CN113999461B - Preparation method of modified composite film based on poly-tetramethyl-pentene-barium titanate nano particles - Google Patents
Preparation method of modified composite film based on poly-tetramethyl-pentene-barium titanate nano particles Download PDFInfo
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Abstract
The preparation method based on the polytetramethyl pentene-barium titanate nano particle modified composite film comprises the steps of weighing polytetramethyl pentene with the first preset mass fraction and dissolving the polytetramethyl pentene in a non-polar polymer solvent; weighing barium titanate nanoparticles with a second predetermined mass fraction, reacting in a NaOH solution to obtain a BaTiO3 hydroxylated solution, cleaning, drying, grinding and sieving to obtain hydroxylated BaTiO3 particles BaTiO3-OH; weighing BaTiO3 particles BaTi03-OH with a third predetermined mass fraction and a coupling agent, reacting in a toluene environment to obtain a BaTiO3 graft solution, cleaning, drying, grinding and sieving to obtain particles BaTiO3-KH570; and weighing a fourth mass fraction of the BaTiO3-KH570 particles, adding the polytetramethylene monopentene solution into the solution, stirring the solution to obtain a mixed solution A, and performing vacuum drying to obtain the polytetramethylene monopentene-barium titanate nanoparticle modified composite film.
Description
Technical Field
The invention relates to the technical field of composite film materials of film capacitors, in particular to a preparation method of a composite film modified based on poly-tetramethyl-pentene-barium titanate nano particles.
Background
With the continuous development of power systems, the role of power capacitors in power systems is becoming more important. In the operation of the power capacitor, due to the working conditions and the heat dissipation problem of the power capacitor, the local over-high temperature of the power capacitor causes the insulation failure in the capacitor, and the operation stability of a power system is reduced. At present, the most commonly used power capacitor material is BOPP (biaxially oriented polypropylene), which is low in cost and easy to process, but has poor high-temperature resistance, low melting initial temperature (85 ℃ -100 ℃), low long-time working temperature (70 ℃ -80 ℃), and low dielectric constant (about 2.2), and currently, nano doping is used as a widely applied means for increasing the dielectric constant, so that the dielectric constant of the composite material can be effectively increased, however, the dielectric constant of the nano filler and the organic matrix is greatly different, and the filler is seriously agglomerated, so that the breakdown strength is seriously reduced compared with that of a pure polymer matrix due to electric field distribution distortion while the dielectric constant is increased, so that a thermally stable material with large dielectric constant and small dielectric loss and capable of resisting high temperature is required to be found, and the breakdown field strength is improved by modifying the doped nano particles.
In view of the above drawbacks and the further needs in the art, those skilled in the art will be able to develop a high temperature resistant high dielectric low loss composite film.
The above information disclosed in this background section is only for enhancement of understanding of the background of the invention and therefore it may contain information that does not form the prior art that is already known to a person of ordinary skill in the art.
Disclosure of Invention
The invention aims to provide a preparation method of a modified composite film based on polytetramethylene monopentene-barium titanate nano particles, so as to provide a high-temperature-resistant high-dielectric-property low-loss composite film.
In order to achieve the above purpose, the invention provides the following technical scheme:
the preparation method of the modified composite film based on the polytetramethylene monopentene-barium titanate nano particles comprises the following steps:
s100, weighing the polytetramethylene monopentene with the-predetermined mass fraction, dissolving the polytetramethylene monopentene in a nonpolar polymer solvent, and dissolving the polytetramethylene monopentene under the condition of uniform stirring to obtain a polytetramethylene monopentene solution;
s200, weighing barium titanate nanoparticles with a second predetermined mass fraction, reacting in a NaOH solution to obtain a BaTiO3 hydroxylated solution, cleaning, drying, grinding and sieving to obtain hydroxylated BaTiO3 particles BaTiO3-OH;
step S300, weighing BaTiO3 particles BaTiO3-OH with a third preset mass fraction and a coupling agent, reacting in a toluene environment to obtain a BaTiO3 graft solution, cleaning, drying, grinding and sieving to obtain particles BaTiO3-KH570;
s400, weighing a fourth mass fraction of BaTiO3-KH570 particles, adding the solution of the polytetramethylene monopentene, and stirring to obtain a mixed solution A;
and S500, drying the mixed solution A in vacuum to obtain the polytetramethylene monopentene-barium titanate nano particle modified composite film.
In the preparation method of the polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film, in step S100, the polytetramethylene monopentene with the first predetermined mass fraction range of 5g-10g is dissolved in 50ml-100ml of non-polar solvent.
