CN110372381A - A kind of rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of texturing and preparation method thereof - Google Patents
A kind of rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of texturing and preparation method thereof Download PDFInfo
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Abstract
The present invention provides rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of a kind of texturing and preparation method thereof, composition is expressed by following general formula, [Rx‑Pb(1‑1.5x)][(Mg1/ 3Nb2/3)(1‑y)Tiy]O3- avol.%BaTiO3;Wherein, 0 < x≤0.03,0.29≤y≤0.325,0.01≤a≤0.1, x, y are molal quantity, and a is percentage by volume;RxFor Sm3+Or Dy3+One of;The present invention passes through rare earth modified first, and higher piezoelectric activity is realized in basis material;Then by texturing, ceramic crystalline grain is realized along a direction oriented growth, further improves the piezoelectric property of ceramic material;The rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of texturing prepared by the present invention is 40-90%, piezoelectric coefficient d along [001] direction texture degree3340%-80% is improved than unmodified non-textured ceramics;Dielectric constant under room temperature 1kHz frequency improves about 1.8-2 times than unmodified non-textured ceramics;It can be applied in the piezoelectric devices such as ultrasonic transducer, driver and sensor;Piezoceramic material of the invention is at low cost, and preparation process is simple, is conducive to industrialized production.
Description
Technical field
The invention belongs to ceramic material technical field, in particular to a kind of rare earth modified lead magnesio-niobate-titanium of texturing
Lead plumbate base piezoelectricity ferro ceramic material and preparation method thereof.
Background technique
As a kind of particularly important functional material of today's society, ferroelectric piezoelectric material since tool is there are two types of polar state,
Area information storage shows great application potential;Simultaneously because it can export electric signal under stress, otherwise
Strain can be generated under voltage driving, and be generally used as piezoelectric transducer, actuator, the core material of the devices such as energy converter,
In sonar contact, medical ultrasonic, information processing, environmental monitoring, micro-move device, the various fields such as communication are widely used.
(1-x)Pb(Mg1/3Nb2/3)O3-xPbTiO3(PMN-PT) relaxation piezoelectric monocrystal has the piezoelectric response of superelevation, pressure
Electrostrictive coefficient d33Up to 2800pC/N;PMN-PT is near the quasi- homotype phase boundary MPB of x=0.35 or so, with PbTiO3Component
Increase, experience is from tripartite mutually to the phase transformation of tetragonal phase;In the area MPB close to tripartite's phase side along [001]cThe monocrystalline of direction growth
Piezoelectric response with superelevation.Although PMN-PT monocrystalline has excellent performance, there are crystalline component and performance profile are uneven
The problems such as even and machining property is poor, in addition its complicated growth course, cost are quite high.Compared with monocrystalline, tradition
PMN-PT ceramics have the production cycle shorter, and cost is relatively low, is easy to the advantages of being mass produced.But due to traditional PMN-PT ceramics
Crystal grain orientation is random distribution so that the performance of all directions some canceled each other out, cause traditional PMN-PT to make pottery
The electric property of porcelain is very low.
Summary of the invention
For above-mentioned the technical problems existing in the prior art, the present invention provides a kind of rare earth modified magnoniobates of texturing
Lead-lead titanate piezoelectricity ferro ceramic material and preparation method thereof, to provide a kind of piezoelectricity ferro that electric property is more excellent
Ceramic material and preparation method thereof.
To realize the above-mentioned technical purpose, the technical solution of the present invention is as follows:
The present invention provides a kind of rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of texturing, groups
It is expressed at by following general formula, [Rx-Pb(1-1.5x)][(Mg1/3Nb2/3)(1-y)Tiy]O3- avol.%BaTiO3;Wherein, 0 < x≤
0.03,0.29≤y≤0.325,0.01≤a≤0.1, x, y are molal quantity, and a is percentage by volume;RxFor Sm3+Or Dy3+In one
Kind.
The present invention also provides a kind of systems of the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of texturing
Preparation Method, comprising the following steps:
Step 1, the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic matrix for preparing pure phase;Prepare perovskite
The BaTiO of structure3Template;
Step 2, by the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic matrix of pure phase and perovskite structure
BaTiO3Template is sufficiently mixed uniformly, obtains film forming slurry;
Film forming slurry is used casting technique by step 3, and membrane material is prepared;Then it dries, cuts, lamination is given birth to
Tile;
Ceramic chips are arranged and are glued by step 4, and sintering obtains the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity of texturing
Ferroelectric ceramic material.
