CN107200858A - A kind of preparation method of high temperature resistant Kynoar dielectric film - Google Patents

A kind of preparation method of high temperature resistant Kynoar dielectric film Download PDF

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Publication number
CN107200858A
CN107200858A CN201710572963.2A CN201710572963A CN107200858A CN 107200858 A CN107200858 A CN 107200858A CN 201710572963 A CN201710572963 A CN 201710572963A CN 107200858 A CN107200858 A CN 107200858A
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kynoar
film
magnesium chloride
high temperature
temperature resistant
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王海军
李镇伟
阮潇潇
杨茜
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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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
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • 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
    • C08J2327/00—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 at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2327/02—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 at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/12—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 at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08J2327/16—Homopolymers or copolymers of vinylidene fluoride
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2217—Oxides; Hydroxides of metals of magnesium
    • C08K2003/222—Magnesia, i.e. magnesium oxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/16—Applications used for films
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Laminated Bodies (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

A kind of preparation method of high temperature resistant Kynoar dielectric film, includes following steps：1）With N, N-dimethylformamide（DMF）As the different quality that solvent compound concentration is 5% than Kynoar/magnesium chloride casting solution；2）By step 1）Middle different quality than casting solution instill on slide, and the film-forming on Thermostatic platform；3）By step 2）Obtained cured film melts elimination thermal history in thermal station, and then fast cooling is fully crystallized to 155 DEG C of thermostatical crystallizations to blend film；The preparation method technique of Kynoar dielectric film of the present invention is simple and convenient to operate and excellent performance, as high temperature resistant, corrosion-resistant, piezoelectricity and ferroelectricity are stronger, it can be achieved as a kind of high temperature resistant functional high molecule material, have potential application value in terms of capacitor, sensor, information storage, electronic device and resistant to elevated temperatures temperature-sensitive material.

