CN106220169B - Modified lead nickle niobate-lead titanate piezoelectric ceramics and preparation method thereof - Google Patents

Modified lead nickle niobate-lead titanate piezoelectric ceramics and preparation method thereof Download PDF

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CN106220169B
CN106220169B CN201610553904.6A CN201610553904A CN106220169B CN 106220169 B CN106220169 B CN 106220169B CN 201610553904 A CN201610553904 A CN 201610553904A CN 106220169 B CN106220169 B CN 106220169B
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piezoelectric ceramics
lead
preparation
wet feed
titanate piezoelectric
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CN106220169A (en
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曾祥明
冯小东
廖建中
刘振华
陈世钗
刘炉
李瑞峰
蹇胜勇
徐莉莲
杨静
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CHONGQING SHENGPU ANGKAI TECHNOLOGY Co Ltd
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Abstract

The invention discloses a kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, chemical constituents are as follows: Pb1‑xMex(Ni1/3Nb2/3)0.326(ZryTi1‑y)0.674O3+ 3%PbO+3%NiO+zwt%A;Me is any one or two kinds in strontium and neodymium in formula, A be antimony and yttrium metal oxide any one.Piezoelectric ceramics of the present invention passes through doping strontium and neodymium, antimony or yttrium form substitution solid solution, obtain the 0.326PNN-0.647PZT piezoelectric ceramics with preferable comprehensive performance, the piezoelectric ceramics has excellent piezoelectricity dielectric properties, higher Curie temperature and electromechanical coupling factor;Meanwhile preparation method is simple, raw material easily obtains, industrially applicable.

