CN116283286A - Sodium niobate-based leadless piezoelectric textured ceramic and preparation method thereof - Google Patents
Sodium niobate-based leadless piezoelectric textured ceramic and preparation method thereof Download PDFInfo
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- CN116283286A CN116283286A CN202310236575.2A CN202310236575A CN116283286A CN 116283286 A CN116283286 A CN 116283286A CN 202310236575 A CN202310236575 A CN 202310236575A CN 116283286 A CN116283286 A CN 116283286A
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- leadless piezoelectric
- sodium niobate
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- 239000000919 ceramic Substances 0.000 title claims abstract description 83
- UYLYBEXRJGPQSH-UHFFFAOYSA-N sodium;oxido(dioxo)niobium Chemical compound [Na+].[O-][Nb](=O)=O UYLYBEXRJGPQSH-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000000126 substance Substances 0.000 claims abstract description 14
- 238000010532 solid phase synthesis reaction Methods 0.000 claims abstract description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 22
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 19
- 229910052709 silver Inorganic materials 0.000 claims description 19
- 239000004332 silver Substances 0.000 claims description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 17
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- 150000003839 salts Chemical class 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 13
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000007599 discharging Methods 0.000 claims description 12
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 12
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 12
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 12
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 11
- 239000002243 precursor Substances 0.000 claims description 10
- 238000005266 casting Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000010955 niobium Substances 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000003292 glue Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 239000011780 sodium chloride Substances 0.000 claims description 8
- 239000010936 titanium Substances 0.000 claims description 8
- 239000004408 titanium dioxide Substances 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 7
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 7
- 229910001887 tin oxide Inorganic materials 0.000 claims description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 6
- 238000007731 hot pressing Methods 0.000 claims description 6
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 239000002270 dispersing agent Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 239000012046 mixed solvent Substances 0.000 claims description 5
- 230000010287 polarization Effects 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 230000000630 rising effect Effects 0.000 claims description 4
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- BAECOWNUKCLBPZ-HIUWNOOHSA-N Triolein Natural products O([C@H](OCC(=O)CCCCCCC/C=C\CCCCCCCC)COC(=O)CCCCCCC/C=C\CCCCCCCC)C(=O)CCCCCCC/C=C\CCCCCCCC BAECOWNUKCLBPZ-HIUWNOOHSA-N 0.000 claims description 3
- PHYFQTYBJUILEZ-UHFFFAOYSA-N Trioleoylglycerol Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC(OC(=O)CCCCCCCC=CCCCCCCCC)COC(=O)CCCCCCCC=CCCCCCCCC PHYFQTYBJUILEZ-UHFFFAOYSA-N 0.000 claims description 3
- 230000005684 electric field Effects 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 claims description 3
- 239000004014 plasticizer Substances 0.000 claims description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- PHYFQTYBJUILEZ-IUPFWZBJSA-N triolein Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CCCCCCCC)COC(=O)CCCCCCC\C=C/CCCCCCCC PHYFQTYBJUILEZ-IUPFWZBJSA-N 0.000 claims description 3
- 229940117972 triolein Drugs 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims 1
- 230000026683 transduction Effects 0.000 abstract description 25
- 238000010361 transduction Methods 0.000 abstract description 25
- 230000008859 change Effects 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 238000010345 tape casting Methods 0.000 description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 2
- 244000137852 Petrea volubilis Species 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- 238000001757 thermogravimetry curve Methods 0.000 description 2
- 241000234642 Festuca Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000002059 diagnostic imaging Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 1
- 239000011777 magnesium 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
- 239000008177 pharmaceutical agent Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a sodium niobate based leadless piezoelectric textured ceramic and a preparation method thereof, wherein the leadless piezoelectric textured ceramic has a chemical general formula of (90-x) NaNbO 3 ‑10Ba(Ti 0.7 Sn 0.3 )O 3 ‑xNaSbO 3 +2‑6wt.％NaNbO 3 X is more than or equal to 0 and less than or equal to 2.0. Compared with the prior art, the invention can obtain the composite material with high-voltage electric performance by combining the traditional solid phase synthesis method with the template grain growth method>400 pC/N) and temperature stabilityGood transduction coefficient (from room temperature to 60 ℃ C., transduction coefficient>10000×10 ‑15 m 2 N, rate of change<25 percent) of sodium niobate based leadless piezoelectric textured ceramic has very important significance for developing environment-friendly leadless piezoelectric materials, and has higher practical value in the fields of low and medium temperature transducers, drivers and the like.
