CN109721352A - A kind of bismuth-sodium titanate base lead-free piezoelectric ceramic and preparation method thereof using the preparation of microwave material research-on-research station - Google Patents
A kind of bismuth-sodium titanate base lead-free piezoelectric ceramic and preparation method thereof using the preparation of microwave material research-on-research station Download PDFInfo
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Abstract
The present invention relates to the preparation fields of leadless piezoelectric ceramics electronic element device materials, and in particular to a method of bismuth-sodium titanate base lead-free piezoelectric ceramic is prepared using microwave material research-on-research station.The present invention can not only effectively solve that the problems such as sintering aid brings fault of construction and reduced performance is added when preparing high the powder complex process of Nano grade, equipment investment and sintering ceramics in Traditional liquid phase chemical technology, and reach scheduled sintering temperature in 10 minutes, and NBT based piezoelectric ceramic materials product can be rapidly fired to while effectively avoiding the segregation of ingredient in sintering process.Finally obtained densification degree is 94.7 ~ 97.1%, piezoelectric modulusd 33The NBT base piezoelectric ceramic that the stability that=183 ~ 265pC/N and Curie temperature are 340 ~ 381 DEG C is high, electric property is excellent.There is huge business potential using application of this efficient, the preparation of energy-efficient microwave material research-on-research station the NBT based leadless piezoelectric ceramics in electronic component.
Description
Technical field
The present invention relates to the preparation fields of leadless piezoelectric ceramics electronic element device materials, and in particular to a kind of to use microwave material
Expect the bismuth-sodium titanate base lead-free piezoelectric ceramic and preparation method thereof of research-on-research station preparation.
Background technique
The electronic product touched in people's daily life be unable to do without piezoelectric ceramic electric component, these electronic components
It is mostly integrated on the core component of electronic product, and has the characteristics that different sizes, big size has tens centimetres and small
Naked eyes are difficult to observe.Piezoelectric ceramics can be applied in current high-end electronic equipment, with its efficient collection of energy mode and
Transform mode is closely related.The most mature piezoceramic material of application is Lead Zirconate Titanate ceramic material at present, however this kind of material
Because containing heavy metal lead ion by global limitation.Therefore, finding enough replaces leaded piezoelectric material to become electronics member device
The inexorable trend of part Materials.It is substituted on leaded piezoelectric material finding, has there is very big challenge but also and develop
The strategic opportunity of lead-free piezoceramic material.
Bismuth-sodium titanate base ceramics (referred to as NBT base ceramics) are one of current research lead-free piezoceramic materials, and
It is considered the leaded piezoceramic material of most potential substitution.Main cause is that NBT base ceramics have the larger tolerance factor
Perovskite structure, piezoelectric property can be improved by components such as the barium titanate of adulterated with Ca and Ti ore structure or potassium-sodium niobates with it is excellent
Change.However NBT base ceramic material bismuth ion and sodium ion are readily volatilized in the case where conventional high-temperature is sintered with long-time, cause ingredient inclined
Analysis, fault of construction increases, densification degree reduces, performance reproducibility is small and electric property decline etc. adversely affect.In order to solve
Conventional sintering technique bring defect problem, starting point concentrate on two aspects: one, low temperature soluble solids is added；Two, solution chemistry
Method prepares the NBT based ceramic powder body of Nano grade.Be added soluble solids, no doubt bring more material components, be unfavorable for component with
Structure regulating；Solution chemical method prepares powder, and step is often comparatively laborious, low yield and equipment investment are higher.It is closed so finding
Suitable sintering process is the key that solve current NBT base ceramics.
Recently, microwave is applied as the heating method of " second flame of the mankind " in more and more heating arts.It is former
Reason is the rotation of tune repeatedly for the free charge rearrangement and dipole for making material internal using the polarization of alternating electromagnetic field,
So that it is generated vibration and friction, and then makes the thermal energy in the energy conversion dielectric material in magnetic field.Therefore, microwave sintering method has
The advantages that sample, heating speed are fast and heating efficiency is high is not contacted, and there are very big potentiality in terms of preparing NBT base ceramics.
