CN106380844A - Preparation method of boron nitride and aluminum nitride co-doped high-heat-conduction and high-insulation polyimide composite thin film - Google Patents
Preparation method of boron nitride and aluminum nitride co-doped high-heat-conduction and high-insulation polyimide composite thin film Download PDFInfo
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Abstract
The invention provides a preparation method of a boron nitride and aluminum nitride co-doped high-heat-conduction and high-insulation polyimide composite thin film and relates to a preparation method of a composite thin film, aiming at solving the problems of an existing polyimide composite thin film that the heat conductivity, insulation property and mechanical properties are poor so that the application of the existing polyimide composite thin film in the field of electric insulation is limited. The preparation method comprises: 1, preparing ultrathin boron nitride powder; 2, preparing a viscous polyamic acid solution containing ultrathin-layer boron nitride and aluminum nitride; 3, preparing a composite thin film to obtain the boron nitride and aluminum nitride co-doped high-heat-conduction and high-insulation polyimide composite thin film. According to the boron nitride and aluminum nitride co-doped high-heat-conduction and high-insulation polyimide composite thin film prepared by the preparation method provided by the invention, the coefficient of heat conductivity is improved by 68 percent to 330 percent, the insulating resistance is improved by 0.8 to 4.1 times and the tensile strength is improved by 1 percent to 31 percent. The preparation method provided by the invention is suitable for preparing the boron nitride and aluminum nitride co-doped high-heat-conduction and high-insulation polyimide composite thin film.
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 frequency conversion motor such as product, is a kind of high performance insulating material, is mainly used in
The turn-to-turn insulation of frequency conversion motor winding and insulation against ground, the exploitation of this product originates from the need of converter technique and frequency control motor
Ask.Du pont company in 1994, ABB AB of Switzerland and Siemens cooperation take the lead in have developed corona-resistant polyimide
Thin film (Kapton FCR), makes the Inverter fed motor life-span of this material reach hundreds of or even thousands of times of common Kapton.
In addition corona-resistant polyimide film also has preferable heat conductivility, and the heat conductivity of Kapton 100CR thin film is
The heat conductivity of 0.385W/ (m.K), plain edition Kapton 100HN only has 0.19W/ (m.K), Kapton FCR can substantially reduce
Temperature rise in running for the electrical equipment and electrical and due to corona cause hot-spot, extend the service life of material.With
Corona-resistant polyimide film, as wire insulation and insulation against ground, is traction electric machine and high-voltage motor miniaturization opens
New road.Other research units put into a large amount of man power and materials' development related fields researchs both at home and abroad, including polymer matrix no
Machine nano composite material preparation method, performance test and application, and obtain the achievement that many attracts people's attention.But it is domestic at present
Composite polyimide material, goes back and same kind of products at abroad in the combination properties such as Inverter fed motor life-span, mechanical performance and thermal property
There is gap.
At present on the premise of keeping high electrical insulation properties and mechanical performance, the heat conductivility improving material is still
The research topic that art circle and industrial quarters face.
Content of the invention
The invention aims to it is equal to solve the heat conductivity of existing polyimide composite film, insulating properties and mechanical property
Difference, applies, in electric insulation field, the problem being restricted, and provides a kind of boron nitride and the high heat conduction of aluminium nitride codope
The preparation method of high dielectric polyimide laminated film.
