CN110963797B - High-temperature giant electrostrictive ceramic material and preparation method thereof - Google Patents
High-temperature giant electrostrictive ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a giant electrostrictive strain ceramic material for high temperature, which is prepared from Bi0.5Na0.5TiO3And Bi0.1Na0.7NbO3Is a matrix, and the chemical composition is (1-x) Bi0.5Na0.5TiO3‑xBi0.1Na0.7NbO3Ceramic materials in which x is 0.05 to 0.2, corresponding to x 0.1, reach a maximum unipolar strain of about 1.6% at 185 ℃, which is comparable to the maximum current single crystal strain values, and have superior performance over current lead-containing or lead-free piezoelectric ceramics. In addition, the electrostriction curve has smaller hysteresis and better linearity, can control the strain value of the material more accurately through a corresponding electric field, is expected to be applied in the field of high-temperature piezoelectric materials, such as an electric control gasoline injection system of an automobile, a high-temperature piezoelectric actuator or a motor and the like, and can be used for an accurate control actuating system at high temperature.
Description
Technical Field
The invention belongs to the technical field of electronic functional materials and devices, and particularly relates to a high-temperature giant electrostrictive ceramic material and a preparation method thereof.
Background
The piezoelectric ceramic material is an important functional material and is widely applied in the fields of aerospace, petrochemical industry, electronic circuits and the like. Piezoelectric actuators or motors can be fabricated using the electrostrictive properties of piezoelectric ceramics. However, since the difference between the electrostrictive strain performance of the current piezoelectric ceramics, especially lead-free piezoelectric ceramics, and the piezoelectric single crystal is large, in order to use a material with huge electrostrictive strain, a single crystal material with complicated production process and high production cost still needs to be selected. In addition, due to the continuous development of industrial technology, higher requirements are put on piezoelectric materials, which are required to be in service under extreme conditions such as high temperature. At present, most piezoelectric materials or devices are limited by physical properties such as Curie temperature, the use temperature is generally low, and the piezoelectric performance is obviously deteriorated along with the increase of the temperature. Therefore, it is important to develop a polycrystalline ceramic material having excellent giant electrostrictive properties, and it is desired that the polycrystalline ceramic material can maintain high performance under extreme conditions such as high temperature, and thus it is suitable for application fields such as an electrically controlled gasoline injection system of an automobile, a high-temperature piezoelectric actuator or a motor.
Disclosure of Invention
In order to solve the problems existing in the prior art, the invention designs a piezoceramic material which comprises the following specific components.
A giant electrostrictive polycrystalline ceramic material capable of being used at high temperature comprises sodium bismuth titanate (BNT) as main component, and (1-x) Bi as specific chemical component0.5Na0.5TiO3-xBi0.1Na0.7NbO3Wherein x is 0.05-0.2. The ceramic material has good dielectric, piezoelectric and ferroelectric properties, the dielectric constant of the ceramic material at room temperature under the frequency of 1kHz is 800-1050, and the maximum dielectric constant under the frequency of 1kHz ism900-. When the temperature is lower than 350 ℃, the dielectric loss at 1kHz is not more than 5 percent. The lead-free ceramic material is lead-free and environment-friendly, but has the electrostrictive strain performance exceeding that of lead-containing ceramic which is mainly used at present, wherein the maximum unipolar strain of the ceramic with the x being 0.1 can reach about 1.6 percent under the condition of about 185 ℃, and the electrostrictive strain value is equivalent to the reported maximum electrostrictive strain value of a single crystal, but the ceramic material has better application prospect due to simple production process and lower production cost. In addition, the electrostrictive property of the piezoceramic material of the invention can be continuously increased from room temperature to high temperature, the electrostrictive property can reach the maximum value at certain high temperature (100-250 ℃), and the optimum use temperature can be increased along with the increase of the electrostrictive propertyThe value of x in the fraction is adjusted by varying (the larger x, the lower the optimum temperature for use). The strain range of this material is 0.5-1.6% at 100 ℃ and 250 ℃, and a unipolar strain maximum (1.6%) is reached at 185 ℃ corresponding to x being 0.1. Therefore, a series of giant electrostrictive ceramic materials suitable for different high temperature ranges are expected to be developed.
