The nucleation and growth of thin films

Brian L. Evans and Shi Xu

J.J. Thomson Physical Laboratory,

University of Reading,
Whiteknights,P.O.Box 220,
Reading, RG6 2AF, U.K.

ABSTRACT

A study has been made of the nucleation and growth of thin microcrystalline
films of Cu,Au,Pt,Ni prepared by ion-beam sputtering. In-situ measurements of
the film resistance during deposition have been analysed in terms of percolation
theory for the early, discontinuous, phase and thin film, grain boundary,
scattering for the quasi—continuous phase. This analysis yields values of the
percolation threshold, fractional coverage and lateral grain dimensions, for
different deposition rates, which are compared with the corresponding values
obtained from direct observations and soft X—ray multilayers reflection spectra.
The minimum thickness of the metallic nuclei is shown to be four atom layers.

1 . INTRODUCTION

Thin films of a material may be deposited on a substrate using the techniques

of chemical vapour deposition (CVD) or physical vapour deposition (PVD) . In the
case of ultra thin films where precise control of the layer thickness is required
the PVD method is used ie. either (i) thermal evaporation using the near stable
flux from an effusion cell or the monitored flow from an electron beam evaporator
or (ii) inert gas atom sputtering from a target as in magnetron or ion-beam
sputtering (IBS) . A major advantage of the sputtering technique is that the
sputtering rate can be precisely controlled so that the deposited layer thickness
is simply proportional to a (calibrated) deposition time.

In lBS a stream of inert gas ions/excited atoms from a self contained gag
discharge (ion-gun) is directed onto a target at an angle of incidence of 60
(to the normal) . Sputtered target atoms are deposited on a substrate which is
vertically above the target and out of line of sight of the ion-gun. The
deposition chamber is continuously pumped so that the dynamic inert gas pressure
within the chamber is maintained at 10 ' torr.
which is 100 x less than that
required to maintain the discharge within the ion-gun.

For a given target material the sputtering rate, hence deposition rate,
depends upon the ion—gun operating parameters such as the dc HT voltage and the
ion—current. Providing these parameters are closely controlled the deposition
rate can be maintained constant over a long period of time. In order to measure
the deposition rate for a given material it is necessary to measure the thickness
t of films of the material prepared for different deposition times T. The
thickness of films having t3nm can be measured from the Talystep trace across
the film 'edge' but for smaller values of t it is necessary to employ a soft
X—ray interferometric technique (see later). Once the deposition rate of a given
material has been established the film thickness t is known at any time T and this

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 allows 'in—situ' measurements of film properties, such as resistivity, to be
directly related to the film thickness. lBS is a comparatively slow deposition
technique, typically O.4nm/min, so the very early stages of film growth may be
studied. This paper reports the results of such an investigation of lBS Cu,Au,
Pt,Ni films, on glass substrates, prepared for arangeof ion—gun HT voltages
(deposition rates).

2 . EXPERIMENTAL METHOD

The thin film deposition rate of metal M (M = Cu,Au,Pt,Ni) was found from
Talystep measurements on single films (t>3nm) and from the Bragg reflection
maxima observed in M/C multilayers at wavelength X = O.834nm. For such a
multilayer reflection maxima are observed at glancing angle of incidence where

2dsin[1-/sin2q] ( integer) (1)

where d = t1+ t2 is the multilayer periodicity and =Yi (1-y)c52, S being the
refractive index decrement, and y = t1/d. The metal M thickness t1 is determined
from equation (1) since the C layer thickness t2 is known from a previously
determined deposition rate. Figure 1 gives, as example, the reflection spectrum
of a 5 1 /50 Ni/C multilayer in which t1 = 1 Qnm , t2 1 .25nm . From measurements
on a series of multilayers 'of different t1 (M layer deposition times) the M layer
deposition rate was determined for different ion-gun HT voltages in the range
1.6 to 2.6 kV. The deposition rates for the extremes of HT voltages used are given
in Table I. In the measurements described here the ion—gun current was kept
constant at 220m amp.

