CN108383522A - A kind of low temperature Fast Sintering prepares the method and piezoelectric ceramics of PZT piezoelectric ceramics - Google Patents
A kind of low temperature Fast Sintering prepares the method and piezoelectric ceramics of PZT piezoelectric ceramics Download PDFInfo
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Abstract
The invention discloses methods and piezoelectric ceramics that a kind of low temperature Fast Sintering prepares PZT piezoelectric ceramics, while being sintered to PZT piezoelectric ceramics green bodies, apply electric field to PZT piezoelectric ceramics green bodies;Solve the problems, such as the PbO volatilizations caused by being grown sintering temperature height and sintering time during conventional sintering and high energy consumption.Present invention process route is simple, and prepared PZT piezoelectric ceramics consistency is high, is able to batch production.
Description
Technical field
The invention belongs to function ceramics fabricating technology fields, and PZT is prepared more particularly to a kind of low temperature Fast Sintering
The method and piezoelectric ceramics of piezoelectric ceramics.
Background technology
Lead zirconate titanate (PbZrxTi1-xO3, abbreviation PZT) and it is a kind of important piezoelectric ceramics, there is Curie temperature height, piezoelectricity
Property strong, easy doping property and the features such as stablized.Due to electric properties such as its excellent piezoelectricity, dielectric and photoelectricity, can widely answer
For high-tech sectors such as electronics, space flight, the electronic components such as sensor, energy converter, reservoir are used to prepare, are a kind of development
The very good ceramic material of foreground.
Under normal conditions, the sintering temperature of PZT piezoelectric ceramics is 1200 DEG C or more, and sintering time is more than 2h.In high temperature and
Under prolonged sintering condition, PbO is readily volatilized so that deviation occurs for the stoichiometric ratio of PZT piezoelectric ceramics, leads to performance not
Stablize, pollutes the environment simultaneously.In order to reduce the volatilization and loss of lead under high temperature, generally it is added in initial p ZT green bodies
Excessive PbO, or sintered body is placed in closed container, and be embedded in PbO and be sintered.However, this method is difficult to accurately
The content of Pb leads to reduced performance so that Pb is excessive or in shortage in final products in control PZT ceramics.Other one
Kind method is that the oxide of low melting point is added in PZT powders, and sintering temperature is reduced by liquid-phase sintering.However, being sintered
It often will produce impurity phase in the process, lead to the reduced performance of PZT piezoelectric ceramics.
Invention content
For the defect and deficiency of existing preparation method, the first purpose of the invention is to provide a kind of low temperature Fast Sinterings
The method for preparing PZT piezoelectric ceramics, this method preparation process is simple, is suitable for producing in batches.
Second object of the present invention is to provide a kind of piezoelectric ceramics, and piezoelectric ceramics method using the present invention is prepared into
It arrives.
To achieve the goals above, the technical solution that the present invention takes includes:
A kind of method that low temperature Fast Sintering prepares PZT piezoelectric ceramics, it is same being sintered to PZT piezoelectric ceramics green bodies
When, apply electric field to PZT piezoelectric ceramics green bodies.
Optionally, the electric field strength is 300~2000V/cm.
Optionally, the sintering includes being started to warm up from room temperature, until temperature be 300~800 DEG C, soaking time 2s
~60min, heating rate are 1~50 DEG C/min.
Optionally, PZT piezoelectric ceramics green bodies are placed in sintering furnace, by platinum filament by PZT piezoelectric ceramics green body and high pressure
Power supply connects.
Optionally, sintering furnace is started to warm up from room temperature, until furnace temperature be 300~800 DEG C, soaking time be 2s~
60min, heating rate are 1~50 DEG C/min.
Optionally, the electric field strength that the high voltage power supply generates is 300~2000V/cm.
Optionally, the carrying current of the high voltage power supply is 10~500mA.
Optionally, the high voltage power supply is DC power supply or AC power.
