CN113999461A - 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 BaTiO 3-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-KH 570; and weighing a fourth mass fraction of the BaTiO3-KH570 particles, adding the solution of the polytetramethylene monopentene, stirring 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. The most commonly used power capacitor material at present is BOPP (biaxially oriented polypropylene), which has low cost and easy processing, but has poor high-temperature resistance, low melting initial temperature (85-100 ℃) and low long-time working temperature (70-80 ℃), and the dielectric constant is low (about 2.2), and the nano doping is used as a means for improving the dielectric constant which is widely applied at present, so that the dielectric constant of the composite material can be effectively improved, however, because the dielectric constant difference between the nano filler and the organic matrix is large and the filler is seriously agglomerated, the electric field distribution can be distorted while the dielectric constant is improved, so that the breakdown strength is seriously reduced compared with that of a pure polymer matrix, therefore, a thermal stable material which has a large dielectric constant and a small dielectric loss and can withstand high temperature needs to be found, and the breakdown field strength is improved by modifying the doped nanoparticles.
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 well known to those of ordinary skill in the art.
Disclosure of Invention
The invention aims to provide a preparation method of a modified composite film based on poly-tetramethyl-pentene-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 preset mass fraction to react in a NaOH solution to obtain a BaTiO3 hydroxylated solution, cleaning, drying, grinding and sieving to obtain hydroxylated BaTiO3 particles BaTiO 3-OH;
s300, weighing BaTiO3-OH particles of BaTiO3 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 of BaTiO3-KH 570;
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 poly-tetramethyl-pentene-barium titanate nano particles, in the step S100, the stirring condition comprises stirring for 5-8 hours at the temperature of 40-85 ℃ and 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 modified composite film based on the polytetramethyl pentene-barium titanate nano particles, in step S200, NaOH solution is stirred for 20-24 hours at 100-120 ℃ and at the rotating speed of 1000r/min-1200r/min to obtain a BaTiO3 hydroxylated solution, the nano particles are washed for 3-5 times by absolute ethyl alcohol, 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 screened by a 200-mesh screen to obtain the hydroxylated BaTiO3 particles BaTiO 3-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 of 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 polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film, in step S300, a toluene solution is stirred for 20-24 hours at 60-90 ℃ and at 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 in a vacuum oven for drying 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 particles BaTiO3-KH570 with KH570 treated surfaces.
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 5 wt% to 20 wt% 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. By doping the modified barium titanate nanoparticles, the 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 10 wt% 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 at-40 to 180 ℃ of a 10 wt% barium titanate/PMP composite film that is not treated with a KH570 silane coupling agent based on a method for preparing a polytetramethyl monopentene-barium titanate nanoparticle modified composite film according to the present invention;
FIG. 4 is a graph of dielectric spectrum and loss of a 10 wt% barium titanate/PMP composite film treated with a 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 10 wt%;
FIG. 7 is a graph showing the breakdown strength of a barium titanate/PMP composite film before and after treatment, which is 10 wt% 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 10 wt% 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 and positional relationships based on those shown in the drawings, and are used only for convenience of description and simplicity of description, and do not indicate or imply that the equipment or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be considered as limiting the present invention.
Furthermore, the terms "first-", "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," 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 expressly specified or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, releasably connected, or integral; either directly or indirectly through intervening media, either internally or in any other relationship. 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, cleaning, drying, grinding and sieving to obtain hydroxylated BaTiO3 particles BaTiO 3-OH;
s300, weighing BaTiO3-OH particles of BaTiO3 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 of BaTiO3-KH 570;
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 doped with KH570 is 10 wt%, 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 treatment 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 intensity of the composite material can be improved, the breakdown field intensity is improved from 319.0MV/m to 366.2MV/m (improved by 14.7%) under the doping concentration of 10 wt%, the requirement of a power capacitor can be met, and the high-dielectric high-temperature resistance of the film capacitor is improved.
In a preferred embodiment of the preparation method of the polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film, in step S100, the first predetermined mass fraction range is 5g to 10g of polytetramethylene monopentene dissolved in 50ml to 100ml of a nonpolar solvent.
In a preferred embodiment of the preparation method of the polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film, the nonpolar 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 preferable embodiment of the preparation method of the modified composite film based on the polytetramethyl pentene-barium titanate nano particles, 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 nano particles are washed for 3-5 times by absolute ethyl alcohol, then 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 screened by a 200-mesh screen to obtain the hydroxylated BaTiO3 particles BaTiO 3-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 range is 5-20g of BaTiO3 particles BaTiO3-OH, and 2-5ml of the coupling agent is added to 50ml-200ml of toluene.
In the preferable embodiment of the preparation method of the modified composite film based on the polytetramethyl monopentene-barium titanate nano particles, the coupling agent is a KH570 silane coupling agent.
In the preferable embodiment of the preparation method of the polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film, in step S300, a toluene solution is stirred for 20-24 hours at 60-90 ℃ and at a rotating speed of 1000r/min-1200r/min 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 the temperature of 60-80 ℃, and then the dried particles BaTiO3-KH570 are ground and sieved by a 200-mesh screen, so that the particles BaTiO3-KH570 with the KH570 treated on the surface are obtained.
