CN118326364A - Preparation method of polarized semen cassiae ferroelectric material - Google Patents
Preparation method of polarized semen cassiae ferroelectric material Download PDFInfo
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- CN118326364A CN118326364A CN202410763157.3A CN202410763157A CN118326364A CN 118326364 A CN118326364 A CN 118326364A CN 202410763157 A CN202410763157 A CN 202410763157A CN 118326364 A CN118326364 A CN 118326364A
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- 239000000463 material Substances 0.000 title claims abstract description 118
- 210000000582 semen Anatomy 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 47
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000002245 particle Substances 0.000 claims abstract description 27
- 229910052802 copper Inorganic materials 0.000 claims abstract description 17
- 239000010949 copper Substances 0.000 claims abstract description 17
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 15
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052738 indium Inorganic materials 0.000 claims abstract description 15
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 15
- 239000011574 phosphorus Substances 0.000 claims abstract description 15
- 230000015654 memory Effects 0.000 claims abstract description 7
- 230000005540 biological transmission Effects 0.000 claims abstract description 5
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 4
- 239000011593 sulfur Substances 0.000 claims abstract description 4
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical group [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 229910052740 iodine Inorganic materials 0.000 claims description 13
- 239000011630 iodine Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 4
- 239000003708 ampul Substances 0.000 description 63
- 239000010453 quartz Substances 0.000 description 63
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 63
- 206010040844 Skin exfoliation Diseases 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- 244000037364 Cinnamomum aromaticum Species 0.000 description 10
- 235000014489 Cinnamomum aromaticum Nutrition 0.000 description 10
- 238000001816 cooling Methods 0.000 description 10
- 239000002243 precursor Substances 0.000 description 10
- 239000002390 adhesive tape Substances 0.000 description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 229910052710 silicon Inorganic materials 0.000 description 8
- 239000010703 silicon Substances 0.000 description 8
- 239000000758 substrate Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
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- HACVPBPJHIPGHT-UHFFFAOYSA-K P(=S)([O-])([O-])[O-].[In+3].[Cu+2] Chemical compound P(=S)([O-])([O-])[O-].[In+3].[Cu+2] HACVPBPJHIPGHT-UHFFFAOYSA-K 0.000 description 3
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- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a preparation method of a polarized semen cassiae ferroelectric material, which comprises the following steps: and (3) growing a copper source, an indium source, a phosphorus source and a sulfur source in a molar ratio of (1.3-2) to (1:2:6) under the conditions of heating and gas phase transmission medium to obtain the polarized spinelle seed ferroelectric material, wherein the particle size of the copper source is 50-200 nm. The polarized Sjog-seed ferroelectric material prepared by the preparation method has a stable spontaneously formed polarized Sjog-seed structure, can be widely applied to the fields of memories, logic operation and the like, has a simple preparation process, and can be industrially produced.
Description
Technical Field
The invention relates to the technical field of polarized semen cassiae ferroelectric materials, in particular to a preparation method of a polarized semen cassiae ferroelectric material.
Background
The polarized spinodal is a topological domain pattern which is intrinsically embedded in ferroelectric materials, is favorable for realizing high-density information storage, has rich physical characteristics (such as negative dielectric constant, chirality and the like), has wide device application prospect (such as ultra-high density memristors exceeding one gigabit per square inch), and provides a brand new platform for researching the emerging nanoscale topological structure and the polarity property thereof. Recently, researchers have observed polarized cassia seeds in the form of particles in oxide ferroelectric superlattices, but current research has shown that such polarized cassia seeds need to exist stably depending on a delicate balance between elastic energy, electrostatic energy, and gradient energy.
