CN112903752B - Method for measuring electric hysteresis loop of substance in diamond anvil cell - Google Patents
Method for measuring electric hysteresis loop of substance in diamond anvil cell Download PDFInfo
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Abstract
The invention discloses a method for measuring an electric hysteresis loop of a substance in a diamond anvil cell, belonging to the technical field of physical quantity measurement under extreme conditions. The invention solves the problems that in the process of measuring the hysteresis loop by using a diamond anvil cell device, the thickness and the area of a sample cannot be accurately obtained, the insulating property of the sample of the device cannot be ensured, the arrangement of a test electrode is complex, and the like, which influence the accuracy of a measurement result and the test period. The measurement method is simple and easy to operate, the materials are easy to obtain, and various problems influencing the measurement result are comprehensively considered, so that the measurement result is more accurate, and the accuracy of each parameter of the hysteresis loop is ensured.
Description
The technical field is as follows:
the invention belongs to the technical field of physical quantity measurement under extreme conditions, and particularly relates to a method for measuring an electric hysteresis loop of a ferroelectric material in a diamond anvil cell.
Background art:
a Diamond Anvil Cell (DAC) is used as an important static high-pressure experimental device capable of generating million atmospheres in the research of the high-pressure scientific field, is already applied to the research fields of electricity, optics, acoustics, thermotics, magnetism and the like in the physical subject, and provides important ideas and experimental technical means for exploring the preparation of new materials under high pressure, intercepting and predicting the high-pressure phase change of substances, improving the physical properties of the materials, earth science and the like.
The research of ferroelectricity of the material, as a new direction in the field of electrical performance research of materials in recent years, mainly obtains macroscopic performance parameters such as saturation polarization (Ps), residual polarization (Pr), coercive field strength (Ec) and the like of the material and physical quantities such as nonlinear relation between dielectric constant and electric field strength and the like by researching an electric hysteresis loop of the ferroelectric material in a periodically changing electric field, thereby utilizing the results to carry out multi-aspect performance research on the piezoelectric material, such as the field of memory research, and based on the electric hysteresis phenomenon in ferroelectricity, the characteristic that a ferroelectric domain can form high polarization charge by reversing under the electric field is utilized, and further manufacturing a high-efficiency memory; in the field of display devices, a series of transparent ferroelectric ceramic display devices have been developed using the ferroelectric remanent polarization (Pr); in the field of photoelectricity, the change relation of the polarization of ferroelectrics along with E is utilized to research the change effect-the electro-optic effect of an external electric field and the crystal refractive index, and optical devices such as an optical modulator, a crystal light valve, an electro-optic switch and the like are prepared.
Under normal pressure, the ferroelectric material has various beneficial properties and provides important support for technological progress, but the normal pressure is used as a conventional technical means, and a certain vacuum area still exists for the exploration of the ferroelectric material. Researchers have also gradually combined ferroelectric materials with high-voltage experimental science to research, and it has been shown that the structural change of a substance at high voltage also causes the property change of ferroelectric domain, thereby affecting the change of ferroelectricity of the substance. If the high-voltage technical means is adopted, the reversal of ferroelectric domains can be accelerated, macroscopic performance parameters such as saturation polarization (Ps), residual polarization (Pr), coercive field intensity (Ec) and the like and the nonlinear relation between dielectric constants and electric field intensities can be changed, and then the performances of a series of ferroelectric materials such as ferroelectric films, ferroelectric ceramics and the like can be optimized, so that the sensing and driving performances of the ferroelectric materials can be fully exerted, thereby providing basis for developers and promoting the development and development of high-performance and high-reliability devices.
The performance research of the ferroelectric material under the high-voltage condition still takes the acquisition and analysis of the ferroelectric hysteresis loop as a main means, however, compared with a test method mature under the normal-voltage condition, the measurement method of the ferroelectric material under the high-voltage condition is still blank, and a series of problems will occur when the existing high-voltage electrical test method is adopted to directly measure the ferroelectric hysteresis loop, such as sample thickness, sample area which can not be accurately obtained, the insulation performance of a device sample which can not be ensured, and the measurement accuracy and the test period of the ferroelectric hysteresis loop can be influenced by factors such as complex arrangement of test electrodes.
Therefore, the test method which can accurately obtain the thickness and area of the sample, ensure the insulativity of the device sample and have relatively short work period is provided, and has great significance for the development of ferroelectric materials and high-voltage subjects.
