WO2015088371A1 - Method of synthesizing a bi-domain structure in ferroelectric single crystal wafers - Google Patents

Method of synthesizing a bi-domain structure in ferroelectric single crystal wafers Download PDF

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Publication number
WO2015088371A1
WO2015088371A1 PCT/RU2013/001115 RU2013001115W WO2015088371A1 WO 2015088371 A1 WO2015088371 A1 WO 2015088371A1 RU 2013001115 W RU2013001115 W RU 2013001115W WO 2015088371 A1 WO2015088371 A1 WO 2015088371A1
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Prior art keywords
single crystal
crystal wafer
ferroelectric single
wafer
ferroelectric
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PCT/RU2013/001115
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French (fr)
Inventor
Mikhail Davydovich MALINKOVICH
Alexander Sergeevich BYKOV
Sedrak Gurgenovich GRIGORYAN
Roman Nikolaevich ZHUKOV
Dmitriy Aleksandrovich KISELEV
Ilya Viktorovich KUBASOV
Yuriy Nikolaevich PARKHOMENKO
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The Federal State Autonomous Educational Institution Of The Higher Professional Education "National University Of Science And Technology "Misis"
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Application filed by The Federal State Autonomous Educational Institution Of The Higher Professional Education "National University Of Science And Technology "Misis" filed Critical The Federal State Autonomous Educational Institution Of The Higher Professional Education "National University Of Science And Technology "Misis"
Priority to RU2014105877/05A priority Critical patent/RU2566142C2/en
Priority to PCT/RU2013/001115 priority patent/WO2015088371A1/en
Priority to EA201600460A priority patent/EA032620B1/en
Publication of WO2015088371A1 publication Critical patent/WO2015088371A1/en

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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/22—Complex oxides
    • C30B29/30—Niobates; Vanadates; Tantalates
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/02—Heat treatment