A kind of preparation method of the high heat conduction high dielectric polyimide laminated film of boron nitride and aluminium nitride codope be by
Following steps complete：
First, prepare ultrathin boron nitride powder：
1., boron nitride powder and oxide are added in concentrated acid, then ice-water bath and mixing speed be 100r/min～
Stirring reaction 60min～120min under 300r/min, obtains mixture A；Mixture A is heated to 50 DEG C, then is 50 in temperature
DEG C and mixing speed be stirring reaction 60min～180min under 100r/min～300r/min, be cooled to room temperature, then to mixing
In thing A, the hydrogen peroxide solution that mass fraction is 30% is instilled with the rate of addition of 1mL/min, obtain mixture B；In ice-water bath
Under, add deionized water in mixture B, obtain mixture C；Again by mixture C in centrifugal speed 6000r/min～8000r/
Centrifugation 5min～15min under min, removes centrifugal liquid, obtains the presoma of thin layer boron nitride；First by 0.5mol/L's
Hydrochloric acid cleans the presoma 3 times of thin layer boron nitride, reuses the presoma 5 times～8 times that deionized water cleans thin layer boron nitride, obtains
The presoma of the thin layer boron nitride to after cleaning；
Step one 1. described in concentrated acid for mass fraction be 98% concentrated sulphuric acid or mixed acid；Described mixed acid is matter
Amount fraction be 98% concentrated sulphuric acid, mass fraction be 85% phosphoric acid and the mixed liquor of nitric acid that mass fraction is 98%；Described
Mixed acid in mass fraction be 98% concentrated sulphuric acid, mass fraction be 85% phosphoric acid and nitric acid that mass fraction is 98%
Volume ratio is 1:1:5；
Step one 1. described in the volume ratio of the quality of boron nitride powder and concentrated acid be (4g～8g):400mL；
Step one 1. described in the volume ratio of the quality of oxide and concentrated acid be (20g～40g):400mL；
Step one 1. described in concentrated acid and mass fraction be 30% volume ratio of hydrogen peroxide solution be 400:(5～
10)；
Step one 1. described in the volume ratio of concentrated acid and deionized water be 400:(300～400)；
2., the presoma of the thin layer boron nitride after cleaning is vacuum dried 12h～24h at temperature is 80 DEG C～100 DEG C,
Obtain the presoma of dried thin layer boron nitride；The presoma of dried thin layer boron nitride is added in organic solvent,
It is 12h～24h ultrasonic under 100W～500W in ultrasonic power again, obtain the precursor solution of thin layer boron nitride；In centrifugal speed
For the precursor solution centrifugation 5min～10min to thin layer boron nitride under 3000r/min, then take upper strata centrifugal liquid, obtain
Superthin layer nitrogenizes B solution；Superthin layer nitridation B solution is carried out vacuum filtration, then by the solid matter obtaining after sucking filtration in temperature
Spend for being vacuum dried 12h～24h at 80 DEG C～100 DEG C, obtain superthin layer boron nitride powder；
Step one 2. described in the quality of presoma of dried thin layer boron nitride with the volume ratio of organic solvent be
(1g～3g):100mL；
2nd, prepare the thick polyamic acid solution containing superthin layer boron nitride and aluminium nitride：
1., by step one 2. in the superthin layer boron nitride powder that obtains be dissolved in organic solvent, then low whipping speed is
Under 100r/min～300r/min stir 10min～30min, then ultrasonic power for 10min ultrasonic under 100W～300W～
30min, adds aluminium nitride powder, then is 20min～40min ultrasonic under 100W～300W in ultrasonic power, obtains containing super
Thin layer boron nitride and the solution of aluminium nitride；
The mass fraction of superthin layer boron nitride in the 1. described solution containing superthin layer boron nitride and aluminium nitride of step 2
For 0.5%～7.5%, the mass fraction of aluminium nitride is 0.5%～7.5%；
2., diamidogen is added in the solution containing superthin layer boron nitride and aluminium nitride, then under ultrasonic power is for 300W
Supersound process 2h～4h, then the condition for 100r/min divides 4 times～5 times addition dianhydrides in ice-water bath and mixing speed, then stirring
Mixing speed is to stir 12h～24h under 100r/min～300r/min, then is placed in standing 2h～6h in the vacuum drying oven of room temperature,
Obtain the thick polyamic acid solution containing superthin layer boron nitride and aluminium nitride；
3rd, prepare laminated film：
1., the thick polyamic acid solution containing superthin layer boron nitride and aluminium nitride prepared by step 2 is cast, revolves
Apply or plastic film mulch is dried 12h～24h on clean glass plate, then by glass plate at 80 DEG C, 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
It is incubated 1h～2h at 350 DEG C, then naturally cool to room temperature, the last demoulding, obtain boron nitride and the high heat conduction of aluminium nitride codope
High dielectric polyimide laminated film.
