3-3 type piezoelectric ceramic composite material and preparation method thereof

Abstract

The invention discloses a 3-3 type piezoelectric ceramic composite material, which comprises piezoelectric ceramic block arrays and a filling phase, cutting gaps among the piezoelectric ceramic block arrays are filled with the filling phase, the piezoelectric ceramic block arrays are completely coated with the filling phase, and the filling phase comprises a polyvinylidene fluoride-based polymer and ionic liquid 1-ethyl-3-methylimidazole bis (trifluoromethylsulfonyl) imide. The invention also discloses a preparation method of the 3-3 type piezoelectric ceramic composite material. The preparation method comprises the following steps: dissolving polyvinylidene fluoride-based polymer powder to obtain a uniform and transparent solution A; adding 1-ethyl-3-methylimidazole bis (trifluoromethylsulfonyl) imide into the solution A, and mixing to obtain a uniform and transparent solution B; the B is dripped on the surfaces of the piezoelectric ceramic block arrays, cutting gaps between the piezoelectric ceramic block arrays are filled, the piezoelectric ceramic block arrays are completely wrapped, curing is conducted after heat treatment, and the 3-3 type piezoelectric ceramic composite material is obtained. The 3-3 type piezoelectric ceramic composite material provided by the invention shows high piezoelectric performance. The preparation method provided by the invention has the advantages of simple process and no destructiveness.

Description

Technical Field

[0001] The present invention belongs to the technical field of composite materials, and in particular relates to a 3-3 type piezoelectric ceramic composite material and a preparation method thereof. Background Art

[0002] With the rapid development of industrial automation and intelligent monitoring technology, the demand for high-performance piezoelectric materials is growing. These materials play a key role in sensors, actuators and other intelligent structures. 3-3 piezoelectric composites are composed of three-dimensional piezoelectric ceramics arranged regularly and connected to polymers in three dimensions. 3-3 piezoelectric composites are more commonly used in the field of piezoelectric materials due to their advantages such as high piezoelectric coefficient, high electromechanical coupling coefficient, good mechanical flexibility and low acoustic impedance. They can provide efficient and reliable performance in various working environments. With the continuous advancement of technology, the application scope of these composite materials is expected to be further expanded. For example, the Chinese patent with publication number CN111187073A discloses a 3-3 piezoelectric ceramic / cement composite material and its preparation method, which uses 3D printing technology to print a cavity sacrificial template for injecting a porous piezoelectric ceramic skeleton structure, injects ceramic slurry and solidifies it, removes the cavity sacrificial template after high-temperature sintering to obtain a porous piezoelectric ceramic skeleton structure, and pours cement slurry to prepare a 3-3 piezoelectric ceramic / cement composite material.

[0003] At present, the common composite types of flexible piezoelectric composite materials are 1-3 types, and the common preparation method is to inject epoxy resin colloid into the piezoelectric ceramic column array to fill the cutting gap, and after vacuum degassing and curing, the excess epoxy resin on the upper and lower surfaces needs to be ground off to expose the ceramic columns. For example, the Chinese patent with publication number CN117580435A discloses a composite piezoelectric material based on compound epoxy resin, its preparation method and application; the composite piezoelectric material includes a plurality of piezoelectric ceramic units arranged in an array, and a filling phase filling the gaps between the piezoelectric ceramic units.

[0004] However, due to the high viscosity of epoxy resin, it is difficult to achieve uniformity without bubbles. On the other hand, the 3-3 type composite of epoxy resin and piezoelectric ceramic column array may have the problem of reduced performance, so it is necessary to grind off the excess epoxy resin on the upper and lower surfaces. The grinding process of the composite material can easily cause damage to the piezoelectric ceramic column, thus affecting its piezoelectric performance. Therefore, it is of great value and significance to develop a simple and non-destructive preparation method for 3-3 type piezoelectric ceramic composite materials with high piezoelectric performance. Summary of the invention

[0005] The object of the present invention is to provide a 3-3 type piezoelectric ceramic composite material and a preparation method thereof. The 3-3 type piezoelectric ceramic composite material provided by the present invention exhibits high piezoelectric performance, and the preparation method provided by the present invention has the advantages of simple process and non-destructiveness.

[0006] The present invention provides the following technical solutions:

[0007] A 3-3 type piezoelectric ceramic composite material, comprising a piezoelectric ceramic block array and a filling phase that fills the cut gaps between the piezoelectric ceramic block arrays and completely covers the piezoelectric ceramic block arrays, the filling phase comprising a polyvinylidene fluoride based polymer and an ionic liquid, and the ionic liquid is 1-ethyl-3-methylimidazole bis(trifluoromethylsulfonyl)imide.