Further, the rare earth modified lead magnesium niobate-lead titanate base of pure phase is prepared in step 1 using two step solid phase methods
Piezoelectricity ferro ceramic matrix, specifically includes the following steps:
S1, with MgO, Nb2O5For raw material, the MgNb of reaction synthesis pure phase2O6Presoma;
S2, the MgNb with pure phase2O6Presoma, PbO, TiO2And Sm2O3Or Dy2O3For raw material, ball milling mixing is dry, burns
Knot, obtains the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic matrix of pure phase.
Further, topochemistry crystallite conversion method is used in step 1, prepares the BaTiO of perovskite structure3When template,
Specifically includes the following steps:
S1, with Bi2O3And TiO2For raw material, by Bi2O3、TiO2After evenly mixing with fused salt one, in 1100-1200 DEG C of condition
Under, Bi is made4Ti3O12Powder;
S2, by Bi4Ti3O12Powder, BaCO3、TiO2After evenly mixing with fused salt two, it is made under the conditions of 1000-1100 DEG C
BaBi4Ti4O15Powder;
S3, by BaBi4Ti4O15Powder, BaCO3After evenly mixing with fused salt three, under the conditions of 900-1000 DEG C, calcium is obtained
The BaTiO of perovskite like structure3Template.
Further, the fused salt one in step S1 is the NaCl fused salt of molar ratio 1:1 and the mixture of KCl fused salt;Step
The BaCl that fused salt two in S2 is molar ratio 1:12·2H2The mixture of O fused salt and KCl fused salt;Fused salt three in step S3 is to rub
The mixture of your the NaCl fused salt and KCl fused salt than 1:1.
Further, in step 2 when preparation film forming slurry, specifically includes the following steps:
S1, pure phase in step 1 rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic matrix in be added it is molten
Agent and dispersing agent, ball milling make solvent infiltrate powder, obtain mixed system;
S2, the BaTiO that perovskite structure is added in mixed system3Template, binder and plasticizer, ball milling are sufficiently mixed
It closes, obtains uniform, stable film forming slurry.
Further, when preparing membrane material in step 3, the technique that the slurry that forms a film is carried out to tape casting on casting machine,
Curtain coating speed is 0.5-1cm/s, and curtain coating scraper height is 70-200 μm.
Further, by ceramic chips, the row of progress is viscous under the conditions of 550-600 DEG C of temperature in step 4;In 1210-1280 DEG C of temperature
It is sintered under the conditions of degree, sintering time 2-10h.
Further, Ball-milling Time is 13-20h in step S1;Dispersing agent uses phosphate, castor oil, three oleics
One of ester or herring oil.
Further, Ball-milling Time 13-20h in step S2;Binder uses PVB;Plasticizer is DBP, DOP or poly- second two
One or more of alcohol.
Compared with prior art, the beneficial effects of the present invention are:
The present invention provides a kind of rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic materials of texturing, pass through
Traditional PMN-PT ceramic material is modified using rare earth, then by texturing, so that the piezoelectric property of ceramic material has
Raising by a relatively large margin;The rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of the texturing of preparation is along [001] side
It is 40-90%, piezoelectric coefficient d to texture degree3340%-80% is improved than unmodified non-textured ceramics;Under room temperature 1kHz frequency
Dielectric constant than it is unmodified it is non-textured ceramics improve about 1.8-2 times;It can be applied to ultrasonic transducer, driver and sensor
In equal piezoelectric devices.
The present invention also provides a kind of systems of the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of texturing
Preparation Method realizes higher piezoelectric activity first by rare earth modified in basis material;Then it by texturing, realizes
Ceramic crystalline grain further improves the piezoelectric property of ceramic material along a direction oriented growth;Piezoelectric ceramics material of the invention
Expect at low cost, preparation process is simple, is conducive to industrialized production.
Further, the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramics of the pure phase prepared by two-step method
Matrix has single Perovskite Phase structure, generates without Jiao Lvshi phase.
Further, with topochemistry crystallite conversion method, the BaTiO for the perovskite structure being prepared3Template has piece
Shape microscopic appearance, width are about 5-15 μm, and thickness is about 0.5-1 μm;Dimensional homogeneity is good, powder granule favorable dispersibility,
Reunite without obvious.
Further, the membrane material surfacing prepared using casting technique, without External Defects such as crackle and bubbles;Stream
Prolong after film cut, laminated, diameter 8-10mm, with a thickness of 0.5-1mm.
