CN111205579A - High-efficiency high-temperature-resistant aluminum nitride/polymer composite material and preparation method thereof - Google Patents
High-efficiency high-temperature-resistant aluminum nitride/polymer composite material and preparation method thereof Download PDFInfo
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
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Abstract
The invention discloses a high-temperature-resistant aluminum nitride/polymer composite material and a preparation method thereof. The capacitive storage performance of the existing dielectric material at high temperature shows great defects. The invention relates to a high-temperature-resistant aluminum nitride/polymer composite material, which comprises aluminum nitride and a matrix polymer. Aluminum nitride is dispersed as filler particles in the matrix polymer. The mass fraction of the aluminum nitride is 0-50%. The composite material film is prepared by adopting the aluminum nitride as the additive particles, the aluminum nitride has high thermal conductivity, high temperature resistance, good high temperature-electric insulation and good dielectric property, the thermal conductivity and other physical properties of the polymer can be improved, the good electric insulation property can be maintained, and the electric displacement value and the breakdown field strength value of the composite material can be effectively improved at the room temperature of 90 ℃, so that the high temperature resistance, the releasable energy density and the energy storage efficiency of the composite material are effectively improved.
Description
Technical Field
The invention belongs to the technical field of electronic material preparation, and particularly relates to a high-energy-density high-efficiency high-temperature-resistant aluminum nitride/polymer composite material and a preparation method thereof.
Background
With the rapid development of microelectronic integration technology, in the field of electronics and microelectronics, devices with small size but still existing functions can be miniaturized, the cost is reduced, and the electrical performance of electronic products is improved. Among such elements, capacitors are of widespread interest, which may serve the functions of decoupling, bypassing, filtering, etc. The polymer film capacitor is widely used due to the advantages of no polarity, high insulation resistance, excellent frequency characteristic and the like, and is mainly applied to a plurality of fields of household appliances, communication, hybrid electric vehicles, aerospace and the like.
The capacitor material is required to have excellent properties such as high dielectric constant, high electric field strength, high energy storage density, high efficiency and the like. The polymer material has the advantages of light weight, low price, easy processing, excellent mechanical property and high breakdown strength, but the dielectric constant is generally not high. Generally, it is difficult to obtain excellent performances in all aspects from a single material, and inorganic particle composite modification is required. The composite modification enables the energy density of the material to be obviously improved.
However, the capacitive storage properties of these materials at high temperatures exhibit significant drawbacks, such as reduced energy density and reduced efficiency, which are commonly found in various energy applications, such as hybrid vehicles and avionics. For example, when the hybrid electric vehicle is operated at 70 ℃, the charge-discharge efficiency of P (VDF-TrFE-CFE) is only 21%, and the low efficiency not only causes a large decrease in energy density (only 1J/cm)3) And a large amount of heat is generated, so that the heat dissipation difficulty brought by the heat generation is seriously influencedTo device accuracy and lifetime. Therefore, the research and preparation of the high polymer material with high temperature resistance and good electric insulation performance and the development of the high-temperature polymer-based composite dielectric material with high charge-discharge efficiency and high energy density are of great significance.
Disclosure of Invention
The first purpose of the invention is to overcome the defect that the dielectric material in the prior art is difficult to work in the environment of 70 ℃, and provide a high-temperature resistant aluminum nitride/polymer composite material with high energy storage density and high efficiency.
The invention relates to a high-temperature-resistant aluminum nitride/polymer composite material, which comprises aluminum nitride and a matrix polymer. Aluminum nitride is dispersed as filler particles in the matrix polymer. The mass fraction of the aluminum nitride is 1-50%.
Preferably, the high-temperature-resistant aluminum nitride/polymer composite material is a film prepared by a casting method. The thickness of the film is 10 to 100 μm.
Preferably, the aluminum nitride is surface treated. The particle size of the aluminum nitride is 20-900 nanometers.
Preferably, the matrix polymer is PMMA or PMMA-based linear material.
A second object of the present invention is to provide a method for preparing the aforementioned composite material.
The preparation method of the high-temperature-resistant aluminum nitride/polymer composite material comprises the following steps:
dissolving a matrix polymer in a polar solvent, and stirring and dissolving to obtain a polymer-based solution.
And step two, adding aluminum nitride powder into the polymer solution, and stirring and carrying out ultrasonic treatment to obtain a suspension. And coating the suspension on a glass slide, and volatilizing the solvent to obtain a composite material prototype.
