CN114478007A - Sodium niobate-based ceramic material with good process tolerance, high piezoelectric property and high dielectric property, and preparation method and application thereof - Google Patents
Sodium niobate-based ceramic material with good process tolerance, high piezoelectric property and high dielectric property, and preparation method and application thereof Download PDFInfo
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- UYLYBEXRJGPQSH-UHFFFAOYSA-N sodium;oxido(dioxo)niobium Chemical compound [Na+].[O-][Nb](=O)=O UYLYBEXRJGPQSH-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 48
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000919 ceramic Substances 0.000 claims abstract description 87
- 238000000498 ball milling Methods 0.000 claims abstract description 29
- 238000005245 sintering Methods 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 20
- 239000010936 titanium Substances 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 11
- 239000011734 sodium Substances 0.000 claims abstract description 10
- 239000010955 niobium Substances 0.000 claims abstract description 8
- 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 claims abstract description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 6
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052788 barium Inorganic materials 0.000 claims abstract description 6
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 6
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 6
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 6
- 239000011230 binding agent Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 44
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 35
- 238000007599 discharging Methods 0.000 claims description 13
- 239000003292 glue Substances 0.000 claims description 10
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Inorganic materials [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 8
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000000748 compression moulding Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- 238000010438 heat treatment Methods 0.000 description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 11
- 239000000203 mixture Substances 0.000 description 11
- 238000004321 preservation Methods 0.000 description 9
- 239000002994 raw material Substances 0.000 description 9
- 238000012360 testing method Methods 0.000 description 6
- 238000003825 pressing Methods 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000001757 thermogravimetry curve 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
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000003921 oil 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
- 239000002245 particle Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research 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
- 238000001228 spectrum Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention relates to a sodium niobate-based ceramic material with good process tolerance, high piezoelectric property and high dielectric property, a preparation method and application thereof, wherein the general chemical formula of the sodium niobate-based ceramic material is (0.90-x) NaNbO3‑0.10Ba(Ti0.7Sn0.3)O3‑xNaSbO3Wherein x is more than or equal to 0.01 and less than or equal to 0.02; the preparation method comprises the following steps: mixing a sodium source, a niobium source, an antimony source, a barium source, a titanium source and a tin source, and then sequentially carrying out primary ball milling, calcining, secondary ball milling, drying, granulating, press forming, binder removal and sintering to obtain the sodium niobate-based ceramic material. Compared with the prior art, the novel sodium niobate-based ceramic prepared by the invention has excellent piezoelectric property, the piezoelectric coefficient can reach 361pC/N, and the dielectric constant is4500, so that the material has good application prospect in electroacoustic devices and medical ultrasonic devices; meanwhile, the invention can prepare the novel sodium niobate-based ceramic with high piezoelectric property and high dielectric constant in a wider sintering temperature zone, and has good process tolerance.
Description
Technical Field
The invention belongs to the technical field of electronic functional materials, and relates to a sodium niobate-based ceramic with high process tolerance, high piezoelectric property and high dielectric property, and a preparation method and application thereof.
Background
Among various types of ferroelectric materials, lead-containing piezoelectric ceramics (PZT) becomes a support for piezoelectric materials due to its excellent piezoelectric properties and temperature stability. Among them, in the late 80 s, relaxor ferroelectric ceramics have been developed as a basic material for a series of electro-acoustic devices and piezoelectric devices, such as lead magnesium niobate (Pb (Mg)1/3Nb2/3)(ZrTi)O3) It can be widely used in sound pick-up and microphone. However, lead is highly toxic and has been listed as the first place on the hazard list. In addition, in the preparation process, PbO is used in a large amount, and the content of PbO exceeds 60%, which causes great harm to human bodies and the environment. Therefore, in many countries and regions, restrictions are being drawn or restrictions have been made or the use of harmful substances has been stopped for the purpose of protecting the environment and humans. The potassium-sodium niobate (KNN) based ceramic in the alkali metal niobate is a lead-free ferroelectric ceramic with good dielectric, piezoelectric and ferroelectric ceramic properties, and is a material which is most expected to replace lead-based piezoelectric ceramic. But leads to complexity of the sintering process due to the hygroscopicity of potassium carbonate and the volatility of potassium oxide at high temperatures. Even in some KNN systems the sintering temperature range is only 5 ℃. This makes industrialization of KNN-based piezoelectric ceramics very difficult. Potassium-free NN-based piezoelectric ceramics having good process tolerance are widely regarded.
