CN106380844B - A kind of preparation method of the high dielectric polyimide laminated film of the high heat conduction of boron nitride and aluminium nitride codope - Google Patents
A kind of preparation method of the high dielectric polyimide laminated film of the high heat conduction of boron nitride and aluminium nitride codope Download PDFInfo
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Abstract
A kind of preparation method of the high dielectric polyimide laminated film of the high heat conduction of boron nitride and aluminium nitride codope, it is related to a kind of preparation method of laminated film.The invention aims to solve the thermal conductivity, insulating properties and mechanical property inequality of existing polyimide composite film, using the problem of being restricted in electric insulation field.Preparation method：First, ultrathin boron nitride powder is prepared；2nd, the thick polyamic acid solution containing superthin layer boron nitride and aluminium nitride is prepared；3rd, laminated film is prepared, obtains the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope.The thermal conductivity factor of the high dielectric polyimide laminated film of boron nitride and the high heat conduction of aluminium nitride codope prepared by the present invention improves 68%~330%, and insulation resistance improves 0.8 times~4.1 times, and tensile strength improves 1%~31%.The present invention is suitable for preparing the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope.
Description
Technical field
The present invention relates to a kind of preparation method of laminated film.
Background technology
High-performance polyimide film is wind-driven generator, high-speed pulling motor, steel mill electric machine, motor in electric automobile, army
The indispensable crucial supplementary material of the high performance variable-frequency motor such as product, is a kind of high performance electrical insulating material, is mainly used for
The turn-to-turn insulation of variable-frequency motor winding and insulation against ground, need of the exploitation originating from converter technique and frequency control motor of the product
Ask.Du pont company in 1994, ABB AB of Switzerland and Siemens cooperation take the lead in have developed corona-resistant polyimide
Film (Kapton FCR), make the material Inverter fed motor life-span reached common Kapton hundreds of so that thousands of times.
In addition corona-resistant polyimide film also has preferable heat conductivility, and the thermal conductivity factor of Kapton 100CR films is
The thermal conductivity factor of 0.385W/ (m.K), plain edition Kapton 100HN only have 0.19W/ (m.K), Kapton FCR substantially to reduce
The temperature rise of electrical equipment and electrical in the process of running and the hot-spot caused by corona, extend the service life of material.With
Corona-resistant polyimide film is opened as wire insulation and insulation against ground for traction electric machine and high-voltage motor miniaturization
New road.Other domestic and international research units put into a large amount of man power and materials and carry out related fields researchs, including polymer matrix without
Machine nanocomposite preparation method, performance test and application, and obtain many achievements to attract people's attention.It is but domestic at present
Composite polyimide material, in the comprehensive performances such as Inverter fed motor life-span, mechanical performance and thermal property also and same kind of products at abroad
There are gap.
At present on the premise of the high electrical insulation properties of holding and mechanical performance, the heat conductivility for improving material is still to learn
The research topic that art circle is faced with industrial quarters.
The content of the invention
Thermal conductivity, insulating properties and mechanical property the invention aims to solve existing polyimide composite film is equal
Difference, using the problem of being restricted in electric insulation field, and provides a kind of high heat conduction of boron nitride and aluminium nitride codope
The preparation method of high dielectric polyimide laminated film.
A kind of preparation method of the high dielectric polyimide laminated film of the high heat conduction of boron nitride and aluminium nitride codope be by
What following steps were completed：
First, ultrathin boron nitride powder is prepared：
1., boron nitride powder and oxide be added in concentrated acid, then ice-water bath and mixing speed for 100r/min~
Stirring reaction 60min~120min, obtains mixture A under 300r/min；Mixture A is heated to 50 DEG C, then in temperature is 50
DEG C and mixing speed be stirring reaction 60min~180min under 100r/min~300r/min, be cooled to room temperature, then to mixing
Mass fraction is instilled as 30% hydrogen peroxide solution using the rate of addition of 1mL/min in thing A, obtains mixture B；In ice-water bath
Under, deionized water is added into mixture B, obtains mixture C；Again by mixture C in centrifugal speed 6000r/min~8000r/
5min~15min is centrifuged under min, centrifugate is removed, obtains the presoma of thin layer boron nitride；First by 0.5mol/L's
The presoma 3 times of hydrochloric acid cleaning thin layer boron nitride, reuses the presoma 5 times~8 times of deionized water cleaning thin layer boron nitride, obtains