Disclosure of Invention
The invention aims to solve the technical problems that: through a brand new test method, the defect problems existing in the traditional technology, namely the problems of influence of factors such as the thickness of a sample, the area of the sample, the material and the mode of the cloth electrode, the insulating property of the device and the like on the measurement of the hysteresis loop and the like are solved. The method is a brand new method for simply measuring the hysteresis loop, and the accuracy of the measured data is ensured.
The invention adopts the following technical scheme:
a method for measuring the electric hysteresis loop of a substance in a diamond anvil cell comprises the following steps:
firstly, placing a gasket A1 and a gasket B2 in a mixed solution of alcohol and acetone for ultrasonic cleaning for 5-10 minutes;
secondly, drying the gasket A1 and the gasket B2 obtained by cleaning in the first step, selecting two enameled wires 3 with the same diameter and length, and respectively welding the two enameled wires 3 on the gasket A1 and the gasket B2 which are subjected to drying treatment by a welding method to be used as test signal wires;
thirdly, placing the A gasket 1 and the B gasket 2 welded with the enameled wire 3 prepared in the second step on a B anvil 6, ensuring that the centroids of the A gasket 1 and the B gasket 2 are coaxially overlapped with the centroid of the B anvil 6, then stacking 0.05-0.15 g of pressure transmitting powder 4 on the A gasket 1, then performing gasket prepressing through mutual extrusion of the A anvil 5 and the B anvil 6 in a DAC press, and after the prepressing is completed, taking down the prepressed A gasket 1 and the B gasket 2 from the middle of the A anvil 5 and the B anvil 6 for cleaning;
fourthly, putting ruby 8 into the center of the shape of the pressure transfer powder 4 on the cleaned A gasket 1 after the prepressing in the third step, resetting the A gasket 1 with the ruby 8 on the A anvil 5 again, and fixing by using plasticine 7;
Fifthly, resetting the B gasket 2 subjected to prepressing in the third step on a B anvil 6, fixing the B gasket by using plasticine 7, then placing a mica sheet 9 with a circular sample filling hole on the B gasket 2, ensuring that the center of the sample filling hole is coaxial with the center of the anvil surface of the B anvil 6, and adding a sample 10 into the sample filling hole;
and sixthly, in a DAC press, closely contacting the laminated body consisting of the A gasket 1, the pressure transmitting powder 4, the ruby 8 and the A anvil 5 obtained in the fourth step with the laminated body consisting of the sample 10, the mica sheet 9, the B gasket 2 and the B anvil 6 obtained in the fifth step from the upper part, and testing after the ruby 8 passes through standard pressing.
Preferably, in the first step, the alcohol to acetone volume ratio is between 2:3 and 3: 2;
preferably, the diameter of the enameled wire 3 is 0.03-0.13 mm;
preferably, the thickness of the mica sheet 9 is 0.02-1 mm;
preferably, the diameter of the sample filling hole of the mica sheet 9 is
Smaller than the diameter of the anvil surface imprints of the anvil A5 and the anvil B6;
preferably, the sample 10 in the sample filling hole of the mica sheet 9 fills the entire sample filling hole.
The invention is designed on the basis of comprehensively considering the influence of various factors in the measuring process and the simplicity degree of the operation method in the measuring process. The influence of the thickness and the area of the sample on the measurement of the hysteresis loop is accurately controlled by using the mica sheet; the copper wire is connected with the gasket, so that the problems of material and mode of electrode distribution, insulating property of the device and the like in the experiment are avoided. The method not only can meet the requirement of real-time measurement, but also ensures the accuracy of the measurement of the hysteresis loop on the basis of simple operation.
In conclusion, the beneficial effects of the invention are as follows:
the invention solves the problems that in the process of measuring the hysteresis loop by using a diamond anvil cell device, the thickness and the area of a sample cannot be accurately obtained, the insulating property of the sample of the device cannot be ensured, the arrangement of a test electrode is complex, and the like, which influence the accuracy of a measurement result and the test period. The measurement method is simple and easy to operate, the materials are easy to obtain, and various problems influencing the measurement result are comprehensively considered, so that the measurement result is more accurate, and the accuracy of each parameter of the hysteresis loop is ensured. The invention has important technical breakthrough in the aspect of measuring the hysteresis loop of the material in the anvil device by the diamond under high pressure, and the application of the invention not only can broaden the development of related tests and improve the test efficiency, but also can greatly improve the accuracy of measuring various parameters of the hysteresis loop of the material in the anvil device by the diamond under high pressure.