The NN-based piezoelectric ceramic has good dielectric, piezoelectric and ferroelectric ceramic properties, and higher piezoelectric properties can be obtained in the NN-based piezoelectric ceramic by introducing different elements. In the patent of Qiman et al (CN 201810749844: a sodium niobate based leadless potassium-free high-power piezoelectric ceramic and a preparation method thereof), NN-based piezoelectric ceramic with higher voltage and high mechanical quality factor is prepared, the piezoelectric activity of 150pC/N is obtained at most, and the dielectric constant is 388. Although a great number of researchers have made continuous innovation in the field of NN-based piezoelectric ceramics, it is difficult to achieve a satisfactory performance, generally, piezoelectric performance (< 300pC/N) and dielectric performance (< 3000) are not ideal. The research adopts a solid-phase sintering method to prepare lead-free (0.90-x) NaNbO3-0.10Ba(Ti0.7Sn0.3)O3-xNaSbO3The relaxation piezoelectric ceramic successfully endows the NN-based relaxation piezoelectric ceramic with high piezoelectric and high dielectric characteristics, and is beneficial to promoting the lead-free development of electroacoustic devices and medical ultrasonic sensing devices.
Disclosure of Invention
The invention aims to provide a sodium niobate-based ceramic material with high process tolerance, high piezoelectric property and high dielectric property, and a preparation method and application thereof.
The purpose of the invention can be realized by the following technical scheme:
a sodium niobate-based ceramic material with high piezoelectric and dielectric properties and good process tolerance, the chemical general formula of which is (0.90-x) NaNbO3-0.10Ba(Ti0.7Sn0.3)O3-xNaSbO3Wherein x is more than or equal to 0.01 and less than or equal to 0.02.
A method for preparing a sodium niobate-based ceramic material with good process tolerance, high piezoelectric property and high dielectric property comprises the following steps: mixing a sodium source, a niobium source, an antimony source, a barium source, a titanium source and a tin source, and then sequentially carrying out primary ball milling, calcining, secondary ball milling, drying, granulating, press forming, binder removal and sintering to obtain the sodium niobate-based ceramic material.
Further, the sodium source comprises Na2CO3Said niobium source comprising Nb2O5The antimony source comprises Sb2O3Said barium source comprises BaCO3The titanium source comprises TiO2Said tin source comprises SnO2。
Further, in the primary ball milling process, the ball milling time is 12-15 h; in the secondary ball milling process, the ball milling time is 12-15 h.
Furthermore, in the calcining process, the heating rate is 3-5 ℃/min, the calcining temperature is 800-.
Further, in the granulation process, the binder is 5-8 wt.% of polyvinyl alcohol solution; in the process of compression molding, the molding pressure is 150-200 MPa.
Further, in the glue discharging process, the glue discharging temperature is 600-800 ℃, and the glue discharging time is 8-12 h.
Furthermore, in the sintering process, the sintering temperature is 1100-1300 ℃, and the sintering time is 4-8 h.
Further, after secondary ball milling and drying, dividing the obtained dried powder into two parts according to the mass ratio (0.8-1.2) of 1, and granulating, press-forming and removing glue to obtain a ceramic blank;
during sintering, the ceramic blank is placed on the zirconia ceramic plate, the second part of dried powder is covered, the crucible is covered, and ZrO is utilized2Filling the gap between the crucible and the zirconia ceramic plate with powder;
wherein, the ZrO2The powder is ZrO obtained after calcining at 1450 ℃ for 3h2The amount of the powder is 1.8-2.2 times of the mass of the ceramic body.
As a preferred technical scheme, a drying process is also included between the primary ball milling process and the calcining process, and the drying temperature is 120 ℃ in both the drying process and the drying process.
The application of the sodium niobate-based ceramic material with high piezoelectric and dielectric properties and good process tolerance comprises applying the sodium niobate-based ceramic material to at least one of a sensor, a transducer, an electroacoustic device or a medical ultrasonic device.
