CN113702130A - High-voltage in-situ ferroelectricity measuring method for lithium niobate ferroelectric material - Google Patents

High-voltage in-situ ferroelectricity measuring method for lithium niobate ferroelectric material Download PDF

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CN113702130A
CN113702130A CN202111023259.4A CN202111023259A CN113702130A CN 113702130 A CN113702130 A CN 113702130A CN 202111023259 A CN202111023259 A CN 202111023259A CN 113702130 A CN113702130 A CN 113702130A
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lithium niobate
voltage
ferroelectric material
ferroelectricity
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韩永昊
李娟�
蒋大伟
马秋
高春晓
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Jilin University
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Abstract

The invention discloses a high-voltage in-situ ferroelectricity measuring method for a lithium niobate ferroelectric material, and belongs to the technical field of measurement of ferroelectric materials under high voltage. The measuring method is designed based on a diamond anvil cell and comprises the steps of preparing lithium niobate ceramic powder, assembling a diamond anvil cell device, manufacturing an electrode and the like. The method makes up the blank that the ferroelectric material has no experimental support in the aspect of high-voltage research, measures the change of the ferroelectricity of the ferroelectric material under high voltage for the first time, is simple and convenient, consumes less time in experiments, and can effectively measure the ferroelectric properties of the ferroelectric material such as the hysteresis loop, the remanent polarization, the energy storage efficiency and the like under high voltage.

