CN106986634A - A kind of calcium barium zirconate titanate base piezoceramics and preparation method thereof - Google Patents
A kind of calcium barium zirconate titanate base piezoceramics and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of calcium barium zirconate titanate base piezoceramics and preparation method thereof, belong to piezoelectric ceramic electric component technical field.The ceramics are as the chemical composition Ba shown in formula1‑x Ca x Ti1‑ y Zr y O3.Preparation method is：Stable chelate colloidal sol is made according to molal weight/volume ratio in the raw materials such as butyl titanate, citric acid, barium acetate, calcium nitrate, zirconium nitrate, ethylene glycol and alcohol, and nano-powder is made through coking, calcining in colloidal sol；Ceramics are made in the sintering schedule that nano-powder stops heating furnace cooling to 1150 ~ 1250 DEG C through granulation, dry-pressing formed, dumping, after being first warming up to 1250 ~ 1290 DEG C.Ceramics are polished, by silver, after polarization process, measure ceramic excellent electric property：Piezoelectric modulusd 33=479~634pC/N；Maximum relative dielectric constantε r=12328~13582。
Description
Technical field
The present invention relates to piezoelectric ceramic electric component technical field, and in particular to a kind of calcium barium zirconate titanate base piezoceramics
And preparation method thereof.
Background technology
Barium calcium zirconate titanate based leadless piezoelectric ceramics（Referred to as BCZT bases are ceramic）Material is acknowledged as " electronic ceramics industry future
Pillar ".BCZT base ceramic materials substitution lead-containing materials can not only reduce environmental pollution, and can effectively by sound,
The signals such as heat, light, electricity are converted into the signal collected with manipulation, are sensor, resonator, converter, driver, resonator etc.
It is indispensable in electronic element device materials selection.With continuing to develop for electronic ceramic fields, to the electrical property of piezoelectric
The sensitivity of energy proposes higher requirement, you can atomic weak signal is received, converts, handles and stored.Furthermore it is required that
Piezoelectric keeps the stabilization of mechanics and electric property in wide temperature is interval, so that electronic component can be special
Environment under very wide temperature range with normally using.In the selection of piezoceramic material, the lead-containing materials of excellent performance are substituted
Application in electronic component has very big challenge, general mainly due to the lead-free including BCZT bases ceramics
It is poor, expensive all over the not good enough of electric property, electrical performance stability.
BCZT base ceramic materials can be applied to the key in electronic ceramics industry：Increase electric property and its stability,
Improve mechanics processability, reduce the cost of material.Powder made from solid phase method is utilized on BCZT base ceramic traditions, using ~ 1450
The pressureless sintering of DEG C high temperature is prepared.The powder composition fluctuation that is prepared in technique is big, diameter of particle distribution is wide；The pottery of preparation
Porcelain fault of construction is more, poor mechanical property, electric property are unstable.
Generally, people add sintering aid to reduce the temperature of the ceramic pressureless sintering of BCZT bases to reduce lacking in structure
Fall into, but this method can form impurities phase in ceramic structure and cause dielectric properties to deteriorate, piezoelectric property is weakened etc..In addition, with
BCZT bases ceramic nano-powder body prepared by liquid chemical method is raw material, can effectively reduce ceramic sintering temperature and improve its electricity
Performance.But liquid chemical method is concentrated mainly on sol-gel process, hydrothermal synthesis method, emulsion polymerization etc., these methods are mostly
Technics comparing complexity, operating difficulties, equipment investment are costly, it is difficult to produce in enormous quantities.On the basis of the powder of preparation, selection
Discharge plasma sintering, hot pressed sintering, microwave sintering etc. prepare BCZT bases ceramics.Although improving ceramics to a certain extent
Electric property, but these precision equipments mostly put into higher, operating process complex process, the fluctuation of ceramic material electric property
Property it is big, and be difficult the extensive use in industrialized production.
