CN110981476A - Potassium sodium niobate-based transparent ceramic material and preparation method thereof - Google Patents
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Abstract
The invention belongs to the technical field of transparent ceramic materials, and relates to a potassium sodium niobate-based transparent ceramic material and a preparation method thereof, wherein the chemical composition of the potassium sodium niobate-based transparent ceramic material is (1-x) (K)0.5Na0.5)NbO3‑xSr(Sc0.5Nb0.5)O3Wherein x is 10 ≦ 20 mol%; the transparent ferroelectric ceramic with compact, uniform and micron-sized grains is successfully prepared by adopting a traditional solid phase sintering method. The ceramic prepared by the invention has high transmissivity (64-72% at 0.3mm thickness) in visible light and near infrared region, and can obtain 4.45J/cm at high breakdown field strength (395kV/cm)3High energy storage density of (2); the system transparent ceramic can well combine the electrical and optical characteristics, realize the multi-functionalization of electronic components, can replace part of lead-containing ceramic, and reduce the environmental pollution of heavy metals.
Description
Technical Field
The invention belongs to the technical field of transparent ceramic materials, and particularly relates to a potassium sodium niobate-based transparent ceramic material and a preparation method thereof.
Background
The transparent ceramic is always an excellent candidate material for preparing the pulse power dielectric energy storage capacitor due to the advantages of wide temperature range, long service life, reliable performance and the like; the ceramic energy storage capacitor can realize instantaneous heavy current and high voltage discharge, is an important electronic component, and has irreplaceable status in future optical computer technology, electronic information technology and national defense and military application development; with the rapid development of electronic information technology, people have higher and higher requirements for using equipment, and in order to achieve higher use performance, miniaturization and integration are the development trends of electronic components.
The research on the ceramic energy storage capacitor is widely concerned, however, the ceramic energy storage capacitor is limited by low energy storage density, and the main research at present focuses on improving the energy storage density, enhancing the performance stability and realizing lead-free devices; its energy storage density WrecThe following can be calculated through the hysteresis loop:
wherein E is the applied electric field strength, PmaxTo saturation of polarization, PrIs the remanent polarization; relaxor ferroelectrics are high P due to theirmaxLow P ofrAnd low hysteresis has obvious advantages in obtaining high energy storage density and efficiency compared with linear dielectric, normal ferroelectric and antiferroelectric; lead-free (K)0.5Na0.5)NbO3The (KNN) ceramic has high Curie temperature and large electromechanical coupling coefficient, and is a lead-free ferroelectric material with excellent performance.
The KNN generally has an orthorhombic phase with low crystal symmetry, and the KNN ceramic has good photoelectric properties, but has low light transmittance, low dielectric constant and poor mechanical strength.
Disclosure of Invention
In order to solve the problems, the invention provides a potassium sodium niobate-based transparent ceramic material which comprises the following raw materials in percentage by mole (1-x) (K)0.5Na0.5)NbO3-xSr(Sc0.5Nb0.5)O3Wherein 0.1 ≦ x ≦ 0.2.
Preferably, the component raw materials and the molar percentage content thereof are 0.825 (K)0.5Na0.5)NbO3-0.175Sr(Sc0.5Nb0.5)O3。
As a further illustration of the scheme, the potassium-sodium niobate-based transparent ceramic material has a pseudo-cubic phase structure and an average particle size of 290 nm.
The invention also provides a preparation method of the potassium sodium niobate-based transparent ceramic material, which comprises the following steps:
(1) preparing materials: with K2CO3Powder, Na2CO3Powder and Nb2O5Powder and SrCO3Powder and Sc2O3Powder is used as a raw material, and ball milling is carried out after the powder is mixed according to the chemical composition of the lead-free potassium sodium niobate-based transparent ceramic material to obtain mixed powder;
(2) pre-burning: pre-sintering the mixed powder at 900-950 ℃;
(3) secondary ball milling: ball-milling and sieving the pre-sintered mixed powder to obtain the compound with the chemical composition general formula of (1-x) (K)0.5Na0.5)NbO3-xSr(Sc0.5Nb0.5)O3The x is 0.1-0.2;
(4) tabletting: adding polyvinyl alcohol PVA into the powder to prepare (1-x) (K)0.5Na0.5)NbO3-xSr(Sc0.5Nb0.5)O3Granulating to obtain (1-x) (K)0.5Na0.5)NbO3-xSr(Sc0.5Nb0.5)O3Green bodies;
(5) and (3) sintering: mixing the (1-x) (K)0.5Na0.5)NbO3-xSr(Sc0.5Nb0.5)O3And (4) preserving the heat of the green body for 4-5 hours at 1250-1270 ℃ to obtain the potassium-sodium niobate-based transparent ceramic material.
