CN107253859B - Luminous ferroelectric ceramic material of the Eu-Bi codope tungsten bronze structure of high-incidence photo and thermal stability and preparation method thereof - Google Patents
Luminous ferroelectric ceramic material of the Eu-Bi codope tungsten bronze structure of high-incidence photo and thermal stability and preparation method thereof Download PDFInfo
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Abstract
The invention discloses luminous ferroelectric ceramic materials of the Eu-Bi codope tungsten bronze structure of a kind of high-incidence photo and thermal stability and preparation method thereof, and the general structure of the ceramic material is Sr1.90Ca0.15Na0.81‑3xEuyBixNb5O15, wherein the value of x is 0.003~0.008, the value of y is 0.02~0.06, and conventional high-temperature solid phase method is used to be prepared, and preparation method is low in cost, easy to operate.The present invention in ceramic material by adulterating Eu and Bi, not only make it have luminescent properties, and significantly improve its thermal stability that shines, and improve its Dielectric, Ferroelectric performance, wherein when x=0.005, y=0.03, its thermal stability that shines is 67%, and maximum dielectric constant is 1345, Curie temperature is 272 DEG C, remanent polarization is 4.29 μ C/cm2, coercive field 21.41kV/cm.
Description
Technical field
The invention belongs to technical field of ceramic material, and in particular to a kind of Eu-Bi codope tungsten of high-incidence photo and thermal stability
Luminous ferroelectric ceramic material of bronze structures and preparation method thereof.
Background technique
In recent years, unleaded weight electric material is also storing up other than research improves weight electrical property to substitute lead-containing materials
The new functional characteristic of energy, strain, electric card, thermoelectricity, photoelectricity, luminous etc. discovery, receives more and more attention it.Tungsten is green
Copper system is an important branch indispensable in unleaded weight electric material system, and composition general formula is (A1)2(A2)4C4(B1)2
(B2)8O30, different metal cation selectively occupies A1, A2, B1, B2 and C this 5 kinds of non-equivalence according to its radius and valence state
Crystallography interstitial site, the filling situation for adjusting crystallography interstitial site can induce flexible and changeable architectural characteristic and function out
Characteristic.Research group where inventor passes through the determination study for adjusting Na tungsten bronze using conventional solid-state method
(Sr0.925Ca0.075)2.5-0.5xNaxNb5O15Architecture and performance contact, as a result, it has been found that structure closer to be full of type when its
Performance is more excellent, but is easy to produce the second phase and deteriorates electric property.And the ceramic material only has electric property, it is contemplated that
Material high-intelligentization at present, highly integrated development, this material property is single, limits its application, is unable to satisfy newest material
Design concept.
Summary of the invention
Technical problem to be solved by the present invention lies in provide one kind to be provided simultaneously with electrical property and luminescent properties and the heat that shines
The high Eu-Bi codope tungsten bronze structure of stability shines ferroelectric ceramic material, and provides a kind of simple process, repeatability for it
Good, low-cost preparation method.
The structural formula for solving ceramic material used by above-mentioned technical problem is Sr1.90Ca0.15Na0.81-3xEuyBixNb5O15,
Wherein the value of x is 0.003~0.008, the value of y is 0.02~0.06, and preferably the value of x is 0.005, the value of y is
0.03。
The luminous ferroelectric ceramic material preparation method of Eu-Bi codope tungsten bronze structure of the present invention is made of following step:
1, according to Sr1.90Ca0.15Na0.81-3xEuyBixNb5O15Stoichiometric ratio weigh respectively purity be 99.00% or more
Na2CO3、SrCO3、Nb2O5、CaCO3、Eu2O3、Bi2O3, ball milling is sufficiently mixed 16~24 hours, dry 12 at 80~100 DEG C
~24 hours, obtain raw mixture.
2, by raw mixture 1180~1250 DEG C pre-burning 5~8 hours, obtain pre-burning powder.
3, it by pre-burning powder after granulation, tabletting, dumping, is sintered 3~6 hours at 1280~1340 DEG C, obtains Eu-Bi and be co-doped with
Miscellaneous tungsten bronze structure shines ferroelectric ceramic material.
In above-mentioned steps 2, preferably by raw mixture 1220 DEG C pre-burning 6 hours.
In above-mentioned steps 3, preferably by pre-burning powder after granulation, tabletting, dumping, it is sintered 4 hours at 1300 DEG C.
The present invention passes through in Sr1.90Ca0.15Na0.90Nb5O15Eu and Bi is adulterated in ceramic systems, is not only made it have luminous
Performance, and its thermal stability that shines is significantly improved, and improve its Dielectric, Ferroelectric performance.
