CN109777009A - A kind of GR-TiO being used to prepare high density capacitors2- PVDF nanocomposite and preparation method thereof - Google Patents
A kind of GR-TiO being used to prepare high density capacitors2- PVDF nanocomposite and preparation method thereof Download PDFInfo
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- CN109777009A CN109777009A CN201811610583.4A CN201811610583A CN109777009A CN 109777009 A CN109777009 A CN 109777009A CN 201811610583 A CN201811610583 A CN 201811610583A CN 109777009 A CN109777009 A CN 109777009A
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Abstract
The invention discloses a kind of GR-TiO for being used to prepare high density capacitors2The preparation method of-PVDF nanocomposite, by nano-graphene and nano-TiO2Disperse is co-doped in organic polymer matrix PVDF, GR-TiO obtained2The dielectric constant of-PVDF nanocomposite greatly promotes.Meanwhile GR-TiO made from above-mentioned preparation method is utilized the invention also discloses a kind of2- PVDF nanocomposite, the material can be used for preparing high density capacitors, and the dielectric constant of obtained high density capacitors is improved to 37, loss reduces, disruptive field intensity is promoted to 356.0MV/m, energy storage density is promoted to 20.5J/m3.Preparation method of the invention is easy to operate, high-efficient, is suitble to large-scale production, GR-TiO obtained2- PVDF nanocomposite dielectric properties are excellent, can be effectively reduced energy consumption, promote energy-efficient performance；Dielectric film thickness is controllable, and Miniaturized, lightness is simultaneously applied to integrated circuit；Energy storage density is higher, and energy storage capacity is promoted, and the ability enhancing of uniform electric field is suitably applied in and prepares in high density capacitors.
Description
Technical field
The invention belongs to capacitor application field of material technology, and in particular to one kind is used to prepare high energy storage density capacitor
The GR-TiO of device2- PVDF nanocomposite and preparation method thereof.
Background technique
It is each to be widely used in household electrical appliances, traffic, Aeronautics and Astronautics etc. as a kind of highly important energy storage device for capacitor
A field.Now, with the rapid development of electronic integration technology, capacitor is also required to be intended to integrated, micromation, light
The direction of type and high stability.However, dielectric substance is as one important component part of capacitor, its energy storage
It can be largely fixed the performance of capacitor, promoted the energy storage density of dielectric substance, it can effectively promotion capacitor
Device stores the ability of charge and uniform electric field, and capacitor can be minimized more, lightness.In daily life, higher storage
The capacitor of energy density can get up power storage used in peak period when the low power consumption phase, realize that electric energy maximizes
Utilization, achieve the purpose that energy sustainable development.This requires dielectric substance that can have higher dielectric constant, lower Jie
Electrical loss and higher resistance to disruptive field intensity.
It common are the features such as machine high molecular polymer is good with anti-breakdown performance, and dielectric loss is low, and flexibility is strong, but be situated between
Electric constant is relatively low；The features such as inorganic ceramic material has very high dielectric constant, but its brittleness is big, flexible weak pole
The earth limits application industrially.
PVDF thin film capacitor, dielectric constant are about 9.5, and being lost is 0.08, and energy storage density is about 13J/cm3.It is logical
Cross filling TiO2Polymer nanocomposites made from nano ceramic；TiO is being made2After PVDF thin film capacitor,
Its dielectric constant is promoted to 31, is 3 times of PVDF thin film capacitor or so, and loss substantially remains unchanged.TiO2-PVDF
Though thin film capacitor has biggish promotion in dielectric constant compared with PVDF thin film capacitor, nano combined material is also brought simultaneously
The disruptive field intensity of material is significantly reduced to 200.0MV/m, and stability is also lower, thus, TiO2The energy storage of PVDF thin film capacitor
Density simultaneously could not be promoted effectively.In addition, the thickness of nano compound film obtained is very big, the response time is long and is unfavorable for device
Miniaturization, limit its application on certain high density integrated circuits.
Summary of the invention
The purpose of the present invention is to provide a kind of GR-TiO for being used to prepare high density capacitors2- PVDF nanometers multiple
Condensation material and preparation method thereof, by by a small amount of nano-graphene and nano-TiO2Disperse is co-doped with into organic polymer matrix, system
Obtain GR-TiO2The material is used to prepare high density capacitors, gained high energy storage density electricity by-PVDF nanocomposite
The dielectric constant of container is improved to 37, and is lost and is reduced, while disruptive field intensity improves and energy storage density is highly improved,
To efficiently solve the above problem and defect.
