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Investigation on reversed domain structures in lithium niobate crystals patterned by interference lithography

Simonetta Grilli, Pietro Ferraro, Sergio De Nicola, Andrea Finizio, Giovanni Pierattini, Paolo De Natale, and Marco Chiarini

Open Access Open Access

Abstract

We demonstrate fabrication of periodically poled lithium niobate samples by electric field poling, after patterning by interference lithography. Furthermore we investigate the poling process at an overpoling regime which caused the appearance of submicron dot domains very similar to those induced by backswitch but different in nature. We show the possibility for realizing submicron-scaled three-dimensional domain patterns that could be applied to the construction of photonic crystals and in nonlinear optics. We show that high etch-rate applied to such structures allows to obtain pyramidal-like submicron relief structures which in principle could find application for waveguide construction in photonic bandgap devices.

©2003 Optical Society of America

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Supplementary Material (3)

Media 1: MOV (135 KB)     
Media 2: MOV (145 KB)     
Media 3: MOV (1561 KB)     

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Figures (15)
Fig. 1.
Fig. 1. Michelson interferometric set-up used to generate the 30µm spaced fringes to be printed on photoresist-coated LN samples. The coherent source is an He-Cd laser emitting at 441.6nm with an output power of 65mW.

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Fig. 2.
Fig. 2. Cross-sectional view of the electrode configuration for electric field poling. The photoresist grating acts as an insulating barrier that lowers the electric field applied through the liquid electrolyte below the coercive field needed to reverse the spontaneous polarization.

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Fig. 3.
Fig. 3. Electrical circuit used to pole LN samples. An High Voltage Amplifier (HVA - 2000x) with a series resistor RS = 50MΩ produces +12kV voltage by using a conventional Signal Generator (SG). A diode rectifier D was connected to the output of the HVA to prevent flowing of backswitch current.

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Fig. 4.
Fig. 4. Optical micrograph of the domain structure with a period of 30µm obtained for a LN sample patterned by IL and revealed by wet etching of 60minutes in a HF:HNO3=1:2 acid mixture. This image is taken in the central area of the pattern and it is representative of the whole pattern obtained in a region of about 20mm in diameter.

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Fig. 5.
Fig. 5. Surface profilometric measurement of the patterned side of the periodically poled and 60minutes etched LN sample shown in Fig. 4. The measurement was performed along the x main axis of the crystal.

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Fig. 6. (a)
Fig. 6. (a) optical micrograph of the aligned dot domains structure observed on the z+ face after electric field overpoling, the structure was revealed by an etching process of 60 minutes in a HF:HNO3=1:2 acid mixture at room temperature; (b) scanning electron microscope image of the dot domains. The crystal sample was periodically patterned by IL at 30µm.

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Fig. 7.
Fig. 7. Optical micrograph of the dot domains in a peripheral region of the pattern. This image clearly shows that the merging of two adjacent domains, due to overpoling, leads to the formation of the dot domains.

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Fig. 8.
Fig. 8. Movie (135 KB) schematically showing the overpoling merging effect under the photoresist strips which leads to the formation of the dot domains in Fig. 6.

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Fig. 9. (a)
Fig. 9. (a) Magnified optical micrograph of the dot domains observed on the z+ face and (b) the corresponding structure observed on the opposite side.

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Fig. 10. (a)
Fig. 10. (a) Optical micrograph of the square array of photoresist dots printed on a lithium niobate sample by interference lithography; (b) optical micrograph of the dot domains obtained by overpoling such patterned lithium niobate sample and revealed by wet etching of 30 minutes; (c)-(d) two different magnified views of the dot domains taken by scanning electron microscope.

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Fig. 11.
Fig. 11. Waveforms of the poling current, the poling voltage and the input voltage acquired by the oscilloscope during the overpoling of a LN sample patterned by the IL dots array pattern with a period of 23µm and using the electrical circuit shown in Fig. 3. The overpoling process took about 3.5s.

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Fig. 12.
Fig. 12. Movie (145 KB) which shows schematically the overpoling merging effect under the photoresist dots which leads to the formation of the dot domains shown in Fig. 10(b) and corresponding to a LN sample patterned by 2D square array of photoresist dots.

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Fig. 13.
Fig. 13. (a) (b) Optical micrographs of the 3D domain patterned samples A and B, etched at 100°C for 45 minutes and for 4 hours, respectively; (c) (d) two different SEM images of the pyramidal-like structures revealed by the 4 hours etching process on the sample B.

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Fig. 14.
Fig. 14. Schematic sectional view of the etched samples A and B. The z- face is flat showing the 3D feature of the obtained crystal structures.

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Fig. 15.
Fig. 15. Movie (1.56 MB) which shows the pyramidal-like morphology of the structures revealed on the 3D domain patterned sample A by 45 minutes etching process at 100°C.

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