CN107245152B - A kind of preparation method of magnesia/polystyrene composite dielectric material - Google Patents
A kind of preparation method of magnesia/polystyrene composite dielectric material Download PDFInfo
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- CN107245152B CN107245152B CN201710340107.4A CN201710340107A CN107245152B CN 107245152 B CN107245152 B CN 107245152B CN 201710340107 A CN201710340107 A CN 201710340107A CN 107245152 B CN107245152 B CN 107245152B
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
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- 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
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- 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
- C08K2003/2224—Magnesium hydroxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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Abstract
The present invention relates to nanocomposite technical fields, it is desirable to provide a kind of preparation method of magnesia/polystyrene composite dielectric material.Include: that polystyrene is added into n,N-Dimethylformamide, transparent clear solution is obtained after stirring；By magnesium oxide dispersion in transparent clear solution, uniform suspension is obtained；It is dry at a temperature of 60 DEG C by suspension after tape casting, obtain magnesia/polystyrene composite dielectric material of film-form.The present invention is distributed more uniform characteristic in magnesia and polystyrene using electric field, under lower packing volume, improves the synthesis dielectric properties of composite material；Preparation process of the present invention is simple, strong operability, and raw material is easy to get to suitable industrialized production.The volume fraction that inorganic filler can be inserted by adjusting, adjusts polymer matrix composite dielectric properties.Inorganic Fillers Filled volume is low, and the promotion of good dielectric properties is obtained under filling fraction only 8%, can keep the good toughness of polymer.
Description
Technical field
The present invention relates to a kind of preparation methods of magnesia polymer thin film composite material, belong to nanocomposite technology
Field.
Background technique
The advantages that polymer composite dielectric material is because of its easy processing, stability is good, light weight is small in integrated circuit, device
Type, energy storage are equipped and electrowetting, microfluid etc. extensive use.It is buried for example, polymer composites can be prepared into
Enter formula capacitor, is conducive to the preparation of electron and electrician integrated circuits；The high polymer composites of resistance to breakdown that are situated between of preparation, are improved
The electric energy energy storage density of material, is conducive to the preparation of energy storage device；The high hydrophobic insulating polymer composites that are situated between of preparation, can
As drain insulating layer, for the preparation in electrowetting, microfluidic device.Polymer composites are because its is excellent on the whole
Performance and wide applicability have the meaning and value of further investigation.
Polystyrene has stable physics and chemical structure as one of industrial polymer is applied to earliest,
Anti- water suction humidity resistance is excellent, and thermal stability and good fluidity when melting, high frequency characteristics is good, is easy to various modes and is processed into
Type, it is suitable for mass production.But the dielectric constant of polystyrene itself is lower, greatly limits it in capacitor, energy storage, electrowetting
Etc. dielectrics field application.
Summary of the invention
The problem to be solved in the present invention is to overcome deficiency in the prior art, and it is compound to provide a kind of magnesia/polystyrene
The preparation method of dielectric material.
In order to solve the technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of magnesia/polystyrene composite dielectric material is provided, is included the following steps:
(1) polystyrene is added into n,N-Dimethylformamide, transparent clear solution is obtained after stirring；By magnesia point
It dissipates in transparent clear solution, obtains uniform suspension；
Wherein, the mass ratio of n,N-Dimethylformamide and polystyrene is 5~10: 1；Magnesia and transparent clear solution
Mass ratio be 2%~8%；
(2) dry at a temperature of 60 DEG C by suspension after tape casting, obtain magnesia/polystyrene of film-form
Composite dielectric material.
In the present invention, the magnesia is prepared by following manner:
A, by four water magnesium acetates (Mg (Ac)2) and polyvinylpyrrolidone (PVP) be added ethylene glycol in, four water magnesium acetates with
The mass ratio of polyvinylpyrrolidone is 1: 100；It moves into and is connected in the reactor of condensation reflux unit after stirring, control reaction temperature
Degree is between 180~185 DEG C；After reaction 2 hours, cooled to room temperature；
When adding reactant, the mass ratio for controlling four water magnesium acetates and ethylene glycol is 1: 29 to prepare sheet magnesia；
Alternatively, the mass ratio of four water magnesium acetates of control and ethylene glycol is 1: 39, to prepare particulate oxidation magnesium；
B, the troubled liquor that centrifuge separation reaction obtains first alternately washs precipitated product at least with ethyl alcohol again with deionized water
After two-wheeled, by precipitated product in 60 DEG C of at a temperature of drying, presoma magnesium hydroxide is obtained；
C, by the calcination in 500 DEG C of air of presoma magnesium hydroxide, magnesia is obtained.
In the present invention, stirring described in step (1) refers to: 6h is stirred at room temperature.