The technical solution used in the present invention is:
A kind of GR-TiO being used to prepare high density capacitors2The preparation method of-PVDF nanocomposite, packet
Include following steps:
S1. nano-TiO is weighed in proportion2, nanometer GR, PVDF and solvent, wherein nano-TiO2, nanometer GR and PVDF make
For solute, DMF is as solvent, and nano-TiO2, nanometer GR and PVDF mass ratio be 1:399:9600；Solute and solvent
Amount ratio is 1g:(10~30) L；
S2. the DMF of 15~25ml is taken, stirring while is slowly added to nano-TiO2, 5~10min of sealing stirring；
S3. sealing cover is opened, stirring while is slowly added to a nanometer GR, continues 20~60min of stirring；
S4. 30~60min of ultrasonic disperse continues 10~30min of stirring；
S5., PVDF is divided into two parts of equivalent, is slowly added in step S4 acquired solution in two times, PVDF is added twice
Interval when a length of 2~5min, 2~4h of magnetic agitation obtains GR-TiO so that PVDF sufficiently dissolves at 30~70 DEG C2-
PVDF nanocomposite.
As a further improvement of the foregoing solution, the nano-TiO2Preparation the following steps are included:
1) citric acid is taken, with deionized water dissolving, is stirred, while being slowly dropped into butyl titanate；
2) 30~60min of ultrasound is carried out after stirring 5~30min, 2~4h of sealing stirring at 70~100 DEG C；
3) sealing cover is opened, is placed at 120~150 DEG C after carrying out gel, dry 30~90min at 170~210 DEG C,
Form the gel of porous space structure；
4) gel for taking out the resulting porous space structure of step 3), is placed in Muffle furnace, calcines at 500~700 DEG C
5~7h takes out, and carries out first time grinding, when grinding a length of 20~40min；
5) it grinds for second: alcohol is added, is placed in ball mill, ball milling is carried out with 4000rad/s~5000rad/s,
Suspension and drying out, then 15~30min of grinding is carried out, obtain nano-TiO2。
As a further improvement of the foregoing solution, nano-TiO2In the step 1) of preparation process, the citric acid with it is described
The molar ratio of butyl titanate is 1:5.
As a further improvement of the foregoing solution, nano-TiO2In the step 5) of preparation process, in second of process of lapping
Ball milling when a length of 6~8h.
A kind of GR-TiO being used to prepare high density capacitors2- PVDF nanocomposite, the GR-TiO2-
PVDF nanocomposite is made through preparation method described in Arbitrary Term as above.
A kind of GR-TiO2The preparation method of-PVDF nano compound film, comprising: use sol evenning machine spin coating on ito glass
GR-TiO2- PVDF nanocomposite film forming, is transferred to 1200rad/s~2700rad/s for revolving speed, when the time is set as 25s
It throws away thickness controllably and is the film of 1~10um；Film is placed in baking oven at once, 1~3h is crystallized at 90~130 DEG C, is obtained
GR-TiO2- PVDF nano compound film.
A kind of GR-TiO2The application of-PVDF nano compound film, by GR-TiO as described above2- PVDF is nano combined thin
Film is applied in preparing high density capacitors: use ion sputtering instrument gold-plated as capacitor positive electrode, after in 70~
Anneal 20~40min at 100 DEG C, and high density capacitors are made.
The beneficial effects of the present invention are:
1. the present invention provides a kind of GR-TiO for being used to prepare high density capacitors2- PVDF nanocomposite
Preparation method, by nano-graphene and nano-TiO2Disperse is co-doped in organic polymer matrix PVDF, wherein addition
Nano-TiO2, using the alternate interfacial polarization of the addition of high-dielectric-constant ceramics phase and ceramics, matrix two, it is multiple to improve nanometer
The dielectric properties of condensation material；Meanwhile the nano-graphene of addition has high conductivity, high-ratio surface since its structure is special
Product etc. excellent properties, with nano-TiO2Common addition polymeric matrix PVDF after, nano-graphene can be in polymeric matrix
It is evenly dispersed in PVDF, and play aggregation space charge and form micro- capacity effect, to make GR-TiO obtained2- PVDF nanometers
The dielectric constant of composite material greatly promotes, and then acquisition is flexible stronger, and energy storage density is higher, the wider array of high storage of application range
It can density capacitor.
2. simultaneously, utilizing GR-TiO made from above-mentioned preparation method the present invention also provides a kind of2- PVDF is nano combined
Material, the material can be used for preparing high density capacitors, and the dielectric constant of obtained high density capacitors improves
To 37, loss reduces, disruptive field intensity is promoted to 356.0MV/m, energy storage density is promoted to 20.5J/m3, dielectric properties are excellent,
It can be effectively reduced energy consumption, promote energy-efficient performance；Dielectric film thickness is controllable, and Miniaturized, lightness is simultaneously applied to integrated
Circuit；Energy storage density is higher, and energy storage capacity is promoted, the ability enhancing of uniform electric field.
