CN114891165B - Piezoelectric composite photosensitive resin material for three-dimensional photocuring molding printing and preparation method and application thereof - Google Patents
Piezoelectric composite photosensitive resin material for three-dimensional photocuring molding printing and preparation method and application thereof Download PDFInfo
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- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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Abstract
The invention discloses a piezoelectric composite photosensitive resin material for stereolithography printing and a preparation method and application thereof, wherein inorganic piezoelectric filler is subjected to surface chemical modification treatment to uniformly disperse the inorganic piezoelectric filler in a mixed photosensitive resin solvent of ethylene glycol diacrylate and isobornyl acrylate, and a functional piezoelectric composite photosensitive resin material for SLA3D printing is obtained. The inorganic piezoelectric powder is uniformly dispersed in the composite resin as an active material with piezoelectric property, and the composite piezoelectric material after photocuring printing has good flexibility and impact resistance and excellent piezoelectric output property. The piezoelectric part printed and prepared by the method can be used as an energy harvester, a sensor, a driver and the like, and is applied to the field of artificial intelligence.
Description
Technical Field
The invention belongs to the technical field of 3D printing, and particularly relates to a piezoelectric composite photosensitive resin material for three-dimensional photocuring molding printing, and a preparation method and application thereof.
Background
The 3D printing technology is a processing mode different from traditional equal material manufacturing and material reduction manufacturing, and is additive manufacturing technology. The core idea of the 3D printing technology is to convert a complex three-dimensional structure model into a combination of simple two-dimensional cross sections, so that it can be realized by digital design (CAD, 3 DMax) with computer software without using a mold and a machine tool. Compared with the traditional processing technology, the 3D printing technology has the characteristics of high product forming speed, short production period, simple processing technology and the like. 3D printing technology has been developed to date, and various types have been developed, but they can be roughly classified into three types according to their molding characteristics, i.e., laser sintering technology, typified by Selective Laser Sintering (SLS); the fused deposition modeling technique, typified by Fused Deposition Modeling (FDM); the stereolithography technique is represented by Stereolithography (SLA).
Photocuring 3D printing technology is a3D printing technology that was developed earlier. It is based on the principle of photo-polymerization and uses photosensitive liquid resin as printing material. The resin can be cured under light conditions while the unirradiated portions remain liquid. Therefore, the three-dimensional model after printing and molding can be easily and quickly extracted from the resin. The model printed by the photocuring technology has the characteristics of high precision, rapid molding polymerization and the like.
For a piezoelectric energy harvesting device, most of inorganic piezoelectric materials are hard and brittle materials, the intrinsic brittleness of the inorganic materials limits the application of the piezoelectric energy harvesting device, and the flexibility of the device needs to be realized through modified materials and designed structures. The method for solving the flexibility problem of the device mainly comprises the steps of attaching a low-dimensional inorganic piezoelectric material on a flexible substrate, and uniformly dispersing the inorganic piezoelectric material serving as a filler in an organic polymer matrix to construct a flexible composite piezoelectric material. Therefore, the construction and preparation of the flexible composite piezoelectric material become the leading trend, the advantages of the high piezoelectric property of inorganic materials and the flexibility of polymer materials are combined, the comprehensive mechanical property and the electric output property of the material are improved, and the application range and the application field of the piezoelectric material and devices are widened. The inorganic piezoelectric ceramic and the semiconductor material have the characteristics of high piezoelectric coefficient, high dielectric coefficient and the like, and can effectively ensure the flexibility and the high-voltage output characteristic of the piezoelectric energy harvesting device as a composite piezoelectric material prepared by uniformly dispersing a piezoelectric active phase in a flexible polymer.
Disclosure of Invention
The invention aims to provide a piezoelectric composite photosensitive resin material for three-dimensional photocuring molding printing, and a preparation method and application thereof, and the piezoelectric composite photosensitive resin material has the advantages of simple process, flexible design of a printing structure, high flexibility, toughness, high piezoelectric conversion efficiency and the like, and can meet the application requirements of the piezoelectric composite photosensitive resin material in the aspects of various functional devices.
