CN116768625A - Sodium lithium niobate based ceramic phase boundary regulation and control and performance optimization method - Google Patents
Sodium lithium niobate based ceramic phase boundary regulation and control and performance optimization method Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 48
- VVNXEADCOVSAER-UHFFFAOYSA-N lithium sodium Chemical compound [Li].[Na] VVNXEADCOVSAER-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000005457 optimization Methods 0.000 title claims abstract description 10
- 230000033228 biological regulation Effects 0.000 title claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 10
- 239000011734 sodium Substances 0.000 claims abstract description 6
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract 6
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract 6
- 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 claims abstract 4
- 229910002056 binary alloy Inorganic materials 0.000 claims abstract 3
- 230000001276 controlling effect Effects 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims 1
- 229910052783 alkali metal Inorganic materials 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 4
- 229910010293 ceramic material Inorganic materials 0.000 abstract 1
- 230000007704 transition Effects 0.000 abstract 1
- 238000000498 ball milling Methods 0.000 description 16
- 239000002994 raw material Substances 0.000 description 13
- 239000000843 powder Substances 0.000 description 8
- 239000011812 mixed powder Substances 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000008878 coupling Effects 0.000 description 4
- 238000010168 coupling process Methods 0.000 description 4
- 238000005859 coupling reaction Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 229920002545 silicone oil Polymers 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 229910013641 LiNbO 3 Inorganic materials 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 2
- 229910052808 lithium carbonate Inorganic materials 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000010897 surface acoustic wave method Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000026683 transduction Effects 0.000 description 1
- 238000010361 transduction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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Abstract
The application provides a phase boundary regulation and control and performance optimization method of sodium lithium niobate (LNN) based ceramic, wherein the ceramic material is composed of (1-x) Li with the chemical general formula shown in the specification α Na 1‑α NbO 3 ‑x BaTiO 3 Wherein alpha is more than or equal to 0.04 and less than or equal to 0.20, and x is more than or equal to 0 and less than or equal to 0.30. The method constructs a binary system for tetragonal Barium Titanate (BT) component at room temperature, successfully reduces the phase transition temperature of the orthorhombic phase and tetragonal phase to the vicinity of the room temperature in the doping component of 0.88LNN-0.12BT, and realizes the piezoelectric constant d 33 Is improved in piezoelectric constant d compared with the original component 33 The improvement is about 77 percent. Enhanced electro-strain is achieved in the LNN ceramic by means of excess Li element compensation, with an increase in the inverse piezoelectric constant of about 41% compared to the non-excess composition. The method provides a new way for modifying the piezoelectric ceramics.
Description
Technical Field
The application relates to the field of sodium lithium niobate based ceramics, in particular to a method for regulating and controlling phase boundaries and optimizing performance of sodium lithium niobate (LNN) based ceramics.
Background
The LNN (lithium sodium niobate) system consists of niobate at both ends, i.e. LiNbO 3 (LN) and NaNbO 3 Nitta et al reported for the first time (NN), 1968, that about 500 high Q in pure LNN m [30] . From the following componentsAt Q m Has been receiving the academic interest for a long time, and thus has a high Q m The LNN system of (c) has the potential to solve the problems faced by piezoelectric ceramics in high power applications. In addition, LNNs are high frequency filter applications due to their ideal frequency constant and reliable electromechanical performance. Historically, (Li, na) NbO 3 The potential use of (LNN) solid solutions in nonlinear photonics, electro-optic devices and Surface Acoustic Wave (SAW) devices has received decades of attention.
Since the displacement amount can be maximized at the resonance frequency, the piezoelectric transducer mainly operates in the resonance state. Operating at the resonant frequency allows the most efficient energy conversion, but at the same time generates a lot of heat. Due to Q m The ratio of the total stored mechanical energy to the energy loss over the resonance period is characterized and therefore becomes one of the most important parameters for evaluating the high power performance of piezoelectric ceramics. In order to obtain high output power with high accuracy, d should be considered at the same time 33 And k p This is particularly critical in the field of ultrasound transduction, such as high intensity focused ultrasound technology. For high power applications, a figure of merit (FOM) may be used to evaluate the potential of the piezoelectric material, defined as Q m And k p (or Q) m And d 33 ) Is a product of (a) and (b). For piezoelectric materials of different compositions, Q m And d 33 Shows obvious inhibition correlation. LNN ceramics, by virtue of their greater Q, compared to other systems m Is remarkable in lead-free piezoelectric ceramics.
Disclosure of Invention
Aiming at the defect of the existing material performance, the application aims to provide a method for regulating and controlling the phase boundary and optimizing the performance of sodium lithium niobate (LNN) based ceramic.
The required raw materials are mixed according to a certain proportion by a wet method, then a proper roasting system is adopted to obtain the required ceramic powder, and a sample blank is obtained through a dry pressing method and a cold isostatic pressing method. Further research on a proper sintering schedule is carried out to obtain a compact and uniform ceramic sample, and ferroelectric analysis is adopted to select proper polarization conditions.