A kind of preparation of the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of texturing of the present invention
Method, by being modified to traditional PMN-PT ceramic material, and by texturing so that the piezoelectric property of ceramic material have compared with
It is greatly improved.First by rare earth modified, higher piezoelectric activity is realized in basis material;Again by texturing, make
Ceramic crystalline grain further increases the piezoelectric property of ceramic material along a direction oriented growth, can significantly improve dependent piezoelectric material
The cost performance and the market competitiveness of material;Technique used in the present invention have equipment it is simple, high production efficiency, it is easy to accomplish from
The advantages that dynamicization is produced in enormous quantities, and industrial production is suitable for.
Detailed description of the invention
Fig. 1 is the BaTiO of perovskite structure of the present invention3The SEM of template schemes;
Fig. 2 is the XRD spectrum for the piezoelectricity ferro ceramic material that embodiment 1 obtains;
Fig. 3 is dielectric thermogram of the obtained piezoelectricity ferro ceramic material of embodiment 1 under room temperature 1kHz frequency;
Fig. 4 is the SEM image in the piezoelectricity ferro ceramic material sample section that embodiment 1 obtains;
Fig. 5 is the XRD spectrum for the piezoelectricity ferro ceramic material that embodiment 2 obtains;
Fig. 6 is the SEM image in the piezoelectricity ferro ceramic material sample section that embodiment 2 obtains.
Specific embodiment
Specific embodiments of the present invention are given below, it should be noted that the invention is not limited to implement in detail below
Example, all equivalent transformations made on the basis of the technical solutions of the present application each fall within protection scope of the present invention.
The rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of a kind of texturing of the present invention is changed
Learn general formula are as follows: [Rx-Pb(1-1.5x)][(Mg1/3Nb2/3)(1-y)Tiy]O3- avol.%BaTiO3;Wherein, 0 < x≤0.03,0.29≤y
≤ 0.325,0.01≤a≤0.1;X, y are molal quantity in general formula, and a is percentage by volume;RxFor Sm3+Or Dy3+One of.
A kind of preparation of the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of texturing provided by the invention
Method, specifically includes the following steps:
Step 1, using CP or AR grades PbO, MgO, Nb2O5、TiO2And Sm2O3Or Dy2O3For raw material, pass through two step solid phases
The rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic matrix of pure phase is prepared in reaction method;
Specifically, using MgO and Nb first2O5Reaction synthesis pure phase MgNb2O6Presoma, then by pure phase MgNb2O6Before
Drive body, PbO, TiO2And Sm2O3Or Dy2O3Ball milling mixing, dry, sintering obtains the rare earth modified lead magnesium niobate-lead titanate of pure phase
Base piezoelectricity ferro ceramic matrix;
Step 2, using Bi2O3、TiO2And BaCO3For raw material, by topochemistry crystallite conversion method, under fused salt environment,
The BaTiO of perovskite structure is prepared3Template;
Specifically, first by Bi2O3、TiO2After evenly mixing with fused salt one, it under the conditions of 1100-1200 DEG C, is made
Bi4Ti3O12Powder;Then by Bi4Ti3O12Powder, BaCO3、TiO2After evenly mixing with fused salt two, in 1000-1100 DEG C of condition
BaBi is made down4Ti4O15Powder;By BaBi4Ti4O15Powder, BaCO3After evenly mixing with fused salt three, in 900-1000 DEG C of condition
Under, obtain the BaTiO of perovskite structure3Template;Wherein, fused salt one is the mixing of the NaCl fused salt and KCl fused salt of molar ratio 1:1
Object;The BaCl that fused salt two in step S2 is molar ratio 1:12·2H2The mixture of O fused salt and KCl fused salt;It is molten in step S3
Salt three is the NaCl fused salt of molar ratio 1:1 and the mixture of KCl fused salt
Step 3, firstly, the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic base that pure phase will be obtained in step 1
After body and dispersant, solvent is added and is opened its particle agglomeration by ball milling, and solvent is made to infiltrate powder, is mixed
System;Then the BaTiO of the perovskite structure in step 2 is added in mixed system3Template, binder and plasticizer, pass through
Ball milling is sufficiently mixed, and the film forming slurry of stable homogeneous is obtained;
Film forming slurry in step 3 is carried out tape casting by step 4 on casting machine, and curtain coating speed is 0.5-1cm/s,
Being cast scraper height is 70-200 μm;Biscuit film is obtained after drying;Biscuit film is cut, lamination, obtains required shape
Ceramic chips;
Step 5, by ceramic chips, the row of progress is viscous at 550-600 DEG C, is then sintered 2-10h under the conditions of 1210-1280 DEG C,
Obtain piezoceramic material.