Description

Modified lead nickle niobate-lead titanate piezoelectric ceramics and preparation method thereof
Technical field
The present invention relates to field of electronic components manufacturing, and in particular to a kind of modified lead nickle niobate-lead zirconate titanate piezoelectric pottery Porcelain and preparation method thereof.
Background technique
Piezoelectric ceramics is a kind of widely used ceramic material, because of its stable mechanical property and excellent electrical property Can, preparation process is simple, cost is relatively low and is incorporated in sharp light or organisms, military information and aviation extensively etc..After second After world war finds barium titanate piezoelectric ceramics, the beginning of the fifties lead zirconate titanate (PZT) system is found, and is developed so far piezoelectricity field Application is exactly at most PZT series piezoelectric ceramic.However, it is common to use piezoelectric material be mainly lead zirconates (PZ), lead titanates (PT) polyploid being combined with the relaxation ferroelectrics such as lead magnesio-niobate (PMN), lead zinc niobate (PZN) and lead nickle niobate (PNN) System, the comprehensive performances such as piezoelectricity, dielectric, Curie temperature of these materials are not able to satisfy industrial demand, with traditional pottery The piezoelectric ceramics that porcelain preparation process develops a kind of high comprehensive performance is just provided with important industrial practical application meaning.
PNN-PZT ceramics have the characteristics of " flexible material ", such as high piezoelectric modulus, relatively high electromechanical coupling Number, high dielectric constant, low mechanical quality factor etc..The Curie temperature and piezoelectric constant of PZT ceramics are relatively high, and PNN Dielectric constant is high, but its Curie temperature is but -120 DEG C, by the compound of PZT and PNN, can prepare a kind of higher pressure electricity With the ceramics of dielectric properties, while Curie temperature is unlikely to too low again, meets the requirement of industrial application.Such as Publication No. The patent of invention of CN102659404A discloses low-temperature sintering lead nickle niobate-lead titanate piezoelectric ceramics and preparation method thereof, should Technology discloses raw material Pb3O4, Ni2O3, Nb2O5, ZrO2, TiO2 and CuO, dry by adding water-powered roller to grind, synthesis, tabletting, row Glue, sintering, is obtained, but its dielectric properties and piezoelectric property are bad by techniques such as galactic poles.
Currently, to there are mainly two types of the improved methods of PNN-PZT system ceramic performance: modification by ion-doping and improving preparation work Skill.Due to traditional ceramic preparation process because its simple process, it is at low cost, preparation ceramic performance it is good the advantages that, improve ceramics The method of performance is mainly modification by ion-doping.In perovskite ABO3 structure, A can be incorporated heteroion replacement with B ions Form substitution solid solution, the lead ion substitution of Nd ion and Sr ion pair A can be improved the dielectric properties of ceramics, Y-ion with After the replacement of B ions of Sb ion pair forms solid solution, ceramic piezoelectric property is greatly improved.To PNN-PZT system ceramics By adjusting Zr/Ti ratio near quasi- homotype phase boundary, doping vario-property ion, and find optimum process condition accurately etc. is expected to Obtain the piezoelectric ceramics of comprehensive electrical better performances.
Summary of the invention
In order to overcome the deficiencies in the prior art, the present invention provide it is a kind of have high tension electricity coefficient, good dielectric constant, compared with Modification lead nickle niobate-lead titanate piezoelectric ceramics of high electromechanical coupling factor and preparation method thereof.
To achieve the goals above, the present invention is achieved through the following technical solutions:
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, chemical constituent are as follows: Pb1-xMex(Ni1/3Nb2/3)0.326 (ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A;Me is any one or two kinds in strontium and neodymium in formula, A be antimony and The metal oxide of yttrium any one;0≤x≤0.05 in formula, 0.418≤y≤0.441,0≤z≤1.0.
Preferably, the Me is neodymium, and A is antimony, x=0.015, y=0.433, z=0.75.
A kind of preparation method of modified lead nickle niobate-lead titanate piezoelectric ceramics, comprising the following steps:
(1) prepared by wet feed: weighing raw material mixing sufficiently according to stoichiometry, dehydrated alcohol mixing and ball milling 4-8h is added, obtains To wet feed;
(2) pre-burning forms: after the wet feed drying in step (1), being placed in corundum crucible and covers, at 750-850 DEG C After temperature lower calcination 1-4h, then dehydrated alcohol mixing and ball milling 4-8h is used to obtain secondary wet feed, will be added after the drying of secondary wet feed After granulating agent is granulated, dry-pressing formed is blank;
(3) sintering polarization: gained blank is placed on corundum plate in batch-type furnace after 550 DEG C of heat preservation 3-5h, blank is set Obtain porcelain billet in 1100~1300 DEG C of sintering 1-3h in buried powder on corundum plate, then by porcelain billet by after silver electrode in 30 DEG C of silicone oil pole Change processing 5~10 minutes to get.
Preferably, raw material described in step (1) is following components: PbO, NiO, Nb2O5、TiO2、ZrO2、Nd2O3、SrCO3、 Y2O3And Sb2O3
Preferably, granulating agent described in step (2) is polyvinyl alcohol.
Preferably, 1.5~2kV/mm of polarizing voltage of polarization process described in step (3).
The beneficial effects of the present invention are: based on lead nickle niobate-lead zirconate titanate, it joined neodymium (Nd) in the feed, Strontium (Sr), the elements such as antimony (Sb) and yttrium (Y), is synthesized using conventional solid synthetic method, is sintered, pass through doping vario-property and technique Adjustment, form substitution solid solution, since the ionic radius of neodymium is 0.129nm, the ionic radius of Pb2+ is 0.119nm.For The big ion of radius will occupy the position of lead (A ions) into after solid solution.Simultaneously as neodymium ion price is high, occupy After lead ion, structure cell just will appear superfluous positive charge.Therefore, in order to keep electroneutral that will accordingly generate lead vacancy, Lattice also will appear distortion.At this point, electric domain wall easy movement.So after neodymium ion doped, the bullet of PNN-PZT piezoceramic material Property ratio of slenderness and dielectric constant can become larger.
