Abstract

A method has been developed for analysis of a series of ellipsometric data taken in situ during deposition. With this method the optical constants n and k and thickness d of growing ion-beam-sputtered films of C, Si, Ni, Nb, Mo, Ru, Rh, Pd, Ag, W, Re, and Au have been determined as a function of deposition time t. The minimum critical thickness dc needed for a film to become optically isotropic has been determined from the n, k, d-versus-t curves. Anomalous behavior of these curves appears in the region ddc resulting from a breakdown of the isotropic film model employed. This is shown, by transmission electron micrographs, to have a correlation with a transition region from island/anisotropic to continuous/isotropic.

© 1992 Optical Society of America

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  1. M. Yamamoto, O. S. Heavens, “A vacuum automatic ellipsometer for principal angle of incidence measurements,” Surf. Sci. 96, 202–216 (1980).
    [CrossRef]
  2. T. Yamaguchi, S. Yoshida, A. Kinbara, “Continuous ellipsometric determination of the optical constants and thickness of a silver film during deposition,” Jpn. J. Appl. Phys. 8(5), 559–567 (1969).
    [CrossRef]
  3. M. Yamamoto, A. Arai, H. Shibata, T. Namioka, “Thickness monitoring of ultra-thin films of multi-layered coatings for VUV mirrors by ellipsometry,” in Digest of the Thirteenth Congress of the International Commission for Optics (Organizing Committee of ICO-13, Sapporo, Japan, 1984), pp. 626–627.
  4. R. P. Netterfield, P. J. Martin, W. G. Sainty, R. M. Duffy, C. G. Pacey, “Characterization of growing thin films by in situ ellipsometry, spectral reflectance and transmittance measurements, and ion-scattering spectroscopy,” Rev. Sci. Instrum. 56, 1995–2003 (1985).
    [CrossRef]
  5. R. P. Netterfield, P. J. Martin, “Nucleation and growth studies of gold films prepared by evaporation and ion-assisted deposition,” Appl. Surf. Sci. 25, 265–278 (1986).
    [CrossRef]
  6. F. L. McCrackin, J. P. Colson, “Computational techniques for the use of the exact Drude equation in reflection problems,” Natl. Bur. Stand. U.S. Misc. Publ. 256, 61–84 (1964).
  7. R. H. Muller, “Present status of automatic ellipsometer,” Surf. Sci. 56, 19–36 (1976).
    [CrossRef]
  8. R. J. Archer, Manual on Ellipsometry (Gaertner Scientific Corporation, Chicago, Ill., 1968), p. 17.
  9. F. Abeles, T. Lopez-Rios, “Ellipsometry of metallic films and surfaces with nonlocal effects,” Surf. Sci. 96, 32–40 (1980).
    [CrossRef]
  10. Y. Yoriume, “Method for numerical inversion of the ellipsometry equations for transparent films,” J. Opt. Soc. Am. 73, 888–891 (1983).
    [CrossRef]

1986

R. P. Netterfield, P. J. Martin, “Nucleation and growth studies of gold films prepared by evaporation and ion-assisted deposition,” Appl. Surf. Sci. 25, 265–278 (1986).
[CrossRef]

1985

R. P. Netterfield, P. J. Martin, W. G. Sainty, R. M. Duffy, C. G. Pacey, “Characterization of growing thin films by in situ ellipsometry, spectral reflectance and transmittance measurements, and ion-scattering spectroscopy,” Rev. Sci. Instrum. 56, 1995–2003 (1985).
[CrossRef]

1983

1980

F. Abeles, T. Lopez-Rios, “Ellipsometry of metallic films and surfaces with nonlocal effects,” Surf. Sci. 96, 32–40 (1980).
[CrossRef]

M. Yamamoto, O. S. Heavens, “A vacuum automatic ellipsometer for principal angle of incidence measurements,” Surf. Sci. 96, 202–216 (1980).
[CrossRef]

1976

R. H. Muller, “Present status of automatic ellipsometer,” Surf. Sci. 56, 19–36 (1976).
[CrossRef]

1969

T. Yamaguchi, S. Yoshida, A. Kinbara, “Continuous ellipsometric determination of the optical constants and thickness of a silver film during deposition,” Jpn. J. Appl. Phys. 8(5), 559–567 (1969).
[CrossRef]

1964

F. L. McCrackin, J. P. Colson, “Computational techniques for the use of the exact Drude equation in reflection problems,” Natl. Bur. Stand. U.S. Misc. Publ. 256, 61–84 (1964).

