| 2.
Engineering Periodic Domain Structure
Crystalline defects play major
role: it is easier to create uniform domain grating in the
stoichiometric LN, LT that have minimal defects, than in congruent
LN and LT.
The kinetics of the domain structure
in spatially nonuniform electric field produced by the electrode
pattern depends on the number of factors: 1) shape of individual
electrode, 2) electrode material, 3) variant of electrode
structure (Fig.2), 4) geometry of the electrode pattern, 5)
parameters of the dielectric layer, 6) poling waveform, 7)
switching current limit, and 8) temperature.
Moreover, the spatial uniformity
of the switching characteristics, conductivity and thickness
of the crystalline wafer is of crucial importance.
The optimization of all technological
factors can be done only the basis of the deep knowledge of
the foundations of domain engineering in ferroelectrics. |
 |
Fig. 2 Variants of electrode structures
for periodical domain patterning by electric field poling.
I – metal electrode pattern, II – metal electrode over
insulator pattern, III – metal electrode pattern covered by
insulator, IV – liquid electrode over insulator pattern, V
– stamper electrode, VI – corona discharge method.
Table 2. Electrode structures
for periodical domain patterning by electric poling

Spectralus’s efforts are directed
towards identifying and optimizing those parameters contributing
most significantly to repeatable, good-quality periodic domain pattern
in LN and LT crystals.
An extensive discussion of domain
structure development including investigations of the domain engineering
aspects in LiNbO3 is contained in: Ferroelectrics, V.221, pp157-167
(1999) by V. Shur, E. Rumyantsev, R. Batchko, G. Miller, M. Fejer,
R. Byer
The domain kinetics during periodical
poling from the single domain state in a spatially inhomogeneous
field can be divided into five main stages: 1) nucleation of new
domains at the surface, 2) forward growth of nucleated domains in
polar direction with subsequent coalescence, 3) broadening of the
strip domains by sideways domain wall motion, 4) stabilization of
the domain structure in external field, and 5) backswitching after
removing of external field (Fig.3).
All stages have to be carefully optimized
to produce a specified domain period and duty cycle with acceptable
uniformity throughout the volume of the wafer.

Fig.3. The main stages of the domain
evolution during periodical poling
After detail analysis of the published
data and basing on our experience we have chosen for the poling
of CLN to use the most simple and easier for realization design
of the electrode structure, so-called “photoresist only”
(Fig. 2 IV). In this case the photoresist pattern is deposited on
one side. The liquid electrolyte in spatial sample holder was used
for application of electric field.
The scheme of used experimental setup is shown on Figure 4. The
setup allows us to apply arbitrary shape poling pulses from TREK
20/20 pulse source to the sample located inside the holder made
from acrylic resin. Accuracy of the poling pulse: time resolution
10 ns (100 MHz sampling rate), voltage resolution 14 bit. The lowered
voltage and switching current are monitored via the digital storage
oscilloscope Tektronix TDS1002, triggered by the generator. Oscilloscope
is connected to the computer, thus downloading the measured data
via RS232 protocol. Optical polarizing microscope with video camera
allows us to record simultaneously the video and instantaneous pictures
with view area about 1 mm2.

