CN110713717A - High-temperature-resistant dopamine-coated barium titanate/polyimide (BT @ PDA/PI) dielectric nano composite film - Google Patents
High-temperature-resistant dopamine-coated barium titanate/polyimide (BT @ PDA/PI) dielectric nano composite film Download PDFInfo
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Abstract
A high-temperature-resistant dopamine-coated barium titanate/polyimide (BT @ PDA/PI) dielectric nano composite film is prepared from 93-99vol% of Polyimide (PI) as a matrix, 1-7vol% of dopamine-coated barium titanate nanoparticles (BT @ PDA) as a filler, wherein the volume ratio of the barium titanate nanoparticles (BT) to the dopamine (PDA) in the filler is (4-5): 1; the preparation method comprises the steps of coating BT nano particles with dopamine hydrochloride solution in the environment of hydroxymethyl aminomethane buffer solution (Tris) to prepare BT @ PDA nano particles with a core-shell structure, mechanically blending the BT @ PDA nano particles with PAA solution, removing bubbles in a BT @ PDA/PAA blending system in vacuum, coating the mixture to form a film, and performing high-temperature hot imidization to obtain the composite dielectric film. After the dopamine layer coats the BT nano particles, the distribution of the BT particles in a PI matrix can be improved, the agglomeration among the BT nano particles is reduced, the interface bonding between the BT nano particles and the PI matrix is enhanced, and the defects in the composite material are reduced, so that the BT @ PDA/PI nano composite film has excellent dielectric properties while maintaining good mechanical properties.
Description
Technical Field
The invention relates to a high-temperature-resistant polyimide dielectric nanocomposite and a preparation method thereof, in particular to a ceramic particle/polyimide nanocomposite film with high dielectric property and a preparation method thereof, belonging to the field of preparation of high-performance dielectric composites.
Background
Applications in the field of avionics and automotive industry, the underground oil and gas exploration industry, and advanced propulsion systems require long-term operation of dielectric materials at temperatures of 150 ℃ and even higher. At present, a commonly used polymer dielectric material is biaxially oriented polypropylene (BOPP), which has excellent high breakdown strength (700 MV/m) and extremely low dissipation factor (0.0002), but its relatively low dielectric constant (2.2) and limited working temperature (below 105 ℃) limit its application in the field of high-temperature dielectric energy storage. Therefore, it is required to develop a polymer dielectric thin film capacitor having high dielectric constant and high temperature resistance in an extreme environment. Polyimide (PI) is a special engineering plastic with very excellent comprehensive performance, has high glass transition temperature (Tg >250 ℃), excellent thermal stability and much better high-temperature resistance than BOPP, and is considered to be one of the most potential dielectric films for high-temperature capacitors. Compared with ceramic dielectric materials, PI has quite low dielectric loss factor and high dielectric breakdown strength, but the low energy storage density caused by the relatively low dielectric constant greatly limits the application of PI in the high-temperature dielectric energy storage field.
Generally, to increase the dielectric constant of PI, ceramic nanofillers with high dielectric constants, such as Barium Titanate (BT), titanium dioxide (TiO), are incorporated into the matrix2) Barium strontium titanate (Ba)1-xSrxTiO3) Etc., are currently the most common and effective methods. Dang et al prepared a BT/PI nanocomposite film by in-situ polymerization, and the dielectric constant of the composite film containing 40vol% of BT nanoparticles was raised to 20, and the dielectric breakdown strength was only 67 kV/mm. (Z.M. Dang, Y.Q. Lin, H.P. Xu, C.Y.Shi, S.T. Li, J.B. Bai, adv. Funct. mater. (2008) 18, 1509-. They also reported a Calcium Copper Titanate (CCTO)/PI hybrid film with a high dielectric constant (49.1) and good thermal stability. (Z.M. Dang, T. Zhou, S.H. Yao, J.K. Yuan, J.W. Zha, H.T. Song, J.Y. Li, Q. Chen, W.T. Yang, J.B. Bai. adv. Mater, 2009) 21, 2077-. Ba Bayer et al0.7Sr0.3TiO3The nano-crystal is blended with PAA, and the composite material prepared by adopting an in-situ polymerization method shows a remarkably improved dielectric constant. (C.W. Beier, J.M. Sanders, R.L. Brutchey, J. Phys. chem. C (2013) 117, 6958-. The ceramic nano particles are directly introduced into the PI, so that the dielectric constant of the PI-based composite material can be effectively improved, but the nano particles are easy to agglomerate, are not easy to disperse uniformly in a PI matrix, and introduce the problems of interface and the like, so that the dielectric breakdown strength of the PI is greatly reduced.
