A preparation method of dielectric energy storage capacitor and dielectric energy storage capacitor

By preparing Bi3.25La0.75Ti3O12 ceramic thin film materials, the environmental pollution and human harm problems of lead-based dielectric energy storage capacitors are solved, the energy storage performance and breakdown field strength of dielectric energy storage capacitors are improved, and the application of lead-free material systems is realized.

CN116313514BActive Publication Date: 2025-09-16SHENZHEN INST OF ADVANCED TECH CHINESE ACAD OF SCI
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Patent Information

Application Number
CN202310195649.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-02-21
Publication Date
2025-09-16
Estimated Expiration
2043-02-21

AI Technical Summary

Technical Problem

Existing dielectric energy storage capacitors are mostly made of lead-based materials, which pose serious environmental pollution and harm to the human body. At the same time, their large residual polarization value and low breakdown field strength limit their application in the energy storage field.

Method used

Bi3.25La0.75Ti3O12 ceramic thin film material was used to prepare a Bi3.25La0.75Ti3O12 ceramic thin film precursor solution, which was spin-coated and annealed in air atmosphere. Combined with metal electrode deposition, a lead-free material system dielectric energy storage capacitor was prepared.

Benefits of technology

It reduces the residual polarization value, improves the breakdown field strength, obtains excellent energy storage density and energy storage efficiency, reduces environmental pollution and human harm, and expands the scope of application.

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Abstract

The preparation method of the dielectric energy storage capacitor and the dielectric energy storage capacitor provided in this application are prepared by 3.25 La 0.75 TiO 12 Ceramic thin film precursor solution, preparation of Bi 3.25 La 0.75 TiO 12 Ceramic thin film, depositing metal electrodes onto the Bi 3.25 La 0.75 TiO 12 The dielectric energy storage capacitor is obtained on the ceramic film. The preparation method of the dielectric energy storage capacitor adopts a lead-free material system, which reduces the pollution to the environment and the harm to the human body, expands the application of the system in the field of energy storage, and has a simple process. And by regulating the annealing process, the Bi 3.25 La 0.75 TiO 12 The synergistic effect of the preferential orientation and interface engineering achieves reduced residual polarization while improving the breakdown field strength, resulting in excellent energy storage density and efficiency.
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Description

Technical Field

[0001] The present application relates to the field of energy storage technology, and in particular to a method for preparing a dielectric energy storage capacitor and a dielectric energy storage capacitor. Background Art

[0002] Dielectric capacitors have extremely fast charge and discharge rates and ultra-high power density. They are an important type of power energy storage device and have good application prospects in the civilian and military fields. Traditional dielectric energy storage capacitors are mostly lead-based materials, which are harmful to the human body and the environment. 3.25 La 0.75 TiO 12 As a lead-free material, it has a large polarization value and good temperature stability and cycle stability, which determines its good application value in the field of energy storage. However, its large residual polarization value and low breakdown field strength limit its application in the field of energy storage. Therefore, reducing its residual polarization value and enhancing its breakdown field strength are crucial for realizing its application in the field of energy storage and obtaining Bi with good energy storage performance. 3.25 La 0.75 TiO 12 Capacitors are beneficial. Existing dielectric energy storage materials are mostly lead-based materials, which are toxic and cause serious environmental pollution and are harmful to the human body. Summary of the Invention

[0003] In view of this, it is necessary to provide a method for preparing a dielectric energy storage capacitor and a dielectric energy storage capacitor with better energy storage performance, less environmental pollution and less harm to the human body in order to address the defects in the prior art.

[0004] To solve the above problems, this application adopts the following technical solutions:

[0005] One of the purposes of this application is to provide a method for preparing a dielectric energy storage capacitor, comprising the following steps:

[0006] Preparation of Bi 3.25 La 0.75 TiO 12 Ceramic thin film precursor solution;

[0007] Preparation of Bi 3.25 La 0.75 TiO 12 Ceramic thin films;

[0008] Depositing metal electrodes onto the Bi 3.25 La 0.75 TiO 12 On the ceramic film, the dielectric energy storage capacitor is obtained.