In order to achieve the purpose, the invention provides a piezoelectric composite photosensitive resin material for stereolithography printing, which comprises the following components: the piezoelectric composite photosensitive resin material comprises a monomer solvent, a functional inorganic piezoelectric filler and a photoinitiator, wherein the monomer solvent comprises isobornyl acrylate and polyethylene glycol diacrylate with the mass ratio of 1-9; the mass fraction of the photoinitiator accounts for 1-3% of the piezoelectric composite photosensitive resin material.
Preferably, the functional inorganic piezoelectric filler is a modified material, and the modification process of the functional inorganic piezoelectric filler comprises the following steps:
the inorganic piezoelectric filler is oxidized to prepare hydroxylated inorganic piezoelectric powder, and the hydroxylated inorganic piezoelectric powder reacts with the mixed solution to prepare surface modified inorganic piezoelectric powder which can be dispersed in photosensitive resin, namely the functional inorganic piezoelectric filler.
Preferably, the mixed solution is a mixed solution of 3- (methacryloyloxy) propyl trimethoxy silicon and anhydrous ethanol, and the mass ratio of the hydroxylated inorganic piezoelectric powder to the 3- (methacryloyloxy) propyl trimethoxy silicon and the anhydrous ethanol is 1.25.
Preferably, the inorganic piezoelectric filler is piezoelectric ceramic or piezoelectric semiconductor powder particles having a piezoelectric effect, and the inorganic piezoelectric filler includes at least one of barium titanate, lead zirconate titanate, lead magnesium niobate, zinc oxide, cadmium telluride, and cadmium selenide.
Preferably, the oxidation process specifically comprises the steps of: mixing the inorganic piezoelectric filler with hydrogen peroxide according to the mass ratio of 1-50, stirring and dispersing for 1-2h, then carrying out thermal reaction for 60-100min at 50-80 ℃ to obtain a mixed liquid, naturally cooling to room temperature, and then sequentially filtering, washing and drying to obtain the hydroxylated inorganic piezoelectric powder.
Preferably, the photoinitiator is photoinitiator 184, photoinitiator TPO, photoinitiator 127, photoinitiator 500, photoinitiator 754, photoinitiator MBF or photoinitiator ITX.
Preferably, the light intensity of the piezoelectric composite photosensitive resin material in 3D printing and forming is 150-250 mW/dm 2 。
The invention also discloses a preparation method of the piezoelectric composite photosensitive resin material for three-dimensional photocuring molding printing, which comprises the following steps of: and co-dissolving the functional inorganic piezoelectric filler and a photoinitiator in a monomer solvent, and performing ultrasonic dispersion for 4-6h to obtain the material.
The invention also discloses application of the piezoelectric composite photosensitive resin material, and the piezoelectric composite photosensitive resin material is subjected to photocuring molding and then used as a piezoelectric energy harvesting device.
In summary, the invention has the following advantages:
1. the inorganic piezoelectric powder subjected to surface treatment is beneficial to uniform dispersion in a photosensitive resin liquid solvent, and meanwhile, the interaction between inorganic particles and a polymer matrix is enhanced, and the printability of the piezoelectric composite photosensitive resin material is enhanced.
2. The photo-cured polymerized composite material has excellent flexibility and enhanced mechanical properties by polymerization of a photosensitive resin monomer polyethylene glycol diacrylate (PEGDA) and isobornyl acrylate (IBA).
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and those skilled in the art can also obtain other related drawings based on the drawings without inventive efforts.
