CN113896532A - Potassium sodium niobate-based ceramic with high piezoelectric performance and preparation method thereof - Google Patents
Potassium sodium niobate-based ceramic with high piezoelectric performance and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 19
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000000498 ball milling Methods 0.000 claims abstract description 10
- 239000011734 sodium Substances 0.000 claims abstract description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 8
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052709 silver Inorganic materials 0.000 claims abstract description 8
- 239000004332 silver Substances 0.000 claims abstract description 8
- 238000007599 discharging Methods 0.000 claims abstract description 6
- 239000003292 glue Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 18
- 230000010287 polarization Effects 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 239000002002 slurry Substances 0.000 claims description 4
- 239000004677 Nylon Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 229920001778 nylon Polymers 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 2
- 230000005684 electric field Effects 0.000 claims description 2
- 238000005469 granulation Methods 0.000 claims description 2
- 230000003179 granulation Effects 0.000 claims description 2
- 239000011268 mixed slurry Substances 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 238000001354 calcination Methods 0.000 abstract 2
- 239000013078 crystal Substances 0.000 abstract 1
- UKDIAJWKFXFVFG-UHFFFAOYSA-N potassium;oxido(dioxo)niobium Chemical compound [K+].[O-][Nb](=O)=O UKDIAJWKFXFVFG-UHFFFAOYSA-N 0.000 abstract 1
- 239000000463 material Substances 0.000 description 5
- 238000011160 research Methods 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling 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
- 239000000203 mixture Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses a potassium niobate-based leadless piezoelectric ceramic and a preparation method thereof, and the potassium sodium niobate-based leadless piezoelectric ceramic comprises the following components in percentage by weight: (0.97-x)K0.48Na0.52NbO3‑0.03(Bi0.5Na0.35Li0.15)ZrO3‑xAgSbO3Whereinx=0, 0.01, 0.015, 0.02, 0.025, 0.03, 0.04. The preparation method is that K is2CO3，Na2CO3，Nb2O5，Sb2O3，Bi2O3，ZrO2，Li2CO3，Ag2Accurately weighing the raw materials O according to the stoichiometric ratio, mixing with ethanol for ball milling, calcining the raw materials after ball milling and drying at the calcining temperature of 870 ℃, and then calciningAnd sintering the sample at 1080 ℃ after secondary ball milling, drying, granulating, tabletting and glue discharging. After the surface of the ceramic is coated with silver paste, the novel piezoelectric ceramic is obtained by planning treatment. In the invention, Sb3+、Ag+Doped to 0.97K0.48Na0.52NbO3‑0.03(Bi0.5Na0.35Li0.15)ZrO3In system crystal lattice, and improves sintering system, realizes multiphase coexistence of ceramics at room temperature, and prepares the novel piezoelectric ceramics. Through testing, the system realizes the piezoelectric ceramicsd 33=168 pC/N，ε rExcellent piezoelectric properties of = 4500.
Description
Technical Field
The invention relates to potassium-sodium niobate based leadless piezoelectric ceramics and a preparation method thereof, belonging to the field of novel leadless functional ceramics.
Background
Lead zirconate titanate (PZT) ceramic is the most representative of the traditional lead-based piezoelectric ceramic, and is widely applied due to good piezoelectric performance and temperature stability. However, the lead-based piezoelectric material contains a large amount of lead, and the lead is volatilized during production and use, so that the lead-based piezoelectric material poses great threats to the environment and human health. In addition, the european union, japan, and other national regions have already issued relevant legal policies to limit the use of lead-based piezoelectric materials. Therefore, it is a very urgent work to develop new piezoelectric ceramics to replace the conventional lead-based piezoelectric materials. Among the lead-free piezoelectric ceramics, those with excellent performance belong to perovskite structure type piezoelectric ceramics, and have great research value. Compared with KNN-based ceramics, both BT-based ceramics and BNT-based ceramics have disadvantages of low piezoelectric coefficient, low mechanical quality factor, and difficulty in polarization. In addition, the KNN-based ceramic has good piezoelectric property, high Curie temperature and large dielectric constant, so the research on the KNN-based piezoelectric ceramic is developed in the experiment.
