中華大學碩士論文 - chur.chu.edu.twchur.chu.edu.tw/bitstream/987654321/4893/1/GM095080460.pdf · 研究中使用光學顯微鏡(om)、場發射掃描式電子顯微鏡

1

M09508046

2

SUS440C

(Arc Ion Deposition)(DLC)

(OM)

(FE-SEM) (FE-AES)

(-Raman) DLC DLC

(Nanoindenter)

(Nanoscratch Test) DLC

DLC 500nm ~ 1100nm

DLC

DLC/TiC/Ti/SUS440C DLC

sp2(G band) sp3(D band) sp3 (D band)

47% ~ 74%D band G band (ID/IG)

0.57~1.15 80 144

(80) DLC D band

(74%)

DLC (Nanoindenter)

3

DLC 24GPa ~ 32GPa (2447Hv ~

3263Hv) 264GPa ~ 347GPa

SUS440C (12GPa)(220GPa)

(100nm depth)DLC (0.144

~ 0.156) SUS440C (0.21)

(80)DLC

:

(Diamond-like carbon)(Arc ion deposition)

(Raman Scattering Spectrometer)

(FE-AES)(Nanoindenter)

4

FE-SEMFE-AES

J500

5

............................................................................................................2

............................................................................................................4

............................................................................................................5

........................................................................................................9

......................................................................................................11

............................................................................................15

1.1 ...........................................................................................15

1.2 ...............................................................................19

....................................................................................21

2.1 ...........................................................21

2.1.1 SUS 440C ..........................................................................21

2.2.....................................................................24

2.2.1..............................................................................26

2.2.2 ................................................................28

2.3 DLC................................................................31

2.3.1 CVD .......................................................................31

2.3.2 PVD.........................................................................32

6

2.3.3 ........................................................................33

2.3.4 ............................................................35

2.4.1 ................................................................................36

2.4.2 ........................................................................36

2.4.3 ............................................................................37

2.5 (FE-AES)...............................................................39

2.5.1 FE-AES ...................................................................................40

2.6 (Raman).............................................................................42

2.6.1 Raman..............................................................................42

2.6.2 Raman .....................................................................44

2.7 ...................................................................46

2.7.1 ............................................................48

2.8 ...........................................................................................51

2.8.1 ................................................................................53

........................................................................55

3.1.............................................................................................55

3.2 ...........................................................................................60

3.3 ...........................................................................................61

3.4 ...........................................................................................61

7

3.5 SEM ...........................................................................................62

3.6 EDS ................................................................................64

3.7 FE-AES ......................................................................................65

3.8 Raman ............................................................................67

3.9 ...............................................................................70

3.10 .........................................................................71

......................................................................73

4.1 SUS440C ..............................................74

4.1.2 SUS440CEDS........................................................76

4.2 DLC....................................................................77

4.2.1 DLC(OM)........................................................................77

4.2.2 DLC-B FE-SEM .................................................80

4.2.3 DLC-C FE-SEM .................................................82

4.2.4 DLC-D FE-SEM................................................84

4.3 DLCEDS...................................................................85

4.3.1 DLC FE-AES..............................................86

4.4 (Raman).....................................................................88

4.4.1 DLC-B ...................................................................89

4.4.2 DLC-C ...................................................................91

8

4.4.3 DLC-D ...................................................................93

4.4.4 ............................................................95

4.4.5 Graphite...............................................................96

4.5 DLC................................................................98

4.5.1..................................................................98

4.5.2 ......................................................101

4.6 .................................................................................103

4.6.1 ( 40nm)..................................................105

4.6.2 ( 100nm) ...............................................107

4.7 .....................................................................................109

..........................................................................................112

..........................................................................114

..................................................................................115

9

1 ..............................................................18

2 ..............................................23

3 ........................................................26

4 ....................................................................33

5 ..................................................35

6 SUS440C .....................................60

7 SUS440C.......................................60

8 ......................................................68

9SUS440C(wt %).................................................74

10 SUS440C180...............................74

11 DLC-B (1448)...................................................90

12 DLC-C (807).................................................92

13 DLC-D (807).....................................................94

14 ....................................................95

15 DLC-DGraphite...................................................97

16 ........................................................................99

17 ......................................................................102

10

18 SUS440C(40nm depth).............................106

19 SUS440C(100nm depth)...........................108

20 ......................................................111

11

1-1 ..........................................................................17

2-1 (a)sp (b)sp2 (c) sp3.......................................25

2-2 ..................................25

2-3 DLC sp2 sp3......................................25

2-4 ..................................................................28

2.5CVD...............................................32

2-6 ..........................................................34

2-7 ..................................................................37

2-8 ..........................................................................38

2-9 ..........................................................38

2-10 ..................39

2-11 ............................41

2-12 ............................................43

2-13 ................................................................................44

2-14 ........................................................47

2-15 ............................................................48

2-16 ............................................................48

12

2-17 ........................................49

2-18 ....................................50

2-19 ....................................................50

2-20 ....................................................52

2-21 Berkovich ....................................................................54

2-22 ................................................................................54

3-1 ..................................................................................59

3-2 ..............................................................................62

