CN110308337A - A kind of the non-contact optical measuring device and method of ferroelectric crystal coercive field - Google Patents
A kind of the non-contact optical measuring device and method of ferroelectric crystal coercive field Download PDFInfo
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- CN110308337A CN110308337A CN201910636469.7A CN201910636469A CN110308337A CN 110308337 A CN110308337 A CN 110308337A CN 201910636469 A CN201910636469 A CN 201910636469A CN 110308337 A CN110308337 A CN 110308337A
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- 239000013078 crystal Substances 0.000 title claims abstract description 100
- 230000003287 optical effect Effects 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 25
- 230000005684 electric field Effects 0.000 claims abstract description 33
- 238000000691 measurement method Methods 0.000 claims abstract description 9
- 230000005540 biological transmission Effects 0.000 claims abstract description 4
- 238000002050 diffraction method Methods 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 230000011514 reflex Effects 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 2
- 230000005284 excitation Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 238000007689 inspection Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 230000005621 ferroelectricity Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000000149 argon plasma sintering Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000005422 blasting Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000009738 saturating Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229910019653 Mg1/3Nb2/3 Inorganic materials 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
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- 230000010287 polarization Effects 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R29/00—Arrangements for measuring or indicating electric quantities not covered by groups G01R19/00 - G01R27/00
- G01R29/08—Measuring electromagnetic field characteristics
- G01R29/0864—Measuring electromagnetic field characteristics characterised by constructional or functional features
- G01R29/0878—Sensors; antennas; probes; detectors
- G01R29/0885—Sensors; antennas; probes; detectors using optical probes, e.g. electro-optical, luminescent, glow discharge, or optical interferometers
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Abstract
A kind of the non-contact optical measuring device and method of ferroelectric crystal coercive field, are related to the technical field of optical detection of material properties, in order to solve the problems, such as that existing ferroelectric crystal electric measurement method is influenced vulnerable to contact condition, space charge or defect charge.Temperature-controlled box is equipped with 2 light holes, ferroelectric crystal is located in temperature-controlled box, the continuous laser of laser output is incident to ferroelectric crystal by a light hole, the light of ferroelectric crystal transmission is incident to the photosurface of photodetector by another light hole, the input terminal of the output end connection digital oscilloscope of photodetector, the transmitted intensity input terminal of the transmitted intensity output end connection computer of digital oscilloscope；Alternating-current voltage source is used to apply alternating voltage for ferroelectric crystal；Computer is used to control the frequency and amplitude of alternating-current voltage source output voltage, is also used to calculate the electric field of application, and stores the electric field of application and the transmitted intensity of digital oscilloscope output.The present invention is suitable for measuring the coercive field of ferroelectric crystal.
Description
Technical field
The present invention relates to the technical field of optical detection of material properties, and in particular to ferroelectric crystal coercive field it is contactless
Optical measuring technique.
Background technique
Ferroelectric crystal is a kind of multifunctional material, has excellent dielectric, piezoelectricity, electric light, Preset grating and acoustic properties,
The fields such as ferroelectric memory, large value capacitor, piezoelectric transducer, electrooptic modulator and ultrasonic transducer have important application.
The excellent macroscopic property of ferroelectric crystal and its microcosmic domain structure are closely related.Ferroelectric domain is that spontaneous polarization is identical inside ferroelectric crystal
Region, the microstructure that domain structure is made of the electricdomain of different orientation, so, understand ferroelectric domain characteristic be explore ferroelectricity
Crystal macroscopic property source and later period are modified the important prerequisite of design.The characteristic of ferroelectric domain, can be from static and dynamic two
Aspect measures.The measurement method of the static characteristic on farmland is more at present, for example, petrographic microscope, scanning electron microscope, thoroughly
Penetrate electron microscope and piezoelectricity force microscope etc., wherein petrographic microscope have micrometer resolution, scanning electron microscope and
Piezoelectricity force microscope etc. has hundred nano-scale resolution ratio, and transmission electron microscope has nanometer resolution.These belong to iron
The static measurement means of electricdomain.