Definitions

  • This invention relates to the formation of bi-domain structure in ferroelectric single crystals and can be used in nanotechnology and micromechanics for the fabrication and operation of precise positioning devices, for example, probe microscopes and tunable laser resonators, as well as for the adjustment of optical systems.
  • the main structural element of devices pertaining to the field of this invention regardless of their design is the electromechanical device transforming electric power into controlled motion, i.e. the microacuator.
  • Promising methods of actuation should include piezoelectric bimorph deformation elements based on the bidomain structures in ferroelectric single crystals.
  • a method of a domain structure formation in a nonlinear optical ferroelectric single crystal wafer e.g. lithium niobate (RU 2371746, published 27.10.2009), by applying high voltage to the wafer from metallic electrodes located at opposite polar faces of the wafer, wherein one of the electrodes is a structure comprising strips having a specific configuration (a strip electrode) for producing a domain structure of a respective configuration.
  • a strip electrode for producing a domain structure of a respective configuration.
  • Disadvantage of said method is the impossibility of producing a bidomain structure with opposite polarization vectors.
  • a method of a domain structure formation in a nonlinear optical ferroelectric single crystal wafer e.g. lithium niobate (RU 2439636, published 10.01.2012)
  • RU 2439636 lithium niobate
  • one of the electrodes is a structure comprising strips having a specific configuration (a strip electrode)
  • a dielectric coating layer is additionally applied to the polar face of the wafer that is opposite to the side having the strip electrode.
  • a method of a domain structure formation in a nonlinear optical ferroelectric single crystal wafer e.g. lithium niobate by applying an electric field to the polar faces of the wafer one of which has a dielectric layer forming a specific pattern
  • a dielectric layer is applied to one of the polar faces of the wafer, following which a pattern is formed in the dielectric layer using of known photolithographic techniques.
  • Electrodes e.g. liquid electrolyte
  • the system is exposed to an electric field of certain magnitude and duration sufficient for the switching of spontaneous polarization.
  • the prototype of the suggested invention is the method of formation a bidomain structure in lithium nobate single crystals (RU 2492283, published 10.09.2013) for nanotechnology devices and micromechanics by applying electrodes to two faces of a crystal with simultaneous heating to the phase transition point, i.e. to the Curie temperature, during application of a non-uniform electric field.
  • the faces of the crystal are plane-parallel, the crystal is oriented at an angle of z+36° relative to the polar axis, and the electrodes are a system of parallel strings.
  • the electrodes are made of palladium paste and applied to sapphire wafers.
  • the technical result achieved by this invention is the formation of a bidomain structure more than 0.4 mm thick with the preset localization and shape of the domain boundary in ferroelectrics single crystal wafers, wherein ferroelectrics single wafers crystal with a formed bidomain structure increase the efficiency and stability of the electric signals to mechanical elastic deformations transformation, raise the sensitivity and precision due to the absence of mechanical hysteresis, creep and residual deformations in a wide range of working temperatures with a high linearity of the voltage vs mechanical deformation dependence.
  • the method of a bidomain structure formation in ferroelectrics single crystal wafers implying the formation in a ferroelectric single crystal wafer of two single- domain regions with opposite polarization vectors and a bidomain boundary comprises contact-free positioning of the ferroelectric single crystal wafer with plane-parallel faces in the working chamber of light heating system with an oxygen-free environment between two light absorbing shields.
  • the larger faces of the single crystal wafer are arranged parallel to the longitudinal axes of the light absorbing shields.
  • each light beam is set to provide the complete heating of the ferroelectric single crystal wafer within the temperature range of not lower than the Curie temperature and not higher than the ferroelectric crystal melting point.
  • ferroelectric single crystal wafer is further heated under the present conditions and cooled.
  • the ferroelectric single crystal wafer is cooled with a preset temperature gradient varying from the minimum value at the opposite larger faces of the ferroelectric single crystal wafer to the maximum value in the domain boundary formation area, e.g. with a 10°C/mm temperature gradient.
  • the ferroelectric single crystal wafer can be cooled with a preset temperature gradient varying from the maximum value at the opposite larger faces of the ferroelectric single crystal wafer to the minimum value in the domain boundary formation area, e.g. with a 3°C/mm temperature gradient.
  • the ferroelectric single crystal wafer is made of lithium niobate LiNb0 3 single crystal.
  • the contact-free positioning of the ferroelectric single crystal wafer is achieved by placing it on sapphire bars.
  • Said light absorbing shields are single crystal silicon plates.
  • the location and shape of the domain boundary are controlled by varying the intensity and power of the light beam.
  • Fig. 1 shows a scheme of ferroelectric single crystal wafer heating
  • Fig. 2 shows the working chamber of light heating system.
  • the ferroelectric single crystal wafer 1, e.g. a lithium niobate LiNb0 3 single crystal wafer, the light absorbing silicon shields 2, light beams 4, sample holder 8, quartz working chamber of light heating system 9.
  • Figure 1 shows the ferroelectric single crystal wafer 1, e.g. a lithium niobate LiNb0 3 single crystal wafer, the light absorbing silicon shields 2, the sapphire bars 3, the light beams 4 and the heat fluxes coming 5 and exiting 6 and 7 the wafer from the side faces.
