CN115093221A - Potassium-sodium niobate-based leadless piezoelectric ceramic sheet, preparation method and application - Google Patents
Potassium-sodium niobate-based leadless piezoelectric ceramic sheet, preparation method and application Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 94
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 41
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- 239000002270 dispersing agent Substances 0.000 claims abstract description 18
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- 238000005520 cutting process Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000010345 tape casting Methods 0.000 claims abstract description 6
- 238000005266 casting Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000012528 membrane Substances 0.000 claims description 33
- 239000011734 sodium Substances 0.000 claims description 22
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
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- 229910052700 potassium Inorganic materials 0.000 claims description 10
- 235000012431 wafers Nutrition 0.000 claims description 10
- 229910052787 antimony Inorganic materials 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 7
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 7
- 239000011591 potassium Substances 0.000 claims description 7
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 6
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 6
- 239000004014 plasticizer Substances 0.000 claims description 6
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 6
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 5
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- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 5
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- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 239000013530 defoamer Substances 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000007599 discharging Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
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- 238000010923 batch production Methods 0.000 description 3
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
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- 239000000758 substrate Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
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- 238000005859 coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- ZBSCCQXBYNSKPV-UHFFFAOYSA-N oxolead;oxomagnesium;2,4,5-trioxa-1$l^{5},3$l^{5}-diniobabicyclo[1.1.1]pentane 1,3-dioxide Chemical compound [Mg]=O.[Pb]=O.[Pb]=O.[Pb]=O.O1[Nb]2(=O)O[Nb]1(=O)O2 ZBSCCQXBYNSKPV-UHFFFAOYSA-N 0.000 description 1
- 229920000334 poly[3-(3'-N,N,N-triethylamino-1-propyloxy)-4-methylthiophene-2,5-diyl hydrochloride] polymer Polymers 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- G10—MUSICAL INSTRUMENTS; ACOUSTICS
- G10K—SOUND-PRODUCING DEVICES; METHODS OR DEVICES FOR PROTECTING AGAINST, OR FOR DAMPING, NOISE OR OTHER ACOUSTIC WAVES IN GENERAL; ACOUSTICS NOT OTHERWISE PROVIDED FOR
- G10K9/00—Devices in which sound is produced by vibrating a diaphragm or analogous element, e.g. fog horns, vehicle hooters or buzzers
- G10K9/12—Devices in which sound is produced by vibrating a diaphragm or analogous element, e.g. fog horns, vehicle hooters or buzzers electrically operated
- G10K9/122—Devices in which sound is produced by vibrating a diaphragm or analogous element, e.g. fog horns, vehicle hooters or buzzers electrically operated using piezoelectric driving means
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Abstract
The invention discloses a potassium-sodium niobate-based lead-free piezoelectric ceramic sheet, a preparation method and application, relates to the technical field of ceramic materials, and aims to solve the problems that the existing medium-voltage piezoelectric ceramic material is required to be lead-free and the lead-free ceramic has poor performance. The preparation method comprises the following steps: weighing the raw materials according to the theoretical composition ratio; preparing the raw materials into ceramic pre-sintering powder; ball-milling the pre-sintered ceramic powder and then drying; adding a solvent, a dispersing agent and a defoaming agent into the dried ceramic powder and fully mixing; casting after secondary ball milling; cutting the cast film into small films; punching the diaphragm; and removing the glue and sintering to obtain the potassium-sodium niobate based lead-free piezoelectric ceramic sheet. The invention prepares the leadless potassium-sodium niobate (KNN) base ceramic diaphragm by the tape casting method, and prepares the prepared potassium-sodium niobate base leadless piezoelectric ceramic sheet into the buzzer, thereby meeting the environmental protection requirement of leadless and playing an important role in the practicability of the KNN base ceramic material.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a potassium-sodium niobate based lead-free piezoelectric ceramic sheet, a preparation method and application thereof.