The presoma of thin layer boron nitride after to cleaning；
Step 1 1. described in concentrated acid be the concentrated sulfuric acid or mixed acid that mass fraction is 98%；The mixed acid is matter
Measure fraction be 98% the concentrated sulfuric acid, mass fraction be 85% phosphoric acid and mass fraction be 98% nitric acid mixed liquor；It is described
Mixed acid in mass fraction be 98% the concentrated sulfuric acid, mass fraction be 85% phosphoric acid and mass fraction be 98% nitric acid
Volume ratio is 1:1:5；
Step 1 1. described in the quality of boron nitride powder and the volume ratio of concentrated acid be (4g~8g):400mL；
Step 1 1. described in the quality of oxide and the volume ratio of concentrated acid be (20g~40g):400mL；
Step 1 1. described in concentrated acid and mass fraction be 30% the volume ratio of hydrogen peroxide solution be 400:(5~
10)；
Step 1 1. described in concentrated acid and deionized water volume ratio be 400:(300~400)；
2., by the presoma of the thin layer boron nitride after cleaning temperature be 80 DEG C~100 DEG C at be dried in vacuo 12h~24h,
Obtain the presoma of dried thin layer boron nitride；The presoma of dried thin layer boron nitride is added in organic solvent,
Ultrasound 12h~24h in the case where ultrasonic power is 100W~500W again, obtains the precursor solution of thin layer boron nitride；In centrifugal speed
To centrifuge 5min~10min to the precursor solution of thin layer boron nitride under 3000r/min, then upper strata centrifugate is taken, obtained
Superthin layer nitrogenizes B solution；Superthin layer nitridation B solution is filtered by vacuum, then by the solid matter obtained after suction filtration in temperature
Spend to be dried in vacuo 12h~24h at 80 DEG C~100 DEG C, obtain superthin layer boron nitride powder；
Step 1 2. described in dried thin layer boron nitride the quality of presoma and the volume ratio of organic solvent be
(1g~3g):100mL；
2nd, the thick polyamic acid solution containing superthin layer boron nitride and aluminium nitride is prepared：
1., by step 1 2. in obtained superthin layer boron nitride powder be dissolved into organic solvent, then low whipping speed is
Under 100r/min~300r/min stir 10min~30min, then ultrasonic power be 100W~300W under ultrasound 10min~
30min, adds aluminium nitride powder, then ultrasound 20min~40min in the case where ultrasonic power is 100W~300W, obtains containing super
The solution of thin layer boron nitride and aluminium nitride；
Step 2 1. in the solution containing superthin layer boron nitride and aluminium nitride superthin layer boron nitride mass fraction
For 0.5%~7.5%, the mass fraction of aluminium nitride is 0.5%~7.5%；
2., diamines is added in the solution containing superthin layer boron nitride and aluminium nitride, then in the case where ultrasonic power is 300W
2h~4h is ultrasonically treated, then divides 4 times~5 times addition dianhydrides in ice-water bath and mixing speed for the condition of 100r/min, then is being stirred
Speed is mixed to stir 12h~24h under 100r/min~300r/min, then is placed in standing 2h~6h in the vacuum drying chamber of room temperature,
Obtain the thick polyamic acid solution containing superthin layer boron nitride and aluminium nitride；
3rd, laminated film is prepared：
1., by step 2 prepare it is thick contain the polyamic acid solution of superthin layer boron nitride and aluminium nitride curtain coating, rotation
Apply or plastic film mulch be on clean glass plate, then by glass plate at 80 DEG C dry 12h~24h, obtain the glass plate of plastic film mulch；
2., by the glass plate of plastic film mulch with the heating rate of 3 DEG C/min~5 DEG C/min from room temperature to 350 DEG C, then
1h~2h, then cooled to room temperature are kept the temperature at 350 DEG C, finally demoulds, obtains the high heat conduction of boron nitride and aluminium nitride codope
High dielectric polyimide laminated film.
Invention advantage：
First, the present invention is improving composite material electric insulation and mechanicalness using two kinds of nitride nano particles of high heat conduction
The thermal conductivity factor of composite material at the same time, can be improved, realizes the nano particle of chondritic and the nano silicon nitride of layer structure
The cooperative effect of boron piece, improves the comprehensive performance of composite polyimide material；
2nd, the present invention is doped with substantial amounts of nano particle, and composites can obtain good synthesis macro property,
Solves the technical barrier of the thermal conductivity of existing polyimide composite film, insulating properties and mechanical property inequality；
3rd, the high dielectric polyimide laminated film of high heat conduction of the boron nitride for preparing of the present invention and aluminium nitride codope is led
Hot coefficient improves 68%~330%；
4th, the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by the present invention is exhausted
Edge resistance improves 0.8 times~4.1 times；
5th, the drawing of the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by the present invention
Stretch intensity and improve 1%~31%.
The present invention is suitable for preparing the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope.
