Abstract

Annealing of micro-structured lithium niobate substrates at temperatures close to, but below the melting point, allows surface tension to reshape preferentially melted surface zones of the crystal. The reshaped surface re-crystallizes upon cooling to form a single crystal again as it is seeded by the bulk which remains solid throughout the process. This procedure yields ultra-smooth single crystal superstructures suitable for the fabrication of photonic micro-components with low scattering loss.

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  1. D. K. Armani, T. J. Kippenberg, S. M. Spillane, and K. J. Vahala, “Ultra-high-Q toroid microcavity on a chip,” Nature 421(6926), 925–928 (2003).
    [CrossRef] [PubMed]
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    [CrossRef] [PubMed]
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  5. I. E. Barry, G. W. Ross, P. G. R. Smith, R. W. Eason, and G. Cook, “Microstructuring of lithium niobate using differential etch-rate between inverted and non-inverted ferroelectric domains,” Mater. Lett. 37(4-5), 246–254 (1998).
    [CrossRef]
  6. C. L. Sones, A. C. Muir, Y. J. Ying, S. Mailis, R. W. Eason, T. Jungk, Á. Hoffmann, and E. Soergel, “Precision nanoscale domain engineering of lithium niobate via UV laser induced inhibition of poling,” Appl. Phys. Lett. 92(7), 072905 (2008).
    [CrossRef]
  7. H. Åhlfeldt, “Single-domain layers formed in heat-treated LiTaO3,” Appl. Phys. Lett. 64(24), 3213–3215 (1994).
    [CrossRef]
  8. C. L. Sones, S. Mailis, W. S. Brocklesby, R. W. Eason, and J. R. Owen, “Differential etch rates in z-cut LiNbO3 for variable HF/HNO3 concentrations,” J. Mater. Chem. 12(2), 295–298 (2002).
    [CrossRef]
  9. T. J. Sono, J. G. Scott, C. L. Sones, C. E. Valdivia, S. Mailis, R. W. Eason, J. G. Frey, and L. Danos, “Reflection second harmonic generation on a z -cut congruent lithium niobate crystal,” Phys. Rev. B 74(20), 205424 (2006).
    [CrossRef]
  10. T. Jungk, A. Hoffmann, and E. Soergel, “Quantitative analysis of ferroelectric domain imaging with piezoresponse force microscopy,” Appl. Phys. Lett. 89(16), 163507 (2006).
    [CrossRef]
  11. F. Johann and E. Soergel, “Quantitative measurement of the surface charge density,” Appl. Phys. Lett. 95(23), 232906 (2009).
    [CrossRef]
  12. A. Ridah, P. Bourson, M. D. Fontana, and G. Malovichko, “The composition dependence of the Raman spectrum and new assignment of the phonons in LiNbO3,” J. Phys. Condens. Matter 9(44), 9687–9693 (1997).
    [CrossRef]

2009

F. Johann and E. Soergel, “Quantitative measurement of the surface charge density,” Appl. Phys. Lett. 95(23), 232906 (2009).
[CrossRef]

2008

C. L. Sones, A. C. Muir, Y. J. Ying, S. Mailis, R. W. Eason, T. Jungk, Á. Hoffmann, and E. Soergel, “Precision nanoscale domain engineering of lithium niobate via UV laser induced inhibition of poling,” Appl. Phys. Lett. 92(7), 072905 (2008).
[CrossRef]

2006

T. J. Sono, J. G. Scott, C. L. Sones, C. E. Valdivia, S. Mailis, R. W. Eason, J. G. Frey, and L. Danos, “Reflection second harmonic generation on a z -cut congruent lithium niobate crystal,” Phys. Rev. B 74(20), 205424 (2006).
[CrossRef]

T. Jungk, A. Hoffmann, and E. Soergel, “Quantitative analysis of ferroelectric domain imaging with piezoresponse force microscopy,” Appl. Phys. Lett. 89(16), 163507 (2006).
[CrossRef]

2003

D. K. Armani, T. J. Kippenberg, S. M. Spillane, and K. J. Vahala, “Ultra-high-Q toroid microcavity on a chip,” Nature 421(6926), 925–928 (2003).
[CrossRef] [PubMed]

