CN106747669B - A kind of high-curie temperature and the good potassium-sodium niobate-based transparent ferroelectric ceramics ceramic material and preparation method thereof of temperature stability - Google Patents

A kind of high-curie temperature and the good potassium-sodium niobate-based transparent ferroelectric ceramics ceramic material and preparation method thereof of temperature stability Download PDF

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CN106747669B
CN106747669B CN201611241556.5A CN201611241556A CN106747669B CN 106747669 B CN106747669 B CN 106747669B CN 201611241556 A CN201611241556 A CN 201611241556A CN 106747669 B CN106747669 B CN 106747669B
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杨祖培
柴启珍
晁小练
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Shaanxi Normal University
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Abstract

The invention discloses the good potassium-sodium niobate-based transparent ferroelectric ceramics ceramic material and preparation method thereof of a kind of high-curie temperature and temperature stability, the general formula of the ceramic material is (1-x) K0.5Na0.5NbO3‑xBa(Zn1/3Nb2/3)O3, x indicates Ba (Zn in formula1/3Nb2/3)O3Molal quantity, the value of x is 0.03~0.05, which is prepared by high temperature solid-state method.Preparation method of the present invention is simple, reproducible, high yield rate, the transparency of gained ceramic material is high, dielectric properties are good, Curie temperature is high, wherein transmitance is 66%~82% (near infrared region), dielectric constant is 1566~1813, Curie temperature is 344~395 DEG C, and in temperature within the scope of 30~500 DEG C, dielectric constant with temperature variation is small, with excellent temperature stability, while there is preferable ferroelectric properties, remanent polarization is 2~4 μ C/cm2, coercive field be 13~16kV/cm.

