CN109626992A - A kind of bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material and preparation method thereof - Google Patents
A kind of bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of bismuth sodium titanate-barium titanate/polyimide-based dielectric composite materials and preparation method thereof, belong to dielectric composite material technical field.Polymeric dielectric constant to solve the problems, such as preparation media capacitor is relatively low, and the present invention prepares bismuth sodium titanate-barium titanate particle using solid phase method；4,4 '-diaminodiphenyl ethers and bismuth sodium titanate-barium titanate particle are added in n,N-Dimethylformamide, then precursor solution is made in pyromellitic dianhydride addition mixed solution；Imidizate processing is carried out after film is made in precursor solution, obtaining doping is 1~15vol.% of dielectric composite material volume, bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material of relative dielectric constant with higher.Dielectric composite material of the present invention, which is used for dielectric capacitor, can be improved the energy density of dielectric capacitor, can be applicable to the electronic equipment of pulse power and further realize the miniaturization of high power electronic equipment.
Description
Technical field
The invention belongs to dielectric composite material technical field more particularly to a kind of bismuth sodium titanate-barium titanates/polyimide-based
Dielectric composite material and preparation method thereof.
Background technique
The thin film capacitor of dielectric material preparation is the basis of all electronic components, is deposited compared to fuel cell and other electric energy
Storage device, dielectric capacitor can discharge the energy of storage in a very short period of time to generate strong electric pulse.This energy
Power is used in dielectric capacitor in the electronic equipment for needing pulse power, such as medical defibrillator, and what is laterally excited is big
Gas laser and advanced electromagnetic system, wherein capacitor is by low-power, and input is converted to high power for a long time, exports in short-term.
However, the Polymeric dielectric constant due to preparation media capacitor is relatively low, the energy density of polymeric media capacitor by
To inhibition, this is the major obstacle of high power electronic device miniaturization.
Summary of the invention
Polymeric dielectric constant to solve the problems, such as preparation media capacitor is relatively low, and the present invention provides a kind of titaniums
Sour bismuth sodium titanate-barium/polyimide-based dielectric composite material and preparation method thereof.
Technical solution of the present invention:
A kind of bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material, including polyimide matrix and evenly dispersed
In the intracorporal bismuth sodium titanate-barium titanate particle of base, the doping of the bismuth sodium titanate-barium titanate particle is dielectric composite material body
1 long-pending~15vol.%.
Further, the preparation method of the bismuth sodium titanate-barium titanate particle be by certain mol proportion by barium carbonate, oxidation
Bismuth, sodium carbonate, titanium oxide are placed in ball grinder, and dispersing agent is added and carries out wet ball grinding, mixes gained after the completion of first ball milling
Slurry carries out secondary ball milling after the completion of drying, calcine for the first time, calcining, and mixed slurry secondary drying obtained by secondary ball milling is obtained titanium
Sour bismuth sodium titanate-barium particle.
Further, the molar ratio of the barium carbonate, bismuth oxide, sodium carbonate and titanium oxide is 0.06:0.47:0.47:1,
The first ball milling of the wet ball grinding and the ratio of grinding media to material of secondary ball milling are 3~5:1, and ball milling speed is 400~600r/min,
Ball-milling Time is 6~12h；The first drying is 80 DEG C of dry 6~12h, and the secondary drying is 80 DEG C of dry 10h, institute
Stating calcining is 800~900 DEG C of 2~4h of calcining.
A kind of preparation method of bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material, steps are as follows:
Step 1: preparing bismuth sodium titanate-barium titanate particle
Barium carbonate, bismuth oxide, sodium carbonate, titanium oxide are placed in ball grinder by certain mol proportion, dispersing agent is added and carries out
Wet ball grinding, first ball milling carry out secondary ball milling after the completion of drying, calcine for the first time by gained mixed slurry after the completion, calcining, will
Mixed slurry secondary drying obtained by secondary ball milling obtains bismuth sodium titanate-barium titanate particle；
Step 2: preparing precursor solution
Doping according to bismuth sodium titanate-barium titanate particle is 1~15vol.% of dielectric composite material volume, by 4,
Bismuth sodium titanate-barium titanate particle made from 4 '-diaminodiphenyl ethers and step 1 is added to N, N- dimethyl by certain mass ratio
In formamide, mixed solution is stirred to get after ultrasonic disperse, by certain pyromellitic dianhydride and 4, the matter of 4 '-diaminodiphenyl ethers
It is molten to stand certain time formation presoma than pyromellitic dianhydride to be added in the mixed solution by several times for amount after being sufficiently stirred
Liquid；
Step 3: preparing bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material
Precursor solution made from step 2 is made after film and carries out the processing of gradient increased temperature imidizate, is obtained after cooling
Bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material.
