CN106478096A - A kind of rare earth base novel non-full of type tungsten bronze ferroelectric material and preparation method thereof - Google Patents
A kind of rare earth base novel non-full of type tungsten bronze ferroelectric material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of rare earth base novel non-full of type tungsten bronze ferroelectric material and preparation method thereof, the non-chemical formula full of type tungsten bronze ferroelectric material of this rare earth base be Ba5(1-x)Ln5xTi5xNb10-5xO30, wherein, Ln=Eu, Sm, Nd;0.15≤x≤0.30.The present invention adopts simple solid reaction process to prepare Ba5(1-x)Ln5xTi5xNb10-5xO30Material, with low cost, easy to operate, it is easy to large-scale production.The Ba of the present invention5(1-x)Ln5xTi5xNb10-5xO30Material is a kind of ferroelectric of more than new room temperature, enriches existing tungsten bronze ferroelectric material system.Study the ferroelectricity showing rare earth ion species and content energy this material of Effective Regulation and dielectric properties, this provides conveniently for the application of its WeiLai Technology.In addition, the Ba of present invention preparation5(1-x)Ln5xTi5xNb10-5xO30Do not contain in material to environmentally undesirable metallic element, belong to unleaded environmental type ferroelectricity system material, there is wide application prospect.
Description
Technical field
The present invention relates to ferroelectric ceramic material field and in particular to a kind of new non-full of type tungsten bronze ferroelectric material
And preparation method thereof.
Background technology
Due in non-volatile random access memory, dynamic RAM, sensor, transducer, infrared acquisition
The important application of the technical fields such as device, ferroelectric material is one of study hotspot of current field of functional materials, quilt
A lot of researcher extensive concerns in the world.In known ferroelectric material, Pb (Zr0.52Ti0.48)O3(PZT)
It is the current material studying the most deep and most widely used.But, PZT material exist serious polarization fatigue and
It contains hypertoxic lead element, and this is the bottleneck of its development of restriction, needs us to develop other novel lead-free greens
Ferroelectric material.
Recently, rare earth base be full of type tungsten bronze ferroelectric due to its colourful physical property thus inhale
Draw the research interest of scientist.Numerous studies show that rare earth base is full of presence in type tungsten bronze ferroelectric
Complicated polarization reciprocal action and the competition of thermal fluctuation, thus leading to show multiple physical phase transition in material,
As normal ferroelectric phase transition, relaxor ferroelectric phase transformation, disperse ferroelectric phase transition, reentry type relaxor ferroelectric phase transformation etc., answer
Miscellaneous microcosmic polarization state or polarization configuration are stored in wherein.
In contrast, rare earth base is non-less full of type tungsten bronze ferroelectric material, and people are to its various physical property
Can be not clear, need to further investigate.At present, for this research direction, design and development novel rare-earth
The non-work still belonging to an exploration and novelty full of type tungsten bronze ferroelectric material of base.Tungsten bronze is ferroelectric
Research not only has important basic science meaning, and it is in microwave communication, senses, storage, many ferrum,
Photovoltaic, the interleaving techniques such as photoelectricity field has important application.
Content of the invention
It is an object of the invention to overcoming the shortcomings of prior art, provide a kind of rare earth base novel non-blue or green full of type tungsten
Copper and iron electric material and preparation method thereof.
For achieving the above object and other purpose, the present invention is achieved by following technical solution:
The invention provides a kind of rare earth base novel non-full of type tungsten bronze ferroelectric material and preparation method thereof, this is dilute
The non-chemical formula full of type tungsten bronze ferroelectric material of soil matrix is Ba5(1-x)Ln5xTi5xNb10-5xO30, wherein, Ln=Eu,
Sm, Nd;0.15≤x≤0.30.