Invention advantage：
First, the present invention utilizes two kinds of nitride nano granules of high heat conduction improving composite electric insulation and mechanicalness
The heat conductivity of composite, can be improved it is achieved that the nano silicon nitride of the nano-particle of chondritic and layer structure simultaneously
The cooperative effect of boron piece, improves the combination property of composite polyimide material；
2nd, the present invention is doped with substantial amounts of nano-particle, and composites can obtain good comprehensive macro property,
Solve the technical barrier of the heat conductivity, insulating properties and mechanical property inequality of existing polyimide composite film；
3rd, the leading of high heat conduction high dielectric polyimide laminated film of the boron nitride of present invention preparation and aluminium nitride codope
Hot coefficient improves 68%～330%；
4th, the high heat conduction high dielectric polyimide laminated film of the boron nitride of present invention preparation and aluminium nitride codope is exhausted
Edge resistance improves 0.8 times～4.1 times；
5th, the drawing of high heat conduction high dielectric polyimide laminated film of the boron nitride of present invention preparation and aluminium nitride codope
Stretch intensity and improve 1%～31%.
The present invention is applied to the high heat conduction high dielectric polyimide laminated film preparing boron nitride and aluminium nitride codope.
Brief description
Fig. 1 is the boron nitride of embodiment one preparation and the high heat conduction high dielectric polyimide laminated film of aluminium nitride codope
SEM figure；
Fig. 2 is the boron nitride of embodiment one preparation and the high heat conduction high dielectric polyimide laminated film of aluminium nitride codope
B element mapping；
Fig. 3 is the boron nitride of embodiment one preparation and the high heat conduction high dielectric polyimide laminated film of aluminium nitride codope
Al Element area profile；
Fig. 4 is the boron nitride of embodiment one preparation and the high heat conduction high dielectric polyimide laminated film of aluminium nitride codope
N element mapping；
Fig. 5 is the boron nitride of embodiment one preparation and the high heat conduction high dielectric polyimide laminated film of aluminium nitride codope
C element mapping；
Fig. 6 is the boron nitride of embodiment one preparation and the high heat conduction high dielectric polyimide laminated film of aluminium nitride codope
Thermal property figure, the heat conductivity of the Kapton that A is prepared for comparative example in Fig. 6, B be embodiment one preparation
The heat conductivity of the high heat conduction high dielectric polyimide laminated film of boron nitride and aluminium nitride codope, C is prepared for embodiment two
Boron nitride and aluminium nitride codope high heat conduction high dielectric polyimide laminated film heat conductivity, D makes for embodiment three
The heat conductivity of the high heat conduction high dielectric polyimide laminated film of standby boron nitride and aluminium nitride codope, E is example IV
The heat conductivity of the high heat conduction high dielectric polyimide laminated film of the boron nitride of preparation and aluminium nitride codope, F is embodiment
The heat conductivity of the high heat conduction high dielectric polyimide laminated film of the boron nitride of five preparations and aluminium nitride codope；
Fig. 7 is the boron nitride of embodiment one preparation and the high heat conduction high dielectric polyimide laminated film of aluminium nitride codope
Mechanical property figure；The tensile strength of the Kapton that A is prepared for comparative example in Fig. 7, B is embodiment one preparation
The tensile strength of the high heat conduction high dielectric polyimide laminated film of boron nitride and aluminium nitride codope, C is prepared for embodiment two
Boron nitride and aluminium nitride codope high heat conduction high dielectric polyimide laminated film tensile strength, D makes for embodiment three
The tensile strength of the high heat conduction high dielectric polyimide laminated film of standby boron nitride and aluminium nitride codope, E is example IV
The tensile strength of the high heat conduction high dielectric polyimide laminated film of the boron nitride of preparation and aluminium nitride codope, F is embodiment