In the preparation method of the polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film, the nonpolar organic solvent comprises cyclohexane or carbon tetrachloride.
In the preparation method of the modified composite film based on the polytetramethyl monopentene-barium titanate nano particles, in the step S100, the stirring condition comprises stirring for 5-8 hours at the temperature of 40-85 ℃ and at the rotating speed of 250-450 r/min.
In the preparation method of the modified composite film based on the polytetramethyl monopentene-barium titanate nano particles, in step S200, the barium titanate nano particles with the second preset mass fraction range of 5-20g are added into a NaOH solution with the concentration of 5-10 mol/L.
In the preparation method of the polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film, in step S200, naOH solution is stirred for 20-24 hours at 100-120 ℃ and 1000r/min-1200r/min to obtain a BaTiO3 hydroxylated solution, the nanoparticles are washed for 3-5 times by absolute ethyl alcohol and then are put into a vacuum oven to be dried for 24-48 hours at 60-80 ℃, and then the dried BaTiO3-OH particles are ground and sieved by a 200-mesh screen to obtain the hydroxylated BaTiO3 particles BaTiO3-OH.
In the preparation method of the polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film, in step S300, the third predetermined mass fraction range is 5-20g BaTiO3 particles BaTiO3-OH, and 2-5ml of coupling agent is added into 50-200 ml of toluene.
In the preparation method of the modified composite film based on the polytetramethyl monopentene-barium titanate nano particles, the coupling agent is KH570 silane coupling agent.
In the preparation method of the polytetramethyl pentene-barium titanate nanoparticle-based modified composite film, in step S300, a toluene solution is stirred for 20-24 hours at the temperature of 60-90 ℃ and the rotating speed of 1000r/min-1200r/min to obtain a BaTiO3 grafted KH570 solution, the solution is washed for 3-5 times by toluene, nano-scale particles BaTiO3-KH570 are placed into a vacuum oven to be dried for 24-48 hours at the temperature of 60-80 ℃, then the dried particles BaTiO3-KH570 are ground and sieved by a 200-mesh screen to obtain the particles BaTiO3-KH570 with KH570 treated on the surface.
In the preparation method of the polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film, the BaTiO3-KH570 with the fourth mass fraction ranging from 5wt% to 20wt% is added into the polytetramethylene monopentene solution.
In the technical scheme, the preparation method of the modified composite film based on the polytetramethylene monopentene-barium titanate nano particles, provided by the invention, has the following beneficial effects: the preparation method of the polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film adopts PMP as a polymer matrix, has excellent high-temperature dielectric property, can keep high breakdown strength, stable dielectric constant and low dielectric loss at the temperature of more than 80 ℃, and has good high-temperature resistance. According to the invention, by doping the modified barium titanate nanoparticles, PMP has low dielectric loss and low dielectric constant, and the overall dielectric constant needs to be improved by doping. In the following description of the embodiments, the inventors are based on that barium titanate nanoparticles can significantly increase the dielectric constant with less influence on the dielectric loss. In addition, the barium titanate nanoparticles treated by KH570 improve the compatibility of organic-inorganic interfaces, so that the nanoparticles are distributed in the matrix more uniformly, and the distortion of the electric field intensity is reduced. Therefore, the inventor fully utilizes the PMP matrix material with small dielectric loss and the modified barium titanate nano particles which are beneficial to improving the overall dielectric constant and the breakdown strength, and compounds the PMP matrix material and the modified barium titanate nano particles to obtain the composite film with high dielectric constant, low dielectric loss and high breakdown strength at high temperature.
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In order to more clearly illustrate the embodiments of the present application or technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only the embodiments described in the present application, and other drawings can be obtained by those skilled in the art according to the drawings.
