CN102604280A - Mixed crystal form inorganic nanometer filler/polymer-based composite dielectric film - Google Patents

Mixed crystal form inorganic nanometer filler/polymer-based composite dielectric film Download PDF

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CN102604280A
CN102604280A CN2012100670061A CN201210067006A CN102604280A CN 102604280 A CN102604280 A CN 102604280A CN 2012100670061 A CN2012100670061 A CN 2012100670061A CN 201210067006 A CN201210067006 A CN 201210067006A CN 102604280 A CN102604280 A CN 102604280A
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dielectric film
polymer
tio
mixed crystal
filler
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CN102604280B (en
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朱红
林爽
匡锡文
王芳辉
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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Abstract

The invention discloses a mixed crystal form inorganic nanometer filler/polymer-based composite dielectric film. The film is formed by mixing a fluorine-containing polymer with mixed crystal form nanometer TiO2 and casting. The molar components of two crystal forms in mixed crystal nanometer TiO2 can be controlled according to reaction time: the content of anatase is 36-45 percent, and the content of rutile is 55-64 percent. The composite dielectric film consists of the following components in percentage by mass: 5-40 percent of mixed crystal nanometer TiO2 and 60-95 percent of fluorine-containing polymer. The composite dielectric film is a novel dielectric material with higher dielectric constant and lower dielectric loss. The composite dielectric film with a required dielectric constant can be prepared by controlling the adding proportion of a filler and the crystal form proportion of the filler. The composite dielectric film has a simple preparation process, low composite temperature and wide application prospect, and is environmental-friendly.