In one embodiment, in step S100: weighing 5g-10g of polytetramethylene monopentene by using an electronic balance, measuring 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 the rotation speed of 250-450r/min by using a mechanical stirrer to obtain the 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 a BaTiO3 hydroxylated solution, cleaning 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 dried 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 BaTiO3-OH particles into 50-200 ml of toluene, dripping 2-5ml of KH570 coupling agent, uniformly stirring, magnetically stirring at 60-90 ℃ and 1000-1200 r/min for 20-24 hours to obtain BaTiO3-KH570 solution, washing the nanoparticles for 3-5 times by using toluene, drying the nanoparticles in a vacuum oven at 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 (2) weighing 5-20 wt% of BaTiO3-KH570 nanoparticles, uniformly adding the nanoparticles into the polytetramethyl monopentene 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 and determining the mass fraction of barium titanate nanoparticles to react in a NaOH solution to obtain a BaTiO3 hydroxylated solution, and cleaning, drying, grinding and sieving the solution to obtain hydroxylated BaTiO3 particles called BaTiO 3-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, wherein the BaTiO3-KH570 particles are named as BaTiO3-KH 570;
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 peak intensity of hydroxyl groups on the surface at 3510 is reduced, which indicates that the number of hydroxyl groups is reduced, and the dehydration condensation reaction of the hydroxyl groups on the BT surface and the silane coupling agent is also proved. 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 10 wt% shows that after the untreated BT is doped, there are many large aggregation points with a diameter of 1-2um, and the treated with the coupling agent causes the material to have significantly fewer aggregation points and a significantly smaller maximum size of aggregation, which indicates that the KH570 coupling agent treatment has an effect of promoting the dispersion of 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 the volume expansion of the polymer 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 10 wt% sample, the dielectric constant before and after treatment is improved from 2.62 to 3.03, which is probably because the dispersibility is better, the contact area between the BT and the PMP matrix is larger, 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 pentene-barium titanate nanoparticle modified/unmodified composite film at 1KHz are shown as the curves of the temperature dependence, and when the temperature is increased from-40 to 160 ℃, the dielectric constant of the composite sample is reduced, which is in combination with the volume expansion of the sample at high temperature, resulting in the reduction of the number of particles participating in polarization in the unit volume, and the reduction 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 10 wt% 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), and from 246.2MV/m to 317.3.2MV/m at 80 ℃ to 28.8% improvement, due to the enhanced surface compatibility, the uniform distribution, and the improved electric field distortion, the breakdown is increased.
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 obtained by one skilled in the art without inventive efforts based on the embodiments in the present application are 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 invention. Accordingly, the drawings and description are illustrative in nature and should not be construed as limiting the scope of the invention.
Claims (10)
1. A preparation method of a composite film modified based on poly-tetramethyl-pentene-barium titanate nano particles is characterized by comprising 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 preset mass fraction to react in a NaOH solution to obtain a BaTiO3 hydroxylated solution, cleaning, drying, grinding and sieving to obtain hydroxylated BaTiO3 particles BaTiO 3-OH;
s300, weighing BaTiO3-OH particles of BaTiO3 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 of BaTiO3-KH 570;
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.
2. The method for preparing the polytetramethylene monopentene-barium titanate nanoparticle-based modified composite film according to claim 1, wherein in step S100, the first predetermined mass fraction of the polytetramethylene monopentene in the range of 5g to 10g is preferably dissolved in 50ml to 100ml of the non-polar solvent.
3. The method of claim 2, wherein the non-polar organic solvent comprises cyclohexane or carbon tetrachloride.
4. The method as claimed in claim 1, wherein the stirring conditions in step S100 include stirring at 40-85 ℃ and at a rotation speed of 450r/min for 5-8 hours.
5. The method for preparing the polytetramethylene monopentene-barium titanate nanoparticle modified composite film as claimed in claim 1, wherein in step S200, the second predetermined mass fraction of barium titanate nanoparticles is 5-20g and is added into 5-10mol/L NaOH solution.
6. The method for preparing 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 BaTiO 3-OH.
7. The method for preparing the polytetramethylene monopentene-barium titanate nanoparticle modified composite film as claimed in claim 1, wherein in step S300, the third predetermined mass fraction is in the range of 5-20g of BaTiO3 particles BaTiO3-OH, and 2-5ml of coupling agent is added to 50ml-200ml of toluene.
8. The preparation method of the composite film based on the polytetramethylene monopentene-barium titanate nanoparticle modification of claim 7, wherein the coupling agent is a KH570 silane coupling agent.
9. The method as claimed in claim 8, wherein the toluene solution is stirred at 60-90 ℃ and 1000r/min-1200r/min for 20-24 hours to obtain BaTiO3 grafted KH570 solution, the solution is washed with toluene 3-5 times, the nano-sized BaTiO3-KH570 is dried in a vacuum oven at 60-80 ℃ for 24-48 hours, and the dried particles BaTiO3-KH570 are ground and sieved with a 200-mesh sieve to obtain the surface KH 570-treated BaTiO3-KH 570.
10. 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 5 wt% to 20 wt% of the particles BaTiO3-KH570 is added to the polytetramethylene monopentene solution.
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