CN111377739A - Preparation method of high-density ultra-thin piezoelectric ceramic piece - Google Patents
Preparation method of high-density ultra-thin piezoelectric ceramic piece Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-density ultra-thin piezoelectric ceramic piece, which has extremely high density reaching 7.52g/cm3Dielectric loss of 1.6%, capacitance of 17.0nF, coupling constant70% and a dielectric constant of 3050; the piezoelectric ceramic piece is prepared by mixing organic matters in a certain proportion into slurry, preparing a film tape by adopting a tape casting process, superposing two layers or multiple layers of tape casting film tapes in the 90-degree direction, performing cold isostatic pressing firstly, and rolling by using double rollers to tightly combine the two layers or the multiple layers of film tapes together to form a single-layer piezoelectric ceramic piece with extremely high density; the raw materials of the invention are coated with the zirconium dioxide powder by sodium carbonate, so that the compactness can be obviously improved.
Description
Technical Field
The invention relates to the technical field of piezoelectric ceramics, in particular to a preparation method of a high-density ultra-thin piezoelectric ceramic piece.
Background
Piezoelectric ceramics are an emerging ceramic material, and have been developed for over a hundred years. In the middle of the last century, the invention of PZT-based piezoelectric ceramics promoted the rapid development of electronic technology, so that various electronic products appeared in the front of us, and the piezoelectric ceramics, as an internal precise element, can convert electric energy into mechanical energy or mechanical energy into electric energy, and plays a key role in electronic products.
The density of the tape-casting membrane cannot be continuously improved under the influence of the granularity of the powder and the content of the components in the slurry, so that various performance indexes of the material cannot be broken through. The piezoelectric ceramic green sheet with higher density can be obtained by the process method and the raw materials, and various electrical properties in the later period are effectively improved.
Disclosure of Invention
The invention provides a preparation method of a high-density ultra-thin piezoelectric ceramic piece. The piezoelectric ceramic piece has extremely high density.
The invention adopts the following technical scheme for solving the technical problems:
a preparation method of a high-density ultra-thin piezoelectric ceramic piece comprises the following steps:
s1: weighing raw materials according to a formula of 60-69 parts of lead tetraoxide, 1-6 parts of barium carbonate, 0.1-5 parts of strontium carbonate, 0.1-0.8 part of antimony pentoxide, 16-25 parts of zirconium dioxide, 8-15 parts of titanium dioxide and 0.2-0.4 part of cobaltous oxide, mixing, adding the mixture into a stirring mill, carrying out ball milling, adding absolute ethyl alcohol and grinding balls, wherein the material body is as follows: anhydrous ethanol: the grinding balls are 1: 0.2-0.4: 2-3; after ball milling treatment, drying to obtain ceramic powder; pre-burning the ceramic powder to obtain lead zirconate titanate composite ceramic powder;
s2: pretreating lead zirconate titanate composite ceramic powder by a ball milling process to ensure that the granularity D50 is below 1 mu m;
s3: taking 70-80 parts of lead zirconate titanate composite ceramic powder, 12-18 parts of butyl acetate, 6-10 parts of an alcohol solvent, 5-8 parts of an adhesive, 1-5 parts of a defoaming agent and 0.6-1 part of triethyl citrate, and fully mixing to obtain slurry;
s4: vacuumizing and defoaming the slurry, and forming on a casting machine to prepare a casting film belt with the thickness of 36-38 mu m;
s5: two or more pieces of the flow extending film belt are overlapped in the direction of 90 degrees;
s6: carrying out cold isostatic pressing on the stacked film strips;
s7: pressing the isostatic membrane belt by a double-roller mill to combine two or more membrane belts to obtain a single piezoelectric ceramic membrane belt;
s8: punching the piezoelectric ceramic film belt by a sheet punching machine, discharging glue at 550-650 ℃, sintering for 1-2 h at 1200-1300 ℃, coating silver, and polarizing to obtain the high-density ultra-thin piezoelectric ceramic sheet, wherein the thickness of the piezoelectric ceramic sheet is 50 μm.
As a preferred embodiment, the body: anhydrous ethanol: the grinding ball is 1:0.3: 2.5.
