CN101329375A - Device and method for measuring dielectric constant and dielectric loss of sample under low temperature and high voltage - Google Patents
Device and method for measuring dielectric constant and dielectric loss of sample under low temperature and high voltage Download PDFInfo
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- CN101329375A CN101329375A CNA2008101173290A CN200810117329A CN101329375A CN 101329375 A CN101329375 A CN 101329375A CN A2008101173290 A CNA2008101173290 A CN A2008101173290A CN 200810117329 A CN200810117329 A CN 200810117329A CN 101329375 A CN101329375 A CN 101329375A
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Abstract
The invention discloses a device and a method used for measuring the dielectric constant and the dielectric loss of samples under low temperature and high pressure. The measurement device comprises a pressure cell, a Be-Cu piston-typed press, a variable temperature system, a data collecting system and a data processing system; the method of the invention used for measuring the dielectric constant and the dielectric loss of the samples under low temperature and high pressure is characterized in that the Be-Cu piston-typed press applies quasi-hydrostatic pressure to the pressure cell; the variable temperature system and a dielectric property testing device are adjusted; by using a temperature measuring device and the dielectric property testing device to collect the capacitance and the dielectric loss of the samples under the temperature change and the frequency change of the samples, the variable frequency and variable temperature scanning curve line measurement is finally realized by the processing of a PC machine; the method of the invention changes the temperature and the frequency of the dielectric constant simultaneously, realizes the variable frequency and variable temperature scanning curve line measurement, and can research the effects of the quasi-hydrostatic pressure on the dielectric property of the ferroelectric samples by changing the externally applied quasi-hydrostatic pressure.
Description
Technical field
The present invention relates to the dielectric properties of dielectric sample under accurate hydrostatic conditions and measure, the measurement of particularly frequency conversion dielectric properties, room temperature arrives specific inductive capacity and the dielectric loss measurement mechanism and the method for sample under the temperature conditions of liquid nitrogen temperature.
Background technology
Ferroelectric material is in ferroelectric or antiferroelectric phase the time, can produce not overlapping of positive and negative charge center in that crystalline material is inner, thereby produces polarization orientation along direction of an electric field at material internal in extra electric field, thereby external manifestation goes out ferroelectric properties.And the space group that allows ferroelectric phase to exist does not all have symcenter.The hydrostatic pressing that adds can change unit cell volume, improves the symmetry of institute's test sample product crystal structure, thereby changes the size of its polarization intensity, with the mutually variable boundary of ferroelectric phase to paraelectric phase.For example defective, crystal boundary and doping factor for the proof theory prophesy, are necessary to carry out the research of the dielectric properties under the hydrostatic pressing simultaneously to the pinning effect of polarization for the Polarization Mechanism of test sample and sample interior.In addition, be in liquid nitrogen to the multi-iron material between the room temperature, can come the analysis of magnetic dielectric effect by the measurement of the specific inductive capacity under the pressure for magnetic phase transition.
Summary of the invention
At above-mentioned problem, the object of the present invention is to provide specific inductive capacity and the dielectric loss measurement mechanism and the method for sample under a kind of low temperature, the accurate hydrostatic conditions.
For achieving the above object, the specific inductive capacity of sample and dielectric loss measurement mechanism under the cryogenic high pressure of the present invention, comprise pressure born of the same parents, beryllium copper piston type press, temperature varying system, data acquisition system (DAS) and data handling system, described data acquisition system (DAS) comprises temperature measuring equipment and dielectric properties proving installation, described temperature measuring equipment is used for the temperature of collected specimens, and image data is transferred to data handling system; Described dielectric properties proving installation is used for the electric capacity and the loss of collected specimens, and image data is transferred to data handling system; Described pressure born of the same parents are arranged in the transformation chamber of beryllium copper piston type press, described pressure born of the same parents are by the polyfluortetraethylene pipe packaged sample, pressure transmitting medium and temperature collecting device constitute, the guide wire of drawing from the pressure born of the same parents links to each other with the dielectric properties proving installation with temperature measuring equipment respectively, described pressure born of the same parents are arranged in the pressurizing chamber of described beryllium copper piston type press, described beryllium copper piston type press is placed in the vessel of a good thermal conduction, these vessel are by unsettled being immersed in the Dewar flask that liquid nitrogen is housed of jacking gear, realize temperature control by the volatilization of liquid nitrogen and the adjusting of height, described data handling system is used for the data that the processing said data acquisition system transmits, obtain under the different temperatures and different frequency under the specific inductive capacity and the dielectric loss of sample.