In a second aspect of the application, the application proposes a method for optimizing said lithium sodium niobate-based ceramic, comprising the steps of:
1) The raw material of the application is analytically pure Li 2 CO 3 、Na 2 CO 3 、Nb 2 O 5 、BaCO 3 、TiO 2 The method comprises the steps of carrying out a first treatment on the surface of the The raw materials are represented by the chemical formula (1-x) Li α Na 1-α NbO 3 -x BaTiO 3 Weighing, mixing and ball milling the mixture ratio to obtain mixed powder;
2) Pre-sintering the mixed powder;
3) Performing secondary ball milling on the powder subjected to the pre-sintering so as to obtain powder subjected to secondary ball milling;
4) Cold press molding is carried out on the powder after the secondary ball milling to obtain a ceramic rough blank;
5) Sintering the ceramic rough blank to obtain a ceramic sample;
6) And carrying out polarization treatment on the ceramic sample to obtain the lithium sodium niobate-based ceramic.
The method for preparing lithium sodium niobate-based ceramics according to the embodiment of the application may also have the following additional technical features:
in the steps 1 and 3, the ball milling and the secondary ball milling are carried out in a ball milling tank by taking absolute ethyl alcohol as a medium, and the ball milling time is 8-24 hours.
In step 2, the presintering is carried out at a temperature of 900-1100 ℃ in an air atmosphere.
In step 5, the secondary sintering is performed at 1150-1300 ℃ in an oxygen atmosphere.
In step 6, the polarization treatment process includes: placing the ceramic sample in silicone oil at 60-120 ℃, and preserving heat and pressure for 15-60 min under the direct current field intensity of 3-6 kV/mm, thereby endowing the piezoelectric ceramic with macroscopic piezoelectric performance.
The application provides a performance optimization method of novel piezoelectric ceramics, which is characterized by respectively having high piezoelectric coefficient, high dielectric constant and high electromechanical coupling coefficient by regulating and controlling components and synthesis flow, and can flexibly regulate and control the performance. The results of the specific examples show that the application isThe prepared lithium sodium niobate based ceramic has a positive piezoelectric constant d of 60-110 pC/N at room temperature 33 An electromechanical coupling coefficient of 0.2 to 0.47 and a dielectric constant of 400 to 5000.
Drawings
The application will be described in further detail with reference to the drawings and the detailed description.
Fig. 1 is XRD patterns of examples 1 to 3.
Fig. 2 is a relationship of piezoelectric constants with compositions of examples 1 to 3.
FIG. 3 shows the dielectric constant of examples 2, 4 and 5 as a function of temperature.
Detailed Description
The following detailed description of embodiments of the application is, however, intended to be illustrative of the application and is not to be construed as limiting the application.
The application discloses a method for regulating and controlling phase boundaries and optimizing performance of lithium sodium niobate-based ceramics, which comprises the following steps:
the required raw materials were weighed according to the stoichiometric ratio of the above chemical formulas, and the raw materials used in this example were analytically pure Li2CO3, na2CO3, nb2O5, tiO2, baCO3.
Adding the prepared raw materials into a ball milling tank with absolute ethyl alcohol as a medium, wherein the mass ratio of zirconium dioxide grinding balls to the absolute ethyl alcohol to the raw materials is 2:1:1, the ball milling time is 8-24 hours, and drying the obtained slurry to obtain mixed powder.
The mixed powder is put into a covered crucible and then presintered in air at 900-1100 ℃ for 4h.
And (3) performing secondary ball milling on the presintered powder for 8-24 hours and drying the slurry.
Cold-pressing the powder after secondary ball milling at 50-200 MPa to form a wafer with the diameter of 10mm and the thickness of 1.2-1.5 mm.
Sintering the wafer in a capping crucible for 1-6 h at 1150-1300 ℃ in air atmosphere.
Silver electrodes are uniformly coated on two ends of the sintered ceramic sheet, the ceramic sheet is placed in silicone oil at 60-120 ℃, and then polarized for 15-60 min under the direct current field intensity of 3-6 kV/mm.
Example 1
Analytically pure Li2CO3, na2CO3, nb2O5, tiO2, baCO3 are weighed according to x=0, α=0.12, i.e. chemical formula li0.12na0.88nbo3.
Adding the prepared raw materials into a ball milling tank with absolute ethyl alcohol as a medium, wherein the mass ratio of zirconium dioxide grinding balls to the absolute ethyl alcohol to the raw materials is 2:1:1, the ball milling time is 24 hours, and drying the obtained slurry to obtain mixed powder.
The mixed powder is put into a covered crucible and then presintered in air at 900-1100 ℃ for 4h.
And (3) performing secondary ball milling on the presintered powder for 12 hours and drying the slurry.
