CN115094574A - Low-dielectric-constant fiber film and preparation method thereof - Google Patents
Low-dielectric-constant fiber film and preparation method thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
- D04H1/43825—Composite fibres
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C7/00—Heating or cooling textile fabrics
Abstract
The invention discloses a low dielectric constant fiber film and a preparation method thereof, wherein the preparation method comprises the following steps: mixing the main resin and the toughening resin with the solvent to obtain a resin dispersion liquid; mixing the filler and the dispersing agent with the solvent to obtain a filler suspension; mixing the resin dispersion liquid and the filler suspension to obtain mixed ink; mixing the mixed ink with the curing agent and the antioxidant to obtain electrostatic spinning ink; and curing the electrostatic spinning ink after an electrostatic spinning process to prepare the low-dielectric-constant fiber film. The low-dielectric-constant fiber film has a dielectric constant of less than 2, and the thickness of the fiber filaments can be adjusted by adjusting the content of the solvent during the formation of the low-dielectric-constant fiber film. The toughening resin, the curing agent and the antioxidant further improve the strength, the physical property and the oxidation resistance of the low-dielectric-constant fiber film respectively. The preparation method has simple process and can be used for industrial production.
Description
Technical Field
The invention relates to the technical field of low dielectric film materials, in particular to a low dielectric constant fiber film and a preparation method thereof.
Background
With the development of science and technology, the integration level of ULSI (Ultra-Large-scale integration) devices is continuously increased, the parasitic capacitance C and the parasitic resistance R caused by the interconnection of metal wires inside nanoscale devices are more and more significant, and the corresponding signal delay and crosstalk of signal devices become the main factors limiting the performance of the devices. In the traditional process, the RC interconnection delay caused by taking aluminum as a metal interconnection line and taking silicon dioxide as an interconnection metal dielectric layer is large, in order to reduce the R interconnection delay, copper with lower resistivity is adopted to replace aluminum as the metal interconnection line, and in order to reduce the influence of the C interconnection delay, a low-dielectric-constant material is required to be used as the interconnection metal dielectric layer. The low dielectric constant material represents the charge storage capacity by a low dielectric constant, the low dielectric constant is low, the insulation property of the material is better, and the C interconnection delay is smaller. However, in the prior art, the dielectric constant of the low dielectric constant material used in the ULSI device is mostly between 2 to 3.5, and the dielectric constant is still not low enough, so that it is necessary to develop a low dielectric constant material with a lower dielectric constant.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a low-dielectric-constant fiber film and a preparation method thereof, wherein the dielectric constant of the low-dielectric-constant fiber film is less than 2, and the preparation process of the low-dielectric-constant fiber film is simple and can be industrially produced.
In order to achieve the purpose, the invention provides the following technical scheme:
a low-dielectric-constant fiber film is prepared by an electrostatic spinning process through electrostatic spinning ink, wherein the electrostatic spinning ink comprises the following components in percentage by mass:
5 to 30 percent of main resin, 1 to 5 percent of toughening resin, 5 to 35 percent of filler, 0.01 to 1 percent of dispersant, 30 to 85 percent of solvent, 0.05 to 1 percent of curing agent and 0.01 to 1 percent of antioxidant;
wherein the low dielectric constant fiber film has a dielectric constant of less than 2.
Preferably, the host resin is selected from at least one of methoxy diphenyl ether resin, cyanate ester modified epoxy resin, tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer, and polyacrylonitrile; and/or the presence of a gas in the gas,
the filler is selected from at least one of graphene oxide, multi-walled carbon nanotubes, silicon oxide and silicon micropowder; and/or the presence of a gas in the gas,
the toughening resin is selected from at least one of thiol-terminated nitrile rubber, chloroprene rubber and polyvinyl chloride rubber; and/or the presence of a gas in the gas,
the curing agent is selected from at least one of anhydride, triethylene tetramine, diethylenetriamine and N-aminoethyl piperazine; and/or the presence of a gas in the gas,
the antioxidant is selected from at least one of triphenyl phosphite, diisooctyl phenyl phosphite and bisphenol A; and/or the presence of a gas in the gas,
the dispersant is selected from at least one of polycarboxylate, poly (meth) acrylic acid derivative and maleic anhydride copolymer; and/or the presence of a gas in the atmosphere,
the solvent is at least one selected from the group consisting of dimethylformamide, dimethylacetamide, dimethylsulfoxide, acetone, and xylene.
