CN112500160A - Potassium-sodium niobate-based lead-free piezoelectric ceramic for piezoelectric atomization sheet and manufacturing process - Google Patents
Potassium-sodium niobate-based lead-free piezoelectric ceramic for piezoelectric atomization sheet and manufacturing process Download PDFInfo
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Abstract
The invention provides a potassium-sodium niobate based leadless piezoelectric ceramic for a piezoelectric atomization sheet and a manufacturing process thereof. The potassium-sodium niobate-based lead-free piezoelectric ceramic is adopted to replace the traditional lead-containing piezoelectric material as the core element of the piezoelectric atomization sheet, is green and environment-friendly, can effectively avoid lead pollution caused by the piezoelectric ceramic material in the production, use and waste processes, and reduces the damage to human health and environment.
Description
Technical Field
The invention relates to the technical field of lead-free piezoelectric ceramics, in particular to potassium-sodium niobate-based lead-free piezoelectric ceramics for a piezoelectric atomization sheet and a manufacturing process thereof.
Background
The piezoelectric ceramic atomizing sheet has the characteristics of small volume, light weight, no contact, no noise, low power consumption, high reliability, long service life, capability of adapting to severe working environment and the like, and is widely applied to the fields of environmental engineering, medical instruments, automobile industry, stage equipment, household appliances and the like. The piezoelectric atomization sheets used at present are all made of piezoelectric materials based on lead zirconate titanate (PZT). In lead zirconate titanate material, lead (Pb) element accounts for about 70% of the total weight of the material, and the ceramic material can cause serious damage to human health and ecological environment in the processes of production, use and waste treatment.
Disclosure of Invention
Aiming at the problems, the invention provides the potassium-sodium niobate-based leadless piezoelectric ceramic for the piezoelectric atomization sheet and the manufacturing process thereof, antimony, barium, zirconium and titanium elements are adopted for doping substitution, and a composite addition method is adopted to realize valence state and vacancy compensation and improve the piezoelectric property of the piezoelectric ceramic, so that the piezoelectric ceramic meets the performance requirement of the piezoelectric atomization sheet.
In order to achieve the above purpose, the invention is realized by the following technical scheme: a potassium-sodium niobate based leadless piezoelectric ceramic for a piezoelectric atomization sheet comprises the following chemical components: (1-x)(K0.4Na0.6)Nb1-ySbyO3+xBaZr0.5Ti0.5O3(ii) a The x and the y are mole percentages, x is more than or equal to 0 and less than or equal to 0.4, and y is more than or equal to 0.01 and less than or equal to 0.2.
Further, the raw materials comprise: the auxiliary materials comprise antimony trioxide, barium carbonate, zirconium dioxide and titanium dioxide.
In the process of synthesizing the potassium-sodium niobate-based lead-free piezoelectric ceramic, the method of doping modification and composite addition is adopted to activate the piezoelectric micro-area, and the piezoelectric constant and the electromechanical coupling coefficient of the potassium-sodium niobate-based lead-free piezoelectric ceramic are effectively improved.
A manufacturing process of potassium-sodium niobate-based lead-free piezoelectric ceramics for a piezoelectric atomization sheet comprises the following steps:
(1) pretreatment of raw materials: putting potassium carbonate, sodium carbonate, niobium pentoxide, antimony trioxide, barium carbonate, zirconium dioxide and titanium dioxide into a culture dish, putting the culture dish into an oven, and preserving heat for 3-6h at the temperature of 120-;
(2) weighing and mixing: weighing the pretreated raw materials according to the chemical composition ratio, dispersing the raw materials in absolute ethyl alcohol, uniformly mixing, drying, crushing and sieving to prepare premixed powder;
(3) pre-burning: placing the premixed powder in a box-type furnace, continuously heating to 850-;
(4) and (3) sintering: dry-pressing the pre-sintering powder into a green body, and preserving heat for 6-12h in an atmosphere sintering furnace at the temperature of 1100-1300 ℃ to obtain a compact piezoelectric ceramic plate;
(5) and (3) post-treatment: and processing the sintered piezoelectric ceramic piece into a required shape, plating silver layers on two sides, labeling a positive electrode and a negative electrode, and then polarizing and aging to obtain the potassium-sodium niobate based leadless piezoelectric ceramic.
Further, the pretreated raw material in the step (2) is dispersed in absolute ethyl alcohol and then is wet-milled and uniformly mixed by a ball mill, the rotating speed of the ball mill is 300-600rpm, and the wet-milling time is 24-48 h.
Further, the sintering gas of the atmosphere sintering furnace in the step (4) is air or oxygen, and the air pressure is 0.1-0.5 MPa.
Further, the silver plating process in the step (5) is as follows: and coating silver paste with the thickness of 0.01mm on the two surfaces of the ceramic wafer by using a silk screen, drying at the temperature of 150 ℃, then heating to 550-650 ℃ in a box type furnace, preserving heat for 60min, and then cooling to room temperature to obtain the silver-coated ceramic wafer.