3-3 ..............................................63

3-4 (FE-SEM) ........................................64

3-5 (FE-AES) .............................................66

3-6 (-Raman)Jobin Yvon T64000.......................69

3-7 ..........................................................................70

3-8 ......................................................................72

3-9 ......................................................................72

4-1 FE-SEM SUS440C 180.........................75

4-2 (a)SUS440C FE-SEM ;(b)A EDS

; (c)BEDS................................................76

4-3 DLC-A(50x) (1448)(OM) ......................................78

13

4-4 DLC-B(200x) (1448) (OM)....................................78

4-5 DLC-C(200x) (807)(OM)........................................79

4-6 DLC-D(200x) (807)(OM) ......................................79

4-7 DLC-B (1448) SEM............................................................81

4-8 DLC-B (1448)SEM.............................................................81

4-9 DLC-B (1448)BEI...............................................................82

4-10 DLC-C (807) FE-SEM ......................83

4-11 DLC-C (807) FE-SEM ......................83

4-12 DLC-D (807) FE-SEM..................................84

4-13 (a)DLCFE-SEM;(b) DLCEDS;(C)

Ti/TiC EDS ..............................................................85

4-14 DLC-B (1448)FE-AES.................87

4-15 DLC-D (807)FE-AES...................87

4-16 DLC-B (1448)DLC-C (807)DLC-D (807)

..........................................................................88

4-17 DLC-B (1448)...................................................90

4-18 DLC-C (807).....................................................92

4-19 DLC-D (807).....................................................94

4-20 DLC-D (807)Graphite.......................................97

14

4-21 SUS440CDLC....................98

4-22 DLC ...............................................99

4-23 SUS440CDLC..................101

4-24 DLC .....................................102

4-25 SUS440C.......................104

4-26 DLC-B...........................104

4-27 SUS440C (40nm depth) ............106

4-28 SUS440C (100nm depth) ..........108

4-29 ..............................................................109

4-30 DLC-CDLC-D

....................................................................................................110

15

1.1

(Surface Modification)

(Diamond-Like CarbonDLC)

[1]

sp3sp2 sp

16

[2-3]

1-1 [7]

[4]

(Physical vapor depositionPVD)(Chemical

vapor depositionCVD)(Arc Ion Plating)

(PVD):[6]

1.

2.

3.

4.

17

5.

PVD 10

PVD

PVD

(Arc ion deposition)

1[7]

1-1 [7]

18

1 [7]

Al ZnCd ZnAl/

Al/

AlWTiTa Al/

AuAg Au /Au/

TiC TiC/

/

Al Al/

/

CrCrNCrCx Cr/ /

/ / /

TiNTaN TiN/ /

TiC TiC/WC

NiCuCr NiCuCr /ABC

AuAlCuNi AuAlNi/Si Pt Pt/ Cu Cu/

Ni-Cr Ni-Cr / SiO2Al2O3 SiO2Al2O3/ FeCoNi FeCoNi /

Be Be/ Pt Pt/Si

AuAg AuAg /

Nb Nb / SiO2TiO2 /

/

Al Al/

MoNb MoNb /Zr-Al

Au Au/

19

1.2

58HRc ~

67 HRc SUS440C

58 HRc

(Diamond-like CarbonDLC)(sp3)

(sp2) (amorphous hydrogenated

diamond-like carbon films)(sp3)

(DLC)

(DLC)

(PVD)

(CVD)

(Arc Ion Deposition)(PVD)

20

SUS440C

(Arc Ion Deposition) (DLC)(Surface

Modification)

(FE-AES)

(Raman Scattering Spectrometer)(DLC)

(Nanoindenter)

(Nanoscratch Test)DLC

21

2.1

2

[5]

11wt%(Cr2O3)

( Martensitic Stainless Steel)

12-17wt%

[41]

2.1.1 SUS 440C

[50]JIS

440SUS440ASUS440B

22

SUS440CSUS440FG4303SUS 440C

1wt%440A440B

16~18wt%304

[41]

440C

7.667g/cm3 (21)10.110-6/(0~100)79.492 w/m2/K(373K) [51]

23

2 [1]

60%

20%

10%

6%

4%

(26%) (74%)

8% 25%

9% 20%

4% 8%

5% 7%

6%

5%

5%

24

2.2

sp3sp2sp

2-1 [33-34](Diamond)(Graphite)

sp3

sp2

2-2 [35-36]

sp3 sp2 (amorphous) [37-38]

2-3 sp3

3

sp3 sp2

[8~10]

25

2-1 (a)sp (b)sp2 (c) sp3 [33-34]

2-2 [35-36]

2-3 DLC sp2 sp3[37-38]

26

3 [8~10]

Layered crystalline

Cubic crystalline Amorphous

sp2 sp3 sp3/sp2

2.462 3.567 -

(g/cm2) 2.26 3.52 1.5~2.0

(103HK) Soft 10 1~5

(N/m2) - 1012 1011

(W/mK) - 11 4.10

(K-1) - 0.810-6 -

(cm) 10-4 109~1013 106~1012

(eV) 0 5.45 0.8~2.0

2.2.1

[13] sp3/ sp2

[14~15]

(1) (diamond~like carbon)

sp3sp2sp3

27

(a)1 atom%

(diamond~like carbon films)(single crystal)

(polycrystal)(nano crystal)(amorphouds)

(b)20~60 atom% (hydrogenated

diamond~like carbon films)

(amorphous hydrogenated diamond~like carbon

films)

(2) (graphite~like carbon)

sp3sp2sp3

30 atom%(

28

(Amorphous Diamond~Like

Carbona~C) 20-60

(Amorphous Hydrogenated

Diamond~Like Carbon a~C:H)sp3

sp2 (random

network)2-4

2-4 [Ferrari A.C.2000]

2.2.2

sp3/sp2

DLC

29

(1)

(2)

(3) ()

(4)

(5)

(1)

[69]

[70]

[71-73]

[74][75]

(Ta) (W) (Ti) (Nb)

(Zr)(Si)..

