CN109721352B - Sodium bismuth titanate-based lead-free piezoelectric ceramic prepared by adopting microwave material scientific workstation and preparation method thereof - Google Patents
Sodium bismuth titanate-based lead-free piezoelectric ceramic prepared by adopting microwave material scientific workstation and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of preparation of lead-free piezoelectric ceramic electronic component materials, in particular to a method for preparing sodium bismuth titanate-based lead-free piezoelectric ceramic by adopting a microwave material science workstation. The method can effectively solve the problems of complex process for preparing nano-grade powder in the traditional liquid phase chemical process, high equipment investment, structural defects, performance reduction and the like caused by adding the sintering aid during sintering of ceramics, can reach the preset sintering temperature within 10 minutes, and can quickly sinter the NBT-based piezoelectric ceramic material product while effectively avoiding component segregation in the sintering process. Finally, the densification degree of the obtained product is 94.7-97.1%, and the piezoelectric coefficient isd 33The NBT-based piezoelectric ceramic has high stability and excellent electrical properties, wherein the stability is = 183-265 pC/N and the Curie temperature is 340-381 ℃. The NBT-based lead-free piezoelectric ceramic prepared by the efficient and energy-saving microwave material scientific workstation has great commercial potential in the application of electronic components.
Description
Technical Field
The invention relates to the field of preparation of lead-free piezoelectric ceramic electronic component materials, in particular to sodium bismuth titanate-based lead-free piezoelectric ceramic prepared by adopting a microwave material scientific workstation and a preparation method thereof.
Background
Electronic products contacted by people in daily life cannot be separated from piezoelectric ceramic electronic components, most of the electronic components are integrated on core components of the electronic products and have the characteristic of different sizes, and the large size is dozens of centimeters, but the small electronic components are difficult to observe by naked eyes. The piezoelectric ceramic can be applied to high-end electronic equipment at present, and is closely related to an efficient energy collection mode and an efficient energy conversion mode. The most mature piezoelectric ceramic material used at present is lead zirconate titanate ceramic material, however, the material is limited worldwide because of the heavy metal lead ion. Therefore, the search for piezoelectric materials capable of replacing lead-containing materials is a necessary trend in the development of electronic component materials. There are significant challenges in finding alternative lead-containing piezoelectric materials, but there is also a strategic opportunity to develop lead-free piezoelectric ceramic materials.
Sodium bismuth titanate-based ceramics (referred to as NBT-based ceramics) are one of the lead-free piezoelectric ceramic materials currently being studied, and are also considered to have the greatest potential as replacements for lead-containing piezoelectric ceramic materials. The main reason is that the NBT-based ceramic has a perovskite structure with a large tolerance factor, and the piezoelectric performance of the NBT-based ceramic can be improved and optimized by doping barium titanate or potassium sodium niobate and other components of the perovskite structure. However, bismuth ions and sodium ions of the NBT-based ceramic material are easily volatilized under the traditional high-temperature and long-time sintering, and cause adverse effects of component segregation, increased structural defects, reduced densification degree, small performance reproducibility, reduced electrical performance and the like. In order to solve the defect problem caused by the traditional sintering process, the starting point is focused on two aspects: firstly, adding a low-temperature solid solution; secondly, preparing nanometer NBT-based ceramic powder by a solution chemical method. Solid solution is added to bring more material components, which is not beneficial to regulation and control of components and structure; the powder is prepared by a solution chemical method, and the steps are often complicated, the yield is low and the equipment investment is high. Therefore, finding a suitable sintering process is key to solving the current NBT-based ceramics.
Recently, microwaves have been used in more and more heating fields as a heating means of "human second group flames". The principle is that free charges in the material are rearranged and dipoles are repeatedly modulated and rotated by utilizing the polarization action of an alternating electromagnetic field, so that the material generates vibration and friction, and the energy of the magnetic field is converted into heat energy in the dielectric material. Therefore, the microwave sintering method has the advantages of no contact with a sample, high heating speed, high heating efficiency and the like, and has great potential in the aspect of preparing NBT-based ceramics.