FIG. 1 is an infrared spectrum of barium titanate nanoparticles before and after treatment with KH570 silane coupling agent in the method for preparing a polytetramethyl monopentene-barium titanate nanoparticle modified composite film according to the present invention;
FIG. 2 is a SEM (scanning Electron microscope) cross-section of a 10wt% barium titanate/PMP composite film before and after being treated with a KH570 silane coupling agent based on the preparation method of the polytetramethyl monopentene-barium titanate nanoparticle modified composite film;
FIG. 3 is a graph of dielectric spectrum and loss of a 10wt% barium titanate/PMP composite film which is not treated with a KH570 silane coupling agent and is prepared based on a method for preparing a polytetramethyl monopentene-barium titanate nanoparticle modified composite film according to the present invention at a temperature of-40 to 180 ℃;
FIG. 4 is a graph of dielectric spectrum and loss of a 10wt% barium titanate/PMP composite film treated with KH570 silane coupling agent at-40-180 ℃ based on a preparation method of a polytetramethyl monopentene-barium titanate nanoparticle modified composite film according to the present invention;
FIG. 5 is a graph showing the change of dielectric constant before and after treatment in the method for preparing a polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film according to the present invention;
FIG. 6 is a graph showing the dielectric constant and dielectric loss of the poly (tetramethylmonopentene-barium titanate) nanoparticle composite film according to the method for preparing a poly (tetramethylmonopentene-barium titanate) nanoparticle-modified composite film of the present invention, as a function of temperature, wherein the amount of barium titanate doped is 10wt%;
FIG. 7 is a graph showing the breakdown strength of a barium titanate/PMP composite film before and after treatment, which is 10wt% based on the preparation method of the polytetramethyl monopentene-barium titanate nanoparticle modified composite film according to the present invention, at 20 ℃;
FIG. 8 is a graph showing the breakdown strength of a barium titanate/PMP composite film before and after treatment, which is 10wt% based on the preparation method of the polytetramethyl monopentene-barium titanate nanoparticle modified composite film according to the present invention, at 20 ℃.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are part of the embodiments of the present invention, not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Thus, the following detailed description of the embodiments of the present invention presented in fig. 1-8 of the drawings is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations or positional relationships based on those shown in the drawings, merely for convenience of description and simplicity of description, and do not indicate or imply that the device or element so referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention.
Furthermore, the terms "first", "second", and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or to implicitly indicate the number of technical features indicated. Thus, a feature defined as "first-" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the present invention, unless otherwise explicitly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrated; they may be directly connected or indirectly connected through intervening media, or may be connected through the use of two elements or the interaction of two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly specified or limited, the first feature "on" or "under" the second feature may comprise the first and second features being in direct contact, or the first and second features may be in contact not directly but via another feature in between. Also, the first feature being "on," "above" and "over" the second feature includes the first feature being directly on and obliquely above the second feature, or merely indicating that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature includes the first feature being directly under and obliquely below the second feature, or simply meaning that the first feature is at a lesser elevation than the second feature.
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings. A process for preparing the composite film modified by nano particles based on polytetramethyl pentene-barium titanate includes such steps as preparing the composite film,
s100, weighing the polytetramethylene monopentene with the-predetermined mass fraction, dissolving the polytetramethylene monopentene in a nonpolar polymer solvent, and dissolving the polytetramethylene monopentene under the condition of uniform stirring to obtain a polytetramethylene monopentene solution;
s200, weighing barium titanate nanoparticles with a second preset mass fraction to react in a NaOH solution to obtain a BaTiO3 hydroxylated solution, and cleaning, drying, grinding and sieving to obtain hydroxylated BaTiO3 particles BaTiO3-OH;
step S300, weighing BaTiO3-OH particles with a third predetermined mass fraction and a coupling agent, reacting in a toluene environment to obtain a BaTiO3 graft solution, cleaning, drying, grinding and sieving to obtain BaTiO3-KH570 particles;
s400, weighing a fourth mass fraction of BaTiO3-KH570 particles, adding the solution of the polytetramethylene monopentene, and stirring to obtain a mixed solution A;
and S500, drying the mixed solution A in vacuum to obtain the polytetramethylene monopentene-barium titanate nano particle modified composite film.
According to the invention, PMP is selected as a polymer matrix to ensure good high temperature resistance, and then barium titanate nanoparticles treated by KH570 coupling agent are added to improve the dielectric constant of the polymer film, so that the high temperature resistance, high dielectric loss and high breakdown field strength of the composite material are realized. When the doping amount of the nano barium titanate after being doped with KH570 is 10wt%, the dielectric constant is increased from 2.15 of pure PMP to 3.03, and the increase ratio is 40.9%, while the dielectric constant of the nano barium titanate composite material without being processed is only 2.62 when the doping amount is 10 wt%. And the dielectric loss in the temperature range of 20-180 ℃ is kept below 0.0025; meanwhile, compared with the untreated BT particles, the breakdown field strength of the composite material can be improved, the breakdown field strength is improved from 319.0MV/m to 366.2MV/m (improved by 14.7%) under the doping concentration of 10wt%, the requirement of a power capacitor can be met, and the high-dielectric and high-temperature-resistant performance of the film capacitor is improved.
