CN107500751A - The preparation method of nanometer piezoceramic material - Google Patents
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Abstract
The present invention relates to the preparation method of a kind of nanometer of piezoceramic material, comprise the following steps：(1) weighed raw material by composition proportion；(2) mixed grinding：Raw material are put into ball mill and are ground；(3) pre-burning：Powder after grinding is put into Muffle furnace and is fired, the temperature of Muffle furnace fires 12 24h at 1,000 1500 degree；(4) secondary fine grinding：Powder after firing is placed again into ball mill and is ground, using absolute ethyl alcohol as medium；(5) it is granulated：Powder after secondary grinding adds adhesive, is granulated；(6) it is compressing；(7) plastic removal：Ceramic blank, which is put into Muffle furnace, heats plastic removal, and plastic removal temperature is 600 700 degree, and the plastic removal time is 2 4h；(8) sinter molding：Ceramic blank after plastic removal, which is put into the Muffle furnace for be connected with nitrogen, to be sintered, and sintering time is 5 10h, and sintering temperature is 1,000 1600 degree, obtains a nanometer piezoceramic material.
Description
Technical field
The present invention relates to chemical material technical field, more particularly to the preparation method of a kind of nanometer of piezoceramic material.
Background technology
Piezoelectric ceramics can realize the mutual conversion between mechanical energy and electric energy, be set using electromechanics made of piezoelectric ceramics
It is standby：Such as sensor, transducer have been widely used in each neck of military affairs, national defence, medical treatment and human being's production life
Domain.PZT base piezoelectric ceramics are since discovery because its excellent electric property is most widely used a kind of ceramic material.Mesh
Before, the PZT bases ceramics of the mainly Mn-modified used in power-type ultrasonic transducer, this kind of piezoelectric ceramics strain constant
The relatively low only 230-330pC/N of d33, have had a strong impact on the conversion efficiency between electric energy and mechanical energy, in addition the temperature of such material
It is poor to spend stability, causes transducer to be not suitable for using in high temperature environments and service life is short, power ultrasonic pair can not be met
The requirement of device, it finally have impact on the development in power ultrasonic field.
Therefore, in order to solve the problems such as piezoelectric ceramics performance is low, temperature stability is poor, service life is short, it is necessary to develop
A kind of method for preparing nanometer piezoceramic material, makes the nanometer piezoelectric of acquisition have good high tension performance high temperature
Spend stability.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of nanometer piezoelectricity pottery of high tension performance high-temperature stability
Ceramic material.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：This nanometer of piezoceramic material, composition
Weight proportion：Barium titanate 60-70 parts, aluminum oxide 10-20 parts, nano magnesia 2-7 parts, antimony oxide 3-6 parts, titanium dioxide
Zirconium 1-10 parts, Polycarbosilane 1-6 parts, sodium fluoride 1-5 parts, prodan 1-6 parts, cerium oxide 1-5 parts, cullet 1-5 parts, carbon
SiClx 1-5 parts.
Alternatively, 62 parts of barium titanate, 13 parts of aluminum oxide, 3 parts of nano magnesia, 4 parts of antimony oxide, zirconium dioxide 5
Part, 1 part of Polycarbosilane, 2 parts of sodium fluoride, 3 parts of prodan, 1 part of cerium oxide, 3 parts of cullet, 3 parts of carborundum.
The present invention further improvement is that, the composition of cullet is by mass percentage：Alundum (Al2O3) 4%, three oxygen
Change two boron 1%, calcium oxide 1%, zinc oxide 7.5%, barium monoxide 2%, three oxidations two receive 0.5%, potassium oxide 3%, three oxidations two
Iron 0.5%, surplus are silica.
The present invention also technical problems to be solved are to provide the preparation method of a kind of nanometer of piezoceramic material.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：The preparation of this nanometer of piezoceramic material
Method, comprise the following steps：
(1) early-stage preparations：Weighed raw material by composition proportion, and remove the granule foreign in dispensing, it is stand-by；
(2) mixed grinding：The raw material prepared in step (1) are put into planetary ball mill and are ground, make powder
Well mixed, particle diameter is in 100-500nm；
(3) pre-burning：Powder after being ground in step (2) is put into Muffle furnace and is fired, the temperature of Muffle furnace exists
1000-1500 degree, fire 12-24h；
(4) secondary fine grinding：Powder after firing in step (3) is placed again into planetary ball mill to be ground, with
Absolute ethyl alcohol is medium, makes the particle diameter of powder in 50-100nm；
(5) it is granulated：Powder in step (4) after secondary grinding is added into adhesive, 3g adhesives are added per 100g,
It is granulated；
(6) it is compressing：Ceramic blank shaping is carried out to blank when pressure is 220-300MPa；
(7) plastic removal：The ceramic blank of step (6) is put into Muffle furnace and heats plastic removal, plastic removal temperature is 600-700 degree, row
The modeling time is 2-4h；
(8) sinter molding：Ceramic blank in step (7) after plastic removal is put into the Muffle furnace for be connected with nitrogen and carried out
Sintering, sintering time 5-10h, sintering temperature is 1000-1600 degree, obtains a nanometer piezoceramic material.