FIG. 1 is an X-ray diffraction pattern (XRD) of a Barium Titanate (BTO) powder, an inorganic piezoelectric ceramic material;
FIG. 2 is a Scanning Electron Microscope (SEM) image of a Barium Titanate (BTO) powder as an inorganic piezoelectric ceramic material;
FIG. 3 shows the flexibility of the piezoelectric composite material of the piezoelectric composite photosensitive resin material system printed by SLA and using inorganic piezoelectric ceramic Barium Titanate (BTO) as the filler;
FIG. 4 is a diagram of a structural part of a piezoelectric composite photosensitive resin material system printed by SLA and taking inorganic piezoelectric ceramic Barium Titanate (BTO) as a filler;
fig. 5 is a graph of the open circuit voltage of SLA-printed structural members of piezoelectric composites with inorganic piezoelectric ceramic Barium Titanate (BTO) as filler as piezoelectric energy harvesting devices.
Detailed Description
The principles and features of this invention are described below in conjunction with embodiments, which are included to explain the invention and not to limit the scope of the invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.
Example 1
The embodiment provides a preparation method of a piezoelectric composite photosensitive resin material for stereolithography printing, which comprises the following steps:
(1) Mixing BTO powder and hydrogen peroxide according to a mass ratio of 1;
(2) Adding hydroxylated BTO powder into a mixed solution of 3- (methacryloyloxy) propyl trimethoxy silane (TMSPM) and absolute ethyl alcohol, wherein the mass ratio of the hydroxylated BTO to the TMSPM to the absolute ethyl alcohol is 1.25, and carrying out ultrasonic dispersion reaction for 10h to obtain surface-modified f-BTO powder which can be used for being dispersed in photosensitive resin.
(3) Adding surface-modified f-BTO powder and a photoinitiator (TPO) into a mixed solvent of polyethylene glycol diacrylate (PEGDA) and isobornyl acrylate (IBA), wherein the mass ratio of the PEGDA to the IBA is 5, the f-BTO accounts for 10% of the total mass of the piezoelectric composite photosensitive resin material, the Photoinitiator (TPO) accounts for 1% of the total mass of the piezoelectric composite photosensitive resin material, and the mixed resin is subjected to ultrasonic dispersion for 6h to obtain the piezoelectric composite photosensitive resin material which can be used for SLA3D printing and takes barium titanate as an inorganic piezoelectric filler.
(4) The piezoelectric composite material is prepared by adopting a method for preparing a piezoelectric composite photosensitive resin material with BTO as an inorganic piezoelectric filler through SLA3D printing, and the light intensity in 3D printing molding is 180mW/dm 2 。
The structural member of the composite piezoelectric material taking BTO as the inorganic piezoelectric filler can be used as a piezoelectric energy harvesting device.
As can be seen from fig. 1, the barium titanate of the inorganic piezoelectric filler used is tetragonal barium titanate having piezoelectric effect; as can be seen from fig. 2, the barium titanate powder of the inorganic piezoelectric filler used has a micro flower-like structure; as can be seen from fig. 3, the piezoelectric composite printed by SLA3D has good flexibility.
Test example 1
(1) Piezoelectric composite photosensitive resin material which takes Barium Titanate (BTO) prepared in example 1 as inorganic piezoelectric filler and is suitable for three-dimensional Stereolithography (SLA) printing is adopted to construct piezoelectric parts with three-dimensional structures through SLA3D printing, and the light intensity in printing and forming is 180mW/dm 2 The designed three-dimensional customized structure is shown in fig. 4.
(2) The printed three-dimensional piezoelectric part is subjected to piezoelectric test by using a universal compressor and a Labview system, electrodes are attached to the upper side and the lower side of the part, the compressor performs pressure impact on the part, and a stable voltage output signal is obtained under a 10N cyclic pressure test, wherein the curve chart of the stable voltage output signal is shown in FIG. 5. As can be seen from FIG. 5, the piezoelectric composite material product has a stable output voltage of 4V under the pressure condition of 10N.
Example 2
The embodiment provides a preparation method of a piezoelectric composite photosensitive resin material for stereolithography printing, which comprises the following steps:
(1) Mixing BTO powder and hydrogen peroxide according to a mass ratio of 1;
(2) Adding hydroxylated BTO powder into a mixed solution of TMSPM and absolute ethyl alcohol, wherein the mass ratio of the hydroxylated BTO to the TMSPM to the absolute ethyl alcohol is 1.