Copper indium thiophosphate (CuInP 2S6) is used as a ferroelectric material, has the advantages of atomic-level thickness, passivation surface without dangling bonds, convenient integration with other material systems without lattice matching, and the like, is favorable for realizing the organic combination of semiconductor properties and nonvolatile storage characteristics on the micro-nano scale, and has great application potential in the fields of high-integration electronic devices, photoelectric devices, energy collection, electromechanical coupling systems and the like. However, due to the great challenges of controlling complex boundary conditions, the research on polarized sigma-type semen is still slow, and copper indium thiophosphate with polarized sigma-type semen structure is still not available at present.
Thus, there is a need for a method capable of preparing ferroelectric materials having a stable polarized segrain structure.
Disclosure of Invention
Based on the above, it is necessary to provide a preparation method of a polarized spinelle ferroelectric material, which has stable spontaneous polarized spinelle structure, simple preparation process, industrialized production and wide application prospect.
A method for preparing a poled segetum ferroelectric material, the method comprising the steps of:
And (3) growing a copper source, an indium source, a phosphorus source and a sulfur source in a molar ratio of (1.3-2) to (1:2:6) under the conditions of heating and gas phase transmission medium to obtain the polarized spinelle seed ferroelectric material, wherein the particle size of the copper source is 50-200 nm.
In one embodiment, the reaction device for carrying out vacuum chemical vapor transport comprises a source region and a growth region, wherein the heating temperature of the source region is 600-650 ℃, and the heating temperature of the growth region is 550-600 ℃.
In one embodiment, the vacuum pressure of the reaction device is 20mTorr to 100mTorr.
In one embodiment, the heating rate of the reaction device is 1 ℃/min to 3 ℃/min.
In one embodiment, the heating time of the reaction device is 72-120 hours.
In one embodiment, the vapor transport medium is selected from iodine vapor.
The polarized semen cassiae ferroelectric material prepared by the preparation method is provided.
In one embodiment, the atomic-level thickness of the polarized segetum ferroelectric material is 5 nm-200 nm.
In one embodiment, when the atomic-level thickness of the polarized semen cassiae ferroelectric material is more than or equal to 60nm, the polarized semen cassiae is in a rod-shaped structure.
In one embodiment, the length of the polarized semen cassiae is 50 nm-300 nm.
In one embodiment, the polarized semen is of circular structure when the atomic-level thickness of the polarized semen ferroelectric material is less than or equal to 30 nm.
In one embodiment, the diameter of the polarized semen cassiae is 10 nm-100 nm.
Use of a poled segrain ferroelectric material as described above in memory or logic operations.
According to the preparation method of the polarized semen cassiae ferroelectric material, the stoichiometric ratio and the particle size of the copper source in the raw materials are regulated, so that the saturated vapor pressure of the copper source is effectively improved, the atomic proportion of copper in the polarized semen cassiae ferroelectric material is improved, the copper defect is reduced, the tensile stress in the polarized semen cassiae ferroelectric material is improved, the stable polarized semen cassiae is facilitated, the preparation process is simple, and the preparation method is suitable for industrial production.
Therefore, the polarized spinelle ferroelectric material has stable spontaneous polarized spinelle structure, can be widely applied to the fields of memories, logic operation and the like, and has wide market prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present invention, and other drawings may be obtained according to the drawings without inventive effort to those skilled in the art.
FIG. 1 is a schematic structural diagram of a manufacturing apparatus according to the present invention, wherein a is a growth region and b is a source region;
FIG. 2 is a diagram of a polarized Gemini ferroelectric material prepared in example 1 of the present invention;
FIG. 3 is an optical microscope image of an atomic-scale thickness sample obtained after mechanical exfoliation of the polarized Szechwan ferroelectric material prepared in example 1 of the present invention;
FIG. 4 is a Raman spectrum of an atomic-scale thickness sample obtained by mechanically peeling the ferroelectric material obtained in example 1 and comparative example 1, wherein (a) is a Raman spectrum of an atomic-scale thickness sample obtained by mechanically peeling the ferroelectric material obtained in comparative example 1, and (b) is a Raman spectrum of an atomic-scale thickness sample obtained by mechanically peeling the polarized Szechwan ferroelectric material obtained in example 1;
Fig. 5 is a diagram of the internal phase of a piezoelectric microscope of an atomic-scale thickness sample obtained by mechanically peeling the polarized segetum ferroelectric material obtained in example 1 and comparative example 1, wherein (a) is a diagram of the internal phase of a piezoelectric microscope of an atomic-scale thickness sample obtained by mechanically peeling the ferroelectric material obtained in comparative example 1, and (b) is a diagram of the internal phase of a piezoelectric microscope of an atomic-scale thickness sample obtained by mechanically peeling the polarized segetum ferroelectric material obtained in example 1.