Description

High-voltage in-situ ferroelectricity measuring method for lithium niobate ferroelectric material
Technical Field
The invention belongs to the technical field of ferroelectric material measurement under high voltage, and particularly relates to LiNbO3A method for measuring ferroelectricity (electric hysteresis loop, remanent polarization, energy storage efficiency and the like) of a ferroelectric material under high voltage.
Background
Ferroelectric materials have been widely studied for their excellent piezoelectric, photoelectric, ferroelectric, and pyroelectric effects, and have been used in the fields of piezoelectric sensors, ferroelectric memories, electronic devices, ferroelectric capacitors, and the like. In practical application, the remanent polarization of the ferroelectric material has important significance. The remanent polarization intensity is the polarization which is still existed when the applied electric field is reduced to zero, and is an important parameter for evaluating the energy storage characteristic of the ferroelectric ceramic, and the smaller the remanent polarization is, the smaller the energy loss is, and the important practical significance is achieved. Therefore, the ferroelectric properties of the material can be grasped, and the material can be used in various fields.
Hysteresis loops are one sign of ferroelectricity. The most basic principle for measuring the ferroelectric hysteresis loop of the ferroelectric material is to regard a sample to be measured as a capacitor and obtain polarization charges on the sample to be measured by measuring current or voltage. There are generally an impulse galvanometer scanning method and a Sawyer-Tower circuit method. The method for measuring the electric hysteresis loop of the material under high voltage adopts a Sawyer-Tower circuit method, and has the advantages of simple operation, less time consumption and high efficiency. In the existing research, the research on ferroelectric materials relates to the field of normal pressure, and the ferroelectric properties of the materials are improved by doping, manufacturing ceramics or films and the like. The research under high voltage is few and few, and only part of the literature judges the change of the ferroelectricity of the ferroelectric material under high voltage through theoretical calculation, while the research on the ferroelectric material under high voltage is still blank experimentally.
LiNbO3The ferroelectric material is an important ferroelectric material, has excellent electro-optic, acousto-optic, piezoelectric, pyroelectric and nonlinear optical effects, and has a very wide application prospect. The pressure effect can regulate and control the lattice constant, electronic state density, mode parameter, etc. of the material to make the crystal structure produce phase change or form new matter, and high pressure is an effective means for regulating the material property. The invention utilizes the diamond anvil cell device to measure the ferroelectricity of the lithium niobate ferroelectric material under high voltage, can obtain how the ferroelectricity such as electric hysteresis loop, coercive field, residual polarization, energy storage density and the like of the lithium niobate material changes under high voltage, provides experimental basis for developers, and expands the application field of the lithium niobate ferroelectric material.
Disclosure of Invention
The invention aims to solveThe method overcomes the defects in the prior art, provides a high-voltage in-situ ferroelectricity measuring method for lithium niobate ferroelectric materials, and particularly relates to LiNbO3Measurement of ferroelectricity (hysteresis loop, coercive field, remanent polarization, energy storage density, etc.) at high voltage for ferroelectric materials.
The specific technical scheme of the invention is as follows:
a method for measuring high-voltage in-situ ferroelectricity of a lithium niobate ferroelectric material comprises the following steps:
the method comprises the following steps: preparing a sample, namely fully grinding lithium niobate powder, then placing the ground lithium niobate powder in a crucible, and putting the crucible into a tubular furnace for annealing treatment to obtain single-phase lithium niobate ceramic powder;
preferably, the annealing temperature is 400 ℃, the annealing time is 3 hours, the temperature is raised for one hour, and then the temperature is maintained for two hours;
step two: prepressing the metal gasket 2 by using a diamond anvil 1 to obtain an anvil face, a chamfer and a side edge indentation of the diamond anvil, putting the prepressed gasket into a mixed solution of ethanol and acetone for 10 minutes, and washing off surface stains;
preferably, the metal gasket is a T301 steel sheet, and the mixing ratio of ethanol to acetone is 1: 1;
step three: the electric soldering iron welds the metal lead copper wire 3 on the metal gasket 2 of the second step, as the electrode lead, in the invention, utilize the metal gasket as an electrode contacting with lower anvil surface in testing;
step four: filling the sample into the indentation pre-pressed by the gasket, pre-pressing by using an anvil to tightly fill the sample into the indentation to obtain a sample slice 4; then, coating the gasket except for the sample with black glue 5 for insulation treatment;
preferably, the pre-pressing pressure is 1GPa, and the pre-pressing pressure is far less than the phase transformation point of the material (about 25 GPa);
step five: an electrode is arranged on the anvil surface of the diamond, the electrode is manufactured by cutting a platinum sheet 6 into a slender strip shape, the width of the platinum sheet is 1/3 of the width of the anvil surface and sticking silver paste to a metal lead 7; placing a ruby in the center of the anvil surface for marking, and slightly closing the diamond anvil to ensure that the platinum sheet electrode is positioned in the center of the sample;
