CN115506029B - Method for regulating topological ferroelectric domain configuration through nano indentation/scratch - Google Patents
Method for regulating topological ferroelectric domain configuration through nano indentation/scratch Download PDFInfo
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- 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
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- 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
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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
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
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Abstract
The invention discloses a method for regulating and controlling topological ferroelectric domain configuration through nano indentation/scratch, which comprises the following steps: the original flaky monocrystal is fixed on a substrate through an adhesive; pressing the first surface of the original flaky monocrystal into the first surface under a first load by adopting a nanometer pressure head to form an indentation; transferring to a heating table to raise the temperature to 80-120 ℃ and separating the original flaky monocrystal from the substrate; transferring the original flaky monocrystal into a crucible, embedding by adopting polycrystalline powder, and placing the crucible into a box-type furnace; raising the temperature from room temperature to 1450-1500 ℃, preserving the temperature for 5-10 min, and performing heat treatment on the original flaky monocrystal; and (3) returning to the room temperature, and obtaining the target flaky single crystal from the crucible, wherein ferroelectric domains of the target flaky single crystal are distributed in a six-fold symmetrical vortex mode near the indentation. The stress/strain is introduced into the hexagonal manganese oxide flaky monocrystal through nano indentation/scratch at room temperature, so that the topology protection ferroelectric domain configuration of spontaneous formation of the monocrystal can be accurately controlled locally.
Description
Technical Field
The invention relates to the technical field of ferroelectric materials, in particular to a method for regulating and controlling topological ferroelectric domain configuration through nano indentation/scratch.
Background
The ferroelectric material has important application value in the fields of polymorphic memories, piezoelectric drivers, ultrasonic transducers and the like because of spontaneous polarization and non-volatility which can be reversed by an external field. Ferroelectric materials have a rich microstructure in which regions with the same polarization direction are called domains and regions dividing different domains are called domain walls. The nanoscale domain walls in ferroelectric materials can exhibit different physical properties from the parent materials, are not constrained by lattice symmetry, and can be created, moved and erased in space by an applied electric field, thereby enabling real-time adjustment of the domain wall position, density and direction, enabling domain wall-based micro-nano electronic devices. In recent years, researchers have found that the hexagonal manganese oxide h-RMnO 3 (r= Y, ho-Lu) system is a type of ferroelectric material with ferroelectric domains and conductive domain walls of rich configuration. In the process of changing the high-temperature paraelectric phase (P6 3/mmc) into the ferroelectric phase (P6 3 cm) after the temperature is reduced by the Curie temperature (T C =950-1400 ℃), the intrinsic topology protection mechanism causes the paraelectric phase to have rich topology protection vortex domain structures, so that domain walls of three different conducting states can coexist.
Ferroelectric materials have hysteresis loops essentially of inversion of domains and movement of domain walls under the influence of an applied electric field, thus providing a means of controlling domain structure at the micro-nano scale. The most commonly used means for electric field regulation, annealing cooling rate regulation and high temperature strain regulation are currently adopted. The electric field regulating means can only regulate domain walls and cannot regulate vortex center movement of hexagonal manganese oxide due to topological protection. The annealing cooling rate regulation means can integrally and macroscopically regulate the vortex center density of the hexagonal manganese oxide by changing different annealing cooling rates in the annealing process, so that the effect of integrally regulating and controlling the vortex center is achieved, but the hexagonal manganese oxide vortex center formed by regulating and controlling is still three-dimensionally and randomly distributed, cannot be manually controlled, cannot locally and accurately regulate and control the position, and brings great difficulty to regulation and control convenience of practical application in the future. The high-temperature strain regulation means can realize local regulation and control of vortex center movement, but the method needs to be applied at high temperature, has high experimental difficulty and cannot be accurately regulated and controlled. The prior art CN110473873A provides a preparation method of an ordered ferroelectric topological domain structure array, the ordered ferroelectric topological domain structure array prepared based on a PZT nano dot array reaches the nano level, and ferroelectric topological domain structures are mutually independent and can be regulated and controlled by a conventional electric field, but a single topological domain (ferroelectric vortex domain or central domain) induced by the electric field on a film or a block has the problems of low density and difficult precise local control of the ferroelectric domain.
Therefore, it is desirable to provide a method for controlling the topology ferroelectric domain configuration by nanoindentation/scratching, which can precisely and locally control the topology protective ferroelectric domain configuration of spontaneous single crystal formation.
Disclosure of Invention
In view of this, the present invention provides a method for controlling topological ferroelectric domain configuration by nanoindentation/scratching, the target raw material comprising a raw sheet-like single crystal and a substrate, the raw sheet-like single crystal being fixed to the substrate by an adhesive; pressing the first surface of the original flaky monocrystal into the first surface of the original flaky monocrystal under a first load by adopting a nanometer pressure head to form an indentation, wherein the first surface is the surface of the side, far away from the substrate, of the original flaky monocrystal; transferring the target raw material with the indentation to a heating table, and heating the heating table to 80-120 ℃ from room temperature according to the heating speed of 60-120 ℃ per hour to separate the original flaky monocrystal from the substrate; transferring the original flaky single crystal into a crucible, embedding the original flaky single crystal by using polycrystalline powder, and placing the crucible into a box-type furnace; raising the temperature in the box furnace from room temperature to 1450-1500 ℃ according to the heating rate of 120-180 ℃/h, and preserving the temperature at 1450-1500 ℃ for 5-10 min to perform heat treatment on the original flaky single crystal; the temperature in the box-type furnace is restored to the room temperature from 1450 ℃ to 1500 ℃ according to the cooling speed of 150 ℃/h to 200 ℃/h, the target flaky monocrystal is obtained from the crucible, and the ferroelectric domains of the target flaky monocrystal are distributed in a six-fold symmetrical vortex mode near the indentation.
Preferably, the first load is 50mN to 400mN.
The invention also provides a method for regulating and controlling topological ferroelectric domain configuration by nano indentation/scratch, wherein the target raw material comprises an original flaky monocrystal and a substrate, and the original flaky monocrystal is fixed on the substrate through an adhesive; pressing a nano pressure head into a second surface of the original flaky monocrystal under a second load, and moving in a direction parallel to a plane where the second surface is positioned to form a first scratch, wherein the second surface is a surface of the original flaky monocrystal, which is far away from one side of the substrate; transferring the target raw material with the first scratch to a heating table, and heating the heating table to 80-120 ℃ from room temperature according to the heating speed of 60-120 ℃ per hour to separate the original flaky monocrystal from the substrate; transferring the original flaky single crystal into a crucible, embedding the original flaky single crystal by using polycrystalline powder, and placing the crucible into a box-type furnace; raising the temperature in the box furnace from room temperature to 1450-1500 ℃ according to the heating rate of 120-180 ℃/h, and preserving the temperature at 1450-1500 ℃ for 5-10 min to perform heat treatment on the original flaky single crystal; and (3) recovering the temperature in the box furnace from 1450-1500 ℃ to room temperature according to the cooling speed of 150-200 ℃/h, and obtaining the target flaky monocrystal from the crucible, wherein ferroelectric domains of the target flaky monocrystal are distributed in high-density stripes on two sides of the first scratch.