2002

C. L. Sones, S. Mailis, W. S. Brocklesby, R. W. Eason, and J. R. Owen, “Differential etch rates in z-cut LiNbO3 for variable HF/HNO3 concentrations,” J. Mater. Chem. 12(2), 295–298 (2002).
[CrossRef]

1998

I. E. Barry, G. W. Ross, P. G. R. Smith, R. W. Eason, and G. Cook, “Microstructuring of lithium niobate using differential etch-rate between inverted and non-inverted ferroelectric domains,” Mater. Lett. 37(4-5), 246–254 (1998).
[CrossRef]

1997

A. Ridah, P. Bourson, M. D. Fontana, and G. Malovichko, “The composition dependence of the Raman spectrum and new assignment of the phonons in LiNbO3,” J. Phys. Condens. Matter 9(44), 9687–9693 (1997).
[CrossRef]

1996

1994

H. Åhlfeldt, “Single-domain layers formed in heat-treated LiTaO3,” Appl. Phys. Lett. 64(24), 3213–3215 (1994).
[CrossRef]

Åhlfeldt, H.

H. Åhlfeldt, “Single-domain layers formed in heat-treated LiTaO3,” Appl. Phys. Lett. 64(24), 3213–3215 (1994).
[CrossRef]

Armani, D. K.

D. K. Armani, T. J. Kippenberg, S. M. Spillane, and K. J. Vahala, “Ultra-high-Q toroid microcavity on a chip,” Nature 421(6926), 925–928 (2003).
[CrossRef] [PubMed]

Barry, I. E.

I. E. Barry, G. W. Ross, P. G. R. Smith, R. W. Eason, and G. Cook, “Microstructuring of lithium niobate using differential etch-rate between inverted and non-inverted ferroelectric domains,” Mater. Lett. 37(4-5), 246–254 (1998).
[CrossRef]

Bourson, P.

A. Ridah, P. Bourson, M. D. Fontana, and G. Malovichko, “The composition dependence of the Raman spectrum and new assignment of the phonons in LiNbO3,” J. Phys. Condens. Matter 9(44), 9687–9693 (1997).
[CrossRef]

Brocklesby, W. S.

C. L. Sones, S. Mailis, W. S. Brocklesby, R. W. Eason, and J. R. Owen, “Differential etch rates in z-cut LiNbO3 for variable HF/HNO3 concentrations,” J. Mater. Chem. 12(2), 295–298 (2002).
[CrossRef]

Cook, G.

I. E. Barry, G. W. Ross, P. G. R. Smith, R. W. Eason, and G. Cook, “Microstructuring of lithium niobate using differential etch-rate between inverted and non-inverted ferroelectric domains,” Mater. Lett. 37(4-5), 246–254 (1998).
[CrossRef]

Danos, L.

T. J. Sono, J. G. Scott, C. L. Sones, C. E. Valdivia, S. Mailis, R. W. Eason, J. G. Frey, and L. Danos, “Reflection second harmonic generation on a z -cut congruent lithium niobate crystal,” Phys. Rev. B 74(20), 205424 (2006).
[CrossRef]

Eason, R. W.

C. L. Sones, A. C. Muir, Y. J. Ying, S. Mailis, R. W. Eason, T. Jungk, Á. Hoffmann, and E. Soergel, “Precision nanoscale domain engineering of lithium niobate via UV laser induced inhibition of poling,” Appl. Phys. Lett. 92(7), 072905 (2008).
[CrossRef]

T. J. Sono, J. G. Scott, C. L. Sones, C. E. Valdivia, S. Mailis, R. W. Eason, J. G. Frey, and L. Danos, “Reflection second harmonic generation on a z -cut congruent lithium niobate crystal,” Phys. Rev. B 74(20), 205424 (2006).
[CrossRef]

C. L. Sones, S. Mailis, W. S. Brocklesby, R. W. Eason, and J. R. Owen, “Differential etch rates in z-cut LiNbO3 for variable HF/HNO3 concentrations,” J. Mater. Chem. 12(2), 295–298 (2002).
[CrossRef]

I. E. Barry, G. W. Ross, P. G. R. Smith, R. W. Eason, and G. Cook, “Microstructuring of lithium niobate using differential etch-rate between inverted and non-inverted ferroelectric domains,” Mater. Lett. 37(4-5), 246–254 (1998).
[CrossRef]

Fontana, M. D.

