Method for preparing flaky PbTiO3 template

The three-step molten salt method was used to prepare the flaky PbTiO3 template, which solved the problem of difficulty in producing pure flaky PbTiO3 templates, achieved the stability and high performance of lead-based textured ceramics, and expanded the application range of lead-based piezoelectric ceramics.

CN120774455APending Publication Date: 2025-10-14GUIZHOU NORMAL UNIVERSITY
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Patent Information

Application Number
CN202510957811.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-07-11
Publication Date
2025-10-14

AI Technical Summary

Technical Problem

In the existing technology, the production of pure flake PbTiO3 templates is difficult, which limits the development of lead-based textured ceramics, and traditional templates are unstable in lead-based piezoelectric ceramics.

Method used

A three-step molten salt method is used to prepare flaky Bi4Ti3O12 by reacting TiO2 with Bi2O3, which is then reacted with PbO and TiO2 to form a PbBi4Ti4O15 precursor. Finally, a flaky PbTiO3 template is prepared by reacting with PbO. The integrity and stability of the crystal structure are ensured by controlling the temperature and time of each step.

Benefits of technology

A stable flake PbTiO3 template was successfully prepared for the directional growth of lead-based grains to form textured lead-based piezoelectric ceramics, which solves the shortcomings of traditional methods, expands the options for texturing lead-based piezoelectric ceramics, and has high economic and social value.

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Abstract

The invention discloses a method for preparing a flaky PbTiO3 template, and relates to the technical field of PbTiO3 preparation, and the method comprises the following steps: preparing pure flaky Bi4Ti3O12, preparing a flaky PbBi4Ti4O15 precursor, preparing flaky PbTiO3, and preparing the pure flaky PbTiO3 template. According to the preparation method, flaky Bi4Ti3O12 is prepared from TiO2 and Bi2O3, flaky PbBi4Ti4O15 is prepared from the flaky Bi4Ti3O12, PbO and TiO2, flaky PbTiO3 is prepared from PbBi4Ti4O15 and PbO, a PbTiO3 template with a complete and stable flaky crystal structure is prepared based on a three-step molten salt method, the PbTiO3 template does not react with a matrix at high temperature, lead-based crystal grains are induced by the flaky PbTiO3 template to form oriented growth, and the textured lead-based piezoelectric ceramic is successfully formed. And the shortages existing in the traditional method are solved.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of PbTiO3 preparation, and particularly relates to a method for preparing a PbTiO3 template in a sheet shape. BACKGROUND

[0002] In the past 20 years, ferroelectric single crystal materials have been widely concerned due to their excellent piezoelectric properties. However, the high production cost and the inhomogeneity of composition limit the application of single crystal materials. In recent years, textured ceramics have attracted extensive attention due to the development of high-performance piezoelectric materials. By controlling the orientation of textured grains, the piezoelectric properties of textured ceramics can be comparable to those of single crystal ceramics. Unlike randomly oriented polycrystalline ceramics, a directional template is introduced into the ceramic to guide the directional growth of ceramic grains. Due to the directional arrangement of these templates, all the grains in the textured ceramic have a nearly uniform crystallographic direction.

[0003] To date, BaTiO3, SrTiO3, (Na 1 / 2 Bi 1 / 2 )TiO3-PbTiO3, etc. particles have been used as templates for textured ceramics. In particular, sheet-shaped BaTiO3 is one of the most widely used templates in the template grain growth (TGG) process. With BaTiO3 as the template, a high texture degree of more than 95% can be achieved. However, the heterogeneous template will also act as an impurity in the lead-based system, which may hinder the inherent piezoelectric contribution. In the process of guiding the directional growth of ceramic matrix grains, PbTiO3 (lead titanate) grains can be well matched with lead-based ceramics. However, there are few reports on PbTiO3 samples as template materials. Due to the crystal anisotropy, the production of pure PbTiO3 templates is very difficult. In summary, the lack of pure sheet-shaped PbTiO3 template materials hinders the development of lead-based textured ceramics. Therefore, the present application proposes a method for preparing a sheet-shaped PbTiO3 template to solve the problems in the prior art. SUMMARY

[0004] In view of the above problems, the purpose of the present application is to propose a method for preparing a sheet-shaped PbTiO3 template, which uses a three-step molten salt method to prepare a sheet-shaped PbTiO3, not only solving the instability of traditional sheet-shaped PbTiO3 templates in lead-based piezoelectric ceramics, but also providing a new idea for the texturing of lead-based piezoelectric ceramics.