Description
Technical Field
The invention belongs to the technical field of electronic functional ceramics, and relates to sodium niobate-based leadless piezoelectric textured ceramics and a preparation method thereof.
Background
The piezoelectric ceramic is an electromechanical coupling electronic information material, and can mutually convert mechanical energy and electric energy; and piezoelectric ceramics have dielectric properties, elasticity, and the like in addition to piezoelectricity, and have been widely used in medical imaging, acoustic sensors, acoustic transducers, ultrasonic motors, and the like.
Among the various types of ferroelectric materials, lead-containing piezoelectric ceramics (PZT) are pillars of piezoelectric materials due to their excellent piezoelectric properties and temperature stability. In the late 80 s, a relaxor ferroelectric ceramic has been developed as a base material for a series of electroacoustic devices and piezoelectric devices, such as a lead magnesium niobate (Pb (Mg) 1/3 Nb 2/3 )(ZrTi)O 3 ) Can be widely applied to sound pick-up and microphone. However, lead is strongly toxic and has been listed as fescue on the hazard list; in addition, lead oxide is used in a large amount in the preparation process, and the content exceeds 60%, which causes great harm to human bodies and the environment. Therefore, many countries and regions are or have been formulated to limit or stop the use of harmful substances for the purpose of protecting the environment and humans.
NN-based piezoelectric ceramics are ceramic materials with good process tolerance and have good dielectric, piezoelectric and ferroelectric properties, and by introducing different elements, higher piezoelectric properties can be obtained in NN-based piezoelectric ceramics. QiPr et al (https:// doi. Org/10.1111/jace.14944: naNbO) 3 -BaTiO 3 -NaSbO 3 lead and potassium-free ceramics with thermally stable small-signal piezoelectric properties) to obtain a NN-based piezoelectric ceramic with high piezoelectric performance, 252pC/N piezoelectric activity, a dielectric constant of 1500, and a transduction coefficient of 4780×10 -15 m 2 N. Although a large number of researchers are continuously innovating in the field of NN-based piezoelectric ceramics, satisfactory performance is difficult to achieve, and the piezoelectric performance is generally [ ]<300 pC/N) is undesirable and causes a large increase in dielectric constant while improving piezoelectric performance, resulting in a decrease in transduction coefficient, which is very unfavorable for the energy collection ability of the material, failing to satisfyApplication requirements of devices such as ultrasonic and transduction.
Patent CN113698204A discloses a potassium-sodium niobate based leadless piezoelectric textured ceramic with high piezoelectric response and high Curie temperature and a preparation method thereof, wherein the chemical general formula of the potassium-sodium niobate based leadless piezoelectric textured ceramic is 0.99K 0.5 Na 0.5 Nb 1-x Ta x -0.01Bi(Ni 2/3 Nb 1/3 )O 3 +4wt.％NaNbO 3 Wherein x is more than or equal to 0.04 and less than or equal to 0.12. Although the patent adopts the sodium niobate seed crystal template to obtain the high-texture KNN-based piezoelectric ceramic, the components do not take sodium niobate as the main component, the lattice suitability is large, the preparation is difficult, the characterization of the transduction coefficient is not available, and the energy collection capability cannot be intuitively judged.
