CN103234914A - Ferroelectric material Curie point measuring method based on ellipsometer - Google Patents
Ferroelectric material Curie point measuring method based on ellipsometer Download PDFInfo
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- CN103234914A CN103234914A CN2013101355730A CN201310135573A CN103234914A CN 103234914 A CN103234914 A CN 103234914A CN 2013101355730 A CN2013101355730 A CN 2013101355730A CN 201310135573 A CN201310135573 A CN 201310135573A CN 103234914 A CN103234914 A CN 103234914A
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Abstract
The invention belongs to the technical field of thermal measuring, and specifically relates to a ferroelectric material Curie point measuring method based on an ellipsometer. According to the invention, ferroelectric material optical properties under different temperatures are measured by using the ellipsometer; according to a principle that the ferroelectric material optical property changes when the ferroelectric material is converted from ferroelectric phase to non-ferroelectric phase, ferroelectric material temperature transition point which is also the Curie point is obtained. With the method provided by the invention, rapid, nondestructive, and precise measuring of ferroelectric material Curie point is realized. The method has wide application prospect in various fields such as physics, chemistry, biomedicine, environmental science, and the like.
Description
Technical field
The invention belongs to the calorifics field of measuring technique, be specifically related to a kind of method of utilizing ellipsometer measurement ferroelectric material Curie point.
Background technology
The Curie point of accurately measuring ferroelectric material is the important technology of research ferroelectric material character.When the temperature of ferroelectric material was lower than Curie point, ferroelectric material was in ferroelectric phase, had good ferroelectricity; And when temperature was higher than Curie point, the ferroelectricity of ferroelectric material disappeared, and was in paraelectric phase, was as good as with the general linear dielectric material.Curie point has directly determined the actual maximum operating temperature of ferroelectric integrated device like this.The method of traditional measurement ferroelectric material Curie point is based on the measurement of ferroelectric materials electric hysteresis loop wire: change under the ferroelectric material temperature, measure its ferroelectric hysteresis loop, the temperature of correspondence is Curie temperature (Curie point) when ferroelectric hysteresis loop disappears.Though this method is intuitively but kept away the upper surface of unavoidable destruction ferroelectric material, because the measurement of ferroelectric hysteresis loop need be at ferroelectric material upper and lower surface growth upper/lower electrode.Moreover, this method many times can't be measured because the leakage current of ferroelectric material is excessive.And elliptic polarization spectrometer (ellipsometer) is a kind of noncontact, non-destruction, measuring method fast, it can be by measuring the optical characteristics that accurately obtains sample through the change of sample reflection rear polarizer polarization state of light, such metering system does not just need upper/lower electrode fully, not only avoid to measure owing to leakage current the embarrassment of Curie point, but also eliminated the influence of " dead band layer " between ferroelectric material and metal electrode.These advantages make this method almost be applicable to the measurement of the Curie point of all ferroelectric materials.Therefore the present invention utilizes ellipsometer can measure the optical constant of ferroelectric material in real time under different temperatures, variation reflection ferroelectric material changes of crystal by optical constant, i.e. transformation from ferroelectric phase to paraelectric phase, corresponding transition temperature are measures required ferroelectric material Curie point.
Summary of the invention
The object of the present invention is to provide a kind of method of can non-ly destroying, reaching fast accurate measurement ferroelectric material Curie point.
The measuring method of the ferroelectric material Curie point based on ellipsometer provided by the present invention, its concrete measuring process is as follows:
(1) at first, utilize the p light of ferroelectric material under the reflective ellipsometer measurement different temperatures, ratio tan Ψ and the phase delay delta of s reflection of light rate;
(2) ellipsometric parameter Ψ, the Δ by measuring then calculates refractive index n, extinction coefficient k and the DIELECTRIC CONSTANT of material
1, ε
2
For the body material, can try to achieve by following formula:
（3）
Wherein ρ is an intermediate variable, and e is the nature truth of a matter, and θ is incident angle, ε
0Be dielectric constant of air;
(3) the calculating optical constant is with the variation of temperature rate, d Ψ/dT, d Δ/dT, dn/dT, dk/dT, d ε
1/ dT and d ε
2/ dT;
(4) relatively optical constant is composed with variation of temperature, and rate of change composes with variation of temperature, determines the Curie point of tested ferroelectric material by observing sudden change.