Description of the drawings:
fig. 1 is a schematic view of the apparatus of the present invention with a pad having an enameled wire soldered thereto.
FIG. 2 is a schematic cross-sectional view of the diamond anvil inner tabletting and powdering device of the present invention.
FIG. 3 is a schematic representation of the relationship of the diamond to the pad variation in the anvil of the present invention.
FIG. 4 is a schematic diagram showing the pad position on the diamond A side and the ruby position in the diamond anvil cell according to the present invention.
FIG. 5 is a schematic diagram of the position and fixation of a pad on the side of diamond B in the diamond anvil cell of the present invention.
FIG. 6 is a schematic illustration of the placement of mica plates in a diamond anvil cell according to the present invention.
Fig. 7 is a schematic cross-sectional view of an overall apparatus for measuring a ferroelectric hysteresis loop in the present invention.
The specific implementation scheme is as follows:
the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
Measurement of PbTiO in Diamond anvil cells 3 The hysteresis loop is operated in combination with the attached figures 1-7The method comprises the following steps:
firstly, placing a gasket A1 and a gasket B2 in a mixed solution of alcohol and acetone for ultrasonic cleaning for 10 minutes;
secondly, firstly drying the gasket A1 and the gasket B2 obtained by cleaning in the first step, then selecting two enameled wires 3 with the same diameter and length, and respectively welding the two enameled wires 3 on the gasket A1 and the gasket B2 which are subjected to drying treatment by a welding method to be used as test signal wires, as shown in figure 1;
Thirdly, placing the A gasket 1 and the B gasket 2 welded with the enameled wire 3 prepared in the second step on a B anvil 6, ensuring that the centroids of the A gasket 1 and the B gasket 2 are coaxially overlapped with the centroid of the B anvil 6, stacking 0.08g of pressure transmitting powder 4 on the A gasket 1, and then performing gasket prepressing through mutual extrusion of the A anvil 5 and the B anvil 6 in a DAC press, as shown in figures 2 and 3, after the prepressing is completed, taking down the prepressed A gasket 1 and the B gasket 2 from the middle of the A anvil 5 and the B anvil 6 for cleaning;
fourthly, putting ruby 8 into the center of the shape of the pressure transfer powder 4 on the cleaned A gasket 1 after the prepressing in the third step, resetting the A gasket 1 with the ruby 8 on the A anvil 5 again, and fixing by using plasticine 7, as shown in figure 4;
fifthly, resetting the B gasket 2 pre-pressed in the third step on a B anvil 6 and fixing the B gasket by using plasticine 7, as shown in figure 5, then placing a mica sheet 9 with a circular sample filling hole on the B gasket 2, ensuring that the sample filling hollow center is coaxial with the center of the anvil surface of the B anvil 6, and adding a sample 10PbTiO into the sample filling hole 3 As shown in fig. 6;
sixthly, the laminated body of the A gasket 1, the pressure transmitting powder 4, the ruby 8 and the A anvil 5 obtained in the fourth step is in close contact with the laminated body of the sample 10, the mica sheet 9, the B gasket 2 and the B anvil 6 obtained in the fifth step from the upper part in the DAC press, and the test is carried out after the ruby 8 passes the standard pressure, as shown in figure 7.
Wherein the ratio of the alcohol to the acetone is 2: 2; the diameter of the enameled wire 3 is 0.03 mm; the thickness of the mica sheet 9 with the round sample filling hole is 0.03 mm; with a circular shapeThe diameter of the sample filling hole of the mica sheet 9 of the sample filling hole is
Smaller than the diameter of the anvil surface imprints of the anvil A5 and the anvil B6; sample 10 in sample filling hole of mica sheet 9 with round sample filling hole was PbTiO 3 Filling the entire sample-filling hole 10.
Fig. 7 shows the device finally used for actually measuring the hysteresis loop.
According to the embodiment, the influence of the thickness and the area of the sample on the measurement of the hysteresis loop can be accurately controlled; and the problems of the material and mode of the cloth electrode, the insulating property of the device and the like in the experiment are avoided. The method not only can meet the requirement of real-time measurement, but also ensures the accuracy of the measurement of the hysteresis loop on the basis of simple operation.
