Ferroelectric ceramic material with high transmittance and ferroelectricity and preparation method thereof

By nanostructuring the ferroelectric domain structure of KNN ceramics with LaF3 dopant, the problems of low light transmittance and difficulty in achieving both ferroelectric properties in KNN-based ceramics are solved, realizing a synergy between high transparency and ferroelectric properties, which is suitable for industrial production.

CN121226015BActive Publication Date: 2026-02-24CHENGDU UNIV OF INFORMATION TECH
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Patent Information

Application Number
CN202511795193.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-12-02
Publication Date
2026-02-24
Estimated Expiration
2045-12-02

AI Technical Summary

Technical Problem

Existing technologies struggle to significantly improve the transmittance of KNN-based ceramics while maintaining their ferroelectric properties, and traditional preparation methods are complex, costly, and difficult to scale up for mass production.

Method used

Using LaF3 as a composite dopant, ferroelectric ceramic materials with the general chemical formula (K0.48Na0.52)NbO3-xLaF3 were prepared by nano-sizing ferroelectric domain structures through the synergistic effect of rare earth cations La3+ and anions F-, thereby achieving efficient control over the ferroelectric domain structure of KNN ceramics.

Benefits of technology

While maintaining good ferroelectricity, the optical transmittance is significantly improved, and the dielectric loss and leakage current are reduced, making the material suitable for industrial production.

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Abstract

The application discloses a ferroelectric ceramic material with synergic light transmittance and ferroelectricity and a preparation method thereof, and belongs to the technical field of ceramic materials. 0.48 Na 0.52 )NbO3- x LaF3, x represents the mole number of LaF3, x is 0.01-0.04; the ceramic material is uniformly distributed with nanoscale polar microzones PNRs, and the polar microzones PNRs are easily flipped under an external electric field. By introducing LaF3 as a composite dopant, the synergic effect of the rare earth cation La 3+ and the anion F ‑ is utilized to realize nanosizing and efficient regulation of the KNN ceramic ferroelectric domain structure, so that the optical transmittance of the ceramic material is significantly improved under the premise of maintaining good ferroelectricity, and the process is simple and suitable for industrialization.
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Description

Technical Field

[0001] This invention relates to the field of ceramic materials technology, and in particular to a ferroelectric ceramic material with synergistic light transmittance and ferroelectricity, and its preparation method. Background Technology

[0002] Transparent ferroelectric ceramics are advanced materials that combine high light transmittance with ferroelectric, piezoelectric, and dielectric properties, attracting widespread attention due to their unique multifunctionality. In terms of optical properties, transparent ferroelectric ceramics are similar to single-crystal materials of the same material, while inheriting the advantages of traditional ceramics such as high melting point, high hardness, and oxidation resistance. With technological advancements and social development, transparent ferroelectric ceramics have shown enormous application potential in medical diagnostics, information technology, and energy fields. For example, in the medical field, they can be used to manufacture highly sensitive transparent transducers, combining the advantages of optical and ultrasonic imaging to improve the resolution of photoacoustic imaging and the accuracy of disease diagnosis. In the field of information technology, transparent ferroelectric ceramics can be used to develop high-speed, high-bandwidth electro-optic modulation devices and highly secure three-dimensional optical information storage devices. In the energy field, they can be used to develop dielectric energy storage devices that simultaneously possess transparency and energy storage characteristics.