Brief description of the drawings
Fig. 1 is the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one
SEM figure；
Fig. 2 is the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one
B element mapping；
Fig. 3 is the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one
Al Element area profiles；
Fig. 4 is the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one
N element mapping；
Fig. 5 is the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one
C element mapping；
Fig. 6 is the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one
Thermal property figure, A is the thermal conductivity factor of Kapton prepared by comparative example in Fig. 6, and B is prepared by embodiment one
The thermal conductivity factor of the high dielectric polyimide laminated film of the high heat conduction of boron nitride and aluminium nitride codope, C are prepared for embodiment two
Boron nitride and aluminium nitride codope the high dielectric polyimide laminated film of high heat conduction thermal conductivity factor, D made for embodiment three
The thermal conductivity factor of standby boron nitride and the high dielectric polyimide laminated film of the high heat conduction of aluminium nitride codope, E is example IV
The thermal conductivity factor of the boron nitride of preparation and the high dielectric polyimide laminated film of the high heat conduction of aluminium nitride codope, F is embodiment
The thermal conductivity factor of the high dielectric polyimide laminated film of high heat conduction of five boron nitride and aluminium nitride codope prepared；
Fig. 7 is the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one
Mechanical property figure；A is the tensile strength of Kapton prepared by comparative example in Fig. 7, and B is prepared by embodiment one
The tensile strength of the high dielectric polyimide laminated film of the high heat conduction of boron nitride and aluminium nitride codope, C are prepared for embodiment two
Boron nitride and aluminium nitride codope the high dielectric polyimide laminated film of high heat conduction tensile strength, D made for embodiment three
The tensile strength of standby boron nitride and the high dielectric polyimide laminated film of the high heat conduction of aluminium nitride codope, E is example IV
The tensile strength of the boron nitride of preparation and the high dielectric polyimide laminated film of the high heat conduction of aluminium nitride codope, F is embodiment
The tensile strength of the high dielectric polyimide laminated film of high heat conduction of five boron nitride and aluminium nitride codope prepared；
Fig. 8 is the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one
Resistivity properties block diagram；A is that the high insulation of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one is poly- in Fig. 8
The volume resistance of acid imide laminated film, B are the high insulation of high heat conduction of boron nitride prepared by embodiment two and aluminium nitride codope
The volume resistance of polyimide composite film, the boron nitride and the high heat conduction of aluminium nitride codope that C is prepared for embodiment three are high absolutely
The volume resistance of edge polyimide composite film, D are the high heat conduction height of boron nitride prepared by example IV and aluminium nitride codope
The volume resistance of dielectric polyimide laminated film, E are the high heat conduction of boron nitride prepared by embodiment five and aluminium nitride codope
The volume resistance of high dielectric polyimide laminated film；
Fig. 9 is the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one
Inverter fed motor life-span block diagram, A is that the high insulation of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one is poly- in Fig. 9
The Inverter fed motor time of acid imide laminated film, the boron nitride and the high heat conduction of aluminium nitride codope that B is prepared for embodiment two are high absolutely
The Inverter fed motor time of edge polyimide composite film, C are the high heat conduction of boron nitride prepared by embodiment three and aluminium nitride codope
The Inverter fed motor time of high dielectric polyimide laminated film, D are the height of boron nitride prepared by example IV and aluminium nitride codope
The Inverter fed motor time of the high dielectric polyimide laminated film of heat conduction, E are boron nitride and aluminium nitride codope prepared by embodiment five
The high dielectric polyimide laminated film of high heat conduction the Inverter fed motor time.
Embodiment
Embodiment one：Present embodiment is a kind of high insulation polyamides of high heat conduction of boron nitride and aluminium nitride codope
The preparation method of imines laminated film, it is characterised in that this method is completed according to the following steps：
First, ultrathin boron nitride powder is prepared：
1., boron nitride powder and oxide be added in concentrated acid, then ice-water bath and mixing speed for 100r/min~
Stirring reaction 60min~120min, obtains mixture A under 300r/min；Mixture A is heated to 50 DEG C, then in temperature is 50
DEG C and mixing speed be stirring reaction 60min~180min under 100r/min~300r/min, be cooled to room temperature, then to mixing
Mass fraction is instilled as 30% hydrogen peroxide solution using the rate of addition of 1mL/min in thing A, obtains mixture B；In ice-water bath
Under, deionized water is added into mixture B, obtains mixture C；Again by mixture C in centrifugal speed 6000r/min~8000r/
5min~15min is centrifuged under min, centrifugate is removed, obtains the presoma of thin layer boron nitride；First by 0.5mol/L's
The presoma 3 times of hydrochloric acid cleaning thin layer boron nitride, reuses the presoma 5 times~8 times of deionized water cleaning thin layer boron nitride, obtains
The presoma of thin layer boron nitride after to cleaning；
Step 1 1. described in concentrated acid be the concentrated sulfuric acid or mixed acid that mass fraction is 98%；The mixed acid is matter
Measure fraction be 98% the concentrated sulfuric acid, mass fraction be 85% phosphoric acid and mass fraction be 98% nitric acid mixed liquor；It is described
Mixed acid in mass fraction be 98% the concentrated sulfuric acid, mass fraction be 85% phosphoric acid and mass fraction be 98% nitric acid
Volume ratio is 1:1:5；
Step 1 1. described in the quality of boron nitride powder and the volume ratio of concentrated acid be (4g~8g):400mL；
Step 1 1. described in the quality of oxide and the volume ratio of concentrated acid be (20g~40g):400mL；
