CN115536391B - KNN-based leadless piezoelectric ceramic and preparation method thereof - Google Patents
KNN-based leadless piezoelectric ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of lead-free piezoelectric ceramic preparation, in particular to KNN-based lead-free piezoelectric ceramic and a preparation method thereof, wherein the lead-free piezoelectric ceramic takes K2CO3, na2CO3, sb2O3, B i2O3, zrO2, nb2O5 and L i2CO3 as raw materials. When the raw materials are dried, the invention can shake the raw materials or powder in the placing box, so that the raw materials or powder is heated more uniformly when being dried in the oven, and the drying efficiency can be improved.
Description
Technical Field
The invention relates to the technical field of lead-free piezoelectric ceramic preparation, in particular to KNN-based lead-free piezoelectric ceramic and a preparation method thereof.
Background
The piezoelectric material is an important functional material for realizing the mutual conversion of mechanical energy and electric energy, has wide application in various electronic components such as sensors, drivers, ultrasonic transducers, resonators, filters, buzzers, electronic igniters and the like, and has more excellent performances in all aspects of KNN lead-free piezoelectric ceramics, namely small dielectric constant, large frequency constant, high piezoelectricity, small density and the like compared with lead-based piezoelectric ceramics such as PZT and the like.
For example, the patent with the application number CN200910027302.7 has the chemical formula of (1-x) Bi0.5Na0.5TiO3-xBi0.8La0.2FeO3, wherein x is more than or equal to 0.0125 and less than or equal to 0.0625; the Bi0.8La0.2FeO3 is introduced to replace Bi0.5Na0.5TiO3 to form a three-way-orthogonal quasi-homotype phase boundary structure, and lead-free piezoelectric ceramic component points with good high Wen Tiedian and piezoelectric properties are formed, so that the depolarization temperature of the ceramic is improved to a certain extent; the piezoelectric coefficient d33 and the electromechanical coupling coefficient kp decrease with increasing parameter x, d33 varies from 20-128pC/N, and kp varies from 0.27-0.30; the saturation polarization, remnant polarization and coercive field of the ceramic all decrease with increasing parameter x; in particular, the depolarization temperature (Td) of the ceramic increases between 163-171 ℃ with increasing x.
In the above preparation method, an oven is required for drying the powder, but the powder is deposited in the oven and heated unevenly, and the drying time is required to be increased to ensure the drying of the powder.
Disclosure of Invention
The invention aims to provide KNN-based lead-free piezoelectric ceramic and a preparation method thereof, which are used for solving the problems in the background technology.
To achieve the above object, the present invention provides, for exampleThe following technical scheme is as follows: KNN-based leadless piezoelectric ceramic, and K is used as leadless piezoelectric ceramic 2 CO 3 、Na 2 CO 3 、Sb 2 O 3 、Bi 2 O 3 、ZrO2、Nb 2 O 5 、Li 2 CO 3 Is a raw material.
According to the technical scheme of the KNN-based lead-free piezoelectric ceramic, a preparation method of the KNN-based lead-free piezoelectric ceramic is provided, and the preparation method of the lead-free piezoelectric ceramic specifically comprises the following steps:
s1, weighing raw materials, and drying in a drying oven (1);
s2, grinding the dried powder respectively;
s3, placing the ground powder into an 80-DEG oven (1) to be dried for 12 hours;
s4, grinding and screening the dried powder again:
s5, mixing and grinding the sieved powder;
s6, granulating the ground powder;
s7, tabletting and sintering the granulated powder;
s8, silver coating the ceramic sheet, and polarizing the ceramic sheet after silver firing;
s9, testing piezoelectric constants, displacement data and calculating hysteresis characteristics.
Preferably, absolute ethanol is added to S2 and S5 for grinding.
Preferably, the temperature rising rate in the sintering process in the step S8 is 3 ℃/min, the sintering temperature is 1090 ℃, and the material is naturally cooled after heat preservation for 3 hours.