Further, the polarization aging process in the step (5) is as follows: putting the silver-coated ceramic wafer marked with the positive electrode and the negative electrode into a polarization device filled with silicon oil, heating the silver-coated ceramic wafer to 60-100 ℃ in an oil bath, polarizing the silver-coated ceramic wafer for 30min under the voltage of 3-5kV/mm, and then standing the silver-coated ceramic wafer for 24h at room temperature for aging to obtain the potassium-sodium niobate-based lead-free piezoelectric ceramic.
The invention adopts the modes of direct dry pressing and atmosphere sintering to prepare the potassium-sodium niobate-based lead-free piezoelectric ceramic with high density and good electrical property, the piezoelectric constant of the piezoelectric ceramic is more than 350pC/N, and the planar electromechanical coupling constant is 0.48-0.52, thus completely meeting the requirements of the piezoelectric atomization sheet on the piezoelectric ceramic material.
The potassium-sodium niobate-based lead-free piezoelectric ceramic is adopted to replace the traditional lead-containing piezoelectric material as the core element of the piezoelectric atomization sheet, is green and environment-friendly, can effectively avoid lead pollution caused by the piezoelectric ceramic material in the production, use and waste processes, and reduces the damage to human health and environment. The potassium sodium niobate-based lead-free piezoelectric ceramic obtained by the invention is prepared into an atomizing sheet with the diameter of 20mm for a piezoelectric atomizing device, the mist output can reach 300-400mL/h, and the service life is more than 3000 hours, which shows that the lead-free piezoelectric atomizing sheet has good mist output capability and meets the application requirement of serving as an atomizing device.
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Detailed Description
The present embodiments are to be considered in all respects as illustrative and not restrictive. Any changes that may be made by one of ordinary skill in the art after reading the specification herein are, within the scope of the appended claims, to be protected by patent law.
Example 1:
a potassium sodium niobate based leadless piezoelectric ceramic for piezoelectric atomization plate comprises the following chemical composition of (K) 90 atom%0.4Na0.6)Nb0.9Sb0.1O3And 10% BaZr0.5Ti0.5O3The preparation method comprises the following steps:
(1) pretreatment of raw materials: putting potassium carbonate, sodium carbonate, niobium pentoxide, antimony trioxide, barium carbonate, zirconium dioxide and titanium dioxide into a culture dish, putting the culture dish into an oven, and keeping the temperature at 120 ℃ for 5 hours;
(2) weighing and mixing: weighing the pretreated raw materials according to the chemical composition ratio, dispersing the raw materials in absolute ethyl alcohol, putting the raw materials into a ball mill for wet milling, wherein the rotating speed of the ball mill is 450rpm, the wet milling time is 24 hours, taking the raw materials out after the wet milling is finished, putting the raw materials into an oven for drying, grinding the raw materials by using an agate mortar, and sieving the ground materials by using a 80-mesh sieve to prepare dry powder;
(3) pre-burning: placing the premixed powder in a box type furnace, continuously heating to 850 ℃, keeping the temperature for 8 hours, cooling to room temperature, crushing and sieving to obtain pre-sintered powder;
(4) and (3) sintering: dry-pressing the pre-sintering powder into a green body, and preserving heat for 6 hours at 1200 ℃ in a sintering furnace in an oxygen atmosphere of 0.1MPa to obtain a compact piezoelectric ceramic piece;
(5) and (3) post-treatment: processing the sintered piezoelectric ceramic plate into a required shape, plating silver layers on two sides, and firing the silver at 600 ℃; marking positive and negative electrodes on the two sides of the silver ceramic wafer respectively, putting the silver ceramic wafer into a polarization device filled with silicon oil, heating the silver ceramic wafer to 80 ℃ in an oil bath, polarizing the silver ceramic wafer for 30min under the voltage of 3kV/mm, and then standing the silver ceramic wafer at room temperature for 24h for aging to obtain the potassium-sodium niobate based lead-free piezoelectric ceramic.
The potassium-sodium niobate based leadless piezoelectric ceramic is made into a piezoelectric atomization sheet with the diameter of 20mm and used for a piezoelectric atomization device, the mist output can reach 350mL/h, and the service life is more than 3500 hours.