Patent CN104860674A discloses a ceramic material of stress sensor capacitor and its preparation method, which comprises BaO and TiO 2 NiO, znO and Nb 2 O 5 As raw material according to BaTi 1-1.5x Ni 0.25x Zn 0.25x Nb x O 3 The preparation method comprises the steps of chemical formula proportioning, calcining, secondary ball milling, drying, granulating, forming, glue discharging and sintering, wherein x=0.01-0.03. Although the patent prepares a pressure sensing capacitor, the piezoelectric coefficient is low, and the energy collection capacity cannot be intuitively judged without characterization of the transduction coefficient.
Disclosure of Invention
The invention aims to overcome at least one defect in the prior art and provide the sodium niobate-based leadless piezoelectric textured ceramic and the preparation method thereof.
The aim of the invention can be achieved by the following technical scheme:
one of the technical proposal of the invention is to provide a sodium niobate based leadless piezoelectric textured ceramic with a chemical general formulaIs (90-x) NaNbO 3 -10Ba(Ti 0.7 Sn 0.3 )O 3 -xNaSbO 3 +2-6wt.% (relative to the mass of the whole powder) NaNbO 3 ，0≤x≤2.0。
As a preferable technical scheme, x is 0, 1.0, 1.5 or 2.0.
The crystal grain orientation of the leadless piezoelectric textured ceramic is that<001> C >85％。
The invention provides a preparation method of sodium niobate-based leadless piezoelectric textured ceramic, which comprises the following steps:
(1) Solid phase synthesis: selecting sodium carbonate (Na) 2 CO 3 ) Barium carbonate (BaCO) 3 ) Niobium pentoxide (Nb) 2 O 5 ) Titanium dioxide (TiO) 2 ) Tin oxide (SnO) 2 ) And antimony trioxide (Sb) 2 O 3 ) Weighing materials according to chemical compositions, adding a ball milling medium for ball milling and mixing completely, discharging and drying, placing the materials into an alumina crucible for calcination, then adding the ball milling medium for ball milling, discharging and drying to obtain a powder base material;
(2) Two-step molten salt method combined separation method: in the first step, bismuth trioxide (Bi 2 O 3 ) Synthesizing, separating and filtering sodium carbonate, niobium pentoxide and molten salt to obtain a flaky precursor Bi 2.5 Na 3.5 Nb 5 O 18 The second step is to reuse the flake precursor and potassium carbonate (K) 2 CO 3 ) And molten salt are synthesized, separated and filtered to obtain high-quality pure sodium niobate (NaNbO) 3 ) A sheet-like template;
(3) Template grain growth method: adding the powder base material obtained in the step (1) and the sheet-shaped template obtained in the step (2) into a mixed solvent and a dispersing agent respectively, performing primary mixing by using a roll mill, then adding a plasticizer and a binder respectively, and performing secondary mixing by using the roll mill to obtain casting slurry;
(4) And (3) a casting process: carrying out tape casting on the tape casting slurry obtained in the step (3) by using a convenient and small-sized coating machine, and then drying to form a dry thick film with certain toughness and plasticity;
(5) And (3) hot pressing: cutting the dried thick film obtained in the step (4) into a required shape, stacking the thick film layer by layer, and finally performing hot pressing to form a ceramic green body;
(6) And (3) a glue discharging process: placing the ceramic green body obtained in the step (5) in a muffle furnace for glue discharging to obtain a ceramic green body;
(7) The sintering process by a two-step method comprises the following steps: sintering the ceramic blank obtained in the step (6) by a two-step method, naturally cooling to room temperature, and polishing by sand paper to obtain a ceramic sheet;
(8) Silver burning process: coating silver paste on the ceramic sheet obtained in the step (7), placing the ceramic sheet in a muffle furnace for silver burning to obtain ceramic coated with silver electrodes, and then carrying out electrical test;
(9) And (3) polarization technology: and (3) placing the ceramic coated with the silver electrode obtained in the step (8) in a silicone oil bath for polarization to obtain the sodium niobate-based leadless piezoelectric textured ceramic.
