Abstract

We propose to combine a few known technologies to print TiOxNy quasi-sinusoidal grating using a direct photo-patternable TiO2 sol-gel thin layer, enabling the conversion of a pure dielectric grating to a metallic one. An expanded laser beam illuminates a photosensitive TiO2 sol-gel layer through a photo-mask grating, creating illuminated and non-illuminated areas in the sol-gel layer, which act as a negative photoresist and leads to a TiO2 based grating. Nitridation is made by heat treatment under NH3 flow to convert TiO2 in TiOxNy grating. This process shows that the sol-gel technology can be extended from a dielectric to metallic layer. The derived meta-material offers an alternative for plasmonic effects in the near-infrared region. This paper describes the experimental processes from the photochemistry of the TiO2 sol-gel layer to its nitridation. Thanks to the optical properties of the obtained micrometric period TiOxNy grating, surface plasmon resonance at TiOxNy-air interface has been excited in the NIR range (around 1500 nm), demonstrating the metallic behavior of the grating and its ability to be used as a plasmonic component.

© 2016 Optical Society of America

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References

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    [Crossref]
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    [Crossref]
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2015 (1)

O. Shavdina, L. Berthod, T. Kämpfe, S. Reynaud, C. Veillas, I. Verrier, M. Langlet, F. Vocanson, P. Fugier, Y. Jourlin, and O. Dellea, “Large area fabrication of periodic TiO2 nanopillars using microsphere photolithography on a photopatternable sol-gel film,” Langmuir 31(28), 7877–7884 (2015).
[Crossref] [PubMed]

2014 (3)

2013 (2)

C. Valsecchi and A. G. Brolo, “Periodic metallic nanostructures as plasmonic chemical sensors,” Langmuir 29(19), 5638–5649 (2013).
[Crossref] [PubMed]

V. Gâté, Y. Jourlin, F. Vocanson, O. Dellea, G. Vercasson, S. Reynaud, D. Riassetto, and M. Langlet, “Sub-micrometric patterns written using a DIL method coupled to a TiO2 photo-resist,” Opt. Mater. 35(9), 1706–1713 (2013).
[Crossref]

2012 (1)

2011 (6)

N. C. Chen, W. C. Lien, C. R. Liu, Y. L. Huang, Y. R. Lin, C. Chou, S. Y. Chang, and C. W. Ho, “Excitation of surface plasma wave at TiN/air interface in the Kretschmann geometry,” J. Appl. Phys. 109(4), 043104 (2011).
[Crossref]

J. N. Munday and H. A. Atwater, “Large integrated absorption enhancement in plasmonic solar cells by combining metallic gratings and antireflection coatings,” Nano Lett. 11(6), 2195–2201 (2011).
[Crossref] [PubMed]

A. Boltasseva and H. A. Atwater, “Materials science. Low-loss plasmonic metamaterials,” Science 331(6015), 290–291 (2011).
[Crossref] [PubMed]

G. V. Naik, J. Kim, and A. Boltasseva, “Oxides and nitrides as alternative plasmonic materials in the optical range,” Opt. Mater. Express 1(6), 1090–1099 (2011).
[Crossref]

S. Briche, Z. Tebby, D. Riassetto, M. Messaoud, E. Gamet, E. Pernot, H. Roussel, O. Dellea, Y. Jourlin, and M. Langlet, “New insight in photo-patternad sol-gel-derived TiO2 films,” J. Mater. Sci. 46(5), 1474–1486 (2011).
[Crossref]

P. Romero-Gómez, V. Rico, J. P. Espinós, R. Agustín, G. Elipe, R. G. Palgrave, and R. G. Egdell, “Nitridation of nanocrystalline TiO2 thin films by treatment with ammonia,” Thin Solid Films 519(11), 3587–3595 (2011).
[Crossref]

2010 (2)

C. C. Chang, Y. D. Sharma, Y. S. Kim, J. A. Bur, R. V. Shenoi, S. Krishna, D. Huang, and S. Y. Lin, “A surface plasmon enhanced infrared photodetector based on InAs quantum dots,” Nano Lett. 10(5), 1704–1709 (2010).
[Crossref] [PubMed]