Background
The piezoelectric material is a functional material widely applied to the fields of information technology, artificial intelligence, aerospace, energy environment, biomedical treatment and the like, and has profound influence on the development of the whole national economy and national defense construction. The piezoelectric ceramic can be widely used in acoustic elements, wherein the buzzer is an electroacoustic device which converts electric energy into sound energy by utilizing a piezoelectric effect, and has the advantages of high sound-electric power conversion efficiency, low power consumption, high reliability, long service life and the like. The core part of the piezoelectric buzzer is a piezoelectric buzzer piece formed by bonding a piezoelectric ceramic piece and a metal sheet, and the performance of a piezoelectric material of the piezoelectric buzzer greatly affects the performance of the buzzer.
Lead-containing materials represented by lead zirconate titanate (PZT) and lead magnesium niobate titanate (PMNT) are most widely used in piezoelectric ceramic materials at present, and cause serious damage to human and ecological environments during production, use and disposal. In recent years, governments around the world have advanced a series of lead-free laws and regulations in the field of electronics industry, and the comprehensive performance of lead-free piezoelectric ceramics is still far from the comprehensive performance of lead-based piezoelectric ceramics.
Potassium sodium niobate ((K, Na) NbO 3 KNN) lead-free piezoelectric ceramic is a piezoelectric material with a perovskite structure, has the characteristics of higher Curie temperature, excellent piezoelectric performance, environmental friendliness and the like, and is one of systems most likely to replace lead-based piezoelectric ceramic manufacturing devices in current research. Piezoelectric constant d of pure sodium potassium niobate ceramic prepared by common sintering process 33 It is only about 80 pC/N. Chemical doping in potassium sodium niobate-based ceramic can effectively improve the sintering characteristic of the ceramic and obtain high sintering temperatureThe piezoelectric performance of the ceramic body with the density can be obviously improved.
At present, the research on potassium-sodium niobate-based leadless piezoelectric ceramics mainly focuses on the preparation by a solid-phase method, and the piezoelectric performance of the ceramics is improved by chemical doping, but the research on device application of the materials is less. Meanwhile, the solid phase method is not beneficial to batch preparation of piezoelectric ceramic sheets, so that a potassium sodium niobate-based lead-free piezoelectric ceramic sheet which is suitable for batch production and has a stable process needs to be developed and formed into a device.
Disclosure of Invention
Aiming at the problems that the ceramic material in the prior art is required to be lead-free and the lead-free ceramic performance is poor, the invention provides a method for preparing potassium-sodium niobate-based lead-free ceramic sheets suitable for batch production, and the potassium-sodium niobate-based lead-free ceramic sheets are prepared into buzzer devices.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a potassium-sodium niobate-based leadless piezoelectric ceramic sheet comprises the following steps:
step 1, according to the general chemical formula (1-x) (K) y Na 1-y )Nb 1-w Sb w O 3 -x(Bi 0.5 Na 0.5 )ZrO 3 -z％Fe 2 O 3 Weighing raw materials according to the theoretical composition ratio;
in the formula: x represents (Bi) 0.5 Na 0.5 )ZrO 3 The mole fraction of (c);
y represents the content of potassium in the potassium-sodium niobate;
z represents Fe 2 O 3 The content of (A);
w represents the content of antimony;
step 2, performing ball milling and pre-synthesis on the raw materials to prepare ceramic pre-sintering powder;
step 3, ball-milling the pre-sintered ceramic powder and then drying;
step 4, adding a solvent, a dispersing agent and a defoaming agent into the ceramic powder dried in the step 3, and fully mixing;
step 5, weighing a certain amount of binder and plasticizer in the slurry obtained in the step 4, carrying out secondary ball milling and then carrying out tape casting;
step 6, cutting the cast membrane into small membranes, and laminating and rolling the membranes;
step 7, punching the membrane obtained in the step 6;
and 8, laminating the wafers punched in the step 7, removing the glue, and sintering to obtain the potassium-sodium niobate based lead-free piezoelectric ceramic sheet.
