CN103073289B - Piezoceramic material, sintering body, piezoceramic device and preparation method of piezoceramic material - Google Patents
Piezoceramic material, sintering body, piezoceramic device and preparation method of piezoceramic material Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000005245 sintering Methods 0.000 title claims abstract description 6
- 239000000463 material Substances 0.000 title abstract description 52
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 14
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 8
- 239000000919 ceramic Substances 0.000 claims description 50
- 239000000203 mixture Substances 0.000 claims description 19
- 238000000465 moulding Methods 0.000 claims description 15
- 239000002075 main ingredient Substances 0.000 claims description 11
- 230000010287 polarization Effects 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 9
- 229910052758 niobium Inorganic materials 0.000 claims description 9
- 229910052788 barium Inorganic materials 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 8
- 229910052712 strontium Inorganic materials 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229910052787 antimony Inorganic materials 0.000 claims description 6
- 238000003475 lamination Methods 0.000 claims description 6
- 238000010298 pulverizing process Methods 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 229910052745 lead Inorganic materials 0.000 claims description 5
- 239000004902 Softening Agent Substances 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 4
- 230000005684 electric field Effects 0.000 claims description 4
- 239000004615 ingredient Substances 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 3
- 238000007766 curtain coating Methods 0.000 claims description 2
- 229920002545 silicone oil Polymers 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 239000010936 titanium Substances 0.000 abstract description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 9
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract description 9
- 239000002131 composite material Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000010955 niobium Substances 0.000 description 14
- 238000000034 method Methods 0.000 description 13
- 230000005611 electricity Effects 0.000 description 5
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 4
- 238000005266 casting Methods 0.000 description 4
- 230000008878 coupling Effects 0.000 description 4
- 238000010168 coupling process Methods 0.000 description 4
- 238000005859 coupling reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000003679 aging effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910002059 quaternary alloy Inorganic materials 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
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- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention provides a piezoceramic material which at least comprises lead, zirconium and titanium composite oxide. The piezoceramic material comprises a main component of which a chemical general formula is shown as follows: PbaBa1-a(NbbSbbSr1-2b)xZryTi1-x-yO3, wherein a is greater than or equal to 0.8 and less than or equal to 0.95; b is greater than or equal to 0.1 and less than or equal to 0.2; x is greater than or equal to 0.03 and less than or equal to 0.1; and y is greater than or equal to 0.45 and less than or equal to 0.55. The piezoceramic material has a high piezoelectric coefficient; on the premise that deformation quantity remains constant, input voltage is reduced, or on the premise that the input voltage of a piezoelectric component remains constant, the energy conversion efficiency is improved, and greater deformation is obtained. In addition, the invention also provides a preparation method of the piezoceramic material, a piezoceramic sintering body and a device adopting the piezoceramic material. The preparation method is simple in technology; a formula is adjustable; and the preparation method facilitates industrial mass production.
Description
Technical field
The present invention relates to a kind of piezoceramic material, sintered compact, piezoelectric ceramic devices of high tension electricity coefficient and adopt the preparation method of described piezoceramic material.
Background technology
It is found that after PZT lead titanate piezoelectric ceramics from 1954, many countries such as the U.S., Japan, Holland have carried out detailed research to piezoelectric ceramics system, and along with the PZT piezoceramic material that has deeply derived a series of superior performances of development, the range of application of piezoceramic material is also expanded greatly.Wherein, taking Pb-based lanthanumdoped zirconate titanates as basis, also all arise at the historic moment with the improved three component system of multiple element, four-component-system piezoelectric ceramics, in nineteen sixty-five PANASONIC electric corporation Pb (Mg
1/3nb
2/3) O
3join and in PZT, made the first ternary system ceramics as the 3rd component, find after deliberation to add some oxide compounds in this ternary system piezoelectric ceramics after, not only can improve electromechanical coupling factor KP and high mechanical quality factor Qm, can also make frequency constant and aging property improve.Ternary system ceramics has more superior performance than binary system ceramics, can regulate significantly alternative composition and piezoelectricity, easily obtains the reception shaped material of high electromechanical coupling number.
Due to the expansion of piezoelectric ceramics range of application, the device of different purposes is more and more higher to piezoceramic material performance requriements, and the quality of piezoceramic material even becomes the development bottleneck in some field.The change of for example ultrasonic cleaning transverter and medical supersonic wave transducer, piezoelectric ceramic transformer and piezoelectric ceramic loudspeaker all exists and directly contacts with piezoceramic material with development.Therefore, make piezoelectric vibrator product have better quality and more superior performance, research and development piezoceramic material and device are the keys that ensures that quality product improves.
