CN103771854A - Piezoceramic material and preparation method thereof - Google Patents

Piezoceramic material and preparation method thereof Download PDF

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CN103771854A
CN103771854A CN201310714087.4A CN201310714087A CN103771854A CN 103771854 A CN103771854 A CN 103771854A CN 201310714087 A CN201310714087 A CN 201310714087A CN 103771854 A CN103771854 A CN 103771854A
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CN103771854B (en
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李玉臣
董显林
姚烈
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Shanghai Institute of Ceramics of CAS
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Abstract

The invention discloses a piezoceramic material and a preparation method thereof. The piezoceramic material has the chemical general formula of Pb1-xMx(Sb1/2Nb1/2)y(Mn1/3Sb2/3)z(ZreTif)1-y-zO3+awt.%Fe2O3+bwt.%Sm2O3+cwt.%MnO2+dwt.%Al2O3, wherein M is Sr<2+> and/or Ba<2+>, x=0.02-0.1, y=0.01-0.1, z=0.01-0.1, e=0.40-0.60, f=0.40-0.60, f meets the condition that e+f=1, a=0-0.4, b=0-0.5, c=0-1.0, d=0-1.0, and the content of at most one of dopants in the four dopants including Fe2O3, Sm2O3, MnO2 and Al2O3 is equal to 0. The piezoceramic material disclosed by the invention has the main performances as follows: d33=210Pc/N, epsilon33T/epsilon0=585, tan delta=0.20%, kp=0.56, kt=0.54, and Qm=1210. Compared with a common power transmitted piezoceramic material, the piezoceramic material disclosed by the invention is lower in dielectric constant, smaller in dielectric loss and higher in mechanical quality factor and electromechanical coupling coefficient and is a power transmitted piezoceramic material with favorable performance, low dielectric constant and high mechanical quality factor.

Description

Piezoceramic material and preparation method thereof
Technical field
The invention belongs to material technology field, be specifically related to a kind of piezoceramic material and preparation method thereof.
Background technology
Along with the fast development of modern science and technology, the research of piezoceramic material is more and more deep, applies also more and more extensive.In recent years, the application of piezoceramic material aspect medical science also constantly expanded, and detects, diagnoses to treatment from medical science, and piezoelectric ceramics has been brought into play vital role as the core component of system.Wherein ultrasonic fracture therapeutic equipment (Sonic Accelerated Fracture Healing System) is exactly the sclerotin healing rehabilitation equipment that development in recent years is got up.It also can be fractured or one-level open fractures of tibia shaft fracture through the new formation closed rear distal ends tip of closed reduction and the fixing orthopaedics therapy of gypsum for grownup for the non-implantation treatment of nonunion except skull and backbone, promotes affected part healing.Ultrasonic fractures is a kind of non-intervention type treatment, and the low intensity ultrasound wave energy that it produces is sent to fracture site by ultrasonic coupling glue, can accelerate the healing of fresh fracture, and fracture delayed union and nonunion are also had to good curative effect.
The core work parts of ultrasonic fracture therapeutic equipment are piezoelectric ceramic transducers, when its transducer designs, adopt the thickness direction vibration modes of piezoelectric ceramics, the ultrasonic energy that it produces is sent to fracture site by ultrasonic coupling glue, it requires the ultrasonic energy intensity can not be too large, can be sent to well again fracture site simultaneously, this just requires piezoelectric ceramics to have lower specific inductivity, less dielectric loss has higher mechanical quality factor and electromechanical coupling factor simultaneously, and this is by the challenge new to researching and proposing of piezoelectric ceramics.Having low specific inductivity, less dielectric loss has the piezoelectric ceramics of higher mechanical quality factor simultaneously often electromechanical coupling factor is lower; And the high piezoelectric ceramics dielectric coefficient of electromechanical coupling factor is larger, this often more difficult realization aspect the design of material composition and material preparation process.
Summary of the invention
The present invention is directed to the piezoceramic material of prior art in the situation that having compared with low-k, less dielectric loss, cannot take into account higher mechanical quality factor and the technical problem of electromechanical coupling factor, object is to provide a kind of new piezoceramic material simultaneously.The present invention adopts niobium Naples yellow, antimony mangaic acid lead and Pb-based lanthanumdoped zirconate titanates (PZT) compound solid solution, and the multiple element that simultaneously adulterates is as added Fe 2o 3, Sm 2o 3, MnO 2and Al 2o 3in 4 kinds at least 3 kinds, carry out modification to piezoceramic material, obtain and have the piezoceramic material of simultaneously taking into account again the excellent properties of higher mechanical quality factor and electromechanical coupling factor compared with low-k, less dielectric loss.