Disclosure of Invention
In order to solve the problems of complex process for preparing nano-level powder, high equipment investment, structural defects and performance reduction caused by adding a sintering aid during sintering of ceramic and the like in the traditional liquid phase chemical method process, the invention provides a method for preparing sodium bismuth titanate-based lead-free piezoelectric ceramic by adopting a microwave material science workstation.
The purpose of the invention is realized by the following method:
a sodium bismuth titanate-based lead-free piezoelectric ceramic prepared by adopting a microwave material science workstation comprises the following materials: titanium dioxide, sodium carbonate, bismuth oxide, niobium pentoxide and potassium carbonate;
the NBT-based piezoelectric ceramic has a chemical formula as follows: (1-x)Na0.5Bi0.5TiO3–xK0.5Na0.5NbO3Whereinx=0.00~0.35；
The particle size of the material powder is nano-grade.
The method for preparing the sodium bismuth titanate-based lead-free piezoelectric ceramic by adopting the microwave material science workstation comprises the following steps:
1) accurately weighing material powder according to the total molar ratio of each ion in the chemical formula, and uniformly mixing for 2 hours under a high-energy ball mill;
2) tabletting the powder prepared in the step 1) under a pressure sampling machine of 1.5Mpa, then moving the powder into a muffle furnace of 850 ℃ for high-temperature calcination for 2 hours, and crushing the tablets and ball-milling the tablets for 2-3 hours by a high-energy ball mill to prepare the NBT-based piezoelectric ceramic early-stage powder;
3) weighing about 1.7g of the powder prepared in the step 2), adding 0.25wt.% of polyvinyl alcohol binder, uniformly mixing, transferring into a grinding tool with the diameter of 20mm, and molding under a pressure sampling machine with the pressure of 20-30 MPa to obtain a disc-shaped ceramic biscuit;
4) embedding the ceramic biscuit prepared in the step 3) in an alumina crucible of high-purity alumina powder, transferring the ceramic biscuit into a furnace chamber of a microwave material science workstation, and sintering the ceramic biscuit into a ceramic sample according to a set sintering heat preservation system;
5) polishing, grinding, electrode coating, polarizing and the like are carried out on the ceramic prepared in the step 4) and then the related electrical properties are tested;
the sample under the high-energy ball mill in the step 1) needs to be added with a grinding aid;
the amount of polyvinyl alcohol needed by 1.7g of the sodium bismuth titanate-based lead-free piezoelectric ceramic early-stage powder in the step 3) is 0.25 ml;
before sintering the ceramic body in the step 4), the ceramic body needs to be placed in the air for 24 hours to release internal stress;
the sintering system in the step 4) is as follows: the time from room temperature to sintering temperature is 7-10 minutes, the sintering temperature is 1050-1080 ℃, and the sintering heat preservation time is 1-2 hours;
the electrode condition in the step 5) is that the silver electrode material is sintered and infiltrated at 570 ℃; the polarization condition is that the polarization is carried out for 30min under an electric field of 30kV/cm in a silicon oil bath at 100 ℃; the piezoelectric performance conditions were measured at room temperature after the ceramic sample was left at room temperature for 24 hours.
The sodium bismuth titanate-based lead-free piezoelectric ceramic prepared in the step 5) has the following properties: piezoelectric coefficientd 33= 183-265 pC/N; the Curie temperature is 340-381 ℃.
The relative density of the sodium bismuth titanate-based lead-free piezoelectric ceramic prepared in the step 5) is 94.7-97.1%.
Has the positive and beneficial effects that: the invention adopts a microwave material science workstation to prepare the sodium bismuth titanate-based lead-free piezoelectric ceramic with excellent electrical properties, and tests the dielectric and piezoelectric properties of the piezoelectric ceramic by a modern test technology. The invention not only can effectively solve the problem of preparing nano-grade powder in the traditional liquid chemical processThe method has the advantages of complex process, high equipment investment, structural defects, performance reduction and the like caused by adding the sintering aid during sintering the ceramic, achieves the preset sintering temperature within 10 minutes, and can quickly sinter the NBT-based piezoelectric ceramic material product while effectively avoiding component segregation in the sintering process. Finally, the densification degree of the obtained product is 94.7-97.1%, and the piezoelectric coefficient isd 33The bismuth titanate sodium-based lead-free piezoelectric ceramic has high stability and excellent electrical properties, wherein the Curie temperature of the bismuth titanate sodium-based lead-free piezoelectric ceramic is 340-381℃ and 183-265 pC/N. The NBT-based lead-free piezoelectric ceramic prepared by the efficient and energy-saving microwave material scientific workstation has great commercial potential in the application of electronic components.