Further, described polyfluortetraethylene pipe top and the bottom are provided with copper ring and copper cap respectively, keep the distance of 1mm between described sample and the temperature collecting device, guarantee not to be in contact with one another between the two.
Further, described pressure transmitting medium is kerosene and 1: 1 mixing material of silicone oil, and described temperature collecting device is thermopair or thermistor.
Further, in the described pressure born of the same parents an above thermopair or thermistor are set.
Further, described temperature measuring equipment and dielectric properties proving installation are respectively multifunctional digital source table KEITHLEY 2400 and Hewlett-Packard's instrument.
Further, can to control the temperature of sample be that room temperature arrives in the scope of liquid nitrogen temperature to described temperature varying system.
Further, the described Hewlett-Packard instrument frequency that can regulate sample changes in 5Hz-13MHz.
Further, the pressurization scope of described beryllium copper piston type press is at 0-2.5GPa.
Further, described data handling system is a PC, adopts I EEE-488 cable to link to each other with temperature measuring equipment with the dielectric properties proving installation, and the dress gpib interface card is realized central authorities' control in the PC, realizes automatic data acquisition with the VB6.0 Programming with Pascal Language.
The specific inductive capacity of sample and dielectric loss measuring method under the cryogenic high pressure of the present invention, be specially, sample thief, pressure transmitting medium and temperature collecting device, at first measure the surface area and the height of sample, then above-mentioned three kinds of article are encapsulated in decomposition pressure born of the same parents in the polyfluortetraethylene pipe, the pressure born of the same parents are applied accurate hydrostatic force, regulate pressure born of the same parents' temperature and frequency respectively by temperature varying system and dielectric properties proving installation, measure alternating temperature, the electric capacity of the sample under frequency conversion and the transformation and dielectric loss, the temperature information and the dielectric properties that collect are transferred to PC, through handling specific inductive capacity and the dielectric loss that obtains under the different temperatures.
Characteristic part of the present invention be designed that can match with beryllium copper piston type press, highly sensitive, system that can outside alternating temperature, and real-time observing and controlling sample temperature, be suitable in room temperature in the temperature range of liquid nitrogen temperature, can be under accurate hydrostatic force continuously evenly to ferroelectric sample variation probe temperature and the pressure born of the same parents that apply the liquid pressure transmitting medium of hydrostatic force.
The present invention has constructed the pressure system with beryllium copper piston type press on the special pressure born of the same parents' that realize accurate hydrostatic force basis, realize that original position steadily changes the system that the accurate hydrostatic force that is applied on the sample and real time altering are measured temperature continuously.
The present invention is the needs according to research ferroelectric material phase transformation under the original position hydrostatic pressing and research magnetic dielectric effect, set up one and can measure ferroelectric and many iron samples under the accurate hydrostatic force of original position in the measurement mechanism and the method for room temperature to the dielectric properties of the low temperature of liquid nitrogen temperature, the present invention changes the frequency of Measuring Dielectric Constant when changing temperature, realize the measurement of change frequency and transformation temperature scanning curve, by changing the accurate hydrostatic force that the outside applies, can study the influence of hydrostatic force to the dielectric properties of ferroelectric sample.
Description of drawings
Fig. 1 is a beryllium copper piston type compression system synoptic diagram of the present invention;
Fig. 2 is the frame diagram of measurement mechanism of the present invention;
Fig. 3 is the experimental curve diagram that measurement mechanism obtained among the embodiment;
Fig. 4 is the experimental curve diagram that measurement mechanism obtained among the embodiment.