Large quantity research shows various relaxation ferroelectrics soluble solids and PZT ceramic combination and the piezoelectric ceramics of this system is carried out to ion exchange and doping vario-property, can obtain high dielectric, high tension performance, and on the basis of three component system, developed more complicated quaternary system, five yuan of series ceramic materials, make the Research Prospects of piezoelectric ceramics more wide.
Piezo component is diversification and complicated requirement day by day, can not meet its requirement to high tension electricity coefficient.
Therefore, the object of this invention is to provide and a kind ofly can meet the piezoceramic material that electromechanical coupling factor is little, resonant resistance is little and piezo-electric modulus is high, and sintered compact and the various piezoelectric ceramic devices of firing formation by these piezoceramic materials are provided.
Summary of the invention
The technical problem that the present invention mainly solves is the low problem that can not meet piezoelectric ceramic devices demand of existing piezoceramic material piezo-electric modulus.
In order to solve the problems of the technologies described above, the embodiment of the invention discloses a kind of piezoceramic material, the composite oxides that it contains lead, zirconium and titanium, described piezoceramic material is containing useful chemical general formula Pb
aba
1-a(Nb
bsb
bsr
1-2b)
xzr
yti
1-x-yo
3represent and meet the main ingredient of following relation: 0.8≤a≤0.95,0.1≤b≤0.2,0.03≤x≤0.1,0.45≤y≤0.55.
In a preferred embodiment of the present invention, described piezoceramic material forms by the doping of niobium, antimony, barium, strontium phase.
A kind of piezoelectricity sintered compact, described piezoelectricity sintered compact is to fire piezoceramic material at 1150 degrees Celsius to being incubated 3 hours in 1200 celsius temperature environment, described piezoceramic material at least contains the composite oxides of lead, zirconium and titanium, and described piezoceramic material is containing useful chemical general formula Pb
aba
1-a(Nb
bsb
bsr
1-2b)
xzr
yti
1-x-yo
3represent and meet the main ingredient of following relation:
0.8≤a≤0.95，0.1≤b≤0.2，0.03≤x≤0.1，0.45≤y≤0.55。
A kind of piezoelectric ceramic devices, adopt piezoceramic material to process, and described piezoceramic material at least contains the composite oxides of lead, zirconium and titanium, and described piezoceramic material is containing useful chemical general formula Pb
aba
1-a(Nb
bsb
bsr
1-2b)
xzr
yti
1-x-yo
3represent and meet the main ingredient of following relation:
0.8≤a≤0.95,0.1≤b≤0.2,0.03≤x≤0.1,0.45≤y≤0.55, also comprises the composite oxides that at least comprise lead, zirconium and titanium, and forms by the doping of niobium, barium, strontium phase.
Piezoceramic material is manufactured a preparation method for piezoelectric ceramics, and it comprises the steps:
Batching: main ingredient and added ingredients are provided and dry respectively;
Batch mixing: mix to form the mixture of the oxide compound that contains Pb, Zr, Ti, Nb, Sb, Sr, Ba or carbonate and dry according to weight proportion;
Synthetic: the mixture after above-mentioned batch mixing is calcined to synthesize to 1050 celsius temperature environment at 1000 degrees Celsius;
Pulverize: pulverize synthetic mixture after above-mentioned calcining, to obtain powder and to dry;
Slurrying: add binding agent, softening agent, dispersion agent, solvent and mix to form ceramic size in the powder after above-mentioned pulverizing;
Moulding: after de-bubble, curtain coating forms ceramic membrane;
Stacked: stacked the ceramic membrane after moulding setting formed to lamination product;
Sintering: be incubated three hours and fire described lamination product formation sintered product in 1150 degrees Celsius to 1200 degrees Celsius environment;
Processed by electrode and polarization: above-mentioned sintered product, by electrode, is implemented to polarization of electrode simultaneously and obtained piezoelectric ceramics.
In a preferred embodiment of the present invention, described synthesis step is to calcine more than 3 hours to synthesize to calcination environment in 1050 celsius temperature environment at 1000 degrees Celsius.
In a preferred embodiment of the present invention, described pulverising step is to be realized mixture after described calcining is pulverized by ball mill pulverizing mode.
In a preferred embodiment of the present invention, the powder of the median that described pulverising step obtains size-grade distribution below 1 micron.
