CN105272234B - It is a kind of high sensitivity in power " transmit/receive " dual-purpose type piezoceramic material and preparation method thereof - Google Patents
It is a kind of high sensitivity in power " transmit/receive " dual-purpose type piezoceramic material and preparation method thereof Download PDFInfo
- Publication number
- CN105272234B CN105272234B CN201510660685.7A CN201510660685A CN105272234B CN 105272234 B CN105272234 B CN 105272234B CN 201510660685 A CN201510660685 A CN 201510660685A CN 105272234 B CN105272234 B CN 105272234B
- Authority
- CN
- China
- Prior art keywords
- dual
- purpose type
- high sensitivity
- power
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention relates to power in a kind of high sensitivity " to transmit/receive " dual-purpose type piezoceramic material and preparation method thereof, belongs to piezoelectric ceramic technology field.Composition formula of the invention are as follows: x Pb (Mg1/3Nb2/3)03‑yPb(Mn1/3Nb2/3)03‑z Pb(ZrmTi1‑m)03；Wherein: 0.01≤x≤0.08；0.01≤y≤0.08；0.8 < z < 1.0；X+y+z=1；0.45≤m≤0.55.The present invention has the advantages that permittivity ε can be obtained using material prescription and preparation process of the inventionT 33520 ± 12.5%, planar electromechanical coupling factor Kp:0.53 ± 6.0%, mechanic quality factor >=500, d33=212 ± 12.5%pC/N, g33=46.7mVm/N, d33·g33: (9900 ± 3.0%) × 10‑15C·V·m/N2, the piezoceramic material of Poisson ratioσ=0.28.Material of the present invention has high sensitivity (g33=46.7) the features such as, dielectric constant is low and middle power (Qm >=500) is that a kind of function admirable " transmits/receives " dual-purpose type piezoceramic material.
Description
Technical field
The invention belongs to piezoelectric ceramic technology field, power " transmits/receives " dual-purpose type piezoelectricity in mainly a kind of high sensitivity
Ceramic material and preparation method thereof.
Background technique
Ultrasonic measurement occupies considerable status in the industrial production, especially in electric power, chemical industry, petroleum, coal etc.
Industry has a wide range of applications.Since the raw material of industry is often volatile, deep-etching, virose substance, traditional contact
Although measurement is easy to operate, often because the problems such as viscous connection, corrosion influences the accuracy measured, ultrasonic measurement is as a kind of typical case
Highest attention of the non-cpntact measurement by industry；
Energy converter is the critical component of ultrasonic measurement, it is responsible for the transmitting of ultrasound and receives task, can by application type
To be divided into emission type, reception type and transmit/receive dual-purpose type；Wherein transmit/receive dual-purpose type can realize automatically mechanical energy and electric energy it
Between mutually convert, have transmitting, receive signal in one particular attribute, can preferably meet market for ultrasonic measurement
Intelligent, miniaturization application demand；
In transceiver type energy converter, core component piezoelectric ceramics will bear high within the fire pulse width time
Driving voltage will be damped to generate enough sound source levels, after transmitting within several milliseconds of times to close to stationary state, prepare to ring
It answers reflected faint sound wave and it is converted into electric signal, it is desirable to which electricity-sound, sound-photoelectric transformation efficiency are relatively high, this is just
It is required that the piezoelectric strain coefficient d of active component piezoelectric ceramics33And piezoelectric voltage coefficient g33Want high, while its product d33·g33?
It wants high, and there is high mechanic quality factor and low Poisson ratioσE；The transmitting-receiving two of major part producer and scientific research institution at present
PZT4 the or PZT5 series material for using Traditional dopant to obtain with type energy converter；PZT4 material mechanical quality factor q m high,
Transmission power is high, but piezoelectric strain coefficient d33It is low；PZT5 material piezoelectric strain coefficient d33Height, but mechanic quality factor is low, hair
Penetrate that power is low, above two material cannot meet the performance need for transmitting/receiving dual-purpose type energy converter to piezoceramic material well
Ask, thus develop it is a kind of receive hair dual-purpose type piezoceramic material seem particularly necessary.