About the dynamic measurement method of ferroelectric domain, currently used is that the ferroelectric hysteresis loop based on Sawyer-Tower circuit is surveyed
Examination method, to determine the coercive field of electricdomain overturning inside ferroelectric crystal.This method is convenient with sample preparation, it is simple etc. excellent to test
Point, but exist simultaneously several disadvantages.Disadvantage first is that Sawyer-Tower circuit test method is a kind of contact electrical measurement side
Method, the contact condition between test fixture and sample electrode have certain influence to the test result of coercive field；Disadvantage second is that this
It is a kind of charge acquisition formula test method, the space charge unrelated with ferroelectricity periodical poling or defect charge also can be to the surveys of coercive field
Test result has an impact, especially the more sample of internal flaw, there is a large amount of non-bound charge in sample, can to measure
As a result insincere, generate so-called " electric leakage " the phenomenon that occur；Disadvantage third is that when high temperature or low-frequency test, due to high temperature or low frequency
The migration of lower defect charge aggravates, and can measuring result error is further amplified.
Summary of the invention
The purpose of the present invention is to solve existing ferroelectric crystal electric measurement method vulnerable to contact condition, space charge or
The problem of defect charge influences, to provide the non-contact optical measuring device and method of a kind of ferroelectric crystal coercive field.
A kind of non-contact optical measuring device of ferroelectric crystal coercive field of the present invention, including alternating-current voltage source 1,
Temperature-controlled box 2, laser 3, photodetector 4, digital oscilloscope 5 and computer 6；
Temperature-controlled box 2 is equipped with 2 light hole 2-1, and ferroelectric crystal 7 is located in temperature-controlled box 2, the continuous laser that laser 3 exports
It is incident to ferroelectric crystal 7 by a light hole 2-1, the light that ferroelectric crystal 7 transmits is incident to light by another light hole 2-1
The photosurface of electric explorer 4, photodetector 4 output end connection digital oscilloscope 5 input terminal, digital oscilloscope 5 it is saturating
Penetrate the transmitted intensity input terminal of luminous intensity output end connection computer 6；
Alternating-current voltage source 1 is used to apply alternating voltage for ferroelectric crystal 7；
Computer 6 is used to control the frequency and amplitude of 1 output voltage of alternating-current voltage source, is also used to calculate the electric field of application,
And store the electric field of application and the transmitted intensity of the output of digital oscilloscope 5.
Preferably, the size of ferroelectric crystal 7 is greater than 2mm × 2mm × 0.5mm.
It preferably, further include reflecting mirror 8；
The continuous laser that laser 3 exports reflexes to ferroelectric crystal 7 through reflecting mirror 8.
It preferably, further include attenuator 9；
The continuous laser that laser 3 exports is incident to ferroelectric crystal 7 after 9 power attenuation of attenuator.
It preferably, further include the first convex lens 10；
First convex lens 10 focuses on continuous laser inside ferroelectric crystal 7.
It preferably, further include the second convex lens 11；
The light that ferroelectric crystal 7 transmits is focused on the photosurface of photodetector 4 by the second convex lens 11.
A kind of non-contact optical measurement method of ferroelectric crystal coercive field of the present invention, this method comprises:
Step 1: alternating-current voltage source 1 is that ferroelectric crystal 7 applies alternating voltage, the continuous laser that laser 3 exports is incident to
Ferroelectric crystal 7, computer 6 store the transmitted intensity that the electric field applied and digital oscilloscope 5 export；
Step 2: being ordinate by abscissa, normalized transmitted intensity of the electric field of application, by ordinate data pair
Transverse and longitudinal coordinate data seek first derivative and take absolute value, and maximum absolute value is worth the coercive field that corresponding electric field is ferroelectric crystal 7；
This method is realized based on a kind of non-contact optical measuring device of ferroelectric crystal coercive field.
Preferably, this method further include: crystallography orientation is carried out to ferroelectric crystal to be measured before step 1, is then pressed
Crystallographic direction is cut, then successively carries out the ferroelectric crystal 7 met the requirements by electrode and polishing treatment.