Piezoceramic material of the present invention, its chemical general formula is: Pb 1-xm x(Sb 1/2nb 1/2) y(Mn 1/3sb 2/3) z(Zr eti f) 1-y-zo 3+ awt.%Fe 2o 3+ bwt.%Sm 2o 3+ cwt.%MnO 2+ dwt.%Al 2o 3,
Wherein, M is Sr 2+and/or Ba 2+;
X=0.02～0.1, y=0.01～0.1, z=0.01～0.1, e=0.40～0.60, f=0.40～0.60 and meet e+f=1;
A=0～0.4, b=0～0.5, c=0～1.0, d=0～1.0 and Fe 2o 3, Sm 2o 3, MnO 2and Al 2o 3in 4 kinds of hotchpotchs, the content of a kind of hotchpotch is 0 at the most,
Wherein, wt.% is with Pb 1-xm x(Sb 1/2nb 1/2) y(Mn 1/3sb 2/3) z(Zr eti f) 1-y-zo 3be 100% to calculate, rather than with
Pb 1-xm x(Sb 1/2nb 1/2) y(Mn 1/3sb 2/3) z(Zr eti f) 1-y-zo 3+ awt.%Fe 2o 3+ bwt.%Sm 2o 3+ cwt.%MnO 2+ dwt.%Al 2o 3be 100% calculating.
In a preferred embodiment of the present invention, a=0.01～0.4, b=0.02～0.5, c=0.02～1.0, d=0.01～1.0.
In another preferred embodiment of the present invention, M is Sr 2+and Ba 2+time, Sr 2+and Ba 2+mol ratio be 2:5.
In the present invention, be preferably x=0.07, y=0.01～0.05, z=0.01～0.04, e=0.50～0.55, f=0.45～0.50 and meet e+f=1; A=0.01～0.06, b=0.02～0.2, c=0.02～0.1, d=0.01～0.05; More preferably, x=0.07, y=0.01～0.02, z=0.01～0.02, e=0.50～0.55, f=0.45～0.50 and meet e+f=1; A=0.01～0.06, b=0.02～0.1, c=0.02～0.1, d=0.01～0.05.
Piezoceramic material of the present invention specifically has several as follows:
Pb 0.93Sr 0.02Ba 0.05(Sb 1/2Nb 1/2) 0.01(Mn 1/3Sb 2/3) 0.02(Zr 0.545Ti 0.455) 0.97O 3+0.02wt.%Fe 2O 3+0.1wt.%Sm 2O 3+0.06wt.%MnO 2+0.01wt.%Al 2O 3；
Pb 0.93Sr 0.02Ba 0.05(Sb 1/2Nb 1/2) 0.005(Mn 1/3Sb 2/3) 0.015(Zr 0.545Ti 0.455) 0.98O 3+0.02wt.%Fe 2O 3+0.1wt.%Sm 2O 3+0.06wt.%MnO 2+0.01wt.%Al 2O 3；
Pb 0.93Sr 0.02Ba 0.05(Sb 1/2Nb 1/2) 0.01(Mn 1/3Sb 2/3) 0.02(Zr 0.545Ti 0.455) 0.97O 3+0.02wt.%Fe 2O 3+0.1wt.%Sm 2O 3+0.05wt.%MnO 2+0.01wt.%Al 2O 3。
Another object of the present invention is to provide a kind of method of preparing piezoelectric ceramics of the present invention, the method comprises the steps:
Steps A) take Pb according to stoichiometric ratio 3o 4, ZrO 2, TiO 2, SrCO 3, BaCO 3, MnCO 3, Sm 2o 3, Sb 2o 3, Fe 2o 3, Nb 2o 5and Al 2o 3raw material powder, obtains ball mill mixing in 6～10 hours with wet ball grinding technique ball milling, wherein, and raw material powder: ball: the mass ratio of water is that 1:1.2～1.8:0.6～1.0 are preferably 1:1.5:0.8;
Step B) carry out briquetting after will ball mill mixing drying, then in 600 ℃～750 ℃ preferably 650 ℃ synthetic 1～4 hour preferably 2 hours, then be warming up to 800～900 ℃ preferably 850 ℃ synthetic 1～4 hour preferably 2 hours;
Step C) pulverize after use again the fine grinding of wet ball grinding technique 12～48 hours preferably 24 hours, wherein, raw material powder: ball: the mass ratio of water is that 1:1.8～2.2:0.4～0.8 is preferably 1:2:0.6, after oven dry, add the binding agent take the concentration of raw material powder weighing scale 6wt% as 9%, granulation in the preferred 150MPa compacted under of 150～200MPa, then in 800 ℃ of plastic removals 1 hour;
Step D) finally in 1260～1320 ℃ preferably 1280 ℃ be for example placed in the airtight sintering 1～3 of alumina crucible preferably 2 hours, obtain piezoceramic material.