As a preferable technical scheme, the first half ((90-x) NaNbO) of the chemical formula 3 -10Ba(Ti 0.7 Sn 0.3 )O 3 -xNaSbO 3 ) Is prepared by solid phase synthesis, the latter half (4 wt.% NaNbO) 3 ) Is realized by a two-step molten salt method and adding a sheet template by combining a separation method.
Further, in the step (1), the ball milling time is 10-15 hours, the calcining temperature is 800-900 ℃ and the time is 3-8 hours.
As a preferable technical scheme, the ball milling medium in the step (1) is deionized water, absolute ethyl alcohol or n-butyl alcohol.
Further, sodium chloride (NaCl) is adopted as molten salt in the step (2), the total mass ratio of raw materials and the molten salt is 1 (1.0-1.2), the heat preservation time is 2-4 hours, the mass ratio of bismuth trioxide, sodium carbonate and niobium pentoxide in the first step is 6.5-7.0, (1.7-2.1) and (5.0-5.5), the melting temperature is 1000-1100 ℃, the mass ratio of the flaky precursor and the potassium carbonate in the second step is 1 (1.75-2.00), and the melting temperature is 900-1000 ℃.
The separating agent adopts sodium tripolyphosphate, the stirring speed is 600-800rpm, the stirring time is 3-4h, the mass ratio of the first-step flaky precursor to the separating agent is (3-4): 1, and the mass ratio of the second-step flaky template to the separating agent is (2-3): 1.
As a preferable technical scheme, the length of the sheet template in the step (2) is 30-40 mu m, and the thickness is 1-2 mu m.
Further, in the step (3), 2-butanone or toluene is adopted as a mixed solvent, absolute ethyl alcohol, triolein is adopted as a dispersing agent, polyethylene glycol and dibutyl phthalate are adopted as a plasticizing agent, polyvinyl butyral is adopted as a binder, powder base material, a sheet template and each reagent have the mass ratio of (9.4-9.8), (9-11), (4-6), (0.32-0.37), (0.9-1.2), and the mixing and stirring speed is 15-17r/min for 3-4h.
Further, the casting doctor blade advancing rate in the step (4) is 30-40cm/min.
As a preferable technical scheme, the thickness of the dry thick film in the step (4) is 100-150 mu m.
As a preferable technical scheme, the hot pressing temperature in the step (5) is 60-80 ℃ and the pressure is 10-12MPa.
Further, the glue discharging temperature in the step (6) is 500-600 ℃, and the heat preservation time is 5-10h.
Further, in the step (7), the temperature rising rate is 3-5 ℃/min, the temperature rising temperature is 1280-1320 ℃, the heat is not preserved, the temperature falling rate is 10-20 ℃/min, the temperature falling temperature is 1180-1220 ℃, and the heat preserving time is 3-9h.
As a preferable technical scheme, the granularity of the abrasive paper in the step (7) is 400-1200 meshes, and the polishing granularity is 0.3-0.5mm.
Further, in the step (8), the diameter of the silver paste is 3-6mm, the silver burning temperature is 450-800 ℃, and the heat preservation time is 5-20min.
Further, in the step (9), the polarization electric field is 20-40kV/mm, and the time is 10-20min.
In previous studies (https:// doi. Org/10.1021/acsami.2c14737: high Piezoelectricity in Eco-friedly NaNbO) 3 Based Ferroelectric Relaxor Ceramics via Phase and Domain Engineering) of random (90-x) NaNbO 3 -10Ba(Ti 0.7 Sn 0.3 )O 3 -xNaSbO 3 Ceramics have excellent piezoelectric activityBut has higher dielectric constant, the dielectric constant is reduced while the piezoelectric activity is further improved by the texturing process, and the NN-based piezoelectric ceramic has high lattice adaptation degree with an NN seed crystal template, so that the preparation is easier.