The present invention further improvement is that, the adhesive in the step (5) is the polyvinyl alcohol that mass concentration is 5%
The aqueous solution.
The present invention further improvement is that, the ball mill is planetary ball mill.
The present invention further improvement is that, the component quality proportioning in the step (1) is：Barium titanate 50-65 parts, oxygen
Change aluminium 10-20 parts, nano magnesia 2-7 parts, antimony oxide 3-6 parts, zirconium dioxide 1-10 parts, Polycarbosilane 1-6 parts, fluorine
Change sodium 1-5 parts, prodan 1-6 parts, cerium oxide 1-5 parts, cullet 1-5 parts, carborundum 1-5 parts.
Compared with prior art, the invention has the advantages that：The nanometer piezoceramic material of the present invention has good
Good stability and practicality, and there is high tension performance high-temperature stability, it can be widely applied to battery, ultrasound etc. neck
Domain.
Embodiment
In order to deepen the understanding of the present invention, the present invention is described in further detail below in conjunction with embodiment, the reality
Apply example to be only used for explaining the present invention, protection scope of the present invention is not formed and limited.
Embodiment 1：This nanometer of piezoceramic material, it is characterised in that composition weight proportion：Barium titanate 500g, aluminum oxide
100g, nano magnesia 20g, antimony oxide 30g, zirconium dioxide 10g, Polycarbosilane 60g parts, sodium fluoride 10g, fluosilicic acid
Sodium 10g, cerium oxide 10g, cullet 10g, carborundum 10g, the composition of wherein cullet are by mass percentage：Three oxidations
Two aluminium 4%, diboron trioxide 1%, calcium oxide 1%, zinc oxide 7.5%, barium monoxide 2%, three oxidations two receive 0.5%, potassium oxide
3%, di-iron trioxide 0.5%, surplus is silica.
Embodiment 2：Barium titanate 620g, aluminum oxide 130g, nano magnesia 30g, antimony oxide 40g, zirconium dioxide
50g, Polycarbosilane 10g, sodium fluoride 20g, prodan 30g, cerium oxide 10g, cullet 30g, carborundum 30g；Wherein useless glass
The composition of glass is by mass percentage：Alundum (Al2O3) 4%, diboron trioxide 1%, calcium oxide 1%, zinc oxide 7.5%,
Barium monoxide 2%, three oxidations two receive 0.5%, and potassium oxide 3%, di-iron trioxide 0.5%, surplus is silica.
Embodiment 3：Barium titanate 700g, aluminum oxide 150g, nano magnesia 40g, antimony oxide 50g, zirconium dioxide
70g, Polycarbosilane 30g, sodium fluoride 30g, prodan 50g, cerium oxide 30g, cullet 50g, carborundum 50g；Wherein useless glass
The composition of glass is by mass percentage：Alundum (Al2O3) 4%, diboron trioxide 1%, calcium oxide 1%, zinc oxide 7.5%,
Barium monoxide 2%, three oxidations two receive 0.5%, and potassium oxide 3%, di-iron trioxide 0.5%, surplus is silica.
Embodiment 4：Barium titanate 700g, aluminum oxide 200g, nano magnesia 70g, antimony oxide 60g, zirconium dioxide
100g, Polycarbosilane 60g, sodium fluoride 50g, prodan 60g, cerium oxide 50g, cullet 50g, carborundum 50g；It is wherein useless
The composition of glass is by mass percentage：Alundum (Al2O3) 4%, diboron trioxide 1%, calcium oxide 1%, zinc oxide
7.5%, barium monoxide 2%, three oxidations two receive 0.5%, and potassium oxide 3%, di-iron trioxide 0.5%, surplus is silica.
Embodiment 1-4 uses following preparation method.