3. preparation method of the invention is easy to operate, high-efficient, it is suitble to large-scale production, GR-TiO obtained2-PVDF
Nanocomposite, which is suitably applied in, to be prepared in high density capacitors.
Detailed description of the invention
Fig. 1 is nano-TiO2Preparation flow figure；
Fig. 2 is GR-TiO2- PVDF nanocomposite and the preparation flow that high density capacitors are prepared using it
Figure；
Fig. 3 is PVDF, TiO2- PVDF and GR-TiO2The relative dielectric constant of-PVDF；
Fig. 4 is PVDF, TiO2- PVDF and GR-TiO2The loss of-PVDF；
Fig. 5 is PVDF, TiO2- PVDF and GR-TiO2The resistance to disruptive field intensity of-PVDF.
Specific embodiment
The present invention is specifically described below with reference to embodiment, in order to technical field personnel to the present invention
Understanding.It is necessary to it is emphasized that embodiment is only intended to, the present invention will be further described herein, should not be understood as
Limiting the scope of the invention, fields person skilled in the art make the present invention according to foregoing invention content non-
Essential modifications and adaptations should still fall within protection scope of the present invention.Mentioned raw materials following simultaneously are unspecified
, it is commercial product；The processing step or preparation method not referred in detail be work known to a person skilled in the art
Skill step or preparation method.
Embodiment 1
A kind of GR-TiO being used to prepare high density capacitors2The preparation method of-PVDF nanocomposite, packet
Include progress nano-TiO first2Preparation, then by nano-TiO obtained2For GR-TiO2The system of-PVDF nanocomposite
It is standby；
With reference to Fig. 1, wherein the nano-TiO2The preparation method is as follows: take citric acid 4.80g, it is molten with deionized water
Solution, stirring, while being slowly dropped into 8.56ml butyl titanate；Ultrasound 30min is carried out after stirring 10min, is sealed at 70 DEG C
Stir 3h；Sealing cover is opened, is placed at 150 DEG C after carrying out gel, dry 60min, forms porous space structure at 200 DEG C
Gel；Gel is taken out, is placed in Muffle furnace, 6h is calcined at 600 DEG C, is taken out, first time grinding is carried out, when grinding is a length of
30min；20ml alcohol is added, is placed in ball mill, carries out second and grinds, with 4000rad/s ball milling 6h, pour out suspension
And it is dry, then 30min is ground, obtain nano-TiO2；
With reference to Fig. 2, the GR-TiO2The preparation side of-PVDF nanocomposite is as follows: the DMF of 18ml is added dropwise in beaker
In, 0.0798g is added through nano-TiO made from above-mentioned steps2, seal stirring 5min and it first spread out；That stirs is same
When be slowly added to 0.0002g nanometers of GR, continue stir 30min, so that nano particle is well dispersed into solvent DMF；Ultrasound
Disperse 30min, reduce the reunion of particles in solution, after continue stir 30min；19.6g PVDF powder is divided into equivalent
Two parts, every part of 9.8g, in its adition process, be slowly added in solution in the non-caking situation of solution, when interval is a length of
5min, magnetic agitation 3h obtains GR-TiO so that PVDF sufficiently dissolves at 40 DEG C2- PVDF nanocomposite.
A kind of GR-TiO2The preparation method of-PVDF nano compound film, comprising: use sol evenning machine spin coating on ito glass
GR-TiO2- PVDF nanocomposite film forming, while revolving speed is adjusted to 2100rad/s and rotational time is set as in 25s
When throw away the film of thickness 3um；Film is placed in baking oven at once, 1.5h is crystallized at 120 DEG C, obtains GR-TiO2- PVDF nanometers
Laminated film.
Use ion sputtering instrument gold-plated as capacitor positive electrode, anneal 30min at 90 DEG C, obtains high energy storage density
Capacitor finished product 1.
To the dielectric film thickness of high density capacitors finished product 1 obtained, capacitor, dielectric constant, disruptive field intensity and
Energy storage density etc. is tested for the property, as a result as shown in table 1 below:
Table 1 carries out multinomial performance test and result to high density capacitors finished product 1
High density capacitors finished product 1 obtained is compared to pure PVDF thin film capacitor and TiO2- PVDF thin-film capacitor
Device has that higher dielectric constant (as shown in Figure 3), loss also decreases (as shown in Figure 4), resistance to disruptive field intensity is improved
(as shown in Figure 5), and then energy storage density is greatly improved (as shown in table 2).