Preferably, the nano pressure head is pressed into the second surface of the original flaky monocrystal under a second load and moves along a direction parallel to and opposite to the first scratch to form a second scratch; transferring the target raw material with the first scratch and the second scratch to a heating table, and heating the heating table to 80-120 ℃ from room temperature according to the heating speed of 60-120 ℃ per hour to separate the original flaky monocrystal from the substrate; transferring the original flaky single crystal into a crucible, embedding the original flaky single crystal by using polycrystalline powder, and placing the crucible into a box-type furnace; raising the temperature in the box furnace from room temperature to 1450-1500 ℃ according to the heating rate of 120-180 ℃/h, and preserving the temperature at 1450-1500 ℃ for 5-10 min to perform heat treatment on the original flaky single crystal; and (3) recovering the temperature in the box furnace from 1450-1500 ℃ to room temperature according to the cooling speed of 150-200 ℃/h, and obtaining the target flaky monocrystal from the crucible, wherein ferroelectric domains of the target flaky monocrystal are distributed in high-density parallel stripes between the first scratches and the second scratches.
Preferably, the second load is 50mN to 100mN.
Preferably, the first and second scratches have a length of 100 μm to 1000 μm and a pitch of 30 μm to 60 μm.
Preferably, the original flaky single crystal and the target flaky single crystal are hexagonal manganese oxide flaky single crystals, and the hexagonal manganese oxide flaky single crystals have a chemical formula of RMnO 3, wherein R is any element of Er, Y, lu, ho, tm or Yb; the polycrystalline powder is RMnO 3 polycrystalline powder, wherein R is any one element of Er, Y, lu, ho, tm or Yb.
Preferably, the ram is any one of a bosch ram, a spherical ram, or a conical ram.
Preferably, the substrate is an iron sheet, a silicon wafer, a glass slide, a zirconia ceramic sheet or a silicon nitride ceramic sheet; the binder is glue or thermosetting resin.
Preferably, the ferroelectric domains of the target platelet single crystal are in a six-fold symmetric vortex type distribution or a high-density stripe type distribution.
Compared with the prior art, the method for regulating and controlling the topological ferroelectric domain configuration through nano indentation/scratch provided by the invention has the following beneficial effects:
According to the method for regulating and controlling the topological ferroelectric domain configuration through the nano-indentation/scratch, stress/strain is introduced into the hexagonal manganese oxide flaky monocrystal through the nano-indentation/scratch at room temperature, and compared with the existing method for applying strain through placing an aluminum rod at a high temperature, the method is safer and more convenient to operate. Meanwhile, the nano indentation/scratch can manually control the load size of the indentation/scratch, the moving direction of the pressure head, the moving distance of the pressure head and other parameters, can regulate and control the ferroelectric domain of the hexagonal manganese oxide flaky monocrystal to be in six-fold symmetrical vortex type distribution or high-density stripe type distribution, paves the way for realizing the application of domain wall base micro-nano electronic devices, can be applied to other perovskite ferroelectric material systems at the same time, and provides brand-new means and degree of freedom for regulating and controlling the ferroelectric domain and domain wall.
Of course, it is not necessary for any one product embodying the invention to achieve all of the technical effects described above at the same time.
Other features of the present invention and its advantages will become apparent from the following detailed description of exemplary embodiments of the invention, which proceeds with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description, serve to explain the principles of the invention.
FIG. 1 is a flow chart of a method for controlling topological ferroelectric domain configuration by nano-indentation provided by the invention;
FIG. 2 is a microscopic view of a six-fold symmetric vortex distribution of ferroelectric domains of a LuMnO 3 single crystal provided by the invention near an indentation;
FIG. 3 is a graph showing the Magnus type force distribution diagram induced by hexagonal lattice under random distribution vortex domain and concentrated force of LuMnO 3 monocrystal provided by the invention;
FIG. 4 shows the formation and evolution of six-fold symmetric vortex domain distribution of LuMnO 3 single crystals provided by the invention;
FIG. 5 is a graph showing six-fold symmetric vortex domains of a LuMnO 3 single crystal provided by the invention in different loading and pressing directions;
FIG. 6 is a graph of densities of six-fold symmetric vortex domains of a LuMnO 3 single crystal provided by the invention under different loads;
FIG. 7 shows the distribution of six-fold symmetrical vortex domains induced by different pressure heads of the LuMnO 3 single crystal provided by the invention;
FIG. 8 is a flow chart of a method for controlling topological ferroelectric domain configuration by nano scratches provided by the present invention;
FIG. 9 is a microscopic image of the ferroelectric domains of the LuMnO 3 single crystal provided by the present invention in a high density stripe distribution near the scratch;
FIG. 10 is a flow chart of another method for controlling topological ferroelectric domain configuration by nano scratches provided by the present invention;
FIG. 11 is a microscopic image of the ferroelectric domains of the LuMnO 3 single crystal provided by the present invention in a high density parallel stripe distribution near the scratch;
FIG. 12 is a graph showing the large area and high density striped domains generated by nano scratch control of the LuMnO 3 single crystal provided by the invention;
FIG. 13 is a graph showing the distribution of large-area high-density parallel stripe domains produced by nano-scratch control of the LuMnO 3 single crystal provided by the invention.
Detailed Description
Various exemplary embodiments of the present invention will now be described in detail with reference to the accompanying drawings. It should be noted that: the relative arrangement of the components and steps, numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless it is specifically stated otherwise.
The following description of at least one exemplary embodiment is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses.
Techniques, methods, and apparatus known to one of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification where appropriate.
In all examples shown and discussed herein, any specific values should be construed as merely illustrative, and not a limitation. Thus, other examples of exemplary embodiments may have different values.
It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further discussion thereof is necessary in subsequent figures.
The most commonly used means for regulating domain structure at present are electric field regulation means, annealing cooling rate regulation means and high-temperature strain regulation means. Wherein, the electric field regulating means can not regulate the vortex center movement of the hexagonal manganese oxide; the hexagonal manganese oxide vortex centers formed by the annealing cooling rate regulation means are still distributed three-dimensionally and randomly, cannot be controlled manually, and cannot regulate the positions locally and accurately; the high-temperature strain regulation means needs to be applied at high temperature, has high experimental difficulty and cannot be accurately regulated.