  • ferroelectric single crystal wafer e.g. a lithium niobate LiNb0 3 single crystal wafer
  • the light absorbing silicon shields 2 the sapphire bars 3
  • the light beams 4 and the heat fluxes coming 5 and exiting 6 and 7 the wafer from the side faces.
  • the invention is implemented as follows.
  • the wafer 1 having plane-parallel faces is positioned in the working chamber of light heating system with an oxygen-free environment on the sample holder 8 Fig. 2.
  • Inaccurate orientation of the wafer 1 relative to the center of the light heating systems working chamber may distort the planar shape of the domain boundary and deleteriously affect the operation parameters of the bidomain deformation element.
  • the orientation of the wafer faces relative to the polar axes of the ferroelectric single crystal is chosen to provide the desired value of the transverse elastic strain of the wafer.
  • the wafer 1 is placed in the light heating system working chamber between two light-absorbing silicon shields 2 with the larger faces of the wafer 1 being parallel to the longitudinal axes of the shields 2.
  • the contact between the wafer 1 and the shields 2 is avoided using sapphire bars 3.
  • Two opposite parallel light beams 4 are generated in the light heating system working chamber, said beams being perpendicular to the larger faces of the wafer 1 and the longitudinal axes of the shields 2.
  • the larger faces of the wafer 1 are light heated with the light beams 4.
  • the power of each light beam is set to provide the complete heating of the wafer 1.
  • the temperature range providing the complete heating of the wafer is set not lower than the Curie temperature and not higher than the ferroelectric crystal melting point.
  • the temperature distribution over the shields 2 is uniform due to the homogeneous light beams 4 produced using parabolic lamp reflectors.
  • the heat flows 6 and 7 are removed through the butt faces of the wafer 1.
  • the shields 2 produce a non-uniform temperature field in the volume of the wafer 1, said field being symmetrical relative to the center of the wafer 1. This develops conditions under which the wafer 1 can be represented as a two-layered structure wherein the temperature gradient is directed from the surface to the center.
  • the temperature gradient value varies across the thickness of the wafer 1 , reaching the maximum value at the faces of the wafer 1 and declining to zero in the domain boundary formation region.
  • Cooling can be with a preset temperature gradient varying from the minimum value at the opposite larger faces of the ferroelectric single crystal wafer to the maximum value in the domain boundary formation area, e.g. with a 10°C/mm temperature gradient.
  • the ferroelectric single crystal wafer can be cooled with a preset temperature gradient varying from the maximum value at the opposite larger faces of the ferroelectric single crystal wafer to the minimum value in the domain boundary formation area, e.g. with a 3°C/mm temperature gradient.
  • two domains form having opposite directions of the polarization vectors and a planar domain boundary.
  • the directions of the polarization vectors are controlled by the distribution and orientation of the thermal fields in the wafer 1.
  • the ferroelectric single crystal polarization occurs due the phase transition point the coercive force in the ferroelectric single crystal becomes close to zero, and metal ions, e.g. lithium ions in lithium niobate or tantalate become capable of shifting to the nearest oxygen octahedron in the unit cell.
  • metal ions e.g. lithium ions in lithium niobate or tantalate become capable of shifting to the nearest oxygen octahedron in the unit cell.
  • the positions of the ions become fixed.
  • the location and shape of the domain boundary in the volume of the wafer 1 is controlled by heating and cooling regime, e.g. due to the variation of the intensity and power of the light beams 4. They can also be set by changing the position of the wafer 1 in the working space of the light heating system chamber as well as by the thickness and shape of the light-absorbing silicon shields 2. Specific embodiment of the method.
  • Shields were made of single crystal silicon plates 100 mm in diameter and 500 um in thickness by cutting two 75x45 mm shields corresponding to the size of the holder.
  • the specimen was a rectangular wafer of lithium niobate single crystal sized 70 mm (the Z + 36° cut) x 20 mm (the X-cut) and 1.6 mm in thickness and positioned between the silicon shields on sapphire bars.
  • the experimental setup was placed in a light heating system.
  • the lithium niobate single crystal wafer was heated to the congruent composition lithium niobate Curie temperature, i.e. 1150°C for 40 min, then the wafer was exposed to that temperature for 5 min and finally cooled to 100-150°C for 90 min.
  • the annealing caused the formation of domains in the center of the single crystal wafer, the domain boundaries propagated throughout the crystal volume, and eventually a single domain boundary formed in the center of the wafer.
  • the efficiency and stability of electric signal transformation into elastic mechanical strain for the experimental setup of the bimorph element which is the cantilever fixed ferroelectric single crystal wafer sized 70x20x1.6 mm had the following parameters: deformation value in the ⁇ 300 V range was 50 um, the residual strain of the elements was within 0.3% and the deformation linearity was not worse tan 0.01% over the working temperature range from room temperature to 850°C.
  • the bending deformations of the resultant bidomain structures are free from mechanical hysteresis, creep and residual strains over a wide range of working temperatures combined with a high linearity of the voltage vs mechanical deformation dependence.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Optical Modulation, Optical Deflection, Nonlinear Optics, Optical Demodulation, Optical Logic Elements (AREA)