The invention also provides a preparation method of the low dielectric constant fiber film, which comprises the following steps:
mixing the main resin, the toughening resin and the solvent to obtain a resin dispersion liquid;
mixing the filler, the dispersing agent and the solvent to obtain a filler suspension;
mixing the resin dispersion liquid and the filler suspension to obtain mixed ink;
mixing the curing agent, the antioxidant and the mixed ink to obtain electrostatic spinning ink;
and curing the electrostatic spinning ink after an electrostatic spinning process to prepare the low-dielectric-constant fiber film.
Preferably, in the electrostatic spinning process, the air humidity is 30-80%, the propelling speed of the injection pump is 0.4-2 mL/h, the spinning needle is a flat needle with the diameter of 0.1-1 mm, the spinning voltage is 5-30 kV, the distance between the spinning needle and the roller is 5-20 cm, and the rotating speed of the roller is 100-1500 rpm.
Preferably, the curing process comprises: and carrying out hot pressing treatment on the fiber membrane obtained by the electrostatic spinning process, and then carrying out hot curing to obtain the low-dielectric-constant fiber membrane.
More preferably, the temperature of the hot-pressing treatment is 80-150 ℃, the pressure is 20-40 PSI, and the time is 10-40 min.
More preferably, the process of heat curing comprises:
heating the hot-pressed fiber membrane from room temperature to a first temperature within 30-60 min;
heating the fiber membrane at the first temperature for 30-60 min at constant temperature;
heating the fiber membrane from the first temperature to the second temperature within 30-60 min;
and heating the fiber membrane at the second temperature for 30-60 min at constant temperature.
Still preferably, the first temperature is 120-180 ℃, and the second temperature is 250-350 ℃.
Preferably, the mixing condition of the main resin and the toughening resin with the solvent is an oil bath kettle at the temperature of 90-200 ℃.
Preferably, the main resin, the toughening resin and the solvent are mixed by stirring at a rotation speed of 400-1000 rpm for 2-6 h; and/or the presence of a gas in the gas,
the mode of mixing the filler, the dispersant and the solvent is stirring, the stirring speed is 400-1000 rpm, and the stirring time is 0.5-2 h; and/or the presence of a gas in the gas,
the mixed ink, the curing agent and the antioxidant are mixed by stirring at the rotating speed of 600-2000 rpm for 0.5-2 h; and/or the presence of a gas in the gas,
the mixed ink, the curing agent and the antioxidant are mixed by stirring at a speed of 500-1000 rpm for 1.5-3 h.
The low-dielectric-constant fiber film provided by the embodiment of the invention is prepared from electrostatic spinning ink through an electrostatic spinning process, wherein the electrostatic spinning ink comprises main resin, toughening resin, filler, a dispersing agent, a solvent, a curing agent and an antioxidant, the dielectric constant of the low-dielectric-constant fiber film prepared through the electrostatic spinning process is lower than 2, and the thickness of fiber yarns can be adjusted by adjusting the content of the solvent in the process of forming the low-dielectric-constant fiber film. The toughening resin, the curing agent and the antioxidant further improve the strength, the physical property and the oxidation resistance of the low-dielectric-constant fiber film respectively.
The preparation method of the low dielectric constant fiber film provided by the embodiment of the invention can obtain the low dielectric constant fiber film only by simple mixing for multiple times and then carrying out electrostatic spinning and curing steps, has simple process and can realize industrial production.
Drawings
FIG. 1 is a process flow diagram of a method for preparing a low dielectric constant fiber film according to an embodiment of the present invention.
Detailed Description
To make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention are described in detail below with reference to the accompanying drawings. Examples of these preferred embodiments are illustrated in the accompanying drawings. The embodiments of the invention shown in the drawings and described in accordance with the drawings are exemplary only, and the invention is not limited to these embodiments.