Compared to correlation technique, piezoceramic material of the present invention has preferably piezo-electric modulus, and wherein d33 is up to 780pC/N, d31 is also high to 360pC/N, this can make piezo component keep, under the prerequisite that deformation quantity is constant, reducing input voltage, thereby reduces the requirement to complete machine; Or make piezo component keeping, under the prerequisite that input voltage is constant, improving effciency of energy transfer, obtain larger deformation.Preparation method's technique of described piezoceramic material is simple, it is adjustable to fill a prescription, can be used in batches suitability for industrialized production and utilize inverse piezoelectric effect to produce the various piezo components of deformation.
Brief description of the drawings
In order to be illustrated more clearly in the technical scheme in the embodiment of the present invention, below the accompanying drawing of required use during embodiment is described is briefly described, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing, wherein:
Fig. 1 is the structure phasor of piezoceramic material of the present invention.
Fig. 2 is the ferroelectric hysteresis loop schematic diagram of piezoceramic material shown in Fig. 1.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only a part of embodiment of the present invention, instead of whole embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art, not making all other embodiment that obtain under creative work prerequisite, belong to the scope of protection of the invention.
The invention provides a kind of piezoceramic material, it is the composite oxides that at least comprise lead, zirconium and titanium.Described piezoceramic material obtains by the doping of niobium, antimony, barium, strontium phase, and it has higher piezo-electric modulus.Described piezoceramic material comprises the main ingredient being expressed from the next:
Pb
aBa
1-a(Nb
bSb
bSr
1-2b)
xZr
yTi
1-x-yO
3，
Wherein meet 0.8≤a≤0.95,0.1≤b≤0.2,0.03≤x≤0.1,0.45≤y≤0.55.By adjusting the proportioning of a, b, x and y, adjust its performance, finally make it reach high tension electricity coefficient, Fig. 1 is the structure phasor of piezoceramic material of the present invention.
The present invention provides a kind of preparation method who adopts above-mentioned piezoceramic material to be processed to form piezoelectric ceramics simultaneously, it is by the various hopcalites to the main ingredient that forms described piezoceramic material, process the synthetic piezoceramic material principal phase of obtaining tool high tension electricity coefficient, prepare required piezoelectric ceramics by doctor-blade casting process again, specifically comprise the steps.
Step S1, batching: main ingredient and added ingredients are provided and dry respectively.
Each main ingredient and added ingredients are provided, and each starting material component at least contains the oxide compound of Pb, Zr, Ti, Nb and Mn.The raw material selection purity that provides is high, fineness is little and active large powder, selects raw materials usedly according to formula or molecular formula, and carries out corrected Calculation by material purity, then carries out the weighing of raw material.
Step S2, batch mixing: mix to form the mixture of the oxide compound that contains Pb, Zr, Ti, Nb, Sb, Sr, Ba or carbonate and dry according to weight proportion.
Correspondence is mixed each starting material component to form the hopcalite that at least contains Pb, Zr, Ti, Nb, Sb, Sr and Ba by ball mill.After pressing stoicheiometry batching, use planetary ball mill that various batchings are mixed.What industry adopted conventionally is that horizontal direction is rotated ball milling method, can certainly select the blending meanss such as vibrations ball milling and comminution by gas stream.
Step S3, synthetic: the mixture after above-mentioned batch mixing is calcined more than 3 hours to synthesize to calcination environment in 1050 celsius temperature environment at 1000 degrees Celsius.
Step S4, pulverizes: pulverize synthetic mixture after above-mentioned calcining, to obtain powder and to dry.Wherein said pulverising step is to be realized mixture after described calcining is pulverized by ball mill pulverizing mode, and the described pulverising step powder of median below 1 micron that obtain size-grade distribution.
Step S5, slurrying: add binding agent, softening agent, dispersion agent, solvent and mix to form ceramic size in the powder after above-mentioned pulverizing.Wherein, described slurrying adds binding agent, softening agent, dispersion agent, solvent are as shown in table 1 below.
Table 1
Step S6, moulding: form ceramic green sheet after de-bubble.
The method of forming ceramic base sheet mainly contains four kinds; Rolling formation, flow casting molding, dry-pressing formed and hydrostaticpressure moulding.Rolling formation is applicable to thin sheet element; Flow casting molding is suitable for thinner element, and thickness can be less than 10m; The dry-pressing formed block elements that is suitable for; Hydrostaticpressure moulding is suitable for abnormity or block elements.Except hydrostaticpressure moulding, other forming methods all need to have tackiness agent, and tackiness agent generally accounts for 3% left and right of raw material weight.Moulding needs binder removal later.The effect of tackiness agent is just beneficial to moulding, but it is the material that a kind of reductibility is strong, should be by its discharge in order to avoid affect sintering quality after moulding.In the present invention, adopt flow casting molding method to form ceramic green sheet.
