CN105016728A - Rear earth doped non-fullness tungsten bronze luminescence ferroelectric material and preparation method thereof - Google Patents
Rear earth doped non-fullness tungsten bronze luminescence ferroelectric material and preparation method thereof Download PDFInfo
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- CN105016728A CN105016728A CN201410168473.2A CN201410168473A CN105016728A CN 105016728 A CN105016728 A CN 105016728A CN 201410168473 A CN201410168473 A CN 201410168473A CN 105016728 A CN105016728 A CN 105016728A
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Abstract
The invention discloses a rear earth doped non-fullness tungsten bronze luminescence ferroelectric material and a preparation method thereof. The chemical formula of the rear earth doped non-fullness tungsten bronze luminescence ferroelectric material is Ba1La[1-x]EuxTiNb9O30, wherein x is larger than or equal to 0 and less than or equal to 1. According to the invention, Ba1La[1-x]EuxTiNb9O30 porcelain is prepared by adopting a simple solid-phase reaction method, so cost is low, operation is convenient, and large-scale production is facilitated. The Ba1La[1-x]EuxTiNb9O30 porcelain has good luminescence performance and also has good dielectric property and ferroelectric property, is a novel and important multifunctional porcelain material and has wide application prospect in the field of photoelectric materials.
Description
Technical field
The present invention relates to ceramic material field, be specifically related to a kind of non-ly be full of the luminous Dielectric, Ferroelectric material of type tungsten bronze(s) and preparation method.
Background technology
Due in micro-wave communication, sensor, transverter, the important application of the technical fields such as ferroelectric information storer, is non-ly full of the research interest that type tungsten bronze(s) material causes a lot of researcher in recent years.The non-electric property being full of type tungsten bronze(s) material is mainly paid close attention in current scientific research, seldom considers other functional attributes.But along with the development of modern science and technology, more and more higher to the requirement of device multifunction, this just needs development to have the novel material of two or more function, to develop the new device that can realize several functions simultaneously simultaneously.Therefore, be necessary is keeping or is improving on the basis of original function attribute in developing material with design, study further and the new capability of expansion material, thus material is had apply more widely.In view of rare earth ion is generally the non-intrinsic ion being full of type tungsten bronze(s) material, by selecting suitable rare earth activation ion, the non-lighting function attribute being full of type tungsten bronze(s) material can be developed, therefore this material is a kind of potential rare earth luminescent material, but the non-luminescent properties being full of type tungsten bronze(s) material potential is not also concerned.If can prepare and both have luminescent properties, can also improve the material of original dielectric, ferroelectric properties, this kind of material will have in future electronic industry to be applied more widely simultaneously.Up to now, rare-earth europium ion (Eu of the present invention
3+) adulterate be non-ly full of type tungsten bronze(s) Ba
1laTiNb
9o
30the characteristics of luminescence of material has no report.
Summary of the invention
The object of the invention is to the deficiency overcoming prior art, provide a kind of newly rear-earth-doped non-to be full of luminous ferroelectric material of type tungsten bronze(s) and preparation method thereof.
For achieving the above object and other object, the present invention is achieved by following technical solution:
The invention provides and a kind of be rear-earth-dopedly non-ly full of luminous ferroelectric material of type tungsten bronze(s) and preparation method thereof, this rear-earth-doped non-chemical formula being full of the luminous ferroelectric material of type tungsten bronze(s) is Ba
1la
1-xeu
xtiNb
9o
30, wherein, 0≤x≤1.