A. Ridah, P. Bourson, M. D. Fontana, and G. Malovichko, “The composition dependence of the Raman spectrum and new assignment of the phonons in LiNbO3,” J. Phys. Condens. Matter 9(44), 9687–9693 (1997).
[CrossRef]

Frey, J. G.

T. J. Sono, J. G. Scott, C. L. Sones, C. E. Valdivia, S. Mailis, R. W. Eason, J. G. Frey, and L. Danos, “Reflection second harmonic generation on a z -cut congruent lithium niobate crystal,” Phys. Rev. B 74(20), 205424 (2006).
[CrossRef]

Gorodetsky, M. L.

Hoffmann, A.

T. Jungk, A. Hoffmann, and E. Soergel, “Quantitative analysis of ferroelectric domain imaging with piezoresponse force microscopy,” Appl. Phys. Lett. 89(16), 163507 (2006).
[CrossRef]

Hoffmann, Á.

C. L. Sones, A. C. Muir, Y. J. Ying, S. Mailis, R. W. Eason, T. Jungk, Á. Hoffmann, and E. Soergel, “Precision nanoscale domain engineering of lithium niobate via UV laser induced inhibition of poling,” Appl. Phys. Lett. 92(7), 072905 (2008).
[CrossRef]

Ilchenko, V. S.

Johann, F.

F. Johann and E. Soergel, “Quantitative measurement of the surface charge density,” Appl. Phys. Lett. 95(23), 232906 (2009).
[CrossRef]

Jungk, T.

C. L. Sones, A. C. Muir, Y. J. Ying, S. Mailis, R. W. Eason, T. Jungk, Á. Hoffmann, and E. Soergel, “Precision nanoscale domain engineering of lithium niobate via UV laser induced inhibition of poling,” Appl. Phys. Lett. 92(7), 072905 (2008).
[CrossRef]

T. Jungk, A. Hoffmann, and E. Soergel, “Quantitative analysis of ferroelectric domain imaging with piezoresponse force microscopy,” Appl. Phys. Lett. 89(16), 163507 (2006).
[CrossRef]

Kippenberg, T. J.

D. K. Armani, T. J. Kippenberg, S. M. Spillane, and K. J. Vahala, “Ultra-high-Q toroid microcavity on a chip,” Nature 421(6926), 925–928 (2003).
[CrossRef] [PubMed]

Mailis, S.

C. L. Sones, A. C. Muir, Y. J. Ying, S. Mailis, R. W. Eason, T. Jungk, Á. Hoffmann, and E. Soergel, “Precision nanoscale domain engineering of lithium niobate via UV laser induced inhibition of poling,” Appl. Phys. Lett. 92(7), 072905 (2008).
[CrossRef]

T. J. Sono, J. G. Scott, C. L. Sones, C. E. Valdivia, S. Mailis, R. W. Eason, J. G. Frey, and L. Danos, “Reflection second harmonic generation on a z -cut congruent lithium niobate crystal,” Phys. Rev. B 74(20), 205424 (2006).
[CrossRef]

C. L. Sones, S. Mailis, W. S. Brocklesby, R. W. Eason, and J. R. Owen, “Differential etch rates in z-cut LiNbO3 for variable HF/HNO3 concentrations,” J. Mater. Chem. 12(2), 295–298 (2002).
[CrossRef]

Malovichko, G.

A. Ridah, P. Bourson, M. D. Fontana, and G. Malovichko, “The composition dependence of the Raman spectrum and new assignment of the phonons in LiNbO3,” J. Phys. Condens. Matter 9(44), 9687–9693 (1997).
[CrossRef]

Muir, A. C.

C. L. Sones, A. C. Muir, Y. J. Ying, S. Mailis, R. W. Eason, T. Jungk, Á. Hoffmann, and E. Soergel, “Precision nanoscale domain engineering of lithium niobate via UV laser induced inhibition of poling,” Appl. Phys. Lett. 92(7), 072905 (2008).
[CrossRef]

Owen, J. R.

C. L. Sones, S. Mailis, W. S. Brocklesby, R. W. Eason, and J. R. Owen, “Differential etch rates in z-cut LiNbO3 for variable HF/HNO3 concentrations,” J. Mater. Chem. 12(2), 295–298 (2002).
[CrossRef]

Ridah, A.