[0008] The polyvinylidene fluoride based polymer is selected from poly(vinylidene fluoride-trifluoroethylene), polyvinylidene fluoride, polyvinylidene fluoride-trifluoroethylene-chlorofluoroethylene or polyvinylidene fluoride-hexafluoropropylene.

[0009] The material of the piezoelectric ceramic block array is lead zirconate titanate (PZT), barium titanate (BTO) or potassium sodium niobate (KNN).

[0010] In the filling phase, 1-ethyl-3-methylimidazole bis(trifluoromethylsulfonyl)imide accounts for 10% to 60% of the polyvinylidene fluoride polymer, and the percentage is mass percentage.

[0011] The present invention also provides a method for preparing the above 3-3 type piezoelectric ceramic composite material, the preparation method comprising the following steps:

[0012] (1) dissolving polyvinylidene fluoride polymer powder in an organic solvent and stirring until completely dissolved to obtain a uniform transparent solution A;

[0013] (2) adding ionic liquid 1-ethyl-3-methylimidazole bis(trifluoromethylsulfonyl)imide to the uniform transparent solution A obtained in step (1), stirring until completely mixed, to obtain a uniform transparent solution B;

[0014] (3) dripping the uniform transparent solution B obtained in step (2) onto the surface of the piezoelectric ceramic block array to fill the cut gaps between the piezoelectric ceramic block arrays and completely cover the piezoelectric ceramic block arrays, and curing after heat treatment to obtain a 3-3 type piezoelectric ceramic composite material.

[0015] The preparation method provided by the present invention prepares a 3-3 type piezoelectric ceramic composite material by compounding a conductive polyvinylidene fluoride-based polymer with a cut ceramic block array.

[0016] In steps (1) and (2), 0.5-2.5 g of polyvinylidene fluoride-based polymer powder is dissolved in 10-20 ml of an organic solvent, and 1-ethyl-3-methylimidazole bistrifluoromethylsulfonimide is added at a mass ratio of 10% to 60% of the polyvinylidene fluoride polymer, wherein the organic solvent is N,N-dimethylformamide.

[0017] In step (3), 0.5 to 2 ml of uniform transparent solution B is dripped per square centimeter of the surface of the piezoelectric ceramic block array.

[0018] In step (3), the heat treatment temperature is 80 to 120° C., and the heat treatment time is 2 to 4 hours.

[0019] In step (3), the method for preparing the piezoelectric ceramic block array includes:

[0020] (3-1) polishing and cleaning the piezoelectric ceramic block, coating a uniform layer of conductive silver paste on the upper and lower surfaces, and polarizing the piezoelectric ceramic after the silver paste solidifies;

[0021] (3-2) cutting the piezoelectric ceramic obtained in step (3-1) into a ceramic block array along a first direction;

[0022] (3-3) Cutting the piezoelectric ceramic obtained in step (3-2) along a second direction to obtain a plurality of independent piezoelectric ceramic block arrays, and then ultrasonically cleaning and drying; the second direction of cutting is on the same plane as the first direction, and the second direction is perpendicular to the first direction.

[0023] Wherein, the cutting depth in steps (3-2) and (3-3) is the same as the thickness of the piezoelectric ceramic.

[0024] In step (3), the specific method of dripping the uniform transparent solution B obtained in step (2) onto the surface of the piezoelectric ceramic block array is:

[0025] (3-4) The piezoelectric ceramic block array obtained in step (3-3) is placed with the front side facing upward, and a uniform transparent solution B is dripped onto the surface to fill the cut gaps between the piezoelectric ceramic block arrays and completely cover the piezoelectric ceramic column array, and then solidified after heat treatment;

[0026] (3-5) The piezoelectric ceramic block array obtained in step (3-4) is placed with the reverse side facing upward, and a uniform transparent solution B is dripped onto its surface to fill the cut gaps between the piezoelectric ceramic block arrays and completely cover the piezoelectric ceramic column array. After heat treatment, the solution is cured to obtain a piezoelectric ceramic composite material.

[0027] The preparation method provided by the present invention uses a cutting-filling method to obtain a 3-3 type piezoelectric composite material, and innovatively uses 1-ethyl-3-methylimidazole bistrifluoromethylsulfonyl imide / polyvinylidene fluoride based polymer to fill a ceramic block array, so that it can be uniform and free of bubbles, and effectively derive bound charges, showing high piezoelectric performance. The preparation method provided by the present invention has a simple process, is non-destructive, controllable process, low cost and strong practicality, and the prepared 3-3 type piezoelectric composite material has high piezoelectric performance. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 The piezoelectric ceramic block arrays cut in Example 1 and Comparative Example 1;

[0029] Figure 2 Schematic diagram of the process for preparing the 3-3 type piezoelectric ceramic composite material in Example 1;

[0030] Figure 3 The piezoelectric properties of the 3-3 type piezoelectric ceramic composite material prepared in Example 1;

[0031] Figure 4 The piezoelectric properties of the 3-3 type piezoelectric ceramic composite material prepared in Comparative Example 1. DETAILED DESCRIPTION

[0032] The technical solution of the present invention is further explained below in conjunction with specific embodiments.