In the present invention, in the step (1) before addition magnesia, first by magnesia in cell disruptor at ultrasonic disperse
Manage 1h.
In the present invention, dispersion described in step (1) refers to: again with magnetic agitation 12h after ultrasonic disperse processing 2h.
In the present invention, suspension obtained by step (1) is moved in vacuum evacuation device, vacuumizes 1h to exclude bubble.
In the present invention, drying time described in step (2) is 6h.
In the present invention, calcination described in step c refers to: 3h is sintered in Muffle furnace.
Inventive principle description:
Present invention employs the methods that filling magnesia improves polystyrene dielectric constant, that is, pass through simply reflux preparation
Technology prepares different-shape nano magnesium oxide powder, prepares composite material by solution blending, tape casting, utilizes electric field
It is distributed more uniform characteristic in magnesia and polystyrene, in the case where magnesia fills the lower situation of content, improves composite wood
The synthesis dielectric properties of material.
Compared with the prior art, the advantages of the present invention are as follows:
1, by the technology of preparing that simply flows back, sheet and the nano oxidized magnesium dust of graininess are prepared, it is total by solution
Mixed, tape casting prepares composite material, more uniform characteristic is distributed in magnesia and polystyrene using electric field, lower
Under packing volume, the synthesis dielectric properties of composite material are improved.
2, preparation process of the present invention is simple, strong operability, and raw material is easy to get to suitable industrialized production.Tune can be passed through
The volume fraction of section filling inorganic filler, adjusts polymer matrix composite dielectric properties.Inorganic Fillers Filled volume is low, is filling out
Sufficiently number only obtains the promotion of good dielectric properties under 8%, can keep the good toughness of polymer.
Detailed description of the invention
Fig. 1 is the SEM photograph of sheet magnesia (M150) prepared in embodiment.
Fig. 2 is the SEM photograph of particulate oxidation magnesium (M200) prepared in embodiment.
Fig. 3 is the magnesia of two kinds of patterns and its XRD spectrum of presoma.
Specific embodiment
The following examples can make the professional technician of this profession that the present invention be more fully understood, but not with any side
The formula limitation present invention:
Below with reference to embodiment and comparative example, the invention will be further described.
Embodiment 1-8
(1) in the three-necked flask of Xiang Shengyou ethylene glycol, four water magnesium acetates and polyvinylpyrrolidone, four water magnesium acetates are added
Mass ratio with polyvinylpyrrolidone is 1: 100；Three-necked flask is moved in heater, condensation reflux unit has been overlapped, is led to
Enter condensed water；Control reaction temperature is at 180~185 DEG C, after reaction two hours, cooled to room temperature.
When adding reactant, the mass ratio for controlling four water magnesium acetates and ethylene glycol is 1: 29 to prepare sheet magnesia
(number M150, flaky)；Alternatively, the mass ratio of four water magnesium acetates of control and ethylene glycol is 1: 39, to prepare graininess oxygen
Change magnesium (number M200, be in granular form).
(2) troubled liquor that centrifuge separation reaction obtains, by white precipitate product deionized water and ethyl alcohol alternately washing 2
Wheel is moved back to baking oven, in 60 DEG C of at a temperature of drying, obtains presoma magnesium hydroxide.Presoma magnesium hydroxide is moved into Muffle furnace
In, it is sintered 3h at 500 DEG C, obtains magnesia.By magnesia in cell disruptor ultrasonic disperse 1h, it is spare.
(3) polystyrene is dissolved in n,N-Dimethylformamide (DMF), 6h is stirred at room temperature, obtained transparent clear
Clear solution.Smashed magnesia is taken to be added in clear solution, magnetic agitation 12h again after ultrasonic disperse 2h.Control N, N- diformazan
The mass ratio of base formamide and polystyrene is 5~10: 1；The mass ratio of magnesia and transparent clear solution is 2%~8%.
(4) above-mentioned well dispersed suspension is moved into vacuum pumping glass vessel, vacuumizes and excludes bubble 1h.Then flowing
Prolong tape casting on machine, moves to vacuum oven drying in 60 DEG C of dry 6h, so that solvent is sufficiently volatilized, obtain the oxidation of film-form
Magnesium/polystyrene composite dielectric material (number is as shown in table 1,2).
(5) it is plated respectively on composite membrane two sides with a thickness of 150nm by vacuum coating equipment, diameter is 20mm fine copper as electricity
Pole carries out subsequent electrical performance testing.
Table 1
Comparative example (embodiment 9)
(1) polystyrene is dissolved in DMF, wherein polystyrene and the control of DMF mass ratio are 1:5, are stirred at room temperature
6h is mixed, transparent clear solution is obtained.
