CN107021753A - A kind of ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material and preparation method thereof - Google Patents
A kind of ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 84
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000000919 ceramic Substances 0.000 title claims abstract description 33
- OOBNORVQFIAGPT-UHFFFAOYSA-N antimony manganese Chemical compound [Mn].[Sb] OOBNORVQFIAGPT-UHFFFAOYSA-N 0.000 title claims abstract description 23
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 22
- 150000002500 ions Chemical class 0.000 claims abstract description 21
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims abstract description 16
- 229910000018 strontium carbonate Inorganic materials 0.000 claims abstract description 16
- 239000011572 manganese Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims description 51
- 238000000498 ball milling Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 19
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 17
- 229910052709 silver Inorganic materials 0.000 claims description 17
- 239000004332 silver Substances 0.000 claims description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000010792 warming Methods 0.000 claims description 14
- 238000001354 calcination Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 9
- 230000032683 aging Effects 0.000 claims description 7
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000000748 compression moulding Methods 0.000 claims description 7
- 238000005238 degreasing Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- 229920002545 silicone oil Polymers 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 2
- 238000005245 sintering Methods 0.000 abstract description 23
- 230000008878 coupling Effects 0.000 abstract description 11
- 238000010168 coupling process Methods 0.000 abstract description 11
- 238000005859 coupling reaction Methods 0.000 abstract description 11
- 238000000034 method Methods 0.000 abstract description 8
- 239000003990 capacitor Substances 0.000 abstract 1
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract 1
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 12
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 10
- 239000004570 mortar (masonry) Substances 0.000 description 10
- 239000000126 substance Substances 0.000 description 8
- 238000004026 adhesive bonding Methods 0.000 description 6
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- 238000011056 performance test Methods 0.000 description 5
- 230000010287 polarization Effects 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- LIABKAQKQSUQJX-UHFFFAOYSA-N [Mn].[Pb] Chemical compound [Mn].[Pb] LIABKAQKQSUQJX-UHFFFAOYSA-N 0.000 description 3
- 229910052787 antimony Inorganic materials 0.000 description 3
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 3
- 229910001422 barium ion Inorganic materials 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 239000002019 doping agent Substances 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000018109 developmental process Effects 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
- 230000005684 electric field Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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- C04B35/493—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates based on lead zirconates and lead titanates, e.g. PZT containing also other lead compounds
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Abstract
The present invention discloses a kind of ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material and preparation method thereof, constitutes and is：Pb1.04(Mn1/ 3Sb2/3)0.05Zr0.47Ti0.48O3+0.1wt%SrCO3+0.2wt%BaCO3+ xwt%V2O5, wherein x=0.05~1.5；The present invention uses process for solid phase synthesis, and calcined temperature is 750 ~ 900 DEG C, and using three-stage sintering method, and maximum sintering temperature is less than 1200 DEG C, obtains piezoceramic material；This material has high piezoelectric modulus, mechanical quality factor and electromechanical coupling factor, with excellent piezoelectric and dielectric properties, is mainly used in the fields such as PZT (piezoelectric transducer), capacitor, sensor, with very big market value.
Description
Technical field
The present invention relates to a kind of piezoceramic material for electronic component industry, more particularly to a kind of ion doping
Lead antimony manganese zirconia titanate piezoelectric ceramics material and preparation method thereof, belongs to electric elements and its material manufacture technical field.
