CN114956815A - Preparation method of novel high-strain high-Curie-temperature potassium-sodium niobate-based ferroelectric ceramic - Google Patents
Preparation method of novel high-strain high-Curie-temperature potassium-sodium niobate-based ferroelectric ceramic Download PDFInfo
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Abstract
The invention relates to the field of potassium-sodium niobate-based ferroelectric ceramics. Discloses the development of a novel high-strain high-Curie temperature potassium sodium niobate-based ferroelectric ceramic. The ceramic has an orthorhombic-tetragonal (O-T) two-phase coexisting crystal structure having a chemical composition of 0.97 (K) 0.48 Na 0.52 )La 0.0075 (Zr 0.0025 Nb 0.9975 )O 3 ‑0.03SrTiO 3 . The potassium-sodium niobate-based ferroelectric ceramic prepared by the invention has good strain performance, the strain reaches 0.22% under an external electric field of 40kV/cm, the Curie temperature is 280 ℃, the preparation is simple, and the cost is low.
Description
Technical Field
The invention relates to the technical field of development of novel high-strain high-Curie-temperature potassium-sodium niobate-based ferroelectric ceramics, in particular to a preparation method of novel high-strain high-Curie-temperature potassium-sodium niobate-based ferroelectric ceramics.
Background
The potassium-sodium niobate based lead-free ferroelectric ceramic becomes one of ferroelectric ceramic systems which have been discussed and researched in recent years, and the traditional ceramic process has difficulty in obtaining a ceramic body with good compactness. Therefore, researchers often use doping modification to adjust the structure to optimize its ferroelectric properties. Potassium sodium niobate (K) 0.5 Na 1-x NbO 3 ) The high strain values of the base ceramics have attracted considerable research attention. Strain is a key property of ferroelectric ceramics in sensor and actuator applications. At present, K 0.5 Na 1-x NbO 3 The polarizable switches on the (KNN) -based ferroelectric ceramic produce a higher strain response at polymorphic phase transition boundaries (abbreviated as PPBs) near room temperature, such as rhombohedral-tetragonal (R-T) and orthorhombic-tetragonal (O-T) phase boundaries. By adding dopants, the rhombohedral-orthonormal phase transition temperature (T) R-O ) Or orthonormal tetragonal transition temperature (T) O-T Moving to room temperature, a KNN-based ferroelectric ceramic having a different phase boundary is obtained.
At present, the KNN-based ferroelectric ceramic mainly improves strain by doping to construct multiphase coexistence, change crystal grains, change the size of domains, enable domain walls to be easy to turn, improve the density of the ceramic and the like. The structure of the phase boundary can effectively improve the electrical property of the ferroelectric ceramic. In addition, a phase boundary is constructed to reduce polarization anisotropy energy, so that polarization steering is facilitated to improve the strain performance of the polarization steering.
The piezoelectric property of the lead-based PZT material can be greatly improved by adjusting the ratio of Zr to Ti, and when the Zr content is 52%, the PZT is in a three-square ferroelectric phase coexisting state. Thus, a regulatory component of 0.97 (K) according to the invention 0.48 Na 0.52 )La 0.0075 (Zr x Nb 1-x )O 3 -0.03SrTiO 3 The B site of the ceramic, when x is 0.0025, the ceramic has an O-T phase boundary, producing a high strain of 0.21% at 40kV/cm electric field.
In the prior art, when the KNN ferroelectric ceramic has two phases of O-T coexisting, the strain S% reaches 0.1-0.2% under 40kV/cm, the Curie temperature is about 250 ℃, and the strain performance is determined to be only when the ceramic is used at the temperature lower than 250 ℃.
Disclosure of Invention
The invention aims to provide a preparation method of a novel high-strain high-Curie-temperature potassium-sodium niobate-based ferroelectric ceramic, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of novel high-strain high-Curie temperature potassium sodium niobate-based ferroelectric ceramic comprises the following steps:
step one, pretreating raw materials;
step two, mixing the raw materials;
step three, drying the raw materials;
step four, sieving the mixture;
step five, calcining the mixture;
step six, ball milling of the calcined material;
seventhly, discharging glue;
step eight, sintering;
step nine, polishing;
step ten, silver burning;
step eleven, cooling;
step twelve, the preparative chemical formula is 0.97 (K) 0.48 Na 0.52 )La 0.0075 (Zr x Nb 1-x )O 3 -0.03SrTiO 3 A ferroelectric ceramic;
step thirteen, for 0.97 (K) 0.48 Na 0.52 )La 0.0075 (Zr x Nb 1-x )O 3 -0.03SrTiO 3 And testing the ferroelectric ceramic structure and performance.
