Umehara
- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
The friction coefficient decreased by UV irradiation.
-
Outline & Summary1.Ultra low friction of Carbon Nitride (1.Ultra low friction of Carbon Nitride (CNxCNx))・・MechanismMechanism Self modification in nm thicknessSelf modification in nm thicknessMechanism Mechanism Self modification in nm thickness Self modification in nm thickness ・・Effect of carbon overcoat on frictionEffect of carbon overcoat on friction
not need runningnot need running--inin・・Effect of Ultraviolet (UV) ray irradiationEffect of Ultraviolet (UV) ray irradiationEffect of Ultraviolet (UV) ray irradiation Effect of Ultraviolet (UV) ray irradiation
on frictionon friction More rapid runningMore rapid running--in by 1/10 , in by 1/10 , L i i f i ti b 1/10L i i f i ti b 1/10Lower minimum friction by 1/10Lower minimum friction by 1/10
2. Low adhesion and friction of rubbero ad es o a d ct o o ubbe・・High dense plasma irradiation to CIIRHigh dense plasma irradiation to CIIR
・・UV ray irradiation to TPE with UV ray irradiation to TPE with PFPEPFPEBasic 14 Micro-Nano Tribology Prof. N. Umehara
- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
yy
-
Industrial products and issueRubber ProductsWidely used asWidely used as components of various industrial productsas Oil seal, Packing,
Tire etc. Tire
p
Production methods
Tire
Production methodsInjection formingPress formingPress forming
Packing Oil seal
RubberIssue: Adhesion to mold or conveying equipment Mold
Rubber
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
y g q p Mold
-
Why rubber can stick to surface?
RubberEngineering plastics MetalCells, Soft tissue
Elastic modulus of various materials
[Pa] 103 106 109 1012
Elastic energy Adhesion energy
RubberThe Contact between Rubber and Steel
Elastic energy2
el hEU 2
ad UAdhesion energy
h
Steel Steel
1el 10U
Adhesion parameter ~ 10mJ/m2 = 10-2 J/m2 ~ 1 m = 10-6 m
1
ad
el 10U
1 m = 10 mE ~ 10 MPa = 107 Pah ~ 0.01 m = 10-8m
Adhesive!
B N J Persson at el
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
B.N.J. Persson at el.
-
Another issue for medicine bottle
Issue:Issue:St dh i f bb fStrong adhesion of rubber for medicine bottle against moldmedicine bottle against mold
DieSeparated !Separated !CIIR
DieDue to high adhesion
Die
Bottle stick todie pressureMedicine bottle
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
-
Various Various plasma treatmenttreatmentThe generator of ion beam irradiation treatment
Microwave Quartz
Electrodes RF
S f WSubstrate
Substrate
Surface Wave
Gas ring Gas inn ≈1011 1013 cm 3 at a frequency of 2 45
To pump
Plasma density : RF plasma < SWP plasmaRF plasma treatment Surface -wave excited plasma treatment
ne≈1011-1013 cm–3 at a frequency of 2.45 GHzne≈108-1010 cm–3
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
Plasma density : RF plasma < SWP plasma
-
Adhesion force measurement
Steppin
Adhesion force appartusLoad-Displacement curvpp
g motor
Linear guide
Approach
pe
Specime oad,
P
Retract
pp
SUS440CF 19.05mm
(2)(3)
n holderDriver
Adh i f
Lo
Displacement, dCIIR sheett: 3mm
(1)
(4)
Adhesion forceUpper side of load cell
SUS440C
(4) SeparationCIIR
(1) Contact (2) Approach (3) Retract
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
(4) Separation(1) Contact (2) Approach (3) Retract
-
Effect of plasma irradiation on adhesion
0.16
Material of sphere: SUS440C
Ion beam irradiation treatment Plasma treatmentMaterial of sphere: SUS440C