It should be noted that, in order to avoid obscuring the present invention with unnecessary details, only the structures and/or processing steps closely related to the scheme according to the present invention are shown in the drawings, and other details not so relevant to the present invention are omitted.
The inventor of the invention provides a low-dielectric-constant fiber film and a preparation method thereof according to the problem that the dielectric constant of a low-dielectric-constant material in the prior art is not low enough, wherein the dielectric constant of the low-dielectric-constant fiber film is less than 2, and the preparation process of the low-dielectric-constant fiber film is simple and can be industrially produced.
The embodiment of the invention firstly provides a low dielectric constant fiber film, which is prepared from electrostatic spinning ink through an electrostatic spinning process, wherein the electrostatic spinning ink comprises the following components in percentage by mass:
5 to 30 percent of main resin, 1 to 5 percent of toughening resin, 5 to 35 percent of filler, 0.01 to 1 percent of dispersant, 30 to 85 percent of solvent, 0.05 to 1 percent of curing agent and 0.01 to 1 percent of antioxidant;
wherein the low dielectric constant fiber film has a dielectric constant of less than 2.
In fact, in the electrostatic spinning ink, the main resin is a film-forming substance, and when the electrostatic spinning ink is subjected to an electrostatic spinning process, the main resin can be crosslinked through a polymer chain, extruded and drawn into filaments in an electrostatic field, and a fiber filament stack-forming fiber film is formed. Therefore, in the electrostatic spinning ink, the mass fraction of the main resin is 5 to 30%, and when the mass fraction of the main resin is within the range, the low dielectric constant fiber film can be obtained when the electrostatic spinning process is carried out again.
Specifically, the main body resin is at least one selected from methoxy diphenyl ether resin, cyanate ester modified epoxy resin, tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer and polyacrylonitrile; in a specific embodiment of the present invention, the preferred host resin is methoxy diphenyl ether resin.
It is worth mentioning that the toughening resin can be crosslinked with the main resin, which is beneficial to improving the toughness of the fiber filaments and the strength of the fiber membrane after membrane formation. Therefore, the electrostatic spinning ink should contain 1-5% by mass of toughening resin to improve the strength of the low dielectric constant fiber film. When the mass fraction of the toughening resin is too low, the toughening resin is too little crosslinked with the main resin, and the strength of the low-dielectric-constant fiber film is not greatly improved; when the mass fraction of the toughening resin is too high, the improvement effect is not obvious compared with that of 1-5%, and resources are wasted. The mass fraction of the toughening resin may be, for example, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5% or 5%.
Specifically, the toughening resin is selected from at least one of thiol-terminated nitrile rubber, chloroprene rubber and polyvinyl chloride rubber; in a specific embodiment of the present invention, the preferred toughening resin is neoprene.
In fact, the filler can further reduce the dielectric constant loss while reducing the thermal expansion coefficient, so as to obtain a lower dielectric constant fiber film. Therefore, when the electrostatic spinning ink contains 5-35% of the filler by mass, the low-dielectric-constant fiber film is obtained by the electrostatic spinning ink through an electrostatic spinning process. In the electrostatic spinning ink, the antioxidant may be present in an amount of, for example, 5%, 10%, 15%, 20%, 25%, 30%, or 35% by mass.
Specifically, the filler is at least one selected from graphene oxide, multi-walled carbon nanotubes, silicon oxide and silicon micropowder; in a particular embodiment of the invention, the preferred filler is silica fume.
The dispersing agent is provided with a polymer chain, one end of the polymer chain is provided with an active group capable of coating the filler, so that the filler is uniformly dispersed in the electrostatic spinning ink, and the other end of the polymer chain is wound with the main resin, so that the stability is improved. Therefore, when the dispersant is contained in the electrostatic spinning ink in a mass fraction of 0.01% to 1%, the filler can be well dispersed and the electrostatic spinning ink is more stable. When the mass fraction of the dispersing agent is too low, the dispersing agent is too small in dosage and has little effect; when the amount of the dispersant is too high, the occupied mass fraction is too large, affecting the film formation of the host resin. In the electrostatic spinning ink, the mass fraction of the dispersant may be, for example, 0.01%, 0.02%, 0.03%, 0.04%, 0.05%, 0.06%, 0.07%, 0.08%, 0.09%, or 0.1%.