(2)

(0.1um)

[76-78](Ti)(Cr)

30

[79-80]

(3) () 500-700

()(

)

[81-82]

(4) Ti/TiN/TiCN//DLC

Ti/TiC/DLC[83-85]Ti

TiN (diffusion barrier) TiCN

[86]

(5)

[87]

(re-sputter)

(ion bombardment)

31

2.3 DLC

(Physical Vapor DepositionPVD)(Chemical

Vapor DepositionCVD)

2.3.1 CVD

(Chemical Vapor DepositionCVD)

[16]CVD

2.5

(adsorption)

(surface migration)

(nucleation)

(island)

(desorption)

32

2.5 CVD [16]

2.3.2 PVD

(Physical Vapor DepositionPVD)

[2]

(Evaporation)

(Sputtering)

PVD

4 PVD PVD CVD PVD

CVD

33

4 [43]

(eV) 10~ -0.1 -0.1~1 1~100

() 150~500 30~200 150~500

2.3.3

(Ion-beam sputtering)[26] (Laser

ablation)[27-28] (DC magnetron)[29-30]

(13.56MHz) [31-32] 2-6

[11]

34

2-6 [11]

[17][18]

[19][20-21]

[22](Doping)[23-24]

Raman[25]

5

35

5 [43]

Filter Cathod Arc

300 4000HV 0.1~0.2

Unbalance Magnetron Sputtering

CxHv

200 1500HV 0.1~0.15

High Ionization Sputtering

170 2800HV 0.1

Magnetron Sputtering

And ECR-CVD

System

150 3000HV 0.07~0.12

2.3.4

[42~44]

(1) 30%~100%

(2) (multiply charged ions)

(3) 10~100eV

36

[42]

(1)

(2)

(3)

(4) (500C )[45]

(5)

2.4.1

1963 Mattox

[42]

(

) TiNTiCZrNVCNbC

[6]

2.4.2

2-7 [42](Trigger)

37

2.4.3

(cathodic arc)

(glow discharge) 2-8[46]

1~20m

(cathode spot)[47]

(micro~crater) 2000C

[48] 2-9 [49]

2-10[42]

2-7 [42]

38

2-8 [46]

2-9 [49]

39

2-10 [42]

2.5 (FE-AES)

(FE-AES)

(FE-AES)

10nm

40

2.5.1 FE-AES

(Auger) 2-11

(K )

K

(L )

K

EK-EL(M )

(Auger

Electron):

EKLM = EK EL EM

EKLM K L K

M

[102]FE-AES :

(1)

(2) &

(3)

(4)

(5) /(ISS)

41

(6)

2-11 [102]

42

2.6 (Raman)

Raman 1928

[69]

(DLC)C-C C-Hsp2 sp3

sp2 sp3

(Raman Spectrum)[55~59]sp2sp3

sp2 (sensitivity)

sp3(diamond band)

2.6.1 Raman

0

0

( Rayleigh scattering )

(0-1)(0+1)

(0-1)Stokes line(0+1)

43

anti-Stokes line0

(Raman shift)

2-12[53-54]

2-12 [53-54]

()[95]

44

[96]2-13[53-54]

2-13 [53-54]

2.6.2 Raman

800cm-1 2300 cm-1

(peak) 1332 cm-1

1350 cm-1 1580 cm-1 [97-99]

1400 cm-1~1700 cm-1

1550 cm-1[100-101]

(Gaussian curve

fitting)

45

D-band(D thedisordered graphite-like structure)

G-band(G the graphite structure)[62-63] D-band

1350 cm-1~1360 cm-1 G-band

1560 cm-1~1590 cm-1[62-67] D band G-band

D-band G-band

sp3

[66]

(1) (intensity ratio)R = I500 cm-1/I1550 cm-1 [88]

500 cm-1 (G-

band)1550 cm-1 R sp3

R sp3

(2) 1100 cm-1~1300 cm-1 S =(I1300 cm-1-I1100 cm-1)/I1100 cm-1

[88]

D-band 1300 cm-1~1400 cm-1

sp3

ID/IG [93-94] D-band

1100 cm-1~1300 cm-1 D-band

S

D-band D-band

46

S sp3/sp2

(3)G-band [66]

G-band (FWHMthe full width at half maximum) D-band

G-band

G-band sp3/sp2

D-band

(sp3))[63]

2.7

(hardness)

(Youngs modulus)

47

(Depth Sensing Technique)

2-14

:

(1) : 2N < F < 30KN

(2) : F < 2N ; h > 200 nm

(3) : h < 200 nm

F: ; h:

2-14 [89]

48

2-15

2-16 2-15

2-16

2-15 2-16 [89]

2.7.1

(Load-Displacement curve)

[89] 2-17

(loading)

49

(unloading)

unloading curve

2-18

2-17 [89]

50

2-18 [89]

2-19

(SPM) 3-D

(3-D Piezo Actuator)(Transducer)

2-19 [61]