Compared to electrical detection method, optical detecting method has the advantages that non-contacting.Since optical wavelength only has hundred nanometers
Scale, when light wave is by ferroelectric crystal with domain structure, it may occur that the scattering phenomenon of light causes to be emitted from ferroelectric crystal
Luminous intensity is different from incident luminous intensity.Based on light scattering principle, when ferroelectric crystal is placed in the electric field of variation, electric field can draw
The state for playing farmland changes, so as to change scattering process of the electricdomain to light, when electric field reaches the coercive field of ferroelectric crystal
When, a large amount of farmland is begun turning, and at this moment light scattering effect is most obvious, can lead to the luminous intensity being emitted from ferroelectric crystal and occurs significantly
Change, the electric field at catastrophe point is exactly the coercive field of ferroelectric crystal.The great advantage of this non-contact method is can to eliminate
Influence of the movement of space charge inside ferroelectric crystal to measurement result, to obtain the coercive of true reflection ferroelectric domain overturning
?.
Light caused by the present invention is overturn with different application electric field stage farmlands, which scatters different methods, realizes ferroelectric crystal
The contactless accurate detection of coercive field.The detection method can also obtain the coercive field of the ferroelectric crystal under different temperatures, with
Just research coercive field variation with temperature rule.The present invention is suitable for measuring the coercive field of all transparent ferroelectric crystals.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the external electric field excitation system in specific embodiment；
Fig. 2 is the structural schematic diagram of the Systems for optical inspection in specific embodiment；
Fig. 3 is a kind of structural schematic diagram of the non-contact optical measuring device of ferroelectric crystal coercive field of the invention；
Fig. 4 is that the PMN-0.33PT relaxor ferroelectric crystal of embodiment [001] orientation is saturating in the case where applying dispatch from foreign news agency field excitation
Penetrate the normalized value of luminous intensity；
Fig. 5 is PMN-0.33PT relaxor ferroelectric crystal the returning in the case where applying dispatch from foreign news agency field excitation of embodiment [001] orientation
One transmitted intensity changed is to the absolute value for applying external electric field first derivative.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art without creative labor it is obtained it is all its
His embodiment, shall fall within the protection scope of the present invention.
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the present invention can phase
Mutually combination.
The present invention will be further explained below with reference to the attached drawings and specific examples, but not as the limitation of the invention.
A kind of non-contact optical measuring device of ferroelectric crystal coercive field of present embodiment, including dispatch from foreign news agency field excitation system
System and Systems for optical inspection；
External electric field excitation system: program control high voltage power supply (1 volt of precision), high-tension bus-bar, gpib bus, (the band light passing of temperature-controlled box 2
Hole), ferroelectric crystal 7 and computer 6.Alternating-current voltage source 1 is realized using program control high voltage power supply.Wherein, program control high voltage power supply passes through
Gpib bus is connect with computer 6, and the output control for realizing the alternating voltage of different frequency and amplitude is programmed by Labview
System.Ferroelectric crystal 7 is fixed in the temperature-controlled box 2 with light hole, germ nucleus is aligned with light hole center, and specific device is as schemed
Shown in 1.
Systems for optical inspection:
Including He-Ne laser, attenuator 9, reflecting mirror 8, the first convex lens 10, the second convex lens 11, photodetector 4,
Digital oscilloscope 5 and computer 6.First with the continuous laser that He-Ne laser output power is 50mW, wavelength is 633nm.When
Laser output power is higher, and the luminous intensity being incident on crystal is reduced using attenuator 9.In the lesser sample of test size
When, the method for the spot diameter for taking reduction to be irradiated in wafer surface issues laser using the first convex lens 10
Directional light is focused, so that the light beam through the first convex lens 10 is focused in crystals.From the light of another surface transmission of crystal
Enter photodetector after the convergence of the second convex lens 11, photodetector is connected with digital oscilloscope to detect and to acquire
Signal completes being automatically stored for data by computer 6, and Systems for optical inspection builds completion, and specific index path is as shown in Figure 2.
