CN101712548A - High efficiency piezoelectric ceramic material with low sintering temperature and preparation technology thereof - Google Patents

High efficiency piezoelectric ceramic material with low sintering temperature and preparation technology thereof Download PDF

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CN101712548A
CN101712548A CN200910192826A CN200910192826A CN101712548A CN 101712548 A CN101712548 A CN 101712548A CN 200910192826 A CN200910192826 A CN 200910192826A CN 200910192826 A CN200910192826 A CN 200910192826A CN 101712548 A CN101712548 A CN 101712548A
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姜德星
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Prestige sensing Science and Technology Co., Ltd. of Guangdong Audi
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GUANGZHOU PANYU AODIWEI ELECTRONIC CO Ltd
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Abstract

The invention discloses a piezoelectric ceramic with low sintering temperature and high piezoelectric property and preparation technology thereof. The piezoelectric ceramic comprises main ingredients and auxiliary ingredients. The chemical formula of the main ingredients is as below, wherein Me is any one or two of Ba, Ca and Sr, and the auxiliary ingredients are SiO2, H3BO3 or the mixture of the two ingredients, and Sb2O5 or Sb2O3, Bi2O3 or Bi2O5, Li2CO3 or Na2CO3 or the mixture of the two ingredients, and CuO. The preparation technology comprises mixing, ball milling, stoving, presintering, ball milling, pelleting, forming, dumping, sintering, silver brushing, silver sintering and polarizing. The piezoelectric ceramic provided by the invention has the advantages of energy saving, environmental protection, low cost, high property and the like, has wide application prospect and is especially suitable for piezoelectric ceramic loudspeakers and piezoelectric buzz films with large power.

Description

High efficiency piezoelectric ceramic material that a kind of sintering temperature is low and preparation technology thereof
Technical field
The present invention relates to piezoelectric ceramics and preparation technology field thereof, relate in particular to a kind of Pb-based lanthanumdoped zirconate titanates (PZT) piezoelectric ceramics, be applicable to piezoelectric ceramics buzzing sheet, multilayer piezoelectric speaker, multi-layer piezoelectric performer (actuator).
Background technology
The PZT piezoelectric ceramics is with plumbic oxide, lead zirconates, the lead titanate polycrystal that forms of sintering at high temperature, be widely used in fields such as industry, agricultural, military affairs, medical treatment, but the PZT piezoelectric ceramics sintering temperature of prior art is mostly about 1300 ℃, plumbous volatilization is serious, not only influence material property, contaminate environment is studied low-temperature sintering and is had great significance: 1. reduces plumbous volatilization, avoid the composition off-design composition of pottery especially; 2. reduce environmental pollution; 3. save the energy, prolong service life of equipment; 4. in multilayer piezoelectric device, the consumption of precious metals such as Pt capable of reducing using, Pd, even can use base metals such as Ag, Ni, Cu as electrode, reduce device cost greatly.
2006 the 4th phases of periodical " silicate journal ", in low-temperature sintering PZT-0.5%PbO-WO3 piezoelectric ceramics one literary composition, a kind of low sintering piezoelectric ceramics is disclosed, its sintering temperature is 1100 ℃, specific inductivity is 1593, d33=364pC/N, Kp=0.596, its piezoelectricity is too low, can not be used to prepare high-power loudspeaker.
Number of patent application is 200410016324.0 Chinese invention patent, " doping manganese niobium lead acid-lead lanthanum zirconate titanate (PLZT) electrooptical ceramics material and preparation technology thereof " disclosed, its sintering temperature is 1050 ℃-1250 ℃, because its piezoelectric property is low, can not be used to make the high-power piezoelectric ceramic loud speaker.
Summary of the invention
For solving the problem that prior art exists, the invention provides the piezoelectric ceramics that a kind of sintering temperature is low, piezoelectric property is high.
Another object of the present invention provides the preparation technology of described piezoelectric ceramics.