In the figure, 1, a quartz ampoule bottle; 2. a solid raw material; 3. a vapor transport medium; 4. polarizing the ferroelectric material of the cassia seed; 5. a tube furnace.
Detailed Description
The present invention will be described in more detail below in order to facilitate understanding of the present invention. It should be understood, however, that the invention may be embodied in many different forms and should not be limited to the implementations or embodiments described herein. Rather, these embodiments or examples are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments or examples only and is not intended to be limiting of the invention. As used herein, the optional scope of the term "and/or" includes any one of the two or more related listed items, as well as any and all combinations of related listed items, including any two or more of the related listed items, or all combinations of related listed items.
The invention provides a preparation method of a polarized spinelle ferroelectric material, comprising the following steps:
And (3) growing a copper source, an indium source, a phosphorus source and a sulfur source in a molar ratio of (1.3-2) to (1:2:6) under the conditions of heating and gas phase transmission medium to obtain the polarized spinelle seed ferroelectric material, wherein the particle size of the copper source is 50-200 nm.
According to the preparation method, the stoichiometric ratio and the particle size of the copper source in the raw materials are regulated, so that the saturated vapor pressure of the copper source is effectively improved, the atomic proportion of copper in the polarized semen cassiae ferroelectric material is improved, the copper defect is reduced, the tensile stress in the polarized semen cassiae ferroelectric material is further improved, and the polarized semen cassiae is stabilized; and the preparation process is simple and is suitable for industrial production.
In one embodiment, the reaction device for carrying out vacuum chemical vapor transport comprises a source region and a growth region, wherein the heating temperature of the source region is 600-650 ℃, and the heating temperature of the growth region is 550-600 ℃, so that raw materials react in the source region to generate gas-phase copper indium thiophosphate, and the polarized semen cassiae ferroelectric material is formed in the growth region by deposition, thereby being beneficial to improving the growth quality and efficiency of the polarized semen cassiae ferroelectric material.
Referring to fig. 1, a reaction apparatus for vacuum chemical vapor transport in an embodiment of the present invention includes a tube furnace 5, and a quartz ampoule 1 placed in the tube furnace 5, wherein the quartz ampoule 1 includes a source region where copper powder, indium block, phosphorus block, sulfur powder raw material 2 and a growth region where polarized segetum ferroelectric material 4 is deposited, and a reaction product in a vapor phase is transported from the source region to the growth region through a vapor phase transport medium 3 for deposition growth.
In order to further improve the growth quality and efficiency of the polarized semen cassiae ferroelectric material, the vacuum pressure of the reaction device is preferably 20 mTorr-100 mTorr.
In order to further improve the growth quality and efficiency of the polarized semen cassiae ferroelectric material, the heating rate of the reaction device is preferably 1-3 ℃/min.
In order to further improve the growth quality and efficiency of the polarized semen cassiae ferroelectric material, the heating time of the reaction device is preferably 72-120 h.
In one embodiment, the vapor transport medium is selected from iodine vapor.
In one embodiment, the cooling treatment is performed after the heating treatment, and the polarized spinelle ferroelectric material is obtained by growth.
The invention also provides the polarized semen cassiae ferroelectric material prepared by the preparation method. The polarized Stokes rule structure of the polarized Stokes rule ferroelectric material exists stably, can be widely applied to the fields of memories, logic operation and the like, and has wide market prospect.