step six: measuring, namely putting the assembled diamond anvil cell into a pressurizing device, connecting a ferroelectric analyzer with two electrode leads, applying an alternating electric field to a sample to be measured, and obtaining hysteresis loop diagrams under different pressures, wherein the alternating voltage waveform of the alternating electric field is triangular wave and the frequency is 50 Hz; finally, data processing is carried out to obtain a relation graph of the change of the remanent polarization intensity along with the pressure, and the relation graph is calculated according to the calculation formula of the total energy storage density, the releasable energy storage density and the energy storage efficiency
Figure BDA0003242475270000021
Wherein E represents the electric field intensity, P represents the polarization intensity, Pr and PmaxRepresenting residual polarization and saturation polarization to obtain a relation graph of energy storage efficiency and pressure change.
Has the advantages that:
the invention provides a high-voltage in-situ ferroelectricity measuring device and method for a lithium niobate ferroelectric material, which firstly carry out high-voltage in-situ measurement on the ferroelectric material so as to explore the influence of pressure on the ferroelectricity of the ferroelectric material, namely LiNbO3The application of the material provides a new research direction, and the method has the characteristics of simple operation, high safety, capability of obtaining accurate ferroelectric parameters and the like.
Drawings
Fig. 1 is a diamond anvil high-voltage in-situ ferroelectricity measuring device under the conditions of example 2.
FIG. 2 is the ferroelectric hysteresis loop of the lithium niobate ferroelectric material under the conditions of example 3 under a pressure of 0-3.63 GPa.
FIG. 3 shows the hysteresis loop of the lithium niobate ferroelectric material under the conditions of example 3 under the pressure of 4.55-6.35 GPa.
Fig. 4 is a graph of the remanent polarization of the lithium niobate ferroelectric material with pressure change under the conditions of example 4.
Fig. 5 is a graph of the energy storage efficiency of the lithium niobate material as a function of pressure under the conditions of example 5.
Detailed Description
In the embodiment of the invention, the high-voltage in-situ ferroelectric performance test is carried out, the experimental condition is room temperature, the experimental apparatus is a Precision Multiferroic ferroelectric analyzer, the maximum value of an externally-added alternating electric field is 44.44KV/cm, the polarization time is 20ms, and the test frequency is 50 Hz.
Example 1 preparation of samples
In the present invention, the ceramic material was selected for testing. Fully grinding the lithium niobate powder, then placing the powder in a crucible, and putting the crucible into a tube furnace for annealing treatment, wherein the annealing temperature is 400 ℃, and the annealing time is 3 hours, and finally obtaining the single-phase lithium niobate ceramic powder with small particle size.
Example 2 high-voltage in-situ ferroelectric measuring device Assembly
The high-voltage in-situ ferroelectricity measuring device can be clearly seen from the attached fig. 1, and the specific manner is as follows:
firstly, prepressing a metal gasket 2 by using a diamond anvil 1 to obtain an anvil face, a chamfer and a side edge indentation of the diamond anvil, putting the prepressed gasket into a mixed solution of ethanol and acetone for 10 minutes by ultrasonic treatment, and washing off surface stains.
And secondly, welding a metal conducting wire copper wire 3 on the gasket 2 in the second step by using an electric soldering iron as an electrode conducting wire, namely, in the invention, the metal gasket is used as an electrode which is in contact with the lower anvil surface in the test.
And thirdly, filling the sample into the indentation pre-pressed by the gasket, pre-pressing by using an anvil to tightly fill the sample into the indentation, and obtaining a sample slice 4. The area of the pad other than the sample was then filled with black gel 5 for insulation.
And fourthly, an electrode is arranged on the diamond anvil surface, the electrode is made by cutting the platinum sheet 6 into a slender strip shape with the width being about 1/3 of the anvil surface and adhering silver paste to the metal lead 7. Putting a ruby in the center of the anvil surface for marking, and slightly closing the diamond anvil to ensure that the platinum sheet electrode is positioned in the center of the sample.
Example 3 ferroelectric measurement of lithium niobate Material
And connecting the assembled diamond anvil cell with a ferroelectric tester, wherein the internal pressure of the sample cavity of the diamond anvil cell device is changed within the range of 0-3.63GPa, and testing the electric hysteresis loop of the diamond anvil cell device. The results of the specific in situ ferroelectric test are shown in figure 2. Then the internal pressure of the diamond anvil cell device sample is slowly increased from 3.63GPa to 6.35GPa, and the sample is tested to obtain an electric hysteresis loop, and the specific test result is shown in figure 3.
Example 4 data processing
The change of the residual polarization and the pressure can be obtained according to the measured electric hysteresis loop, and the graph is shown in figure 4. According to the calculation formula of total energy storage density, releasable energy storage density and energy storage efficiency
Figure BDA0003242475270000041
Figure BDA0003242475270000042
Wherein E represents the electric field intensity, P represents the polarization intensity, Pr and PmaxRepresenting the remanent polarization and the saturation polarization, a graph of energy storage efficiency versus pressure change is obtained, see fig. 5.
The method can simply and effectively measure the ferroelectric properties of the ferroelectric material under high voltage, including the electric hysteresis loop, the remanent polarization and the energy storage efficiency, and provides experimental support for the research of the ferroelectric material in the high voltage direction. In the invention, lithium niobate powder ceramics are selected as the research object, but the device and the method of the invention can also be used for the research of ferroelectricity of other powder ceramics under high voltage.