Preferably, the working chamber has been seted up to the inside of oven, the heater is installed to the interior roof of working chamber, the working chamber is located the below of heater and is equipped with the mounting panel, the upper surface of mounting panel is installed through fixed subassembly and is placed the case, the mounting panel lower surface is connected with the inner bottom plate of working chamber through auxiliary assembly, the cavity has been seted up to the below that the oven is inside to be located the working chamber, be equipped with in the cavity and rock the subassembly, the executive component that rocks the subassembly runs through the inner wall between cavity and the working chamber and is connected with lower surface one side of mounting panel.
Preferably, the auxiliary assembly comprises a supporting plate vertically connected with the bottom plate of the working cavity, a fixing plate is welded at the top end of the supporting plate, a connecting plate is welded on the upper surface of the fixing plate, one surface of the connecting plate, which is close to the mounting plate, is set to be a cambered surface, the connecting plate is movably connected with the lower surface of the mounting plate, a telescopic rod is fixedly arranged on one side, which is far away from the supporting plate, of the working cavity, the telescopic end of the telescopic rod is fixedly connected with the lower surface of the mounting plate, a supporting spring is sleeved on the outer side of the telescopic rod, and two ends of the supporting spring are respectively connected with the bottom plate of the working cavity and the lower surface of the mounting plate.
Preferably, the shaking assembly comprises a driving motor arranged in the cavity through a bolt, a turntable is fixedly arranged at the output end of the driving motor, a fixed rod is welded on one surface of the turntable, which is far away from the driving motor, a connecting plate is fixedly arranged on the fixed rod, the other end of the connecting plate penetrates through an installation seat movably connected with the inner wall between the cavity and the working cavity, and the installation seat is fixedly connected with the lower surface of the installation plate.
Preferably, the locating piece has been welded to the upper surface central authorities department of mounting panel, the jack-in groove has all been seted up to the both sides wall bottom of placing the case, just place the bottom central authorities department of case set up with locating piece assorted constant head tank, fixed subassembly includes mounting panel upper surface both sides welded fastening's perpendicular board, two one side of perpendicular board is equipped with horizontally connecting rod, two the one end of connecting rod runs through the perpendicular board and is connected with the arm-tie, two the other end welding of connecting rod has the limiting plate, and two the cover is equipped with reset spring on the connecting rod, two the one side welding that the connecting rod was kept away from to the limiting plate has the grafting piece, two the grafting piece is all pegged graft fixedly with the jack-in groove.
Compared with the prior art, the invention has the beneficial effects that: to the problem that the background art put forward, this application is when using oven 1 to the raw materials respectively and grind good powder and dry, will wait to dry raw materials or powder and put into and place the case 103, then the arm-tie 502 in the fixed subassembly 5 is pulled to the staff, arm-tie 502 removes and drives connecting rod 503 and remove, connecting rod 503 drives limiting plate 504 and removes, limiting plate 504 that removes drives plug block 505 and extrudees reset spring 506, will place the case 103 and place on mounting panel 2 through locating piece 201 and constant head tank 1031 this moment, then loosen arm-tie 502, limit plate 504 and plug block 505 reset under reset spring 506's effect, accomplish the quick installation to placing the case 103 in the jack block 505, conveniently place the case 103 and dismantle, then close 1's sealing door, start heater 102 and shake subassembly 4 through the temperature controller, drive motor 401 work in the rocking assembly 4 drives carousel 402 and rotates, rotatory carousel 402 drives connecting plate 404 activity through the dead lever 403, movable connecting plate 404 drives mounting panel 2 activity through mount pad 405, 2 drives telescopic link 304 and supporting spring 305 and moves the angle along movable plate 305, thereby make the raw materials can evenly dry the case or shake the drying efficiency in the case when it is more evenly shaking the activity of drying at the side of the drying plate 303.
Drawings
FIG. 1 is a schematic diagram of an oven according to the present invention;
FIG. 2 is a cross-sectional view of the oven of the present invention;
FIG. 3 is a schematic view of an accessory assembly and a stationary assembly of the present invention;
FIG. 4 is a schematic view of a wobble assembly according to the present invention.