Embodiment 1
The composition of the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of texturing are as follows:
[Rx-Pb(1-1.5x)][(Mg1/3Nb2/3)(1-y)Tiy]O3- avol.%BaTiO3;
Wherein, R=Sm3+, x=0.01, y=0.29, a=0.05.
Step 1, using CP or AR grades PbO, MgO, Nb2O5、TiO2And Sm2O3It is sufficiently spare after drying for raw material;It utilizes
MgO and Nb2O5Reaction synthesis pure phase MgNb2O6Presoma, then by pure phase MgNb2O6Presoma and PbO, TiO2And Sm2O3Ball milling
Mixing, dry, sintering obtains the rare earth modified lead magnesium niobate-lead titanate ceramic matrix of pure phase;
Step 2, by Bi2O3、TiO2With fused salt one after evenly mixing under the conditions of 1100-1200 DEG C, Bi is made4Ti3O12Powder
Body, wherein fused salt one is the NaCl fused salt of molar ratio 1:1 and the mixture of KCl fused salt;By Bi4Ti3O12Powder, BaCO3、TiO2
It is mixed with fused salt two, BaBi is made under the conditions of 1000-1100 DEG C4Ti4O15Powder;Wherein, fused salt two is molar ratio 1:1
BaCl2·2H2The mixture of O fused salt and KCl fused salt;By BaBi4Ti4O15Powder, BaCO3It is mixed with fused salt three, in 900-
The BaTiO of perovskite structure is obtained under the conditions of 1000 DEG C3Template;Wherein, fused salt three is the NaCl fused salt and KCl of molar ratio 1:1
The mixture of fused salt;
Step 3 after obtaining rare earth modified lead magnesium niobate-lead titanate ceramic matrix and dispersant in step 1, is added
In alcohol, by ball milling 13h, its particle agglomeration is opened, and alcohol is made to infiltrate powder, wherein dispersing agent uses phosphate, castor
One of sesame oil, olein or herring oil;Then the BaTiO of the perovskite structure in step 2 is added3Template is glued
Knot agent and plasticizer are sufficiently mixed by ball milling 13h, obtain the film forming slurry of stable homogeneous;Wherein binder uses
PVB, one or more of plasticizer DBP, DOP or polyethylene glycol;
Film forming slurry in step 3 is carried out tape casting by step 4 on casting machine, and curtain coating speed is 0.78cm/s, stream
The height for prolonging scraper is set as 90 μm;Biscuit film is obtained after drying;Biscuit film is cut, lamination, obtains required shape
Ceramic chips;
Step 5, by ceramic chips, the row of progress is viscous at 550 DEG C, is then sintered 2h under the conditions of 1280 DEG C, it is dilute to obtain texturing
Land reform lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material.
Attached drawing 1 is the BaTiO of perovskite structure3Template SEM figure, it can be seen that template has good sheet-like morphology, ruler
More uniform, the favorable dispersibility of very little distribution.
Attached drawing 2 is the XRD diagram of piezoelectricity ferro ceramic material sample in embodiment 1, and ceramics are pure calcium as we can see from the figure
Perovskite like structure, no Jiao Lvshi phase generate, and texture degree is about 62%.
Attached drawing 3 is dielectric thermogram of the piezoelectricity ferro ceramic material sample under room temperature 1kHz frequency in embodiment 1, from figure
In the available ceramic material TmIt is 105 DEG C.
Attached drawing 4 is the SEM figure in piezoelectricity ferro ceramic material sample section in embodiment 1, it can be observed that the piezoelectricity ferro
Ceramic material structure is comparatively dense, and crystallite dimension is about 5-15 μm, quasi-static d33Tester is tested to obtain d33Value is 890-
930pC/N, the same component matrix ceramics compared to common process preparation improve about 70%.
Embodiment 2
The composition of the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of texturing are as follows:
[Rx-Pb(1-1.5x)][(Mg1/3Nb2/3)(1-y)Tiy]O3- avol.%BaTiO3;
Wherein, R=Sm3+, x=0.025, y=0.29, a=0.05.