Abeles, F.

F. Abeles, T. Lopez-Rios, “Ellipsometry of metallic films and surfaces with nonlocal effects,” Surf. Sci. 96, 32–40 (1980).
[CrossRef]

Arai, A.

M. Yamamoto, A. Arai, H. Shibata, T. Namioka, “Thickness monitoring of ultra-thin films of multi-layered coatings for VUV mirrors by ellipsometry,” in Digest of the Thirteenth Congress of the International Commission for Optics (Organizing Committee of ICO-13, Sapporo, Japan, 1984), pp. 626–627.

Archer, R. J.

R. J. Archer, Manual on Ellipsometry (Gaertner Scientific Corporation, Chicago, Ill., 1968), p. 17.

Colson, J. P.

F. L. McCrackin, J. P. Colson, “Computational techniques for the use of the exact Drude equation in reflection problems,” Natl. Bur. Stand. U.S. Misc. Publ. 256, 61–84 (1964).

Duffy, R. M.

R. P. Netterfield, P. J. Martin, W. G. Sainty, R. M. Duffy, C. G. Pacey, “Characterization of growing thin films by in situ ellipsometry, spectral reflectance and transmittance measurements, and ion-scattering spectroscopy,” Rev. Sci. Instrum. 56, 1995–2003 (1985).
[CrossRef]

Heavens, O. S.

M. Yamamoto, O. S. Heavens, “A vacuum automatic ellipsometer for principal angle of incidence measurements,” Surf. Sci. 96, 202–216 (1980).
[CrossRef]

Kinbara, A.

T. Yamaguchi, S. Yoshida, A. Kinbara, “Continuous ellipsometric determination of the optical constants and thickness of a silver film during deposition,” Jpn. J. Appl. Phys. 8(5), 559–567 (1969).
[CrossRef]

Lopez-Rios, T.

F. Abeles, T. Lopez-Rios, “Ellipsometry of metallic films and surfaces with nonlocal effects,” Surf. Sci. 96, 32–40 (1980).
[CrossRef]

Martin, P. J.

R. P. Netterfield, P. J. Martin, “Nucleation and growth studies of gold films prepared by evaporation and ion-assisted deposition,” Appl. Surf. Sci. 25, 265–278 (1986).
[CrossRef]

R. P. Netterfield, P. J. Martin, W. G. Sainty, R. M. Duffy, C. G. Pacey, “Characterization of growing thin films by in situ ellipsometry, spectral reflectance and transmittance measurements, and ion-scattering spectroscopy,” Rev. Sci. Instrum. 56, 1995–2003 (1985).
[CrossRef]

McCrackin, F. L.

F. L. McCrackin, J. P. Colson, “Computational techniques for the use of the exact Drude equation in reflection problems,” Natl. Bur. Stand. U.S. Misc. Publ. 256, 61–84 (1964).

Muller, R. H.

R. H. Muller, “Present status of automatic ellipsometer,” Surf. Sci. 56, 19–36 (1976).
[CrossRef]

Namioka, T.

M. Yamamoto, A. Arai, H. Shibata, T. Namioka, “Thickness monitoring of ultra-thin films of multi-layered coatings for VUV mirrors by ellipsometry,” in Digest of the Thirteenth Congress of the International Commission for Optics (Organizing Committee of ICO-13, Sapporo, Japan, 1984), pp. 626–627.

Netterfield, R. P.

R. P. Netterfield, P. J. Martin, “Nucleation and growth studies of gold films prepared by evaporation and ion-assisted deposition,” Appl. Surf. Sci. 25, 265–278 (1986).
[CrossRef]

R. P. Netterfield, P. J. Martin, W. G. Sainty, R. M. Duffy, C. G. Pacey, “Characterization of growing thin films by in situ ellipsometry, spectral reflectance and transmittance measurements, and ion-scattering spectroscopy,” Rev. Sci. Instrum. 56, 1995–2003 (1985).
[CrossRef]

Pacey, C. G.

R. P. Netterfield, P. J. Martin, W. G. Sainty, R. M. Duffy, C. G. Pacey, “Characterization of growing thin films by in situ ellipsometry, spectral reflectance and transmittance measurements, and ion-scattering spectroscopy,” Rev. Sci. Instrum. 56, 1995–2003 (1985).
[CrossRef]

Sainty, W. G.