Step C) in, described binding agent is polyvinyl chloride (PVC) binding agent.
Positive progressive effect of the present invention is: the present invention obtained a kind ofly there is lower specific inductivity, less dielectric loss is taken into account higher mechanical quality factor and the piezoceramic material of electromechanical coupling factor simultaneously, is a kind of ultrasonic fracture therapeutic equipment piezoceramic material of excellent property.The salient features of this piezoceramic material standard film is: d 33=210pC/N, ε 33 t/ ε 0=585, tan δ=0.20%, kp=0.56, kt=0.54, Qm=1210.
Embodiment
Embodiment 1
Pb 0.93sr 0.02ba 0.05(Sb 1/2nb 1/2) 0.01(Mn 1/3sb 2/3) 0.02(Zr 0.545ti 0.455) 0.97o 3+ 0.02wt.%Fe 2o 3+ 0.1wt.%Sm 2o 3+ 0.06wt.%MnO 2+ 0.01wt.%Al 2o 3piezoceramic material
First take Pb according to stoichiometric ratio 3o 4, ZrO 2, TiO 2, SrCO 3, BaCO 3, MnCO 3, Sm 2o 3, Sb 2o 3, Fe 2o 3, Nb 2o 5and Al 2o 3raw material powder, obtains ball mill mixing in 6 hours through drum ball milling by wet ball grinding technique, wherein, and raw material powder: steel ball: the mass ratio of deionized water is 1:1.5:0.8.After will ball mill mixing drying, carry out briquetting, then in 650 ℃ synthetic 2 hours, then be warming up to 850 ℃ synthetic 2 hours.After pulverizing, then use wet ball grinding technique through drum fine grinding 24 hours, wherein, raw material powder: steel ball: the mass ratio of deionized water is 1:2:0.6, adds the PVC binding agent take the concentration of raw material powder weighing scale 6wt% as 9%, granulation after oven dry, in 150MPa compacted under, then in 800 ℃ of plastic removals 1 hour.Finally be placed in the airtight sintering of alumina crucible 2 hours in 1280 ℃, obtain piezoceramic material.
Embodiment 2
Pb 0.93sr 0.02ba 0.05(Sb 1/2nb 1/2) 0.005(Mn 1/3sb 2/3) 0.015(Zr 0.545ti 0.455) 0.98o 3+ 0.02wt.%Fe 2o 3+ 0.1wt.%Sm 2o 3+ 0.06wt.%MnO 2+ 0.01wt.%Al 2o 3piezoceramic material
According to stoichiometric ratio weighing, preparation technology is with embodiment 1.
Embodiment 3
Pb 0.93sr 0.02ba 0.05(Sb 1/2nb 1/2) 0.01(Mn 1/3sb 2/3) 0.02(Zr 0.545ti 0.455) 0.97o 3+ 0.02wt.%Fe 2o 3+ 0.1wt.%Sm 2o 3+ 0.05wt.%MnO 2+ 0.01wt.%Al 2o 3piezoceramic material
According to stoichiometric ratio weighing, preparation technology is with embodiment 1.
Embodiment 4
Pb 0.93sr 0.07(Sb 1/2nb 1/2) 0.01(Mn 1/3sb 2/3) 0.02(Zr 0.545ti 0.455) 0.97o 3+ 0.02wt.%Fe 2o 3+ 0.1wt.%Sm 2o 3+ 0.05wt.%MnO 2+ 0.01wt.%Al 2o 3piezoceramic material
According to stoichiometric ratio weighing, preparation technology is with embodiment 1.