Drawings
FIG. 1 is a scanning electron micrograph of a cross section of NBT-based ceramic prepared in the present invention in example 3.
Detailed Description
The invention will be further described with reference to specific examples:
example 1
Preparation of 0.74Na0.5Bi0.5TiO3–0.26K0.5Na0.5NbO3Ceramic: respectively taking 2.9563g of nano-grade titanium dioxide, 1.3249g of sodium carbonate, 4.3101g of bismuth oxide, 0.8639g of niobium pentoxide and 0.4492g of potassium carbonate as material powder; uniformly mixing for 2 hours in a high-energy ball mill, putting into a pressure sampling machine of 1.5Mpa, and tabletting; the tablets were crushed and mixed for 3 hours in a high energy ball mill to obtain 0.74Na0.5Bi0.5TiO3–0.26K0.5Na0.5NbO3Ceramic powder; 1.7g of 0.74Na were weighed out0.5Bi0.5TiO3–0.26K0.5Na0.5NbO3Adding 0.25ml of polyvinyl alcohol binder with the mass fraction of 0.25wt.% into the ceramic powder, uniformly mixing, transferring the mixture into a grinding tool with the diameter of 20mm, and molding under a pressure sampling machine with the pressure of 30MPa to obtain a disc-shaped ceramic biscuit; after the ceramic biscuit is placed in the air for 24 hours, embedding the ceramic biscuit in an alumina crucible of high-purity alumina powder; the crucible is placed in a sintering system as follows: the time from room temperature to sintering temperature is 10 minutes, and the sintering temperature is 1080 DEG CAnd in a furnace chamber of a microwave material science workstation with the sintering heat preservation time of 2 hours, the biscuit is sintered into ceramic; the ceramic sample is polished, electrode-coated, polarized and the like, and then the related electrical properties of the ceramic sample are tested.
0.74Na0.5Bi0.5TiO3–0.26K0.5Na0.5NbO3The relative density of the ceramic was 97.1%, the Curie temperature was 370 ℃ and the piezoelectric constant was 248 pC/N.
Example 2
Preparation of Na0.5Bi0.5TiO3Ceramic: respectively taking 3.9950g of nano-grade titanium dioxide, 1.3249g of sodium carbonate and 5.8245g of bismuth oxide material powder; uniformly mixing for 2 hours in a high-energy ball mill, putting into a pressure sampling machine of 1.5Mpa, and tabletting; crushing the flakes and mixing in a high energy ball mill for 2.5 hours to produce Na0.5Bi0.5TiO3Ceramic powder; 1.7g of Na were weighed0.5Bi0.5TiO3Adding 0.25ml of polyvinyl alcohol binder with the mass fraction of 0.25wt.% into the ceramic powder, uniformly mixing, transferring the mixture into a grinding tool with the diameter of 20mm, and molding under a pressure sampling machine with the pressure of 25MPa to obtain a disc-shaped ceramic biscuit; after the ceramic biscuit is placed in the air for 24 hours, embedding the ceramic biscuit in an alumina crucible of high-purity alumina powder; the crucible is placed in a sintering system as follows: in a furnace chamber of a microwave material science workstation, biscuit is sintered into ceramic, wherein the time from room temperature to sintering temperature is 9 minutes, the sintering temperature is 1050 ℃, and the sintering heat preservation time is 1.5 hours; the ceramic sample is polished, electrode-coated, polarized and the like, and then the related electrical properties of the ceramic sample are tested.
Na0.5Bi0.5TiO3The relative density of the ceramic was 95.2%, the Curie temperature was 340 ℃ and the piezoelectric constant was 183 pC/N.