Described luminous ferroelectric material is for adopting the preparation of simple solid reaction process, and described method comprises the steps:
Step 1: with the BaCO of analytical pure level
3, TiO
2, Nb
2o
5, the La of high-purity grade
2o
3, Eu
2o
3for raw material, according to chemical formula Ba
1la
1-xeu
xtiNb
9o
30, wherein, 0≤x≤1, carries out proportioning in accordance with mol ratio;
Step 2: with analytical pure dehydrated alcohol for medium, is placed in agate tank by the raw material prepared, and planetary ball mill carries out ball milling, and Ball-milling Time is 24 hours;
Step 3: the slurry after ball milling is placed in beaker, dries in an oven, drying time 12 hours, bake out temperature 95 degree, obtains and dries powder;
Step 4: oven dry powder agate mortar is ground, is then placed in corundum crucible, puts into box-type furnace, continuous warming to 1250 ~ 1300 degree pre-burning 8 ~ 12 hours, program determination after being cooled to 500 degree, cools to room temperature with the furnace, comes out of the stove;
Step 5: the mode ball milling identical with step 2, the mode identical with step 3 is dried, and then with agate mortar grinding, makes pre-burning powder;
Step 6: pre-burning powder is crossed screen cloth, adds the polyvinylpyrrolidone that concentration is 1 ~ 20%, fully grinds, mix, seasoning, granulation in powder, crosses screen cloth, prepares spherical powder;
Step 7: spherical powder is placed in and adds a cover corundum crucible, be placed in box-type furnace, continuous warming, carry out plastic removal, then 1300 ~ 1350 degree of pre-burnings 8 ~ 12 hours, program determination after being cooled to 500 degree, cools to room temperature with the furnace, come out of the stove, obtain rear-earth-doped being non-ly full of the luminous ferroelectric material of type tungsten bronze(s).
Or by the pre-burning powder in step 5, add concentration be 1 ~ 20% polyvinylpyrrolidone carry out granulation, under 10MPa pressure, prepare the ceramic green blank of diameter 13mm, then sinter according to step 7 same way, obtain rear-earth-doped being non-ly full of the luminous ferroelectric ceramic material of type tungsten bronze(s).
Preferably, crossing the order number that pre-burning powder crosses screen cloth in step 6 is 200 orders.
Preferably, the order number crossing screen cloth in step 6 after granulation is 80 orders.
Preferably, in step 7, plastic removal condition is 600 ~ 700 degree of insulations 1 ~ 2 hour.
Compared with prior art, the present invention has following beneficial effect:
(1) the rear-earth-doped non-type tungsten bronze(s) material that is full of that prepared by the present invention has excellent luminescent properties, and luminous monochromaticity is good, and intensity is higher, and in future optical display, photoelectric sensing, the technical fields such as photoelectricity is integrated have broad prospect of application.
(2) the rear-earth-doped non-type tungsten bronze(s) material that is full of that prepared by the present invention has excellent ferroelectric and dielectric properties, rare earth activation ion doping can not only give this material emission characteristic, effectively can also improve the ferroelectrie Curie temperature of material, strengthen specific inductivity, improve iron electric polarization intensity.This material is the ferroelectrics of more than a kind of new room temperature.
(3) rear-earth-doped non-being full of in the luminous ferroelectric material of type tungsten bronze(s) that prepared by the present invention does not contain the disadvantageous lead element of environment, belongs to non-plumbum ferroelectric system material.
(4) preparation method of the present invention has that technique is simple, process stabilizing, is easy to the advantages such as large-scale industrialization promotion.
Accompanying drawing illustrates:
Fig. 1 is Ba
4la
1-xeu
xtiNb
9o
30, wherein x=0, ceramics sample dielectric temperature is composed, and additional frequency test signal is 1MHz, and signal amplitude is 1V.
Fig. 2 is Ba
4la
1-xeu
xtiNb
9o
30, wherein x=0.5, ceramics sample dielectric temperature is composed, and additional frequency test signal is 1MHz, and signal amplitude is 1V.
Fig. 3 is Ba
4la
1-xeu
xtiNb
9o
30, wherein x=1, ceramics sample dielectric temperature is composed, and additional frequency test signal is 1MHz, and signal amplitude is 1V.
Fig. 4 is Ba
4la
1-xeu
xtiNb
9o
30, wherein x=0, the emmission spectrum of ceramics sample under 399nm near ultraviolet excitation, probe temperature is room temperature.
