Abstract

A design-of-experiments statistical approach was taken to determine the optimum ion gun operating parameters for the deposition of moisture-stable, low-absorbing hafnium oxide films by ion-assisted electron-beam evaporation. Factors identified as affecting the quality of hafnia films were chamber pressure, deposition rate, ion gun source gas composition, and ion gun current. Both oxygen and argon were used as source gases. High and low levels of the factors were chosen on the basis of our experience with the operating range of the system, and we made a series of 24 runs with all possible combinations of these factors. From a statistical analysis of the data, we find that the best films are obtained with a 1:1 mixture of argon and oxygen, 3–3.5 × 10-4 Torr chamber pressure, 0.3-nm/s deposition rate, and 0.5-A ion gun current. X-ray diffraction measurements show that the ion-assisted films exhibit a partial monoclinic crystalline structure, whereas the unassisted films are amorphous.

© 2002 Optical Society of America

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  1. F. Rainer, W. H. Lowdermilk, D. Milam, C. K. Carniglia, T. T. Hart, T. L. Lichtenstein, “Materials for optical coatings in the ultraviolet,” Appl. Opt. 24, 496–500 (1985).
    [Crossref] [PubMed]
  2. P. Baumeister, O. Arnon, “Use of hafnium dioxide in multilayer dielectric reflectors for the near UV,” Appl. Opt. 16, 439–444 (1977).
    [Crossref] [PubMed]
  3. T. R. Jensen, R. L. Johnson, J. Ballou, W. Prohaska, S. E. Morin, “Environmentally stable UV Raman edge filters,” Soc. Vac. Coaters Proc. Annu. Tech. Conf. 505, 239–243 (2000).
  4. J. F. Anzellotti, D. J. Smith, R. J. Sczupak, Z. R. Chrzan, “Stress and environmental shift characteristics of HfO2/SiO2 multilayer coatings,” in Laser-Induced Damage in Optical Materials: 1996, H. E. Bennett, A. H. Guenther, M. R. Kozlowski, B. E. Newnam, M. J. Soileau, eds., Proc. SPIE2966, 258–264 (1997).
  5. J. P. Lehan, Y. Mao, B. G. Bovard, H. A. Macleod, “Optical and microstructural properties of hafnium dioxide thin films,” Thin Solid Films 203, 227–250 (1991).
    [Crossref]
  6. M. Gilo, N. Croitoru, “Study of HfO2 films prepared by ion-assisted deposition using a gridless end-hall ion source,” Thin Solid Films 350, 203–208 (1999).
    [Crossref]
  7. R. Götzelmann, H. Hagedorn, A. Zöller, “UV coatings produced with plasma-ion-assisted deposition,” in Advances in Optical Interference Coatings, C. Amra, H. A. Macleod, eds., Proc. SPIE3738, 48–57 (1999).
  8. M. Alvisi, S. Scaglione, S. Martelli, A. Rizzo, L. Vasanelli, “Structural and optical modification in hafnium oxide thin films related to the momentum parameter transferred by ion beam assistance,” Thin Solid Films 354, 19–23 (1999).
    [Crossref]
  9. J. J. McNally, G. A. Al-Jumaily, S. R. Wilson, J. R. McNeil, “Ion beam assisted deposition of optical thin films—recent results,” in Southwest Conference on Optics, ’85, S. C. Stotlar, ed., Proc. SPIE540, 479–485 (1985).
  10. O. Zabeida, J. E. Klemberg-Sapieha, L. Martinu, D. Morton, “Ion bombardment characteristics during the growth of optical films using a cold cathode ion source,” Soc. Vac. Coaters Proc. Annu. Tech. Conf. 504, 267–271 (1999).
  11. D. Morton, Denton Vacuum, Moorestown, N.J. (personal communication, 2000).

2000 (1)

T. R. Jensen, R. L. Johnson, J. Ballou, W. Prohaska, S. E. Morin, “Environmentally stable UV Raman edge filters,” Soc. Vac. Coaters Proc. Annu. Tech. Conf. 505, 239–243 (2000).