(3) Adding the surface modified f-BTO powder and a photoinitiator (184) into a mixed solvent of PEGDA and isobornyl acrylate, wherein the mass ratio of PEGDA to IBA is 5, the f-BTO accounts for 1% of the total mass of the piezoelectric composite photosensitive resin material, the photoinitiator 184 accounts for 1% of the total mass of the piezoelectric composite photosensitive resin material, and ultrasonic dispersion is carried out for 5h, so as to obtain the piezoelectric composite photosensitive resin material which can be used for SLA3D printing and takes barium titanate as an inorganic piezoelectric filler.
(4) The piezoelectric composite material is prepared by adopting a method for preparing a piezoelectric composite photosensitive resin material with BTO as an inorganic piezoelectric filler through SLA3D printing, and the light intensity in 3D printing molding is 150mW/dm 2 。
The method provided in test example 1 was used to obtain a customized three-dimensional piezoelectric device using the barium titanate matrix composite material of example 2 as a raw material, and the highest output voltage obtained under a cyclic pressure of 10N was 1.4V.
Example 3
The embodiment provides a preparation method of a piezoelectric composite photosensitive resin material for stereolithography, which comprises the following steps:
(1) Mixing BTO powder and hydrogen peroxide according to a mass ratio of 1;
(2) Adding hydroxylated BTO powder into a quantitative mixed solution of 3- (methacryloyloxy) propyl trimethoxy silane and absolute ethyl alcohol, wherein the mass ratio of the hydroxylated BTO to the TMSPM to the absolute ethyl alcohol is 1.
(3) Adding surface-modified f-BTO powder and a photoinitiator (127) into a mixed solvent of polyethylene glycol diacrylate and isobornyl acrylate (IBA), wherein the mass ratio of PEGDA to IBA is 5, the mass ratio of f-BTO to IBA is 15 percent of the total mass of the piezoelectric composite photosensitive resin material, the mass ratio of the photoinitiator (127) to the total mass of the piezoelectric composite photosensitive resin material is 1.5 percent, and the mixed resin is subjected to ultrasonic dispersion for 5 hours to obtain the piezoelectric composite photosensitive resin material which can be used for SLA3D printing and takes barium titanate as an inorganic piezoelectric filler.
(4) The piezoelectric composite material prepared by the method for preparing the piezoelectric composite photosensitive resin material with BTO as the inorganic piezoelectric filler by SLA3D printing has the light intensity of 250mW/dm in 3D printing forming 2 。
The highest output voltage of the custom three-dimensional piezoelectric article obtained using the barium titanate matrix composite material of example 3 as a starting material using the method provided in test example 1 was 3.4V at a cyclic pressure of 10N.
Example 4
The embodiment provides a preparation method and application of a piezoelectric composite photosensitive resin material which takes Barium Titanate (BTO) as an inorganic piezoelectric filler and is suitable for stereo photo-curing molding (SLA) printing, and the preparation method comprises the following steps:
(1) Mixing BTO powder and hydrogen peroxide according to a mass ratio of 1;
(2) Adding hydroxylated BTO powder into a quantitative mixed solution of 3- (methacryloyloxy) propyl trimethoxy silane and absolute ethyl alcohol, wherein the mass ratio of the hydroxylated BTO to the TMSPM to the absolute ethyl alcohol is 1.
(3) Adding surface-modified f-BTO powder and a photoinitiator (754) into a mixed solvent of polyethylene glycol diacrylate (PEGDA) and isobornyl acrylate (IBA), wherein the mass ratio of the PEGDA to the IBA is 5, the f-BTO accounts for 10% of the total mass of the piezoelectric composite photosensitive resin material, the photoinitiator (754) accounts for 1.5% of the total mass of the piezoelectric composite photosensitive resin material, and the mixed resin is subjected to ultrasonic dispersion for 6 hours to obtain the piezoelectric composite photosensitive resin material which can be used for SLA3D printing and takes barium titanate as an inorganic piezoelectric filler.