Fig. 5 is Ba
4la
1-xeu
xtiNb
9o
30, wherein x=0.5, the emmission spectrum of ceramics sample under 399nm near ultraviolet excitation, probe temperature is room temperature.
Fig. 6 is Ba
4la
1-xeu
xtiNb
9o
30, wherein x=1, the emmission spectrum of ceramics sample under 399nm near ultraviolet excitation, probe temperature is room temperature.
Embodiment:
Now in conjunction with specific embodiments the present invention is done and describes further:
Embodiment 1
Preparation Ba
1la
1-xeu
xtiNb
9o
30, wherein x=0, preparation method is as follows:
Adopt the BaCO of analytical pure level
3(99%), TiO
2(99%), Nb
2o
5(99%), the La of high-purity grade
2o
3(99.99%) be raw material, carry out proportioning according to mol ratio, weigh various raw material.With analytical pure dehydrated alcohol for medium, the raw material prepared is placed in agate tank, planetary ball mill carries out ball milling, Ball-milling Time is 24 hours.Slurry after ball milling is placed in beaker, dries in an oven, drying time 12 hours, bake out temperature 95 degree, obtain and dry powder.Ground by oven dry powder agate mortar, be then placed in corundum crucible, put into box-type furnace, continuous warming to 1250 ~ 1300 degree pre-burning 8 ~ 12 hours, program determination after being cooled to 500 degree, after furnace cooling, ball milling is dried in the same fashion.Granulating powders after oven dry, shaping, be finally placed in corundum boat 1350 DEG C of calcination, 8 hours one-tenth porcelain in atmosphere.
That Fig. 1 represents is Ba
4la
1-xeu
xtiNb
9o
30the dielectric temperature spectrum of pottery (x=0), the emmission spectrum of this sample as shown in Figure 4.
Embodiment 2
Preparation Ba
4la
1-xeu
xtiNb
9o
30, wherein x=0.5, preparation method is as follows:
Adopt the BaCO of analytical pure level
3(99%), TiO
2(99%), Nb
2o
5(99%), the La of high-purity grade
2o
3(99.99%), Eu
2o
3(99.99%) be raw material, carry out proportioning according to mol ratio, weigh various raw material.With analytical pure dehydrated alcohol for medium, the raw material prepared is placed in agate tank, planetary ball mill carries out ball milling, Ball-milling Time is 24 hours.Slurry after ball milling is placed in beaker, dries in an oven, drying time 12 hours, bake out temperature 95 degree, obtain and dry powder.Ground by oven dry powder agate mortar, be then placed in corundum crucible, put into box-type furnace, continuous warming to 1250 ~ 1300 degree pre-burning 8 ~ 12 hours, program determination after being cooled to 500 degree, after furnace cooling, ball milling is dried in the same fashion.Granulating powders after oven dry, shaping, be finally placed in corundum boat 1350 DEG C of calcination, 8 hours one-tenth porcelain in atmosphere.
That Fig. 2 represents is Ba
4la
1-xeu
xtiNb
9o
30the dielectric temperature spectrum of pottery (x=0.5), the emmission spectrum of this sample as shown in Figure 5.
Embodiment 3
Preparation Ba
1la
1-xeu
xtiNb
9o
30, wherein x=1, preparation method is as follows:
Adopt the BaCO of analytical pure level
3(99%), TiO
2(99%), Nb
2o
5(99%), the Eu of high-purity grade
2o
3(99.99%) be raw material, carry out proportioning according to mol ratio, weigh various raw material.With analytical pure dehydrated alcohol for medium, the raw material prepared is placed in agate tank, planetary ball mill carries out ball milling, Ball-milling Time is 24 hours.Slurry after ball milling is placed in beaker, dries in an oven, drying time 12 hours, bake out temperature 95 degree, obtain and dry powder.Ground by oven dry powder agate mortar, be then placed in corundum crucible, put into box-type furnace, continuous warming to 1250 ~ 1300 degree pre-burning 8 ~ 12 hours, program determination after being cooled to 500 degree, after furnace cooling, ball milling is dried in the same fashion.Granulating powders after oven dry, shaping, be finally placed in corundum boat 1350 DEG C of calcination, 8 hours one-tenth porcelain in atmosphere.