Therefore, the ceramic preparation technology of existing BCZT bases is further improved, its cost is reduced and improves its electric property, is
One urgent problem to be solved.
The content of the invention
In order to overcome liquid chemical method in the prior art prepare BCZT base ceramic nano-powder bodies technique it is not enough and improve it
Electric property, the invention provides a kind of new BCZT base piezoelectric ceramics and preparation method thereof.
The object of the present invention is achieved like this：
A kind of calcium barium zirconate titanate base piezoceramics, including following raw materials according：Butyl titanate, barium acetate, calcium nitrate, zirconium nitrate, lemon
Lemon acid, ethylene glycol and alcohol；
The composition composition of described calcium barium zirconate titanate base piezoceramics can be expressed as with chemical formula：Ba1-x Ca x Ti1-y Zr y O3, whereinx=0.00~0.20；y=0.00~0.15；
Described butyl titanate：Ethylene glycol：The volume ratio of alcohol is 2:5:8；
Described citric acid and alcohol mol ratio are 1:2；
The preparation method of described calcium barium zirconate titanate base piezoceramics, comprises the following steps：
1）Butyl titanate is dissolved in ethylene glycol and alcohol, then the mixed solution of citric acid and alcohol is added dropwise to
In above-mentioned solution, and 0.5 ~ 1 hour obtained settled solution 1 is stirred at room temperature；
2）In deionized water, then it will dropwise be added according to the barium acetate dissolving of metal ion molar ratio weighing in chemical formula
To step 1）Temperature is made in 50 ~ 65 DEG C of settled solution 1, to stir 0.5 ~ 1 hour obtained uniform solution 2；
3）It will be dissolved in deionized water respectively according to the zirconium nitrate of metal ion molar ratio weighing, calcium nitrate in chemical formula, and
The order that calcium nitrate is added dropwise after zirconium nitrate according to being first added dropwise is added drop-wise to step 2）In the uniform solution 2 of preparation, in 60 ~ 85 DEG C of temperature
The lower stirring of degree obtains the chelate colloidal sol of stable homogeneous for 0.5 ~ 1 hour；
4）Step 3）The coking in 350 ~ 400 DEG C of Muffle furnace of the gel of preparation obtains black foamed in 1 ~ 2 hour, by foamed
Calcining obtains BCZT base ceramic nano-powder bodies for 1 ~ 2 hour in 700 ~ 900 DEG C of high temperature furnace after grinding；
5）Step 4）The nano-powder of preparation through granulation, dry-pressing formed obtain ceramic green, high temperature of the green compact at 1150 ~ 1250 DEG C
Sintering obtains BCZT bases ceramics for 2 ~ 3 hours in stove；
Described step 5）The adhesive that middle granulation is added is that mass fraction is 5% 0.3 ~ 0.5ml of polyvinyl alcohol, to be easy to powder
Shaping cohere；The thickness of dry-pressing formed BCZT bases ceramics is 2 ~ 3mm, and a diameter of 16mm, pressure is 150Mpa；Life after shaping
Base need to stand 12 ~ 24 hours in atmosphere, to exclude stress remaining in structure；Green compact dumping 1 ~ 2 at 550 ~ 650 DEG C is small
When, prevent adhesive to be mothballed in ceramic structure；Green compact after dumping are embedded in the nano alumina powder of high-purity, with equal
It is even heated；Sintering schedule in the present invention：The high temperature furnace of sintered body is warming up to 1250 ~ 1290 DEG C first, then stops heating
Furnace cooling is finally completed sintering process to 1150 ~ 1250 DEG C；
Described step 5）The ceramics sample of preparation is polished, by after the handling process such as silver electrode, polarization, is surveyed by measuring technology
Obtain the dielectric and piezoelectric properties of BCZT bases ceramics.