And cold-pressing the powder subjected to secondary ball milling at 100MPa to form a wafer with the diameter of 10mm and the thickness of 1.4 mm.
The discs were sintered in a capped crucible at a temperature of 1210 ℃ and in an air atmosphere for 2h.
And uniformly coating silver electrodes on two ends of the sintered ceramic sheet, placing the ceramic sheet in silicone oil at 100 ℃, and polarizing the ceramic sheet for 30min under the direct current field intensity of 5kV/mm to obtain the lithium sodium niobate-based ceramic with the chemical formula of Li0.12Na0.88NbO3. After 24 hours of standing, the piezoelectric performance of the sample is tested by using a quasi-static piezoelectric coefficient tester, the electromechanical coupling coefficient of the sample is tested by using an impedance analyzer, and the electromechanical coupling coefficient of the obtained sample is 0.47.
Figure 1 gives the XRD pattern of example 1 from which it can be seen that the sample has a typical orthorhombic perovskite structure.
The piezoelectric constants of example 1 are shown in Table 1, and as can be seen from the graph, the piezoelectric constants of the samples at room temperature were 42pC/N.
Example 2
The required raw materials were weighed out according to x=0.1, α=0.12, i.e., chemical formula 0.9li0.12na0.88nbo3-0.1batio3, and lithium sodium niobate-based ceramics were prepared by the above-described preparation method.
Figure 1 gives the XRD pattern of example 2 from which it can be seen that the sample has a typical perovskite structure.
The piezoelectric constants of example 2 are shown in FIG. 2, and it can be seen from the graph that the piezoelectric constant of the sample at room temperature is 61pC/N.
The mesophilic spectrum of example 3 is given in figure 3, from which it can be seen that the dielectric constant of the sample at room temperature is 440.
Example 3
The required raw materials were weighed according to x=0.124, α=0.12, i.e. the chemical formula 0.876li0.12na0.88nbo3-0.124batio3, and lithium sodium niobate-based ceramics were prepared according to the steps of the above preparation method.
Figure 1 gives the XRD pattern of example 3 from which it can be seen that the sample has a typical perovskite structure.
The piezoelectric constants of example 3 are shown in FIG. 2, and it can be seen from the graph that the piezoelectric constant of the sample at room temperature is 110pC/N.
Example 4
The required raw materials were weighed according to x=0.2, α=0.12, i.e., chemical formula 0.8li0.12na0.88nbo3-0.2batio3, and lithium sodium niobate-based ceramics were prepared according to the steps of the above-described preparation method.
FIG. 3 shows the mesophilic spectrum of example 3, from which it can be seen that the dielectric constant of the sample at room temperature is 1740.
Example 5
The required raw materials were weighed out according to x=0.3, α=0.12, i.e., chemical formula 0.7li0.12na0.88nbo3-0.3batio3, and lithium sodium niobate-based ceramics were prepared according to the steps of the above-described preparation method.
The mesophilic spectrum of example 3 is given in figure 3, from which it can be seen that the dielectric constant of the sample at room temperature is 3500.
Claims (6)
1. A method for regulating and controlling phase boundary and optimizing performance of lithium sodium niobate (LNN) based ceramic is characterized by comprising the following steps:
is composed of (1-x) Li represented by the following chemical formula α Na 1-α NbO 3 -x BaTiO 3 Wherein alpha represents the atomic percentage of lithium element in the sodium lithium niobate component, alpha is more than or equal to 0.04 and less than or equal to 0.20, x represents BaTiO 3 The atomic percentage of the lithium sodium niobate based ceramic is more than or equal to 0 and less than or equal to 0.30;
the component is Li 0.12 Na 0.88 NbO 3 As a performance optimization carrier;
for LNN-based piezoelectric ceramics with orthogonal phases at room temperature, a binary system is constructed by selecting Barium Titanate (BT) components with tetragonal phases at room temperature;
the influence of volatilization of alkali metal elements in the LNN piezoelectric ceramic on performance in the preparation process is improved in a mode of compensating excessive Li elements.
2. The LNN ceramic phase boundary control and performance optimization method of claim 1, wherein the LNN piezoelectric ceramic is a dense LNN ceramic with a relative density of over 98%.
3. The method for phase boundary control and performance optimization of LNN ceramic according to claim 1, wherein the ceramic selection component is Li 0.12 Na 0.88 NbO 3 As a performance optimizing carrier.
4. The method for phase boundary control and performance optimization of LNN ceramic according to claim 1, wherein Barium Titanate (BT) component of tetragonal phase at room temperature is selected to construct a binary system.
5. The method for phase boundary control and performance optimization of LNN ceramics according to any one of claims 1 to 4, characterized by the way of compensation of excess Li element.
6. An optimization method comprising the lithium sodium niobate (LNN) -based ceramic phase boundary regulation of any one of claims 1 to 5.
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