In the figure: 1. an oven; 101. a working chamber; 102. a heater; 103. placing a box; 1031. a positioning groove; 1032. a plug-in groove; 104. a cavity; 2. a mounting plate; 201. a positioning block; 3. an auxiliary component; 301. a support plate; 302. a fixing plate; 303. a movable plate; 304. a telescopic rod; 305. a support spring; 4. shaking the assembly; 401. a driving motor; 402. a turntable; 403. a fixed rod; 404. a connecting plate; 405. a mounting base; 5. a fixing assembly; 501. a vertical plate; 502. pulling a plate; 503. a connecting rod; 504. a limiting plate; 505. a plug block; 506. and a return spring.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by those skilled in the art without making any inventive effort based on the embodiments of the present invention are within the scope of protection of the present invention.
In order that the invention may be readily understood, a more complete description of the invention will be rendered by reference to the appended drawings. Several embodiments of the invention are presented. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "mounted" on another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "left," "right," and the like are used herein for illustrative purposes only.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
KNN-based leadless piezoelectric ceramic, and K is used as leadless piezoelectric ceramic 2 CO 3 、Na 2 CO 3 、Sb 2 O 3 、Bi 2 O 3 、ZrO2、Nb 2 O 5 、Li 2 CO 3 Is a raw material.
According to the above embodiment, there is also provided a method for preparing a KNN-based leadless piezoelectric ceramic, including the steps of:
s1, weighing raw materials, and drying in a drying oven 1; s2, grinding the dried powder respectively; s3, placing the ground powder into an 80-DEG oven 1 again for drying for 12 hours; s4, grinding and screening the dried powder again; s5, mixing and grinding the sieved powder; s6, granulating the ground powder; s7, tabletting and sintering the granulated powder; s8, silver coating the ceramic sheet, and polarizing the ceramic sheet after silver firing; s9, testing piezoelectric constants and displacement data, calculating hysteresis characteristics, adding absolute ethyl alcohol into S2 and S5 for grinding, wherein the heating rate in the sintering process is 3 ℃/min, the sintering temperature is 1090 ℃, and naturally cooling after heat preservation for 3 hours.
1-4, a working chamber 101 is provided in the oven 1, a heater 102 is installed on an inner top plate of the working chamber 101, the heater 102 adopts the prior art, a temperature controller is installed on the front surface of the oven 1 for controlling the heater 102 and a shaking assembly 4, a mounting plate 2 is provided below the heater 102 in the working chamber 101, a placement box 103 is installed on the upper surface of the mounting plate 2 through a fixing assembly 5, a positioning block 201 is welded in the center of the upper surface of the mounting plate 2, inserting slots 1032 are provided at the bottoms of two side walls of the placement box 103, positioning slots 1031 matched with the positioning block 201 are provided in the center of the bottom of the placement box 103, the fixing assembly 5 comprises vertical plates 501 welded and fixed on two sides of the upper surface of the mounting plate 2, one sides of the two vertical plates 501 are provided with horizontal connecting rods 503, one ends of the two connecting rods 503 penetrate through the vertical plates 501 to be connected with a pulling plate 502, the other ends of the two connecting rods 503 are welded with limiting plates 504, the two connecting rods 503 are sleeved with reset springs 506, the sides of the two limiting plates 504 far away from the connecting rods 503 are welded with inserting blocks 505, the two inserting blocks 505 are respectively fixedly inserted with inserting grooves 1032, the lower surface of the mounting plate 2 is connected with the inner bottom plate of the working cavity 101 through an auxiliary assembly 3, the auxiliary assembly 3 comprises a supporting plate 301 vertically connected with the bottom plate of the working cavity 101, the top ends of the supporting plate 301 are welded with a fixed plate 302, the upper surface of the fixed plate 302 is welded with a movable plate 303, one side of the movable plate 303 close to the mounting plate 2 is provided with an arc surface, the movable plate 303 is movably connected with the lower surface of the mounting plate 2, one side of the working cavity 101 far away from the supporting plate 301 is fixedly provided with a telescopic rod 304, the telescopic end of the telescopic rod 304 is fixedly connected with the lower surface of the mounting plate 2, the outer side of the telescopic rod 304 is sleeved with a supporting spring 305, the both ends of supporting spring 305 are connected with the fixed surface under working chamber 101 bottom plate and mounting panel 2 respectively, cavity 104 has been seted up to the below that oven 1 inside lies in working chamber 101, be equipped with in cavity 104 and shake subassembly 4, the executive component that shakes subassembly 4 runs through the inner wall between cavity 104 and the working chamber 101 and is connected with the lower surface one side of mounting panel 2, shake subassembly 4 and include the driving motor 401 of installing in cavity 104 through the bolt, driving motor 401's output fixed mounting has carousel 402, the one side that carousel 402 kept away from driving motor 401 has welded dead lever 403, fixed mounting has connecting plate 404 on the dead lever 403, the inner wall swing joint that the connecting plate 404 other end runs through between cavity 104 and the working chamber 101 has mount pad 405, mount pad 405 and the lower fixed surface of mounting panel 2 are connected.