1999 (3)

M. Gilo, N. Croitoru, “Study of HfO2 films prepared by ion-assisted deposition using a gridless end-hall ion source,” Thin Solid Films 350, 203–208 (1999).
[Crossref]

M. Alvisi, S. Scaglione, S. Martelli, A. Rizzo, L. Vasanelli, “Structural and optical modification in hafnium oxide thin films related to the momentum parameter transferred by ion beam assistance,” Thin Solid Films 354, 19–23 (1999).
[Crossref]

O. Zabeida, J. E. Klemberg-Sapieha, L. Martinu, D. Morton, “Ion bombardment characteristics during the growth of optical films using a cold cathode ion source,” Soc. Vac. Coaters Proc. Annu. Tech. Conf. 504, 267–271 (1999).

1991 (1)

J. P. Lehan, Y. Mao, B. G. Bovard, H. A. Macleod, “Optical and microstructural properties of hafnium dioxide thin films,” Thin Solid Films 203, 227–250 (1991).
[Crossref]

1985 (1)

1977 (1)

P. Baumeister, O. Arnon, “Use of hafnium dioxide in multilayer dielectric reflectors for the near UV,” Appl. Opt. 16, 439–444 (1977).
[Crossref] [PubMed]

Al-Jumaily, G. A.

J. J. McNally, G. A. Al-Jumaily, S. R. Wilson, J. R. McNeil, “Ion beam assisted deposition of optical thin films—recent results,” in Southwest Conference on Optics, ’85, S. C. Stotlar, ed., Proc. SPIE540, 479–485 (1985).

Alvisi, M.

M. Alvisi, S. Scaglione, S. Martelli, A. Rizzo, L. Vasanelli, “Structural and optical modification in hafnium oxide thin films related to the momentum parameter transferred by ion beam assistance,” Thin Solid Films 354, 19–23 (1999).
[Crossref]

Anzellotti, J. F.

J. F. Anzellotti, D. J. Smith, R. J. Sczupak, Z. R. Chrzan, “Stress and environmental shift characteristics of HfO2/SiO2 multilayer coatings,” in Laser-Induced Damage in Optical Materials: 1996, H. E. Bennett, A. H. Guenther, M. R. Kozlowski, B. E. Newnam, M. J. Soileau, eds., Proc. SPIE2966, 258–264 (1997).

Arnon, O.

P. Baumeister, O. Arnon, “Use of hafnium dioxide in multilayer dielectric reflectors for the near UV,” Appl. Opt. 16, 439–444 (1977).
[Crossref] [PubMed]

Ballou, J.

T. R. Jensen, R. L. Johnson, J. Ballou, W. Prohaska, S. E. Morin, “Environmentally stable UV Raman edge filters,” Soc. Vac. Coaters Proc. Annu. Tech. Conf. 505, 239–243 (2000).

Baumeister, P.

P. Baumeister, O. Arnon, “Use of hafnium dioxide in multilayer dielectric reflectors for the near UV,” Appl. Opt. 16, 439–444 (1977).
[Crossref] [PubMed]

Bovard, B. G.

J. P. Lehan, Y. Mao, B. G. Bovard, H. A. Macleod, “Optical and microstructural properties of hafnium dioxide thin films,” Thin Solid Films 203, 227–250 (1991).
[Crossref]

Carniglia, C. K.

Chrzan, Z. R.

J. F. Anzellotti, D. J. Smith, R. J. Sczupak, Z. R. Chrzan, “Stress and environmental shift characteristics of HfO2/SiO2 multilayer coatings,” in Laser-Induced Damage in Optical Materials: 1996, H. E. Bennett, A. H. Guenther, M. R. Kozlowski, B. E. Newnam, M. J. Soileau, eds., Proc. SPIE2966, 258–264 (1997).

Croitoru, N.

M. Gilo, N. Croitoru, “Study of HfO2 films prepared by ion-assisted deposition using a gridless end-hall ion source,” Thin Solid Films 350, 203–208 (1999).
[Crossref]

Gilo, M.

M. Gilo, N. Croitoru, “Study of HfO2 films prepared by ion-assisted deposition using a gridless end-hall ion source,” Thin Solid Films 350, 203–208 (1999).
[Crossref]

Götzelmann, R.

R. Götzelmann, H. Hagedorn, A. Zöller, “UV coatings produced with plasma-ion-assisted deposition,” in Advances in Optical Interference Coatings, C. Amra, H. A. Macleod, eds., Proc. SPIE3738, 48–57 (1999).

Hagedorn, H.

R. Götzelmann, H. Hagedorn, A. Zöller, “UV coatings produced with plasma-ion-assisted deposition,” in Advances in Optical Interference Coatings, C. Amra, H. A. Macleod, eds., Proc. SPIE3738, 48–57 (1999).

Hart, T. T.

Jensen, T. R.

T. R. Jensen, R. L. Johnson, J. Ballou, W. Prohaska, S. E. Morin, “Environmentally stable UV Raman edge filters,” Soc. Vac. Coaters Proc. Annu. Tech. Conf. 505, 239–243 (2000).

Johnson, R. L.

T. R. Jensen, R. L. Johnson, J. Ballou, W. Prohaska, S. E. Morin, “Environmentally stable UV Raman edge filters,” Soc. Vac. Coaters Proc. Annu. Tech. Conf. 505, 239–243 (2000).

Klemberg-Sapieha, J. E.

O. Zabeida, J. E. Klemberg-Sapieha, L. Martinu, D. Morton, “Ion bombardment characteristics during the growth of optical films using a cold cathode ion source,” Soc. Vac. Coaters Proc. Annu. Tech. Conf. 504, 267–271 (1999).

Lehan, J. P.

J. P. Lehan, Y. Mao, B. G. Bovard, H. A. Macleod, “Optical and microstructural properties of hafnium dioxide thin films,” Thin Solid Films 203, 227–250 (1991).
[Crossref]

Lichtenstein, T. L.

Lowdermilk, W. H.

Macleod, H. A.

J. P. Lehan, Y. Mao, B. G. Bovard, H. A. Macleod, “Optical and microstructural properties of hafnium dioxide thin films,” Thin Solid Films 203, 227–250 (1991).
[Crossref]

Mao, Y.

J. P. Lehan, Y. Mao, B. G. Bovard, H. A. Macleod, “Optical and microstructural properties of hafnium dioxide thin films,” Thin Solid Films 203, 227–250 (1991).
[Crossref]

Martelli, S.

M. Alvisi, S. Scaglione, S. Martelli, A. Rizzo, L. Vasanelli, “Structural and optical modification in hafnium oxide thin films related to the momentum parameter transferred by ion beam assistance,” Thin Solid Films 354, 19–23 (1999).
[Crossref]

Martinu, L.

O. Zabeida, J. E. Klemberg-Sapieha, L. Martinu, D. Morton, “Ion bombardment characteristics during the growth of optical films using a cold cathode ion source,” Soc. Vac. Coaters Proc. Annu. Tech. Conf. 504, 267–271 (1999).

McNally, J. J.

J. J. McNally, G. A. Al-Jumaily, S. R. Wilson, J. R. McNeil, “Ion beam assisted deposition of optical thin films—recent results,” in Southwest Conference on Optics, ’85, S. C. Stotlar, ed., Proc. SPIE540, 479–485 (1985).

McNeil, J. R.

J. J. McNally, G. A. Al-Jumaily, S. R. Wilson, J. R. McNeil, “Ion beam assisted deposition of optical thin films—recent results,” in Southwest Conference on Optics, ’85, S. C. Stotlar, ed., Proc. SPIE540, 479–485 (1985).

Milam, D.

Morin, S. E.

T. R. Jensen, R. L. Johnson, J. Ballou, W. Prohaska, S. E. Morin, “Environmentally stable UV Raman edge filters,” Soc. Vac. Coaters Proc. Annu. Tech. Conf. 505, 239–243 (2000).