Further, the molar ratio of barium carbonate, bismuth oxide described in step 1, sodium carbonate and titanium oxide is 0.06:0.47:
0.47:1, the first ball milling of the wet ball grinding and the ratio of grinding media to material of secondary ball milling are 3~5:1, and ball milling speed is 400~
600r/min, Ball-milling Time are 6~12h；The first drying is 80 DEG C of dry 6~12h, and the secondary drying is 80 DEG C dry
Dry 10h, the calcining are 800~900 DEG C of 2~4h of calcining.
Further, 4,4 '-diaminodiphenyl ethers and pyromellitic dianhydride described in step 2 are dry at 70~80 DEG C
It is used after 12h, the n,N-Dimethylformamide uses preceding processType molecular sieve filtration is to remove wherein moisture.
Further, 4,4 '-diaminodiphenyl ethers, bismuth sodium titanate-barium titanate particle described in step 2 and N, N- dimethyl
The mass ratio of formamide is 1:(0.06~1.03): the power of (14~18), the ultrasonic disperse is 400~600W, when ultrasonic
Between 60~120min, the revolving speed stirred after the ultrasonic disperse is 300~500r/min, and it is 1~2h that the time, which is stirred at room temperature,.
Further, the mass ratio of pyromellitic dianhydride described in step 2 and 4,4 '-diaminodiphenyl ethers is 1:0.9, is added
Described be sufficiently stirred is that 12h is stirred under ice-water bath after entering pyromellitic dianhydride, and speed of agitator is 400~600r/min, described
Time of repose is 10h.
Further, precursor solution described in step 3 be made film be by precursor solution with ultrasonic power 400~
600W is ultrasonically treated 30~60min, vacuumizes under the pressure of 0.08MPa after 30~60min removes bubble, with 0.05~
The blade coating speed of 0.2m/s scratches precursor solution to glass plate, and coating thickness is 20~40 μm, and 60~80 DEG C of vacuum are dry
Dry 1~2h sizing film forming.
Further, the heating of gradient increased temperature described in step 3 imidizate treatment conditions are successively to be warming up to 160 DEG C, 200
DEG C, 240 DEG C, 280 DEG C, 320 DEG C and 350 DEG C, isothermal holding at a temperature of 160 DEG C, 200 DEG C, 240 DEG C, 280 DEG C and 320 DEG C
Time is 0.5h, and isothermal holding time at a temperature of 350 DEG C is 1h.
Beneficial effects of the present invention:
Bismuth sodium titanate-barium titanate provided by the invention/polyimide-based dielectric composite material opposite dielectric with higher
Constant, when the doping of bismuth sodium titanate-barium titanate is 9vol.%, dielectric composite material opposite dielectric when frequency is 1Hz is normal
Number is 4.58, and relatively pure Kapton improves 30%；When the doping of bismuth sodium titanate-barium titanate is 15vol.%,
Relative dielectric constant is 4.92 when frequency is 1Hz, and relatively pure Kapton improves 40%.
It is sub- that the present invention can effectively improve bismuth sodium titanate-barium titanate/polyamides in the case where ceramics adulterate the lower situation of phase content
The relative dielectric constant of amido dielectric composite material, avoiding excessive doping leads to lacking for dielectric composite material breakdown performance decline
It falls into.Dielectric composite material, which is used for dielectric capacitor, can further improve the energy density of dielectric capacitor, can
It is applicable to the electronic equipment of pulse power and further realizes the miniaturization of high power electronic equipment.
Bismuth sodium titanate-barium titanate provided by the invention/polyimide-based dielectric composite material preparation method simple process,
It is low in cost, it is suitble to large-scale production；Bismuth sodium titanate-barium titanate ceramic particle using solid phase method preparation has high dielectric normal
Number, and no pollution to the environment.
Detailed description of the invention
Fig. 1 is the SEM figure of bismuth sodium titanate-barium titanate particle prepared by embodiment 3；
Fig. 2 is the XRD comparison diagram of the dielectric composite material of embodiment 7-12 preparation and the dielectric material of the preparation of comparative example 1；
Fig. 3 is the dielectric composite material of embodiment 7-12 preparation and dielectric material prepared by comparative example 1 in frequency is 1Hz
When, the relative dielectric constant comparison diagram under room temperature；
Fig. 4 is dielectric composite material prepared by embodiment 11,12 and dielectric material prepared by comparative example 1 in frequency is 1Hz
When, comparison diagram that relative dielectric constant varies with temperature；
Fig. 5 is dielectric composite material prepared by embodiment 11,12 and dielectric material prepared by comparative example 1 in frequency is 1Hz
When, relative dielectric constant comparison diagram when temperature is 50 DEG C.