51

2.8

2-20 [39](adhesion failure)(spalling

failure)(buckling failure)(chipping failure)

(cohesion failure) (conformal

cracking)(tensile cracking)[40]

(critical load)

52

2-20 [39]

53

2.8.1

(Critical loadLc)

2D

(X)(Z

)

(Normal force) (Lateral

force)

Berkovich142.3

65.3 100~200 2-21

2-22

Berkovich

54

2-21Berkovich [61]

2-22 [61]

55

3.1

SUS440C

1030-120

180(arc ion

deposition)(DLC):

(1) ;

(2) Ti;

(3) TiC;

(2)(3)(DLC)

(Ti)

(TiC)

(4)

DLC

DLC-ADLC-BDLC-CDLC-D

DLC-ADLC-B

(1448)DLC-CDLC-D(807)3-1

56

DLC-ADLC-B:

(1) Surface Cleaning:

Ar: 235 ~236 sccm

(V): 600 ~654

(I): 60~65 Amp

(2) Ti Layer Coating:

Ar: 20~30 sccm

(V): 250

(3)TiC Layer Coating (Ti + C2H2):

C2H2: 35~70 sccm

Ar: 20~60 sccm

(V): 100~200

: 3

(4) DLC Coating:

Ar: 60 sccm

: 1448

(V): 100

: 1hr 5min~ 1hr 13min

57

DLC-CDLC-D:

(1) Surface Cleaning:

Ar: 345~350 sccm

(V): 555

(I): 65 Amp

(2) Ti Layer Coating:

Ar: 20~30 sccm

(V): 250

(3)TiC Layer Coating (Ti + C2H2):

C2H2: 35~70 sccm

Ar: 10~20 sccm

(V): 100~250

: 3~4

(4) DLC Coating:

Ar: 10 sccm

: 807

(V): 100

: 1hr 27min~ 1hr 35min

Ar

58

100g/15s

(DLC)(OM)

(FE-SEM)

(FE-AES)

(-Raman)

DLCsp2sp3

CC

DLC(nanoindenter)

(Young's modulus)

DLCDLC

SUS440C

DLCSUS440C

59

SUS440C(18Cr-1C)

SUS440C(18Cr-1C)

DLC

Nanoindenter

DLC

Nanoindenter

FE-SEM (SEI/BEI)

FE-SEM (SEI/BEI)

(AIP)

:

(Vb): -250~100 V(P): 510-3 Pa

ArCH4: 20~60 sccm: 1448 & 807

(AIP)

:

(Vb): -250~100 V(P): 510-3 Pa

ArCH4: 20~60 sccm: 1448 & 807

: 1030: 180

: -120

: 1030: 180

: -120

OM

OM

RamanDLC

sp2sp3Raman

RamanDLC

sp2sp3Raman

FE-AES

FE-AES

FE-AES

FE-AES

1448:DLC-A&B807:DLC-C&D


SUS440C(18Cr-1C)

SUS440C(18Cr-1C)

SUS440C(18Cr-1C)

SUS440C(18Cr-1C)

DLC

Nanoindenter

DLC

Nanoindenter

DLC

Nanoindenter

DLC

Nanoindenter

FE-SEM (SEI/BEI)

FE-SEM (SEI/BEI)

FE-SEM (SEI/BEI)

FE-SEM (SEI/BEI)

(AIP)

:

(Vb): -250~100 V(P): 510-3 Pa

ArCH4: 20~60 sccm: 1448 & 807

(AIP)

:

(Vb): -250~100 V(P): 510-3 Pa

ArCH4: 20~60 sccm: 1448 & 807

(AIP)

:

(Vb): -250~100 V(P): 510-3 Pa

ArCH4: 20~60 sccm: 1448 & 807

(AIP)

:

(Vb): -250~100 V(P): 510-3 Pa

ArCH4: 20~60 sccm: 1448 & 807

: 1030: 180

: -120

: 1030: 180

: -120

OM

OM

OM

OM

RamanDLC

sp2sp3Raman

RamanDLC

sp2sp3Raman

RamanDLC

sp2sp3Raman

RamanDLC

sp2sp3Raman

FE-AES

FE-AES

FE-AES

FE-AES

FE-AES

FE-AES

FE-AES

FE-AES





3-1

60

3.2

SUS440C

6SUS440C

7

SUS 440C 0.95~1.20 wt%

16~18 wt%

6 SUS440C

Standard Grade C Si Mn P S Cr Mo

JISG4303 SUS440C 0.95~ 1.20

1.00 MAX

1.00 MAX

0.04 MAX

0.03 MAX

16.00~ 18.00

0.75 MAX

7 SUS440C

NO. () (Hv) (HRc)

()

(kgf/

mm2)

(kgf/

mm2)

(%)

(%)

(%) (Hv) (HRc)

SUS

440C 1038 610 60 315 200.3 193.3 2 10 2 580 58

61

3.3

SUS440C

1200

Vilellas reagent(1g

15ml 100ml ) (OM)

(SEM)

3.4

MitutoyoMVK-G1

3-2Micro Vikers hardness

100g

5ASTM E 140 [52]

HvHRc

62

3-2

3.5 SEM

0.2~40kv

(CRT)

CRT CRT

CRT

63

(Brightness)(Coherency)

3-3

-

(FE-SEM) JEOL JSM-6500F

Field-Emission SEM3-4

DLC

DLCDLCDLC

SUS440

3-3

64

3-4 (FE-SEM)