[0003] However, current high-performance transparent ferroelectric ceramics are mainly based on lead-based materials (such as PLZT). However, due to their high lead oxide content, they pose serious threats to the environment and human health during production, use, and disposal, and international environmental regulations (such as RoHS) have strictly restricted their use. Therefore, the research and development of high-performance lead-free transparent ferroelectric ceramics is of profound significance to electronic information technology, environmental protection, and sustainable development strategies. Potassium sodium niobate (KNN)-based lead-free ceramics are considered one of the most promising material systems to replace lead-based ceramics due to their high Curie temperature and good piezoelectric properties. However, pure KNN ceramics have an orthorhombic phase structure at room temperature, exhibiting significant optical anisotropy, severe birefringence and scattering (grain boundaries, domains), and low transmittance. To improve their transparency, doping is usually required to induce a transformation to a highly symmetric cubic or pseudo-cubic phase, but this often leads to a deterioration in ferroelectric and piezoelectric properties, making it difficult to achieve multifunctional characteristics. For example, doping with cations (such as La2O3) can improve the density and transmittance of KNN ceramics, but it can also lead to an increase in remanent polarization (…). P r The dielectric loss is significantly reduced and the leakage current is increased, making it difficult to achieve synergistic optimization of optical and electrical properties. In addition, the traditional solid-state method for preparing KNN ceramics is prone to poor density and high dielectric loss due to the volatilization of alkali metals. Although special sintering processes (such as hot pressing sintering and plasma sintering) can improve performance, they are costly and complex, making it difficult to scale up production.

[0004] Existing technologies mostly focus on macroscopic composition adjustment and special densification processes (e.g., isostatic pressing, special sintering), but lack proactive and precise means to control the microscopic ferroelectric domain structure, which plays a decisive role in material properties. The domain structures obtained by most methods are random and non-uniform in size, becoming light scattering centers and performance bottlenecks. Therefore, developing a new method that can actively design and stabilize specific domain structures to synergistically improve the optical and ferroelectric properties of KNN-based ceramics has become an urgent technical problem to be solved in this field. Summary of the Invention

[0005] The purpose of this invention is to provide a ferroelectric ceramic material with synergistic light transmittance and ferroelectricity, and its preparation method thereof. This is achieved by introducing LaF3 as a composite dopant and utilizing the rare earth cation La... 3+ and anion F - The synergistic effect of these technologies enables the nano-sizing and efficient control of the ferroelectric domain structure of KNN ceramics, thereby significantly improving its optical transmittance while maintaining good ferroelectricity. Furthermore, the process is simple and suitable for industrialization.

[0006] To achieve the above objectives, this invention provides a ferroelectric ceramic material with synergistic light transmittance and ferroelectricity, having the general chemical formula (K... 0.48 Na 0.52 NbO3- x LaF3, x Indicates the number of moles of LaF3. x The value ranges from 0.01 to 0.04; nanoscale polar microregions PNRs are uniformly distributed inside the ceramic material, and these polar microregions PNRs are easily flipped under an external electric field.

[0007] Preferably, the x The value is 0.035.

[0008] A method for preparing a ferroelectric ceramic material with synergistic light transmittance and ferroelectricity includes the following steps:

[0009] S1. Weigh analytical grade sodium carbonate (Na2CO3), potassium carbonate (K2CO3), niobium pentoxide (Nb2O5), and lanthanum fluoride (LaF3) as raw materials according to the stoichiometric ratio of the general chemical formula.

[0010] S2. The raw materials are ball-milled once, dried, and then crushed to obtain a mixed powder.

[0011] S3. Pour the mixed powder into a small crucible and pre-fire it to obtain the pre-fired material;

[0012] S4. The pre-burned material is crushed and then ball-milled in a ball mill jar. The powder is dried and then ground to obtain a secondary mixed powder.

[0013] S5. Add polyvinyl alcohol aqueous solution to the secondary mixed powder for granulation, dry and grind the granulated powder, and obtain fine powder after sieving.

[0014] S6. The fine powder is pressed into sheets and debinded in sequence to obtain a ceramic body;

[0015] S7. Sinter the ceramic blank to obtain a ceramic body;

[0016] S8. A silver electrode is plated onto the ceramic body, and a voltage is applied to polarize it to obtain the ceramic material.

[0017] Preferably, in S2 and S4, the medium for the first and second ball milling is anhydrous ethanol, the rolling ball milling time for the first ball milling in the nylon ball milling jar is 8h~10h, the ball milling time for the second ball milling is 8h~10h, and the grinding balls are zirconium balls.

[0018] Preferably, in step S3, the pre-firing temperature is 850℃~900℃ and the pre-firing time is 4h~6h.