The invention adopts the following technical route:
(1) respectively weighing raw material powder in proper proportion, including sodium carbonate, bismuth oxide, titanium dioxide (rutile phase) and niobium oxide. Adding alcohol with proper content as ball milling medium, mixing and ball milling for over 4 hr in the ball material ratio of 15 to 1 and rotation speed of 300 rpm.
(2) Mixing uniformly Bi0.5Na0.5TiO3(BNT) and Bi0.1Na0.7NbO3(BNN) the slurry is dried and sieved by a 60-mesh sieve, and presintered for 2 to 4 hours at the temperature of 800-.
(3) Mixing the pre-sintered BNT and BNN powder according to the required proportion, remixing and carrying out planetary ball milling for more than 4 hours, wherein the ball-material ratio is 15:1, and the rotating speed is 300 r/min.
(4) Drying the powder, sieving with a 60-mesh sieve, adding appropriate amount of polyvinyl alcohol (PVA) or polyvinyl butyral (PVB) solution, grinding, granulating, and dry-pressing to obtain the final product with axial pressure of 100-.
(5) The green body is subjected to glue removal treatment at 600 ℃ for 2 hours, and the ceramic is sintered at 1060-1180 ℃ for 1-3 hours.
The invention has the beneficial effects that: (1) the present invention designs a novel ceramic composition with a large unipolar electrostrictive strain; (2) compared with the lead-containing ceramic which is mainly used at present, the ceramic does not contain toxic elements such as lead and the like, has simpler raw materials, better meets the requirements of environmental protection and energy conservation, and has larger strain value; (3) compared with the single crystal which is mainly used at present, the synthesis process of the ceramic is simpler, the cost is greatly reduced, and the strain value is equivalent or better; (4) the use temperature of the maximum strain of the ceramic can be changed through the design of components, so that a series of giant electrostrictive ceramic materials suitable for different high temperature ranges can be obtained, and the giant electrostrictive ceramic materials are expected to be applied to the fields of electric control gasoline injection systems of automobiles, high-temperature piezoelectric actuators or motors and the like; (5) the hysteresis of the electrostrictive strain curve is small, and the linearity is good, so that the electrostrictive strain curve is expected to be applied to the fields of accurate control and the like.
Drawings
FIG. 1 is a surface microtopography of a ceramic of example 1 of the present invention.
FIG. 2 is an X-ray diffraction (XRD) spectrum of the ceramic of example 1 of the present invention.
FIG. 3 shows the maximum electrostrictive strain of the ceramics at different temperatures and d in example 2 of the present invention33 *＝Smax/EmaxThe numerical value of (c).
Fig. 4 is a temperature change hysteresis loop and a temperature change electrostrictive curve of the ceramic of example 3 of the present invention.
Detailed Description
The invention is further illustrated by the following figures and examples, but is not limited to these examples. In the examples, the reagents and materials were all commercially available unless otherwise specified.
Example 1
According to 0.95Bi0.5Na0.5TiO3-0.05Bi0.1Na0.7NbO3The chemical composition of (1) is that raw materials of bismuth oxide, sodium carbonate, titanium dioxide (rutile phase), niobium oxide and the like are weighed, and the ceramic is sintered by a traditional solid-phase reaction method.
Respectively according to Bi0.5Na0.5TiO3(BNT) and Bi0.1Na0.7NbO3(BNN), weighing the raw materials, adding alcohol with proper content, and carrying out planetary ball milling for 4 hours; then, drying the slurry, sieving the slurry, and presintering the slurry for 2 hours at 850 ℃; and mixing and ball-milling the obtained BNT and BNN pre-sintering powder for 4 hours according to the proportion of 0.95BNT-0.05BNN, drying and sieving, adding a proper amount of polyvinyl alcohol (PVA), grinding and granulating, and performing dry pressing and molding. Finally, the green body is degummed for 2 hours at 600 ℃, and then sintered for 2 hours at 1080 ℃ to obtain the required chemical componentsA proportion of a ceramic material.