Embodiment 5
Pb 0.93ba 0.07(Sb 1/2nb 1/2) 0.01(Mn 1/3sb 2/3) 0.02(Zr 0.545ti 0.455) 0.97o 3+ 0.02wt.%Fe 2o 3+ 0.1wt.%Sm 2o 3+ 0.05wt.%MnO 2+ 0.01wt.%Al 2o 3piezoceramic material
According to stoichiometric ratio weighing, preparation technology is with embodiment 1.
Embodiment 6
Pb 0.93sr 0.02ba 0.05(Sb 1/2nb 1/2) 0.01(Mn 1/3sb 2/3) 0.02(Zr 0.60ti 0.40) 0.97o 3+ 0.02wt.%Fe 2o 3+ 0.1wt.%Sm 2o 3+ 0.05wt.%MnO 2+ 0.01wt.%Al 2o 3piezoceramic material
According to stoichiometric ratio weighing, preparation technology is with embodiment 1.
Embodiment 7
Pb 0.93sr 0.02ba 0.05(Sb 1/2nb 1/2) 0.01(Mn 1/3sb 2/3) 0.02(Zr 0.40ti 0.60) 0.97o 3+ 0.02wt.%Fe 2o 3+ 0.1wt.%Sm 2o 3+ 0.05wt.%MnO 2+ 0.01wt.%Al 2o 3piezoceramic material
According to stoichiometric ratio weighing, preparation technology is with embodiment 1.
Embodiment 8
Pb 0.93sr 0.02ba 0.05(Sb 1/2nb 1/2) 0.01(Mn 1/3sb 2/3) 0.02(Zr 0.545ti 0.455) 0.97o 3+ 0.06wt.%Fe 2o 3+ 0.1wt.%Sm 2o 3+ 0.1wt.%MnO 2+ 0.05wt.%Al 2o 3piezoceramic material
According to stoichiometric ratio weighing, preparation technology is with embodiment 1.
Embodiment 9
Pb 0.93sr 0.02ba 0.05(Sb 1/2nb 1/2) 0.01(Mn 1/3sb 2/3) 0.02(Zr 0.545ti 0.455) 0.97o 3+ 0.06wt.%Fe 2o 3+ 0.1wt.%Sm 2o 3+ 0.08wt.%MnO 2piezoceramic material
According to stoichiometric ratio weighing, preparation technology is with embodiment 1.
Raw material Pb in embodiment 3o 4, ZrO 2, TiO 2, SrCO 3, BaCO 3, MnCO 3and Sb 2o 3, be the marketable material of technical pure level, Sm 2o 3, Fe 2o 3and Al 2o 3be the marketable material of chemical pure level, Nb 2o 5for the marketable material of electronic pure level.
Performance test embodiment
The piezoceramic material that embodiment 1～9 is obtained carries out machinery according to specification requirement and is cold worked into standard film, first ultrasonic cleaning 10 minutes in gasoline and liquid detergent successively, then ultrasonic cleaning twice in water, each 10 minutes.After oven dry, put into the above silver electrode of van-type electric furnace silver ink firing, the sample that has silver electrode is placed in silicone oil at 150 ℃, apply the high-voltage electric field polarization 15min of 4kv/mm, finally carry out correlated performance test, as shown in table 1.
The performance perameter of table 1 piezoceramic material of the present invention
Figure DEST_PATH_IMAGE002

Claims (8)

1. a piezoceramic material, is characterized in that its chemical general formula is: Pb 1-xm x(Sb 1/2nb 1/2) y(Mn 1/3sb 2/3) z(Zr eti f) 1-y-zo 3+ awt.%Fe 2o 3+ bwt.%Sm 2o 3+ cwt.%MnO 2+ dwt.%Al 2o 3,
Wherein, M is Sr 2+and/or Ba 2+;
X=0.02～0.1, y=0.01～0.1, z=0.01～0.1, e=0.40～0.60, f=0.40～0.60 and meet e+f=1;
A=0～0.4, b=0～0.5, c=0～1.0, d=0～1.0 and Fe 2o 3, Sm 2o 3, MnO 2and Al 2o 3in 4 kinds of hotchpotchs, the content of a kind of hotchpotch is 0 at the most.
2. piezoceramic material as claimed in claim 1, is characterized in that: a=0.01～0.4, b=0.02～0.5, c=0.02～1.0, d=0.01～1.0.