Specific embodiment
Below with reference to embodiment, the following further describes the technical solution of the present invention, and however, it is not limited to this, all right
Technical solution of the present invention is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be contained
Lid is within the protection scope of the present invention.
Embodiment 1
A kind of bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material, including polyimide matrix and evenly dispersed
In the intracorporal bismuth sodium titanate-barium titanate particle of base, the doping of the bismuth sodium titanate-barium titanate particle is dielectric composite material body
1 long-pending~15vol.%.
Embodiment 2
A kind of bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material, including polyimide matrix and evenly dispersed
In the intracorporal bismuth sodium titanate-barium titanate particle of base, the doping of the bismuth sodium titanate-barium titanate particle is dielectric composite material body
1 long-pending~15vol.%.
Wherein, bismuth sodium titanate-barium titanate particle the preparation method comprises the following steps: being in molar ratio 0.06:0.47:0.47:1 by carbonic acid
Barium, bismuth oxide, sodium carbonate and titanium oxide are placed in ball grinder, are that agate ball is added in 3~5:1 by ratio of grinding media to material, are made with dehydrated alcohol
For dispersing agent, the dehydrated alcohol of ball milling tank volume 1/2 is added, ball grinder is put into planetary ball mill and carries out the first of wet ball grinding
Ball milling, ball milling speed are 400~600r/min, and Ball-milling Time is 6~12h, do 80 DEG C of gained mixed slurry after the completion of ball milling
Dry 6~12h, powder is then put into 800~900 DEG C of 2~4h of calcining of Muffle furnace, particle will be put into two in ball grinder obtained by calcining
Secondary ball milling, secondary ball milling condition is identical as first ball milling, and 80 DEG C of mixed slurry dry 10h obtained by secondary ball milling obtain bismuth titanates
Sodium titanate-barium particle.
The present embodiment is simple using the bismuth sodium titanate-barium titanate ceramic particle preparation process of solid phase method preparation, low in cost,
It is suitble to large-scale production, and the bismuth sodium titanate-barium titanate ceramic particle no pollution to the environment prepared, there is high dielectric constant.
Embodiment 3
A kind of bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material, including polyimide matrix and evenly dispersed
In the intracorporal bismuth sodium titanate-barium titanate particle of base, the doping of the bismuth sodium titanate-barium titanate particle is dielectric composite material body
1 long-pending~15vol.%.
Wherein, bismuth sodium titanate-barium titanate particle the preparation method comprises the following steps: being in molar ratio 0.06:0.47:0.47:1 by carbonic acid
Barium, bismuth oxide, sodium carbonate and titanium oxide are placed in ball grinder, by ratio of grinding media to material be 3:1 be added agate ball, using dehydrated alcohol as divide
The dehydrated alcohol of ball milling tank volume 1/2 is added in powder, and ball grinder is put into the first ball that planetary ball mill carries out wet ball grinding
Mill, ball milling speed 550r/min, Ball-milling Time 12h, ball milling are incited somebody to action by 80 DEG C of gained mixed slurry dry 6h, then after the completion
Powder is put into 900 DEG C of calcining 2h of Muffle furnace, and calcining gained particle is put into secondary ball milling in ball grinder, secondary ball milling condition and just
Secondary ball milling is identical, and 80 DEG C of mixed slurry dry 10h obtained by secondary ball milling obtain bismuth sodium titanate-barium titanate particle.
Fig. 1 is the SEM figure of bismuth sodium titanate-barium titanate particle prepared by embodiment 3；As seen from Figure 1, the metatitanic acid of preparation
Bismuth sodium titanate-barium nanoparticle size is uniform, and partial size is 400~600nm.
Embodiment 4
A kind of preparation method of bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material, steps are as follows:
Step 1: preparing bismuth sodium titanate-barium titanate particle
Barium carbonate, bismuth oxide, sodium carbonate, titanium oxide are placed in ball grinder by certain mol proportion, dispersing agent is added and carries out
Wet ball grinding, first ball milling carry out secondary ball milling after the completion of drying, calcine for the first time by gained mixed slurry after the completion, calcining, will
Mixed slurry secondary drying obtained by secondary ball milling obtains bismuth sodium titanate-barium titanate particle；
Step 2: preparing precursor solution
Doping according to bismuth sodium titanate-barium titanate particle is 1~15vol.% of dielectric composite material volume, by 4,
Bismuth sodium titanate-barium titanate particle made from 4 '-diaminodiphenyl ethers and step 1 is added to N, N- dimethyl by certain mass ratio
In formamide, mixed solution is stirred to get after ultrasonic disperse, by certain pyromellitic dianhydride and 4, the matter of 4 '-diaminodiphenyl ethers
It is molten to stand certain time formation presoma than pyromellitic dianhydride to be added in the mixed solution by several times for amount after being sufficiently stirred
Liquid；
Step 3: preparing bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material
Precursor solution made from step 2 is made after film and carries out gradient increased temperature heating imidizate processing, after cooling
Obtain bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material.