0.12
0.14
N
Material of sphere: SUS440CDiameter of sphere: φ19.05mm contact time: 90s, Ion gas: ArgonRetracting speed: 0.1mm/minHumidity: 45-50% Temperature: 22-24゜CMaximum load: 1N
Diameter of sphere: φ19.05mm contact time: 90s, Ion gas: ArgonRetracting speed: 0.1mm/minHumidity: 45-50% Temperature: 22-24゜CMaximum load: 1N
0.08
0.10
orce
F, N
Maximum load: 1N Mean value that treated 5 timesMeasured 3 times
Mean value that treated 5 timesMeasured 3 times
0.04
0.06
ull-o
ff fo Surface -wave
excited plasmaRF plasma
n ≈1011-1013 cm–3ne≈108-1010 cm–3
0 00
0.02
0.04
Pu
0.002N0.001N0.001N0.008N
(92.3%) (99.1%) (99.1%) (98.1%)0.005N
(95.2%)0.005N ≒ 0N ≒ 0N
0.015N 0.01N(≒100%)(95.2%)(90.2%)(85.9%)
ne≈10 -10 cm
0.00
Untreated 500V, 50W 30min
1000V, 100W
30min
1000V, 100W
60min
2500V, 150W,
30min32Pa 300W
12min Untreated 30Pa 200W
5min
30Pa 200W
10min
30Pa 250W
5min
32Pa 300W
30min
50Pa 300W
12min
Treatment time Ion beam >> surface-wave plasma treatment Surface-wave plasma treatment reduced adhesion almost 0 N between stainless steel ball and CIIR sheet
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
-
Contact microscope device
Prof. Isami NITTA, Niigata University, Japan
CIIR
CIIRCIIR
CIIR
The procedure of calculate the real contact areaSchematic diagram of a contact microscope with an elliptically polarized light
Lights pass through the prismThe procedure of calculate the real contact area
Prism fixed jig
The analyzer blocks the light when the asperity exists between prism and CIIR
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
j gThe asperity appear to be dark dot.
-
Real contact area Real contact area Unreated
20 ArgonOxygenm
m2
10
15Oxygen
area
Ar,
m
Temperature : 18-20℃Humidity : 30-40%M i l d 5NArgon-1 min Oxygen-1 min
5
10
cont
act a Maximum load : 5N
Argon-5 min Oxygen-5 min 0
5
Rea
l
Plasma treatment time, min0 5 10 15 20
Argon-10 min Oxygen-10 min Real contact areas were
decreased in all conditions !
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
-
Effect of real contact area on adhesion
0.10 Argon
0.08NOxygen
0.06forc
e, N
0.04
hesi
on f
0.02Adh
0 2 4 6 8 10 12 14 160.00
0 2 4 6 8 10 12 14 16
Real contact area,mm2
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
-
Surface topography of rubber surfaceSputter coated with platinum for 1mintues
(a)( )The subsurface on the CIIR looks less granular and generally has a smoother shape(c)Growing rougher as the t ti ti i i
(a) (b)treating time increasing
(d)(d)Microwave power pattern has changed - Roughest surface
≈ ≈ 25 25 μμmm
Roughest surface observed
The cross-section FE-SEM micrographs of oxygen plasma treated to CIIR rubber for (d)(c) Etching effect !Etching effect !
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
(a) Untreated (b) 200 W, 5 min (c) 200 W, 10 min and, (d) 200 W 20 min
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Surface roughness of argon plasma treated to CIIR rubber
Untreated Argon 1 min
40 μm
Argon 15 min
280 μm0 μm 280 μm0 μm
25
30
Rmax RaRz
25.78
15
20
Rz Rq (RMS)
8 96
13.98
ght, μm
5
10
3.01 4.15
8.96
Hei
g
0 2 4 6 8 10 12 14 160
Treatment time min
3D laser scanning microscope images of CIIR sheets after oxygen plasma treatment
Treatment time, minSurface profile with argon plasma treatment, as a function of treatment time
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
g p g yg pwith 200 W at a gas pressure of 30 Pa for treatment times of (a)1, (b)5, (c)10, and (d)15 min.