The present invention is achieved in that
The high efficiency piezoelectric ceramic material that a kind of sintering temperature is low comprises major ingredient and auxiliary composition,
Described major ingredient chemical formula is:
Wherein Me is any one or two kinds of elements among Ba, Ca, the Sr, and 0.97≤a≤1.05,0.03≤b≤0.10,0.05≤c≤0.15,0.05≤d≤0.15,0.35≤e≤0.45,0.35≤f≤0.45, and c+d+e+f=1;
Gross weight with main component is the following auxiliary composition of 100% interpolation:
0.008%～0.1%SiO 2Or 0.008%～0.1%H 3BO 3Or both mixtures;
0.10%～0.60% Sb 2O 5Or Sb 2O 3
0.10%～0.60% Bi 2O 3Or Bi 2O 5
0.03%～0.20%Li 2CO 5Or Na 2CO 3Or both mixtures;
0.08％～0.2％CuO。
The main component of preferred following content and auxiliary composition in the piezoelectric ceramics provided by the invention:
Described major ingredient chemical formula is:
Pb 0.995-0?08Sr 0?05Ba 0?03(Ni 1/3Nb 2/3) 0?08(Zn 1/3Nb 2/3) 0?12Ti 0?40Zr 0?40O 3????(2)
Gross weight with main component is the following auxiliary composition of 100% interpolation:
0.05%SiO 2And 0.05%H 3BO 3Mixture, 0.30% Sb 2O 3, 0.40% Bi 2O 5, 0.15% Li 2CO 3, 0.15% CuO.
A kind of preparation technology who prepares described piezoceramic material comprises the steps:
By the chemical formula batching of main component, in mixed main component, add following ancillary component: CuO, SiO 2Or H 3BO 3Or both mixtures, Sb 2O 5Or Sb 2O 3, Bi 2O 3Or Bi 2O 5, Li 2CO 3Or Na 2CO 3
Above-mentioned ceramic raw material is dropped in the planetary ball mill with deionized water, mix discharging after 6～10 hours, oven dry;
Above-mentioned steps gained mixing raw material 780 ℃～800 ℃ pre-burnings 2～3 hours, is mixed the preburning powder that obtains with deionized water, use planetary ball mill 6～10 hours, up to d 50≤ 0.40 μ M, d 9O≤ 0.60 μ M, oven dry;
To dry powder and add polyvinyl alcohol solution, granulation, dry-pressing formed;
Binder removal, sintering, described sintering temperature is 890 ℃～950 ℃;
With the product face machined flat behind the sintering, carry out silk screen printing silver slurry then, silver ink firing;
Product behind the silver ink firing is polarized, and placed 24 hours the polarization back, promptly obtains described piezoelectric ceramics.
Main component among the present invention
Figure G2009101928261D00031
In:
0.97≤a≤1.05, if a＜0.97, coking property descends, and sintering temperature rises, simultaneously excessive with the stoichiometric ratio deviation, generate heterogeneously easily, piezoelectric property worsens, if a＞1.05, Pb too high levels then, the piezoelectric property of sintered products descends, and environmental pollution is serious;
0.03≤b≤0.10, if b＜0.03, the specific inductivity of piezoceramic material and piezoelectric strain constant d33 are on the low side, if b＞0.1, the Curie temperature of piezoceramic material descends and sintering character descends;
0.05≤c≤0.15,0.05≤d≤0.15, if c＜0.05, d＜0.05, the then specific inductivity of piezoceramic material, piezoelectric strain constant d 33Big inadequately, if c＞0.15, d＞0.15, then the decline of the Curie temperature of piezoceramic material is very big, and if Nb 2O 5Content is big, because Nb 2O 5The price height is so can increase the cost of piezoceramic material;
0.35≤e≤0.45,0.35≤f≤0.45, the composition that keeps piezoelectric ceramics guarantees that piezoelectric ceramics has bigger specific inductivity and higher piezoelectric strain constant near phase interface (MPB).
In main component, add an amount of SiO 2Or H 3BO 3, CuO, Bi 2O 3Or Bi 2O 5, Li 2CO 3Or Na 2CO 3, Sb 2O 5Or Sb 2O 3Main purpose is in order to form eutectic mixture, form liquid phase, the good wetting ceramic particle of liquid phase energy in that sintering forms in earlier stage quickens the process of sintering mass transfer, makes to be diffused rapidly to lattice, reduce sintering temperature from face, in the sintering later stage, described additive enters lattice mostly, thereby improves the piezoelectricity of piezoelectric ceramics.