Described step 5）The performance of obtained calcium barium zirconate titanate base piezoceramics is：Piezoelectric modulusd 33=479~634pC/
N；Maximum relative dielectric constantε r=12328~13582。
Described test condition is：Silver electrode burning infiltration temperature is 570 ~ 580 DEG C, and the burning infiltration time is 10 ~ 15 minutes；Polarized
The DC voltage used in journey is 3 ~ 5kV/cm, and poling temperature is room temperature ~ 45 DEG C, and the polarization time is 30 ~ 45 minutes.
Positive beneficial effect：The present invention prepares BCZT base ceramic nano-powder bodies by being modified to Via Polymeric Precursor Method；Adopt
The BCZT bases ceramics of densification degree height, Stability Analysis of Structures, excellent performance are prepared with pressureless sintering；By by processing such as silver, polarization
The electric property of ceramics is tested afterwards.The present invention can solve the problem that liquid chemical method prepare BCZT base ceramic nano-powder bodies technique answer
The problems such as miscellaneous, operating difficulties and higher cost, and BCZT base ceramic nano-powder body high-volume continuous productions can be realized.Prefabricated
On the basis of standby nano-powder, the non-pressure sintering technology of use can effectively reduce ceramic sintering temperature, and can obtain being densified journey
The BCZT bases ceramics that degree is high and electric property is excellent.Meanwhile, the BCZT bases ceramics with excellent electric property（Piezoelectric modulusd 33=
479~634pC/N；Maximum relative dielectric constantε r=12328~13582）Have in piezoelectric ceramic electric component technical field non-
Chang Keguan application value and commercial promise.
Brief description of the drawings
Fig. 1 is flow chart prepared by BCZT bases ceramic nano-powder body of the present invention；
Fig. 2 is the BCZT base ceramic nano-powder body transmission electron microscope pictures that prepare in the present invention；
Fig. 3 is the cross-section morphology figure of the BCZT bases ceramics prepared in the present invention.
Embodiment
With reference to specific embodiment, the present invention is described further：
A kind of calcium barium zirconate titanate base piezoceramics, including following raw materials according：Butyl titanate, barium acetate, calcium nitrate, zirconium nitrate, lemon
Lemon acid, ethylene glycol and alcohol；
The composition composition of described calcium barium zirconate titanate base piezoceramics can be expressed as with chemical formula：Ba1-x Ca x Ti1-y Zr y O3, whereinx=0.00~0.20；y=0.00~0.15；
Described butyl titanate：Ethylene glycol：The volume ratio of alcohol is 2:5:8；
Described citric acid and alcohol mol ratio are 1:2；
As shown in figure 1, the preparation method of described calcium barium zirconate titanate base piezoceramics, comprises the following steps：
1）Butyl titanate is dissolved in ethylene glycol and alcohol, then the mixed solution of citric acid and alcohol is added dropwise to
In above-mentioned solution, and 0.5 ~ 1 hour obtained settled solution 1 is stirred at room temperature；
2）In deionized water, then it will dropwise be added according to the barium acetate dissolving of metal ion molar ratio weighing in chemical formula
To step 1）Temperature is made in 50 ~ 65 DEG C of settled solution 1, to stir 0.5 ~ 1 hour obtained uniform solution 2；
3）It will be dissolved in deionized water respectively according to the zirconium nitrate of metal ion molar ratio weighing, calcium nitrate in chemical formula, and
The order that calcium nitrate is added dropwise after zirconium nitrate according to being first added dropwise is added drop-wise to step 2）In the uniform solution 2 of preparation, in 60 ~ 85 DEG C of temperature