[0009] In some of the embodiments, in the preparation of Bi 3.25 La 0.75 TiO 12 The steps of preparing the ceramic thin film precursor solution specifically include the following steps:

[0010] According to Bi 3.25 La 0.75 TiO 12 The stoichiometric ratio is selected, bismuth acetate, lanthanum acetate, tetrabutyl titanate are selected as raw materials, propionic acid is used as solvent, ethanolamine is used as viscosity regulator, and Bi is prepared with a concentration of 0.02-0.15 mol / L. 3.25 La 0.75 TiO 12 The ceramic film precursor solution comprises 2-8 mol% excess bismuth acetate and a volume ratio of propionic acid to ethanolamine of 9:1-39:1.

[0011] In some of the embodiments, in the preparation of Bi 3.25 La 0.75 TiO 12 The steps of forming a ceramic film specifically include the following steps:

[0012] The Bi 3.25 La 0.75 TiO 12 The ceramic thin film precursor solution is spin-coated onto the substrate and dried at 300-500°C;

[0013] The dried Bi 3.25 La 0.75 TiO 12 The substrate of the ceramic thin film precursor solution is annealed in an air atmosphere;

[0014] Repeat the above steps until the target spin coating times are reached to obtain the Bi 3.25 La 0.75 TiO 12 Ceramic film.

[0015] In some embodiments, the Bi 3.25 La 0.75 TiO 12 The ceramic thin film precursor solution is spin-coated onto a substrate and dried at 300-500° C. The spin-coating speed is 3000-8000 rpm and the drying time is 10-40 seconds. The substrate is a platinum-coated silicon wafer.

[0016] In some embodiments, the dried Bi-coated 3.25 La 0.75 TiO 12In the step of annealing the substrate of the ceramic thin film precursor solution in an air atmosphere, the annealing temperature is 600-750° C. and the annealing time is 3-30 minutes.

[0017] In some embodiments, the Bi 3.25 La 0.75 TiO 12 Before the ceramic thin film precursor solution is spin-coated onto the substrate, the method further includes a step of cleaning the substrate, wherein the cleaning includes a step of wiping the substrate with an organic solvent.

[0018] In some embodiments, before depositing the metal electrode onto the Bi 3.25 La 0.75 TiO 12 The step of obtaining the dielectric energy storage capacitor on the ceramic film specifically includes the following steps:

[0019] A mask with small holes is covered on the Bi 3.25 La 0.75 TiO 12 The metal electrode is then deposited onto the Bi by magnetron sputtering. 3.25 La 0.75 TiO 12 The dielectric energy storage capacitor is prepared on the ceramic film.

[0020] The second purpose of this application is to provide a dielectric energy storage capacitor, which is prepared by the preparation method of the dielectric energy storage capacitor.

[0021] This application adopts the above technical solution, and its beneficial effects are as follows:

[0022] The preparation method of the dielectric energy storage capacitor and the dielectric energy storage capacitor provided in this application are prepared by 3.25 La 0.75 TiO 12 Ceramic thin film precursor solution, preparation of Bi 3.25 La 0.75 TiO 12 Ceramic thin film, depositing metal electrodes onto the Bi 3.25 La 0.75 TiO 12 The dielectric energy storage capacitor is obtained on the ceramic film. The preparation method of the dielectric energy storage capacitor adopts a lead-free material system, which reduces pollution to the environment and harm to the human body, expands the application of the system in the energy storage field, and has a simple process.