Described tungsten bronze ferroelectric material is using the preparation of simple solid reaction process, and described method includes walking as follows
Suddenly:
Step 1:To analyze the BaCO of pure level3、Nb2O5、TiO2, high-purity grade of Nd2O3、Sm2O3、
Eu2O3For raw material, according to chemical formula Ba5(1-x)Ln5xTi5xNb10-5xO30, wherein, Ln=Eu, Sm, Nd;0.15
≤ x≤0.30, carries out proportioning in accordance with mol ratio;
Step 2:With dehydrated alcohol (99.7%) as medium, the raw material preparing is placed in clean agate pot,
Ball milling is carried out on planetary ball mill, Ball-milling Time is 24 hours;
Step 3:Slurry after ball milling is placed in beaker, dries in electric heating convection oven, drying time
12 hours, 95 degree of drying temperature, obtain and dry powder body;
Step 4:Powder body agate mortar will be dried grind, and be subsequently placed in and add a cover in corundum crucible, put into box
In stove, continuous warming, to 1300 degree of pre-burnings 8 hours, program determination after being cooled to 550 degree, cools to the furnace
Room temperature, comes out of the stove;
Step 5:The product that step 4 is obtained is ground with agate mortar, makes pre-burning powder body;
Step 6:Add concentration to be~5% PVP in pre-burning powder body, be fully ground, mix homogeneously, from
So it is dried, pelletize;
Step 7:Step 6 gained powder body is prepared diameter~13mm, thickness~2mm under 10MPa pressure
Ceramic green blank;
Step 8;By step 7 ceramic green blank, it is placed in batch-type furnace, continuous warming, in 700 degree of insulations 2
Individual hour carries out plastic removal, then sinters 8 hours at 1350 degree, program determination after being cooled to 550 degree, with stove
Be cooled to room temperature, come out of the stove, obtain rare earth base novel non-full of type tungsten bronze ferroelectric material.
Compared with prior art, the invention has the advantages that:
(1) present invention synthesized a kind of rare earth base novel non-full of type tungsten bronze ferroelectric material, have studied material
Crystal structure, dielectric properties and ferroelectricity attribute.This material is a kind of ferroelectric of more than new room temperature, rich
Rich existing tungsten bronze ferroelectric material system.
(2) rare earth ion species and content energy Effective Regulation present invention synthesis non-full of type tungsten bronze ferroelectricity material
The ferroelectricity of material and dielectric properties, this is that the application of such material WeiLai Technology provides conveniently.
(3) without to environmentally undesirable lead in the non-tungsten bronze ferroelectric material full of type of rare earth base of present invention preparation
Element, belongs to non-plumbum ferroelectric system material.
(4) material synthesis method of the present invention has the advantages that process is simple it is easy to large-scale industrialization promotion.
Brief description:
That Fig. 1 is given is Ba5(1-x)Nd5xTi5xNb10-5xO30, wherein 0.15≤x≤0.30, the X of ferroelectric material
X ray diffraction collection of illustrative plates.
That Fig. 2 is given is Ba5(1-x)Sm5xTi5xNb10-5xO30, wherein 0.15≤x≤0.30, the X of ferroelectric material
X ray diffraction collection of illustrative plates.
That Fig. 3 is given is Ba5(1-x)Eu5xTi5xNb10-5xO30, wherein 0.15≤x≤0.30, the X of ferroelectric material
X ray diffraction collection of illustrative plates.
Fig. 4 is Ba5(1-x)Nd5xTi5xNb10-5xO30, wherein 0.15≤x≤0.30, the dielectric temperature spectrum of ferroelectric material,
Additional frequency test signal is 10KHz to 1MHz.
Fig. 5 is Ba5(1-x)Sm5xTi5xNb10-5xO30, wherein 0.15≤x≤0.30, the dielectric temperature spectrum of ferroelectric material,
Additional frequency test signal is 10KHz to 1MHz.
Fig. 6 is Ba5(1-x)Eu5xTi5xNb10-5xO30, wherein 0.15≤x≤0.30, the dielectric temperature spectrum of ferroelectric material,
Additional frequency test signal is 10KHz to 1MHz.
That Fig. 7 is given is Ba5(1-x)Nd5xTi5xNb10-5xO30, wherein 0.15≤x≤0.30, the room of ferroelectric material
Warm ferroelectric hysteresis loop.
That Fig. 8 is given is Ba5(1-x)Sm5xTi5xNb10-5xO30, wherein 0.15≤x≤0.30, the room of ferroelectric material
Warm ferroelectric hysteresis loop.
That Fig. 9 is given is Ba5(1-x)Eu5xTi5xNb10-5xO30, wherein 0.15≤x≤0.30, the room of ferroelectric material
Warm ferroelectric hysteresis loop.