Step 1, using CP or AR grades PbO, MgO, Nb2O5、TiO2And Sm2O3It is sufficiently spare after drying for raw material;It utilizes
MgO and Nb2O5Reaction synthesis pure phase MgNb2O6Presoma, then by pure phase MgNb2O6Presoma and PbO, TiO2And Sm2O3Ball milling
Mixing, dry, sintering obtains the rare earth modified lead magnesium niobate-lead titanate ceramic matrix of pure phase;
Step 2, by Bi2O3、TiO2With fused salt one after evenly mixing under the conditions of 1100-1200 DEG C, Bi is made4Ti3O12Powder
Body, wherein fused salt one is the NaCl fused salt of molar ratio 1:1 and the mixture of KCl fused salt;By Bi4Ti3O12Powder, BaCO3、TiO2
It is mixed with fused salt two, BaBi is made under the conditions of 1000-1100 DEG C4Ti4O15Powder;Wherein, fused salt two is molar ratio 1:1
BaCl2·2H2The mixture of O fused salt and KCl fused salt;By BaBi4Ti4O15Powder, BaCO3It is mixed with fused salt three, in 900-
The BaTiO of perovskite structure is obtained under the conditions of 1000 DEG C3Template;Wherein, fused salt three is the NaCl fused salt and KCl of molar ratio 1:1
The mixture of fused salt;
Step 3 after obtaining rare earth modified lead magnesium niobate-lead titanate ceramic matrix and dispersant in step 1, is added
In alcohol, by ball milling 15h, its particle agglomeration is opened, and alcohol is made to infiltrate powder, wherein dispersing agent uses phosphate, castor
One of sesame oil, olein or herring oil;Then the BaTiO of the perovskite structure in step 2 is added3Template is glued
Knot agent and plasticizer are sufficiently mixed by ball milling 15h, obtain the film forming slurry of stable homogeneous;Wherein binder uses
PVB, one or more of plasticizer DBP, DOP or polyethylene glycol;
Film forming slurry in step 3 is carried out tape casting by step 4 on casting machine, and curtain coating speed is 0.5cm/s, stream
The height for prolonging scraper is set as 70 μm;Biscuit film is obtained after drying;Biscuit film is cut, lamination, obtains required shape
Ceramic chips;
Step 5, by ceramic chips, the row of progress is viscous at 580 DEG C, is then sintered 4h under the conditions of 1260 DEG C, it is dilute to obtain texturing
Land reform lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material.
Attached drawing 5 is the XRD diagram of piezoelectricity ferro ceramic material sample in embodiment 2, it can be seen that ceramics are pure perovskite knot
Structure, no Jiao Lvshi phase generate, and texture degree is about 47%.
Attached drawing 6 is the SEM figure in piezoelectricity ferro ceramic material sample section in embodiment 2, it can be observed that the piezoelectricity ferro
Ceramic material structure is comparatively dense, and crystallite dimension is about 5-15 μm;Show the reliability and high sensitivity of the method;It is quasi-static
d33Tester is tested to obtain d33Value is 800-880pC/N, and the non-textured ceramics compared to unmodified same PT content improve about
60%.
Embodiment 3
The composition of the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of texturing are as follows:
[Rx-Pb(1-1.5x)][(Mg1/3Nb2/3)(1-y)Tiy]O3- avol.%BaTiO3;
Wherein, R=Sm3+, x=0.025, y=0.29, a=0.02.
Step 1, using CP or AR grades PbO, MgO, Nb2O5、TiO2And Sm2O3It is sufficiently spare after drying for raw material;It utilizes
MgO and Nb2O5Reaction synthesis pure phase MgNb2O6Presoma, then by pure phase MgNb2O6Presoma and PbO, TiO2And Sm2O3Ball milling
Mixing, dry, sintering obtains the rare earth modified lead magnesium niobate-lead titanate ceramic matrix of pure phase;
Step 2, by Bi2O3、TiO2With fused salt one after evenly mixing under the conditions of 1100-1200 DEG C, Bi is made4Ti3O12Powder
Body, wherein fused salt one is the NaCl fused salt of molar ratio 1:1 and the mixture of KCl fused salt;By Bi4Ti3O12Powder, BaCO3、TiO2
It is mixed with fused salt two, BaBi is made under the conditions of 1000-1100 DEG C4Ti4O15Powder;Wherein, fused salt two is molar ratio 1:1
BaCl2·2H2The mixture of O fused salt and KCl fused salt;By BaBi4Ti4O15Powder, BaCO3It is mixed with fused salt three, in 900-
The BaTiO of perovskite structure is obtained under the conditions of 1000 DEG C3Template;Wherein, fused salt three is the NaCl fused salt and KCl of molar ratio 1:1
The mixture of fused salt;
Step 3 after obtaining rare earth modified lead magnesium niobate-lead titanate ceramic matrix and dispersant in step 1, is added
In alcohol, by ball milling 18h, its particle agglomeration is opened, and alcohol is made to infiltrate powder, wherein dispersing agent uses phosphate, castor
One of sesame oil, olein or herring oil;Then the BaTiO of the perovskite structure in step 2 is added3Template is glued
Knot agent and plasticizer are sufficiently mixed by ball milling 17h, obtain the film forming slurry of stable homogeneous;Wherein binder uses
PVB, one or more of plasticizer DBP, DOP or polyethylene glycol;
Film forming slurry in step 3 is carried out tape casting by step 4 on casting machine, and curtain coating speed is 0.5cm/s, stream
The height for prolonging scraper is set as 120 μm;Biscuit film is obtained after drying;Biscuit film is cut, lamination, obtains required shape
Ceramic chips;
Step 5, by ceramic chips, the row of progress is viscous at 580 DEG C, is then sintered 10h under the conditions of 1210 DEG C, obtains texturing
Rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material.
