CN107244897A - A kind of giant dielectric ceramic material and preparation method thereof - Google Patents
A kind of giant dielectric ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of giant dielectric ceramic material and preparation method thereof, with barium carbonate, cobalt sesquioxide and niobium pentaoxide are raw material, in 200~450 revs/min of speed mixing and ball milling 8~24 hours, by the powder after ball milling under 200~400MPa of uniaxial pressure it is compressing；Then it is put into high pressure combustion freezing of a furnace, first add high pressure 3~7GPa, then 1000~1200 DEG C is warming up to 20~40 DEG C/min heating rate and sinter 30~120 minutes, room temperature is then down to 20~50 DEG C/min speed, high pressure is finally removed.The present invention is sintered under super-pressure, is conducive to Ba (Co0.5Nb0.5)O3Ceramic body keeps stable；Compound is held in superelevation pressure condition during whole high―temperature nuclei, it is suppressed that due to the appearance of the second phase caused by lattice strain etc., so as to obtain pure Ba (Co0.5Nb0.5)O3Ceramic body.
Description
Technical field
The present invention relates to electronic ceramic fields, and in particular to a kind of Ba (Co0.5Nb0.5)O3Giant dielectric ceramic material and its system
Preparation Method.
Background technology
Microelectronics information technology it is fast-developing to being miniaturized of electronic component, it is integrated propose higher requirement,
As the important component part of electronic component, the research of dielectric ceramics is more and more paid close attention to by people.With information
The need of work of the technical field especially development of electronics and microelectronic industry and extreme environment, with good temperature and
The huge dielectric constant of frequency stability, the dielectric substance of low-dielectric loss have a wide range of applications.
Ceramic material with perovskite structure always because its huge dielectric constant and and very low dielectric loss and it is standby
It is concerned, and perovskite structure ceramic material can keep stability in very wide temperature and frequency range.In recent years, it is electric
Sub- component makes rapid progress, and miniaturization, high-effect and low-power consumption turn into important development direction, and to the various acousto-optic-electrics of device
The performance such as pyromagnetic has more careful requirements.This also requires that the physical and chemical performance for studying more multielement, develops more
New material species meet the demand of different levels.
It is non-ferromagnetic elements positioned at three kinds of elemental vanadiums of the 5th subgroup, niobium, tantalum, and in production and life
Find broad application, the application studied and further develop these elements has important economic benefit.For example, using tantalum capacitor
Used in consumer fields such as military and national defenses, but tantalum element resource scarcity, therefore tantalum element is into a kind of strategic resources.Niobium element
Alkali metal compound, such as Li2NbO3(lithium niobate) has the inclined tripartite's crystal structure of Ca-Ti ore type, and cobalt acid lithium is a kind of common
Electrode material.Research has shown that Nb and Co codopes can form composite perofskite based structures, and due to both most
Outer-shell electron number is different, can be in crystals formation disfigurement model, while discharging delocalized electron.Therefore trial carbonic acid
Barium, niobium pentaoxide, cobalt sesquioxide go to synthesize Co in composite perofskite base ceramic material, chemical formula3+、Nb5+, pass through alms giver
Acted on acceptor's codope, form disfigurement model, and barium ions has close atomic radius with the two, and be common system
Standby giant dielectric ceramic body raw material.At present on Ba (Co0.5Nb0.5)O3The report of ceramic preparation is also rarely found, is used as one kind
With the potential material extensively using value, it is necessary to preparation technology that is a kind of suitable and being beneficial to popularization is explored, with more preferable
Research Ba (Co0.5Nb0.5)O3The properity of ceramics.
The content of the invention
It is an object of the invention to overcoming the problem above that prior art is present there is provided a kind of giant dielectric ceramic material and its
Preparation method, the Ba (Co that the present invention is obtained0.5Nb0.5)O3Ceramics are one of typical Nb bases complex perovskite structure materials, and
And measure it and have very high dielectric constant and good temperature and frequency stability.
To realize above-mentioned technical purpose and the technique effect, the present invention is achieved through the following technical solutions：
A kind of giant dielectric ceramic material, giant dielectric ceramic material is according to chemical equation 4BaCO3+Nb2O5+ Co2O3=4Ba
(Co0.5Nb0.5)O3+4CO2It is made,
Wherein, barium carbonate, niobium pentaoxide, the mol ratio of cobalt sesquioxide are 4:1:1, every kind of material molar ratio content is inclined
Poor scope is 0-5%.
Further comprise, the barium carbonate, niobium pentaoxide, cobalt sesquioxide are to analyze pure or high pure raw material.