In an embodiment, the lateral dimension of the polarized segetum ferroelectric material is 2 mm-20 mm, and the thickness of the polarized segetum ferroelectric material is not particularly limited in the invention.
It will be appreciated that the layers of the polarized stopper rod ferroelectric material are bonded by a strong covalent bond, while the layers are bonded by a weak van der waals bond, and a mechanical lift-off treatment can be performed to obtain a thinner polarized stopper rod ferroelectric material, including but not limited to an atomic thickness polarized stopper rod ferroelectric material, and the mechanical lift-off is performed by a method known in the art, which is not repeated in the present invention.
It should be noted that the thinner polarized stopper ferroelectric material obtained by the mechanical peeling treatment includes, but is not limited to, an atomic-scale thickness polarized stopper ferroelectric material, which still has a stable spontaneously formed polarized stopper structure.
In an embodiment, the atomic-scale thickness of the polarized segetum ferroelectric material is preferably 5 nm-200 nm, and the transverse dimension of the polarized segetum ferroelectric material with atomic-scale thickness is not particularly limited.
Specifically, when the atomic-level thickness of the polarized semen cassiae ferroelectric material is more than or equal to 60nm, the polarized semen cassiae is in a rod-shaped structure.
Preferably, the length of the polarized semen cassiae is 50 nm-300 nm.
Specifically, when the atomic-level thickness of the polarized semen cassiae ferroelectric material is less than or equal to 30nm, the polarized semen cassiae is in a circular structure.
Preferably, the diameter of the polarized semen cassiae is 10 nm-100 nm.
The invention also provides an application of the polarized Sjog-seed ferroelectric material in a memory or logic operation.
Hereinafter, the method for preparing the polarized segmeans ferroelectric material will be further described by the following specific examples.
Example 1
1.3Mmol of copper powder, 1mmol of indium block, 2mmol of phosphorus block and 6mmol of sulfur powder are filled into a quartz ampoule bottle, wherein the particle size of the copper powder is 50nm, and the precursors are mixed with 5g of iodine particles; the quartz ampoule is evacuated to 20mTorr and sealed with a flame; subsequently, the quartz ampoule bottle is put into a tube furnace for heating, the heating rate is 1 ℃/min, the temperature of a source area is increased to 650 ℃, the temperature of a growth area is increased to 600 ℃, and the quartz ampoule bottle is maintained at the temperature for 3 days; the tube furnace was stopped from heating, the quartz ampoule was allowed to cool naturally to room temperature, and polarized spinelle ferroelectric material was obtained on the wall of the quartz ampoule, as shown in fig. 2, with a lateral dimension of 4mm.
The polarized Szechwan cassia ferroelectric material is placed on a transparent adhesive tape for repeated pasting and peeling, so that the polarized Szechwan cassia ferroelectric material with atomic-scale thickness is obtained, the polarized Szechwan cassia ferroelectric material is transferred onto a silicon wafer substrate, the adhesive tape is slowly peeled after the adhesive tape is stationary for a period of time, and the polarized Szechwan cassia ferroelectric material with atomic-scale thickness is placed on the silicon wafer substrate, and an optical microscope diagram of the polarized Szechwan cassia ferroelectric material is shown in figure 3.
Example 2
Filling 1.6mmol of copper powder, 1mmol of indium block, 2mmol of phosphorus block and 6mmol of sulfur powder into a quartz ampoule bottle, wherein the particle size of the copper powder is 100nm, and mixing the precursors with 5g of iodine particles; the quartz ampoule is evacuated to 60mTorr and sealed with a flame; subsequently, the quartz ampoule bottle is put into a tube furnace for heating, the heating rate is 3 ℃/min, the temperature of a source area is increased to 630 ℃, the temperature of a growing area is increased to 580 ℃, and the quartz ampoule bottle is maintained at the temperature for 5 days; stopping heating the tube furnace, naturally cooling the quartz ampoule bottle to room temperature, and obtaining the polarized spinelle ferroelectric material with the transverse dimension of 3mm on the bottle wall of the quartz ampoule bottle.