Preferably, the alcohol solvent is absolute ethyl alcohol.
Preferably, the binder is polyvinyl butyral.
Preferably, the defoaming agent is polydimethylsiloxane.
Preferably, the isostatic pressure is 140 to 170 MPa, and the pressure maintaining time is 1 to 5 min.
As a preferable scheme, the zirconium dioxide is sodium carbonate-coated zirconium dioxide powder, the inner layer of the sodium carbonate-coated zirconium dioxide powder is zirconium dioxide powder, and the outer layer is sodium carbonate.
As a preferred scheme, the preparation method of the sodium carbonate coated zirconium dioxide powder comprises the following steps: adding 2-4 parts of zirconium dioxide into 8-12 parts of deionized water, performing ultrasonic treatment for 25-35 min to prepare a zirconium dioxide suspension, adding sulfuric acid to adjust the pH value to 5.5-6.5, dissolving 0.6-1 part of sodium carbonate into 2-4 parts of water, adding 0.1-0.2 part of triethanolamine to form a sodium carbonate sol, dropping the sodium carbonate sol into the zirconium dioxide suspension while stirring to adsorb the sol on the surface of the zirconium dioxide, stirring and heating the solution in a water bath at 80-90 ℃ for 15-25 min, drying after the water bath, calcining for 1.5-2.5 h at 800-1000 ℃, and sieving with a 150-250 mesh sieve to obtain the sodium carbonate coated zirconium dioxide powder.
As an optimal string scheme, the preparation method of the sodium carbonate-coated zirconium dioxide powder comprises the following steps: adding 3 parts of zirconium dioxide into 10 parts of deionized water, carrying out ultrasonic treatment for 30min to prepare a zirconium dioxide suspension, adding sulfuric acid to adjust the pH value to 6, dissolving 0.8 part of sodium carbonate into 3 parts of water, adding 0.15 part of triethanolamine to form a sodium carbonate sol, dropping the sodium carbonate sol into the zirconium dioxide suspension while stirring to enable the sol to be adsorbed on the surface of the zirconium dioxide, stirring and heating the solution in a water bath at 85 ℃ for 20min, drying after the water bath, calcining at 900 ℃ for 2h, and sieving with a 200-mesh sieve to obtain the sodium carbonate coated zirconium dioxide powder.
As a preferred scheme, the zirconium dioxide powder is tetragonal zirconium dioxide powder.
The invention has the beneficial effects that: the piezoelectric ceramic sheet has extremely high density which reaches 7.52g/cm3Dielectric loss is 1.6%, capacitance is 17.0nF, coupling constant is 70%, and dielectric constant is 3050; the piezoelectric ceramic piece is prepared by mixing organic matters in a certain proportion into slurry, preparing a film tape by adopting a tape casting process, superposing two or more layers of tape casting film tapes at 90 degrees, performing cold isostatic pressing firstly, and rolling by a double-roll mill to tightly combine the two or more layers of film tapes together to form the piezoelectric ceramic piece with extremely high density; the raw materials of the invention are coated with the zirconium dioxide powder by sodium carbonate, so that the compactness can be obviously improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a high-density ultra-thin piezoelectric ceramic piece comprises the following steps:
s1: weighing raw materials according to a formula of 65 parts of lead tetraoxide, 4 parts of barium carbonate, 3 parts of strontium carbonate, 0.5 part of antimony pentoxide, 20 parts of zirconium dioxide, 12 parts of titanium dioxide and 0.3 part of cobaltous oxide, mixing, adding the mixture into a stirring mill, carrying out ball milling, and adding absolute ethyl alcohol and grinding balls, wherein the material body is as follows: anhydrous ethanol: the grinding ball is 1:0.3: 2.5; after ball milling treatment, drying to obtain ceramic powder; pre-burning the ceramic powder to obtain lead zirconate titanate composite ceramic powder;
s2: pretreating lead zirconate titanate composite ceramic powder by a ball milling process to ensure that the granularity D50 is below 1 mu m;
s3: taking 75 parts of lead zirconate titanate composite ceramic powder, 15 parts of butyl acetate, 8 parts of absolute ethyl alcohol, 6 parts of adhesive, 3 parts of defoaming agent and 0.8 part of triethyl citrate, and fully mixing to obtain slurry;
s4: vacuumizing and defoaming the slurry, and forming on a casting machine to prepare a casting film belt with the thickness of 37 mu m;
s5: two sheets of the flow extending film belt are overlapped in the direction of 90 degrees;
s6: carrying out cold isostatic pressing on the stacked film strips;
s7: pressing the isostatic membrane belt by a double-roller mill to combine the two membrane belts to obtain a single piezoelectric ceramic membrane belt;
s8: punching the piezoelectric ceramic film belt by a sheet punching machine, discharging glue at 600 ℃, sintering for 1.5h at 1250 ℃, coating silver, and polarizing to obtain the high-density ultrathin piezoelectric ceramic sheet, wherein the thickness of the piezoelectric ceramic sheet is 50 μm.
