„ .

“ ”

TIN,

”
01.03.25 “ ,
”

: . . . . . . . . . . . . . . . . . .

. /

2007

1
 :

- .

- . P . J. Ke l l y

- ,

2
......................................................................................................1

I. .............................................................................2

I.1.

(PVD ) ..................................................................2

.1.1 .....................................................2

.1.2. ( ) ....................................3

.1.3. ...........................................6

.1.4. ....................7

.1.5.

(CFUBMS) .......................................................................8

I.2.

............................................................12

I.2.1.

...................................................12

I.2.2. „ ” ( ) ..................16

I.2.3. ...........................................18

I.3. ,

....24

I.3.1. ........................................24

I.3.2. ( ) ………26

I.3.3. ( ) ……………27

I.3.4. ………………... 29

I.3.5. ……………………………………………….30

I.3.5.1. ……………………………30

I.3.5.2 ……………………… … 30

I. 3.5.3.

(RBS) ………… ………………………………………………………….31

3
 I.3.6.

………………………………………………………………………32

I.3.6.1. ( ) …………32

I. 3.6.2.

(XPS)…………………………………………………………………………………33

I. 4. ,

T iN……………………………………………………………………………………34

I.4.1.

TiN ……………… ……………………………………… 34

I. 4.2. T iN

……………36

I. 4.3.

T iN …………41

II. ....................................44

II.1. ..............................................................................44

II.1.1. TiN 2 0.5 m 4

m, (DC) 4 , 6 , 8

-50V .....................................46

II.1.2. TiN 2 0.5 m 4

m, (DC) 4 , 6 , 8

........................47

II.2. ,

TiN .................................................49

2.2.1. .......................................49

II.2.2.

TiN …………………………………………..60

4
 II.2.3. …………..60

III. ............................................................62

III.1. TiN 2 ,

(bias) -50V ..........................................62

III.1.1. ………………………………..62

III.1.1.1. TiN (~100nm)

Ti …………………………………………………………….62

III.1.1.2. TiN 0.5 m

Ti ………………………………………………………………………………67

III. 1.2.

…………………………………………………………………………..69

III.1.2.1. TiN (~100n m)

Ti …………………………………………………………….69

III. 1.2.2. TiN 500nm Ti

………………………………………………………………………………….88

III.1.3. ………………………… 95

III.1.4. TiN 98

III.1.5. …………………………… 102

III.2. TiN 2 ,

(bias) ……………………… …………….108

III.2.1. ………………………………108

III. 2.2.

………………………………………………………………………….109

IV. .................................................................................115

.................118

.............................................................121

I T iN .........................I

II , ............II

5
 .

, ,

T iN,

1
I.1.

(PVD )

[1] ,

(PVD )

.1.1

- ;

- ;

2
 :

- ;

- ,

( )

N 2 , O 2 ).

.1.2. ( )

.1.

.1 [1]

3
 , ,

, .

( ~ 0.1-0.01 Torr),

( ),

( ) ( ).

( 30 eV [2]), ,

, .

~ 10 5

[1].

[1].

, ,

(bias) .

( )

4
 ,

[3, 4].

, ,

. ,

, [1],

20 mTorr,

, ,

1-5

mTorr [1].

5
 ,

PVD ,

.1.3.

70- XX [5,6].

, ,

, . ( .2),

, .

( , ).

6
 a) b)

.2.
( ) ( ) [1]

.1.4.

Window

Savvides [7-9] 80-

, “ ”

( .3).

( )

, .

7
 .1.5.
(CFUBMS)

90- XX

(CFUBMS)

Teer [10]

Sproul [11]. ,

~ 10-15 .

8
.3.
[12]

CFUBS

[12-15]. .4

. .4

.4

( ).

R.D. Ar nel P.J.Ke lly

- - .

9
 .4. CFUB S
,

[12]

, .4 .

[16]

, ,

CFUB S

CFUB S .

( , ), CFUB S

10
 ,

( , ),

[17,18].

(DC) .

( ),

, ( ) .

(RFS).

CFUB S :

- –

50-80 nm/ min (

);

- ;

- (

4) , –

, ,

, ,

).

11
I.2.

, ,

PVD , .

[19]

[1,20,21]. , ,

I.2.1.

[20] .5.

12
 .5.
[20]

, ,

. ( ),

(R)

, .

, , .

(R)

13
. ,

“ ”.

. ,

[20,21]:

( R / N0D 1, R -

, N0-

, D –

),

( .6 )

- ,

R / N 02 D 1

, .6(b),

(layer gro wt h) Frank

van der M er ve.

14
.6.
, (PVD)

.6 ).