Description

A kind of high-curie temperature and the good potassium-sodium niobate-based transparent ferroelectric ceramics of temperature stability Material and preparation method thereof
Technical field
The invention belongs to ferroelectric ceramic material technical fields, and in particular to a kind of high-curie temperature and temperature stability are good Potassium-sodium niobate-based transparent ferroelectric ceramics ceramic material and preparation method thereof.
Background technique
Transparent ferroelectric ceramics is the extremely fierce new function material of a kind of important, international competition.Since it is with excellent Different ferroelectricity, mechanical performance and significant photoelectric effect, and also have high temperature resistant, corrosion-resistant, high rigidity and high transparency etc. special Property, so that such material is used double-deck goggles, tank transparent bulletproof composite armour, rocket projectile in nuclear tests personnel and aircrew Occupy extremely important status in the military affairs such as the shaped-charge plate armour of adapted, aviation field；Simultaneously also SAW device, swash The commercial field of the optical devices such as optical modulator, laser frequency multiplier, fiber waveguide device, optical holographic storage shows huge answer With potentiality, become the critical material in the indispensable following optical computer technology and modern advanced.
Since lead base transparent ferroelectric ceramics contains about 70%PbO or Pb3O4, production, using and it is discarded after it is processed It can all cause serious harm to the mankind and ecological environment in journey, therefore R and D novel lead-free transparent ferroelectric ceramics is for state The development of family's safety and electronic information field has great strategic significance.Japanese professor Saito is successfully prepared niobium within 2004 Sour potassium sodium (KNN) ceramics, piezoelectric constant have reached 490, while Curie temperature with higher, have reached 390 DEG C, become most It is hopeful to substitute the lead-free ceramics material of lead zirconate titanate (PZT) and lead magnesium niobate-lead titanate (PMN-PT) etc..Then, 2007 Du et al. is in research KNN-LiNbO3When have found its Transparency Phenomenon.And then the Du of in August, 2007 passes through doping Bi2O3, it is for the first time System has studied potassium-sodium niobate-based transparent lead-free ferroelectric ceramics.Later, potassium-sodium niobate-based ceramics cause the extensive pass of researcher Note.
But in the report in relation to potassium-sodium niobate base transparent ceramic, in order to obtain high transparency or high dielectricity Can, when by being doped modified to potassium-sodium niobate-based ceramics, Curie temperature all decreases, be difficult obtain high-curie temperature, The potassium-sodium niobate-based ceramics of high dielectric constant, high transparency.
Summary of the invention
It is a kind of normal with high transparency, high-curie temperature, high dielectric technical problem to be solved by the present invention lies in providing The preparation method of several and good temperature stability potassium-sodium niobate-based transparent ferroelectric ceramics ceramic material and the ceramic material.
Solving technical solution used by above-mentioned technical problem is: the composition general formula of the ceramic material is (1-x) (K0.5Na0.5)NbO3-xBa(Zn1/3Nb2/3)O3, x indicates Ba (Zn in formula1/3Nb2/3)O3Molal quantity, the value of x is 0.03~ 0.05。
Above-mentioned potassium-sodium niobate-based transparent ferroelectric ceramics ceramic material the preparation method is as follows:
1, ingredient
According to (1-x) (K0.5Na0.5)NbO3-xBa(Zn1/3Nb2/3)O3Stoichiometry weigh respectively purity be 99.99% Raw material Na2CO3、K2CO3、Nb2O5、BaCO3, ZnO, be uniformly mixed, raw mixture is fitted into nylon tank, with zirconium ball be grind Ball, dehydrated alcohol are ball-milling medium, are sufficiently mixed ball milling 18~24 hours, separating zirconium ball, by raw mixture at 80~100 DEG C Lower drying 12~24 hours crosses 80 meshes with mortar grinder.
2, pre-burning
Raw mixture after step 1 to be crossed to 80 meshes is placed in alumina crucible, is compacted with agate stick, is kept its compacting close Degree is 1.5g/cm3, cover, 850 DEG C pre-burning 5 hours, cooled to room temperature obtains pre-burning powder with mortar grinder.