3. piezoceramic material as claimed in claim 1, is characterized in that: M is Sr 2+and Ba 2+time, Sr 2+and Ba 2+mol ratio be 2:5.
4. piezoceramic material as claimed in claim 3, is characterized in that:
X=0.07, y=0.01～0.05, z=0.01～0.04, e=0.50～0.55, f=0.45～0.50 and e+f=1; A=0.01～0.06, b=0.02～0.2, c=0.02～0.1, d=0.01～0.05;
Preferably,
X=0.07, y=0.01～0.02, z=0.01～0.02, e=0.50～0.55, f=0.45～0.50 and e+f=1; A=0.01～0.06, b=0.02～0.1, c=0.02～0.1, d=0.01～0.05.
5. piezoceramic material as claimed in claim 3, is characterized in that: this piezoceramic material is: Pb 0.93sr 0.02ba 0.05(Sb 1/2nb 1/2) 0.01(Mn 1/3sb 2/3) 0.02(Zr 0.545ti 0.455) 0.97o 3+ 0.02wt.%Fe 2o 3+ 0.1wt.%Sm 2o 3+ 0.06wt.%MnO 2+ 0.01wt.%Al 2o 3; Pb 0.93sr 0.02ba 0.05(Sb 1/2nb 1/2) 0.005(Mn 1/3sb 2/3) 0.015(Zr 0.545ti 0.455) 0.98o 3+ 0.02wt.%Fe 2o 3+ 0.1wt.%Sm 2o 3+ 0.06wt.%MnO 2+ 0.01wt.%Al 2o 3; Or Pb 0.93sr 0.02ba 0.05(Sb 1/2nb 1/2) 0.01(Mn 1/3sb 2/3) 0.02(Zr 0.545ti 0.455) 0.97o 3+ 0.02wt.%Fe 2o 3+ 0.1wt.%Sm 2o 3+ 0.05wt.%MnO 2+ 0.01wt.%Al 2o 3.
6. prepare a method for piezoelectric ceramics as claimed in claim 1, it is characterized in that comprising the steps:
Steps A) take Pb according to stoichiometric ratio 3o 4, ZrO 2, TiO 2, SrCO 3, BaCO 3, MnCO 3, Sm 2o 3, Sb 2o 3, Fe 2o 3, Nb 2o 5and Al 2o 3raw material powder, obtains ball mill mixing in 6～10 hours with wet ball grinding technique ball milling, wherein, and raw material powder: ball: the mass ratio of water is 1:1.2～1.8:0.6～1.0;
Step B) carry out briquetting after will ball mill mixing drying, then in 600 ℃～750 ℃ synthetic 1～4 hour, then be warming up to 800～900 ℃ synthetic 1～4 hour;
Step C) use again wet ball grinding technique fine grinding 12～48 hours after pulverizing, wherein, raw material powder: ball: the mass ratio of water is 1:1.8～2.2:0.4～0.8, adds binding agent after oven dry, granulating and forming, then in 780～820 ℃ of plastic removals 0.5～1.5 hour;
Step D) finally in 1260～1320 ℃ of sintering 1～3 hour, obtain piezoceramic material.
7. method as claimed in claim 6, is characterized in that:
Steps A) in, within 6 hours, obtain ball mill mixing with wet ball grinding technique ball milling, wherein, raw material powder: ball: the mass ratio of water is 1:1.5:0.8;
Step B) carry out briquetting after will ball mill mixing drying, then in 650 ℃ synthetic 2 hours, then be warming up to 850 ℃ synthetic 2 hours;
Step C) in, after pulverizing, use again wet ball grinding technique fine grinding 24 hours, wherein, raw material powder: ball: the mass ratio of water is 1:2:0.6, after oven dry, add the binding agent take the concentration of raw material powder weighing scale 6wt% as 9%, granulation in the preferred 150MPa forming under the pressure of 150～200MPa, then in 800 ℃ of plastic removals 1 hour;
Step D) be finally placed in alumina crucible in 1280 ℃ of airtight sintering 2 hours, obtain piezoceramic material.
8. method as claimed in claim 6, is characterized in that: step C) in, described binding agent is polyvinyl chloride.
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CN115894021B (en) * 2022-12-26 2024-01-16 西安创研电子科技有限公司 High mechanical quality factor hard piezoelectric ceramic material and preparation method thereof

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