- ,

15
 (3D)

.6d). ,

Vo lmer- Weber

, ,

.8 ). .6f

3D ;

- ,

, ( .

6f).

I.2.2. „ ” ( )

, ,

. ,

, ,

16
 . ,

Thor nton [24],

. 7.

.7 ,
[21]

17
 ,

( .7 ).

. ,

( .7 ). ,

( .7 ),

. , .7d, ,

).

I.2.3.

PVD .

18
 Movchan Demchisin [22],

( .8).

. Ts Tm , Ts - Tm -

.8. Mov chan Demchisi n [22]

( Ts Tm =0.3)

. ,

( Ts Tm = 0.3-0.5)

, .

( Ts Tm >0.5)

, ,

, Sanders [23],

19
 .

Thornt on [24],

. 11. Thornton [24]

). .9,

, :

– (

), ;

1 ,

, .

, Messier [25,26],

T hornton,

20
 .

.10, ,

1.

.10 Messier [25]

. ,

[26-35].

Arnell Kelly ( .11) ,

CFUBMS,

. (

(Ji / J a )

, 1

, CFUBMS.

~ 0.13

21
 ,

2.

.11. , CFUBMS

[12,13]

.12 ,

Arnell Kelly

Thornto n Messier.

. 12. ,
(
“this study”) , CFUBMS

22
) 1, 2 3

23
 I.3. ,

I.3.1.

( ),

, “ ” (Grazing

Incide nce Geo metr y) [36-38].

1Å

a b

.13. ( )
“ ” ( )

24
 , ,

, 1 0 ),

, “ ”,

[39],

[40,41] ,

). (1)

, [39] ,

true fit true

2 hkl 2 hkl (2 / sin 2 hkl ) (1)

: (e 2 / mc 2 ).( N Av. 2 . . Zi / Ai ) -

fit
(1); hkl -

true
; hkl -

true
, . hkl

(1) .

25
 (D)

( ) ,

sin
D( ) (2)

, ,

I.3.2. ( )

TE M

. , ,

TEM .

~ .

26
 , [42,43].

. -

, -

( ,

.).

( select ed area diffract ion)

I.3.3. ( )

“ ”.

. -

27
 .

.14. , ,
,
[43].

, ~ 3

- 5 eV, ,

~ +200V [43]. .14

. ,

, ( )

, .

, ,

28
 , , – .

, ,

[44].

11 ( Na).

I.3.4.

“ ” (Scanning

pro be micro scopy),

( )

( ).

29
 ,

, .

I.3.5.

I.3.5.1.

, .

I.3.5.2

. ,

( ),

( 511 k eV),

30
 . ,

, ( -, -

), [45-47].

10 -7 -

10 -4 [47].

I.3.5.3. (RBS)

RBS

, ( ~

m).

).

( 0)

( ) ( ):

E [(m1 cos m 22 m12 sin 2 )]2

(3)
E0 (m1 m2 ) 2

: m1 , m2 -

; -

, .

, .

31
[48-51]. ,

, ,

I.3.6.

I.3.6.1. ( )

, P. V.

Auger, ,

.3.3.,

Z>11,

, .

Z<15 E 2000 eV [43,5 2,53].

, ,

32
 .

~ 2nm,

. ,

I.3.6.2. (XPS)

, .

XPS K

h ~ 1.2-1.4 eV [36,52].

Mg (h =1.2536 eV) Al ( h =1.486 6

eV) .

, :

.= h -E . (4)

: E . ,

. ,

, .

),

33
 I.4. ,
-
TIN

TiN

), , .

[54-57] .

T iN

- -

- - .

I.4.1.
,
TiN

34
 .

. [29,55-64],

i U s is
E p eU i (5)
m ad

: Ui – ; i, m –

; Us –

( bia s) ; i s – ; a d-

[65, 66-68] ,

, , [65],

Ar nell- Kelly. [65]

i
, J i /J a ),
m

. ,

, Ji/ Ja,

, . , J i /J a ,

35
CFUBMS [65, 68-71]. ,

, ( s)

, ( Tsmax ),

(DC)

8 . [72] s Tsmax ,

. ,

0.5 mTorr 3

mTor r, Tsmax . [65, 68, 73],

DC. [74] J i /J a

(DC) Ji/ Ja

I.4.2. TiN

T iN

, .

s, . [75] ,

[72,75]

36
 ( . ,

). -100V

[72].

[76-78] T iN

Ji/ Ja (-30V)

. , J i /J a ( 0.1 8.6),

( . ),

. J i /J a ,

, ,

T iN .

[79,80], ,

T iN

, ,

, .