Embodiment
As illustrated in fig. 1 and 2, the specific inductive capacity of sample and dielectric loss measurement mechanism comprise the pressure born of the same parents under the cryogenic high pressure of the present invention, beryllium copper piston type press, temperature varying system, thermistor 12, data acquisition system (DAS) and PC, described data acquisition system (DAS) comprises temperature measuring equipment and dielectric properties proving installation, temperature measuring equipment and dielectric properties proving installation adopt multifunctional digital source table KEITHLEY 2400 and Hewlett-Packard's instrument respectively, beryllium copper piston type press is formed the pressurization main frame by pressurization spiral shell button 1 and pressurizing chamber 2, hollow copper post 6 plays fixation pressure born of the same parents effect, and wherein copper post 3 is the pressure transmission parts that are connected press and pressure born of the same parents with tungsten carbide post 5.The pressure born of the same parents are by polyfluortetraethylene pipe 7 packaged sample 8, pressure transmitting medium 9 and thermistor 12 constitute, wherein suit copper ring 10 bottoms, polyfluortetraethylene pipe 7 top are provided with copper cap 11, it is in order to prevent when the pressure born of the same parents are pressurizeed that copper ring 10 is set, seal its mouth of pipe and be in when being under pressure because polyfluortetraethylene pipe top is circle, pressure concentrates on this place easily with polyfluortetraethylene pipe 7 crushing, one copper ring 10 is set at mouth of pipe place can prevents that this situation from taking place, polyfluortetraethylene pipe 7 bottoms are provided with copper cap 11 and are convenient to guide wire 14 installations, can guarantee that again the teflon duct occlusion is tight simultaneously.Pressure transmitting medium 9 is kerosene and 1: 1 mixing material of silicone oil, keep the distance about 1mm between sample 8 and the thermistor 12, guarantee that both do not contact with each other, sample 8 diameter dimensions can be between 3-4mm and are plated silver or gold electrode in the mode of plane-parallel capacitor at sample 8 two ends, drawing the coaxial enameled wire of drawing on coaxial enameled wire 13 and the thermistor 12 on it links to each other with multifunctional digital source table KEITHLEY 2400 by deriving respectively with the Hewlett-Packard instrument with the guide wire 14 that the pressure born of the same parents connect, this Hewlett-Packard's instrument links to each other by the IEEE-488 cable with PC with multifunctional digital source table KEITHLEY 2400 again, dress GPI B interface card is realized central authorities' control in the PC, realizes automatic data acquisition with the VB6.0 Programming with Pascal Language; The pressure born of the same parents are arranged in the pressurizing chamber 2 of beryllium copper piston type press, copper ring 10 and copper cap 11 that pressure born of the same parents' upper and lower end face is provided with, the pressure transmission that links to each other with hardness ratio is bigger in the beryllium copper piston type press tungsten carbide 5, wherein the tungsten carbide 5 that is provided with of pressure born of the same parents top connects pressure transmission copper billets 3 and is connected with the pressurization steel cylinder 4 of beryllium copper piston type press.Described beryllium copper piston type press is placed in the vessel of a good thermal conduction, these vessel are immersed in the Dewar flask that liquid nitrogen is housed, by suspension rod control vessel lifting and guarantee that these vessel do not touch described Dewar flask and constitute described temperature varying system, realize temperature control by the volatilization of liquid nitrogen and the adjusting of height.During the dielectric properties of measuring samples 8, control beryllium copper piston type press gives the pressure born of the same parents with accurate hydrostatic force, this accurate hydrostatic force can be selected applied pressure according to the beryllium copper piston type press of different tonnages, by the inner thermosensitive resistance measurement temperature that is provided with of pressure born of the same parents, temperature information after gathering is transferred to PC by multifunctional digital source table KEITHLEY 2400, simultaneously, utilize Hewlett-Packard's instrument to measure the electric capacity and the dielectric loss of the sample under the different frequency, and image data is transferred to PC; According to parameters such as institute's test sample product surface area and height, just can calculate specific inductive capacity and the dielectric loss of sample under frequency conversion, alternating temperature by PC.