Preferably, the ceramic has a chemical composition of 0.97 (K) 0.48 Na 0.52 )La 0.0075 (Zr 0.0025 Nb 0.9975 )O 3 -0.03SrTiO 3 。
Preferably, the ceramic chemical group is characterized by adding ZrO 2 、La 2 O 3 、SrTiO 3 The three materials are matched together to construct an orthogonal-tetragonal two-phase coexisting structure, namely an (O-T) phase boundary.
Preferably, the firing of silver results in a ceramic with a strain of 0.22% at an external electric field E of 40kV/cm and a Curie temperature of up to 280 ℃.
Preferably, step thirteen, when x is 0.0025, gives the ceramic phase: XRD tests show that the ceramic has an O-T two-phase coexisting structure and the Curie temperature is 280 ℃; microscopic morphology: the average grain size is 0.34 μm by microscopic morphology SEM test; the density was measured to be 4.28g/cm using a densitometer 3 (ii) a Ferroelectricity: maximum polarization P max 17.08 mu C/cm 2 (ii) a Strain performance: when E ═ 40kV/cm, the strain S% reached 0.22%.
Compared with the prior art, the invention has the beneficial effects that:
the invention has the technical characteristics that when the KNN-based ferroelectric ceramic has two O-T phases, the strain S% reaches 0.22% under 40kV/cm, and the general strain performance is higher than 0.1% so as to be used in equipment. The Curie temperature of the piezoelectric ceramic reaches up to 280 ℃, the piezoelectric ceramic has strain performance when used at the temperature lower than 280 ℃, and the potassium-sodium niobate-based piezoelectric ceramic prepared by the method has good strain performance, is simple to prepare and has low cost.
Drawings
FIG. 1 is FIG. 10.97 (K) of the present invention 0.48 Na 0.52 )La 0.0075 (Zr 0.0025 Nb 0.9975 )O 3 -0.03SrTiO 3 A microscopic topography of the ferroelectric ceramic, (a) SEM image; (b) a particle size distribution map;
FIG. 2 shows 0.97 (K) according to the invention 0.48 Na 0.52 )La 0.0075 (Zr 0.0025 Nb 0.9975 )O 3 -0.03SrTiO 3 XRD pattern of ferroelectric ceramic;
FIG. 3 shows 0.97 (K) according to the invention 0.48 Na 0.52 )La 0.0075 (Zr 0.0025 Nb 0.9975 )O 3 -0.03SrTiO 3 A dielectric temperature spectrum of the ferroelectric ceramic;
FIG. 4 shows 0.97 (K) according to the invention 0.48 Na 0.52 )La 0.0075 (Zr 0.0025 Nb 0.9975 )O 3 -0.03SrTiO 3 Testing of ferroelectric ceramics (a) P-E curves, (b) S-E curves
FIG. 5 is a process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "front", "rear", "both ends", "one end", "the other end", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "connected," and the like are to be construed broadly, and for example, "connected" may be a fixed connection, a detachable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Referring to fig. 1, fig. 2, fig. 3, fig. 4 and fig. 5, an embodiment of the present invention: a method for preparing novel high-strain high-Curie-temperature potassium-sodium niobate-based ferroelectric ceramics,
in a first embodiment, the preparation method comprises the following steps:
step one, pretreating raw materials;
step two, mixing the raw materials;
step three, drying the raw materials;
step four, sieving the mixture;
step five, calcining the mixture;
step six, ball milling of the calcined material;
seventhly, discharging glue;
step eight, sintering;
step nine, polishing;
step ten, silver burning;
step eleven, cooling;
step twelve, the preparative chemical formula is 0.97 (K) 0.48 Na 0.52 )La 0.0075 (Zr 0.0025 Nb 0.9975 )O 3 -0.03SrTiO 3 A ferroelectric ceramic;
step thirteen, for 0.97 (K) 0.48 Na 0.52 )La 0.0075 (Zr 0.0025 Nb 0.9975 )O 3 -0.03SrTiO 3 And testing the ferroelectric ceramic structure and performance.
