Abstract

The composition-dependent structural, microstructural, optical, and mechanical properties of TiO2–MgF2 composite films prepared by reactive electron-beam coevaporation at a substrate temperature of 280 °C are systematically investigated with an x-ray diffractometer, transmission electron microscope, spectrophotometer and varied angle of incidence spectroscopic ellipsometry, and microhardness tester, respectively. A comparison of the films prepared by reactive ion-assisted coevaporation shows that the films prepared by reactive electron-beam coevaporation have lower refractive indices and hardnesses. However, TiO2–MgF2 composite films prepared by both techniques exhibit similar softening and hardening phenomena and similar microstructures.

© 1996 Optical Society of America

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  1. R. Jacobsson, J. O. Martensson, “Evaporated inhomogeneous thin films,” Appl. Opt. 5, 29–34 (1965).
    [CrossRef]
  2. R. Jacobsson, “Inhomogeneous and coevaporated homogeneous films for optical applications,” Phys. Thin Films 8, 51–98 (1975).
  3. B. Abeles, J. I. Gittleman, “Composite material films: optical properties and applications,” Appl. Opt. 15, 2328–2332 (1976).
    [CrossRef] [PubMed]
  4. D. M. Sanders, E. N. Farabaugh, W. K. Haller, “Glassy optical coatings by multisource evaporation,” in Thin Film Technologies and Special Applications, W. R. Hunter, ed., Proc. SPIE346, 31–38 (1982).
  5. W. J. Gunning, R. L. Hall, F. J. Woodberry, W. H. Southwell, N. S. Gluck, “Codeposition of continuous composition rugate filters,” Appl. Opt. 28, 2945–2948 (1989).
    [CrossRef] [PubMed]
  6. N. S. Gluck, H. Sankur, J. DeNatale, W. J. Gunning, “Microstructure and composition of composite SiO2/TiO2 thin films,” J. Appl. Phys. 69, 3037–3045 (1991).
    [CrossRef]
  7. S. Chao, C.-K. Chang, J.-S. Chen, “TiO2–SiO2 mixed films prepared by the fast alternating sputter method,” Appl. Opt. 30, 3233–3237 (1991).
    [CrossRef] [PubMed]
  8. R. Laird, A. Belkind, “Cosputtered films of mixed TiO2/SiO2,” J. Vac. Sci. Technol. A 10, 1908–1912 (1992).
    [CrossRef]
  9. R.-Y. Tsai, M.-Y. Hua, F. C. Ho, “Influences of the deposition rate on the microstructure and hardness of composite films prepared by reactive ion-assisted coevaporation,” Opt. Eng. 34, 3075–3082 (1995).
    [CrossRef]
  10. E. Ritter, “Dielectric film materials for optical applications,” Phys. Thin Films 8, 1–49 (1975).
  11. C. M. Kennemore, U. J. Gibson, “Ion beam processing for coating MgF2 onto ambient temperature substrates,” Appl. Opt. 23, 3608–3611 (1984).
    [CrossRef] [PubMed]
  12. P. J. Martin, R. P. Netterfield, “Ion-assisted deposition of magnesium fluoride films on substrates at ambient temperatures,” Appl. Opt. 24, 1732–1733 (1985).
    [CrossRef]
  13. K. Balasubramanian, X. F. Han, K. H. Guenther, “Comparative study of titanium dioxide thin films produced by electron-beam evaporation and by reactive low-voltage ion plating,” Appl. Opt. 32, 5594–5600 (1993).
    [CrossRef] [PubMed]
  14. W. C. Martyny, R. J. Olwert, “Electric lamp envelope having clear protective coating and method of making,” U.S. patent3,775,161 (27November1973).
  15. K. Memarzadeh, J. A. Woollam, A. Belkind, “Variable angle of incidence spectroscopic ellipsometric characterization of TiO2/Ag/TiO2 optical coatings,” J. Appl. Phys. 64, 3407–3410 (1988).
    [CrossRef]
  16. M. F. Doerner, W. D. Nix, “A method for interpreting the data from depth-sensing indentation instruments,” J. Mater. Res. 1, 601–609 (1986).
    [CrossRef]
  17. H. S. Coleman, A. F. Turner, O. A. Ullrich, “Crystal orientation and refractive index of thick evaporated MgF2 films,” J. Opt. Soc. Am. 37, 521 (1947).
  18. Inorganic File, Plate 6-290 (International Center for Diffraction Data, 1977).
  19. R.-Y. Tsai, M.-Y. Hua, C.-T. Wei, F. C. Ho, “Characterizations of composite TiO2–MgF2 films prepared by reactive ion-assisted coevaporation,” Opt. Eng. 33, 3411–3418 (1994).
    [CrossRef]
  20. D. E. Gray, ed., American Institute of Physics Handbook (McGraw-Hill, New York, 1972), pp. 6–50.
  21. J. M. Bennett, E. Pelletier, G. Albrand, J. P. Borgogno, B. Lazarides, C. K. Carniglia, R. A. Schmell, T. H. Allen, T. Tuttle-Hart, K. H. Guenther, A. Saxer, “Comparison of the properties of titanium dioxide films prepared by various techniques,” Appl. Opt. 28, 3303–3317 (1989).
    [CrossRef] [PubMed]
  22. T. Takagi, “Role of ions in ion-based film formation,” Thin Solid Films 92, 1–17 (1982).
    [CrossRef]