Based on the above study, the application provides a method for regulating and controlling topological ferroelectric domain configuration through nano-indentation/scratch, wherein stress/strain is introduced into hexagonal manganese oxide flaky single crystal through nano-indentation/scratch at room temperature, meanwhile, the nano-indentation/scratch can manually control the load size of the indentation/scratch, the moving direction of the pressure head, the moving distance of the pressure head and other parameters, so that the ferroelectric domain of the hexagonal manganese oxide flaky single crystal can be regulated and controlled to be in six-fold symmetrical vortex type distribution or high-density stripe type distribution, and the manufacturing process is simple and safe. The method for controlling the topological ferroelectric domain configuration through nano indentation/scratch provided by the application has the technical effects, and is described in detail below.
Example 1
Referring to fig. 1, fig. 1 is a flowchart of a method for adjusting and controlling a topological ferroelectric domain configuration by nano-indentation, which includes the following steps:
S101, the target raw material comprises an original flaky single crystal and a substrate, wherein the original flaky single crystal is fixed on the substrate through an adhesive;
S102, pressing a nano pressure head into a first surface of an original flaky single crystal under a first load to form an indentation, wherein the first surface is the surface of the original flaky single crystal, which is far away from the substrate side;
S103, transferring the target raw material with the indentation to a heating table, and heating the heating table to 80-120 ℃ from room temperature according to the heating speed of 60-120 ℃ per hour to separate the original flaky monocrystal from the substrate;
S104, transferring the original flaky single crystal into a crucible, embedding the original flaky single crystal by using polycrystalline powder, and placing the crucible in a box-type furnace;
S105, raising the temperature in the box furnace from room temperature to 1450-1500 ℃ according to the heating rate of 120-180 ℃/h, and preserving the temperature at 1450-1500 ℃ for 5-10min to perform heat treatment on the original flaky single crystal;
S106, recovering the temperature in the box-type furnace from 1450-1500 ℃ to room temperature according to the cooling speed of 150-200 ℃/h;
S107, obtaining a target flaky single crystal from the crucible, wherein ferroelectric domains of the target flaky single crystal are distributed in a six-fold symmetrical vortex mode near the indentation.
Specifically, the method for regulating and controlling topological ferroelectric domain configuration through nano indentation provided in the embodiment comprises the following steps:
S101, selecting a target raw material according to elements contained in a hexagonal manganese oxide flaky single crystal, wherein the target raw material comprises an original flaky single crystal and a substrate, and the original flaky single crystal is fixed on the substrate through an adhesive;
Alternatively, the adhesive may be 502 glue, AB glue or thermosetting resin, but is not limited thereto, and no matter what material is used, it is only required that the original sheet-like single crystal can be fixed on the substrate.
Optionally, the substrate is an iron sheet, a silicon wafer, a glass slide, a zirconia ceramic sheet or a silicon nitride ceramic sheet, but is not limited to the above, and no matter what material is adopted, only the surface smoothness of the substrate is required.
S102, pressing a nano pressure head on a nano indentation instrument into a first surface of an original flaky single crystal to form an indentation under a first load, wherein the first surface is a surface of the original flaky single crystal, which is far away from a substrate, of the target raw material obtained in the step S101, and then lifting the pressure head and leaving the pressure head from the target raw material;
Optionally, the pressure head is any one of a glass pressure head, a spherical pressure head or a conical pressure head, and the shape and size of the pressure head are not particularly limited herein.
Alternatively, the first load is 50mN to 400mN, for example 50mN, 100mN, 200mN, 300mN, 400mN, etc.
Alternatively, the nanoindenter may be replaced with other instruments, such as an atomic force microscope, a diamond glass knife, and the like.
S103, transferring the target raw material with the indentation obtained in the step S102 to a heating table, heating the temperature of the heating table from room temperature to 80-120 ℃ at a heating rate of 60-120 ℃/h, such as 80 ℃, 90 ℃, 100 ℃, 110 ℃, 120 ℃ and the like, removing the binder, separating the original flaky single crystal from the substrate and taking down the original flaky single crystal;
s104, transferring the original flaky single crystal obtained in the step S103 into a crucible, embedding the original flaky single crystal by using polycrystalline powder, and placing the crucible into a box-type furnace;
Alternatively, the crucible is an alumina crucible.
S105, raising the temperature in the box-type furnace in the step S104 from room temperature to 1450-1500 ℃ according to the heating speed of 120-180 ℃/h, and preserving the temperature at 1450-1500 ℃ for 5-10 min, such as 1450-1465 ℃, 1475 ℃, 1485 ℃, 1500 ℃ and the like, and performing heat treatment on the original flaky single crystal;
S106, recovering the temperature in the box-type furnace from 1450-1500 ℃ to room temperature according to the cooling speed of 150-200 ℃/h;
S107, obtaining the target flaky monocrystal with the ferroelectric domains in six-fold symmetrical vortex distribution near the indentation from the crucible.
Referring to fig. 3, fig. 3 is a magnus-type force distribution diagram induced by hexagonal lattice under random distribution vortex domain and concentrated force of the LuMnO 3 monocrystal provided by the invention. After high-temperature annealing, as shown in fig. 3a, random vortex domains and vortex-vortex pairs are formed in the LuMnO 3 monocrystal, and the hexagonal manganese oxide flaky monocrystal generates random ferroelectric vortex domains through the high-temperature annealing process. The vortex domains form a Z 2×Z3 type vortex-anti-vortex pair due to lattice distortion and trimerization. The topology protection mechanism of the six-domain vortex center is very stable and cannot be regulated and controlled by a common external electric field. Referring to fig. 3b, in the present embodiment, concentrated stress distribution is introduced on the surface of the single crystal by nanoindentation obtained by finite element simulation, and the introduced stress and interaction energy between the vortex center and the anti-vortex center of the surface of the single crystal are as shown in the following formula (1):
Wherein, (x V,yV),(xA,yA) is the Cartesian coordinates of the vortex center and the anti-vortex center, respectively; epsilon ij is the strain tensor; λ is the energy coupling coefficient; h is the thickness of the hexagonal manganese oxide flake single crystal. The magnus-type force applied to the center of the vortex and the center of the anti-vortex can be obtained by differentiating the cartesian coordinates of the center of the vortex and the center of the anti-vortex as shown in the following formula (2):
Wherein, (x V,yV),(xA,yA) is the Cartesian coordinates of the vortex center and the anti-vortex center, respectively; epsilon ij is the strain tensor; λ is the energy coupling coefficient; h is the thickness of the hexagonal manganese oxide flake single crystal.