The tensile strength of the high heat conduction high dielectric polyimide laminated film of the boron nitride of five preparations and aluminium nitride codope；
Fig. 8 is the boron nitride of embodiment one preparation and the high heat conduction high dielectric polyimide laminated film of aluminium nitride codope
Resistivity properties block diagram；In Fig. 8, A is the boron nitride of embodiment one preparation and the high insulation of high heat conduction of aluminium nitride codope gathers
The volume resistance of acid imide laminated film, B is the boron nitride of embodiment two preparation and the high insulation of high heat conduction of aluminium nitride codope
The volume resistance of polyimide composite film, C is the boron nitride of embodiment three preparation and the high heat conduction of aluminium nitride codope is high absolutely
The volume resistance of edge polyimide composite film, the boron nitride that D is prepared for example IV and the high heat conduction of aluminium nitride codope are high
The volume resistance of dielectric polyimide laminated film, E is the boron nitride of embodiment five preparation and the high heat conduction of aluminium nitride codope
The volume resistance of high dielectric polyimide laminated film；
Fig. 9 is the boron nitride of embodiment one preparation and the high heat conduction high dielectric polyimide laminated film of aluminium nitride codope
Inverter fed motor life-span block diagram, in Fig. 9 A be the boron nitride of embodiment one preparation and aluminium nitride codope the high insulation of high heat conduction poly-
The Inverter fed motor time of acid imide laminated film, B is the boron nitride of embodiment two preparation and the high heat conduction of aluminium nitride codope is high absolutely
The Inverter fed motor time of edge polyimide composite film, C is the boron nitride of embodiment three preparation and the high heat conduction of aluminium nitride codope
The Inverter fed motor time of high dielectric polyimide laminated film, boron nitride and the height of aluminium nitride codope that D is prepared for example IV
The Inverter fed motor time of heat conduction high dielectric polyimide laminated film, E is boron nitride and the aluminium nitride codope of embodiment five preparation
High heat conduction high dielectric polyimide laminated film the Inverter fed motor time.
Specific embodiment
Specific embodiment one：Present embodiment is the high heat conduction high insulation polyamides of a kind of boron nitride and aluminium nitride codope
The preparation method of imines laminated film is it is characterised in that the method completes according to the following steps：
First, prepare ultrathin boron nitride powder：
1., boron nitride powder and oxide are added in concentrated acid, then ice-water bath and mixing speed be 100r/min～
Stirring reaction 60min～120min under 300r/min, obtains mixture A；Mixture A is heated to 50 DEG C, then is 50 in temperature
DEG C and mixing speed be stirring reaction 60min～180min under 100r/min～300r/min, be cooled to room temperature, then to mixing
In thing A, the hydrogen peroxide solution that mass fraction is 30% is instilled with the rate of addition of 1mL/min, obtain mixture B；In ice-water bath
Under, add deionized water in mixture B, obtain mixture C；Again by mixture C in centrifugal speed 6000r/min～8000r/
Centrifugation 5min～15min under min, removes centrifugal liquid, obtains the presoma of thin layer boron nitride；First by 0.5mol/L's
Hydrochloric acid cleans the presoma 3 times of thin layer boron nitride, reuses the presoma 5 times～8 times that deionized water cleans thin layer boron nitride, obtains
The presoma of the thin layer boron nitride to after cleaning；
Step one 1. described in concentrated acid for mass fraction be 98% concentrated sulphuric acid or mixed acid；Described mixed acid is matter
Amount fraction be 98% concentrated sulphuric acid, mass fraction be 85% phosphoric acid and the mixed liquor of nitric acid that mass fraction is 98%；Described
Mixed acid in mass fraction be 98% concentrated sulphuric acid, mass fraction be 85% phosphoric acid and nitric acid that mass fraction is 98%
Volume ratio is 1:1:5；
Step one 1. described in the volume ratio of the quality of boron nitride powder and concentrated acid be (4g～8g):400mL；
Step one 1. described in the volume ratio of the quality of oxide and concentrated acid be (20g～40g):400mL；
Step one 1. described in concentrated acid and mass fraction be 30% volume ratio of hydrogen peroxide solution be 400:(5～
