CN107253859A - Luminous ferroelectric ceramic material of the Eu Bi codopes tungsten bronze structure of photo and thermal stability occurred frequently and preparation method thereof - Google Patents
Luminous ferroelectric ceramic material of the Eu Bi codopes tungsten bronze structure of photo and thermal stability occurred frequently and preparation method thereof Download PDFInfo
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Abstract
The invention discloses luminous ferroelectric ceramic material of the Eu Bi codopes tungsten bronze structure of a kind of photo and thermal stability occurred frequently and preparation method thereof, the general structure of the ceramic material is Sr1.90Ca0.15Na0.81‑3xEuyBixNb5O15, wherein x value is that 0.003~0.008, y value is 0.02~0.06, and it uses conventional high-temperature solid phase method to be prepared from, and preparation method is with low cost, easy to operate.The present invention passes through the Eu and Bi that adulterated in ceramic material, not only make it have luminescent properties, and significantly improve its luminous heat endurance, and improve its Dielectric, Ferroelectric performance, wherein x=0.005, y=0.03 when, its luminous heat endurance is 67%, maximum dielectric constant be 1345, Curie temperature be 272 DEG C, remanent polarization be 4.29 μ C/cm2, coercive field be 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 photo and thermal stability occurred frequently
Luminous ferroelectric ceramic material of bronze structures and preparation method thereof.
Background technology
In recent years, unleaded foundary weight electric material is in addition to research improves foundary weight electrical property to substitute lead-containing materials, also in storage
Energy, strain, electric card, thermoelectricity, photoelectricity, it is luminous in terms of find new functional characteristic, receive more and more attention it.Tungsten is blue or green
Copper system is an important branch indispensable in unleaded foundary weight electric material system, and composition formula is (A1)2(A2)4C4(B1)2
(B2)8O30, different metal cation according to its radius and valence state optionally occupy A1, A2, B1, B2 and C this 5 kinds it is non-etc.
The crystallography interstitial site of valency, the filling situation of regulation crystallography interstitial site can induce out flexible and changeable architectural characteristic and work(
Can characteristic.Research group where inventor is using conventional solid-state method by adjusting Na determination study tungsten bronze
(Sr0.925Ca0.075)2.5-0.5xNaxNb5O15Architecture and performance are contacted, and as a result find when structure is closer to full of type it
Performance is more excellent, but easily produces second and mutually deteriorate electric property.And the ceramic material only has electric property, it is contemplated that
Current material high-intelligentization, highly integrated development, this material property are single, limit its application, it is impossible to meet newest material
Design concept.
The content of the invention
The technical problems to be solved by the invention are that providing one kind is provided simultaneously with electrical property and luminescent properties and luminous heat
The high Eu-Bi codopes tungsten bronze structure of stability lights ferroelectric ceramic material, and provides for it that a kind of technique is simple, repeatability
Good, preparation method with low cost.
The structural formula for the ceramic material that above-mentioned technical problem is used is solved for Sr1.90Ca0.15Na0.81-3xEuyBixNb5O15,
Wherein x value is that 0.003~0.008, y value is 0.02~0.06, and preferably x value is that 0.005, y value is
0.03。
The luminous ferroelectric ceramic material preparation method of Eu-Bi codopes tungsten bronze structure of the present invention is made up of following step：
1st, according to Sr1.90Ca0.15Na0.81-3xEuyBixNb5O15Stoichiometric proportion weigh purity respectively for more than 99.00%
Na2CO3、SrCO3、Nb2O5、CaCO3、Eu2O3、Bi2O3, it is sufficiently mixed ball milling 16~24 hours, 12 is dried at 80~100 DEG C
~24 hours, obtain raw mixture.
2nd, raw mixture was obtained into pre-burning powder in 1180~1250 DEG C of pre-burnings 5~8 hours.
3rd, by pre-burning powder after granulation, tabletting, dumping, sintered 3~6 hours at 1280~1340 DEG C, obtain Eu-Bi and be total to
The luminous ferroelectric ceramic material of the tungsten bronze structure that adulterates.
In above-mentioned steps 2, preferably by raw mixture in 1220 DEG C of pre-burnings 6 hours.
In above-mentioned steps 3, preferably by pre-burning powder after granulation, tabletting, dumping, sintered 4 hours at 1300 DEG C.
The present invention is by Sr1.90Ca0.15Na0.90Nb5O15Adulterate Eu and Bi in ceramic systems, not only makes it have luminous
Performance, and its luminous heat endurance is significantly improved, and improve its Dielectric, Ferroelectric performance.
Brief description of the drawings
Fig. 1 is the XRD of ceramic material prepared by comparative example 1, comparative example 2 and embodiment 1~3.