Summary of the invention
The object of the invention is in order to overcome above-mentioned problems of the prior art, and provide in a kind of high sensitivity
Power " transmits/receives " dual-purpose type piezoceramic material and preparation method thereof, in terms of being mainly used in ultrasonic measurement.
The object of the present invention is achieved by the following technical solutions.The present invention is directed to by drawing in PZT binary system
Enter Pb (Mn1/3Nb2/3)03、Pb(Mg1/3Nb2/3)03、Fe203Or Ce02It is doped substituting modification and adjustment Zr/Ti ratio, for ultrasound
Measurement provide it is a kind of high sensitivity in power " transmit/receive " dual-purpose type piezoceramic material and preparation method thereof.This high sensitivity
Middle power " transmits/receives " dual-purpose type piezoceramic material, composition formula are as follows: xPb (Mg1/3Nb2/3)03-yPb(Mn1/3Nb2/3)03-zPb
(ZrmTi1-m)03；Wherein: 0.01≤x≤0.08；0.01≤y≤0.08；0.8 < z < 1.0；X+y+z=1；0.45≤m≤
0.55。
The material composition are as follows: Pb (Mg1/3Nb2/3)0.03(Mn1/3Nb2/3)0.04(Ti0.49Zr0.51)0.9303。
The material composition are as follows: Pb (Mg1/3Nb2/3)0.03(Mn1/3Nb2/3)0.05(Ti0.485Zr0.515)0.9203。
The material composition are as follows: Pb (Mg1/3Nb2/3)0.03(Mn1/3Nb2/3)0.06(Ti0.48Zr0.52)0.9103。
The material composition, also can further include one of following substance: accounting for bulk composition weight ratio 0.1wt%
Fe203Or 0.2wt%Ce02。
Power " transmits/receives " dual-purpose type piezoceramic material and preparation method thereof in this high sensitivity of the present invention,
Processing step is as follows:
Step 1, ingredient: with Pb304、Zr02、Ti02、Nb205、Mg0、Mn02For raw material, by xPb (Mg1/3Nb2/3)03-yPb
(Mn1/3Nb2/3)03-zPb(ZrmTi1-m)03；Proportion weighed, in which: 0.01≤x≤0.08；0.01≤y≤0.08；
0.8 < z < 1.0；X+y+z=1；0.45≤m≤0.55；It is small that above-mentioned raw materials are placed in wet ball grinding mixing 15-25 in ball grinder
When after pulp dry；
Step 2, synthesis: Al will be put into after the powder briquetting after step 1 drying203It is small in 650 DEG C of heat preservation 1-2 in crucible
When, 800~900 DEG C of heat preservations are synthesized for 2-3 hours；
Step 3, molding and plastic removal: after the synthetic material block coarse crushing of step 2, through wet ball grinding 30-50 hours, after drying
Weight percent is added as the granulation of 3~7% polyvinyl alcohol adhesives, polyvinyl alcohol adhesive is to dry powder after wet ball grinding
On the basis of weight, 25 × 2.5~2.8mm of Φ green body is made by the uniaxial method of forming；Green body after molding is at 750~850 DEG C
Keep the temperature 2-5 hours plastic removals；
Step 4, sintering: the green body after step 3 plastic removal is placed in Al203On load bearing board, Al is used203Crucible covers green body, shape
At closed environment, then it is sintered within heat preservation 2-3 hours in oxidizing atmosphere in 1230~1280 DEG C；
Step 5, machining: the piezoelectric ceramics porcelain piece that step 4 sinters is ground to 20 × 1mm of Φ；
Step 6, top electrode: being printed electrode using silk-screen printing technique in piezoelectric ceramics porcelain piece upper and lower surfaces, electrode drying
It is placed in heating furnace, is warming up to 750 DEG C and keeps the temperature 30 minutes, cooled to room temperature completes top electrode process；