Claims (4)

1. A method for measuring high-voltage in-situ ferroelectricity of a lithium niobate ferroelectric material comprises the following steps:
the method comprises the following steps: preparing a sample, namely fully grinding lithium niobate powder, then placing the ground lithium niobate powder in a crucible, and putting the crucible into a tubular furnace for annealing treatment to obtain single-phase lithium niobate ceramic powder;
step two: prepressing a metal gasket (2) by using a diamond anvil cell (1) to obtain an anvil surface, a chamfer and a side edge indentation of the diamond anvil cell, putting the prepressed gasket into a mixed solution of ethanol and acetone for 10 minutes by ultrasonic treatment, and washing off surface stains;
step three: welding a metal lead copper wire (3) on the metal gasket (2) in the second step by the electric soldering iron to serve as an electrode lead, wherein the metal gasket is used as an electrode which is in contact with the lower anvil surface in the test;
step four: filling the sample into the indentation pre-pressed by the gasket, pre-pressing by using an anvil to tightly fill the sample into the indentation to obtain a sample slice (4); then, coating the area of the gasket except the sample with black glue (5) for insulation treatment;
step five: an electrode is arranged on the anvil surface of the diamond, the electrode is manufactured by cutting a platinum sheet (6) into a slender strip shape, the width of the platinum sheet is 1/3 of the width of the anvil surface and sticking silver paste to a metal lead (7); placing a ruby in the center of the anvil surface for marking, and slightly closing the diamond anvil to ensure that the platinum sheet electrode is positioned in the center of the sample;
step six: measuring, namely putting the assembled diamond anvil cell into a pressurizing device, connecting a ferroelectric analyzer with two electrode leads, applying an alternating electric field to a sample to be measured, and obtaining hysteresis loop diagrams under different pressures, wherein the alternating voltage waveform of the alternating electric field is triangular wave and the frequency is 50 Hz; finally, data processing is carried out to obtain a relation graph of the change of the remanent polarization intensity along with the pressure, and the relation graph is calculated according to the calculation formula of the total energy storage density, the releasable energy storage density and the energy storage efficiency
Figure FDA0003242475260000011
Wherein E represents the electric field intensity, P represents the polarization intensity, Pr and PmaxRepresenting residual polarization and saturation polarization to obtain a relation graph of energy storage efficiency and pressure change.
2. The method for measuring high-voltage in-situ ferroelectricity of a lithium niobate ferroelectric material according to claim 1, wherein in the step one, the annealing temperature is 400 ℃, the annealing time is 3 hours, and the temperature is raised for one hour and then maintained for two hours.
3. The method for measuring high-voltage in-situ ferroelectricity of a lithium niobate ferroelectric material according to claim 1, wherein in the second step, the metal gasket is a T301 steel sheet, and the mixing ratio of ethanol to acetone is 1: 1.
4. The method for measuring high-voltage in-situ ferroelectricity of a lithium niobate ferroelectric material according to claim 1, wherein in the fourth step, the pre-pressing pressure is 1 Gpa.
CN202111023259.4A 2021-09-02 2021-09-02 High-voltage in-situ ferroelectricity measuring method for lithium niobate ferroelectric material Pending CN113702130A (en)

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JPH11174098A (en) * 1997-12-09 1999-07-02 Fujitsu Ltd Polarization characteristic measuring method for ferroelectric material
US20040163596A1 (en) * 2002-06-28 2004-08-26 Miles Ronald O. Method and apparatus for increasing bulk conductivity of a ferroelectric material
CN102183693A (en) * 2011-01-19 2011-09-14 吉林大学 Electrodes for high pressure in situ resistivity survey and manufacturing method of electrodes
CN102288824A (en) * 2011-05-17 2011-12-21 吉林大学 Electrode for high-voltage in-situ impedance measurement and preparation method and application of same
CN104744033A (en) * 2013-12-25 2015-07-01 中国科学院上海硅酸盐研究所 Sodium bismuth titanate-barium titanate lead-free transparent electro-optic ceramic and preparation method thereof
CN104793287A (en) * 2015-04-07 2015-07-22 南京大学 Production method of ferroelectric superlattice
CN111879425A (en) * 2020-08-10 2020-11-03 吉林大学 In-situ temperature measuring gasket in diamond anvil cell press and preparation method thereof

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