Background technology
Lead titanate piezoelectric ceramics are that PZT ceramics are current using class-1 piezoelectric material widely, due to piezoelectricity pottery
The application of ceramic material is quite varied, in different application fields, there is different requirements to its performance.In order to adapt to different uses
It is required that, various piezoelectric ceramics formulas are developed and designed.Such as to the piezoelectric for making underwater acoustic transducer, category is received
Type（Such as hydrophone pick-up dipole）, it is necessary to assure high electromechanical coupling factor kpAnd big piezoelectric strain constant g31Or g33；Should
For launching field（Such as sonar transmission oscillator）, then need with high Qm Qm, while requiring in the strong of high frequency
Dielectric loss tan δ are small under electric field, and piezoelectric property is difficult decline；The common prescription of piezoelectric transducer material is electromechanical coupling factor
Greatly, dielectric constant is high.But these performances are often conflicting first, for example, the big material of dielectric constant, tan δ are often
Also it is big；kpThe high material of value, QmValue is relatively low, and less stable etc..Secondly for the piezoelectric ceramics of PZT bases, it is sintered
Temperature all more than 1200 DEG C, causes the PbO in raw material to volatilize mostly, and this aspect can cause the chemical composition meeting of ceramics
Nonstoichiometry ratio, has a strong impact on the performance of piezoelectric ceramics, and the volatilization of another aspect lead can also be caused not to human body and environment
Good influence.In current production, the main method for making up lead volatility is to use to bury burning method, sealed sintering method or make PbO
Excessive, these can not all be inherently eliminated PbO volatilization, and it is to realize that piezoelectricity is made pottery to suppress PbO volatilizations more effective method
The sintering temperature of piezoceramic material, i.e., be reduced to below the temperature of PbO volatilizations by the low-temperature sintering of ceramic material.
The content of the invention
The present invention uses Sr, Ba ion compounding doping combination V2O5Antimony dopant manganese lead zirconate titanate（PMS-PZT）Piezoelectric ceramics,
By optimizing piezoelectric ceramics and its preparation technology to obtaining high-performance PMS-PZT piezoceramic materials.
An object of the present invention is to provide a kind of with high tension electricity coefficient, high mechanical quality factor, high mechanical-electric coupling
The antimony manganese of coefficient-lead zirconate titanate base piezoelectric ceramic (PMS-PZT), is suitable for the devices such as high intensity ultrasound transducer, piezoelectric transducer
The application of part, consisting of：Pb1.04(Mn1/3Sb2/3)0.05Zr0.47Ti0.48O3+0.1wt%SrCO3+0.2wt%BaCO3+ xwt%
V2O5 , wherein x=0.05~1.5, wt% represents mass percent, represents to account for the mass percentage content of gross mass.
The doping of Sr, Ba ion compounding and V that the present invention is provided2O5Antimony dopant manganese lead zirconate titanate (PMS-PZT) piezoelectricity is made pottery
Porcelain, by Pb1.04(Mn1/3Sb2/3)0.05Zr0.47Ti0.4803+ 0.1wt%SrCO3+ 0.2wt%BaCO3+xwt%V2O5(wherein x=
The raw material that 0.05~stoichiometric proportion 1.5) is weighed are Pb3O4、SrCO3、MnO、Sb2O3、TiO2、ZrO2、BaCO3、V2O5。
Ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material of the present invention is the doping of Sr, Ba ion compounding and V2O5
Antimony dopant manganese lead zirconate titanate（PMS-PZT）Piezoelectric ceramics has single perovskite structure.
Another object of the present invention is to provide the preparation side of the ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material
Method, specifically includes following steps：
（1）The good raw material of proportionally accurate weighing is added in ball grinder and enters planetary type ball-milling, when material adds ball grinder
It should be noted that the order of the raw material added, first adds the raw material more than a deal and adds the few raw material of a deal, it is few according to more than one one
Order raw material is sequentially added in ball grinder, prevent the less material of content from gluing the deviation of chemical ratio that wall is caused, ball be set
Mill rotating speed is 200 ~ 300rad/min, 10 ~ 12h of ball mill mixing, after 80 ~ 90 DEG C dry, ground 60 ~ 80 mesh sieve；
（2）By step（1）Material after sieving, carries out precompressed, and the lump material after precompressed is forged for 750 ~ 900 DEG C in confined conditions
Burn 1.5 ~ 2h；
（3）By step（2）Material grinding after calcining, secondary ball milling, drying crosses 250 ~ 325 mesh sieves, according to raw material gross mass 6%
Ratio add mass concentration be 11% ~ 12% the PVA aqueous solution, be fully ground, after 60 ~ 80 mesh sieves；
（4）By step（3）Screened material, compression molding obtains green sheet；
（5）By step（4）Then obtained green sheet is warming up to first in 500 ~ 600 DEG C of degreasings with 2 DEG C/min heating rate
1020 ~ 1080 DEG C, 1120 ~ 1180 DEG C/min is warming up to 5 DEG C/min heating rate, 10 ~ 30min is incubated, with 10 DEG C/min
Rate of temperature fall cool to 700 ~ 1000 DEG C, be incubated 2h, obtain sintered body；
（6）By step（5）Obtained sintered body is polished, after the middle temperature silver paste of surface smear, 80 ~ 90 DEG C of drying, 600 ~
Sinter 2 hours, obtained by silver-colored potsherd at 700 DEG C；
（7）By step（6）What is obtained is put into by silver-colored potsherd in 120 ~ 130 DEG C of silicone oil, with 2.5 ~ 3kv/mm DC voltages pole
Change after 15 ~ 20min, take out natural aging 24h in atmosphere, obtain potsherd.