Compared with prior art, by the piezoelectric ceramics that prescription of the present invention and preparation technology produce, piezoelectric property significantly improves, and its specific inductivity is 3500-4800, dielectric loss＜2%, planar electromechanical coupling factor 〉=65%, piezoelectric strain constant d 33〉=550PV/N, mechanical quality factor Q m is 50-150, in the purpose that keeps above-mentioned high tension performance, sintering temperature is also reduced to 890 ℃-950 ℃, and optimum temperature range is 910 ℃-930 ℃, piezoelectric ceramics provided by the invention, have energy-conserving and environment-protective, cost is low, the performance advantages of higher, be with a wide range of applications, be particularly useful for piezoelectric ceramic loudspeaker and high-power piezoelectricity singing piece.
Embodiment
Describe the present invention in detail below in conjunction with specific embodiment, be used for explaining the present invention in this illustrative examples of the present invention and explanation, but not as a limitation of the invention.
Embodiment 1:
Pb 0.97-0.10Sr 0.10(Ni 1/3Nb 2/3) 0.05(Zn 1/3Nb 2/3) 0.15Zr 0.35Ti 0.45O 3??(1)
Main component is Pb 3O 4, ZrO 2, TiO 2, SrCO 3, NiCO 3, ZnO, Nb 2O 5, the prescription weighing of pressing chemical formula (1) is 100% with above-mentioned major ingredient gross weight, adds following additive: 0.008%H 3BO 3, 0.60% Sb 2O 5, 0.10% Bi 2O 3, 0.03% Li 2CO 3, 0.2%CuO;
Then, above-mentioned ceramic raw material is dropped in the planetary ball mill with deionized water, mix discharging after 6-10 hour, oven dry, wherein in the planetary ball mill process, compound: ball: water=1: 3.5: 0.7;
With mixing raw material 780 ℃-800 ℃ pre-burning 2-3 hour, the preburning powder that obtains is mixed with deionized water, with planetary ball mill 6-10 hour, up to d 50≤ 0.40 μ m, d 90≤ 0.60 μ m, oven dry;
Weight ratio is 5%～10% with adding in the oven dry powder, concentration is 6%～10% polyvinyl alcohol solution, and granulation is dry-pressing formed;
Binder removal, sintering, the agglomerating temperature range is 890 ℃-950 ℃;
With the product face machined flat behind the sintering, carry out silk screen printing silver slurry then, silver ink firing;
Polarization, the polarization temperature is 100 ℃-150 ℃, polarized electric field is 10-15min for the 2KV-4KV polarization time, places 24 hours.
Place its dielectric properties of test and piezoelectric property after 24 hours, its performance is as follows:
??Kp ??d 33×10 -12C/N ??εr ??tgδ ??Q m Optimal sintering temperature Porcelain body density
??0.65 ??610 ??4100 ??1.5％ ??120 ??920℃ ??7.75g/cm 3
Embodiment 2:
Pb 0.995-0.08Sr 0.05Ba 0.03(Ni 1/3Nb 2/3) 0.08(Zn 1/3Nb 2/3) 0.12Ti 0.40Zr 0.40O 3(2)
Main component is Pb 3O 4, ZrO 2, TiO 2, SrCO 3, BaCO 3, NiCO 3, ZnO, Nb 2O 5, the prescription weighing of pressing chemical formula (2) is 100% with above-mentioned major ingredient gross weight, adds following additive: 0.05% SiO 2And 0.05%H 3BO 3Mixture, 0.30% Sb 2O 3, 0.40% Bi 2O 5, 0.15% Li 2CO 3, 0.15% CuO;
Then, above-mentioned ceramic raw material is dropped in the planetary ball mill with deionized water, mix discharging after 6-10 hour, oven dry, wherein in the planetary ball mill process, compound: ball: water=1: 3.5: 0.9;
With mixing raw material 780 ℃-800 ℃ pre-burning 2-3 hour, the preburning powder that obtains is mixed with deionized water, with planetary ball mill 6-10 hour, up to d 50≤ 0.40 μ m, d 90≤ 0.60 μ m, oven dry;
Weight ratio is 5%～10% with adding in the oven dry powder, concentration is 6%～10% polyvinyl alcohol solution, and granulation is dry-pressing formed;
Binder removal, sintering, the agglomerating temperature range is 890 ℃-950 ℃;
With the product face machined flat behind the sintering, carry out silk screen printing silver slurry then, silver ink firing;
Polarization, the polarization temperature is 100 ℃-150 ℃, polarized electric field is 10-15min for the 2KV-4KV polarization time, places 24 hours.