1995

R.-Y. Tsai, M.-Y. Hua, F. C. Ho, “Influences of the deposition rate on the microstructure and hardness of composite films prepared by reactive ion-assisted coevaporation,” Opt. Eng. 34, 3075–3082 (1995).
[CrossRef]

1994

R.-Y. Tsai, M.-Y. Hua, C.-T. Wei, F. C. Ho, “Characterizations of composite TiO2–MgF2 films prepared by reactive ion-assisted coevaporation,” Opt. Eng. 33, 3411–3418 (1994).
[CrossRef]

1993

1992

R. Laird, A. Belkind, “Cosputtered films of mixed TiO2/SiO2,” J. Vac. Sci. Technol. A 10, 1908–1912 (1992).
[CrossRef]

1991

N. S. Gluck, H. Sankur, J. DeNatale, W. J. Gunning, “Microstructure and composition of composite SiO2/TiO2 thin films,” J. Appl. Phys. 69, 3037–3045 (1991).
[CrossRef]

S. Chao, C.-K. Chang, J.-S. Chen, “TiO2–SiO2 mixed films prepared by the fast alternating sputter method,” Appl. Opt. 30, 3233–3237 (1991).
[CrossRef] [PubMed]

1989

1988

K. Memarzadeh, J. A. Woollam, A. Belkind, “Variable angle of incidence spectroscopic ellipsometric characterization of TiO2/Ag/TiO2 optical coatings,” J. Appl. Phys. 64, 3407–3410 (1988).
[CrossRef]

1986

M. F. Doerner, W. D. Nix, “A method for interpreting the data from depth-sensing indentation instruments,” J. Mater. Res. 1, 601–609 (1986).
[CrossRef]

1985

1984

1982

T. Takagi, “Role of ions in ion-based film formation,” Thin Solid Films 92, 1–17 (1982).
[CrossRef]

1976

1975

R. Jacobsson, “Inhomogeneous and coevaporated homogeneous films for optical applications,” Phys. Thin Films 8, 51–98 (1975).

E. Ritter, “Dielectric film materials for optical applications,” Phys. Thin Films 8, 1–49 (1975).

1965

1947

H. S. Coleman, A. F. Turner, O. A. Ullrich, “Crystal orientation and refractive index of thick evaporated MgF2 films,” J. Opt. Soc. Am. 37, 521 (1947).

Abeles, B.

Albrand, G.

Allen, T. H.

Balasubramanian, K.

Belkind, A.

R. Laird, A. Belkind, “Cosputtered films of mixed TiO2/SiO2,” J. Vac. Sci. Technol. A 10, 1908–1912 (1992).
[CrossRef]

K. Memarzadeh, J. A. Woollam, A. Belkind, “Variable angle of incidence spectroscopic ellipsometric characterization of TiO2/Ag/TiO2 optical coatings,” J. Appl. Phys. 64, 3407–3410 (1988).
[CrossRef]

Bennett, J. M.

Borgogno, J. P.

Carniglia, C. K.

Chang, C.-K.

Chao, S.

Chen, J.-S.

Coleman, H. S.

H. S. Coleman, A. F. Turner, O. A. Ullrich, “Crystal orientation and refractive index of thick evaporated MgF2 films,” J. Opt. Soc. Am. 37, 521 (1947).

DeNatale, J.

N. S. Gluck, H. Sankur, J. DeNatale, W. J. Gunning, “Microstructure and composition of composite SiO2/TiO2 thin films,” J. Appl. Phys. 69, 3037–3045 (1991).
[CrossRef]

Doerner, M. F.

