CN103641478A - Ferroelectric piezoelectric ceramic material of large-power energy transducer and preparation method thereof - Google Patents
Ferroelectric piezoelectric ceramic material of large-power energy transducer and preparation method thereof Download PDFInfo
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- CN103641478A CN103641478A CN201310624343.0A CN201310624343A CN103641478A CN 103641478 A CN103641478 A CN 103641478A CN 201310624343 A CN201310624343 A CN 201310624343A CN 103641478 A CN103641478 A CN 103641478A
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- 238000002360 preparation method Methods 0.000 title claims description 10
- 229910010293 ceramic material Inorganic materials 0.000 title abstract 4
- 239000000919 ceramic Substances 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 239000011701 zinc Substances 0.000 claims description 22
- 238000005303 weighing Methods 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000001354 calcination Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 10
- SSYBETHNRHYQGU-UHFFFAOYSA-N [Pb].[Lu].[Nb] Chemical compound [Pb].[Lu].[Nb] SSYBETHNRHYQGU-UHFFFAOYSA-N 0.000 claims description 7
- 239000010955 niobium Substances 0.000 claims description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 238000000748 compression moulding Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- 238000001272 pressureless sintering Methods 0.000 claims description 2
- 239000006104 solid solution Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 abstract 1
- 239000003129 oil well Substances 0.000 abstract 1
- JQJCSZOEVBFDKO-UHFFFAOYSA-N lead zinc Chemical compound [Zn].[Pb] JQJCSZOEVBFDKO-UHFFFAOYSA-N 0.000 description 13
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 229910002367 SrTiO Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 238000001757 thermogravimetry curve Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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Abstract
本发明公开了一种利用B位离子自掺杂的方法控制烧绿石相，从而制备出高居里点、高矫顽场、高压电系数的铁电压电陶瓷材料。所述陶瓷材料的组成通式为：(1-x-y)Pb(Lu1/2Nb1/2)O3-xPb(Zn1/3Nb2/3)O3-yPbTiO3（简记为PLuN-PZN-PT），其中：x，y为摩尔比，且0.21≤x≤0.51、0.20≤y≤0.45。该材料的制备是首先利用ZnO进行B位自掺杂制备出纯相钙钛矿结构的PLuN-PZN-PT陶瓷粉体，在进行二步法烧结。本发明提供的陶瓷材料的机械品质因子得到极大提高，可满足其应用在油井探测、海底声呐及其他大功率换能器件的性能要求。
The invention discloses a method for controlling the pyrochlore phase by using a B-site ion self-doping method, thereby preparing a ferroelectric piezoelectric ceramic material with a high Curie point, a high coercive field and a high piezoelectric coefficient. The general composition formula of the ceramic material is: (1-xy)Pb(Lu 1/2 Nb 1/2 )O 3 -xPb(Zn 1/3 Nb 2/3 )O 3 -yPbTiO 3 (abbreviated as PLuN -PZN-PT), where: x, y are the molar ratio, and 0.21≤x≤0.51, 0.20≤y≤0.45. The material is prepared by firstly using ZnO for B-site self-doping to prepare PLuN-PZN-PT ceramic powder with a pure phase perovskite structure, and then sintering in two steps. The mechanical quality factor of the ceramic material provided by the invention is greatly improved, which can meet the performance requirements of its application in oil well detection, seabed sonar and other high-power transducer devices.
Description
Technical field
The present invention relates to a kind of piezoceramic material for high-power transverter and preparation method thereof.Particularly, the present invention relates to a kind of niobium lutetium lead plumbate-lead zinc niobate-lead titanate tri compound perovskite typed piezoceramic material and preparation method thereof, belong to technical field of function materials.
Background technology
Nearly ten years, novel Pb-Based Relaxor Ferroelectric Materials arouses great concern with its excellent piezoelectric property.Most study and most widely used be mainly the relaxation ferroelectric of lead base complex perovskite structure, this type of ferroelectrics general formula Pb (B ' B 〞) O
3, wherein B position atom has two kinds of occupy-places, B '=Zn
2+, Mg
2+, Fe
3+, Sc
3+, B 〞=Nb
5+, Ta
5+, W
6+Typical relaxation ferroelectric lead zinc niobate-lead titanate (PZN-PT) wherein, with its excellent piezoelectric property (d
33～2000pC/N), electromechanical coupling performance (K
33～90%) and electrostrictive property (electric field induction strain up to 1.7%) and receiving much concern, lead zinc niobate-lead titanate monocrystal material has very wide application prospect in imaging of medical, sonar projector and solid-state actuators field.
