CN109320235A - A kind of piezoelectric structured ceramics of NBT base and preparation method thereof - Google Patents

A kind of piezoelectric structured ceramics of NBT base and preparation method thereof Download PDF

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CN109320235A
CN109320235A CN201811230303.7A CN201811230303A CN109320235A CN 109320235 A CN109320235 A CN 109320235A CN 201811230303 A CN201811230303 A CN 201811230303A CN 109320235 A CN109320235 A CN 109320235A
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preparation
ceramics
nbt
piezoelectric structured
piezoelectric
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张昌松
赵珂迪
陈勃新
王楚
郭晨洁
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a kind of NBT base leadless piezoelectricity textured ceramics and preparation method thereof, bismuth-sodium titanate powder is prepared using solid phase method, molten-salt growth method prepares sheet-like barium titanate crystallite, by 0.94NBT-0.06BT powder and organic binder, slurry is made in uniform stirring on magnetic stirring apparatus, the slurry prepared is injected in barrel, it pushes the material grain in barrel to pass through electric field generation device and temperature heating zone along barrel by screw rod, has in effigurate mold by nozzle injection.It is degreased and sintered in normal pressure-sintered furnace after ceramic green cooling and demolding, the two sides of sintered part applies silver paste, it is placed in polarization device and polarizes by silver-colored sintered part, through comparing the 0.94NBT-0.06BT piezoelectric ceramics for using the 0.94NBT-0.06BT piezoelectric ceramics performance of extra electric field injection moulding preparation to be higher than conventional solid-state method preparation, and prepared by injection moulding piezoelectric ceramics is high-efficient, the period is short, is easy to produce in batches.

Description

A kind of piezoelectric structured ceramics of NBT base and preparation method thereof
Technical field
The invention belongs to piezoelectric ceramics and preparation technical fields, and in particular to a kind of NBT base is piezoelectric structured ceramic and its makes Preparation Method.
Background technique
There is piezoelectric ceramics excellent electromechanical transformation energy to have been widely used for the neck such as sensor, driver, energy converter Domain.Conventional piezoelectric ceramics such as lead zirconate titanate (PZT) main component lead oxide can be brought in use very big to environment and human health Damage.Therefore developing leadless piezoelectric ceramics has great Practical significance.
Although domestic and foreign scholars have carried out a large amount of research in terms of leadless piezoelectric ceramics and have achieved phasic results, But do not find that one kind in terms of piezoelectric property and temperature stability, can really substitute the leadless piezoelectric ceramics of PZT ceramics yet.Mesh Before, many experiments in the piezoelectric ceramics that a certain polarization direction possesses height crystal grain orientation (highly-textured degree) it was demonstrated that will show Substantially it is better than the electrical property of non-textured ceramics.The preparation of textured ceramic can apply mechanical force, electric field by adding template grains Or it is obtained using the methods of temperature gradient.And ceramic injection forming technology (CIM) is a kind of near net-shape ceramics plastic molding Method, the especially batch production to high, the complex-shaped ceramic of dimension precision requirement, have at home and abroad obtained extensive Research and application.
Summary of the invention
The problems such as in order to improve existing leadless piezoelectric ceramics high performance requirements, the object of the present invention is to provide one kind to be injected into Type mode prepares leadless piezoelectric structured ceramics, micro- in the anisotropic crystal grain orienting of power drive and electric field driven crystallite using injecting The orientation problem that farmland turns to prepares high-performance Pb-free piezoelectric ceramics, which is suitble to prepare high performance piezoelectric textured ceramic.
To achieve the goals above, the technical solution of the present invention is as follows: a kind of piezoelectric structured ceramics of NBT base, with 0.94Na0.5Bi0.5TiO3-0.06BaTiO3Powder is that raw material is sintered.