M. F. Doerner, W. D. Nix, “A method for interpreting the data from depth-sensing indentation instruments,” J. Mater. Res. 1, 601–609 (1986).
[CrossRef]

Farabaugh, E. N.

D. M. Sanders, E. N. Farabaugh, W. K. Haller, “Glassy optical coatings by multisource evaporation,” in Thin Film Technologies and Special Applications, W. R. Hunter, ed., Proc. SPIE346, 31–38 (1982).

Gibson, U. J.

Gittleman, J. I.

Gluck, N. S.

N. S. Gluck, H. Sankur, J. DeNatale, W. J. Gunning, “Microstructure and composition of composite SiO2/TiO2 thin films,” J. Appl. Phys. 69, 3037–3045 (1991).
[CrossRef]

W. J. Gunning, R. L. Hall, F. J. Woodberry, W. H. Southwell, N. S. Gluck, “Codeposition of continuous composition rugate filters,” Appl. Opt. 28, 2945–2948 (1989).
[CrossRef] [PubMed]

Guenther, K. H.

Gunning, W. J.

N. S. Gluck, H. Sankur, J. DeNatale, W. J. Gunning, “Microstructure and composition of composite SiO2/TiO2 thin films,” J. Appl. Phys. 69, 3037–3045 (1991).
[CrossRef]

W. J. Gunning, R. L. Hall, F. J. Woodberry, W. H. Southwell, N. S. Gluck, “Codeposition of continuous composition rugate filters,” Appl. Opt. 28, 2945–2948 (1989).
[CrossRef] [PubMed]

Hall, R. L.

Haller, W. K.

D. M. Sanders, E. N. Farabaugh, W. K. Haller, “Glassy optical coatings by multisource evaporation,” in Thin Film Technologies and Special Applications, W. R. Hunter, ed., Proc. SPIE346, 31–38 (1982).

Han, X. F.

Ho, F. C.

R.-Y. Tsai, M.-Y. Hua, F. C. Ho, “Influences of the deposition rate on the microstructure and hardness of composite films prepared by reactive ion-assisted coevaporation,” Opt. Eng. 34, 3075–3082 (1995).
[CrossRef]

R.-Y. Tsai, M.-Y. Hua, C.-T. Wei, F. C. Ho, “Characterizations of composite TiO2–MgF2 films prepared by reactive ion-assisted coevaporation,” Opt. Eng. 33, 3411–3418 (1994).
[CrossRef]

Hua, M.-Y.

R.-Y. Tsai, M.-Y. Hua, F. C. Ho, “Influences of the deposition rate on the microstructure and hardness of composite films prepared by reactive ion-assisted coevaporation,” Opt. Eng. 34, 3075–3082 (1995).
[CrossRef]

R.-Y. Tsai, M.-Y. Hua, C.-T. Wei, F. C. Ho, “Characterizations of composite TiO2–MgF2 films prepared by reactive ion-assisted coevaporation,” Opt. Eng. 33, 3411–3418 (1994).
[CrossRef]

Jacobsson, R.

R. Jacobsson, “Inhomogeneous and coevaporated homogeneous films for optical applications,” Phys. Thin Films 8, 51–98 (1975).

R. Jacobsson, J. O. Martensson, “Evaporated inhomogeneous thin films,” Appl. Opt. 5, 29–34 (1965).
[CrossRef]

Kennemore, C. M.

Laird, R.

R. Laird, A. Belkind, “Cosputtered films of mixed TiO2/SiO2,” J. Vac. Sci. Technol. A 10, 1908–1912 (1992).
[CrossRef]

Lazarides, B.

Martensson, J. O.

Martin, P. J.

Martyny, W. C.

W. C. Martyny, R. J. Olwert, “Electric lamp envelope having clear protective coating and method of making,” U.S. patent3,775,161 (27November1973).

Memarzadeh, K.

K. Memarzadeh, J. A. Woollam, A. Belkind, “Variable angle of incidence spectroscopic ellipsometric characterization of TiO2/Ag/TiO2 optical coatings,” J. Appl. Phys. 64, 3407–3410 (1988).
[CrossRef]

Netterfield, R. P.

Nix, W. D.

M. F. Doerner, W. D. Nix, “A method for interpreting the data from depth-sensing indentation instruments,” J. Mater. Res. 1, 601–609 (1986).
[CrossRef]

Olwert, R. J.

W. C. Martyny, R. J. Olwert, “Electric lamp envelope having clear protective coating and method of making,” U.S. patent3,775,161 (27November1973).

Pelletier, E.

Ritter, E.