Although embodiments of the present invention have been described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made herein without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.
Claims (6)
1. A method for measuring the electric hysteresis loop of a substance in a diamond anvil cell comprises the following steps:
Firstly, placing a gasket A (1) and a gasket B (2) in a mixed solution of alcohol and acetone for ultrasonic cleaning for 5-10 minutes;
secondly, drying the gasket A (1) and the gasket B (2) obtained by cleaning in the first step, selecting two enameled wires (3) with the same diameter and length, and respectively welding the two enameled wires (3) on the dried gasket A (1) and the dried gasket B (2) through a welding method to serve as test signal wires;
thirdly, placing the A gasket (1) and the B gasket (2) welded with the enameled wire (3) prepared in the second step on a B anvil (6), ensuring that the centroids of the A gasket (1) and the B gasket (2) are coaxially overlapped with the centroid of the B anvil (6), then stacking 0.05-0.15 g of pressure transmission powder (4) on the A gasket (1), then performing gasket prepressing through mutual extrusion of the A anvil (5) and the B anvil (6) in a DAC press, and taking down the prepressed A gasket (1) and the B gasket (2) from the middle of the A anvil (5) and the B anvil (6) for cleaning after the prepressing is completed;
fourthly, putting ruby (8) into the center of the shape of the pressure transfer powder (4) on the cleaned A gasket (1) after the prepressing in the third step, resetting the A gasket (1) with the ruby (8) after the prepressing on an A anvil (5) again, and fixing by using plasticine (7);
Fifthly, resetting the pre-pressed B gasket (2) on a B anvil (6) and fixing the B gasket by using plasticine (7), then placing a mica sheet (9) with a circular sample filling hole on the B gasket (2), ensuring that the center of the sample filling hole is coaxial with the center of the anvil surface of the B anvil (6), and adding a sample (10) into the sample filling hole;
and sixthly, in a DAC press, closely contacting the laminated body formed by the A gasket (1), the pressure transmission powder (4), the ruby (8) and the A anvil (5) obtained in the fourth step with the laminated body formed by the sample (10), the mica sheet (9), the B gasket (2) and the B anvil (6) obtained in the fifth step from the upper part, and testing after marking and pressing the ruby (8).
2. A method of measuring the hysteresis loop of a substance in a diamond anvil according to claim 1, wherein in the first step, the volume ratio of alcohol to acetone is between 2:3 and 3: 2.
3. The method for measuring the electric hysteresis loop of the substance in the diamond anvil cell according to claim 1, wherein the diameter of the enameled wire (3) is 0.03-0.13 mm.
4. The method for measuring the electric hysteresis loop of the substance in the diamond anvil cell according to claim 1, wherein the thickness of the mica sheet (9) is 0.02-1 mm.
5. A method for measuring the electric hysteresis loop of a substance in a diamond anvil according to claim 1, wherein the mica sheet (9)The diameter of the sample-filling hole of
Is smaller than the anvil surface indentation diameter of the anvil A (5) and the anvil B (6).
6. A diamond anvil cell electric hysteresis loop measuring method according to claim 1, wherein the sample (10) in the sample filling hole of the mica sheet (9) fills the whole sample filling hole.
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| CA2005622A1 (en) * | 1989-12-15 | 1991-06-15 | Patrick T.T. Wong | Infrared absorption spectra recording, high pressure sample holder |
| CN100545575C (en) * | 2007-04-09 | 2009-09-30 | 吉林大学 | The measuring method of thickness of sample on the adamas opposed anvils |
| 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 |
| CN103076501B (en) * | 2013-01-05 | 2016-03-23 | 吉林大学 | The measuring method of original position dielectric properties on diamond anvil cell |
| CN106501046B (en) * | 2016-12-06 | 2018-12-04 | 中国工程物理研究院流体物理研究所 | The assembly method of salt piece and sample is insulated in diamond anvil cell laboratory sample hole |
| CN110702018B (en) * | 2019-11-08 | 2021-04-16 | 吉林大学 | Device and method for measuring thickness of sample in diamond anvil cell |
| CN111918424B (en) * | 2020-08-10 | 2021-04-16 | 吉林大学 | Diamond anvil cell heating gasket and preparation method thereof |
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