A kind of method that the piezoelectric structured ceramic system of NBT is standby, comprising the following steps:
(1) bismuth-sodium titanate (Na is prepared0.5Bi0.5TiO3) powder；
(2) anisotropic BaTiO is prepared using molten-salt growth method3Crystallite, the BaTiO3Crystallite is sheet；
(3) barium titanate obtained by step (2) is introduced into bismuth-sodium titanate (Na prepared by step (1)0.5Bi0.5TiO3) in powder Prepare 0.94Na0.5Bi0.5TiO3-0.06BaTiO3(0.94NBT-0.06BT) ceramic powder；
(4) hybrid ceramic powder and organic binder: ceramic powder and organic binder are mixed in magnetic stirring apparatus It is even to obtain injection molding mixture.
The powder is 0.94Na0.5Bi0.5TiO3-0.06BaTiO3Ceramic powder, wherein 0.94Na0.5Bi0.5TiO3- 0.03BaTiO3Powder is using conventional solid-state method by BiO2、Na2CO3、Ba2CO3、TiO2By mixing, ball milling, pre-burning, secondary The dry preparation of ball milling, prepares anisotropic BaTiO using molten-salt growth method3Crystallite, from crystal morphology anisotropy and performance respectively to Anisotropic angle is set out, by the BaTiO of sheet3Crystallite is introduced into injection molding powder component, to realize each of crystal structure Anisotropy, the organic binder are polyvinyl alcohol (PVA) solution of 3wt%~5wt% with mass percentage concentration.
(5) be injection moulded: slurry injection moulding on injection moulding platform obtains green body, injection temperature range 60~100 DEG C, demoulding obtains molding blank in 1~3min after injection mold, and injection pressure is 1~3MPa, while in injection process, The two sides extra electric field of barrel, electric field strength range: 1~10KV/mm.By way of extra electric field and the combination of injection force is real The double orientation of existing structure and performance, the high 0.94Na of preparation orientation consistency0.5Bi0.5TiO3-0.06BaTiO3Ceramics.
(6) degrease and sinter: ceramic green carries out in normal pressure-sintered furnace, in order to prevent green compact during heating Green compact contraction is set unevenly sample to be caused to crack in thickness direction and the radial gradation of moisture that generates, with 2 DEG C/min before degreasing Rate be warming up to 120 DEG C, heat preservation 30min sloughs the moisture of green compact, rise to 500 DEG C again after having kept the temperature with the rate of 2 DEG C/min, 2h is kept the temperature, to ensure that binder is excluded entirely；Then 1050 DEG C of sintering are risen to 2 DEG C/min of heating rate, keeps the temperature 2h with true It protects binder to be excluded entirely, furnace cooling after being reduced to 500 DEG C at the same rate obtains ceramic component.
(7) polarize: sintered potsherd is polishing to 1~1.5mm thickness, applies silver, the heating of 2 DEG C/min in potsherd two sides Rate rises to 550 DEG C and keeps the temperature 30min, after with furnace natural cooling, the potsherd after silver ink firing is put into 70 DEG C of methyl-silicone oils, additional It polarizes 20 minutes in 3KV/mm DC electric field.
Compared with prior art, the present invention at least has the advantages that can make piezoelectricity make pottery using injection molding technology Porcelain products are produced in batches, are with short production cycle, high-efficient, and can be conducive to improve the piezoelectric property of piezoelectric ceramics；Using note The stomata for penetrating the molding 0.94NBT-0.06BT ceramic microstructures crystal grain of method significantly reduces, and consistency improves, and crystal grain is uniform；Injection method The density of the 0.94NBT-0.06BT leadless piezoelectric ceramics of preparation is 5.54gcm-3, piezoelectric constant d33=138pC/N, dielectric Constant ε=1436；It is superior to the 0.94NBT-0.06BT leadless piezoelectric ceramics of conventional solid-state method preparation.
Detailed description of the invention
Fig. 1 is the piezoelectric structured ceramic injection forming schematic diagram of NBT base of the present invention.
Fig. 2 is the X ray diffracting spectrum of 0.94NBT-0.06BT ceramics.
Fig. 3 is the SEM figure of the 0.94NBT-0.06BT ceramics of solid phase method preparation.
Fig. 4 is the SEM figure of the 0.94NBT-0.06BT ceramics of injection method preparation.
In attached drawing: 1- barrel, 2- screw rod, 3- hopper, 4- heating apparatus, 5- extra electric field, 6- nozzle, 7- mold, 8- are de- Rouge device, 9- sintering equipment.