R. P. Netterfield, P. J. Martin, W. G. Sainty, R. M. Duffy, C. G. Pacey, “Characterization of growing thin films by in situ ellipsometry, spectral reflectance and transmittance measurements, and ion-scattering spectroscopy,” Rev. Sci. Instrum. 56, 1995–2003 (1985).
[CrossRef]

Shibata, H.

M. Yamamoto, A. Arai, H. Shibata, T. Namioka, “Thickness monitoring of ultra-thin films of multi-layered coatings for VUV mirrors by ellipsometry,” in Digest of the Thirteenth Congress of the International Commission for Optics (Organizing Committee of ICO-13, Sapporo, Japan, 1984), pp. 626–627.

Yamaguchi, T.

T. Yamaguchi, S. Yoshida, A. Kinbara, “Continuous ellipsometric determination of the optical constants and thickness of a silver film during deposition,” Jpn. J. Appl. Phys. 8(5), 559–567 (1969).
[CrossRef]

Yamamoto, M.

M. Yamamoto, O. S. Heavens, “A vacuum automatic ellipsometer for principal angle of incidence measurements,” Surf. Sci. 96, 202–216 (1980).
[CrossRef]

M. Yamamoto, A. Arai, H. Shibata, T. Namioka, “Thickness monitoring of ultra-thin films of multi-layered coatings for VUV mirrors by ellipsometry,” in Digest of the Thirteenth Congress of the International Commission for Optics (Organizing Committee of ICO-13, Sapporo, Japan, 1984), pp. 626–627.

Yoriume, Y.

Yoshida, S.

T. Yamaguchi, S. Yoshida, A. Kinbara, “Continuous ellipsometric determination of the optical constants and thickness of a silver film during deposition,” Jpn. J. Appl. Phys. 8(5), 559–567 (1969).
[CrossRef]

Appl. Surf. Sci.

R. P. Netterfield, P. J. Martin, “Nucleation and growth studies of gold films prepared by evaporation and ion-assisted deposition,” Appl. Surf. Sci. 25, 265–278 (1986).
[CrossRef]

J. Opt. Soc. Am.

Jpn. J. Appl. Phys.

T. Yamaguchi, S. Yoshida, A. Kinbara, “Continuous ellipsometric determination of the optical constants and thickness of a silver film during deposition,” Jpn. J. Appl. Phys. 8(5), 559–567 (1969).
[CrossRef]

Natl. Bur. Stand. U.S. Misc. Publ.

F. L. McCrackin, J. P. Colson, “Computational techniques for the use of the exact Drude equation in reflection problems,” Natl. Bur. Stand. U.S. Misc. Publ. 256, 61–84 (1964).

Rev. Sci. Instrum.

R. P. Netterfield, P. J. Martin, W. G. Sainty, R. M. Duffy, C. G. Pacey, “Characterization of growing thin films by in situ ellipsometry, spectral reflectance and transmittance measurements, and ion-scattering spectroscopy,” Rev. Sci. Instrum. 56, 1995–2003 (1985).
[CrossRef]

Surf. Sci.

M. Yamamoto, O. S. Heavens, “A vacuum automatic ellipsometer for principal angle of incidence measurements,” Surf. Sci. 96, 202–216 (1980).
[CrossRef]

R. H. Muller, “Present status of automatic ellipsometer,” Surf. Sci. 56, 19–36 (1976).
[CrossRef]

F. Abeles, T. Lopez-Rios, “Ellipsometry of metallic films and surfaces with nonlocal effects,” Surf. Sci. 96, 32–40 (1980).
[CrossRef]

Other

R. J. Archer, Manual on Ellipsometry (Gaertner Scientific Corporation, Chicago, Ill., 1968), p. 17.

M. Yamamoto, A. Arai, H. Shibata, T. Namioka, “Thickness monitoring of ultra-thin films of multi-layered coatings for VUV mirrors by ellipsometry,” in Digest of the Thirteenth Congress of the International Commission for Optics (Organizing Committee of ICO-13, Sapporo, Japan, 1984), pp. 626–627.

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Figures (21)

Fig. 1
Fig. 1

Schematic of the ion-beam sputtering system.

Fig. 2
Fig. 2

Schematic of the in situ ellipsometric monitor (plan view).

Fig. 3
Fig. 3

Illustration of an accurate method for setting the angle of incidence by means of an alignment prism. An angle of incidence of 56.70° and a BK7 prism are assumed.