And step three, heating the composite material prototype obtained in the step two, and then carrying out quenching treatment to obtain the composite material film.
Preferably, the aluminum nitride is surface treated. The surface treatment process is as follows: mixing aluminum nitride in a coupling agent, and heating and stirring in water bath on a magnetic stirrer. Centrifuging the obtained solution, washing the precipitate with distilled water and alcohol for several times, and centrifuging; and drying the precipitate to obtain the aluminum nitride after surface treatment.
Preferably, the coupling agent is dopamine hydrochloride, a silane coupling agent or tetrabutyl titanate.
Preferably, the polar solvent used in step one is DMF. The concentration of the matrix polymer in the polymer-based solution obtained in the first step is 3-30 g/L.
Preferably, the solvent volatilization conditions in the second step are as follows: heating for 30-60 min at 50-120 ℃. The heating conditions in the third step are as follows: heating the mixture in a drying oven at 150-250 ℃ for 0.5-10 h. The quenching temperature in the third step is 0-200 ℃, and the quenching time is 5-60 min.
The invention has the beneficial effects that:
1. the composite material film is prepared by adopting the aluminum nitride as the additive particles, the aluminum nitride has high thermal conductivity, high temperature resistance, good high temperature-electric insulation and good dielectric property, the thermal conductivity and other physical properties of the polymer can be improved, the good electric insulation property can be maintained, and the electric displacement value and the breakdown field strength value of the composite material can be effectively improved at the room temperature of 90 ℃, so that the high temperature resistance, the releasable energy density and the energy storage density efficiency of the composite material are effectively improved. This enables the invention to be used in thin film capacitors in electric vehicle power plants, operating continuously for long periods at operating temperatures of 70 ℃.
2. In the process of preparing the composite material solution, the invention improves the dispersibility of the particles in the polymer through multiple times of stirring and ultrasound, further reduces the agglomeration of the particles in the polymer, and improves the film forming quality.
3. The invention modifies the aluminum nitride by using the dopamine hydrochloride, so that the particles are better dispersed in the polymer, and the breakdown field strength and the effective energy storage density of the composite material film are improved. The aluminum nitride/polymer composite material film prepared by the invention has the characteristics of high breakdown, high efficiency and high temperature resistance, and the preparation process is simple and reliable, and is suitable for large-scale popularization and use.
Drawings
FIG. 1 is a dielectric diagram of a composite material and a pure polymer material prepared according to the present invention;
FIG. 2 is a graph of breakdown field strength of a composite material prepared in accordance with the present invention versus a pure polymer material at different temperatures;
FIG. 3 is a hysteresis loop plot of a composite material prepared in accordance with the present invention versus a pure polymer material at different temperatures;
FIG. 4 is a graph of releasable energy density and efficiency at room temperature with the addition of a composite material prepared in accordance with the present invention and a neat polymer material;
FIG. 5 is a graph of releasable energy density and efficiency at 90 ℃ with the addition of composite materials prepared according to the present invention and neat polymer materials at room temperature.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
Example 1
A high-temperature resistant aluminum nitride/polymer composite material is characterized in that PMMA is adopted as a base material, aluminum nitride with high thermal conductivity and high-temperature resistance is selected as filler particles, and the composition of the composite material is adjusted by changing the addition amount of the filler particles.
The preparation method of the high-temperature-resistant aluminum nitride/polymer composite material comprises the following steps:
step one, weighing aluminum nitride, adding the aluminum nitride into a dopamine hydrochloride solution, and heating in a water bath at 50 ℃ for 10 hours to obtain a mixed solution; putting the mixed solution into a centrifuge tube, centrifuging for 30min at the rotating speed of 5000r/min, taking out, pouring out supernatant, washing with alcohol and centrifuging for three times; the precipitate was transferred to a petri dish and dried at 70 ℃ for 24 hours to obtain modified aluminum nitride.
The aluminum nitride has high thermal conductivity, high temperature resistance and good high-temperature-electric insulation performance. The particle size of the modified aluminum nitride is between 20 and 900 nanometers, and the modified aluminum nitride is not limited to the aluminum nitride treated by the surface coupling agent.