As a further preferable scheme of the invention, in the step 1, x is more than 0.00 and less than or equal to 0.055, y is more than 0.00 and less than or equal to 0.5, z is more than 0.00 and less than 0.5, and w is more than or equal to 0.00 and less than or equal to 0.05; in the step 1, the raw material is oxide or carbonate containing seven elements of K, Na, Nb, Bi, Zr, Fe and Sb.
As a further preferable aspect of the present invention, step 2 comprises the steps of:
step 2a, placing the prepared raw materials into a nylon ball milling tank, adding absolute ethyl alcohol as a dispersing agent, and ball milling for 8-24 h by using a planetary ball mill at the rotating speed of 100-450 rpm;
step 2b, baking the slurry obtained by ball milling for 2-3 h;
and 2c, heating to 800-900 ℃ in a program temperature control box type furnace, and preserving the heat for 4-6 h to obtain the ceramic pre-sintering powder.
As a further preferable aspect of the present invention, step 3 comprises the steps of:
step 3a, placing the ceramic powder in a nylon ball-milling tank, adding absolute ethyl alcohol as a dispersing agent, and ball-milling for 8-24 h by using a planetary ball mill at the rotating speed of 100-450 rpm;
and 3b, baking the slurry obtained by ball milling for 2-3 h.
As a further preferable scheme of the invention, the added solvent in the step 4 is 80-90 wt% of alcohol and ethyl acetate, the dispersing agent is 0.5-5 wt% of triethanolamine, and the defoaming agent is 0.2-0.6 wt% of tributyl phosphate.
As a further preferred embodiment of the present invention, the binder to be added in step 5 is 5 to 10% by weight of polyvinyl butyral (PVB) and the plasticizer is 1 to 5% by weight of dioctyl phthalate (DOP).
As a further preferable scheme of the invention, the thickness of the film after casting in the step 5 is 0.1 mm-0.25 mm; and in the step 7, the diameter of the round punching sheet is 10-30 mm.
As a further preferable scheme of the invention, the binder removal temperature in the step 8 is 500-700 ℃, the sintering temperature is 1000-1200 ℃, and the sintering time is 3-7 h.
A potassium sodium niobate based leadless piezoelectric ceramic sheet applied to the preparation method, the chemical general formula is (1-x) (K) y Na 1-y )Nb 1-w Sb w O 3 -x(Bi 0.5 Na 0.5 )ZrO 3 -z％Fe 2 O 3 The raw materials are weighed according to the theoretical composition ratio of (A), wherein x represents (Bi) 0.5 Na 0.5 )ZrO 3 0.00 mol fraction of<x is less than or equal to 0.055, y represents the content of potassium in the potassium-sodium niobate, 0.00<y is less than or equal to 0.5, and z represents Fe 2 O 3 Content of (1), 0.00<z is less than 0.5, w represents the content of antimony, and w is more than or equal to 0.00 and less than 0.05.
The application of the potassium-sodium niobate-based lead-free piezoelectric ceramic sheet is characterized in that the potassium-sodium niobate-based lead-free piezoelectric ceramic sheet is applied to a buzzer.
The invention has the beneficial effects that:
the invention provides a preparation method of potassium-sodium niobate-based lead-free piezoelectric ceramic sheets suitable for batch production, and the prepared potassium-sodium niobate-based lead-free piezoelectric ceramic sheets are prepared into buzzers, so that the lead-free environmental protection requirement is met; the piezoelectric constant of the potassium-sodium niobate-based lead-free piezoelectric ceramic sheet prepared by the method provided by the invention is 263 pC/N; when the driving voltage of the buzzer prepared by the potassium-sodium niobate-based leadless piezoelectric ceramic membrane prepared by the invention is 1.75Vp-p, the driving frequency is 4.25kHz, and the testing distance is 10cm, the sound pressure is 73.9 dB.
Drawings
FIG. 1 is an X-ray diffraction pattern of the ceramic membrane prepared in example 1 of the present invention.
Fig. 2 is a Scanning Electron Micrograph (SEM) of the ceramic membrane prepared in example 2 of the present invention.