3, secondary ball milling
Pre-burning powder is fitted into nylon tank, is ball-milling medium by abrading-ball, dehydrated alcohol of zirconium ball, be sufficiently mixed ball milling 12~ 24 hours, separating zirconium ball was 12~24 hours dry at 80~100 DEG C by pre-burning powder, with mortar grinder, crossed 160 meshes.
4, granulation and tabletting
The polyvinyl alcohol water solution that mass fraction is 5%, polyethylene are added in pre-burning powder after crossing from 160 meshes to step 3 The additional amount of alcohol solution is the 40%~50% of pre-burning silty amount, is granulated, and crosses 80~120 meshes, is suppressed with powder compressing machine At cylindric blank.
5, sintering is closed without densification
Cylindric blank is placed on zirconium oxide plate, zirconium oxide plate is placed in the closed saggar of aluminium oxide, first with 118 Minute is warming up to 500 DEG C, keeps the temperature 2 hours, then is warming up to 1130~1160 DEG C with 3 DEG C/min of heating rate, and sintering 5~8 is small When, with furnace cooled to room temperature.
6, it polishes
The sand paper polishing that the sintered ceramics of step 5 are chosen to 320 mesh of one of sample surfaces, then with 800 mesh Sand paper polishing, it is finally thick to 0.5~0.6mm with the sand paper of 1500 mesh and diamond polishing, be wiped over completely with alcohol.
7, silver ink firing
The silver paste that ceramic upper and lower surface coating thickness after step 6 polishing is 0.01~0.03mm, is placed in resistance furnace 840 DEG C keep the temperature 30 minutes, and cooled to room temperature is prepared into potassium-sodium niobate-based transparent ferroelectric ceramics ceramic material.
In above-mentioned steps 5,1150 DEG C preferably are warming up to 3 DEG C/min of heating rate, is sintered 6 hours.
Preparation method of the present invention is simple, reproducible, high yield rate, and the transparency of gained ceramic material is high, dielectric properties Good, Curie temperature height, wherein transmitance is 66%~82% (near infrared region), dielectric constant is 1566~1813, Curie temperature It is 344~395 DEG C, and is within the scope of 30~500 DEG C in temperature, dielectric constant with temperature variation is small, steady with excellent temperature It is qualitative, while there is preferable ferroelectric properties, remanent polarization is 2~4 μ C/cm2, coercive field be 13~16kV/cm.This Invention ceramic material optically isotropism, it is practical, be readily produced, electric property and optical property can be taken into account, be one The Lead-free transparent ferroelectric ceramics of kind function admirable.
Detailed description of the invention
Fig. 1 is the XRD diagram of the potassium-sodium niobate-based transparent ferroelectric ceramics ceramic material of Examples 1 and 2 preparation.
Fig. 2 is the transmitance figure of the potassium-sodium niobate-based transparent ferroelectric ceramics ceramic material of Examples 1 and 2 preparation.
Fig. 3 is dielectric constant of the potassium-sodium niobate-based transparent ferroelectric ceramics ceramic material of Examples 1 and 2 preparation at 1MHz with temperature The variation relation figure of degree.
Fig. 4 is Curie temperature of the potassium-sodium niobate-based transparent ferroelectric ceramics ceramic material at 1MHz and most of Examples 1 and 2 preparation Big dielectric constant with x value variation relation figure.
Fig. 5 is the ferroelectric hysteresis loop figure of the potassium-sodium niobate-based transparent ferroelectric ceramics ceramic material of Examples 1 and 2 preparation.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention is not limited only to These embodiments.
Embodiment 1
1, ingredient
According to 0.97 (K0.5Na0.5)NbO3-0.03Ba(Zn1/3Nb2/3)O3Stoichiometry weigh purity respectively and be 99.99% Na2CO33.9036g, the K that purity is 99.99%2CO35.0903g, the Nb that purity is 99.99%2O5 19.9834g, the BaCO that purity is 99.99%30.8991g, the ZnO 0.1236g that purity is 99.99%, are uniformly mixed, will Raw mixture is fitted into nylon tank, is ball-milling medium using zirconium ball as abrading-ball, dehydrated alcohol, dehydrated alcohol and raw mixture Mass ratio is 1:1.2, and with 401 revs/min of ball mill ball milling 24 hours, separating zirconium ball puts in a drying box raw mixture It is 10 hours dry at 80 DEG C, with mortar grinder 30 minutes, cross 80 meshes.