The specific inductive capacity of sample and dielectric loss measuring method under the cryogenic high pressure of the present invention, be specially, sample thief, pressure transmitting medium and temperature collecting device, at first measure the surface area and the height of sample, then above-mentioned three kinds of article are encapsulated in decomposition pressure born of the same parents in the polyfluortetraethylene pipe, the pressure born of the same parents are applied accurate hydrostatic force, regulate pressure born of the same parents' temperature and frequency respectively by temperature varying system and dielectric properties proving installation, measure alternating temperature, the electric capacity of sample and dielectric loss under frequency conversion and the transformation, the temperature information and the dielectric properties that collect are transferred to PC, through handling specific inductive capacity and the dielectric loss that obtains under the different temperatures.
Embodiment 1:
Sample thief Bi (Fe
1/2Cr
1/2) O
3The polycrystalline multi-iron material, measure parameters such as the surface area of this sample and height, adopt said apparatus and method then, specific inductive capacity and dielectric loss under the frequency conversion obtain relenting, as Fig. 3 is specific inductive capacity-temperature scanning test result, illustrate that native system can obtain in room temperature between the liquid nitrogen temperature curve map of frequency range any frequency between 5Hz-13MHz.
Embodiment 2:
Sample thief BaTiO
3Nano ceramic material is measured parameters such as the surface area of this sample and height, adopts said apparatus and method then, specific inductive capacity and dielectric loss under the frequency conversion that obtains relenting, and that be that specific inductive capacity-temperature scanning test result provides as Fig. 4 is BaTiO
3Two phase transformation peaks of nano ceramic material are along with the variation of pressure.In the pressure limit of 0-2.5GPa, this system can provide the variation of dielectric phase transformation peak along with pressure accurately, and then provides the equipment support to analyzing the research of ferroelectric material Transformation Mechanism.
It should be noted that frequency can change because the tonnage of the press that uses is different with the model of Hewlett-Packard's instrument or LCR instrument, and pressure limit can be between 0-20GPa between 5Hz-110MHz.And specimen can be ferroelectric, and is antiferroelectric, dielectric, many iron, or the pottery of microwave or monocrystalline.Above in conjunction with the embodiments technical scheme of the present invention is had been described in detail, but those skilled in the art will find apparent that, on the technical solution of the present invention basis, can carry out variations and modifications to technical scheme of the present invention, for example can with four the lead-in wire methods come measuring samples resistance under different pressures with the variation of temperature curve.But do not break away from the scope that the present invention's claims required for protection are summarized.
Claims (10)
1. the specific inductive capacity of sample and dielectric loss measurement mechanism under the cryogenic high pressure, it is characterized in that, comprise pressure born of the same parents, beryllium copper piston type press, temperature varying system, data acquisition system (DAS) and data handling system, described data acquisition system (DAS) comprises temperature measuring equipment and dielectric properties proving installation, described temperature measuring equipment is used for the temperature of collected specimens, and image data is transferred to data handling system; Described dielectric properties proving installation is used for the electric capacity and the loss of collected specimens, and image data is transferred to data handling system; Described pressure born of the same parents are arranged in the transformation chamber of beryllium copper piston type press, described pressure born of the same parents are made of packaged sample, pressure transmitting medium and temperature collecting device on the polyfluortetraethylene pipe, the guide wire of drawing from temperature collecting device and sample links to each other with the dielectric properties proving installation with temperature measuring equipment respectively, described beryllium copper piston type press is placed in the vessel of a good thermal conduction, these vessel constitute described temperature varying system by unsettled being immersed in the Dewar flask that liquid nitrogen is housed of jacking gear, realize temperature control by the volatilization of liquid nitrogen and the adjusting of height; Described data handling system is used for the data that the processing said data acquisition system transmits, obtain under the different temperatures and different frequency under the specific inductive capacity and the dielectric loss of sample.
2. the specific inductive capacity of sample and dielectric loss measurement mechanism under the cryogenic high pressure as claimed in claim 1, it is characterized in that, described polyfluortetraethylene pipe top and the bottom are provided with copper ring and copper cap respectively, keep the distance of 1mm between described sample and the temperature collecting device, guarantee not to be in contact with one another between the two.