Step 1 1. described in concentrated acid and mass fraction be 30% the volume ratio of hydrogen peroxide solution be 400:(5~
10)；
Step 1 1. described in concentrated acid and deionized water volume ratio be 400:(300~400)；
2., by the presoma of the thin layer boron nitride after cleaning temperature be 80 DEG C~100 DEG C at be dried in vacuo 12h~24h,
Obtain the presoma of dried thin layer boron nitride；The presoma of dried thin layer boron nitride is added in organic solvent,
Ultrasound 12h~24h in the case where ultrasonic power is 100W~500W again, obtains the precursor solution of thin layer boron nitride；In centrifugal speed
To centrifuge 5min~10min to the precursor solution of thin layer boron nitride under 3000r/min, then upper strata centrifugate is taken, obtained
Superthin layer nitrogenizes B solution；Superthin layer nitridation B solution is filtered by vacuum, then by the solid matter obtained after suction filtration in temperature
Spend to be dried in vacuo 12h~24h at 80 DEG C~100 DEG C, obtain superthin layer boron nitride powder；
Step 1 2. described in dried thin layer boron nitride the quality of presoma and the volume ratio of organic solvent be
(1g~3g):100mL；
2nd, the thick polyamic acid solution containing superthin layer boron nitride and aluminium nitride is prepared：
1., by step 1 2. in obtained superthin layer boron nitride powder be dissolved into organic solvent, then low whipping speed is
Under 100r/min~300r/min stir 10min~30min, then ultrasonic power be 100W~300W under ultrasound 10min~
30min, adds aluminium nitride powder, then ultrasound 20min~40min in the case where ultrasonic power is 100W~300W, obtains containing super
The solution of thin layer boron nitride and aluminium nitride；
Step 2 1. in the solution containing superthin layer boron nitride and aluminium nitride superthin layer boron nitride mass fraction
For 0.5%~7.5%, the mass fraction of aluminium nitride is 0.5%~7.5%；
2., diamines is added in the solution containing superthin layer boron nitride and aluminium nitride, then in the case where ultrasonic power is 300W
2h~4h is ultrasonically treated, then divides 4 times~5 times addition dianhydrides in ice-water bath and mixing speed for the condition of 100r/min, then is being stirred
Speed is mixed to stir 12h~24h under 100r/min~300r/min, then is placed in standing 2h~6h in the vacuum drying chamber of room temperature,
Obtain the thick polyamic acid solution containing superthin layer boron nitride and aluminium nitride；
3rd, laminated film is prepared：
1., by step 2 prepare it is thick contain the polyamic acid solution of superthin layer boron nitride and aluminium nitride curtain coating, rotation
Apply or plastic film mulch be on clean glass plate, then by glass plate at 80 DEG C dry 12h~24h, obtain the glass plate of plastic film mulch；
2., by the glass plate of plastic film mulch with the heating rate of 3 DEG C/min~5 DEG C/min from room temperature to 350 DEG C, then
1h~2h, then cooled to room temperature are kept the temperature at 350 DEG C, finally demoulds, obtains the high heat conduction of boron nitride and aluminium nitride codope
High dielectric polyimide laminated film.
Present embodiment advantage：
First, present embodiment is improving composite material electric insulation and machine using two kinds of nitride nano particles of high heat conduction
Tool performance at the same time, improves the thermal conductivity factor of composite material, realizes the nano particle of chondritic and the nanometer of layer structure
The cooperative effect of boron nitride piece, improves the comprehensive performance of composite polyimide material；
2nd, present embodiment is doped with substantial amounts of nano particle, and composites can obtain good comprehensive macroscopic view
Performance, solves the technical barrier of the thermal conductivity of existing polyimide composite film, insulating properties and mechanical property inequality；
3rd, the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by present embodiment
Thermal conductivity factor improve 68%~330%；
4th, the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by present embodiment
Insulation resistance improve 0.8 times~4.1 times；
5th, the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by present embodiment
Tensile strength improve 1%~31%.
Present embodiment is suitable for preparing the high dielectric polyimide THIN COMPOSITE of high heat conduction of boron nitride and aluminium nitride codope
Film.
Embodiment two：Present embodiment is with one difference of embodiment：Step 2 1. described in have
Solvent is 1-methyl-2-pyrrolidinone or dinethylformamide.Other steps are identical with embodiment one.
Embodiment three：Present embodiment is with one of embodiment one or two difference：Step 2 2. in
The diamines is 4,4 '-diaminodiphenyl ether.Other steps are the same as one or two specific embodiments.
Embodiment four：Present embodiment is with one of embodiment one to three difference：Step 2 2. in
The dianhydride is biphenyl type dianhydride or equal benzene-type dianhydride；The biphenyl type dianhydride is 3,3', 4,4'- biphenyltetracarboxyacid acids two
Acid anhydride；The equal benzene-type dianhydride is pyromellitic acid anhydride.Other steps are identical with embodiment one to three.
Embodiment five：Present embodiment is with one of embodiment one to four difference：Step 2 1. in
The particle diameter of the aluminium nitride is 20nm~50nm.Other steps are identical with embodiment one to four.
Embodiment six：Present embodiment is with one of embodiment one to five difference：Step 3 2. in
The thickness of the boron nitride and the high dielectric polyimide laminated film of the high heat conduction of aluminium nitride codope is 30 μm~50 μm.Its
His step is identical with embodiment one to five.
Embodiment seven：Present embodiment is with one of embodiment one to six difference：Step 1 1. in
The oxide is potassium permanganate or potassium ferrate.Other steps are identical with embodiment one to six.
Embodiment eight：Present embodiment is with one of embodiment one to seven difference：Step 1 2. in
The organic solvent is 1-methyl-2-pyrrolidinone, dimethylformamide or dimethylacetylamide.Other steps and specific implementation
Mode one to seven is identical.
Embodiment nine：Present embodiment is with one of embodiment one to eight difference：Step 2 1. institute
The mass fraction of superthin layer boron nitride is 0.5%~1.5% in the solution containing superthin layer boron nitride and aluminium nitride stated, nitridation
The mass fraction of aluminium is 0.5%~1.5%.Other steps are identical with embodiment one to eight.