10)；
Step one 1. described in the volume ratio of concentrated acid and deionized water be 400:(300～400)；
2., the presoma of the thin layer boron nitride after cleaning is vacuum dried 12h～24h at temperature is 80 DEG C～100 DEG C,
Obtain the presoma of dried thin layer boron nitride；The presoma of dried thin layer boron nitride is added in organic solvent,
It is 12h～24h ultrasonic under 100W～500W in ultrasonic power again, obtain the precursor solution of thin layer boron nitride；In centrifugal speed
For the precursor solution centrifugation 5min～10min to thin layer boron nitride under 3000r/min, then take upper strata centrifugal liquid, obtain
Superthin layer nitrogenizes B solution；Superthin layer nitridation B solution is carried out vacuum filtration, then by the solid matter obtaining after sucking filtration in temperature
Spend for being vacuum dried 12h～24h at 80 DEG C～100 DEG C, obtain superthin layer boron nitride powder；
Step one 2. described in the quality of presoma of dried thin layer boron nitride with the volume ratio of organic solvent be
(1g～3g):100mL；
2nd, prepare the thick polyamic acid solution containing superthin layer boron nitride and aluminium nitride：
1., by step one 2. in the superthin layer boron nitride powder that obtains be dissolved in organic solvent, then low whipping speed is
Under 100r/min～300r/min stir 10min～30min, then ultrasonic power for 10min ultrasonic under 100W～300W～
30min, adds aluminium nitride powder, then is 20min～40min ultrasonic under 100W～300W in ultrasonic power, obtains containing super
Thin layer boron nitride and the solution of aluminium nitride；
The mass fraction of superthin layer boron nitride in the 1. described solution containing superthin layer boron nitride and aluminium nitride of step 2
For 0.5%～7.5%, the mass fraction of aluminium nitride is 0.5%～7.5%；
2., diamidogen is added in the solution containing superthin layer boron nitride and aluminium nitride, then under ultrasonic power is for 300W
Supersound process 2h～4h, then the condition for 100r/min divides 4 times～5 times addition dianhydrides in ice-water bath and mixing speed, then stirring
Mixing speed is to stir 12h～24h under 100r/min～300r/min, then is placed in standing 2h～6h in the vacuum drying oven of room temperature,
Obtain the thick polyamic acid solution containing superthin layer boron nitride and aluminium nitride；
3rd, prepare laminated film：
1., the thick polyamic acid solution containing superthin layer boron nitride and aluminium nitride prepared by step 2 is cast, revolves
Apply or plastic film mulch is dried 12h～24h on clean glass plate, then by glass plate at 80 DEG C, 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
It is incubated 1h～2h at 350 DEG C, then naturally cool to room temperature, the last demoulding, obtain boron nitride and the high heat conduction of aluminium nitride codope
High dielectric polyimide laminated film.
Present embodiment advantage：
First, present embodiment utilizes two kinds of nitride nano granules of high heat conduction improving composite electric insulation and machine
Tool performance simultaneously, improves the heat conductivity of composite it is achieved that the nanometer of the nano-particle of chondritic and layer structure
The cooperative effect of boron nitride piece, improves the combination property 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 heat conductivity, insulating properties and mechanical property inequality of existing polyimide composite film；
3rd, the high heat conduction high dielectric polyimide laminated film of the boron nitride of present embodiment preparation and aluminium nitride codope
Heat conductivity improve 68%～330%；
4th, the high heat conduction high dielectric polyimide laminated film of the boron nitride of present embodiment preparation and aluminium nitride codope
Insulation resistance improve 0.8 times～4.1 times；
5th, the high heat conduction high dielectric polyimide laminated film of the boron nitride of present embodiment preparation and aluminium nitride codope
Tensile strength improve 1%～31%.
Present embodiment is applied to the high heat conduction high dielectric polyimide THIN COMPOSITE preparing boron nitride and aluminium nitride codope
Film.
Specific embodiment two：Present embodiment with specific embodiment one difference is：Step 2 1. described in have
Machine solvent is N-Methyl pyrrolidone or dinethylformamide.Other steps are identical with specific embodiment one.