Beneficial effects of the present invention：
Ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material produced by the present invention compares the piezoelectricity system of PMS-PZT base piezoelectric ceramics
Number, mechanical quality factor and electromechanical coupling factor are improved, its piezoelectric coefficient d33=313 ~ 326PC/N, mechanical quality factor Qm=
1387 ~ 1888, electromechanical coupling factor kp=0.60 ~ 0.63, relative dielectric coefficient εr=1419~1466；The inventive method is simple, roasting
Burn temperature and be less than 1180 DEG C, do not result in a large amount of volatilizations of lead oxide, environmental protection, and ensure that the stability of material.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material of the embodiment of the present invention 1；
Fig. 2 is the XRD spectrum of 1-5 ion doping lead antimony manganese zirconia titanate piezoelectric ceramics materials of the embodiment of the present invention.
Embodiment
The present invention will be further described with specific embodiment below in conjunction with the accompanying drawings, but protection scope of the present invention is not limited
In the content.
Embodiment 1
A kind of ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material of the present embodiment, its raw material, which is constituted, is：Pb1.04(Mn1/ 3Sb2/3)0.05Zr0.47Ti0.4803+0.1wt%SrCO3+0.2wt%MnO2 +0.05wt%V2O5, wt% represents to account for material gross mass
Mass percent, its raw material are Pb3O4、SrCO3、MnO、Sb2O3、TiO2、ZrO2、BaCO3、V2O5。
The preparation method of ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material, specifically includes following step described in the present embodiment
Suddenly：
（1）The good raw material of proportionally accurate weighing is added in ball grinder and enters planetary type ball-milling, when material adds ball grinder
It should be noted that the order of the raw material added, first adds the raw material more than a deal and adds the few raw material of a deal, it is few according to more than one one
Order raw material is sequentially added in ball grinder, prevent the less material of content from gluing the deviation of chemical ratio that wall is caused, and ball milling
Ball in tank：Material：The weight ratio of absolute ethyl alcohol is the ︰ 0.7 of 2 ︰ 1, and rotational speed of ball-mill is taking-up general after 200rad/min, ball mill mixing 12h
Compound is put into baking oven, after 90 DEG C of drying, is put into ground 60 mesh sieve in mortar body；
（2）By step（1）Material after sieving is put into mould and carries out precompressed, and the lump material after precompressed is put into crucible and is capped
Sealing, 850 DEG C of calcining 2h；
（3）By step（2）Material grinding after calcining, secondary ball milling, drying crosses 325 mesh sieves, according to the ratio of raw material gross mass 6%
Example plus the PVA aqueous solution that mass concentration is 12%, are fully ground in mortar, after 60 mesh sieves；
（4）By step（3）Screened material, compression molding obtains green sheet；
（5）By step（4）Obtained green sheet is first in 500 DEG C of degreasing dumpings, then by the blank after dumping with 2 DEG C/min liter
Warm speed is warming up to 1020 DEG C of progress first paragraph sintering, is warming up to 1180 DEG C/min with 5 DEG C/min heating rate, is incubated
30min carries out second segment sintering, with 10 DEG C/min rate of temperature fall fast cooling to 1000 DEG C, and insulation 2h carries out the 3rd section of burning
Knot, obtains sintered body；
（6）By step（5）Obtained sintered body is polished, after the middle temperature silver paste of its surface smear, after 80 DEG C of drying, 600 DEG C
Lower sintering 2h, is obtained by silver-colored potsherd, and used middle temperature silver paste is the model PC- that Guiyan Platium Co., Ltd produces
Ag-5310 middle temperature silver paste；
（7）By step（6）What is obtained is put into by silver-colored potsherd in 120 DEG C of silicone oil, with 3kv/mm DC voltages polarization 15min
Afterwards, natural aging 24h in atmosphere is taken out, potsherd is obtained.