The present invention utilizes the noncontact of measuring method, non-destruction, characteristics fast, based on optical property and the structure of material inseparable relation is arranged, and changes and the essence of ferroelectric material from the ferroelectric phase transition to the paraelectric phase is its crystal structure.This method is mainly utilized the optical constant of ellipsometer measurement sample, reflects the change of ferroelectric material crystal structure by the change of optical constant, thereby obtains the Curie point of ferroelectric material.
The ultimate principle of the inventive method is as follows:
The flashlight of a branch of known polarization attitude incides tested ferroelectric sample surfaces, and light beam and sample are had an effect, and makes radiative polarization state change (native system for become elliptical polarization by linear polarization).Because polarization state of light changes with sample structure substantial connection is arranged, by measuring the variation of polarization state, can inverting obtain structures of samples information.And the most direct reflection of structural information is exactly the optical constant of material.Utilize ellipsometer, just can measure the optical constant of ferroelectric material under the different temperatures.Because temperature can influence the energy of electronics and phonon in the material, thereby influence the interaction of photon and electroacoustic, and then change the optical characteristics of material, so the optical constant of material varies with temperature and changes.The character of material itself is depended in this variation, and in general, for ferroelectric material, its optical constant depends primarily on electronic transition and lattice vibration with variation of temperature with variation of temperature.Yet ferroelectric material changes paraelectric phase into from ferroelectric phase, is essential variation has taken place on the structure, and namely dipole is unordered for polarization from the polarization ordering transition in its crystal, and just temperature can be destroyed the order that dipole is arranged in the ferroelectric material.Dipole is in complete disordered state in ferroelectric material, and showing as remanent polarization on the macroscopic view is zero, and namely ferroelectricity disappears, and can't measure ferroelectric hysteresis loop on the electricity, and the complete fail temperature of its correspondence is the Curie point of ferroelectric material.Therefore the optical constant of ferroelectric material can be undergone mutation at the Curie point place with the variation of temperature curve.Utilize this principle, by observing the generation of this sudden change, thereby can determine the Curie point of ferroelectric material.As shown in Figure 1.
The invention has the advantages that can quick, non-destruction, accurately measure the Curie point of ferroelectric material, is with a wide range of applications in various fields such as physics, chemistry, biomedicine, bad border science.
Description of drawings
Fig. 1 is the principle of work synoptic diagram of typical reflective elliptic polarization spectrometer.
Fig. 2 is that the extinction coefficient k of PZT ferroelectric material is with the variation of temperature curve.
Number in the figure: 1 is light source, and 2 is the polarizer, and 3 is the sample platform, and 4 is analyzer, and 5 is detector, and 6 is temperature controller, and 7 is thermal resistance, and 8 is K type thermocouple, and 9 is relay, and 10 is power supply.
Embodiment
Below by this example of Curie point of measuring the PZT ferroelectric material concrete implementing method of the present invention is described.
1, utilizes the PZT ferroelectric thin film of about 2000 nanometer thickness of Prepared by Sol Gel Method one deck.
2, measure with elliptic polarization spectrometer then.As shown in Figure 1, wherein the sample platform carries a temperature control equipment, by thermal resistance the copper sample platform is heated, then by the temperature of K type thermocouple measurement sample platform and feed back to temperature controller, again by the temperature controller pilot relay so that control thermal resistance power supply, thereby reach temperature controlled effect.
3, the reflection angle of Ce Lianging is 65 °, and lambda1-wavelength is 300 nanometers, and extinction coefficient k varies with temperature figure, and temperature range is 50-275 ℃, approximately per 25 ℃ of measurements once, as shown in Figure 2.
4, as can see from Figure 2, k tangible peak value occurs with variation of temperature, and the temperature that this peak value takes place is about 248 ℃, and is approaching with 223 ℃ of the actual Curie points of PZT, proved the feasibility of this method.