Fig. 3 is a graph showing the variation of sound pressure with frequency of the buzzer manufactured in application example 1 of the present invention.
Fig. 4 is a graph showing the variation of sound pressure with frequency of the buzzer manufactured in application example 2 of the present invention.
Detailed Description
The embodiments of the present invention will be described in more detail with reference to the drawings and the reference numerals, so that those skilled in the art can implement the embodiments of the present invention after reading the specification. 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 invention provides a preparation method of a potassium-sodium niobate-based lead-free ceramic material, which develops a potassium-sodium niobate-based lead-free piezoelectric ceramic sheet which is suitable for mass production and has stable process, and prepares the potassium-sodium niobate-based lead-free piezoelectric ceramic sheet into a buzzer, thereby meeting the environmental protection requirement of lead-free.
Specific examples are as follows.
Example 1
Referring to fig. 1, the present embodiment provides a method for preparing a potassium sodium niobate-based lead-free piezoelectric ceramic sheet, including the following steps:
step 1, according to the general chemical formula (1-x) (K) y Na 1-y )Nb 1-w Sb w O 3 -x(Bi 0.5 Na 0.5 )ZrO 3 -z％Fe 2 O 3 The raw materials are weighed according to the theoretical composition ratio of (A), wherein x represents (Bi) 0.5 Na 0.5 )ZrO 3 Y represents the potassium content in the potassium-sodium niobate, and z represents Fe 2 O 3 W represents the content of antimony, x is 0.05, y is 0.45, z is 0.2, w is 0;
step 2, placing the prepared raw materials into a nylon ball milling tank, adding absolute ethyl alcohol as a dispersing agent, and carrying out ball milling for 12 hours by using a planetary ball mill with the rotating speed of 300 rpm; then baking the slurry obtained by ball milling for 2 hours; finally, putting the ceramic powder into a program temperature control box type furnace, heating the ceramic powder to 850 ℃, and preserving the heat for 6 hours to obtain ceramic powder;
step 3, placing the pre-sintered ceramic powder in a nylon ball milling tank, adding absolute ethyl alcohol as a dispersing agent, and carrying out ball milling for 12 hours by using a planetary ball mill at the rotating speed of 300 rpm; then baking the slurry obtained by ball milling for 2 hours;
step 4, weighing 110g of dried ceramic powder, adding 85 wt% of solvent (ethyl acetate: 30:70), 1 wt% of dispersant triethanolamine and 0.4 wt% of defoaming agent tributyl phosphate, and fully mixing;
step 5, weighing 7 wt% of PVB and 3 wt% of DOP as a plasticizer in the slurry obtained in the step 4, carrying out secondary ball milling, and then carrying out tape casting;
step 6, cutting the cast membrane into small membranes, and laminating and rolling the membranes to obtain membranes with the thickness of 0.20 mm;
step 7, punching the membrane sheet obtained in the step 6, wherein the diameter of the membrane sheet is 18 mm;
and 8, laminating 8 wafers of the wafer, and carrying out glue discharging, wherein the glue discharging temperature is set to be 600 ℃, the sintering temperature is 1080 ℃, and the sintering time is 6 hours, so as to prepare the potassium-sodium niobate based lead-free piezoelectric ceramic wafer.