Piezoelectricity ferro ceramic material structure is comparatively dense in embodiment 3, and crystallite dimension is about 5-15 μm;Quasi-static d33Test
Instrument is tested to obtain d33Value is 1100-1200pC/N, and the non-textured ceramics compared to unmodified same PT content improve about 80%;Room
The lower dielectric constant of temperature is 6240, and the non-textured ceramics compared to unmodified same PT content improve about 2 times.
Embodiment 4
The composition of the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of texturing are as follows:
[Rx-Pb(1-1.5x)][(Mg1/3Nb2/3)(1-y)Tiy]O3- avol.%BaTiO3;
Wherein, R=Dy3+, x=0.03, y=0.325, a=0.1.
Step 1, using CP or AR grades PbO, MgO, Nb2O5、TiO2And Dy2O3It is sufficiently spare after drying for raw material;It utilizes
MgO and Nb2O5Reaction synthesis pure phase MgNb2O6Presoma, then by pure phase MgNb2O6Presoma and PbO, TiO2And Dy2O3Ball milling
Mixing, dry, sintering obtains the rare earth modified lead magnesium niobate-lead titanate ceramic matrix of pure phase;
Step 2, by Bi2O3、TiO2With fused salt one after evenly mixing under the conditions of 1100-1200 DEG C, Bi is made4Ti3O12Powder
Body, wherein fused salt one is the NaCl fused salt of molar ratio 1:1 and the mixture of KCl fused salt;By Bi4Ti3O12Powder, BaCO3、TiO2
It is mixed with fused salt two, BaBi is made under the conditions of 1000-1100 DEG C4Ti4O15Powder;Wherein, fused salt two is molar ratio 1:1
BaCl2·2H2The mixture of O fused salt and KCl fused salt;By BaBi4Ti4O15Powder, BaCO3It is mixed with fused salt three, in 900-
The BaTiO of perovskite structure is obtained under the conditions of 1000 DEG C3Template;Wherein, fused salt three is the NaCl fused salt and KCl of molar ratio 1:1
The mixture of fused salt;
Step 3 after obtaining rare earth modified lead magnesium niobate-lead titanate ceramic matrix and dispersant in step 1, is added
In alcohol, by ball milling 20h, its particle agglomeration is opened, and alcohol is made to infiltrate powder, wherein dispersing agent uses phosphate, castor
One of sesame oil, olein or herring oil;Then the BaTiO of the perovskite structure in step 2 is added3Template is glued
Knot agent and plasticizer are sufficiently mixed by ball milling 20h, obtain the film forming slurry of stable homogeneous;Wherein binder uses
PVB, one or more of plasticizer DBP, DOP or polyethylene glycol;
Film forming slurry in step 3 is carried out tape casting by step 4 on casting machine, and curtain coating speed is 1.0cm/s, stream
The height for prolonging scraper is set as 200 μm;Biscuit film is obtained after drying;Biscuit film is cut, lamination, obtains required shape
Ceramic chips;
Step 5, by ceramic chips, the row of progress is viscous at 600 DEG C, is then sintered 6h under the conditions of 1235 DEG C, it is dilute to obtain texturing
Land reform lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material.
Piezoelectricity ferro ceramic material sample is pure perovskite structure in embodiment 4, and no Jiao Lvshi phase generates, and texture degree is about
70%;The piezoelectricity ferro ceramic material sample structure is comparatively dense, and crystallite dimension is about 5-15 μm;Quasi-static d33Tester test
Obtain d33Value is 900-920pC/N, and the non-textured ceramics compared to unmodified same PT content improve about 40%.
Embodiment 5
The composition of the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of texturing are as follows:
[Rx-Pb(1-1.5x)][(Mg1/3Nb2/3)(1-y)Tiy]O3- avol.%BaTiO3;
Wherein, R=Sm3+, x=0.01, y=0.325, a=0.01.