The physical structure of the single M film was determined from transmission
electron microscope (TEM) measurements on single films of known t deposited on
carbon coated EM grids . The crystallographic structure of the films was determined
from the associated electron diffraction patterns.
The dc resistance R of the M films was measured during deposition using a
Keithley 617 programmable electrometer. Prior to deposition two conducting silver
electrodes, separation 3±0.2mm, were painted on the glass substrate surface.
The film was deposited through the rectangular aperture in a mask, held in close
proximity to the substrate surface, to form a strip 3mm wide which overcoated
both electrodes and the substrate region between. Resistance R measurements
were made at is intervals during the early stages of deposition and at 30s
intervals after the onset of continuous film foxmation. Since the deposition
rate appropriate to the particular ion-gun HT voltage had previously been
determined, Table I, the R versus T measurements could be translated into R
versus t traces where t is the equivalent continuous film thickness.
3. EXPERIMENTAL RESULTS

Figure 2 shows the TEM pictures of Au,Pt,Ni, films of thicknesses t = 0.5,

1.0,1.5 and 2.Onm (ion-gun HT 2.0kv) and demonstrates the different nucleation
behaviour of these elements. The Cu films oxidised after removal from the
deposition chamber so their TEM pictures are not shown. The t = 0.5nm films of
Au,Pt consist of isolated metallic particles, the particle size being larger in

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 the Au film; there is no resolvable detail in the Ni film of this thickness.
When t = 1.Onm the Au and Pt particles have clustered to form short chains of
irregular length and shape but there is still no detail present in the Ni
film at the magnification employed. When t increases to 1.5nm the substrate
coverage has further increased and it is possible to see connecting paths across
an appreciable area of film. In the Ni film (t = 1.5nm) the appearance is that
of the Pt film at t = 1.Onm. When t = 2.Onm the Au film appears to cover the
substrate surface whereas the Pt, Ni films still appear as a connecting network.

Figures 3,4,5,6 show the measured film resistance R versus equivalent

continuous film thickness t for lBS Au,Pt,Ni and Cu films deposited using
different ion-gun HT voltages, ie deposition rates, Table I. The inset to these
Figures shows the initial R versus t behaviour in more detail. All the graphs
of Figures 3-6 show similar behaviour in that initially there is a comparatively
slow decrease in R with increase in t followed by a rapid decrease (over
approximately six orders of magnitude) which eventually tails off to give a slow
decrease in R with increasing t. However the scale range over which these
effects occur is different for the different metals.

4. DISCUSSION

The electron diffraction ring/spot patterns of the Au,Pt,Ni and Cu films

were all consistent with the face centred cubic (fcc) structure, the orientation
of the crystallites composing the film being that in which the hexagonally close
packed (111) atomic planes are parallel to the (carbon) substrate. Four such
atomic layers (stacking sequence ABC/ABC) are required to define the fcc unit
cell (of side a) . The thickness, measured perpendicular to the substrate,
of the microcrystals is thus n (a13) , n integer.

From measurements of the TEM pictures it is possible to estimate the lateral

particle dimensions, in the early stages of film growth, and also the fractional
coverage of the (carbon) substrate. Some of these parameter values, for Au and
Pt films of different (equivalent film) thickness are given in Table II . Also
shown in Table II are the parameter values for Au films of the same equivalent
thickness (ie the same value of the product deposition rate x time, viz 15
deposited, on carbon, using different ion—gun HT voltages. There it is seen
that decreasing the HT voltage, ie deposition rate, Table I, has the effect of
decreasing the lateral dimensions of the Au particles while increasing the
fractional coverage (due to the greater number of particles).

In measurements of the film resistance R, Figures 3,4,5,6, the film sample

dimensions were such that R = p /t where p is the film resistivity appropriate
to a particle film thickness t. It is evident from the TEM pictures that the
slow decrease in R which occurs at the larger values of t is that of the quasi—
continuous film which completely covers the (glass) substrate. It is convenient
to first consider this portion of the R versus t graphs.