Example 2
Referring to fig. 2, this embodiment provides a method for preparing a potassium sodium niobate-based lead-free piezoelectric ceramic sheet, including the following steps:
step 1, according to the general chemical formula (1-x) (K) y Na 1-y )Nb 1-w Sb w O 3 -x(Bi 0.5 Na 0.5 )ZrO 3 -z％Fe 2 O 3 The raw materials are weighed according to the theoretical composition ratio of (A), wherein x represents (Bi) 0.5 Na 0.5 )ZrO 3 Y represents the potassium content in the potassium-sodium niobate, z represents Fe 2 O 3 W represents the content of antimony, x is 0.05, y is 0.45, z is 0.2, w is 0;
step 2, placing the prepared raw materials into a nylon ball milling tank, adding absolute ethyl alcohol as a dispersing agent, and carrying out ball milling for 12 hours by using a planetary ball mill with the rotating speed of 300 rpm; baking the slurry obtained by ball milling for 2 hours; finally, putting the ceramic powder into a program temperature control box type furnace, heating the ceramic powder to 850 ℃, and preserving the heat for 6 hours to obtain ceramic powder;
step 3, placing the pre-sintered ceramic powder in a nylon ball milling tank, adding absolute ethyl alcohol as a dispersing agent, and carrying out ball milling for 12 hours by using a planetary ball mill at the rotating speed of 300 rpm; then baking the slurry obtained by ball milling for 2 hours;
step 4, weighing 110g of dried ceramic powder, adding 85 wt% of solvent (ethyl acetate: 25:75), 1 wt% of dispersant triethanolamine and 0.4 wt% of defoaming agent tributyl phosphate, and fully mixing;
step 5, weighing 7 wt% of PVB and 2.8 wt% of DOP as a plasticizer in the slurry obtained in the step 4, carrying out secondary ball milling and then carrying out tape casting;
step 6, cutting the cast membrane into small membranes, and laminating and rolling the membranes to obtain membranes with the thickness of 0.20 mm;
step 7, punching the membrane obtained in the step 6, wherein the diameter of the membrane is 18 mm;
and step 8, laminating 9 wafers, and discharging the glue, wherein the glue discharging temperature is set to be 600 ℃, the sintering temperature is 1080 ℃, and the sintering time is 6 hours, so as to prepare the potassium-sodium niobate-based lead-free piezoelectric ceramic wafer.
Example 3
The embodiment provides a preparation method of a potassium sodium niobate-based lead-free piezoelectric ceramic sheet, which comprises the following steps:
step 1, according to the general chemical formula (1-x) (K) y Na 1-y )Nb 1-w Sb w O 3 -x(Bi 0.5 Na 0.5 )ZrO 3 -z％Fe 2 O 3 The raw materials are weighed according to the theoretical composition ratio of (A), wherein x represents (Bi) 0.5 Na 0.5 )ZrO 3 Y represents the potassium content in the potassium-sodium niobate, and z represents Fe 2 O 3 W represents the content of antimony, x is 0.045, y is 0.5, z is 0.3, and w is 0.035;
step 2, placing the prepared raw materials into a nylon ball milling tank, adding absolute ethyl alcohol as a dispersing agent, and carrying out ball milling for 12 hours by using a planetary ball mill at the rotating speed of 350 rpm; baking the slurry obtained by ball milling for 2 hours; finally, putting the ceramic powder into a program temperature control box type furnace, heating the ceramic powder to 850 ℃, and preserving the heat for 6 hours to obtain ceramic powder;
step 3, placing the pre-sintered ceramic powder in a nylon ball milling tank, adding absolute ethyl alcohol as a dispersing agent, and carrying out ball milling for 12 hours by using a planetary ball mill at the rotating speed of 350 rpm; then baking the slurry obtained by ball milling for 2 hours;
step 4, weighing 110g of dried ceramic powder, adding 85 wt% of solvent (ethyl acetate: 30:70), 1 wt% of dispersant triethanolamine and 0.4 wt% of defoaming agent tributyl phosphate, and fully mixing;
step 5, weighing 7 wt% of PVB and 3 wt% of DOP as a bonding agent in the slurry obtained in the step 4, carrying out secondary ball milling, and then carrying out tape casting;
step 6, cutting the cast membrane into small membranes, and laminating and rolling the membranes to obtain membranes with the thickness of 0.25 mm;
step 7, punching the membrane sheet obtained in the step 6, wherein the diameter of the membrane sheet is 18 mm;
and 8, laminating 8 wafers of the wafer, and carrying out glue discharging, wherein the glue discharging temperature is set to be 600 ℃, the sintering temperature is 1080 ℃, and the sintering time is 6 hours, so as to prepare the potassium-sodium niobate based lead-free piezoelectric ceramic wafer.