A kind of preparation method of giant dielectric ceramic material, comprises the following steps：
(1) using barium carbonate, niobium pentaoxide and cobalt sesquioxide as raw material, by Formula B a (Co0.5Nb0.5)O3Chemistry meter
Amount obtains raw mixture than carrying out dispensing；
(2) raw mixture for preparing step (1) is put into ball mill, adds zirconia ball and absolute ethyl alcohol is
Ball-milling medium, is well mixed in ball mill, then dries mixed slurry, obtains powder；
(3) by the powder obtained in step (2) under 200~400MPa of uniaxial pressure it is compressing, obtain block；
(4) block for being molded step (3), is placed in high pressure combustion freezing of a furnace and is sintered, drop to after room temperature, remove high pressure,
Obtain Ba (Co0.5Nb0.5)O3Giant dielectric ceramic body.
Further comprise, the zirconia ball quality is 4~8 times of raw material mixture quality in (1), the absolute ethyl alcohol
Quality is 0.5~2 times of raw mixture quality.
Further comprise, the ball mill in step (2) is planetary ball mill, and raw mixture is in planetary ball mill
Ball milling mixing 8~24 hours, rotating speed is 200~450 revs/min.
Further comprise, take out the slurry after ball milling mixing in step (2), dry, obtain at a temperature of 80 DEG C~140 DEG C
Obtain powder.
Further comprise, the condition of step (4) high temperature sintering is：First add high pressure 3~8GPa, with 20~40 DEG C/min
Heating rate rise to 1000~1200 DEG C, insulation is sintered for 30~120 minutes, is then dropped with 20~50 DEG C/min speed
To room temperature, high pressure is finally removed.
The beneficial effects of the invention are as follows:
1. the invention provides a kind of Ba (Co0.5Nb0.5)O3The method of giant dielectric ceramic material, and under super-pressure,
Be conducive to Ba (Co0.5Nb0.5)O3Ceramic body keeps stable.Compound involved in the present invention is equal during whole high―temperature nuclei
It is maintained at superelevation pressure condition, it is suppressed that due to the appearance of the second phase caused by lattice strain etc., so as to obtain pure Ba
(Co0.5Nb0.5)O3Ceramic body.
2. Ba (the Co that the present invention is obtained0.5Nb0.5)O3Ceramics are one of typical Nb bases complex perovskite structure materials, and
And measure it and have very high dielectric constant and good temperature and frequency stability.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, below with presently preferred embodiments of the present invention and coordinate accompanying drawing describe in detail as after.
The embodiment of the present invention is shown in detail by following examples and its accompanying drawing.
Brief description of the drawings
Technical scheme in technology in order to illustrate the embodiments of the present invention more clearly, in being described below to embodiment technology
The required accompanying drawing used is briefly described, it should be apparent that, drawings in the following description are only some realities of the present invention
Example is applied, for those of ordinary skill in the art, on the premise of not paying creative work, can also be according to these accompanying drawings
Obtain other accompanying drawings.
Fig. 1 is that the embodiment of the present invention 1 adds high pressure and is not added with the Ba (Co that are prepared under condition of high voltage with comparative example 10.5Nb0.5)O3
Powder X ray diffracting spectrum.
Fig. 2 is Ba (Co prepared by the embodiment of the present invention 10.5Nb0.5)O3The scanning electron microscope image of powder.
Fig. 3 is the Ba (Co that comparative example 1 of the present invention is prepared under conditions of not adding high pressure0.5Nb0.5)O3The scanning electricity of powder
Sub- MIcrosope image.
Fig. 4 is Ba (Co prepared by comparative example 2 of the present invention0.5Nb0.5)O3The scanning electron microscope image of powder.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
Giant dielectric ceramic material in following examples is according to chemical equation 4BaCO3+Nb2O5+Co2O3=4Ba
(Co0.5Nb0.5)O3+4CO2It is made,
Wherein, barium carbonate, niobium pentaoxide, the mol ratio of cobalt sesquioxide are 4:1:1, every kind of material molar ratio content is inclined
Poor scope is 0-5%.
Embodiment 1
Ba (Co are prepared in embodiment 10.5Nb0.5)O3Giant dielectric ceramic material, specific preparation process is：
(1) using barium carbonate, cobalt sesquioxide and niobium pentaoxide as raw material, by Formula B a (Co0.5Nb0.5)O3Stoichiometry
Than carrying out dispensing, barium carbonate, niobium pentaoxide, the mol ratio of cobalt sesquioxide are 4:1:1.