[0005] In order to achieve the purpose of the present application, the present application realizes the following technical scheme: a method for preparing a sheet-shaped PbTiO3 template, comprising the following steps:

[0006] Step 1: Under molten salt conditions, TiO2 and Bi2O3 are mixed in a preset ratio, and then ball-milled to obtain a slurry. After drying the slurry, the slurry is reacted at a preset temperature. The reaction product is washed with molten salt to prepare pure flake Bi4Ti3O 12 ;

[0007] Step 2: Under molten salt conditions, use magnetic stirring to mix the flake Bi4Ti3O 12 , PbO and TiO2 are mixed in a preset ratio, ball-milled to obtain a slurry, dried and reacted at a preset temperature, and the reaction product is washed with molten salt to prepare a flake PbBi4Ti4O 15 Precursor;

[0008] Step 3: Under molten salt conditions, use magnetic stirring to mix the flake PbBi4Ti4O 15 The precursor and PbO are mixed in a preset ratio, ball-milled to obtain a slurry, dried, and reacted at a preset temperature. The reaction product is washed with molten salt to prepare flake PbTiO3.

[0009] Step 4: Add acid solution to the flaky PbTiO3 to clean Bi2O3, then add deionized water to wash and remove the molten salt, filter and dry to obtain a pure flaky PbTiO3 template.

[0010] Further improvements are: in the step 1, the TiO2 and Bi2O3 are mixed under NaCl-KCl molten salt conditions, the ball milling medium after mixing is anhydrous ethanol, the ball milling time is 12 hours, and the mixing mass ratio of the TiO2, Bi2O3 and NaCl-KCl molten salt is 3:2:5.

[0011] A further improvement is that in step 1, the TiO2 and Bi2O3 are mixed and reacted at a temperature of 950 to 1150°C for 1 to 6 hours, and the reaction product is washed with molten salt using deionized water at 70°C.

[0012] A further improvement is that in the step 2, the flaky Bi4Ti3O 12 and PbO in NaCl-KCl molten salt conditions, the mixed ball milling medium is anhydrous ethanol, the ball milling time is 12h, the flaky Bi4Ti3O 12 , PbO, TiO2 and NaCl-KCl molten salt have a mixing mass ratio of 1:1:1:1.

[0013] A further improvement is that in the step 2, the flaky Bi4Ti3O 12 The reaction is carried out with PbO under magnetic stirring for 1 to 6 hours at a temperature of 800 to 1000° C. for 1 to 6 hours. The reaction product is washed with molten salt using deionized water at 70° C.

[0014] A further improvement is that in step 3, the flaky PbBi4Ti4O 15 The precursor and PbO are mixed under NaCl-KCl molten salt conditions, the mixed ball milling medium is anhydrous ethanol, the ball milling time is 12h, the flaky PbBi4Ti4O 15 The mixing mass ratio of the precursor, PbO and NaCl-KCl molten salt is 1:3.5:1.

[0015] A further improvement is that in step 3, the flaky PbBi4Ti4O 15 The precursor and PbO are stirred magnetically for 1 to 6 hours and reacted at a temperature of 800 to 1050° C. for 1 to 6 hours. The reaction product is washed with 70° C. deionized water to remove the molten salt.

[0016] A further improvement is that in step 4, the acid solution is dilute nitric acid with a concentration of 2 mol / L, the temperature of the deionized water is 70°C, and the flaky PbTiO3 is washed and filtered and then dried at a temperature of 60°C.