Summary of the invention
In order to solve to prepare in Traditional liquid phase chemical process, the powder complex process of Nano grade, equipment investment is high and burns
The problems such as sintering aid brings fault of construction and reduced performance is added when knot ceramics, uses microwave material the present invention provides a kind of
The method that research-on-research station prepares bismuth-sodium titanate base lead-free piezoelectric ceramic.
The purpose of the present invention is what is realized by the following method:
A kind of bismuth-sodium titanate base lead-free piezoelectric ceramic prepared using microwave material research-on-research station, including following materials: dioxy
Change titanium, sodium carbonate, bismuth oxide, niobium pentaoxide and potassium carbonate；
The Components Chemical formula of the NBT base piezoelectric ceramic indicates are as follows: (1x)Na0.5Bi0.5TiO3–xK0.5Na0.5NbO3, whereinx=0.00~0.35；
The particle size of the material powder is Nano grade.
The method that bismuth-sodium titanate base lead-free piezoelectric ceramic is prepared using microwave material research-on-research station, including it is following
Step:
1) the molar ratio precise material powder total according to ion each in chemical formula, uniformly mixes 2 under high energy ball mill
Hour；
2) it by powder made from step 1) after the pressure sampling machine lower sheeting of 1.5Mpa, then moves into high in 850 DEG C of Muffle furnace
Preparation NBT base piezoelectric ceramic powder early period was made with high energy ball mill ball milling 2 ~ 3 hours through broken in temperature calcining 2 hours, sheet body；
3) powder prepared in the step 2) of about 1.7g is weighed, the polyvinyl alcohol adhesive that mass fraction is 0.25wt.% is added,
It is moved into the grinding tool that diameter is 20mm after evenly mixing, is formed in the case where pressure is the pressure sampling machine of 20 ~ 30MPa and disk is made
Shape biscuit of ceramics；
4) biscuit of ceramics prepared by step 3) is embedded in the alumina crucible of high-purity mangesium oxide aluminium powder, is moved into microwave material
In the furnace chamber at research-on-research station, ceramics sample is sintered into according to the sintered heat insulating system of setting；
5) by ceramics made from step 4) by polishing, polishing, by electrode, polarization and etc. after test its relevant electrical property
Energy；
Sample in the step 1) under high energy ball mill needs that grinding aid is added；
Bismuth-sodium titanate base lead-free piezoelectric ceramic powder early period of 1.7g needs the amount of polyvinyl alcohol to be in the step 3)
0.25ml；
In the step 4) before sintering ceramic body, need to place in air for 24 hours to discharge internal stress；
Sintering schedule in the step 4) are as follows: the time from room temperature to sintering temperature is 7 ~ 10 minutes, sintering temperature be 1050 ~
1080 DEG C, the sintered heat insulating time be 1 ~ 2 hour；
It is the silver electrode material of the burning infiltration at 570 DEG C by electrode conditions in the step 5)；Polarization condition is the silicon at 100 DEG C
Polarize under the electric field of 30kV/cm 30min in oil bath；Testing piezoelectric property condition is placed at room temperature 24 hours in ceramics sample
It is later to test at room temperature.
The performance of bismuth-sodium titanate base lead-free piezoelectric ceramic made from the step 5) are as follows: piezoelectric modulusd 33=183~
265pC/N；Curie temperature is 340 ~ 381 DEG C.
The relative density of bismuth-sodium titanate base lead-free piezoelectric ceramic made from the step 5) is 94.7 ~ 97.1%.
Positive beneficial effect: the present invention prepares the excellent bismuth-sodium titanate base of electric property using microwave material research-on-research station
Leadless piezoelectric ceramics tests its dielectric and piezoelectric properties by modern test technology.The present invention can not only effectively solve tradition
Sintering aid is added when preparing powder complex process, equipment investment height and the sintering ceramics of Nano grade in liquid chemical technology to bring
The problems such as fault of construction and reduced performance, and reach scheduled sintering temperature in 10 minutes, and can avoid burning effectively
NBT based piezoelectric ceramic materials product is rapidly fired to during knot while the segregation of ingredient.Finally obtained densification degree is
94.7 ~ 97.1%, piezoelectric modulusd 33The stability that=183 ~ 265pC/N and Curie temperature are 340 ~ 381 DEG C is high, electric property is excellent
Bismuth-sodium titanate base lead-free piezoelectric ceramic.It is unleaded using this efficient, the preparation of energy-efficient microwave material research-on-research station NBT base
Application of the piezoelectric ceramics in electronic component has huge business potential.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of the NBT base ceramics section prepared in the present invention.