[0023] The preparation method of the dielectric energy storage capacitor provided in this application rationally utilizes Bi by regulating the annealing process. 3.25La 0.75 TiO 12 The synergistic effect of the preferential orientation and interface engineering not only reduces the residual polarization value but also improves the breakdown field strength, thus obtaining excellent energy storage density and efficiency. Under an external electric field of 3451.37 kV / cm, 62.97 J / cm 3 The energy storage density is increased while maintaining an energy storage efficiency of 85.88%, and the energy storage performance of the capacitor is significantly improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the following briefly introduces the drawings required for use in the embodiments of the present application or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without any creative work.

[0025] Figure 1 Bi provided in the embodiment of this application 3.25 La 0.75 TiO 12 Schematic diagram of the thin film material structure.

[0026] Figure 2 Bi obtained in different embodiments 3.25 La 0.75 TiO 12 XRD patterns of thin film materials.

[0027] Figure 3 Bi obtained in different embodiments 3.25 La 0.75 TiO 12 Dielectric properties of thin film materials.

[0028] Figure 4 Bi obtained in different embodiments 3.25 La 0.75 TiO 12 Leakage current characteristics of thin film materials.

[0029] Figure 5 Bi obtained in different embodiments 3.25 La 0.75 TiO 12 Weibull distribution of the breakdown field strength of thin film materials.

[0030] Figure 6 Bi obtained in different embodiments 3.25 La 0.75 TiO 12 (a) Hysteresis loop (b) polarization value (c) energy storage performance of thin film materials at maximum electric field strength.

[0031] Figure 7 The Bi obtained in Example 2 at 2212 kV / cm 3.25 La 0.75 TiO 12 (a) PE hysteresis loops of thin film materials at different frequencies and their corresponding (b) polarization values, (c) energy storage characteristics; (d) PE hysteresis loops at different temperatures and their corresponding (e) polarization values, (f) energy storage characteristics. DETAILED DESCRIPTION

[0032] The following describes in detail embodiments of the present application, examples of which are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements having the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are intended to be used to explain the present application, and should not be construed as limiting the present application.

[0033] In the description of this application, it should be understood that the terms "upper", "lower", "horizontal", "inside", "outside", etc., indicating orientations or positional relationships, are based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing this application and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on this application.

[0034] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of the technical features being referred to. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the features. Throughout the description of this application, "plurality" means two or more, unless otherwise specifically defined.

[0035] In order to make the purpose, technical solutions and advantages of this application more clear, this application is further described in detail below with reference to the accompanying drawings and embodiments.

[0036] The present application provides a method for preparing a dielectric energy storage capacitor, including the following steps S110 to S130. The implementation of each step is described in detail below.

[0037] Step S110: Preparation of Bi 3.25 La 0.75 TiO 12 Ceramic thin film precursor solution.

[0038] In this embodiment, when preparing Bi 3.25 La 0.75 TiO 12The steps of preparing the ceramic thin film precursor solution specifically include the following steps:

[0039] According to Bi 3.25 La 0.75 TiO 12 The stoichiometric ratio is selected, bismuth acetate, lanthanum acetate, tetrabutyl titanate are selected as raw materials, propionic acid is used as solvent, ethanolamine is used as viscosity regulator, and Bi is prepared with a concentration of 0.02-0.15 mol / L. 3.25 La 0.75 TiO 12 The ceramic film precursor solution comprises 2-8 mol% excess bismuth acetate and a volume ratio of propionic acid to ethanolamine of 9:1-39:1.

[0040] Specifically, a container containing propionic acid was placed on a hot plate at 80°C, and then bismuth acetate, lanthanum acetate, and tetrabutyl titanate were added in sequence. When stirred until completely dissolved, a certain amount of ethanolamine was added to stabilize the colloid. The precursor solution was then stirred at room temperature for 2 days, and then the precursor solution was allowed to stand for 3 days for use.

[0041] Step S120: Preparation of Bi 3.25 La 0.75 TiO 12 Ceramic film.