Description

A kind of mixing crystal formation inorganic nano-filler/polymer-based carbon compound dielectric film
Technical field
The invention belongs to the compound dielectric film preparation field, particularly a kind of mixing crystal formation nano-TiO 2/ polymer-based carbon compound dielectric film.
Background technology
Polymer-based carbon composite dielectric material with high-k, low-dielectric loss, workability is because the ability of good flexible and store charge, uniform electric field; Therefore unique as a kind of function, widely used functional materials have in hybrid locomotrives, transmitter, space flight military affairs and power storage field etc. very widely and use.At present, dielectric materials mainly contains three types:
1, common dielectric ceramic material: like CaCu 3 Ti 4 O (CCTO), its electric capacity is bigger, and specific inductivity is up to 10 4-10 5(Lin Zhang, et al., Ferroelectrics.2010,405,92.), but this material sintering temperature is high, frangible, and workability is affected.2, polymer materials: high like pvdf (PVDF) snappiness, dielectric loss is little, but the specific inductivity of itself too small (Baojin Chu, et al., science.2006,313,334.) seriously limits its application.3, high dielectric property polymer matrix composite: conductive carbonized titanium (TiC) as additive, is filled into and forms matrix material among the PVDF, and the specific inductivity of matrix material can reach 540 (Fajun Wang under the 100Hz; Et al., Phys.Status Solidi (RRL) .2009,3; 22.); But it receives the serious restriction of seepage flow threshold value, and dielectric loss has very big raising near the seepage flow threshold value, wayward loading level.And be additive by general ceramic material, polymkeric substance is substrate, in conjunction with ceramic high dielectric property and the advantage of polymkeric substance workability, it has advantages such as dielectric properties, higher voltage breaking down field strength and easy-formation preferably, so very big using value is arranged.Like the barium titanate (BaTiO with surface-treated such as Philseok Kim 3) be additive, vinylidene-trifluoro-ethylene copolymer [P (VDF-TrFE)] is substrate, works as BaTiO 3Addition is 50% o'clock, and the specific inductivity of matrix material can reach 33 (Philseok Kim, et al., ACSNANO.2009,3,2581.) under the 100Hz.
But the shortcoming of this method is most of pottery adds comparatively complicacy of preparation methods, and relatively poor with the polymer phase capacitive, is difficult for processing film.The ultra-high dielectric coefficient and the polymeric substrates of most of stupalith differ bigger, and in the time spent of doing that receives external electric field, composite inner can produce inhomogenous electric field, can reduce the compressive strength of matrix material greatly.
Summary of the invention
The object of the invention is to provide a kind of mixing crystal formation inorganic nano-filler/polymer-based carbon compound dielectric film.This laminated film has dielectric properties preferably.
This mixes crystal formation inorganic nano-filler/polymer-based carbon compound dielectric film by the mixed crystal nano-TiO 2Form with fluoropolymer.Its mass percent consists of:
The mixed crystal nano-TiO 25%-40%;
Fluoropolymer 60%-95%.
Said fluoropolymer is a kind of in vinylidene-trifluoro-ethylene copolymer [P (VDF-TrFE)], vinylidene-trifluoro-ethylene-fluorine vinyl chloride copolymer [P (VDF-TrFE-CFE)], the vinylidene-trifluoro-ethylene-chlorotrifluoroethylene [P (VDF-TrFE-CTFE)].
Said mixed crystal nano-TiO 2Be made up of anatase octahedrite, two kinds of crystal formations of rutile, its molar percentage consists of:
Anatase octahedrite 36%-45%;
Rutile 55%-64%.
The present invention's mixing crystal formation inorganic nano-filler/polymer-based carbon compound dielectric film can be made by following method:
1, prepares different crystal forms ratio mixed crystal nano-TiO through circumfluence method 2, mixed crystal TiO 2Different crystal form ratio can be controlled by the reaction times, and its molar percentage consists of:
Anatase octahedrite 36%-45%;
Rutile 55%-64%.
Said return time is 6-18h.
2, the mixed crystal TiO that step 1 is prepared 2, fluoropolymer and solvent N, after dinethylformamide (DMF) mixed, ultrasonic agitation was uniformly dispersed, and formed stable sols; Its mass percent consists of:
The mixed crystal nano-TiO 25%-40%;
Fluoropolymer 60%-95%.
Mixed crystal TiO 2With the mass ratio of fluoropolymer total mass and DMF be 1: 7-10.
3, colloidal sol 80 ± 1 ℃ of casting film-formings on mould that step 2 prepared; Dry 18 ± 1h; Pass through naturally cooling, 120 ± 1 ℃ of annealing 8 ± 1h again, remove residual solvent, promptly obtaining thickness is mixing crystal formation inorganic nano-filler/polymer-based carbon compound dielectric film of 110-150 μ m.