As shown in FIG. 1, the surface morphology of the SEM of the ceramic shows that the density of the ceramic is high, the pores are few, and the grain size is more than 1-3 μm. The XRD spectrum of the ceramic is shown in figure 2, and the main phase structure of the ceramic is a perovskite phase, and no obvious second phase exists. The unipolar electric strain of the ceramic is in a range of 0.58-0.94% in a temperature range of 100 ℃ and 250 ℃ and under the condition of an electric field of 90kV/cm, and the strain reaches a maximum value under the condition of about 220 ℃. Correspondingly, it is within the temperature interval of 100-33 *＝Smax/EmaxThe value of (b) is in the range of 644.4-1044.4 pm/V.
Example 2
According to 0.925Bi0.5Na0.5TiO3-0.075Bi0.1Na0.7NbO3The chemical composition of (1) is that raw materials of bismuth oxide, sodium carbonate, titanium dioxide (rutile phase), niobium oxide and the like are weighed, and the ceramic is sintered by a traditional solid-phase reaction method.
Respectively according to Bi0.5Na0.5TiO3(BNT) and Bi0.1Na0.7NbO3(BNN), weighing the raw materials, adding alcohol with proper content, and carrying out planetary ball milling for 4 hours; then, drying the slurry, sieving the slurry, and presintering the slurry for 2 hours at 850 ℃; and mixing and ball-milling the obtained BNT and BNN pre-sintering powder for 4 hours according to the proportion of 0.925BNT-0.075BNN, drying and sieving, adding a proper amount of polyvinyl alcohol (PVA), grinding and granulating, and performing dry pressing and molding. And finally, gluing the green body at 600 ℃ for 2 hours, and sintering at 1080 ℃ for 2 hours to obtain the ceramic material with the required chemical component ratio.
Unipolar electrostriction of ceramics and d33 *＝Smax/EmaxThe temperature dependence of the value of (A) is shown in FIG. 3, the unipolar electric strain of the ceramic is in the range of 0.5-1.24% in the temperature range of 100-250 ℃ and under the condition of 110kV/cm electric field, and the strain reaches the maximum value under the condition of about 205 ℃. Correspondingly, it is within the temperature interval of 100-33 *＝Smax/EmaxThe numerical value of (A) is in the range of 454.5-1127.3pm/V。
Example 3
According to 0.9Bi0.5Na0.5TiO3-0.1Bi0.1Na0.7NbO3The chemical composition of (1) is that raw materials of bismuth oxide, sodium carbonate, titanium dioxide (rutile phase), niobium oxide and the like are weighed, and the ceramic is sintered by a traditional solid-phase reaction method.
Respectively according to Bi0.5Na0.5TiO3(BNT) and Bi0.1Na0.7NbO3(BNN), weighing the raw materials, adding alcohol with proper content, and carrying out planetary ball milling for 4 hours; then, drying the slurry, sieving the slurry, and presintering the slurry for 2 hours at 850 ℃; and mixing and ball-milling the obtained BNT and BNN pre-sintering powder for 4 hours according to the proportion of 0.9BNT-0.1BNN, drying and sieving, adding a proper amount of polyvinyl alcohol (PVA), grinding and granulating, and performing dry pressing and molding. And finally, gluing the green body at 600 ℃ for 2 hours, and sintering at 1080 ℃ for 2 hours to obtain the ceramic material with the required chemical component ratio.
As shown in fig. 4(a), the temperature-changing hysteresis loop of the ceramic causes depolarization of the ceramic to some extent as the temperature increases. As shown in fig. 4(b), the temperature-variable unipolar strain of the ceramic increases with increasing temperature, and reaches a maximum value of approximately 1.6% at about 185 ℃. The unipolar electric strain of the ceramic is in a range of 0.84-1.58% in a temperature range of 100 ℃ and 250 ℃ and under the condition of an electric field of 130kV/cm, and the strain reaches a maximum value under the condition of about 185 ℃. Correspondingly, it is within the temperature interval of 100-33 *＝Smax/EmaxThe value of (b) is in the range of 646.2-1215.4 pm/V.