Potsherd is subjected to performance test, obtained result is respectively：d33=313PC/N, mechanical quality factor Qm=1748、
Electromechanical coupling factor kp=0.63, relative dielectric coefficientε r=1420。
Fig. 1 is the scanning electron microscope (SEM) photograph for the potsherd section that the present embodiment is prepared, as can be seen from the figure crystallite dimension
About 5 μm, grain development is preferably, uniform in size, and crystal boundary combines fine and close.
Embodiment 2
A kind of ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material of the present embodiment, its raw material, which is constituted, is：Pb1.04(Mn1/ 3Sb2/3)0.05Zr0.47Ti0.4803+0.1wt%SrCO3+0.2wt%MnO2 +0.1wt%V2O5, wt% represents to account for the matter of material gross mass
Percentage is measured, its raw material is Pb3O4、SrCO3、MnO、Sb2O3、TiO2、ZrO2、BaCO3、V2O5。
The preparation method of ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material, specifically includes following step described in the present embodiment
Suddenly：
（1）The good raw material of proportionally accurate weighing is added in ball grinder and enters planetary type ball-milling, when material adds ball grinder
It should be noted that the order of the raw material added, first adds the raw material more than a deal and adds the few raw material of a deal, it is few according to more than one one
Order raw material is sequentially added in ball grinder, prevent the less material of content from gluing the deviation of chemical ratio that wall is caused, and ball milling
Ball in tank：Material：The weight ratio of absolute ethyl alcohol is the ︰ 0.7 of 2 ︰ 1, and rotational speed of ball-mill is taking-up general after 250rad/min, ball mill mixing 12h
Compound is put into baking oven, after 85 DEG C of drying, is put into ground 65 mesh sieve in mortar body；
（2）By step（1）Material after sieving is put into mould and carries out precompressed, and the lump material after precompressed is put into crucible and is capped
Sealing, 900 DEG C of calcining 1.5h；
（3）By step（2）Material grinding after calcining, secondary ball milling, drying crosses 250 mesh sieves, according to the ratio of raw material gross mass 6%
Example plus the PVA aqueous solution that mass concentration is 12%, are fully ground in mortar, after 65 mesh sieves；
（4）By step（3）Screened material, compression molding obtains green sheet；
（5）By step（4）Obtained green sheet is first in 600 DEG C of degreasing dumpings, then by the blank after dumping with 2 DEG C/min liter
Warm speed is warming up to 1040 DEG C of progress first paragraph sintering, is warming up to 1120 DEG C/min with 5 DEG C/min heating rate, is incubated
25min carries out second segment sintering, with 10 DEG C/min rate of temperature fall fast cooling to 950 DEG C, and insulation 2h carries out three-stage sintering,
Obtain sintered body；
（6）By step（5）Obtained sintered body is polished, after the middle temperature silver paste of its surface smear, after 85 DEG C of drying, 600 DEG C
Lower sintering 2h, is obtained by silver-colored potsherd, and used middle temperature silver paste is the model PC- that Guiyan Platium Co., Ltd produces
Ag-5310 middle temperature silver paste；
（7）By step（6）What is obtained is put into by silver-colored potsherd in 125 DEG C of silicone oil, with 2.5kv/mm DC voltages polarization 20min
Afterwards, natural aging 24h in atmosphere is taken out, potsherd is obtained.