-
Young’s modulus of CIIR rubberYoung’s modulus of CIIR rubber after argon plasma treated
300
A l f 5 ti d250
aAverage value of 5 times measured Maximum load : 50 μN
150
200
us E
, MPa
6 22
6.335 94
100
150
ng's
mod
lu 6.22 5.94
50You
n 3.96
0 5 10 15 200
Plasm a treatm ent tim e, m in MPa
1.04
untreated 1 5 10 15 2038 39.8 151.4 236.4 240.8 225.9
, MPa
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
-
Explanation by the GW model
2/1* )/(2.3 aa
re REAPA
2
22
1
21
*
)1()1(1EEE
)/( pp RE p : RMS
pR : asperity of radius = 1μmaP : apparent pressure
A20 Oxygen
aA : apparent area
a, m
m2
15
yg
ArgonPoisson’s ratio ν
ntac
t are
a
10
stainless steel ball : 0.3CIIR rubber : 0.5
Young’s modulus of
Rea
l con
0
5g
stainless steel ball : 210 GpaCIIR rubber : Measured
)1( NAPAPW aarer
R
0 5 10 15 20
0
Comparison between GW model & real contact area (Stainless steel ball and CIIR contact)
2/1* )/(1
pp RE , μm−1MPa −1
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
Comparison between GW model & real contact area (Stainless steel ball and CIIR contact)
-
Outline & Summary1.Ultra low friction of Carbon Nitride (1.Ultra low friction of Carbon Nitride (CNxCNx))・・MechanismMechanism Self modification in nm thicknessSelf modification in nm thicknessMechanism Mechanism Self modification in nm thickness Self modification in nm thickness ・・Effect of carbon overcoat on frictionEffect of carbon overcoat on friction
not need runningnot need running--inin・・Effect of Ultraviolet (UV) ray irradiationEffect of Ultraviolet (UV) ray irradiationEffect of Ultraviolet (UV) ray irradiation Effect of Ultraviolet (UV) ray irradiation
on frictionon friction More rapid runningMore rapid running--in by 1/10 , in by 1/10 , L i i f i ti b 1/10L i i f i ti b 1/10Lower minimum friction by 1/10Lower minimum friction by 1/10
2. Low adhesion and friction of rubbero ad es o a d ct o o ubbe・・High dense plasma irradiation to CIIRHigh dense plasma irradiation to CIIR
b L E & R h S llb L E & R h S ll AA
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Tendency in Medical syringe products
Medical syringeMedical syringey gy g
Glass syringeGlass syringey gy g・Easy to crack・High cost UndesirableHigh cost・inferior to the size accuracy
Undesirable
Plastic syringePlastic syringeP d ti
Plastic syringePlastic syringe・・Productive・・Lubricated with silicone oilsilicone oil
Replacing glass syringes with plastic ones is desired.