Compared with the prior art, the invention has the following advantages:
(1) The invention adopts the solid phase synthesis method and the template grain growth method to prepare the composite material with high-voltage electric performance>400 pC/N), high transduction coefficient (=13100×10 -15 m 2 N) and good temperature stability (room temperature to 60 ℃ C., transduction coefficient>10000×10 -15 m 2 N, rate of change<25%) lead-free piezoelectric textured ceramic;
(2) The preparation method is simple, economical and practical, belongs to a lead-free material, does not pollute the environment in the preparation, application and waste processes, and is an environment-friendly high-performance piezoelectric material.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of a sodium niobate-based leadless piezoelectric textured ceramic according to example 2 of the present invention;
FIG. 2 is an XRD pattern of sodium niobate-based leadless piezoelectric textured ceramics in examples 1, 3 and 4 of the invention;
FIG. 3 is a Scanning Electron Microscope (SEM) image of a sodium niobate-based leadless piezoelectric textured ceramic of example 2 of the present invention;
FIG. 4 is a dielectric thermogram of sodium niobate-based leadless piezoelectric textured ceramic of example 2 of the present invention;
FIG. 5 is a dielectric thermogram of sodium niobate-based leadless piezoelectric textured ceramics of examples 1, 3 and 4 of the present invention;
FIG. 6 is a graph showing the hysteresis loop of the sodium niobate-based leadless piezoelectric textured ceramic of example 2 of the present invention;
FIG. 7 is a graph showing the statistics of piezoelectric coefficient and transduction coefficient of sodium niobate-based leadless piezoelectric textured ceramic in example 2 of the present invention;
FIG. 8 is a graph of the transduction coefficient versus temperature for sodium niobate-based leadless piezoelectric textured ceramics in example 2 of the invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. The present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following examples.
The equipment used in the following examples is representative of conventional equipment in the art unless otherwise specified; unless otherwise indicated, all reagents used are commercially available or prepared by methods conventional in the art, and all of the following examples, not specifically described, are accomplished by means of conventional experimentation in the art.
Sodium carbonate (Na) 2 CO 3 ) Barium carbonate (BaCO) 3 ) Niobium pentoxide (Nb) 2 O 5 ) Titanium dioxide (TiO) 2 ) Tin oxide (SnO) 2 ) Antimony trioxide (Sb) 2 O 3 ) Bismuth trioxide (Bi) 2 O 3 ) Sodium chloride (NaCl) and potassium carbonate (K) 2 CO 3 ) Purity is more than 99%, and all medicines are from national pharmaceutical and chemical reagent limited company.
Example 1:
the chemical composition of the sodium niobate-based leadless piezoelectric textured ceramic is (90-x) NaNbO 3 -10Ba(Ti 0.7 Sn 0.3 )O 3 -xNaSbO 3 +4wt.％NaNbO 3 Wherein x=1.0, and the preparation method comprises the following specific steps:
(1) 6.83g sodium carbonate (Na) 2 CO 3 ) 2.99g of barium carbonate (BaCO) 3 ) 16.92g of niobium pentoxide (Nb) 2 O 5 ) 0.86g of titanium dioxide (TiO 2 ) 0.68g of tin oxide (SnO) 2 ) And 0.22g of antimony trioxide (Sb 2 O 3 ) Weighing raw materials serving as lead-free piezoelectric ceramic materials according to chemical compositions, adding absolute ethyl alcohol serving as a ball milling medium, ball milling for 12 hours, discharging, drying, placing into an alumina crucible, calcining for 5 hours at 900 ℃, then adding absolute ethyl alcohol, ball milling for 12 hours, discharging, and drying to obtain a powder base material;