Embodiment ten：Present embodiment is with one of embodiment one to nine difference：Step 2 1. institute
The mass fraction of superthin layer boron nitride is 1.5%~7.5% in the solution containing superthin layer boron nitride and aluminium nitride stated, nitridation
The mass fraction of aluminium is 1.5%~7.5%.Other steps are identical with embodiment one to nine.
Beneficial effects of the present invention are verified using following embodiments：
Embodiment one：A kind of preparation of the high dielectric polyimide laminated film of the high heat conduction of boron nitride and aluminium nitride codope
Method is completed according to the following steps：
First, ultrathin boron nitride powder is prepared：
1., 6g boron nitride powders and 20g oxides be added in 400mL concentrated acids, then be in ice-water bath and mixing speed
Stirring reaction 60min, obtains mixture A under 100r/min；Mixture A is heated to 50 DEG C, then for 50 DEG C and is stirred in temperature
Speed is stirring reaction 60min under 100r/min, is cooled to room temperature, then dripped with the rate of addition of 1mL/min into mixture A
Enter the hydrogen peroxide solution that 10mL mass fractions are 30%, obtain mixture B；Under ice-water bath, 350mL is added into mixture B
Deionized water, obtains mixture C；Mixture C is centrifuged into 5min in the case where centrifugal speed is 6000r/min again, removes centrifugation
Liquid, obtains the presoma of thin layer boron nitride；First by the presoma 3 times of the hydrochloric acid cleaning thin layer boron nitride of 0.5mol/L, then
Use the presoma 5 times of deionized water cleaning thin layer boron nitride, the presoma of the thin layer boron nitride after being cleaned；
Step 1 1. described in concentrated acid be the concentrated sulfuric acid that mass fraction is 98%；
Step 1 1. described in oxide be potassium permanganate；
2., by the presoma of the thin layer boron nitride after cleaning temperature be 80 DEG C at be dried in vacuo 12h, obtain dried
The presoma of thin layer boron nitride；The presoma of dried thin layer boron nitride is added in organic solvent, then in ultrasonic power
For ultrasound 12h under 300W, the precursor solution of thin layer boron nitride is obtained；Thin layer is nitrogenized in the case where centrifugal speed is 3000r/min
The precursor solution of boron centrifuges 5min, then takes upper strata centrifugate, obtains superthin layer nitridation B solution；By superthin layer boron nitride
Solution is filtered by vacuum, then the solid matter obtained after suction filtration is dried in vacuo 12h in the case where temperature is 80 DEG C, obtains superthin layer
Boron nitride powder；
Step 1 2. described in dried thin layer boron nitride the quality of presoma and the volume ratio of organic solvent be
1g:100mL；
Step 1 2. described in organic solvent be dimethylacetylamide；
2nd, the thick polyamic acid solution containing superthin layer boron nitride and aluminium nitride is prepared：
1., by step 1 2. in obtained superthin layer boron nitride powder be dissolved into organic solvent, then low whipping speed is
20min, then the ultrasound 20min in the case where ultrasonic power is 200W are stirred under 200r/min, adds alumina powder, then in ultrasonic work(
Rate is ultrasound 30min under 200W, obtains the solution containing superthin layer boron nitride and aluminium nitride；
Step 2 1. described in the particle diameter of aluminium nitride powder be 20nm~50nm；
Step 2 1. described in organic solvent be 1-methyl-2-pyrrolidinone；
Step 2 1. in the solution containing superthin layer boron nitride and aluminium nitride superthin layer boron nitride mass fraction
For 0.5%, the mass fraction of aluminium nitride is 0.5%；
2., diamines is added in the solution containing superthin layer boron nitride and aluminium nitride, then in the case where ultrasonic power is 300W
2h is ultrasonically treated, then divides 4 times for the condition of 100r/min in ice-water bath and mixing speed and adds dianhydrides, then low whipping speed is
12h is stirred under 200r/min, then is placed in the vacuum drying chamber of room temperature and stands 4h, obtain it is thick containing superthin layer boron nitride and
The polyamic acid solution of aluminium nitride；
Step 2 2. described in diamines be 4,4 '-diaminodiphenyl ether；
Step 2 2. described in dianhydride be pyromellitic acid anhydride；
3rd, laminated film is prepared：
1., by step 2 prepare it is thick contain the polyamic acid solution of superthin layer boron nitride and aluminium nitride curtain coating, rotation
Apply or plastic film mulch be on clean glass plate, then by glass plate at 80 DEG C dry 12h, obtain the glass plate of plastic film mulch；
2., by the glass plate of plastic film mulch with the heating rate of 3 DEG C/min from room temperature to 350 DEG C, then kept the temperature at 350 DEG C
2h, then cooled to room temperature, finally demould, and the high dielectric polyimide of high heat conduction for obtaining boron nitride and aluminium nitride codope is answered
Close film；
Step 3 2. described in boron nitride and aluminium nitride codope high heat conduction high dielectric polyimide laminated film
Thickness is 45 μm.