[0019] Preferably, in step S5, the mass concentration of the polyvinyl alcohol aqueous solution is 6wt%~8wt%, and after granulation and grinding, it is sieved through a 200-mesh sieve.

[0020] Preferably, in step S6, the tableting pressure is 8MPa~10MPa, and the glue is discharged at 550℃.

[0021] Preferably, in step S7, the ceramic blank is buried in sieved coarse powder, and a crucible is inverted. The crucible is then sealed with zirconium oxide micro powder and placed in a muffle furnace for sintering. The sintering is carried out in two steps: first, sintering at 1100℃~1150℃ for 3h~5h, and then sintering at 1150℃~1180℃ for 3h~5h.

[0022] Preferably, the prepared ceramic material has an optical transmittance of 70% in the near-infrared region at 1600 nm and a remanent polarization intensity of [missing information]. P r It is 17.45 .

[0023] The advantages and positive effects of the ferroelectric ceramic material with synergistic light transmittance and ferroelectricity described in this invention and its preparation method are as follows:

[0024] 1. This invention uses lanthanum fluoride (LaF3) as the dopant source, and the cation La... 3+ Entering the A-site of the perovskite structure, the introduced chemical disorder effectively disrupts the long-range ferroelectric order, inducing a pseudo-cubic phase transformation of the crystal structure and laying the foundation for the formation of nanoscale ferroelectric domains (polar nanodomains, PNRs). More importantly, the anion F... -The introduction of La effectively suppresses the formation of oxygen vacancies through unique defect chemical reactions, significantly weakens the domain wall pinning effect, and makes the nanodomains easier to flip under an external electric field, thus maintaining excellent ferroelectric properties while achieving high transparency. 3+ For position A and F - Doping the O-site with both cation and anion sites effectively suppresses oxygen vacancy formation, reduces leakage current and dielectric loss, and improves the resistivity and stability of the material.

[0025] 2. The ceramic prepared by this invention possesses both extremely high optical transparency and excellent ferroelectricity, with a LaF3 doping amount... x When the polarization is 0.035, its optical transmittance can reach up to 70% in the near-infrared region at 1600 nm, while the residual polarization intensity ( P r It can be maintained at 17.45. The high level of technology has successfully resolved the contradiction between transparency and ferroelectricity in traditional doping techniques.

[0026] 3. The ferroelectric ceramic material described in this invention does not contain lead and is an environmentally friendly material. The preparation method of the ferroelectric ceramic material is simple and conducive to large-scale production.

[0027] The technical solution of the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. Attached Figure Description

[0028] Figure 1 These are the X-ray diffraction patterns of the ferroelectric ceramic materials in Examples 1-5 of this invention;

[0029] Figure 2 These are the transmittance curves of the ferroelectric ceramic materials in Examples 1-5 of this invention;

[0030] Figure 3 This is a schematic diagram showing the relative permittivity of the ferroelectric ceramic materials in Examples 1-5 of the present invention as a function of temperature at 100 kHz.

[0031] Figure 4 This is a schematic diagram showing the change of dielectric loss of the ferroelectric ceramic materials in Embodiments 1-5 of the present invention at 100 kHz as a function of temperature.

[0032] Figure 5 These are scanning electron microscope images of the ferroelectric ceramic material of Embodiment 4 of the present invention;

[0033] Figure 6 These are the hysteresis loops of the ferroelectric ceramic material in Embodiment 4 of the present invention under different test electric field conditions;

[0034] Figure 7The amplitude and phase diagrams of the ferroelectric ceramic material of the present invention obtained by piezoelectric microscopy (PFM) testing are shown below; (a) is the amplitude diagram of the ferroelectric ceramic material of Example 1, (b) is the phase diagram of the ferroelectric ceramic material of Example 1, (c) is the amplitude diagram of the ferroelectric ceramic material of Example 4, and (d) is the phase diagram of the ferroelectric ceramic material of Example 4. Detailed Implementation

[0035] The embodiments of the present invention will now be described in detail with reference to the accompanying drawings.