3.6 EDS

X-ray

X-ray X-ray

(characteristic)X-ray

X-ray

65

3.7 FE-AES

-

(FE - AES) Thermo VG Microlab 350 3-5

3 kev; 100ev~800ev

EDSBEIUHV XPS(R)EELS

DLC

66

3-5 (FE-AES)

67

3.8 Raman

(Raman shift) 500 -1 2000 -1

sp3 sp2

(Gaussian

Function)

LABSPEC 3.0 Gaussian

G Band D Band (Position)

(FWHM)(Intensity) ID/IG

8 [68]

68

8 [68]

69

-

(-Raman) Jobin Yvon T64000 Micro-PL/Raman

3-6 sp2sp3

DLC sp2 sp3

3-6 (-Raman)Jobin Yvon T64000

70

3.9

(

)

(Nanoindenter)(TriboLabHysitronUSA)

3-7 DLC

3-7

71

3.10

(Nanoscratch test) DLC SUS440C

3-8 [12]

(Nanoscratch Test)(UMISBased Model

CSIROAustralia) 3-9

40nm 100nm

72

3- 8 [12]

3-9

73

(sp3)

(sp2)

SUS440C

SUS440C

Raman

DLC sp2 sp3

DLC

74

4.1 SUS440C

SUS440C 9

SUS440C (wt%) SUS440C

:

(1) : 1030;

(2) : 180;

(3) : -120

100g/15s Hv 10

SUS440C SUS440C

Hv 715.7 SUS440C 180 Hv

695.9 HRc 60.8 59.9

9 SUS440C (wt %)

Elements C Si Mn P S Cr Mo

wt.% 1.02 0.39 0.38 0.025 0.010 16.44 0.44

10 SUS440C 180

SUS440C Hv HRc

Quenched 715.7 60.8

Tempered at 180 695.9 59.9

75

(FE-SEM) SUS440C

180 4-1

M7C3

M23C6 [90]

4-1 FE-SEMSUS440C 180

M7C3

M23C6

76

4.1.2 SUS440CEDS

(EDS)SUS440C

4-2EDS(A)CrFe

M7C3

M23C6[90] (B)Fe

A.EDS B.EDS

4-2 (a)SUS440CFE-SEM;(b)AEDS;

(c)BEDS

(a)

(b) (c) Cr

Fe

Fe Fe

77

4.2 DLC

4.2.1 DLC (OM)

4-3 4-4 4-5 4-6 DLC-A(50x)DLC-B(200x)

DLC-C(200x)DLC-D(200x)(OM)

(DLC) 4-3 DLC-A

DLC DLC

SUS440C DLC

DLC-A

DLC-B 4-4 DLC-A DLC

DLC

DLC-C DLC-D 4-5

4-6

FE-SEM DLC

DLC-A

DLC-B

DLC-CDLC-D

78

4-3 DLC-A(50x) (1448)(OM)

4-4 DLC-B(200x) (1448)(OM)

79

4-5 DLC-C(200x) (807)(OM)

4-6 DLC-D(200x) (807)(OM)

80

4.2.2 DLC-B (FE-SEM)

DLC-BDLC-CDLC-D

Vilellas solution (FE-SEM)

4-7 DLC-B FE-SEM DLC

DLC-B 800nm~1100nm

Ti/TiC DLC 920nm

DLC 400nm~550nm

4-8FE-SEM

DLC-B Ti/TiC DLC

DLC

(BEI) DLC

4-9 BEI Ti/TiC

DLC DLC

DLC

81

4-7 DLC-B (1448) SEM

4-8 DLC-B (1448)SEM

SUS440C Carbide

TiC/Ti

DLC

919nm

544nm

384nm

82

4-9 DLC-B (1448) BEI

4.2.3 DLC-C(FE-SEM)

4-10DLC-CFE-SEM

DLC-C500nm~800nm

FE-SEM4-11Ti/TiC

DLC

DLC-B

83

4-10 DLC-C (807)FE-SEM

4-11 DLC-C (807)FE-SEM

84

4.2.4 DLC-D (FE-SEM)

4-12 DLC-D FE-SEM DLC-D

500nm~800nm DLC-D

DLC

Ti/TiC

DLC-D DLC-B DLC-C

4-12 DLC-D (807) FE-SEM

Carbide SUS440C

TiC/Ti DLC

85

4.3 DLC

4-13 (a) DLC FE-SEM ;(b) DLC EDS

;(C) Ti/TiC EDS EDS

DLC C Ti/TiC

Ti C

(A)DLC EDS (B)Ti/TiC EDS

4-13 (a)DLC FE-SEM ;(b) DLC EDS

;(C) Ti/TiC EDS

(a)

(b) (c) C C

Ti

86

DLC-B

(807)DLC-C DLC-D (1448)

DLC-B DLC-D FE-AES

4.3.1 DLC

4-14 4-15 DLC-BDLC-D

(FE-AES) DLC

200

DLC TiC Ti

SUS440C DLC C TiC

Ti C Ti Ti O

SUS440C FeCr C

FE-AES

DLC DLC/TiC/Ti/SUS440C

FE-SEM DLC

Ti Ti TiC

DLCDLC

FE-AESetching time (sec)DLC-B

87

10000DLC-D6000DLC

DLC-BDLC-D

4-14 DLC-B (1448) FE-AES

4-15 DLC-D (807) FE-AES

88

4.4 (Raman)

sp3 sp2

DLC

[91-92] C-C

DLC

sp3 peak

1332 cm-1 sp2 peak 1580 cm-1 DLC

peak sp3(D band) sp2(G

band) 4-16 DLC-BDLC-CDLC-D

4-16 DLC-B (1448)DLC-C (807)DLC-D (807)