The invention aims to prepare the lead-free piezoelectric ceramic with high density and good piezoelectric property by adopting a simple preparation process. Compared with the traditional sintering method, the production cost is reduced, the piezoelectric performance is improved, and the further development of the lead-free piezoelectric ceramic is promoted.
Disclosure of Invention
1. In view of the problems mentioned in the background of the invention, the invention aims to prepare potassium-sodium niobate based lead-free piezoelectric ceramics with good electrical properties, and aims to provide a ceramic green body sintering method which effectively improves the sintering property and piezoelectric property of KNN based ceramics.
2. In order to achieve the technical purpose, the technical scheme of the invention is as follows:
the preparation method of the potassium-sodium niobate based leadless piezoelectric ceramic comprises the following raw materials and the mol percentage content of the raw materials is (0.97-x)K0.48Na0.52NbO3-0.03(Bi0.5Na0.35Li0.15)ZrO3-xAgSbO3Whereinx=0, 0.01, 0.015, 0.02, 0.025, 0.03, 0.04, the main raw materials are: k2CO3，Na2CO3， Nb2O5，Sb2O3，Bi2O3， ZrO2，Li2CO3，Ag2And O. The preparation method is characterized by comprising the following steps:
and (4) batching. Will K2CO3，Na2CO3， Nb2O5，Sb2O3，Bi2O3， ZrO2，Li2CO3，Ag2Accurately weighing and mixing O powder according to a stoichiometric ratio, ball-milling the O powder for 24 hours in a nylon tank filled with zirconia balls as grinding balls by taking absolute ethyl alcohol as a medium to obtain uniformly mixed slurry, and drying the slurry for 12 hours in an oven at 100 ℃;
and (6) pre-burning. Sieving the dried powder, pre-sintering, heating to 870 ℃ at 4 ℃/min, preserving heat for 6 hours, and naturally cooling to room temperature. In order to mix the raw materials more uniformly and crush the raw materials more completely, achieve the best mixing effect and obtain the required granularity, the raw materials need to be subjected to secondary ball milling. Drying the slurry subjected to ball milling in a drying oven at 100 ℃ for 12 hours;
and (4) granulating and tabletting. Adding 7 wt% of polyvinyl alcohol (PVA) into the dried powder, fully grinding the powder to complete granulation operation, tabletting the powder, and pressing the powder into a cylindrical green body with the diameter of 10 mm and the thickness of 0.8-1.2 mm;
and (6) discharging the glue. Placing the pressed green body in a muffle furnace for glue discharging, wherein the heating rate is 1 ℃/min, and keeping the temperature of a sample at 120 ℃ and 850 ℃ for 60min and 120 min respectively to finish the glue discharging treatment;
and (5) sintering. Carrying out powder embedding sintering on the ceramic wafer subjected to binder removal, and carrying out sectional sintering during sintering, wherein the optimal sintering temperature is 1080 ℃ and the heat preservation time is 10 h, so that a high-density ceramic sample is obtained;
silver-coated polarization. And (3) grinding and polishing the sintered ceramic wafer, then coating a layer of silver paste on the surface of the ceramic wafer, and then, preserving heat at 550 ℃ for 60min to sinter a silver electrode to finish the silver coating operation. And applying voltage to the silver-coated ceramic for polarization, wherein the polarization electric field is 3 kV/mm, the polarization time is 30 min, and the polarization temperature is room temperature, so that the potassium sodium niobate based lead-free piezoelectric ceramic sample is finally obtained.
Researches show that a sintering system has great influence on the sintering characteristics and the electrical properties of the KNN lead-free piezoelectric ceramic.
The invention has the beneficial effects that:
(1) the density of the KNN ceramic chip prepared by the preparation method of the lead-free piezoelectric ceramic powder is about 93 percent, and is greatly improved compared with that of the KNN ceramic chip prepared by the traditional solid-phase sintering method;
(2) the KNN-based lead-free piezoelectric ceramic prepared by the method has good electrical property and dielectric constantε r =4500，d 33 =168pC/N。
Drawings
FIG. 1 is an XRD pattern of a piezoelectric ceramic sample; FIG. 2 is a dielectric curve of a piezoelectric ceramic sample.