[0042] In this embodiment, when preparing Bi 3.25 La 0.75 TiO 12 The steps of forming the ceramic film specifically include the following steps S121 to S123, and the implementation method of each step is described in detail below.

[0043] Step S121: Bi 3.25 La 0.75 TiO 12 The ceramic thin film precursor solution is spin-coated onto the substrate and dried at 300-500°C.

[0044] In this embodiment, the spin coating speed is 3000-8000 rpm, and the time is 10-40 s; and the substrate is a platinum-coated silicon wafer.

[0045] It can be understood that at this rotation speed, the precursor solution is easier to spread evenly, making the formed film thin and uniform, reducing the surface roughness of the ceramic film, improving the uniformity of the film, and helping to improve the energy storage properties of the ceramic film.

[0046] Step S122: drying the coated 3.25 La 0.75 TiO 12 The substrate of the ceramic thin film precursor solution is annealed in an air atmosphere.

[0047] In this embodiment, the annealing temperature is 600-750° C., and the annealing time is 3-30 minutes.

[0048] It can be understood that by carrying out crystallization under this annealing condition, a ceramic film with good crystallinity and fewer internal defects can be obtained, thereby obtaining a ceramic film with excellent energy storage performance.

[0049] Step S123: Repeat the above steps according to the set process until the target spin coating times are reached to obtain the Bi 3.25 La 0.75 TiO 12 Ceramic film.

[0050] It can be understood that the present invention prepares Bi with different preferred orientations by gradual annealing or one-step annealing. 3.25 La 0.75 TiO 12 The thin film material achieved a reduced residual polarization value; by gradual annealing and one-step annealing in Bi 3.25 La 0.75 TiO 12 The interface is formed inside the thin film material, and the development of the electron tree is hindered by the interface, thereby achieving enhanced breakdown field strength; the synergistic effect of preferential orientation and interface engineering is used to achieve Bi 3.25 La 0.75 TiO 12 The application of thin film materials in the field of energy storage has high energy storage efficiency while having high energy storage density.

[0051] In this embodiment, the Bi 3.25 La 0.75 TiO 12 Before the ceramic thin film precursor solution is spin-coated onto the substrate, the method further includes a step of cleaning the substrate, wherein the cleaning includes a step of wiping the substrate with an organic solvent.

[0052] Step S130: Depositing a metal electrode onto the Bi 3.25 La 0.75 TiO 12 On the ceramic film, the dielectric energy storage capacitor is obtained.

[0053] In this embodiment, the metal electrode is deposited onto the Bi 3.25 La 0.75 TiO 12 The step of obtaining the dielectric energy storage capacitor on the ceramic film specifically includes the following steps: covering the Bi 3.25 La 0.75 TiO12 The metal electrode is then deposited onto the Bi by magnetron sputtering. 3.25 La 0.75 TiO 12 The dielectric energy storage capacitor is prepared on the ceramic film.

[0054] The preparation method of the dielectric energy storage capacitor provided in the above embodiment of the present application adopts a lead-free material system, which reduces pollution to the environment and harm to the human body, expands the application of the system in the field of energy storage, and has a simple process.

[0055] The preparation method of the dielectric energy storage capacitor provided in the above embodiment of the present application reasonably utilizes Bi by regulating the annealing process. 3.25 La 0.75 TiO 12 The synergistic effect of the preferential orientation and interface engineering not only reduces the residual polarization value but also improves the breakdown field strength, thus obtaining excellent energy storage density and efficiency. Under an external electric field of 3451.37 kV / cm, 62.97 J / cm 3 The energy storage density is increased while maintaining an energy storage efficiency of 85.88%, and the energy storage performance of the capacitor is significantly improved.

[0056] The above technical solutions of the present application are described in detail below in conjunction with specific embodiments.