Research shows that the improved coating of the surface of the nano-particles, especially the construction of the nano-filler with a core-shell structure, can adjust the interface polarization inside the composite material after being introduced into a polymer matrix, and weaken the permeation current in the composite material. The dielectric constant of the composite material is improved, and the dielectric breakdown strength is kept or even improved, so that the energy storage density is improved. Lin et al utilize TiO2Coated barium titanate nanofibers (BT @ TiO)2NFs) was compounded with polyvinylidene fluoride (PVDF), 3vol% BT @ TiO2The dielectric constant of the NFs/PVDF composite material reaches 17.5, and 10.94J/cm is obtained under the electric field of 360 kV/mm3High energy storage density. (X, Lin, P, Hu, Z, Jia, S, Gao, J, Mater, chem. A (2016)4, 2314-. Pan et al incorporated BaTiO into PVDF by incorporation of BaTiO3@Al2O3NFs，5vol% BT@Al2O3The dielectric constant of NFs/PI nano composite film is up to 15.5, and under the electric field of 400kV/mm, the energy storage density of the material is obviously improved to 12.18J/cm3。（Z. Pan,L. Yao, J. Zhai, B. Shen, S. Liu, H. Wang, J. Liu,J. Mater. Chem. A. (2016)4,13259-13264）。
Chinese patent CN108794813A discloses a composite filler of polyimide and barium titanate and a preparation method thereof, a composite dielectric material and a preparation method thereof. The method adopts an in-situ polymerization method to prepare the core-shell structure nano-particles of BT @ PI, and then the BT @ PI nano-particles are used as a filler to be blended with polyvinylidene fluoride (PVDF) to prepare the BT @ PI/PVDF composite material. The matrix material of the patent is PVDF, and the temperature resistance of the composite film is still poor.
Disclosure of Invention
The invention aims to provide a high-temperature-resistant BT @ PDA/PI dielectric nano composite film and a preparation method thereof. The BT @ PDA/PI nano composite film is prepared by taking PI with excellent heat resistance as a matrix and BT @ PDA nano particles as a filler. The film has the advantages of high dielectric constant, high breakdown strength, high temperature resistance, high mechanical property and the like.
The method is implemented specifically as follows: the high-temperature-resistant BT @ PDA/PI dielectric nano composite film is characterized in that 93-99vol% of PI is used as a substrate, 1-7vol% of BT @ PDA nano particles are used as a filler, and the volume ratio of Barium Titanate (BT) nano particles to Dopamine (DA) in the filler is 4-5: 1;
the preparation method comprises the following steps: in the environment of hydroxymethyl aminomethane buffer solution (Tris), coating BT nano particles with dopamine hydrochloride solution to prepare BT @ PDA nano particles with a core-shell structure, then mechanically blending the BT @ PDA nano particles with PAA solution, removing bubbles in a BT @ PDA/PAA blending system in vacuum, coating the mixture to form a film, and then carrying out high-temperature thermal imidization to obtain the composite dielectric film. In the composite dielectric film, the surface of the BT nano-particles has a dopamine shell layer, so that the interface bonding between BT and a PI substrate is improved, the agglomeration among the BT nano-particles is reduced, and the defects in the composite film are reduced, thereby endowing the composite film with good mechanical properties and excellent dielectric properties at high temperature.
The barium titanate nano-particles are barium titanate nano-particles with the average particle size of 50nm-100 nm.
The dopamine hydrochloride of the present invention is any commercially available dopamine hydrochloride.
In the preparation method, the preparation of the BT @ PDA nano-particles comprises the following steps: blending BT nano particles with 0.1mol/L hydroxymethyl aminomethane buffer (Tris) and deionized water at room temperature, and magnetically stirring to uniformly disperse a mixed system; turning off magnetic stirring, and adding anhydrous ethanol and dopamine hydrochloride powder into the system; starting magnetic stirring until the system turns into black brown; filtering, and stirring and washing the obtained product by using a 1:1 ethanol water solution; standing, centrifuging and washing, and retaining the lower-layer precipitate; and (3) repeating centrifugation, stirring and washing until the pH value of the mixed system is close to 7, and finally drying the obtained product in an oven to obtain BT @ PDA nano-particles, wherein the dosage ratio of the BT nano-particles, Tris buffer solution, deionized water, absolute ethyl alcohol and dopamine hydrochloride is 3 g: 100 mL: 200 mL: 100 mL: 1 g. Tris buffer solution, deionized water and absolute ethyl alcohol are used for forming a coating buffer environment, the dosage of dopamine hydrochloride is usually added to ensure that BT nanoparticles can be fully coated, the dosage ratio of BT nanoparticles, Tris buffer solution, deionized water, absolute ethyl alcohol and dopamine hydrochloride and the concentration of Tris buffer solution can be adjusted according to common knowledge, BT @ PDA after full coating is detected, and the volume ratio of Barium Titanate (BT) nanoparticles to dopamine (PDA) is 4-5: 1.