89

DLC-BDLC-CDLC-D

LABSPEC 3.0

P: Peak A: W: S:

curve

fitting

DLC

(peak) DLC peak

1355 cm-1 1550 cm-1 sp3 sp2

4.4.1 DLC-B

4-17 DLC-B 1544 cm-1

G-band

sp2 sp2 1342

cm-1 D-band sp3

11sp3 5385.4

290.1sp2 9432.5 187.1ID/IG

0.57 sp3(D band) 47%

90

4-17 DLC-B (1448)

11 DLC-B (1448)

10.99.7Slope

187.1290.1FWHM

0.57Intensity RatioID/IG

47%ADLC/ATotal (%)

9432.55385.4Intensity (a.u)

Peak 1544(sp2 - G band)

Peak 1342(sp3 - D band)

DLC-B(144 8)

10.99.7Slope

187.1290.1FWHM


47%ADLC/ATotal (%)




DLC-B(144 8)

91

4.4.2 DLC-C

4-18 DLC-C 1561 cm-1

G-band

sp2 sp2 1397

cm-1 D-band sp3

12sp3 8494.1

304.2sp2 9891.5 155ID/IG

0.86 sp3(D band) 63%

92

4-18 DLC-C (807)

12 DLC-C (807)

155304.2FWHM

9.516Slope


63 %ADLC/ATotal (%)




DLC-C(80 7)

155304.2FWHM

9.516Slope


63 %ADLC/ATotal (%)




DLC-C(80 7)

93

4.4.3 DLC-D

4-19 DLC-C 1572 cm-1

G-band

sp2 sp2 1404

cm-1 D-band sp3

13sp3 11207.9

308.9sp2 9737.8 124.9ID/IG

1.15 sp3(D band) 74%

94

4-19 DLC-D (807)

13 DLC-D (807)

124.9308.9FWHM

7.521.2Slope


74 %ADLC/ATotal (%)

9737.811207.9Intensity (a.u)



DLC-D(80 7)

124.9308.9FWHM

7.521.2Slope


74 %ADLC/ATotal (%)

9737.811207.9Intensity (a.u)



DLC-D(80 7)

95

4.4.4

14 DLC-B

144 8 DLC-C DLC-D

80 7 DLC-B ID/IGDLC-B

0.57DLC-C 0.86DLC-D 1.15

D-band G-band ID/IG

ID/IG[60] ID/IG

DLC-B sp3(D band)

47% DLC-C DLC-D sp3(D band) 63% 74%

ID/IG sp3(D band)

DLC-C DLC-D DLC-B

14

1.150.860.57Intensity RatioID/IG

74 %63%47 %ADLC/ATotal (%)

(sp2)1572

(sp3)1404

(sp2)1561

(sp3)1397

(sp2)1544

(sp3)1342

Peak

DLC-D(at 80 7)

DLC-C(at 80 7)

DLC-B(at 144 8)

1.150.860.57Intensity RatioID/IG

74 %63%47 %ADLC/ATotal (%)

(sp2)1572

(sp3)1404

(sp2)1561

(sp3)1397

(sp2)1544

(sp3)1342

Peak

DLC-D(at 80 7)

DLC-C(at 80 7)

DLC-B(at 144 8)

96

4.4.5 Graphite

DLC-D peak 1580 cm-1

4-20 DLC-D Graphite

1572 cm-1 1580 cm-1 G-band

sp2 1404 cm-1 D-band

sp3

15sp3 11116.1

308.61572 cm-1 1580 cm-1 sp2 9078.4

955.5 130.1 46.9Graphite sp2(D band)

26%

DLC OM

FE-SEM DLC

97

4-20 DLC-D Graphite

15 DLC-D Graphite

308.6

11116.1

Peak 1404(sp3 - D Band)

46.9130.1FWHM

26 %AGraphite/ATotal (%)


Peak 1580(sp2 - G Band)


DLC-D-Graphite(80 7)

308.6

11116.1

Peak 1404(sp3 - D Band)

46.9130.1FWHM

26 %AGraphite/ATotal (%)




DLC-D-Graphite(80 7)

98

4.5 DLC

4.5.1

4-21

SUS440C DLC SUS440C

8GPa ~ 16GPa DLC-B 17GPa ~ 30GPa

DLC-C30GPa ~ 34GPaDLC-D21GPa ~ 30GPa

12 13 14 15 16 17 18 19 201416182022242628303234363840

DLC-C

Har

dnes

s (G

Pa)

Depth (nm)12 13 14 15 16 17 18 19 20

1416182022242628303234363840

DLC-D

Har

dnes

s (G

Pa)

Depth (nm)

12 13 14 15 16 17 18 19 201416182022242628303234363840

DLC-B

Har

dnes

s (G

Pa)

Depth (nm)10 15 20 25 300

510152025303540

Har

dnes

s (G

Pa)

Depth (nm)