Embodiment two：The present embodiment and the difference of embodiment one are：Step 2 is 1. described to contain superthin layer boron nitride
Mass fraction with superthin layer boron nitride in the solution of aluminium nitride is 1.5%, and the mass fraction of aluminium nitride is 1.5%.Other steps
Rapid and parameter is identical with embodiment one.
Embodiment three：The present embodiment and the difference of embodiment one are：Step 2 is 1. described to contain superthin layer boron nitride
Mass fraction with superthin layer boron nitride in the solution of aluminium nitride is 2.5%, and the mass fraction of aluminium nitride is 2.5%.Other steps
Rapid and parameter is identical with embodiment one.
Example IV：The present embodiment and the difference of embodiment one are：Step 2 is 1. described to contain superthin layer boron nitride
Mass fraction with superthin layer boron nitride in the solution of aluminium nitride is 5%, and the mass fraction of aluminium nitride is 5%.Other steps and
Parameter is identical with embodiment one.
Embodiment five：The present embodiment and the difference of embodiment one are：Step 2 is 1. described to contain superthin layer boron nitride
Mass fraction with superthin layer boron nitride in the solution of aluminium nitride is 7.5%, and the mass fraction of aluminium nitride is 7.5%.Other steps
Rapid and parameter is identical with embodiment one.
Comparative example：The present embodiment and the difference of embodiment one are：Step 2 is 1. described to be nitrogenized containing superthin layer
The mass fraction of superthin layer boron nitride is 0% in the solution of boron and aluminium nitride, and the mass fraction of aluminium nitride is 0%.Other steps
And parameter is identical with embodiment one.
Fig. 1 is the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one
SEM figure；
From fig. 1, it can be seen that boron nitride and aluminium nitride that the boron nitride of stratiform is prepared with spherical aluminium nitride in embodiment one are total to
It is evenly distributed in the high dielectric polyimide laminated film of high heat conduction of doping, and polyimide matrix produces to have and necessarily crystallizes spy
The cluster body of property, this is dispersed can to realize lifting composite property.
Fig. 2 is the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one
B element mapping；
Fig. 3 is the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one
Al Element area profiles；
Fig. 4 is the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one
N element mapping；
Fig. 5 is the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one
C element mapping；
It was found from Fig. 2~Fig. 5, the high insulation polyamides of boron nitride and the high heat conduction of aluminium nitride codope prepared by embodiment one is sub-
B, Al, N, C element are evenly distributed in amine laminated film, prove that layered nitride boron has been carried out and gathers with spherical aluminium nitride first
Imido success is compound, secondly proves that the two is uniformly distributed in the base.
Fig. 6 is the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one
Thermal property figure, A is the thermal conductivity factor of Kapton prepared by comparative example in Fig. 6, and B is prepared by embodiment one
The thermal conductivity factor of the high dielectric polyimide laminated film of the high heat conduction of boron nitride and aluminium nitride codope, C are prepared for embodiment two
Boron nitride and aluminium nitride codope the high dielectric polyimide laminated film of high heat conduction thermal conductivity factor, D made for embodiment three
The thermal conductivity factor of standby boron nitride and the high dielectric polyimide laminated film of the high heat conduction of aluminium nitride codope, E is example IV
The thermal conductivity factor of the boron nitride of preparation and the high dielectric polyimide laminated film of the high heat conduction of aluminium nitride codope, F is embodiment
The thermal conductivity factor of the high dielectric polyimide laminated film of high heat conduction of five boron nitride and aluminium nitride codope prepared；
As can be seen from Figure 6, the doping stratiform boron nitride in proper ratio and spherical aluminium nitride, prepared boron nitride and nitridation
The thermal conductivity factor of the high dielectric polyimide laminated film of high heat conduction of aluminium codope is greatly enhanced.Thermal conductivity factor improves
68%~330%.
Fig. 7 is the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one
Mechanical property figure；A is the tensile strength of Kapton prepared by comparative example in Fig. 7, and B is prepared by embodiment one
The tensile strength of the high dielectric polyimide laminated film of the high heat conduction of boron nitride and aluminium nitride codope, C are prepared for embodiment two
Boron nitride and aluminium nitride codope the high dielectric polyimide laminated film of high heat conduction tensile strength, D made for embodiment three
The tensile strength of standby boron nitride and the high dielectric polyimide laminated film of the high heat conduction of aluminium nitride codope, E is example IV
The tensile strength of the boron nitride of preparation and the high dielectric polyimide laminated film of the high heat conduction of aluminium nitride codope, F is embodiment
The tensile strength of the high dielectric polyimide laminated film of high heat conduction of five boron nitride and aluminium nitride codope prepared；
As can be seen from Figure 7, when the stratiform doping boron nitride of proper ratio is with spherical aluminium nitride, prepared boron nitride and nitrogen
Change the getable reinforcement of mechanical property of the high dielectric polyimide laminated film of high heat conduction of aluminium codope, tensile strength improves
1%~31%.