E. Ritter, “Dielectric film materials for optical applications,” Phys. Thin Films 8, 1–49 (1975).

Sanders, D. M.

D. M. Sanders, E. N. Farabaugh, W. K. Haller, “Glassy optical coatings by multisource evaporation,” in Thin Film Technologies and Special Applications, W. R. Hunter, ed., Proc. SPIE346, 31–38 (1982).

Sankur, H.

N. S. Gluck, H. Sankur, J. DeNatale, W. J. Gunning, “Microstructure and composition of composite SiO2/TiO2 thin films,” J. Appl. Phys. 69, 3037–3045 (1991).
[CrossRef]

Saxer, A.

Schmell, R. A.

Southwell, W. H.

Takagi, T.

T. Takagi, “Role of ions in ion-based film formation,” Thin Solid Films 92, 1–17 (1982).
[CrossRef]

Tsai, R.-Y.

R.-Y. Tsai, M.-Y. Hua, F. C. Ho, “Influences of the deposition rate on the microstructure and hardness of composite films prepared by reactive ion-assisted coevaporation,” Opt. Eng. 34, 3075–3082 (1995).
[CrossRef]

R.-Y. Tsai, M.-Y. Hua, C.-T. Wei, F. C. Ho, “Characterizations of composite TiO2–MgF2 films prepared by reactive ion-assisted coevaporation,” Opt. Eng. 33, 3411–3418 (1994).
[CrossRef]

Turner, A. F.

H. S. Coleman, A. F. Turner, O. A. Ullrich, “Crystal orientation and refractive index of thick evaporated MgF2 films,” J. Opt. Soc. Am. 37, 521 (1947).

Tuttle-Hart, T.

Ullrich, O. A.

H. S. Coleman, A. F. Turner, O. A. Ullrich, “Crystal orientation and refractive index of thick evaporated MgF2 films,” J. Opt. Soc. Am. 37, 521 (1947).

Wei, C.-T.

R.-Y. Tsai, M.-Y. Hua, C.-T. Wei, F. C. Ho, “Characterizations of composite TiO2–MgF2 films prepared by reactive ion-assisted coevaporation,” Opt. Eng. 33, 3411–3418 (1994).
[CrossRef]

Woodberry, F. J.

Woollam, J. A.

K. Memarzadeh, J. A. Woollam, A. Belkind, “Variable angle of incidence spectroscopic ellipsometric characterization of TiO2/Ag/TiO2 optical coatings,” J. Appl. Phys. 64, 3407–3410 (1988).
[CrossRef]

Appl. Opt.

R. Jacobsson, J. O. Martensson, “Evaporated inhomogeneous thin films,” Appl. Opt. 5, 29–34 (1965).
[CrossRef]

B. Abeles, J. I. Gittleman, “Composite material films: optical properties and applications,” Appl. Opt. 15, 2328–2332 (1976).
[CrossRef] [PubMed]

S. Chao, C.-K. Chang, J.-S. Chen, “TiO2–SiO2 mixed films prepared by the fast alternating sputter method,” Appl. Opt. 30, 3233–3237 (1991).
[CrossRef] [PubMed]

C. M. Kennemore, U. J. Gibson, “Ion beam processing for coating MgF2 onto ambient temperature substrates,” Appl. Opt. 23, 3608–3611 (1984).
[CrossRef] [PubMed]

P. J. Martin, R. P. Netterfield, “Ion-assisted deposition of magnesium fluoride films on substrates at ambient temperatures,” Appl. Opt. 24, 1732–1733 (1985).
[CrossRef]

K. Balasubramanian, X. F. Han, K. H. Guenther, “Comparative study of titanium dioxide thin films produced by electron-beam evaporation and by reactive low-voltage ion plating,” Appl. Opt. 32, 5594–5600 (1993).
[CrossRef] [PubMed]

W. J. Gunning, R. L. Hall, F. J. Woodberry, W. H. Southwell, N. S. Gluck, “Codeposition of continuous composition rugate filters,” Appl. Opt. 28, 2945–2948 (1989).
[CrossRef] [PubMed]

J. M. Bennett, E. Pelletier, G. Albrand, J. P. Borgogno, B. Lazarides, C. K. Carniglia, R. A. Schmell, T. H. Allen, T. Tuttle-Hart, K. H. Guenther, A. Saxer, “Comparison of the properties of titanium dioxide films prepared by various techniques,” Appl. Opt. 28, 3303–3317 (1989).
[CrossRef] [PubMed]