Example 3
1.6Mmol of copper powder, 1mmol of indium block, 2mmol of phosphorus block and 6mmol of sulfur powder are filled into a quartz ampoule bottle, wherein the particle size of the copper powder is 200nm, and the precursors are mixed with 5g of iodine particles; the quartz ampoule is evacuated to 100mTorr and sealed with a flame; subsequently, the quartz ampoule bottle is put into a tube furnace for heating, the heating rate is 3 ℃/min, the temperature of a source area is increased to 600 ℃, the temperature of a growth area is increased to 550 ℃, and the quartz ampoule bottle is maintained at the temperature for 5 days; stopping heating the tube furnace, naturally cooling the quartz ampoule bottle to room temperature, and obtaining the polarized spinelle ferroelectric material with the transverse dimension of 3.5mm on the bottle wall of the quartz ampoule bottle.
Example 4
Filling 2mmol of copper powder, 1mmol of indium block, 2mmol of phosphorus block and 6mmol of sulfur powder into a quartz ampoule bottle, wherein the particle size of the copper powder is 50nm, and mixing the precursors with 5g of iodine particles; the quartz ampoule is evacuated to 20mTorr and sealed with a flame; subsequently, the quartz ampoule bottle is put into a tube furnace for heating, the heating rate is 3 ℃/min, the temperature of a source area is increased to 650 ℃, the temperature of a growth area is increased to 550 ℃, and the quartz ampoule bottle is maintained at the temperature for 3 days; stopping heating the tube furnace, naturally cooling the quartz ampoule bottle to room temperature, and obtaining the polarized spinelle ferroelectric material with the transverse dimension of 4mm on the bottle wall of the quartz ampoule bottle.
Example 5
Filling 2mmol of copper powder, 1mmol of indium block, 2mmol of phosphorus block and 6mmol of sulfur powder into a quartz ampoule bottle, wherein the particle size of the copper powder is 50nm, and mixing the precursors with 5g of iodine particles; the quartz ampoule is evacuated to 8mTorr and sealed with a flame; subsequently, the quartz ampoule bottle is put into a tube furnace for heating, the heating rate is 4 ℃/min, the temperature of a source area is increased to 660 ℃, the temperature of a growth area is increased to 540 ℃, and the quartz ampoule bottle is maintained at the temperature for 3 days; stopping heating the tube furnace, naturally cooling the quartz ampoule bottle to room temperature, and obtaining the polarized spinelle ferroelectric material with the transverse dimension of 3mm on the bottle wall of the quartz ampoule bottle.
Example 6
Filling 2mmol of copper powder, 1mmol of indium block, 2mmol of phosphorus block and 6mmol of sulfur powder into a quartz ampoule bottle, wherein the particle size of the copper powder is 50nm, and mixing the precursors with 5g of iodine particles; the quartz ampoule is evacuated to 110mTorr and sealed with a flame; subsequently, the quartz ampoule bottle is put into a tube furnace for heating, the heating rate is 3 ℃/min, the temperature of a source area is increased to 610 ℃, the temperature of a growth area is increased to 605 ℃, and the quartz ampoule bottle is maintained at the temperature for 3 days; stopping heating the tube furnace, naturally cooling the quartz ampoule bottle to room temperature, and obtaining the polarized spinelle ferroelectric material with the transverse dimension of 4mm on the bottle wall of the quartz ampoule bottle.