Fig. 8 is the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one
Resistivity properties block diagram；A is that the high insulation of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one is poly- in Fig. 8
The volume resistance of acid imide laminated film, B are the high insulation of high heat conduction of boron nitride prepared by embodiment two and aluminium nitride codope
The volume resistance of polyimide composite film, the boron nitride and the high heat conduction of aluminium nitride codope that C is prepared for embodiment three are high absolutely
The volume resistance of edge polyimide composite film, D are the high heat conduction height of boron nitride prepared by example IV and aluminium nitride codope
The volume resistance of dielectric polyimide laminated film, E are the high heat conduction of boron nitride prepared by embodiment five and aluminium nitride codope
The volume resistance of high dielectric polyimide laminated film；
As it can be observed in the picture that when the stratiform doping boron nitride of proper ratio is with spherical aluminium nitride, prepared boron nitride and nitrogen
The insulation resistance for changing the high dielectric polyimide laminated film of high heat conduction of aluminium codope increases substantially, and insulation resistance improves
0.8 times~4.1 times.
Fig. 9 is the high dielectric polyimide laminated film of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one
Inverter fed motor life-span block diagram, A is that the high insulation of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one is poly- in Fig. 9
The Inverter fed motor time of acid imide laminated film, the boron nitride and the high heat conduction of aluminium nitride codope that B is prepared for embodiment two are high absolutely
The Inverter fed motor time of edge polyimide composite film, C are the high heat conduction of boron nitride prepared by embodiment three and aluminium nitride codope
The Inverter fed motor time of high dielectric polyimide laminated film, D are the height of boron nitride prepared by example IV and aluminium nitride codope
The Inverter fed motor time of the high dielectric polyimide laminated film of heat conduction, E are boron nitride and aluminium nitride codope prepared by embodiment five
The high dielectric polyimide laminated film of high heat conduction the Inverter fed motor time.
As can be seen from Figure 9, the high dielectric polyimide of high heat conduction of boron nitride and aluminium nitride codope prepared by embodiment one is answered
The Inverter fed motor life-span for closing film has obtained the lifting of substance, and Inverter fed motor life-span improves 8.1 times~36.1 times.
Claims (9)
1. a kind of preparation method of the high dielectric polyimide laminated film of the high heat conduction of boron nitride and aluminium nitride codope, its feature
It is that this method is completed according to the following steps：
First, ultrathin boron nitride powder is prepared：
1., boron nitride powder and oxide be added in concentrated acid, then in ice-water bath and mixing speed be 100r/min~300r/
Stirring reaction 60min~120min, obtains mixture A under min；Mixture A is heated to 50 DEG C, then for 50 DEG C and is stirred in temperature
Speed is mixed as stirring reaction 60min~180min under 100r/min~300r/min, is cooled to room temperature, then into mixture A
Mass fraction is instilled as 30% hydrogen peroxide solution using the rate of addition of 1mL/min, obtains mixture B；Under ice-water bath, to mixed
Deionized water is added in compound B, obtains mixture C；Again by mixture C under centrifugal speed 6000r/min~8000r/min from
The heart separates 5min~15min, removes centrifugate, obtains the presoma of thin layer boron nitride；It is clear first by the hydrochloric acid of 0.5mol/L
The presoma 3 times of thin layer boron nitride is washed, the presoma 5 times~8 times of deionized water cleaning thin layer boron nitride is reused, is cleaned
The presoma of thin layer boron nitride afterwards；
Step 1 1. described in concentrated acid be the concentrated sulfuric acid or mixed acid that mass fraction is 98%；The mixed acid is quality point
Count the concentrated sulfuric acid for 98%, the mixed liquor for the nitric acid that the phosphoric acid that mass fraction is 85% and mass fraction are 98%；Described is mixed
Close acid in mass fraction be 98% the concentrated sulfuric acid, mass fraction be 85% phosphoric acid and mass fraction be 98% nitric acid volume
Than for 1:1:5；
Step 1 1. described in oxide be potassium permanganate or potassium ferrate；
Step 1 1. described in the quality of boron nitride powder and the volume ratio of concentrated acid be (4g~8g):400mL；
Step 1 1. described in the quality of oxide and the volume ratio of concentrated acid be (20g~40g):400mL；
Step 1 1. described in concentrated acid and mass fraction be 30% the volume ratio of hydrogen peroxide solution be 400:(5~10)；
Step 1 1. described in concentrated acid and deionized water volume ratio be 400:(300~400)；
2., by the presoma of the thin layer boron nitride after cleaning temperature be 80 DEG C~100 DEG C at be dried in vacuo 12h~24h, obtain
The presoma of dried thin layer boron nitride；The presoma of dried thin layer boron nitride is added in organic solvent, then
Ultrasonic power is ultrasound 12h~24h under 100W~500W, obtains the precursor solution of thin layer boron nitride；It is in centrifugal speed
5min~10min is centrifuged to the precursor solution of thin layer boron nitride under 3000r/min, then takes upper strata centrifugate, is surpassed
Thin layer nitrogenizes B solution；Superthin layer nitridation B solution is filtered by vacuum, then by the solid matter obtained after suction filtration in temperature
To be dried in vacuo 12h~24h at 80 DEG C~100 DEG C, superthin layer boron nitride powder is obtained；