Early theories of electrical conduction in thin films assumed a homogeneous,

single crystal, film in which case the enhanced film resistivity over that of
the bulk material, p, occured a?ia2rult of non—specular reflection of electrons
'
at the film surfaces. This gave

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 F :: 3
(P) (k>>1) 2(a)
- 8k

k !±E k in !1 (k<<1) 2(b)

1—p kJ
L4

where p is
the eiectronic specuiar reflection coefficient, k = t/X and X is the
electron mean free path in the bulk material. When the film is polycrysa1line
however, as in the case considered here, the average grain diameter D in the
film becomes comParable(th Xc that grain boundary scattering be
included. In this case

co 2pC2X
t (1+p) 3(a)

where co the resistivity of the infinitely thick film, is given by

cx 0 (1 + +c1 C2)
3(b)

in which C1 = -C =-4/rr, C2 = 0.375 and

\) = D i+t 3(c)
2 (1-t1)

where the electron transmission coefficient t' at a grain boundary plays the same
role as the coefficient p at the film surface. Writing equation 3(a) as

PFt =pt+2pC2X
0 0(1—p) 4
(1+p)
it is evident that, if equation (4) applies, a graph of Rt2 (=pFt) versus t
should be a straight line of slope p.

Figures 7,8,9,10 show the larger t values of R in Figures 3,4,5,6 plotted

as Rt2 versus t. It is noticeable that all these graphs exhibit a minimum in
Rt2 to the large t side of which the graphs are approximately linear; as
required by equation (4) . From the slope of the linear portion of each graph
itis possible to obtain p and hence D as itemised in Table III. In the case
of Au it is seen that the alues of D re consistent with the measured lateral
particle dimensions given in Table II'whereas in Pt the values of D for the
quasi—continuous film are, as exected, greater than measured in th particulate
film. The small value of D (15A) in Ni is much less than in Au, Pt, which is
consistent with the TEM obsrvations. In Cu the values of D are consistently
greater than Au. g

Returning to Figures 7,8,9,10 it is tempting to assume that the minimum

in each Rt2 versus t graph at t marks the transition from a discontinuous to
mm

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 a continuous film. Thus t • decreases in the seqence Cu,Au,Pt which is generally
in line with the decrease IrD . In the case of Ni however t- > t whereas
Ni Pt g mm mm
Dg < tg . The parameter values in Table II show that in the case of Au (on
carbon) decreased particle lateraldimensionsgave increased substrate coverage.

In the R versus t measurements gien in Figures 3,4,5,6 the range Ott

mi
corresponds to the nucleation and growth of metallic nuclei. Over this
thickness range the conductivity is thermally activated ie the film exhibits a
negative temperature coefficient of resstance(TCR) whereas for t > t . the TCR is
positive. The conductance of the particulate film over the range O< is
min
a composite of the substrate surface conductance and metallic particle
conductance and, as such, can be described by some form of percolation theory.
Systems consisting of randomly distributed metallic and dielectric regions
exhibit a metal - non metal transition (MT) when the volume fraction x of the
metal reaches the percolation threshold x . The effective gductivit a(x) = 0
for x<x while for x>x the conductivity ncrses with x as
c c
t
a(x) = a (x—x ) (5)
m c
where t = 1.6 for the three dimensional case and 1.3 for the two dimensional case.
If the dielectric regions have non-zero conductivity GD then for() symmetrical,
two dimensional, distribution of metal and dielectric components

c(x) aD(xc _x)t x<x

c
(6)
. .
where (7) G(x ) = (aDa) . There is no exact eqjimvalent relation for the three
m
dimensional cse.

Equations (5) and (6) are not directly applicable to the case under
investigation viz. that of discrete metal particles on a substrate having a
finite surface conductance, since it is not possible to define the conductivity
of such an assembly. For this reason a modified form of the equations was
employed ie.

R(x) = A(x-x )P x>x

(7)
B(xx) , x<x

where R(x) is the measured resistance of the assembly at a fractional metal coverage
x. Assuming x = t/t.
and taking p = 1.3 in equation (7) then

R(0) = B x 1.3 = R
c D
R(1) = A(1—x )1.3 R
c m
2
If R(x ) = (RDR the thickness t corresponding to x can be determined also
parameers A an B. Values of these parameters derives from the measured R versus
t (tt ) graphs for Au,Pt,Ni and Cu films; Figures 3,4,5 and 6, are listed in
Table fand Figures 11 and 12 show the resulting fit of the computed curves,
equation (7) , to the experimental R versus t traces for Au and Pt. In the case
of the Pt film a better fit was obtained using p = 2 instead of p = 1.3.