[0057] Example 1: Obtaining Bi 3.25 La 0.75 TiO 12 The precursor solution was spin-coated on a platinum-coated silicon wafer and then pyrolyzed on a 400°C hot plate for 5 minutes, followed by annealing at 700°C for 5 minutes. After annealing, the spin-coating-pyrolysis-annealing process was repeated until annealing was repeated 6 times to obtain Bi 3.25 La 0.75 TiO 12 The film material is formed and an electrode is deposited on the top to obtain a dielectric capacitor. The dielectric capacitor obtained in Example 1 is named 1-6 (see Figure 1 ).

[0058] Example 2: Obtaining Bi 3.25 La 0.75 TiO 12 The precursor solution was spin-coated on a platinum-coated silicon wafer and then pyrolyzed on a 400°C hot plate for 5 minutes. The solution was then spin-coated. After the second spin-coating, the solution was baked on a 400°C hot plate for 5 minutes. The solution was then annealed at 700°C for 5 minutes. The above steps were repeated 3 times for a total of 3 annealings to obtain Bi 3.25 La 0.75 TiO 12The film material is formed and an electrode is deposited on the top to obtain a dielectric capacitor. The dielectric capacitor obtained in Example 2 is named 2-6 (see Figure 1 ).

[0059] Example 3: Obtaining Bi 3.25 La 0.75 TiO 12 The precursor solution was spin-coated on a platinum-coated silicon wafer and then baked on a hot plate at 400°C for 5 minutes. The dried sample was then spin-coated and pyrolyzed for a total of 3 times. It was then annealed at 700°C for 5 minutes. The above steps were repeated once for a total of 2 annealing times to obtain Bi 3.25 La 0.75 TiO 12 The film material is formed and an electrode is deposited on the top to obtain a dielectric capacitor. The dielectric capacitor obtained in Example 3 is named 3-6 (see Figure 1 ).

[0060] Example 4: Obtaining Bi 3.25 La 0.75 TiO 12 The precursor solution was spin-coated on a platinum-coated silicon wafer and then baked on a 400°C hot plate for 5 minutes. The dried sample was then spin-coated and pyrolyzed for a total of 6 times, and then annealed at 700°C for 5 minutes, for a total of 1 annealing, to obtain Bi 3.25 La 0.75 TiO 12 The film material is formed and an electrode is deposited on the top to obtain a dielectric capacitor. The dielectric capacitor obtained in Example 4 is named 6-6 (see Figure 1 ).

[0061] See also Figure 2 , represents Bi obtained from the above different embodiments 3.25 La 0.75 TiO 12 XRD patterns of thin film materials.

[0062] Understandable, combined Figure 2 It can be seen that the above examples of this application all exhibit good crystallinity and have a typical mixed crystal structure with a-, c-, and (117) preferred orientations. The preferred orientation degrees of different examples were calculated based on the XRD patterns, and the results are shown in Table 1.

[0063] Please refer to Table 1 below, which shows the Bi obtained for different embodiments. 3.25 La 0.75 TiO 12 The number of interfaces, thickness and orientation of thin film materials.

[0064] name Number of interfaces Thickness (nm) Monolayer thickness (nm) α006 α117 α200 1-6 5 230 38.33 0.30 0.23 0.47 2-6 2 225 75.00 0.32 0.38 0.30 3-6 1 230 115.00 0.24 0.57 0.19 6-6 0 200 200 0.08 0.71 0.21

[0065] Orientation calculation formula:

[0066]

[0067]

[0068]

[0069] From the above table, it can be seen that the c-axis preferred orientation degrees of Examples 1-6, 2-6, 3-6 and 6-6 are 0.30, 0.32, 0.24 and 0.08, respectively, among which 2-6 has the highest c-axis orientation degree, and the c-axis oriented BLT film has the smallest residual polarization, which indicates that the 2-6 film may have excellent energy storage performance.

[0070] See also Figure 3 , are Bi obtained in different embodiments 3.25 La 0.75 TiO 12 Dielectric properties of thin film materials.