Example 3
Preparation of 0.65Na0.5Bi0.5TiO3–0.35K0.5Na0.5NbO3Ceramic: respectively taking 2.5968g of nano-grade titanium dioxide, 1.3249g of sodium carbonate, 3.7860g of bismuth oxide, 1.1629g of niobium pentoxide and 0.6047g of potassium carbonate as material powder; in high energy ball millingUniformly mixing under the machine for 2 hours, putting into a pressure sampling machine of 1.5Mpa, and tabletting; crushing the tablets and mixing for 2 hours in a high energy ball mill to obtain 0.65Na0.5Bi0.5TiO3–0.35K0.5Na0.5NbO3Ceramic powder; 1.7g of 0.65Na was weighed0.5Bi0.5TiO3–0.35K0.5Na0.5NbO3Adding 0.25ml of polyvinyl alcohol binder with the mass fraction of 0.25wt.% into the ceramic powder, uniformly mixing, transferring the mixture into a grinding tool with the diameter of 20mm, and molding under a pressure sampling machine with the pressure of 30MPa to obtain a disc-shaped ceramic biscuit; after the ceramic biscuit is placed in the air for 24 hours, embedding the ceramic biscuit in an alumina crucible of high-purity alumina powder; the crucible is placed in a sintering system as follows: in a furnace chamber of a microwave material science workstation, biscuit is sintered into ceramic, wherein the time from room temperature to sintering temperature is 8 minutes, the sintering temperature is 1060 ℃ and the sintering heat preservation time is 1.5 hours; the ceramic sample is polished, electrode-coated, polarized and the like, and then the related electrical properties of the ceramic sample are tested.
0.65Na0.5Bi0.5TiO3–0.35K0.5Na0.5NbO3The relative density of the ceramic was 96.6%, the Curie temperature was 381 deg.C, and the piezoelectric constant was 265pC/N, as shown in FIG. 1.
Example 4
Preparation of 0.82Na0.5Bi0.5TiO3–0.18K0.5Na0.5NbO3Ceramic: respectively taking 3.2759g of nano-grade titanium dioxide, 1.3249g of sodium carbonate, 4.7761g of bismuth oxide, 0.5981g of niobium pentoxide and 0.3110g of potassium carbonate as material powder; uniformly mixing for 2 hours in a high-energy ball mill, putting into a pressure sampling machine of 1.5Mpa, and tabletting; the tablets were crushed and mixed in a high energy ball mill for 2 hours to produce 0.82Na0.5Bi0.5TiO3–0.18K0.5Na0.5NbO3Ceramic powder; 1.7g of 0.82Na was weighed0.5Bi0.5TiO3–0.18K0.5Na0.5NbO3Adding 0.25ml of polyvinyl alcohol binder with the mass fraction of 0.25wt.% into the ceramic powder, uniformly mixing, and transferring the ceramic powder into a ceramic powder with the diameter of 20mmIn a grinding tool, a disc-shaped ceramic biscuit is prepared by molding under a pressure sampling machine with the pressure of 25 MPa; after the ceramic biscuit is placed in the air for 24 hours, embedding the ceramic biscuit in an alumina crucible of high-purity alumina powder; the crucible is placed in a sintering system as follows: in a furnace chamber of a microwave material science workstation, biscuit is sintered into ceramic, wherein the time from room temperature to sintering temperature is 7 minutes, the sintering temperature is 1080 ℃ and the sintering heat preservation time is 2 hours; the ceramic sample is polished, electrode-coated, polarized and the like, and then the related electrical properties of the ceramic sample are tested.
0.82Na0.5Bi0.5TiO3–0.18K0.5Na0.5NbO3The relative density of the ceramic was 96.7%, the Curie temperature was 355 ℃ and the piezoelectric constant was 234 pC/N.