Compared with the prior art, the invention has the following characteristics:
1) the novel sodium niobate-based ceramic prepared by the invention has excellent piezoelectric property, the piezoelectric coefficient can reach 361pC/N, and the dielectric constant can reach 4500, so that the novel sodium niobate-based ceramic has good application prospect in the aspects of electroacoustic devices and medical ultrasonic devices; meanwhile, the novel sodium niobate-based ceramic with high piezoelectric property and high dielectric constant can be prepared in a wider sintering temperature zone, and has good process tolerance;
2) the preparation method is simple, economical and practical, the material is lead-free, and the environment is not polluted in the preparation, application and waste processes, so that the piezoelectric material is an environment-friendly piezoelectric material.
Drawings
FIG. 1 is a dielectric thermogram of the novel sodium niobate-based piezoelectric ceramic prepared in example 1, example 2 and example 3 after polarization;
fig. 2 is an XRD spectrum of the novel sodium niobate-based piezoelectric ceramic material prepared in example 1, example 2 and example 3;
fig. 3 is an SEM image of the novel sodium niobate-based piezoelectric ceramic material prepared in example 1, example 2, and example 3;
FIG. 4 is a hysteresis loop of the novel sodium niobate-based piezoelectric ceramic prepared in example 1 at room temperature;
FIG. 5 is a hysteresis loop of the novel sodium niobate-based piezoelectric ceramic prepared in example 2 at room temperature;
FIG. 6 is a hysteresis loop of the novel sodium niobate-based piezoelectric ceramic prepared in example 3 at room temperature;
FIG. 7 shows the results of the piezoelectric property test and dielectric constant at room temperature of the novel sodium niobate-based piezoelectric ceramics prepared in examples 1, 2 and 3,
fig. 8 shows the results of the piezoelectric performance test at room temperature for the novel sodium niobate-based piezoelectric ceramics prepared at different sintering temperatures in example 2.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
A sodium niobate-based ceramic material with high piezoelectric and dielectric properties and good process tolerance, the chemical general formula of which is (0.90-x) NaNbO3-0.10Ba(Ti0.7Sn0.3)O3-xNaSbO3Wherein x is more than or equal to 0.01 and less than or equal to 0.02.
The preparation method of the sodium niobate-based ceramic material comprises the following steps:
1) a sodium source (preferably Na)2CO3) Niobium source (preferably Nb)2O5) Antimony source (preferably Sb)2O3) Barium source (preferably BaCO)3) A titanium source (preferably TiO)2) A tin source (preferably SnO)2) Mixing to obtain a mixed raw material;
2) adding ethanol into the mixed raw materials, adding the mixture into a ball mill for primary ball milling for 12-15h, and drying after discharging to obtain dried powder;
3) putting the dried powder into an alumina crucible, transferring the alumina crucible into a muffle furnace, heating to 800-;
4) adding ethanol into the calcined powder, adding the calcined powder into a ball mill for secondary ball milling for 12-15h, discharging, drying, mixing the calcined powder with 5-8 wt.% of polyvinyl alcohol aqueous solution, granulating, and pressing under the pressure of 150-;
5) placing the ceramic wafer in a muffle furnace, and removing the glue for 8-12h at the temperature of 600-800 ℃; and then sintering at 1100-1300 ℃ for 4-8h to obtain the sodium niobate-based ceramic material.
As a preferred technical solution, it is proposed that,
after secondary ball milling and drying, dividing the obtained dried powder into two parts according to the mass ratio (0.8-1.2) of 1, and granulating, press-forming and removing glue to obtain a ceramic blank;
during sintering, the ceramic blank is placed on the zirconia ceramic plate, the second part of dried powder is covered, the round crucible is covered, and ZrO is utilized2Filling the gap between the crucible and the zirconia ceramic plate with powder;
wherein, the ZrO2The powder is commercially available ZrO2ZrO from powders calcined at 1450 ℃ for 3h2The amount of the powder is 1.8-2.2 times of the mass of the ceramic body.
The application of the sodium niobate-based ceramic material with high piezoelectric and dielectric properties and good process tolerance comprises applying the sodium niobate-based ceramic material to at least one of a sensor, a transducer, an electroacoustic device or a medical ultrasonic device.