The lower stirring of degree obtains the chelate colloidal sol of stable homogeneous for 0.5 ~ 1 hour；
4）Step 3）The coking in 350 ~ 400 DEG C of Muffle furnace of the gel of preparation obtains black foamed in 1 ~ 2 hour, by foamed
Calcining obtains BCZT base ceramic nano-powder bodies for 1 ~ 2 hour in 700 ~ 900 DEG C of high temperature furnace after grinding；
5）Step 4）The nano-powder of preparation through granulation, dry-pressing formed obtain ceramic green, high temperature of the green compact at 1150 ~ 1250 DEG C
Sintering obtains BCZT bases ceramics for 2 ~ 3 hours in stove；
Described step 5）The adhesive that middle granulation is added is that mass fraction is 5% 0.3 ~ 0.5ml of polyvinyl alcohol, to be easy to powder
Shaping cohere；The thickness of dry-pressing formed BCZT bases ceramics is 2 ~ 3mm, and a diameter of 16mm, pressure is 150Mpa；Life after shaping
Base need to stand 12 ~ 24 hours in atmosphere, to exclude stress remaining in structure；Green compact dumping 1 ~ 2 at 550 ~ 650 DEG C is small
When, prevent adhesive to be mothballed in ceramic structure；Green compact after dumping are embedded in the nano alumina powder of high-purity, with equal
It is even heated；Sintering schedule in the present invention：The high temperature furnace of sintered body is warming up to 1250 ~ 1290 DEG C first, then stops heating
Furnace cooling is finally completed sintering process to 1150 ~ 1250 DEG C；
Described step 5）The ceramics sample of preparation is polished, by after the handling process such as silver electrode, polarization, is surveyed by measuring technology
Obtain the dielectric and piezoelectric properties of BCZT bases ceramics.
Described step 5）The performance of obtained calcium barium zirconate titanate base piezoceramics is：Piezoelectric modulusd 33=479~634pC/
N；Maximum relative dielectric constantε r=12328~13582。
Described test condition is：Silver electrode burning infiltration temperature is 570 ~ 580 DEG C, and the burning infiltration time is 10 ~ 15 minutes；Polarized
The DC voltage used in journey is 3 ~ 5kV/cm, and poling temperature is room temperature ~ 45 DEG C, and the polarization time is 30 ~ 45 minutes.
Embodiment 1
Prepare Ba0.85Ca0.15Ti0.90Zr0.10O3Ceramics：3.0632g butyl titanates are taken to be dissolved in 7.5ml alcohol and 12ml second
In two mixed alkoxide solutions, it is sufficiently stirred at room temperature 1 hour；By the mixed solution of 6.3042g citric acids and 2.7642g alcohol by
Above-mentioned solution is added dropwise to, is stirred at room temperature 45 minutes and obtains settled solution 1；2.1711g barium acetates are dissolved in deionization
In water, it is added dropwise in the settled solution 1 that temperature is 55 DEG C, stirring obtains uniform solution 2 in 1 hour；By 0.4293g zirconium nitrates
Dissolved in deionized water respectively with 0.3542g calcium nitrate, and the order that calcium nitrate is added dropwise again according to first dropwise addition zirconium nitrate is added
Into solution 2, in the case where temperature is 80 DEG C, stirring obtains the chelate colloidal sol of stable homogeneous for 40 minutes；Muffle of the colloidal sol at 380 DEG C
Coking obtains black foamed in 1.5 hours in stove, calcines and obtains in 800 DEG C of high temperature furnace after foamed is ground for 1.5 hours
Nano-powder；Nano-powder prepares ceramic body after dry-pressing formed, and base substrate is warming up to 1280 DEG C, then stopped first after dumping
Only heat and be as cold as 1200 DEG C with stove, sintering obtains Ba in 2.5 hours0.85Ca0.15Ti0.90Zr0.10O3Ceramics.