S. Assefa, F. Xia, and Y. A. Vlasov, “Reinventing germanium avalanche photodetector for nanophotonic on-chip optical interconnects,” Nature 464(7285), 80–84 (2010).
[Crossref] [PubMed]

2009 (1)

P. Berini, “Long-range surface plasmon-polaritons,” Adv. Opt. Photonics 1(3), 484–588 (2009).
[Crossref]

2007 (1)

S. Pillai, K. R. Catchpole, T. Trupke, and M. A. Green, “Surface plasmon enhanced silicon solar cells,” J. Appl. Phys. 101(9), 093105 (2007).
[Crossref]

2005 (2)

S. Tian, N. R. Armstrong, and W. Knoll, “Electrochemically tunable surface-plasmon-enhanced diffraction gratings and their (bio-)sensing applications,” Langmuir 21(10), 4656–4660 (2005).
[Crossref] [PubMed]

Y. Kuroda, T. Mori, K. Yagi, N. Makihata, Y. Kawahara, M. Nagao, and S. Kittaka, “Preparation of visible-light-responsive TiO2-xNx photocatalyst by a sol-gel method: analysis of the active center on TiO2 that reacts with NH3.,” Langmuir 21(17), 8026–8034 (2005).
[Crossref] [PubMed]

2002 (1)

Y. Djaoued, R. Taj, R. Brüning, S. Badilescu, P. V. Ashrit, G. Bader, and T. V. Van, “Study of the phase transition and the thermal nitridation of nanocrystalline sol-gel films,” J. Non-Cryst. Solids 297(1), 55–66 (2002).
[Crossref]

2001 (2)

N. Martin, O. Banakh, A. M. E. Santo, S. Springer, R. Sanjinès, J. Takadoum, and F. Lévy, “Correlation between processing and properties of TiOxNy thin films sputter deposited by the reactive gas pulsing technique,” Appl. Surf. Sci. 185(1–2), 123–133 (2001).
[Crossref]

R. Asahi, T. Morikawa, T. Ohwaki, K. Aoki, and Y. Taga, “Visible-light photocatalysis in nitrogen-doped titanium oxides,” Science 293(5528), 269–271 (2001).
[Crossref] [PubMed]

1999 (1)

L. Wicikowski, B. Kusz, L. Murawski, K. Szaniawska, and B. Susła, “AFM and XPS study of nitrided TiO2 and SiO2-TiO2 sol-gel derived films,” Vacuum 54(1–4), 221–225 (1999).
[Crossref]

1994 (1)

C. Jiménez and M. Langlet, “Formation of TiN by nitridation of TiO2 films deposited by ultrasonically assisted sol-gel technique,” Surf. Coat. Tech. 69, 249–252 (1994).
[Crossref]

1990 (1)

K. Kamiya, T. Nishijima, and K. Tanaka, “Nitridation of the sol-gel derived titanium oxide films by heating in ammonia gas,” J. Am. Ceram. Soc. 73(9), 2750–2752 (1990).
[Crossref]

1987 (1)

K. Kamiya, T. Yoko, and M. Bessho, “Nitridation of TiO2 fibres prepared by the sol-gel method,” J. Mater. Sci. 22(3), 937–941 (1987).
[Crossref]

1985 (1)

J. E. Sundgren, “Structure and properties of TiN coatings,” Thin Solid Films 128(1–2), 21–44 (1985).
[Crossref]

Agustín, R.

P. Romero-Gómez, V. Rico, J. P. Espinós, R. Agustín, G. Elipe, R. G. Palgrave, and R. G. Egdell, “Nitridation of nanocrystalline TiO2 thin films by treatment with ammonia,” Thin Solid Films 519(11), 3587–3595 (2011).
[Crossref]

Aoki, K.

R. Asahi, T. Morikawa, T. Ohwaki, K. Aoki, and Y. Taga, “Visible-light photocatalysis in nitrogen-doped titanium oxides,” Science 293(5528), 269–271 (2001).
[Crossref] [PubMed]

Armstrong, N. R.