(2) The first step was carried out by a conventional two-stage molten salt method in combination with separation, using 6.5g of bismuth trioxide (Bi 2 O 3 ) 1.9g of carbonSynthesizing sodium acid, 5.3g of niobium pentoxide and 15.0g of sodium chloride (NaCl) fused salt, melting and preserving heat for 3 hours at 1100 ℃, adding 3.5g of sodium tripolyphosphate at 600rpm for separation for 4 hours, and filtering to obtain 11g of flaky precursor Bi 2.5 Na 3.5 Nb 5 O 18 In the second step, 10g of the flake precursor and 20g of potassium carbonate (K) 2 CO 3 ) And 30g sodium chloride fused salt are synthesized, the mixture is melted and kept at 950 ℃ for 3 hours, 0.6g sodium tripolyphosphate is added at 600rpm for 4 hours, and 1.2g high-quality pure sodium niobate (NaNbO) is obtained after filtration 3 ) A sheet template having a length of 30 μm and a thickness of 1 μm;
(3) Adding 10g of 2-butanone and 5g of absolute ethyl alcohol into 9.6g of the powder base material obtained in the step (1) and 0.4g of the sheet template obtained in the step (2) as mixed solvents respectively, primarily mixing for 4 hours by a roll mill at 16r/min with 0.35g of triolein as a dispersing agent, and secondarily mixing for 4 hours by a roll mill at 16r/min with 0.35g of polyethylene glycol and 0.35g of dibutyl phthalate as plasticizers and 1.1g of polyvinyl butyral as binders to obtain casting slurry;
(4) Carrying out tape casting on the tape casting slurry obtained in the step (3) by using a convenient and small-sized coating machine, wherein the travelling speed of a scraper is 30cm/min, and then drying to form a dry thick film with certain toughness and plasticity, wherein the thickness is 120 mu m;
(5) Cutting the dried thick film obtained in the step (4) into a required shape, stacking the thick film layer by layer, and finally hot-pressing the thick film at 70 ℃ and 10-12MPa to form a ceramic green body;
(6) Placing the ceramic green body obtained in the step (5) in a muffle furnace for glue discharging, and preserving heat for 10 hours at 550 ℃ to obtain a ceramic green body;
(7) Sintering the ceramic blank obtained in the step (6) by a two-step method, wherein the temperature is raised to 1320 ℃ at 3 ℃/min, the temperature is not kept, then 10 ℃/min is lowered to 1220 ℃, the temperature is kept for 9 hours, the ceramic blank is naturally cooled to room temperature, and then the ceramic blank is ground and polished to 0.4mm by using 800-mesh sand paper to obtain a ceramic sheet;
(8) Silver burning process: coating silver paste with the diameter of 4mm on the ceramic sheet obtained in the step (7), placing the ceramic sheet in a muffle furnace for silver burning, preserving heat at 560 ℃ for 10min to obtain ceramic coated with silver electrodes, and then carrying out electrical test;
(9) And (3) polarization technology: and (3) placing the ceramic coated with the silver electrode obtained in the step (8) in a silicone oil bath, and polarizing the ceramic for 15min under an electric field of 30kV/mm to obtain the sodium niobate-based leadless piezoelectric textured ceramic with high piezoelectric performance and temperature insensitive transduction coefficient.
As shown in FIG. 2, the present embodiment is that<001> C The direction has a very high degree of texture (f=91%).
As shown in FIG. 5, the present example has a relatively high Curie temperature (125 ℃ C.).
As shown in fig. 7, the present embodiment has excellent piezoelectric characteristics and transduction coefficient (piezoelectric coefficient=340 pC/N, transduction coefficient=10200×10 -15 m 2 /N)。
Example 2:
the chemical composition of the sodium niobate-based leadless piezoelectric textured ceramic is (90-x) NaNbO 3 -10Ba(Ti 0.7 Sn 0.3 )O 3 -xNaSbO 3 +4wt.％NaNbO 3 Wherein x=1.5, sodium carbonate 6.83g, barium carbonate 2.99g, niobium pentoxide 16.82g, titanium dioxide 0.86g, tin oxide 0.68g, antimony trioxide 0.33g, the same procedure as in example 1 was followed.
As shown in fig. 1 and 3, the present embodiment is that<001> C The direction has a very high texture (f=93%) and the grain size is large.
As shown in FIG. 4, the present example has a relatively high Curie temperature (100 ℃ C.).
As shown in fig. 6, this embodiment also exhibits a very saturated hysteresis loop.