According to above-mentioned preparation method, at described nano-TiO 2In the mass ratio range, regulate its mass ratio, promptly make the compound dielectric film of required differing dielectric constant, the preferred mass ratio is: mixed crystal TiO 2Be 40%, fluoropolymer is 60%.
According to above-mentioned preparation method, at said nano-TiO 2Mix in the crystal formation proportional range, regulate its two kinds of crystal form ratio, promptly make the compound dielectric film of required differing dielectric constant, preferred crystal form ratio is: anatase octahedrite is 37%, and rutile is 63%.
The present invention has following beneficial effect:
A. this mixed crystal nano-TiO 2Filler has overcome the problems that exist in the background technology, and its preparation condition is simple, easy to operate, and the different ratios of two kinds of crystal formations can be controlled through the reaction times.The advantage that it has combined two kinds of different crystal forms has higher dielectric constant and low-dielectric loss very.
B. this filler and substrate dielectric constant differ less; And good with the substrate consistency, so compound dielectric film has dielectric properties preferably, and its dielectric loss does not significantly promote (seeing accompanying drawing); Still maintaining a lower position, is a kind of novel high-dielectric composite material.
C. this film mixes crystal formation TiO through regulating 2The mass ratio range of component and TiO 2Two kinds of crystal form ratio scopes can significantly change the dielectric properties of material, thereby prepare required high dielectric constant film.
D. the preparation technology of this film is simple, combined temp is low and environmentally friendly, can change the shape size of mould as requested, thereby be applicable in different electronicss, the energy storage material.
Laminated film of the present invention, dielectric properties do not have very big sudden change to occur along with the variation of frequency is relatively stable.Laminated film, specific inductivity can be brought up to about 26.
Description of drawings
Fig. 1 is the different mixed crystal TiO of preparation among the embodiment 1,2,3,6 2The relation of specific inductivity of massfraction compound dielectric film (ε) and dielectric loss (tan δ) and frequency.
Fig. 2 is the different mixed crystal ratio TiO of preparation among the embodiment 3,4,5,6 2The relation (100Hz and 1000Hz) of specific inductivity of compound dielectric film (ε) and dielectric loss (tan δ) and frequency, wherein mixed crystal TiO 2Mass percent is 40%.
Embodiment
Below through product and preparation method among concrete embodiment narration the present invention.Unless stated otherwise, used technique means is method known in those skilled in the art among the present invention.In addition, embodiment is interpreted as illustrative, and unrestricted scope of the present invention, essence of the present invention and scope are only limited claims.To those skilled in the art, under the prerequisite that does not deviate from essence of the present invention and scope, various changes or change that conditions such as ratio in these embodiments and solvent are carried out also belong to protection scope of the present invention.
Embodiment 1:
A. prepare the mixed crystal nano-TiO through circumfluence method 2, return time is 6h, and wherein the molar constituent of two kinds of crystal formations is: anatase octahedrite is 45%, and rutile is 55%;
Circumfluence method prepares mixed crystal nano TiO 2 method: use the 100mL deionized water, the 10mL ydrogen peroxide 50 is made into mixed solvent, to wherein slowly dripping butyl(tetra)titanate 2.2g, stirs 30min under the room temperature, 98 ℃ of refluxed 6h afterwards, and the deposition that obtains is from washing 80 ℃ of dry 20h.
B. the mixed crystal TiO2 that 0.0054g step a is prepared; After 0.1000g vinylidene-trifluoro-ethylene copolymer [P (VDF-TrFE)] and 1.0005g solvent DMF are mixed; Ultrasonic agitation is uniformly dispersed, and forms stable sols, and this batching mass percent consists of: mixed crystal TiO 2Be 5%, polymkeric substance is 95%;
C. the colloidal sol 80 ℃ of casting film-formings on mould that step b prepared, dry 18h; Through naturally cooling, 120 ℃ of annealing 8h, promptly prepare TiO again 2/ P (VDF-TrFE) compound dielectric film.Specific inductivity can reach 11.7.Specific inductivity can reach 11.7.
Embodiment 2:
A. prepare the mixed crystal nano-TiO through circumfluence method 2, return time is 6h, and wherein the molar constituent of two kinds of crystal formations is: anatase octahedrite is 45%, and rutile is 55%;