Example 5
Preparation of 0.96Na0.5Bi0.5TiO3–0.04K0.5Na0.5NbO3Ceramic: respectively taking 3.8352g of nano-grade titanium dioxide, 1.3249g of sodium carbonate, 5.5915g of bismuth oxide, 0.1329g of niobium pentoxide and 0.0691g of potassium carbonate as material powder; uniformly mixing for 2 hours in a high-energy ball mill, putting into a pressure sampling machine of 1.5Mpa, and tabletting; the tablets were crushed and mixed in a high energy ball mill for 2.5 hours to produce 0.96Na0.5Bi0.5TiO3–0.04K0.5Na0.5NbO3Ceramic powder; 1.7g of 0.96Na was weighed0.5Bi0.5TiO3–0.04K0.5Na0.5NbO3Adding 0.25ml of polyvinyl alcohol binder with the mass fraction of 0.25wt.% into the ceramic powder, uniformly mixing, transferring the mixture into a grinding tool with the diameter of 20mm, and molding under a pressure sampling machine with the pressure of 20MPa to obtain a disc-shaped ceramic biscuit; after the ceramic biscuit is placed in the air for 24 hours, embedding the ceramic biscuit in an alumina crucible of high-purity alumina powder; the crucible is placed in a sintering system as follows: in a furnace chamber of a microwave material science workstation, biscuit is sintered into ceramic, wherein the time from room temperature to sintering temperature is 7 minutes, the sintering temperature is 1060 ℃ and the sintering heat preservation time is 1 hour; the ceramic sample is polished, electrode-coated, polarized and the like, and then the related electrical properties of the ceramic sample are tested.
0.96Na0.5Bi0.5TiO3–0.04K0.5Na0.5NbO3The relative density of the ceramic was 94.7%, the Curie temperature was 346 ℃ and the piezoelectric constant was 201 pC/N.
Example 6
Preparation of 0.90Na0.5Bi0.5TiO3–0.10K0.5Na0.5NbO3Ceramic: respectively taking 3.5955g of nano-grade titanium dioxide, 1.3249g of sodium carbonate, 5.2421g of bismuth oxide, 0.3323g of niobium pentoxide and 0.1728g of potassium carbonate as material powder; uniformly mixing for 3 hours in a high-energy ball mill, and then putting the mixture into a 1.5Mpa pressure sampling machine for tabletting; crushing the tablets and mixing for 3 hours in a high energy ball mill to obtain 0.90Na0.5Bi0.5TiO3–0.10K0.5Na0.5NbO3Ceramic powder; 1.7g of 0.90Na was weighed0.5Bi0.5TiO3–0.10K0.5Na0.5NbO3Adding 0.25ml of polyvinyl alcohol binder with the mass fraction of 0.25wt.% into the ceramic powder, uniformly mixing, transferring the mixture into a grinding tool with the diameter of 20mm, and molding under a pressure sampling machine with the pressure of 30MPa to obtain a disc-shaped ceramic biscuit; after the ceramic biscuit is placed in the air for 24 hours, embedding the ceramic biscuit in an alumina crucible of high-purity alumina powder; the crucible is placed in a sintering system as follows: in a furnace chamber of a microwave material science workstation, biscuit is sintered into ceramic, wherein the time from room temperature to sintering temperature is 10 minutes, the sintering temperature is 1070 ℃ and the sintering heat preservation time is 1.5 hours; the ceramic sample is polished, electrode-coated, polarized and the like, and then the related electrical properties of the ceramic sample are tested.
0.90Na0.5Bi0.5TiO3–0.10K0.5Na0.5NbO3The relative density of the ceramic was 95.8%, the Curie temperature was 339 ℃ and the piezoelectric constant was 210 pC/N.
The invention adopts a microwave material science workstation to prepare the sodium bismuth titanate-based lead-free piezoelectric ceramic with excellent electrical properties, and tests the dielectric and piezoelectric properties of the piezoelectric ceramic by a modern test technology. The invention not only can effectively solve the problems of complex process and equipment for preparing nano-level powder in the traditional liquid phase chemical processThe method has the advantages that the method has high investment, the problems of structural defects, performance reduction and the like caused by adding a sintering aid during sintering of ceramics are solved, the preset sintering temperature is reached within 10 minutes, and the NBT-based piezoelectric ceramic material product can be quickly sintered while the segregation of components in the sintering process is effectively avoided. Finally, the densification degree of the obtained product is 94.7-97.1%, and the piezoelectric coefficient isd 33The NBT-based piezoelectric ceramic has high stability and excellent electrical properties, wherein the stability is = 183-265 pC/N and the Curie temperature is 340-381 ℃. The NBT-based lead-free piezoelectric ceramic prepared by the efficient and energy-saving microwave material scientific workstation has great commercial potential in the application of electronic components.
