CN114890790B - Preparation method of annular textured piezoelectric ceramic for ultrasonic scalpel driver - Google Patents

Preparation method of annular textured piezoelectric ceramic for ultrasonic scalpel driver Download PDF

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CN114890790B
CN114890790B CN202210383216.5A CN202210383216A CN114890790B CN 114890790 B CN114890790 B CN 114890790B CN 202210383216 A CN202210383216 A CN 202210383216A CN 114890790 B CN114890790 B CN 114890790B
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piezoelectric ceramic
annular
driver
ultrasonic scalpel
preparing
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CN114890790A (en
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杨彬
刘迎春
张洪军
吴丰民
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Jiangsu Acoustic Industry Technology Innovation Center
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Abstract

The invention discloses a preparation method of annular textured piezoelectric ceramic for an ultrasonic scalpel driver, and belongs to the technical field of preparation of textured piezoelectric ceramic materials. The invention solves the problems of poor piezoelectric performance, low electromechanical coupling coefficient, large loss, short service life caused by processing defects and the like of the annular piezoelectric ceramic for the traditional ultrasonic scalpel driver. The invention prepares the piezoelectric ceramic diaphragm containing highly oriented <001>, <011> or <111> oriented barium titanate template seed crystals by a tape casting process, realizes the accurate control of the diaphragm size by utilizing a laser cutting technology, and then adopts hot press molding and hot isostatic pressing molding technologies to ensure that the ceramic green body is uniformly pressed in all directions in the molding process, thereby greatly improving the density and the accurate controllability of the size of the piezoelectric ceramic. The preparation method provided by the invention can improve the piezoelectric property and the electromechanical coupling property of the piezoelectric ceramic and simultaneously give consideration to high compactness and high mechanical quality factor.