SUS440C

12 13 14 15 16 17 18 19 201416182022242628303234363840

DLC-C

Har

dnes

s (G

Pa)

Depth (nm)12 13 14 15 16 17 18 19 20

1416182022242628303234363840

DLC-D

Har

dnes

s (G

Pa)

Depth (nm)

12 13 14 15 16 17 18 19 201416182022242628303234363840

DLC-B

Har

dnes

s (G

Pa)

Depth (nm)10 15 20 25 300

510152025303540

Har

dnes

s (G

Pa)

Depth (nm)

SUS440C

4-21 SUS440C DLC

99

4-22 DLC

16 SUS440C

123.4GPa DLC-B 244.4GPa DLC-C

321.2GPa DLC-D 262.7GPa

4-22 DLC

16

123.4

SUS440C

262.7321.2244.4Hardness(GPa)

DLC-D(80 7)

DLC-C(80 7)

DLC-B(144 8)

123.4

SUS440C

262.7321.2244.4Hardness(GPa)

DLC-D(80 7)

DLC-C(80 7)

DLC-B(144 8)

100

DLC-C DLC-B

DLC-B

SUS440C

(nanoindenter) DLC

DLC

24GPa ~ 32GPa 2447Hv ~ 3263Hv (1GPa = 101.97Hv)

12.3GPa

696 Hv (59.9 HRc)

101

4.5.2

4-23 SUS440C DLC-BDLC-CDLC-D

SUS440C

180GPa ~ 260GPa DLC-B 220GPa ~

340GPa DLC-C 320GPa ~ 370GPa DLC-D

280GPa ~ 350GPa

10 15 20 25 30100

150

200

250

300

350

400

Mod

ulus

(GP

a)

Depth (nm)

SUS440C

12 13 14 15 16 17 18 19 20200220240260280300320340360380400

Mod

ulus

(GP

a)

Depth (nm)

DLC-B

12 13 14 15 16 17 18 19 20200220240260280300320340360380400

Mod

ulus

(GP

a)

Depth (nm)

DLC-C

12 13 14 15 16 17 18 19 20200220240260280300320340360380400

Mod

ulus

(GP

a)

Depth (nm)

DLC-D

10 15 20 25 30100

150

200

250

300

350

400

Mod

ulus

(GP

a)

Depth (nm)

SUS440C

12 13 14 15 16 17 18 19 20200220240260280300320340360380400

Mod

ulus

(GP

a)

Depth (nm)

DLC-B

12 13 14 15 16 17 18 19 20200220240260280300320340360380400

Mod

ulus

(GP

a)

Depth (nm)

DLC-C

12 13 14 15 16 17 18 19 20200220240260280300320340360380400

Mod

ulus

(GP

a)

Depth (nm)

DLC-D

4-23 SUS440C DLC

102

4-24 DLC-BDLC-CDLC-D

17

SUS440C 22032.7GPaDLC-B

26429.5GPa DLC-C 34714.3GPa DLC-D

31321.3GPa

4-24 DLC

17

22032.7

SUS440C

31321.334714.326429.5Modulus(GPa)

DLC-D(80 7)

DLC-C(80 7)

DLC-B(144 8)

22032.7

SUS440C

31321.334714.326429.5Modulus(GPa)

DLC-D(80 7)

DLC-C(80 7)

DLC-B(144 8)

103

DLC-C DLC-B

DLC-B

SUS440C (Nanoindenter)

DLC

DLC 264GPa ~ 347GPa

SUS440C 220GPaDLC

SUS440C

4.6

4-25 4-26 SUS440C DLC

DLC DLC-B SUS440C

DLC-B DLC

DLC

104

4-25 SUS440C

4-26 DLC-B

105

4.6.1 ( 40nm)


40nm

18 SUS440C

40nm 0.6mN 1.130.12

DLC-B 40nm 0.8mN

0.9110.09 DLC-C 40nm

0.86mN 0.7930.06

DLC-D 40nm 0.83mN

0.7340.04

40 nm DLC

0.7340.04 ~ 0.9110.09

SUS440C 1.130.12

106

0 500 1000 1500 20001E-3

0.01

0.1

1

10

100

1000

Fric

tion

Coe

ffici

ent

Displacement

SUS440C Scratch Depth 40nmLoad 0.6mN

0 500 1000 1500 20001E-3

0.01

0.1

1

10

100

1000

Fric

tion

Coe

ffici

ent

Displacement

DLC-BScratch Depth 40nmLoad 0.8 mN

0 500 1000 1500 20001E-3

0.01

0.1

1

10

100

1000

Fric

tion

Coe

ffici

ent

Displacement

DLC-CScratch Depth 40nmLoad 0.86 mN

0 500 1000 1500 20001E-3

0.01

0.1

1

10

100

1000

Fric

tion

Displacement

DLC-DScratch Depth 40nmLoad 0.83 mN

0 500 1000 1500 20001E-3

0.01

0.1

1

10

100

1000

Fric

tion

Coe

ffici

ent

Displacement

SUS440C Scratch Depth 40nmLoad 0.6mN

0 500 1000 1500 20001E-3

0.01

0.1

1

10

100

1000

Fric

tion

Coe

ffici

ent

Displacement

DLC-BScratch Depth 40nmLoad 0.8 mN

0 500 1000 1500 20001E-3

0.01

0.1

1

10

100

1000

Fric

tion

Coe

ffici

ent

Displacement

DLC-CScratch Depth 40nmLoad 0.86 mN

0 500 1000 1500 20001E-3

0.01

0.1

1

10

100

1000

Fric

tion

Displacement

DLC-DScratch Depth 40nmLoad 0.83 mN

4-27 SUS440C (40nm depth)