(2) raw material for preparing step (1) is put into ball mill, is added zirconia ball and absolute ethyl alcohol and is situated between for ball milling
Matter, added zirconia ball quality is 4 times of material quality, and added absolute ethyl alcohol quality is 0.5 times of material quality, is expert at
Ball milling mixing 8 hours in planetary ball mill, rotating speed is 450 revs/min, and mixed slurry is taken out in 140 DEG C of drying.
(3) powder for drying step (2) is compressing under uniaxial pressure 200MPa.
(4) block for being molded step (3), is placed in high pressure combustion freezing of a furnace, first add high pressure 3GPa, with 20 DEG C/min liter
Warm speed rises to 1000 DEG C, and insulation is sintered for 60 minutes, is then dropped to room temperature with 20 DEG C/min, is finally removed high pressure, produces
To Compound perovskite oxide Ba (Co0.5Nb0.5)O3Ceramic body.
Embodiment 2
Ba (Co are prepared in embodiment 20.5Nb0.5)O3Giant dielectric ceramic material, specific preparation process is：
(1) using barium carbonate, cobalt sesquioxide and niobium pentaoxide as raw material, by Formula B a (Co0.5Nb0.5)O3Chemistry meter
Amount is than carrying out dispensing, and barium carbonate, niobium pentaoxide, the mol ratio of cobalt sesquioxide are 4:1.025:1.
(2) raw material for preparing step (1) is put into ball grinder, is added zirconia ball and absolute ethyl alcohol and is situated between for ball milling
Matter, added zirconia ball quality is 6 times of material quality, and added absolute ethyl alcohol quality is 1 times of material quality, in planet
Ball milling mixing 12 hours in formula ball mill, rotating speed is 350 revs/min, and mixed slurry is taken out in 100 DEG C of drying.
(3) powder for drying step (2) is compressing under uniaxial pressure 300MPa.
(4) block for being molded step (3), is placed in high pressure combustion freezing of a furnace, first add high pressure 5GPa, with 30 DEG C/min liter
Warm speed rises to 1200 DEG C, and insulation is sintered for 120 minutes, is then dropped to room temperature with 30 DEG C/min, is finally removed high pressure, i.e.,
Obtain Compound perovskite oxide Ba (Co0.5Nb0.5)O3。
Embodiment 3
Ba (Co are prepared in embodiment 30.5Nb0.5)O3Giant dielectric ceramic material, specific preparation process is：
(1) using barium carbonate, cobalt sesquioxide and niobium pentaoxide as raw material, by Formula B a (Co0.5Nb0.5)O3Chemistry meter
Amount is than carrying out dispensing, and barium carbonate, niobium pentaoxide, the mol ratio of cobalt sesquioxide are 4:1:1.05.
(2) raw material for preparing step (1) is put into ball grinder, is added zirconia ball and absolute ethyl alcohol and is situated between for ball milling
Matter, added zirconia ball quality is 8 times of material quality, and added absolute ethyl alcohol quality is 2 times of material quality, in planet
Ball milling mixing 24 hours in formula ball mill, rotating speed is 400 revs/min, and mixed slurry is taken out in 80 DEG C of drying.
(3) powder for drying step (2) is compressing under uniaxial pressure 400MPa.
(4) block for being molded step (3), is placed in high pressure combustion freezing of a furnace, first add high pressure 8GPa, with 40 DEG C/min liter
Warm speed rises to 1000 DEG C, and insulation is sintered for 30 minutes, is then dropped to room temperature with 50 DEG C/min, is finally removed high pressure, produces
To Ba (Co0.5Nb0.5)O3Ceramic body.
Comparative example 1
Comparative example 1 is contrasted with method and step in embodiment 1, is not sintered in a high voltage state in comparative example 1, specific side
Method step is：
(1) using barium carbonate, cobalt sesquioxide and niobium pentaoxide as raw material, by Formula B a (Co0.5Nb0.5)O3Stoichiometry
Than carrying out dispensing.
(2) raw material for preparing step (1) is put into ball grinder, is added zirconia ball and absolute ethyl alcohol and is situated between for ball milling
Matter, added zirconia ball quality is 4 times of material quality, and added absolute ethyl alcohol quality is 0.5 times of material quality, is expert at
Ball milling mixing 8 hours in planetary ball mill, rotating speed is 450 revs/min, and mixed slurry is taken out in 140 DEG C of drying.
(3) powder for drying step (2) is compressing under uniaxial pressure 200MPa.