Specific embodiment:
In conjunction with specific embodiment, the present invention is further described through:
Embodiment 1
Preparation Ba5(1-x)Nd5xTi5xNb10-5xO30, wherein 0.15≤x≤0.30, preparation method is as follows:
Using the BaCO analyzing pure level3(99%), Nb2O5(99%), TiO2(99%), high-purity grade
Nd2O3(99.99%) it is raw material, carry out proportioning, weigh various raw materials according to mol ratio.With dehydrated alcohol
(99.7%) it is medium, the raw material preparing is placed in clean agate pot, planetary ball mill is carried out
Ball milling, Ball-milling Time is 24 hours.Slurry after ball milling is placed in beaker, dries in an oven, dry
12 hours time, 95 degree of drying temperature, obtain and dry powder body.Powder body agate mortar will be dried grind,
It is subsequently placed in corundum crucible, puts in batch-type furnace, continuous warming, to 1300 degree of pre-burnings 8 hours, is cooled to
Program determination after 550 degree.After furnace cooling, products therefrom is levigate with agate mortar, adds binding agent, fully grinds
Mill, mix homogeneously, prepare the ceramic green blank of diameter 13mm under 10MPa pressure, be finally placed in corundum
1350 DEG C of calcination become porcelain in 8 hours to crucible in atmosphere.
Embodiment 2
Preparation Ba5(1-x)Sm5xTi5xNb10-5xO30, wherein 0.15≤x≤0.30, preparation method is as follows:
Using the BaCO analyzing pure level3(99%), Nb2O5(99%), TiO2(99%), high-purity grade of Sm2O3
(99.99%) it is raw material, carry out proportioning, weigh various raw materials according to mol ratio.With dehydrated alcohol (99.7%)
For medium, the raw material preparing is placed in clean agate pot, ball milling, ball are carried out on planetary ball mill
Consume time as 24 hours.Slurry after ball milling is placed in beaker, dries in an oven, drying time 12
Hour, 95 degree of drying temperature, obtain and dry powder body.Powder body agate mortar will be dried grind, be subsequently placed in
In corundum crucible, put in batch-type furnace, continuous warming to 1300 degree of pre-burnings 8 hours, after being cooled to 550 degree
Program determination.After furnace cooling, products therefrom is levigate with agate mortar, adds binding agent, is fully ground, and mixes
Close uniformly, prepare the ceramic green blank of diameter 13mm under 10MPa pressure, be finally placed in corundum crucible and exist
1350 DEG C of calcination of in the air become porcelain in 8 hours.
Embodiment 3
Preparation Ba5(1-x)Eu5xTi5xNb10-5xO30, wherein 0.15≤x≤0.30, preparation method is as follows:
Using the BaCO analyzing pure level3(99%), Nb2O5(99%), TiO2(99%), high-purity grade of Eu2O3
(99.99%) it is raw material, carry out proportioning, weigh various raw materials according to mol ratio.With dehydrated alcohol (99.7%)
For medium, the raw material preparing is placed in clean agate pot, ball milling, ball are carried out on planetary ball mill
Consume time as 24 hours.Slurry after ball milling is placed in beaker, dries in an oven, drying time 12
Hour, 95 degree of drying temperature, obtain and dry powder body.Powder body agate mortar will be dried grind, be subsequently placed in
In corundum crucible, put in batch-type furnace, continuous warming to 1300 degree of pre-burnings 8 hours, after being cooled to 550 degree
Program determination.After furnace cooling, products therefrom is levigate with agate mortar, adds binding agent, is fully ground, and mixes
Close uniformly, prepare the ceramic green blank of diameter 13mm under 10MPa pressure, be finally placed in corundum crucible and exist
1350 DEG C of calcination of in the air become porcelain in 8 hours.
Claims (2)
1. a kind of rare earth base novel non-full of type tungsten bronze ferroelectric material and preparation method thereof, rare earth base is non-fills for this
The chemical formula of full type tungsten bronze ferroelectric material is Ba5(1-x)Ln5xTi5xNb10-5xO30, wherein, Ln=Eu, Sm, Nd;
0.15≤x≤0.30.