The adhesive is polyvinyl butyral.
The defoaming agent is polydimethylsiloxane.
The isostatic pressure is 155 MPa, and the pressure maintaining time is 1-53 min.
The zirconium dioxide is sodium carbonate-coated zirconium dioxide powder, the inner layer of the sodium carbonate-coated zirconium dioxide powder is zirconium dioxide powder, and the outer layer of the sodium carbonate-coated zirconium dioxide powder is sodium carbonate.
The preparation method of the sodium carbonate coated zirconium dioxide powder comprises the following steps: adding 3 parts of zirconium dioxide into 10 parts of deionized water, carrying out ultrasonic treatment for 30min to prepare a zirconium dioxide suspension, adding sulfuric acid to adjust the pH value to 6, dissolving 0.8 part of sodium carbonate into 3 parts of water, adding 0.15 part of triethanolamine to form a sodium carbonate sol, dropping the sodium carbonate sol into the zirconium dioxide suspension while stirring to enable the sol to be adsorbed on the surface of the zirconium dioxide, stirring and heating the solution in a water bath at 85 ℃ for 20min, drying after the water bath, calcining at 900 ℃ for 2h, and sieving with a 200-mesh sieve to obtain the sodium carbonate coated zirconium dioxide powder.
The zirconium dioxide powder is tetragonal crystal zirconium dioxide powder.
The density of the piezoelectric ceramic sheet is 7.52g/cm3The dielectric loss was 1.6%, the capacitance was 17.0nF, the coupling constant was 70%, and the dielectric constant was 3050.
Example 2
A preparation method of a high-density ultra-thin piezoelectric ceramic piece comprises the following steps:
s1: weighing raw materials according to a formula of 60 parts of lead tetraoxide, 1 part of barium carbonate, 1 part of strontium carbonate, 0.1 part of antimony pentoxide, 16 parts of zirconium dioxide, 8 parts of titanium dioxide and 0.2 part of cobaltous oxide, mixing, adding the mixture into a stirring mill, carrying out ball milling, adding absolute ethyl alcohol and milling balls, wherein the material body is as follows: anhydrous ethanol: the grinding ball is 1:0.2: 2; after ball milling treatment, drying to obtain ceramic powder; pre-burning the ceramic powder to obtain lead zirconate titanate composite ceramic powder;
s2: pretreating lead zirconate titanate composite ceramic powder by a ball milling process to ensure that the granularity D50 is below 1 mu m;
s3: taking 70 parts of lead zirconate titanate composite ceramic powder, 12 parts of butyl acetate, 6 parts of absolute ethyl alcohol, 5 parts of adhesive, 1 part of defoaming agent and 0.6 part of triethyl citrate, and fully mixing to obtain slurry;
s4: vacuumizing and defoaming the slurry, and forming on a casting machine to prepare a casting film belt with the thickness of 36 mu m;
s5: two sheets of the flow extending film belt are overlapped in the direction of 90 degrees;
s6: carrying out cold isostatic pressing on the stacked film strips;
s7: pressing the isostatic membrane belt by a double-roller mill to combine the two membrane belts to obtain a single piezoelectric ceramic membrane belt;
s8: punching the piezoelectric ceramic film belt by a sheet punching machine, discharging glue at 550 ℃, sintering for 1h at 1200 ℃, coating silver, and polarizing to obtain the high-density ultra-thin piezoelectric ceramic sheet, wherein the thickness of the piezoelectric ceramic sheet is 50 microns.