Embodiment 5
A kind of doping of bismuth sodium titanate-barium titanate particle is the metatitanic acid of 1~15vol.% of dielectric composite material volume
Bismuth sodium titanate-barium/polyimide-based dielectric composite material preparation method, steps are as follows:
Step 1: preparing bismuth sodium titanate-barium titanate particle
Bismuth sodium titanate-barium titanate particle the preparation method comprises the following steps: being in molar ratio 0.06:0.47:0.47:1 by barium carbonate, oxygen
Change bismuth, sodium carbonate and titanium oxide to be placed in ball grinder, is that agate ball is added in 3~5:1 by ratio of grinding media to material, using dehydrated alcohol as dispersion
The dehydrated alcohol of ball milling tank volume 1/2 is added in agent, and ball grinder is put into the first ball milling that planetary ball mill carries out wet ball grinding,
Ball milling speed is 400~600r/min, and Ball-milling Time is 6~12h, after the completion of ball milling by the 80 DEG C of dryings 6 of gained mixed slurry~
12h, powder is then put into 800~900 DEG C of 2~4h of calcining of Muffle furnace, secondary ball in ball grinder will be put by particle obtained by calcining
Mill, secondary ball milling condition is identical as first ball milling, and 80 DEG C of mixed slurry dry 10h obtained by secondary ball milling obtain bismuth-sodium titanate-titanium
Sour titanate particle.
Step 2: preparing precursor solution
4,4 '-diaminodiphenyl ethers and pyromellitic dianhydride use after dry 12h at 70~80 DEG C, N, N- dimethyl
Formamide uses preceding processType molecular sieve filtration is to remove wherein moisture.
Mass ratio according to 4,4 '-diaminodiphenyl ethers, bismuth sodium titanate-barium titanate particle and N,N-dimethylformamide is
1:(0.06~1.03): (14~18) add bismuth sodium titanate-barium titanate particle made from 4,4 '-diaminodiphenyl ethers and step 1
Enter into n,N-Dimethylformamide, is after 400~600W carries out 60~120min of ultrasonic disperse with ultrasonic power, with 300~
The speed of agitator of 500r/min is stirred at room temperature 1~2h and obtains mixed solution, by pyromellitic dianhydride and 4,4 '-diaminodiphenyl ethers
Mass ratio be that pyromellitic dianhydride points 6~10 times are added in the mixed solution 1:0.9, under ice-water bath, turned with stirring
After 400~600r/min of speed stirs 12h, stands 10h and form precursor solution；
Step 3: preparing bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material
By precursor solution made from step 2 with ultrasonic power be 400~600W be ultrasonically treated 30~60min,
It is vacuumized under the pressure of 0.08MPa after 30~60min removes bubble, with the blade coating speed of 0.05~0.2m/s by precursor solution
On blade coating to glass plate, coating thickness is 20~40 μm, and film is put into constant temperature after molding by 60~80 DEG C of 1~2h of vacuum drying
In baking oven carry out gradient increased temperature heating imidizate processing, be successively warming up to 160 DEG C, 200 DEG C, 240 DEG C, 280 DEG C, 320 DEG C and
350 DEG C, soaking time at a temperature of 160 DEG C, 200 DEG C, 240 DEG C, 280 DEG C and 320 DEG C is 0.5h, at a temperature of 350 DEG C
The isothermal holding time be 1h, then cool to room temperature with the furnace, it is compound to obtain bismuth sodium titanate-barium titanate/polyimide-based dielectric
Material, wherein the doping of bismuth sodium titanate-barium titanate particle is 1~15vol.% of dielectric composite material volume.
Embodiment 6
A kind of doping of bismuth sodium titanate-barium titanate particle is the metatitanic acid of 1~15vol.% of dielectric composite material volume
Bismuth sodium titanate-barium/polyimide-based dielectric composite material preparation method, steps are as follows:
Step 1: preparing bismuth sodium titanate-barium titanate particle
Bismuth sodium titanate-barium titanate particle the preparation method comprises the following steps: being in molar ratio 0.06:0.47:0.47:1 by barium carbonate, oxygen
Change bismuth, sodium carbonate and titanium oxide to be placed in ball grinder, is that agate ball is added in 4:1 by ratio of grinding media to material, using dehydrated alcohol as dispersing agent,
The dehydrated alcohol of ball milling tank volume 1/2 is added, ball grinder is put into the first ball milling that planetary ball mill carries out wet ball grinding, ball milling
Speed is 500r/min, Ball-milling Time 10h, is put after the completion of ball milling by 80 DEG C of gained mixed slurry dry 10h and then by powder
Enter 800 DEG C of calcining 3h of Muffle furnace, calcining gained particle is put into secondary ball milling in ball grinder, secondary ball milling condition and first ball milling
Identical, 80 DEG C of mixed slurry dry 10h obtained by secondary ball milling obtain bismuth sodium titanate-barium titanate particle.
