CN1260175C - Doped lead antimony manganese zirconia titanate piezoelectric ceramic materials suitable for industrial production and method for preparing same - Google Patents
Doped lead antimony manganese zirconia titanate piezoelectric ceramic materials suitable for industrial production and method for preparing same Download PDFInfo
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- CN1260175C CN1260175C CN200310109138.7A CN200310109138A CN1260175C CN 1260175 C CN1260175 C CN 1260175C CN 200310109138 A CN200310109138 A CN 200310109138A CN 1260175 C CN1260175 C CN 1260175C
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- piezoelectric ceramic
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- ceramic materials
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- piezoelectric
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 17
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 8
- OOBNORVQFIAGPT-UHFFFAOYSA-N antimony manganese Chemical compound [Mn].[Sb] OOBNORVQFIAGPT-UHFFFAOYSA-N 0.000 title claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 229910010293 ceramic material Inorganic materials 0.000 title abstract description 7
- 238000009776 industrial production Methods 0.000 title description 3
- 239000000463 material Substances 0.000 claims abstract description 34
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 239000000126 substance Substances 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims description 11
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 10
- 239000011572 manganese Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 4
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 claims description 3
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims 1
- 230000002194 synthesizing effect Effects 0.000 claims 1
- 239000000919 ceramic Substances 0.000 abstract description 12
- 230000008878 coupling Effects 0.000 abstract description 3
- 238000010168 coupling process Methods 0.000 abstract description 3
- 238000005859 coupling reaction Methods 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 abstract 1
- 230000000996 additive effect Effects 0.000 abstract 1
- 229910000420 cerium oxide Inorganic materials 0.000 abstract 1
- 229910000423 chromium oxide Inorganic materials 0.000 abstract 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 abstract 1
- 229910052814 silicon oxide Inorganic materials 0.000 abstract 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 238000010344 co-firing Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000009766 low-temperature sintering Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910020203 CeO Inorganic materials 0.000 description 1
- 229910016287 MxOy Inorganic materials 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- HWHWBMBTCNLBGY-UHFFFAOYSA-N [Pb].[Ni].[Nb] Chemical compound [Pb].[Ni].[Nb] HWHWBMBTCNLBGY-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention relates to doped lead antimony manganese zirconia titanate group piezoelectric ceramic materials which belong to the field of piezoelectric materials. Additive substances such as silicon oxide, cerium oxide and chromium oxide are added to piezoelectric ceramic materials on the basis of lead antimony manganese zirconia titanate (PMS-PZT), and the sintering temperature is from 1100 to 1200 DEG C. Under the condition that the piezoelectric properties such as electromechanical coupling coefficients Kp, mechanical quality factors Qm, etc. are not lowered, the piezoelectric ceramic materials simultaneously have high mechanical strength. The piezoelectric ceramic materials are especially suitable for high-power piezoelectric ceramic devices and multilayer cofired piezoelectric ceramic devices using Ag/Pd as electrodes.
Description
Technical field
The present invention relates to doped lead antimony manganese zirconia titanate piezoceramic material of a kind of suitable suitability for industrialized production and preparation method thereof, belong to the piezoceramic material field.
Background technology
The PZT pottery is one of present the most widely used commercial electronic material.In recent years, application development at the high-power aspects of using down such as piezoelectric ceramic actuator, transformer, micro positioner, motor and various ultrasonic transducers is very rapid, this just requires piezoceramic material can export bigger power under free state or tension stress, has high electromechanical coupling factor K
p, the mechanical quality factor Q
m, piezoelectric constant d
33And low dielectric loss Tan δ, should possess high physical strength and time, temperature stability simultaneously.
The sintering temperature of leaded PZT pottery is generally 1200-1300 ℃ and since sintering temperature when too high lead volatile, cause the nonstoichiometry ratio, cause ceramic performance to be difficult to control; And plumbous volatilization causes environmental pollution, healthy very harmful to the mankind.Widely used in recent years piezoceramic multilayer device (as piezoelectric actuator, piezoelectric transformer etc.) because its sintering temperature height all uses precious metals such as platinum, palladium as interior electrode usually, has improved use cost greatly.Therefore, at the piezoelectric property that does not reduce material (high K
p, Q
m, ε
33 T) and the situation of physical strength under, by mixing or modification reduces the sintering temperature of high power piezoelectric ceramic material, to the preparation of material and use particularly that the application of multilayer co-firing piezoelectric ceramic devices has very important significance.