A. Ridah, P. Bourson, M. D. Fontana, and G. Malovichko, “The composition dependence of the Raman spectrum and new assignment of the phonons in LiNbO3,” J. Phys. Condens. Matter 9(44), 9687–9693 (1997).
[CrossRef]

Ross, G. W.

I. E. Barry, G. W. Ross, P. G. R. Smith, R. W. Eason, and G. Cook, “Microstructuring of lithium niobate using differential etch-rate between inverted and non-inverted ferroelectric domains,” Mater. Lett. 37(4-5), 246–254 (1998).
[CrossRef]

Savchenkov, A. A.

Scott, J. G.

T. J. Sono, J. G. Scott, C. L. Sones, C. E. Valdivia, S. Mailis, R. W. Eason, J. G. Frey, and L. Danos, “Reflection second harmonic generation on a z -cut congruent lithium niobate crystal,” Phys. Rev. B 74(20), 205424 (2006).
[CrossRef]

Smith, P. G. R.

I. E. Barry, G. W. Ross, P. G. R. Smith, R. W. Eason, and G. Cook, “Microstructuring of lithium niobate using differential etch-rate between inverted and non-inverted ferroelectric domains,” Mater. Lett. 37(4-5), 246–254 (1998).
[CrossRef]

Soergel, E.

F. Johann and E. Soergel, “Quantitative measurement of the surface charge density,” Appl. Phys. Lett. 95(23), 232906 (2009).
[CrossRef]

C. L. Sones, A. C. Muir, Y. J. Ying, S. Mailis, R. W. Eason, T. Jungk, Á. Hoffmann, and E. Soergel, “Precision nanoscale domain engineering of lithium niobate via UV laser induced inhibition of poling,” Appl. Phys. Lett. 92(7), 072905 (2008).
[CrossRef]

T. Jungk, A. Hoffmann, and E. Soergel, “Quantitative analysis of ferroelectric domain imaging with piezoresponse force microscopy,” Appl. Phys. Lett. 89(16), 163507 (2006).
[CrossRef]

Sones, C. L.

C. L. Sones, A. C. Muir, Y. J. Ying, S. Mailis, R. W. Eason, T. Jungk, Á. Hoffmann, and E. Soergel, “Precision nanoscale domain engineering of lithium niobate via UV laser induced inhibition of poling,” Appl. Phys. Lett. 92(7), 072905 (2008).
[CrossRef]

T. J. Sono, J. G. Scott, C. L. Sones, C. E. Valdivia, S. Mailis, R. W. Eason, J. G. Frey, and L. Danos, “Reflection second harmonic generation on a z -cut congruent lithium niobate crystal,” Phys. Rev. B 74(20), 205424 (2006).
[CrossRef]

C. L. Sones, S. Mailis, W. S. Brocklesby, R. W. Eason, and J. R. Owen, “Differential etch rates in z-cut LiNbO3 for variable HF/HNO3 concentrations,” J. Mater. Chem. 12(2), 295–298 (2002).
[CrossRef]

Sono, T. J.

T. J. Sono, J. G. Scott, C. L. Sones, C. E. Valdivia, S. Mailis, R. W. Eason, J. G. Frey, and L. Danos, “Reflection second harmonic generation on a z -cut congruent lithium niobate crystal,” Phys. Rev. B 74(20), 205424 (2006).
[CrossRef]

Spillane, S. M.

D. K. Armani, T. J. Kippenberg, S. M. Spillane, and K. J. Vahala, “Ultra-high-Q toroid microcavity on a chip,” Nature 421(6926), 925–928 (2003).
[CrossRef] [PubMed]

Vahala, K. J.

D. K. Armani, T. J. Kippenberg, S. M. Spillane, and K. J. Vahala, “Ultra-high-Q toroid microcavity on a chip,” Nature 421(6926), 925–928 (2003).
[CrossRef] [PubMed]

Valdivia, C. E.

T. J. Sono, J. G. Scott, C. L. Sones, C. E. Valdivia, S. Mailis, R. W. Eason, J. G. Frey, and L. Danos, “Reflection second harmonic generation on a z -cut congruent lithium niobate crystal,” Phys. Rev. B 74(20), 205424 (2006).
[CrossRef]

Ying, Y. J.