That Fig. 3 represents is Ba
4la
1-xeu
xtiNb
9o
30the dielectric temperature spectrum of pottery (x=1), the emmission spectrum of this sample as shown in Figure 6.
Claims (5)
1. be rear-earth-dopedly non-ly full of the luminous ferroelectric material of type tungsten bronze(s), the chemical formula of described luminous ferroelectric material is Ba
4la
1-xeu
xtiNb
9o
30, wherein, 0≤x≤1.
2. the rear-earth-doped non-preparation method being full of the luminous ferroelectric material of type tungsten bronze(s) as claimed in claim 1, it is characterized in that, described luminous ferroelectric material is for adopting the preparation of simple solid reaction process, and described method comprises the steps:
Step 1: with the BaCO of analytical pure level
3, TiO
2, Nb
2o
5, the La of high-purity grade
2o
3, Eu
2o
3for raw material, according to chemical formula Ba
1la
1-xeu
xtiNb
9o
30, wherein, 0≤x≤1, carries out proportioning according to mol ratio;
Step 2: with analytical pure dehydrated alcohol for medium, is placed in agate tank by the raw material prepared, and planetary ball mill carries out ball milling, and Ball-milling Time is 24 hours;
Step 3: the slurry after ball milling is placed in beaker, dries in an oven, drying time 12 hours, bake out temperature 95 degree, obtains and dries powder;
Step 4: oven dry powder agate mortar is ground, is then placed in corundum crucible, puts into box-type furnace, continuous warming to 1250 ~ 1300 degree pre-burning 8 ~ 12 hours, program determination after being cooled to 500 degree, cools to room temperature with the furnace, comes out of the stove;
Step 5: the mode ball milling identical with step 2, the mode identical with step 3 is dried, and then with agate mortar grinding, makes pre-burning powder;
Step 6: pre-burning powder is crossed screen cloth, adds the polyvinylpyrrolidone that concentration is 1 ~ 20%, fully grinds, mix, seasoning, granulation in powder, crosses screen cloth, prepares spherical powder;
Step 7: spherical powder is put into and adds a cover corundum crucible, be placed in box-type furnace, continuous warming, carry out plastic removal, then 1300 ~ 1350 degree of calcinings 8 ~ 12 hours, program determination after being cooled to 500 degree, cools to room temperature with the furnace, come out of the stove, obtain rear-earth-doped being non-ly full of the luminous ferroelectric material of type tungsten bronze(s).
3. as the preparation method of the luminous ferroelectric material in claim 2, it is characterized in that, the preburning powdered material that obtains in step 5, add concentration be 1 ~ 20% polyvinylpyrrolidone carry out granulation, the ceramic green blank of diameter 13mm is prepared under 10MPa pressure, then sinter according to step 7 same way, obtain rear-earth-doped being non-ly full of the luminous ferroelectric ceramic material of type tungsten bronze(s).
4. as the preparation method of the luminous ferroelectric material in claim 2, it is characterized in that, the order number crossing screen cloth in step 6 is respectively 200 orders and 80 orders.
5. as the preparation method of the luminous ferroelectric material in claim 2, it is characterized in that, in step 7, plastic removal condition is 600 ~ 700 degree of insulations 1 ~ 2 hour.