Description

A kind of preparation method of high temperature resistant Kynoar dielectric film
Technical field
The invention belongs to the preparing technical field of γ ' phase polyvinylidene fluoride based coextruded films, and in particular to a kind of high temperature resistant The preparation method of Kynoar dielectric film.
Background technology
The functionalization of polymer thin-film material is constantly subjected to extensive concern, has the polymeric material of property by it Become research focus.
Kynoar is that, with polymorphous polymer, wherein α phase polyvinylidene fluorides have excellent mechanical property, can With used in electronics, chemical industry, solar device etc.；Beta phase polyvinylidene fluoride has good piezo-electric effect, is widely used in each The energy transducer in field, such as pressure-sensitive device, wet sensitive device；γ ' mutually has good ferroelectricity, piezoelectricity and high temperature resistant, can To be applied in terms of memory device with intelligent electric appliance, but the γ ' phases crystal formation of Kynoar is typically prepared, it is necessary at high temperature For a long time, it is unfavorable for industrialization.
The content of the invention
To overcome above-mentioned the deficiencies in the prior art, it is an object of the invention to provide a kind of high temperature resistant Kynoar dielectric film Preparation method, with reaction temperature is low, the time is short, be easy to industrialized feature.
To achieve these goals, the technical solution adopted by the present invention is：A kind of high temperature resistant Kynoar dielectric film Preparation method, chlorination mg-doped makes Kynoar γ phases induce α phase phase transformations, comprises the following steps：
1）By magnesium chloride powder using the particle that mortar grinder is 1 μm of average grain diameter, weigh matter average molecular weight for 107000 it is poly- Vinylidene pellet, uses DMF（DMF）As solvent compound concentration for 5% different quality than polyvinylidene fluoride Alkene/magnesium chloride casting solution, blending mass ratio is respectively 0.5:0.0005,0.5:0.0015；
2）By step 1）Middle different quality than casting solution instill on slide, and the film-forming on Thermostatic platform；
3）By step 2）Obtained cured film melts 10min in 200 DEG C ~ 230 DEG C of thermal station and eliminates thermal history, then fast prompt drop Temperature is fully crystallized to 155 DEG C of 4 ~ 12h of thermostatical crystallization to blend film.
Blend film after crystallization is used into differential scanning calorimeter, infrared spectrum, the means such as petrographic microscope characterize poly- The crystal formation of vinylidene based coextruded film is the shape characteristic of γ ' crystal formations and γ ' crystal formations.
The beneficial effects of the invention are as follows：
The method that the present invention prepares high temperature resistant Kynoar dielectric composite film using solution-casting method, in certain condition Under, it is prepared for the poly-vinylidene-fluoride composite film of a kind of high content high temperature resistant and the γ ' crystal with pole.Present invention employs macromolecule Crystalline material composite inorganic material, preparing, there is dielectricity multifunctional composite film to replace traditional ceramic-like dielectric material, system Preparation Method technique is simple and convenient to operate, imparts Kynoar excellent dielectric properties and heat-resisting quantity, is expected to pass in pressure Applied in the fields such as sensor, lithium ion battery, automobile motor, high-temperature-resisting thermosensitive resistance device.
Brief description of the drawings
Fig. 1 is the melting polarisation shape appearance figure in situ of the embodiment of the present invention 1, embodiment 2；Wherein Fig. 1（a）Exist for embodiment 1 The polarisation shape appearance figure of crystal is cultivated at 155 DEG C；Fig. 1（b）Cultivated for embodiment 1 at 155 DEG C after crystal, it is molten at 174 DEG C Melt polarisation shape appearance figure；Fig. 1（c）Cultivated for embodiment 1 at 155 DEG C after crystal, the melting polarisation shape appearance figure at 180 DEG C；Fig. 1 （d）The polarisation shape appearance figure of crystal is cultivated at 155 DEG C for embodiment 2；Fig. 1（e）Cultivated for embodiment 2 at 155 DEG C after crystal, Melting polarisation shape appearance figure at 174 DEG C；Fig. 1（f）Cultivated at 155 DEG C after crystal, the melting polarisation pattern at 180 DEG C Figure.
Fig. 2 is differential scanning calorimeter schematic diagram of the invention；Wherein PVDF is the differential scanning calorimeter of embodiment 1； PVDF/MgCl2It is the differential scanning calorimeter of embodiment 2.