In a preferred embodiment of the preparation method of the composite film modified based on the polytetramethyl monopentene-barium titanate nano particles, in step S100, the first predetermined mass fraction of the polytetramethyl monopentene in the range of 5g to 10g is dissolved in 50ml to 100ml of the non-polar solvent.
In a preferred embodiment of the preparation method of the polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film, the non-polar organic solvent comprises cyclohexane or carbon tetrachloride.
In a preferred embodiment of the preparation method of the polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film, in step S100, the stirring conditions include stirring at 40-85 ℃ and at a rotation speed of 250-450r/min for 5-8 hours.
In a preferred embodiment of the preparation method of the modified composite film based on the polytetramethyl monopentene-barium titanate nanoparticles, in step S200, the second predetermined mass fraction range is 5-20g of barium titanate nanoparticles added into 5-10mol/L of NaOH solution.
In the preferred embodiment of the preparation method of the modified composite film based on the polytetramethyl pentene-barium titanate nanoparticles, in step S200, naOH solution is stirred for 20-24 hours at 100-120 ℃ and 1000r/min-1200r/min to obtain a BaTiO3 hydroxylated solution, the nanoparticles are washed for 3-5 times by absolute ethyl alcohol, then the nanoparticles are put into a vacuum oven for drying for 24-48 hours at 60-80 ℃, and then the dried BaTiO3-OH particles are ground and sieved by a 200-mesh screen to obtain the hydroxylated BaTiO3 particles BaTiO3-OH.
In a preferred embodiment of the preparation method of the polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film, in step S300, the third predetermined mass fraction is in a range of 5-20g of BaTiO3 particles BaTiO3-OH, and 2-5ml of the coupling agent is added to 50ml-200ml of toluene.
In a preferred embodiment of the preparation method of the polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film, the coupling agent is a KH570 silane coupling agent.
In the preferred embodiment of the preparation method of the polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film, in step S300, a toluene solution is stirred at 60-90 ℃ and a rotation speed of 1000-1200 r/min for 20-24 hours to obtain a BaTiO3 grafted KH570 solution.
In the preferable embodiment of the preparation method of the polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film, after being washed for 3-5 times by toluene, nano-scale particles BaTiO3-KH570 are put into a vacuum oven to be dried for 24-48 hours at 60-80 ℃, and then the dried particles BaTiO3-KH570 are ground and sieved by a 200-mesh screen to obtain the particles BaTiO3-KH570 with KH570 treated surface.
In one embodiment, in step S100: weighing 5g-10g of polytetramethylene monopentene by using an electronic balance, weighing 50ml-100ml of nonpolar solvent by using a measuring cylinder, dissolving the polytetramethylene monopentene in the nonpolar solvent, and stirring for 5-8 hours at 40-85 ℃ and 250-450r/min by using a mechanical stirrer to obtain a polytetramethylene monopentene solution.
In one embodiment, the non-polar solvent described in step S100 is any of: cyclohexane, carbon tetrachloride.
In one embodiment, step S200 includes: weighing 5-20g of barium titanate nano particles, uniformly adding the barium titanate nano particles into 5-10mol/L NaOH solution, stirring the barium titanate nano particles for 20-24 hours at 100-120 ℃ and 1000r/min-1200r/min by using magnetic stirring to obtain BaTiO3 hydroxylated solution, washing the nano particles for 3-5 times by using absolute ethyl alcohol, then drying the nano particles in a vacuum oven at 60-80 ℃ for 24-48 hours, then grinding the dried BaTiO3-OH particles, and sieving the ground BaTiO3-OH particles by using a 200-mesh sieve to obtain the BaTiO3-OH particles.
In one embodiment, step S300 further comprises: weighing 5-20g of BaTiO3-OH particles, uniformly adding the particles into 50-200 ml of toluene, dripping 2-5ml of KH570 coupling agent, uniformly stirring, stirring for 20-24 hours at the temperature of 60-90 ℃ and the rotating speed of 1000r/min-1200r/min by using magnetic force to obtain BaTiO3-KH570 solution, washing the nanoparticles for 3-5 times by using the toluene, drying the nanoparticles in a vacuum oven at the temperature of 60-80 ℃ for 24-48 hours, grinding the dried BaTiO3-KH570 particles, and sieving by using a 200-mesh sieve to obtain the BaTiO3-KH570 particles.