Description

Preparation method of annular textured piezoelectric ceramic for ultrasonic scalpel driver
Technical Field
The invention relates to a preparation method of annular textured piezoelectric ceramic for an ultrasonic scalpel driver, belonging to the technical field of preparation of textured piezoelectric ceramic materials.
Background
The driver of the ultrasonic scalpel is a high-power transducer, and the internal piezoelectric ceramic element of the driver is required to have high vibration speed (V) under a resonance condition rms ) And the vibration speed and the piezoelectric coefficient d ij And a mechanical quality factor Q m Is proportional to the product of (i.e. V) rms ∝d ij ×Q m . In addition, under the condition of high-speed vibration of the piezoelectric ceramic, the high dielectric loss can cause the heat generation in the ceramic to be increased rapidly, and the piezoelectric performance of the ceramic is seriously reduced; processing defects can lead to structural failure and performance failure of the ceramic under high speed vibration. Therefore, the piezoelectric ceramic used for the ultrasonic knife has high compactness,High piezoelectric coefficient and high mechanical quality factor.
At present, PZT-8 ceramics are mostly adopted as piezoelectric ceramics for drivers, and the mechanical quality factor Q is adopted m 1000 or less, but its piezoelectric performance is low and its piezoelectric coefficient d 33 Only about 200pC/N to 300pC/N; poor electromechanical coupling performance, electromechanical coupling coefficient k p -0.5; and the stress in the annular ceramic blank formed by uniaxial pressing is uneven, so that the internal defects are more and the deformation is serious after the ceramic is sintered, further the external dimension grinding is needed, the mechanical processing damage is obvious, and the development and the application of the ultrasonic scalpel on high performance are seriously restricted.
Therefore, it is necessary to provide a method for preparing a novel annular piezoelectric ceramic having both high piezoelectric performance and mechanical quality factor and few defects.
Disclosure of Invention
The invention provides a preparation method of annular texture piezoelectric ceramic for an ultrasonic scalpel driver, aiming at solving the problems of poor piezoelectric performance, low electromechanical coupling coefficient, large loss, short service life caused by processing defects and the like of the annular piezoelectric ceramic for the existing ultrasonic scalpel driver.
The technical scheme of the invention is as follows:
a method for preparing annular textured piezoelectric ceramics for an ultrasonic scalpel driver comprises the following steps:
step 1, mixing base ceramic powder and MnCO 3 Ball milling and mixing the solvent, the dispersant, the adhesive and the plasticizer, and adding BaTiO 3 Performing seed ball milling on the template for 30-60 min to obtain casting slurry;
step 2, preparing the casting slurry obtained in the step 1 into a casting film belt by adopting a casting forming technology;
step 3, cutting the casting film belt obtained in the step 2 by adopting laser to obtain an annular casting film;
step 4, stacking the annular casting diaphragms obtained in the step 3 according to the required thickness, then performing hot-press molding treatment by adopting a radial uniform expansion hot-press mold, and finally placing the annular casting diaphragms into an elastic diaphragm sleeve for hot water isostatic pressing treatment to obtain annular piezoelectric ceramic green bodies;
step 5, placing the annular piezoelectric ceramic green body obtained in the step 4 in a muffle furnace at 500-650 ℃, carrying out glue discharging treatment for 2-12 h, and then carrying out cold isostatic pressing treatment to obtain an annular piezoelectric ceramic biscuit;
step 6, placing the annular piezoelectric ceramic biscuit obtained in the step 5 into a hot isostatic pressing furnace, and carrying out heat preservation and pressure maintaining sintering in an argon or nitrogen atmosphere to obtain annular texture piezoelectric ceramic;
and 7, screen-printing symmetrical silver electrodes on the upper surface and the lower surface of the annular texture piezoelectric ceramic obtained in the step 6, and carrying out polarization treatment for 15-30 min under the conditions that the temperature is 120 ℃ and the polarization field intensity is 2-5 times of the coercive field to obtain the annular texture piezoelectric ceramic for the ultrasonic scalpel driver.
Further limiting, the grain diameter of the matrix ceramic powder in the step 1 is 100-500 nm; the BaTiO 3 The direction of the maximum crystal face normal of the template seed crystal is<001>、<011>Or<111>And BaTiO 3 The grain diameter of the template seed crystal is 3-15 mu m.
Further limiting, in step 1, the base ceramic powder and BaTiO 3 The molar ratio of the template is 1: (0.01-0.1).
Further limiting, in step 1, the base ceramic powder and MnCO 3 In a molar ratio of 1: (0.02-0.15).
Further defined, the width of the casting film band obtained in the step 2 is more than 20cm, and the thickness is 50-200 μm.
Further limiting, the inner diameter of the annular casting membrane obtained in the step 3 is 3-6 mm, and the outer diameter is 15-25 mm.
Further limiting, the hot-press molding process parameters in the step 4 are as follows: the temperature is 70-90 ℃, the pressure is 10-30 MPa, and the pressure maintaining time is 10-30 min.
Further limiting, the hot water isostatic pressing treatment process parameters in the step 4 are as follows: the temperature is 75-85 ℃, the pressure is 10-30 MPa, and the pressure maintaining time is 20-40 min.
Further limiting, the cold isostatic pressing process parameters in step 5 are as follows: the pressure is 150-300 MPa, and the pressure maintaining time is 2-5 min.
Further limiting, the parameters of the hot isostatic pressing treatment in the step 6 are as follows: the pressure is 10-20 MPa, the sintering temperature is 900-1200 ℃, and the heat preservation and pressure maintaining sintering time is 4-9 h.
The invention has the following beneficial effects: the invention utilizes the crystal orientation texture, hot water isostatic pressing and hot-pressing sintering technologies to prepare the annular texture piezoelectric ceramic which has high compactness, high piezoelectric performance, high electromechanical coupling performance, high mechanical quality factor and low dielectric loss, can accurately control the size of the piezoelectric ceramic, avoids secondary mechanical processing of the piezoelectric ceramic, reduces the problem of short service life caused by processing defects, and realizes great improvement of the performance of the traditional ultrasonic scalpel driver.