Step 2: preparing precursor solution
4,4 '-diaminodiphenyl ethers and pyromellitic dianhydride use after dry 12h at 80 DEG C, N, N- dimethyl formyl
Amine uses preceding processType molecular sieve filtration is to remove wherein moisture.
Mass ratio according to 4,4 '-diaminodiphenyl ethers, bismuth sodium titanate-barium titanate particle and N,N-dimethylformamide is
1:(0.06~1.03): bismuth sodium titanate-barium titanate particle made from 4,4 '-diaminodiphenyl ethers and step 1 is added to N by 16,
It is after 500W carries out ultrasonic disperse 90min, with the speed of agitator room temperature of 400r/min with ultrasonic power in dinethylformamide
Stirring 2h obtains mixed solution, and by pyromellitic dianhydride and 4, the mass ratioes of 4 '-diaminodiphenyl ethers is 1:0.9 by equal benzene tetramethyl
Acid anhydrides, which divides 6~10 times, to be added in the mixed solution, under ice-water bath, after stirring 12h with speed of agitator 500r/min, is stood
10h forms precursor solution；
Step 3: preparing bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material
Precursor solution made from step 2 is ultrasonically treated 45min with ultrasonic power for 500W, in the pressure of 0.08MPa
Under vacuumize 45min remove bubble after, precursor solution is scratched to glass plate with the blade coating speed of 0.15m/s, apply film thickness
Degree is 30 μm, 70 DEG C of vacuum drying 2h, and film is put into constant temperature oven after molding and is carried out at gradient increased temperature heating imidizate
Reason, be successively warming up to 160 DEG C, 200 DEG C, 240 DEG C, 280 DEG C, 320 DEG C and 350 DEG C, at 160 DEG C, 200 DEG C, 240 DEG C, 280 DEG C and
Soaking time at a temperature of 320 DEG C is 0.5h, and isothermal holding time at a temperature of 350 DEG C is 1h, is then cooled to the furnace
Room temperature obtains bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material, wherein the doping of bismuth sodium titanate-barium titanate particle
Amount is 1~15vol.% of dielectric composite material volume.
Embodiment 7
A kind of doping of bismuth sodium titanate-barium titanate particle is the bismuth-sodium titanate-of the 1vol.% of dielectric composite material volume
Barium titanate/polyimide-based dielectric composite material preparation method, steps are as follows:
Step 1: preparing bismuth sodium titanate-barium titanate particle
Bismuth sodium titanate-barium titanate particle the preparation method comprises the following steps: being in molar ratio 0.06:0.47:0.47:1 by barium carbonate, oxygen
Change bismuth, sodium carbonate and titanium oxide to be placed in ball grinder, is that agate ball is added in 3:1 by ratio of grinding media to material, using dehydrated alcohol as dispersing agent,
The dehydrated alcohol of ball milling tank volume 1/2 is added, ball grinder is put into the first ball milling that planetary ball mill carries out wet ball grinding, ball milling
Speed is 550r/min, Ball-milling Time 12h, is put after the completion of ball milling by 80 DEG C of gained mixed slurry dry 6h and then by powder
Enter 900 DEG C of calcining 2h of Muffle furnace, calcining gained particle is put into secondary ball milling in ball grinder, secondary ball milling condition and first ball milling
Identical, 80 DEG C of mixed slurry dry 10h obtained by secondary ball milling obtain bismuth sodium titanate-barium titanate particle.
Step 2: preparing precursor solution
4,4 '-diaminodiphenyl ethers and pyromellitic dianhydride use after dry 12h at 70 DEG C, N, N- dimethyl formyl
Amine uses preceding processType molecular sieve filtration is to remove wherein moisture.