2. rare earth base novel as claimed in claim 1 non-full of type tungsten bronze ferroelectric material and preparation method thereof,
It is characterized in that, described ferroelectric material be using simple solid reaction process preparation, described method include as
Lower step:
Step 1:To analyze the BaCO of pure level3、Nb2O5、TiO2, high-purity grade of Nd2O3、Sm2O3、
Eu2O3For raw material, according to chemical formula Ba5(1-x)Ln5xTi5xNb1O-5xO30, wherein, Ln=Eu, Sm, Nd;0.15
≤ x≤0.30, carries out proportioning in accordance with mol ratio;
Step 2:With dehydrated alcohol (99.7%) as medium, the raw material preparing is placed in clean agate pot,
Ball milling is carried out on planetary ball mill, Ball-milling Time is 24 hours;
Step 3:Slurry after ball milling is placed in beaker, dries in electric heating convection oven, drying time
12 hours, 95 degree of drying temperature, obtain and dry powder body;
Step 4:Powder body agate mortar will be dried grind, and be subsequently placed in and add a cover in corundum crucible, put into box
In stove, continuous warming, to 1300 degree of pre-burnings 8 hours, program determination after being cooled to 550 degree, cools to the furnace
Room temperature, comes out of the stove;
Step 5:The product that step 4 is obtained is ground with agate mortar, makes pre-burning powder body;
Step 6:Add concentration to be~5% PVP in pre-burning powder body, be fully ground, mix homogeneously, from
So it is dried, pelletize;
Step 7:Step 6 gained powder body is prepared diameter~13mm, thickness~2mm under 10MPa pressure
Ceramic green blank;
Step 8;By step 7 ceramic green blank, it is placed in batch-type furnace, continuous warming, in 700 degree of insulations 2
Individual hour carries out plastic removal, then sinters 8 hours at 1350 degree, program determination after being cooled to 550 degree, with stove
Be cooled to room temperature, come out of the stove, obtain rare earth base novel non-full of type tungsten bronze ferroelectric material.
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CN108147815A (en) * | 2017-12-29 | 2018-06-12 | 陕西科技大学 | A kind of single-phase multiferroic ceramic material of tungsten bronze type and preparation method thereof |
CN111087023A (en) * | 2019-11-28 | 2020-05-01 | 郑州轻工业大学 | Room temperature multiferroic material Ba4SmFe0.5Nb9.5O30Preparation method of (1) and prepared room-temperature multiferroic material |
CN114804871A (en) * | 2022-05-18 | 2022-07-29 | 中国民航大学 | Tungsten bronze-based photochromic ceramic material and preparation method thereof |
CN115286387A (en) * | 2022-08-12 | 2022-11-04 | 中国民航大学 | Tungsten bronze-based ceramic material, flexible material based on tungsten bronze-based ceramic material and preparation method of flexible material |
WO2023160504A1 (en) * | 2022-02-24 | 2023-08-31 | 华为技术有限公司 | Dielectric ceramic, dielectric ceramic material, filter, radio frequency unit, and communication device |
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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Cited By (9)
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CN108147815A (en) * | 2017-12-29 | 2018-06-12 | 陕西科技大学 | A kind of single-phase multiferroic ceramic material of tungsten bronze type and preparation method thereof |
CN108147815B (en) * | 2017-12-29 | 2021-04-06 | 陕西科技大学 | Tungsten bronze type single-phase multiferroic ceramic material and preparation method thereof |
CN111087023A (en) * | 2019-11-28 | 2020-05-01 | 郑州轻工业大学 | Room temperature multiferroic material Ba4SmFe0.5Nb9.5O30Preparation method of (1) and prepared room-temperature multiferroic material |
CN111087023B (en) * | 2019-11-28 | 2022-05-20 | 郑州轻工业大学 | Room temperature multiferroic material Ba4SmFe0.5Nb9.5O30Preparation method of (2) and prepared room-temperature multiferroic material |
WO2023160504A1 (en) * | 2022-02-24 | 2023-08-31 | 华为技术有限公司 | Dielectric ceramic, dielectric ceramic material, filter, radio frequency unit, and communication device |
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 |
CN115286387A (en) * | 2022-08-12 | 2022-11-04 | 中国民航大学 | Tungsten bronze-based ceramic material, flexible material based on tungsten bronze-based ceramic material and preparation method of flexible material |
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