Specifically, the dispersant is selected from at least one of polycarboxylate, poly (meth) acrylic acid derivative and maleic anhydride copolymer; in a particular embodiment of the invention, the preferred dispersant is a maleic anhydride copolymer.
The solvent can uniformly disperse the main resin, the toughening resin and the dispersing agent, and can adjust the viscosity of the ink to a proper value, thereby facilitating the ink extrusion during electrostatic spinning and adjusting the thickness of the cellosilk. Therefore, when the solvent is contained in the electrostatic spinning ink in a mass fraction of 30% to 85%, the dispersion degree and viscosity in the electrostatic spinning ink are optimal. When the mass fraction of the solvent is too low, the electrostatic spinning ink cannot be uniformly dispersed; when the mass fraction of the solvent is too high, the viscosity of the electrospinning ink is too low, which is not favorable for obtaining a low dielectric constant fiber film.
Specifically, the solvent is selected from at least one of dimethylformamide, dimethylacetamide, dimethyl sulfoxide, acetone, and xylene; in a particular embodiment of the invention, the preferred solvent is dimethyl sulfoxide.
It is worth mentioning that the curing agent can further crosslink or accelerate crosslinking of the resin polymer chains, so that the fiber membrane has better physical properties, such as: the electrostatic spinning ink is added with 0.05 to 1 mass percent of curing agent, so as to be beneficial to forming a low-dielectric-constant fiber film. In the electrostatic spinning ink, the mass fraction of the curing agent may be, for example, 0.05%, 0.06%, 0.07%, 0.08%, 0.09%, or 0.1%.
Specifically, the curing agent is at least one selected from anhydride, triethylene tetramine, diethylene triamine and N-aminoethyl piperazine; in a particular embodiment of the invention, the preferred curing agent is diethylenetriamine.
In addition, during the manufacturing, storage and use processes of the fiber film, free radicals can be generated under the action of ultraviolet rays and heat to generate oxidative degradation, so that the electrostatic spinning ink contains 0.01-1% of antioxidant by mass fraction to avoid the oxidative degradation of the low-dielectric-constant fiber film. In the electrostatic spinning ink, the antioxidant may be, for example, 0.01%, 0.02%, 0.03%, 0.04%, 0.05%, 0.06%, 0.07%, 0.08%, 0.09%, or 0.1% in mass fraction.
Specifically, the antioxidant is selected from at least one of triphenyl phosphite, diisooctyl phenyl phosphite and bisphenol A; in a particular embodiment of the invention, the preferred antioxidant is bisphenol a.
The low-dielectric-constant fiber film provided by the embodiment of the invention is prepared from electrostatic spinning ink through an electrostatic spinning process, wherein the electrostatic spinning ink comprises main resin, toughening resin, filler, a dispersing agent, a solvent, a curing agent and an antioxidant, the dielectric constant of the low-dielectric-constant fiber film prepared through the electrostatic spinning process is lower than 2, and the thickness of fiber yarns can be adjusted by adjusting the content of the solvent in the process of forming the low-dielectric-constant fiber film. The toughening resin, the curing agent and the antioxidant further improve the strength, the physical property and the oxidation resistance of the low-dielectric-constant fiber film respectively.
The embodiment of the invention also provides a preparation method of the low dielectric constant fiber film, as shown in fig. 1, the preparation method comprises the following steps:
and step S1, dispersing the main resin and the toughening resin in a solvent to obtain a resin dispersion liquid.
In fact, in the step S1, the mixing manner of the host resin and the toughening resin with the solvent is not limited, and the host resin and the toughening resin may be heated and stirred to increase the dispersion speed of the host resin and the toughening resin in the solvent. The heating temperature is 90-200 deg.C, such as 90 deg.C, 110 deg.C, 130 deg.C, 1500 deg.C, 170 deg.C, 180 deg.C, 190 deg.C or 200 deg.C.