[0017] The beneficial effects of the present invention are as follows: the present invention prepares flaky Bi4Ti3O by TiO2 and Bi2O3 12 , through the flake Bi4Ti3O 12 PbBi4Ti4O flakes were prepared by mixing with PbO and TiO2 15 , through PbBi4Ti4O 15 Flake PbTiO3 was prepared with PbO, and a PbTiO3 template with complete and stable flake crystal structure was prepared based on the three-step molten salt method. It did not react with the matrix at high temperature, and the flake PbTiO3 template was used to induce directional growth of lead-based grains, successfully forming textured lead-based piezoelectric ceramics. This solves the shortcomings of traditional methods and expands the choice of textured templates for lead-based piezoelectric ceramics, and has high economic and social value. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 1 is a schematic flow chart of a method for preparing a flaky PbTiO3 template according to the present invention;

[0019] Figure 2 The pure flaky Bi4Ti3O in Example 1 of the present invention 12 Schematic diagram of the flake microstructure;

[0020] Figure 3 The flaky PbBi4Ti4O in the first embodiment of the present invention 15 Schematic diagram of the flake microstructure;

[0021] Figure 4Schematic diagram of the microscopic morphology of the pure flaky PbTiO3 template in Example 1 of the present invention;

[0022] Figure 5 The pure flaky Bi4Ti3O in the second embodiment of the present invention 12 Schematic diagram of the flake microstructure;

[0023] Figure 6 The flaky PbBi4Ti4O in the second embodiment of the present invention 15 Schematic diagram of the flake microstructure;

[0024] Figure 7 Schematic diagram of the microscopic morphology of the pure flaky PbTiO3 template in Example 2 of the present invention;

[0025] Figure 8 The pure flaky Bi4Ti3O in the third embodiment of the present invention 12 Schematic diagram of the flake microstructure;

[0026] Figure 9 The flaky PbBi4Ti4O in the third embodiment of the present invention 15 Schematic diagram of the flake microstructure;

[0027] Figure 10 Schematic diagram of the microscopic morphology of the pure flaky PbTiO3 template in Example 3 of the present invention;

[0028] Figure 11 The pure flaky Bi4Ti3O in the fourth embodiment of the present invention 12 Schematic diagram of the flake microstructure;

[0029] Figure 12 The flaky PbBi4Ti4O in the fourth embodiment of the present invention 15 Schematic diagram of the flake microstructure;

[0030] Figure 13 Schematic diagram of the flaky microscopic morphology of the pure flaky PbTiO3 template in Example 4 of the present invention. DETAILED DESCRIPTION

[0031] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making any creative efforts shall fall within the scope of protection of the present invention.

[0032] Ferroelectric single crystal materials are single crystal materials that exhibit ferroelectricity, a highly ordered crystal structure, and the absence of grain boundaries. Their atoms are regularly arranged in a periodic pattern in three-dimensional space, and their spontaneous polarization direction can be reversibly reversed under the influence of an external electric field, exhibiting significant piezoelectric, dielectric, and pyroelectric properties. Due to their lack of grain boundary defects and anisotropy, ferroelectric single crystal materials far surpass polycrystalline ceramics in piezoelectric performance, making them a core material for high-end transducers and sensors. Despite high costs and environmental concerns, their irreplaceable nature in fields such as medicine and defense is driving innovation in manufacturing technology and research into lead-free materials.

[0033] By controlling grain orientation, textured piezoelectric ceramics achieve piezoelectric properties comparable to those of single-crystal materials, overcoming the limitations of single-crystal materials, such as high cost and uneven composition. By controlling grain orientation, textured piezoelectric ceramics achieve piezoelectric properties comparable to those of single-crystal materials, while overcoming the limitations of single-crystal materials, such as high cost and uneven composition. Their excellent performance and cost advantages give them broad application prospects in the field of high-performance piezoelectric materials.