Abstract

Invention relates to the information of bidomain structure in ferroelectric single crystals and can be used in nanotech and micromechanics for fabrication and operation of precise positioning devices, such as probe microscopes, tunable laser resonators, optics adjustment etc. The technical result achieved is the formation of bi-domain boundary, along with increased efficiency and stability of transforming electric signals to elastic deformations, raising sensitivity and precision due to the absence of mechanical hysteresis, creep and residual deformations in wide range of working temperatures with a high linearity of the voltage-to-mechanical deformation dependence.

Description

Method of Synthesizing a Bi-Domain Structure in Ferroelectric Single Crystal
Wafers
Field of Invention. This invention relates to the formation of bi-domain structure in ferroelectric single crystals and can be used in nanotechnology and micromechanics for the fabrication and operation of precise positioning devices, for example, probe microscopes and tunable laser resonators, as well as for the adjustment of optical systems.
State of the Art. The main structural element of devices pertaining to the field of this invention regardless of their design is the electromechanical device transforming electric power into controlled motion, i.e. the microacuator. Promising methods of actuation should include piezoelectric bimorph deformation elements based on the bidomain structures in ferroelectric single crystals.
Known is a method of a domain structure formation in a nonlinear optical ferroelectric single crystal wafer, e.g. lithium niobate (RU 2371746, published 27.10.2009), by applying high voltage to the wafer from metallic electrodes located at opposite polar faces of the wafer, wherein one of the electrodes is a structure comprising strips having a specific configuration (a strip electrode) for producing a domain structure of a respective configuration. According to this known method, at the wafer surface with a strip electrode exposed by the pulsed laser radiation providing a non-uniform heating of the wafer surface layer and formation, under said strip electrode, superficial domains during subsequent cooling after the end of laser radiation pulse. High voltage is applied between the electrodes simultaneously with the laser radiation pulse or after its end, this resulting in the formation of a domain structure consisting of passing through domains exactly replicating the pattern of the strip electrode.
Disadvantage of said method is the impossibility of producing a bidomain structure with opposite polarization vectors. Known is a method of a domain structure formation in a nonlinear optical ferroelectric single crystal wafer, e.g. lithium niobate (RU 2439636, published 10.01.2012), by applying high voltage to the wafer from metallic electrodes located at opposite polar faces of the wafer, wherein one of the electrodes is a structure comprising strips having a specific configuration (a strip electrode), and a dielectric coating layer is additionally applied to the polar face of the wafer that is opposite to the side having the strip electrode.
Disadvantage of said known method is that is can only form regular domain structures consisting of alternate opposite signs domains. Such structures cannot be used as an electromechanical deformation element.
Known is a method of a domain structure formation in a nonlinear optical ferroelectric single crystal wafer, e.g. lithium niobate by applying an electric field to the polar faces of the wafer one of which has a dielectric layer forming a specific pattern (US 5756263, published 26.05.1998). according to said known method, a dielectric layer is applied to one of the polar faces of the wafer, following which a pattern is formed in the dielectric layer using of known photolithographic techniques. Electrodes (e.g. liquid electrolyte) are brought in contact with the polar faces of the wafer, following which the system is exposed to an electric field of certain magnitude and duration sufficient for the switching of spontaneous polarization.
Disadvantage of said known method is also that is possible to form a regular domain structure consisting of alternate opposite signs domains. Such structures cannot be used as an electromechanical deformation element.
The prototype of the suggested invention is the method of formation a bidomain structure in lithium nobate single crystals (RU 2492283, published 10.09.2013) for nanotechnology devices and micromechanics by applying electrodes to two faces of a crystal with simultaneous heating to the phase transition point, i.e. to the Curie temperature, during application of a non-uniform electric field. The faces of the crystal are plane-parallel, the crystal is oriented at an angle of z+36° relative to the polar axis, and the electrodes are a system of parallel strings. According to said known method, the electrodes are made of palladium paste and applied to sapphire wafers.