As a further explanation of the scheme, the rotation speed of the ball milling in the step (1) and the step (3) is 350-420 r/min.
As a further illustration of the scheme, the ball milling time in the step (1) is 10-15h, and the ball milling time in the step (3) is 15-18 h.
As a further explanation of the scheme, the temperature rising rate of the pre-sintering in the step (2) is 3-5 ℃/min for 4-5 h.
As a further explanation of the scheme, the aperture of the sieved screen in the step (3) is 60-120 meshes.
As a further illustration of the scheme, the glue discharging in the step (4) is carried out at the temperature of 600 ℃ for 3-5 hours.
As a further illustration of the scheme, the pressure of the tabletting in the step (4) is 200-300 MPa, the pressure maintaining time is 1-3 min, the size of the obtained green body is 13-17 mm, and the thickness is 1-1.4 mm.
The invention has the beneficial effects that:
(1) the invention can obtain the potassium sodium niobate-based transparent ceramic material under the conventional pressureless sintering by utilizing the component control and regulation;
(2) the potassium-sodium niobate-based transparent ceramic material obtained by the invention has the advantages of few defects, high density, good crystallinity, uniform grain size, average grain size of about 290nm and fine crystal structure;
(3) the potassium-sodium niobate-based transparent ceramic material obtained by the invention has high dielectric relaxation property and breakdown-resistant electric field, and can obtain a slender electric hysteresis loop;
(4) the potassium sodium niobate-based transparent ceramic material obtained by the invention has excellent energy storage characteristics, and under an external electric field of 395kV/cm, the discharge energy density reaches 2.67J/cm3, and the energy storage density is 4.45J/cm3The energy storage efficiency reaches 60 percent;
(5) the potassium-sodium niobate-based transparent ceramic material obtained by the invention has excellent optical performance, and shows higher transmissivity (64% -72% under the thickness of 0.3 mm) in visible light and near infrared regions.
Drawings
FIG. 1: (1-x) (K) provided in example 10.5Na0.5)NbO3-xSr(Sc0.5Nb0.5)O3XRD pattern of transparent ceramic sample;
FIG. 2: (1-x) (K) provided in example 10.5Na0.5)NbO3-xSr(Sc0.5Nb0.5)O3An optical transmittance graph and a polished physical graph of the transparent ceramic sample.
FIG. 3: fruit of Chinese wolfberry(1-x) (K) provided in example 10.5Na0.5)NbO3-xSr(Sc0.5Nb0.5)O3The transparent ceramic sample has a hysteresis loop at room temperature.
FIG. 4: example 2 provides 0.825 (K)0.5Na0.5)NbO3-0.175Sr(Sc0.5Nb0.5)O3The transparent ceramic sample has a hysteresis loop at room temperature.
Detailed Description
The invention will be further explained with reference to the drawings and the embodiments.
Example 1:
referring to FIGS. 1 to 3, this example provides a component material and its molar percentage content is (1-x) (K)0.5Na0.5)NbO3-xSr(Sc0.5Nb0.5)O3The preparation method of the potassium sodium niobate-based transparent ceramic material comprises the following steps:
the first step is as follows: mixing, firstly calculating each component K in the powder raw material according to the chemical formula2CO3、Na2CO3、Nb2O、SrCO3、Sc2O3The components are prepared according to the composition proportion, and ball milling is carried out after mixing to obtain mixed powder; and then carrying out first ball milling, adding a ball milling medium into the mixture, putting the mixture into a ball milling tank for ball milling for 10 hours, wherein the ball milling rotating speed is 350r/min, after the ball milling is finished, drying the mixture in an oven at the temperature of 80 ℃, and sieving the mixture by using a 60-80-mesh sieve to obtain mixed powder.
The second step is that: pre-burning, adding the ground mixture into a crucible, compacting, placing in a muffle furnace, heating to 950 ℃ at a heating rate of 3 ℃/min, preserving heat for 5h for pre-burning, naturally cooling to room temperature, and taking out the crucible.