[0036] A ferroelectric ceramic material with synergistic properties of light transmittance and ferroelectricity, having the general chemical formula (K... 0.48 Na 0.52 NbO3- x LaF3, x Indicates the number of moles of LaF3. x The value ranges from 0.01 to 0.04; nanoscale polar microregions PNRs are uniformly distributed inside the ceramic material, and these polar microregions PNRs are easily flipped under an external electric field.

[0037] Preferred, x The value is 0.035.

[0038] Lanthanum fluoride (LaF3) was used as the dopant source. The cation La... 3+ Entering the A-site of the perovskite structure, the introduced chemical disorder effectively disrupts the long-range ferroelectric order, inducing a pseudo-cubic phase transformation of the crystal structure and laying the foundation for the formation of nanoscale ferroelectric domains (polar nanoregions, PNRs). Anion F - The introduction of La effectively suppresses the formation of oxygen vacancies through unique defect chemical reactions, significantly weakens the domain wall pinning effect, and makes the nanodomains easier to flip under an external electric field, thus maintaining excellent ferroelectric properties while achieving high transparency. 3+ For position A and F - Doping the O-site with both cation and anion sites effectively suppresses oxygen vacancy formation, reduces leakage current and dielectric loss, and improves the resistivity and stability of the material.

[0039] As the LaF3 doping concentration increases, the domain size of the ceramic decreases. Nanoscale PNRs, due to their size being much smaller than the visible light wavelength, can significantly reduce light scattering loss, which is beneficial for achieving high optical transmittance. Simultaneously, the low energy barrier of PNRs makes them readily reorientable under an external electric field, giving the ceramic a certain degree of polarization response and piezoelectric activity. Therefore, controlling LaF3 doping to induce the formation of PNRs can synergistically achieve high transparency and good ferroelectric properties.

[0040] Furthermore, LaF3 doping enhances the crystal symmetry of KNN, promotes grain refinement, improves material density and uniformity, reduces grain boundary scattering, thereby reducing light scattering loss and enhancing optical transparency. When LaF3 is doped into ABO3 perovskite-structured KNN ceramics, the defect chemical equation is as follows: , cationic La 3+ For A site, anion F - Co-doping at O ​​sites can reduce oxygen vacancy concentration, and the resulting defect pairs can reduce dielectric loss, regulate phase transition temperature, and improve the stability of KNN ceramics.

[0041] A method for preparing a ferroelectric ceramic material with synergistic light transmittance and ferroelectricity includes the following steps:

[0042] S1. Weigh analytically pure sodium carbonate (Na2CO3), potassium carbonate (K2CO3), niobium pentoxide (Nb2O5), and lanthanum fluoride (LaF3) as raw materials according to the stoichiometric ratio of the general chemical formula.

[0043] S2. The raw materials are ball-milled once, dried, and then crushed to obtain a mixed powder.

[0044] The medium for the first ball milling is anhydrous ethanol. The rolling ball milling time in the nylon ball milling jar is 8 to 10 hours. The grinding balls are zirconium balls.

[0045] S3. Pour the mixed powder into a small crucible and pre-fire it to obtain the pre-fired material.

[0046] The pre-firing temperature is 850℃~900℃, and the pre-firing time is 4h~6h.

[0047] S4. The pre-burned material is crushed and then ball-milled in a ball mill jar. The powder is dried and then ground to obtain a secondary mixed powder.

[0048] The medium for secondary ball milling is anhydrous ethanol. The rolling ball milling time in the nylon ball milling jar is 8 to 10 hours, and the grinding balls are zirconium balls.

[0049] S5. Add polyvinyl alcohol aqueous solution to the secondary mixed powder for granulation, dry and grind the granulated powder, and obtain fine powder after sieving.

[0050] The mass concentration of the polyvinyl alcohol aqueous solution is 6wt%~8wt%, preferably 7wt%. After granulation and grinding, it is sieved through a 200-mesh sieve to obtain fine powder and coarse powder.