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 Referring to Table IV it is seen that the values of t , ie the equivalent
film thickness at which conducting links occur through thecfilm on glass, increase
in the sequence Pt,Ni,Au and Cu. This agrees with the TEM pictures shown in
Figure 2 where the appearance of the t = 1.5nm Ni film is similar to that of the
t = 1.Onm Pt film in showing the presence of short conducting links. In the case
of Au the value of t (-4nm) on glass is greater than the thickness t2nm at which
the Au film, on carbgn, Figure 2, appeared to cover the substrate surface.

Figure 1 shows the soft X-ray reflection spectrum of a 51/50 Ni/C multilayer
from which the Ni layer thickness t1 can be determined. From a series of such
measurements on Ni/C multilayers a graph of Ni layer thickness t1 versus
deposition time T was obtained as shown in Figure 13. For values of ti > 2nrn
the graph of ti versus T is linear but the graph departs from this straight line
at smaller values of t1. This is because the Ni is now in the form of discrete
particles whose thickness is greater than that of the equivalent continuous film.
The graph of Figure 13 would appear to intercept the Ni film thickness axis at
O.8nm. This evidently represents the minimum particle thickness and corresponds
to a thickness of four atomic layers.
Over the range t1<2nm the first order multilayer reflection can also occur
as a doublet, as shown in Figure 14. In this case the particles have thicknesses
of 1.0 and 1.2nm, corresponding to five and six atomic layers respectively.
With a slight increase in Ni deposition time the reflection doublet reverts to a
singlet corresponding to a preponderence of Ni particles of thickness 1.2nm.
With further increase in T the sequence is repeated.

The deviation from the straight line graph in Figure 13 associated with the
discontinuous, particulate, Ni film can be translated into a graph of fractional
substrate coverage versus equivalent film thickness as shown in Figure 15. There
it is seen that complete substrate coverage (corresponding to x=1 at t=t
equation (7)) occurs at t=1.6nm and x evidently reduces to 0.25 at t=O.2n1
since the minimum particle thickness is O.8nm. In this respect the mathematical
analysis leading to Table IV and Figures 11,12 is unrealistic since it assumed
that x varied continuously from 0 to 1. The value of t . ('4nm) obtained from
the R measurements of Ni on glass, Table IV, is greater in the value of 1.6nm
obtained from Figure 15 for Ni on carbon. This may be due to the different
properties of glass and carbon substrates or the erroneous attribution of
t . tox=1.
mm
CONCLUSION

It has been shown that 'in—situ' resistance R measurements on lBS metal

M films on glass identify (a) the nucleation and growth stage of the M film
leadingup to the formation of (b) the quasi-continuous film. The stage (a)-(b)
transition occurs at a film thickness t.
identified with the minimum in the Rt2
versus t plot. Values of t •, corresding
to complete substrate coverage
(x=1), are equal (for Pt) ormreater (for Au) than thQ$e deduced from TEM
Cu Au > Ni
observations of M films on carbon and t
mm
> t .
mm
tmm>tPt
mm
.
Describing
stage (a) by a simple form of percolation theory gives values for th citica.
coverage x and thickness t at which conducting links occur with t U u >
c c c c
i
c
>

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 Stage (b) can be described by a thin film, grain boundary scattering, theory
which enables the lateral grain dimension D to be deter-
Cu experiental
u 1ues
as also observed in the TEM masurements.
mined viz. D > D > D > D
g g g g
In the case of Ni soft X—ray reflection measurements on Ni/C multilayers showed
that the fractional coverage decreased from unity as t1 decreased from 1.6nm and
that the Ni partic1e8iad a minimum thickness of four atomic layers, as previously
observed in Pt films

6 . ACKNOWLEDGEMENTS

The authors gratefully acknowledge the co'operation of B.J.Kent who measured

the multilayer reflection spectra leading to Figure 13.