Clear 42-25276 of Japanese Patent and 42-66779 have introduced the Pb (Mn that different ingredients is formed
1/3Sb
2/3) O
3-PbTiO
3-PbZrO
3The piezoelectric property of stupalith, but its sintering temperature is all between 1200-1300 ℃, and this is restricted their application in the multilayer co-firing piezoelectric ceramic devices.
Guo Xiaobo, Meng Zhongyan etc. (silicate journal 200230 (1) 125-127) have studied Pb
1-xSr
x(Mn
1/3Sb
2/3)
aZr
bTi
cO
3The piezoelectric property of material, this material is piezoelectric property the best when 1200 ℃ of sintering, but when temperature when being lower than this temperature, K
p, Q
m, ε
33 TDescend significantly Deng all having, wherein Q
mValue has only 850 when burning till for 1150 ℃.It is narrow and unstable that this material can satisfy the sintering range of performance requriements, and significant discomfort is used for the application of suitability for industrialized production.In addition, because its sintering temperature is higher relatively, need to use the very high even interior electrode of precious metal 100% of Pd.
Chinese patent 85100051 reported in the PZT two component system and to have added B-Bi-Cd low-melting-point glass material, develops 960-1000 ℃ of following low-temperature sintering and has the material of good piezoelectric property.Chinese patent 86108741 has reported that niobium nickel lead zirconate titanate piezoelectric material adds SiO
2, MnO
2And excessive PbO, sintering temperature can be reduced to 840-1000 ℃, and has good piezoelectric property.Above two China patent report under the prerequisite that does not reduce piezoelectric property, can reduce the sintering temperature of stupalith, but the mechanical quality factor of these materials has only 800-1000, and does not illustrate and reduce the influence of ceramic sintering temperature ceramic machinery intensity.
For high power piezoelectric ceramic material, its amplitude when the resonance working order is bigger, must have high physical strength.Therefore, how when reducing the stupalith sintering temperature, take into account piezoelectric property, machinery and electrical losses and the physical strength of material, just become a great problem anxious to be solved.
Summary of the invention
The object of the present invention is to provide a kind of piezoceramic material with middle low temperature (1100-1200 ℃) sintering characteristic, this material has higher piezoelectric constant d
33, electromechanical coupling factor K
p, the mechanical quality factor Q
m, DIELECTRIC CONSTANT
33 T, and physical strength, can use at the high-power piezoelectric ceramic device and in the piezoceramic multilayer common burning porcelain device of Ag/Pd as interior electrode.
Specifically, low temperature sintering piezoelectric ceramics provided by the invention consists of
Pb
1-aSr
a(Mn
1/3Sb
2/3)
bZr
cTi
dO
3+Nwt％M
xO
y，
Wherein: 0≤a≤0.1,0＜b≤0.1,0.4≤c≤0.5,0.4≤d≤0.5,0.01≤N≤1, b+c+d=1.This doping oxide MxOy is SiO
2, CeO
2, Cr
2O
3In a kind of, two or three, the material after the doping still keeps cubic phase perovskite structure.
Preparation technology of the present invention is with chemical pure Pb
3O
4, SrCO
3, MnCO
3, Sb
2O
3, ZrO
2, TiO
2, SiO
2, Cr
2O
3, CeO
2Be raw material,, mix back ball milling, drying, 850-900 ℃ of pre-synthetic 1-2h according to the accurate weighing of stoichiometric.Pulverize the back fine grinding, the fineness of powder is at 0.5-1 μ m.The oven dry back adds 5-10%PVA as binding agent, granulation, at 1-2T/cm
2Pressure under dry-pressing formed be the rectangular of the disk of φ 12 * 1mm and 36 * 4 * 3mm.The plastic removal temperature is 800-850 ℃, insulation 1-2h.Sintering temperature is 1100-1200 ℃, insulation 1-2h.Disk is machined to 0.5mm, cleans the two-sided silver electrode that plates in back, and the 20-30min that polarizes in 130 ℃ silicone oil, polarized electric field are 2.5-3.5KV/mm.Polarized sample is tested every performance after placing 24h.Rectangularly be used for doing bending strength test.
The characteristics of this piezoceramic material are:
1. material can use 70Ag/30Pd even lower Pd ratio as interior electrode at densified sintering product under the lower temperature (1100-1200 ℃), greatly reduces cost; And the material property of sintering preparation is stable in this temperature range, can overcome temperature deviation to effect of material performance, is fit to very much need of industrial production.
2. material has good piezoelectric property: d
33=300-400PC/N, K
p=0.5-0.6, Q
m=1500-1800,
Tanδ≤0.5％；
3. the mechanical property of material satisfies the actual needs that use: bending strength is at 70-110MPa.