(4) block for being molded step (3), is placed in Muffle furnace, and 1000 DEG C, guarantor are risen to 20 DEG C/min heating rate
Temperature is sintered for 60 minutes, is then dropped to room temperature with 20 DEG C/min, is finally removed high pressure, that is, obtains Compound perovskite oxide Ba
(Co0.5Nb0.5)O3Ceramic body.
Comparative example 2
Comparative example 2 is contrasted with method and step in embodiment 1, is sintered in a high voltage state in comparative example 2, but giant dielectric
Ceramic material uses tantalum pentoxide, cobalt sesquioxide, and barium carbonate is raw material
Specific method step be：
(1) using barium carbonate, cobalt sesquioxide and tantalum pentoxide as raw material, by Formula B a (Co0.5Nb0.5)O3Stoichiometry
Than carrying out dispensing.
(2) raw material for preparing step (1) is put into ball grinder, is added zirconia ball and absolute ethyl alcohol and is situated between for ball milling
Matter, added zirconia ball quality is 4 times of material quality, and added absolute ethyl alcohol quality is 0.5 times of material quality, is expert at
Ball milling mixing 8 hours in planetary ball mill, rotating speed is 450 revs/min, and mixed slurry is taken out in 140 DEG C of drying.
(3) powder for drying step (2) is compressing under uniaxial pressure 200MPa.
(4) block for being molded step (3), is placed in high pressure combustion freezing of a furnace, first add high pressure 3GPa, with 20 DEG C/min liter
Warm speed rises to 1000 DEG C, and insulation is sintered for 60 minutes, is then dropped to room temperature with 20 DEG C/min, is finally removed high pressure, produces
To Compound perovskite oxide Ba (Co0.5Nb0.5)O3Ceramic body.
Barium carbonate, cobalt sesquioxide, niobium pentaoxide, the tantalum pentoxide used in embodiment 1-3, comparative example 1-2 is equal
It is pure to analyze.
Performance comparison
Ba (Co in Fig. 1 to synthesize under elevated pressure conditions0.5Nb0.5)O3The x-ray diffraction pattern of ceramics, is pure perovskite
Structure.In the case of same material composition proportioning is shown in Fig. 1 but is not added high pressure, its reaction condition is mutually simultaneously synthesizing
Ceramics, then cannot get pure perovskite structure.
1st, influence of the pressure sintering conditions to giant dielectric ceramic material physicochemical property
As a comparison, Ba (Co are prepared using solid-phase synthesis in the case where not adding high pressure in comparative example 10.5Nb0.5)
O3Ceramics, by the way that the contrast of SEM pictures is found in Fig. 2 and Fig. 3, have synthesized finer and close ceramics under conditions of adding high pressure, and
And stomata quantity is reduced.
2nd, influence of the raw material to giant dielectric ceramic material physicochemical property
With tantalum pentoxide in comparative example 2, cobalt sesquioxide, when barium carbonate is raw material, one in preparation method such as embodiment 1
Cause, by being contrasted in Fig. 2 and Fig. 4, the gentle hole number of ceramic body compactness for sintering out in comparative example 2 is above Ba
(Co0.5Nb0.5)O3Ceramic body, poor-performing.
Also, the data distribution measured with the ceramic body prepared in comparative example 2 in comparative example 1 is into scatter diagram, and temperature liter
It is high to a certain extent when, its dielectric constant drastically declines.The ceramic performance that comparative example 1 and comparative example 2 are prepared is not so good as the application
The ceramic performance of gained is good, therefore is not suitable for promoting the use of.
In embodiment 1-3, under super-pressure, be conducive to Ba (Co0.5Nb0.5)O3Ceramic body keeps stable.It is of the invention involved
And compound superelevation pressure condition is held in during whole high―temperature nuclei, it is suppressed that due to caused by lattice strain etc.
The appearance of two-phase, so as to obtain pure Ba (Co0.5Nb0.5)O3Ceramic body.Ba (the Co obtained in embodiment0.5Nb0.5)O3Pottery
Porcelain is one of typical Nb bases complex perovskite structure material, and measures it and have very high dielectric constant and good temperature
And frequency stability.
The foregoing description of the disclosed embodiments, enables professional and technical personnel in the field to realize or using the present invention.
A variety of modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The most wide scope caused.
Claims (7)
1. a kind of giant dielectric ceramic material, it is characterised in that giant dielectric ceramic material is according to chemical equation 4BaCO3+Nb2O5+
Co2O3=4Ba (Co0.5Nb0.5)O3+4CO2It is made,
Wherein, barium carbonate, niobium pentaoxide, the mol ratio of cobalt sesquioxide are 4:1:1, every kind of material molar ratio content deviation model
Enclose for 0-5%.
