Filme nanostructurate functionale

obtinute prin metoda arcului

termoionic in vid
C. P. Lungu1, I. Jepu1, C. Porosnicu1, A.
Anghel1, A.M.Lungu1, P. Chiru1, C.Ticos1, I.
Mustata1, V. Kuncser2, V. Ionescu3, V.
Ciupina3, M. Osiac4, G.E. Iacobescu4
INCD pentru Fizica Laserilor, Plasmei si Radiatiei,

INCD pentru Fizica Materialelor,

Universitatea Ovidius din Constanta,

Facultatea de Fizica, Universitatea Craiova din Craiova

CUPRINS

Metoda Arcului Termoionic in Vid (TVA);

Filme GMR/TMR multistrat ;
Filme tribologice
Filme pentru tehnologii nucleare

Principiul metodei arcului termoionic in vid (TVA)

Vid inalt 10-6 Torr

Aprinderea plasmei TVA

Simetrie cilindrica TVA

Optimizarea parametrilor plasmei TVA

Forma plasmei si
controlul energetic al
ionilor

Optimizarea parametrilor plasmei TVA

Caracteristicile I-V ale unei plasme TVA in vapori de Ag si Cu, pentru

diferite distante intre anod si catod, curentul pe filament fiind constant

Cu

Optimizarea parametrilor plasmei TVA

Caracteristicile I-V ale plasmei TVA in vapori de Ag si Cu pentru

diferiti curenti de filament, distanta anod catod fiind constanta

Principalele avantaje ale metodei

TVA
Puritatea ridicata a straturilor (datorita vidului

inalt in care se efectueaza depunerea)

Filmele cresc din plasma creat in vaporii puri
ai materialului depus;
Filmele sunt bombardate continuu de ioni
energetici de aceeasi natura cu cei ai filmului
depus;
Energia ionilor poate fi controlata prin reglarea
temperaturii catodului si tensiunea anod catod

Depuneri Multistrat

Sistemul Anodic pentru depunerea multistrat

Depuneri Multistrat

Depuneri Multistrat

Depuneri Multistrat

Ta
Ta

Co + Cu + MgO

Sticla/ Siliciu

Depuneri Multistrat

Analizele SEM ale filmelor multistrat

Proba 2.10
C0/MgO/Cu

Proba 2.6
Co/MgO/Cu

Concentratiile masice ale fiecarui material in parte

14
WtCu Randul 1
WtCu Randul 2
WtCu Randul 3
WtCu Randul 4

12

14

Wt %

12

10

Cu

10

Pozitia probei

4
2

Ta/MgO+Cu+Co

12

WtMg Randul 1
WtMg Randul 2
WtMg Randul 3
WtMg Randul 4

10

Pozitia probei

10

Co

Wt %

Wt %

10

WtCo Randul 1
WtCo Randul 2
WtCo Randul 3
WtCo Randul 4

MgO

Ta/MgO+Cu+Co
2

Pozitie probe

10

Schema contactelor masuratorii in patru puncte

Masuratori electrice efectuate pe probele multistrat

0.008
0.008

13.03.09_St1-1_I-V_0-200 A

13.03.09_St1-1_I-V_200-0 A

0.006

0.006

0.004

U(V)

U(V)

0.004

0.002

0.002

0.000

0.000

-25

25

50

75

100

-25

125

25

50

0.008

75

100

125

I( A)

I( A)

St3-3_I-V_0-100mA

St3-3_I-V_100-0mA

0.008

0.006

0.006

0.004

U(V)

U(V)

0.004

0.002

0.002

0.000
0.000

-0.002
0

20

40

60

I(mA)

80

100

20

40

60

I(mA)

80

100

Masuratori MOKE efectuate pe probele multistrat

-4
-6

MOKE Signal (mdeg)

MOKE Signal (mdeg)

-2

-8
-10
-12
-14
-16
-18

-2
-4
-6
-8

-20

-10

-22

Si_2-2

-24
-0.02

-0.01

0.00

0.01

Si_1-4
-12

0.02

-0.03

B (T)

-0.02

-0.01

0.00

0.01

0.02

0.03

0.04

B (T)

Concentratie mare de Co

Concentratie mare de Cu
2

MOKE Signal (mdeg)

1
0
-1
-2
-3
-4
-5
-6
-7
-8
-9

Si_1-10

-10
-0.03

-0.02

-0.01

0.00

0.01

0.02

0.03

0.04

B (T)

Concentratie mare de MgO

Masuratori MR pe probele multistrat

MR
Gauss FIT

MR%

-0.06

-0.04

-0.02

0.00

0.02

B (T)

0.04

0.06

0.08

0.10

Proba 2.3

MR (%)

Masuratori MR pe probe multistrat

36
34
32
30
28
26
24
22
20
18
16
14
12
10
8
6
4
2
0
-2

C
Gauss fit of proba29ne_C
-0.4

-0.2

0.0

0.2

0.4

0.6

B_analog (T)

Proba 2.9

FILME GRANULARE MAGNETOREZISTIVES

Microscopie de forta magnetica (MFM):

filme Fe-Cu

Topographic AFM image of a

Fe-Cu film (B)

Magnetic domain distribution in

a Fe-Cu film (B)

100
nm

Topographic MFM image

Magnetic domains distribution of a Fe-Cu film

FeCu
prob no. 5
dFe=32.5 cm
dCu=38.5 cm
non treated
thermal treated

0.00
-0.05
-0.10
-0.15

(Rh/R0)-1 (%)