in the preparation method, the polyamide acid (PAA) solution can be a finished product, or the PAA solution can be prepared by an in-situ polymerization method, the solid content of a solution system is 20 ~ 25%, the preparation of the PAA solution by the in-situ polymerization method is the prior method, a three-neck flask with mechanical stirring is placed in an ice-water bath, nitrogen is introduced, diamine powder is added into the flask, a proper amount of N, N-dimethylacetamide (DMAc) solvent after dehydration and purification is added into the flask by using an injector, mechanical stirring is started to fully dissolve the diamine monomer, the dianhydride monomer with the amount of diamine and other substances is added into the flask after the diamine monomer is fully dissolved, a proper amount of DMAc solvent is added to fully dissolve the dianhydride monomer, the mechanical stirring is carried out for 12 hours in the ice-water bath under the nitrogen atmosphere to obtain a viscous tawny PAA solution, the amount of the DMAc solvent is added and adjusted to keep the solid content of the system at 20 ~ 25%, and the polyimide synthetic monomer is any commercially available diamine and dianhydride monomer.
In the preparation method, PAA solution and BT @ PDA nano particles are mechanically blended, namely, a certain amount of BT @ PDA powder is added into a proper amount of DMAc solvent according to a formula, and ultrasonic treatment is carried out; and adding the BT @ PDA suspension subjected to ultrasonic treatment into the PAA solution, and vigorously stirring to obtain a viscous black-brown BT @ PDA/PAA blending system. The ultrasonic treatment time of the BT @ PDA powder in the DMAc solvent and the stirring time of the BT @ PDA suspension in the PAA solution are adjusted according to the actual situation so as to achieve a good blending effect.
In the preparation method, a BT @ PDA/PAA blending system is vacuumized to remove bubbles, coated on a coating machine to form a film, then transferred to a high-temperature air-blast drying oven to be thermally imidized, and finally naturally cooled to room temperature, so that the BT @ PDA/PI nano composite film is obtained. The temperature during thermal imidization was controlled as follows: heating from room temperature to 300 deg.C at a heating rate of 2 deg.C/min, and maintaining at 100 deg.C, 200 deg.C and 300 deg.C for 60 min.
The dielectric constant, dielectric loss and temperature stability of the sample are tested by using an Alpha-A type wide-frequency dielectric impedance spectrometer. The dielectric breakdown voltage performance of the sample is tested by adopting a PRECISION WORKSTATIO type dielectric breakdown voltage tester.
The invention has the following advantages:
1) the components of the patent are simple, and the selected raw materials are all commercial products.
2) When the addition amount of BT @ PDA is lower, the dielectric constant of the composite material can be obviously improved, and meanwhile, the composite material has excellent mechanical properties.
3) The method has the advantages of simple process, simple equipment and low cost.
4) The method is easy to implement, simple in equipment maintenance and cleaning and free of harsh requirements on environmental conditions.
Drawings
FIG. 1 is a graph showing the change of dielectric constant with temperature (at 100 Hz) of example 1 ~ 4 and comparative example 1 ~ 5.
FIG. 2 is a graph of the mechanical properties of example 1 ~ 4 and comparative example 1 ~ 5 as a function of filler content, showing (a) tensile strength and (b) elongation at break.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The following examples are given to illustrate the present invention and it should be noted that the following examples are only for illustrative purposes and should not be construed as limiting the scope of the present invention, and the non-essential modifications and variations of the present invention by those skilled in the art according to the above disclosure will still fall within the scope of the present invention.
