CN106950444B - A kind of measuring method of ferroelectric materials electric hysteresis loop wire - Google Patents
A kind of measuring method of ferroelectric materials electric hysteresis loop wire Download PDFInfo
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- CN106950444B CN106950444B CN201710134572.2A CN201710134572A CN106950444B CN 106950444 B CN106950444 B CN 106950444B CN 201710134572 A CN201710134572 A CN 201710134572A CN 106950444 B CN106950444 B CN 106950444B
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- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
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Abstract
The present invention discloses a kind of measuring method of ferroelectric materials electric hysteresis loop wire, and ferroelectric material is placed on the object plane of cross-polarization imaging system by step 1;Step 2 makes its poling to positive (or reversed) electric field of ferroelectric material load, then gradually unloads/loads electric field circulation a cycle, record the ferroelectric domain structure under not same electric field;Domain wall when loading electric field poling is displaced sideways direction as ferroelectric domain direction of displacement by step 3, extracts the length vector on new farmlandIt willDisplacement as ferroelectric domain under the electric field;Step 4 extracts the relative displacement that the domain wall between electric field adjacent to each other is displaced sideways, then obtains the displacement of ferroelectric domain under not same electric fieldStep 5 draws the data described point measured, obtainsCurve.Compared with prior art, the present invention not only records domain structure of the ferroelectric material in polarization process in real time, but also obtains the ferroelectric hysteresis loop of characterization ferroelectric material characteristic, has the features such as simple and convenient, intuitive.
Description
Technical field
The invention belongs to the field of test technology of ferroelectric material, in particular to a kind of optically measurement ferroelectric material electricity
The measuring technology of hysteresis curves.
Background technique
Ferroelectric hysteresis loop is a ferroelectric mark.The basic principle for measuring ferroelectric materials electric hysteresis loop wire is by sample to be tested
It is considered as capacitor, obtains the polarization charge in test sample by measuring current or voltage.There are two types of measurement method is usual: impact inspection
Flowmeter scanning method and Sawyer-Tower circuit method.
Wherein, ballistic galvanometer scanning method is to utilize the charge generated in ballistic galvanometer record ferroelectric material polarization process
Amount, to obtain ferroelectric ferroelectric hysteresis loop.Electronic device needed for this method is more, more complicated.
Sawyer-Tower circuit method, also referred to as oscillograph method, by by ferroelectric material and the very big mark of capacitance
Pseudo-capacitance is connected in series, and the voltage at measurement standard capacitor both ends obtains ferroelectric ferroelectric hysteresis loop.This method is compared to impact inspection stream
Meter scanning method is easier, is the classical way for measuring ferroelectric hysteresis loop, and follow-up study person has done many improvement on this basis.
Above method belongs to electric measurement method, more with intrinsic electronic component in electrical measurement, circuit design is multiple
The disadvantages of miscellaneous, expensive, and not it is observed that in ferroelectric material domain structure with electric field variation.
Summary of the invention
The present invention proposes a kind of measuring method of ferroelectric materials electric hysteresis loop wire.This method is imaged based on cross-polarization
System, by measuring not same electric fieldUnder, displacement of the ferroelectric domain along domain wall lateral movement direction in polarization processTo obtain
The ferroelectric hysteresis loop of ferroelectric material.