4. be applicable to the sintering range of broad, performance index difference is less behind 1100-1200 ℃ of following sintering, can satisfy the actual needs of suitability for industrialized production.
Description of drawings
Fig. 1 is the piezoceramic material typical X RD collection of illustrative plates that the present invention proposes, and as can be seen from the figure, the material after the doping still keeps cubic phase perovskite structure.
Embodiment
Further set forth characteristics of the present invention below by embodiment, but content of the present invention is not limited thereto.
Embodiment 1
With Pb
3O
4, SrCO
3, MnCO
3, Sb
2O
3, ZrO
2, TiO
2, SiO
2, CeO
2, (chemical pure) be raw material, presses Pb
0.95Sr
0.05(Mn
1/3Sb
2/3)
0.03Zr
0.50Ti
0.47O
3+ 0.2wt%SiO
2+ 0.5wt%CeO
2The stoichiometry weighing, adopt general ceramic preparation technology to prepare burden, synthetic in advance after ball milling, mixing, the oven dry (850 ℃/2h), fine grinding 10h, drying, adding additives, moulding (forming pressure 2T/cm
2), plastic removal (850 ℃/1h), sintering (1100-1200 ℃/2h).Form the as above piezoceramic material of the cubic phase perovskite structure of prescription.
Table 1 is embodiment 1 piezoelectric property of (1100-1200 ℃) under differing temps.
Table 1
| Sintering temperature (℃) | K p | Q m | d 33 (PC/N) | ε 33 T | tanδ(％) | ρ (g/cm 3) |
| 1100 | 0.535 | 1756 | 310 | 1122 | 0.7 | 7.49 |
| 1120 | 0.548 | 1704 | 318 | 1183 | 0.7 | 7.52 |
| 1140 | 0.550 | 1635 | 326 | 1271 | 0.5 | 7.65 |
| 1160 | 0.567 | 1605 | 339 | 1320 | 0.5 | 7.72 |
| 1180 | 0.581 | 1548 | 356 | 1375 | 0.4 | 7.81 |
| 1200 | 0.596 | 1497 | 364 | 1406 | 0.4 | 7.89 |
Embodiment 2
By prescription Pb
0.975r
0.03(Mn
1/3Sb
2/3)
0.05Zr
0.48Ti
047O
3+ 0.2wt%SiO
2+ 0.6wt%CeO
2+ 0.5wt%Cr
2O
3Accurate proportioning, preparation technology is with embodiment 1, and sintering temperature is 1140 ℃, and its piezoelectric property is:
K
p＝0.576、Q
m＝1750、d
33＝341PC/N、tanδ＝0.7％。
Embodiment 3
By prescription Pb
0.99Sr
0.01(Mn
1/3Sb
2/3)
0.08Zr
0.46Ti
0.46O
3+ 0.8wt%SiO
2+ 0.5wt%CeO
2+ 0.6wt%Cr
2O
3Accurate proportioning, preparation technology is with embodiment 1, and sintering temperature is 1140 ℃, and its piezoelectric property is:
K
p＝0.568、Q
m＝1678、d
33＝352PC/N、tanδ＝0.4％。
Table 2 is the piezoelectric property of embodiment 1-3 and the comparison of mechanical property.
Table 2
| K p | Q m | d 33 (PC/N) | ε 33 T | tanδ (％) | Bending strength (MPa) | |
| Embodiment 1 | 0.550 | 1635 | 326 | 1271 | 0.5 | 86 |
| Embodiment 2 | 0.576 | 1750 | 341 | 1356 | 0.7 | 94 |
| Embodiment 3 | 0.568 | 1678 | 352 | 1324 | 0.4 | 103 |
(sintering temperature is 1140 ℃, insulation 2h)
As can be seen, (1100-1200 ℃) can both sintering in quite wide firing temperature for material, and has piezoelectricity and mechanical property preferably from table 1, table 2.Illustrating that this material can adapt in high-power piezoelectric ceramic device and piezoceramic multilayer common burning porcelain device uses, and is very suitable for industrial production.
Claims (4)
1, the doped lead antimony manganese zirconia titanate piezoceramic material that is fit to suitability for industrialized production is characterized in that the Pb that consists of of material
1-aSr
a(Mn
1/3Sb
2/3)
bZr
cTi
dO
3+ N wt%M
xO
y, wherein: 0≤a≤0.1,0＜b≤0.1,0.4≤c≤0.5,0.4≤d≤0.5,0.01≤N≤1, b+c+d=1, M
xO
yBe SiO
2, CeO
2, Cr
2O
3In a kind of, two or three.