TiN , PVD ,

[81],

[82-84] [85].

TiN,

37
[86]. ,

T iN ,

( DC ), <111>

[73,81,82,87-97]. ),

T iN , <100>

[98-102]. [98,99]

J i /J .

J i /J T i 1, <111> , -

~ J i /J T i >5, <10 0> .

[100-102] ,

Ar+N 2 <111>

<100> . [97] ,

T iN

. Ar+ N 2 ,

<111>, + N2

<100>.

TiN

38
 [31,86,103],

, ,

[31,86]

, , {200}

T iN

, T iN

<100>.

[104,105] , T iN {110}

{111}- , {200}

. [86,103]

( <uvw >)

TiN (E < 1 1 1 > < E < 1 1 0 > < E < 1 0 0 > ), [86,103]

39
<111> ,

( )

. ,

<100>

<111>

. [86]

(~0.5µ m) T iN ,

TiN ,

<111 >, <100>.

[85] , T iN ,

10nm ( .

), <111 > . [106]

<100> <111>,

T iN ,

1.5 m , .

, , 0.85 m

(~14 sccm), <111 >.

N2

<100>

, , ~20 sccm.

<111> <100>

(N 2 ) [107,108]. [109,110],

<111> <100> ,

40
 .

<111> <100> Ji 60 160

m 2 [111].

TiN .

. [112] ,

( ~12.5 sccm)

0.13GPa ( ) - 4.7 GPa ( ).

[59]

(N 2 /Ar)

, ,

[59].

I.4.3.
TiN

[13,59,95,113-118].

[75] T iN

, ,

0.22 1.68µm, -5.93

41
GPa -2. 7 GPa, 14.9

32.1 GPa.

~25 GPa [119-122]. [123,124]

T iN

. [124]

90%, =0.7.

[115] 20%

0.75 0.95.

[58, 73, 125] , T i2 N

T iN ,

, .

, T iO 2

TiN ,

T iO 2 (~15 GPa) TiN

[100].

[126,127] XPS ,

TiN : 397.2 eV

396.3 eV,

. [128]

, .

[128]

( ~ 1µm)

42
, .

T iN

(CFUBMS) ,

, :

1.

, .

2. ,

3. ,

“ .

”.

43
 II

II.1.

E 2,

1.

1. E 2, wt.%

C Cr Mo W V Fe

0.9 4.2 5.0 6.4 1.8 base

(Teer Coat ings Ltd. UDP450), <10 -3 Pa,

30

(12.6 sccm 0.8Pa),

(DC) 0.05 kW

(bias) –1000V .

(300mm x 100mm) 100 mm.

Ar N2

~ 0.25Pa.

44
 ,

(OEM). , 1-2 , ,

OEM ,

(~100 nm) Ti

TiN .

: 500nm ( ) 4000n m

). ,

(I d ) - 4 , 6 8 .

(bias) -50V.

(0. 5µ m)

);

- 0.5µ m T iN ,

, -

, <100>

<111> .

45
 II.1.1. TiN 2 0.5 m 4
m, (DC) 4 , 6 , 8
-50V

T iN,

Ti 100 nm (

min T i) , Ti 0.5

m.

-50V.

2 3.

2. ,
Ti ( min. Ti)

Sp. DC, d, Deposition Deposition Base Coating Target Target Nitrogen

A m time for time for pressure, pressure, voltage, power, signal
Ti, min TiN, min mbar mbar V kW

1 8 1 52 6.5x10-6 380 3.00

4
2 6 1 70 2.2x10-5 365 2.20

3 4 1 92 1.3x10-5 355 1.40

2.5x10-3 500
10 8 1 7 9.5x10-6 380 3.00
0.5
11 6 1 9 4.6x10-6 365 2.20

12 4 1 12 4.6x10-6 355 1.40

46
 3. ,
Ti 0.5 m (0.5 m Ti)

Sp. DC, d, dTi, Deposition Deposition Base Coating Target Target Nitrogen
A m m time for time for pressure, pressure, voltage, power, signal
Ti, min TiN, min mbar mbar V kW

7 8 4.5 52 2.6x10-3 380 3.00

4
8 6 5 70 1.2x10-5 365 2.20

9 4 0.5 9 92 2.6x10-3 2.5x10-3 355 1.40 500

13 8 4.5 7 1.6x10-5 380 3.00
0.5
14 6 3 9 1.1x10-5 365 2.20

15 4 9 12 1.1x10-5 355 1.40

, II.1.1,

(II.1.2.).

II.1.2. TiN 2 0.5 m 4

m, (DC) 4 , 6 , 8

Ti 0.5 m

4.