Fig. 4
Fig. 4

Gaussian-plane plots of the relative amplitude attenuation ρ measured during the deposition of C on a BK7 substrate (growth curve of C).

Fig. 5
Fig. 5

Growth curves of Si, Ni, Mo, Ru, Rh, Ag, Re, and Au films deposited on BK7 substrates. The points that correspond to a film thickness d of 10 nm are indicated by open circles.

Fig. 6
Fig. 6

Growth curves of C, Nb, Pd, and W films deposited on BK7 substrates. The points that correspond to a film thickness d of 10 nm are indicated by open circles.

Fig. 7
Fig. 7

Plots of n, k, and d versus deposition time t for Au film.

Fig. 8
Fig. 8

Plots of n, k, and d versus deposition time t for Ag film.

Fig. 9
Fig. 9

Plots of n, k, and d versus deposition time t for Ni film.

Fig. 10
Fig. 10

Plots of n, k, and d versus deposition time t for Ru film.

Fig. 11
Fig. 11

Plots of n, k, and d versus deposition time t for Rh film.

Fig. 12
Fig. 12

Plots of n, k, and d versus deposition time t for Pd film.

Fig. 13
Fig. 13

Plots of n, k, and d versus deposition time t for Re film.

Fig. 14
Fig. 14

Plots of n, k, and d versus deposition time t for Nb film.

Fig. 15
Fig. 15

Plots of n, k, and d versus deposition time t for C film.

Fig. 16
Fig. 16

Plots of n, k, and d versus deposition time t for Si film.

Fig. 17
Fig. 17

Plots of n, k, and d versus deposition time t for Mo film.

Fig. 18
Fig. 18

Plots of n, k, and d versus deposition time t for W film. Definitions of tc and dc are illustrated.

Fig. 19
Fig. 19

(a) Observed growth curve (small open circles) of Au film and its simulation curve (solid curve) calculated with n = 0.44 and k = 3.50. The open circles with numerals indicate the growth stages at which TEM specimens were prepared. (b) TEM’s and electron diffraction patterns taken at the growth stages that are indicated by the numbered open circles in (a). In each picture the deposition stage is identified by the corresponding number in the lower left corner.

Fig. 20
Fig. 20

(a) Observed growth curve (small open circles) of Mo film and its simulation curve (solid curve) calculated with n = 3.84 and k = 3.55. The open circles with numerals indicate the growth stages at which TEM specimens were prepared. (b) TEM’s and electron diffraction patterns taken at the growth stages that are indicated by the numbered open circles in (a). In each picture the deposition stage is identified by the corresponding number in the lower left corner.

Fig. 21
Fig. 21

(a) Observed growth curve (small open circles) of Si film and its simulation curve (solid curve) calculated with n = 4.22 and k = 0.46. The open circles with numerals indicate the growth stages at which TEM specimens were prepared, (b) TEM’s and electron diffraction patterns taken at the growth stages that are indicated by the numbered open circles in (a). In each picture the deposition stage is identified by the corresponding number in the lower left corner.

Tables (1)

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Table I Refractive Index n, Extinction Coefficient k, and the Critical Thickness dc of Various Ultrathin Films

Equations (13)

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R p , s = [ r p , s + r p , s exp ( 1 i δ ) ] [ 1 + r p , s r p , s exp ( 1 i δ ) ] ,
δ = ( 4 π d / λ ) ( n ˜ 2 sin 2 ϕ ) 1 / 2 .
ρ R p / R s .
α X 2 + β X + γ = 0 ,
X = exp ( 1 i δ ) , α = r p r s ( r p ρ r s ) , β = r p r s ( r p ρ r s ) + r s ρ r p , γ = r s ρ r p .
exp ( i δ ) = [ β ± ( β 2 4 αγ ) 1 / 2 ] / 2 α .
exp ( i 4 π d / λ ) = [ [ β ± ( β 2 4 αγ ) 1 / 2 ] / 2 α ( n ˜ 2 sin 2 ϕ ) 1 / 2 f ( n ˜ , ρ )
| f ( n ˜ , ρ ) | 2 = 1 .
X X * = 1 ,
α X + β + γ X * = 0 ,
α * X * + β* + γ* X = 0 .
X = ( β * γ α*β ) / ( αα * γγ * ) .
( β*γ α * β ) ( βγ * αβ * ) / ( αα * γγ * ) = 1 .

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