The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
Example 1:
a leadless piezoelectric ceramic with chemical composition of 0.89NaNbO3-0.10Ba(Ti0.7Sn0.3)O3-0.01NaSbO3The preparation method comprises the following steps:
1) selecting Na with purity of more than 99%2CO3、Nb2O5、Sb2O3、BaCO3、TiO2、SnO2As a raw material for ceramic materials;
2) weighing the raw materials according to the chemical composition proportion by taking 0.1mol of lead-free piezoelectric ceramic as a target product, adding 2 times of ethanol as a ball milling medium for ball milling for 12 hours, then discharging, and placing in a 120 ℃ oven for drying;
3) putting the dried powder into an alumina crucible, then putting the alumina crucible into a muffle furnace, heating the alumina crucible to 900 ℃ at a heating rate of 5 ℃/min, and carrying out heat preservation and calcination for 5 hours to obtain calcined powder;
4) adding ethanol with the weight 2 times that of the calcined powder as a medium, carrying out secondary ball milling for 15 hours, discharging, placing in a 120 ℃ oven for drying, equally dividing the obtained powder into two parts by mass, adding 8 wt% of polyvinyl alcohol aqueous solution into one part of the powder for granulation, and pressing under the pressure of 150MPa to prepare a ceramic wafer;
5) placing the ceramic wafer in a muffle furnace, heating to 600 ℃ at the heating rate of 1 ℃/min, and carrying out heat preservation and glue removal for 10 hours to obtain a ceramic blank;
6) placing the ceramic blank on a zirconia ceramic plate, covering the zirconia ceramic plate with the second part of dried powder, covering a round crucible, and utilizing the calcined ZrO2Filling the gap between the crucible and the zirconia ceramic plate with powder, wherein the using amount of the powder is about 2 times of the mass of the ceramic body; then placing the mixture into a muffle furnace to heat to 1230 ℃ at the heating rate of 3 ℃/min, carrying out heat preservation sintering for 6h, and naturally cooling to room temperature to obtain the sodium niobate-based ceramic material.
Example 2:
a leadless piezoelectric ceramic with chemical composition of 0.885NaNbO3-0.10Ba(Ti0.7Sn0.3)O3-0.015NaSbO3The preparation method comprises the following steps:
1) selecting Na with purity of more than 99%2CO3、Nb2O5、Sb2O3、BaCO3、TiO2、SnO2As a raw material for ceramic materials;
2) taking 0.1mol of lead-free piezoelectric ceramic as a target product, weighing the raw materials according to the chemical composition ratio, adding 2 times of ethanol as a ball milling medium by weight of the raw materials, performing ball milling for 12 hours, discharging, and placing in an oven at 120 ℃ for drying;
3) putting the dried powder into an alumina crucible, then putting the alumina crucible into a muffle furnace, heating the alumina crucible to 900 ℃ at a heating rate of 5 ℃/min, and carrying out heat preservation and calcination for 5 hours to obtain calcined powder;
4) adding ethanol with the weight 2 times that of the calcined powder as a medium, carrying out secondary ball milling for 15 hours, discharging, placing in a 120 ℃ oven for drying, equally dividing the obtained powder into two parts by mass, adding 8 wt% of polyvinyl alcohol aqueous solution into one part of the powder for granulation, and pressing under the pressure of 150MPa to prepare a ceramic wafer;
5) placing the ceramic wafer in a muffle furnace, heating to 600 ℃ at the heating rate of 1 ℃/min, and carrying out heat preservation and glue removal for 10 hours to obtain a ceramic blank;
6) preparing a plurality of ceramic blanks by adopting the method of the same steps 1) -5), and preparing a second drying powder with the same mass; placing the ceramic blank on a zirconia ceramic plate, respectively covering with corresponding second drying powder, covering with a round crucible, and using the calcined ZrO2Filling the gap between the crucible and the zirconia ceramic plate with powder; then the mixture is put into a muffle furnace to be respectively heated to 1140 ℃, 1170 ℃, 1190 ℃, 1210 ℃, 1230 ℃, 1250 ℃, 1270 ℃ and 1290 ℃ at the heating rate of 3 ℃/min, and is sintered for 6 hours under the condition of heat preservation, and the mixture is naturally cooled to the room temperature to obtain the sodium niobate-based ceramic material.