Yet lead zinc niobate-lead titanate crystal or stupalith have three problems in preparation and the process used: one, in preparation process, easily form pyrrhite phase and make it cannot realize large-scale production always, tracing it to its cause is the less stable due to the phase structure with the relevant piezoelectric monocrystal of lead zinc niobate component and stupalith, and its crystallisation process is always in metastable condition.In order to stablize the perovskite structure of lead zinc niobate-lead titanate, at present conventional method is by lead zinc niobate and stable uhligite body (BaTiO
3, SrTiO
3, KN etc.) form sosoloid and suppress pyrrhite phase.Two, the Curie temperature of lead zinc niobate-lead titanate material of pure phase is lower, especially exists one compared with the umpolarization temperature of low tripartite-cubic phase transformation, to make it cannot realize the application of high-temperature field.Three, the coercive field of lead zinc niobate-lead titanate material of pure phase is lower, cannot meet the demand of high-power energy transducer.
Given this, in order to develop high curie point, high voltage electric effect, the ferroelectric piezoelectric of high coercive field, the niobium lutetium lead plumbate that we are higher Curie temperature and stability is higher is incorporated in lead zinc niobate-lead titanate structure, thereby expect the ferroelectric piezoelectric of niobium lutetium lead plumbate-lead zinc niobate-lead titanate of high curie point, thereby meet the application in high temp. energy transduce field.
Summary of the invention
In order to solve the problems such as the low curie point of lead zinc niobate-lead titanate relaxor ferroelectric piezoelectric, low coercive field and the mechanical quality factor are not high, the invention provides the ion auto-doping of a kind of B position and prepare the complex perouskite type piezoelectric ceramics material of lead zinc niobate base, thereby effectively suppress the formation of pyrrhite phase, obtain sintering quality high, the piezoelectric ceramics of excellent performance.The present invention, by B position ion auto-doping method, introduces antiferroelectric niobium lutetium lead plumbate in lead zinc niobate-lead titanate structure, has not only realized the preparation of pure perovskite phase structure, and has also improved the mechanical quality factor of material simultaneously.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
The ferroelectric sosoloid pottery niobium lutetium lead plumbate-lead zinc niobate-lead titanate that is applicable to high-power transverter, its composition general formula is: (1-x-y) Pb (Lu
1/2nb
1/2) O
3-xPb (Zn
1/3nb
2/3) O
3-yPbTiO
3, wherein: x, y is mol ratio, and 0.21<x<0.51,0.21<y<0.42.
The preparation method of the described ferroelectric sosoloid pottery niobium lutetium lead plumbate-lead zinc niobate-lead titanate that is applicable to high-power transverter, comprises the steps:
A) according to LuNbO
4and ZnNbO
6the Lu of general formula accurate weighing stoichiometric ratio
2o
3, ZnO and Nb
2o
5, through ball milling, calcining, the step of ball milling again, the LuNbO of system
4and ZnNbO
6ceramic powder;
B) according to (1-x-y) Pb (Lu
1/2nb
1/2) O
3-xPb (Zn
1/3nb
2/3) O
3-yPbTiO
3general formula, accurate weighing PbO, TiO
2the LuNbO that adds step a) to make
4and ZnNbO
6ceramic powder, in addition, accurate weighing surpasses general formula metering than 10% ZnO, as the component of B position auto-doping, through ball milling, dry, and calcining, ball milling step again make (1-x-y) Pb (Lu of Zn doping
1/2nb
1/2) O
3-xPb (Zn
1/3nb
2/3) O
3-yPbTiO
3ceramic powder;
C) add binding agent, granulation, compression moulding, plastic removal;
D) carry out two step method sintering, obtain being applicable to the ferroelectric piezoelectric ceramics material of high-power transverter.
Described ball milling recommend adoption deionized water or dehydrated alcohol be as medium, planetary ball mill 8～12 hours; The calcining temperature of step in a) is 900-950 ℃; Step b) calcining temperature in is 900-1000 ℃; Step c) described step c) pressure of described compression moulding is 200MPa, and the temperature of plastic removal is 500 ℃; Steps d) the pressureless sintering temperature in is recommended as 1100-1150 ℃ of sintering 1.5-2.5 hour.