A kind of non-contact optical measurement method of ferroelectric crystal coercive field described in present embodiment, this method comprises:
Step 1: using X-ray diffractometer to ferroelectric crystal to be measured carry out crystallography orientation, then by crystallographic direction into
Row cutting, obtains crystal to be measured, it is desirable that crystalline size is greater than 2mm × 2mm × 0.5mm, and wherein 2mm thickness direction is ferroelectric crystal
Apply the direction of alternating electric field, 0.5mm thickness direction is the direction that laser passes through.Crystal distinguished by after Electrode treatment
Wafer surface is processed by shot blasting using 9 μm, 3 μm of grounds travel and 0.5 μm of diamond polishing liquid, keeps plane of crystal complete
Meet the needs of Experiments of Optics, obtains ferroelectric crystal 7.The too small electrode area that will lead to of crystalline size is small, not easy to handle therefore right
Crystal minimum dimension requires；The direction that the direction for using crystal most thin passes through for laser is conducive to improve light transmittance.
Step 2: alternating-current voltage source 1 is that ferroelectric crystal 7 applies alternating voltage, the continuous laser that laser 3 exports is incident to
Ferroelectric crystal 7, computer 6 store the electric field applied, at the same time, acquire the electric signal shown on digital oscilloscope 5 and record
The size of electric signal；
Step 3: being ordinate by abscissa, normalized transmitted intensity of the electric field of application, as shown in Figure 4.It will indulge
Coordinate data seeks first derivative to transverse and longitudinal coordinate data and takes absolute value, as shown in figure 5, becoming in the highest point corresponding diagram 4 in Fig. 5
Change violent position, electric field herein is the coercive field of ferroelectric crystal 7；
This method is realized based on a kind of non-contact optical measuring device of ferroelectric crystal coercive field.
Embodiment:
A kind of non-contact optical measurement method of ferroelectric crystal coercive field, this method comprises:
Step 1: using X-ray diffractometer to 0.67Pb (Mg1/3Nb2/3)O3-0.33PbTiO3(referred to as PMN-
0.33PT) ferroelectric crystal carries out crystallography orientation, is then cut by crystallographic direction, and the crystal of [001] orientation is obtained, brilliant
Body is having a size of 2mm × 3mm × 1mm, and wherein 2mm thickness direction is the direction that ferroelectric crystal applies alternating electric field, 1mm thickness direction
The direction passed through for laser.Crystal is carried out by after Electrode treatment, respectively using 9 μm, 3 μm of grounds travel and 0.5 μm of Buddha's warrior attendant
Stone polishing fluid is processed by shot blasting wafer surface, so that wafer surface is fully met the demand of Experiments of Optics, obtains ferroelectric crystal
7。
Step 2: computer control alternating voltage output frequency is 0.005Hz, alternating-current voltage source 1 is the application of ferroelectric crystal 7
Alternating voltage, the continuous laser that laser 3 exports are incident to ferroelectric crystal 7, and computer 6 stores the electric field applied, at the same time,
Acquire the electric signal shown on digital oscilloscope 5 and the size for recording electric signal；
Step 3: being ordinate by abscissa, normalized transmitted intensity of the electric field of application, Fig. 4 is [001] orientation
Transmitted intensity of the PMN-0.33PT relaxor ferroelectric crystal in the case where applying dispatch from foreign news agency field excitation normalized value, be oriented to the right side in figure
Arrow correspond to the curve that electric field gradually rises, be oriented to left arrow and correspond to the curve that electric field gradually decreases.Electric field is increased
Ordinate data in the process seek first derivative to abscissa data and take absolute value, and Fig. 5 is the PMN-0.33PT of [001] orientation
Normalized transmitted intensity of the relaxor ferroelectric crystal in the case where applying dispatch from foreign news agency field excitation is absolute to application external electric field first derivative
Value.The corresponding electric field in highest point in Fig. 5 is 180V/mm, changes most violent position in corresponding diagram 4, this electric field is PMN-
The coercive field E of 0.33PT ferroelectricity chipc。
This method is realized based on a kind of non-contact optical measuring device of ferroelectric crystal coercive field.