47
 4. ,
Ti 0.5 m (0.5 m Ti)
(substrat e bias = 0V)

PR DC, d, dTi, Deposition Deposition Base Coating Target Target Nitrogen

A m m time for time for pressure, pressure, voltage, power, signal
Ti, min TiN, min mbar mbar V kW

4 8 4.5 52 2.7x10-6 380 3.00

4
5 6 6 70 2.6x10-6 365 2.20

6 4 0.5 11 70 1.9x10-6 2.5x10-3 355 1.40 500

-6
16 8 4.5 7 2.5x10 380 3.00
0.5
17 6 6 8 1.6x10-5 365 2.20

18 4 11 9 2.5x10-6 355 1.40

48
 II.2. ,
TiN

T iN, XPS ,

. . . –

, . Kelly.

2.2.1.

URD6

Seiferd&Co CuK

(B-B) „ ” (GI ABD).

0.1 (

) 10 - 60

: ,

, .

49
 . ( ,

, ,

, ,

: Gaussian, Lore nt zian and Pseudo-Voight [129].

Pseudo -Voight

JCPDS .

( ),

JCPDS .

Powder. : ,

50
P < u v w>

[130].

Te

P < u v w> ,

<uvw> .

, , . 00

. 15).

.15.

,
, ) [130]

51
 :

I {film s tan dard

hkl } / I {hkl }
P uvw (6)
1 I {film
hkl }

n n
tan dard
I {shkl }

: I {film s tan dard

hkl } , I { hkl } - ,

; n- (

).

(1D ODF)

» (GI ABD) ( ),

. ,

, 00 ( )

, : ( ) [130].

( y) ( x).

52
 .16 ,

(1D

ODF).

.16. ,

[130]

(3D ODF)

),

{hkl}.

, ,

Schult z [131].

, .17.

53
 (ND) ,

(Ro lling Direct ion - RD)

(Transver se direct ion-TD).

.17.

ND

, TD - .

( ) .

, ,

. , ,

, ,

( ) 0-90 0 ( 0-360 0 ,

).

3D ODF

– ,

54
 ) ,

( ), .

: [100], [010] [001].

( 1 , , 2 ),

, ( .18).

( ) ,

.18.
; 1 , , 2

F(g), (3D ODF),

. F(g)

55
 ,

Bunge Roe [132,133,134].

3D ODF.

F(g),

, :

2 2
1
F ( g )dg 2
F( 1, , 2 )d 1 sin d d 2 1 (7)
8 0 0 0

( 1 , , 2 ),

M (1) N (1)
F ( 1, , 2 )= Cl ( 1 , , 2 ) (8)
l 0 1 1

( l). Cl

(8)

l ( l m a x ).

, l m a x =22 ,

56
(ODF).

lma x.

“Po pla”,

Los Alamo s, US A,

, .

. .19

(d 0 ) -

.19. ,
(d 0 )

57
 ,

d0

d<d 0 . , d>d 0 .

, .20 [135].

.20 -

, 1 2

3 0 ,

1 , 2 , , [135]:

1
x sin 2 x( 1 2 ) (9)
E E

58
 d d0
: ,
d0

, =0,

( 1 2 )

E
( 1 2 ) x 0 (10)

0, ,

[135]:

E 1 d
x x (11)
1 d 0 sin 2

« »

d=f(sin 2 ),

d
d 0 .
sin 2

(11)

59
 II.2.2.
TiN

Cambridge St ereo scan 60 0

II.2.3.

XPS

VG ESCALAB Mk II Al K (1486.6 eV),

~1eV 1 10 -8 Pa. C1s

C1s, O1s, N1s T i2p

TiN.

, Ar +

60
 , ,

61
 III

III.1. TiN 2 ,
(bias) -50V

T iN Ti

III.1.1.

III.1.1.1. TiN (~100nm)

Ti

. 21

(0.5µm) (4µm) T iN .

CuK ( )

”.

T iN ( FCC), NaCl ,

. ,

, .

. T iN,

Ti ( ),

( ) T i-O (T iO, T iO 2 ,

T i 3 O 5 , T iO 0 . 3 4 N 0 . 7 4 ).

62
 .21. , “ ”
TiN Ti : )
(0.5 m) ,
=2 0 ; b) (4 m), =2 0 ; c)
, =10 0 ; DC –
[136]

2 < 30 o ). ,

63
 , ,

=2 0

) ( .21 .21b). ,

.21 ,

=10 0 ( . ),

, . ,

[136]. 2 69 0 ,

T iN

(T iO 0 . 3 4 N 0 . 7 4 )

, ,

. ,

( .21 , b) ,

, .