Step S7, stacked: folded the ceramic green sheet after moulding setting formed to lamination product.
Step S8, sintering: be incubated three hours and fire described lamination product formation sintered product in 1150 degrees Celsius to 1200 degrees Celsius environment.
Step S9, is processed by electrode and polarization: above-mentioned sintered product, by electrode, is implemented to polarization of electrode simultaneously and obtained piezoelectric ceramics.
On described ceramic green sheet, form electrode layer with realize piezoelectric ceramics by electrode, wherein available electrode materials has silver, copper, gold, platinum etc.The method that forms described electrode layer has vacuum-evaporation, electroless plating etc. multiple.Adopt in the present embodiment, coat silver slurry, fired electrodes in air.Described polarization adopts conventional polarization mode: the thickness direction along ceramic plate under air at room temperature adds certain voltage, and pressurize certain hour.
By step S8 gained sinter, be placed in the silicone oil of 130 DEG C, apply the DC electric field of 5KV/mm, polarization 1min, then removes electric field, so obtains the piezoelectric ceramics of above-mentioned sintered product execution polarization of electrode.
Step S10, test piezoelectric property;
The piezoelectric ceramics that step S9 polarization is processed is tested its piezoelectric property after standing 24h under room temperature.Concrete sample test is the results detailed in Table 2.
Table 2
Wherein, calculate specific inductivity by measure sample size and LCR;
Directly read dielectric loss by LCR;
Read d33 by quasistatic d33 tester;
Read resonant frequency, anti-resonance frequency, resonance impedance, antiresonance impedance, first overtone frequency etc. by the accurate electric impedance analyzer of agilent4294A and calculate electromechanical coupling factor (Kp, K31, Kt), piezoelectric coefficient d 31, mechanic quality factor etc.;
Test ferroelectric hysteresis loop by ferroelectric tester;
Observe microstructure by scanning electron microscope.
Through verification experimental verification, the piezoelectric ceramics that adopts above-mentioned preparation method to be processed to form has preferably piezo-electric modulus, specifically as shown in Figure 2, wherein d33 is up to 788pC/N, d31 also exceedes 360pC/N, this can make piezo component keep, under the prerequisite that deformation quantity is constant, reducing input voltage, thereby reduces the requirement to complete machine; Or make piezo component keeping, under the prerequisite that input voltage is constant, improving effciency of energy transfer, obtain larger deformation.
In above-mentioned preparation method, preparation method's technique of described piezoceramic material is simple, it is adjustable to fill a prescription, can be used in batches suitability for industrialized production and utilize inverse piezoelectric effect to produce the various piezo components of deformation.
Separately, at the corresponding piezoelectric ceramics sintered compact that generates of step S8, described piezoelectric ceramics sintered compact is in 1150 celsius temperature environment, to be incubated 3 hours to fire piezoceramic material, the composite oxides that described piezoceramic material contains lead, zirconium and titanium, and described piezoceramic material is containing useful chemical general formula Pb
aba
1-a(Nb
bsb
bsr
1-2b)
xzr
yti
1-x-yo
3represent and meet the main ingredient of following relation:
0.8≤a≤0.95，0.1≤b≤0.2，0.03≤x≤0.1，0.45≤y≤0.55。
Simultaneously, the present invention also provides a kind of piezoelectric ceramic devices that adopt above-mentioned piezoceramic material to process, described piezoelectric ceramic devices adopt piezoceramic material to process, the composite oxides that described piezoceramic material contains lead, zirconium and titanium, described piezoceramic material is containing useful chemical general formula Pb
aba
1-a(Nb
bsb
bsr
1-2b)
xzr
yti
1-x-yo
3represent and meet the main ingredient of following relation:
0.8≤a≤0.95,0.1≤b≤0.2,0.03≤x≤0.1,0.45≤y≤0.55, also comprises the composite oxides that at least comprise lead, zirconium and titanium, and forms by the doping of niobium, barium, strontium phase.
Described piezoceramic material can be used for batch suitability for industrialized production and utilizes inverse piezoelectric effect to produce the piezoelectric ceramic devices of the various high tension electricity coefficients of deformation.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes specification sheets of the present invention and accompanying drawing content to do; or be directly or indirectly used in other relevant technical field, be all in like manner included in scope of patent protection of the present invention.