Step 7, polarization: the top electrode product of step 6 is placed in 150~160 DEG C of silicone oil, applies 2.5~3.0kv/
The DC electric field of mm, polarizes；
Step 8, measurement: its piezoelectric property is tested after the piezoelectric element of step 7 is placed 5~7 days at room temperature；Using electric bridge
Method measures free capacitance CTAnd Loss tangent；Resonance frequency f is measured using resonance-antiresonance methodr, anti-resonance frequency faWith it is general
Sound resonant frequency fr1；By tabling look-up and calculating finds out electromechanical coupling factor kp, permittivity εT 33And mechanic quality factor；Benefit
D is measured with quasi-static method33And then calculate g33；Utilize resonance frequency frWith overtone resonant frequency fr1Calculate the Poisson ratioσ of materialE。
Further, ingredient in step 1: with Pb304、Zr02、Ti02、Nb205、Mg0、Mn02For raw material, by xPb
(Mg1/3Nb2/3)03-yPb(Mn1/3Nb2/3)03-zPb(ZrmTi1-m)03；Proportion weighed, in which: 0.01≤x≤0.08；
0.01≤y≤0.08；0.8 < z < 1.0；X+y+z=1；0.45≤m≤0.55；It weighs simultaneously and accounts for bulk composition weight ratio
0.1wt%Fe203Or 0.2wt%Ce02, above-mentioned raw materials are placed in ball grinder pulp after wet ball grinding mixing 15-25 hours and are dried
It is dry.
Further, raw material when wet ball grinding: agate ball: water weight ratio is 1:1:0.5~0.6.
Further, heating rate when plastic removal is 1~1.5 DEG C/min.
The invention has the benefit that permittivity ε can be obtained using material prescription and preparation process of the inventionT 33
520 ± 12.5%, planar electromechanical coupling factor Kp:0.53 ± 6.0%, mechanic quality factor >=500, d33=212 ±
12.5%pC/N, g33=46.7mVm/N, d33·g33: (9900 ± 3.0%) × 10-15C·V·m/N2, Poisson ratioσ=
0.28 piezoceramic material.Material of the present invention has high sensitivity (g33=46.7), dielectric constant is low and middle power (Qm >=
500) the features such as is that a kind of function admirable " transmits/receives " dual-purpose type piezoceramic material.
Specific embodiment
The present invention will be described in more detail based on actual embodiment below, but the content invented is not limited to
This.
Power " transmits/receives " dual-purpose type piezoceramic material, composition formula in this high sensitivity of the present invention are as follows: xPb
(Mg1/3Nb2/3)03-yPb(Mn1/3Nb2/3)03-zPb(ZrmTi1-m)03；Wherein: 0.01≤x≤0.08；0.01≤y≤0.08；
0.8 < z < 1.0；X+y+z=1；0.45≤m≤0.55；
The material composition are as follows: Pb (Mg1/3Nb2/3)0.03(Mn1/3Nb2/3)0.04(Ti0.49Zr0.51)0.9303
The material composition are as follows: Pb (Mg1/3Nb2/3)0.03(Mn1/3Nb2/3)0.05(Ti0.485Zr0.515)0.9203
The material composition are as follows: Pb (Mg1/3Nb2/3)0.03(Mn1/3Nb2/3)0.06(Ti0.48Zr0.52)0.9103
The material composition, also can further include one of following substance: 0.1wt%Fe203Or 0.2wt%
Ce02。
Embodiment 1:
With Pb304、Zr02、Ti02、Nb205、Mg0、Mn02For raw material, by Pb (Mg1/3Nb2/3)0.03(Mn1/3Nb2/3)0.04
(Ti0.49Zr0.51)0.9303Proportion calculated；
Preparation method the following steps are included:
Step 1: ingredient
With Pb304、Zr02、Ti02、Nb205、Mg0、Mn02For raw material, by Pb (Mg1/3Nb2/3)0.03(Mn1/3Nb2/3)0.04
(Ti0.49Zr0.51)0.9303Proportion carry out weighing ingredient, it is small that above-mentioned raw materials are placed in wet ball grinding mixing 15-25 in ball grinder