Potsherd is subjected to performance test, obtained result is respectively：d33=326PC/N, mechanical quality factor Qm=1387、
Electromechanical coupling factor kp=0.61, relative dielectric coefficientε r=1466。
Embodiment 3
A kind of ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material of the present embodiment, its raw material, which is constituted, is：Pb1.04(Mn1/ 3Sb2/3)0.05Zr0.47Ti0.4803+0.1wt%SrCO3+0.2wt%MnO2 +0.5wt%V2O5, wt% represents to account for the matter of material gross mass
Percentage is measured, its raw material is Pb3O4、SrCO3、MnO、Sb2O3、TiO2、ZrO2、BaCO3、V2O5。
The preparation method of ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material, specifically includes following step described in the present embodiment
Suddenly：
（1）The good raw material of proportionally accurate weighing is added in ball grinder and enters planetary type ball-milling, when material adds ball grinder
It should be noted that the order of the raw material added, first adds the raw material more than a deal and adds the few raw material of a deal, it is few according to more than one one
Order raw material is sequentially added in ball grinder, prevent the less material of content from gluing the deviation of chemical ratio that wall is caused, and ball milling
Ball in tank：Material：The weight ratio of absolute ethyl alcohol is the ︰ 0.7 of 2 ︰ 1, and rotational speed of ball-mill is taking-up general after 300rad/min, ball mill mixing 10h
Compound is put into baking oven, after 90 DEG C of drying, is put into ground 60 mesh sieve in mortar body；
（2）By step（1）Material after sieving is put into mould and carries out precompressed, and the lump material after precompressed is put into crucible and is capped
Sealing, 750 DEG C of calcining 2h；
（3）By step（2）Material grinding after calcining, secondary ball milling, drying crosses 270 mesh sieves, according to the ratio of raw material gross mass 6%
Example plus the PVA aqueous solution that mass concentration is 11%, are fully ground in mortar, after 60 mesh sieves；
（4）By step（3）Screened material, compression molding obtains green sheet；
（5）By step（4）Obtained green sheet is first in 550 DEG C of degreasing dumpings, then by the blank after dumping with 2 DEG C/min liter
Warm speed is warming up to 1050 DEG C of progress first paragraph sintering, is warming up to 1150 DEG C/min with 5 DEG C/min heating rate, is incubated
20min carries out second segment sintering, with 10 DEG C/min rate of temperature fall fast cooling to 900 DEG C, and insulation 2h carries out three-stage sintering,
Obtain sintered body；
（6）By step（5）Obtained sintered body is polished, after the middle temperature silver paste of its surface smear, after 90 DEG C of drying, 650 DEG C
Lower sintering 2h, is obtained by silver-colored potsherd, and used middle temperature silver paste is the model PC- that Guiyan Platium Co., Ltd produces
Ag-5310 middle temperature silver paste；
（7）By step（6）What is obtained is put into by silver-colored potsherd in 130 DEG C of silicone oil, with 3kv/mm DC voltages polarization 20min
Afterwards, natural aging 24h in atmosphere is taken out, potsherd is obtained.
Potsherd is subjected to performance test, obtained result is respectively：d33=315PC/N, mechanical quality factor Qm=1888、
Electromechanical coupling factor kp=0.60, relative dielectric coefficientε r=1419。
Embodiment 4
A kind of ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material of the present embodiment, its raw material, which is constituted, is：Pb1.04(Mn1/ 3Sb2/3)0.05Zr0.47Ti0.4803+0.1wt%SrCO3+0.2wt%MnO2 +1wt%V2O5, wt% represents to account for the quality of material gross mass
Percentage, its raw material are Pb3O4、SrCO3、MnO、Sb2O3、TiO2、ZrO2、BaCO3、V2O5。
The preparation method of ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material, specifically includes following step described in the present embodiment
Suddenly：
（1）The good raw material of proportionally accurate weighing is added in ball grinder and enters planetary type ball-milling, when material adds ball grinder
It should be noted that the order of the raw material added, first adds the raw material more than a deal and adds the few raw material of a deal, it is few according to more than one one
Order raw material is sequentially added in ball grinder, prevent the less material of content from gluing the deviation of chemical ratio that wall is caused, and ball milling
Ball in tank：Material：The weight ratio of absolute ethyl alcohol is the ︰ 0.7 of 2 ︰ 1, and rotational speed of ball-mill is taking-up general after 250rad/min, ball mill mixing 11h
Compound is put into baking oven, after 80 DEG C of drying, is put into ground 80 mesh sieve in mortar body；