[0051] S6. The fine powder is pressed into sheets and then debinded to obtain a ceramic body.

[0052] The powder is pressed into round tablets using an electric tablet press. The pressure of the tablet press is 10 MPa, and the glue is discharged at 550°C to fully evaporate and discharge the glue.

[0053] S7. Sinter the ceramic blank to obtain the ceramic body.

[0054] The ceramic blank is buried in sieved coarse powder, and then the crucible is inverted and sealed with zirconium oxide micro powder. It is then placed in a muffle furnace for sintering. The sintering is carried out in two steps: first, sintering at 1100℃~1150℃ for 3h~5h, and then sintering at 1150℃~1180℃ for 3h~5h to obtain ceramic material.

[0055] Example 1

[0056] Using analytically pure Na₂CO₃, K₂CO₃, Nb₂O₅, and LaF₃ as raw materials, according to (K 0.48 Na 0.52 Accurately weigh the stoichiometric amounts of NbO3-0.01 LaF3. Use anhydrous ethanol as the ball milling medium, and then ball mill the raw materials for 10 hours before drying to obtain a mixed dry powder. Hold the resulting dry powder at 900 °C for 4 hours, then add a 7 wt% polyvinyl alcohol aqueous solution to the pre-calcined powder to granulate. After granulation, press the granulated material into small discs with a diameter of 10 mm and a thickness of 1 mm using a 10 mm diameter mold under a pressure of 10 MPa, and remove the binder. Sinter the small discs at 1100 °C~1150 °C for 3-5 hours, then raise the temperature to 1150 °C~1180 °C and sinter for another 3-5 hours. Polish the ceramic discs to a thickness of 0.3 mm to test their optical properties. Apply silver electrodes to the sintered ceramic discs to test their ferroelectric properties.

[0057] Example 2

[0058] The method for preparing the ferroelectric ceramic material in this embodiment is the same as that in Example 1. The difference is that the LaF3 doping amount is 0.02.

[0059] Example 3

[0060] The method for preparing the ferroelectric ceramic material in this embodiment is the same as that in Example 1. The difference is that the LaF3 doping amount is 0.03.

[0061] Example 4

[0062] The method for preparing the ferroelectric ceramic material in this embodiment is the same as that in Example 1. The difference is that the LaF3 doping amount is 0.035.

[0063] Example 5

[0064] The method for preparing the ferroelectric ceramic material in this embodiment is the same as that in Example 1. The difference is that the LaF3 doping amount is 0.04.

[0065] Figure 1 These are the X-ray diffraction patterns of the ferroelectric ceramic materials of Examples 1-5 of this invention. Figure 1 As shown, there are eight characteristic peaks between 20° and 80°, which, in descending order of angle, are: (100), (110), (200), (210), (211), (220), (221), and (310), indicating that the ceramic has a perovskite structure. In Example 1, split peaks appear near 45°-46°, namely (002) and (200) peaks, with an intensity ratio of approximately 2:1, indicating an orthorhombic phase. In contrast, Example 5 shows a single peak near 45°-46°, indicating that the ceramic is a pseudo-cubic phase. This shows that LaF3 doping induces the KNN ceramic to transform into a pseudo-cubic phase. No impurity peaks were observed in any of the examples, indicating that the doped LaF3 entered the matrix to form a solid solution.

[0066] Figure 2 These are the transmittance curves of the ferroelectric ceramic materials in Examples 1-5 of this invention. The addition of an appropriate amount of LaF3 enhances transmittance; in the visible and near-infrared range, Example 4 exhibits the highest transmittance, reaching 70% at 1600 nm.

