CN112876721B - High-performance 3D printing piezoelectric part and preparation method thereof - Google Patents
High-performance 3D printing piezoelectric part and preparation method thereof Download PDFInfo
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Abstract
The invention provides a high-performance 3D printing piezoelectric part and a preparation method thereof, wherein the preparation method comprises the following steps: preparing polymer and ceramic material into polymer/ceramic piezoelectric composite powder; coating a wave absorbing material on the surface of the polymer/ceramic piezoelectric composite powder, and then carrying out selective laser sintering on the wave absorbing material to obtain a piezoelectric part; the piezoelectric part is subjected to microwave treatment. The piezoelectric part prepared by the method can effectively solve the problems of low efficiency, high energy consumption and low mechanical property of the part in the prior art.
Description
Technical Field
The invention belongs to the technical field of 3D printing, and particularly relates to a high-performance 3D printing piezoelectric part and a preparation method thereof.
Background
3D printing technology is a non-traditional advanced manufacturing method based on CAD model data to build layer by layer with added material that has been rapidly developed in recent years. The Selective Laser Sintering (SLS) technology is one of the main technologies of 3D printing, a high-energy laser beam is controlled by a computer to melt a powder material, the powder material is bonded into a thin layer, and the thin layer is superposed layer by layer to prepare a three-dimensional workpiece. Due to the excellent characteristics of low molding temperature, high melt viscosity and the like, the high polymer material becomes the most widely and successfully applied material in the SLS processing field at present. However, because SLS processing has high requirements on materials, the types of polymer materials currently available for SLS processing are few and lack functionality, which greatly limits the development and application of SLS processing technology.
Piezoelectric materials are one of the important functional materials that convert mechanical energy into electrical energy. The polymer/ceramic piezoelectric composite material has higher piezoelectric output performance of piezoelectric ceramic and good processing performance of a high polymer material, and is widely applied to the fields of electronics, sensing, ultrasound, energy harvesting and the like. However, since most polymers have a dielectric constant lower than that of the piezoelectric ceramic material, the piezoelectric performance of the piezoelectric composite material is limited by the effective polarization of the ceramic particles; meanwhile, most of the traditional piezoelectric composite materials are thin films or sheets, and piezoelectric parts with complex shapes cannot be designed and prepared, so that the improvement of the performance of the piezoelectric parts and the wider application in the high-tech field are limited.
The piezoelectric composite material is designed and processed by the SLS technology, and a piezoelectric part with excellent performance and a complex shape can be obtained. However, due to the unique process characteristics of SLS processing laser instantaneous heating and fusing of powder particles and layer-by-layer stacking, the powder particles cannot be completely fused and bonded to form a compact product. Therefore, pores are inevitably generated in the SLS part, the interlayer bonding force is weak, the mechanical property is seriously reduced compared with the part obtained by the traditional extrusion and injection molding processing method, for example, the mechanical property along the molding direction (Z-axis direction) is often less than 50% of that of the injection molded part made of the same material, the performance of the part is seriously influenced, the part is difficult to be used as a structural part, and the part becomes an important obstacle for hindering the development and application of the 3D printing technology. Meanwhile, as a piezoelectric material, good piezoelectric and dielectric properties are required. The defects generated by the pore structure in the part can increase the dielectric loss of the material to a certain extent, and the high electric leakage makes the polarization process difficult to be smoothly carried out, further influences the piezoelectric performance of the material and limits the application of the material.
Therefore, it is important to improve the mechanical property and the piezoelectric property of the 3D printed product. The current methods for improving the mechanical properties of SLS articles are focusing more and more on post-processing of the articles. A common post-processing method is to heat or cure the 3D printed part for post-processing. However, when the post-treatment is performed by a conventional heat treatment method, the purpose of improving the material performance can be achieved only by keeping the temperature of the workpiece above the glass transition temperature of the material for a long time. The long-time high-temperature treatment has low efficiency and high energy consumption, and the workpiece is easy to deform and oxidize, so that the performance of the workpiece is influenced.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for improving the performance of a 3D printing piezoelectric part, and the method can effectively solve the problems of low efficiency, high energy consumption and low performance of the part in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of a high-performance 3D printing piezoelectric workpiece comprises the following steps:
(1) preparing polymer and ceramic material into polymer/ceramic piezoelectric composite powder;
(2) coating a wave absorbing material on the surface of the polymer/ceramic piezoelectric composite powder in the step (1), and then carrying out selective laser sintering on the wave absorbing material to obtain a piezoelectric part;
(3) and (3) carrying out microwave treatment on the piezoelectric part obtained in the step (2).