18 SUS440C (40nm depth)

0.830.860.80.6Load (mN)

1.130.12

SUS440C

0.7340.040.7930.060.9110.09Friction

Coefficient(40 nm)

DLC-D(807)

DLC-C(807)

DLC-B(1448)

0.830.860.80.6Load (mN)

1.130.12

SUS440C

0.7340.040.7930.060.9110.09Friction

Coefficient(40 nm)

DLC-D(807)

DLC-C(807)

DLC-B(1448)

107

4.6.2 (100nm)


100nm

19 SUS440C

100nm 1.0mN 0.210.01

DLC-B 100nm 4.0mN

0.1560.01 DLC-C 100nm

4.5mN 0.1440.01

DLC-D 100nm 4.0mN

0.1490.01

100 nm DLC

0.1440.01 ~ 0.1560.01

SUS440C 0.210.01

SUS440C DLC

DLC DLC

SUS440C DLC

SUS440C

108

0 500 1000 1500 20001E-3

0.01

0.1

1

10

100

1000

Fric

tion

Coe

ffici

ent

Displacement

SUS440CScratch Depth 100nmLoad 1mN

0 500 1000 1500 20001E-3

0.01

0.1

1

10

100

1000DLC-BScratch Depth 100nmLoad 4.0 mN

Fric

tion

Displacement

0 500 1000 1500 20001E-3

0.01

0.1

1

10

100

1000DLC-CScratch Depth 100nmLoad 4.5 mN

Fric

tion

Coe

ffici

ent

Displacement0 500 1000 1500 2000

1E-3

0.01

0.1

1

10

100

1000DLC-DScratch Depth 100nmLoad 4.0 mN

Fric

tion

Coe

ffici

ent

Displacement

0 500 1000 1500 20001E-3

0.01

0.1

1

10

100

1000

Fric

tion

Coe

ffici

ent

Displacement

SUS440CScratch Depth 100nmLoad 1mN

0 500 1000 1500 20001E-3

0.01

0.1

1

10

100

1000DLC-BScratch Depth 100nmLoad 4.0 mN

Fric

tion

Displacement

0 500 1000 1500 20001E-3

0.01

0.1

1

10

100

1000DLC-CScratch Depth 100nmLoad 4.5 mN

Fric

tion

Coe

ffici

ent

Displacement0 500 1000 1500 2000

1E-3

0.01

0.1

1

10

100

1000DLC-DScratch Depth 100nmLoad 4.0 mN

Fric

tion

Coe

ffici

ent

Displacement

4-28 SUS440C (100nm depth)

19 SUS440C (100nm depth)

4.04.54.01.0Load (mN)

0.210.01

SUS440C

0.1490.010.1440.010.1560.01Friction

Coefficient(100 nm)

DLC-D(807)

DLC-C(807)

DLC-B(1448)

4.04.54.01.0Load (mN)

0.210.01

SUS440C

0.1490.010.1440.010.1560.01Friction

Coefficient(100 nm)

DLC-D(807)

DLC-C(807)

DLC-B(1448)

109

4.7

(Critical Load)

100 mN

4-29 - 4-30 DLC-C

DLC-D

4-29

110

4-30 DLC-C DLC-D

20DLC-B

695.0mNDLC-C 885.0 mNDLC-D

783.1 mN DLC-C

DLC-C

DLC

DLC

DLC-C DLC-D

111

20

0.4185.400.3783.1DLC-D

(807)

0.495.000.2885.0DLC-C

(807)

0.425.40.2695.0DLC-B

(1448)

Stress (GPa)

Scratch Width (um)

Critical Load (mN)

0.4185.400.3783.1DLC-D

(807)

0.495.000.2885.0DLC-C

(807)

0.425.40.2695.0DLC-B

(1448)

Stress (GPa)

Scratch Width (um)

Critical Load (mN)

112

SUS440C

(arc ion deposition)

(DLC)(surface modification)

(1) SUS440C

Fe-16Cr-1C 180

695.9 Hv (59.9 HRc)

58 HRc

M7C3 M23C6

(2) DLC FE-SEM FE-AES

DLC 500nm~1100nm

DLC

DLC/TiC/Ti/SUS440C DLC

TiC Ti SUS440C

Ti/TiC

113

(3) DLC

DLC

peak1342cm-1 ~ 1404cm-11544cm-1 ~ 1572cm-1

sp3 (D band)sp2 (G band) sp3

(D band)47% ~

74%D bandG band(ID/IG)0.57 ~ 1.15

(80)DLC(DLC-D)D band

(74%)

(4) OMFE-SEMDLC

DLC

(5) DLC(Nanoindentor)

DLC24GPa ~ 32GPa (2447Hv ~ 3263Hv)

264GPa ~ 347GPa

SUS440C (12GPa) (220 GPa)

(6) (100nm depth)DLC

(0.144 ~ 0.156)SUS440C

(0.21)(80)DLC

114

1. SUS440C

DLC DLC

DLC

2. DLC sp3 (D band)

DLC DLC

DLC

DLC DLC

3. DLC TiC/Ti

DLC

115

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