Specific embodiment
Combined with specific embodiments below, the present invention is described further:
Embodiment 1
Prepare 0.74Na0.5Bi0.5TiO3–0.26K0.5Na0.5NbO3Ceramics: take respectively Nano grade titanium dioxide 2.9563g,
Sodium carbonate 1.3249g, bismuth oxide 4.3101g, niobium pentaoxide 0.8639g and potassium carbonate 0.4492g material powder；In high energy ball
The pressure sampling machine lower sheeting of 1.5Mpa is put into after uniformly mixing under grinding machine 2 hours；Sheet body is crushed and under high energy ball mill
Mix 3 hours obtained 0.74Na0.5Bi0.5TiO3–0.26K0.5Na0.5NbO3Ceramic powder；Weigh 1.7g's
0.74Na0.5Bi0.5TiO3–0.26K0.5Na0.5NbO3The polyethylene that 0.25ml mass fraction is 0.25wt.% is added in ceramic powder
Alcohol binder, move it into after evenly mixing diameter be 20mm grinding tool in, pressure be 30MPa pressure sampling machine under at
Disc biscuit of ceramics is made in type；After biscuit of ceramics is placed for 24 hours in air, it is embedded in the oxygen of high-purity mangesium oxide aluminium powder
Change in aluminium crucible；Crucible is placed in sintering schedule are as follows: the time of room temperature to sintering temperature is 10 minutes, sintering temperature be 1080 DEG C and
In the furnace chamber at the microwave material research-on-research station that the sintered heat insulating time is 2 hours, biscuit sinters ceramics into；Ceramics sample is through throwing
Light, polishing, by electrode, polarization and etc. rear its relevant electric property of test.
0.74Na0.5Bi0.5TiO3–0.26K0.5Na0.5NbO3The relative density of ceramics is 97.1%, Curie temperature is 370 DEG C
It is 248pC/N with piezoelectric constant, as shown in Figure 1.
Embodiment 2
Prepare Na0.5Bi0.5TiO3Ceramics: the titanium dioxide 3.9950g, sodium carbonate 1.3249g and oxidation of Nano grade are taken respectively
Bismuth 5.8245g material powder；The pressure sampling machine lower sheeting of 1.5Mpa is put into after uniformly mixing under high energy ball mill 2 hours；
Sheet body is crushed to and is mixed under high energy ball mill 2.5 hours obtained Na0.5Bi0.5TiO3Ceramic powder；Weigh 1.7g's
Na0.5Bi0.5TiO3The polyvinyl alcohol adhesive that 0.25ml mass fraction is 0.25wt.% is added, after evenly mixing in ceramic powder
It moves it into the grinding tool that diameter is 20mm, is formed in the case where pressure is the pressure sampling machine of 25MPa and disc ceramics element is made
Base；After biscuit of ceramics is placed for 24 hours in air, it is embedded in the alumina crucible of high-purity mangesium oxide aluminium powder；Crucible is set
In sintering schedule are as follows: the time of room temperature to sintering temperature is 9 minutes, sintering temperature is 1050 DEG C and the sintered heat insulating time is 1.5
In the furnace chamber at the microwave material research-on-research station of hour, biscuit sinters ceramics into；Ceramics sample is polished, polishes, by electrode, pole
Change and etc. rear its relevant electric property of test.
Na0.5Bi0.5TiO3The relative density of ceramics is 95.2%, Curie temperature is 340 DEG C and piezoelectric constant is 183pC/N,
As shown in Figure 1.