2. giant dielectric ceramic material according to claim 1, it is characterised in that the barium carbonate, niobium pentaoxide, three oxygen
Change two cobalts to analyze pure or high pure raw material.
3. a kind of preparation method of giant dielectric ceramic material, it is characterised in that comprise the following steps：
(1) using barium carbonate, niobium pentaoxide and cobalt sesquioxide as raw material, by Formula B a (Co0.5Nb0.5)O3Stoichiometric proportion
Dispensing is carried out, raw mixture is obtained；
(2) raw mixture for preparing step (1) is put into ball mill, and it is ball milling to add zirconia ball and absolute ethyl alcohol
Medium, is well mixed in ball mill, then dries mixed slurry, obtains powder；
(3) by the powder obtained in step (2) under 200~400MPa of uniaxial pressure it is compressing, obtain block；
(4) block for being molded step (3), is placed in high pressure combustion freezing of a furnace and is sintered, drop to after room temperature, remove high pressure, produce
To Ba (Co0.5Nb0.5)O3Giant dielectric ceramic body.
4. a kind of preparation method of giant dielectric ceramic material according to claim 3, it is characterised in that the zirconia ball
Quality is 4~8 times of raw material mixture quality in (1), and the absolute ethyl alcohol quality is 0.5~2 times of raw mixture quality.
5. the preparation method of a kind of giant dielectric ceramic material according to claim 3, it is characterised in that in step (2)
Ball mill is planetary ball mill, raw mixture ball milling mixing 8~24 hours in planetary ball mill, rotating speed is 200~
450 revs/min.
6. the preparation method of a kind of giant dielectric ceramic material according to claim 3, it is characterised in that will in step (2)
Slurry after ball milling mixing takes out, and is dried at a temperature of 80 DEG C~140 DEG C, obtains powder.
7. the preparation method of a kind of giant dielectric ceramic material according to claim 3, it is characterised in that high in step (4)
Temperature sintering condition be：First added high pressure 3~8GPa, and 1000~1200 DEG C, insulation are risen to 20~40 DEG C/min heating rate
It is sintered within 30~120 minutes, room temperature is then dropped to 20~50 DEG C/min speed, high pressure is finally removed.
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| CN112159213A (en) * | 2020-10-29 | 2021-01-01 | 贵州赛义光电科技有限公司 | Zero-light-decay luminescent ceramic and preparation method thereof |
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| CN102219510A (en) * | 2011-04-13 | 2011-10-19 | 浙江大学 | Giant dielectric constant composite material and preparation method thereof |
| CN103204677A (en) * | 2013-03-12 | 2013-07-17 | 西北大学 | High-dielectric-property X8R-type ceramic capacitor dielectric materials and preparation method thereof |
| CN104844194A (en) * | 2015-04-13 | 2015-08-19 | 电子科技大学 | A-B site simultaneously substituting microwave dielectric ceramic material and preparation method thereof |
| CN105777111A (en) * | 2016-03-23 | 2016-07-20 | 武汉理工大学 | Dielectric ceramic material with giant dielectric constant and low dielectric loss and method for preparing dielectric ceramic material |
| CN105967678A (en) * | 2016-04-29 | 2016-09-28 | 江苏大学 | Giant-dielectric ceramic capacitor medium and preparation method thereof |
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| CN102219510A (en) * | 2011-04-13 | 2011-10-19 | 浙江大学 | Giant dielectric constant composite material and preparation method thereof |
| CN103204677A (en) * | 2013-03-12 | 2013-07-17 | 西北大学 | High-dielectric-property X8R-type ceramic capacitor dielectric materials and preparation method thereof |
| CN104844194A (en) * | 2015-04-13 | 2015-08-19 | 电子科技大学 | A-B site simultaneously substituting microwave dielectric ceramic material and preparation method thereof |
| CN105777111A (en) * | 2016-03-23 | 2016-07-20 | 武汉理工大学 | Dielectric ceramic material with giant dielectric constant and low dielectric loss and method for preparing dielectric ceramic material |
| CN105967678A (en) * | 2016-04-29 | 2016-09-28 | 江苏大学 | Giant-dielectric ceramic capacitor medium and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112159213A (en) * | 2020-10-29 | 2021-01-01 | 贵州赛义光电科技有限公司 | Zero-light-decay luminescent ceramic and preparation method thereof |
| CN112159213B (en) * | 2020-10-29 | 2023-07-18 | 贵州赛义光电科技有限公司 | Zero-light-attenuation luminous ceramic and preparation method thereof |
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