In one embodiment, step S400 includes: and weighing 5-20 wt% of BaTiO3-KH570 nanoparticles, uniformly adding the nanoparticles into the poly-tetramethyl-pentene solution, and stirring for 10-18 hours at 40-85 ℃ and 1500-2000 r/min by using a mechanical stirrer to obtain a mixed solution A.
In one embodiment, the quartz glass plate is wiped by alcohol and dried simultaneously, the quartz glass plate is heated to 30-50 ℃, the solution A is poured on the quartz glass plate and is scraped off by a scraper, the quartz glass plate attached with the solution A is placed in a vacuum oven and is subjected to vacuum drying for 24-48 hours at 30-50 ℃, then the quartz glass plate is placed in warm water for demoulding to obtain the polytetramethyl-pentene-barium titanate nano particle modified composite film, and the film is placed in the vacuum oven and is dried for 24-48 hours at 60-80 ℃ to obtain the dried polytetramethyl-pentene-barium titanate nano particle modified composite film.
In one embodiment, the preparation method of the composite film based on the polytetramethyl monopentene-barium titanate nano particles comprises the following steps:
s100, weighing and dissolving the polytetramethylene monopentene in a non-polar polymer solvent under the condition of uniform stirring to obtain a pure polytetramethylene monopentene solution;
s200, weighing barium titanate nanoparticles with a certain mass fraction, reacting in a NaOH solution to obtain a BaTiO3 hydroxylation solution, cleaning, drying, grinding and sieving to obtain hydroxylated BaTiO3 particles, namely BaTiO3-OH;
s300, weighing and determining mass fraction of BaTiO3-OH particles and KH570 silane coupling agent, reacting in a toluene environment to obtain BaTiO3 grafted KH570 solution, cleaning, drying, grinding and sieving to obtain BaTiO3 particles with KH570 treated surfaces, namely BaTiO3-KH570;
s400, weighing and fixing BaTiO3-KH570 in mass fraction, adding the polytetramethylene monopentene solution, and stirring to obtain a mixed solution A;
s500, drying the solution A in vacuum to obtain the polytetramethylene monopentene-barium titanate nano particle modified composite film.
As shown in FIG. 1, the infrared spectrum of barium titanate nanoparticles before and after KH570 silane coupling agent treatment shows that after KH570 is grafted, the intensity of hydroxyl peak at 3510 part of the surface is reduced, which indicates that the number of hydroxyl peaks is reduced, and also proves that the hydroxyl groups on the surface of BT and the silane coupling agent undergo dehydration condensation reaction. Secondly, the groups located at 2956 and 1717 are also unique to KH570, with the most compelling evidence that the peak of Si-O-Ti produced at 1168 is present, indicating that KH570 treatment was successful.
As shown in fig. 2, a cross-sectional SEM image of the barium titanate/PMP composite film before and after being treated with the KH570 silane coupling agent with a content of 10wt% shows that after doping, untreated BT has more large aggregation points with a diameter reaching 1-2um level, and after treatment with the coupling agent, the aggregation points of the material are significantly reduced, and the maximum size of the aggregation is significantly reduced, which indicates that the KH570 coupling agent treatment has a promoting effect on the dispersion of the nanoparticles.
As shown in fig. 3-5, the temperature-40 ℃ to 180 ℃ dielectric spectrum and dielectric loss are shown, it can be seen that the dielectric constant of the composite sample decreases slightly with increasing temperature, which may lead to a decrease in the number of dipoles per unit volume with expansion of the polymer volume at high temperature, resulting in a decrease in the dielectric constant. The loss can be maintained below 0.005. The dielectric constant of the composite material can be improved to a greater extent by the BT particles treated by the silane coupling agent, and for a 10wt% sample, the dielectric constant before and after treatment is improved from 2.62 to 3.03, which is probably because the dispersity becomes good, the contact area of the BT and the PMP matrix becomes large, the interface polarization is enhanced, and the dielectric constant is increased.
As shown in fig. 6, the dielectric constant and dielectric loss of the polytetramethyl monopentene-barium titanate nanoparticle modified/unmodified composite film at 1KHz are shown as temperature variation curves, and when the temperature is increased from-40 to 160 ℃, the dielectric constant of the composite sample is decreased, which is associated with the volume expansion of the sample at high temperature, resulting in the decrease of the number of particles participating in polarization in the unit volume, resulting in the decrease of the dielectric constant. For dielectric loss, the dielectric loss increases first and then decreases with increasing temperature, peaking at 40-80 ℃, which is related to the glass transition temperature of PMP. Above 80 ℃, the loss of the composite dielectric is reduced, and the composite dielectric is in the order of magnitude of 10-3 and is less than 0.5 percent of the specified power capacitor, which shows that the composite film can meet the requirement of the power capacitor at high temperature.