A kind of measuring method of ferroelectric materials electric hysteresis loop wire of the invention, method includes the following steps:
Step 1 builds cross-polarization imaging system, ferroelectric material is placed at the object plane of cross-polarization imaging system,
Ferroelectric material constant temperature is controlled, and is at ferroelectric state;
Step 2 loads electric field to ferroelectric material using electric field loading system, when extra electric field is greater than material threshold electric field
When, new farmland generates, and domain wall setting in motion is gradually increased electric field to ferroelectric and is polarized to single domain state;Then unloading applied field-
The electric field of load and reversed electric field-load and this opposite direction added by this reversed electric field-unloading recycles a cycle, complete
At hysteresis, ferroelectric domain structure of the various process not under same electric field is recorded;
The domain structure that step 3, analytical procedure 2 are recorded, using load electric field poling when domain wall lateral movement direction as
Ferroelectric domain direction of displacement extracts the length vector on new farmland in the directionIt willDisplacement as ferroelectric domain under the electric field;
Step 4, the domain structure recorded to step 2 are used as initial position from new farmland generation place, extract electricity adjacent with new farmland
The relative displacement of domain wall lateral movement off fieldThen the displacement of ferroelectric domain is under the electric fieldAgain under the electric field
Farmland as initial position, extract the relative displacement that domain wall under electric field adjacent thereto is displaced sidewaysThen iron under its adjacent electric field
The displacement of electricdomain isI.e.Method according to this extracts the domain wall between electric field adjacent to each other
The relative displacement of lateral movementThe displacement that ferroelectric domain under any electric field then can be obtained isI.e.N=1 in formula, 2 ...,The displacement of ferroelectric domain under respectively adjacent two electric field;Work as domain wall
When lateral movement direction is identical as ferroelectric domain direction of displacement,Value is positive, when opposite with ferroelectric domain direction of displacement,Value is
It is negative;
Step 5, the data described point for obtaining step 4 are drawn, and ferroelectric domain displacement is obtainedWith extra electric fieldBetweenCurve;It, should according to dipole theoryCurve is the ferroelectric hysteresis loop of ferroelectric material.Change ferroelectric material
Test temperature obtains under different temperaturesCurve.
Ferroelectric domain displacement that is not collinear on direction along the step 3, obtainingIt is different, butCurve
Shape is identical.
The cartographic represenation of area of the step 3, its domain wall drift of the domain wall drift of ferroelectric domain described in 4, obtains it
Curve.
Compared with prior art, the present invention can both record domain structure of the ferroelectric material in polarization process in real time,
The ferroelectric hysteresis loop that can get characterization ferroelectric material characteristic has many advantages, such as simply, conveniently, intuitively, is ferroelectric material measuring technology
The research in field provides a kind of new method.
Detailed description of the invention
Fig. 1 is a kind of measuring method flow chart of ferroelectric materials electric hysteresis loop wire proposed by the present invention;
Fig. 2 is cross-polarization imaging system structural schematic diagram proposed by the present invention;
Appended drawing reference: 1, laser, 2, the polarizer, 3, crystal, 4, microcobjective, 5, analyzer, 6, CCD, 7, computer,
8, voltage-drop loading system, 9, temperature control system;
Fig. 3 be present example in Mn:Fe:KTN crystal poling and its unloading electric field when, E=0.0kV/cm,
Domain structure figure when 1.0kV/cm, 1.75kV/cm, 3.0kV/cm, 0.5kV/cm and 0.0kV/cm, in crystal.
Fig. 4 is Mn:Fe:KTN crystal measured in present exampleCurve graph.