Magnus-type forces on the scroll center and the anti-scroll center pull the scroll center and the anti-scroll center away from each other. Referring to the magnus-type force distribution around the nanoindentation shown in fig. 3c to 3d, it can be seen visually that the magnus-type force distribution exhibits alternating triple symmetry, which divides the area around the indentation into six areas. As shown by the black and grey dashed arrows in fig. 3d, these six areas are separated by six main directions of radial magnus-type forces, which are mainly distributed along a tangent line, and under the action of the magnus-type forces, a movement process of the vortex center and the anti-vortex center of six-fold symmetrical distribution is formed. Referring to fig. 4, fig. 4 is a schematic diagram showing formation and evolution of six-fold symmetric vortex domain distribution of a LuMnO 3 single crystal provided by the invention, wherein the movement of a vortex center and a non-vortex center under the action of magnus type force is shown in fig. 4a, the vortex center and the non-vortex center are alternately gathered and arranged near six main radial directions of magnus type force under the action of tangential magnus type force, 1, 3 and 5 are the non-vortex centers, and 2, 4 and 6 are the vortex centers. While the primary component of the magnus-type force in the primary direction is radial, resulting in the local or anti-vortex center being far from or near the indentation in six primary directions. Finally, under the simultaneous action of tangential and radial magnus type forces, the vortex center and the anti-vortex center move in opposite directions to form six-fold symmetrical domain distribution. The six-fold symmetrical domain distribution of the pressure head under different evolution time is obtained through the phase field simulation as shown in fig. 4b to 4e, the evolution process of the vortex center is shown, and the movement directions of the vortex center and the anti-vortex center are opposite. As shown in fig. 4f, the finite element simulation also demonstrates that the hexagonal lattice induces a magnus-type force distribution that is triplet symmetrical under the concentrated forces generated by the nanoindentation.
Alternatively, in the step S101 of this embodiment, the chemical formula of the hexagonal manganese oxide sheet single crystal is RMnO 3, R may be any one element of Er element, Y element, lu element, ho element, tm element or Yb element, and it may be understood that, by the above steps S101 to S107, the original sheet single crystal and the target sheet single crystal obtained are both hexagonal manganese oxide sheet single crystals, the chemical formula is RMnO 3, and R may be any one element of Er element, Y element, lu element, ho element, tm element or Yb element; thus, the present embodiment has a wide range of applications, and various types of hexagonal manganese oxide sheet single crystals can be used.
Optionally, the polycrystalline powder is RMnO 3 polycrystalline powder, where R may be any one element of Er element, Y element, lu element, ho element, tm element, or Yb element.
In order to illustrate the effect of six-fold symmetrical vortex type distribution of the ferroelectric domains of the target lamellar single crystal prepared in example 1 near the indentation, a relevant observation test is carried out on the effect of the ferroelectric domains of the target lamellar single crystal after the heat treatment is completed, the test result is shown in fig. 2, and fig. 2 is a microscope image of six-fold symmetrical vortex type distribution of the ferroelectric domains of the LuMnO 3 single crystal near the indentation, and the test method is as follows:
s108, obtaining a target flaky single crystal from the crucible, and performing relevant observation test on ferroelectric domain distribution effect of the target flaky single crystal after heat treatment;
S1081, soaking a target flaky single crystal in phosphoric acid, heating to 210 ℃, preserving heat for 1 hour, then cooling to room temperature, taking out the target flaky single crystal, cleaning with alcohol, wiping, and observing under an optical microscope to obtain a six-fold symmetrical vortex distribution of ferroelectric domains of the target flaky single crystal near an indentation;
s1082, scanning the target flaky monocrystal near the indentation by using a piezoelectric microscope PFM, and observing by using the piezoelectric microscope PFM to obtain that ferroelectric domains of the target flaky monocrystal are distributed in a six-fold symmetrical vortex mode near the indentation.
In order to illustrate the beneficial technical effects of the target lamellar single crystal with the ferroelectric domains distributed in the six-fold symmetric vortex near the indentation of the target lamellar single crystal prepared in example 1, nano indentation experiments are carried out on the target lamellar single crystal after the heat treatment is completed under different loading forces, the test results are shown in fig. 5, fig. 5 is the distribution diagram of the LuMnO 3 single crystal with the six-fold symmetric vortex in different loading and pressing directions, wherein, referring to fig. 5a to 5b, fig. 5a is the optical microscope photographs of the vortex domains, fig. 5b is the relationship between the orientation of the six-fold symmetric domains and the shape of the LuMnO 3 single crystal, the results prove that the LuMnO 3 single crystal with the six-fold symmetric vortex in different loading and pressing directions, and in combination with fig. 5c to 5e, six-fold symmetric domain distributions under 50mN, 100mN and 400mN, respectively, i.e., nano-indentation experiments showing that the nano-indentation experiments under different loading forces confirm good reproducibility, and in combination with fig. 6, fig. 6 is a density map of the six-fold symmetric vortex domain of the LuMnO 3 single crystal provided by the present invention under different loading, wherein as shown in fig. 6a to 6c, AFM scan images of the six-fold symmetric domain after chemical etching under 50mN, 100mN and 400mN, respectively, and as shown in fig. 6d to 6f, respectively, height change maps of the same length line segments in fig. 6a to 6c, also demonstrate that the periodicity of domain distribution decreases with increasing mechanical load. Notably, even though the indenter is pressed into the single crystal surface in random arbitrary directions, the direction of creating six-fold symmetry is uniform, highlighting the nano-indentation induced strain profile coupled with the hexagonal lattice. And carrying out nanoindentation experiments on the target flaky monocrystal subjected to heat treatment under different pressure heads, wherein the test results are shown in fig. 7, fig. 7 is six-fold symmetrical vortex domain distribution induced by different pressure heads of the LuMnO 3 monocrystal provided by the invention, wherein fig. 7a is six-fold symmetrical domain distribution induced by a Bosch pressure head, fig. 7b is six-fold symmetrical domain distribution induced by a Bosch pressure head in a phase field simulation, fig. 7c is six-fold symmetrical domain distribution induced by a spherical pressure head, fig. 7d is six-fold symmetrical domain distribution induced by a spherical pressure head in a phase field simulation, and the shape symmetry of the pressure head is excluded from being related to the six-fold symmetrical domain distribution by comparing the same nanoindentation experiments of the spherical pressure head and the Bosch pressure head with the phase field simulation results of different pressure heads. Therefore, by a mechanism of introducing stress by nano indentation, stress/strain is introduced into the hexagonal manganese oxide flaky monocrystal by the nano indentation at room temperature, and compared with the current method of applying strain by placing an aluminum rod at a high temperature, the method is safer and more convenient to operate. Meanwhile, the nano indentation can manually control the parameters such as the load of the indentation, the moving direction of the pressure head, the moving distance of the pressure head and the like, can regulate and control the ferroelectric domains of the hexagonal manganese oxide flaky monocrystal to be in six-fold symmetrical vortex type distribution, paves a road for the application of domain wall-based micro-nano electronic devices, can be applied to other perovskite ferroelectric material systems, and provides a brand-new means and degree of freedom for regulating and controlling the ferroelectric domains and domain walls.