Embodiment 3
Prepare 0.65Na0.5Bi0.5TiO3–0.35K0.5Na0.5NbO3Ceramics: take respectively Nano grade titanium dioxide 2.5968g,
Sodium carbonate 1.3249g, bismuth oxide 3.7860g, niobium pentaoxide 1.1629g and potassium carbonate 0.6047g material powder；In high energy ball
The pressure sampling machine lower sheeting of 1.5Mpa is put into after uniformly mixing under grinding machine 2 hours；Sheet body is crushed and under high energy ball mill
Mix 2 hours obtained 0.65Na0.5Bi0.5TiO3–0.35K0.5Na0.5NbO3Ceramic powder；Weigh 1.7g's
0.65Na0.5Bi0.5TiO3–0.35K0.5Na0.5NbO3The polyethylene that 0.25ml mass fraction is 0.25wt.% is added in ceramic powder
Alcohol binder, move it into after evenly mixing diameter be 20mm grinding tool in, pressure be 30MPa pressure sampling machine under at
Disc biscuit of ceramics is made in type；After biscuit of ceramics is placed for 24 hours in air, it is embedded in the oxygen of high-purity mangesium oxide aluminium powder
Change in aluminium crucible；Crucible is placed in sintering schedule are as follows: the time of room temperature to sintering temperature is 8 minutes, sintering temperature be 1060 DEG C and
In the furnace chamber at the microwave material research-on-research station that the sintered heat insulating time is 1.5 hours, biscuit sinters ceramics into；Ceramics sample is through throwing
Light, polishing, by electrode, polarization and etc. rear its relevant electric property of test.
0.65Na0.5Bi0.5TiO3–0.35K0.5Na0.5NbO3The relative density of ceramics is 96.6%, Curie temperature is 381 DEG C
It is 265pC/N with piezoelectric constant, as shown in Figure 1.
Embodiment 4
Prepare 0.82Na0.5Bi0.5TiO3–0.18K0.5Na0.5NbO3Ceramics: take respectively Nano grade titanium dioxide 3.2759g,
Sodium carbonate 1.3249g, bismuth oxide 4.7761g, niobium pentaoxide 0.5981g and potassium carbonate 0.3110g material powder；In high energy ball
The pressure sampling machine lower sheeting of 1.5Mpa is put into after uniformly mixing under grinding machine 2 hours；Sheet body is crushed and under high energy ball mill
Mix 2 hours obtained 0.82Na0.5Bi0.5TiO3–0.18K0.5Na0.5NbO3Ceramic powder；Weigh 1.7g's
0.82Na0.5Bi0.5TiO3–0.18K0.5Na0.5NbO3The polyethylene that 0.25ml mass fraction is 0.25wt.% is added in ceramic powder
Alcohol binder, move it into after evenly mixing diameter be 20mm grinding tool in, pressure be 25MPa pressure sampling machine under at
Disc biscuit of ceramics is made in type；After biscuit of ceramics is placed for 24 hours in air, it is embedded in the oxygen of high-purity mangesium oxide aluminium powder
Change in aluminium crucible；Crucible is placed in sintering schedule are as follows: the time of room temperature to sintering temperature is 7 minutes, sintering temperature be 1080 DEG C and
In the furnace chamber at the microwave material research-on-research station that the sintered heat insulating time is 2 hours, biscuit sinters ceramics into；Ceramics sample is through throwing
Light, polishing, by electrode, polarization and etc. rear its relevant electric property of test.
0.82Na0.5Bi0.5TiO3–0.18K0.5Na0.5NbO3The relative density of ceramics is 96.7%, Curie temperature is 355 DEG C
It is 234pC/N with piezoelectric constant, as shown in Figure 1.