Ba0.85Ca0.15Ti0.90Zr0.10O3The post processing of ceramics and electrical performance testing：Ceramics sample is silver-colored by polishing
Electrode, polarization etc. aftertreatment technology, the electric property obtained by test：Piezoelectric modulusd 33=634pC/N；Maximum relative dielectric
Constantε r=13177。
Embodiment 2
Prepare Ba0.85Ca0.15Ti0.95Zr0.05O3Ceramics：3.2334g butyl titanates are taken to be dissolved in 8ml alcohol and 13ml second two
In mixed alkoxide solution, it is sufficiently stirred at room temperature 1 hour；By the mixed solution of 6.6544g citric acids and 2.9178g alcohol dropwise
Above-mentioned solution is added to, is stirred at room temperature 45 minutes and obtains settled solution 1；2.1711g barium acetates are dissolved in deionized water
In, it is added dropwise in the settled solution 1 that temperature is 55 DEG C, stirring obtains uniform solution 2 in 1 hour；By 0.2147g zirconium nitrates with
0.3542g calcium nitrate is dissolved in deionized water respectively, and the order that calcium nitrate is added dropwise again according to first dropwise addition zirconium nitrate is added to
In solution 2, in the case where temperature is 80 DEG C, stirring obtains the chelate colloidal sol of stable homogeneous for 40 minutes；Muffle furnace of the colloidal sol at 380 DEG C
Middle coking obtains black foamed in 1.5 hours, and calcining obtains nanometer in 2 hours in 800 DEG C of high temperature furnace after foamed is ground
Powder；Nano-powder prepares ceramic body after dry-pressing formed, and base substrate is warming up to 1280 DEG C first after dumping, then stops adding
Heat is as cold as 1200 DEG C with stove, and sintering obtains Ba in 2.5 hours0.85Ca0.15Ti0.95Zr0.05O3Ceramics.
Ba0.85Ca0.15Ti0.95Zr0.05O3The post processing of ceramics and electrical performance testing：Ceramics sample is silver-colored by polishing
Electrode, polarization etc. aftertreatment technology, the electric property obtained by test：Piezoelectric modulusd 33=553pC/N；Maximum relative dielectric
Constantε r=12328。
Embodiment 3
Prepare Ba0.95Ca0.05Ti0.95Zr0.05O3Ceramics：3.2334g butyl titanates are taken to be dissolved in 8ml alcohol and 13ml second two
In mixed alkoxide solution, it is sufficiently stirred at room temperature 1 hour；By the mixed solution of 6.6544g citric acids and 2.9178g alcohol dropwise
Above-mentioned solution is added to, is stirred at room temperature 45 minutes and obtains settled solution 1；2.4265g barium acetates are dissolved in deionized water
In, it is added dropwise in the settled solution 1 that temperature is 55 DEG C, stirring obtains uniform solution 2 in 1 hour；By 0.2147g zirconium nitrates with
0.1181g calcium nitrate is dissolved in deionized water respectively, and the order that calcium nitrate is added dropwise again according to first dropwise addition zirconium nitrate is added to
In solution 2, in the case where temperature is 80 DEG C, stirring obtains the chelate colloidal sol of stable homogeneous for 40 minutes；Muffle furnace of the colloidal sol at 380 DEG C
Middle coking obtains black foamed in 1.5 hours, and calcining obtains nanometer in 2 hours in 800 DEG C of high temperature furnace after foamed is ground
Powder；Nano-powder prepares ceramic body after dry-pressing formed, and base substrate is warming up to 1280 DEG C first after dumping, then stops adding
Heat is as cold as 1200 DEG C with stove, and sintering obtains Ba in 2.5 hours0.95Ca0.05Ti0.95Zr0.05O3Ceramics.