The adhesive is polyvinyl butyral.
The defoaming agent is polydimethylsiloxane.
The isostatic pressure is 140 MPa, and the pressure maintaining time is 1 min.
The zirconium dioxide is sodium carbonate-coated zirconium dioxide powder, the inner layer of the sodium carbonate-coated zirconium dioxide powder is zirconium dioxide powder, and the outer layer of the sodium carbonate-coated zirconium dioxide powder is sodium carbonate.
The preparation method of the sodium carbonate coated zirconium dioxide powder comprises the following steps: adding 3 parts of zirconium dioxide into 10 parts of deionized water, carrying out ultrasonic treatment for 30min to prepare a zirconium dioxide suspension, adding sulfuric acid to adjust the pH value to 6, dissolving 0.8 part of sodium carbonate into 3 parts of water, adding 0.15 part of triethanolamine to form a sodium carbonate sol, dropping the sodium carbonate sol into the zirconium dioxide suspension while stirring to enable the sol to be adsorbed on the surface of the zirconium dioxide, stirring and heating the solution in a water bath at 85 ℃ for 20min, drying after the water bath, calcining at 900 ℃ for 2h, and sieving with a 200-mesh sieve to obtain the sodium carbonate coated zirconium dioxide powder.
The zirconium dioxide powder is tetragonal crystal zirconium dioxide powder.
The density of the piezoelectric ceramic sheet is 7.04g/cm3The dielectric loss was 1.7%, the capacitance was 16.5nF, the coupling constant was 68%, and the dielectric constant was 2960.
Example 3
A preparation method of a high-density ultra-thin piezoelectric ceramic piece is characterized by comprising the following steps:
s1: weighing raw materials according to a formula of 69 parts of lead tetraoxide, 6 parts of barium carbonate, 5 parts of strontium carbonate, 0.8 part of antimony pentoxide, 25 parts of zirconium dioxide, 15 parts of titanium dioxide and 0.4 part of cobaltous oxide, mixing, adding the mixture into a stirring mill, carrying out ball milling, and adding absolute ethyl alcohol and grinding balls, wherein the material body is as follows: anhydrous ethanol: the grinding ball is 1:0.4: 3; after ball milling treatment, drying to obtain ceramic powder; pre-burning the ceramic powder to obtain lead zirconate titanate composite ceramic powder;
s2: pretreating lead zirconate titanate composite ceramic powder by a ball milling process to ensure that the granularity D50 is below 1 mu m;
s3: taking 80 parts of lead zirconate titanate composite ceramic powder, 18 parts of butyl acetate, 10 parts of absolute ethyl alcohol, 8 parts of adhesive, 1-5 parts of defoaming agent and 0.6-1 part of triethyl citrate, and fully mixing to obtain slurry;
s4: vacuumizing and defoaming the slurry, and forming on a casting machine to prepare a casting film belt with the thickness of 38 mu m;
s5: two sheets of the flow extending film belt are overlapped in the direction of 90 degrees;
s6: carrying out cold isostatic pressing on the stacked film strips;
s7: pressing the isostatic membrane belt by a double-roller mill to combine the two membrane belts to obtain a single piezoelectric ceramic membrane belt;
s8: punching the piezoelectric ceramic film belt by a sheet punching machine, discharging glue at 650 ℃, sintering for 2h at 1300 ℃, coating silver, and polarizing to obtain the high-density ultra-thin piezoelectric ceramic sheet, wherein the thickness of the piezoelectric ceramic sheet is 50 μm.
The adhesive is polyvinyl butyral.
The defoaming agent is polydimethylsiloxane.
The isostatic pressure is 170 MPa, and the dwell time is 5 min.
The zirconium dioxide is sodium carbonate-coated zirconium dioxide powder, the inner layer of the sodium carbonate-coated zirconium dioxide powder is zirconium dioxide powder, and the outer layer of the sodium carbonate-coated zirconium dioxide powder is sodium carbonate.