[0071] Combine Figure 3 It can be seen that the above embodiments all have moderate dielectric constants and low dielectric loss. Among them, at 1kHz, the dielectric constants and dielectric losses of 1-6, 2-6, 3-6 and 6-6 are 273, 201, 234, 219 and 0.04196, 0.01554, 0.02058, 0.02791 respectively. Among them, 2-6 has the lowest dielectric constant. The lower dielectric constant is beneficial for improving the breakdown field strength, and it has the lowest dielectric loss, which means smaller leakage current and energy loss, which is beneficial for improving the energy storage density and energy storage efficiency of the material.

[0072] See also Figure 4 , are Bi obtained in different embodiments 3.25 La 0.75 TiO 12 Leakage current characteristics of thin film materials.

[0073] Combine Figure 4 It can be seen that the above embodiments of the present application all have relatively low leakage current density. Among them, 2-6 achieves an extremely low leakage current density, which is only 3.08× at 428kV / cm.

[0074] 10 -9 A / cm 2 , a smaller leakage current density can ensure the reliability of the device operation, and a smaller leakage current density is beneficial to the improvement of the breakdown field strength, and has better energy storage performance.

[0075] See also Figure 5 , are Bi obtained in different embodiments 3.25 La 0.75 TiO 12 Weibull distribution of the breakdown field strength of thin film materials.

[0076] Combine Figure 5 It can be seen that the breakdown field strength of the film was analyzed using the two-parameter Weibull distribution. The results show that E B The value is 3232.72 kV / cm, indicating that 2-6 has a strong breakdown field strength, and its β value is 13.03, indicating that the fitted E B The values ​​have good reliability and the sample uniformity is good.

[0077] See also Figure 6 , are Bi obtained in different embodiments 3.25 La 0.75 TiO 12 (a) Hysteresis loop (b) polarization value (c) energy storage performance of thin film materials at maximum electric field strength.

[0078] Combine Figure 6 It can be seen that 2-6 has the largest P max (51.38μC / cm 2 ) while having the smallest P r (6.30μC / cm 2 ), which is consistent with the P of 1-6, 3-6 and 6-6 max (43.61, 41.18, 35.62 μC / cm 2 ) and Pr (7.35, 8.70, 7.56 μC / cm 2 ) compared to the max and reduced P r , and 2-6 has the largest ΔP (45.08μC / cm 2 ) This is beneficial to the improvement of energy storage density and efficiency. The results show that 62.97 J / cm 3 The energy storage density is 2.33 % while maintaining an energy storage efficiency of 85.88%. This shows that the energy storage properties of the material can be effectively improved through the synergistic effect of preferential orientation and interface engineering.

[0079] See also Figure 7 , expressed as Bi obtained in Example 2 at 2212 kV / cm 3.25 La 0.75 TiO 12(a) PE hysteresis loops of thin film materials at different frequencies and their corresponding (b) polarization values ​​and (c) energy storage characteristics; (d) PE hysteresis loops at different temperatures and their corresponding (e) polarization values ​​and (f) energy storage characteristics.

[0080] Combine Figure 7 It can be seen that (ac) in the range of 100Hz to 10kHz, with the increase of frequency, the PE curve has no obvious change and remains thin. max and P r There is a slight decrease, but ΔP is almost stable, and the corresponding energy storage density is between 30.14 and 32.61 J / cm 3 The energy storage efficiency remains above 79.27% ​​and the energy storage density changes by 7.57%, indicating good frequency stability. (df) When the applied electric field is 2212 kV / cm, the PE curve of 2-6 in the temperature range of 25℃-150℃ has an energy storage density of 30.50 J / cm 3 Up to 32.00J / cm 3 The energy storage efficiency remained above 76.97%, and the energy storage density varied by only 4.69%, demonstrating good temperature stability. This indicates that 2-6 can be used in multiple application scenarios and maintain good performance.