Ba0.95Ca0.05Ti0.95Zr0.05O3The post processing of ceramics and electrical performance testing：Ceramics sample is silver-colored by polishing
Electrode, polarization etc. aftertreatment technology, the electric property obtained by test：Piezoelectric modulusd 33=522pC/N；Maximum relative dielectric
Constantε r=12983。
Embodiment 4
Prepare Ba0.90Ca0.10Ti0.90Zr0.10O3Ceramics：3.0632g butyl titanates are taken to be dissolved in 7.5ml alcohol and 12ml second
In two mixed alkoxide solutions, it is sufficiently stirred at room temperature 1 hour；By the mixed solution of 6.3042g citric acids and 2.7642g alcohol by
Above-mentioned solution is added dropwise to, is stirred at room temperature 45 minutes and obtains settled solution 1；2.2988g barium acetates are dissolved in deionization
In water, it is added dropwise in the settled solution 1 that temperature is 55 DEG C, stirring obtains uniform solution 2 in 1 hour；By 0.4293g zirconium nitrates
Dissolved in deionized water respectively with 0.1181g calcium nitrate, and the order that calcium nitrate is added dropwise again according to first dropwise addition zirconium nitrate is added
Into solution 2, in the case where temperature is 80 DEG C, stirring obtains the chelate colloidal sol of stable homogeneous for 40 minutes；Muffle of the colloidal sol at 380 DEG C
Coking obtains black foamed in 1.5 hours in stove, calcines and is received in 800 DEG C of high temperature furnace after foamed is ground for 2 hours
Ground rice body；Nano-powder prepares ceramic body after dry-pressing formed, and base substrate is warming up to 1280 DEG C, then stopped first after dumping
Heating is as cold as 1200 DEG C with stove, and sintering obtains Ba in 2.5 hours0.90Ca0.10Ti0.90Zr0.10O3Ceramics.
Ba0.90Ca0.10Ti0.90Zr0.10O3The post processing of ceramics and electrical performance testing：Ceramics sample is silver-colored by polishing
Electrode, polarization etc. aftertreatment technology, the electric property obtained by test：Piezoelectric modulusd 33=479pC/N；Maximum relative dielectric
Constantε r=13582。
The present invention prepares BCZT base ceramic nano-powder bodies by being modified to Via Polymeric Precursor Method；Prepared using pressureless sintering
Densification degree height, Stability Analysis of Structures, the BCZT bases ceramics of excellent performance；By the electricity that ceramics are tested after the processing such as silver, polarization
Learn performance.Can solve the problem that liquid chemical method prepare BCZT base ceramic nano-powder bodies complex process, operating difficulties and cost it is higher
The problems such as, and BCZT base ceramic nano-powder body high-volume continuous productions can be realized.On the basis of pre-prepared nano-powder, adopt
Non-pressure sintering technology, can effectively reduce ceramic sintering temperature, and it is excellent to obtain densification degree height, electric property
BCZT bases ceramics.Meanwhile, the BCZT bases ceramics with excellent electric property（Piezoelectric modulusd 33=479~634pC/N；It is maximum relative
Dielectric constantε r=12328~13582）There is considerable application value and business in piezoelectric ceramic electric component technical field
Industry prospect.
Above example is merely to illustrate the preferred embodiment of the present invention, but the present invention is not limited to above-mentioned embodiment party
Formula, in the knowledge that the field those of ordinary skill possesses, that is made within the spirit and principles in the present invention is any
Modification, equivalent substitute and improvement etc., it all should cover within the scope of claimed technical scheme of the invention.
Claims (9)
1. a kind of calcium barium zirconate titanate base piezoceramics, it is characterised in that including following raw materials according：Butyl titanate, barium acetate, nitric acid
Calcium, zirconium nitrate, citric acid, ethylene glycol and alcohol.
2. a kind of calcium barium zirconate titanate base piezoceramics according to claim 1, it is characterised in that：Described barium calcium zirconate titanate
The composition composition of base piezoelectric ceramic can be expressed as with chemical formula：Ba1-x Ca x Ti1-y Zr y O3, whereinx=0.00~0.20；y=0.00~
0.15。
3. a kind of calcium barium zirconate titanate base piezoceramics according to claim 1, it is characterised in that：The described fourth of metatitanic acid four
Ester：Ethylene glycol：The volume ratio of alcohol is 2:5:8.