The preparation method of the sodium carbonate coated zirconium dioxide powder comprises the following steps: adding 3 parts of zirconium dioxide into 10 parts of deionized water, carrying out ultrasonic treatment for 30min to prepare a zirconium dioxide suspension, adding sulfuric acid to adjust the pH value to 6, dissolving 0.8 part of sodium carbonate into 3 parts of water, adding 0.15 part of triethanolamine to form a sodium carbonate sol, dropping the sodium carbonate sol into the zirconium dioxide suspension while stirring to enable the sol to be adsorbed on the surface of the zirconium dioxide, stirring and heating the solution in a water bath at 85 ℃ for 20min, drying after the water bath, calcining at 900 ℃ for 2h, and sieving with a 200-mesh sieve to obtain the sodium carbonate coated zirconium dioxide powder.
The zirconium dioxide powder is tetragonal crystal zirconium dioxide powder.
The density of the piezoelectric ceramic sheet is 7.01g/cm3The dielectric loss was 1.7%, the capacitance was 16.3nF, the coupling constant was 66%, and the dielectric constant was 2924.
Comparative example 1
Comparative example differs from example 1 in that comparative example 1 does not employ step S6, i.e., the cold isostatic pressing step, and the other steps are the same.
The density of the piezoelectric ceramic sheet is 6.91g/cm3The dielectric loss is 1.8%, the capacitance is 16.0nF, the coupling constant is 64% and the dielectric constant is 2880.
Comparative example 2
Comparative example 2 differs from example 1 in that comparative example 2 does not employ step S5, i.e., a step of superposing two sheets of a cast film tape in a 90-degree direction, and the others are the same.
The density of the piezoelectric ceramic sheet is 6.95g/cm3The dielectric loss was 1.8%, the capacitance was 16.3nF, the coupling constant was 63%, and the dielectric constant was 2924.
Comparative example 3
Comparative example 3 is different from example 1 in that comparative example 3 uses zirconium dioxide instead of sodium carbonate to coat zirconium dioxide powder, and the other is the same.
The density of the piezoelectric ceramic sheet is 6.13g/cm3The dielectric loss was 2.3%, the capacitance was 15.2nF, the coupling constant was 60%, and the dielectric constant was 2700.
In conclusion, the piezoelectric ceramic piece has extremely high density which reaches 7.52g/cm3Dielectric loss1.6%, capacitance of 17.0nF, coupling constant of 70%, dielectric constant of 3050; it can be known from comparative examples 1 to 3 that different preparation parameters of the high-density ultra-thin piezoelectric ceramic sheet disclosed by the invention can affect the performance of the piezoelectric ceramic sheet, wherein example 1 is the best parameter, and it can be known from comparative examples 1 and comparative examples 1 to 2 that steps S5 and S6 cannot be eliminated, so that the performance of the piezoelectric ceramic sheet disclosed by the invention can be remarkably improved, and it can be known from comparative examples 1 and 3 that the sodium carbonate coated zirconium dioxide powder disclosed by the invention can be remarkably improved.
In light of the foregoing description of preferred embodiments according to the invention, it is clear that many changes and modifications can be made by the person skilled in the art without departing from the scope of the invention. The technical scope of the present invention is not limited to the contents of the specification, and must be determined according to the scope of the claims.