[0067] Figure 3 This is a schematic diagram showing the relative permittivity of the ferroelectric ceramic materials in Examples 1-5 of the present invention as a function of temperature at 100 kHz. Figure 3 The curves showing the dielectric constant of the ferroelectric ceramic materials shown in Examples 1-5 as a function of temperature are displayed. It can be seen that the relative dielectric constant of Example 1... ε r There are two dielectric anomalous peaks as the temperature changes. The first peak, from low to high temperature, is the dielectric anomalous peak that appears during the transition from the orthorhombic phase to the tetragonal phase. The phase transition temperature measured here is... T O-T Approximately 161℃; the second peak is the dielectric anomalous peak that appears when transitioning from the tetragonal to the cubic phase; the phase transition temperature measured here is the Curie temperature. T C The temperature is 324℃. With increasing LaF3 doping concentration, the two dielectric peaks gradually converge and merge, then begin to broaden, exhibiting strong relaxor ferroelectric properties in the ceramic; simultaneously, the Curie temperature... T C Reduce and T O-T The combination of these elements indicates that the addition of LaF3 promotes the transformation of the phase structure from an orthorhombic phase to a pseudocubic phase, and the crystal structure symmetry of Examples 2-5 gradually increases.

[0068] Figure 4This is a schematic diagram showing the change in dielectric loss of the ferroelectric ceramic materials of Examples 1-5 of the present invention at 100 kHz as a function of temperature. The dielectric loss of Example 1 shows a peak between 200℃ and 300℃, which is related to internal defects caused by the volatilization of K and Na. In Examples 2-5, the peaks gradually flatten and eventually disappear within this temperature range, indicating that LaF3 effectively improves the lattice structure and reduces defects, which helps to reduce light scattering and increase transmittance.

[0069] Figure 5 These are scanning electron microscope images of the ferroelectric ceramic material of Embodiment 4 of the present invention. The LaF3-doped KNN ceramic has fine and dense grains and is almost pore-free.

[0070] Figure 6 These are the hysteresis loops of the ferroelectric ceramic material of Example 4 of this invention under different test electric field conditions. The hysteresis loop of the ceramic sample in Example 4 is generally slender, and gradually becomes larger and more fully polarized as the test electric field strength increases, indicating that PNRs will respond under high electric fields. E =70 At that time, the maximum polarization intensity P m It is 28.93 Residual polarization intensity P r It is 17.45 stubborn field E c is 24.1 .

[0071] Figure 7 The images show the amplitude and phase diagrams of the ferroelectric ceramic material of the present invention obtained by piezoelectric force microscopy (PFM) testing; (a) is the amplitude diagram of the ferroelectric ceramic material of Example 1, (b) is the phase diagram of the ferroelectric ceramic material of Example 1, (c) is the amplitude diagram of the ferroelectric ceramic material of Example 4, and (d) is the phase diagram of the ferroelectric ceramic material of Example 4. With the increase of LaF3 doping concentration, the domain size of the ceramic decreases. In comparison, Example 1 has stray domains of uneven size, ranging from micrometers to hundreds of nanometers, exhibiting a certain polarization response, supporting the ferroelectric properties. P r It is 26.17 The electric domains in Example 4 are mainly nanoscale polar nanoregions (PNRs). Because the size of nanoscale PNRs is much smaller than the wavelength of visible light, they can greatly reduce light scattering loss, which is beneficial for obtaining high optical transmittance. At the same time, the low energy barrier of PNRs makes them very easy to reorient under an external electric field, resulting in good polarization response in the ceramic. P r It is 17.45 Therefore, by adjusting the LaF3 doping amount to induce the formation of PNRs, a synergistic effect of high transparency and good ferroelectric properties was achieved.

[0072] The ferroelectric ceramic materials of Examples 1-5 were tested, and the results are shown in Table 1.

[0073] Table 1. Properties of ferroelectric ceramic materials in Examples 1-5

[0074]

[0075] Therefore, by employing the ferroelectric ceramic material and its preparation method that synergizes transmittance and ferroelectricity as described in this invention, and by introducing LaF3 as a composite dopant, the rare earth cation La... 3+ and anion F - The synergistic effect of these technologies enables the nano-sizing and efficient control of the ferroelectric domain structure of KNN ceramics, thereby significantly improving its optical transmittance while maintaining good ferroelectricity. Furthermore, the process is simple and suitable for industrialization.