Example 3:
a leadless piezoelectric ceramic with chemical composition of 0.88NaNbO3-0.10Ba(Ti0.7Sn0.3)O3-0.02NaSbO3The preparation method comprises the following steps:
1) selecting Na with purity of more than 99%2CO3、Nb2O5、Sb2O3、BaCO3、TiO2、SnO2As a raw material for ceramic materials;
2) weighing the raw materials according to the chemical composition proportion by taking 0.1mol of lead-free piezoelectric ceramic as a target product, adding 2 times of ethanol as a ball milling medium for ball milling for 12 hours, then discharging, and placing in a 120 ℃ oven for drying;
3) putting the dried powder into an alumina crucible, then putting the alumina crucible into a muffle furnace, heating the alumina crucible to 900 ℃ at a heating rate of 5 ℃/min, and carrying out heat preservation and calcination for 5 hours to obtain calcined powder;
4) adding ethanol with the weight 2 times that of the calcined powder as a medium, carrying out secondary ball milling for 15 hours, discharging, placing in a 120 ℃ oven for drying, equally dividing the obtained powder into two parts by mass, adding 8 wt% of polyvinyl alcohol aqueous solution into one part of the powder for granulation, and pressing under the pressure of 150MPa to prepare a ceramic wafer;
5) placing the ceramic wafer in a muffle furnace, heating to 600 ℃ at the heating rate of 1 ℃/min, and carrying out heat preservation and glue removal for 10 hours to obtain a ceramic blank;
6) placing the ceramic blank on a zirconia ceramic plate, covering the zirconia ceramic plate with the second part of dried powder, covering a round crucible, and utilizing the calcined ZrO2Filling the gap between the crucible and the zirconia ceramic plate with powder; then placing the mixture into a muffle furnace to heat to 1230 ℃ at the heating rate of 3 ℃/min, carrying out heat preservation sintering for 6h, and naturally cooling to room temperature to obtain the sodium niobate-based ceramic material.
Example 4:
in this example, the electrical properties of the sodium niobate-based ceramic material prepared in examples 1 to 3 were measured, and the electrical properties thereof were measured as follows:
s1: grinding and polishing the sodium niobate-based ceramic material sheet to 0.4-0.5mm by using abrasive paper with different particle sizes;
s2: coating silver paste on the double surfaces of the polished sodium niobate-based ceramic material sheet, then preserving the heat in a muffle furnace at 560 ℃ for 10min, and then naturally cooling to room temperature to obtain lead-free piezoelectric ceramic coated with silver electrodes of 10-30 mu m;
s3: polarizing the lead-free piezoelectric ceramic coated with the silver electrode for 15min in a silicon oil bath at 50 ℃ under an electric field of 3.0 kV/mm;
s4: testing the piezoelectric property of the polarized ceramic by using a static piezoelectric coefficient tester of Chinese academy of sciences; testing the dielectric properties of the polarized ceramic and the unpolarized ceramic by using an LCR tester; and testing the ferroelectric property of the ceramic by adopting a ferroelectric analyzer.
The test results were as follows:
FIG. 1 shows the dielectric thermograms of the novel sodium niobate-based piezoelectric ceramics prepared in example 1, example 2 and example 3 after polarization; as can be seen from the graph, the curie temperature of the polarizing electrode corresponding to the sodium niobate-based piezoelectric ceramic prepared in example 1 was about 115 ℃, the curie temperature of the polarizing electrode corresponding to the sodium niobate-based piezoelectric ceramic prepared in example 2 was about 100 ℃, and the curie temperature of the polarizing electrode corresponding to the sodium niobate-based piezoelectric ceramic prepared in example 3 was about 85 ℃.
As shown in fig. 2, XRD spectra of the novel sodium niobate-based piezoelectric ceramic materials prepared in example 1, example 2 and example 3; as can be seen from the figure, the sodium niobate-based piezoelectric ceramic materials prepared in example 1, example 2 and example 3 all have a pure perovskite structure, and have coexistent orthorhombic, tetragonal and pseudocubic phases, and no other impurity phase.
As shown in fig. 3, SEM images of the novel sodium niobate-based piezoelectric ceramic materials prepared in example 1, example 2, and example 3; as can be seen from the figure, the sodium niobate-based piezoelectric ceramic materials prepared in examples 1, 2 and 3 all exhibited the characteristics of good crystal grain crystallinity, dense structure, large crystal grains (about 3 μm) and uniform distribution.