（2）By step（1）Material after sieving is put into mould and carries out precompressed, and the lump material after precompressed is put into crucible and is capped
Sealing, 900 DEG C of calcining 1.5h；
（3）By step（2）Material grinding after calcining, secondary ball milling, drying crosses 300 mesh sieves, according to the ratio of raw material gross mass 6%
Example plus the PVA aqueous solution that mass concentration is 11.5%, are fully ground in mortar, after 80 mesh sieves；
（4）By step（3）Screened material, compression molding obtains green sheet；
（5）By step（4）Obtained green sheet is first in 600 DEG C of degreasing dumpings, then by the blank after dumping with 2 DEG C/min liter
Warm speed is warming up to 1060 DEG C of progress first paragraph sintering, is warming up to 1140 DEG C/min with 5 DEG C/min heating rate, is incubated
15min carries out second segment sintering, with 10 DEG C/min rate of temperature fall fast cooling to 850 DEG C, and insulation 2h carries out three-stage sintering,
Obtain sintered body；
（6）By step（5）Obtained sintered body is polished, after the middle temperature silver paste of its surface smear, after 80 DEG C of drying, 700 DEG C
Lower sintering 2h, is obtained by silver-colored potsherd, and used middle temperature silver paste is the model PC- that Guiyan Platium Co., Ltd produces
Ag-5310 middle temperature silver paste；
（7）By step（6）What is obtained is put into by silver-colored potsherd in 120 DEG C of silicone oil, with 2.8kv/mm DC voltages polarization 18min
Afterwards, natural aging 24h in atmosphere is taken out, potsherd is obtained.
Potsherd is subjected to performance test, obtained result is respectively：d33=324PC/N, mechanical quality factor Qm=1484、
Electromechanical coupling factor kp=0.62, relative dielectric coefficientε r=1463。
Embodiment 5
A kind of ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material of the present embodiment, its raw material, which is constituted, is：Pb1.04(Mn1/ 3Sb2/3)0.05Zr0.47Ti0.4803+0.1wt%SrCO3+0.2wt%MnO2 +1.5wt%V2O5, wt% represents to account for the matter of material gross mass
Percentage is measured, its raw material is Pb3O4、SrCO3、MnO、Sb2O3、TiO2、ZrO2、BaCO3、V2O5。
The preparation method of ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material, specifically includes following step described in the present embodiment
Suddenly：
（1）The good raw material of proportionally accurate weighing is added in ball grinder and enters planetary type ball-milling, when material adds ball grinder
It should be noted that the order of the raw material added, first adds the raw material more than a deal and adds the few raw material of a deal, it is few according to more than one one
Order raw material is sequentially added in ball grinder, prevent the less material of content from gluing the deviation of chemical ratio that wall is caused, and ball milling
Ball in tank：Material：The weight ratio of absolute ethyl alcohol is the ︰ 0.7 of 2 ︰ 1, and rotational speed of ball-mill is taking-up general after 300rad/min, ball mill mixing 12h
Compound is put into baking oven, after 90 DEG C of drying, is put into ground 60 mesh sieve in mortar body；
（2）By step（1）Material after sieving is put into mould and carries out precompressed, and the lump material after precompressed is put into crucible and is capped
Sealing, 850 DEG C of calcining 2h；
（3）By step（2）Material grinding after calcining, secondary ball milling, drying crosses 270 mesh sieves, according to the ratio of raw material gross mass 6%
Example plus the PVA aqueous solution that mass concentration is 12%, are fully ground in mortar, after 60 mesh sieves；
（4）By step（3）Screened material, compression molding obtains green sheet；
（5）By step（4）Obtained green sheet is first in 600 DEG C of degreasing dumpings, then by the blank after dumping with 2 DEG C/min liter
Warm speed is warming up to 1080 DEG C of progress first paragraph sintering, is warming up to 1160 DEG C/min with 5 DEG C/min heating rate, is incubated
10min carries out second segment sintering, with 10 DEG C/min rate of temperature fall fast cooling to 700 DEG C, and insulation 2h carries out three-stage sintering,
Obtain sintered body；
（6）By step（5）Obtained sintered body is polished, after the middle temperature silver paste of its surface smear, after 85 DEG C of drying, 660 DEG C
Lower sintering 2h, is obtained by silver-colored potsherd, and used middle temperature silver paste is the model PC- that Guiyan Platium Co., Ltd produces
Ag-5310 middle temperature silver paste；
（7）By step（6）What is obtained is put into by silver-colored potsherd in 120 DEG C of silicone oil, with 3kv/mm DC voltages polarization 20min
Afterwards, natural aging 24h in atmosphere is taken out, potsherd is obtained.