Disadvantage of said known method is that the bidomain structure thickness cannot exceed 600 um. This limitation is due to the fact that at high temperatures the electric field shielding length in the specimen is limited to 200-300 um because free charge carriers formed at those temperatures shield the external electric field.
Disclosure of the Invention. The technical result achieved by this invention is the formation of a bidomain structure more than 0.4 mm thick with the preset localization and shape of the domain boundary in ferroelectrics single crystal wafers, wherein ferroelectrics single wafers crystal with a formed bidomain structure increase the efficiency and stability of the electric signals to mechanical elastic deformations transformation, raise the sensitivity and precision due to the absence of mechanical hysteresis, creep and residual deformations in a wide range of working temperatures with a high linearity of the voltage vs mechanical deformation dependence.
Said technical result is achieved as follows.
The method of a bidomain structure formation in ferroelectrics single crystal wafers implying the formation in a ferroelectric single crystal wafer of two single- domain regions with opposite polarization vectors and a bidomain boundary comprises contact-free positioning of the ferroelectric single crystal wafer with plane-parallel faces in the working chamber of light heating system with an oxygen-free environment between two light absorbing shields. The larger faces of the single crystal wafer are arranged parallel to the longitudinal axes of the light absorbing shields.
Then, two opposite parallel light beams are generated in the light heating systems chamber, said beams being perpendicular to the larger faces of the ferroelectric single crystal wafer and the longitudinal axes of the light absorbing screens. The power of each light beam is set to provide the complete heating of the ferroelectric single crystal wafer within the temperature range of not lower than the Curie temperature and not higher than the ferroelectric crystal melting point.
Then the ferroelectric single crystal wafer is further heated under the present conditions and cooled.
In a specific embodiment of the method the ferroelectric single crystal wafer is cooled with a preset temperature gradient varying from the minimum value at the opposite larger faces of the ferroelectric single crystal wafer to the maximum value in the domain boundary formation area, e.g. with a 10°C/mm temperature gradient.
Alternatively, the ferroelectric single crystal wafer can be cooled with a preset temperature gradient varying from the maximum value at the opposite larger faces of the ferroelectric single crystal wafer to the minimum value in the domain boundary formation area, e.g. with a 3°C/mm temperature gradient.
In a specific embodiment the ferroelectric single crystal wafer is made of lithium niobate LiNb03 single crystal.
Furthermore, the contact-free positioning of the ferroelectric single crystal wafer is achieved by placing it on sapphire bars.
Said light absorbing shields are single crystal silicon plates.
Also, the location and shape of the domain boundary are controlled by varying the intensity and power of the light beam.
Embodiments of the Invention. The invention is explained with drawings wherein Fig. 1 shows a scheme of ferroelectric single crystal wafer heating and Fig. 2 shows the working chamber of light heating system. The ferroelectric single crystal wafer 1, e.g. a lithium niobate LiNb03 single crystal wafer, the light absorbing silicon shields 2, light beams 4, sample holder 8, quartz working chamber of light heating system 9.
Figure 1 shows the ferroelectric single crystal wafer 1, e.g. a lithium niobate LiNb03 single crystal wafer, the light absorbing silicon shields 2, the sapphire bars 3, the light beams 4 and the heat fluxes coming 5 and exiting 6 and 7 the wafer from the side faces.
The invention is implemented as follows.
The wafer 1 having plane-parallel faces is positioned in the working chamber of light heating system with an oxygen-free environment on the sample holder 8 Fig. 2.
Inaccurate orientation of the wafer 1 relative to the center of the light heating systems working chamber may distort the planar shape of the domain boundary and deleteriously affect the operation parameters of the bidomain deformation element.
The orientation of the wafer faces relative to the polar axes of the ferroelectric single crystal is chosen to provide the desired value of the transverse elastic strain of the wafer.
The wafer 1 is placed in the light heating system working chamber between two light-absorbing silicon shields 2 with the larger faces of the wafer 1 being parallel to the longitudinal axes of the shields 2. The contact between the wafer 1 and the shields 2 is avoided using sapphire bars 3.