Specific embodiment
The present invention will be further described with reference to the accompanying drawings and detailed description.
A kind of NBT base leadless piezoelectricity textured ceramic preparation process, including following preparation step:
Step 1) sheet BaTiO3Preparation: by BaCO3, TiO2, NaCl-KCl obtains ball milling material through dehydrated alcohol wet-milling, dries Intermediate product Ba is obtained in 950 degrees Celsius of lower synthetic reaction 3h after dry4Ti13O30, by intermediate product and BaCO3Mixing and ball milling is done Dry, sintering, obtains sheet BaTiO3。
Step 2) 0.94Na0.5Bi0.5TiO3-0.06BaTiO3Powder preparation: using conventional solid-state method by BiO2、Na2CO3、 Ba2CO3、TiO2By mixing, ball milling, pre-burning, the dry preparation of secondary ball milling.By sheet BaTiO3Crystallite and Na0.5Bi0.5TiO3Powder Body mixing and ball milling, drying.
Step 3) wet end furnish: it by powder and bonding agent, at a certain temperature, stirs 1 hour and makes on magnetic stirring apparatus It is standby to arrive uniform slurry.
Step 4) injection moulding: the slurry prepared is packed into hopper 3, is moved from hydraulic coupling lead-screw 2 to 7 direction of mold Dynamic, material grain flows into barrel 1 through hopper 3, and the screw rod 2 with pressure pushes the material grain in barrel 1 to fill along barrel by electric field 5 and temperature heating zone 4 are set, crystallite when by certain outer plus field strength electric field of the ceramic microcrystalline with certain viscosity prolongs electric field side To orientation, injected in mold 7 by nozzle 6, subsequently into degreasing plant 8 and sintering equipment 9.
Step 5) is degreasing sintered: to improve preparation efficiency, ceramic green degreases and sinters in normal pressure-sintered furnace, in order to Prevent green compact during heating from so that green compact is shunk uneven in thickness direction and the radial generation gradation of moisture and leading to sample Cracking is warming up to 120 DEG C before degreasing with the rate of 2 DEG C/min, and heat preservation 30min sloughs the moisture of green compact, again with 2 after having kept the temperature DEG C/rate of min rises to 500 DEG C, 2h is kept the temperature, to ensure that binder is excluded entirely.Then it is risen to 2 DEG C/min of heating rate 1050 DEG C are sintered, and furnace cooling after being reduced to 500 DEG C at the same rate after heat preservation 2h obtains ceramic component.
Step 6) polarization: the two-face printing silver paste of sintered part, the heating rate of 2 DEG C/min rise to 550 DEG C and keep the temperature 30min, after cool to room temperature with the furnace, obtain by silver-colored sintered part.It will be placed in polarization device by silver-colored sintered part, in 70 DEG C of methyl silicon Under oil, polarize 20min at 3kV/mm, and NBT base leadless piezoelectricity textured ceramic is just made.
Fig. 2 under no electric field action injection moulding and DC Electric Field under be injection moulded the 0.94NBT- prepared The XRD spectrum of 0.06BT piezoelectric ceramics, it can be seen from the figure that using injection moulding preparation under DC Electric Field Much higher than the ceramics sample for being injection moulded preparation under no electric field action, this says the bimodal diffracted intensity of 0.94NBT-0.06BT ceramics Ceramic crystallinity is higher under the bright technique.
Fig. 3 is the SEM microscopic appearance photo after solid phase method 0.94NBT-0.06BT ceramic post sintering, and Fig. 4 is injection method preparation The SEM of NBT-BT ceramics schemes, and the ceramic phase ratio of crystal grain and the preparation of Fig. 3 solid phase method is made pottery using traditional 0.94NBT-0.06BT The microcosmic crystal grain agglomeration of porcelain is more obvious, and the stomata of sample is more, and ceramic consistency is lower；Using under DC Electric Field The stomata of injection molding 0.94NBT-0.06BT ceramic microstructures crystal grain significantly reduces, and consistency improves, and crystal grain is uniform.