When after pulp dry；
Step 2: synthesis
Al will be put into after powder briquetting after step 1 drying203In crucible, 650 DEG C heat preservation 1-2 hours, 800~900 DEG C
Heat preservation is synthesized for 2-3 hours；
Step 3: molding and plastic removal
After the synthetic material block coarse crushing of step 2, it is 3 that weight percent is added through wet ball grinding 30-50 hours, after drying
~7% polyvinyl alcohol adhesive is granulated, and polyvinyl alcohol adhesive is passed through on the basis of drying powder weight after wet ball grinding
25 × 2.5~2.8mm of Φ green body is made in the uniaxial method of forming；Green body after molding is in 2-5 hours dumpings of 750~850 DEG C of heat preservations；
Step 4: sintering
Green body after step 3 plastic removal is placed in Al203On load bearing board, Al is used203Crucible covers green body, forms closed environment,
Then it is sintered within heat preservation 2-3 hours in oxidizing atmosphere in 1230~1280 DEG C；
Step 5: machining
The piezoelectric ceramics porcelain piece grinding that step 4 is sintered is to 20 × 1mm of Φ；
Step 6: top electrode
It is printed electrode using silk-screen printing technique in piezoelectric ceramics porcelain piece upper and lower surfaces, electrode drying is placed on heating furnace
In, it is warming up to 750 DEG C and keeps the temperature 30 minutes, cooled to room temperature completes top electrode process；
Step 7: polarization
The top electrode product of step 6 is placed in 150~160 DEG C of silicone oil, the direct current of 2.5~3.0kv/mm is applied
, it polarizes；
Step 8: measurement
Its piezoelectric property is tested after the piezoelectric element of step 7 is placed 5~7 days at room temperature；Using bridge measurement freedom
Capacitor CTAnd Loss tangent；Resonance frequency f is measured using resonance-antiresonance methodr, anti-resonance frequency faWith overtone resonant frequency
fr1；By tabling look-up and calculating finds out electromechanical coupling factor kp, permittivity εT 33And mechanic quality factor；Utilize quasi-static method
Measure d33And then calculate g33；Utilize resonance frequency frWith overtone resonant frequency fr1Calculate the Poisson ratioσ of materialE。
Embodiment 2:
With Pb304、Zr02、Ti02、Nb205、Mg0、Mn02For raw material, by Pb (Mg1/3Nb2/3)0.03(Mn1/3Nb2/3)0.05
(Ti0.485Zr0.515)0.9203Proportion calculated；
Preparation method specifically comprises the following steps: (1) ingredient with embodiment one；(2) it synthesizes；(3) molding and plastic removal；(4)
Sintering；(5) it machines；(6) top electrode；(7) it polarizes；(8) it measures.
Embodiment 3:
With Pb304、Zr02、Ti02、Nb205、Mg0、Mn02For raw material, by Pb (Mg1/3Nb2/3)0.03(Mn1/3Nb2/3)0.06
(Ti0.48Zr0.52)0.9103Proportion calculated；Preparation method specifically comprises the following steps: (1) ingredient with embodiment one；
(2) it synthesizes；(3) molding and plastic removal；(4) it is sintered；(5) it machines；(6) top electrode；(7) it polarizes；(8) it measures.
Embodiment 4:
With Pb304、Zr02、Ti02、Nb205、Mg0、Mn02、Fe203For raw material, by Pb (Mg1/3Nb2/3)0.03(Mn1/ 3Nb2/3)0.05(Ti0.485Zr0.515)0.9203+ 0.1wt%Fe203Proportion calculated；Preparation method is with embodiment one, specifically
Include the following steps: (1) ingredient；(2) it synthesizes；(3) molding and plastic removal；(4) it is sintered；(5) it machines；(6) top electrode；(7) pole
Change；(8) it measures.