When the oven 1 is used for drying raw materials or ground powder respectively, the raw materials or powder to be dried are placed in the placement box 103, then a worker pulls the pull plate 502 in the fixed assembly 5, the pull plate 502 moves to drive the connecting rod 503 to move, the connecting rod 503 drives the limiting plate 504 to move, the moving limiting plate 504 drives the plug block 505 to move and extrude the reset spring 506, at the moment, the placement box 103 is placed on the mounting plate 2 through the positioning block 201 and the positioning groove 1031, then the pull plate 502 is loosened, the limiting plate 504 and the plug block 505 are reset under the action of the reset spring 506, the plug block 505 is inserted into the plug groove 1032 to complete quick installation of the placement box 103, the removal of the placement box 103 is facilitated, then the sealing door of the oven 1 is closed, the heater 102 is started through the temperature controller and the shaking assembly 4 is started, the driving motor 401 in the shaking assembly 4 is operated to drive the turntable 402 to rotate, the rotating turntable 402 drives the 404 to move through the fixing rod 403, the movable mounting plate 405 drives the mounting plate 2 to move, at the moment, the mounting plate 2 drives the telescopic rod 304 and the support spring 303 to stretch and move along the movable plate 303 to move along the angle, the movable plate 303 is enabled to enable the powder to be placed in the insertion groove 1032 to be quickly installed, the quick installation box 103 is convenient, and the drying efficiency of the raw materials can be dried, and the raw materials can be dried evenly.
The working flow of the invention is as follows: when the oven 1 is used for drying raw materials and ground powder respectively, the raw materials or the powder to be dried are placed in the placement box 103, then a worker pulls the pull plate 502 in the fixed assembly 5, the pull plate 502 moves to drive the connecting rod 503 to move, the connecting rod 503 drives the limiting plate 504 to move, the moving limiting plate 504 drives the plug block 505 to move and extrude the reset spring 506, the placement box 103 is placed on the mounting plate 2 through the positioning block 201 and the positioning groove 1031, then the pull plate 502 is loosened, the limiting plate 504 and the plug block 505 are reset under the action of the reset spring 506, the plug block 505 is inserted into the plug groove 1032 to complete quick installation of the placement box 103, the detachment of the placement box 103 is facilitated, then the sealing door of the oven 1 is closed, the heater 102 is started through the temperature controller and the shaking assembly 4 is started, the driving motor 401 in the shaking assembly 4 is operated to drive the rotary table 402 to rotate, the rotary table 402 drives the 404 to move through the fixing rod 403, the movable connecting plate 404 is driven by the mounting plate 405 to move through the mounting plate 2, the mounting plate 2 drives the telescopic rod 304 and the support spring 303 to stretch and move along the movable connecting plate 303 to enable the movable connecting plate to shake the angle along the movable plate 303, the powder to be placed in the insertion groove 103 is subjected to quick installation of the placement box 103, the box 103 is convenient to detach the raw materials or the raw materials to be dried, and the raw materials are dried.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. The preparation method of the KNN-based leadless piezoelectric ceramic is characterized by comprising the following steps of:
s1, weighing raw materials, and drying in a drying oven (1);
s2, grinding the dried powder respectively;
s3, placing the ground powder into an 80-DEG oven (1) to be dried for 12 hours;
s4, grinding and screening the dried powder again:
s5, mixing and grinding the sieved powder;
s6, granulating the ground powder;
s7, tabletting and sintering the granulated powder;
s8, silver coating the ceramic sheet, and polarizing the ceramic sheet after silver firing;
s9, testing piezoelectric constants, displacement data and calculating hysteresis characteristics;