[0076] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit them. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can still be made to the technical solutions of the present invention, and these modifications or equivalent substitutions cannot cause the modified technical solutions to deviate from the spirit and scope of the technical solutions of the present invention.

Claims

1. A ferroelectric ceramic material with synergistic light transmittance and ferroelectricity, characterized in that: The general chemical formula is (K 0.48 Na 0.52 NbO3- x LaF3, x Indicates the number of moles of LaF3. x The value ranges from 0.01 to 0.04; LaF3 is used as the dopant source, and the cation La... 3+ Entering the A site of the perovskite structure, F - The O sites are incorporated into the perovskite structure; nanoscale polar microregions PNRs are uniformly distributed inside the ceramic material, and these polar microregions PNRs are easily flipped under an external electric field.

2. The ferroelectric ceramic material with synergistic light transmittance and ferroelectricity according to claim 1, characterized in that: The x The value is 0.

035.

3. A method for preparing a ferroelectric ceramic material with synergistic light transmittance and ferroelectricity according to claim 1 or 2, characterized in that, Includes the following steps: S1. Weigh analytical grade sodium carbonate (Na2CO3), potassium carbonate (K2CO3), niobium pentoxide (Nb2O5), and lanthanum fluoride (LaF3) as raw materials according to the stoichiometric ratio of the general chemical formula. S2. The raw materials are ball-milled once, dried, and then crushed to obtain a mixed powder. S3. Pour the mixed powder into a small crucible and pre-fire it to obtain the pre-fired material; S4. The pre-burned material is crushed and then ball-milled in a ball mill jar. The powder is dried and then ground to obtain a secondary mixed powder. S5. Add polyvinyl alcohol aqueous solution to the secondary mixed powder for granulation, dry and grind the granulated powder, and obtain fine powder after sieving. S6. The fine powder is pressed into sheets and debinded in sequence to obtain a ceramic body; S7. Sinter the ceramic blank to obtain a ceramic body; S8. A silver electrode is plated onto the ceramic body, and a voltage is applied to polarize it to obtain the ceramic material.

4. The method for preparing a ferroelectric ceramic material with synergistic light transmittance and ferroelectricity according to claim 3, characterized in that: In S2 and S4, the medium for the first and second ball milling is anhydrous ethanol. The rolling ball milling time for the first ball milling in the nylon ball milling jar is 8h~10h, and the ball milling time for the second ball milling is 8h~10h. The grinding balls are zirconium balls.

5. The method for preparing a ferroelectric ceramic material with synergistic light transmittance and ferroelectricity according to claim 3, characterized in that: In S3, the pre-firing temperature is 850℃~900℃, and the pre-firing time is 4h~6h.

6. The method for preparing a ferroelectric ceramic material with synergistic light transmittance and ferroelectricity according to claim 3, characterized in that: In step S5, the mass concentration of the polyvinyl alcohol aqueous solution is 6wt%~8wt%, and after granulation and grinding, it is sieved through a 200-mesh sieve.

7. The method for preparing a ferroelectric ceramic material with synergistic light transmittance and ferroelectricity according to claim 3, characterized in that: In step S6, the tableting pressure is 8MPa~10MPa, and the glue is discharged at 550℃.

8. The method for preparing a ferroelectric ceramic material with synergistic light transmittance and ferroelectricity according to claim 3, characterized in that: In step S7, the ceramic blank is buried in sieved coarse powder, and the crucible is inverted. The crucible is sealed with zirconium oxide micro powder and placed in a muffle furnace for sintering. The sintering is carried out in two steps: first, sintering at 1100℃~1150℃ for 3h~5h, and then sintering at 1150℃~1180℃ for 3h~5h.

9. The method for preparing a ferroelectric ceramic material with synergistic light transmittance and ferroelectricity according to claim 3, characterized in that: The prepared ceramic material achieved an optical transmittance of 70% at 1600 nm in the near-infrared region, with a remanent polarization intensity of [missing information]. for

Citation Information

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