Embodiment 5:
With Pb304、Zr02、Ti02、Nb205、Mg0、Mn02、Ce02For raw material, by Pb (Mg1/3Nb2/3)0.03(Mn1/ 3Nb2/3)0.05(Ti0.485Zr0.515)0.9203+ 0.2wt%Ce02Proportion calculated；Preparation method is specific to wrap with embodiment one
Include following steps: (1) ingredient；(2) it synthesizes；(3) molding and plastic removal；(4) it is sintered；(5) it machines；(6) top electrode；(7) it polarizes；
(8) it measures.
The ceramic material that above-described embodiment is prepared is tested for the property, and piezoelectric property is as shown in table 1 below:
Table 1,20 × 1 element piezoelectric property situation table of Φ
The performance parameter of piezoceramic material performance and the prior art of the invention is compared as follows shown in table 2:
Table 2, the present invention are compared with the prior art
Certainly, the invention may also have other embodiments, and those skilled in the art can make according to the present invention
Various corresponding changes and modifications, but these corresponding changes and modifications all should belong to the protection of appended claims of the invention
Range.
Claims (2)
1. power " transmits/receives " dual-purpose type piezoceramic material in a kind of high sensitivity, it is characterised in that: the material composition
Are as follows: Pb (Mg1/3Nb2/3)0.03 (Mn1/3Nb2/3)0.04(Ti0.49Zr0.51)0.9303,
Or the material composition are as follows: Pb (Mg1/3Nb2/3)0.03 (Mn1/3Nb2/3)0.05(Ti0.485Zr0.515)0.9203,
Or the material composition are as follows: Pb (Mg1/3Nb2/3)0.03 (Mn1/3Nb2/3)0.06(Ti0.48Zr0.52)0.9103 。
2. power " transmits/receives " dual-purpose type piezoceramic material in a kind of high sensitivity, it is characterised in that: the material is by main body
Ingredient and the Fe for accounting for 0.1 wt% of bulk composition203Or 0.2 wt% Ce02Composition；
The material of the bulk composition forms are as follows: Pb (Mg1/3Nb2/3)0.03 (Mn1/3Nb2/3)0.04(Ti0.49Zr0.51)0.9303,
Or are as follows: Pb (Mg1/3Nb2/3)0.03 (Mn1/3Nb2/3)0.05(Ti0.485Zr0.515)0.9203,
Or are as follows: Pb (Mg1/3Nb2/3)0.03 (Mn1/3Nb2/3)0.06(Ti0.48Zr0.52)0.9103。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510660685.7A CN105272234B (en) | 2015-10-14 | 2015-10-14 | It is a kind of high sensitivity in power " transmit/receive " dual-purpose type piezoceramic material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510660685.7A CN105272234B (en) | 2015-10-14 | 2015-10-14 | It is a kind of high sensitivity in power " transmit/receive " dual-purpose type piezoceramic material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105272234A CN105272234A (en) | 2016-01-27 |
| CN105272234B true CN105272234B (en) | 2019-01-08 |
Family
ID=55142155
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510660685.7A Active CN105272234B (en) | 2015-10-14 | 2015-10-14 | It is a kind of high sensitivity in power " transmit/receive " dual-purpose type piezoceramic material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105272234B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105801129B (en) * | 2016-03-04 | 2019-01-15 | 森霸传感科技股份有限公司 | The sintering modified additive of pyroelectric ceramic material |
| JP6683029B2 (en) * | 2016-06-20 | 2020-04-15 | コニカミノルタ株式会社 | Piezoelectric element, ultrasonic probe, and ultrasonic imaging device |
| CN114133243A (en) * | 2021-12-17 | 2022-03-04 | 中国船舶重工集团公司第七一五研究所 | High-dielectric-constant high-voltage electric strain emission type piezoelectric ceramic material and preparation method thereof |