Example 2:
a potassium-sodium niobate based leadless piezoelectric ceramic for piezoelectric atomization plate comprises the following chemical composition (K) in atomic percentage of 92%0.4Na0.6)Nb0.85Sb0.15O3And 8% of BaZr0.5Ti0.5O3The preparation method comprises the following steps:
(1) pretreatment of raw materials: putting potassium carbonate, sodium carbonate, niobium pentoxide, antimony trioxide, barium carbonate, zirconium dioxide and titanium dioxide into a culture dish, putting the culture dish into an oven, and preserving heat for 3 hours at 150 ℃;
(2) weighing and mixing: weighing the pretreated raw materials according to the chemical composition ratio, dispersing the raw materials in absolute ethyl alcohol, putting the raw materials into a ball mill for wet milling, wherein the rotating speed of the ball mill is 400rpm, the wet milling time is 36h, taking the raw materials out after the wet milling is finished, putting the raw materials into an oven for drying, grinding the raw materials by using an agate mortar, and sieving the ground materials by using a 80-mesh sieve to prepare dry powder;
(3) pre-burning: placing the premixed powder in a box furnace, continuously heating to 900 ℃, keeping the temperature for 6 hours, cooling to room temperature, crushing and sieving to obtain pre-sintered powder;
(4) and (3) sintering: dry-pressing the pre-sintering powder into a green body, and preserving heat for 10 hours at 1200 ℃ in a 0.1MPa air atmosphere sintering furnace to obtain a compact piezoelectric ceramic piece;
(5) and (3) post-treatment: processing the sintered piezoelectric ceramic plate into a required shape, plating silver layers on two sides, and firing the silver at 600 ℃; marking positive and negative electrodes on the two sides of the silver ceramic wafer respectively, putting the silver ceramic wafer into a polarization device filled with silicon oil, heating the silver ceramic wafer to 80 ℃ in an oil bath, polarizing the silver ceramic wafer for 30min under the voltage of 3kV/mm, and then standing the silver ceramic wafer at room temperature for 24h for aging to obtain the potassium-sodium niobate based lead-free piezoelectric ceramic.
The potassium-sodium niobate based leadless piezoelectric ceramic is made into a piezoelectric atomization sheet with the diameter of 20mm and used for a piezoelectric atomization device, the mist output can reach 400mL/h, and the service life is more than 3000 hours.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. A potassium-sodium niobate based leadless piezoelectric ceramic for piezoelectric atomization slice is characterized in that: the potassium sodium niobate based leadless piezoelectric ceramic comprises the following chemical components: (1-x)(K0.4Na0.6)Nb y1-Sb y O3+xBaZr0.5Ti0.5O3(ii) a The above-mentionedx，yIs more than or equal to 0 percent in mol percentagex≤0.4，0.01≤y≤0.2。
2. A process for producing a potassium sodium niobate-based lead-free piezoelectric ceramic as claimed in claim 1, comprising the steps of:
(1) pretreatment of raw materials: putting potassium carbonate, sodium carbonate, niobium pentoxide, antimony trioxide, barium carbonate, zirconium dioxide and titanium dioxide into a culture dish, putting the culture dish into an oven, and preserving heat for 3-6h at the temperature of 120-;
(2) weighing and mixing: weighing the pretreated raw materials according to the chemical composition ratio, dispersing the raw materials in absolute ethyl alcohol, uniformly mixing, drying, crushing and sieving to prepare premixed powder;
(3) pre-burning: placing the premixed powder in a box-type furnace, continuously heating to 850-;
(4) and (3) sintering: dry-pressing the pre-sintering powder into a green body, and preserving heat for 6-12h in an atmosphere sintering furnace at the temperature of 1100-1300 ℃ to obtain a compact piezoelectric ceramic plate;
(5) and (3) post-treatment: and processing the sintered piezoelectric ceramic piece into a required shape, plating silver layers on two sides, labeling a positive electrode and a negative electrode, and then polarizing and aging to obtain the finished product of the potassium-sodium niobate-based leadless piezoelectric ceramic.
3. The process for manufacturing a potassium sodium niobate-based lead-free piezoelectric ceramic according to claim 2, characterized in that: and (3) dispersing the pretreated raw material in absolute ethyl alcohol, and wet-grinding and uniformly mixing the raw material by using a ball mill, wherein the rotating speed of the ball mill is 300-600rpm, and the wet-grinding time is 24-48 h.
4. The process for manufacturing a potassium sodium niobate-based lead-free piezoelectric ceramic according to claim 2, characterized in that: and (4) sintering gas of the atmosphere sintering furnace in the step (4) is air or oxygen, and the air pressure is 0.1-0.5 MPa.
5. The process for manufacturing a potassium sodium niobate-based lead-free piezoelectric ceramic according to claim 2, characterized in that: the silver plating process in the step (5) is as follows: and coating silver paste with the thickness of 0.01mm on the two surfaces of the ceramic wafer by using a silk screen, drying at the temperature of 150 ℃, then heating to 550-650 ℃ in a box type furnace, preserving heat for 60min, and then cooling to room temperature to obtain the silver-coated ceramic wafer.
6. The process for manufacturing a potassium sodium niobate-based lead-free piezoelectric ceramic according to claim 2, characterized in that: the polarization aging process in the step (5) is as follows: putting the silver-coated ceramic wafer marked with the positive electrode and the negative electrode into a polarization device filled with silicon oil, heating the silver-coated ceramic wafer to 60-100 ℃ in an oil bath, polarizing the silver-coated ceramic wafer for 30min under the voltage of 3-5kV/mm, and then standing the silver-coated ceramic wafer for 24h at room temperature for aging to obtain the potassium-sodium niobate-based lead-free piezoelectric ceramic.
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