Specifically, in the step S1, the main resin, the toughening resin and the solvent are added into a first reaction flask, and the mixture is placed in an oil bath kettle at 90-200 ℃ and stirred, wherein the stirring speed is 400-1000 rpm, and the stirring time is 2-6 hours, so as to obtain a resin dispersion liquid;
and step S2, dispersing the filler and the dispersing agent in a solvent to obtain a filler suspension.
Specifically, in the step S2, the filler, the dispersant and the solvent are added into a second reaction bottle and then stirred, wherein the stirring speed is 400rpm to 1000rpm, and the stirring time is 0.5h to 2.5h, so as to obtain a filler suspension.
The steps S1 and S2 are not limited to a sequence, and may be performed simultaneously or not simultaneously.
And step S3, mixing the resin dispersion liquid and the filler suspension to obtain the mixed ink.
In practice, the mixing manner of the resin dispersion liquid and the filler suspension is not limited, and for example, the resin dispersion liquid may be added to the filler suspension and then the mixture may be left to stand or stirred; the filler suspension may be added to the resin dispersion and then the mixture may be left to stand or stirred.
Specifically, in the step S3, the resin dispersion liquid is added into the filler suspension, and then stirred and mixed, wherein the stirring speed is 600rpm to 2000rpm, and the stirring time is 0.5h to 2h, so as to obtain the mixed ink.
And step S4, mixing the curing agent, the antioxidant and the mixed ink to obtain the electrostatic spinning ink.
Specifically, in the step S4, the curing agent and the antioxidant are added to the mixed ink obtained in the step S3, and then the mixture is stirred, wherein the stirring speed is 500rpm to 1000rpm, and the stirring time is 1.5h to 3h, so that the electrostatic spinning ink is obtained.
And S5, curing the electrostatic spinning ink after an electrostatic spinning process to prepare the low-dielectric-constant fiber film.
Actually, the step S51 includes S51 and step S52.
And in the step S51, the electrostatic spinning ink is subjected to an electrostatic spinning process to obtain a fiber membrane.
In the step S51, the air humidity of the electrospinning process is 30% to 80%, the propulsion speed of the injection pump is 0.4mL/h to 2mL/h, the spinning needle is a flat needle of 0.1mm to 1mm, the spinning voltage is 5kV to 30kV, the distance between the spinning needle and the roller is 5cm to 20cm, and the rotation speed of the roller is 100rpm to 1500 rpm.
The step S52 includes obtaining the low dielectric constant fiber film by performing heat-pressing treatment and then heat-curing on the fiber film obtained by the electrospinning process.
In practice, the fibrous membrane should be cut to a suitable size for the autoclave treatment before the autoclave treatment is performed.
Specifically, the hot-pressing treatment temperature is 80-150 ℃, the pressure is 20-40 PSI, and the time is 10-40 min.
Specifically, the heating and curing process comprises the following steps:
heating the hot-pressed fiber membrane from room temperature to a first temperature within 30-60 min;
heating the fiber membrane at the first temperature for 30-60 min at constant temperature;
heating the fiber membrane from the first temperature to the second temperature within 30-60 min;
and heating the fiber membrane at the second temperature for 30-60 min.
More specifically, the first temperature is 120-180 ℃, and the second temperature is 250-350 ℃.
The preparation method of the low dielectric constant fiber film provided by the embodiment of the invention can obtain the low dielectric constant fiber film only by simple multiple mixing and then electrostatic spinning and curing steps, has simple process and can be industrially produced.
In order to further illustrate the present invention, the following examples are provided to describe a low dielectric constant fiber film and a method for preparing the same in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
A low dielectric constant nanofiber membrane is prepared by an electrostatic spinning process using electrostatic spinning ink, wherein the electrostatic spinning ink comprises the components shown in Table 1.
TABLE 1
The preparation method of the low dielectric constant nanofiber membrane comprises the following steps:
step S1, adding the methoxy diphenyl ether resin, the chloroprene rubber and the dimethyl sulfoxide into a first reaction bottle, placing the mixture into an oil bath kettle at 130 ℃, and stirring the mixture for 3 hours at a stirring speed of 500rpm to obtain a resin dispersion liquid.