Table 2 PVDF, TiO2- PVDF and GR-TiO2The energy storage density of-PVDF compares
| Material | PVDF | TiO2-PVDF | GR-TiO2-PVDF |
| Energy storage density (J/cm3) | 15.3 | 5.9 | 20.5 |
Embodiment 2
The present embodiment and the difference of embodiment 1 be only that, revolving speed when the present embodiment spin-coating film is different, obtained
GR-TiO2The thickness of-PVDF nano compound film is different.Shown in table 3 specific as follows:
GR-TiO obtained when different rotating speeds is arranged in table 32The thickness of-PVDF nano compound film
| Revolving speed (rad/s) | 1600 | 1800 | 2100 | 2400 | 2700 |
| Thickness (um) | 5 | 4 | 3 | 2 | 1 |
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitution, combination, letter
Change, should be equivalent substitute mode, be included within the scope of the present invention.
Claims (7)
1. a kind of GR-TiO for being used to prepare high density capacitors2The preparation method of-PVDF nanocomposite, feature
It is, the preparation method comprises the following steps:
S1. nano-TiO is weighed in proportion2, nanometer GR, PVDF and solvent, wherein nano-TiO2, nanometer GR and PVDF be as molten
Matter, DMF is as solvent, and nano-TiO2, nanometer GR and PVDF mass ratio be 1:399:9600；The amount ratio of solute and solvent
For 1g:(10~30) L；
S2. the DMF of 15~25ml is taken, stirring while is slowly added to nano-TiO2, 5~10min of sealing stirring；
S3. sealing cover is opened, stirring while is slowly added to a nanometer GR, continues 20~60min of stirring；
S4. 30~60min of ultrasonic disperse continues 10~30min of stirring；
S5., PVDF is divided into two parts of equivalent, is slowly added in step S4 acquired solution in two times, the interval of PVDF is added twice
2~5min of Shi Changwei, 2~4h of magnetic agitation obtains GR-TiO so that PVDF sufficiently dissolves at 30~70 DEG C2- PVDF nanometers multiple
Condensation material.
2. preparation method according to claim 1, which is characterized in that the nano-TiO2Preparation the following steps are included:
1) citric acid is taken, with deionized water dissolving, is stirred, while being slowly dropped into butyl titanate；
2) 30~60min of ultrasound is carried out after stirring 5~30min, 2~4h of sealing stirring at 70~100 DEG C；
3) sealing cover is opened, is placed at 120~150 DEG C after carrying out gel, dry 30~90min, forms at 170~210 DEG C
The gel of porous space structure；
4) take out the resulting porous space structure of step 3) gel, be placed in Muffle furnace, at 500~700 DEG C calcine 5~
7h takes out, and carries out first time grinding, when grinding a length of 20~40min；
5) it grinds for second: alcohol is added, is placed in ball mill, ball milling is carried out with 4000rad/s~5000rad/s, is poured out outstanding
Turbid and drying, then 15~30min of grinding is carried out, obtain nano-TiO2。
3. preparation method according to claim 2, which is characterized in that in step 1), the citric acid and the metatitanic acid four
The molar ratio of butyl ester is 1:5.
4. preparation method according to claim 2, which is characterized in that the ball milling in step 5), in second of process of lapping
6~8h of Shi Changwei.
5. a kind of GR-TiO for being used to prepare high density capacitors2- PVDF nanocomposite, which is characterized in that described
GR-TiO2- PVDF nanocomposite is made through preparation method described in claim 1-4 Arbitrary Term.
6. a kind of GR-TiO2The preparation method of-PVDF nano compound film, which is characterized in that revolved on ito glass with sol evenning machine
Apply GR-TiO described in claim 52- PVDF nanocomposite film forming, while by revolving speed be adjusted to 1200rad/s~
2700rad/s and to be set as throwing away thickness in 25s for rotational time controllable and be the film of 1~10um；Film is set at once
In baking oven, 1~3h is crystallized at 90~130 DEG C, obtains GR-TiO2- PVDF nano compound film.
7. a kind of GR-TiO2The application of-PVDF nano compound film, which is characterized in that by GR-TiO as claimed in claim 62-
PVDF nano compound film is applied in preparing high density capacitors.
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| CN113501542A (en) * | 2021-07-12 | 2021-10-15 | 中国石油大学(华东) | Dielectric film based on plate-barrier structure nano filler composition |
| CN115058117A (en) * | 2022-06-30 | 2022-09-16 | 佛山科学技术学院 | Ultra-high temperature resistant polymer-based dielectric energy storage nano composite film and preparation method thereof |
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