The above description is only an exemplary embodiment of the present invention, and should not be taken as limiting the scope of the present invention, and any equivalent changes and modifications made by those skilled in the art without departing from the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. The sodium bismuth titanate-based lead-free piezoelectric ceramic prepared by adopting a microwave material science workstation is characterized in that: comprises the following materials: titanium dioxide, sodium carbonate, bismuth oxide, niobium pentoxide and potassium carbonate, and the chemical formula of the components is as follows: (1-x)Na0.5Bi0.5TiO3–xK0.5Na0.5NbO3Whereinx= 0.00-0.35; the particle size of the material powder is nano-grade;
the preparation method of the sodium bismuth titanate-based lead-free piezoelectric ceramic prepared by adopting the microwave material science workstation comprises the following steps:
1) accurately weighing material powder according to the total molar ratio of each ion in the chemical formula, and uniformly mixing for 2 hours under a high-energy ball mill;
2) tabletting the powder prepared in the step 1) under a pressure sampling machine of 1.5Mpa, then moving the powder into a muffle furnace of 850 ℃ for high-temperature calcination for 2 hours, and crushing the tablets and ball-milling the tablets for 2-3 hours by a high-energy ball mill to prepare NBT-based piezoelectric ceramic early-stage powder;
3) weighing 1.7g of the powder prepared in the step 2), adding 0.25wt% of polyvinyl alcohol binder, uniformly mixing, transferring into a mold with the diameter of 20mm, and molding under a pressure sampling machine with the pressure of 20-30 MPa to obtain a disc-shaped ceramic biscuit;
4) embedding the ceramic biscuit prepared in the step 3) in an alumina crucible of high-purity alumina powder, transferring the ceramic biscuit into a furnace chamber of a microwave material science workstation, and sintering the ceramic biscuit into a ceramic sample according to a set sintering heat preservation system;
5) polishing, grinding, electrode coating and polarizing the ceramic prepared in the step 4), and then testing the related electrical properties of the ceramic;
before sintering the ceramic body in the step 4), the ceramic body needs to be placed in the air for 24 hours to release internal stress; the sintering system in the step 4) is as follows: the time from room temperature to sintering temperature is 7-10 minutes, the sintering temperature is 1050-1080 ℃, and the sintering heat preservation time is 1-2 hours.
2. The sodium bismuth titanate-based lead-free piezoelectric ceramic prepared by adopting a microwave material science workstation according to claim 1, which is characterized in that: the sample under the high-energy ball mill in the step 1) needs to be added with a grinding aid.
3. The sodium bismuth titanate-based lead-free piezoelectric ceramic prepared by adopting a microwave material science workstation according to claim 1, which is characterized in that: the amount of polyvinyl alcohol required for 1.7g of NBT-based piezoelectric ceramic early-stage powder in the step 3) is 0.25 ml.
4. The sodium bismuth titanate-based lead-free piezoelectric ceramic prepared by adopting a microwave material science workstation according to claim 1, which is characterized in that: the electrode condition in the step 5) is that the silver electrode material is sintered and infiltrated at 570 ℃; the polarization condition is that the polarization is carried out for 30min under an electric field of 30kV/cm in a silicon oil bath at 100 ℃; the piezoelectric performance test conditions were a room temperature test after the ceramic sample was left at room temperature for 24 hours.
5. The microwave material science workstation system as claimed in claim 1The prepared sodium bismuth titanate-based lead-free piezoelectric ceramic is characterized in that: the NBT-based lead-free piezoelectric ceramic prepared in the step 5) has the following properties: piezoelectric coefficientd 33= 183-265 pC/N; the Curie temperature is 340-381 ℃; the NBT-based piezoelectric ceramic prepared in the step 5) has a relative density of 94.7-97.1%.
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