5, the measuring accuracy of the Curie point of this method depends on the precision of temperature controller and the interval temperature of measurement, and the precision of temperature controller is 0.1 ℃ in this example, and measuring is 25 ℃ at interval, so measuring accuracy is 25 ℃.
In sum, the present invention proposes a kind of measuring method of the ferroelectric material Curie point based on ellipsometer, and the PZT ferroelectric material of collosol and gel preparation is example, verified the feasibility of this method.This method has quick, non-destruction, advantage such as can accurately measure.Be with a wide range of applications in various fields such as physics, chemistry, biomedicine, environmental sciences.
Claims (1)
1. measuring method based on the ferroelectric material Curie point of ellipsometer is characterized in that concrete steps are:
(1) at first, utilize the p light of ferroelectric material under the reflective ellipsometer measurement different temperatures, ratio tan Ψ and the phase delay delta of s reflection of light rate;
(2) ellipsometric parameter Ψ, the Δ by measuring then calculates refractive index n, extinction coefficient k and the DIELECTRIC CONSTANT of material
1, ε
2
For the body material, can try to achieve by following formula:
Wherein ρ is an intermediate variable, and e is the nature truth of a matter, and θ is incident angle, ε
0Be dielectric constant of air;
(3) the calculating optical constant is with the variation of temperature rate, d Ψ/dT, d Δ/dT, dn/dT, dk/dT, d ε
1/ dT and d ε
2/ dT;
(4) compose with variation of temperature by optical constant relatively, with and rate of change compose with variation of temperature, determine the Curie point of tested ferroelectric material by observing sudden change.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106950444A (en) * | 2017-03-08 | 2017-07-14 | 天津大学 | A kind of measuring method of ferroelectric materials electric hysteresis loop wire |
| CN108593563A (en) * | 2018-05-15 | 2018-09-28 | 中国科学院福建物质结构研究所 | Optical material test method and optic analytical instrument used |
| CN110376136A (en) * | 2019-07-19 | 2019-10-25 | 华中科技大学 | The device and method of the lower measurement thin-film optical constant of high temperature load and structural parameters |
| CN111693561A (en) * | 2020-05-28 | 2020-09-22 | 复旦大学 | Method and system for measuring ignition point of nano material |
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| CN1253286A (en) * | 1999-12-15 | 2000-05-17 | 谭成忠 | Phase-change temp measurer |
| CN102507040A (en) * | 2011-11-10 | 2012-06-20 | 复旦大学 | Thin film temperature measurement method based on ellipsometer |
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2013
- 2013-04-18 CN CN2013101355730A patent/CN103234914A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1253286A (en) * | 1999-12-15 | 2000-05-17 | 谭成忠 | Phase-change temp measurer |
| CN102507040A (en) * | 2011-11-10 | 2012-06-20 | 复旦大学 | Thin film temperature measurement method based on ellipsometer |
Non-Patent Citations (4)
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| M. ERBER 等: "Variations in the glass transition temperature of polyester with special architectures confined in thin films", 《POLYMER》 * |
| M. ERBER 等: "Variations in the glass transition temperature of polyester with special architectures confined in thin films", 《POLYMER》, vol. 51, 31 January 2010 (2010-01-31) * |
| 张荣君等: "反射式 RAP 型椭圆偏振光谱仪及其应用", 《实验室研究与探索》 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106950444A (en) * | 2017-03-08 | 2017-07-14 | 天津大学 | A kind of measuring method of ferroelectric materials electric hysteresis loop wire |
| CN108593563A (en) * | 2018-05-15 | 2018-09-28 | 中国科学院福建物质结构研究所 | Optical material test method and optic analytical instrument used |
| CN110376136A (en) * | 2019-07-19 | 2019-10-25 | 华中科技大学 | The device and method of the lower measurement thin-film optical constant of high temperature load and structural parameters |
| CN111693561A (en) * | 2020-05-28 | 2020-09-22 | 复旦大学 | Method and system for measuring ignition point of nano material |
| CN111693561B (en) * | 2020-05-28 | 2023-02-10 | 复旦大学 | Method and system for measuring ignition point of nano material |
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Application publication date: 20130807 |