Specific embodiment three：Present embodiment with one of specific embodiment one or two difference is：Step 2 2. in
Described diamidogen is 4,4 '-diaminodiphenyl ether.Other steps are identical with specific embodiment one or two.
Specific embodiment four：Present embodiment with one of specific embodiment one to three difference is：Step 2 2. in
Described dianhydride is biphenyl type dianhydride or equal benzene-type dianhydride；Described biphenyl type dianhydride is 3,3', 4,4'- biphenyltetracarboxyacid acid two
Acid anhydride；Described equal benzene-type dianhydride is pyromellitic acid anhydride.Other steps are identical with specific embodiment one to three.
Specific embodiment five：Present embodiment with one of specific embodiment one to four difference is：Step 2 1. in
The particle diameter of described aluminium nitride is 20nm～50nm.Other steps are identical with specific embodiment one to four.
Specific embodiment six：Present embodiment with one of specific embodiment one to five difference is：Step 3 2. in
The thickness of the high heat conduction high dielectric polyimide laminated film of described boron nitride and aluminium nitride codope is 30 μm～50 μm.Its
His step is identical with specific embodiment one to five.
Specific embodiment seven：Present embodiment with one of specific embodiment one to six difference is：Step one 1. in
Described oxide is potassium permanganate or potassium ferrate.Other steps are identical with specific embodiment one to six.
Specific embodiment eight：Present embodiment with one of specific embodiment one to seven difference is：Step one 2. in
Described organic solvent is N-Methyl pyrrolidone, dimethylformamide or dimethyl acetylamide.Other steps be embodied as
Mode one to seven is identical.
Specific embodiment nine：Present embodiment with one of specific embodiment one to eight difference is：Step 2 1. institute
In the solution containing superthin layer boron nitride and aluminium nitride stated, the mass fraction of superthin layer boron nitride is 0.5%～1.5%, nitridation
The mass fraction of aluminum is 0.5%～1.5%.Other steps are identical with specific embodiment one to eight.
Specific embodiment ten：Present embodiment with one of specific embodiment one to nine difference is：Step 2 1. institute
In the solution containing superthin layer boron nitride and aluminium nitride stated, the mass fraction of superthin layer boron nitride is 1.5%～7.5%, nitridation
The mass fraction of aluminum is 1.5%～7.5%.Other steps are identical with specific embodiment one to nine.
Verify beneficial effects of the present invention using following examples：
Embodiment one：A kind of preparation of the high heat conduction high dielectric polyimide laminated film of boron nitride and aluminium nitride codope
Method completes according to the following steps：
First, prepare ultrathin boron nitride powder：
1., 6g boron nitride powder and 20g oxide are added in 400mL concentrated acid, then in ice-water bath and mixing speed are
Stirring reaction 60min under 100r/min, obtains mixture A；Mixture A is heated to 50 DEG C, then is 50 DEG C and stirring in temperature
Speed is stirring reaction 60min under 100r/min, is cooled to room temperature, then is dripped with the rate of addition of 1mL/min in mixture A
Enter the hydrogen peroxide solution that 10mL mass fraction is 30%, obtain mixture B；Under ice-water bath, add 350mL in mixture B
Deionized water, obtains mixture C；Again mixture C is centrifugation 5min under 6000r/min in centrifugal speed, removes centrifugation
Liquid, obtains the presoma of thin layer boron nitride；Hydrochloric acid first by 0.5mol/L cleans the presoma 3 times of thin layer boron nitride, then
Clean the presoma 5 times of thin layer boron nitride, the presoma of the thin layer boron nitride after being cleaned using deionized water；
Step one 1. described in concentrated acid be 98% for mass fraction concentrated sulphuric acid；
Step one 1. described in oxide be potassium permanganate；
2., the presoma of the thin layer boron nitride after cleaning is vacuum dried 12h at temperature is 80 DEG C, obtains 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 12h ultrasonic under 300W, obtain the precursor solution of thin layer boron nitride；Under centrifugal speed is for 3000r/min, thin layer is nitrogenized
The precursor solution centrifugation 5min of boron, then take upper strata centrifugal liquid, obtain superthin layer nitridation B solution；By superthin layer boron nitride