(2) above-mentioned clear solution is moved into vacuum glass vessel, vacuumizes and excludes bubble 1h.Then it is cast on casting machine
Molding moves to vacuum oven drying in 60 DEG C of dry 6h, solvent is made sufficiently to volatilize, obtains control polystyrene film.
(3 are plated respectively on composite membrane two sides with a thickness of 150nm by vacuum coating equipment, and diameter is 20mm fine copper as electricity
Pole carries out subsequent electrical performance testing.
Implementation result compares
Fig. 1, Fig. 2 show the SEM figure of two kinds of pattern MgO of preparation, and Fig. 1 M150 is flaky；Fig. 2 is M200, is in
Graininess, particle size 50-100nm.It can be seen that the MgO stable appearance prepared, size uniformity.Fig. 3 is two kinds of patterns
The XRD spectrum of magnesia and its presoma, it can be seen that presoma powder is hexagonal phase magnesium hydroxide (PDF#07-0239), through sky
In gas after 500 DEG C of sintering 3h, it is completely transformed into cubic phase magnesia (PDF#45-0946).
Table 1 gives the dielectric properties for the laminated film that example in embodiment and comparative example is prepared.It can be with from table
Find out, whether sheet magnesia (M150) or particulate oxidation magnesium (M200), dielectric constant is with Inorganic Fillers Filled
The raising of amount and increase, when filling fraction is only 6%, dielectric constant reaches maximum, is the 1.5 of pure polystyrene dielectric constant
Times or so, and dielectric loss is held in reduced levels.In general, the draw ratio of filler particles is higher, is more advantageous to and reaches
The dielectric constant of material is improved to percolation threshold, under identical filling fraction, sheet magnesia dielectric constant is higher.
Table 2
It should be noted that above-described embodiment is only illustrative of the invention and is not intended to limit the scope of the invention.Furthermore
It should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or be repaired to the present invention
Change, these equivalent forms also fall within the scope of the appended claims of the present application.
Claims (7)
1. a kind of magnesia/polystyrene composite dielectric material preparation method, which is characterized in that include the following steps:
(1) polystyrene is added into n,N-Dimethylformamide, transparent clear solution is obtained after stirring；By magnesium oxide dispersion in
In transparent clear solution, uniform suspension is obtained；
Wherein, the mass ratio of n,N-Dimethylformamide and polystyrene is 5 ~ 10: 1；The matter of magnesia and transparent clear solution
Amount is than being 2% ~ 8%；
The magnesia is prepared by following manner:
A, four water magnesium acetates and polyvinylpyrrolidone are added in ethylene glycol, the matter of four water magnesium acetates and polyvinylpyrrolidone
Amount is than being 1: 100；After stirring move into be connected in the reactor of condensation reflux unit, control reaction temperature 180~185 DEG C it
Between；After reaction 2 hours, cooled to room temperature；
When adding reactant, the mass ratio for controlling four water magnesium acetates and ethylene glycol is 1: 29 to prepare sheet magnesia；Alternatively,
The mass ratio for controlling four water magnesium acetates and ethylene glycol is 1: 39, to prepare particulate oxidation magnesium；
B, the troubled liquor that centrifuge separation reaction obtains first alternately washs precipitated product at least two-wheeled with deionized water with ethyl alcohol again
Afterwards, precipitated product is obtained into presoma magnesium hydroxide in 60 DEG C of at a temperature of drying；
C, by the calcination in 500 DEG C of air of presoma magnesium hydroxide, magnesia is obtained；
(2) dry at a temperature of 60 DEG C by suspension after tape casting, the magnesia/polystyrene for obtaining film-form is compound
Dielectric material.
2. the method according to claim 1, wherein stirring as described in step (1) refers to: being stirred at room temperature
6h。
3. the method according to claim 1, wherein in step (1) add magnesia before, first by magnesia
Ultrasonic disperse handles 1h in cell disruptor.
4. the method according to claim 1, wherein dispersion as described in step (1) refers to: ultrasonic disperse processing
Again with magnetic agitation 12h after 2h.
5. the method according to claim 1, wherein suspension obtained by step (1) is moved in vacuum evacuation device,
1h is vacuumized to exclude bubble.
6. the method according to claim 1, wherein drying time described in step (2) is 6h.
7. the method according to claim 1, wherein calcination described in step c refers to: being sintered in Muffle furnace
3h。
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| EP0227037A2 (en) * | 1985-12-23 | 1987-07-01 | MITSUI TOATSU CHEMICALS, Inc. | Process for producing a porous film |
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| CN101323692A (en) * | 2008-07-04 | 2008-12-17 | 清华大学 | Polymer-based high energy storage density material and preparing method thereof |
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| EP0227037A2 (en) * | 1985-12-23 | 1987-07-01 | MITSUI TOATSU CHEMICALS, Inc. | Process for producing a porous film |
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