Step 1 weighs required PbO, MgO, Nb according to above-mentioned chemical formula composition2O5、TiO2And Sm2O3, sufficiently after drying
It is spare;Utilize MgO and Nb2O5Reaction synthesis pure phase MgNb2O6Presoma, then by pure phase MgNb2O6Presoma and PbO, TiO2
And Sm2O3Ball milling mixing, dry, sintering obtains the rare earth modified lead magnesium niobate-lead titanate ceramic matrix of pure phase;
Step 2, by Bi2O3、TiO2With fused salt one after evenly mixing under the conditions of 1100-1200 DEG C, Bi is made4Ti3O12Powder
Body, wherein fused salt one is the NaCl fused salt of molar ratio 1:1 and the mixture of KCl fused salt;By Bi4Ti3O12Powder, BaCO3、TiO2
It is mixed with fused salt two, BaBi is made under the conditions of 1000-1100 DEG C4Ti4O15Powder;Wherein, fused salt two is molar ratio 1:1
BaCl2·2H2The mixture of O fused salt and KCl fused salt;By BaBi4Ti4O15Powder, BaCO3It is mixed with fused salt three, in 900-
The BaTiO of perovskite structure is obtained under the conditions of 1000 DEG C3Template;Wherein, fused salt three is the NaCl fused salt and KCl of molar ratio 1:1
The mixture of fused salt;
Step 3 after obtaining rare earth modified lead magnesium niobate-lead titanate ceramic matrix and dispersant in step 1, is added
In alcohol, by ball milling 20h, its particle agglomeration is opened, and alcohol is made to infiltrate powder, wherein dispersing agent uses phosphate, castor
One of sesame oil, olein or herring oil;Then the BaTiO of the perovskite structure in step 2 is added3Template is glued
Knot agent and plasticizer are sufficiently mixed by ball milling 20h, obtain the film forming slurry of stable homogeneous;Wherein binder uses
PVB, plasticizer are DOP and polyethylene glycol;
Film forming slurry in step 3 is carried out tape casting by step 4 on casting machine, and curtain coating speed is 0.5cm/s, stream
The height for prolonging scraper is set as 100 μm;Biscuit film is obtained after drying;Biscuit film is cut, lamination, obtains required shape
Ceramic chips;
Step 5, by ceramic chips, the row of progress is viscous at 600 DEG C, is then sintered 10h under the conditions of 1260 DEG C, obtains texturing
Rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material.
Piezoelectricity ferro ceramic material sample is pure perovskite structure in embodiment 5, and no Jiao Lvshi phase generates;The piezoelectricity ferro
Ceramic material sample structure is comparatively dense, and crystallite dimension is about 5-15 μm;Quasi-static d33Tester is tested to obtain d33Value is 880-
916pC/N, the non-textured ceramics compared to unmodified same PT content improve about 40%.
A kind of preparation of the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of texturing of the present invention
Method, by being modified to traditional PMN-PT ceramic material, and by texturing so that the piezoelectric property of ceramic material have compared with
It is greatly improved.First by rare earth modified, higher piezoelectric activity is realized in basis material;Again by texturing, make
Ceramic crystalline grain further increases the piezoelectric property of ceramic material along a direction oriented growth, can significantly improve dependent piezoelectric material
The cost performance and the market competitiveness of material;Technique used in the present invention have equipment it is simple, high production efficiency, it is easy to accomplish from
The advantages that dynamicization is produced in enormous quantities, and industrial production is suitable for.
XRD test data is to be tested to obtain with the sharp shadow X-ray diffractometer of Panaco company Empyrean in the present invention,
Dielectric modal data is tested to obtain using 4980 dielectric spectrometer of Agilent, and SEM image is FEI Co. Quanta 250FEG environment
Scanning electron microscope test obtains.
Claims (10)
1. a kind of rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of texturing, which is characterized in that its form by
Following general formula expression, [Rx-Pb(1-1.5x)][(Mg1/3Nb2/3)(1-y)Tiy]O3- avol.%BaTiO3;Wherein, 0 < x≤0.03,
0.29≤y≤0.325,0.01≤a≤0.1, x, y are molal quantity, and a is percentage by volume;RxFor Sm3+Or Dy3+One of.
2. the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of a kind of texturing according to claim 1
Preparation method, which comprises the following steps:
Step 1, the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic matrix for preparing pure phase;Prepare perovskite structure
BaTiO3Template;
Step 2, by the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic matrix of pure phase and perovskite structure
BaTiO3Template is sufficiently mixed uniformly, obtains film forming slurry;
Film forming slurry is used casting technique by step 3, and membrane material is prepared;Then it dries, cuts, lamination obtains green
Piece;
Ceramic chips are arranged and are glued by step 4, and sintering obtains the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro of texturing
Ceramic material.