Compare with existing binary or ternary Pb-Based Relaxor Ferroelectric Materials, the Curie temperature of stupalith provided by the invention is higher than 300 ℃, and umpolarization temperature is higher than 180 ℃, piezoelectric coefficient d
33can reach 400pC/N, the mechanical quality factor is greater than 1000.And preparation method of the present invention has simple to operate, the cycle is short, and old low and be easy to the advantages such as large-scale production.
Accompanying drawing explanation
Fig. 1 is the Regional Phase Diagram of the accurate homotype phase boundary of this ternary system pottery.
Fig. 2 is component (1-x-y) Pb (Lu
1/2nb
1/2) O
3-xPb (Zn
1/3nb
2/3) O
3-yPbTiO
3the XRD diffractogram of ceramics sample.
Fig. 3 is the SEM photo of component 0.33PLuN-0.30PZN-0.37PT ceramics sample section.
Fig. 4 is component (1-x-y) Pb (Lu
1/2nb
1/2) O
3-xPb (Zn
1/3nb
2/3) O
3-yPbTiO
3the ferroelectric loop line figure of ceramics sample.
Fig. 5 is component (1-x-y) Pb (Lu
1/2nb
1/2) O
3-xPb (Zn
1/3nb
2/3) O
3-yPbTiO
3the Curie temperature of ceramics sample with the variation diagram of component.
Fig. 6 is component (1-x-y) Pb (Lu
1/2nb
1/2) O
3-xPb (Zn
1/3nb
2/3) O
3-yPbTiO
3the piezo-electric modulus of ceramics sample with the variation diagram of component.
Embodiment:
Below in conjunction with example, the present invention is done to further detailed, complete explanation.
Embodiment mono-((1-0.21-y) PLuN-0.21PZN-yPT):
A) according to LuNbO
4and ZnNbO
6the Lu of general formula accurate weighing stoichiometric ratio
2o
3, ZnO and Nb
2o
5, adopt deionized water or dehydrated alcohol to do medium, planetary ball mill 9 hours, calcines 1.5 hours at 950 ℃ and 900 ℃ respectively, again adopts ionized water or dehydrated alcohol to do medium, planetary ball mill 4 hours, the LuNbO of system
4and ZnNbO
6ceramic powder;
B) according to (1-x-y) Pb (Lu
1/2nb
1/2) O
3-xPb (Zn
1/3nb
2/3) O
3-yPbTiO
3general formula, x=0.21 wherein, y=0.33-0.41, accurate weighing PbO, TiO
2the LuNbO that adds step a) to make
4and ZnNbO
6ceramic powder, in addition, accurate weighing surpasses the ZnO of stoichiometric ratio 5-10%, as the component of B position auto-doping, adopts deionized water or dehydrated alcohol to make medium, planetary ball mill 12 hours, dry, 900 ℃ of calcinings, again adopt deionized water or dehydrated alcohol to make medium, planetary ball mill 6 hours, makes (1-x-y) Pb (Lu that Zn adulterates
1/2nb
1/2) O
3-xPb (Zn
1/3nb
2/3) O
3-yPbTiO
3ceramic powder;
C) add binding agent, granulation is pressed into the disk that diameter is 10mm under the pressure of 200MPa, at 500 ℃ of plastic removals;
D) carry out two step method sintering, in air atmosphere, with PbO, as atmosphere material, 1150 ℃ of sintering 2.5 hours, obtain ferroelectric piezoelectric ceramics material.
The stupalith making is carried out to its material phase analysis with MiniFlex-II powder diffractometer, and the XRD spectra obtaining is shown in shown in Fig. 2 (a).From Fig. 2 (a): the principal phase of this component is the structure of pure phase uhligite.
Fig. 3 is the scanning electron microscope (SEM) photograph of the part stupalith that makes of the present embodiment, and as seen from Figure 3, prepared stupalith crystallinity is fine, without miscellaneous pyrrhite, has obvious crystal boundary.
Fig. 4 is the ferroelectric hysteresis loop figure that the present embodiment makes stupalith, and from Fig. 4 (a), prepared stupalith has larger coercive field (>10kV/cm).
Fig. 5 is the dielectric thermogram that the present embodiment makes stupalith, from Fig. 5 (a), prepared stupalith there is higher Curie temperature (>300 ℃) and umpolarization temperature (>180 ℃).