, (8 ),

, -

64
 ,

(DC=6 )

.21

( . ).

( )

XPS

, – Manchester Metropolit en Univer sit y,

UK. .22 N1s T i2p XPS

, (

Ti N),

Ti O). , T i2p

455. 6 eV,

XPS ,

N1s ,

T iN.

65
 .22. N1s Ti2p XPS TiN 4µm,
CFUBMS DC=8A

6 ,

XPS ,

Ar + .

6. XPS TiN ,
8 (DC),

Specimen Ti/ Ti/N

As applied, 4000nm, 8A (DC) 0.57 0.91
* 0.58 0.91
4000nm, 8A (DC), 2minAr+
4000nm, 8A (DC), 7minAr+ 1.05 0.97
+
4000nm, 8A (DC), 12minAr 1.06 0.99
As applied, 500nm, 8A (DC) 1.00 0.90
500nm, 8A (DC), 2minAr+ 1.06 0.90
+
500nm, 8A (DC), 7minAr 1.21 0.97
500nm, 8A (DC), 12minAr+ 1.32 0.99

*
Ar +

3 nm/min.

66
 XPS

T iN,

III.1.1.2. TiN 0.5 m Ti

23

GIABD =2 0 ( . 23 a, b)

( . 23 ) Ti

500nm. ,

Ti ,

. ,

, ,

T iN. T iN

Ti Fe,

, -

(T iO, T iO 2 , T i3 O 5

T iN 0 . 7 4 O 0 . 3 4 ).

« »

, , ,

, ,

67
 .23. TiN 0.5
m Ti: ) 0.5 m TiN, DC=4A, 8A-“ ” =2 0 ;
) 4 m TiN, DC=4A, 8A-“ ” =2 0 ; ) 4 m TiN, DC=8A – .

, ( .

, .

68
 , .

, T iN

, ,

( Ti

TiN) .

III.1.2.

III.1.2.1. TiN (~100nm)

Ti

.24

<21 0>

, ,

=0 0 =90 0 . ,

69
 .

. 24. <210>

: - (0.5µm) (4µm)
TiN, DC=4 DC=8 [137] ; ) – 4µm
, DC=6

, ,

, .

15–25 0 40-45 0 ,

, ( .24 a, b)

( .24 c, d) . FCC

T iN , , 40-45 0

70
 <111> (o ut -of-p lane) ,

{111}

. 15–25 0

: {100}, {110}, {211}, {311}, {331}

=0 0 =90 0 ,

( 40–45 0 )

, 15–25 0 .

, P{ hkl},

). P{ hkl}

(6) .25. , -

71
{111}, {100} {110}. , {111}

, . ,

DC=4 , 80%

, ,

(8 ), 70%.

.25 , ,

4 8

{111}.

a b

c d
.25. Phkl TiN
(DC) ,
DC= 4 DC= 8 [136]

72
 .25 ,

( 0.5 4µm),

<111>

, .

.25d,

, -

DC=8A {111}

, {220}

. , DC=4A DC=6A (

), {111}

{111 },

, TiN FCC ,

.26.

73
 a)

b) c) d)

.26. TiN
{111}, {100 } {110} [136]

FCC T iN

FCC ,

. ,

( .

),

: 0.91 ( {111}), 0.92 ( {100}) 0.65 ( {110}) [136] .

, ( ) FCC

, FCC T iN,

{111} ,

74
 . ,

{111} .

T iN <111 >,

« » « » . 26 ,

. 26 , .

[136] ,

{111} 0.5 m

Vo lmer-Weber .

{100} {110}

, ,

{100} {110 }. “shado wing”

{111} ,

75
 . 27. {111}, {200} {220},
( )
)

{100} ,

76
 T iN ,

, ,

.27. , ,

{111} , ,

0.5 m , , {200} {220}

. , -

, {111} ,

, ,

, {100}

{110} , 20-30%,

. {111}

Vo lmer- Weber,

<111>

. {100} {110} ,

[136].

77
 7

T iN,

- . ,

),

. ,

( )

. ,

7.
TiN [136]

No of Films Target Magne Substrate Coating Substrate Film Final

the thickn current tron bias, V pressure ion current depositi substrate
sample ess, (Id), A Voltage (Pa) density (is), on rate temperature,
0
nm (Ud), V mA (ad), C
(mA/cm2)* nm/min
1 500 4 354 -50 0.25 3.2 (2.0) 42 130
2 4000 4 354 -50 0.25 3.2 (2.0) 43 220
3 500 8 373 -50 0.26 7.1 (3.5) 71 160
4 4000 8 376 -50 0.26 7.1 (3.5) 75 270

e .