[0034] The present invention uses a three-step molten salt method to prepare a flaky PbTiO3 template. The three-step molten salt method matrix steps are: first, TiO2 and Bi2O3 are used to prepare a flaky Bi4Ti3O 12 , then the flake Bi4Ti3O 12 Reacts with PbO and TiO2 to form PbBi4Ti4O 15 Precursor, finally the excess PbO and PbBi4Ti4O 15 The precursors reacted successfully at high temperature to produce a flake PbTiO3 template.

[0035] Example 1

[0036] See also Figure 1 、 Figure 2 、 Figure 3 、 Figure 4 This embodiment provides a method for preparing a flaky PbTiO3 template, comprising the following steps:

[0037] Step 1: Preparation of pure flake Bi4Ti3O 12 (2Bi2O3+3TiO2=Bi4Ti3O 12 )

[0038] TiO2 and Bi2O3 were first mixed in a mass ratio of 3:2, and then NaCl-KCl molten salt was added in a mass ratio of 1:1 and continued to mix. After mixing, the mixture was ball-milled with anhydrous ethanol for 12 hours to obtain a slurry. The slurry obtained by ball milling was dried and reacted at a temperature of 1050°C for 1 hour. The reaction product containing molten salt was washed with deionized water at 70°C to remove the molten salt until there was no Cl - , prepare pure flake Bi4Ti3O12 , its flaky microstructure is as follows Figure 2 As shown;

[0039] Step 2: Preparation of PbBi4Ti4O flakes 15 Precursor (Bi4Ti3O 12 +PbO+TiO2=PbBi4Ti4O 15 )

[0040] Pure flake Bi4Ti3O 12 , PbO and TiO2 were mixed in a mass ratio of 1:1:1 and stirred for 6 hours. After mixing, NaCl-KCl molten salt was added in a mass ratio of 1:1 and continued to mix. After mixing, the slurry was ball-milled with anhydrous ethanol for 12 hours to obtain a slurry. The slurry obtained by ball milling was dried and reacted at a temperature of 800℃ for 3 hours. The reaction product containing molten salt was washed with deionized water at 70℃ to remove the molten salt until there was no Cl - , prepared flake PbBi4Ti4O 15 The precursor has a flake-like microstructure. Figure 3 As shown;

[0041] Step 3: Preparation of PbTiO3 (PbBi4Ti4O 15 +3PbO=4PbTiO3+2Bi2O3)

[0042] The flake PbBi4Ti4O 15 The precursor and PbO were mixed and stirred at a mass ratio of 1:3.5 for 6 hours. After mixing, NaCl-KCl molten salt was added at a mass ratio of 1:1 and continued to mix. After mixing, the mixture was ball-milled with anhydrous ethanol for 12 hours to obtain a slurry. The ball-milled slurry was dried and reacted at a temperature of 850°C for 3 hours. The reaction product containing molten salt was washed with deionized water at 70°C to remove the molten salt until there was no Cl. - , to prepare flake PbTiO3;

[0043] Step 4: Preparation of pure flake PbTiO3 template

[0044] Add 2 mol / L dilute nitric acid to the flaky PbTiO3 to clean Bi2O3, then add deionized water at 70°C to wash and remove the molten salt until there is no Cl - After filtration, it was dried at 60℃ to obtain a pure flaky PbTiO3 template. Its flaky micromorphology is as follows: Figure 4 shown.

[0045] Example 2

[0046] See also Figure 1 、 Figure 5 、Figure 6 、 Figure 7 This embodiment provides a method for preparing a flaky PbTiO3 template, comprising the following steps:

[0047] Step 1: Preparation of pure flake Bi4Ti3O 12

[0048] TiO2 and Bi2O3 were first mixed in a mass ratio of 3:2, and then NaCl-KCl molten salt was added in a mass ratio of 1:1 and continued to mix. After mixing, the mixture was ball-milled with anhydrous ethanol for 12 hours to obtain a slurry. The slurry obtained by ball milling was dried and reacted at a temperature of 1050°C for 1 hour. The reaction product containing molten salt was washed with deionized water at 70°C to remove the molten salt until there was no Cl - , prepare pure flake Bi4Ti3O 12 , its flaky microstructure is as follows Figure 5 As shown;