Example 2
Referring to fig. 8, fig. 8 is a flowchart of a method for controlling a topological ferroelectric domain configuration by nano scratches, which includes the following steps:
s201, the target raw material comprises an original flaky single crystal and a substrate, wherein the original flaky single crystal is fixed on the substrate through an adhesive;
S202, pressing a nano pressure head into a second surface of an original flaky single crystal under a second load, and moving along a direction parallel to a plane where the second surface is positioned to form a first scratch, wherein the second surface is a surface of the original flaky single crystal, which is far away from the substrate side;
S203, transferring the target raw material with the first scratch to a heating table, and heating the heating table to 80-120 ℃ from room temperature according to the heating speed of 60-120 ℃ per hour to separate the original flaky monocrystal from the substrate;
S204, transferring the original flaky single crystal into a crucible, embedding the original flaky single crystal by using polycrystalline powder, and placing the crucible in a box-type furnace;
S205, raising the temperature in the box furnace from room temperature to 1450-1500 ℃ according to the heating rate of 120-180 ℃/h, and preserving the temperature at 1450-1500 ℃ for 5-10 min to perform heat treatment on the original flaky single crystal;
s206, recovering the temperature in the box-type furnace from 1450-1500 ℃ to room temperature according to the cooling speed of 150-200 ℃/h;
s207, obtaining a target flaky single crystal from the crucible, wherein ferroelectric domains of the target flaky single crystal are distributed in a high-density stripe manner on two sides of the first scratch.
Specifically, the method for regulating and controlling topological ferroelectric domain configuration through nano scratches provided in the embodiment comprises the following steps:
s201, selecting a target raw material according to elements contained in a hexagonal manganese oxide flaky single crystal, wherein the target raw material comprises an original flaky single crystal and a substrate, and the original flaky single crystal is fixed on the substrate through an adhesive;
Alternatively, the adhesive may be 502 glue, AB glue or thermosetting resin, but is not limited thereto, and no matter what material is used, it is only required that the original sheet-like single crystal can be fixed on the substrate.
Optionally, the substrate is an iron sheet, a silicon wafer, a glass slide, a zirconia ceramic sheet or a silicon nitride ceramic sheet, but is not limited to the above, and no matter what material is adopted, only the surface smoothness of the substrate is required.
S202, pressing a nano pressure head on a nano indentation instrument into a second surface of the original flaky single crystal by adopting the nano pressure head on the nano indentation instrument under a second load, and linearly moving along a direction parallel to a plane where the second surface is positioned to form a first scratch, wherein the second surface is a surface of the original flaky single crystal, which is far away from one side of a substrate, and then lifting the pressure head and leaving the pressure head from the target raw material;
Optionally, the pressure head is any one of a glass pressure head, a spherical pressure head or a conical pressure head, and the shape and size of the pressure head are not particularly limited herein.
Alternatively, the second load is 50mN to 100mN, for example 50mN, 60mN, 70mN, 80mN, 100mN, etc.
Alternatively, the nanoindenter may be replaced with other instruments, such as an atomic force microscope, a diamond glass knife, and the like.
Alternatively, the first scratch length is 100 μm to 1000 μm, e.g. 100 μm, 300 μm, 500 μm, 800 μm, 1000 μm.
S203, transferring the target raw material with the first scratch obtained in the step S202 to a heating table, heating the temperature of the heating table to 80-120 ℃ from room temperature according to a heating speed of 60-120 ℃/h, removing the binder, such as 80 ℃, 90 ℃, 100 ℃, 110 ℃, 120 ℃ and the like, separating the original flaky single crystal from the substrate and taking down the original flaky single crystal;
S204, transferring the original flaky monocrystal obtained in the step S203 into a crucible, embedding the original flaky monocrystal by using polycrystalline powder, and placing the crucible into a box-type furnace;
Alternatively, the crucible is an alumina crucible.
S205, raising the temperature in the box-type furnace in the step S204 from room temperature to 1450-1500 ℃ according to the heating speed of 120-180 ℃/h, and preserving the temperature at 1450-1500 ℃ for 5-10 min, such as 1450-1465 ℃, 1475 ℃, 1485 ℃, 1500 ℃ and the like, and performing heat treatment on the original flaky single crystal;
s206, recovering the temperature in the box-type furnace from 1450-1500 ℃ to room temperature according to the cooling speed of 150-200 ℃/h;
s207, obtaining target flaky monocrystal with ferroelectric domains distributed in high-density stripes on two sides of the scratch from a crucible.
Alternatively, in this embodiment, in the foregoing step S201, the chemical formula of the hexagonal manganese oxide sheet single crystal is RMnO 3, R may be any one element of Er element, Y element, lu element, ho element, tm element, or Yb element, and it may also be understood that, in the foregoing steps S201 to S207, the original sheet single crystal and the target sheet single crystal obtained are both hexagonal manganese oxide sheet single crystals, the chemical formula is RMnO 3, and R may be any one element of Er element, Y element, lu element, ho element, tm element, or Yb element; thus, the present embodiment has a wide range of applications, and various types of hexagonal manganese oxide sheet single crystals can be used.
Optionally, the polycrystalline powder is RMnO 3 polycrystalline powder, where R may be any one element of Er element, Y element, lu element, ho element, tm element, or Yb element.
In order to illustrate the effect of the ferroelectric domains of the target flaky monocrystal manufactured in the embodiment 2 on the distribution of the ferroelectric domains on both sides of the first scratch in a high-density stripe manner, a relevant observation test is carried out on the effect of the ferroelectric domains of the target flaky monocrystal after the heat treatment is completed, the test result is shown in fig. 9, and fig. 9 is a microscopic image of the ferroelectric domains of the LuMnO 3 monocrystal provided by the invention on the distribution of the ferroelectric domains of the target flaky monocrystal in a high-density stripe manner near the scratch, and the test method is as follows:
S208, obtaining a target flaky single crystal from the crucible, and performing relevant observation test on ferroelectric domain distribution effect of the target flaky single crystal after heat treatment;
s2081, soaking a target flaky single crystal in phosphoric acid, heating to 210 ℃, preserving heat for 1 hour, then cooling to room temperature, taking out the target flaky single crystal, cleaning with alcohol, wiping, and observing under an optical microscope to obtain that ferroelectric domains of the target flaky single crystal are distributed in high-density stripes on two sides of a first scratch;
S2082, scanning the target flaky monocrystal near the indentation by using a piezoelectric microscope PFM, and observing by using the piezoelectric microscope PFM to obtain the ferroelectric domains of the target flaky monocrystal, wherein the ferroelectric domains are distributed in high-density stripes on two sides of the first scratch.