Embodiment bis-((1-0.30-y) PLuN-0.30PZN-yPT):
A) according to LuNbO
4and ZnNbO
6the Lu of general formula accurate weighing stoichiometric ratio
2o
3, ZnO and Nb
2o
5, adopt deionized water or dehydrated alcohol to do medium, planetary ball mill 9 hours, calcines 1.5 hours at 950 ℃ and 900 ℃ respectively, again adopts ionized water or dehydrated alcohol to do medium, planetary ball mill 4 hours, the LuNbO of system
4and ZnNbO
6ceramic powder;
B) according to (1-x-y) Pb (Lu
1/2nb
1/2) O
3-xPb (Zn
1/3nb
2/3) O
3-yPbTiO
3general formula, x=0.30 wherein, y=0.29-0.37, accurate weighing PbO, TiO
2the LuNbO that adds step a) to make
4and ZnNbO
6ceramic powder, in addition, accurate weighing surpasses the ZnO of stoichiometric ratio 5-10%, as the component of B position auto-doping, adopts deionized water or dehydrated alcohol to make medium, planetary ball mill 12 hours, dry, 1000 ℃ of calcinings, again adopt deionized water or dehydrated alcohol to make medium, planetary ball mill 6 hours, makes (1-x-y) Pb (Lu that Zn adulterates
1/2nb
1/2) O
3-xPb (Zn
1/3nb
2/3) O
3-yPbTiO
3ceramic powder;
C) add binding agent, granulation is pressed into the disk that diameter is 10mm under the pressure of 200MPa, at 500 ℃ of plastic removals;
D) carry out two step method sintering, in air atmosphere, with PbO, as atmosphere material, 1100 ℃ of sintering 2.5 hours, obtain ferroelectric piezoelectric ceramics material.
Follow-up sign step is as embodiment mono-.
Embodiment tri-((1-0.42-y) PLuN-0.42PZN-yPT):
E) according to LuNbO
4and ZnNbO
6the Lu of general formula accurate weighing stoichiometric ratio
2o
3, ZnO and Nb
2o
5, adopt deionized water or dehydrated alcohol to do medium, planetary ball mill 9 hours, calcines 1.5 hours at 950 ℃ and 900 ℃ respectively, again adopts ionized water or dehydrated alcohol to do medium, planetary ball mill 4 hours, the LuNbO of system
4and ZnNbO
6ceramic powder;
F) according to (1-x-y) Pb (Lu
1/2nb
1/2) O
3-xPb (Zn
1/3nb
2/3) O
3-yPbTiO
3general formula, x=0.42 wherein, y=0.24-0.32, accurate weighing PbO, TiO
2the LuNbO that adds step a) to make
4and ZnNbO
6ceramic powder, in addition, accurate weighing surpasses the ZnO of stoichiometric ratio 5-10%, as the component of B position auto-doping, adopts deionized water or dehydrated alcohol to make medium, planetary ball mill 12 hours, dry, 1050 ℃ of calcinings, again adopt deionized water or dehydrated alcohol to make medium, planetary ball mill 6 hours, makes (1-x-y) Pb (Lu that Zn adulterates
1/2nb
1/2) O
3-xPb (Zn
1/3nb
2/3) O
3-yPbTiO
3ceramic powder;
G) add binding agent, granulation is pressed into the disk that diameter is 10mm under the pressure of 200MPa, at 500 ℃ of plastic removals;
H) carry out two step method sintering, in air atmosphere, with PbO, as atmosphere material, 1100 ℃ of sintering 2.5 hours, obtain ferroelectric piezoelectric ceramics material.
Sign step is below as embodiment mono-.
In sum, the Curie temperature of stupalith provided by the invention and coercive field have great raising than lead zinc niobate-lead titanate, and have higher piezo-electric modulus and the mechanical quality factor.
It is important to point out: above embodiment is only further described for the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.
Claims (9)
1. a ferroelectric piezoelectric ceramics material that is applicable to high-power transverter, is characterized in that: described material consists of niobium lutetium lead plumbate-lead zinc niobate-titanate lead solid solution, forms general formula to be: (1-x-y) Pb (Lu
1/2nb
1/2) O
3-xPb (Zn
1/3nb
2/3) O
3-yPbTiO
3, wherein: x, y is mol ratio, and 0.21<x<0.51,0.21<y<0.42, belongs to complex perovskite structure.
