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금속-폴리머 접착력 증진을 위한
플라즈마 표면처리
KISTAdvanced Metals Research Center
Seunghee Han
◆ 1 eV = 10,000 K
◆ Ti ,Tn << Te
◆ h<1 %
◆ Radical species
Plasma Properties
(eV)log10 eT
⊗
HighPressure
arcs
Shocktubes Theta
pinch
FocusLaser
plasma
FusionReactor
Flames
Solarcorona
InterplanatarySolarwind
Fusionexperiments
n34 <π
10-2 10-1 1 10 102 103 104 105
05
1015
20
전형적인 산업적응용 저온 플라즈마
⊗
HighPressure
arcs
Shocktubes Theta
pinch
FocusLaser
plasma
FusionReactor
Alkalimetal
plasmas
Solid Si
Lowpressure
glowdischargesFlames
Solarcorona
InterplanatarySolarwind
Fusionexperiments
10-2 10-1 1 10 102 103 104 105
05
1015
20
산업적 응용저온 플라즈마
Earth’s ionosphere
)(c
mn
log
-310
)(c
mn
log
-310
)(c
mn
log
-310
e
e
e
e
e
e
e
e
e
e
e
e
e
ee
Plasma Sheath
+
+
+
+-V
DC RF MWCCP
ICPDC-Magnetron
ECRDC
◆ Helicon, SW, Laser,Arc, etc
Plasma Generation
Ion Implantation
Injection of high energy ions into materials surface
%
Z
Advantages of ion implantation
Selective improvement of surface regionNo sharp interfaceNo dimensional change or distortionHigh-energy / non-equilibrium processEasy process control
Ion-beam ion implantation
Ext. & Acc. Rastering
Ion BeamMask Target
3-Axis TargetManipulator
Plasma Source Ion Implantation (PSII, PIII)
HV Pulser
Advantages of PSIIUniform implantation over 3-D & large targetSimple and economicHigh dose rateImplantation capability on insulatorsModular design
Plasma
Plas
ma
Phys
ics
High Voltage
Pulse Eng.
MaterialScience
PSIISemiconductor Polymer
Ceramic
Metal
Plasma Source Ion Implantation - Principle
-HV
Target
Vacuum chamber wall
Child-Langmuir Sheath
Dynamic Sheath
Debye Sheath
Plasma
Expanding sheathIncoming ions
Ion Matrix Sheath
HV Pulser0
CW Plasma + HV pulseor
Pulsed Plasma + DC biasor
Pulsed Plasma + HV pulse
PSII Modes
0 2 4 6 8 10 12 14 16 18 200
2
4
6
8
10
12
pulse bias -40 k Vpulse bias -30 k Vpulse bias -20 k V
Shea
th p
ositi
on (c
m)
Sheath propagation time (usec) μ
Advantages of Pulsed Plasma
Pulsed plasma has been widely used in many processes because it has several advantages over continuous (CW) plasma.
Ion species can be varied.
Discharge chemistry is changed.
Charging damage is low.
Film quality is improved in deposition.
Etch and deposition rate increase.
Very well suited for pulsed-process nature of PSII.
Amplifier RF-Deck
13.56 MHz, 50 kW peak, 3 kW avg.4CX5000A RF TetrodePi-tank matching network to 50 Ω(2 vacuum caps / roller inductor)L-R anode parasitic suppression Forward / reflected RF powermonitored using 1-5/8” rigid LS and Bird RF elementsMicroprocessor-controlled powermeasurement and SWR protection Easy and safe tuning with stepperMotors
4CX5000A
CTCL
LCB
RFC
Line S.Anode S.
Amp CTRL / Display
Time-resolved Plasma Parameters
Peak RF power : 10 kW, RF pulse width : 1ms, pulse repetition frequency : 25 Hz
At early stage, the electron density is low and electron temperature and plasma potential is high.
During the RF pulse on time, plasma parameters reach the steady state after about 500 μs.
Plasma parameters are similar to continuous wave (CW) operation from about 500 μs to the end of the RF pulse except the electron density.
After the RF pulse is turned off, plasma parameters decrease gradually.
0 500 1000 1500 20000
10
20
30
40
50(c)
peak 10 kW CW 2 kW CW 1 kW
Time (μs)
Vp
(V)
0 500 1000 1500 20000
2
4
6
8
10(b)
peak 10 kW CW 2 kW CW 1 kWT e (
eV)
0 500 1000 1500 20000
1
2
3(a)
n e (
1011
cm-3
)
peak 10 kW CW 2 kW CW 1 kW
Schematic Diagram of PSII Equipment
2
3
10
9
128
13
4
1916
15
6
7
111415
17
18
1. Vac. chamber 2. Antenna3. RF generator 4. Matching box5. Plasma 6. Target stage 7. Target 8. Vac. Pump9. Ion gauge 10. Langmuir probe11. MFC 12. Working gas13. HV pulse gen. 14. CT15. HV divider 16. Oscilloscope17. Magnets 18. Lead shield19. Chamber ground
PSII Equipments
PSII - I (100L, 100kV, 10A) PSII - II (60L, 10kV, 2A)
Internal ICP Antenna
New PSII Facility for Large Sample Implantation
Ceramic-insulated, internal antenna (water-cooled)Protected by inner-liners Oil-cooled sample stageOil-insulated HVFT
RF Antenna
Sample Stage
Matching Box 1m x 1m x 1mNd-Fe-B magnet cuspsWater-cooled walls2000 L/s turbo-pumpedLead-shielded (6 mm T)Sliding-door type
CTRL / PS
PSII - III (1000L, 100kV, 30A)
RF Antenna / Matching Box
Standard-type matching networkTwo vacuum capacitors and oneceramic capacitorStepper-motor driven from remotecontroller
Antenna
Ceramic Support
Machinable Ceramic
Stepper Motors
Vacuum Caps.