Example 4
According to 0.875Bi0.5Na0.5TiO3-0.125Bi0.1Na0.7NbO3The chemical composition of (1) is that raw materials of bismuth oxide, sodium carbonate, titanium dioxide (rutile phase), niobium oxide and the like are weighed, and the ceramic is sintered by a traditional solid-phase reaction method.
Respectively according to Bi0.5Na0.5TiO3(BNT) and Bi0.1Na0.7NbO3(BNN), weighing the raw materials, adding alcohol with proper content, and carrying out planetary ball milling for 4 hours; then, drying the slurry, sieving the slurry, and presintering the slurry for 2 hours at 850 ℃; and mixing and ball-milling the obtained BNT and BNN pre-sintering powder for 4 hours according to the proportion of 0.875BNT to 0.125BNN, drying and sieving, adding a proper amount of polyvinyl alcohol (PVA) aqueous solution, grinding and granulating, and performing dry pressing and molding. And finally, gluing the green body at 600 ℃ for 2 hours, and sintering at 1080 ℃ for 2 hours to obtain the ceramic material with the required chemical component ratio.
The unipolar electric strain of the ceramic is in the range of 0.51-1.34% in the temperature range of 100-250 ℃ and under the condition of an electric field of 130kV/cm, and the strain reaches the maximum value under the condition of about 170 ℃. Correspondingly, it is within the temperature interval of 100-33 *＝Smax/EmaxThe value of (A) is in the range of 392.3-1030.8 pm/V.
The above embodiments describe the technical solutions of the present invention in detail. It will be clear that the invention is not limited to the described embodiments. Based on the embodiments of the present invention, those skilled in the art can make various changes, but any changes equivalent or similar to the present invention are within the protection scope of the present invention.
Claims (6)
1. A giant electrostrictive polycrystalline ceramic material is characterized in that Bi is used0.5Na0.5TiO3And Bi0.1Na0.7NbO3Is a matrix, and the chemical composition is (1-x) Bi0.5Na0.5TiO3-xBi0.1Na0.7NbO3Wherein x is 0.05-0.2, the dielectric constant of the ceramic material at room temperature is 800-1050 at the frequency of 1kHz, and the maximum dielectric constant is 1kHzm2350, 900 times; when the temperature is lower than 350 ℃, the dielectric loss is not more than 5% under 1 kHz; the unipolar strain of the material reaches a maximum at high temperatures of 100-250 ℃, where the maximum unipolar strain value of the composition can reach 1.6% when x is 0.1.
2. The method of preparing a giant electrostrictive polycrystalline ceramic material as recited in claim 1, comprising the steps of:
(1) respectively weighing raw material powder in proper proportion, including sodium carbonate, bismuth oxide, titanium dioxide and niobium oxide; performing ball milling;
(2) mixing uniformly Bi0.5Na0.5TiO3And Bi0.1Na0.7NbO3Drying and sieving the slurry, and presintering; the presintering temperature range is 800-900 ℃, and the presintering time is 2-4 hours;
(3) mixing the presintered powder, and performing ball milling again;
(4) drying the product obtained in the step (3), sieving, adding a polyvinyl alcohol aqueous solution or a polyvinyl butyral alcohol solution, grinding and granulating, and performing dry pressing and molding;
(5) and carrying out glue discharging treatment and sintering on the pressed green body, wherein the glue discharging treatment temperature is 600 ℃, the glue discharging time is 2 hours, the sintering temperature is 1060-1180 ℃, and the sintering time is 1-3 hours.
3. The method according to claim 2, wherein the titanium dioxide in step (1) is rutile phase, an appropriate amount of alcohol is added as a ball milling medium, and the mixture is subjected to ball milling for more than 4 hours by using a mixing planetary ball mill, wherein the ball-material ratio is 15:1, and the rotating speed is 300 revolutions per minute.
4. The method of claim 2, wherein the sieving in step (2) is through a 60 mesh sieve.
5. The method according to claim 2, wherein the ball milling in the step (3) is carried out by planetary ball milling for more than 4 hours at a ball-to-material ratio of 15:1 and a rotation speed of 300 revolutions per minute.
6. The method as claimed in claim 2, wherein the sieving in step (4) is 60 mesh sieving, the pressure of the dry pressing is 100-200 MPa, and the pressure is applied in an axial direction.
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