The invention uses ceramic texturing technology to promote the crystal grain to grow preferentially along the dominant direction, so that the piezoelectric coefficient of the prepared annular textured piezoelectric ceramic reaches up to 550pC/N, which is 1.8-2.8 times of that of PZT-8 ceramic, and d 33 ×Q m Is 1.5 to 2.5 times of PZT-8 ceramics, and realizes the balance of high density, high piezoelectric performance and high mechanical quality. Meanwhile, the invention utilizes the laser cutting technology to realize the accurate control of the size of the diaphragm, and then adopts the hot press forming and hot isostatic pressing forming technologies to ensure that the ceramic green body is uniformly pressed in all directions in the forming process, thereby avoiding the problems of uneven internal stress, more defects, easy deformation and the like of the annular ceramic green body formed by single axial press forming, and greatly improving the compactness and the accurate controllability of the size of the piezoelectric ceramic. In addition, the preparation process provided by the invention is simple, has good stability and is suitable for batch production.
Drawings
FIG. 1 is a physical diagram of a ring-shaped textured piezoelectric ceramic prepared in example 1;
FIG. 2 is an XRD curve of the ring-shaped textured piezoelectric ceramic prepared in example 1;
FIG. 3 is a graph comparing the piezoelectric coefficient and dielectric loss of the ring-textured piezoelectric ceramic and PZT-8 ceramic prepared in example 1;
FIG. 4 shows d of the ring-shaped textured piezoelectric ceramic and PZT-8 ceramic prepared in example 1 33 ×Q m And (6) comparing the graphs.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The experimental procedures used in the following examples are conventional unless otherwise specified. The materials, reagents, methods and apparatus used, unless otherwise specified, are conventional in the art and are commercially available to those skilled in the art.
Example 1:
(1) 20g of 24Pb (In) 1/2 Nb 1/2 )O 3 -42Pb(Mg 1/3 Nb 2/3 )O 3 -34PbTiO 3 (24 PIN-42PMN-34 PT) ceramic matrix powder, 0.03g MnCO 3 3g of ethanol and 3g of xylene as solvents, 0.3g of fish oil dispersant, 0.6g of polyvinyl butyral (PVB) binder, 0.3g of Butylbenzyl phthalate (BBP) and 0.3g of polyalkyltoluene (Polyalkyllene glycol, PAG) as plasticizers, after ball-milling and mixing, 0.4g of BaTiO was added 3 Preparing casting slurry after ball milling of template seed crystal for 45min, wherein the particle size of matrix ceramic powder is 150-300nm 3 The maximum crystal face normal direction of the template seed crystal is<001>And the grain diameter is 5-10 μm;
(2) Preparing a casting film belt containing highly-oriented barium titanate template seed crystals by adopting a casting forming technology, wherein the width of the casting film belt is 30cm, and the thickness of the casting film belt is 80 mu m;
(3) According to the design requirement of an ultrasonic scalpel driver, cutting a casting film strip by adopting laser to obtain an annular casting film, wherein the inner diameter of the annular casting film is 6mm, the outer diameter of the annular casting film is 16mm, so as to ensure that the resonance frequency of the annular casting film meets the requirement of the driver on the resonance frequency of piezoelectric ceramics, after the ceramic film is stacked to the thickness of 4.5mm according to the required size, carrying out hot press molding by means of a radial uniform expansion hot press mold at the temperature of 75 ℃, the pressure of 20MPa and the pressure of 15min, then putting the annular casting film into an elastic film sleeve, and carrying out hot water isostatic pressing at the temperature of 80 ℃, the pressure of 20MPa and the pressure of 30min to obtain an annular piezoelectric ceramic green body;
(4) Placing the annular piezoelectric ceramic green body in a muffle furnace at 600 ℃, discharging glue for 2h, carrying out cold isostatic pressing on the annular piezoelectric ceramic green body after glue discharging at the pressure of 200MPa, and keeping the pressure for 2min to obtain an annular piezoelectric ceramic biscuit;
(5) Placing the annular piezoelectric ceramic biscuit in a hot isostatic pressing furnace, sintering in a nitrogen protective atmosphere at 1050 ℃ under 15MPa of isostatic pressure, and carrying out heat preservation and pressure-maintaining sintering for 6 hours to prepare annular textured piezoelectric ceramic highly oriented along the <001 >;
(6) Screen-printing symmetrical silver electrodes on the upper and lower surfaces of the annular textured piezoelectric ceramic, and polarizing the annular textured piezoelectric ceramic at 120 ℃ and a polarizing field intensity of 3 times of a coercive field for 20min to obtain the annular textured piezoelectric ceramic for the ultrasonic scalpel driver, wherein a physical diagram is shown in FIG. 1;
the annular texture piezoelectric ceramic is characterized by an XRD (X-ray diffraction) pattern, as shown in figure 2, the piezoelectric ceramic is of a pure-phase perovskite structure, and no second phase exists. Compared with non-oriented ceramic, [001 ] of the ring-shaped textured piezoelectric ceramic] C And [002] C The intensity of the diffraction peak is very high, not {001} C The diffraction peak is very weak, which indicates that the ring-shaped texture piezoelectric ceramic edge<001>Highly preferred orientation.
Calculating F 00l (Lotgering factor F 00l (0<F 00l <1) Is often used to measure the texture quality of ceramics, F 00l The higher the texture quality, the better the piezoelectric properties are close to single crystals) is 98%, which indicates that the texture quality is good and the piezoelectric properties are close to single crystals.
Comparing the piezoelectric coefficient and dielectric loss of the ring texture piezoelectric ceramic with that of the existing PZT-8 ceramic, as shown in FIG. 3, the piezoelectric coefficient of the existing PZT-8 ceramic is not higher than 300pC/N, but the invention uses the texturing technology to promote the crystal grain to preferentially grow along the dominant direction, so that the piezoelectric coefficient d of the piezoelectric ceramic 33 Up to 550pC/N, which is more than 2 times of that of PZT-8 ceramics. Furthermore, the bookElectromechanical coupling coefficient k of ring-shaped textured piezoelectric ceramic prepared by invention p 0.65, higher than PZT-8 ceramic (k) p 0.5).
FIG. 4 shows the above-mentioned ring-shaped textured piezoelectric ceramic and the conventional PZT-8 ceramic d 33 ×Q m In contrast, it can be seen from the figure that d prepared according to the invention 33 ×Q m Is more than 1.5 times of that of PZT-8 ceramics. The preparation method has the advantages and the unique characteristics that the crystal orientation texture, hot water isostatic pressing and hot pressing sintering technology are utilized, the piezoelectric property and the electromechanical coupling property of the piezoelectric ceramic are improved, and simultaneously, high density and high mechanical quality factor are considered.
The above description is intended to be illustrative of the preferred embodiment of the present invention and should not be taken as limiting the invention, but rather, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.