S. Tian, N. R. Armstrong, and W. Knoll, “Electrochemically tunable surface-plasmon-enhanced diffraction gratings and their (bio-)sensing applications,” Langmuir 21(10), 4656–4660 (2005).
[Crossref] [PubMed]

Asahi, R.

R. Asahi, T. Morikawa, T. Ohwaki, K. Aoki, and Y. Taga, “Visible-light photocatalysis in nitrogen-doped titanium oxides,” Science 293(5528), 269–271 (2001).
[Crossref] [PubMed]

Ashrit, P. V.

Y. Djaoued, R. Taj, R. Brüning, S. Badilescu, P. V. Ashrit, G. Bader, and T. V. Van, “Study of the phase transition and the thermal nitridation of nanocrystalline sol-gel films,” J. Non-Cryst. Solids 297(1), 55–66 (2002).
[Crossref]

Assefa, S.

S. Assefa, F. Xia, and Y. A. Vlasov, “Reinventing germanium avalanche photodetector for nanophotonic on-chip optical interconnects,” Nature 464(7285), 80–84 (2010).
[Crossref] [PubMed]

Atwater, H. A.

J. N. Munday and H. A. Atwater, “Large integrated absorption enhancement in plasmonic solar cells by combining metallic gratings and antireflection coatings,” Nano Lett. 11(6), 2195–2201 (2011).
[Crossref] [PubMed]

A. Boltasseva and H. A. Atwater, “Materials science. Low-loss plasmonic metamaterials,” Science 331(6015), 290–291 (2011).
[Crossref] [PubMed]

Babicheva, V. E.

Bader, G.

Y. Djaoued, R. Taj, R. Brüning, S. Badilescu, P. V. Ashrit, G. Bader, and T. V. Van, “Study of the phase transition and the thermal nitridation of nanocrystalline sol-gel films,” J. Non-Cryst. Solids 297(1), 55–66 (2002).
[Crossref]

Badilescu, S.

Y. Djaoued, R. Taj, R. Brüning, S. Badilescu, P. V. Ashrit, G. Bader, and T. V. Van, “Study of the phase transition and the thermal nitridation of nanocrystalline sol-gel films,” J. Non-Cryst. Solids 297(1), 55–66 (2002).
[Crossref]

Banakh, O.

N. Martin, O. Banakh, A. M. E. Santo, S. Springer, R. Sanjinès, J. Takadoum, and F. Lévy, “Correlation between processing and properties of TiOxNy thin films sputter deposited by the reactive gas pulsing technique,” Appl. Surf. Sci. 185(1–2), 123–133 (2001).
[Crossref]

Berini, P.

P. Berini, “Long-range surface plasmon-polaritons,” Adv. Opt. Photonics 1(3), 484–588 (2009).
[Crossref]

Berthod, L.

O. Shavdina, L. Berthod, T. Kämpfe, S. Reynaud, C. Veillas, I. Verrier, M. Langlet, F. Vocanson, P. Fugier, Y. Jourlin, and O. Dellea, “Large area fabrication of periodic TiO2 nanopillars using microsphere photolithography on a photopatternable sol-gel film,” Langmuir 31(28), 7877–7884 (2015).
[Crossref] [PubMed]

Bessho, M.

K. Kamiya, T. Yoko, and M. Bessho, “Nitridation of TiO2 fibres prepared by the sol-gel method,” J. Mater. Sci. 22(3), 937–941 (1987).
[Crossref]

Boltasseva, A.

Briche, S.

S. Briche, Z. Tebby, D. Riassetto, M. Messaoud, E. Gamet, E. Pernot, H. Roussel, O. Dellea, Y. Jourlin, and M. Langlet, “New insight in photo-patternad sol-gel-derived TiO2 films,” J. Mater. Sci. 46(5), 1474–1486 (2011).
[Crossref]

Brolo, A. G.

C. Valsecchi and A. G. Brolo, “Periodic metallic nanostructures as plasmonic chemical sensors,” Langmuir 29(19), 5638–5649 (2013).
[Crossref] [PubMed]

Brüning, R.