4. a kind of calcium barium zirconate titanate base piezoceramics according to claim 1, it is characterised in that：Described citric acid and wine
Smart mol ratio is 1:2.
5. the preparation method of calcium barium zirconate titanate base piezoceramics as claimed in claim 1, it is characterised in that including following step
Suddenly：
1）Butyl titanate is dissolved in ethylene glycol and alcohol, then the mixed solution of citric acid and alcohol is added dropwise to
In above-mentioned solution, and 0.5 ~ 1 hour obtained settled solution 1 is stirred at room temperature；
2）In deionized water, then it will dropwise be added according to the barium acetate dissolving of metal ion molar ratio weighing in chemical formula
To step 1）Temperature is made in 50 ~ 65 DEG C of settled solution 1, to stir 0.5 ~ 1 hour obtained uniform solution 2；
3）It will be dissolved in deionized water respectively according to the zirconium nitrate of metal ion molar ratio weighing, calcium nitrate in chemical formula, and
The order that calcium nitrate is added dropwise after zirconium nitrate according to being first added dropwise is added drop-wise to step 2）In the uniform solution 2 of preparation, in 60 ~ 85 DEG C of temperature
The lower stirring of degree obtains the chelate colloidal sol of stable homogeneous for 0.5 ~ 1 hour；
4）Step 3）The coking in 350 ~ 400 DEG C of Muffle furnace of the gel of preparation obtains black foamed in 1 ~ 2 hour, by foamed
Calcining obtains BCZT base ceramic nano-powder bodies for 1 ~ 2 hour in 700 ~ 900 DEG C of high temperature furnace after grinding；
5）Step 4）The nano-powder of preparation through granulation, dry-pressing formed obtain ceramic green, high temperature of the green compact at 1150 ~ 1250 DEG C
Sintering obtains BCZT bases ceramics for 2 ~ 3 hours in stove.
6. a kind of preparation method of calcium barium zirconate titanate base piezoceramics according to claim 5, it is characterised in that：Described
Step 5）The adhesive that middle granulation is added is that mass fraction is 5% 0.3 ~ 0.5ml of polyvinyl alcohol, is cohered with the shaping for being easy to powder；
The thickness of dry-pressing formed BCZT bases ceramics is 2 ~ 3mm, and a diameter of 16mm, pressure is 150Mpa；Green compact after shaping need to be in air
It is middle to stand 12 ~ 24 hours, to exclude stress remaining in structure；Green compact dumping 1 ~ 2 hour at 550 ~ 650 DEG C, prevents bonding
Agent is mothballed in ceramic structure；Green compact after dumping are embedded in the nano alumina powder of high-purity, with thermally equivalent；This hair
Sintering schedule in bright：The high temperature furnace of sintered body is warming up to 1250 ~ 1290 DEG C first, then stops heating furnace cooling and arrives
1150 ~ 1250 DEG C, it is finally completed sintering process.
7. a kind of preparation method of calcium barium zirconate titanate base piezoceramics according to claim 5, it is characterised in that：Described
Step 5）The ceramics sample of preparation is polished, by after the handling process such as silver electrode, polarization, measures BCZT bases by measuring technology and makes pottery
The dielectric and piezoelectric properties of porcelain.
8. a kind of preparation method of calcium barium zirconate titanate base piezoceramics according to claim 5, it is characterised in that：Described
Step 5）The performance of obtained calcium barium zirconate titanate base piezoceramics is：Piezoelectric modulusd 33=479~634pC/N；Maximum relative dielectric
Constantε r=12328~13582。
9. a kind of preparation method of calcium barium zirconate titanate base piezoceramics according to claim 5, it is characterised in that：Described
Test condition is：Silver electrode burning infiltration temperature is 570 ~ 580 DEG C, and the burning infiltration time is 10 ~ 15 minutes；The direct current used in polarization process
Voltage is 3 ~ 5kV/cm, and poling temperature is room temperature ~ 45 DEG C, and the polarization time is 30 ~ 45 minutes.