(4) The piezoelectric composite material prepared by the method for preparing the piezoelectric composite photosensitive resin material with BTO as the inorganic piezoelectric filler by SLA3D printing has the light intensity of 220mW/dm in 3D printing forming 2 。
The customized three-dimensional piezoelectric device obtained by using the barium titanate matrix composite material of example 4 as a raw material according to the method provided in test example 1 has a stable output voltage of 2.9V under a cyclic pressure of 10N.
While the present invention has been described in detail with reference to the specific embodiments thereof, it should not be construed as limited by the scope of the present patent. Various modifications and changes may be made by those skilled in the art without inventive step within the scope of the appended claims.
Claims (6)
1. The piezoelectric composite photosensitive resin material for three-dimensional photocuring molding printing is characterized by comprising the following components: the piezoelectric composite photosensitive resin material comprises a monomer solvent, a functional inorganic piezoelectric filler and a photoinitiator, wherein the monomer solvent comprises isobornyl acrylate and polyethylene glycol diacrylate in a mass ratio of 1; the mass fraction of the photoinitiator accounts for 1 to 3 percent of the piezoelectric composite photosensitive resin material;
the functional inorganic piezoelectric filler is a modified material, and the modification process of the functional inorganic piezoelectric filler comprises the following steps:
oxidizing the inorganic piezoelectric filler to obtain hydroxylated inorganic piezoelectric powder, and reacting the hydroxylated inorganic piezoelectric powder with the mixed solution to obtain surface-modified inorganic piezoelectric powder which is dispersed in photosensitive resin and is the functional inorganic piezoelectric filler;
wherein the mixed solution is a mixed solution of 3- (methacryloyloxy) propyl trimethoxy silicon and absolute ethyl alcohol, and the mass ratio of the hydroxylated inorganic piezoelectric powder to the 3- (methacryloyloxy) propyl trimethoxy silicon and the absolute ethyl alcohol is 1.25;
wherein the oxidation process specifically comprises the steps of: mixing the inorganic piezoelectric filler with hydrogen peroxide according to the mass ratio of 1-50, stirring and dispersing for 1-2h, then carrying out thermal reaction for 60-100min at 50-80 ℃ to obtain a mixed liquid, naturally cooling to room temperature, and then sequentially filtering, washing and drying to obtain the hydroxylated inorganic piezoelectric powder.
2. The piezoelectric composite photosensitive resin material for stereolithographic printing according to claim 1, wherein said inorganic piezoelectric filler is a piezoelectric ceramic or a piezoelectric semiconductor powder particle having a piezoelectric effect, and said inorganic piezoelectric filler comprises at least one of barium titanate, lead zirconate titanate, lead magnesium niobate, zinc oxide, cadmium telluride, and cadmium selenide.
3. The piezoelectric composite photosensitive resin material for stereolithographic printing as claimed in claim 1, wherein said photoinitiator is photoinitiator 184, photoinitiator TPO, photoinitiator 127, photoinitiator 500, photoinitiator 754, photoinitiator MBF or photoinitiator ITX.
4. The piezoelectric composite photosensitive resin material for stereolithography printing according to claim 1, wherein the light intensity of said piezoelectric composite photosensitive resin material in 3D printing lithography is 150 to 250mW/dm 2 。
5. The method for preparing the piezoelectric composite photosensitive resin material for stereolithographic printing as claimed in any one of claims 1 to 4, comprising the steps of:
and co-dissolving the functional inorganic piezoelectric filler and a photoinitiator in a monomer solvent, and performing ultrasonic dispersion for 4-6h to obtain the material.
6. The use of the piezoelectric composite photosensitive resin material for stereolithographic printing as claimed in any one of claims 1 to 4, wherein the piezoelectric composite photosensitive resin material is used as a piezoelectric energy harvesting device after being photocured and patterned.
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