3. the specific inductive capacity of sample and dielectric loss measurement mechanism is characterized in that under the cryogenic high pressure as claimed in claim 1, and described pressure transmitting medium is kerosene and 1: 1 mixing material of silicone oil, and described temperature collecting device is thermopair or thermistor.
4. the specific inductive capacity of sample and dielectric loss measurement mechanism is characterized in that under the cryogenic high pressure as claimed in claim 3, and an above thermopair or thermistor are set in the described pressure born of the same parents.
5. the specific inductive capacity of sample and dielectric loss measurement mechanism is characterized in that under the cryogenic high pressure as claimed in claim 1, and described temperature measuring equipment and dielectric properties proving installation are respectively multifunctional digital source table KEITHLEY 2400 and Hewlett-Packard's instrument.
6. the specific inductive capacity of sample and dielectric loss measurement mechanism is characterized in that under the cryogenic high pressure as claimed in claim 1, and the temperature that described temperature varying system can be controlled sample is that room temperature arrives in the scope of liquid nitrogen temperature.
7. the specific inductive capacity of sample and dielectric loss measurement mechanism is characterized in that under the cryogenic high pressure as claimed in claim 1, and the pressurization scope of described beryllium copper piston type press is at 0-2.5GPa.
8. the specific inductive capacity of sample and dielectric loss measurement mechanism is characterized in that under the cryogenic high pressure as claimed in claim 5, and the frequency that described Hewlett-Packard instrument can be regulated sample changes in 5Hz-13MHz.
9. the specific inductive capacity of sample and dielectric loss measurement mechanism under the cryogenic high pressure as claimed in claim 1, it is characterized in that, described data handling system is a PC, adopt the IEEE-488 cable to link to each other with temperature measuring equipment with the dielectric properties proving installation, the dress gpib interface card is realized central authorities' control in the PC, realizes automatic data acquisition with the VB6.0 Programming with Pascal Language.
10. adopt the specific inductive capacity of sample under the measurement device cryogenic high pressure as claimed in claim 1 and the method for dielectric loss, it is characterized in that, be specially, sample thief, pressure transmitting medium and temperature collecting device, at first measure the surface area and the height of sample, then above-mentioned three kinds of article are encapsulated in decomposition pressure born of the same parents in the polyfluortetraethylene pipe, the pressure born of the same parents are applied accurate hydrostatic force, regulate pressure born of the same parents' temperature and frequency respectively by temperature varying system and dielectric properties proving installation, measure the electric capacity and the dielectric loss of sample under different temperatures and the different frequency, the temperature information and the dielectric properties that collect are transferred to PC, through handling specific inductive capacity and the dielectric loss that obtains under the different temperatures
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| CN2008101173290A CN101329375B (en) | 2008-07-29 | 2008-07-29 | Device and method for measuring dielectric constant and dielectric loss of sample under low temperature and high voltage |
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| CN102103166A (en) * | 2010-11-30 | 2011-06-22 | 西安交通大学 | Method for lossless detection on performance evaluation of ZnO piezoresistor |
| CN104407233A (en) * | 2014-12-02 | 2015-03-11 | 中国科学院广州能源研究所 | Device for testing dielectric property of hydrate in sediment |
| CN105911361A (en) * | 2016-04-13 | 2016-08-31 | 青岛大学 | Structural ceramic sample dielectric performance measuring device and method thereof |