Examples 1 to 3 above were prepared as # 1 to # 3 ceramic diaphragms, respectively, and the 3 kinds of ceramic diaphragms were subjected to quasi-static d 33 The tester and the impedance analyzer respectively perform piezoelectric constant d 33 Electromechanical coupling coefficient k p The results of the measurement are shown in Table 1. The experimental methods used are conventional methods unless otherwise specified.
TABLE 11-3 # ceramic Membrane's relevant piezoelectric Properties
The phase structure of the 1# ceramic membrane was analyzed by PANALYtic/DY 120X-ray diffractometer, and the results are shown in FIG. 1. In fig. 1, the abscissa is a double angle and the ordinate is diffraction intensity, and the results show that: the potassium-sodium niobate-based lead-free piezoelectric ceramic sheet is of a single perovskite structure and has no second phase, and the evidence proves that all doping elements can be dissolved in KNN lattices to form a solid solution with the KNN.
The surface morphology of the 2# ceramic membrane was observed by using a Hitachi/S-3400N electron microscope, as shown in FIG. 2. The results show that: the crystal grain size of the potassium sodium niobate-based lead-free piezoelectric ceramic sheet is in a bimodal state, and no obvious hole is found, so that the diaphragm has high density, and the excellent electrical property of the ceramic can be obtained.
Application example 1
The 1# ceramic membrane prepared in the above example 1 was polarized, adhered to a copper substrate with an epoxy resin adhesive, and cured to prepare a potassium sodium niobate-based lead-free piezoelectric buzzer. The sound pressure of the buzzer is tested according to the change curve of the sound pressure along with the frequency, as shown in figure 3, the driving voltage is 1.75Vp-p, the driving frequency is 4.25kHz, and the sound pressure is 73.9dB when the distance is tested to be 10 cm.
Application example 2
The 2# ceramic membrane prepared in the above example 2 was polarized, adhered to a copper substrate with an epoxy resin adhesive, and cured to prepare a potassium sodium niobate based lead-free piezoelectric buzzer. The sound pressure of the buzzer is tested according to the change curve of the sound pressure along with the frequency, as shown in fig. 4, the driving voltage is 1.75Vp-p, the driving frequency is 4.25kHz, and the sound pressure is 73.3dB when the test distance is 10 cm.
The above is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, without departing from the principle of the present invention, several improvements and modifications may be made, which should also be regarded as the protection scope of the present invention, and other parts of the present invention which are not described in detail belong to the prior art, and therefore are not described herein again, and finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for preparing a potassium-sodium niobate-based leadless piezoelectric ceramic sheet is characterized by comprising the following steps: the method comprises the following steps:
step 1, according to the general chemical formula (1-x) (K) y Na 1-y )Nb 1-w Sb w O 3 -x(Bi 0.5 Na 0.5 )ZrO 3 -z％Fe 2 O 3 Weighing raw materials according to the theoretical composition ratio;
in the formula: x represents (Bi) 0.5 Na 0.5 )ZrO 3 The mole fraction of (c);
y represents the content of potassium in the potassium-sodium niobate;
z represents Fe 2 O 3 The content of (A);
w represents the content of antimony;
step 2, performing ball milling and pre-synthesis on the raw materials to prepare ceramic pre-sintering powder;
step 3, ball-milling the pre-sintered ceramic powder and then drying;
step 4, adding a solvent, a dispersing agent and a defoaming agent into the ceramic powder dried in the step 3, and fully mixing;
step 5, weighing a certain amount of binder and plasticizer in the slurry obtained in the step 4, carrying out secondary ball milling and then carrying out tape casting;
step 6, cutting the cast membrane into small membranes, and laminating and rolling the membranes;
step 7, punching the film obtained in the step 6;
and 8, laminating the wafers punched in the step 7, removing the glue, and sintering to obtain the potassium-sodium niobate based lead-free piezoelectric ceramic sheet.