2. material according to claim 1, is characterized in that: described sosoloid exists accurate homotype phase boundary, and its accurate homotype phase boundary scope is x=0.21-0.51, y=0.23-0.39.
3. the preparation method of material described in claim 1, is characterized in that: the sintering process that adopts the ion auto-doping of B position; Comprise the steps:
(1) according to LuNbO
4and ZnNbO
6the Lu of general formula accurate weighing stoichiometric ratio
2o
3, ZnO and Nb
2o
5, through ball milling, calcining, the step of ball milling, makes LuNbO again
4and ZnNbO
6ceramic powder;
(2) according to (1-x-y) Pb (Lu
1/2nb
1/2) O
3-xPb (Zn
1/3nb
2/3) O
3-yPbTiO
3general formula, accurate weighing PbO, TiO
2the LuNbO that adds step (1) to make
4and ZnNbO
6ceramic powder, in addition, accurate weighing surpasses general formula metering than 10% ZnO, as the component of B position auto-doping, through ball milling, dry, and calcining, ball milling step again make (1-x-y) Pb (Lu of Zn doping
1/2nb
1/2) O
3-xPb (Zn
1/3nb
2/3) O
3-yPbTiO
3ceramic powder;
(3) add binding agent, granulation, compression moulding, plastic removal;
(4) carry out two step method sintering, obtain being applicable to the ferroelectric piezoelectric ceramics material of high-power transverter.
4. method according to claim 3, is characterized in that: described ball-milling medium is deionized water or dehydrated alcohol planetary ball mill 8～12 hours.
5. method according to claim 3, is characterized in that: the calcining temperature in described step (1) is 900-950 ℃.
6. method according to claim 3, is characterized in that: the calcining temperature in described step (2) is 900-1000 ℃.
7. method according to claim 3, is characterized in that: the pressure of the compression moulding that described step (3) is described is 200MPa, and the temperature of plastic removal is 500 ℃.
8. method according to claim 3, is characterized in that: the pressureless sintering temperature in described step (4) is 1100-1150 ℃.
9. material claimed in claim 1 is for powerful electromechanical transducer, stimulator, electrical condenser, driving mechanism, microwave communication, micro-wave dielectric, wave filter, ultrasonator and piezoelectric buzzer field.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115894021A (en) * | 2022-12-26 | 2023-04-04 | 西安创研电子科技有限公司 | High-mechanical-quality-factor rigid piezoelectric ceramic material and preparation method thereof |
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| CN103011815A (en) * | 2012-12-06 | 2013-04-03 | 中国科学院福建物质结构研究所 | Ternary ferroelectric solid solution lead lutecium niobate-lead magnesium niobate-lead titanate |
| CN103044023A (en) * | 2011-10-12 | 2013-04-17 | 中国科学院福建物质结构研究所 | Ferroelectric solid solution barium lutecium niobate-lead titanate |
| CN103172373A (en) * | 2012-12-12 | 2013-06-26 | 中国科学院福建物质结构研究所 | Ternary ferroelectric solid solution lead niobate ytterbate-lead zinc niobate-lead titanate |
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2013
- 2013-11-28 CN CN201310624343.0A patent/CN103641478A/en active Pending
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| CN103044023A (en) * | 2011-10-12 | 2013-04-17 | 中国科学院福建物质结构研究所 | Ferroelectric solid solution barium lutecium niobate-lead titanate |
| CN102649643A (en) * | 2012-04-25 | 2012-08-29 | 中国科学院福建物质结构研究所 | Lead lutecium niobate-lead zirconate titanate piezoceramic material |
| CN103011815A (en) * | 2012-12-06 | 2013-04-03 | 中国科学院福建物质结构研究所 | Ternary ferroelectric solid solution lead lutecium niobate-lead magnesium niobate-lead titanate |
| CN103172373A (en) * | 2012-12-12 | 2013-06-26 | 中国科学院福建物质结构研究所 | Ternary ferroelectric solid solution lead niobate ytterbate-lead zinc niobate-lead titanate |
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| CN115894021A (en) * | 2022-12-26 | 2023-04-04 | 西安创研电子科技有限公司 | High-mechanical-quality-factor rigid piezoelectric ceramic material and preparation method thereof |
| 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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