3. the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of a kind of texturing according to claim 2
Preparation method, which is characterized in that rare earth modified lead magnesio-niobate-titanium of pure phase is prepared using two step solid phase methods in step 1
Lead plumbate base piezoelectricity ferro ceramic matrix, specifically includes the following steps:
S1, with MgO, Nb2O5For raw material, the MgNb of reaction synthesis pure phase2O6Presoma;
S2, the MgNb with pure phase2O6Presoma, PbO, TiO2And Sm2O3Or Dy2O3For raw material, ball milling mixing is dry, and sintering obtains
To the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic matrix of pure phase.
4. the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of a kind of texturing according to claim 2
Preparation method, which is characterized in that in step 1 use topochemistry crystallite conversion method, prepare the BaTiO of perovskite structure3Mould
When plate, specifically includes the following steps:
S1, with Bi2O3And TiO2For raw material, by Bi2O3、TiO2After evenly mixing with fused salt one, under the conditions of 1100-1200 DEG C,
Bi is made4Ti3O12Powder;
S2, by Bi4Ti3O12Powder, BaCO3、TiO2After evenly mixing with fused salt two, it is made under the conditions of 1000-1100 DEG C
BaBi4Ti4O15Powder;
S3, by BaBi4Ti4O15Powder, BaCO3After evenly mixing with fused salt three, under the conditions of 900-1000 DEG C, perovskite is obtained
The BaTiO of structure3Template.
5. the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of a kind of texturing according to claim 4
Preparation method, which is characterized in that fused salt one in step S1 is the NaCl fused salt of molar ratio 1:1 and the mixture of KCl fused salt;
The BaCl that fused salt two in step S2 is molar ratio 1:12·2H2The mixture of O fused salt and KCl fused salt;Fused salt three in step S3
For the NaCl fused salt of molar ratio 1:1 and the mixture of KCl fused salt.
6. the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of a kind of texturing according to claim 2
Preparation method, which is characterized in that in step 2 preparation film forming slurry when, specifically includes the following steps:
S1, pure phase in step 1 rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic matrix in be added solvent and
Dispersing agent, ball milling make solvent infiltrate powder, obtain mixed system;
S2, the BaTiO that perovskite structure is added in mixed system3Template, binder and plasticizer, ball milling are sufficiently mixed, and are obtained
Uniform, stable film forming slurry.
7. the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of a kind of texturing according to claim 2
Preparation method, which is characterized in that when preparing membrane material in step 3, will film forming slurry tape casting is carried out on casting machine
Technique, curtain coating speed are 0.5-1cm/s, and curtain coating scraper height is 70-200 μm.
8. the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of a kind of texturing according to claim 6
Preparation method, which is characterized in that by ceramic chips, the row of progress is viscous under the conditions of 550-600 DEG C of temperature in step 4;In 1210-
It is sintered under the conditions of 1280 DEG C of temperature, sintering time 2-10h.
9. the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of a kind of texturing according to claim 6
Preparation method, which is characterized in that in step S1 Ball-milling Time be 13-20h;Dispersing agent uses phosphate, castor oil, three oleic acid
One of glyceride or herring oil.
10. the rare earth modified lead magnesium niobate-lead titanate base piezoelectricity ferro ceramic material of a kind of texturing according to claim 2
Preparation method, which is characterized in that Ball-milling Time 13-20h in step S2;Binder uses PVB;Plasticizer be DBP, DOP or
One or more of polyethylene glycol.
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CN114621009A (en) * | 2022-03-16 | 2022-06-14 | 南京理工大学 | Lead magnesium niobate-lead titanate-based piezoelectric ceramic material and preparation method thereof |
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Cited By (5)
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CN113563076A (en) * | 2021-07-23 | 2021-10-29 | 华南理工大学 | Relaxation ferroelectric ceramic with high field strain temperature stability and preparation method thereof |
CN114349506A (en) * | 2022-01-07 | 2022-04-15 | 森霸传感科技股份有限公司 | Preparation method and application of low-loss high-dielectric-constant lead magnesium niobate-lead titanate dielectric ceramic material |
CN114621009A (en) * | 2022-03-16 | 2022-06-14 | 南京理工大学 | Lead magnesium niobate-lead titanate-based piezoelectric ceramic material and preparation method thereof |
CN114621009B (en) * | 2022-03-16 | 2023-02-28 | 南京理工大学 | Lead magnesium niobate-lead titanate-based piezoelectric ceramic material and preparation method thereof |
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