[0049] Step 2: Preparation of PbBi4Ti4O flakes 15 Precursor

[0050] Pure flake Bi4Ti3O 12 , PbO and TiO2 were mixed in a mass ratio of 1:1:1 and stirred for 6 hours. After mixing, NaCl-KCl molten salt was added in a mass ratio of 1:1 and continued to mix. After mixing, the slurry was ball-milled with anhydrous ethanol for 12 hours to obtain a slurry. The slurry obtained by ball milling was dried and reacted at a temperature of 900℃ for 3 hours. The reaction product containing molten salt was washed with deionized water at 70℃ to remove the molten salt until there was no Cl - , prepared flake PbBi4Ti4O 15 The precursor has a flake-like microstructure. Figure 6 As shown;

[0051] Step 3: Preparation of PbTiO3 flakes

[0052] The PbBi4Ti4O flakes were stirred by magnetic stirring. 15 The precursor and PbO were mixed and stirred at a mass ratio of 1:3.5 for 6 hours. After mixing, NaCl-KCl molten salt was added at a mass ratio of 1:1 and continued to mix. After mixing, the slurry was ball-milled with anhydrous ethanol for 12 hours to obtain a slurry. The ball-milled slurry was dried and reacted at a temperature of 1000°C for 3 hours. The reaction product containing molten salt was washed with deionized water at 70°C to remove the molten salt until there was no Cl. - , to prepare flake PbTiO3;

[0053] Step 4: Preparation of pure flake PbTiO3 template

[0054] Add 2 mol / L dilute nitric acid to the flaky PbTiO3 to clean Bi2O3, then add deionized water at 70°C to wash and remove the molten salt until there is no Cl - After filtration, it was dried at 60℃ to obtain a pure flaky PbTiO3 template. Its flaky micromorphology is as follows: Figure 7 shown.

[0055] Example 3

[0056] See also Figure 1 、 Figure 8 、 Figure 9 、 Figure 10 This embodiment provides a method for preparing a flaky PbTiO3 template, comprising the following steps:

[0057] Step 1: Preparation of pure flake Bi4Ti3O 12

[0058] TiO2 and Bi2O3 were first mixed in a mass ratio of 3:2, and then NaCl-KCl molten salt was added in a mass ratio of 1:1 and continued to mix. After mixing, the mixture was ball-milled with anhydrous ethanol for 12 hours to obtain a slurry. The slurry obtained by ball milling was dried and reacted at a temperature of 1050°C for 1 hour. The reaction product containing molten salt was washed with deionized water at 70°C to remove the molten salt until there was no Cl - , prepare pure flake Bi4Ti3O 12 , its flaky microstructure is as follows Figure 8 As shown;

[0059] Step 2: Preparation of PbBi4Ti4O flakes 15 Precursor

[0060] Pure flake Bi4Ti3O 12 , PbO and TiO2 were mixed and stirred at a mass ratio of 1:1:1 for 6 hours, and then NaCl-KCl molten salt was added at a mass ratio of 1:1 and continued to mix. After mixing, the slurry was ball-milled with anhydrous ethanol for 12 hours to obtain a slurry. The slurry obtained by ball milling was dried and reacted at a temperature of 1000℃ for 3 hours. The reaction product containing molten salt was washed with deionized water at 70℃ to remove the molten salt until there was no Cl - , prepared flake PbBi4Ti4O 15 The precursor has a flake-like microstructure. Figure 9 As shown;