Embodiment 5：The preparation method of this nanometer of piezoceramic material, comprises the following steps：
(1) early-stage preparations：Weighed raw material by composition proportion, and remove the granule foreign in dispensing, it is stand-by；
(2) mixed grinding：The raw material prepared in step (1) are put into planetary ball mill and are ground, make powder
Well mixed, particle diameter is in 100-500nm；
(3) pre-burning：Powder after being ground in step (2) is put into Muffle furnace and is fired, the temperature of Muffle furnace exists
1000 degree, fire 24h；
(4) secondary fine grinding：Powder after firing in step (3) is placed again into planetary ball mill to be ground, with
Absolute ethyl alcohol is medium, makes the particle diameter of powder in 50-100nm；
(5) it is granulated：Powder in step (4) after secondary grinding is added into adhesive, 3g adhesives are added per 100g,
It is granulated；Adhesive is the polyvinyl alcohol water solution that mass concentration is 5%；
(6) it is compressing：Ceramic blank shaping is carried out to blank when pressure is 220MPa；
(7) plastic removal：The ceramic blank of step (6) is put into Muffle furnace and heats plastic removal, plastic removal temperature is 600 degree, during plastic removal
Between be 4h；
(8) sinter molding：Ceramic blank in step (7) after plastic removal is put into the Muffle furnace for be connected with nitrogen and carried out
Sintering, sintering time 10h, sintering temperature are 1000 degree, obtain a nanometer piezoceramic material.
Embodiment 6：The preparation method of this nanometer of piezoceramic material, comprises the following steps：
(1) early-stage preparations：Weighed raw material by composition proportion, and remove the granule foreign in dispensing, it is stand-by；
(2) mixed grinding：The raw material prepared in step (1) are put into planetary ball mill and are ground, make powder
Well mixed, particle diameter is in 100-500nm；
(3) pre-burning：Powder after being ground in step (2) is put into Muffle furnace and is fired, the temperature of Muffle furnace exists
1200 degree, fire 17h；
(4) secondary fine grinding：Powder after firing in step (3) is placed again into planetary ball mill to be ground, with
Absolute ethyl alcohol is medium, makes the particle diameter of powder in 50-100nm；
(5) it is granulated：Powder in step (4) after secondary grinding is added into adhesive, 3g adhesives are added per 100g,
It is granulated；Adhesive is the polyvinyl alcohol water solution that mass concentration is 5%；
(6) it is compressing：Ceramic blank shaping is carried out to blank when pressure is 220-300MPa；
(7) plastic removal：The ceramic blank of step (6) is put into Muffle furnace and heats plastic removal, plastic removal temperature is 650 degree, during plastic removal
Between be 2h；
(8) sinter molding：Ceramic blank in step (7) after plastic removal is put into the Muffle furnace for be connected with nitrogen and carried out
Sintering, sintering time 5h, sintering temperature are 1300 degree, obtain a nanometer piezoceramic material.
The nanometer piezoceramic material that embodiment 1 to embodiment 4 is prepared using the method for embodiment 5 and embodiment 6
Performance test is carried out respectively, and result of the test is respectively such as table 1：
The property of nanometer piezoceramic material made from the method for embodiment 5 and embodiment 6 is respectively adopted in the embodiment 1-4 of table 1
Can test
Simultaneously will above-mentioned 8 kinds of laboratory samples progress stability test, applied subzero 10 degrees Celsius, 20 degrees Celsius,
Used under 30 degrees Celsius, carry out dielectric constant, compressive resistance respectively 1 month, 3 months, 6 months, 9 months, 12 months and break
Toughness detection is split, at first 6 months, dielectric constant, compressive resistance and fracture toughness did not change, illustrated this nanometer of piezoelectricity
Ceramic material has good stability and cold resistance, and when at -12 months 9 months, dielectric constant have dropped 1.0%, pressure-resistant
Intensity and fracture toughness have dropped 0.8% or so.
For the ordinary skill in the art, simply the present invention is exemplarily described for specific embodiment,
Obviously present invention specific implementation is not subject to the restrictions described above, as long as employing the inventive concept and technical scheme of the present invention
Carry out various unsubstantialities improvement, or it is not improved by the present invention design and technical scheme directly apply to other fields
Close, within protection scope of the present invention.