And step two, weighing the matrix polymer, adding the matrix polymer into a DMF (N, N-dimethylformamide) solvent, and stirring until the polymer is completely dissolved to obtain a polymer-based solution. The matrix polymer adopts PMMA (polymethyl methacrylate) or a linear material with PMMA as the matrix. One class of linear materials with PMMA as the matrix includes PMMA/PEMA (polymethyl methacrylate/polyethyl methacrylate), PMMA/PC (polymethyl methacrylate/polycarbonate) and PMMA/PVDF (polymethyl methacrylate/polyvinylidene fluoride).
Step three, weighing the modified aluminum nitride obtained in the step one, and adding the modified aluminum nitride into the polymer base solution obtained in the step two; firstly stirring for 10-60 min, and then carrying out ultrasonic treatment for 10-60 min; stirring and ultrasonic circulation are repeated for 1-10 times to form uniform suspension. Uniformly coating the suspension on a glass slide, wherein the coating amount is 1-20 ml; and heating the glass slide coated with the solution at 50-120 ℃ for 30-60 min to completely volatilize the solvent, thereby obtaining the composite material prototype.
And step four, putting the composite material prototype prepared in the step three into a drying oven, and heating for 0.5-10 hours at the temperature of 150-250 ℃ to fully melt the polymer in the composite material film, so as to obtain the molten composite material.
And step five, quenching the molten composite material obtained in the step four at the temperature of 0-200 ℃ for 5-60 min to obtain a quenched composite material film with the thickness of 10-100 microns. The mass fraction of aluminum nitride in the composite material film is 10%.
The graph of the change of the dielectric constant value of the composite material film obtained in this embodiment with the operating frequency is shown in fig. 1, and at each operating frequency, the dielectric constant of the composite material film containing 10 wt% of aluminum nitride is higher than that of a pure PMMA polymer, which indicates that the dielectric property of the polymer is improved by the addition of the aluminum nitride.
The breakdown field strength value of the composite material film obtained in the embodiment is shown in fig. 2, at room temperature of 25 ℃, the breakdown field strength of the composite material film containing 10 wt% of aluminum nitride reaches 400MV/m, and is increased by about 33% compared with the breakdown field strength of pure polymer PMMA, which shows that the addition of the particles effectively increases the breakdown field strength value of the dielectric material; at room temperature of 90 ℃, the breakdown field strength of the composite material film containing 10 wt% of aluminum nitride is basically kept unchanged, and high breakdown field strength is still kept, which shows that the addition of the particles not only improves the breakdown field strength value of the composite material film, but also improves the high temperature resistance of the dielectric material.
The hysteresis loop diagram of the composite material film obtained in this example is shown in fig. 3, and it can be seen from the diagram that, compared with the PMMA material, the composite material with 10 wt% aluminum nitride added at room temperature of 25 ℃ has both increased electric displacement and residual polarization, and the composite material with 10 wt% aluminum nitride has more increased electric displacement value and less increased residual polarization, thereby contributing to increase of energy storage density; at room temperature of 90 ℃, the electric potential shift and the residual polarization of the composite material containing 10 wt% of aluminum nitride are not increased or decreased, which shows that the addition of the particles not only contributes to the improvement of the energy storage density, but also improves the high temperature resistance of the dielectric material.
The energy storage density of the composite material obtained in the example at 25 ℃ is shown in FIG. 4, and the energy storage density of the composite material containing 10 wt% of aluminum nitride reaches up to 5.4J/cm3While the storage density of pure PMMA polymer is only 2J/cm at most3. The energy storage density performance of the composite material containing 10 wt% aluminum nitride is 2.7 times that of the pure PMMA polymer. The energy storage density efficiency of the composite material containing 10 wt% of aluminum nitride is as high as 86%, and the high energy storage density efficiency is still maintained after the particles are added, which shows that the addition of the particles effectively improves the energy storage density and the energy storage density efficiency of the dielectric material, and enhances the electrical property of the dielectric material.
The energy storage density of the composite material obtained in this example at 90 ℃ is shown in fig. 5, and the performance of the composite material containing 10 wt% of aluminum nitride at 90 ℃ and at room temperature is basically unchanged, and the excellent characteristics of high energy storage density and high efficiency are still maintained, which indicates that the high temperature resistance of the dielectric material is improved by adding the particles.
Example 2
This example differs from example 1 in that: the mass fraction of aluminum nitride in the composite material film is 4%, and the composite material obtained in the embodiment has the highest energy storage density of 2.3J/cm at 25 DEG C3The energy storage density is 2J/cm higher than that of pure PMMA polymer3Lower than 5.4J/cm of the composite material in example 13The energy storage density of (1).