In order to create a relatively large strain distribution range, the indenter is moved in a certain direction under a constant mechanical load to realize nano scratches. Referring to fig. 12, fig. 12 is a graph showing a distribution of large-area high-density striped domains generated by nano scratch control of a LuMnO 3 single crystal provided by the present invention, referring to fig. 12a to 12d, fig. 12a is a starting point region of high-density striped domains generated by nano scratch control, fig. 12b is a schematic drawing of nano scratch generation, fig. 12c is an end point region of high-density striped domains generated by nano scratch control, and fig. 12d is a high-density striped domain generated by nano scratch control, and nano scratches are obtained by the same annealing process. The movement of the vortex center and the anti-vortex center can be analyzed in a graphical manner, and as shown in fig. 12e, the nano scratches regulate the movement process of the vortex center and the anti-vortex center, and the six-fold symmetric domain distribution of the nano scratch start points is consistent with the six-fold symmetric domain distribution of the nano indentations. As the ram moves, the three primary directions (6,1,2) induced strain is gradually reconstructed from the (5, 4, 3) induced strain. As a result, the single nano scratches as shown in fig. 12f regulate the distribution of the vortex center and the anti-vortex center, and high-density stripes forming an included angle of 120 ° with the nano scratches direction are formed due to the reverse movement of the tangential magnus force driving the vortex center and the anti-vortex center. At the end point, another six-fold symmetric domain distribution is left as it is not affected by the hysteresis magnus-type force, with the vortex center gathering near the first scratch and the anti-vortex center being pushed away. Therefore, the stress/strain is introduced into the hexagonal manganese oxide flaky monocrystal through the mechanism of introducing the stress by the nano scratches, and compared with the current method of applying the strain by placing the aluminum rod at a high temperature, the method is safer and more convenient to operate. Meanwhile, the nano scratches can manually control the parameters such as the load of the scratches, the moving direction of the pressure head, the moving distance of the pressure head and the like, and can enable ferroelectric domains of hexagonal manganese oxide flaky single crystals to be distributed in high-density stripes on two sides of the first scratches, so that a road is paved for realizing the application of domain wall-based micro-nano electronic devices, and meanwhile, the nano scratches can be applied to other perovskite ferroelectric material systems, and brand-new means and degrees of freedom are provided for the regulation and control of ferroelectric domains and domain walls.
Example 3
Referring to fig. 10, fig. 10 is a flowchart of another method for controlling a topological ferroelectric domain configuration by nano scratches according to the present invention, the method for controlling a topological ferroelectric domain configuration by nano scratches according to the present invention includes the following steps:
S301, the target raw material comprises an original flaky single crystal and a substrate, wherein the original flaky single crystal is fixed on the substrate through an adhesive;
S302, pressing the nano pressure head into the second surface of the original flaky single crystal under a second load and moving along the direction parallel to the plane where the second surface is positioned to form a first scratch, and pressing the nano pressure head into the second surface of the original flaky single crystal under the second load and moving along the direction parallel to the direction opposite to the first scratch to form a second scratch; the second surface is the surface of the original flaky monocrystal, which is far away from one side of the substrate;
s303, transferring the target raw material with the first scratch and the second scratch to a heating table, and heating the heating table to 80-120 ℃ from room temperature according to the heating speed of 60-120 ℃ per hour to separate the original flaky monocrystal from the substrate;
S304, transferring the original flaky single crystal into a crucible, embedding the original flaky single crystal by using polycrystalline powder, and placing the crucible in a box-type furnace;
s305, raising the temperature in the box furnace from room temperature to 1450-1500 ℃ according to the heating rate of 120-180 ℃/h, and preserving the temperature at 1450-1500 ℃ for 5-10 min, so as to perform heat treatment on the original flaky single crystal;
s306, recovering the temperature in the box-type furnace from 1450 ℃ to 1500 ℃ to room temperature according to the cooling speed of 150 ℃/h to 200 ℃/h;
s307, obtaining a target flaky single crystal from the crucible, wherein ferroelectric domains of the target flaky single crystal are distributed in high-density parallel stripes between the first scratch and the second scratch.
Specifically, the method for regulating and controlling topological ferroelectric domain configuration through nano scratches provided in the embodiment comprises the following steps:
s301, selecting a target raw material according to elements contained in a hexagonal manganese oxide flaky single crystal, wherein the target raw material comprises an original flaky single crystal and a substrate, and the original flaky single crystal is fixed on the substrate through an adhesive;
Alternatively, the adhesive may be 502 glue, AB glue or thermosetting resin, but is not limited thereto, and no matter what material is used, it is only required that the original sheet-like single crystal can be fixed on the substrate.
Optionally, the substrate is an iron sheet, a silicon wafer, a glass slide, a zirconia ceramic sheet or a silicon nitride ceramic sheet, but is not limited to the above, and no matter what material is adopted, only the surface smoothness of the substrate is required.
S302, pressing a nano pressure head on a nano indentation instrument into a second surface of an original flaky single crystal under a second load by using the target raw material obtained in the step S301, linearly moving the nano pressure head in a direction parallel to a plane where the second surface is positioned to form a first scratch, pressing the same nano pressure head into the second surface of the original flaky single crystal under the same load, moving the same nano pressure head in a direction parallel to a direction opposite to the first scratch to form a second scratch, and then lifting the pressure head and leaving the pressure head from the target raw material;
Optionally, the pressure head is any one of a glass pressure head, a spherical pressure head or a conical pressure head, and the shape and size of the pressure head are not particularly limited herein.
Alternatively, the second load is 50mN to 100mN, for example 50mN, 60mN, 70mN, 80mN, 100mN, etc.
Alternatively, the nanoindenter may be replaced with other instruments, such as an atomic force microscope, a diamond glass knife, and the like.
Alternatively, the first scratch length and the second scratch length are each 100 μm to 1000 μm, e.g. 100 μm, 300 μm, 500 μm, 800 μm, 1000 μm; the first and second scratches may have a pitch of 30 μm to 60 μm, for example, 30 μm, 40 μm, 45 μm, 50 μm, or 60 μm.