Detailed description of the invention
Fig. 1 is the XRD diagram of the ceramic material of comparative example 1, comparative example 2 and Examples 1 to 3 preparation.
Fig. 2 is the luminous thermal stability figure of ceramic material prepared by comparative example 2.
Fig. 3 is the luminous thermal stability figure of ceramic material prepared by embodiment 2.
Fig. 4 be comparative example 1, comparative example 2 and Examples 1 to 3 preparation ceramic material under 10kHz test frequency Curie's temperature
Degree and maximum dielectric constant comparison diagram.
Fig. 5 is the ferroelectric hysteresis loop of the ceramic material of comparative example 2 and Examples 1 to 3 preparation.
Fig. 6 is the remanent polarization and coercive field comparison diagram of the ceramic material of comparative example 2 and Examples 1 to 3 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, according to Sr1.90Ca0.15Na0.801Eu0.03Bi0.003Nb5O15Stoichiometry respectively to weigh purity be 99.80%
Na2CO30.8409g, the SrCO that purity is 99.00%35.6016g, the Nb that purity is 99.99%2O513.1394g, purity
For 99.00% CaCO30.2998g, the Eu that purity is 99.99%2O30.1044g, the Bi that purity is 99.99%2O3
0.0138g is fitted into nylon tank, is ball-milling medium by abrading-ball, dehydrated alcohol of zirconium ball, with 401 revs/min of ball millings 24 of ball mill
Hour, drying 15 hours at 80 DEG C are put in a drying box, with mortar grinder 30 minutes, 80 meshes is crossed, obtains raw mixture.
2, raw mixture is placed in alumina crucible, is compacted with agate stick, makes its compacted density 1.5g/cm3, add
Lid, is placed in resistance furnace, is warming up to 1220 DEG C of pre-burnings 6 hours with 3 DEG C/min of heating rate, cooled to room temperature, out
Furnace was crossed 120 meshes, and was obtained pre-burning powder with mortar grinder 10 minutes.
3, the polyvinyl alcohol water solution that the mass fraction of its quality 50% is 5% is added into pre-burning powder, is granulated, crosses 120
Spherical powder is made in mesh, spherical powder is put into the stainless steel mould that diameter is 15mm, with powder compressing machine in 300MPa
Pressure under be compressed into cylindric blank with a thickness of 1.5mm, cylindric blank is placed on zirconium oxide plate, will be aoxidized
Zirconium plate is placed in the closed saggar of aluminium oxide, is first warming up to 500 DEG C, is kept the temperature 2 hours dumpings, is cooled to room temperature, then with 10 DEG C/minute
The heating rate of clock is warming up to 1000 DEG C, is warming up to 1300 DEG C in 3 DEG C/min of heating rates, is sintered 4 hours, with furnace nature
It is cooled to room temperature, obtains the luminous ferroelectric ceramic material of Eu-Bi codope tungsten bronze structure.
Embodiment 2
In the step 1 of the present embodiment, according to Sr1.90Ca0.15Na0.795Eu0.03Bi0.005Nb5O15Stoichiometry claim respectively
Taking purity is 99.80% Na2CO30.8345g, the SrCO that purity is 99.00%35.6008g, purity are 99.99%
Nb2O513.1375g, the CaCO that purity is 99.00%30.2998g, the Eu that purity is 99.99%2O30.1044g, purity are
99.99% Bi2O30.0230g, other steps are same as Example 1, obtain the luminous ferroelectricity of Eu-Bi codope tungsten bronze structure
Ceramic material.
Embodiment 3
In the step 1 of the present embodiment, according to Sr1.90Ca0.15Na0.786Eu0.03Bi0.008Nb5O15Stoichiometry claim respectively
Taking purity is 99.80% Na2CO30.8249g, the SrCO that purity is 99.00%35.5996g, purity are 99.99%
Nb2O513.1347g, the CaCO that purity is 99.00%30.2997g, the Eu that purity is 99.99%2O30.1043g, purity are
99.99% Bi2O30.0368g, other steps are same as Example 1, obtain the luminous ferroelectricity of Eu-Bi codope tungsten bronze structure
Ceramic material.
Comparative example 1
According to Sr1.90Ca0.15Na0.90Nb5O15Stoichiometry weigh respectively purity be 99.80% Na2CO3
0.9455g, the SrCO that purity is 99.00%35.6056g, the Nb that purity is 99.99%2O513.1488g, purity be
99.00% CaCO30.3000g, other steps are same as Example 1, obtain Sr1.90Ca0.15Na0.90Nb5O15Ceramic material.