Two opposite parallel light beams 4 are generated in the light heating system working chamber, said beams being perpendicular to the larger faces of the wafer 1 and the longitudinal axes of the shields 2.
The larger faces of the wafer 1 are light heated with the light beams 4. The power of each light beam is set to provide the complete heating of the wafer 1. The temperature range providing the complete heating of the wafer is set not lower than the Curie temperature and not higher than the ferroelectric crystal melting point.
The temperature distribution over the shields 2 is uniform due to the homogeneous light beams 4 produced using parabolic lamp reflectors. The heat flows 6 and 7 are removed through the butt faces of the wafer 1. The shields 2 produce a non-uniform temperature field in the volume of the wafer 1, said field being symmetrical relative to the center of the wafer 1. This develops conditions under which the wafer 1 can be represented as a two-layered structure wherein the temperature gradient is directed from the surface to the center. The temperature gradient value varies across the thickness of the wafer 1 , reaching the maximum value at the faces of the wafer 1 and declining to zero in the domain boundary formation region.
After the complete heating of the wafer 1 under the abovementioned conditions the wafer is cooled. Cooling can be with a preset temperature gradient varying from the minimum value at the opposite larger faces of the ferroelectric single crystal wafer to the maximum value in the domain boundary formation area, e.g. with a 10°C/mm temperature gradient.
Alternatively, the ferroelectric single crystal wafer can be cooled with a preset temperature gradient varying from the maximum value at the opposite larger faces of the ferroelectric single crystal wafer to the minimum value in the domain boundary formation area, e.g. with a 3°C/mm temperature gradient.
In either case when the wafer 1 is cooled from the Curie temperature, two domains form having opposite directions of the polarization vectors and a planar domain boundary. The directions of the polarization vectors are controlled by the distribution and orientation of the thermal fields in the wafer 1.
The ferroelectric single crystal polarization occurs due the phase transition point the coercive force in the ferroelectric single crystal becomes close to zero, and metal ions, e.g. lithium ions in lithium niobate or tantalate become capable of shifting to the nearest oxygen octahedron in the unit cell. When the temperature declines to below the phase transition point the positions of the ions become fixed.
The location and shape of the domain boundary in the volume of the wafer 1 is controlled by heating and cooling regime, e.g. due to the variation of the intensity and power of the light beams 4. They can also be set by changing the position of the wafer 1 in the working space of the light heating system chamber as well as by the thickness and shape of the light-absorbing silicon shields 2. Specific embodiment of the method.
Shields were made of single crystal silicon plates 100 mm in diameter and 500 um in thickness by cutting two 75x45 mm shields corresponding to the size of the holder.
The specimen was a rectangular wafer of lithium niobate single crystal sized 70 mm (the Z + 36° cut) x 20 mm (the X-cut) and 1.6 mm in thickness and positioned between the silicon shields on sapphire bars. The experimental setup was placed in a light heating system.
In the light heating system, the lithium niobate single crystal wafer was heated to the congruent composition lithium niobate Curie temperature, i.e. 1150°C for 40 min, then the wafer was exposed to that temperature for 5 min and finally cooled to 100-150°C for 90 min. The annealing caused the formation of domains in the center of the single crystal wafer, the domain boundaries propagated throughout the crystal volume, and eventually a single domain boundary formed in the center of the wafer.
Morphological studies and visualization of the domain structure in the lithium niobate single crystal by selective etching, X-ray topography and scanning probe microscopy confirmed that a stable bidomain structure formed as a result of annealing.
The efficiency and stability of electric signal transformation into elastic mechanical strain for the experimental setup of the bimorph element, which is the cantilever fixed ferroelectric single crystal wafer sized 70x20x1.6 mm had the following parameters: deformation value in the ±300 V range was 50 um, the residual strain of the elements was within 0.3% and the deformation linearity was not worse tan 0.01% over the working temperature range from room temperature to 850°C.
In the invention claimed herein, the bending deformations of the resultant bidomain structures are free from mechanical hysteresis, creep and residual strains over a wide range of working temperatures combined with a high linearity of the voltage vs mechanical deformation dependence.