Embodiment 5
Prepare 0.96Na0.5Bi0.5TiO3–0.04K0.5Na0.5NbO3Ceramics: take respectively Nano grade titanium dioxide 3.8352g,
Sodium carbonate 1.3249g, bismuth oxide 5.5915g, niobium pentaoxide 0.1329g and potassium carbonate 0.0691g material powder；In high energy ball
The pressure sampling machine lower sheeting of 1.5Mpa is put into after uniformly mixing under grinding machine 2 hours；Sheet body is crushed and under high energy ball mill
Mix 2.5 hours obtained 0.96Na0.5Bi0.5TiO3–0.04K0.5Na0.5NbO3Ceramic powder；Weigh 1.7g's
0.96Na0.5Bi0.5TiO3–0.04K0.5Na0.5NbO3The polyethylene that 0.25ml mass fraction is 0.25wt.% is added in ceramic powder
Alcohol binder, move it into after evenly mixing diameter be 20mm grinding tool in, pressure be 20MPa pressure sampling machine under at
Disc biscuit of ceramics is made in type；After biscuit of ceramics is placed for 24 hours in air, it is embedded in the oxygen of high-purity mangesium oxide aluminium powder
Change in aluminium crucible；Crucible is placed in sintering schedule are as follows: the time of room temperature to sintering temperature is 7 minutes, sintering temperature be 1060 DEG C and
In the furnace chamber at the microwave material research-on-research station that the sintered heat insulating time is 1 hour, biscuit sinters ceramics into；Ceramics sample is through throwing
Light, polishing, by electrode, polarization and etc. rear its relevant electric property of test.
0.96Na0.5Bi0.5TiO3–0.04K0.5Na0.5NbO3The relative density of ceramics is 94.7%, Curie temperature is 346 DEG C
It is 201pC/N with piezoelectric constant, as shown in Figure 1.
Embodiment 6
Prepare 0.90Na0.5Bi0.5TiO3–0.10K0.5Na0.5NbO3Ceramics: take respectively Nano grade titanium dioxide 3.5955g,
Sodium carbonate 1.3249g, bismuth oxide 5.2421g, niobium pentaoxide 0.3323g and potassium carbonate 0.1728g material powder；In high energy ball
The pressure sampling machine lower sheeting of 1.5Mpa is put into after uniformly mixing under grinding machine 3 hours；Sheet body is crushed and under high energy ball mill
Mix 3 hours obtained 0.90Na0.5Bi0.5TiO3–0.10K0.5Na0.5NbO3Ceramic powder；Weigh 1.7g's
0.90Na0.5Bi0.5TiO3–0.10K0.5Na0.5NbO3The polyethylene that 0.25ml mass fraction is 0.25wt.% is added in ceramic powder
Alcohol binder, move it into after evenly mixing diameter be 20mm grinding tool in, pressure be 30MPa pressure sampling machine under at
Disc biscuit of ceramics is made in type；After biscuit of ceramics is placed for 24 hours in air, it is embedded in the oxygen of high-purity mangesium oxide aluminium powder
Change in aluminium crucible；Crucible is placed in sintering schedule are as follows: the time of room temperature to sintering temperature is 10 minutes, sintering temperature be 1070 DEG C and
In the furnace chamber at the microwave material research-on-research station that the sintered heat insulating time is 1.5 hours, biscuit sinters ceramics into；Ceramics sample is through throwing
Light, polishing, by electrode, polarization and etc. rear its relevant electric property of test.
0.90Na0.5Bi0.5TiO3–0.10K0.5Na0.5NbO3The relative density of ceramics is 95.8%, Curie temperature is 339 DEG C
It is 210pC/N with piezoelectric constant, as shown in Figure 1.
The present invention prepares the excellent bismuth-sodium titanate base lead-free piezoelectric ceramic of electric property using microwave material research-on-research station,
Its dielectric and piezoelectric properties is tested by modern test technology.The present invention can not only effectively solve in Traditional liquid phase chemical technology
Sintering aid is added when preparing powder complex process, equipment investment height and the sintering ceramics of Nano grade and brings fault of construction and property
The problems such as capable of reducing, and reach scheduled sintering temperature in 10 minutes, and can effectively avoid ingredient in sintering process
Segregation while be rapidly fired to NBT based piezoelectric ceramic materials product.Finally obtained densification degree is 94.7 ~ 97.1%, piezoelectricity
Coefficientd 33The NBT base piezoelectricity pottery that the stability that=183 ~ 265pC/N and Curie temperature are 340 ~ 381 DEG C is high, electric property is excellent
Porcelain.Using this efficient, the preparation of energy-efficient microwave material research-on-research station NBT based leadless piezoelectric ceramics in electronic component
Application have huge business potential.