The third step: performing secondary ball milling, performing ball milling on the pre-sintered mixed powder for 15 hours at the ball milling speed of 350r/min, drying the mixed material after the ball milling is finished, and sieving the dried mixed material by using a 80-mesh sieve to obtain powder with the chemical composition general formula of (1-x) (K)0.5Na0.5)NbO3-xSr(Sc0.5Nb0.5)O3；
The fourth step: tabletting, mixing the powder with 5 wt% polyvinyl alcohol solution, pressing into sealed bag of blank device, standing for 12 hr, sieving with 60 mesh and 120 mesh sieves, and collecting powder in the middle layer of the sieve to obtain 0.85 (K)0.5Na0.5)NbO3-0.15Sr(Sc0.5Nb0.5)O3(ii) a pellet; adding the treated powder into a die with the diameter of 13cm, and pressing into a green body with the thickness of 1.2mm under the pressure of 300 MPa; and (3) placing the green body on an alumina plate, placing the green body in a muffle furnace, preserving heat for 5 hours at the temperature of 600 ℃ for removing glue, and naturally cooling the green body to room temperature along with the furnace.
The fifth step: and sintering, namely putting the green body into an alumina crucible, placing the alumina crucible into a muffle furnace, sintering for 5 hours at 1263 ℃, and naturally cooling to room temperature to obtain the potassium-sodium niobate-based transparent ceramic.
And (3) grinding and polishing the sintered ceramic block, coating high-temperature silver paste on two surfaces, heating to 800 ℃ at a speed of 3 ℃/min, and preserving heat for 20min to obtain a silver electrode.
The detection method of the crystalline phase of the fine crystalline transparent ceramic material is X-ray diffraction analysis (XRD). As shown in fig. 1, it can be seen that the prepared ceramic material is a pure perovskite structure, no impurity phase exists, no trigonal or tetragonal lattice distortion exists in the XRD result, and a pseudo cubic phase structure is presented.
The obtained product was 0.825 (K)0.5Na0.5)NbO3-0.175Sr(Sc0.5Nb0.5)O3The transparent ceramic material is tested by a high-temperature impedance analyzer, and the ceramic has obvious relaxation property through a dielectric temperature spectrum.
The obtained product was 0.825 (K)0.5Na0.5)NbO3-0.175Sr(Sc0.5Nb0.5)O3Grinding and polishing the transparent ceramic sample to 0.3mm, and measuring the light transmittance by using a spectrophotometer, wherein the test result shows that the transmittance in visible light and infrared regions is 64% -72%, as shown in figure 2.
The ceramic element prepared in this example was subjected toAfter the ferroelectric property test of different electric fields at room temperature, the electric hysteresis loop is shown in figure 3, and the maximum polarization intensity is 24.33 mu C/cm2The remanent polarization is 5.74 mu C/cm2The maximum breakdown field intensity is 395kV/cm, and the energy storage density W is 4.45J/cm3Reversible energy storage density Wrec＝2.67J/cm3The efficiency η is 60%.
Example 2:
a potassium-sodium niobate-based transparent ceramic material having a composition of 0.85 (K) was prepared according to the preparation method described in example 10.5Na0.5)NbO3-0.15Sr(Sc0.5Nb0.5)O3The ferroelectric property test of different electric fields at room temperature is carried out, and the electric hysteresis loop is shown as figure 4. Maximum polarization intensity of 18.14 μ C/cm2The remanent polarization is 2.47 mu C/cm2The maximum breakdown field strength is 265kV/cm, and the energy storage density W is 2.0657J/cm3Reversible energy storage density Wrec＝1.593J/cm3Efficiency η was 77.12%.
Example 3:
the other conditions were the same as in example 1 except that the sintering temperature was 1266 ℃. Micropores exist in the potassium-sodium niobate-based transparent ceramic prepared at the sintering temperature, and the breakdown-resistant electric field of the potassium-sodium niobate-based transparent ceramic is 250 kV/cm. Its electric hysteresis is fat although PmaxHigher value, but at the same time PrToo large a value, resulting in W thereofrecIs only 1.2J/cm3η is only 46%.
Example 4:
the other conditions were the same as in example 1 except that the holding time was 6 hours at a sintering temperature of 1263 ℃. The potassium sodium niobate-based transparent ceramic prepared in the heat preservation time can observe abnormal growth of crystal grains and uneven and compact crystal grain structure through a scanning electron microscope.