Fig. 2 is the luminous heat endurance figure of ceramic material prepared by comparative example 2.
Fig. 3 is the luminous heat endurance figure of ceramic material prepared by embodiment 2.
Fig. 4 is the ceramic material for preparing of comparative example 1, comparative example 2 and embodiment 1~3 Curie's temperature under 10kHz test frequencies
Degree and maximum dielectric constant comparison diagram.
Fig. 5 is the ferroelectric hysteresis loop of ceramic material prepared by comparative example 2 and embodiment 1~3.
Fig. 6 is the remanent polarization and coercive field comparison diagram of ceramic material prepared by comparative example 2 and embodiment 1~3.
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
1st, according to Sr1.90Ca0.15Na0.801Eu0.03Bi0.003Nb5O15Stoichiometry respectively to weigh purity be 99.80%
Na2CO30.8409g, purity are 99.00% SrCO35.6016g, purity are 99.99% Nb2O513.1394g, purity
For 99.00% CaCO30.2998g, purity are 99.99% Eu2O30.1044g, purity are 99.99% Bi2O3
0.0138g, is fitted into nylon tank, by abrading-ball of zirconium ball, absolute ethyl alcohol be ball-milling medium, with 401 revs/min of ball millings 24 of ball mill
Hour, it is placed in drying box and is dried 15 hours at 80 DEG C, with mortar grinder 30 minutes, crosses 80 mesh sieves, obtain raw mixture.
2nd, raw mixture is placed in alumina crucible, be compacted with agate rod, it is 1.5g/cm to make its compacted density3, plus
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, naturally cools to room temperature, go out
Stove, with mortar grinder 10 minutes, crosses 120 mesh sieves, obtains pre-burning powder.
3rd, the mass fraction that its quality 50% is added into pre-burning powder is 5% polyvinyl alcohol water solution, and granulation crosses 120
Mesh sieve, is made spherical powder, in the stainless steel mould that spherical powder is put into a diameter of 15mm, with powder compressing machine in 300MPa
Pressure under be compressed into thickness be 1.5mm cylindric blank, cylindric blank is placed on zirconium oxide flat board, will be aoxidized
Zirconium flat board is placed in the closed saggar of aluminum oxide, is first warming up to 500 DEG C, is incubated 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, and 1300 DEG C are warming up in 3 DEG C/min of heating rates, sinters 4 hours, natural with stove
Room temperature is cooled to, the luminous ferroelectric ceramic material of Eu-Bi codopes tungsten bronze structure is obtained.
Embodiment 2
In the step 1 of the present embodiment, according to Sr1.90Ca0.15Na0.795Eu0.03Bi0.005Nb5O15Stoichiometry claim respectively
Take the Na that purity is 99.80%2CO30.8345g, purity are 99.00% SrCO35.6008g, purity are 99.99%
Nb2O513.1375g, purity are 99.00% CaCO30.2998g, purity are 99.99% Eu2O30.1044g, purity are
99.99% Bi2O30.0230g, other steps are same as Example 1, obtain the luminous iron of Eu-Bi codopes tungsten bronze structure
Electroceramics material.
Embodiment 3
In the step 1 of the present embodiment, according to Sr1.90Ca0.15Na0.786Eu0.03Bi0.008Nb5O15Stoichiometry claim respectively
Take the Na that purity is 99.80%2CO30.8249g, purity are 99.00% SrCO35.5996g, purity are 99.99%
Nb2O513.1347g, purity are 99.00% CaCO30.2997g, purity are 99.99% Eu2O30.1043g, purity are
99.99% Bi2O30.0368g, other steps are same as Example 1, obtain the luminous iron of Eu-Bi codopes tungsten bronze structure
Electroceramics material.
Comparative example 1
According to Sr1.90Ca0.15Na0.90Nb5O15Stoichiometry weigh respectively purity be 99.80% Na2CO3
0.9455g, purity are 99.00% SrCO35.6056g, purity are 99.99% Nb2O513.1488g, purity be
99.00% CaCO30.3000g, other steps are same as Example 1, obtain Sr1.90Ca0.15Na0.90Nb5O15Ceramic material
Material.
Comparative example 2
According to Sr1.90Ca0.15Na0.81Eu0.03Nb5O15Stoichiometry weigh respectively purity be 99.80% Na2CO3
0.8506g, purity are 99.00% SrCO35.6028g, purity are 99.99% Nb2O513.1423g, purity be
99.00% CaCO30.2999g, purity are 99.99% Eu2O30.1044g, other steps are same as Example 1, obtain
The luminous ferroelectric ceramic material of Eu doping tungsten bronze structures.