Optionally, the platinum filament can be replaced with platinum-rhodium wire.
A kind of piezoelectric ceramics, the piezoelectric ceramics prepare the side of PZT piezoelectric ceramics using the low temperature Fast Sintering
Method is prepared.
The method provided by the invention for preparing PZT piezoelectric ceramics, has the following advantages:
By applying external electrical field, Fast Sintering fine and close PZT piezoelectric ceramics can be prepared under cryogenic;Pass through
Electric field strength is controlled, the crystallite dimension of gained PZT piezoelectric ceramics can be controlled;By adjusting carrying current, gained can be controlled
The crystallite dimension of PZT piezoelectric ceramics.This method preparation process is simple, being capable of mass production PZT piezoelectric ceramics.
Description of the drawings
Fig. 1 is the schematic device of the invention;
Fig. 2 is the SEM photograph for applying PZT piezoelectric ceramics prepared by not same electric field in embodiment;
Fig. 3 is the SEM photograph for applying PZT piezoelectric ceramics prepared by otherwise limit electric current in embodiment;
Fig. 4 is that electric field strength is 1500V/cm in embodiment, and carrying current 100mA, furnace temperature is prepared at 300 DEG C
The SEM photograph of PZT piezoelectric ceramics;
Fig. 5 is that electric field strength is 500V/cm in embodiment, and carrying current 500mA, furnace temperature is prepared PZT at 600 DEG C
The SEM photograph of piezoelectric ceramics.
The present invention is illustrated below in conjunction with specification drawings and specific embodiments.
Specific implementation mode
It finds in the course of the research, applies external electrical field, sintering densification process can be greatly promoted, it is low to realize
Warm Fast Sintering prepares ceramic material.By controlling electric field strength and carrying current, gained PZT piezoelectric ceramics can also be controlled
Grain size.Based on this, inventor develops the method that low temperature Fast Sintering prepares densification PZT piezoelectric ceramics.
The method that the present invention prepares PZT piezoelectric ceramics is that ceramic body is placed in sintering furnace, by platinum filament by ceramic blank
Body and high voltage power supply are connected to apply electric field, are then carried out under specific sintering temperature, electric field strength and carrying current
Sintering, to obtain fine and close PZT piezoelectric ceramics.
Specifically, the method that a kind of low temperature Fast Sintering of the present invention prepares PZT piezoelectric ceramics, includes the following steps:
1) PZT ceramic bodies are placed in sintering furnace, and are connected ceramic body and high voltage power supply by platinum filament;
2) sintering furnace is started to warm up from room temperature, until furnace temperature is 300~800 DEG C, soaking time is 2s~60min, is risen
Warm rate is 1~50 DEG C/min;
3) in sintering furnace temperature-rise period, electric field, electric field level 300 are applied to PZT ceramic bodies by high voltage power supply
~2000V/cm;And it is 10~500mA to be arranged through the carrying current in PZT ceramic bodies;
4) sintering furnace and power supply are closed;
Step 1) mesohigh power supply is direct current or AC power.
Platinum filament can be replaced with Pt-Rh wire in step 1).
The present invention promotes the sintering densification process of ceramic material by extra electric field, realize low temperature (<600 DEG C) it is fast
Speed (<PZT piezoelectric ceramics 30min) is prepared, the defect and deficiency of existing preparation method are overcome.The preparation method is simple for process,
It is suitble to mass production.
With reference to specific embodiment and Figure of description, the present invention is further described.
Embodiment one:
First, PZT ceramic powders (commercially available) are compressed to by green body using dry-pressing formed technology, pressure 60MPa, when pressurize
Between be 120s.PZT ceramic bodies are placed in sintering furnace, are connected green body and DC high-voltage power supply by platinum filament, such as Fig. 1
It is shown.Setting electric field strength is 300~600V/cm, then carrying current 100mA begins to warm to sintering furnace from room temperature
800 DEG C, sintering rate is 10 DEG C/min, when 800 DEG C of sintering furnace temperature arrival, after keeping the temperature 30s, closes sintering furnace and high voltage power supply.