2. The method for preparing a potassium sodium niobate-based lead-free piezoelectric ceramic sheet as claimed in claim 1, wherein the method comprises the steps of: in the step 1, x is more than 0.00 and less than or equal to 0.055, y is more than 0.00 and less than or equal to 0.5, z is more than 0.00 and less than 0.5, and w is more than or equal to 0.00 and less than or equal to 0.05; the raw material is oxide or carbonate containing seven elements of K, Na, Nb, Bi, Zr, Fe and Sb.
3. The method for preparing a potassium sodium niobate-based lead-free piezoelectric ceramic sheet as claimed in claim 1, wherein the method comprises the steps of: the step 2 comprises the following steps:
step 2a, placing the prepared raw materials into a nylon ball milling tank, adding absolute ethyl alcohol as a dispersing agent, and ball milling for 8-24 h by using a planetary ball mill at the rotating speed of 100-450 rpm;
step 2b, baking the slurry obtained by ball milling for 2-3 h;
and 2c, heating to 800-900 ℃ in a program temperature control box type furnace, and preserving heat for 4-6 h to obtain the ceramic pre-sintering powder.
4. The method for preparing a potassium sodium niobate-based lead-free piezoelectric ceramic sheet as claimed in claim 1, wherein the method comprises the steps of: the step 3 comprises the following steps:
step 3a, placing the ceramic powder in a nylon ball-milling tank, adding absolute ethyl alcohol as a dispersing agent, and ball-milling for 8-24 h by using a planetary ball mill at the rotating speed of 100-450 rpm;
and 3b, baking the slurry obtained by ball milling for 2-3 h.
5. The method for preparing a potassium sodium niobate-based lead-free piezoelectric ceramic sheet as claimed in claim 1, wherein the method comprises the steps of: in the step 4, the added solvent is 80 to 90 weight percent of alcohol and ethyl acetate, the dispersant is 0.5 to 5 weight percent of triethanolamine, and the defoamer is 0.2 to 0.6 weight percent of tributyl phosphate.
6. The method for preparing a potassium sodium niobate-based lead-free piezoelectric ceramic sheet as claimed in claim 1, wherein the method comprises the steps of: in the step 5, the added adhesive is 5 to 10 weight percent of polyvinyl butyral, and the plasticizer is 1 to 5 weight percent of dioctyl phthalate.
7. The method for preparing a potassium sodium niobate-based lead-free piezoelectric ceramic sheet as claimed in claim 1, wherein the method comprises the steps of: the thickness of the film after casting in the step 5 is 0.1 mm-0.25 mm; and in the step 7, the diameter of the round punching sheet is 10-30 mm.
8. The method for preparing a potassium sodium niobate-based lead-free piezoelectric ceramic sheet as claimed in claim 1, wherein the method comprises the steps of: in the step 8, the binder removal temperature is 500-700 ℃, the sintering temperature is 1000-1200 ℃, and the sintering time is 3-7 h.
9. A potassium sodium niobate-based lead-free piezoelectric ceramic sheet to be used for the production method according to any one of claims 1 to 8, characterized in that: general chemical formula (1-x) (K) y Na 1-y )Nb 1-w Sb w O 3 -x(Bi 0.5 Na 0.5 )ZrO 3 -z％Fe 2 O 3 The raw materials are weighed according to the theoretical composition ratio of (A), wherein x represents (Bi) 0.5 Na 0.5 )ZrO 3 0.00 mol fraction of<x is less than or equal to 0.055, y represents the content of potassium in the potassium-sodium niobate, 0.00<y is less than or equal to 0.5, and z represents Fe 2 O 3 Content of (1), 0.00<z is less than 0.5, w represents the content of antimony, and w is more than or equal to 0.00 and less than 0.05.
10. The use of the potassium sodium niobate-based lead-free piezoelectric ceramic sheet as set forth in claim 9, wherein: the potassium-sodium niobate-based lead-free piezoelectric ceramic sheet is applied to a buzzer.
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