Comparative example 2
According to Sr1.90Ca0.15Na0.81Eu0.03Nb5O15Stoichiometry weigh respectively purity be 99.80% Na2CO3
0.8506g, the SrCO that purity is 99.00%35.6028g, the Nb that purity is 99.99%2O513.1423g, purity be
99.00% CaCO30.2999g, the Eu that purity is 99.99%2O30.1044g, other steps are same as Example 1, obtain
Eu adulterates the luminous ferroelectric ceramic material of tungsten bronze structure.
D/max-2200X type x ray diffraction is respectively adopted in above-mentioned comparative example 1 and 2 and the ceramic material of Examples 1 to 3 preparation
Instrument (company produces by Rigaku) carries out XRD test, using F-4600 type sepectrophotofluorometer and connection temperature regulating device
(THMS600) its thermal stability is tested, the result is shown in Figure 1~3.As seen from Figure 1, comparative example 1, comparative example 2 and embodiment 1
~3 to prepare ceramic material be pure tungsten bronze phase.By Fig. 2 and Fig. 3 as it can be seen that in comparative example 2 by
Sr1.90Ca0.15Na0.90Nb5O15Although Eu is adulterated in ceramic material makes ceramic material be provided with luminescent properties, but the heat that shines is steady
Qualitative poor, the present invention passes through in Sr1.90Ca0.15Na0.90Nb5O15Eu and Bi are adulterated simultaneously in ceramic material, not only makes ceramic material
Material is provided with luminescent properties, and relative to comparative example 2, the thermal stability of ceramic material is increased to by original 33%
67%.
Ceramic material surfaces prepared by comparative example 1, comparative example 2 and Examples 1 to 3 are successively used into 320 mesh, 800 mesh, 1500
Mesh sand paper is polished to 0.5~0.6mm thickness, then in the silver paste that ceramic upper and lower surface coating thickness is 0.01~0.03mm, is placed in
30 minutes are kept the temperature for 840 DEG C in resistance furnace.Using HIOKI3532-50 and Agilient4980A type precise impedance analyzer (by pacifying
The production of prompt Lun Science & technology Co., Ltd) etc. carry out the test of ceramic dielectric ferroelectric properties, as a result see Fig. 4~6.By Fig. 4~6 as it can be seen that with
Comparative example 1 is compared with the ceramic material of comparative example 2, and the present invention improves pottery by adulterating Eu and Bi simultaneously in ceramic material
The electrical property of ceramic material, when x value is 0.005, the value of y is 0.03, maximum dielectric constant is 1345, Curie temperature is
272 DEG C, remanent polarization be 4.29 μ C/cm2, coercive field 21.41kV/cm.
Claims (4)
- The ferroelectric ceramic material 1. a kind of Eu-Bi codope tungsten bronze structure of high-incidence photo and thermal stability shines, it is characterised in that: should The structural formula of ceramic material is Sr1.90Ca0.15Na0.81-3xEuyBixNb5O15, wherein the value of x is taking for 0.003~0.008, y Value is 0.02~0.06；The ceramic material is prepared by the following method to obtain:(1) according to Sr1.90Ca0.15Na0.81-3xEuyBixNb5O15Stoichiometric ratio weigh respectively purity be 99.00% or more Na2CO3、SrCO3、Nb2O5、CaCO3、Eu2O3、Bi2O3, ball milling is sufficiently mixed 16~24 hours, dry 12 at 80~100 DEG C ~24 hours, obtain raw mixture；(2) by raw mixture 1180~1250 DEG C pre-burning 5~8 hours, obtain pre-burning powder；(3) it by pre-burning powder after granulation, tabletting, dumping, is sintered 3~6 hours at 1280~1340 DEG C, obtains Eu-Bi codope Tungsten bronze structure shines ferroelectric ceramic material.
- The ferroelectric ceramics material 2. the Eu-Bi codope tungsten bronze structure of high-incidence photo and thermal stability according to claim 1 shines Material, it is characterised in that: the value of the x is 0.005, the value of y is 0.03.
- The ferroelectric ceramic material 3. Eu-Bi codope tungsten bronze structure according to claim 1 shines, it is characterised in that: In In step (2), by raw mixture 1220 DEG C pre-burning 6 hours.
- The ferroelectric ceramic material 4. Eu-Bi codope tungsten bronze structure according to claim 1 shines, it is characterised in that: In In step (3), by pre-burning powder after granulation, tabletting, dumping, it is sintered 4 hours at 1300 DEG C.
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| CN115180944B (en) * | 2022-07-11 | 2023-03-24 | 中国科学院上海硅酸盐研究所 | Full-filled tungsten bronze structure high-entropy ferroelectric ceramic material and preparation method thereof |
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| CN105541413A (en) * | 2016-02-03 | 2016-05-04 | 陕西师范大学 | High-d33 lead-free strontium calcium niobate sodium tungsten bronze piezo-ferroelectric ceramic material and preparation method thereof |
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