-0.20
-0.25
-0.30
-0.35
-0.40
-0.45
-0.50
-0.55
-0.60
-0.8

-0.6

-0.4

-0.2

0.0

0.2

0.4

0.6

0.8

GMR in Fe-Cu thermally B(T)

treated and as deposited= high abrupt
variation=uniform dimensional distribution of formed domains

NiCu
prob no. 6
dNi=32.9 cm
dCu=38.2 cm
non treated
thermal treated

0.00

(R h/R 0)-1 (%)

-0.02

-0.04

-0.06

-0.08

-0.10
-0.8

-0.6

-0.4

-0.2

0.0

0.2

0.4

0.6

0.8

B(T)

GMR in Ni-Cu composite layer

NILPRP
prob no. 11
Cu-permalloy
non treated
0
treated at 350 C (60 min)
dCu=35.8 cm
dpermalloy=39.5 cm

0.05
0.00
-0.05
-0.10
-0.15

(Rh/R0)-1 (%)

-0.20
-0.25
-0.30
-0.35
-0.40
-0.45
-0.50
-0.55
-0.60
-0.65
-2000

-1500

-1000

-500

500

B (G)

GMR in Cu-permalloy

1000

1500

2000

AFM images of the Co-Cu films

AFM images of the Fe-Cu films

Magnetoresistance vs. applied magnetic field:

- As deposited (black line)
- Thermally treated (red line)
The decrease of the TMR effect after the thermal treatment is caused by:
-Strong oxidation of magnetic grains
-Partial percolation

a)

b)

HRTEM images on Co MgO granular TMR films:

b) As deposited
c) Thermally treated
Observation: formation of large crystalline magnetic domains during the thermal
treatment

Filme compozite
Substrat

Ecran
Catod 1

Nacela

Catod 2

Material pentru
evaporare

TVA Plasma Symmetry

Wear scar on C-W film

AFM of the wear track

Film characterization

Sample

Distance to
W rod
(mm)

Thickness

Hardness

(m)

(GPa)

(at%)

(at%)

C-W 1

200

1.4

5.2

94.8

C-W 2

220

1.6

11

9.5

89.5

C-W 3

240

1.9

10

15

85

C-W 4

260

2.0

14

20

80

C-W 5

275

2.1

16

25

75

0.6

Coefficient of friction

0.5

0.4

0.3

C-W 1

C-W 2

C-W 3

Sample name

C-W 4

C-W 5

(DLC) structure

SAED
5nm

HRTEM

Rhombohedra structures of the film with following

parameters: a = 0.25221 nm, c = 4.3245nm (ASTM pattern:
79-1473) corresponding to diamond/carbon.

Coefficient of friction C-Ni

Coefficient of friction

1.2
1.0
0.8
0.6

Tribological test:
Type: Ball-on disc
Ball: 6mm diameter
Load: 1 N
Sliding speed: 5mm/s

Ni coating on Fe
Ni-C (3/1) on Fe
Ni-C (3/3) on Fe
Ni-C (3-4) on Fe
Ni-C (3-5) on Fe
C coating on Fe

0.4
0.2
0

Sliding distance, m

10

12

Coefficient of friction C-Ni

Tribological test:
Type: Ball-on disc
Ball: 6mm diameter
Load: 1 N
Sliding speed: 5mm/s

Coefficient of friction

0.35

0.30

0.25

0.20

Ni-C (3/1) on Fe
Ni-C (3/3) on Fe
Ni-C (3-4) on Fe
Ni-C (3-5) on Fe
C coating on Fe

0.15
0

Sliding distance, m

10

Images of the structure of the upper layer: tubular features with about 10 nm width
and 50-100 nm length appear together with small grains with a lateral size of about 5
nm. The mentioned features are surrounded by a brighter matrix.

High resolution image of grains in the upper layer: in most of the grains a
crystalline structure is visible, while the surrounding matrix is amorphous.

2 nm
High resolution image of grains in the upper layer: in most of the grains a
crystalline structure is visible, while the surrounding matrix is amorphous.

Aplicatii in tehnologia fuziunii nucleare

Acoperiri cu beriliu pe metale

(Inconel si Nichel)

Primul perete ITER &

Materiale pentru
Divertor
~ 700m2 Be first wall :
low Z + Oxygen getter
~ 100m2 W Baffle/Dome :
low erosion, long lifetime
~ 50 m2 CFC Divertor Target
no melting, C good radiator

Straturi marker din Be

Suprafata
de
acoperit
Be 7-9m
Ni 2-3 m

30 mm

20 mm

26 mm

Sectiune transversala in caramizi inteligente

Bias:

+430 V

Bias:

0V

Bias:

-750 V

0V

2500
120

60

2000

a.u.

a.u.

a.u.

80

Bias: -750 V

2500

Bias: O V (grounded)

2000
100

3000

Be (101)

3000

Bias: + 430V

140

3500

Be (002)

3500

160

-750 V

1500

1500

1000

1000

500

500

Be (002)

+430 V

Be (101)

Bias:

40
42

44

46

48

50

52

54

42

44

46

48

50

52

54

42

44

46

48

50

52

54

56

Concluzii
Folosind metoda TVA (arc termoionic in vid) sau obtinut filme nanostructurate,
functionale cu aplicatii in:
Electronica (filme magnetorezistive)
Mecanica (lubrifianti solizi)
Tehnologii nucleare (filme compacte pentru
acoperirea peretilor instalatiilor de fuziune)