Mass ratio according to 4,4 '-diaminodiphenyl ethers, bismuth sodium titanate-barium titanate particle and N,N-dimethylformamide is
Bismuth sodium titanate-barium titanate particle made from 4,4 '-diaminodiphenyl ethers and step 1 is added to N, N- dimethyl by 1:0.06:15
It is after 600W carries out ultrasonic disperse 60min, 2h to be stirred at room temperature with the speed of agitator of 500r/min and is obtained with ultrasonic power in formamide
To mixed solution, by pyromellitic dianhydride and 4, pyromellitic dianhydride is divided 6 for 1:0.9 by the mass ratio of 4 '-diaminodiphenyl ethers
It is added in the mixed solution for~10 times, under ice-water bath, after stirring 12h with speed of agitator 600r/min, stands before 10h formed
Drive liquid solution；
Step 3: preparing bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material
Precursor solution made from step 2 is ultrasonically treated 30min with ultrasonic power for 600W, in the pressure of 0.08MPa
Under vacuumize 30min remove bubble after, precursor solution is scratched to glass plate with the blade coating speed of 0.1m/s, coating thickness
It is 40 μm, film is put into constant temperature oven after molding and carries out gradient increased temperature heating imidizate processing by 80 DEG C of vacuum drying 2h,
160 DEG C, 200 DEG C, 240 DEG C, 280 DEG C, 320 DEG C and 350 DEG C are successively warming up to, at 160 DEG C, 200 DEG C, 240 DEG C, 280 DEG C and 320
Soaking time at a temperature of DEG C is 0.5h, and isothermal holding time at a temperature of 350 DEG C is 1h, then cools to room with the furnace
Temperature, obtain bismuth sodium titanate-barium titanate particle doping be dielectric composite material volume 1vol.% bismuth sodium titanate-barium titanate/
Polyimide-based dielectric composite material.
Embodiment 8
The present embodiment and the difference of embodiment 7 be only that, 4,4 '-diamino when the present embodiment step 2 prepares precursor solution
The mass ratio of yl diphenyl ether, bismuth sodium titanate-barium titanate particle and N,N-dimethylformamide is 1:0.18:15；Bismuth titanates is made
The doping of sodium titanate-barium particle is bismuth sodium titanate-barium titanate/polyimide-based Jie of dielectric composite material volume 3vol.%
Composite.
Embodiment 9
The present embodiment and the difference of embodiment 7 be only that, 4,4 '-diamino when the present embodiment step 2 prepares precursor solution
The mass ratio of yl diphenyl ether, bismuth sodium titanate-barium titanate particle and N,N-dimethylformamide is 1:0.31:15；Bismuth titanates is made
The doping of sodium titanate-barium particle is bismuth sodium titanate-barium titanate/polyimide-based Jie of dielectric composite material volume 5vol.%
Composite.
Embodiment 10
The present embodiment and the difference of embodiment 7 be only that, 4,4 '-diamino when the present embodiment step 2 prepares precursor solution
The mass ratio of yl diphenyl ether, bismuth sodium titanate-barium titanate particle and N,N-dimethylformamide is 1:0.44:15；Bismuth titanates is made
The doping of sodium titanate-barium particle is bismuth sodium titanate-barium titanate/polyimide-based Jie of dielectric composite material volume 7vol.%
Composite.
Embodiment 11
The present embodiment and the difference of embodiment 7 be only that, 4,4 '-diamino when the present embodiment step 2 prepares precursor solution
The mass ratio of yl diphenyl ether, bismuth sodium titanate-barium titanate particle and N,N-dimethylformamide is 1:0.58:15；Bismuth titanates is made
The doping of sodium titanate-barium particle is bismuth sodium titanate-barium titanate/polyimide-based Jie of dielectric composite material volume 9vol.%
Composite.
Embodiment 12
The present embodiment and the difference of embodiment 7 be only that, 4,4 '-diamino when the present embodiment step 2 prepares precursor solution
The mass ratio of yl diphenyl ether, bismuth sodium titanate-barium titanate particle and N,N-dimethylformamide is 1:1.03:15；Bismuth titanates is made
The doping of sodium titanate-barium particle is bismuth sodium titanate-barium titanate/polyimide-based Jie of dielectric composite material volume 15vol.%
Composite.
Comparative example 1
This comparative example provides a kind of pure polymide dielectric material, and preparation method is as follows:
4,4 '-diaminodiphenyl ethers and pyromellitic dianhydride use after dry 12h at 70~80 DEG C, N, N- dimethyl
Formamide uses preceding processType molecular sieve filtration is to remove wherein moisture.