Y. Djaoued, R. Taj, R. Brüning, S. Badilescu, P. V. Ashrit, G. Bader, and T. V. Van, “Study of the phase transition and the thermal nitridation of nanocrystalline sol-gel films,” J. Non-Cryst. Solids 297(1), 55–66 (2002).
[Crossref]

Bur, J. A.

C. C. Chang, Y. D. Sharma, Y. S. Kim, J. A. Bur, R. V. Shenoi, S. Krishna, D. Huang, and S. Y. Lin, “A surface plasmon enhanced infrared photodetector based on InAs quantum dots,” Nano Lett. 10(5), 1704–1709 (2010).
[Crossref] [PubMed]

Catchpole, K. R.

S. Pillai, K. R. Catchpole, T. Trupke, and M. A. Green, “Surface plasmon enhanced silicon solar cells,” J. Appl. Phys. 101(9), 093105 (2007).
[Crossref]

Chang, C. C.

C. C. Chang, Y. D. Sharma, Y. S. Kim, J. A. Bur, R. V. Shenoi, S. Krishna, D. Huang, and S. Y. Lin, “A surface plasmon enhanced infrared photodetector based on InAs quantum dots,” Nano Lett. 10(5), 1704–1709 (2010).
[Crossref] [PubMed]

Chang, S. Y.

N. C. Chen, W. C. Lien, C. R. Liu, Y. L. Huang, Y. R. Lin, C. Chou, S. Y. Chang, and C. W. Ho, “Excitation of surface plasma wave at TiN/air interface in the Kretschmann geometry,” J. Appl. Phys. 109(4), 043104 (2011).
[Crossref]

Chen, F.

Chen, N. C.

N. C. Chen, W. C. Lien, C. R. Liu, Y. L. Huang, Y. R. Lin, C. Chou, S. Y. Chang, and C. W. Ho, “Excitation of surface plasma wave at TiN/air interface in the Kretschmann geometry,” J. Appl. Phys. 109(4), 043104 (2011).
[Crossref]

Chen, X.

Chou, C.

N. C. Chen, W. C. Lien, C. R. Liu, Y. L. Huang, Y. R. Lin, C. Chou, S. Y. Chang, and C. W. Ho, “Excitation of surface plasma wave at TiN/air interface in the Kretschmann geometry,” J. Appl. Phys. 109(4), 043104 (2011).
[Crossref]

Dellea, O.

O. Shavdina, L. Berthod, T. Kämpfe, S. Reynaud, C. Veillas, I. Verrier, M. Langlet, F. Vocanson, P. Fugier, Y. Jourlin, and O. Dellea, “Large area fabrication of periodic TiO2 nanopillars using microsphere photolithography on a photopatternable sol-gel film,” Langmuir 31(28), 7877–7884 (2015).
[Crossref] [PubMed]

V. Gâté, Y. Jourlin, F. Vocanson, O. Dellea, G. Vercasson, S. Reynaud, D. Riassetto, and M. Langlet, “Sub-micrometric patterns written using a DIL method coupled to a TiO2 photo-resist,” Opt. Mater. 35(9), 1706–1713 (2013).
[Crossref]

S. Briche, Z. Tebby, D. Riassetto, M. Messaoud, E. Gamet, E. Pernot, H. Roussel, O. Dellea, Y. Jourlin, and M. Langlet, “New insight in photo-patternad sol-gel-derived TiO2 films,” J. Mater. Sci. 46(5), 1474–1486 (2011).
[Crossref]

Djaoued, Y.

Y. Djaoued, R. Taj, R. Brüning, S. Badilescu, P. V. Ashrit, G. Bader, and T. V. Van, “Study of the phase transition and the thermal nitridation of nanocrystalline sol-gel films,” J. Non-Cryst. Solids 297(1), 55–66 (2002).
[Crossref]

Egdell, R. G.

P. Romero-Gómez, V. Rico, J. P. Espinós, R. Agustín, G. Elipe, R. G. Palgrave, and R. G. Egdell, “Nitridation of nanocrystalline TiO2 thin films by treatment with ammonia,” Thin Solid Films 519(11), 3587–3595 (2011).
[Crossref]

Elipe, G.