Further, the method for preparing the polymer/ceramic piezoelectric composite powder in the step (1) comprises the following steps: uniformly mixing the polymer and the ceramic material, placing the mixture in solid-phase shearing grinding equipment, controlling the temperature of cooling circulating water to be 5-30 ℃ in the grinding process, the grinding pressure to be 10-50MPa, the grinding rotating speed to be 10-100rpm and the grinding times to be 5-20 times, grinding to obtain composite powder, screening the composite powder, and selecting composite powder with the granularity of 100-800 meshes, namely the polymer/ceramic piezoelectric composite material.
Further, the mass ratio of the polymer to the ceramic material in the step (1) is 1: 0.5-3.
Further, the average particle size of the ceramic material in the step (1) is 0.3 to 50 μm.
Further, the polymer in the step (1) is a thermoplastic polymer.
Further, the polymer in the step (1) is nylon 11, polyvinylidene fluoride or polyvinylidene fluoride-trifluoroethylene.
Further, the ceramic material in the step (1) is barium titanate, lead zirconate titanate or potassium niobate.
Further, the specific operation of coating the wave-absorbing material in the step (2) is as follows: the wave-absorbing material is placed in an ethanol solution to prepare a uniformly dispersed wave-absorbing material solution, the prepared polymer/ceramic piezoelectric composite powder is added into the wave-absorbing material solution, the mixture is stirred under the ultrasonic condition, so that the wave-absorbing material is uniformly coated on the surface of the polymer/ceramic piezoelectric composite powder, and then the polymer/ceramic piezoelectric composite powder coated with the wave-absorbing material is prepared by filtering and drying.
Furthermore, the mass ratio of the wave-absorbing material to the polymer/ceramic piezoelectric composite powder is 0.003-0.01: 1.
Further, the wave-absorbing material in the step (2) is graphene, carbon nanotubes or graphite.
In the scheme, the polymer and the ceramic material are compounded to obtain the polymer/ceramic piezoelectric composite powder, so that the structure and functional properties of the existing material can be effectively improved, and high-performance and functionalization are realized.
Further, the selective laser sintering process parameters in the step (2) are as follows: the preheating temperature is 150-.
In the scheme, the powder is preheated during selective laser sintering processing, then the laser scans a specific area, and the laser energy compensation leads the powder to be fused, bonded and molded. The preheating temperature is set to be 150-180 ℃, so that the preheating temperature is lower than the melting temperature of the material and higher than the crystallization temperature, the shrinkage of the material in the cooling and recrystallization processes can be reduced to the greatest extent, the dimensional precision of parts is improved, the deformation risk is reduced, and the laser compensation energy is minimized.
The laser energy density is too low, the powder absorption energy is not enough to compensate to the melting temperature, and adjacent powder particles cannot be completely melted and bonded, so that the mechanical property of a workpiece is poor and even the workpiece cannot be molded; the laser energy density is too high, so that the temperature of a workpiece is too high, the sintering surplus phenomenon is generated, the precision of the workpiece is influenced, and even the material decomposition is caused to influence the comprehensive performance of the workpiece. When the powder is stacked and sintered layer by layer, the powder layers cannot be bonded due to the fact that the powder is spread on each layer to be too thick, and sintering surplus can be generated due to the fact that the powder is too thin.
Further, the power of the microwave in the step (3) is 500-.
In the scheme, too low microwave power or too short processing time can cause the material temperature to be lower, further fusion bonding cannot be realized, and the sintering effect cannot be achieved; if the power is too high or the processing time is too long, the temperature of the material is too high, the fluidity of the material is enhanced, the original shape and structure of the part can be damaged, and even the part can be degraded. The powder is further fused and bonded within the process parameter range of 500-1500W and 20-180s, and the shape of the powder cannot be damaged, and the specific power and time need to be adjusted according to the structure and the size of the part.