It is 1:15 by 4,4 '-diamino two according to the mass ratio of 4,4 '-diaminodiphenyl ethers and N,N-dimethylformamide
Phenylate is added in n,N-Dimethylformamide, is after 600W carries out ultrasonic disperse 60min, with 500r/min's with ultrasonic power
Speed of agitator is stirred at room temperature 2h and obtains mixed solution, and by pyromellitic dianhydride and 4, the mass ratio of 4 '-diaminodiphenyl ethers is 1:
0.9 pyromellitic dianhydride points 6~10 times are added in the mixed solution, under ice-water bath, are stirred with speed of agitator 600r/min
After mixing 12h, stands 10h and form precursor solution；
Precursor solution obtained is ultrasonically treated 30min with ultrasonic power for 600W, is taken out very under the pressure of 0.08MPa
After empty 30min removes bubble, precursor solution is scratched to glass plate with the blade coating speed of 0.1m/s, coating thickness is 40 μ
Film is put into constant temperature oven after molding and carries out gradient increased temperature heating imidizate processing, successively by m, 80 DEG C of vacuum drying 2h
160 DEG C, 200 DEG C, 240 DEG C, 280 DEG C, 320 DEG C and 350 DEG C are warming up to, in 160 DEG C, 200 DEG C, 240 DEG C, 280 DEG C and 320 DEG C temperature
Soaking time under degree is 0.5h, and isothermal holding time at a temperature of 350 DEG C is 1h, then cools to room temperature with the furnace, obtains
To pure polymide dielectric material.
Fig. 2 is the XRD comparison diagram of the dielectric composite material of embodiment 7-12 preparation and the dielectric material of the preparation of comparative example 1；
NBBT is bismuth sodium titanate-barium titanate in figure, and PI is pure polyimides；Bismuth-sodium titanate-titanium of different dopings as seen from Figure 2
Sour barium/polyimide-based dielectric composite material does not have miscellaneous peak in XRD spectrum, illustrate preparation bismuth sodium titanate-barium titanate/it is poly-
There is no the introducings of other impurity in imide dielectric composite material.
Fig. 3 is the dielectric composite material of embodiment 7-12 preparation and dielectric material prepared by comparative example 1 in frequency is 1Hz,
Relative dielectric constant comparison diagram under room temperature；As seen from Figure 3, bismuth sodium titanate-barium titanate/polyimide-based dielectric composite wood
The relative dielectric constant of material is promoted with the content of bismuth sodium titanate-barium titanate and is increased, and adulterates bismuth-sodium titanate-metatitanic acid of 9vol.%
Barium/polyimide-based dielectric composite material relative dielectric constant is 4.58, and relatively pure Kapton improves 30%；Doping
The bismuth sodium titanate-barium titanate of 15vol.%/polyimide-based dielectric composite material relative dielectric constant is 4.92, relatively pure poly-
Imide membrane improves 40%.
Fig. 4 is dielectric composite material prepared by embodiment 11,12 and dielectric material prepared by comparative example 1 in frequency is 1Hz
When, comparison diagram that relative dielectric constant varies with temperature；As seen from Figure 4, bismuth sodium titanate-barium titanate/polyimide-based Jie
The relative dielectric constant of composite rises with temperature to be occurred first increasing the trend reduced afterwards, peak value occurs at 50 DEG C.
Fig. 5 is dielectric composite material prepared by embodiment 11,12 and dielectric material prepared by comparative example 1 in frequency is 1Hz
When, relative dielectric constant comparison diagram when temperature is 50 DEG C；As seen from Figure 5, bismuth sodium titanate-barium titanate/polyimide-based
The relative dielectric constant of dielectric composite material is promoted with the content of bismuth sodium titanate-barium titanate and is increased, and adulterates the metatitanic acid of 9vol.%
Relative dielectric constant of the bismuth sodium titanate-barium/polyimide-based dielectric composite material at 50 DEG C is 4.62, adulterates 15vol.%'s
Relative dielectric constant of the bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material at 50 DEG C is 5.02.
Claims (10)
1. a kind of bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material, which is characterized in that including polyimide matrix
Be dispersed in the intracorporal bismuth sodium titanate-barium titanate particle of base, the doping of the bismuth sodium titanate-barium titanate particle is dielectric
1~15vol.% of composite material volume.
2. a kind of bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material according to claim 1, which is characterized in that
The preparation method of the bismuth sodium titanate-barium titanate particle is by certain mol proportion by barium carbonate, bismuth oxide, sodium carbonate, titanium oxide
It is placed in ball grinder, dispersing agent is added and carries out wet ball grinding, gained mixed slurry is dried for the first time, is forged after the completion of first ball milling
It burns, carry out secondary ball milling after the completion of calcining, mixed slurry secondary drying obtained by secondary ball milling is obtained into bismuth sodium titanate-barium titanate
Grain.