[0061] Step 3: Preparation of PbTiO3 flakes

[0062] The PbBi4Ti4O flakes were stirred by magnetic stirring. 15The precursor and PbO were mixed and stirred at a mass ratio of 1:3.5 for 6 hours. After mixing, NaCl-KCl molten salt was added at a mass ratio of 1:1 and continued to mix. After mixing, the mixture was ball-milled with anhydrous ethanol for 12 hours to obtain a slurry. The ball-milled slurry was dried and reacted at a temperature of 1050°C for 3 hours. The reaction product containing molten salt was washed with deionized water at 70°C to remove the molten salt until there was no Cl. - , to prepare flake PbTiO3;

[0063] Step 4: Preparation of pure flake PbTiO3 template

[0064] Add 2 mol / L dilute nitric acid to the flaky PbTiO3 to clean Bi2O3, then add deionized water at 70°C to wash and remove the molten salt until there is no Cl - After filtration, it was dried at 60℃ to obtain a pure flaky PbTiO3 template. Its flaky micromorphology is as follows: Figure 10 shown.

[0065] Example 4

[0066] See also Figure 1 、 Figure 11 、 Figure 12 、 Figure 13 This embodiment provides a method for preparing a flaky PbTiO3 template, comprising the following steps:

[0067] Step 1: Preparation of pure flake Bi4Ti3O 12

[0068] TiO2 and Bi2O3 were first mixed in a mass ratio of 3:2, and then NaCl-KCl molten salt was added in a mass ratio of 1:1 and continued to mix. After mixing, the mixture was ball-milled with anhydrous ethanol for 12 hours to obtain a slurry. The slurry obtained by ball milling was dried and reacted at a temperature of 1050°C for 1 hour. The reaction product containing molten salt was washed with deionized water at 70°C to remove the molten salt until there was no Cl - , prepare pure flake Bi4Ti3O 12 , its flaky microstructure is as follows Figure 11 As shown;

[0069] Step 2: Preparation of PbBi4Ti4O flakes 15 Precursor

[0070] Pure flake Bi4Ti3O 12, PbO and TiO2 were mixed and stirred at a mass ratio of 1:1:1 for 6 hours, and then NaCl-KCl molten salt was added at a mass ratio of 1:1 and continued to mix. After mixing, the slurry was ball-milled with anhydrous ethanol for 12 hours to obtain a slurry. The slurry obtained by ball milling was dried and reacted at a temperature of 1000℃ for 3 hours. The reaction product containing molten salt was washed with deionized water at 70℃ to remove the molten salt until there was no Cl - , prepared flake PbBi4Ti4O 15 The precursor has a flake-like microstructure. Figure 12 As shown;

[0071] Step 3: Preparation of PbTiO3 flakes

[0072] The flake PbBi4Ti4O 15 The precursor and PbO were mixed and stirred at a mass ratio of 1:3.5 for 6 hours. After mixing, NaCl-KCl molten salt was added at a mass ratio of 1:1 and continued to mix. After mixing, the mixture was ball-milled with anhydrous ethanol for 12 hours to obtain a slurry. The ball-milled slurry was dried and reacted at a temperature of 1050°C for 6 hours. The reaction product containing molten salt was washed with deionized water at 70°C to remove the molten salt until there was no Cl. - , to prepare flake PbTiO3;

[0073] Step 4: Preparation of pure flake PbTiO3 template

[0074] Add 2 mol / L dilute nitric acid to the flaky PbTiO3 to clean Bi2O3, then add deionized water at 70°C to wash and remove the molten salt until there is no Cl - After filtration, it was dried at 60℃ to obtain a pure flaky PbTiO3 template. Its flaky micromorphology is as follows: Figure 13 shown.

[0075] A comprehensive comparison of Example 1, Example 2 and Example 3 shows that the present invention controls the formation of flaky PbBi4Ti4O 15 The reaction time of the precursor was 1000℃ for 3h and the PbBi4Ti4O 15 Has the best flake morphology.

[0076] A comprehensive comparison of Example 3 and Example 4 shows that the best flaky PbTiO3 template can be obtained by reacting at 1050°C for 6 hours.