The beneficial effects produced by the invention are as follows:
according to the invention, the wave-absorbing material is coated on the polymer/ceramic piezoelectric composite material powder, the piezoelectric part is obtained after selective laser sintering molding, then microwave post-processing is carried out on the 3D printed piezoelectric part by using a microwave technology, in the microwave processing process, the wave-absorbing material coated on the surface of the powder is directly coupled with microwaves, so that on one hand, the piezoelectric part can absorb the microwaves to heat up, the incompletely-melted powder in the part is further melted and bonded, the interaction between material layers is improved, the internal pores of the piezoelectric material part are reduced, and the bonding force between the layers is improved, thereby the mechanical property of the part is improved, the time of heat conduction in conventional heating is greatly shortened by adopting a microwave heating mode, the advantages of high heating speed and short processing time are achieved, the rapid processing at low temperature is realized, and the oxidative degradation, the oxidation degradation, the corrosion and the corrosion of the material caused by long-time high-temperature processing are avoided, The problem of deformation cracking caused by thermal stress inside the part; in the process, the appearance of the product can be controlled by controlling the processing time and power of the microwave, and the product performance can be adjusted;
on the other hand, the wave-absorbing material coated on the surface of the powder is distributed at the sintering interface, so that an isolation network structure is formed inside the part, more conductive paths are provided, and a local electric field acting on the ceramic particles is improved, so that the effective voltage of the polymer/ceramic piezoelectric composite material in the polarization process is enhanced, the dielectric and piezoelectric properties are improved, and the 3D printing piezoelectric part with excellent comprehensive properties is obtained.
Drawings
FIG. 1 is a scanning electron micrograph of a section of a microwave-treated article of comparative example 1;
FIG. 2 is a scanning electron micrograph of a cross section of the microwave-treated article of example 1;
FIG. 3 is a comparison of the mechanical properties of the microwave treatment of the articles of example 1 and the heat treatment of the articles of comparative example 1;
FIG. 4 is a graph of the dielectric constant as a function of frequency for the microwave treatment of the article of example 1 and for the heat treatment of the article of comparative example 1.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings.
Example 1
A high-performance 3D printing piezoelectric part is prepared by the following steps:
(1) 200gPA11 pellets and 300g of BaTiO having an average particle diameter of 0.5 μm3Uniformly mixing the powder, adding the powder into a solid-phase shearing and grinding device, controlling the cooling circulating water temperature to be 30 ℃, the grinding pressure to be 20MPa, the grinding rotating speed to be 35rpm and the grinding times to be 10 times in the grinding process, grinding to obtain composite powder, sieving the composite powder, and selecting the composite powder with the granularity of 300 meshes, namely PA11/BaTiO3Piezoelectric composite powder;
(2) PA11/BaTiO in step (1)3The surface of the piezoelectric composite powder is coated with a graphene wave-absorbing material, and the specific coating operation is as follows: adding 2g of graphene into 1L of ethanol solution, and performing ultrasonic dispersion for 1h under the ultrasonic power of 800W to obtain stable graphene dispersion liquid; 500g of the PA11/BaTiO thus obtained were mixed3Adding the piezoelectric composite powder into the graphene dispersion liquid, stirring for 2h at the speed of 600rpm under the ultrasonic condition of 800W, filtering and drying to obtain the graphene coated PA11/BaTiO3The composite powder is then selectively laser sintered to obtain piezoelectric part, selective laserThe sintering operation is as follows: graphene coated PA11/BaTiO3Spreading the piezoelectric composite material powder in a selective laser sintering device by using a roller to form a powder bed with a flat surface, closing a cavity sealing door, filling nitrogen, and selectively sintering the powder according to a program set by a computer to obtain PA11/BaTiO3The parameters of the sintering process of the graphene piezoelectric part sample are as follows: preheating temperature is 180 ℃, laser power is 20W, scanning distance is 0.2mm, scanning speed is 7.0m/s, and powder layer thickness is 0.1 mm;
(3) performing microwave treatment on the piezoelectric part obtained in the step (2), wherein the specific technological parameters are as follows: the power is 800W, and the microwave action is 100s, so that the high-performance 3D printing piezoelectric part is prepared.