Fig. 4. Scheme of the poling setup: 1 – sample
in the holder, 2 - polarizer, 3 - analyzer, 4 - video camera, 5
- light source, 6 - acrylic resin box.
3” wafer with patterned photoresist is placed
in the sample holder for poling with liquid electrolyte –
saturated water solution of LiCl. Two holders different in the rubber
pads shape: (1) circular and (2) rectangular with rounded corners
were used during the poling process.
The periodical poling of the MgO doped LN can be achieved
only at the elevated temperatures. As a result we use another variant
of the electrode structure with the metal electrodes (Fig.2 I).
The whole poling process contains several operations.
- Optical inspection of the wafer using polarized
microscope to reveal the bulk macro-defects and residual domains
(deviations from single domain state).
- Creation of metal electrode pattern by lithography
with controlled heating/cooling rates during baking of photoresist
- Inspection of the domain structure in the wafer just
before poling to avoid appearance of residual domains
by polarizing or phase contrast microscopy without application
of the external field.
- Periodical poling at elevated temperature
above 100OC in silicon oil with observation of domain kinetics
in transmitted or reflected light with subsequent low cooling
rate to avoid wafer cracking and to uncontrolled change of the
tailored domain structure.
The quality of a periodically-poled (PP) structure is mainly determined
by two factors: periodicity and duty cycle (DC). The periodicity
of the PP structure strongly affects the phase-matching wavelength
of a conversion device, while the DC of the PP structure affects
conversion efficiency. Maximum conversion efficiency can be achieved
for a perfect uniform DC of 0.5. Therefore, to estimate the uniformity
of the DC, the optically microscope images of the etched (in pure
hydrofluoric acid) periodically poled surface were carried out (Fig.
5). The widths of domain inverted region were measured on the Z+
and Z- surfaces in the fabricated PPLN element. Uniform PP structure
with a 6.75 ?m period and 0.5?0.1 DC has been fabricated from the
Z+ surface to more than 400 ?m depth over an area of 5 mm by 10
mm.

Fig. 5. Optical microscopic image of the etched PP structure for
the 0.5 mm thick PPLN element with a 6.78 ?m domain inverted period
on Z+ surface.
Fig. 6. Scanning probe microscopy observation of the periodical
domain structure revealed by etching in 0.5 mm thick MgO:LN
3. Applications
An important application of periodically poled ferroelectrics
is wavelength conversion of commercial diode and compact DPSS near-IR
lasers to blue, green, and medium-IR spectral regions. Periodically
poled LN and LT have clear advantages over the birefringence phase-matched
KTP, LiB3O5 (LBO) and BaB2O4 (BBO) nonlinear crystals in terms of
3-5 times lager effective nonlinearity and a possibility to phase-match
any second-order interaction within the transmission band of material.
Due to high conversion efficiency, PPLN devices are well suited
as a nonlinear component for SHG from compact, low power consumption
(<10W) lasers, capable of producing 0.1-1W optical power. For
the testing of our PPLN elements, the YAG:Nd DPSS laser, that produces
300mW cw at 1064?0.1nm in single-transverse mode, has been used.
Figure 6 present the dependence of the SHG (532nm) outputs on
temperature. Excellent fitting of experiment and calculations demonstrates
higher quality of fabricated periodically-poled grating, presented
in Fig. 5.
A doubling of frequency of diode laser by high-efficient PPLN
or PPMgOLN nonlinear-optical components is likely to be the winning
technology for low-power blue-green laser market needs.
The diode laser used in present work was InGaAs VECSEL surface-emitting
laser . Both their optical mode characteristics and wavelength were
controlled by an extended compound optical cavity. These lasers
produced ~0.15 W cw at 1064?0.2 nm in single mode operation.
The PPLN components have narrow acceptance bandwidths of about
2 nm/mm and therefore 5mm of length conversion elements are optimal
for doubling of VECSEL diode lasers. On the other hands, conversion
efficiency of periodically-poled elements is proportional to the
fundamental optical power of laser. To increase the conversion efficiency,
pulsed laser, modulated by an injection current, has been used.
By using 2 A current pulse, 0.5 W optical power was generated in
single-transverse mode.

Fig. 7. Temperature dependence of the green light maximum intensity
(532 nm output power) for MgO PPLN period 6.95 microns. The dots
are experimental data and the solid curve is theoretical curve for
a 5 mm length.
Detail analysis of pulse regime has shown that a wavelength chirp
of 5nm/?s rate takes place.
Therefore, for optimization of SHG process, pulse duration and length
of PPLN element was restricted to 100 ns and 3mm. We have demonstrated
10mW average and 1W peak green power light generation from the intracavity-doubled
VECSEL laser (Fig. 8).
No degradation of green light power was observed during 100 hours
of operation.
Fig. 8. Pulsed 532nm output generated by the intracavity-doubled
of VECSEL (1064nm) laser.
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