D/max-2200X type x ray diffractions are respectively adopted in ceramic material prepared by above-mentioned comparative example 1 and 2 and embodiment 1~3
Instrument (company produces by Rigaku) carries out XRD tests, using F-4600 types sepectrophotofluorometer and connection temperature regulating device
(THMS600) its heat endurance is tested, as a result sees Fig. 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.In Fig. 2 and Fig. 3, comparative example 2 by
Sr1.90Ca0.15Na0.90Nb5O15Although the Eu that adulterated in ceramic material makes ceramic material be provided with luminescent properties, but luminous heat is steady
Qualitative poor, the present invention is by Sr1.90Ca0.15Na0.90Nb5O15Adulterate Eu and Bi simultaneously in ceramic material, not only makes ceramics
Material is provided with luminescent properties, and relative to comparative example 2, the heat endurance of ceramic material is brought up to by original 33%
67%.
By comparative example 1, comparative example 2 and embodiment 1~3 prepare ceramic material surfaces successively with 320 mesh, 800 mesh,
1500 mesh sand paper are polished to 0.5~0.6mm thickness, then in the silver paste that ceramic upper and lower surface coating thickness is 0.01~0.03 mm,
It is placed in resistance furnace 840 DEG C and is incubated 30 minutes.Using HIOKI3532-50 and Agilient4980A type precise impedance analyzers
(being produced by Anjelen Sci. ＆ Tech. Inc) etc. carries out ceramic dielectric ferroelectric properties test, as a result sees Fig. 4~6.Can by Fig. 4~6
See, compared with the ceramic material of comparative example 1 and comparative example 2, the present invention is improved by the Eu and Bi that adulterated in ceramic material simultaneously
The electrical property of ceramic material, when the value that x values are 0.005, y is 0.03, its maximum dielectric constant is 1345, Curie
Temperature is 272 DEG C, remanent polarization is 4.29 μ C/cm2, coercive field be 21.41kV/cm.
Claims (5)
- The ferroelectric ceramic material 1. a kind of Eu-Bi codopes tungsten bronze structure of photo and thermal stability occurred frequently lights, it is characterised in that：Should The structural formula of ceramic material is Sr1.90Ca0.15Na0.81-3xEuyBixNb5O15, wherein x value is taking for 0.003~0.008, y It is worth for 0.02~0.06.
- The ferroelectric ceramics material 2. the Eu-Bi codopes tungsten bronze structure of photo and thermal stability occurred frequently according to claim 1 lights Material, it is characterised in that：The value that the value of the x is 0.005, y is 0.03.
- Ferroelectric ceramic material preparation method, its feature 3. the Eu-Bi codopes tungsten bronze structure described in a kind of claim 1 lights It is that it is made up of following step：(1) according to Sr1.90Ca0.15Na0.81-3xEuyBixNb5O15Stoichiometric proportion weigh purity respectively for more than 99.00% Na2CO3、SrCO3、Nb2O5、CaCO3、Eu2O3、Bi2O3, it is sufficiently mixed ball milling 16~24 hours, 12 is dried at 80~100 DEG C ~24 hours, obtain raw mixture；(2) raw mixture was obtained into pre-burning powder in 1180~1250 DEG C of pre-burnings 5~8 hours；(3) by pre-burning powder after granulation, tabletting, dumping, sintered 3~6 hours at 1280~1340 DEG C, obtain Eu-Bi codopes Tungsten bronze structure lights ferroelectric ceramic material.
- The preparation method of ferroelectric ceramic material 4. Eu-Bi codopes tungsten bronze structure according to claim 3 lights, it is special Levy and be：In step (2), by raw mixture in 1220 DEG C of pre-burnings 6 hours.
- The preparation method of ferroelectric ceramic material 5. Eu-Bi codopes tungsten bronze structure according to claim 3 lights, it is special Levy and be：In step (3), by pre-burning powder after granulation, tabletting, dumping, sintered 4 hours at 1300 DEG C.
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| CN114605151A (en) * | 2022-04-24 | 2022-06-10 | 西安理工大学 | Gd-Ta co-doped tungsten bronze structure ferroelectric energy storage ceramic material and preparation method thereof |
| CN115180944A (en) * | 2022-07-11 | 2022-10-14 | 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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|---|---|---|---|---|
| CN114605151A (en) * | 2022-04-24 | 2022-06-10 | 西安理工大学 | Gd-Ta co-doped tungsten bronze structure ferroelectric energy storage ceramic material and preparation method thereof |
| CN114605151B (en) * | 2022-04-24 | 2022-12-09 | 西安理工大学 | Gd-Ta co-doped tungsten bronze structure ferroelectric energy storage ceramic material and preparation method thereof |
| CN115180944A (en) * | 2022-07-11 | 2022-10-14 | 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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