After about 2~5h, sample is taken out in sintered body furnace cooling to room temperature.
Fig. 2 be respectively electric field strength be (a) 300V/cm, (b) 400V/cm, (c) 500V/cm, (d) 600V/cm, the limit
Electric current is the SEM photograph of prepared PZT piezoelectric ceramics under 100mA, it can be clearly seen that, gained ceramics are completely fine and close.Meanwhile also
As can be seen that with the increase of electric field strength, average grain size reduces.In 300V/cm, 400V/cm, 500V/cm, 600V/
Under the electric field strength of cm, average grain size is respectively 3.97 μm, 2.83 μm, 1.89 μm, 1.68 μm.
Embodiment two:
First, PZT ceramic powders (commercially available) are compressed to by green body using dry-pressing formed technology, pressure 60MPa, when pressurize
Between be 120s.PZT ceramic bodies are placed in sintering furnace, are connected green body and DC high-voltage power supply by platinum filament, such as Fig. 1
It is shown.Setting electric field strength is 500V/cm, and carrying current is respectively 10mA, 20mA, 30mA, 50mA, then by sintering furnace from room
Temperature begins to warm to 590 DEG C, and sintering rate is 10 DEG C/min, keeps the temperature 30min after sintering furnace temperature reaches 590 DEG C, is then shut off
Sintering furnace and high voltage power supply.After about 2~5h, sample is taken out in sintered body furnace cooling to room temperature.
It is 500V/cm that Fig. 3, which is in electric field strength, and carrying current is respectively (a) 10mA, (b) 20mA, (c) 30mA, (d)
The SEM photograph of prepared PZT piezoelectric ceramics under 50mA, it can be clearly seen that, gained ceramics are completely fine and close.At the same time it can also see
Go out, with the increase of carrying current, average grain size increases.It is average at 10mA, 20mA, 30mA, the carrying current of 50mA
Crystallite dimension is respectively 0.37 μm, 0.91 μm, 1.63 μm, 2.13 μm.
Embodiment three:
First, PZT ceramic powders (commercially available) are compressed to by green body using dry-pressing formed technology, pressure 60MPa, when pressurize
Between be 120s.PZT ceramic bodies are placed in sintering furnace, are connected green body and DC high-voltage power supply by platinum filament, such as Fig. 1
It is shown.Setting electric field strength is 1500V/cm, then sintering furnace is begun to warm to 300 by carrying current 100mA from room temperature
DEG C, sintering rate is 10 DEG C/min, when 300 DEG C of sintering furnace temperature arrival, after keeping the temperature 30min, closes sintering furnace and high voltage power supply.About
After 2~5h, sample is taken out in sintered body furnace cooling to room temperature.
Fig. 4 is the SEM photograph of prepared PZT piezoelectric ceramics, it can be clearly seen that, gained ceramics almost realize complete cause
It is close, average grain size 450nm.
Example IV:
First, PZT ceramic powders (commercially available) are compressed to by green body using dry-pressing formed technology, pressure 60MPa, when pressurize
Between be 120s.PZT ceramic bodies are placed in sintering furnace, are connected green body and DC high-voltage power supply by platinum filament, such as Fig. 1
It is shown.Setting electric field strength is 500V/cm, carrying current 500mA, and sintering furnace is then begun to warm to 600 DEG C from room temperature,
Sintering rate is 10 DEG C/min, when 600 DEG C of sintering furnace temperature arrival, after keeping the temperature 30s, closes sintering furnace and high voltage power supply.About 2~5h
Afterwards, sintered body furnace cooling takes out sample to room temperature.
Fig. 5 is the SEM photograph of prepared PZT piezoelectric ceramics, it can be clearly seen that, gained ceramics are completely fine and close, average crystalline substance
Particle size is 2.35 μm.