2, pre-burning
Raw mixture after step 1 to be crossed to 80 meshes is placed in alumina crucible, is compacted with agate stick, is kept its compacting close Degree is 1.5g/cm3, it covers, is placed in resistance furnace, 850 DEG C of pre-burnings 5 hours are warming up to 3 DEG C/min of heating rate, it is natural It is cooled to room temperature, comes out of the stove, with mortar grinder 10 minutes, obtain pre-burning powder.
3, secondary ball milling
Pre-burning powder is fitted into nylon tank, is ball-milling medium, dehydrated alcohol and pre-burning powder by abrading-ball, dehydrated alcohol of zirconium ball Mass ratio be 1:1.2, with 401 revs/min of ball mill ball milling 24 hours, separating zirconium ball puts in a drying box pre-burning powder It is 15 hours dry at 80 DEG C, with mortar grinder 10 minutes, cross 160 meshes.
4, granulation and tabletting
The polyvinyl alcohol water solution that mass fraction is 5%, polyethylene are added in pre-burning powder after crossing from 160 meshes to step 3 The additional amount of alcohol solution is the 50% of pre-burning silty amount, is granulated, and crosses 120 meshes, spherical powder is made, spherical powder is put into Diameter is to be compressed into the stainless steel mould of 15mm with powder compressing machine under the pressure of 300MPa with a thickness of 1.5mm's Cylindric blank.
5, sintering is closed without densification
Cylindric blank is placed on zirconium oxide plate, zirconium oxide plate is placed in the closed saggar of aluminium oxide, first with 118 Minute is warming up to 500 DEG C, keeps the temperature 2 hours, then is warming up to 1150 DEG C with 3 DEG C/min of heating rate, is sintered 6 hours, certainly with furnace So it is cooled to room temperature.
6, it polishes
The sand paper polishing that the sintered ceramics of step 5 are chosen to 320 mesh of one of surface, then with the sand of 800 mesh Paper polishing is finally wiped over completely to 0.5mm thickness with alcohol with the sand paper of 1500 mesh and diamond polishing.Using Rigaku MiniFlex600 type diffractometer carries out XRD test, carries out light using UV-3600 type UV, visible light near infrared light spectrophotometer Learn transmission measurement, the result is shown in Figure 1~2.
7, silver ink firing
The silver paste that ceramic upper and lower surface coating thickness after step 6 polishing is 0.02mm is placed in 840 DEG C of guarantors in resistance furnace Temperature 30 minutes, cooled to room temperature is prepared into 0.97 (K0.5Na0.5)NbO3-0.03Ba(Zn1/3Nb2/3)O3Ceramic material.It adopts With Agilient4980A type precise impedance analyzer and AixACCT-TF2000 sections electric parameter tester respectively to ceramic material Dielectric properties and ferroelectric properties tested, as a result see Fig. 3~5.
Embodiment 2
In the batching step 1 of the present embodiment, according to 0.95 (K0.5Na0.5)NbO3-0.05Ba(Zn1/3Nb2/3)O3Chemistry meter Amount weighs the Na that purity is 99.99% respectively2CO33.7776g, the K that purity is 99.99%2CO34.9260g, purity be 99.99% Nb2O519.6123g, the BaCO that purity is 99.99%31.4806g, the ZnO that purity is 99.99% 0.2036g, other steps are same as Example 1, are prepared into 0.95 (K0.5Na0.5)NbO3-0.05Ba(Zn1/3Nb2/3)O3Ceramic material Material.
As seen from Figure 1, the ceramic material of Examples 1 and 2 preparation is pure perovskite structure.From Figure 2 it can be seen that embodiment The higher transparency is presented in the ceramic material of 1 and 2 preparations, reaches as high as near infrared region (790~2000nm) transmitance 80% or more.By Fig. 3~5 as it can be seen that the ceramic material of Examples 1 and 2 preparation also has preferably while with high transparency Electric property, wherein when x=0.03, the dielectric constant of ceramic material is 1813, Curie temperature is 395 DEG C, residual polarization is strong Degree is 2 μ C/cm2, coercive field 13kV/cm, x=0.05 when, the dielectric constant of ceramic material is 1566, Curie temperature 344 DEG C, remanent polarization be 4 μ C/cm2, coercive field 16kV/cm, and gained ceramic material temperature be 30~500 DEG C of ranges Interior, dielectric constant with temperature variation is small, has excellent temperature stability.