Example 3
This example differs from example 1 in that: the mass fraction of aluminum nitride in the composite material film is 8%, and the composite material obtained in the embodiment has the highest energy storage density of 4.1J/cm at 25 DEG C3The energy storage density of the PMMA polymer is 2J/cm higher than that of the pure PMMA polymer3Lower than 5.4J/cm of the composite material in example 13The energy storage density of (1).
Example 4
This example differs from example 1 in that: the mass fraction of aluminum nitride in the composite material film is 12%, and the composite material obtained in the embodiment has the highest energy storage density of 4J/cm at 25 DEG C3The energy storage density of the PMMA polymer is 2J/cm higher than that of the pure PMMA polymer3Lower than 5.4J/cm of the composite material in example 13The energy storage density of (1).
From examples 1 to 4, it can be seen that when the mass fraction of aluminum nitride is selected to be 10%, the energy storage density of the composite material is obviously higher than that of the composite material under the mass fraction of other aluminum nitride; therefore, the mass fraction of 10% is a significant advantage which is not intended to be expected in the present invention.
Example 5
This example differs from example 1 in that: and D, replacing the dopamine hydrochloride solution in the step one with a silane coupling agent solution or a tetrabutyl titanate solution.
Claims (5)
1. A high temperature resistant aluminum nitride/polymer composite material includes a matrix polymer; the method is characterized in that: also includes aluminum nitride; the aluminum nitride is dispersed in the matrix polymer as filler particles; the mass fraction of the aluminum nitride is 1-50%.
2. A refractory aluminum nitride/polymer composite in accordance with claim 1, wherein: the high-temperature resistant aluminum nitride/polymer composite material is a film prepared by a tape casting method; the thickness of the film is 10 to 100 μm.
3. A refractory aluminum nitride/polymer composite in accordance with claim 1, wherein: the aluminum nitride is subjected to surface treatment; the particle size of the aluminum nitride is 20-900 nanometers; the surface treatment of the aluminum nitride is realized by a coupling agent; the coupling agent adopts dopamine hydrochloride, silane coupling agent or tetrabutyl titanate.
4. A refractory aluminum nitride/polymer composite in accordance with claim 1, wherein: the matrix polymer is PMMA or PMMA-based linear material.
5. The method of claim 1, wherein the aluminum nitride/polymer composite material is prepared by the following steps: dissolving a matrix polymer in a polar solvent to obtain a polymer-based solution; the concentration of a matrix polymer in the polymer-based solution is 3-30 g/L; adding aluminum nitride powder into the polymer solution, and stirring and ultrasonically treating to obtain a suspension; the stirring and the ultrasonic treatment are alternately and repeatedly executed for 1-10 times; stirring for 10-60 min each time; the ultrasonic treatment lasts for 10-60 min each time; coating the suspension on a glass slide, and volatilizing a solvent to obtain a composite material prototype; heating the composite material prototype, and then carrying out quenching treatment to obtain a composite material film; the heating conditions are as follows: heating in a drying oven at 150-250 ℃ for 0.5-10 h; the quenching temperature is 0 to-200 ℃, and the quenching time is 5 to 60 min.
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| CN108395658A (en) * | 2018-03-05 | 2018-08-14 | 西安交通大学 | PVDF matrix composite dielectrics with self-crosslinking characteristic and preparation method thereof |
| CN109320888A (en) * | 2018-11-02 | 2019-02-12 | 湖北光合生物科技有限公司 | A kind of polymethyl methacrylate heat-conductive composite material and preparation method thereof |
| CN110330676A (en) * | 2019-06-20 | 2019-10-15 | 杭州电子科技大学 | A kind of preparation method of the high dielectric constant compound film material based on ceramic packing |
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| CN108395658A (en) * | 2018-03-05 | 2018-08-14 | 西安交通大学 | PVDF matrix composite dielectrics with self-crosslinking characteristic and preparation method thereof |
| CN109320888A (en) * | 2018-11-02 | 2019-02-12 | 湖北光合生物科技有限公司 | A kind of polymethyl methacrylate heat-conductive composite material and preparation method thereof |
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| CN112898777A (en) * | 2021-02-08 | 2021-06-04 | 上海交通大学 | High-thermal-conductivity radiation refrigeration and heat dissipation material, and preparation method and application thereof |
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| CN111205579B (en) | 2022-04-22 |
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