The chemical composition of the ceramic is 0.97 (K) 0.48 Na 0.52 )La 0.0075 (Zr 0.0025 Nb 0.9975 )O 3 -0.03SrTiO 3
The ceramic chemical group is mainly characterized in that ZrO is added 2 、La 2 O 3 、SrTiO 3 The three materials are matched together to construct an orthogonal-tetragonal two-phase coexisting structure, namely an (O-T) phase boundary.
And (3) obtaining the ceramic after silver sintering, and densifying the ceramic through processing, wherein the strain is 0.21% under the external electric field E of 40kV/cm, and the Curie temperature is as high as 280 ℃.
Step thirteen, obtaining a ceramic phase: XRD tests show that the ceramic has an O-T two-phase coexisting structure and the Curie temperature is 280 ℃; microscopic morphology: the average grain size is 0.34 μm by microscopic morphology SEM test; the density was measured to be 4.28g/cm using a densitometer 3 (ii) a Ferroelectricity: maximum polarization P max 17.08 mu C/cm 2 (ii) a Strain performance: when E ═ 40kV/cm, the strain S% reached 0.21%.
In a second embodiment, the preparation method comprises the following steps:
step one, pretreating raw materials;
step two, mixing the raw materials;
step three, drying the raw materials;
step four, sieving the mixture;
step five, calcining the mixture;
step six, ball milling of the calcined material;
seventhly, discharging glue;
step eight, sintering;
step nine, polishing;
step ten, silver burning;
step eleven, cooling;
step twelve, the preparative chemical formula is 0.97 (K) 0.48 Na 0.52 )La 0.0075 (Zr 0.0025 Nb 0.9975 )O 3 -0.03SrTiO 3 A ferroelectric ceramic;
step thirteen, for 0.97 (K) 0.48 Na 0.52 )La 0.0075 (Zr 0.0025 Nb 0.9975 )O 3 -0.03SrTiO 3 And testing the ferroelectric ceramic structure and performance.
The chemical composition of the ceramic is 0.97 (K) 0.48 Na 0.52 )La 0.0075 (Zr 0.0025 Nb 0.9975 )O 3 -0.03SrTiO 3 。
The ceramic chemical group is mainly characterized in that ZrO is added 2 、La 2 O 3 、SrTiO 3 The three materials are matched together to construct an orthogonal-tetragonal two-phase coexisting structure, namely an (O-T) phase boundary.
And (3) obtaining the ceramic after silver sintering, and densifying the ceramic through processing, wherein the strain is 0.22% under the external electric field E of 40kV/cm, and the Curie temperature is as high as 280 ℃.
Step thirteen, when x is 0.0025, 0.97 (K) 0.48 Na 0.52 )La 0.0075 (Zr 0.0025 Nb 0.9975 )O 3 -0.03SrTiO 3 Ferroelectric ceramic structure and performance measurementAs an attempt is made to find out below,
ceramic phase: XRD test shows that the ceramic has coexisting O-T two-phase structure and Curie temperature of 280 deg.c.
Microscopic morphology: the average grain size is 0.34 μm by microscopic morphology SEM test.
The density was measured to be 4.28g/cm using a densitometer 3
Ferroelectricity: maximum polarization P max 17.08 mu C/cm 2
Strain performance: when E ═ 40kV/cm, the strain S% reached 0.21%.
In a third embodiment, the preparation method comprises the following steps:
crushing raw materials;
step two, mixing the raw materials;
step three, drying the raw materials;
step four, sieving the mixture;
step five, calcining the mixture;
step six, ball milling the calcined material;
seventhly, discharging glue;
step eight, sintering;
step nine, sintering;
step ten, polishing;
step eleven, silver burning;
the ferroelectric ceramic has a composition of 0.97 (K) 0.48 Na 0.52 )La 0.0075 (Zr 0.0025 Nb 0.9975 )O 3 -0.03SrTiO 3 The piezoelectric ceramic has high compactness, proper grain size and an orthogonal-tetragonal two-phase coexisting crystal structure, and the polarized dipoles in the piezoelectric ceramic of the structure are easy to rotate, so that the polarization is increased, and the strain performance of the piezoelectric ceramic under an external electric field is improved.