3. a kind of bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material according to claim 2, which is characterized in that
The barium carbonate, bismuth oxide, sodium carbonate and titanium oxide molar ratio be 0.06:0.47:0.47:1, the wet ball grinding it is first
The ratio of grinding media to material of ball milling and secondary ball milling is 3~5:1, and ball milling speed is 400~600r/min, and Ball-milling Time is 6~
12h；The first drying is 80 DEG C of dry 6~12h, and the secondary drying is 80 DEG C of dry 10h, and the calcining is 800~900
DEG C calcining 2~4h.
4. a kind of bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material preparation method, which is characterized in that step is such as
Under:
Step 1: preparing bismuth sodium titanate-barium titanate particle:
Barium carbonate, bismuth oxide, sodium carbonate, titanium oxide are placed in ball grinder by certain mol proportion, dispersing agent is added and carries out wet process
Ball milling, first ball milling carry out secondary ball milling after the completion of drying, calcine for the first time by gained mixed slurry after the completion, calcining, will be secondary
Mixed slurry secondary drying obtained by ball milling obtains bismuth sodium titanate-barium titanate particle；
Step 2: preparing precursor solution:
Doping according to bismuth sodium titanate-barium titanate particle is 1~15vol.% of dielectric composite material volume, by 4,4 '-two
Bismuth sodium titanate-barium titanate particle made from amino-diphenylethers and step 1 is added to N,N-dimethylformamide by certain mass ratio
In, mixed solution is stirred to get after ultrasonic disperse, by certain pyromellitic dianhydride and 4, the mass ratio of 4 '-diaminodiphenyl ethers will
Pyromellitic dianhydride is added in the mixed solution by several times, and certain time is stood after being sufficiently stirred and forms precursor solution；
Step 3: preparing bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material:
Precursor solution made from step 2 is made after film and carries out the processing of gradient increased temperature imidizate, obtains metatitanic acid after cooling
Bismuth sodium titanate-barium/polyimide-based dielectric composite material.
5. a kind of bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material preparation method according to claim 4,
It is characterized in that, the molar ratio of barium carbonate, bismuth oxide described in step 1, sodium carbonate and titanium oxide is 0.06:0.47:0.47:1,
The first ball milling of the wet ball grinding and the ratio of grinding media to material of secondary ball milling are 3~5:1, and ball milling speed is 400~600r/min,
Ball-milling Time is 6~12h；The first drying is 80 DEG C of dry 6~12h, and the secondary drying is 80 DEG C of dry 10h, institute
Stating calcining is 800~900 DEG C of 2~4h of calcining.
6. a kind of bismuth sodium titanate-barium titanate according to claim 4 or 5/polyimide-based dielectric composite material preparation side
Method, which is characterized in that the dry 12h at 70~80 DEG C of 4,4 '-diaminodiphenyl ethers and pyromellitic dianhydride described in step 2
After use, the n,N-Dimethylformamide use preceding processType molecular sieve filtration is to remove wherein moisture.
7. a kind of bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material preparation method according to claim 6,
It is characterized in that, 4,4 '-diaminodiphenyl ethers, bismuth sodium titanate-barium titanate particle and n,N-Dimethylformamide described in step 2
Mass ratio be 1:(0.06~1.03): (14~18), the power of the ultrasonic disperse are 400~600W, ultrasonic time 60~
120min, the revolving speed stirred after the ultrasonic disperse are 300~500r/min, and it is 1~2h that the time, which is stirred at room temperature,.
8. a kind of bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material preparation method according to claim 7,
It is characterized in that, pyromellitic dianhydride described in step 2 and 4, the mass ratio of 4 '-diaminodiphenyl ethers is 1:0.9, and equal benzene is added
Described be sufficiently stirred is that 12h is stirred under ice-water bath after tetracarboxylic acid anhydride, and speed of agitator is 400~600r/min, when the standing
Between be 10h.
9. a kind of bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material preparation method according to claim 8,
It is characterized in that, it is by precursor solution with ultrasonic power 400~600W ultrasound that film, which is made, in precursor solution described in step 3
After handling 30~60min, vacuumizing 30~60min removing bubble under the pressure of 0.08MPa, with the blade coating of 0.05~0.2m/s
Speed scratches precursor solution to glass plate, and coating thickness is 20~40 μm, and 60~80 DEG C of 1~2h of vacuum drying are shaped into
Film.
10. a kind of bismuth sodium titanate-barium titanate/polyimide-based dielectric composite material preparation method according to claim 9,
It is characterized in that, gradient increased temperature imidizate treatment conditions described in step 3 be successively be warming up to 160 DEG C, 200 DEG C, 240 DEG C,
280 DEG C, 320 DEG C and 350 DEG C, isothermal holding time at a temperature of 160 DEG C, 200 DEG C, 240 DEG C, 280 DEG C and 320 DEG C is
0.5h, isothermal holding time at a temperature of 350 DEG C are 1h.
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