[0033] Example 1

[0034] (1) polishing and cleaning the lead zirconate titanate piezoelectric ceramic block, coating a uniform layer of conductive silver paste on the upper and lower surfaces, and polarizing the piezoelectric ceramic after the silver paste is solidified;

[0035] (2) cutting the piezoelectric ceramic obtained in step (1) into a ceramic block array along a first direction;

[0036] (3) cutting the piezoelectric ceramic obtained in step (2) along a second direction to obtain a plurality of independent piezoelectric ceramic block arrays, and then ultrasonically cleaning and drying; the second direction of cutting is on the same plane as the first direction, and the second direction is perpendicular to the first direction; the piezoelectric ceramic block array obtained by cutting is as follows: Figure 1 As shown;

[0037] (4) Dissolve 1.5 g of poly(vinylidene fluoride-trifluoroethylene) powder in 10 mL of N,N-dimethylformamide and stir until completely dissolved to obtain a uniform transparent solution A;

[0038] (5) adding 0.75 g of ionic liquid (1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide) to the uniform transparent solution obtained in step (4), stirring until completely mixed, to obtain a uniform transparent solution B;

[0039] (6) The piezoelectric ceramic block array obtained in step (3) is placed face up, and the uniform transparent solution B obtained in step (5) is dripped onto its surface to fill the cut gaps and completely cover the piezoelectric ceramic column array, and then heat treated at 100° C. for 3 h to solidify;

[0040] (7) The piezoelectric ceramic block array obtained in step (6) is placed with the reverse side facing upward, and the uniform transparent solution B obtained in step (5) is dripped onto its surface to fill the cut gaps and completely cover the piezoelectric ceramic column array. The piezoelectric ceramic composite material is solidified after heat treatment at 100° C. for 3 h to obtain the piezoelectric ceramic composite material.

[0041] The schematic diagram of the process of steps (6)-(7) is as follows: Figure 2 shown.

[0042] In this embodiment, 1 ml of uniform transparent solution B is dripped per square centimeter of the surface of the piezoelectric ceramic block array.

[0043] Comparative Example 1

[0044] (1) polishing and cleaning the lead zirconate titanate piezoelectric ceramic block, coating a uniform layer of conductive silver paste on the upper and lower surfaces, and polarizing the piezoelectric ceramic after the silver paste is solidified;

[0045] (2) cutting the piezoelectric ceramic obtained in step (1) into a ceramic block array along a first direction;

[0046] (3) cutting the piezoelectric ceramic obtained in step (2) along a second direction to obtain a plurality of independent piezoelectric ceramic block arrays, and then ultrasonically cleaning and drying; the second direction of cutting is on the same plane as the first direction, and the second direction is perpendicular to the first direction; the piezoelectric ceramic block array obtained by cutting is as follows: Figure 1 As shown;

[0047] (4) Dissolve 1.5 g of poly(vinylidene fluoride-trifluoroethylene) powder in 10 mL of N,N-dimethylformamide and stir until completely dissolved to obtain a uniform transparent solution;

[0048] (5) The piezoelectric ceramic block array obtained in step (4) is placed face up, and the solution obtained in step (5) is dripped onto its surface to fill the cut gaps and completely cover the piezoelectric ceramic column array, and then heat treated at 100° C. for 3 h to solidify;

[0049] (6) The piezoelectric ceramic block array obtained in step (5) is placed with the reverse side facing upward, and the solution obtained in step (5) is dripped onto its surface to fill the cut gaps and completely cover the piezoelectric ceramic column array. The piezoelectric ceramic composite material is solidified after heat treatment at 100° C. for 3 h to obtain the piezoelectric ceramic composite material.

[0050] Figure 3 and Figure 4 The piezoelectric properties of the 3-3 piezoelectric ceramic composite materials prepared in Example 1 and Comparative Example 1 are 185 pC / N and 0.1 pC / N, respectively. It can be clearly seen that the 3-3 piezoelectric ceramic composite material prepared by compounding the conductive polyvinylidene fluoride-based polymer with the cut ceramic block array has excellent piezoelectric properties.