| CN106707033A (en) * | 2016-12-08 | 2017-05-24 | 北京师范大学 | Variable-temperature dielectric constant measurement pool for liquid and solid-liquid phase change |
| CN108918976A (en) * | 2018-04-18 | 2018-11-30 | 杭州电子科技大学 | A kind of multichannel high-temperature dielectric temperature spectrum test device |
| CN109164303A (en) * | 2018-09-19 | 2019-01-08 | 东南大学 | Alternating temperature dielectric constant precision measurement apparatus and measurement method |
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| CN110031682A (en) * | 2019-03-22 | 2019-07-19 | 金华职业技术学院 | A kind of dielectric spectra measuring device |
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| CN113406397A (en) * | 2021-07-15 | 2021-09-17 | 中国科学院上海微系统与信息技术研究所 | Low-temperature solid dielectric constant measuring method |
| CN116380664A (en) * | 2023-04-14 | 2023-07-04 | 北京航空航天大学 | Bridgman piston pressurizing device for measuring comprehensive physical properties of sample |
| CN116381572A (en) * | 2023-04-18 | 2023-07-04 | 北京航空航天大学 | Bridgman piston cylinder ultrahigh hydrostatic pressure magnetic measurement device and method |
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2008
- 2008-07-29 CN CN2008101173290A patent/CN101329375B/en not_active Expired - Fee Related
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| CN102103166B (en) * | 2010-11-30 | 2013-07-10 | 西安交通大学 | Method for lossless detection on performance evaluation of ZnO piezoresistor |
| CN102103166A (en) * | 2010-11-30 | 2011-06-22 | 西安交通大学 | Method for lossless detection on performance evaluation of ZnO piezoresistor |
| CN104407233A (en) * | 2014-12-02 | 2015-03-11 | 中国科学院广州能源研究所 | Device for testing dielectric property of hydrate in sediment |
| CN104407233B (en) * | 2014-12-02 | 2017-10-27 | 中国科学院广州能源研究所 | Hydrate dielectric property test device in a kind of deposit |
| CN105911361A (en) * | 2016-04-13 | 2016-08-31 | 青岛大学 | Structural ceramic sample dielectric performance measuring device and method thereof |
| CN106707033A (en) * | 2016-12-08 | 2017-05-24 | 北京师范大学 | Variable-temperature dielectric constant measurement pool for liquid and solid-liquid phase change |
| CN106707033B (en) * | 2016-12-08 | 2019-06-21 | 北京师范大学 | A kind of alternating temperature dielectric constant measurement pond for liquid and solid-liquid phase change |
| CN108918976B (en) * | 2018-04-18 | 2020-11-27 | 杭州电子科技大学 | Multichannel high-temperature dielectric temperature spectrum testing device |
| CN108918976A (en) * | 2018-04-18 | 2018-11-30 | 杭州电子科技大学 | A kind of multichannel high-temperature dielectric temperature spectrum test device |
| CN109164303A (en) * | 2018-09-19 | 2019-01-08 | 东南大学 | Alternating temperature dielectric constant precision measurement apparatus and measurement method |
| CN109612700A (en) * | 2018-12-11 | 2019-04-12 | 东南大学 | Components Performance Test System under deep cooling hyperbaric environment |
| CN110031682A (en) * | 2019-03-22 | 2019-07-19 | 金华职业技术学院 | A kind of dielectric spectra measuring device |
| CN110031682B (en) * | 2019-03-22 | 2024-06-11 | 金华职业技术学院 | Dielectric spectrum measuring device |
| CN110160482A (en) * | 2019-04-26 | 2019-08-23 | 云南电网有限责任公司电力科学研究院 | The measurement method and device of cable insulation damaged area under a kind of hypobaric |
| CN111257704A (en) * | 2020-01-22 | 2020-06-09 | 同济大学 | Pressure cavity structure for measuring comprehensive dielectric property under high pressure and measuring method thereof |
| CN113406397A (en) * | 2021-07-15 | 2021-09-17 | 中国科学院上海微系统与信息技术研究所 | Low-temperature solid dielectric constant measuring method |
| CN113406397B (en) * | 2021-07-15 | 2022-07-08 | 中国科学院上海微系统与信息技术研究所 | Low-temperature solid dielectric constant measuring method |
| CN116380664A (en) * | 2023-04-14 | 2023-07-04 | 北京航空航天大学 | Bridgman piston pressurizing device for measuring comprehensive physical properties of sample |
| CN116381572A (en) * | 2023-04-18 | 2023-07-04 | 北京航空航天大学 | Bridgman piston cylinder ultrahigh hydrostatic pressure magnetic measurement device and method |
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