Claims (8)
1. a kind of non-contact optical measuring device of ferroelectric crystal coercive field, which is characterized in that including alternating-current voltage source (1),
Temperature-controlled box (2), laser (3), photodetector (4), digital oscilloscope (5) and computer (6)；
Temperature-controlled box (2) is equipped with 2 light holes (2-1), and ferroelectric crystal (7) is located in temperature-controlled box (2), the company of laser (3) output
Continuous laser is incident to ferroelectric crystal (7) by a light hole (2-1), and the light of ferroelectric crystal (7) transmission passes through another light passing
Hole (2-1) is incident to the photosurface of photodetector (4), and the output end of photodetector (4) connects the defeated of digital oscilloscope (5)
Enter end, the transmitted intensity input terminal of transmitted intensity output end connection computer (6) of digital oscilloscope (5)；
Alternating-current voltage source (1) is used to apply alternating voltage for ferroelectric crystal (7)；
Computer (6) is used to control the frequency and amplitude of alternating-current voltage source (1) output voltage, is also used to calculate the electric field of application,
And store the electric field of application and the transmitted intensity of digital oscilloscope (5) output.
2. a kind of non-contact optical measuring device of ferroelectric crystal coercive field according to claim 1, which is characterized in that
The size of the ferroelectric crystal (7) is greater than 2mm × 2mm × 0.5mm.
3. a kind of non-contact optical measuring device of ferroelectric crystal coercive field according to claim 1, which is characterized in that
It further include reflecting mirror (8)；
The continuous laser of laser (3) output reflexes to ferroelectric crystal (7) through reflecting mirror (8).
4. a kind of non-contact optical measuring device of ferroelectric crystal coercive field according to claim 1, which is characterized in that
It further include attenuator (9)；
The continuous laser of laser (3) output is incident to ferroelectric crystal (7) after attenuator (9) power attenuation.
5. a kind of non-contact optical measuring device of ferroelectric crystal coercive field according to claim 1, which is characterized in that
It further include the first convex lens (10)；
It is internal that first convex lens (10) makes continuous laser focus on ferroelectric crystal (7).
6. a kind of non-contact optical measuring device of ferroelectric crystal coercive field according to claim 1, which is characterized in that
It further include the second convex lens (11)；
The light that ferroelectric crystal (7) transmits is focused on the photosurface of photodetector (4) by the second convex lens (11).
7. a kind of non-contact optical measurement method of ferroelectric crystal coercive field, which is characterized in that this method comprises:
Step 1: alternating-current voltage source (1) is that ferroelectric crystal (7) apply alternating voltage, the continuous laser of laser (3) output is incident
To ferroelectric crystal (7), the transmitted intensity of electric field and digital oscilloscope (5) output that computer (6) storage applies；
Step 2: being ordinate by abscissa, normalized transmitted intensity of the electric field of application, by ordinate data to transverse and longitudinal
Coordinate data seeks first derivative and takes absolute value, and the corresponding electric field of maximum absolute value value is the coercive field of ferroelectric crystal (7)；
This method is measured based on a kind of non-contact optical of ferroelectric crystal coercive field described in above-mentioned any one claim
Device is realized.
8. a kind of non-contact optical measurement method of ferroelectric crystal coercive field according to claim 7, which is characterized in that
This method further include: crystallography orientation is carried out to ferroelectric crystal to be measured before step 1, is then cut by crystallographic direction
It cuts, then successively carries out the ferroelectric crystal (7) met the requirements by electrode and polishing treatment.
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| CN113092824A (en) * | 2020-05-05 | 2021-07-09 | 台湾积体电路制造股份有限公司 | Method for detecting ferroelectric signals and piezoelectric force microscope device |
| CN113176455A (en) * | 2021-04-23 | 2021-07-27 | 西安交通大学 | Device and method for measuring piezoelectric performance parameters of ferroelectric crystal under strong electric field |
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