| CN114804866A (en) * | 2022-04-29 | 2022-07-29 | 杭州瑞声海洋仪器有限公司 | High-sensitivity high-Curie-temperature piezoelectric ceramic material and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603294A (en) * | 2012-03-23 | 2012-07-25 | 天津大学 | Method for preparing high-performance lanthanum-doped lead zinc niobate and lead zirconate titanate piezoelectric ceramic under condition with excessive lead |
| CN102795854B (en) * | 2012-08-28 | 2013-12-11 | 中国船舶重工集团公司第七一五研究所 | High-power density piezoceramic material and method for preparing same |
-
2015
- 2015-10-14 CN CN201510660685.7A patent/CN105272234B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN105272234A (en) | 2016-01-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Stevenson et al. | Piezoelectric materials for high temperature transducers and actuators | |
| Yan et al. | Composition-driven phase boundary and its energy harvesting performance of BCZT lead–free piezoelectric ceramic | |
| CN105272234B (en) | It is a kind of high sensitivity in power " transmit/receive " dual-purpose type piezoceramic material and preparation method thereof | |
| CN111302797B (en) | Potassium-sodium niobate-based leadless piezoelectric ceramic and preparation method thereof | |
| US7352113B2 (en) | Piezoelectric actuator | |
| Islam et al. | High‐Energy Density Ceramic Composition in the System Pb (Zr, Ti) O3–Pb [(Zn, Ni) 1/3Nb2/3] O3 | |
| CN105884350B (en) | A kind of barium calcium zirconate titanate lead-free piezoceramic material and preparation method thereof | |
| JP2006105964A (en) | Piezoelectric sensor | |
| Wang et al. | Modified Pb (Mg1/3Nb2/3) O3‐PbZrO3–PbTiO3 ceramics with high piezoelectricity and temperature stability | |
| CN104844202B (en) | Lead manganous antimonate doped niobium nickel-lead zirconate titanate piezoelectric ceramic | |
| Yan et al. | High energy conversion efficiency in Mn‐modified Ba0. 9Ca0. 1Ti0. 93Zr0. 07O3 lead‐free energy harvester | |
| US8231803B2 (en) | Piezoelectric ceramic and piezoelectric ceramic composition | |
| CN114133243A (en) | High-dielectric-constant high-voltage electric strain emission type piezoelectric ceramic material and preparation method thereof | |
| CN104230333A (en) | High-temperature piezoelectric ceramic material and preparation method thereof | |
| Bahanurddin et al. | Effects of CIP compaction pressure on piezoelectric properties of K 0.5 Na 0.5 NbO 3 | |
| CN107056281B (en) | High-strain sodium bismuth titanate-based ceramic and preparation method thereof | |
| CN107117964B (en) | A kind of PZT piezoelectric ceramics and preparation method thereof of different temperatures Preburning material mixing | |
| Kim et al. | Piezoelectric properties of (Na1− xKx) NbO3‐based lead‐free piezoelectric ceramics and their application in knocking sensor | |
| CN104557038A (en) | Composite pyroelectric ceramic material and preparation method thereof | |
| JP2009012997A (en) | Unleaded piezoelectric porcelain composition | |
| WO2006093002A1 (en) | Piezoelectric porcelain composition | |
| Zeng et al. | Correlation between temperature-dependent permittivity dispersion and depolarization behaviours in Zr 4+-modified BiFeO 3–BaTiO 3 piezoelectric ceramics | |
| RU2453518C2 (en) | Piezoceramic material | |
| KR101239275B1 (en) | Low temperature sintering piezoelectric ceramic composition, manufacturing method thereof, and piezoelectric ceramic device using the same ceramic composition | |
| CN103787656A (en) | High-sensitivity piezoelectric ceramic piece formula and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |