Abstract

Surface crystallization was induced in Ge-doped silica glass samples from a graded-index optical fiber preform by re-heating them at 1100°C for several hours. X-ray diffraction and second-harmonic generation (SHG) microscopy have been utilized to investigate the crystalline phases formed. Experimental results indicate that the predominant crystalline phase is α-cristobalite. The cross-sectional distribution of the crystal particles has also been measured with the SHG microscopy and the result is in good agreement with that from traditional bright field light microscopy.

©2004 Optical Society of America

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References

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  1. P. M. McMillan, Glass-ceramics (Academic, 1964), Chap. 4.
  2. A. Narazaki, K. Tanaka, and K. Hirao, “Optical second-order nonlinearity of transparent glass-ceramics containing BaTiO3 precipitated via surface crystallization,” J. Mater. Res. 14, 3640–3646 (1999).
    [Crossref]
  3. Y. Takahashi, Y. Benino, T. Fujiwara, and T. Komatsu, “Second harmonic generation in transparent surface crystallized glasses with stillwellite-type LaBGeO5,” J. Appl. Phys. 89, 5282–5287 (2001).
    [Crossref]
  4. T. Fujiwara, H. Nagata, Y. Benino, and T. Komatsu, “Crystallization behaviors with pre-treatments of thermal annealing and ultraviolet laser irradiation in Ge-doped SiO2 glass fiber preforms,” J. Ceram. Soc. Jpn. 111, 8–10 (2003).
    [Crossref]
  5. T. Fujiwara, T. Sawada, Y. Benino, T. Komatsu, M. Takahashi, T. Yoko, and J. Nishii, “Direct observation of second-harmonic generation from crystalline particles in Ge-doped SiO2 glass films,” Opt. Express 11, 1598 (2003), http://www.opticsexpress.org/abstract.cfm?URI=OPEX-11-14-1598.
    [Crossref] [PubMed]
  6. Y. Uesu, S. Kurimura, and Y. Yamamoto, “Optical second harmonic images of 90° domain structure in BaTiO3 and periodically inverted antiparallel domains in LiTaO3,” Appl. Phys. Lett. 66, 2165–2167 (1995).
    [Crossref]
  7. D. M. Hatch and S. Ghose, “The alpha-beta phase-transition in cristobalite, SiO2-symmetry analysis, domain-structure, and the dynamic nature of the beta-phase,” Phys. Chem. Miner. 17, 554–562 (1991).
    [Crossref]
  8. C. H. Chao and H. Y. Lu, “Stress-induced β→α-cristobalite phase transformation in (Na2O+Al2O3)-codoped silica,” Mater. Sci. Eng. A328, 267–276 (2002).
  9. C. Cabrillo, F.J. Bermejo, J.M. Gibson, J.A. Johnson, D. Faccio, V. Pruneri, and P.G. Kazansky, “Thermally poled silica samples are structurally heterogeneous: Electron diffraction evidence of partial crystallization,” Appl. Phys. Lett. 78, 1991–1993 (2001).
    [Crossref]

2003 (2)

T. Fujiwara, H. Nagata, Y. Benino, and T. Komatsu, “Crystallization behaviors with pre-treatments of thermal annealing and ultraviolet laser irradiation in Ge-doped SiO2 glass fiber preforms,” J. Ceram. Soc. Jpn. 111, 8–10 (2003).
[Crossref]

T. Fujiwara, T. Sawada, Y. Benino, T. Komatsu, M. Takahashi, T. Yoko, and J. Nishii, “Direct observation of second-harmonic generation from crystalline particles in Ge-doped SiO2 glass films,” Opt. Express 11, 1598 (2003), http://www.opticsexpress.org/abstract.cfm?URI=OPEX-11-14-1598.
[Crossref] [PubMed]

2002 (1)

C. H. Chao and H. Y. Lu, “Stress-induced β→α-cristobalite phase transformation in (Na2O+Al2O3)-codoped silica,” Mater. Sci. Eng. A328, 267–276 (2002).

2001 (2)

C. Cabrillo, F.J. Bermejo, J.M. Gibson, J.A. Johnson, D. Faccio, V. Pruneri, and P.G. Kazansky, “Thermally poled silica samples are structurally heterogeneous: Electron diffraction evidence of partial crystallization,” Appl. Phys. Lett. 78, 1991–1993 (2001).
[Crossref]

Y. Takahashi, Y. Benino, T. Fujiwara, and T. Komatsu, “Second harmonic generation in transparent surface crystallized glasses with stillwellite-type LaBGeO5,” J. Appl. Phys. 89, 5282–5287 (2001).
[Crossref]

1999 (1)

A. Narazaki, K. Tanaka, and K. Hirao, “Optical second-order nonlinearity of transparent glass-ceramics containing BaTiO3 precipitated via surface crystallization,” J. Mater. Res. 14, 3640–3646 (1999).
[Crossref]

1995 (1)

Y. Uesu, S. Kurimura, and Y. Yamamoto, “Optical second harmonic images of 90° domain structure in BaTiO3 and periodically inverted antiparallel domains in LiTaO3,” Appl. Phys. Lett. 66, 2165–2167 (1995).
[Crossref]

1991 (1)

D. M. Hatch and S. Ghose, “The alpha-beta phase-transition in cristobalite, SiO2-symmetry analysis, domain-structure, and the dynamic nature of the beta-phase,” Phys. Chem. Miner. 17, 554–562 (1991).
[Crossref]

Benino, Y.

T. Fujiwara, H. Nagata, Y. Benino, and T. Komatsu, “Crystallization behaviors with pre-treatments of thermal annealing and ultraviolet laser irradiation in Ge-doped SiO2 glass fiber preforms,” J. Ceram. Soc. Jpn. 111, 8–10 (2003).
[Crossref]

T. Fujiwara, T. Sawada, Y. Benino, T. Komatsu, M. Takahashi, T. Yoko, and J. Nishii, “Direct observation of second-harmonic generation from crystalline particles in Ge-doped SiO2 glass films,” Opt. Express 11, 1598 (2003), http://www.opticsexpress.org/abstract.cfm?URI=OPEX-11-14-1598.
[Crossref] [PubMed]

Y. Takahashi, Y. Benino, T. Fujiwara, and T. Komatsu, “Second harmonic generation in transparent surface crystallized glasses with stillwellite-type LaBGeO5,” J. Appl. Phys. 89, 5282–5287 (2001).
[Crossref]

Bermejo, F.J.

C. Cabrillo, F.J. Bermejo, J.M. Gibson, J.A. Johnson, D. Faccio, V. Pruneri, and P.G. Kazansky, “Thermally poled silica samples are structurally heterogeneous: Electron diffraction evidence of partial crystallization,” Appl. Phys. Lett. 78, 1991–1993 (2001).
[Crossref]

Cabrillo, C.

C. Cabrillo, F.J. Bermejo, J.M. Gibson, J.A. Johnson, D. Faccio, V. Pruneri, and P.G. Kazansky, “Thermally poled silica samples are structurally heterogeneous: Electron diffraction evidence of partial crystallization,” Appl. Phys. Lett. 78, 1991–1993 (2001).
[Crossref]

Chao, C. H.

C. H. Chao and H. Y. Lu, “Stress-induced β→α-cristobalite phase transformation in (Na2O+Al2O3)-codoped silica,” Mater. Sci. Eng. A328, 267–276 (2002).

Faccio, D.

C. Cabrillo, F.J. Bermejo, J.M. Gibson, J.A. Johnson, D. Faccio, V. Pruneri, and P.G. Kazansky, “Thermally poled silica samples are structurally heterogeneous: Electron diffraction evidence of partial crystallization,” Appl. Phys. Lett. 78, 1991–1993 (2001).
[Crossref]

Fujiwara, T.

T. Fujiwara, T. Sawada, Y. Benino, T. Komatsu, M. Takahashi, T. Yoko, and J. Nishii, “Direct observation of second-harmonic generation from crystalline particles in Ge-doped SiO2 glass films,” Opt. Express 11, 1598 (2003), http://www.opticsexpress.org/abstract.cfm?URI=OPEX-11-14-1598.
[Crossref] [PubMed]

T. Fujiwara, H. Nagata, Y. Benino, and T. Komatsu, “Crystallization behaviors with pre-treatments of thermal annealing and ultraviolet laser irradiation in Ge-doped SiO2 glass fiber preforms,” J. Ceram. Soc. Jpn. 111, 8–10 (2003).
[Crossref]

Y. Takahashi, Y. Benino, T. Fujiwara, and T. Komatsu, “Second harmonic generation in transparent surface crystallized glasses with stillwellite-type LaBGeO5,” J. Appl. Phys. 89, 5282–5287 (2001).
[Crossref]

Ghose, S.