[0077] In summary, the method for preparing flaky PbTiO3 templates provided by the present invention can successfully produce stable PbTiO3 templates with excellent flaky morphology. This method overcomes the shortcomings of traditional methods and expands the selection of templates for texturing lead-based piezoelectric ceramics, thus possessing high economic and social value.

[0078] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A method for preparing a flaky PbTiO3 template, characterized in that: The following steps are involved: Step 1: Under molten salt conditions, TiO2 and Bi2O3 are mixed in a preset ratio, and then ball-milled to obtain a slurry. After drying the slurry, the slurry is reacted at a preset temperature. The reaction product is washed with molten salt to prepare pure flake Bi4Ti3O 12 ; Step 2: Under molten salt conditions, use magnetic stirring to mix the flake Bi4Ti3O 12 , PbO and TiO2 are mixed in a preset ratio, ball-milled to obtain a slurry, dried and reacted at a preset temperature, and the reaction product is washed with molten salt to prepare a flake PbBi4Ti4O 15 Precursor; Step 3: Under molten salt conditions, use magnetic stirring to mix the flake PbBi4Ti4O 15 The precursor and PbO are mixed in a preset ratio, ball-milled to obtain a slurry, dried, and reacted at a preset temperature. The reaction product is washed with molten salt to prepare flake PbTiO3. Step 4: Add acid solution to the flaky PbTiO3 to clean Bi2O3, then add deionized water to wash and remove the molten salt, filter and dry to obtain a pure flaky PbTiO3 template.

2. The method for preparing a flaky PbTiO3 template according to claim 1, wherein: In the step 1, the TiO2 and Bi2O3 are mixed under NaCl-KCl molten salt conditions, the ball milling medium after mixing is anhydrous ethanol, the ball milling time is 12 hours, and the mixing mass ratio of the TiO2, Bi2O3 and NaCl-KCl molten salt is 3:2:

5.

3. The method for preparing a flaky PbTiO3 template according to claim 1, wherein: In the step 1, the TiO2 and Bi2O3 are mixed and reacted at a temperature of 950 to 1150°C for 1 to 6 hours, and the reaction product is washed with molten salt using deionized water at 70°C.

4. The method for preparing a flaky PbTiO3 template according to claim 1, wherein: In the step 2, the flaky Bi4Ti3O 12 and PbO in NaCl-KCl molten salt conditions, the mixed ball milling medium is anhydrous ethanol, the ball milling time is 12h, the flaky Bi4Ti3O 12 , PbO, TiO2 and NaCl-KCl molten salt have a mixing mass ratio of 1:1:1:

1.

5. The method for preparing a flaky PbTiO3 template according to claim 1, wherein: In the step 2, the flaky Bi4Ti3O 12 The reaction is carried out with PbO under magnetic stirring for 1 to 6 hours at a temperature of 800 to 1000° C. for 1 to 6 hours. The reaction product is washed with molten salt using deionized water at 70° C.

6. The method for preparing a flaky PbTiO3 template according to claim 1, wherein: In the step 3, the flaky PbBi4Ti4O 15 The precursor and PbO are mixed under NaCl-KCl molten salt conditions, the mixed ball milling medium is anhydrous ethanol, the ball milling time is 12h, the flaky PbBi4Ti4O 15 The mixing mass ratio of the precursor, PbO and NaCl-KCl molten salt is 1:3.5:

1.

7. The method for preparing a flaky PbTiO3 template according to claim 1, wherein: In the step 3, the flaky PbBi4Ti4O 15 The precursor and PbO are stirred magnetically for 1 to 6 hours and reacted at a temperature of 800 to 1050° C. for 1 to 6 hours. The reaction product is washed with 70° C. deionized water to remove the molten salt.

8. The method for preparing a flaky PbTiO3 template according to claim 1, wherein: In the step 4, the acid solution is dilute nitric acid with a concentration of 2 mol / L, the temperature of the deionized water is 70°C, and the flaky PbTiO3 is washed and filtered and then dried at a temperature of 60°C.

Citation Information

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