The following figures are specifically demonstrated.
FIG. 1 is a microstructure of a ceramic, and FIG. 1(a) shows that the crystal grain size distribution is tight, the pores are few, and the ceramic is very dense; the average particle size is 0.34 μm by counting the particle size as shown in FIG. 1 (b);
figure 2 is a schematic representation of an XRD test,FIG. 2 shows that the ceramic has a perovskite structure, and the diffraction angles 44-47 are shown in the upper right hand small diagram 0 On the enlarged scale, the peak heights (002) and (200) are close, indicating that the ceramic is orthorhombic-tetragonal two-phase coexisting;
further, the analysis of fig. 3 by the mesophilic spectrum shows that the ceramic is in the orthorhombic-tetragonal phase transition around the room temperature, which means that the ceramic has a crystal phase in which orthorhombic-tetragonal two phases coexist; having a Curie temperature T C About 280 ℃, is the tetragonal-cubic phase transition temperature;
FIG. 4(a) is a hysteresis loop (P-E curve) of a ceramic, showing that the ceramic has ferroelectricity, the magnitude of which is the maximum available polarization P max To represent P max Reaches 17.08 mu C/cm 2 (ii) a FIG. 4(b) is an electrostrictive loop (S-E curve) of the ceramic, showing that the ceramic has a strain S% equal to 0.22% at an electric field (E) of 40 kV/cm.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (5)
1. A preparation method of novel high-strain high-Curie temperature potassium sodium niobate-based ferroelectric ceramic is characterized by comprising the following steps:
step one, pretreating raw materials;
step two, mixing the raw materials;
step three, drying the raw materials;
step four, sieving the mixture;
step five, calcining the mixture;
step six, ball milling of the calcined material;
seventhly, discharging glue;
step eight, sintering;
step nine, polishing;
step ten, silver burning;
step eleven, cooling;
step twelve, the preparative chemical formula is 0.97 (K) 0.48 Na 0.52 )La 0.0075 (Zr 0.0025 Nb 0.9975 )O 3 -0.03SrTiO 3 A ferroelectric ceramic;
step thirteen, for 0.97 (K) 0.48 Na 0.52 )La 0.0075 (Zr 0.0025 Nb 0.9975 )O 3 -0.03SrTiO 3 And testing the ferroelectric ceramic structure and performance.
2. The preparation method of the novel high-strain high-curie-temperature potassium-sodium niobate-based ferroelectric ceramic according to claim 1, characterized in that: the chemical composition of the ceramic is 0.97 (K) 0.48 Na 0.52 )La 0.0075 (Zr 0.0025 Nb 0.9975 )O 3 -0.03SrTiO 3 。
3. The preparation method of the novel high-strain high-curie-temperature potassium-sodium niobate-based ferroelectric ceramic according to claim 1, characterized in that: the ceramic chemical group is mainly characterized in that ZrO is added 2 、La 2 O 3 、SrTiO 3 The three materials are matched together to construct an orthogonal-tetragonal two-phase coexisting structure, namely an (O-T) phase boundary.
4. The preparation method of the novel high-strain high-curie-temperature potassium-sodium niobate-based ferroelectric ceramic according to claim 1, characterized in that: the ceramic obtained after silver firing has a strain of 0.22% at an external electric field E of 40kV/cm and a Curie temperature of up to 280 ℃.
5. The preparation method of the novel high-strain high-curie-temperature potassium-sodium niobate-based ferroelectric ceramic according to claim 1, characterized in that: thirteen step, when x is 0.002And 5, obtaining a ceramic phase: XRD tests show that the ceramic has an O-T two-phase coexisting structure and the Curie temperature is 280 ℃; microscopic morphology: the average grain size is 0.34 μm by microscopic morphology SEM test; the density was measured to be 4.28g/cm using a densitometer 3 (ii) a Ferroelectricity: maximum polarization P max 17.08 mu C/cm 2 (ii) a Strain performance: when E ═ 40kV/cm, the strain S% reached 0.22%.
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| US20100264354A1 (en) * | 2007-12-06 | 2010-10-21 | Konica Minolta Holdings, Inc. | Piezoelectric ceramic composition |
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