Example 2
A high-performance 3D printing piezoelectric part is prepared by the following steps:
(1)100g of PVDF pellets and 300g of BaTiO having an average particle diameter of 50 μm3Uniformly mixing the powder, adding the powder into a solid phase shearing and grinding device, controlling the cooling circulating water temperature to be 5 ℃, the grinding pressure to be 50MPa, the grinding rotating speed to be 100rpm and the grinding times to be 20 times in the grinding process, grinding to obtain composite powder, sieving the composite powder, and selecting the composite powder with the granularity of 800 meshes, namely PVDF/BaTiO composite powder3Piezoelectric composite powder;
(2) PVDF/BaTiO in step (1)3The surface of the piezoelectric composite powder is coated with a graphene wave-absorbing material, and the specific coating operation is as follows: adding 2.5g of graphene into 1L of ethanol solution, and performing ultrasonic dispersion for 1h under the ultrasonic power of 800W to obtain stable graphene dispersion liquid; 400g of the PVDF/BaTiO obtained are mixed3Adding the piezoelectric composite powder into the graphene dispersion liquid, stirring for 2h at the speed of 600rpm under the ultrasonic condition of 800W, filtering and drying to obtain the graphene-coated PVDF/BaTiO3And (2) carrying out selective laser sintering on the composite powder to obtain a piezoelectric part, wherein the selective laser sintering comprises the following specific operations: PVDF/BaTiO coated with graphene3Spreading the piezoelectric composite material powder in selective laser sintering equipment by using a roller to form a powder bed with a smooth surface, closing a cavity sealing door, filling nitrogen, and setting a program according to a computerSelectively sintering the powder to obtain PVDF/BaTiO3The sintering process parameters of the graphene piezoelectric part sample are as follows: preheating temperature 155 ℃, laser power 40W, scanning interval 0.3mm, scanning speed 7.6m/s and powder layer thickness 0.15 mm;
(3) performing microwave treatment on the piezoelectric part obtained in the step (2), wherein the specific technological parameters are as follows: the power is 1500W, and the microwave action is 20s, so that the high-performance 3D printing piezoelectric part is prepared.
Example 3
A high-performance 3D printing piezoelectric part is prepared by the following steps:
(1) uniformly mixing 200gPA11 granules and 100g of lead zirconate titanate powder with the average particle size of 0.3 mu m, adding the mixture into a solid-phase shearing grinding device, controlling the cooling circulating water temperature to be 20 ℃, the grinding pressure to be 30MPa, the grinding rotating speed to be 80rpm and the grinding times to be 15 times in the grinding process, grinding to obtain composite powder, screening the composite powder, and selecting the composite material powder with the particle size of 500 meshes, namely the PA 11/lead zirconate titanate piezoelectric composite powder;
(2) coating the surface of the PA 11/lead zirconate titanate piezoelectric composite powder in the step (1) with a CNTs wave-absorbing material, wherein the coating operation is as follows: adding 3.0g of CNTs into 1L of ethanol solution, and performing ultrasonic dispersion for 1h under the ultrasonic power of 800W to obtain a stable CNTs dispersion liquid; adding 300g of prepared PA 11/lead zirconate titanate piezoelectric composite powder into CNTs dispersion, stirring for 2h at the speed of 600rpm under the ultrasonic condition of 800W, filtering and drying to obtain CNTs coated PA 11/lead zirconate titanate composite powder, and then carrying out selective laser sintering to obtain a piezoelectric part, wherein the specific operation of the selective laser sintering is as follows: the method comprises the following steps of spreading the powder of the PA 11/lead zirconate titanate piezoelectric composite material coated with CNTs in a selective laser sintering device by using a roller to form a powder bed with a smooth surface, closing a cavity sealing door, filling nitrogen, selectively sintering the powder according to a computer set program to obtain a PA 11/lead zirconate titanate/CNTs piezoelectric part sample, wherein the sintering process parameters are as follows: preheating temperature 178 ℃, laser power 10W, scanning interval 0.1mm, scanning speed 7.8m/s and powder layer thickness 0.08 mm;
(3) performing microwave treatment on the piezoelectric part obtained in the step (2), wherein the specific technological parameters are as follows: the power is 500W, and the microwave action is 180s, so that the high-performance 3D printing piezoelectric part is prepared.