2, by the preparation method of the doped lead antimony manganese zirconia titanate piezoceramic material of the described suitable suitability for industrialized production of claim 1, comprise batching, mixings, synthesize in advance, moulding, sintering, it is characterized in that:
(1) presses Pb
1-aSr
a(Mn
1/3Sb
2/3)
bZr
cTi
dO
3+ N wt%M
xO
yThe proportioning raw material, wherein: 0≤a≤0.1,0＜b≤0.1,0.4≤c≤0.5,0.4≤d≤0.5,0.01≤N≤1, b+c+d=1, M
xO
yBe SiO
2, CeO
2, Cr
2O
3In a kind of, two or three;
(2) raw material that uses is Pb
3O
4, SrCO
3, MnCO
3, Sb
2O
3, ZrO
2, TiO
2, SiO
2, Cr
2O
3, CeO
2
(3) sintering temperature is 1100-1200 ℃, insulation 1-2h.
3, press the preparation method of the doped lead antimony manganese zirconia titanate piezoceramic material of the described suitable suitability for industrialized production of claim 2, fine grinding after the raw material pulverizing after it is characterized in that synthesizing in advance, the fineness of powder is controlled at 0.5-1 μ m.
4, press the preparation method of the doped lead antimony manganese zirconia titanate piezoceramic material of the described suitable suitability for industrialized production of claim 2, it is characterized in that used raw material is a chemical pure.
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|---|---|---|---|
| CN200310109138.7A CN1260175C (en) | 2003-12-05 | 2003-12-05 | Doped lead antimony manganese zirconia titanate piezoelectric ceramic materials suitable for industrial production and method for preparing same |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200310109138.7A CN1260175C (en) | 2003-12-05 | 2003-12-05 | Doped lead antimony manganese zirconia titanate piezoelectric ceramic materials suitable for industrial production and method for preparing same |
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| CN1260175C true CN1260175C (en) | 2006-06-21 |
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| US7494602B2 (en) * | 2005-04-11 | 2009-02-24 | Piezotech, Llc | Compositions for high power piezoelectric ceramics |
| CN100422110C (en) * | 2007-04-26 | 2008-10-01 | 浙江大学 | Seepage type Ag-PbTiO3 composite ceramic film and preparation method therefor |
| CN101767994B (en) * | 2010-01-18 | 2012-05-09 | 哈尔滨理工大学 | Method for preparing modified lead zirconate titanate (PZT) piezoelectric ceramics powder |
| CN102260079B (en) * | 2010-05-31 | 2013-10-02 | 中国科学院上海硅酸盐研究所 | PZT-Pb (Sb2/3Mn1/3) ternary system piezoelectric ceramic material with dual usage of receiving/sending and its preparation method |
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| CN101913866B (en) * | 2010-08-18 | 2012-08-01 | 郴州功田电子陶瓷技术有限公司 | Gas ignition piezoelectric ceramics and manufacture process thereof |
| CN101948309B (en) * | 2010-08-20 | 2013-08-21 | 暨南大学 | PPSMZT-doped piezoelectric ceramic, preparation method thereof and use thereof |
| CN104152997B (en) * | 2013-05-14 | 2018-07-20 | 中国科学院上海硅酸盐研究所 | Quaternary system relaxation type monocrystalline piezoelectric material and its growing method |
| CN103467090A (en) * | 2013-09-03 | 2013-12-25 | 瑞声精密制造科技(常州)有限公司 | Piezoelectric ceramic material, sintered body and preparation method thereof, and piezoelectric ceramic device |
| CN106518070B (en) * | 2016-10-19 | 2019-06-04 | 常州大学 | A kind of polynary system high-voltage electricity active piezoelectric ceramic material and preparation method thereof |
| CN107226698B (en) * | 2017-06-15 | 2018-04-20 | 华中科技大学 | A kind of piezoceramic material and preparation method applied to underwater acoustic transducer |
| CN111704461B (en) * | 2020-05-22 | 2022-06-07 | 江苏波速传感器有限公司 | Formula and preparation method of high Curie point low temperature co-fired piezoelectric ceramic |
| CN114075073B (en) * | 2020-08-17 | 2022-12-13 | 中国科学院上海硅酸盐研究所 | PZT-Pb (Sb) 1/2 Nb 1/2 ) Ternary system piezoelectric ceramic material and preparation method and application thereof |
| CN115417671A (en) * | 2022-07-07 | 2022-12-02 | 南京航空航天大学 | Lead zirconate titanate based piezoelectric ceramic for high-power scene and preparation method thereof |
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