Specific embodiment
Below by taking experiment optical path shown in Fig. 2 as an example, the specific measurement process of measurement method of the present invention is illustrated;
Step 1 builds cross-polarization imaging system.The cross-polarization imaging system includes laser 1, the polarizer 2, Mn:
Fe:KTN crystal 3, microcobjective (× 25) 4, analyzer 5, CCD 6, computer 7, voltage-drop loading system 8 and temperature control system
9.Wherein Mn:Fe:KTN crystal 3 is using the monocrystalline of top seed crystal flux method growth, having a size of 3.4(x)×2.0(y)×
0.94(z)mm3, Curie temperature is 27 DEG C, carries out optical polish, two electroplate electrode of xz and conducting wire on two surface xy.Electric field
It is loaded on crystal 3 along the y-axis direction by voltage-drop loading system 8, i.e.,Laser 1 is wavelength X=532nm
Semiconductor laser, the laser beam of sending reaches on CCD 6 through the polarizer 2, microcobjective 4, analyzer 5, at this moment the polarizer 2
It is orthogonal with analyzer 5, that is, it is in delustring state;After being put into crystal, crystal 3, microcobjective 4 and CCD 6 form imaging system,
It can observe that the ferroelectric domain structure in crystal, the enlargement ratio of this cross-polarization imaging system are 25 times on CCD.By crystal
3 are placed at the object plane of cross-polarization imaging system, keep crystal temperature effect to be constant at 25 DEG C using temperature control system 9, at this point,
The crystal is in ferroelectric state;
Step 2 gives crystal to load positive electric field, gradually increases electric field to 3.0kV/cm, at this time the complete poling of crystal, CCD6
Record the ferroelectric domain structure under not same electric field.(a) of Fig. 3-(d) gives extra electric field
Ferroelectric domain structure distribution when 1.0kV/cm, 1.75kV/cm and 3.0kV/cm, in crystal;
The domain structure under not same electric field is analyzed, as shown in Fig. 3 (a), when extra electric field is zero, the domain structure observed is
The spontaneous polarization farmland of crystal;As shown in Fig. 3 (b), work as extra electric fieldWhen, new farmland generates, which is threshold value
Electric field;As shown in Fig. 3 (c), work as extra electric fieldWhen, domain wall is displaced sideways, and part domain wall merges;Such as
Shown in Fig. 3 (d), work as extra electric fieldWhen, crystal is single domain state.If loading domain wall lateral movement side when electric field
To the positive direction (direction that solid arrow indicates in Fig. 3) being displaced as ferroelectric domain;
Step 3 is used as initial position from new farmland generation place, and the length arrow on new farmland is extracted along the dotted line position in Fig. 3 (b)
Amount, the vector length on new farmland is in viewing areaIt willAs electric fieldWhen ferroelectric domain displacement.As shown in Fig. 3 (c), mention
Take electric fieldWith electric fieldBetween domain wall lateral movement relative displacementThen electric fieldWhen, ferroelectric domain
DisplacementAs shown in Fig. 3 (d), electric field is extractedWithBetween domain wall lateral movement relative displacementThen electric fieldWhen, the displacement of ferroelectric domainI.e.For the displacement of crystal poling.Crystal list
Behind farmland, ferroelectric domain shift invariant.At this moment domain wall lateral movement direction is identical as the ferroelectric domain direction of displacement of setting,
For positive value.
At this moment step 4, the crystal poling after step 2 and 3 gradually unload electric field to crystal, record is not under same electric field
Ferroelectric domain structure.When single domain, the displacement of ferroelectric domainElectric field isElectric field is reduced to arrive Such as
Shown in Fig. 3 (e), electric field is extractedWithBetween domain wall lateral movement relative displacementThen electric fieldWhen,
The displacement of ferroelectric domainElectric field is reduced to arriveAs shown in Fig. 3 (f), electric field is extractedWithIt
Between domain wall be displaced sideways relative displacementThen electric fieldWhen, the displacement of ferroelectric domainI.e.At this moment domain wall lateral movement direction and setting ferroelectric domain direction of displacement on the contrary,For
Negative value.
Step 5, after step 4, gradually load reversed negative electric field to crystal, the record not ferroelectric domain structure under same electric field.
In electric fieldThe displacement of ferroelectric domainAs shown in Fig. 3 (f).Increase electric field to arriveExtract electricity
?WithBetween domain wall lateral movement relative displacementThen electric fieldWhen, the displacement of ferroelectric domainIncrease electric field to arriveThe reversed poling of crystal extracts electric fieldWithBetween domain wall side
To mobile relative displacementThen electric fieldWhen, the displacement of ferroelectric domainI.e.At this moment domain wall lateral movement direction and setting ferroelectric domain direction of displacement on the contrary,
For negative value.
Step 6, after step 5, negative electric field gradually unloaded to crystal, the record not ferroelectric domain structure under same electric field.When single domain,
The displacement of ferroelectric domainElectric field isElectric field is reduced to arriveExtract electric fieldWithBetween
The relative displacement of domain wall lateral movementThen electric fieldWhen, the displacement of ferroelectric domainDrop
Existing fringing field arrivesExtract electric fieldWithBetween domain wall lateral movement relative displacementThen electric fieldWhen, the displacement of ferroelectric domainI.e.At this moment domain wall is lateral
Moving direction is identical as the ferroelectric domain direction of displacement of setting,For positive value.
Step 7, after step 6, positive electric field gradually loaded again to crystal, the record not ferroelectric domain structure under same electric field.?
Electric fieldThe displacement of ferroelectric domainIncrease electric field to arriveExtract electric fieldWithBetween domain wall
The relative displacement of lateral movementThen electric fieldWhen, the displacement of ferroelectric domainIncrease electricity
Field is arrivedWhen, crystal forward direction poling extracts electric fieldWithBetween domain wall lateral movement relative displacementThen electric fieldWhen, the displacement of ferroelectric domainI.e.This
When domain wall lateral movement direction it is identical as the ferroelectric domain direction of displacement of setting,For positive value.
Step 8 will draw through the data described point that step 4-step 7 measures, and obtain ferroelectric domain displacementWith extra electric field
BetweenCurve, as shown in Figure 4.It, should according to dipole theoryCurve is the ferroelectric hysteresis loop of crystal.
Electric field interval is smaller,Curve data point is more,Curve is more smooth.
Claims (4)
1. a kind of measuring method of ferroelectric materials electric hysteresis loop wire, which is characterized in that method includes the following steps:
Step 1 builds cross-polarization imaging system, ferroelectric material is placed at the object plane of cross-polarization imaging system, control
Ferroelectric material constant temperature, and it is at ferroelectric state;
Step 2 loads electric field to ferroelectric material using electric field loading system, when extra electric field is greater than material threshold electric field, newly
Farmland generates, and domain wall setting in motion is gradually increased electric field to ferroelectric and is polarized to single domain state;Then unloading applied field-load with
The electric field of reversed electric field-load and this opposite direction added by this reversed electric field-unloading recycles a cycle, completes electric hysteresis
Loop testing, the record various process not ferroelectric domain structure under same electric field;
The domain structure that step 3, analytical procedure 2 are recorded, using domain wall lateral movement direction when loading electric field poling as ferroelectricity
Farmland direction of displacement extracts the length vector on new farmland in the directionIt willDisplacement as ferroelectric domain under the electric field;
Step 4, the domain structure recorded to step 2 are used as initial position from new farmland generation place, under extraction and new farmland adjacent electric field
The relative displacement of domain wall lateral movementThen the displacement of ferroelectric domain is under the electric fieldMade again with the farmland under the electric field
For initial position, the relative displacement that domain wall is displaced sideways under electric field adjacent thereto is extractedThen under its adjacent electric field ferroelectric domain position
Shifting isI.e.Method according to this extracts the domain wall lateral movement between electric field adjacent to each other
Relative displacementThe displacement that ferroelectric domain under any electric field then can be obtained isI.e.
N=1 in formula, 2 ...,The displacement of ferroelectric domain under respectively adjacent two electric field;When domain wall is displaced sideways direction and ferroelectricity
When farmland direction of displacement is identical,Value is positive, when opposite with ferroelectric domain direction of displacement,Value is negative;
Step 5, the data described point for obtaining step 4 are drawn, and ferroelectric domain displacement is obtainedWith extra electric fieldBetween
Curve;It, should according to dipole theoryCurve is the ferroelectric hysteresis loop of ferroelectric material.
2. a kind of measuring method of ferroelectric materials electric hysteresis loop wire as described in claim 1, which is characterized in that change ferroelectricity
Testing of materials temperature obtains under different temperaturesCurve.
3. a kind of measuring method of ferroelectric materials electric hysteresis loop wire as described in claim 1, which is characterized in that along the step
Ferroelectric domain displacement not collinear on direction in rapid 3, obtainingIt is different, butCurve shape is identical.
4. a kind of measuring method of ferroelectric materials electric hysteresis loop wire as described in claim 1, which is characterized in that the step
3, the cartographic represenation of area of its domain wall drift of the domain wall drift of ferroelectric domain described in 4, obtains itCurve.
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