FIGS. 7 and 8 are graphs showing a comparison of the breakdown strengths of the barium titanate/PMP composite film before and after treatment at 10wt% at 20 ℃ and 80 ℃; it can be seen that the breakdown field strength of the treated film becomes high, from 319.0MV/m at 20 ℃ to 366.2MV/m (14.7% improvement), from 246.2MV/m to 317.3.2MV/m at 80 ℃ (28.8% improvement), due to the enhanced surface compatibility, the uniform distribution, the improved electric field distortion, and the increased breakdown.
Finally, it should be noted that: the described embodiments are only some of the present application, not all embodiments, and all other embodiments that can be derived by one skilled in the art from the embodiments in the present application without making any inventive effort fall within the scope of protection of the present application.
While certain exemplary embodiments of the present invention have been described above by way of illustration only, it will be apparent to those of ordinary skill in the art that the described embodiments may be modified in various different ways without departing from the spirit and scope of the present invention. Accordingly, the drawings and description are illustrative in nature and should not be construed as limiting the scope of the invention.
Claims (5)
1. A preparation method of a modified composite film based on polytetramethylene monopentene-barium titanate nano particles is characterized by comprising the following steps:
s100, weighing and dissolving a first predetermined mass fraction of polytetramethylene monopentene in a nonpolar solvent, and dissolving under the condition of uniform stirring to obtain a polytetramethylene monopentene solution, wherein the first predetermined mass fraction is 5-10 g of polytetramethylene monopentene dissolved in 50-100 ml of nonpolar solvent;
s200, weighing barium titanate nanoparticles with a second predetermined mass fraction, reacting in a NaOH solution to obtain a BaTiO3 hydroxylated solution, cleaning, drying, grinding and sieving to obtain hydroxylated BaTiO3 particles BaTiO3-OH;
step S300, weighing BaTiO3 particles BaTiO3-OH with a third preset mass fraction and a coupling agent KH570, reacting in a toluene environment to obtain a BaTiO3 graft solution, cleaning, drying, grinding and sieving to obtain particles BaTiO3-KH570;
s400, weighing a fourth mass fraction of BaTiO3-KH570 particles, adding the solution of the polytetramethylene monopentene, and stirring to obtain a mixed solution A;
step S500, drying the mixed solution A in vacuum to obtain a polytetramethylene monopentene-barium titanate nano particle modified composite film, wherein the dielectric loss is kept below 0.0025 within the temperature range of 20-180 ℃;
wherein the content of the first and second substances,
the non-polar solvent comprises cyclohexane or carbon tetrachloride;
in the step S200, the barium titanate nano particles with the second preset mass fraction range of 5-20g are added into a NaOH solution with the concentration of 5-10 mol/L;
in step S300, the third predetermined mass fraction is in the range of 5-20g BaTiO3 particles BaTiO3-OH, and 2-5ml of coupling agent KH570 is added into 50-200 ml of toluene.
2. The method for preparing the polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film according to claim 1, wherein the stirring conditions in step S100 include stirring at 40-85 ℃ and 250-450r/min for 5-8 hours.
3. The preparation method of the polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film according to claim 1, wherein in step S200, the NaOH solution is stirred at 100-120 ℃ and 1000r/min-1200r/min for 20-24 hours to obtain a BaTiO3 hydroxylated solution, the nanoparticles are washed with absolute ethyl alcohol for 3-5 times, then dried in a vacuum oven at 60-80 ℃ for 24-48 hours, and then the dried BaTiO3-OH particles are ground and sieved by a 200-mesh screen to obtain the hydroxylated BaTiO3 particles BaTiO3-OH.
4. The method of claim 1, wherein in step S300, the toluene solution is stirred at 60-90 ℃ and 1000r/min-1200r/min for 20-24 hours to obtain a BaTiO3 grafted KH570 solution, the solution is washed with toluene for 3-5 times, the nano-sized BaTiO3-KH570 is dried in a vacuum oven at 60-80 ℃ for 24-48 hours, and the dried BaTiO3-KH570 is ground and sieved with a 200-mesh sieve to obtain BaTiO3-KH570 treated with KH570 on the surface.
5. The method for preparing the polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film according to claim 1, wherein a fourth mass fraction ranging from 5wt% to 20wt% of the particulate BaTiO3-KH570 is added to the polytetramethylene monopentene solution.
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