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| CN201410168473.2A CN105016728A (en) | 2014-04-23 | 2014-04-23 | Rear earth doped non-fullness tungsten bronze luminescence ferroelectric material and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106905969A (en) * | 2017-03-29 | 2017-06-30 | 江苏师范大学 | In fluorescent material, the preparation method and application of near ultraviolet excitated lower transmitting gold-tinted |
| CN107099291A (en) * | 2017-03-29 | 2017-08-29 | 江苏师范大学 | It is a kind of can be by the red fluorescence material of near ultraviolet excitation, preparation method and application |
| CN107188564A (en) * | 2017-07-14 | 2017-09-22 | 陕西师范大学 | A kind of Eu of high dielectric property3+Luminous ferroelectric ceramic material of the sodium calcium strontium niobate that adulterates and preparation method thereof |
| CN109135352A (en) * | 2018-06-07 | 2019-01-04 | 太仓萃励新能源科技有限公司 | A kind of preparation method of nano anion slurry |
| CN114804871A (en) * | 2022-05-18 | 2022-07-29 | 中国民航大学 | Tungsten bronze-based photochromic ceramic material and preparation method thereof |
| CN116789450A (en) * | 2022-08-22 | 2023-09-22 | 中国科学院上海硅酸盐研究所 | Non-full tungsten bronze structure high-entropy ferroelectric ceramic material and preparation method and application thereof |
| CN116813340A (en) * | 2023-06-27 | 2023-09-29 | 浙江大学 | High-temperature-stability A-site high-configuration entropy filling tungsten bronze ceramic and preparation method thereof |
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| CN1165380A (en) * | 1996-03-13 | 1997-11-19 | 株式会社日立制作所 | Ferroelectric element and method of producing the same |
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| N.K. SINGH ET AL.: "Structural and dielectric properties of Ba5EuTi3-xZrxNb7O30 relaxor ferroelectrics", 《MATERIALS LETTERS》 * |
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Cited By (11)
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|---|---|---|---|---|
| CN106905969A (en) * | 2017-03-29 | 2017-06-30 | 江苏师范大学 | In fluorescent material, the preparation method and application of near ultraviolet excitated lower transmitting gold-tinted |
| CN107099291A (en) * | 2017-03-29 | 2017-08-29 | 江苏师范大学 | It is a kind of can be by the red fluorescence material of near ultraviolet excitation, preparation method and application |
| CN106905969B (en) * | 2017-03-29 | 2019-04-16 | 江苏师范大学 | Fluorescent material, preparation method and application near ultraviolet excitated lower transmitting yellow light |
| CN107099291B (en) * | 2017-03-29 | 2019-06-28 | 江苏师范大学 | It is a kind of can be by the red fluorescence material of near ultraviolet excitation, preparation method and application |
| CN107188564A (en) * | 2017-07-14 | 2017-09-22 | 陕西师范大学 | A kind of Eu of high dielectric property3+Luminous ferroelectric ceramic material of the sodium calcium strontium niobate that adulterates and preparation method thereof |
| CN109135352A (en) * | 2018-06-07 | 2019-01-04 | 太仓萃励新能源科技有限公司 | A kind of preparation method of nano anion slurry |
| CN114804871A (en) * | 2022-05-18 | 2022-07-29 | 中国民航大学 | Tungsten bronze-based photochromic ceramic material and preparation method thereof |
| CN114804871B (en) * | 2022-05-18 | 2023-01-24 | 中国民航大学 | Tungsten bronze-based photochromic ceramic material and preparation method thereof |
| CN116789450A (en) * | 2022-08-22 | 2023-09-22 | 中国科学院上海硅酸盐研究所 | Non-full tungsten bronze structure high-entropy ferroelectric ceramic material and preparation method and application thereof |
| CN116789450B (en) * | 2022-08-22 | 2024-04-12 | 中国科学院上海硅酸盐研究所 | Non-full tungsten bronze structure high-entropy ferroelectric ceramic material and preparation method and application thereof |
| CN116813340A (en) * | 2023-06-27 | 2023-09-29 | 浙江大学 | High-temperature-stability A-site high-configuration entropy filling tungsten bronze ceramic and preparation method thereof |
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