Fig. 4 to 6 show the hysteresis loops of the novel sodium niobate-based piezoelectric ceramic materials prepared in examples 1, 2 and 3 at room temperature, respectively, and fig. 7 shows the piezoelectric property test and the dielectric constant results of the novel sodium niobate-based piezoelectric ceramic materials prepared in examples 1, 2 and 3 at room temperature, and it can be seen from the graphs that the sample prepared in example 1 has good ferroelectric and piezoelectric properties, the piezoelectric coefficient can reach 305pC/N, and the dielectric constant is 3500; the sample prepared in the embodiment 2 has good ferroelectric and piezoelectric properties, the piezoelectric coefficient can reach 361pC/N, and the dielectric constant is 4500; the sample prepared in the embodiment 3 has good ferroelectric and piezoelectric properties, the piezoelectric coefficient can reach 301pC/N, and the dielectric constant is 5000.
As shown in FIG. 8, the piezoelectric performance test results of the novel sodium niobate-based piezoelectric ceramic prepared at different sintering temperatures in example 2 are shown, and it can be seen from the figure that the piezoelectric coefficient can reach over 300pC/N at the sintering temperature of 1210-1270 ℃, and the piezoelectric ceramic has good process tolerance.
The sodium niobate-based ceramic with high piezoelectric coefficient (361 pC/N) and high dielectric constant (4500) is obtained by the traditional electronic ceramic preparation process, and more importantly, the sintering temperature zone of the system is wider (1210-.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, 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 embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. The sodium niobate-based ceramic material with high piezoelectric and high dielectric properties and good process tolerance is characterized in that the chemical general formula of the sodium niobate-based ceramic material is (0.90-x) NaNbO3-0.10Ba(Ti0.7Sn0.3)O3-xNaSbO3Wherein x is more than or equal to 0.01 and less than or equal to 0.02.
2. The method for preparing the sodium niobate-based ceramic material with high voltage and high dielectric property with good process tolerance as claimed in claim 1, wherein the method comprises
Mixing a sodium source, a niobium source, an antimony source, a barium source, a titanium source and a tin source, and then sequentially carrying out primary ball milling, calcining, secondary ball milling, drying, granulating, press forming, binder removal and sintering to obtain the sodium niobate-based ceramic material.
3. High voltage and high voltage tolerance with good process tolerance according to claim 2The preparation method of the sodium niobate-based ceramic material with dielectric property is characterized in that the sodium source comprises Na2CO3Said niobium source comprising Nb2O5Said antimony source comprising Sb2O3Said barium source comprises BaCO3The titanium source comprises TiO2Said tin source comprises SnO2。
4. The preparation method of the sodium niobate-based ceramic material with good process tolerance, high piezoelectricity and high dielectric property as claimed in claim 2, wherein in the primary ball milling process, the ball milling time is 12-15 h; in the secondary ball milling process, the ball milling time is 12-15 h.
5. The method for preparing the sodium niobate-based ceramic material with high voltage and high dielectric property and good process tolerance as claimed in claim 2, wherein the temperature rise rate is 3-5 ℃/min, the calcination temperature is 800-.
6. The method for preparing the sodium niobate-based ceramic material with good process tolerance, high voltage and high dielectric property according to claim 2, wherein in the granulation process, the binder is 5-8 wt.% of polyvinyl alcohol aqueous solution; in the process of compression molding, the molding pressure is 150-200 MPa.
7. The method for preparing the sodium niobate-based ceramic material with high piezoelectric and dielectric properties and good process tolerance as claimed in claim 2, wherein the gel discharging temperature is 600-800 ℃ and the gel discharging time is 8-12 h.
8. The method as claimed in claim 2, wherein the sintering temperature is 1100-1300 ℃ and the sintering time is 4-8 h.
9. The preparation method of the sodium niobate-based ceramic material with good process tolerance, high voltage and high dielectric property according to claim 2, wherein after secondary ball milling and drying, the obtained dried powder is divided into two parts according to the mass ratio (0.8-1.2) of 1, and the first part is granulated, pressed and molded and subjected to glue discharge to obtain a ceramic blank;
during sintering, the ceramic blank is placed on the zirconia ceramic plate, the second part of dried powder is covered on the ceramic blank, the crucible is covered, and ZrO is utilized2Filling the gap between the crucible and the zirconia ceramic plate with powder;
wherein, the ZrO2The powder is ZrO obtained after calcining at 1450 ℃ for 3h2The amount of the powder is 1.8-2.2 times of the mass of the ceramic body.
10. The use of the sodium niobate-based ceramic material with high piezoelectric and dielectric properties and good process tolerance according to claim 1, wherein the sodium niobate-based ceramic material is used in a sensor, a transducer, an electroacoustic device or a medical ultrasonic device.
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