Claims

1. A 3-3 type piezoelectric ceramic composite material, characterized in that: The 3-3 type piezoelectric ceramic composite material includes a piezoelectric ceramic block array and a filling phase that fills the cut gaps between the piezoelectric ceramic block arrays and completely covers the piezoelectric ceramic block array. The filling phase includes a polyvinylidene fluoride polymer and an ionic liquid. The ionic liquid is 1-ethyl-3-methylimidazole bis(trifluoromethylsulfonyl)imide.

2. The 3-3 type piezoelectric ceramic composite material according to claim 1, characterized in that: The polyvinylidene fluoride based polymer is selected from poly(vinylidene fluoride-trifluoroethylene), polyvinylidene fluoride, polyvinylidene fluoride-trifluoroethylene-chlorofluoroethylene or polyvinylidene fluoride-hexafluoropropylene.

3. The 3-3 type piezoelectric ceramic composite material according to claim 1, characterized in that: The material of the piezoelectric ceramic block array is lead zirconate titanate, barium titanate or potassium sodium niobate.

4. The 3-3 type piezoelectric ceramic composite material according to claim 1, characterized in that: The amount of 1-ethyl-3-methylimidazole bis(trifluoromethylsulfonyl)imide in the filling phase is 10% to 60% of the polyvinylidene fluoride polymer, and the percentage is mass percentage.

5. A method for preparing the 3-3 type piezoelectric ceramic composite material according to any one of claims 1 to 4, characterized in that: The preparation method comprises the following steps: (1) dissolving polyvinylidene fluoride polymer powder in an organic solvent and stirring until completely dissolved to obtain a uniform transparent solution A; (2) adding 1-ethyl-3-methylimidazole bis(trifluoromethylsulfonyl)imide to the uniform transparent solution A obtained in step (1), stirring until completely mixed, to obtain a uniform transparent solution B; (3) dripping the uniform transparent solution B obtained in step (2) onto the surface of the piezoelectric ceramic block array to fill the cut gaps between the piezoelectric ceramic block arrays and completely cover the piezoelectric ceramic block arrays, and curing after heat treatment to obtain a 3-3 type piezoelectric ceramic composite material.

6. The method for preparing the 3-3 type piezoelectric ceramic composite material according to claim 5, characterized in that: In steps (1) and (2), 0.5-2.5 g of polyvinylidene fluoride-based polymer powder is dissolved in 10-20 ml of an organic solvent, and 1-ethyl-3-methylimidazole bistrifluoromethylsulfonimide is added at a mass ratio of 10% to 60% of the polyvinylidene fluoride polymer.

7. The method for preparing the 3-3 type piezoelectric ceramic composite material according to claim 6, characterized in that: In step (3), 0.5 to 2 ml of uniform transparent solution B is dripped per square centimeter of the surface of the piezoelectric ceramic block array.

8. The method for preparing the 3-3 type piezoelectric ceramic composite material according to claim 5, characterized in that: In step (3), the heat treatment temperature is 80 to 120° C., and the heat treatment time is 2 to 4 hours.

9. The method for preparing the 3-3 type piezoelectric ceramic composite material according to claim 5, characterized in that: In step (3), the method for preparing the piezoelectric ceramic block array includes: (3-1) polishing and cleaning the piezoelectric ceramic block, coating a uniform layer of conductive silver paste on the upper and lower surfaces, and polarizing the piezoelectric ceramic after the silver paste solidifies; (3-2) cutting the piezoelectric ceramic obtained in step (3-1) into a ceramic block array along a first direction; (3-3) Cutting the piezoelectric ceramic obtained in step (3-2) along a second direction to obtain a plurality of independent piezoelectric ceramic block arrays, and then ultrasonically cleaning and drying; the second direction of cutting is on the same plane as the first direction, and the second direction is perpendicular to the first direction.

10. The method for preparing the 3-3 type piezoelectric ceramic composite material according to claim 9, characterized in that: The specific method of dripping the uniform transparent solution B obtained in step (2) onto the surface of the piezoelectric ceramic block array is: (3-4) The piezoelectric ceramic block array obtained in step (3-3) is placed with the front side facing upward, and a uniform transparent solution B is dripped onto the surface to fill the cut gaps between the piezoelectric ceramic block arrays and completely cover the piezoelectric ceramic column array, and then solidified after heat treatment; (3-5) The piezoelectric ceramic block array obtained in step (3-4) is placed with the reverse side facing upward, and a uniform transparent solution B is dripped onto its surface to fill the cut gaps between the piezoelectric ceramic block arrays and completely cover the piezoelectric ceramic column array. After heat treatment, the solution is cured to obtain a piezoelectric ceramic composite material.

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