B. the mixed crystal TiO that 0.0247g step a is prepared 2, after 0.1000g vinylidene-trifluoro-ethylene copolymer [P (VDF-TrFE)] and 11313g solvent DMF were mixed, ultrasonic agitation was uniformly dispersed, and formed stable sols, and this batching mass percent consists of: mixed crystal TiO 2Be 20%, polymkeric substance is 80%;
C. the colloidal sol 80 ℃ of casting film-formings on mould that step b prepared, dry 18h; Through naturally cooling, 120 ℃ of annealing 8h, promptly prepare TiO again 2/ P (VDF-TrFE) compound dielectric film.Specific inductivity can reach 17.3.Embodiment 3:
A. prepare the mixed crystal nano-TiO through circumfluence method 2, return time is 6h, and wherein the molar constituent of two kinds of crystal formations is: anatase octahedrite is 45%, and rutile is 55%;
B. the mixed crystal TiO that 0.0667g step a is prepared 2, after 0.1000g vinylidene-trifluoro-ethylene copolymer [P (VDF-TrFE)] and 1.2830g solvent DMF were mixed, ultrasonic agitation was uniformly dispersed, and formed stable sols, and this batching mass percent consists of: mixed crystal TiO 2Be 40%, polymkeric substance is 60%;
C. the colloidal sol 80 ℃ of casting film-formings on mould that step b prepared, dry 18h; Through naturally cooling, 120 ℃ of annealing 8h, promptly prepare TiO again 2/ P (VDF-TrFE) compound dielectric film.Specific inductivity can reach 23.9.
Embodiment 4:
A. prepare the mixed crystal nano-TiO through circumfluence method 2, return time is 9h, and wherein the molar constituent of two kinds of crystal formations is: anatase octahedrite is 37%, and rutile is 63%;
B. the mixed crystal TiO that 0.0667g step a is prepared 2, after 0.1000g vinylidene-trifluoro-ethylene copolymer [P (VDF-TrFE)] and 1.5009g solvent DMF were mixed, ultrasonic agitation was uniformly dispersed, and formed stable sols, mixed crystal TiO 2Be 40%, polymkeric substance is 60%;
C. the colloidal sol 80 ℃ of casting film-formings on mould that step b prepared, dry 18h; Through naturally cooling, 120 ℃ of annealing 8h, promptly prepare TiO again 2/ P (VDF-TrFE) compound dielectric film.Specific inductivity can reach 25.8.
Embodiment 5:
A. prepare the mixed crystal nano-TiO through circumfluence method 2, return time is 18h, and wherein the molar constituent of two kinds of crystal formations is: anatase octahedrite is 36%, and rutile is 64%;
B. the mixed crystal TiO that 0.0667g step a is prepared 2, after 0.1000g vinylidene-trifluoro-ethylene copolymer [P (VDF-TrFE)] and 1.5009g solvent DMF were mixed, ultrasonic agitation was uniformly dispersed, and formed stable sols, mixed crystal TiO 2Be 40%, polymkeric substance is 60%;
C. the colloidal sol 80 ℃ of casting film-formings on mould that step b prepared, dry 18h; Through naturally cooling, 120 ℃ of annealing 8h, promptly prepare TiO2/P (VDF-TrFE) compound dielectric film again.Specific inductivity can reach 22.7.
Embodiment 6:
This group embodiment is the comparative example.0.1000g after vinylidene-trifluoro-ethylene copolymer [P (VDF-TrFE)] and 1.0000g solvent DMF were mixed, ultrasonic agitation was uniformly dispersed, and formed stable sols; With colloidal sol 80 ℃ of casting film-formings on mould of preparation, dry 18h; Through naturally cooling, 120 ℃ of annealing 8h, promptly prepare P (VDF-TrFE) compound dielectric film again.Specific inductivity can reach 12.4.
Embodiment 7:
A. prepare the mixed crystal nano-TiO through circumfluence method 2, return time is 6h, and wherein the molar constituent of two kinds of crystal formations is: anatase octahedrite is 45%, and rutile is 55%;
B. the mixed crystal TiO that 0.0054g step a is prepared 2, after 0.1000g vinylidene-trifluoro-ethylene-fluorine vinyl chloride copolymer [P (VDF-TrFE-CFE)] and 1.0005g solvent DMF were mixed, ultrasonic agitation was uniformly dispersed, and formed stable sols, and this batching mass percent consists of: mixed crystal TiO 2Be 5%, polymkeric substance is 95%;
C. the colloidal sol 80 ℃ of casting film-formings on mould that step b prepared, dry 18h; Through naturally cooling, 120 ℃ of annealing 8h, promptly prepare TiO again 2/ P (VDF-TrFE-CFE) compound dielectric film.
Embodiment 8:
A. prepare the mixed crystal nano-TiO through circumfluence method 2, return time is 6h, and wherein the molar constituent of two kinds of crystal formations is: anatase octahedrite is 45%, and rutile is 55%;
B. the mixed crystal TiO that 0.0247g step a is prepared 2, after 0.1000g vinylidene-trifluoro-ethylene-chlorotrifluoroethylene [P (VDF-TrFE-CTFE)] and 1.1313g solvent DMF were mixed, ultrasonic agitation was uniformly dispersed, and formed stable sols, and this batching mass percent consists of: mixed crystal TiO 2Be 20%, polymkeric substance is 80%;
C. the colloidal sol 80 ℃ of casting film-formings on mould that step b prepared, dry 18h; Through naturally cooling, 120 ℃ of annealing 8h, promptly prepare TiO again 2/ P (VDF-TrFE-CTFE) compound dielectric film.