Circuit Diagram of HV Pulse Generator
in
out
Internal View of HV Pulse Modulator
• Dual-mode hard tube type high voltage pulse generator.
• Using high voltage tetrode(TH-5188) and capacitor bank.• 100 kV, 10 A, 10~60 μsec, 10~10000 Hz.
-1 0 0 -5 0 0-7 0
-6 0
-5 0
-4 0
-3 0
-2 0
-1 0
0
-6 0 k V P u ls e B ia s
Bia
s V
olta
ge (k
V)
- 1 0 0 -5 0 0-2
0
2
4
6
8
Impl
anta
tion
Cur
rent
(A)
T im e (u s e c )
Implantation voltage and current
High Voltage Pulse Modulator
Hard-tube type using CB and TH-5188’s2 x TH5188 - MOSFET cascode circuit 100 kV, 30 A HV pulseDC-mode possible for sputter cleaningRC Voltage divider for Vi monitoring(10000 : 1) Immersed in oil tank Will be upgraded using IGBT stack
TH-5188 x 2
Cap. Bank
R / D Array
Mod. CTRL
Un-implanted N2-10 min N2-20 min N2-40 min0
50
100
150
Wea
r D
epth
(nm
)
0 5 10 15 200
20
40
60
80
100
60 kV, 25 usec
150 Hz, 10 min.
Φ = 1017/cm2
Sputter Rate : 130 A SiO2/min
O C
N W
Co
Ato
mic
%
Sputter Time (min.)
PSII N2-implantation on Co-cemented WC
PSII N2-implantation on Cr-plated SKD61
20 um Hard-Cr plating on polished SKD61
N ion implantation(N2, 60 kV, 25 usec, 30 min.)
Pin-on-disc wear tester(100 g, 200 rpm, 10000 rev. 3 mm-Dia. Ruby ball)
α-step Measurement of wear-track
U n -im planted
1 m Torr 200 W R F
100 Hz
1 m Torr 200 W R F
200 Hz
0.5 m Torr 100 W R F
200 Hz
0.5 m Torr 100 W R F
100 Hz
1059 nm 56 nm 101 nm 106 nm 56 nm
PSII N2-implantation on Nimonic (Cr-Ni, Al, Ti….)
Polished Nimonic
N ion implantation(N2, 60 kV, 30 usec, 1 hr & 2 hr, RT & HT)
Knoop Hardness Test, SEM, Auger
Un -implanted
RT 1 hr.
RT 2 hr.
HT 1 hr.
HT 2 hr.
350 HK 396 HK 405 HK 1129 HK 1246 HK
Polymer Surface Modification
고분자 고분자
ChemicalFlameCorona (UV, Laser)
플라즈마 ( 이온빔 )중간층 (Tie-layer)
고분자
금속박막
Polymer Surface Modification using PSII
0 5 10 15 200
10
20
30
40
50
60
70
80
N2 Plasma Ar Plasma O2 Plasma N2 PSII Ar PSII O2 PSII Untreated
Cont
act a
ngle
(deg
)
Aging time (day)
Water contact angles of PS as a function of aging time
Improvement of Cu-PI adhesion using PSII
0 200 400 600 800 1000 1200 14000
50
100
150
200
250
300
350
400
1500 Å Cu pre-deposition on PIPSII-IBM (20 kV, 20 us, 500 Hz)3000 Å Cu deposition
gf/c
m
Implantation Time (sec)
Un-measurable
Polymer Surface Modification using PSII
0 2 4 6 8 10 12 14 16106
107
108
109
1010
1011
1012
1013
1014
1015
1016
Ar 100W 1mTorr -30kV 20μs 100Hz -50kV 20μs 100Hz
Surfa
ce re
sistiv
ity (
Ω/sq
.)
Implantation time (min.)
Surface resistivity of MPPO as a function of ion energy
Epon’s PSII chamber for IC-tray implantation
Plas
ma
Phys
ics
High Voltage
Pulse Eng.
MaterialScience
PSII
Metal
금속 소재
PolymerSemiconductor
Ceramic
Plasma / PSII is a very promising tool for materials surface modification !!
Conclusion