[0081] The above description is only a preferred embodiment of the present invention. All equivalent changes and modifications made according to the scope of the patent application of the present invention should fall within the scope of the present invention.

[0082] It can be understood that the various technical features of the above-described embodiments can be combined arbitrarily. In order to make the description concise, not all possible combinations of the various technical features in the above-described embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0083] The above are merely preferred embodiments of the present application and only specifically describe the technical principles of the present application. These descriptions are intended only to explain the principles of the present application and should not be construed in any way as limiting the scope of protection of the present application. Based on the explanations herein, any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present application, as well as other specific implementations of the present application that can be conceived by those skilled in the art without inventive effort, shall be included within the scope of protection of the present application.

Claims

1. A method for preparing a dielectric energy storage capacitor, characterized in that: The steps include: Preparation of Bi 3.25 La 0.75 TiO 12 Ceramic thin film precursor solution; Preparation of Bi 3.25 La 0.75 TiO 12 Ceramic thin films; Depositing metal electrodes onto the Bi 3.25 La 0.75 TiO 12 On the ceramic film, the dielectric energy storage capacitor is obtained; In the preparation of Bi 3.25 La 0.75 TiO 12 The steps of preparing the ceramic thin film precursor solution specifically include the following steps: According to Bi 3.25 La 0.75 TiO 12 The stoichiometric ratio is selected, bismuth acetate, lanthanum acetate, tetrabutyl titanate are selected as raw materials, propionic acid is used as solvent, ethanolamine is used as viscosity regulator, and Bi is prepared with a concentration of 0.02-0.15 mol / L. 3.25 La 0.75 TiO 12 A ceramic thin film precursor solution, wherein bismuth acetate is in excess of 2-8 mol%, and the volume ratio of propionic acid to ethanolamine is 9:1-39:1; In the preparation of Bi 3.25 La 0.75 TiO 12 The steps of forming a ceramic film specifically include the following steps: Take Bi 3.25 La 0.75 TiO 12 The precursor solution was spin-coated on a platinum-coated silicon wafer and then pyrolyzed on a 400°C hot plate for 5 minutes. The solution was then spin-coated. After the second spin-coating, the solution was baked on a 400°C hot plate for 5 minutes. The solution was then annealed at 700°C for 5 minutes. The above steps were repeated 3 times for a total of 3 annealings to obtain Bi 3.25 La 0.75 TiO 12 Thin film materials.

2. The method for preparing a dielectric energy storage capacitor according to claim 1, wherein: The Bi 3.25 La 0.75 TiO 12 The ceramic thin film precursor solution is spin-coated onto the substrate and dried at 400° C. The spin-coating speed is 3000-8000 rpm and the drying time is 10-40 seconds.

3. The method for preparing a dielectric energy storage capacitor according to claim 1, wherein: In the Bi 3.25 La 0.75 TiO 12 Before the ceramic thin film precursor solution is spin-coated onto the substrate, the method further includes a step of cleaning the substrate, wherein the cleaning includes a step of wiping the substrate with an organic solvent.

4. The method for preparing a dielectric energy storage capacitor according to claim 1, wherein: In depositing the metal electrode onto the Bi 3.25 La 0.75 TiO 12 The step of obtaining the dielectric energy storage capacitor on the ceramic film specifically includes the following steps: A mask with small holes is covered on the Bi 3.25 La 0.75 TiO 12 The metal electrode is then deposited onto the Bi by magnetron sputtering. 3.25 La 0.75 TiO 12 The dielectric energy storage capacitor is prepared on the ceramic film.

5. A dielectric energy storage capacitor, characterized in that: The dielectric energy storage capacitor is prepared by the preparation method according to any one of claims 1 to 4.

Citation Information

Patent Citations

  • Lanthanide-doped bismuth titanate film and preparation method thereof

    CN101811889A

  • Ceramic film precursor, preparation method thereof and dielectric energy storage capacitor

    CN115215652A