In summary, the following steps: the preparation method adopts the preparation technical scheme of the embodiment 1 to successfully prepare the compact and uniform transparent ferroelectric ceramic with the nano-scale crystal grains; the potassium-sodium niobate-based transparent ceramic prepared by the invention shows higher transmissivity (64% -72% under the thickness of 0.3 mm) in visible light and near infrared regions, and can achieve 4.45J/board obtained under high breakdown field strength (395kV/cm)cm3High energy storage density of (2); the electrical and optical characteristics are well combined, and the multi-functionalization of electronic components is realized; (1-x) (K)0.5Na0.5)NbO3-xSr(Sc0.5Nb0.5)O3Can replace partial lead-containing ceramic, not only ensures good photoelectric property, but also reduces environmental pollution.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by using the contents of the present specification and the accompanying drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. The potassium-sodium niobate-based transparent ceramic material is characterized by comprising the following raw materials in percentage by mole (1-x) (K)0.5Na0.5)NbO3-xSr(Sc0.5Nb0.5)O3Wherein 0.1 ≦ x ≦ 0.2.
2. The transparent potassium sodium niobate-based ceramic material as claimed in claim 1, wherein the component materials and the molar percentage content thereof are 0.825 (K)0.5Na0.5)NbO3-0.175Sr(Sc0.5Nb0.5)O3。
3. The potassium-sodium niobate-based transparent ceramic material according to claim 1 or 2, wherein the lead-free potassium-sodium niobate-based transparent ceramic material has a pseudo-cubic phase structure and an average particle diameter of 290 nm.
4. The method for preparing a potassium sodium niobate-based transparent ceramic material according to any one of claims 1 to 3, comprising the steps of:
(1) preparing materials: with K2CO3Powder, Na2CO3Powder and Nb2O5Powder and SrCO3Powder and Sc2O3Powder, as raw material, according toMixing the chemical compositions of the lead-free potassium sodium niobate-based transparent ceramic material, and then carrying out ball milling to obtain mixed powder;
(2) pre-burning: pre-sintering the mixed powder at 900-950 ℃;
(3) secondary ball milling: ball-milling and sieving the pre-sintered mixed powder to obtain the compound with the chemical composition general formula of (1-x) (K)0.5Na0.5)NbO3-xSr(Sc0.5Nb0.5)O3The x is 0.1-0.2;
(4) tabletting: adding polyvinyl alcohol PVA into the powder to prepare (1-x) (K)0.5Na0.5)NbO3-xSr(Sc0.5Nb0.5)O3Granulating to obtain (1-x) (K)0.5Na0.5)NbO3-xSr(Sc0.5Nb0.5)O3Green bodies;
(5) and (3) sintering: mixing the (1-x) (K)0.5Na0.5)NbO3-xSr(Sc0.5Nb0.5)O3And (4) preserving the heat of the green body for 4-5 h at 1250-.
5. The method for preparing a potassium sodium niobate-based transparent ceramic material as claimed in claim 4, wherein the rotation speed of the ball milling in the steps (1) and (3) is 350 to 420 r/min.
6. The preparation method of the potassium sodium niobate-based transparent ceramic material as claimed in claim 5, wherein the ball milling time in the step (1) is 10-15h, and the ball milling time in the step (3) is 15-18 h.
7. The method for preparing the potassium sodium niobate-based transparent ceramic material as claimed in claim 4, wherein the pre-sintering in the step (2) is carried out for 4-5 h at a heating rate of 3-5 ℃/min.
8. The method for preparing a potassium sodium niobate-based transparent ceramic material as claimed in claim 4, wherein the mesh size of the sieved mesh in the step (3) is 60-120 mesh.
9. The preparation method of the potassium sodium niobate-based transparent ceramic material as claimed in claim 4, wherein the step (4) of discharging the gel is carried out at 600 ℃ for 3-5 h.
10. The method for preparing a potassium sodium niobate-based transparent ceramic material according to claim 4, wherein the pressure of the pressed sheet in the step (4) is 200-300 MPa, the pressure maintaining time is 1-3 min, the size of the obtained green body is 13-17 mm, and the thickness is 1-1.4 mm.
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| CN112028624A (en) * | 2020-08-27 | 2020-12-04 | 西安工业大学 | BNT-based energy storage ceramic material and preparation method and application thereof |
| CN112408983A (en) * | 2020-11-26 | 2021-02-26 | 四川大学 | Lanthanum bismuthate-doped potassium-sodium niobate-based multifunctional ceramic material and preparation method thereof |
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| CN112830781B (en) * | 2021-01-19 | 2022-10-28 | 桂林电子科技大学 | Lead-free transparent ferroelectric ceramic material and preparation method and application thereof |
| CN115490514A (en) * | 2021-06-18 | 2022-12-20 | 阜新德尔汽车部件股份有限公司 | Piezoelectric ceramic and preparation method and application thereof |
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