P. Romero-Gómez, V. Rico, J. P. Espinós, R. Agustín, G. Elipe, R. G. Palgrave, and R. G. Egdell, “Nitridation of nanocrystalline TiO2 thin films by treatment with ammonia,” Thin Solid Films 519(11), 3587–3595 (2011).
[Crossref]

Espinós, J. P.

P. Romero-Gómez, V. Rico, J. P. Espinós, R. Agustín, G. Elipe, R. G. Palgrave, and R. G. Egdell, “Nitridation of nanocrystalline TiO2 thin films by treatment with ammonia,” Thin Solid Films 519(11), 3587–3595 (2011).
[Crossref]

Ferrera, M.

Fugier, P.

O. Shavdina, L. Berthod, T. Kämpfe, S. Reynaud, C. Veillas, I. Verrier, M. Langlet, F. Vocanson, P. Fugier, Y. Jourlin, and O. Dellea, “Large area fabrication of periodic TiO2 nanopillars using microsphere photolithography on a photopatternable sol-gel film,” Langmuir 31(28), 7877–7884 (2015).
[Crossref] [PubMed]

Gamet, E.

S. Briche, Z. Tebby, D. Riassetto, M. Messaoud, E. Gamet, E. Pernot, H. Roussel, O. Dellea, Y. Jourlin, and M. Langlet, “New insight in photo-patternad sol-gel-derived TiO2 films,” J. Mater. Sci. 46(5), 1474–1486 (2011).
[Crossref]

Gâté, V.

V. Gâté, Y. Jourlin, F. Vocanson, O. Dellea, G. Vercasson, S. Reynaud, D. Riassetto, and M. Langlet, “Sub-micrometric patterns written using a DIL method coupled to a TiO2 photo-resist,” Opt. Mater. 35(9), 1706–1713 (2013).
[Crossref]

Green, M. A.

S. Pillai, K. R. Catchpole, T. Trupke, and M. A. Green, “Surface plasmon enhanced silicon solar cells,” J. Appl. Phys. 101(9), 093105 (2007).
[Crossref]

Ho, C. W.

N. C. Chen, W. C. Lien, C. R. Liu, Y. L. Huang, Y. R. Lin, C. Chou, S. Y. Chang, and C. W. Ho, “Excitation of surface plasma wave at TiN/air interface in the Kretschmann geometry,” J. Appl. Phys. 109(4), 043104 (2011).
[Crossref]

Huang, D.

C. C. Chang, Y. D. Sharma, Y. S. Kim, J. A. Bur, R. V. Shenoi, S. Krishna, D. Huang, and S. Y. Lin, “A surface plasmon enhanced infrared photodetector based on InAs quantum dots,” Nano Lett. 10(5), 1704–1709 (2010).
[Crossref] [PubMed]

Huang, Y. L.

N. C. Chen, W. C. Lien, C. R. Liu, Y. L. Huang, Y. R. Lin, C. Chou, S. Y. Chang, and C. W. Ho, “Excitation of surface plasma wave at TiN/air interface in the Kretschmann geometry,” J. Appl. Phys. 109(4), 043104 (2011).
[Crossref]

Jiménez, C.

C. Jiménez and M. Langlet, “Formation of TiN by nitridation of TiO2 films deposited by ultrasonically assisted sol-gel technique,” Surf. Coat. Tech. 69, 249–252 (1994).
[Crossref]

Jourlin, Y.