C. L. Sones, A. C. Muir, Y. J. Ying, S. Mailis, R. W. Eason, T. Jungk, Á. Hoffmann, and E. Soergel, “Precision nanoscale domain engineering of lithium niobate via UV laser induced inhibition of poling,” Appl. Phys. Lett. 92(7), 072905 (2008).
[CrossRef]

Appl. Phys. Lett.

C. L. Sones, A. C. Muir, Y. J. Ying, S. Mailis, R. W. Eason, T. Jungk, Á. Hoffmann, and E. Soergel, “Precision nanoscale domain engineering of lithium niobate via UV laser induced inhibition of poling,” Appl. Phys. Lett. 92(7), 072905 (2008).
[CrossRef]

H. Åhlfeldt, “Single-domain layers formed in heat-treated LiTaO3,” Appl. Phys. Lett. 64(24), 3213–3215 (1994).
[CrossRef]

T. Jungk, A. Hoffmann, and E. Soergel, “Quantitative analysis of ferroelectric domain imaging with piezoresponse force microscopy,” Appl. Phys. Lett. 89(16), 163507 (2006).
[CrossRef]

F. Johann and E. Soergel, “Quantitative measurement of the surface charge density,” Appl. Phys. Lett. 95(23), 232906 (2009).
[CrossRef]

J. Mater. Chem.

C. L. Sones, S. Mailis, W. S. Brocklesby, R. W. Eason, and J. R. Owen, “Differential etch rates in z-cut LiNbO3 for variable HF/HNO3 concentrations,” J. Mater. Chem. 12(2), 295–298 (2002).
[CrossRef]

J. Phys. Condens. Matter

A. Ridah, P. Bourson, M. D. Fontana, and G. Malovichko, “The composition dependence of the Raman spectrum and new assignment of the phonons in LiNbO3,” J. Phys. Condens. Matter 9(44), 9687–9693 (1997).
[CrossRef]

Mater. Lett.

I. E. Barry, G. W. Ross, P. G. R. Smith, R. W. Eason, and G. Cook, “Microstructuring of lithium niobate using differential etch-rate between inverted and non-inverted ferroelectric domains,” Mater. Lett. 37(4-5), 246–254 (1998).
[CrossRef]

Nature

D. K. Armani, T. J. Kippenberg, S. M. Spillane, and K. J. Vahala, “Ultra-high-Q toroid microcavity on a chip,” Nature 421(6926), 925–928 (2003).
[CrossRef] [PubMed]

Opt. Lett.

Phys. Rev. B

T. J. Sono, J. G. Scott, C. L. Sones, C. E. Valdivia, S. Mailis, R. W. Eason, J. G. Frey, and L. Danos, “Reflection second harmonic generation on a z -cut congruent lithium niobate crystal,” Phys. Rev. B 74(20), 205424 (2006).
[CrossRef]

Other

V. S. Ilchenko, X. S. Yao, and L. Maleki, “Microsphere integration in active and passive photonics devices,” in Proc. SPIE 3930, 154–162 (2000).

R. Lipowsky, “Surface-induced disorder and surface melting,” in Springer Proc. in Physics, (Springer, 1990), 158–166.

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Figures (5)

Fig. 1
Fig. 1

SEM images of the micro-structured lithium niobate crystal surface (45° tilted) a) after deep etching of a 2D lattice of inverted ferroelectric domains and b) after thermal treatment.

Fig. 2
Fig. 2

SEM images of a) the initial structure, comprising an undercut, produced by inhibition of poling followed by deep chemical etching using HF acid, b) corresponding annealed structure showing a quasi-oblate spheroid top. In both images the sample is tilted by 45°.

Fig. 3
Fig. 3

Etching of the y-face of a z-cut crystal slab annealed at T = 1200°C (above the Curie temperature) for 10 hrs revealing the ferroelectric domain structure.

Fig. 4
Fig. 4

Raman spectra acquired from different points on the annealed microstructured sample shown in Fig. 1b and with different focusing conditions as indicated in the legend. The solid line corresponds to a spectrum that was taken from a virgin z-cut sample in the z(yy)z configuration. An offset was introduced between spectra for clarity.

Fig. 5
Fig. 5

a) SEM image of a surface tension reshaped feature, b) SEM image of a feature briefly etched in HF showing characteristic y-face differential etching as indicated by the arrows.

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