Similarly, Sb ion due to ionic radius it is smaller, into the position the B ion position that will occupy perovskite structure after solid solution It sets.And due to the unstability of Sb3+, during the sintering process+trivalent Sb ion can transform into the Sb ion of+5 valences, with height Valence state carries out the position the B ion for replacing+4 valences, to keep electroneutral that can still generate lead vacancy, becomes easier to ferroelectric domain steering, It is promoted after Sb ion doping so as to cause the piezoelectricity dielectric properties of PNN-PZT piezoelectric ceramics.Grain is mixed used in the present invention The 0.326PNN-0.647PZT piezoelectric ceramics with preferable comprehensive performance is obtained after son, which has excellent piezoelectricity Dielectric properties, higher Curie temperature and electromechanical coupling factor;Meanwhile preparation method is simple, raw material easily obtains, and has industry real The property used.
Detailed description of the invention
Fig. 1 is lead nickle niobate-Lead Zirconate Titanate ceramic material X-ray diffractogram prepared by embodiment 15;Diffraction in figure Peak and standard card compare, and what is obtained is the perovskite structure of pure phase, and no miscellaneous phase occurs.
Fig. 2 is lead nickle niobate-Lead Zirconate Titanate ceramic material stereoscan photograph prepared by embodiment 15;Crystalline substance in photo Grain size μm is differed from 1 μm to 8, and crystal boundary is high-visible, and porosity is on the low side, and ceramic structure is finer and close.
Fig. 3 is lead nickle niobate-Lead Zirconate Titanate ceramic material dielectric temperature curve prepared by embodiment 12.Figure dielectric is normal The corresponding temperature of number peak value is 190 DEG C, i.e. Curie temperature.
Specific embodiment
Combined with specific embodiments below and attached drawing come present invention be described in more detail.
Embodiment 1
A kind of preparation method of modified lead nickle niobate-lead titanate piezoelectric ceramics, comprising the following steps:
(1) ingredient: with commercially available analysis pure PbO, NiO, Nb2O5、TiO2、ZrO2、Nd2O3、SrCO3、Y2O3And Sb2O3For original Material, stoichiometrically after ingredient, being put into ball grinder using dehydrated alcohol is to obtain within medium wet-milling 4 hours wet feed and to dry;
(2) pre-burning: the mixed powder after will be dry in step (1) is placed in alumina crucible, is compacted, is covered, box In 800 DEG C of calcining 2h in furnace, repeats wet-milling and once obtain preburning powdered material;
(3) it tabletting: after preburning powdered material is ground, then using dehydrated alcohol as solvent wet-milling 8 hours, is added after dry The polyvinyl alcohol (PVA) of 5wt%~10wt% is granulated into the fine sand grain of mobility, dry-pressing formed under 10~20MPa pressure, The blank being pressed into is the disk of 1 centimetre of diameter, about 1 millimeter of thickness;
(4) dumping: the disk blank being pressed into being placed on corundum plate and is put into batch-type furnace, and 550 DEG C keep the temperature 4 hours, heating Rate is 3~6 DEG C/min, carries out the exclusion of organic matter;
(5) it is sintered: dumping blank being placed on corundum plate and covers son, material is buried with similar powder and buries burning, heating rate 3 ~6 DEG C/min, it is sintered 2 hours to obtain porcelain billet at 1250 DEG C, naturally cools to room temperature with furnace;
(6) it polarizes: by obtained porcelain billet by polarization process 5~10 minutes, polarization are electric in 30 DEG C of silicone oil after silver electrode Pressure is 1.5~2kV/mm;The piezoelectric ceramic piece completed that polarizes carries out the survey of piezoelectricity and mechanical-electric coupling performance according to the standard of IRE Examination.
Embodiment 2
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, chemical composition are as follows:
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A;According to embodiment 1 preparation method, according to different stoichiometries, wherein x=0.005, y=0.426, z=0.
Embodiment 3
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, chemical composition are as follows:
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A;According to embodiment 1 preparation method, according to different stoichiometries, wherein x=0.01, y=0.426, z=0.
Embodiment 4
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, chemical composition are as follows:
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A;According to embodiment 1 preparation method, according to different stoichiometries, wherein x=0.015, y=0.426, z=0.
Embodiment 5
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, chemical composition are as follows:
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A;According to embodiment 1 preparation method, according to different stoichiometries, wherein x=0.02, y=0.426, z=0.
Embodiment 6
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb0.985-xNd0.015Srx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A;According to The preparation method of embodiment 1, according to different stoichiometries, wherein x=0.00, y=0.426, z=0.
Embodiment 7
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb0.985-xNd0.015Srx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A;According to The preparation method of embodiment 1, according to different stoichiometries, wherein x=0.01, y=0.426, z=0.
Embodiment 8
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb0.985-xNd0.015Srx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A;According to The preparation method of embodiment 1, according to different stoichiometries, wherein x=0.03, y=0.426, z=0.
Embodiment 9
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb0.985-xNd0.015Srx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A;According to The preparation method of embodiment 1, according to different stoichiometries, wherein x=0.05, y=0.426, z=0.
Embodiment 10
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%Y2O3, according to embodiment 1 Preparation method, wherein sintering temperature be 1150 DEG C, x=0.015, y=0.426, z=0.
Embodiment 11
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%Y2O3, according to embodiment 1 Preparation method, wherein sintering temperature be 1150 DEG C, x=0.015, y=0.426, z=0.1.
Embodiment 12
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%Y2O3, according to embodiment 1 Preparation method, wherein sintering temperature be 1150 DEG C, x=0.015, y=0.426, z=0.3.
Embodiment 13
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%Y2O3, according to embodiment 1 Preparation method, wherein sintering temperature be 1150 DEG C, x=0.015, y=0.426, z=0.5.
Embodiment 14
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%Sb2O3, according to embodiment 1 preparation method, wherein sintering temperature is 1300 DEG C, x=0.015, y=0.433, z=0.5.
Embodiment 15
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%Sb2O3, according to embodiment 1 preparation method, wherein sintering temperature is 1300 DEG C, x=0.015, y=0.433, z=0.75.
Embodiment 16
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%Sb2O3, according to embodiment 1 preparation method, wherein sintering temperature is 1300 DEG C, x=0.015, y=0.433, z=1.00.
The dielectric and voltage performance of testing example 2-16, the results are shown in Table 1:
Table 1
As can be seen from Table 1, work as x=0.015, when y=0.433, z=0.75, A doping neodymiums when B doping Sb, are burnt Junction temperature is 1300 DEG C, optimal performance: εT 330=5540, d33=880pC/N, kp=0.65.