Comparative example 1
1Mmol of copper powder, 1mmol of indium block, 2mmol of phosphorus block and 6mmol of sulfur powder are filled into a quartz ampoule bottle, wherein the particle size of the copper powder is 50nm, and the precursors are mixed with 5g of iodine particles; the quartz ampoule is evacuated to 20mTorr and sealed with a flame; subsequently, the quartz ampoule bottle is put into a tube furnace for heating, the heating rate is 1 ℃/min, the temperature of a source area is increased to 650 ℃, the temperature of a growth area is increased to 600 ℃, and the quartz ampoule bottle is maintained at the temperature for 3 days; and stopping heating the tube furnace, naturally cooling the quartz ampoule bottle to room temperature, and obtaining the ferroelectric material on the bottle wall of the quartz ampoule bottle, wherein the transverse dimension of the ferroelectric material is 4mm.
Comparative example 2
2.1Mmol of copper powder, 1mmol of indium block, 2mmol of phosphorus block and 6mmol of sulfur powder are filled into a quartz ampoule bottle, wherein the particle size of the copper powder is 50nm, and the precursors are mixed with 5g of iodine particles; the quartz ampoule is evacuated to 20mTorr and sealed with a flame; subsequently, the quartz ampoule bottle is put into a tube furnace for heating, the heating rate is 1 ℃/min, the temperature of a source area is increased to 650 ℃, the temperature of a growth area is increased to 600 ℃, and the quartz ampoule bottle is maintained at the temperature for 3 days; and stopping heating the tube furnace, naturally cooling the quartz ampoule bottle to room temperature, and obtaining the ferroelectric material on the bottle wall of the quartz ampoule bottle, wherein the transverse dimension of the ferroelectric material is 3.5mm.
Comparative example 3
Filling 1.3mmol of copper powder, 1mmol of indium block, 2mmol of phosphorus block and 6mmol of sulfur powder into a quartz ampoule bottle, wherein the particle size of the copper powder is 30nm, and mixing the precursors with 5mmol of iodine particles; the quartz ampoule is evacuated to 20mTorr and sealed with a flame; subsequently, the quartz ampoule bottle is put into a tube furnace for heating, the heating rate is 1 ℃/min, the temperature of a source area is increased to 650 ℃, the temperature of a growth area is increased to 600 ℃, and the quartz ampoule bottle is maintained at the temperature for 3 days; and stopping heating the tube furnace, naturally cooling the quartz ampoule bottle to room temperature, and obtaining the ferroelectric material on the bottle wall of the quartz ampoule bottle, wherein the transverse dimension of the ferroelectric material is 3.5mm.
Comparative example 4
Filling 1.3mmol of copper powder, 1mmol of indium block, 2mmol of phosphorus block and 6mmol of sulfur powder into a quartz ampoule bottle, wherein the particle size of the copper powder is 500nm, and mixing the precursors with 5mmol of iodine particles; the quartz ampoule is evacuated to 20mTorr and sealed with a flame; subsequently, the quartz ampoule bottle is put into a tube furnace for heating, the heating rate is 1 ℃/min, the temperature of a source area is increased to 650 ℃, the temperature of a growth area is increased to 600 ℃, and the quartz ampoule bottle is maintained at the temperature for 3 days; and stopping heating the tube furnace, naturally cooling the quartz ampoule bottle to room temperature, and obtaining the ferroelectric material on the bottle wall of the quartz ampoule bottle, wherein the transverse dimension of the ferroelectric material is 4mm.
The ferroelectric materials prepared in all examples and comparative examples were subjected to characterization tests, the test indexes are as follows:
(1) Raman spectrum test: and (3) repeatedly pasting and peeling the prepared ferroelectric material on a transparent adhesive tape to obtain the ferroelectric material with atomic-scale thickness, transferring the ferroelectric material to a silicon wafer substrate, slowly peeling the adhesive tape after standing for a period of time, placing the ferroelectric material with atomic-scale thickness on the silicon wafer substrate, using laser with the wavelength of 532nm for excitation at room temperature, and testing Raman spectrum.