Fig. 3 is wide-angle X ray diffractor figure of the present invention；Wherein, PVDF is the wide-angle X ray diffractor figure of embodiment 1； PVDF/MgCl2It is the wide-angle X ray diffractor figure of embodiment 3.
Embodiment
The present invention is described in further detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1：
1）By magnesium chloride powder using the particle that mortar grinder is 1 μm of average grain diameter, weigh matter average molecular weight for 107000 it is poly- Vinylidene pellet, uses DMF（DMF）As solvent compound concentration for 5% different quality than polyvinylidene fluoride Alkene/magnesium chloride casting solution, blending mass ratio is divided into 0.5g:0；What is be blended is the conclusion gone out compared with pure, at 155 DEG C, Pure PVDF can not generate γ ' crystal formations；
2）By step 1）Middle different quality than casting solution instill on slide, and the film-forming on Thermostatic platform；
3）By step 2）Obtained cured film melts 10min in 200 DEG C of thermal station and eliminates thermal history, and then fast cooling is arrived 155 DEG C of thermostatical crystallization 12h, are fully crystallized to blend film；
Blend film after crystallization is used into infrared spectrum, Raman spectrum, differential scanning calorimeter, petrographic microscope, scanning electricity The crystal formation that the means such as sub- microscope characterize Kynoar based coextruded film only has alpha-crystal form.
Embodiment 2：
1）By magnesium chloride powder using the particle that mortar grinder is 1 μm of average grain diameter, weigh matter average molecular weight for 107000 it is poly- Vinylidene pellet, uses DMF（DMF）As solvent compound concentration for 5% different quality than polyvinylidene fluoride Alkene/magnesium chloride casting solution, Kynoar pellet is 0.4g, and magnesium chloride is 0.0004g；
2）By step 1）Middle different quality than casting solution instill on slide, and the film-forming on Thermostatic platform；
3）By step 2）Obtained cured film melts 10min in 200 DEG C of thermal station and eliminates thermal history, and then fast cooling is arrived 155 DEG C of thermostatical crystallization 12h, are fully crystallized to blend film；
Blend film after crystallization is used into infrared spectrum, Raman spectrum, differential scanning calorimeter, petrographic microscope, scanning electricity The means such as sub- microscope, which characterize Kynoar based coextruded film, γ ' crystal formation shape characteristics, and at 180 DEG C of γ crystal formations fusing point Do not melt.
Embodiment 3：
1）By magnesium chloride powder using the particle that mortar grinder is 1 μm of average grain diameter, weigh matter average molecular weight for 107000 it is poly- Vinylidene pellet, uses DMF（DMF）Cast as solvent compound concentration for 5% Kynoar/magnesium chloride Film liquid, Kynoar pellet is 0.45g, and magnesium chloride is 0.00135g；
2）By step 1）Middle different quality than casting solution instill on slide, and the film-forming on Thermostatic platform；
3）By step 2）Obtained cured film melts 10min in 230 DEG C of thermal station and eliminates thermal history, and then fast cooling is arrived 155 DEG C of thermostatical crystallization 4h, are fully crystallized to blend film；
Blend film after crystallization is used into infrared spectrum, Raman spectrum, differential scanning calorimeter, petrographic microscope, scanning electricity It is γ ' crystal formation characteristic peaks that the means such as sub- microscope, which characterize Kynoar based coextruded film,.
Embodiment 4：
1）By magnesium chloride powder using the particle that mortar grinder is 1 μm of average grain diameter, weigh matter average molecular weight for 107000 it is poly- Vinylidene pellet, uses DMF（DMF）As solvent compound concentration for 5% different quality than polyvinylidene fluoride Alkene/magnesium chloride casting solution, Kynoar pellet is 0.45g, and magnesium chloride is 0.00135g；
2）By step 1）Middle different quality than casting solution instill on slide, and the film-forming on Thermostatic platform；
3）By step 2）Obtained cured film melts 10min in 215 DEG C of thermal station and eliminates thermal history, and then fast cooling is arrived 155 DEG C of thermostatical crystallization 7h, are fully crystallized to blend film；
Referring to Fig. 1（a~c）With Fig. 1（d~f）Understand, under certain condition, add after magnesium chloride, Kynoar has high content γ ' crystal generation.
It can be seen from Fig. 2, pure Kynoar only occurs in that a melting peak, adds after magnesium chloride, Kynoar exists 183 DEG C occur in that γ ' crystal melting peaks.
It can be seen from Fig. 3, pure Kynoar only has alpha-crystal characteristic peak, adds after magnesium chloride, and the α of Kynoar is brilliant Body characteristicses peak disappears, and only occurs in that γ ' crystal characteristic peaks.