<111> ,

78
 < u v w>

d < u vw>

{111},

{200} {220} ,

, Pseudo -Vo ight

centr .
(2 hkl ),

d < u v w> .

uvw :

d uvw d 0 uvw
uvw (12)
d 0 uvw

: d < u v w> -

; d o uvw -

(38-1420/1997

JCPDS file).

U < u v w>

[11]:

3
U uvw E uvw ( uvw )2 (13)
2

79
 : uvw

; E uvw ,

T iN.

sij ,

T iN : s 1 1 = 2.17.10 -3 ; s 1 2 = -0.38. 10 -3 ; s 4 4 = 5.95.10 -3 [GPa -1 ].

E<uvw>

1
[ s11 (2s11 2s12 s 44 )]. (14)
E uvw

u 2v 2 v 2 w2 u 2 w2
: ; <uvw> -
(u 2 v 2 w 2 ) 2

( GPa): E < 1 1 1 > = 408, E < 2 0 0 > = 461 E < 2 2 0 > = 420.

(12) (13)

.28 [136]. ,

: 111 220 200

U 111 U 220 U 200 ,

, T iN ,

, <100 > <111>

80
 . [138, 139] ,

U.

(E < 1 1 1 > < E < 1 0 0 > )

, U <111> , .

<111> , U<111> < U<200>.

<100 > <111 >.

.28. ( )
U <uv w>,
TiN : ) ; ) .

.28 ,

, .

. <111>

. , ,

U < u vw> ,

81
 ,

T iN . ,

<111> <110> <100>,

, -

( . 25 , ).

, .

( 0.5 4 m)

, -

, ,

{311}, {331} {420},

. ,

{220} , DC=8A

.25d), {111}

. ,

82
 .

.29.

c d

.29. ,

); DC: 4A (a); 6A (b); 8A (c, d) [136, 140,143]

, ,

83
 ~0.5 µm .

(DC).

, -

( {111}) -

, ( {111}

),

T iN, ,

. ,

, ,

( .24).

84
 ,

[130].

(4µm) ,

4 , .30. ,

<110 > .

.30. ( )
<111>, <100> <110> 4µm TiN (min. Ti -50V bias) [130]

POPLA

(3D ODF).

, .

, ,

[141]. (F, F 1 , F 2 )

(001),

.31, : F –

85
 ;; F 2 –

; F1 – , 90 0

, F F2 ,

F1 ( )

. , F F2

(hkl),

, , ( F1 ) ,

[uvw], ( hkl)

=0 0 ,

( .31 ).

86
 )

.31. (001)
( ) 3D ODF
(hkl)[uv w] ( )

, (111)

87
 [110] ,

=0 0 (

). ,

{111}<110 >. ,

<110>

III.1.2.2. TiN 500nm Ti

.32

, P < u vw>

, Ti (0.5 m)

(4 m) T iN. , 40%

<110 > out -o f-p lane ,

60% <200>, <211>,

<220> and <310>. Ti

70%) <001>,

, . Ti

{001}

. ,

T iN,

{111} .

88
 , T iN

{111} ,

{001}

T i.

a) b)

c) d)

.32. ,
( ),
Ti ( ), TiN ( , d)

.32,c ,

T iN <111> .

T iN (

DC) 75% ( DC=8A) 90% ( DC=4A)

<111> ,

, ( min. T i),

89
 ( ),

. ,

{111}.

, .

.33. , {111}

, (

) ,

{200} {220} , -

TiN,

, .

Vo lmer-Weber

, <111>

, .

90
 .33. {111}, {200} {220} TiN,
: - 0.5 m TiN ; 4 m TiN

{200} {220}),

. « »

, <111> ,

{200} {220}

91
 ( 500 nm 4000 nm)

.32d). Ti -

<111>

Ti TiN

. 34.

. 34.
(
) ( ) TiN, 500nm
Ti

92
 ,

{111} ,

{220} ( .33).

T iN,

U 111 U 220 U 200 .

, , , -

Ti, .

Ti

, .

<111> )

, ,

93
 .34

Ti

( ) ( )

T iN . ,

Ti <111>,

, ,

( ,

DC=6 ,

).

) )
.34. ,
( ) ( ) TiN;
: –DC=8 , min Ti; - DC=8 , 500nm
Ti [142]

94
 III.1.3.

s in 2 ( 1 2)

( II).

, d-sin 2

sin 2

1 2) . .35.

{200 }

500 nm 4000 nm T iN.