Claims (10)
1. A preparation method of a high-density ultra-thin piezoelectric ceramic piece is characterized by comprising the following steps:
s1: weighing raw materials according to a formula of 60-69 parts of lead tetraoxide, 1-6 parts of barium carbonate, 0.1-5 parts of strontium carbonate, 0.1-0.8 part of antimony pentoxide, 16-25 parts of zirconium dioxide, 8-15 parts of titanium dioxide and 0.2-0.4 part of cobaltous oxide, mixing, adding the mixture into a stirring mill, carrying out ball milling, adding absolute ethyl alcohol and grinding balls, wherein the material body is as follows: anhydrous ethanol: the grinding balls are 1: 0.2-0.4: 2-3; after ball milling treatment, drying to obtain ceramic powder, and presintering the ceramic powder to obtain lead zirconate titanate composite ceramic powder;
s2: pretreating lead zirconate titanate composite ceramic powder by a ball milling process to ensure that the granularity D50 is below 1 mu m;
s3: taking 70-80 parts of lead zirconate titanate composite ceramic powder, 12-18 parts of butyl acetate, 6-10 parts of an alcohol solvent, 5-8 parts of an adhesive, 1-5 parts of a defoaming agent and 0.6-1 part of triethyl citrate, and fully mixing to obtain slurry;
s4: vacuumizing and defoaming the slurry, and forming on a casting machine to prepare a casting film belt with the thickness of 36-38 mu m;
s5: two or more pieces of the flow extending film belt are overlapped in the direction of 90 degrees;
s6: carrying out cold isostatic pressing on the stacked film strips;
s7: pressing the isostatic membrane belt by a double-roller mill to combine two or more membrane belts to obtain a single-layer piezoelectric ceramic membrane belt;
s8: punching the piezoelectric ceramic film strip by a sheet punching machine, discharging glue at 550-650 ℃, sintering for 1-2 h at 1200-1300 ℃, coating silver, and polarizing to obtain the high-density ultra-thin piezoelectric ceramic sheet, wherein the thickness of the piezoelectric ceramic sheet is 50 microns.
2. The method for preparing the high-density ultra-thin piezoelectric ceramic sheet according to claim 1, wherein the material body is: anhydrous ethanol: the grinding ball is 1:0.3: 2.5.
3. The method of claim 1, wherein the alcohol solvent is absolute ethyl alcohol.
4. The method for preparing a high-density ultra-thin piezoelectric ceramic plate according to claim 1, wherein the binder is polyvinyl butyral.
5. The method for preparing the high-density ultra-thin piezoelectric ceramic sheet according to claim 1, wherein the defoaming agent is polydimethylsiloxane.
6. The method for preparing the high-density ultra-thin piezoelectric ceramic plate according to claim 1, wherein the isostatic pressure is 140-170 MPa, and the dwell time is 1-5 min.
7. The method of claim 1, wherein the zirconium dioxide is sodium carbonate coated zirconium dioxide powder, the inner layer of the sodium carbonate coated zirconium dioxide powder is zirconium dioxide powder, and the outer layer is sodium carbonate.
8. The method for preparing the high-density ultra-thin piezoelectric ceramic sheet according to claim 7, wherein the method for preparing the sodium carbonate coated zirconium dioxide powder comprises the following steps: adding 2-4 parts of zirconium dioxide into 8-12 parts of deionized water, performing ultrasonic treatment for 25-35 min to prepare a zirconium dioxide suspension, adding sulfuric acid to adjust the pH value to 5.5-6.5, dissolving 0.6-1 part of sodium carbonate into 2-4 parts of water, adding 0.1-0.2 part of triethanolamine to form a sodium carbonate sol, dropping the sodium carbonate sol into the zirconium dioxide suspension while stirring to adsorb the sol on the surface of the zirconium dioxide, stirring and heating the solution in a water bath at 80-90 ℃ for 15-25 min, drying after the water bath, calcining for 1.5-2.5 h at 800-1000 ℃, and sieving with a 150-250 mesh sieve to obtain the sodium carbonate coated zirconium dioxide powder.
9. The method for preparing the high-density ultra-thin piezoelectric ceramic sheet according to claim 8, wherein the method for preparing the sodium carbonate coated zirconium dioxide powder comprises the following steps: adding 3 parts of zirconium dioxide into 10 parts of deionized water, carrying out ultrasonic treatment for 30min to prepare a zirconium dioxide suspension, adding sulfuric acid to adjust the pH value to 6, dissolving 0.8 part of sodium carbonate into 3 parts of water, adding 0.15 part of triethanolamine to form a sodium carbonate sol, dropping the sodium carbonate sol into the zirconium dioxide suspension while stirring to enable the sol to be adsorbed on the surface of the zirconium dioxide, stirring and heating the solution in a water bath at 85 ℃ for 20min, drying after the water bath, calcining at 900 ℃ for 2h, and sieving with a 200-mesh sieve to obtain the sodium carbonate coated zirconium dioxide powder.
10. The method of claim 8, wherein the zirconium dioxide powder is tetragonal zirconia powder.
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