Claims (3)

1. a kind of high-curie temperature and the good potassium-sodium niobate-based transparent ferroelectric ceramics ceramic material of temperature stability, it is characterised in that: should The general formula of ceramic material is (1-x) K0.5Na0.5NbO3-xBa(Zn1/3Nb2/3)O3, x indicates Ba (Zn in formula1/3Nb2/3)O3Mole Number, the value of x are 0.03~0.05；Transmitance of the ceramic material near infrared region is 66%~82%, and dielectric constant is 1566~1813, Curie temperature is 344~395 DEG C, remanent polarization is 2~4 μ C/cm2, coercive field be 13~16kV/cm.
2. a kind of preparation method of potassium-sodium niobate-based transparent ferroelectric ceramics ceramic material described in claim 1, it is characterised in that it by Following step composition:
(1) ingredient
According to (1-x) (K0.5Na0.5)NbO3-xBa(Zn1/3Nb2/3)O3Stoichiometry weigh respectively purity be 99.99% original Expect Na2CO3、K2CO3、Nb2O5、BaCO3, ZnO, be uniformly mixed, raw mixture is fitted into nylon tank, using zirconium ball as abrading-ball, Dehydrated alcohol is ball-milling medium, is sufficiently mixed ball milling 18~24 hours, separating zirconium ball, by raw mixture at 80~100 DEG C It is 12~24 hours dry, with mortar grinder, cross 80 meshes；
(2) pre-burning
Raw mixture after step (1) to be crossed to 80 meshes is placed in alumina crucible, is compacted with agate stick, is made its compacted density For 1.5g/cm3, cover, 850 DEG C pre-burning 5 hours, cooled to room temperature obtains pre-burning powder with mortar grinder；
(3) secondary ball milling
Pre-burning powder is fitted into nylon tank, is ball-milling medium by abrading-ball, dehydrated alcohol of zirconium ball, it is small to be sufficiently mixed ball milling 12~24 When, separating zirconium ball is 12~24 hours dry at 80~100 DEG C by pre-burning powder, with mortar grinder, crosses 160 meshes；
(4) granulation and tabletting
The polyvinyl alcohol water solution that mass fraction is 5% is added into the pre-burning powder after 160 meshes excessively, polyvinyl alcohol water solution Additional amount is the 40%~50% of pre-burning silty amount, is granulated, and crosses 80~120 meshes, is pressed into cylindric base with powder compressing machine Part；
(5) sintering is closed without densification
Cylindric blank is placed on zirconium oxide plate, zirconium oxide plate is placed in the closed saggar of aluminium oxide, first with 118 minutes 500 DEG C are warming up to, keeps the temperature 2 hours, then is warming up to 1130~1160 DEG C with 3 DEG C/min of heating rate, is sintered 5~8 hours, With furnace cooled to room temperature；
(6) it polishes
The sand paper polishing that the sintered ceramics of step (5) are chosen to 320 mesh of one of surface, then with the sand paper of 800 mesh Polishing is finally wiped over completely to 0.5~0.6mm thickness with alcohol with the sand paper of 1500 mesh and diamond polishing；
(7) silver ink firing
The silver paste that ceramic upper and lower surface coating thickness after step (6) polishing is 0.01~0.03mm, is placed in 840 in resistance furnace DEG C heat preservation 30 minutes, cooled to room temperature is prepared into potassium-sodium niobate-based transparent ferroelectric ceramics ceramic material.
3. the preparation method of potassium-sodium niobate-based transparent ferroelectric ceramics ceramic material according to claim 2, it is characterised in that: in step Suddenly in (5), cylindric blank is placed on zirconium oxide plate, zirconium oxide plate is placed in the closed saggar of aluminium oxide, first with 118 Minute is warming up to 500 DEG C, keeps the temperature 2 hours, then is warming up to 1150 DEG C with 3 DEG C/min of heating rate, is sintered 6 hours, certainly with furnace So it is cooled to room temperature.
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CN109180185B (en) * 2018-11-16 2021-03-23 陕西师范大学 Method for preparing high-energy-storage potassium-sodium niobate ferroelectric ceramic material in ultra-short time
CN109206137A (en) * 2018-11-19 2019-01-15 福州大学 A kind of preparation method of potassium-sodium niobate-zinc titanate strontium crystalline ceramics
CN113004038B (en) * 2021-03-25 2023-04-07 陕西师范大学 Sodium niobate-based lead-free ferroelectric ceramic material with high breakdown field strength and high photocurrent density and preparation method thereof
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102070337A (en) * 2010-10-29 2011-05-25 景德镇陶瓷学院 Low-temperature sintered potassium sodium niobate lead-free piezoelectric ceramic and preparation method thereof
WO2014123488A1 (en) * 2013-02-06 2014-08-14 Agency For Science, Technology And Research Electro-optic ceramic materials
CN105819856A (en) * 2016-03-14 2016-08-03 陕西师范大学 Potassium sodium niobate base lead free transparent ferroelectric ceramic material and preparation method thereof
CN105819855A (en) * 2016-03-14 2016-08-03 陕西师范大学 Bismuth magnesium niobate modified potassium sodium niobate transparent ferroelectric ceramic material and preparation method thereof adopting low purity raw materials

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102070337A (en) * 2010-10-29 2011-05-25 景德镇陶瓷学院 Low-temperature sintered potassium sodium niobate lead-free piezoelectric ceramic and preparation method thereof
WO2014123488A1 (en) * 2013-02-06 2014-08-14 Agency For Science, Technology And Research Electro-optic ceramic materials
CN105819856A (en) * 2016-03-14 2016-08-03 陕西师范大学 Potassium sodium niobate base lead free transparent ferroelectric ceramic material and preparation method thereof
CN105819855A (en) * 2016-03-14 2016-08-03 陕西师范大学 Bismuth magnesium niobate modified potassium sodium niobate transparent ferroelectric ceramic material and preparation method thereof adopting low purity raw materials

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