Step 1 2. described in dried thin layer boron nitride presoma quality and organic solvent volume ratio for (1g~
3g):100mL；
2nd, the thick polyamic acid solution containing superthin layer boron nitride and aluminium nitride is prepared：
1., by step 1 2. in obtained superthin layer boron nitride powder be dissolved into organic solvent, then low whipping speed is 100r/
10min~30min, then ultrasound 10min~30min in the case where ultrasonic power is 100W~300W are stirred under min~300r/min, then
Aluminium nitride powder, then ultrasound 20min~40min in the case where ultrasonic power is 100W~300W are added, obtains nitrogenizing containing superthin layer
The solution of boron and aluminium nitride；
1. the mass fraction of superthin layer boron nitride is step 2 in the solution containing superthin layer boron nitride and aluminium nitride
0.5%~7.5%, the mass fraction of aluminium nitride is 0.5%~7.5%；
2., diamines is added in the solution containing superthin layer boron nitride and aluminium nitride, then the ultrasound in the case where ultrasonic power is 300W
2h~4h is handled, then divides 4 times~5 times addition dianhydrides in ice-water bath and mixing speed for the condition of 100r/min, then in stirring speed
Spend to stir 12h~24h under 100r/min~300r/min, then be placed in standing 2h~6h in the vacuum drying chamber of room temperature, obtain
The thick polyamic acid solution containing superthin layer boron nitride and aluminium nitride；
3rd, laminated film is prepared：
1., by step 2 prepare it is thick containing the polyamic acid solution of superthin layer boron nitride and aluminium nitride curtain coating, spin coating or
Plastic film mulch on clean glass plate, then by glass plate at 80 DEG C dry 12h~24h, obtain the glass plate of plastic film mulch；
2., by the glass plate of plastic film mulch with the heating rate of 3 DEG C/min~5 DEG C/min from room temperature to 350 DEG C, then at 350 DEG C
Lower insulation 1h~2h, then cooled to room temperature, last demoulding, obtain the high insulation of high heat conduction of boron nitride and aluminium nitride codope
Polyimide composite film.
2. the high dielectric polyimide THIN COMPOSITE of the high heat conduction of a kind of boron nitride according to claim 1 and aluminium nitride codope
The preparation method of film, it is characterised in that step 2 1. described in organic solvent be 1-methyl-2-pyrrolidinone or N, N- dimethyl methyl
Acid amides.
3. the high dielectric polyimide THIN COMPOSITE of the high heat conduction of a kind of boron nitride according to claim 1 and aluminium nitride codope
The preparation method of film, it is characterised in that step 2 2. described in diamines be 4,4 '-diaminodiphenyl ether.
4. the high dielectric polyimide THIN COMPOSITE of the high heat conduction of a kind of boron nitride according to claim 1 and aluminium nitride codope
The preparation method of film, it is characterised in that step 2 2. described in dianhydride be biphenyl type dianhydride or equal benzene-type dianhydride；The connection
Benzene-type dianhydride is 3,3', 4,4'- biphenyl tetracarboxylic dianhydrides；The equal benzene-type dianhydride is pyromellitic acid anhydride.
5. the high dielectric polyimide THIN COMPOSITE of the high heat conduction of a kind of boron nitride according to claim 1 and aluminium nitride codope
The preparation method of film, it is characterised in that step 2 1. described in the particle diameter of aluminium nitride be 20nm~50nm.
6. the high dielectric polyimide THIN COMPOSITE of the high heat conduction of a kind of boron nitride according to claim 1 and aluminium nitride codope
The preparation method of film, it is characterised in that step 3 2. described in boron nitride and aluminium nitride codope the high insulation polyamides of high heat conduction
The thickness of imines laminated film is 30 μm~50 μm.
7. the high dielectric polyimide THIN COMPOSITE of the high heat conduction of a kind of boron nitride according to claim 1 and aluminium nitride codope
The preparation method of film, it is characterised in that step 1 2. described in organic solvent for 1-methyl-2-pyrrolidinone, dimethylformamide
Or dimethylacetylamide.
8. the high dielectric polyimide THIN COMPOSITE of the high heat conduction of a kind of boron nitride according to claim 1 and aluminium nitride codope
The preparation method of film, it is characterised in that step 2 1. superthin layer nitrogen in the solution containing superthin layer boron nitride and aluminium nitride
The mass fraction for changing boron is 0.5%~1.5%, and the mass fraction of aluminium nitride is 0.5%~1.5%.
9. the high dielectric polyimide THIN COMPOSITE of the high heat conduction of a kind of boron nitride according to claim 1 and aluminium nitride codope
The preparation method of film, it is characterised in that step 2 1. superthin layer nitrogen in the solution containing superthin layer boron nitride and aluminium nitride
The mass fraction for changing boron is 1.5%~7.5%, and the mass fraction of aluminium nitride is 1.5%~7.5%.
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| CN108751927B (en) * | 2018-07-09 | 2020-08-18 | 陕西科技大学 | Preparation method of high-thermal-conductivity graphene oxide and boron nitride composite film material |
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| CN102673047A (en) * | 2012-05-28 | 2012-09-19 | 珠海亚泰电子科技有限公司 | Fabricating method of thermal conducting halogen-free binderless copper clad foil |
| CN103626141A (en) * | 2013-12-12 | 2014-03-12 | 山东大学 | Method for preparing hexagonal boron nitride nanosheets by chemical stripping |
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| CN103626141A (en) * | 2013-12-12 | 2014-03-12 | 山东大学 | Method for preparing hexagonal boron nitride nanosheets by chemical stripping |
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