Potsherd is subjected to performance test, obtained result is respectively：d33=315PC/N, mechanical quality factor Qm=1582、
Electromechanical coupling factor kp=0.61, relative dielectric coefficientε r=1432。
Fig. 2 show the XRD of potsherd section obtained by embodiment 1-5, it can be seen that embodiment 1-5 is prepared
Sample be perovskite structure, and without finding burnt green stone phase or other impurities phases, { 200 } crystalline substance when 2 θ=45 ° near
The characteristic peak in face splits into two characteristic peaks of (200) T (002) T, i.e., in quasi- homotype phase boundary, material property is optimal.
Claims (3)
1. a kind of ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material, it is characterised in that constitute and be：Pb1.04(Mn1/ 3Sb2/3)0.05Zr0.47Ti0.48O3+0.1wt%SrCO3+0.2wt%BaCO3+ xwt%V2O5 , wherein x=0.05~1.5.
2. ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material according to claim 1, it is characterised in that the composition
Raw material is Pb3O4、SrCO3、MnO、Sb2O3、TiO2、ZrO2、BaCO3、V2O5。
3. the preparation method of ion doping lead antimony manganese zirconia titanate piezoelectric ceramics material described in claim 2, it is characterised in that specific
Comprise the following steps：
（1）Weigh in proportion and ball milling is carried out after raw material, rotational speed of ball-mill is 200 ~ 300rad/min, 10 ~ 12h of ball milling, 80 ~ 90 DEG C of bakings
After dry, ground 60 ~ 80 mesh sieve；
（2）By step（1）Material after sieving, carries out precompressed, and the lump material after precompressed is forged for 750 ~ 900 DEG C in confined conditions
Burn 1.5 ~ 2h；
（3）By step（2）Material grinding after calcining, secondary ball milling, drying crosses 250 ~ 325 mesh sieves, according to raw material gross mass 6%
Ratio add mass concentration be 11% ~ 12% the PVA aqueous solution, be fully ground, after 60 ~ 80 mesh sieves；
（4）By step（3）Screened material, compression molding obtains green sheet；
（5）By step（4）Then obtained green sheet is warming up to first in 500 ~ 600 DEG C of degreasings with 2 DEG C/min heating rate
1020 ~ 1080 DEG C, 1120 ~ 1180 DEG C/min is warming up to 5 DEG C/min heating rate, 10 ~ 30min is incubated, with 10 DEG C/min
Rate of temperature fall cool to 700 ~ 1000 DEG C, be incubated 2h, obtain sintered body；
（6）By step（5）Obtained sintered body is polished, after the middle temperature silver paste of surface smear, 80 ~ 90 DEG C of drying, 600 ~ 700
Sinter 2 hours, obtained by silver-colored potsherd at DEG C；
（7）By step（6）What is obtained is put into by silver-colored potsherd in 120 ~ 130 DEG C of silicone oil, with 2.5 ~ 3kv/mm DC voltages pole
Change after 15 ~ 20min, take out natural aging 24h in atmosphere, obtain potsherd.
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| CN112919906A (en) * | 2021-04-23 | 2021-06-08 | 苏州攀特电陶科技股份有限公司 | High-performance PZT piezoelectric ceramic based on 3D printing and preparation method thereof |
| CN115403375A (en) * | 2022-08-31 | 2022-11-29 | 山东国瓷功能材料股份有限公司 | Lead zirconate titanate piezoelectric ceramic material and preparation method thereof |
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| CN112919906A (en) * | 2021-04-23 | 2021-06-08 | 苏州攀特电陶科技股份有限公司 | High-performance PZT piezoelectric ceramic based on 3D printing and preparation method thereof |
| CN115403375A (en) * | 2022-08-31 | 2022-11-29 | 山东国瓷功能材料股份有限公司 | Lead zirconate titanate piezoelectric ceramic material and preparation method thereof |
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