E 2 0 0 =461GPa 2 0 0 =0.17,

T iN,

( 1 2)

, ,

( 1 2) ,

, ,

95
 ) b)

.35. ( 1+ 2)

(DC) , min Ti
(a) 500nm Ti (b) [144]

, ,

[137].

, .

, DC ( 1 2)

Ti .

96
 DC

( Ji,

, , .) ,

(4 000 nm)

d 4 2 0 -sin 2 , (11)

( ),

( =0 0 )

, ( =90 0 ).

.36.

) b)

.36. ,
(4000 nm) TiN ,
Ti ( ) 500nm (b)

, Ti.

97
TiN, (

),

Ti.

III.1.4. TiN

, ,

(a d )

, . ,

(~100 nm) Ti . 37.

. 37. TiN,
(~100 nm) Ti

98
 (DC).

.38

T iN, 1 Ti,

1 .

Ti T iN.

.38. TiN,
DC: 4 ); 6 ( ) 8 ( ); ,
– Ti , – TiN

99
 ,

, TiN

, -

T iN .

. 39.

a b

. 39.
TiN , DC=4A (a); DC= 6A (b); DC = 8A (c)

100
 . 38

DC.

. 40.

a) b)

. 40. ( )
Ti TiN

. ,

. 40, . 37 ,

Ti , ,

101
III.1.5.

T iN

( ,

, ,

).

, ,

[145] ,

1/2 ( FWHM),

( h k l ),

, {111}, {200} {220}

( hkl ), FWHM

, P seudo-Vo ight ,

102
 ,

. :

2 2
hkl Bhkl bhkl
(15)

: B h k l and b h k l

FWHM {hkl} ,

B-B (

(500 0 C, 1 , ) TiN ( ).

. 41. ,

(DC); TiN min Ti (a, c);

TiN 500 nm Ti (b,d)

103
 ,

(DC) .41.

, hkl

4 8 , ,

hkl.

, {220}

{111} {200}

hkl

. ,

{220} , ,

( .27 .33).

.41

111 200 ,

{111} {200} .

[146]

104
 T iN ,

. ,

, .

, {111}

( . 27 .33).

T iN.

{hkl} ,

Pseudo-Vo ight (2 hkl) ,

duvw

<uvw>

2d uvw sin n
hkl (16)

; n .

(a u v w ) ,

105
 auvw d uvw u 2 v2 w2 (17)

a) b)

c) d)

.42. uvw

Ti N ,
( , , , d)
amean
(min Ti)

a mea n ,

=2 0 .

TiN

(2 ). a mea n

POWDE R, :

106
 T iN, (2 )

.42 (a, b, c) ,

a 1 1 1 >a 1 0 0 ,

[146, 147] ,

107
 III.2. TiN 2 ,
(bias)

III.2. 1.

. 43. TiN 0.5 m ( ) 4 m ( ,

), bias
” ( , ) ( )

. 43 (0.5µm)

(4µm) TiN.

108
 , ,

, (bias) -

50V. ,

.43 .21 .23,

. ,

, , ,

T iN.

III.2.2.

.44

<210> -

=0 0 =90 0 .

, , -50V bias ,

40-45 0 15-25 0 .

109
 .44. <210>

(0.5µm) (4µm) TiN,

CFUBMS DC=4 DC=8 bias

.45

P{hkl} .

<111> -

( .45 , ).

110
 a b

c d
45. ,
TiN
0.5µm Ti: bias - 0.5µm ( ); 4µm (b); )
(0.5µm) ,
DC=8 , -50V bias ( ) bias ( ); d)
), (4 µm) [148]

.45 ( , d) ,

(bias) -

, bias

, . ,

<111> <200 >

50% ..

{200}

111
 ,

, .

( .46).

46.
( ) ( )
TiN, ,
.

112
 , TiN

, <111 >

, , <200> <220 >

TiN ,

T iN [136].

{200} {220} .

( 1 2 ),

{200} . .47.

47. ( 1 2)

) , DC=8A
bias ( )

113
 , ,

, bias

.47 ( ) ,

), (

).

114
 IV

1. T iN,

(DC)

(CFUBMS)

2.

Ti ,

3.

TiN,

CFUBMS .

T iN. {111}

115
 ,

4. ,

Ti .

5. , Ti

T iN

{111}

6.

, ,

7. -

« »

116
”, .