Claims (4)
1. a preparation method for piezoelectric ceramics, is characterized in that, described preparation method comprises the steps:
Batching: provide by chemical general formula Pb
aba
1-a(Nb
bsb
bsr
1-2b)
xzr
yti
1-x-yo
3represent, and meet 0.8≤a≤0.95,0.1≤b≤0.2; 0.03≤x≤0.1, the main ingredient of 0.45≤y≤0.55 relation and added ingredients are also dried respectively;
Batch mixing: mix to form the mixture of the oxide compound that contains Pb, Zr, Ti, Nb, Sb, Sr, Ba or carbonate and dry according to the weight proportion of above-mentioned chemical general formula;
Synthetic: the mixture after above-mentioned batch mixing is calcined to synthesize to 1050 celsius temperature environment at 1000 degrees Celsius;
Pulverize: pulverize synthetic mixture after above-mentioned calcining, to obtain powder and to dry;
Slurrying: add binding agent, softening agent, dispersion agent, solvent and mix to form ceramic size in the powder after above-mentioned pulverizing;
Moulding: after de-bubble, curtain coating forms ceramic membrane;
Stacked: stacked the ceramic membrane after moulding setting formed to lamination product;
Sintering: be incubated three hours and fire described lamination product formation sintered product in 1150 degrees Celsius to 1200 degrees Celsius environment;
Processed by electrode and polarization: above-mentioned sintered product, by electrode, is then placed in to the silicone oil of 130 DEG C, applies the DC electric field of 5KV/mm the 1min that polarizes, then remove electric field and obtain piezoelectric ceramics.
2. the preparation method of piezoelectric ceramics according to claim 1, is characterized in that, described synthesis step is to calcine more than 3 hours to synthesize to calcination environment in 1050 celsius temperature environment at 1000 degrees Celsius.
3. the preparation method of piezoelectric ceramics according to claim 1, is characterized in that, described pulverising step is to be realized mixture after described calcining is pulverized by ball mill pulverizing mode.
4. the preparation method of piezoelectric ceramics according to claim 3, is characterized in that, the powder of the median that described pulverising step obtains size-grade distribution below 1 micron.
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| CN103360069B (en) * | 2013-07-17 | 2014-12-17 | 肇庆捷成电子科技有限公司 | Lead zirconate titanate B-site niobium-antimony composite substitution modified piezoelectric ceramic and preparation method thereof |
| CN103539448A (en) * | 2013-10-09 | 2014-01-29 | 瑞声声学科技(深圳)有限公司 | Piezoelectric ceramic material, piezoelectric ceramic component and preparation method and anti-aging method of piezoelectric ceramic |
| CN106478149A (en) * | 2016-09-12 | 2017-03-08 | 华南理工大学 | A kind of piezoelectric with anti-microbial property and preparation method and application |
| CN109678501B (en) * | 2018-12-17 | 2021-11-19 | 贵州振华红云电子有限公司 | Formula and preparation method of piezoelectric vibrator porcelain special for smoke alarm |
| CN111606707B (en) * | 2020-06-05 | 2021-11-30 | 江苏波速传感器有限公司 | Temperature-holding stable piezoelectric ceramic material and preparation method thereof |
| CN111778458A (en) * | 2020-07-09 | 2020-10-16 | 苏州市高科百年工贸有限公司 | Formula and preparation process of ceramic material for 5G communication ceramic dielectric filter |
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| JPH07280571A (en) * | 1994-04-07 | 1995-10-27 | Murata Mfg Co Ltd | Piezoelectric ceramic for vibrating gyro and vibrating gyro |
| JP3874229B2 (en) * | 1999-07-02 | 2007-01-31 | Ｔｄｋ株式会社 | Piezoelectric ceramics and piezoelectric device using the same |
| JP4631246B2 (en) * | 2002-03-20 | 2011-02-16 | 株式会社豊田中央研究所 | Piezoelectric ceramic composition, manufacturing method thereof, piezoelectric element and dielectric element |
| CN101265090A (en) * | 2008-04-21 | 2008-09-17 | 天津大学 | Strontium and barium doping lead niobium-stibium zirconate-titanate series piezoelectric ceramic and preparation method thereof |
| CN102757217B (en) * | 2011-04-29 | 2015-04-29 | 深圳振华富电子有限公司 | Water-base tape casting slurry and water-base tape casting wet method for preparing multilayer chip component |
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