Example 4
A high-performance 3D printing piezoelectric part is prepared by the following steps:
(1) uniformly mixing 200g of PVDF granules and 300g of potassium niobate powder with the average particle size of 10 microns, adding the mixture into a solid-phase shearing grinding device, controlling the cooling circulating water temperature to be 15 ℃ in the grinding process, the grinding pressure to be 25MPa, the grinding rotating speed to be 40rpm and the grinding times to be 15 times, grinding to obtain composite powder, screening the composite powder, and selecting the composite material powder with the granularity within 400 meshes, namely the PVDF/potassium niobate piezoelectric composite powder;
(2) coating graphite wave-absorbing material on the surface of the PVDF/potassium niobate piezoelectric composite powder in the step (1), wherein the specific coating operation is as follows: adding 2g of graphite into 1L of ethanol solution, and performing ultrasonic dispersion for 1h under the ultrasonic power of 800W to obtain stable graphite dispersion liquid; adding 500g of prepared PVDF/potassium niobate piezoelectric composite powder into graphite dispersion liquid, stirring for 2h at the speed of 600rpm under the ultrasonic condition of 800W, filtering and drying to obtain graphite-coated PVDF/potassium niobate composite powder, and then carrying out selective laser sintering to obtain a piezoelectric part, wherein the specific operation of the selective laser sintering is as follows: the PVDF/potassium niobate piezoelectric composite material powder coated with graphite is spread in selective laser sintering equipment by using a roller to form a powder bed with a smooth surface, a cavity sealing door is closed, nitrogen is filled, the powder is selectively sintered according to a computer set program to obtain a PVDF/potassium niobate/graphite piezoelectric part sample, and the sintering process parameters are as follows: preheating temperature is 157 ℃, laser power is 30W, scanning distance is 0.15mm, scanning speed is 7.6m/s, and powder layer thickness is 0.1 mm;
(3) performing microwave treatment on the piezoelectric part obtained in the step (2), wherein the specific technological parameters are as follows: the power is 1000W, and the microwave action is 50s, so that the high-performance 3D printing piezoelectric part is prepared.
Comparative example 1
A3D printing piezoelectric part is prepared by the following steps:
(1) 200g of PA11 pellets and 300g of panBaTiO with average particle size of 0.5 mu m3Uniformly mixing the powder, adding the powder into a solid-phase shearing and grinding device, controlling the cooling circulating water temperature to be 30 ℃, the grinding pressure to be 20MPa, the grinding rotating speed to be 35rpm and the grinding times to be 10 times in the grinding process, grinding to obtain composite powder, sieving the composite powder, and selecting the composite powder with the granularity of 300 meshes, namely PA11/BaTiO3Piezoelectric composite powder;
(2) PA11/BaTiO in step (1)3The surface of the piezoelectric composite powder is coated with a graphene wave-absorbing material, and the specific coating operation is as follows: adding 2g of graphene into 1L of ethanol solution, and performing ultrasonic dispersion for 1h under the ultrasonic power of 800W to obtain stable graphene dispersion liquid; 500g of the PA11/BaTiO thus obtained3Adding the piezoelectric composite powder into the graphene dispersion liquid, stirring for 2h at the speed of 600rpm under the ultrasonic condition of 800W, filtering and drying to obtain the graphene coated PA11/BaTiO3And (2) carrying out selective laser sintering on the composite powder to obtain a piezoelectric part, wherein the selective laser sintering comprises the following specific operations: graphene coated PA11/BaTiO3Spreading the piezoelectric composite material powder in a selective laser sintering device by using a roller to form a powder bed with a flat surface, closing a cavity sealing door, filling nitrogen, and selectively sintering the powder according to a program set by a computer to obtain PA11/BaTiO3The sintering process parameters of the graphene piezoelectric part sample are as follows: preheating temperature is 180 ℃, laser power is 20W, scanning distance is 0.2mm, scanning speed is 7.0m/s, and powder layer thickness is 0.1 mm;
(3) carrying out heat treatment on the piezoelectric part obtained in the step (2), wherein the specific technological parameters are as follows: and (5) carrying out heat treatment for 24 hours at the temperature of 85 ℃ to obtain the 3D printing piezoelectric part.