117
I.

1. R. Mirchev, V. Antonov, I. Iordanova, P.J.Kelly “Influence of magnetron sputtering

conditions on the parameters of TiN coatings on a steel substrate”, Zeitschrift für

Kristallographie, 23 (2006), 269-274

2. I.Iordanova, P.J.Kelly, R.Mirchev, V.Antonov, Vacuum, 81 (2007), 830-842

3. I.Iordanova, R.Mirchev, P.J. Kelly, V.Antonov, “X-ray and SEM investigation of TiN

coatings applied on M2 tool steel by reactive DC and pulsed CFUBMS”, Mater. XIII

Workshop Plasmatechnik, June, 2006, Ilmenau, Germany, 86-93

4. I.Iordanova, R.Mirchev, P.J.Kelly, V.Antonov, “Evolution of micro- and

substructure parameters of TiN films applied by reactive CFUBMS on steel

substrates during their growth”, paper accepted for publication in Galvanotechnik

5. R.Mirchev, I.Iordanova, I.Marek, N.Ganev, “X-RAY methods for investigation of

preferred crystallographic orientation and their application to texture analysis in

magnetron sputtered TiN coatings”, Meetings in Physics, Heron Press Science

series, 7, (2006), 42-45

6. I.Iordanova, R.Mirchev, P.J.Kelly, V.Antonov, Technological conditions Influence on

the Crystallographic Parameters Evolution During the Growth of TiN Films Applied

on Steel Substrates by Reactive DC and Pulsed CFUBMS, ”, Mater. XIV Workshop

Plasmatechnik, June, (2007), Ilmenau, Germany, 63-70

118
II.

1. R. Mirchev, V. Antonov, I. Iordanova, P.J.Kelly “Influence of magnetron sputtering

conditions on the parameters of TiN coatings on a steel substrate”, European

Powder Diffraction Conference – EPDIC IX, September 2 - 5, (2004), Prague

2. R. Mirchev, I. Iordanova, V. Antonov, P.J.Kelly, X-ray investigation of

crystallographic texture evolution in TiN coatings applied by Closed-field unbalanced

magnetron sputtering, Fourteen International Summer School on Vaccum,

Electron and Ion Technologies – VEIT 2005, September 12–16, (2005) Sunny

Beach, Bulgaria

3. R.Mirchev, I.Iordanova, I.Marek, N.Ganev, X-RAY methods for investigation of

preferred crystallographic orientation and their application to texture analysis in

magnetron sputtered TiN coatings, Meetings in Physics, February 23 – 24, (2006)

Sofia, Bulgaria

4. R. Mirchev, I. Iordanova, V. Antonov, P.J.Kelly, Investigation by X-ray diffraction

methods of structure-formation process in magnetron sputtered TiN coatings, 5th PSI

Summer School on Condensed Matter Research Neutron, X-ray and Muon

Studies of Nano Scale Structures, August 19–26, (2006), Lyceum Alpinum, Zuoz,

Switzerland

5. R. Mirchev, I. Iordanova, V. Antonov, P.J.Kelly, Investigation of texture and residual

streses in reactive magnetron sputtered TiN coatings on M2 steel substrates, 6th

International Conference of Balkan Physical Union, (BPU6), August 22 – 26,

(2006), Istanbul, Turkey

6. I. Iordanova, R. Mirchev, V. Antonov, P.J.Kelly, Analysis of substructure parameters

in different texture components and structure-formation in magnetron sputtered TiN

119
 coatings 6th International Conference of Balkan Physical Union, (BPU6), August

22 – 26, (2006), Istanbul, Turkey

7. I.Iordanova, P.J.Kelly, V. Antonov, R. Mirchev, Influence the Target Power and

Substrate Bias on Microstructure parameters of TiN Coatings Applied by Reactive

Closed Field Unbalanced Magnetron Sputtering (CFUBMS) on EM2 Steel Substrates,

XV International Summer School on Vaccum, Electron and Ion Technologies –

VEIT (2007), September, 2007, Sozopol,Bulgaria

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130
 TiN

(TiN) PVD

, .

( ), ,

, ,

, ,

, , ,

, , ,

, ,

- , .

.I.1 ,

TiN

. I.1

I
Fig.I.1. , TiN ( )
- TiN
( )

II
.I.1.
TiN

TiN >99%
PVD (CFUMS)

0.25 12 m. 1 5 m
2
2000 kg/mm Knoop
. 2500-3500.
85 Rc.
.

,
.

,
, : ,
, , ,
, .
. TiN
0.05÷0.90. TiN 0.65.
.
.
0
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.
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25 µOhm-cm
, , ,

9.4 x 10-6 /°C.

0.046 Cal/sec.-cm-°C.
5.22 g/cm3.

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0.25
80,750 Cal/mole. (3.5 eV/molecule).
3.35 – 3.45 eV

III
 II

IV
V
VI
VII
VIII