And step S2, adding the silicon micropowder, the maleic anhydride copolymer and the dimethyl sulfoxide into a second reaction bottle, and stirring at a stirring speed of 1000rpm for 1h to obtain a filler suspension.
And step S3, adding the resin dispersion liquid obtained in the first reaction bottle into the filler suspension liquid obtained in the second reaction bottle, and stirring at a stirring speed of 1800rpm for 1.5h to obtain the mixed ink.
And step S4, adding diethylenetriamine and bisphenol A into the mixed ink obtained from the second reaction bottle, and stirring for 3 hours at a stirring speed of 500rpm to obtain the electrostatic spinning ink.
And step S5, carrying out electrostatic spinning on the electrostatic spinning ink under the conditions that the air humidity is 35%, the propelling speed of an injection pump is 1.2mL/h, a spinning needle head is a flat needle head with the diameter of 0.3mm, the spinning voltage is 25kV, the distance between the spinning needle head and a roller is 12cm, and the rotating speed of the roller is 680rpm, so as to obtain the fiber membrane.
Cutting the fiber membrane, carrying out hot-pressing treatment for 15min under the conditions of 150 ℃ and 40PSI, then placing the fiber membrane in a muffle furnace, heating the hot-pressed fiber membrane from room temperature to 140 ℃ within 45min, carrying out constant temperature heating at 140 ℃ for 60min, then heating the fiber membrane from 140 ℃ to 320 ℃ within 30min, carrying out constant temperature heating at 320 ℃ for 30min, and finally obtaining the low-dielectric-constant fiber membrane.
And (3) detecting the dielectric constant of the low-dielectric-constant fiber film, wherein the dielectric constant obtained by detection is 1.77.
Example 2
The low-dielectric-constant nanofiber membrane is prepared from electrostatic spinning ink through an electrostatic spinning process, and the components of the electrostatic spinning ink are shown in table 2.
TABLE 2
| Composition (I) | Mass fraction |
| Methoxy |
5 |
| Neoprene | |
| 5％ | |
| Silicon micropowder | 20％ |
| Maleic anhydride copolymer | 0.1％ |
| Dimethyl sulfoxide | 69.8％ |
| Diethylenetriamine | 0.05％ |
| Bisphenol A | 0.05％ |
The method for producing a nanofiber membrane having a low dielectric constant as described above is different from the method for producing example 1 in that the mass fractions of the respective substances in the electrostatic spinning ink are shown in table 2; in the step S1, the stirring speed is 500rpm, and the stirring time is 3 h; in the step S2, the stirring speed is 800rpm, and the stirring time is 2 h; in the step S3, the stirring speed is 1500rpm, and the stirring time is 1.5 h; in the step S5, in the electrospinning process, the advancing speed of the injection pump is 1.8mL/h, and the spinning needle is a 0.5mm flat needle. The other preparation processes in this embodiment are completely the same as those in embodiment 1, and thus are not described again.
And detecting the dielectric constant of the low-dielectric-constant fiber film, wherein the dielectric constant obtained by detection is 1.32.
As can be seen from examples 1 and 2, the low dielectric constant fiber film provided in the embodiments of the present invention has a dielectric constant of less than 2, and the preparation method of the low dielectric constant fiber film is simple and can be used for industrial production.
The foregoing is directed to embodiments of the present application and it is noted that numerous modifications and adaptations may be made by those skilled in the art without departing from the principles of the present application and are intended to be within the scope of the present application.
Claims (10)
1. The low dielectric constant fiber film is characterized in that the low dielectric constant fiber film is prepared by an electrostatic spinning process through electrostatic spinning ink, and the electrostatic spinning ink comprises the following components in percentage by mass:
5 to 30 percent of main resin, 1 to 5 percent of toughening resin, 5 to 35 percent of filler, 0.01 to 1 percent of dispersant, 30 to 85 percent of solvent, 0.05 to 1 percent of curing agent and 0.01 to 1 percent of antioxidant;
wherein the low dielectric constant fiber film has a dielectric constant of less than 2.