Morton, D.

O. Zabeida, J. E. Klemberg-Sapieha, L. Martinu, D. Morton, “Ion bombardment characteristics during the growth of optical films using a cold cathode ion source,” Soc. Vac. Coaters Proc. Annu. Tech. Conf. 504, 267–271 (1999).

D. Morton, Denton Vacuum, Moorestown, N.J. (personal communication, 2000).

Prohaska, W.

T. R. Jensen, R. L. Johnson, J. Ballou, W. Prohaska, S. E. Morin, “Environmentally stable UV Raman edge filters,” Soc. Vac. Coaters Proc. Annu. Tech. Conf. 505, 239–243 (2000).

Rainer, F.

Rizzo, A.

M. Alvisi, S. Scaglione, S. Martelli, A. Rizzo, L. Vasanelli, “Structural and optical modification in hafnium oxide thin films related to the momentum parameter transferred by ion beam assistance,” Thin Solid Films 354, 19–23 (1999).
[Crossref]

Scaglione, S.

M. Alvisi, S. Scaglione, S. Martelli, A. Rizzo, L. Vasanelli, “Structural and optical modification in hafnium oxide thin films related to the momentum parameter transferred by ion beam assistance,” Thin Solid Films 354, 19–23 (1999).
[Crossref]

Sczupak, R. J.

J. F. Anzellotti, D. J. Smith, R. J. Sczupak, Z. R. Chrzan, “Stress and environmental shift characteristics of HfO2/SiO2 multilayer coatings,” in Laser-Induced Damage in Optical Materials: 1996, H. E. Bennett, A. H. Guenther, M. R. Kozlowski, B. E. Newnam, M. J. Soileau, eds., Proc. SPIE2966, 258–264 (1997).

Smith, D. J.

J. F. Anzellotti, D. J. Smith, R. J. Sczupak, Z. R. Chrzan, “Stress and environmental shift characteristics of HfO2/SiO2 multilayer coatings,” in Laser-Induced Damage in Optical Materials: 1996, H. E. Bennett, A. H. Guenther, M. R. Kozlowski, B. E. Newnam, M. J. Soileau, eds., Proc. SPIE2966, 258–264 (1997).

Vasanelli, L.

M. Alvisi, S. Scaglione, S. Martelli, A. Rizzo, L. Vasanelli, “Structural and optical modification in hafnium oxide thin films related to the momentum parameter transferred by ion beam assistance,” Thin Solid Films 354, 19–23 (1999).
[Crossref]

Wilson, S. R.

J. J. McNally, G. A. Al-Jumaily, S. R. Wilson, J. R. McNeil, “Ion beam assisted deposition of optical thin films—recent results,” in Southwest Conference on Optics, ’85, S. C. Stotlar, ed., Proc. SPIE540, 479–485 (1985).

Zabeida, O.

O. Zabeida, J. E. Klemberg-Sapieha, L. Martinu, D. Morton, “Ion bombardment characteristics during the growth of optical films using a cold cathode ion source,” Soc. Vac. Coaters Proc. Annu. Tech. Conf. 504, 267–271 (1999).

Zöller, A.

R. Götzelmann, H. Hagedorn, A. Zöller, “UV coatings produced with plasma-ion-assisted deposition,” in Advances in Optical Interference Coatings, C. Amra, H. A. Macleod, eds., Proc. SPIE3738, 48–57 (1999).

Appl. Opt. (1)

P. Baumeister, O. Arnon, “Use of hafnium dioxide in multilayer dielectric reflectors for the near UV,” Appl. Opt. 16, 439–444 (1977).
[Crossref] [PubMed]

Appl. Opt. (1)

Soc. Vac. Coaters Proc. Annu. Tech. Conf. (1)

T. R. Jensen, R. L. Johnson, J. Ballou, W. Prohaska, S. E. Morin, “Environmentally stable UV Raman edge filters,” Soc. Vac. Coaters Proc. Annu. Tech. Conf. 505, 239–243 (2000).