(2) Piezoelectric power microscope (PFM) characterization: and (3) repeatedly pasting and peeling the prepared ferroelectric material on a transparent adhesive tape to obtain an atomic-scale-thickness ferroelectric material, transferring the ferroelectric material to a silicon wafer substrate, slowly peeling the adhesive tape after standing for a period of time, placing the atomic-scale-thickness ferroelectric material on the silicon wafer substrate, obtaining the in-plane polarization condition of the polarized Szechwan cassia seed ferroelectric material through PFM, and representing the polarized Szechwan cassia seed structure.
(3) Atomic force microscope testing: and (3) repeatedly pasting and peeling the prepared ferroelectric material on a transparent adhesive tape to obtain the ferroelectric material with atomic-scale thickness, transferring the ferroelectric material to a silicon wafer substrate, slowly peeling the adhesive tape after standing for a period of time, placing the ferroelectric material with atomic-scale thickness on the silicon wafer substrate, and characterizing the atomic-scale thickness of the polarized Sje ferroelectric material through atomic-force microscope testing.
Fig. 4 shows raman spectrum test results of the ferroelectric materials of atomic scale thickness in example 1 and comparative example 1, and it can be seen that the peak of the polarized segetum ferroelectric material prepared in example 1 near 310cm -1 is significantly stronger than the peak of the ferroelectric material prepared in comparative example 1 near 310cm -1, indicating that the content of copper ions in the polarized segetum ferroelectric material obtained by the preparation method of the present invention is higher, thereby being beneficial to reducing copper defects, further improving tensile stress in the polarized segetum ferroelectric material, and being beneficial to stabilizing polarized segetum.
Fig. 5 shows PFM in-plane phase diagrams of the ferroelectric materials of atomic scale thickness in example 1 and comparative example 1, and it can be seen from (b) in fig. 5 that the polarized segrain ferroelectric material prepared in example 1 has a topology domain structure of polarized segrain type with uniform orientation of half bright and half dark, whereas the ferroelectric material prepared in (a) in fig. 5 shows a general ferroelectric domain shape of "maze" shape without polarized segrain structure.
The characterization results of the polarized structure of the ferroelectric materials prepared in all examples and comparative examples are shown in table 1.
TABLE 1
As can be seen from the results in Table 1, all the polarized Szechwan ferroelectric materials prepared in the examples have stable spontaneously formed polarized Szechwan structures, the polarized Szechwan structures are rod-shaped or round, and the Szechwan structures cannot be observed in all the ferroelectric materials prepared in the comparative examples, so that the preparation method of the invention can effectively prepare the polarized Szechwan ferroelectric materials, can be widely applied to the fields of memories, logic operation and the like, and has wide market prospect.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. A method for preparing a polarized segetum ferroelectric material, comprising the steps of:
And (3) growing a copper source, an indium source, a phosphorus source and a sulfur source in a molar ratio of (1.3-2) to (1:2:6) under the conditions of heating and gas phase transmission medium to obtain the polarized spinelle seed ferroelectric material, wherein the particle size of the copper source is 50-200 nm.
2. The method for preparing the polarized semen cassiae ferroelectric material according to claim 1, wherein the reaction device for carrying out vacuum chemical vapor transport comprises a source region and a growth region, wherein the heating temperature of the source region is 600-650 ℃, and the heating temperature of the growth region is 550-600 ℃.
3. The method for preparing a polarized segetum ferroelectric material as claimed in claim 2, wherein the vacuum pressure of the reaction device is 20 mtorr-100 mtorr;
and/or the heating rate of the reaction device is 1-3 ℃/min;
And/or the heating time of the reaction device is 72-120 hours;
And/or the gas phase transmission medium is selected from iodine vapor.
4. A poled segetum ferroelectric material as claimed in any one of claims 1 to 3.
5. The polarized segetum ferroelectric material as claimed in claim 4, wherein the atomic-scale thickness of the polarized segetum ferroelectric material is 5 nm-200 nm.
6. The polarized segetum ferroelectric material as claimed in claim 4 or claim 5, wherein the polarized segetum is rod-like structure when the atomic-scale thickness of the polarized segetum ferroelectric material is equal to or greater than 60 nm.