Using the piezoelectric constant d of the 0.94NBT-0.06BT piezoelectric ceramics of solid phase method preparation33=101pC/N, permittivity ε =1029.The density of the 0.94NBT-0.06BT leadless piezoelectric ceramics of injection method preparation is 5.54gcm-3, piezoelectric constant d33= 138pC/N, permittivity ε=1436；By it was found that the 0.94NBT-0.06BT leadless piezoelectric ceramics prepared with injection method Performance be better than conventional solid-state method preparation 0.94NBT-0.06BT leadless piezoelectric ceramics.

Claims (10)

1. a kind of piezoelectric structured ceramics of NBT base, which is characterized in that with 0.94Na0.5Bi0.5TiO3-0.06BaTiO3Powder is raw material It is sintered.
2. a kind of preparation method of the piezoelectric structured ceramics of NBT base as described in claim 1, which is characterized in that including following step It is rapid: step 1, to prepare bismuth-sodium titanate powder；
Step 2, barium titanate is prepared；
Step 3, step 2 gained barium titanate is introduced into bismuth-sodium titanate powder prepared by step 1 and is prepared 0.94Na0.5Bi0.5TiO3-0.06BaTiO3Ceramic powder；
Step 4, by step 3 gained 0.94Na0.5Bi0.5TiO3-0.06BaTiO3Ceramic powder is mixed evenly with bonding agent, Form mixed slurry；
Step 5, step 4 gained mixed slurry is injection moulded, and cooling obtains ceramic green；
Step 6, step 5 gained ceramic green is subjected to degreasing and sintering；
Step 7, the sintered potsherd of step 6 is polarised to obtain the piezoelectric structured ceramics of NBT base.
3. the preparation method of the piezoelectric structured ceramics of NBT base according to claim 2, which is characterized in that in step 1, NBT powder Body component is by BiO2、Na2CO3、Ba2CO3And TiO2It is prepared by mixing, ball milling, pre-burning and secondary ball milling are dry.
4. the preparation method of the piezoelectric structured ceramics of NBT base according to claim 2, which is characterized in that in step 2, use Molten-salt growth method prepares anisotropic BaTiO3Crystallite, the BaTiO3Crystallite is sheet.
5. the preparation method of the piezoelectric structured ceramics of NBT base according to claim 2, which is characterized in that bonding agent in step 4 It is 3%~5% polyvinyl alcohol for mass fraction；The mass fraction of ceramic powder and binder ratio is 4:1, in magnetic stirring apparatus plus Hot uniform stirring is mixed to get injection moulding mixed slurry in 1 hour.
6. the preparation method of the piezoelectric structured ceramics of NBT base according to claim 2, which is characterized in that step 5 forming process In is applied by electric field and is heated for slurry after through nozzle inject mold, electric field strength is 1KV/mm~10KV/mm；Injection temperature is 20 ~40 DEG C.
7. the preparation method of the piezoelectric structured ceramics of NBT base according to claim 2, which is characterized in that in step 6, degreasing Be warming up to 120 DEG C in the process with the rate of 2 DEG C/min, heat preservation 30min sloughs the moisture of green compact, after the completion of heat preservation again with 2 DEG C/ The rate of min rises to 500 DEG C, keeps the temperature 2h.
8. the preparation method of the piezoelectric structured ceramics of NBT base according to claim 2, which is characterized in that degreasing is complete in step 6 1050 DEG C of sintering are risen at subsequent continuous 2 DEG C/min of heating rate, it is cold with furnace after being reduced to 500 DEG C at the same rate after heat preservation 2h But.
9. the preparation method of the piezoelectric structured ceramics of NBT base according to claim 2, which is characterized in that after being sintered in step 6 Potsherd thickness be polishing to 1~1.5mm, coat silver paste in potsherd two sides, the heating rate of 2 DEG C/min rises to 550 DEG C simultaneously Keep the temperature 30min, after with furnace natural cooling.
10. the preparation method of the piezoelectric structured ceramics of NBT base according to claim 2, which is characterized in that 70 in step 6 In DEG C methyl-silicone oil, electric field strength is that the piezoelectric structured ceramics of NBT base are made in 3KV/mm polarization process 20min.
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