The foregoing is merely the schematical specific embodiment of the present invention, the range being not intended to limit the invention is any
The equivalent changes and modifications that those skilled in the art is made under the premise of not departing from present inventive concept and principle should all belong to
In the scope of protection of the invention.
Claims (8)
1. a kind of bismuth-sodium titanate base lead-free piezoelectric ceramic prepared using microwave material research-on-research station, which is characterized in that including
Following materials: titanium dioxide, sodium carbonate, bismuth oxide, niobium pentaoxide and potassium carbonate, Components Chemical formula indicate are as follows: (1x)
Na0.5Bi0.5TiO3–xK0.5Na0.5NbO3, whereinx=0.00~0.35。
2. it is according to claim 1 it is a kind of using microwave material research-on-research station preparation
Bismuth-sodium titanate base lead-free piezoelectric ceramic, it is characterised in that: the particle size of the material powder is Nano grade.
3. as described in claim 1 using the system of the bismuth-sodium titanate base lead-free piezoelectric ceramic of microwave material research-on-research station preparation
Preparation Method, comprising the following steps:
1) the molar ratio precise material powder total according to ion each in chemical formula, uniformly mixes 2 under high energy ball mill
Hour；
2) it by powder made from step 1) after the pressure sampling machine lower sheeting of 1.5Mpa, then moves into high in 850 DEG C of Muffle furnace
Preparation NBT base piezoelectric ceramic powder early period was made with high energy ball mill ball milling 2 ~ 3 hours through broken in temperature calcining 2 hours, sheet body；
3) powder prepared in the step 2) of 1.7g is weighed, the polyvinyl alcohol adhesive that mass fraction is 0.25wt.% is added,
It is moved into after even mixing in the grinding tool that diameter is 20mm, is formed in the case where pressure is the pressure sampling machine of 20 ~ 30MPa and disc is made
Biscuit of ceramics；
4) biscuit of ceramics prepared by step 3) is embedded in the alumina crucible of high-purity mangesium oxide aluminium powder, is moved into microwave material
In the furnace chamber at research-on-research station, ceramics sample is sintered into according to the sintered heat insulating system of setting；
5) by ceramics made from step 4) by polishing, polishing, by electrode, polarization and etc. after test its relevant electrical property
Energy.
4. the bismuth-sodium titanate base lead-free piezoelectric ceramic according to claim 4 using the preparation of microwave material research-on-research station
Preparation method, it is characterised in that: the sample in the step 1) under high energy ball mill needs that grinding aid is added.
5. the bismuth-sodium titanate base lead-free piezoelectric ceramic according to claim 4 using the preparation of microwave material research-on-research station
Preparation method, it is characterised in that: NBT base piezoelectric ceramic powder early period of 1.7g needs the amount of polyvinyl alcohol in the step 3)
For 0.25ml.
6. the bismuth-sodium titanate base lead-free piezoelectric ceramic according to claim 4 using the preparation of microwave material research-on-research station
Preparation method, it is characterised in that: in the step 4) before sintering ceramic body, need to place in air for 24 hours in release
Portion's stress；Sintering schedule in step 4) are as follows: the time from room temperature to sintering temperature is 7 ~ 10 minutes, sintering temperature be 1050 ~
1080 DEG C, the sintered heat insulating time be 1 ~ 2 hour.
7. the bismuth-sodium titanate base lead-free piezoelectric ceramic according to claim 4 using the preparation of microwave material research-on-research station
Preparation method, it is characterised in that: be the silver electrode material of the burning infiltration at 570 DEG C by electrode conditions in the step 5)；Polarization
Condition is the 30min that polarizes under the electric field of 30kV/cm in 100 DEG C of silicone oil bath；Testing piezoelectric property condition is in ceramics sample
Later test at room temperature in 24 hours is placed at room temperature.
8. the bismuth-sodium titanate base lead-free piezoelectric ceramic according to claim 4 using the preparation of microwave material research-on-research station
Preparation method, it is characterised in that: the performance of NBT based leadless piezoelectric ceramics made from step 5) are as follows: piezoelectric modulusd 33=183~
265pC/N；Curie temperature is 340 ~ 381 DEG C；The relative density of NBT base piezoelectric ceramic made from step 5) is 94.7 ~ 97.1%.
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