Example 1 ~ 4:
(1) preparing BT @ PDA nano-particles: at normal temperature, 3gBT nanoparticles (Shanghai Aladdin Biotechnology Co., Ltd., purity 99.9%) and 100mL of 0.1mol/L hydroxymethyl aminomethane buffer (Tris) (Beijing chemical plant product, purity 99%) were mixed with 200 mL of deionized water, and stirred magnetically for 20 min; adding 100mL of absolute ethyl alcohol and 1g of dopamine hydrochloride solution (a product of Beijing chemical plant, the purity is 98%) into the system, and continuously stirring and coating for 6 hours until the system turns into black brown; filtering, and washing the obtained product by using a 1:1 ethanol water solution; standing, centrifuging and washing, and retaining the lower-layer precipitate; and repeating the centrifugation process for 5 times until the pH value of the system is close to 7, and finally putting the obtained product in an oven to dry for 8 hours at 60 ℃ to obtain the BT @ PDA nano-particles.
(2) Synthesis of Polyamic acid (PAA): PAA solution is prepared by adopting an in-situ polymerization method. A three-necked flask equipped with mechanical stirring was placed in an ice-water bath and nitrogen was passed through. The flask was charged with 5 mmol of 4,4，Powder of dimethyl diphenyl ether (ODPA, product of shanghai alatin biochemistry technologies ltd., purity 98%), 4 ml of water-removed and purified N, N-dimethylacetamide (DMAc) solvent was added to the flask using a syringe, and mechanical stirring was started to sufficiently dissolve the ODA. After ODA was completely dissolved, 5 mmol of a biphenyl ether dianhydride (ODPA, a product of Shanghai Arlatin Biotechnology Co., Ltd., purity 98%) monomer was added to the flask, and 4 ml of DMA solvent was added to dissolve ODPA sufficiently. Mechanically stirring for 12 hours in ice water bath under nitrogen atmosphere,and (3) obtaining a viscous tawny PAA solution, and adding a proper amount of DMAc solvent if the viscosity of the system is too high in the reaction process, wherein the solid content of the system is kept at 20 ~ 25%.
(3) Preparation of BT @ PDA/PAA blending system: the content of BT @ PDA particles is adjusted to be 1vol%, 3vol%, 5vol% and 7vol%, 0.1144g, 0.3503g, 0.5962g and 0.8526g of BT @ PDA powder are respectively added into a proper amount of DMAc solvent according to the content of BT @ PDA nano particles, and ultrasonic treatment is carried out for 1 h. And adding the BT @ PDA suspension subjected to ultrasonic treatment into the PAA solution, and stirring vigorously for 12 hours to obtain a viscous black-brown BT @ PDA/PAA blending system.
(4) Preparing a BT @ PDA/PI composite film: and vacuumizing the BT @ PDA/PAA blending system to remove bubbles, and coating the BT @ PDA/PAA blending system on a coating machine to form a film so as to obtain the BT @ PDA/PAA composite film. And then transferred to a high-temperature air-blast drying oven for thermal imidization: heating from room temperature to 300 deg.C at a heating rate of 2 deg.C/min, and maintaining at 100 deg.C, 200 deg.C and 300 deg.C for 60 min. And finally, naturally cooling to room temperature to obtain the BT @ PDA/PI composite film.
Example 5 ~ 8 preparation of BT @ PDA nanoparticles the stir coating time was extended to 10h, with the other process conditions being the same.
Comparative examples 1 to 5, BT nanoparticles were first blended with PAA using the same process conditions, and then BT/PI composite films were prepared with filler contents of 0, 1vol%, 3vol%, 5vol%, and 7vol%, respectively, as comparative examples. The specific formula is shown in table one:
TABLE A formulation of example 1 ~ 8 and comparative example 1 ~ 5
Table two dielectric property test results for example 1 ~ 8 and comparative example 1 ~ 5:
as can be seen from the graph, when the BT @ PDA content is 1 part (example 1), at a frequency of 100Hz, the dielectric constant of the PI composite film is 4.4, which is 25% higher than that of pure PI (comparative example 1), the dielectric loss is only 0.006, which is substantially equal to that of pure PI, the dielectric breakdown field strength can reach 315 kV/mm, which is 20 kV/mm higher than that of pure PI, the dielectric constant of the composite film is almost unchanged within a range of 25 ~ 200 ℃ (as shown in FIG. 1), meanwhile, the BT @ PDA/PI composite material also has excellent mechanical properties (as shown in FIG. 2), under the same filler content, the tensile strength of the BT @ PDA/PI composite film is improved by about 4 MPa compared with that of the BT/PI composite film, and the elongation at break is improved by about 40%, and when the BT @ PDA/PI composite material is prepared, the performance of the composite film is not greatly influenced by the extension of the stirring coating time.