7. The polarized segetum ferroelectric material as claimed in claim 6, wherein the length of the polarized segetum is 50 nm-300 nm.
8. The polarized segetum ferroelectric material as claimed in claim 4 or claim 5, wherein the polarized segetum is of circular structure when the atomic scale thickness of the polarized segetum ferroelectric material is less than or equal to 30 nm.
9. The polarized segetum ferroelectric material as claimed in claim 8, wherein the diameter of the polarized segetum is 10 nm-100 nm.
10. Use of a poled segmeans ferroelectric material as claimed in any one of claims 4 to 9 in a memory or logic operation.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000007430A (en) * | 1998-06-19 | 2000-01-11 | Yamaha Corp | Ferroelectric material and ferroelectric memory |
| US7998762B1 (en) * | 2007-11-14 | 2011-08-16 | Stion Corporation | Method and system for large scale manufacture of thin film photovoltaic devices using multi-chamber configuration |
| CN108190942A (en) * | 2017-12-19 | 2018-06-22 | 昆明理工大学 | A kind of nanocrystalline preparation method of the controllable copper silver-colored zinc tin sulphur of crystalline phase |
| CN110295357A (en) * | 2018-03-21 | 2019-10-01 | 北京大学 | A kind of quick magnanimity prepares the method and device of oversize two-dimensional material film |
| CN111074129A (en) * | 2019-12-05 | 2020-04-28 | 杭州电子科技大学 | Rare earth-based magnetic sigmin material, preparation method and application thereof |
| CN114400284A (en) * | 2022-01-14 | 2022-04-26 | 南京大学 | Composite film based on polar topological domain structure, ferroelectric memory and preparation method of composite film |
| CN114715871A (en) * | 2022-04-26 | 2022-07-08 | 张粒新 | Modified lithium iron phosphate cathode material for lithium battery and preparation method |
| CN117486178A (en) * | 2023-12-27 | 2024-02-02 | 上海交通大学 | Negative electrode material and preparation method and application thereof |
-
2024
- 2024-06-13 CN CN202410763157.3A patent/CN118326364B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000007430A (en) * | 1998-06-19 | 2000-01-11 | Yamaha Corp | Ferroelectric material and ferroelectric memory |
| US7998762B1 (en) * | 2007-11-14 | 2011-08-16 | Stion Corporation | Method and system for large scale manufacture of thin film photovoltaic devices using multi-chamber configuration |
| CN108190942A (en) * | 2017-12-19 | 2018-06-22 | 昆明理工大学 | A kind of nanocrystalline preparation method of the controllable copper silver-colored zinc tin sulphur of crystalline phase |
| CN110295357A (en) * | 2018-03-21 | 2019-10-01 | 北京大学 | A kind of quick magnanimity prepares the method and device of oversize two-dimensional material film |
| CN111074129A (en) * | 2019-12-05 | 2020-04-28 | 杭州电子科技大学 | Rare earth-based magnetic sigmin material, preparation method and application thereof |
| CN114400284A (en) * | 2022-01-14 | 2022-04-26 | 南京大学 | Composite film based on polar topological domain structure, ferroelectric memory and preparation method of composite film |
| CN114715871A (en) * | 2022-04-26 | 2022-07-08 | 张粒新 | Modified lithium iron phosphate cathode material for lithium battery and preparation method |
| CN117486178A (en) * | 2023-12-27 | 2024-02-02 | 上海交通大学 | Negative electrode material and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| J.F. MALTA ET AL.: "Synthesis and magnetic studies of nanocrystalline Cu2OSeO3, a chiral topological magnet", JOURNAL OF MAGNETISM AND MAGNETIC MATERIALS, no. 474, 31 December 2019 (2019-12-31), pages 122 - 126 * |
| 王皓瑶;刘海;孙剑飞;顾宁;: "磁性纳米颗粒的磁矩测量", 中国科学:技术科学, no. 09, 4 September 2018 (2018-09-04) * |
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