Claims (3)

1. a kind of preparation method of high temperature resistant Kynoar dielectric film, it is characterised in that include following steps：
1）With N, N-dimethylformamide（DMF）As the different quality that solvent compound concentration is 5% than Kynoar/magnesium chloride Casting solution, blending mass ratio is respectively 0.5:0.0005,0.5:0.0015；
2）By step 1）Middle different quality than casting solution instill on slide, and the film-forming on Thermostatic platform；
3）By step 2）Obtained cured film melts 10min in 200 DEG C ~ 230 DEG C of thermal station and eliminates thermal history, then fast prompt drop Temperature is fully crystallized to 155 DEG C of 4 ~ 12h of thermostatical crystallization to blend film.
2. a kind of preparation method of high temperature resistant Kynoar dielectric film according to claim 1, it is characterised in that including There are following steps：
1）By magnesium chloride powder using the particle that mortar grinder is 1 μm of average grain diameter, weigh matter average molecular weight for 107000 it is poly- Vinylidene pellet, uses DMF（DMF）Cast as solvent compound concentration for 5% Kynoar/magnesium chloride Film liquid, Kynoar pellet is 0.4g, and magnesium chloride is 0.0004g；
2）By step 1）Middle casting solution is instilled on slide, and the film-forming on Thermostatic platform；
3）By step 2）Obtained cured film melts 10min in 200 DEG C of thermal station and eliminates thermal history, and then fast cooling is arrived 155 DEG C of thermostatical crystallization 6h, are fully crystallized to blend film.
3. a kind of preparation method of high temperature resistant Kynoar dielectric film according to claim 1, it is characterised in that including There are following steps：
1）By magnesium chloride powder using the particle that mortar grinder is 1 μm of average grain diameter, weigh matter average molecular weight for 107000 it is poly- Vinylidene pellet, uses DMF（DMF）Cast as solvent compound concentration for 5% Kynoar/magnesium chloride Film liquid, Kynoar pellet is 0.45g, and magnesium chloride is 0.00135g；
2）By step 1）Middle casting solution is instilled on slide, and the film-forming on Thermostatic platform；
3）By step 2）Obtained cured film melts 10min in 230 DEG C of thermal station and eliminates thermal history, and then fast cooling is arrived 155 DEG C of thermostatical crystallization 4h, are fully crystallized to blend film.
CN201710572963.2A 2017-07-14 2017-07-14 A kind of preparation method of high temperature resistant Kynoar dielectric film Pending CN107200858A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112708154A (en) * 2021-01-08 2021-04-27 陕西科技大学 Nucleation method for improving polyvinylidene fluoride gamma phase
CN113773531A (en) * 2021-08-04 2021-12-10 聚埃麦德(苏州)科技有限公司 Preparation method of polyimide film

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20090030825A (en) * 2007-09-21 2009-03-25 경희대학교 산학협력단 METHOD FOR PRODUCING POLY(VINYLIDENE FLUORIDE) FILM WITH HIGH beta-TYPE CRYSTAL STRUCTURE
CN104923089A (en) * 2015-06-16 2015-09-23 陕西科技大学 Method for preparing polyvinylidene fluoride porous membrane
CN105540535A (en) * 2015-12-29 2016-05-04 陕西科技大学 Method for preparing multi-scale high-gamma-phase polyvinylidene fluoride hollow nanowires
CN106009426A (en) * 2016-05-26 2016-10-12 陕西科技大学 Preparation method of MgCl2-doped annular gamma-phase polyvinylidene-fluoride-base composite film

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20090030825A (en) * 2007-09-21 2009-03-25 경희대학교 산학협력단 METHOD FOR PRODUCING POLY(VINYLIDENE FLUORIDE) FILM WITH HIGH beta-TYPE CRYSTAL STRUCTURE
CN104923089A (en) * 2015-06-16 2015-09-23 陕西科技大学 Method for preparing polyvinylidene fluoride porous membrane
CN105540535A (en) * 2015-12-29 2016-05-04 陕西科技大学 Method for preparing multi-scale high-gamma-phase polyvinylidene fluoride hollow nanowires
CN106009426A (en) * 2016-05-26 2016-10-12 陕西科技大学 Preparation method of MgCl2-doped annular gamma-phase polyvinylidene-fluoride-base composite film

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112708154A (en) * 2021-01-08 2021-04-27 陕西科技大学 Nucleation method for improving polyvinylidene fluoride gamma phase
CN112708154B (en) * 2021-01-08 2022-06-07 陕西科技大学 Nucleation method for improving polyvinylidene fluoride gamma phase
CN113773531A (en) * 2021-08-04 2021-12-10 聚埃麦德(苏州)科技有限公司 Preparation method of polyimide film

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Application publication date: 20170926