Claims (8)
1. The high-temperature-resistant polydopamine-coated barium titanate/polyimide (BT @ PDA/PI) dielectric nano composite film is characterized in that the raw material of the composite film is composed of 93-99vol% of Polyimide (PI) as a matrix and 1-7vol% of polydopamine-coated barium titanate nanoparticles (BT @ PDA) as a filler, wherein the volume ratio of Barium Titanate (BT) nanoparticles to Dopamine (DA) in the filler is 4-5: 1;
the preparation method comprises the following steps: in the environment of hydroxymethyl aminomethane buffer solution (Tris), coating BT nano particles by dopamine hydrochloride solution to prepare BT @ PDA nano particles with a core-shell structure, then mechanically blending the BT @ PDA nano particles with polyamide acid (PAA) solution, removing bubbles in a BT @ PDA/PAA blending system in vacuum, coating the mixture to form a film, and then carrying out high-temperature thermal imidization to obtain the composite dielectric film.
2. The high temperature BT @ PDA/PI dielectric nanocomposite film as claimed in claim 1, wherein the barium titanate nanoparticles are barium titanate nanoparticles having an average particle size of 50nm to 100 nm.
3. The high temperature BT @ PDA/PI dielectric nanocomposite film as claimed in claim 1, wherein in the preparation method, the BT @ PDA nanoparticles are prepared by: blending BT nano particles with 0.1mol/L hydroxymethyl aminomethane buffer (Tris) and deionized water at room temperature, and magnetically stirring to uniformly disperse a mixed system; turning off magnetic stirring, and adding anhydrous ethanol and dopamine hydrochloride powder into the system; starting magnetic stirring until the system turns into black brown; filtering, and stirring and washing the obtained product by using a 1:1 ethanol water solution; standing, centrifuging and washing, and retaining the lower-layer precipitate; and (3) repeating centrifugation, stirring and washing until the pH value of the mixed system is close to 7, and finally drying the obtained product in an oven to obtain BT @ PDA nano-particles, wherein the dosage ratio of the BT nano-particles, Tris buffer solution, deionized water, absolute ethyl alcohol and dopamine hydrochloride is 3 g: 100 mL: 200 mL: 100 mL: 1 g.
4. The high temperature BT @ PDA/PI dielectric nanocomposite film as claimed in claim 1, wherein the polyamic acid (PAA) solution is prepared as a finished product or as a PAA solution by in situ polymerization, and the solid content of the solution system is 20 ~ 25%.
5. The high temperature resistant BT @ PDA/PI dielectric nanocomposite film as claimed in claim 4, wherein PAA solution is prepared by in situ polymerization, a three-neck flask equipped with mechanical stirring is placed in an ice water bath, and nitrogen is introduced; adding diamine powder into a flask, adding a proper amount of N, N-dimethylacetamide (DMAc) solvent subjected to water removal and purification into the flask by using an injector, and starting mechanical stirring to fully dissolve diamine monomers; after the diamine monomer is completely dissolved, adding dianhydride monomer in the amount equal to that of diamine and the like into the flask, and then adding a proper amount of DMAc solvent to fully dissolve the dianhydride monomer; mechanically stirring in ice water bath under nitrogen atmosphere for 12h to obtain viscous tawny PAA solution.
6. The high temperature BT @ PDA/PI dielectric nanocomposite film as claimed in claim 1, wherein the mechanical blending of the PAA solution and BT @ PDA nanoparticles is formulated by adding a certain amount of BT @ PDA powder to a proper amount of DMAc solvent, sonicating; and adding the BT @ PDA suspension subjected to ultrasonic treatment into the PAA solution, and vigorously stirring to obtain a viscous black-brown BT @ PDA/PAA blending system.
7. The high temperature resistant BT @ PDA/PI dielectric nanocomposite film as claimed in claim 1, wherein in the preparation method, a BT @ PDA/PAA blending system is vacuumized to remove bubbles, coated on a coating machine to form a film, then transferred to a high temperature air blowing drying oven to be subjected to thermal imidization, and finally naturally cooled to room temperature to obtain the BT @ PDA/PI nanocomposite film.
8. The high temperature BT @ PDA/PI dielectric nanocomposite film as claimed in claim 7, wherein the temperature during thermal imidization is controlled as follows: heating from room temperature to 300 deg.C at a heating rate of 2 deg.C/min, and maintaining at 100 deg.C, 200 deg.C and 300 deg.C for 60 min.
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