S303, transferring the target raw material with the first scratch and the second scratch obtained in the step S302 to a heating table, heating the temperature of the heating table to 80-120 ℃ from room temperature according to a heating speed of 60-120 ℃/h, removing the binder, such as 80 ℃, 90 ℃,100 ℃, 110 ℃, 120 ℃ and the like, separating the original flaky single crystal from the substrate and taking down the original flaky single crystal;
S304, transferring the original flaky monocrystal obtained in the step S303 into a crucible, embedding the original flaky monocrystal by using polycrystalline powder, and placing the crucible into a box-type furnace;
Alternatively, the crucible is an alumina crucible.
S305, raising the temperature in the box-type furnace in the step S304 from room temperature to 1450-1500 ℃ according to the heating speed of 120-180 ℃/h, and preserving the temperature at 1450-1500 ℃ for 5-10 min, such as 1450-1465 ℃, 1475 ℃, 1485 ℃, 1500 ℃ and the like, and performing heat treatment on the original flaky single crystal;
s306, recovering the temperature in the box-type furnace from 1450 ℃ to 1500 ℃ to room temperature according to the cooling speed of 150 ℃/h to 200 ℃/h;
s307, obtaining the target flaky monocrystal with ferroelectric domains distributed in high-density parallel stripes between the first scratch and the second scratch from the crucible.
Alternatively, in this embodiment, in the foregoing step S301, the chemical formula of the hexagonal manganese oxide sheet single crystal is RMnO 3, R may be any one element of Er element, Y element, lu element, ho element, tm element, or Yb element, and it may also be understood that, in the foregoing steps S301 to S307, the original sheet single crystal and the target sheet single crystal obtained are both hexagonal manganese oxide sheet single crystals, the chemical formula is RMnO 3, and R may be any one element of Er element, Y element, lu element, ho element, tm element, or Yb element; thus, the present embodiment has a wide range of applications, and various types of hexagonal manganese oxide sheet single crystals can be used.
Optionally, the polycrystalline powder is RMnO 3 polycrystalline powder, where R may be any one element of Er element, Y element, lu element, ho element, tm element, or Yb element.
In order to illustrate the effect of the ferroelectric domains of the target flaky monocrystal manufactured in example 3 in the form of high-density parallel stripes between the first scratch and the second scratch, the ferroelectric domains of the target flaky monocrystal after the heat treatment are subjected to relevant observation test, the test result is shown in fig. 11, and fig. 11 is a microscopic image of the ferroelectric domains of the LuMnO 3 monocrystal provided by the invention in the form of high-density parallel stripes near the scratches, and the test method is as follows:
S308, obtaining a target flaky single crystal from a crucible, and performing relevant observation test on ferroelectric domain distribution effect of the target flaky single crystal after heat treatment;
S3081, soaking a target flaky single crystal in phosphoric acid, heating to 210 ℃, preserving heat for 1 hour, cooling to room temperature, taking out the target flaky single crystal, cleaning with alcohol, wiping, and observing under an optical microscope to obtain the ferroelectric domains of the target flaky single crystal which are distributed in high-density parallel stripes between a first scratch and a second scratch;
S3082, scanning the target flaky monocrystal near the indentation by using a piezoelectric microscope PFM, and observing by using the piezoelectric microscope PFM to obtain the ferroelectric domains of the target flaky monocrystal, wherein the ferroelectric domains are distributed in high-density parallel stripes between the first scratch and the second scratch.
Based on the mechanism that the vortex domain is in six-fold symmetrical distribution under the control of the nano indentation, the nano scratch is realized by moving the pressure head along a certain direction under a constant mechanical load in order to create a relatively large strain distribution range. The nano scratches as shown in fig. 12e regulate the movement process of the vortex center and the anti-vortex center, and the movement of the vortex center and the anti-vortex center can be analyzed in a graphic manner. The six-fold symmetric domain distribution of the nanometer scratch starting point is consistent with the six-fold symmetric domain distribution of the nanometer indentation. As the ram moves, the three primary directions (6,1,2) induced strain is gradually reconstructed from the (5, 4, 3) induced strain. On the basis of single scratch, under the action of applying a nano scratch again in the anti-parallel direction, the nano scratch is subjected to the same annealing process to obtain a high-density parallel stripe domain, the gathering positions of a vortex center and a non-vortex center are shown in figure 13, figure 13 shows that the nano scratch regulation of the LuMnO 3 monocrystal provided by the invention generates a large-area high-density parallel stripe domain distribution diagram, for double-parallel reverse scratch, the vortex center and the non-vortex center are gathered near the first scratch and the second scratch respectively, and the ferroelectric domain is distributed in the form of high-density parallel stripe between the first scratch and the second scratch, and the experimental result of figure 11 also proves the mechanism. Therefore, the stress/strain is introduced into the hexagonal manganese oxide flaky monocrystal through the mechanism of introducing the stress by the nano scratches, and compared with the current method of applying the strain by placing the aluminum rod at a high temperature, the method is safer and more convenient to operate. Meanwhile, the nano scratches can manually control the parameters such as the load of the scratches, the moving direction of the pressure head, the moving distance of the pressure head and the like, and can enable ferroelectric domains of hexagonal manganese oxide flaky single crystals to be distributed in high-density parallel stripes on two sides of the first scratches, so that a road is paved for realizing the application of domain wall-based micro-nano electronic devices, and meanwhile, the nano scratches can be applied to other perovskite ferroelectric material systems, and brand-new means and degrees of freedom are provided for the regulation and control of ferroelectric domains and domain walls.
According to the embodiment, the method for regulating and controlling the topological ferroelectric domain configuration through nano indentation/scratch provided by the invention has the following beneficial effects:
According to the method for regulating and controlling the topological ferroelectric domain configuration through the nano-indentation/scratch, stress/strain is introduced into the hexagonal manganese oxide flaky monocrystal through the nano-indentation/scratch at room temperature, and compared with the existing method for applying strain through placing an aluminum rod at a high temperature, the method is safer and more convenient to operate. Meanwhile, the nano indentation/scratch can manually control the load size of the indentation/scratch, the moving direction of the pressure head, the moving distance of the pressure head and other parameters, can regulate and control the ferroelectric domain of the hexagonal manganese oxide flaky monocrystal to be in six-fold symmetrical vortex type distribution or high-density stripe type distribution, paves the way for realizing the application of domain wall base micro-nano electronic devices, can be applied to other perovskite ferroelectric material systems at the same time, and provides brand-new means and degree of freedom for regulating and controlling the ferroelectric domain and domain wall.
While certain specific embodiments of the invention have been described in detail by way of example, it will be appreciated by those skilled in the art that the above examples are for illustration only and are not intended to limit the scope of the invention. It will be appreciated by those skilled in the art that modifications may be made to the above embodiments without departing from the scope and spirit of the invention. The scope of the invention is defined by the appended claims.