2. The low dielectric constant fiber film of claim 1, wherein the host resin is selected from at least one of a methoxy diphenyl ether resin, a cyanate-modified epoxy resin, a tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer, and polyacrylonitrile; and/or the presence of a gas in the gas,
the filler is selected from at least one of graphene oxide, multi-walled carbon nanotubes, silicon oxide and silicon micropowder; and/or the presence of a gas in the gas,
the toughening resin is selected from at least one of thiol-terminated nitrile rubber, chloroprene rubber and polyvinyl chloride rubber; and/or the presence of a gas in the gas,
the curing agent is selected from at least one of anhydride, triethylene tetramine, diethylenetriamine and N-aminoethyl piperazine; and/or the presence of a gas in the gas,
the antioxidant is selected from at least one of triphenyl phosphite, diisooctyl phenyl phosphite and bisphenol A; and/or the presence of a gas in the gas,
the dispersant is selected from at least one of polycarboxylate, poly (meth) acrylic acid derivative and maleic anhydride copolymer; and/or the presence of a gas in the gas,
the solvent is at least one selected from the group consisting of dimethylformamide, dimethylacetamide, dimethylsulfoxide, acetone, and xylene.
3. A method for preparing a low dielectric constant fiber film according to claim 1 or 2, comprising the steps of:
dispersing the main resin and the toughening resin in a solvent to obtain a resin dispersion liquid;
dispersing the filler and the dispersing agent in a solvent to obtain a filler suspension;
mixing the resin dispersion liquid and the filler suspension to obtain mixed ink;
mixing the curing agent, the antioxidant and the mixed ink to obtain electrostatic spinning ink;
and curing the electrostatic spinning ink after an electrostatic spinning process to prepare the low-dielectric-constant fiber film.
4. The method of claim 3, wherein in the electrospinning process, the air humidity is 30% to 80%, the driving speed of the injection pump is 0.4mL/h to 2mL/h, the spinning needle is a flat needle of 0.1mm to 1mm, the spinning voltage is 5kV to 30kV, the distance between the spinning needle and the drum is 5cm to 20cm, and the drum rotation speed is 100rpm to 1500 rpm.
5. The method of claim 3, wherein the curing process comprises: and carrying out hot pressing treatment on the fiber membrane obtained by the electrostatic spinning process, and then carrying out hot curing to obtain the low-dielectric-constant fiber membrane.
6. The method of claim 5, wherein the heat pressing is performed at 80-150 ℃ under 20-40 PSI for 10-40 min.
7. The method for producing a low dielectric constant fiber film according to claim 5 or 6, wherein the heat curing process comprises:
heating the hot-pressed fiber membrane from room temperature to a first temperature within 30-60 min;
heating the fiber membrane at the first temperature for 30-60 min at constant temperature;
heating the fiber membrane from the first temperature to the second temperature within 30-60 min;
and heating the fiber membrane at the second temperature for 30-60 min at constant temperature.
8. The method of claim 7, wherein the first temperature is 120 ℃ to 180 ℃ and the second temperature is 250 ℃ to 350 ℃.
9. The method for producing a low dielectric constant fiber film as defined in claim 3, wherein the mixing conditions of the host resin and the toughening resin with the solvent are an oil bath at 90 to 200 ℃.
10. The method for preparing a low dielectric constant fiber film according to claim 3, wherein the main resin, the toughening resin and the solvent are mixed by stirring at a rotation speed of 400-1000 rpm for 2-6 h; and/or the presence of a gas in the gas,
the mode of mixing the filler, the dispersant and the solvent is stirring, the stirring speed is 400-1000 rpm, and the stirring time is 0.5-2 h; and/or the presence of a gas in the gas,
the mixed ink, the curing agent and the antioxidant are mixed by stirring at the rotating speed of 600-2000 rpm for 0.5-2 h; and/or the presence of a gas in the gas,
the mixed ink, the curing agent and the antioxidant are mixed by stirring at a speed of 500-1000 rpm for 1.5-3 h.
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