D. M. Hatch and S. Ghose, “The alpha-beta phase-transition in cristobalite, SiO2-symmetry analysis, domain-structure, and the dynamic nature of the beta-phase,” Phys. Chem. Miner. 17, 554–562 (1991).
[Crossref]

Gibson, J.M.

C. Cabrillo, F.J. Bermejo, J.M. Gibson, J.A. Johnson, D. Faccio, V. Pruneri, and P.G. Kazansky, “Thermally poled silica samples are structurally heterogeneous: Electron diffraction evidence of partial crystallization,” Appl. Phys. Lett. 78, 1991–1993 (2001).
[Crossref]

Hatch, D. M.

D. M. Hatch and S. Ghose, “The alpha-beta phase-transition in cristobalite, SiO2-symmetry analysis, domain-structure, and the dynamic nature of the beta-phase,” Phys. Chem. Miner. 17, 554–562 (1991).
[Crossref]

Hirao, K.

A. Narazaki, K. Tanaka, and K. Hirao, “Optical second-order nonlinearity of transparent glass-ceramics containing BaTiO3 precipitated via surface crystallization,” J. Mater. Res. 14, 3640–3646 (1999).
[Crossref]

Johnson, J.A.

C. Cabrillo, F.J. Bermejo, J.M. Gibson, J.A. Johnson, D. Faccio, V. Pruneri, and P.G. Kazansky, “Thermally poled silica samples are structurally heterogeneous: Electron diffraction evidence of partial crystallization,” Appl. Phys. Lett. 78, 1991–1993 (2001).
[Crossref]

Kazansky, P.G.

C. Cabrillo, F.J. Bermejo, J.M. Gibson, J.A. Johnson, D. Faccio, V. Pruneri, and P.G. Kazansky, “Thermally poled silica samples are structurally heterogeneous: Electron diffraction evidence of partial crystallization,” Appl. Phys. Lett. 78, 1991–1993 (2001).
[Crossref]

Komatsu, T.

T. Fujiwara, T. Sawada, Y. Benino, T. Komatsu, M. Takahashi, T. Yoko, and J. Nishii, “Direct observation of second-harmonic generation from crystalline particles in Ge-doped SiO2 glass films,” Opt. Express 11, 1598 (2003), http://www.opticsexpress.org/abstract.cfm?URI=OPEX-11-14-1598.
[Crossref] [PubMed]

T. Fujiwara, H. Nagata, Y. Benino, and T. Komatsu, “Crystallization behaviors with pre-treatments of thermal annealing and ultraviolet laser irradiation in Ge-doped SiO2 glass fiber preforms,” J. Ceram. Soc. Jpn. 111, 8–10 (2003).
[Crossref]

Y. Takahashi, Y. Benino, T. Fujiwara, and T. Komatsu, “Second harmonic generation in transparent surface crystallized glasses with stillwellite-type LaBGeO5,” J. Appl. Phys. 89, 5282–5287 (2001).
[Crossref]

Kurimura, S.

Y. Uesu, S. Kurimura, and Y. Yamamoto, “Optical second harmonic images of 90° domain structure in BaTiO3 and periodically inverted antiparallel domains in LiTaO3,” Appl. Phys. Lett. 66, 2165–2167 (1995).
[Crossref]

Lu, H. Y.

C. H. Chao and H. Y. Lu, “Stress-induced β→α-cristobalite phase transformation in (Na2O+Al2O3)-codoped silica,” Mater. Sci. Eng. A328, 267–276 (2002).

McMillan, P. M.

P. M. McMillan, Glass-ceramics (Academic, 1964), Chap. 4.

Nagata, H.

T. Fujiwara, H. Nagata, Y. Benino, and T. Komatsu, “Crystallization behaviors with pre-treatments of thermal annealing and ultraviolet laser irradiation in Ge-doped SiO2 glass fiber preforms,” J. Ceram. Soc. Jpn. 111, 8–10 (2003).
[Crossref]

Narazaki, A.

A. Narazaki, K. Tanaka, and K. Hirao, “Optical second-order nonlinearity of transparent glass-ceramics containing BaTiO3 precipitated via surface crystallization,” J. Mater. Res. 14, 3640–3646 (1999).
[Crossref]

Nishii, J.

Pruneri, V.