7. REFERENCES

1. Thomson, J.J. 1920. Proc.Camb.Phil.Soc., 11,120.

2. Fuchs, K. 1938. Proc.Camb.Phil.Soc., 34, 100.
3. Sondheimer, E .H. 1952. Adv . Phys. 1,1.
4. Bedda, M; Pichard,C.R. and Tosser,A.J. 1986. J.Mat.Sci. 21,1405.
5. Kirkpatrick, S. 1973, Rev.Mod.Phys. 45,574.
6. Efros,A.L. and Shklovskii, B.I. 1976. Phys.Stat.Sol. (b) 76,475.
7. Dykhne, A.M. 1970. Zh.eksper.teor. Fiz. 59,111.
8. Evans, B.L. and Kent,B.J. 1987. B.J.Appl.Optics. 26, 4491.

Table I. The measured lBS deposition rates for different metals at ion-gun
voltage V and current I.

Metal V(kV) I(mA) Deposition rate

(/min)

Pt 2.2 260 2.12

1.8 260 1.5

Ni 2.2 220 2.45

1.6 220 1.61

Cu 2.2 220 4.9

1.6 220 3.5

Au 2.2 220 4.2

1.6 220 3.0

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 Table II. TEM measurement of particle size and fractional area x of (carbon)
substrate covered by the metal for different (equivalent) film thicknesses t
and ion—gun parameters (V,I)

t() x(%) Particle V,I

size ()
Pt 5 20 20 2kV,180mA
10 42 20x50
15 66 25x50
20 83 30x55
Au 7 20 30 2kV,l8OmA
14 30 60
21 82
28 100
15 22 80 2.6kV,220mA
15 28 70 2.OkV,220mA
15 38 60 1.2kV,22OrnA

Table III. The parameters of equations (3) and (4) which describe (with
p = t'
= 0.5) the linear portions of the Rt2 versus t graphs shown in
Figures 7,8,9,10. (a) 1.6kV, (b) 2.2kv.

Au Pt Ni Cu
(a) (b) (a) (b) (a) (b) (a) (b)

p (10 acm) 2.132 1.292 3.41 4.14 7.2 7.2 1.06 0.6

p (10 acm) 0.235 1.06 0.684 0.1673

() 380 220 110 387

v 0.236 0.390 0.666 0.549 0.2036 0.339 0.598

D 60 99 98 81 15 87.5 154
g

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 Table IV The parameters of equation (7), p = 1.3, used to describe the R versus
t behaviour of Au,Pt,Ni,Cu for tt •,
mi Figures 3,4,5,6 - see Figures
11,12.

Metal Au(22OmA) Pt(26OmA) Ni(22OmA) Cu(220rnA)

Sputtering
voltage (kV) 2.2 1.6 2.2 1.8 2.2 1.6 2.2 1.6
x
c 0.57 0.51 0.27 0.30 0.33 0.32 0.24 0.31

5E9 5E9 2E9 2E9 2E9 2E9 2E9 2E9

RD
Rm (W 18.36 33.9 380 260 476 480 9.11 9.36

t mm
() 70 90 30 28 44 42 200 160

t =x t
c c mm () 40 46 8.1 8.4 15 14 48 50

09

08

0.7

0•5 .10'
cr
04 .10'

0)
0•3 E
*10'

02 ILl
1-) .10'

01
C'-)
uJ
5 10 15
(degrees)
.10'

Figure 1. The soft X-ray (X=0.834nm)

reflectivity, versus the glancing angle .10'

of incidence , of a 51/50 Ni/C multi- 150 200 0 300 000

layer in which t1 = 1.Onm, t2 = 1.25nm.
100

THICKNESS (Angst roms)

Figure 3. lBS Au on glass. The

measured change in resistance R with
equivalent Au film thickness t. Ion
Figure 2. — see the gun HT voltage 1.6kv (dotted line),
following page.
2.2kV (full line). Inset shows the
initial stage in greater detail.

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 O5 n m

1•Onm

l5nm

2•Onm

Gold Platinum Nickel

Figure 2. TEM pictures of Au,Pt,Ni

films of thicknesses t = 0.5, 1.0,
1.5 and 2.Onm on carbon substrates.