the oven is characterized in that a working cavity (101) is formed in the oven (1), a heater (102) is arranged on an inner top plate of the working cavity (101), a mounting plate (2) is arranged below the working cavity (101) and positioned below the heater (102), a placing box (103) is arranged on the upper surface of the mounting plate (2) through a fixing component (5), the lower surface of the mounting plate (2) is connected with an inner bottom plate of the working cavity (101) through an auxiliary component (3), a cavity (104) is formed in the oven (1) and positioned below the working cavity (101), a shaking component (4) is arranged in the cavity (104), and an executing piece of the shaking component (4) penetrates through the inner wall between the cavity (104) and the working cavity (101) and is connected with one side of the lower surface of the mounting plate (2);
the utility model discloses a swing assembly, including rocking subassembly (4), including installing driving motor (401) in cavity (104) through the bolt, driving motor (401) output fixed have carousel (402), carousel (402) are kept away from driving motor (401) one side welding has dead lever (403), fixed mounting has connecting plate (404) on dead lever (403), inner wall swing joint between cavity (104) and working chamber (101) is run through to the connecting plate (404) other end has mount pad (405), lower fixed surface of mount pad (405) and mounting panel (2) is connected.
2. The method for preparing the KNN-based leadless piezoelectric ceramic according to claim 1, wherein absolute ethyl alcohol is added in S2 and S5 for grinding.
3. The preparation method of the KNN-based lead-free piezoelectric ceramic according to claim 1, wherein the temperature rising rate in the sintering process in the S8 is 3 ℃/min, the sintering temperature is 1090 ℃, and the ceramic is naturally cooled after being kept for 3 hours.
4. The preparation method of the KNN-based leadless piezoelectric ceramic according to claim 1, wherein the auxiliary assembly (3) comprises a supporting plate (301) vertically connected with a bottom plate of the working cavity (101), a fixed plate (302) is welded at the top end of the supporting plate (301), a movable plate (303) is welded on the upper surface of the fixed plate (302), one surface of the movable plate (303) close to the mounting plate (2) is set to be an arc surface, the movable plate (303) is movably connected with the lower surface of the mounting plate (2), a telescopic rod (304) is fixedly arranged on one side, far away from the supporting plate (301), of the working cavity (101), a telescopic end of the telescopic rod (304) is fixedly connected with the lower surface of the mounting plate (2), a supporting spring (305) is sleeved on the outer side of the telescopic rod (304), and two ends of the supporting spring (305) are fixedly connected with the bottom plate of the working cavity (101) and the lower surface of the mounting plate (2) respectively.
5. The preparation method of the KNN-based leadless piezoelectric ceramic according to claim 1, wherein a positioning block (201) is welded at the center of the upper surface of the mounting plate (2), inserting grooves (1032) are formed in the bottoms of two side walls of the placement box (103), positioning grooves (1031) matched with the positioning block (201) are formed in the center of the bottom of the placement box (103), the fixing assembly (5) comprises vertical plates (501) welded and fixed on two sides of the upper surface of the mounting plate (2), one side of each vertical plate (501) is provided with a horizontal connecting rod (503), one end of each connecting rod (503) penetrates through each vertical plate (501) to be connected with a pulling plate (502), the other end of each connecting rod (503) is welded with a limiting plate (504), each connecting rod (503) is sleeved with a reset spring (506), one side, far away from each connecting rod (503), of each limiting plate (504) is welded with an inserting block (505), and each inserting block (505) is fixed with each inserting groove (1032).
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