Claims (10)
1. a kind of method that low temperature Fast Sintering prepares PZT piezoelectric ceramics, which is characterized in that PZT piezoelectric ceramics green body into
While row sintering, apply electric field to PZT piezoelectric ceramics green bodies.
2. the method that low temperature Fast Sintering according to claim 1 prepares PZT piezoelectric ceramics, which is characterized in that described
Electric field strength is 300~2000V/cm.
3. the method that low temperature Fast Sintering according to claim 1 or 2 prepares PZT piezoelectric ceramics, which is characterized in that described
Sintering include being started to warm up from room temperature, until temperature be 300~800 DEG C, soaking time be 2s~60min, heating rate 1
~50 DEG C/min.
4. the method that low temperature Fast Sintering according to claim 1 prepares PZT piezoelectric ceramics, which is characterized in that press PZT
Electroceramics green body is placed in sintering furnace, is connected PZT piezoelectric ceramics green bodies with high voltage power supply by platinum filament.
5. the method that low temperature Fast Sintering as claimed in claim 4 prepares PZT piezoelectric ceramics, which is characterized in that by sintering furnace
Started to warm up from room temperature, until furnace temperature be 300~800 DEG C, soaking time be 2s~60min, heating rate be 1~50 DEG C/
min。
6. the method that low temperature Fast Sintering as claimed in claim 4 prepares PZT piezoelectric ceramics, which is characterized in that the height
The electric field strength that voltage source generates is 300~2000V/cm.
7. the method that low temperature Fast Sintering as claimed in claim 4 prepares PZT piezoelectric ceramics, which is characterized in that the height
The carrying current of voltage source is 10~500mA.
8. the method that low temperature Fast Sintering as claimed in claim 4 prepares PZT piezoelectric ceramics, which is characterized in that the height
Voltage source is DC power supply or AC power.
9. the method that low temperature Fast Sintering as claimed in claim 4 prepares PZT piezoelectric ceramics, which is characterized in that the platinum
Silk can be replaced with platinum-rhodium wire.
10. a kind of piezoelectric ceramics, which is characterized in that the piezoelectric ceramics is using described in claim 1-9 any claims
The low temperature Fast Sintering method for preparing PZT piezoelectric ceramics be prepared.
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CN109357528A (en) * | 2018-08-14 | 2019-02-19 | 长安大学 | A kind of ceramic material sintering furnace and its control method using electric field-assisted |
CN109534809A (en) * | 2019-01-22 | 2019-03-29 | 陕西科技大学 | A kind of method of the low temperature Fast Sintering barium titanate PTC ceramics of electric field-assisted |
CN110451990A (en) * | 2019-09-06 | 2019-11-15 | 西北工业大学 | A kind of method that Fast Sintering prepares metal oxide texture ceramic material under room temperature |
CN114206802A (en) * | 2019-05-17 | 2022-03-18 | 马里兰大学派克分院 | High temperature sintering system and method |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109357528A (en) * | 2018-08-14 | 2019-02-19 | 长安大学 | A kind of ceramic material sintering furnace and its control method using electric field-assisted |
CN109534809A (en) * | 2019-01-22 | 2019-03-29 | 陕西科技大学 | A kind of method of the low temperature Fast Sintering barium titanate PTC ceramics of electric field-assisted |
CN114206802A (en) * | 2019-05-17 | 2022-03-18 | 马里兰大学派克分院 | High temperature sintering system and method |
CN114206802B (en) * | 2019-05-17 | 2024-03-01 | 马里兰大学派克分院 | High temperature sintering system and method |
CN110451990A (en) * | 2019-09-06 | 2019-11-15 | 西北工业大学 | A kind of method that Fast Sintering prepares metal oxide texture ceramic material under room temperature |
CN110451990B (en) * | 2019-09-06 | 2022-06-28 | 西北工业大学 | Method for preparing metal oxide textured ceramic material by rapid sintering at normal temperature |
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Application publication date: 20180810 |