Claims (7)

1. one kind is mixed crystal formation inorganic nano-filler/polymer-based carbon compound dielectric film, it is characterized in that said compound dielectric film is by fluoropolymer and mixed crystal nano-TiO 2Form, its mass percent consists of: the mixed crystal nano-TiO 25%-40%, fluoropolymer 60%-95%; Said mixing crystal formation inorganic nano-filler/polymer-based carbon compound dielectric film is logical to be made by following method, prepares the mixed crystal nano-TiO through circumfluence method by anatase octahedrite, two kinds of crystal formations of rutile 2, with the mixed crystal nano-TiO 2, fluoropolymer and solvent N, after dinethylformamide mixed, ultrasonic agitation was uniformly dispersed, and formed stable sols; The casting film-forming after drying, residual solvent is removed in cooling, 120 ± 1 ℃ of annealing, promptly gets and mixes crystal formation inorganic nano-filler/polymer-based carbon compound dielectric film.
2. mixing crystal formation inorganic nano-filler according to claim 1/polymer-based carbon compound dielectric film; It is characterized in that said fluoropolymer is a kind of in vinylidene-trifluoro-ethylene copolymer, vinylidene-trifluoro-ethylene-fluorine vinyl chloride copolymer, the vinylidene-trifluoro-ethylene-chlorotrifluoroethylene.
3. mixing crystal formation inorganic nano-filler according to claim 1/polymer-based carbon compound dielectric film is characterized in that, said mixed crystal nano-TiO 2Mixed by anatase octahedrite, two kinds of crystal formations of rutile, its molar percentage consists of: anatase octahedrite 36%-45%, rutile 55%-64%.
4. according to claim 1 or 3 described mixing crystal formation inorganic nano-filler/polymer-based carbon compound dielectric films, it is characterized in that said mixed crystal TiO 2Be 40%, fluoropolymer is 60%.
5. according to claim 1 or 3 described mixing crystal formation inorganic nano-filler/polymer-based carbon compound dielectric films, it is characterized in that said anatase octahedrite is 37%, rutile is 63%.
6. mixing crystal formation inorganic nano-filler according to claim 1/polymer-based carbon compound dielectric film is characterized in that, said mixed crystal TiO 2With the mass ratio of fluoropolymer total mass and DMF be 1: 7-10.
7. according to claim 1 or 3 described mixing crystal formation inorganic nano-filler/polymer-based carbon compound dielectric films, it is characterized in that said anatase octahedrite is 36%, rutile is 64%.
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CN105874030A (en) * 2014-01-02 2016-08-17 汉高知识产权控股有限责任公司 Film containing nano-particulate filler
CN111315817A (en) * 2017-08-09 2020-06-19 阿克马法国公司 Electroactive fluoropolymer composition, preparation, film, electronic device and field effect organic transistor
CN111548515A (en) * 2020-04-15 2020-08-18 哈尔滨理工大学 Post-treatment process of non-oxide ceramic/polyvinylidene fluoride composite film

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105874030A (en) * 2014-01-02 2016-08-17 汉高知识产权控股有限责任公司 Film containing nano-particulate filler
CN105874030B (en) * 2014-01-02 2019-07-26 汉高知识产权控股有限责任公司 Film containing nanoparticle filler
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CN111315817A (en) * 2017-08-09 2020-06-19 阿克马法国公司 Electroactive fluoropolymer composition, preparation, film, electronic device and field effect organic transistor
CN111548515A (en) * 2020-04-15 2020-08-18 哈尔滨理工大学 Post-treatment process of non-oxide ceramic/polyvinylidene fluoride composite film
CN111548515B (en) * 2020-04-15 2023-05-09 哈尔滨理工大学 Post-treatment process of non-oxide ceramic/polyvinylidene fluoride composite film

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