J. Appl. Phys.

N. S. Gluck, H. Sankur, J. DeNatale, W. J. Gunning, “Microstructure and composition of composite SiO2/TiO2 thin films,” J. Appl. Phys. 69, 3037–3045 (1991).
[CrossRef]

K. Memarzadeh, J. A. Woollam, A. Belkind, “Variable angle of incidence spectroscopic ellipsometric characterization of TiO2/Ag/TiO2 optical coatings,” J. Appl. Phys. 64, 3407–3410 (1988).
[CrossRef]

J. Mater. Res.

M. F. Doerner, W. D. Nix, “A method for interpreting the data from depth-sensing indentation instruments,” J. Mater. Res. 1, 601–609 (1986).
[CrossRef]

J. Opt. Soc. Am.

H. S. Coleman, A. F. Turner, O. A. Ullrich, “Crystal orientation and refractive index of thick evaporated MgF2 films,” J. Opt. Soc. Am. 37, 521 (1947).

J. Vac. Sci. Technol. A

R. Laird, A. Belkind, “Cosputtered films of mixed TiO2/SiO2,” J. Vac. Sci. Technol. A 10, 1908–1912 (1992).
[CrossRef]

Opt. Eng.

R.-Y. Tsai, M.-Y. Hua, F. C. Ho, “Influences of the deposition rate on the microstructure and hardness of composite films prepared by reactive ion-assisted coevaporation,” Opt. Eng. 34, 3075–3082 (1995).
[CrossRef]

R.-Y. Tsai, M.-Y. Hua, C.-T. Wei, F. C. Ho, “Characterizations of composite TiO2–MgF2 films prepared by reactive ion-assisted coevaporation,” Opt. Eng. 33, 3411–3418 (1994).
[CrossRef]

Phys. Thin Films

E. Ritter, “Dielectric film materials for optical applications,” Phys. Thin Films 8, 1–49 (1975).

R. Jacobsson, “Inhomogeneous and coevaporated homogeneous films for optical applications,” Phys. Thin Films 8, 51–98 (1975).

Thin Solid Films

T. Takagi, “Role of ions in ion-based film formation,” Thin Solid Films 92, 1–17 (1982).
[CrossRef]

Other

D. E. Gray, ed., American Institute of Physics Handbook (McGraw-Hill, New York, 1972), pp. 6–50.

D. M. Sanders, E. N. Farabaugh, W. K. Haller, “Glassy optical coatings by multisource evaporation,” in Thin Film Technologies and Special Applications, W. R. Hunter, ed., Proc. SPIE346, 31–38 (1982).

Inorganic File, Plate 6-290 (International Center for Diffraction Data, 1977).

W. C. Martyny, R. J. Olwert, “Electric lamp envelope having clear protective coating and method of making,” U.S. patent3,775,161 (27November1973).

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Figures (6)

Fig. 1
Fig. 1

XRD patterns of TiO2–MgF2 composite films prepared by reactive EBC at the substrate temperature of 280 °C as a function of the composition.

Fig. 2
Fig. 2

XRD patterns of pure MgF2 films deposited by reactive EB evaporation at the substrate temperature of 280 °C as a function of the working pressure.

Fig. 3
Fig. 3

TEM micrographs and electron diffraction patterns of TiO2–MgF2 composite films with different TiO2 contents prepared by reactive EBC at the substrate temperature of 280 °C. The EB energy is 120 keV. a, b, Pure MgF2; c, d, 39.3 at. % TiO2; e, f, 60 at. % TiO2; g, h, pure TiO2.

Fig. 4
Fig. 4

Spectral transmittance curves of TiO2–MgF2 composite films with different TiO2 contents prepared by reactive EBC at the substrate temperature of 280 °C.

Fig. 5
Fig. 5

Refractive index versus wavelength for the TiO2–MgF2 composite films with various composition ratios of TiO2:MgF2 prepared by reactive EBC at the substrate temperature of 280 °C.

Fig. 6
Fig. 6

Hardnesses of the TiO2–MgF2 composite films prepared by reactive EBC at the substrate temperature of 280 °C as a function of TiO2 composition. Hardnesses of the films prepared by reactive IAC at ambient substrate temperatures are also included for comparison.

Tables (1)

Tables Icon

Table 1 Comparison of the Chemical Compositions (Atomic Fraction) of the TiO2–MgF2 Composite Films prepared by Reactive EBC and IAC as Functions of the Evaporation Rate of MgF2, while the Evaporation Rate of TiO2 is Maintained at 0.2 nm/s

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