Claims (9)
1. A method for regulating and controlling topological ferroelectric domain configuration by nano indentation/scratch, which is characterized in that: the target raw material includes a raw sheet-like single crystal and a substrate, the raw sheet-like single crystal being fixed to the substrate by an adhesive;
Pressing a first surface of the original flaky single crystal into the substrate by adopting a nanometer pressure head under a first load to form an indentation, wherein the first surface is the surface of one side of the original flaky single crystal away from the substrate;
transferring the target raw material with the indentation to a heating table, wherein the temperature of the heating table is raised to 80-120 ℃ from room temperature according to the heating speed of 60-120 ℃ per hour, and separating the original flaky single crystal from the substrate;
transferring the original flaky single crystal into a crucible, embedding the original flaky single crystal by polycrystalline powder, and placing the crucible into a box-type furnace;
Raising the temperature in the box furnace from room temperature to 1450-1500 ℃ according to the heating rate of 120-180 ℃/h, and preserving the temperature at 1450-1500 ℃ for 5-10 min to perform heat treatment on the original flaky single crystal;
Recovering the temperature in the box furnace from 1450-1500 ℃ to room temperature according to the cooling speed of 150-200 ℃/h, and obtaining a target flaky monocrystal from the crucible, wherein ferroelectric domains of the target flaky monocrystal are distributed in a six-fold symmetrical vortex manner near the indentation;
The original flaky single crystal and the target flaky single crystal are hexagonal manganese oxide flaky single crystals, and the chemical formula of the hexagonal manganese oxide flaky single crystals is RMnO 3, wherein R is any element of Er, Y, lu, ho, tm or Yb; the polycrystalline powder is RMnO 3 polycrystalline powder, wherein R is any one element of Er, Y, lu, ho, tm or Yb.
2. A method of controlling topological ferroelectric domain configuration by nano-indentation/scoring as claimed in claim 1, wherein: the first load is 50 mN-400 mN.
3. A method for regulating and controlling topological ferroelectric domain configuration by nano indentation/scratch, which is characterized in that: the target raw material includes a raw sheet-like single crystal and a substrate, the raw sheet-like single crystal being fixed to the substrate by an adhesive;
Pressing the nano pressure head into a second surface of the original flaky monocrystal under a second load, and moving the nano pressure head along a direction parallel to a plane where the second surface is positioned to form a first scratch, wherein the second surface is a surface of the original flaky monocrystal, which is far away from one side of the substrate;
Transferring the target raw material with the first scratch to a heating table, wherein the temperature of the heating table is increased from room temperature to 80-120 ℃ according to the heating speed of 60-120 ℃/h, and separating the original flaky monocrystal from the substrate;
transferring the original flaky single crystal into a crucible, embedding the original flaky single crystal by polycrystalline powder, and placing the crucible into a box-type furnace;
Raising the temperature in the box furnace from room temperature to 1450-1500 ℃ according to the heating rate of 120-180 ℃/h, and preserving the temperature at 1450-1500 ℃ for 5-10 min to perform heat treatment on the original flaky single crystal;
Recovering the temperature in the box furnace from 1450-1500 ℃ to room temperature according to the cooling speed of 150-200 ℃/h, and obtaining target flaky single crystals from the crucible, wherein ferroelectric domains of the target flaky single crystals are distributed in high-density stripes on two sides of the first scratch;
The original flaky single crystal and the target flaky single crystal are hexagonal manganese oxide flaky single crystals, and the chemical formula of the hexagonal manganese oxide flaky single crystals is RMnO 3, wherein R is any element of Er, Y, lu, ho, tm or Yb; the polycrystalline powder is RMnO 3 polycrystalline powder, wherein R is any one element of Er, Y, lu, ho, tm or Yb.
4. A method of controlling topological ferroelectric domain configuration by nano-indentation/scoring as claimed in claim 3, wherein: pressing the second surface of the original flaky monocrystal under the second load by adopting a nanometer pressure head, and moving in a direction parallel to and opposite to the first scratch to form a second scratch;
Transferring the target raw material having the first scratch and the second scratch to a heating table, wherein the temperature of the heating table is raised to 80-120 ℃ from room temperature according to a heating rate of 60-120 ℃/h, and separating the original flaky single crystal from the substrate;
transferring the original flaky single crystal into a crucible, embedding the original flaky single crystal by polycrystalline powder, and placing the crucible into a box-type furnace;
Raising the temperature in the box furnace from room temperature to 1450-1500 ℃ according to the heating rate of 120-180 ℃/h, and preserving the temperature at 1450-1500 ℃ for 5-10 min to perform heat treatment on the original flaky single crystal;
And recovering the temperature in the box furnace from 1450-1500 ℃ to room temperature according to the cooling speed of 150-200 ℃/h, and obtaining the target flaky monocrystal from the crucible, wherein ferroelectric domains of the target flaky monocrystal are distributed in high-density parallel stripes between the first scratches and the second scratches.
5. The method for controlling topological ferroelectric domain configuration by nano-indentation/scratch according to claim 4, wherein: the second load is 50 mN-100 mN.
6. The method for controlling topological ferroelectric domain configuration by nano-indentation/scratch according to claim 4, wherein: the length of the first scratch and the second scratch is 100-1000 mu m, and the distance between the first scratch and the second scratch is 30-60 mu m.
7. A method of controlling topological ferroelectric domain configuration by nano-indentation/scoring as claimed in claim 1 or 3, characterized in that: the pressure head is any one of a Boss pressure head, a spherical pressure head or a conical pressure head.
8. A method of controlling topological ferroelectric domain configuration by nano-indentation/scoring as claimed in claim 1 or 3, characterized in that: the substrate is an iron sheet, a silicon wafer, a glass slide, a zirconia ceramic sheet or a silicon nitride ceramic sheet; the binder is glue or thermosetting resin.
9. A target platelet-shaped single crystal produced by a method of nano-indentation/scratch modulation topological ferroelectric domain configuration according to claim 1 or 3, characterized in that: the ferroelectric domains of the target flaky monocrystal are distributed in a six-fold symmetrical vortex type or high-density stripe type mode.
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| US6353495B1 (en) * | 1998-08-18 | 2002-03-05 | Matsushita Electric Industrial Co., Ltd. | Method for forming a ferroelectric domain-inverted structure |
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| CN113388892A (en) * | 2021-05-18 | 2021-09-14 | 西安交通大学 | Method for preparing lead magnesium niobate titanate optical waveguide by titanium diffusion |
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| US6353495B1 (en) * | 1998-08-18 | 2002-03-05 | Matsushita Electric Industrial Co., Ltd. | Method for forming a ferroelectric domain-inverted structure |
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