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
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Issues in advanced plastic syringe
G k (TPE)
Plastic syringe Float of silicone oil droplets※In certain medicinesIGasket(TPE) Plunger(PP)
TPE:Thermoplastic Elastomer
Risk of the accumulation
※In certain medicinesIssue
in the body
Silicone oil Barrel(PP)PP:Polypropylene
Constituent
yp py
Adsorption of medicineSilicone oil
Improper dosage
Silicone oilIssue
Improper dosage
To design the plastic syringe without the silicone oilTo design the plastic syringe without the silicone oilBasic 14 Micro-Nano Tribology Prof. N. Umehara
- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
To design the plastic syringe without the silicone oilTo design the plastic syringe without the silicone oil
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Photochemically fluorination
Fused silica glassIn vacuum
RealReal contact areacontact area
Surface free energySurface free energy
UV 172nm (695kj/mol)Fused silica glass
PFPE(Perfluoropolyether) Association energyAssociation energy
RealReal contact areacontact area
TPECC--C 350kj/molC 350kj/molCC--H 410kj/molH 410kj/mol Low frictionLow friction
UV (172 nm) Fused silica glassUV (172 nm) Fused silica glass
Bridge formation
UV 172nm Fused silica glass( )
Reaction area
( )
Reaction area
UV 172nmUV 172nm
CF3*
CF3*
CF3*
F*F*F*
CF3*
F* F* F*F*
*F*CF3
*F*
F* F*F*Dissociation of PFPE
CF3*
CF3*
CF3*
F*F*F*
CF3*
F* F* F*F*
*F*CF3
*F*
F* F*F*Dissociation of PFPE
FF b id f tib id f ti
C-F
C-FC-F
C-F C
-F
C-F
C-H C-F
TPE
C-C
F 3
C-C
F 3
C-C
F 3
C-F
C-C
F 3
F*F*
F F* F*F*
C-F
F* rich
C-F
C-FC-F
C-F C
-F
C-F
C-H C-F
TPE
C-C
F 3
C-C
F 3
C-C
F 3
C-F
C-C
F 3
F*F*
F F* F*F*
C-F
F* rich Form Form bridge formation bridge formation
TPE
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
Increase Increase Young's modulus Young's modulus TPE
-
Effect of Photochemically fluorination on friction
Friction test in flat specimen W=1 Nイメージを表示できません。メモリ不足のためにイメージを開くことができないか、イメージが破損している可能性があります。コンピュータを再起動して再度ファイルを開いてください。それでも赤い x が表示される場合は、イメージを削除して挿入してください。
6.0
Normal load W: 1 N , Sliding speed V: 2 mm/sWavelength of UV: 172 nm
4 0
5.0
ficie
nt
in air (30-50 %RH)TPE vs. Non-treated PP
Wavelength of UV: 172 nmDropped PFPE & Cleaned by HFE
3.0
4.0
n co
eff
77%2.0
Fric
tion -77%
0 0
1.0
0.00 20 40 60 80 100
I di ti ti t TPE t iBasic 14 Micro-Nano Tribology Prof. N. Umehara
- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
Irradiation time to TPE t , min
-
Effect of Photochemically fluorination on friction
Friction test in TPE gasket
60.0Initial resistance- 40%- 40%
40 0
50.0
ce ,
N Average dynamic resistanceSize of syringe: 20 ml , Injection liquid: Water
40%40%
30.0
40.0
ance
forc
Dropped PFPE
Compression velocity: 100 mm/minWavelength of UV: 172 nm
20.0Res
ista Cleaned by HFE
10.0
0.0Non-treated Silicone oilIrradiated 90 min
Basic 14 Micro-Nano Tribology Prof. N. Umehara- Ultra low friction of Carbon Nitride (CNx) and Low adhesion and friction of rubber -
COE for Education and Research of Micro-Nano Mechatronics, Nagoya University
-
1 Ult l f i ti f C b Nit id (1 Ult l f i ti f C b Nit id (CNCN ))Outline & Summary1.Ultra low friction of Carbon Nitride (1.Ultra low friction of Carbon Nitride (CNxCNx))・・Mechanism Mechanism Self modification in nm thickness Self modification in nm thickness ec a sec a s・・Effect of carbon overcoat on frictionEffect of carbon overcoat on friction
t d it d i iinot need runningnot need running--inin・・Effect of Ultraviolet (UV) ray irradiation Effect of Ultraviolet (UV) ray irradiation ( ) y( ) y
on frictionon friction More rapid runningMore rapid running--in by 1/10 , in by 1/10 , Lower minimum friction by 1/10Lower minimum friction by 1/10Lower minimum friction by 1/10Lower minimum friction by 1/10
2. Low adhesion and friction of rubber・・High dense plasma irradiation to CIIRHigh dense plasma irradiation to CIIR
by Larger E & Roughness Smallerby Larger E & Roughness Smaller ArAr