Claims (4)
1. the preparation method of a kind of nanometer of piezoceramic material, it is characterised in that comprise the following steps：
(1) early-stage preparations：Weighed raw material by composition proportion, and remove the granule foreign in dispensing, it is stand-by；
(2) mixed grinding：The raw material prepared in step (1) are put into ball mill and are ground, are well mixed powder, grain
Footpath is in 100-500nm；
(3) pre-burning：Powder after being ground in step (2) is put into Muffle furnace and is fired, the temperature of Muffle furnace is in 1000-
1500 degree, fire 12-24h；
(4) secondary fine grinding：Powder after firing in step (3) is placed again into ball mill to be ground, using absolute ethyl alcohol as
Medium, make the particle diameter of powder in 50-100nm；
(5) it is granulated：Powder in step (4) after secondary grinding is added into adhesive, 3g adhesives are added per 100g, are made
Grain；
(6) it is compressing：Ceramic blank shaping is carried out to blank when pressure is 220-300MPa；
(7) plastic removal：The ceramic blank of step (6) is put into Muffle furnace and heats plastic removal, plastic removal temperature is 600-700 degree, during plastic removal
Between be 2-4h；
(8) sinter molding：Ceramic blank in step (7) after plastic removal is put into the Muffle furnace for be connected with nitrogen and is sintered,
Sintering time is 5-10h, and sintering temperature is 1000-1600 degree, obtains a nanometer piezoceramic material.
2. the preparation method of according to claim 1 nanometer of piezoceramic material, it is characterised in that in the step (5)
Adhesive be polyvinyl alcohol water solution that mass concentration is 5%.
3. the preparation method of according to claim 2 nanometer of piezoceramic material, it is characterised in that the ball mill is row
Planetary ball mill.
4. the preparation method of according to claim 3 nanometer of piezoceramic material, it is characterised in that in the step (1)
Component quality proportioning be：Barium titanate 60-70 parts, aluminum oxide 10-20 parts, nano magnesia 2-7 parts, antimony oxide 3-6 parts,
Zirconium dioxide 1-10 parts, Polycarbosilane 1-6 parts, sodium fluoride 1-5 parts, prodan 1-6 parts, cerium oxide 1-5 parts, cullet 1-5
Part, carborundum 1-5 parts.
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| CN201710654415.4A CN107500751A (en) | 2017-08-03 | 2017-08-03 | The preparation method of nanometer piezoceramic material |
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| CN201710654415.4A CN107500751A (en) | 2017-08-03 | 2017-08-03 | The preparation method of nanometer piezoceramic material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109626520A (en) * | 2019-01-24 | 2019-04-16 | 华禹环保(南京)有限公司 | A kind of efficient electric catalysis oxidation electrode production technology |
| CN111704458A (en) * | 2020-05-24 | 2020-09-25 | 福建华夏金刚科技股份有限公司 | Fine functional ceramic containing silicon dioxide nanocrystals and preparation method thereof |
| CN112279638A (en) * | 2020-10-23 | 2021-01-29 | 山东工业陶瓷研究设计院有限公司 | Lead-free PTC thermistor ceramic with far infrared performance and preparation method thereof |
| CN115254610A (en) * | 2022-08-02 | 2022-11-01 | 浙江元集新材料有限公司 | Fine classifier impeller for processing ceramic powder for copper-clad plate and manufacturing method thereof |
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| CN102718482A (en) * | 2012-05-24 | 2012-10-10 | 成都汇通西电电子有限公司 | Piezoceramic material and preparation method thereof, and piezoelectric generating oscillator |
| CN105254287A (en) * | 2015-09-29 | 2016-01-20 | 苏州宽温电子科技有限公司 | Nano piezoceramic material and preparation method thereof |
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| CN102718482A (en) * | 2012-05-24 | 2012-10-10 | 成都汇通西电电子有限公司 | Piezoceramic material and preparation method thereof, and piezoelectric generating oscillator |
| CN105254287A (en) * | 2015-09-29 | 2016-01-20 | 苏州宽温电子科技有限公司 | Nano piezoceramic material and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109626520A (en) * | 2019-01-24 | 2019-04-16 | 华禹环保(南京)有限公司 | A kind of efficient electric catalysis oxidation electrode production technology |
| CN111704458A (en) * | 2020-05-24 | 2020-09-25 | 福建华夏金刚科技股份有限公司 | Fine functional ceramic containing silicon dioxide nanocrystals and preparation method thereof |
| CN111704458B (en) * | 2020-05-24 | 2022-05-27 | 福建华夏金刚科技股份有限公司 | Fine functional ceramic containing silicon dioxide nanocrystals and preparation method thereof |
| CN112279638A (en) * | 2020-10-23 | 2021-01-29 | 山东工业陶瓷研究设计院有限公司 | Lead-free PTC thermistor ceramic with far infrared performance and preparation method thereof |
| CN115254610A (en) * | 2022-08-02 | 2022-11-01 | 浙江元集新材料有限公司 | Fine classifier impeller for processing ceramic powder for copper-clad plate and manufacturing method thereof |
| CN115254610B (en) * | 2022-08-02 | 2023-09-15 | 浙江元集新材料有限公司 | Fine classifier impeller for processing ceramic powder for copper-clad plate and manufacturing method thereof |
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Application publication date: 20171222 |