C. Cabrillo, F.J. Bermejo, J.M. Gibson, J.A. Johnson, D. Faccio, V. Pruneri, and P.G. Kazansky, “Thermally poled silica samples are structurally heterogeneous: Electron diffraction evidence of partial crystallization,” Appl. Phys. Lett. 78, 1991–1993 (2001).
[Crossref]

Sawada, T.

Takahashi, M.

Takahashi, Y.

Y. Takahashi, Y. Benino, T. Fujiwara, and T. Komatsu, “Second harmonic generation in transparent surface crystallized glasses with stillwellite-type LaBGeO5,” J. Appl. Phys. 89, 5282–5287 (2001).
[Crossref]

Tanaka, K.

A. Narazaki, K. Tanaka, and K. Hirao, “Optical second-order nonlinearity of transparent glass-ceramics containing BaTiO3 precipitated via surface crystallization,” J. Mater. Res. 14, 3640–3646 (1999).
[Crossref]

Uesu, Y.

Y. Uesu, S. Kurimura, and Y. Yamamoto, “Optical second harmonic images of 90° domain structure in BaTiO3 and periodically inverted antiparallel domains in LiTaO3,” Appl. Phys. Lett. 66, 2165–2167 (1995).
[Crossref]

Yamamoto, Y.

Y. Uesu, S. Kurimura, and Y. Yamamoto, “Optical second harmonic images of 90° domain structure in BaTiO3 and periodically inverted antiparallel domains in LiTaO3,” Appl. Phys. Lett. 66, 2165–2167 (1995).
[Crossref]

Yoko, T.

Appl. Phys. Lett. (2)

Y. Uesu, S. Kurimura, and Y. Yamamoto, “Optical second harmonic images of 90° domain structure in BaTiO3 and periodically inverted antiparallel domains in LiTaO3,” Appl. Phys. Lett. 66, 2165–2167 (1995).
[Crossref]

C. Cabrillo, F.J. Bermejo, J.M. Gibson, J.A. Johnson, D. Faccio, V. Pruneri, and P.G. Kazansky, “Thermally poled silica samples are structurally heterogeneous: Electron diffraction evidence of partial crystallization,” Appl. Phys. Lett. 78, 1991–1993 (2001).
[Crossref]

J. Appl. Phys. (1)

Y. Takahashi, Y. Benino, T. Fujiwara, and T. Komatsu, “Second harmonic generation in transparent surface crystallized glasses with stillwellite-type LaBGeO5,” J. Appl. Phys. 89, 5282–5287 (2001).
[Crossref]

J. Ceram. Soc. Jpn. (1)

T. Fujiwara, H. Nagata, Y. Benino, and T. Komatsu, “Crystallization behaviors with pre-treatments of thermal annealing and ultraviolet laser irradiation in Ge-doped SiO2 glass fiber preforms,” J. Ceram. Soc. Jpn. 111, 8–10 (2003).
[Crossref]

J. Mater. Res. (1)

A. Narazaki, K. Tanaka, and K. Hirao, “Optical second-order nonlinearity of transparent glass-ceramics containing BaTiO3 precipitated via surface crystallization,” J. Mater. Res. 14, 3640–3646 (1999).
[Crossref]

Mater. Sci. Eng. (1)

C. H. Chao and H. Y. Lu, “Stress-induced β→α-cristobalite phase transformation in (Na2O+Al2O3)-codoped silica,” Mater. Sci. Eng. A328, 267–276 (2002).

Opt. Express (1)

Phys. Chem. Miner. (1)

D. M. Hatch and S. Ghose, “The alpha-beta phase-transition in cristobalite, SiO2-symmetry analysis, domain-structure, and the dynamic nature of the beta-phase,” Phys. Chem. Miner. 17, 554–562 (1991).
[Crossref]

Other (1)

P. M. McMillan, Glass-ceramics (Academic, 1964), Chap. 4.

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Figures (5)

Fig. 1.
Fig. 1. Refractive index profile of the VAD optical fiber preform.
Fig. 2.
Fig. 2. XRD patterns of surface-crystallized Ge-doped SiO2 glass. (a) Sample annealed at 1100°C for 3 hours; (b) Sample annealed at 1150°C for 2.5 hours.
Fig. 3.
Fig. 3. Images under optical microscopes, (a) Phase contrast, (b) SHG. Image length is 206.5µm.
Fig. 4.
Fig. 4. SHG z-series scan images. The step size is one micron.
Fig. 5.
Fig. 5. Bright-field light microscopy image of the sample cross-section.

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