As shown in fig. 7, the present embodiment has excellent piezoelectric characteristics and transduction coefficient (piezoelectric coefficient=423 pC/N, transduction coefficient=13100×10) -15 m 2 /N)。
As shown in FIG. 8, the transduction coefficient of the present embodiment decreases with increasing temperature, and then decreases rapidly, the transduction coefficient change rate is 23% from room temperature to 60 ℃, and the value is greater than 10.1X10 -12 m 2 N, exhibits excellent temperature stability. The piezoelectric coefficient can be greatly changed along with the temperature due to the texturing process, and the embodiment is greatly changedThe temperature stability of the transduction coefficient of the sodium niobate base is improved.
Example 3:
the chemical composition of the sodium niobate-based leadless piezoelectric textured ceramic is (90-x) NaNbO 3 -10Ba(Ti 0.7 Sn 0.3 )O 3 -xNaSbO 3 +4wt.％NaNbO 3 Wherein x=2.0, sodium carbonate 6.83g, barium carbonate 2.99g, niobium pentoxide 16.71g, titanium dioxide 0.86g, tin oxide 0.68g, antimony trioxide 0.44g, and the same preparation as in example 1.
As shown in FIG. 2, the present embodiment is that<001> C The direction has a very high degree of texture (f=89%).
As shown in FIG. 5, the present example has a relatively high Curie temperature (65 ℃ C.).
As shown in fig. 7, the present embodiment has excellent piezoelectric characteristics and transduction coefficient (piezoelectric coefficient=350pc/N, transduction coefficient=6920×10) -15 m 2 /N)。
Example 4:
the chemical composition of the sodium niobate-based leadless piezoelectric textured ceramic is (90-x) NaNbO 3 -10Ba(Ti 0.7 Sn 0.3 )O 3 -xNaSbO 3 +4wt.％NaNbO 3 Wherein x=0, 6.83g of sodium carbonate, 2.99g of barium carbonate, 17.12g of niobium pentoxide, 0.86g of titanium dioxide and 0.68g of tin oxide, the same preparation method as in example 1.
As shown in FIG. 2, the present embodiment is that<001> C The direction has a very high degree of texture (f=92%).
As shown in FIG. 5, the present example has a relatively high Curie temperature (150 ℃ C.).
As shown in fig. 7, the present embodiment has excellent piezoelectric characteristics and transduction coefficient (piezoelectric coefficient=280 pC/N, transduction coefficient=12600×10) -15 m 2 /N)。
Comparing four examples, it can be found that the textured ceramic prepared in example 2 has higher texture degree, higher piezoelectric coefficient and higher transduction coefficient, and has higher curie temperature, better thermal stability of transduction coefficient, and very strong potential for application in high electromechanical coupling devices.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (10)
1. A sodium niobate-based leadless piezoelectric textured ceramic is characterized in that the chemical general formula of the leadless piezoelectric textured ceramic is (90-x) NaNbO 3 -10Ba(Ti 0.7 Sn 0.3 )O 3 -xNaSbO 3 +2-6wt.％NaNbO 3 ，0≤x≤2.0。
2. A method for preparing the sodium niobate-based leadless piezoelectric textured ceramic according to claim 1, comprising the steps of:
(1) Solid phase synthesis: sodium carbonate, barium carbonate, niobium pentoxide, titanium dioxide, tin oxide and antimonous oxide are selected, weighing is carried out according to chemical composition, ball milling and calcination are carried out, and then ball milling is carried out again, so as to obtain a powder base material;
(2) Two-step molten salt method combined separation method: firstly, synthesizing, separating and filtering bismuth trioxide, sodium carbonate, niobium pentoxide and molten salt to obtain a flaky precursor Bi 2.5 Na 3.5 Nb 5 O 18 Secondly, synthesizing the sodium niobate sheet template by using a sheet precursor, potassium carbonate and molten salt, separating and filtering;
(3) Template grain growth method: respectively adding the powder base material obtained in the step (1) and the sheet-shaped template obtained in the step (2) into a mixed solvent and a dispersing agent for primary mixing, and then respectively adding a plasticizing agent and a binding agent for secondary mixing to obtain casting slurry;
(4) And (3) a casting process: casting the casting slurry obtained in the step (3), and then drying to form a dry thick film;
(5) And (3) hot pressing: stacking the dried thick films obtained in the step (4) layer by layer, and finally performing hot pressing to form a ceramic green body;
(6) And (3) a glue discharging process: discharging glue from the ceramic green body obtained in the step (5) to obtain a ceramic green body;
(7) The sintering process by a two-step method comprises the following steps: sintering the ceramic blank obtained in the step (6) by a two-step method, and naturally cooling to room temperature to obtain a ceramic sheet;
(8) Silver burning process: coating silver paste on the ceramic sheet obtained in the step (7) for silver burning to obtain ceramic coated with a silver electrode;
(9) And (3) polarization technology: and (3) polarizing the ceramic coated with the silver electrode obtained in the step (8) to obtain the sodium niobate-based leadless piezoelectric textured ceramic.