Place its dielectric properties of test and piezoelectric property after 24 hours, its performance is as follows:
??Kp ??d 33×10 -12C/N ??εr ??tgδ ??Q m Best sintering Porcelain body density
Temperature
??0.66 ??590 ??3950 ??1.8％ ??100 ??930℃ ??7.70g/cm 3
Embodiment 3
Pb 1.05-0.03Ba 0.03(Ni 1/3Nb 2/3) 0.15(Zn 1/3Nb 2/3) 0.05Ti 0.45Zr 0.35O 3????(3)
Main component is Pb 3O 4, ZrO 2, TiO 2, BaCO 3, NiCO 3, ZnO, Nb 2O 5, the prescription weighing of pressing chemical formula (3) is 100% with above-mentioned major ingredient gross weight, adds following additive: 0.1% SiO 2, 0.10% Sb 2O 5, 0.60% Bi 2O 3, 0.2% Na 2CO 3, 0.08% CuO;
Then, above-mentioned ceramic raw material is dropped in the planetary ball mill with deionized water, mix discharging after 6-10 hour, oven dry, wherein in the planetary ball mill process, compound: ball: water=1: 3.5: 0.8;
With mixing raw material 780 ℃-800 ℃ pre-burning 2-3 hour, the preburning powder that obtains is mixed with deionized water, with planetary ball mill 6-10 hour, up to d 50≤ 0.40 μ m, d 90≤ 0.60 μ m, oven dry;
Weight ratio is 5%～10% with adding in the oven dry powder, concentration is 6%～10% polyvinyl alcohol solution, and granulation is dry-pressing formed;
Binder removal, sintering, the agglomerating temperature range is 890 ℃-950 ℃;
With the product face machined flat behind the sintering, carry out silk screen printing silver slurry then, silver ink firing;
Polarization, the polarization temperature is 100 ℃-150 ℃, polarized electric field is 10-15min for the 2KV-4KV polarization time, places 24 hours.
Place its dielectric properties of test and piezoelectric property after 24 hours, its performance is as follows:
??Kp ??d 33×10 -12C/N ??εr ??tgδ ??Q m Optimal sintering temperature Porcelain body density
??0.61 ??550 ??3400 ??1.8％ ??60 ??940℃ ??7.65??g/cm 3
Embodiment 4:
Pb 1.00-0.10Sr 0.06Ca 0.04(Ni 1/3Nb 2/3) 0.10(Zn 1/3Nb 2/3) 0.10Ti 0.38Zr 0.42O 3(4)
Main component is Pb 3O 4, ZrO 2, TiO 2, SrCO 3, CaCO 3, NiCO 3, ZnO, Nb 2O 5, the prescription weighing of pressing chemical formula (4) is 100% with above-mentioned major ingredient gross weight, adds following additive: 0.008% SiO 2, 0.30% Sb 2O 5, 0.40% Bi 2O 5, 0.10% Li 2CO 3With 0.05% Na 2CO 3Mixture, 0.10% CuO;
Then, above-mentioned ceramic raw material is dropped in the planetary ball mill with deionized water, mix discharging after 6-10 hour, oven dry, wherein in the planetary ball mill process, compound: ball: water=1: 3.5: 0.7;
With mixing raw material 780 ℃-800 ℃ pre-burning 2-3 hour, the preburning powder that obtains is mixed with deionized water, with planetary ball mill 6-10 hour, up to d 50≤ 0.40 μ m, d 90≤ 0.60 μ m, oven dry;
Weight ratio is 5%～10% with adding in the oven dry powder, concentration is 6%～10% polyvinyl alcohol solution, and granulation is dry-pressing formed;
Binder removal, sintering, the agglomerating temperature range is 890 ℃-950 ℃;
With the product face machined flat behind the sintering, carry out silk screen printing silver slurry then, silver ink firing;
Polarization, the polarization temperature is 100 ℃-150 ℃, polarized electric field is 10-15min for the 2KV-4KV polarization time, places 24 hours.