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| CN108546124A (en) * | 2018-05-03 | 2018-09-18 | 佛山九陌科技信息咨询有限公司 | A kind of preparation method of BCZT based leadless piezoelectric ceramics |
| CN108558369A (en) * | 2018-05-18 | 2018-09-21 | 郦璋 | A kind of preparation method of composite ceramics capacitance material |
| CN109336572A (en) * | 2018-10-24 | 2019-02-15 | 湖南科技大学 | A kind of cold-rolled sintered method preparing oxide ceramics |
| CN109667067A (en) * | 2018-12-18 | 2019-04-23 | 中国科学院过程工程研究所 | A kind of barium calcium zirconate titanate base flexible piezoelectric composite fiber thin film and preparation method thereof and the flexible piezoelectric nano generator containing the film |
| CN110600266A (en) * | 2019-10-14 | 2019-12-20 | 河南师范大学 | Preparation method of BCZT energy storage ceramic material with adjustable Curie temperature |
| US10770645B2 (en) * | 2018-06-20 | 2020-09-08 | Canon Kabushiki Kaisha | Oriented piezoelectric film, method for producing the oriented piezoelectric film, and liquid dispensing head |
| CN111807837A (en) * | 2020-06-19 | 2020-10-23 | 西安交通大学 | Ferroelectric ceramic material, piezoelectric sensor and preparation method |
| CN114262225A (en) * | 2021-12-29 | 2022-04-01 | 湖南省嘉利信陶瓷科技有限公司 | High-purity nano electronic ceramic and preparation method thereof |
| CN114736015A (en) * | 2022-04-26 | 2022-07-12 | 信阳师范学院 | Intercalation barium calcium zirconate titanate based leadless piezoelectric ceramic prepared by adopting vacuum hot-pressing sintering furnace and preparation method thereof |
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| CN108546124B (en) * | 2018-05-03 | 2021-07-30 | 景德镇市鑫惠康电子有限责任公司 | Preparation method of BCZT-based lead-free piezoelectric ceramic |
| CN108558369A (en) * | 2018-05-18 | 2018-09-21 | 郦璋 | A kind of preparation method of composite ceramics capacitance material |
| US10770645B2 (en) * | 2018-06-20 | 2020-09-08 | Canon Kabushiki Kaisha | Oriented piezoelectric film, method for producing the oriented piezoelectric film, and liquid dispensing head |
| CN109336572A (en) * | 2018-10-24 | 2019-02-15 | 湖南科技大学 | A kind of cold-rolled sintered method preparing oxide ceramics |
| CN109667067A (en) * | 2018-12-18 | 2019-04-23 | 中国科学院过程工程研究所 | A kind of barium calcium zirconate titanate base flexible piezoelectric composite fiber thin film and preparation method thereof and the flexible piezoelectric nano generator containing the film |
| CN110600266A (en) * | 2019-10-14 | 2019-12-20 | 河南师范大学 | Preparation method of BCZT energy storage ceramic material with adjustable Curie temperature |
| CN111807837A (en) * | 2020-06-19 | 2020-10-23 | 西安交通大学 | Ferroelectric ceramic material, piezoelectric sensor and preparation method |
| CN114262225A (en) * | 2021-12-29 | 2022-04-01 | 湖南省嘉利信陶瓷科技有限公司 | High-purity nano electronic ceramic and preparation method thereof |
| CN114262225B (en) * | 2021-12-29 | 2022-10-21 | 湖南省嘉利信陶瓷科技有限公司 | High-purity nano electronic ceramic and preparation method thereof |
| CN114736015A (en) * | 2022-04-26 | 2022-07-12 | 信阳师范学院 | Intercalation barium calcium zirconate titanate based leadless piezoelectric ceramic prepared by adopting vacuum hot-pressing sintering furnace and preparation method thereof |
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