Claims (10)

1. A method for preparing annular textured piezoelectric ceramics for an ultrasonic scalpel driver is characterized by comprising the following steps:
step 1, mixing matrix ceramic powder and MnCO 3 Ball milling and mixing the solvent, the dispersant, the adhesive and the plasticizer, and adding BaTiO 3 Continuing ball milling the template seed crystals for 30-60 min to obtain casting slurry;
step 2, preparing the casting slurry obtained in the step 1 into a casting film belt by adopting a casting forming technology;
step 3, cutting the casting film belt obtained in the step 2 by adopting laser to obtain an annular casting film;
step 4, stacking the annular casting diaphragms obtained in the step 3 according to the required thickness, then carrying out hot-press molding treatment by adopting a radial uniform expansion hot-press mold, and finally putting the annular casting diaphragms into an elastic diaphragm sleeve for hot water isostatic pressing treatment to obtain annular piezoelectric ceramic green bodies;
step 5, placing the annular piezoelectric ceramic green body obtained in the step 4 in a muffle furnace at 500-650 ℃, carrying out glue discharging treatment for 2-12 h, and then carrying out cold isostatic pressing treatment to obtain an annular piezoelectric ceramic biscuit;
step 6, placing the annular piezoelectric ceramic biscuit obtained in the step 5 into a hot isostatic pressing furnace, and carrying out heat preservation and pressure maintaining sintering in an argon or nitrogen atmosphere to obtain annular texture piezoelectric ceramic;
and 7, screen-printing symmetrical silver electrodes on the upper surface and the lower surface of the annular texture piezoelectric ceramic obtained in the step 6, and carrying out polarization treatment for 15-30 min under the conditions that the temperature is 120 ℃ and the polarization field intensity is 2-5 times of the coercive field to obtain the annular texture piezoelectric ceramic for the ultrasonic scalpel driver.
2. The method for preparing the ring-shaped textured piezoelectric ceramic for the ultrasonic scalpel driver according to claim 1, wherein the particle size of the matrix ceramic powder in the step 1 is 100-500 nm; the BaTiO 3 The direction of the maximum crystal face normal of the template seed crystal is<001>、<011>Or<111>And BaTiO 3 The grain diameter of the template seed crystal is 3-15 mu m.
3. The method for preparing the ring-shaped textured piezoelectric ceramic for the driver of the ultrasonic scalpel according to claim 1, wherein the base ceramic powder and BaTiO in the step 1 3 The molar ratio of the template is 1: (0.01-0.1).
4. The method for preparing the ring-shaped textured piezoelectric ceramic for the driver of the ultrasonic scalpel according to claim 1, wherein the base ceramic powder and the MnCO in the step 1 3 In a molar ratio of 1: (0.02-0.15).
5. The method for preparing the ring-shaped textured piezoelectric ceramic for the ultrasonic scalpel driver as claimed in claim 1, wherein the width of the casting film band obtained in the step 2 is more than 20cm, and the thickness of the casting film band is 50-200 μm.
6. The method for preparing the ring-shaped textured piezoelectric ceramic for the ultrasonic scalpel driver according to the claim 1, wherein the inner diameter of the ring-shaped cast membrane obtained in the step 3 is 3-6 mm, and the outer diameter is 15-25 mm.
7. The method for preparing the ring-shaped textured piezoelectric ceramic for the ultrasonic scalpel driver as claimed in claim 1, wherein the hot-press molding process parameters in the step 4 are as follows: the temperature is 70-90 ℃, the pressure is 10-30 MPa, and the pressure maintaining time is 10-30 min.
8. The method for preparing the annular textured piezoelectric ceramic for the ultrasonic scalpel driver as claimed in claim 1, wherein the hot water isostatic pressing treatment process parameters in the step 4 are as follows: the temperature is 75-85 ℃, the pressure is 10-30 MPa, and the pressure maintaining time is 20-40 min.
9. The method for preparing the ring-shaped textured piezoelectric ceramic for the ultrasonic scalpel driver as claimed in claim 1, wherein the cold isostatic pressing process parameters in the step 5 are as follows: the pressure is 150-300 MPa, and the pressure maintaining time is 2-5 min.
10. The method for preparing the ring-shaped textured piezoelectric ceramic for the ultrasonic scalpel driver as claimed in claim 1, wherein the hot isostatic pressing process parameters in the step 6 are as follows: the pressure is 10-20 MPa, the sintering temperature is 900-1200 ℃, and the heat preservation and pressure maintaining sintering time is 4-9 h.
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