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N. C. Chen, W. C. Lien, C. R. Liu, Y. L. Huang, Y. R. Lin, C. Chou, S. Y. Chang, and C. W. Ho, “Excitation of surface plasma wave at TiN/air interface in the Kretschmann geometry,” J. Appl. Phys. 109(4), 043104 (2011).
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J. Lightwave Technol. (1)

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Langmuir (4)

O. Shavdina, L. Berthod, T. Kämpfe, S. Reynaud, C. Veillas, I. Verrier, M. Langlet, F. Vocanson, P. Fugier, Y. Jourlin, and O. Dellea, “Large area fabrication of periodic TiO2 nanopillars using microsphere photolithography on a photopatternable sol-gel film,” Langmuir 31(28), 7877–7884 (2015).
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C. Valsecchi and A. G. Brolo, “Periodic metallic nanostructures as plasmonic chemical sensors,” Langmuir 29(19), 5638–5649 (2013).
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S. Tian, N. R. Armstrong, and W. Knoll, “Electrochemically tunable surface-plasmon-enhanced diffraction gratings and their (bio-)sensing applications,” Langmuir 21(10), 4656–4660 (2005).
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Y. Kuroda, T. Mori, K. Yagi, N. Makihata, Y. Kawahara, M. Nagao, and S. Kittaka, “Preparation of visible-light-responsive TiO2-xNx photocatalyst by a sol-gel method: analysis of the active center on TiO2 that reacts with NH3.,” Langmuir 21(17), 8026–8034 (2005).
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Nano Lett. (2)

C. C. Chang, Y. D. Sharma, Y. S. Kim, J. A. Bur, R. V. Shenoi, S. Krishna, D. Huang, and S. Y. Lin, “A surface plasmon enhanced infrared photodetector based on InAs quantum dots,” Nano Lett. 10(5), 1704–1709 (2010).
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Nature (1)

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V. Gâté, Y. Jourlin, F. Vocanson, O. Dellea, G. Vercasson, S. Reynaud, D. Riassetto, and M. Langlet, “Sub-micrometric patterns written using a DIL method coupled to a TiO2 photo-resist,” Opt. Mater. 35(9), 1706–1713 (2013).
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Figures (10)

Fig. 1
Fig. 1 X-ray diffraction patterns for pre-treatment at 300°C and ammonolysis at a = 800°C, b = 900°C and c = 1000°C: a) entire patterns and b) zoom around the most intense (200) peak
Fig. 2
Fig. 2 Resistance measurements according to the pre-treatment temperature for ammonolysis at 800°C, 900°C and 1000°C
Fig. 3
Fig. 3 Real part (n’ in blue) and imaginary part (n” in red) of the refractive index according to the wavelength (Vis-NIR), for pre-treatment at 300°C and 500°C and ammonolysis at 900°C and 1000°C
Fig. 4
Fig. 4 Permittivity according to the wavelength for pre-treatment at 300°C and 500°C and for ammonolysis at 900°C and 1000°C: a) real part (ε’) and b) imaginary part (ε”)
Fig. 5
Fig. 5 AFM profile before a) after pre-treatment and ammonolysis and b) performed on a TiO2 xerogel grating.
Fig. 6
Fig. 6 a) Picture of a TiOxNy grating on silicon and b) SEM image of the TiOxNy grating in cross section view.
Fig. 7
Fig. 7 Coupling of the −1st order diffractive order into the plasmon mode.
Fig. 8
Fig. 8 a) Sinusoidal structure of the grating modeled with MC grating and b) power in false colors (from blue to red) of the TM 0th reflected order versus wavelength and angle of incidence.
Fig. 9
Fig. 9 Optical set-up for the measurement of the 0th reflected order of the TiOxNy grating.
Fig. 10
Fig. 10 0th reflected order of the TiOxNy grating for incidence angles of 25°, 30° and 35° and for TE or TM incidence: a) modeling curves and b) experimental measurement.

Tables (1)

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Table 1 Resistivity and conductivity of the TiOxNy films after a pre-treatment at 300°C and ammonolysis at 800°C, 900°C and 1000°C

Equations (9)

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2N H 3 Δ N 2 +3 H 2
2Ti O 2 + H 2 Δ T i 2 O 3 + H 2 O
T i 2 O 3 +2N H 3 Δ 2TiN+3 H 2 O
ρ=Rs*d
σ=1/ρ
ε dielectric < ε TiON
ε r =ε/ε0= ε +i ε with ε = n 2 n 2 and ε =2 n n
mλ=Λ(sinα+sin β m )
sin α c =1 λ Λ

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