3. The method for preparing the sodium niobate-based leadless piezoelectric textured ceramic according to claim 2, wherein the ball milling time in the step (1) is 10-15 hours, the calcination temperature is 800-900 ℃ and the time is 3-8 hours.
4. The preparation method of the sodium niobate-based leadless piezoelectric textured ceramic is characterized in that sodium chloride is adopted in the molten salt in the step (2), the total mass ratio of raw materials to the molten salt is 1 (1.0-1.2), the heat preservation time is 2-4h, the mass ratio of bismuth trioxide, sodium carbonate to niobium pentoxide in the first step is 6.5-7.0, (1.7-2.1) and 5.0-5.5, the melting temperature is 1000-1100 ℃, the mass ratio of the flaky precursor to potassium carbonate in the second step is 1.75-2.00, and the melting temperature is 900-1000 ℃;
the separating agent adopts sodium tripolyphosphate, the stirring speed is 600-800rpm, the stirring time is 3-4h, the mass ratio of the first-step flaky precursor to the separating agent is (3-4): 1, and the mass ratio of the second-step flaky template to the separating agent is (2-3): 1.
5. The preparation method of the sodium niobate-based leadless piezoelectric textured ceramic is characterized in that in the step (3), 2-butanone or toluene is adopted as a mixed solvent, triolein is adopted as a dispersing agent, polyethylene glycol and dibutyl phthalate are adopted as a plasticizer, polyvinyl butyral is adopted as a binder, powder base material, a sheet template and the mass ratio of each reagent is (9.4-9.8), (9-11), (4-6), (0.32-0.37), (0.9-1.2), and the mixing and stirring speed is 15-17r/min for 3-4h.
6. The method for preparing a sodium niobate-based leadless piezoelectric textured ceramic according to claim 2, wherein the running speed of the casting doctor blade in the step (4) is 30-40cm/min.
7. The method for preparing the sodium niobate-based leadless piezoelectric textured ceramic according to claim 2, wherein the glue discharging temperature in the step (6) is 500-600 ℃, and the heat preservation time is 5-10h.
8. The method for preparing the sodium niobate-based leadless piezoelectric textured ceramic according to claim 2, wherein in the step (7), the temperature rising rate is 3-5 ℃/min in the first step, the temperature rising temperature is 1280-1320 ℃, the temperature lowering rate is 10-20 ℃/min in the second step, the temperature lowering temperature is 1180-1220 ℃, and the heat preservation time is 3-9h.
9. The method for preparing the sodium niobate-based leadless piezoelectric textured ceramic according to claim 2, wherein the silver paste in the step (8) has a diameter of 3-6mm, a silver firing temperature of 450-800 ℃ and a heat preservation time of 5-20min.
10. The method for preparing the sodium niobate-based leadless piezoelectric textured ceramic according to claim 2, wherein the polarizing electric field in the step (9) is 20-40kV/mm for 10-20min.
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