Place its dielectric properties of test and piezoelectric property after 24 hours, its performance is as follows:
??Kp ??d 33×10 -12C/N ??εr ??tgδ ??Q m Optimal sintering temperature Porcelain body density
??0.62 ??580 ??3800 ??1.9％ ??70 ??930℃ ??7.72??g/cm 3
More than the technical scheme that the embodiment of the invention provided is described in detail, used specific case herein the principle and the embodiment of the embodiment of the invention are set forth, the explanation of above embodiment only is applicable to the principle that helps to understand the embodiment of the invention; Simultaneously, for one of ordinary skill in the art, according to the embodiment of the invention, the part that on embodiment and range of application, all can change, in sum, this description should not be construed as limitation of the present invention.

Claims (7)

1. high efficiency piezoelectric ceramic material that sintering temperature is low, it is characterized in that: described piezoelectric ceramics comprises major ingredient and auxiliary composition,
Described major ingredient chemical formula is:
Figure F2009101928261C00011
Wherein Me is any one or two kinds of elements among Ba, Ca, the Sr, and 0.97≤a≤1.05,0.03≤b≤0.10,0.05≤c≤0.15,0.05≤d≤0.15,0.35≤e≤0.45,0.35≤f≤0.45, and c+d+e+f=1;
Gross weight with main component is the following auxiliary composition of 100% interpolation:
0.008%～0.1% SiO 2Or 0.008%～0.1% H 3BO 3Or both mixtures;
0.10%～0.60% Sb 2O 5Or Sb 2O 3
0.10%～0.60% Bi 2O 3Or Bi 2O 5
0.03%～0.20% Li 2CO 3Or Na 2CO 3Or both mixtures;
0.08％～0.2％?CuO。
2. the low high efficiency piezoelectric ceramic material of sintering temperature as claimed in claim 1 is characterized in that:
Described piezoelectric ceramics comprises major ingredient and auxiliary composition,
Described major ingredient chemical formula is:
Pb 0?995-0?08Sr 0?05Ba 0?03(Ni 1/3Nb 2/3) 0?08(Zn 1/3Nb 2/3) 0?12?Ti 0?40Zr 0?40O 3????(2)
Gross weight with main component is the following auxiliary composition of 100% interpolation:
0.05% SiO 2With 0.05% H 3BO 3Mixture, 0.30% Sb 2O 3, 0.40% Bi 2O 5, 0.15% Li 2CO 3, 0.15% CuO.
3. preparation technology who prepares claim 1 or 2 described piezoceramic materials, it is characterized in that: described technology comprises the steps:
By the chemical formula batching of main component, in mixed main component, add following ancillary component: CuO, SiO 2Or H 3BO 3Or both mixtures, Sb 2O 5Or Sb 2O 3, Bi 2O 3Or Bi 2O 5, Li 2CO 3Or Na 2CO 3
Above-mentioned ceramic raw material is dropped in the planetary ball mill with deionized water, mix discharging after 6～10 hours, oven dry;
Above-mentioned steps gained mixing raw material 780 ℃～800 ℃ pre-burnings 2～3 hours, is mixed the preburning powder that obtains with deionized water, use planetary ball mill 6～10 hours, up to d 50≤ 0.40 μ M, d90≤0.60 μ M, oven dry;
To dry powder and add polyvinyl alcohol solution, granulation, dry-pressing formed;
Binder removal, sintering, described sintering temperature is 890 ℃～950 ℃;
With the product face machined flat behind the sintering, carry out silk screen printing silver slurry then, silver ink firing;
Product behind the silver ink firing is polarized, and placed 24 hours the polarization back, promptly obtains described piezoelectric ceramics.
4. the preparation technology of piezoceramic material as claimed in claim 3 is characterized in that: with main component Pb 3O 4, ZrO 2, TiO 2, Ba CO 3/ CaCO 3/ SrCO 3In any or two kinds, NiCO 3, ZnO, Nb 2O 5Chemical formula batching by main component.
5. the preparation technology of piezoceramic material as claimed in claim 3 is characterized in that: in the described planetary ball mill process, and compound: ball: water=1: 3.5: (0.7-0.9).
6. the preparation technology of piezoceramic material as claimed in claim 3, it is characterized in that: described polarization condition is: will dry add in the powder that weight ratio is 5%～10%, concentration is 6%～10% polyvinyl alcohol solution.
7. the preparation technology of piezoceramic material as claimed in claim 3, it is characterized in that: described polarization condition is: temperature is 100 ℃～150 ℃, and polarized electric field is 2KV～4KV, and the polarization time is 10～15min.
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