Soc. Vac. Coaters Proc. Annu. Tech. Conf. (1)

O. Zabeida, J. E. Klemberg-Sapieha, L. Martinu, D. Morton, “Ion bombardment characteristics during the growth of optical films using a cold cathode ion source,” Soc. Vac. Coaters Proc. Annu. Tech. Conf. 504, 267–271 (1999).

Thin Solid Films (1)

J. P. Lehan, Y. Mao, B. G. Bovard, H. A. Macleod, “Optical and microstructural properties of hafnium dioxide thin films,” Thin Solid Films 203, 227–250 (1991).
[Crossref]

Thin Solid Films (2)

M. Gilo, N. Croitoru, “Study of HfO2 films prepared by ion-assisted deposition using a gridless end-hall ion source,” Thin Solid Films 350, 203–208 (1999).
[Crossref]

M. Alvisi, S. Scaglione, S. Martelli, A. Rizzo, L. Vasanelli, “Structural and optical modification in hafnium oxide thin films related to the momentum parameter transferred by ion beam assistance,” Thin Solid Films 354, 19–23 (1999).
[Crossref]

Other (4)

J. J. McNally, G. A. Al-Jumaily, S. R. Wilson, J. R. McNeil, “Ion beam assisted deposition of optical thin films—recent results,” in Southwest Conference on Optics, ’85, S. C. Stotlar, ed., Proc. SPIE540, 479–485 (1985).

D. Morton, Denton Vacuum, Moorestown, N.J. (personal communication, 2000).

R. Götzelmann, H. Hagedorn, A. Zöller, “UV coatings produced with plasma-ion-assisted deposition,” in Advances in Optical Interference Coatings, C. Amra, H. A. Macleod, eds., Proc. SPIE3738, 48–57 (1999).

J. F. Anzellotti, D. J. Smith, R. J. Sczupak, Z. R. Chrzan, “Stress and environmental shift characteristics of HfO2/SiO2 multilayer coatings,” in Laser-Induced Damage in Optical Materials: 1996, H. E. Bennett, A. H. Guenther, M. R. Kozlowski, B. E. Newnam, M. J. Soileau, eds., Proc. SPIE2966, 258–264 (1997).

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Figures (7)

Fig. 1
Fig. 1

Configuration of the experimental setup.

Fig. 2
Fig. 2

Transmission of hafnia films deposited with and without ion assist compared with a bare substrate. Ion assist parameters correspond to run 3 in Table 1. IAD, ion-assisted deposition.

Fig. 3
Fig. 3

Transmission of fused-silica substrates after 15-min exposure to the ion gun with various bottom liner materials. In each case, chamber pressure was 3–3.5 × 10-4 Torr, ion gun current was 0.85 A (gun voltage was 150 V), and a 1:5 O2:Ar source gas ratio was used.

Fig. 4
Fig. 4

Prediction plots derived by JMP software showing the effect of each of the five factors on the moisture shift and UV transmission. The desirability was maximized, and the dotted lines show the optimal settings for minimum moisture shift and maximum UV transmission.

Fig. 5
Fig. 5

Refractive index n of ion-assisted and non-ion-assisted hafnia films deposited at 130°C as a function of wavelength. Ion-assisted film was deposited with optimal parameters. IAD, ion-assisted deposition.

Fig. 6
Fig. 6

X-ray diffraction patterns of hafnia films. (a) Non-ion-assisted film deposited at 130°C. (b) Ion-assisted film deposited at 130°C with optimal parameters.

Fig. 7
Fig. 7

High-phase-thickness hafnia silica edge filter stack deposited under optimal hafnia ion assist conditions. The filter exhibits no measurable moisture shift.

Tables (2)

Tables Icon

Table 1 List of Experimental Run Settings with Measured Resultsa

Tables Icon

Table 2 Moisture Shift and UV Transmission of Hafnia Films Produced under Different Process Conditions

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