Claims

What is claimed is a
1. Method of a bidomain structure formation in ferroelectrics single crystal wafers implying the formation in a ferroelectric single crystal wafer of two single- domain regions with opposite polarization vectors and a bidomain boundary comprises contact-free positioning of the ferroelectric single crystal wafer with plane-parallel faces in the working chamber of light heating system with an oxygen-free environment between two light absorbing shields, wherein larger faces of the single crystal wafer are arranged parallel to the longitudinal axes of the light absorbing shields, following which two opposite parallel light beams are generated in the light heating systems chamber, said beams being perpendicular to the larger faces of the ferroelectric single crystal wafer and the longitudinal axes of the light absorbing screens. The power of each light beam is set to provide the complete heating of the ferroelectric single crystal wafer within the temperature range of not lower than the Curie temperature and not higher than the ferroelectric crystal melting point and finally then the ferroelectric single crystal wafer is further heated under the preset conditions and cooled.
2. Method of Claim 1 wherein said ferroelectric single crystal wafer is cooled with a preset temperature gradient varying from the minimum value at the opposite larger faces of the ferroelectric single crystal wafer to the maximum value in the domain boundary formation area, e.g. with a 10°C/mm temperature gradient.
3. Method of Claim 1 wherein said ferroelectric single crystal wafer is cooled with a preset temperature gradient varying from the maximum value at the opposite larger faces of the ferroelectric single crystal wafer to the minimum value in the domain boundary formation area, e.g. with a 3°C/mm temperature gradient.
4. Method of Claim 1 wherein said ferroelectric single crystal wafer is made of lithium niobate LiNb03.
5. Method of Claim 1 wherein the contact-free positioning of said ferroelectric single crystal wafer is achieved by placing it on sapphire bars.
6. Method of Claim 1 wherein said light-absorbing shields are single crystal silicon plates.
7. Method of Claim 1 wherein the location and shape of the domain boundary are controlled by the intensity and power of the light beam.
PCT/RU2013/001115 2013-12-12 2013-12-12 Method of synthesizing a bi-domain structure in ferroelectric single crystal wafers WO2015088371A1 (en)

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RU2014105877/05A RU2566142C2 (en) 2013-12-12 2013-12-12 Method of forming bidomain structure in ferrielectric monocrystal plates
PCT/RU2013/001115 WO2015088371A1 (en) 2013-12-12 2013-12-12 Method of synthesizing a bi-domain structure in ferroelectric single crystal wafers
EA201600460A EA032620B1 (en) 2013-12-12 2013-12-12 Method of a bidomain structure formation in ferroelectric single crystal wafers

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CN110670134A (en) * 2019-09-20 2020-01-10 南开大学 Preparation method of p-type and n-type conductive lithium niobate nanowires

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RU196011U1 (en) * 2019-12-13 2020-02-13 Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский технологический университет "МИСиС" Three-axis positioning device

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US5756263A (en) * 1995-05-30 1998-05-26 Eastman Kodak Company Method of inverting ferroelectric domains by application of controlled electric field
WO2009015474A1 (en) * 2007-07-31 2009-02-05 Ye Hu Method of ferroelectronic domain inversion and its applications
RU2492283C2 (en) * 2011-12-08 2013-09-10 Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Национальный исследовательский технологический университет "МИСиС" Method for formation of bidomain structure in single-crystal plates

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Publication number Priority date Publication date Assignee Title
US5756263A (en) * 1995-05-30 1998-05-26 Eastman Kodak Company Method of inverting ferroelectric domains by application of controlled electric field
WO2009015474A1 (en) * 2007-07-31 2009-02-05 Ye Hu Method of ferroelectronic domain inversion and its applications
RU2492283C2 (en) * 2011-12-08 2013-09-10 Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Национальный исследовательский технологический университет "МИСиС" Method for formation of bidomain structure in single-crystal plates

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CN110670134A (en) * 2019-09-20 2020-01-10 南开大学 Preparation method of p-type and n-type conductive lithium niobate nanowires
WO2021051844A1 (en) * 2019-09-20 2021-03-25 南开大学 Lithium niobate having p-type nanowire region or n-type nanowire region and preparation method therefor, and method for converting carrier type thereof
US11834755B2 (en) 2019-09-20 2023-12-05 Nankai University Lithium niobate having p-type nanowire region or n-type nanowire region, method for preparing the same, and method for converting charge carrier type of nanowire region

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