Test examples
The piezoelectric members in examples 1 to 4 and comparative example 1 were each subjected to linear motor at 5m/s2The impact is carried out under the acceleration condition, and the open-circuit voltage output by each workpiece is recorded; the piezoelectric members of examples 1 to 4 and comparative example 1 were tested for tensile strength by a universal material testing machine in accordance with GB/T1040-.
Table 1: tensile strength and dielectric constant after microwave treatment and open circuit voltage of a workpiece after impact
As can be seen from the data in the table, the tensile strength, dielectric constant and open circuit voltage of the fabricated parts prepared according to the methods in examples 1 to 4 are all greater than those of the fabricated part in comparative example 1, which proves that the 3D printed piezoelectric fabricated parts obtained by the preparation method in the application have better performance.
As can be seen from the attached figure 1, the cross section of the workpiece has more pores, and the workpiece is easily oxidized and denatured to influence the performance of the workpiece, so that the mechanical property and the piezoelectric property of the workpiece are poor.
As can be seen from the attached figure 2, after the microwave treatment, the powder inside the workpiece is further fused and bonded obviously, unfused powder hardly appears, internal pores are reduced, and the density is improved.
As can be seen from figure 3, the tensile strength of the articles produced by the process of example 1 (right) is superior to the performance of the articles of comparative example 1 (left).
As can be seen from fig. 4, the process of example 1 (above) produced articles having higher dielectric constants than the articles of comparative example 1 (below).
Claims (5)
1. A preparation method of a high-performance 3D printing piezoelectric part is characterized by comprising the following steps:
(1) the polymer/ceramic piezoelectric composite powder is prepared from a polymer and a ceramic material, and the specific method comprises the following steps: uniformly mixing a polymer and a ceramic material, placing the mixture in solid-phase shearing grinding equipment, controlling the temperature of cooling circulating water to be 5-30 ℃ in the grinding process, the grinding pressure to be 10-50MPa, the grinding rotating speed to be 10-100rpm and the grinding times to be 5-20 times, grinding to obtain composite powder, screening the composite powder, and selecting composite powder with the granularity of 100-800 meshes, namely the polymer/ceramic piezoelectric composite material; the polymer is nylon 11, polyvinylidene fluoride or polyvinylidene fluoride-trifluoroethylene; the ceramic material is barium titanate, lead zirconate titanate or potassium niobate;
(2) coating a wave absorbing material on the surface of the polymer/ceramic piezoelectric composite powder in the step (1), and then performing selective laser sintering on the wave absorbing material to obtain a piezoelectric part, wherein the parameters of the selective laser sintering process are as follows: preheating temperature is 150-;
(3) and (3) performing microwave treatment on the piezoelectric part obtained in the step (2), wherein the power of the microwave is 500-1500W, and the microwave time is 20-180 s.
2. The method of making a high performance 3D printed piezoelectric article of claim 1, wherein the polymer in step (1) is a thermoplastic polymer.
3. The method for preparing the high-performance 3D printed piezoelectric part according to claim 1, wherein the step (2) of coating the wave-absorbing material comprises the following specific operations: the wave-absorbing material is placed in an ethanol solution to prepare a uniformly dispersed wave-absorbing material solution, the prepared polymer/ceramic piezoelectric composite powder is added into the wave-absorbing material solution, the mixture is stirred under the ultrasonic condition, so that the wave-absorbing material is uniformly coated on the surface of the polymer/ceramic piezoelectric composite powder, and then the polymer/ceramic piezoelectric composite powder coated with the wave-absorbing material is prepared by filtering and drying.
4. The method according to claim 1, wherein the wave-absorbing material in step (2) is graphene, carbon nanotubes or graphite.
5. A high-performance 3D printed piezoelectric article made by the method of any one of claims 1-4.
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