Detailed Description
The present invention will be further specifically described in detail with reference to specific examples to enable those skilled in the art to better understand the present invention, but the present invention is not limited to the following examples, and the process parameters not particularly mentioned may be performed according to conventional techniques.
Example 1
(1) Mixing the raw materials according to the chemical formula of 0.96K0.48Na0.52Nb0.96Sb0.04-0.04Bi x0.5(1+)Na0.5HfO3The mixture ratio of the components is weighed and proportioned.
(2) And (2) filling the powder obtained in the step (1) into a nylon tank, adding zirconia ball stones, taking absolute ethyl alcohol as a ball milling medium, performing ball milling for 24 hours, discharging, drying, and sieving with a 300-mesh sieve to obtain mixed powder with good fluidity.
(3) Putting the mixed powder in the step (2) into a corundum crucible, and presintering for 6 hours at 870 ℃, wherein the presintering temperature curve is as follows: keeping the temperature from normal temperature to 870 ℃ for 6 h (the heating rate is 3 ℃/min), and then naturally cooling. Grinding the prepared powder by using 7 wt% of polyvinyl alcohol as a binder, granulating, sieving by using a 100-mesh sieve, and pressing the obtained powder into a cylindrical green compact with the diameter of 10 mm and the thickness of 0.8-1.2 mm.
(4) After the ceramic chip in the step (3) is subjected to glue removal, sealing and burying materials with the same components, and sintering in a muffle furnace at 1080 ℃ for 10 hours to finally obtain a lead-free piezoelectric ceramic sample; and applying 3 kV/mm direct current voltage after coating silver electrodes on two surfaces of the ceramic wafer, and polarizing in silicon oil. Having a piezoelectric constant ofd 33 =180pC/N。
Claims (2)
1. The preparation method of the potassium-sodium niobate based leadless piezoelectric ceramic is characterized in that the components and the molar percentage content thereof are (0.97-x)K0.48Na0.52NbO3-0.03(Bi0.5Na0.35Li0.15)ZrO3-xAgSbO3Whereinx=0，0.01，0.015，0.02，0.025，0.03，0.04。
2. The method of claim 1, wherein the process comprises the following steps in sequence: (1) will K2CO3，Na2CO3， Nb2O5，Sb2O3，Bi2O3， ZrO2，Li2CO3，Ag2Accurately weighing and mixing O powder according to a stoichiometric ratio, ball-milling the O powder for 24 hours in a nylon tank filled with zirconia balls as grinding balls by taking absolute ethyl alcohol as a medium to obtain uniformly mixed slurry, and drying the slurry for 12 hours in an oven at 100 ℃; (2) sieving the powder obtained in the step (1), pre-burning, heating to 870 ℃ at a speed of 4 ℃/min, preserving heat for 6 hours, naturally cooling to room temperature, performing secondary ball milling on the raw materials in order to mix the raw materials more uniformly and crush the raw materials more completely, realizing the optimal mixing effect and obtaining the required granularity, and drying the ball-milled slurry in a 100 ℃ oven for 12 hours; (3) adding 7 wt% of polyvinyl alcohol (PVA) into the powder obtained in the step (2) to complete granulation, tabletting the powder and removing glueThe temperature rise rate is 1 ℃/min, so that the samples are respectively kept at 120 ℃ and 850 ℃ for 60min and 120 min to finish the glue discharging treatment; (4) carrying out powder embedding sintering on the ceramic wafer obtained in the step (3), and carrying out sectional sintering during sintering, wherein the optimal sintering temperature is 1080 ℃, and the heat preservation time is 10 h, so that a high-density ceramic sample is obtained; (5) and (4) carrying out silver coating and polarization on the ceramic wafer obtained in the step (4), wherein the polarization electric field is 3 kV/mm, the polarization time is 30 min, and the polarization temperature is room temperature, so as to finally obtain the potassium sodium niobate based lead-free piezoelectric ceramic sample.
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