Claims (5)

1. a kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, it is characterised in that: chemical constituent are as follows: Pb1-xMex(Ni1/ 3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A;
The Me is neodymium, and A is the oxide of antimony, x=0.015, y=0.433, z=0.75;
The preparation methods of the ceramics the following steps are included:
(1) prepared by wet feed: weighing raw material mixing sufficiently according to stoichiometry, dehydrated alcohol mixing and ball milling 4-8h is added, obtains wet Material;
(2) pre-burning forms: after the wet feed drying in step (1), being placed in corundum crucible and covers, in 750-850 DEG C of temperature After lower calcining 1-4h, then dehydrated alcohol mixing and ball milling 4-8h is used to obtain secondary wet feed, granulation will be added after the drying of secondary wet feed After agent is granulated, dry-pressing formed is blank;
(3) sintering polarization: gained blank is placed on corundum plate in batch-type furnace after 550 DEG C of heat preservation 3-5h, blank is placed in just Buried powder obtains porcelain billet in 1100~1300 DEG C of sintering 1-3h on beautiful plate, then by porcelain billet by after silver electrode in 30 DEG C of silicone oil at polarization Reason 5~10 minutes to get.
2. a kind of preparation method of modified lead nickle niobate-lead titanate piezoelectric ceramics according to claim 1, feature exist In: the following steps are included:
(1) prepared by wet feed: weighing raw material mixing sufficiently according to stoichiometry, dehydrated alcohol mixing and ball milling 4-8h is added, obtains wet Material;
(2) pre-burning forms: after the wet feed drying in step (1), being placed in corundum crucible and covers, in 750-850 DEG C of temperature After lower calcining 1-4h, then dehydrated alcohol mixing and ball milling 4-8h is used to obtain secondary wet feed, granulation will be added after the drying of secondary wet feed After agent is granulated, dry-pressing formed is blank;
(3) sintering polarization: gained blank is placed on corundum plate in batch-type furnace after 550 DEG C of heat preservation 3-5h, blank is placed in just Buried powder obtains porcelain billet in 1100~1300 DEG C of sintering 1-3h on beautiful plate, then by porcelain billet by after silver electrode in 30 DEG C of silicone oil at polarization Reason 5~10 minutes to get.
3. the preparation method of modified lead nickle niobate-lead titanate piezoelectric ceramics according to claim 2, it is characterised in that: Raw material described in step (1) is following components: PbO, NiO, Nb2O5、TiO2、ZrO2、Nd2O3And Sb2O3
4. the preparation method of modified lead nickle niobate-lead titanate piezoelectric ceramics according to claim 3, it is characterised in that: Granulating agent described in step (2) is polyvinyl alcohol.
5. the preparation method of modified lead nickle niobate-lead titanate piezoelectric ceramics according to claim 3, it is characterised in that: 1.5~2kV/mm of polarizing voltage of polarization process described in step (3).
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