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 300 550
20
500

3
260
Ion the
450
240 with
The
220
The
R t. line), 400 Figure

the
200 shows
350 of for
110 detail.
t
glass.
300
160
(dotted
glass. Inset
(Angstroms) (Angstroms) on
140
resistance thickness
000 t.
120
on .
greater
Au versus
in of
00
Ni 1.6kV 200
film in
line)
50 lBS measurements
Rt2

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00 THICKNESS THICKNESS
lBS Ni t
60 as
change
100
7. values
1,0 stage
5. voltage
(full
50
20
versus
HT
0 0
Figure R plotted larger
.10' .i0'
—%
0)0) 0 LiC-) I—Co C', Ui
Figure measured equivalent gun 2.2.kv initial
**
C") 0)0) C *0) 0 ** *
C")
500
220
200
Ion
180 450 with
with Ion the
R
the R t.
II
line), (1990)
400 The
160
The t. line),
300
140 shows detail.
Films
shows detail.
300
120
Thin
(dotted
glass.
(dotted
glass.
(Angstr-oms)
(Angstroms)
resistance thickness
Inset
300
100
thickness Inset
resistance
on
on .
greater Optical
.
in .6kV
1
greater
80 in .8kV 200 of
Pt 1 Cu
film in
film in
150
60 line)
THICKNESS
THICKNESS
line) lBS Cu
lBS Pt
Modeling
100
40 change
change stage
stage
6. voltage
4. voltage
50
(full 1324
20 (full
HT Vol.
HT
1o'
0) 0)
-c 9
xrn'
(-)

I0.
(I) (0Li.J
xlO'
c
.io' .10'
Figure measured equivalent gun 2.2kV initial
.10' .10'
0 C-)

.io'
Co

.10' "a' Figure measured equivalent gun 2.2kV initial

/
SPIE
icx;'
 c'j
*
*. *10k
(0
0)
C
*(0
-C
D
c'J
*
*
*

0 20 40 60 00 100 120 140 160 10 2(0 220 0 20 00 60 % 00 120 140 160 leO 200 220 2O 260 210
THICKNESS (Angst roms) THICKNESS (Angstroms)

Figure 8. lBS Pt on glass. The Figure 9. lBS Ni on glass. The

R versus t measurements of Figure 4 R versus t measurements of Figure 5
plotted as Rt2 versus t for the plotted as Rt2 versus t for the
larger values of t. larger values of t.

Gold 2.2kV Cosputer Fit

LE+1D ————____________________________________

* (•...... exptt.
*
*10' (a)
0)
10.00 ( b) p =1.3
C
*
E
C 10000

** 1.) 100000
C
I- a
* 111 10000

1000
a:

100

0 50 100 150 200 200 300 350 400 450 5 550 0.0 1 .2 .3 4 S .6 7 .8 .9 10
THICKNESS (Angstroms) Fractional coverage

Figure 10. lBS Cu on glass. The Figure 11. lBS Au on glass. The fit
R versus t measurements of Figure 6
of the percolation equations (7),
plotted as Rt2 versus t for the p = 1.3, to the measured variation
larger values of t. of R with fractional coverage
x = t/t . for HT voltage 2.2kV.
mm

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 C
a;
U
C
U)
U)
a)

3 .4 5 .6
FrcictionciL coverage 1 10 100
deDositlon time (mm)
Figure 12. lBS Pt on glass. The
fit of the percolation equations (7) Figure 13. The measured thickness tj.
with p = 1 .3, p = 2, to the measured of the Ni layers in Ni/C multilayers
variation of R with fractional as a function of the Ni layer deposition
coverage x = t/tmm
for HT voltage time.
1.8kV.

O•6
I I 1 1 1 1 I I

05 a;
08

r
a;
>
0.L.
0
U

03 ta
I-
0.2

Ii- I I I I I I I I I
0•2 0 2 4 6 8 10 12 14 16 18
EquivaLent film thickness (A)

O1 Figure 15. The fractional area of

substrate covered by an lBS Ni film
compared with that covered by the
5 10 15 same mass of material in the form
0 (degrees) of a continuous film.
Figure 14. The soft X-ray (X = 0.834nm)
reflectivity, versus the glancing angle
of incidence , of a 51/50 Ni/C multi-
layer in which the reflection maximum
is a doublet because each Ni layer is
a composite of ti = 1.0 and 1.2nm.

102 / SPIE Vol. 1324 Modeling of Optical Thin Films 11(1990)

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