Solution carries out vacuum filtration, then the solid matter obtaining after sucking filtration is vacuum dried 12h at temperature is 80 DEG C, obtains superthin layer
Boron nitride powder；
Step one 2. described in the quality of presoma of dried thin layer boron nitride with the volume ratio of organic solvent be
1g:100mL；
Step one 2. described in organic solvent be dimethyl acetylamide；
2nd, prepare the thick polyamic acid solution containing superthin layer boron nitride and aluminium nitride：
1., by step one 2. in the superthin layer boron nitride powder that obtains be dissolved in organic solvent, then low whipping speed is
Stir 20min under 200r/min, then be 20min ultrasonic under 200W in ultrasonic power, add alumina powder, then in ultrasonic work(
Rate is ultrasonic 30min under 200W, obtains the solution containing superthin layer boron nitride and aluminium nitride；
Step 2 1. described in aluminium nitride powder particle diameter be 20nm～50nm；
Step 2 1. described in organic solvent be N-Methyl pyrrolidone；
The mass fraction of superthin layer boron nitride in the 1. described solution containing superthin layer boron nitride and aluminium nitride of step 2
For 0.5%, the mass fraction of aluminium nitride is 0.5%；
2., diamidogen is added in the solution containing superthin layer boron nitride and aluminium nitride, then under ultrasonic power is for 300W
Supersound process 2h, then the condition for 100r/min divides 4 addition dianhydrides in ice-water bath and mixing speed, then low whipping speed is
Stir 12h under 200r/min, then be placed in the vacuum drying oven of room temperature standing 4h, obtain thick containing superthin layer boron nitride and
The polyamic acid solution of aluminium nitride；
Step 2 2. described in diamidogen be 4,4 '-diaminodiphenyl ether；
Step 2 2. described in dianhydride be pyromellitic acid anhydride；
3rd, prepare laminated film：
1., the thick polyamic acid solution containing superthin layer boron nitride and aluminium nitride prepared by step 2 is cast, revolves
Apply or plastic film mulch is dried 12h on clean glass plate, then by glass plate at 80 DEG C, 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 at 350 DEG C be incubated
2h, then naturally cool to room temperature, the last demoulding, obtains boron nitride and the high dielectric polyimide of high heat conduction of aluminium nitride codope is multiple
Close thin 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 difference from embodiment one for the present embodiment is：Step 2 1. described containing 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 all identical with embodiment one.
Embodiment three：The difference from embodiment one for the present embodiment is：Step 2 1. described containing 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 all identical with embodiment one.
Example IV：The difference from embodiment one for the present embodiment is：Step 2 1. described containing 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 all identical with embodiment one.
Embodiment five：The difference from embodiment one for the present embodiment is：Step 2 1. described containing 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 all identical with embodiment one.
Comparative example：The difference from embodiment one for the present embodiment is：Step 2 1. described containing superthin layer nitridation
In the solution of boron and aluminium nitride, the mass fraction of superthin layer boron nitride is 0%, and the mass fraction of aluminium nitride is 0%.Other steps
And parameter is all identical with embodiment one.
Fig. 1 is the boron nitride of embodiment one preparation and the high heat conduction high dielectric polyimide laminated film of aluminium nitride codope
SEM figure；
From fig. 1, it can be seen that the boron nitride prepare in embodiment one of the boron nitride of stratiform and spherical aluminium nitride and aluminium nitride are total to
It is evenly distributed in the high heat conduction high dielectric polyimide laminated film of doping, and polyimide matrix produces and has certain crystallization spy
Property cluster body, this is dispersed can to realize lifting composite property.
Fig. 2 is the boron nitride of embodiment one preparation and the high heat conduction high dielectric polyimide laminated film of aluminium nitride codope
B element mapping；
Fig. 3 is the boron nitride of embodiment one preparation and the high heat conduction high dielectric polyimide laminated film of aluminium nitride codope
Al Element area profile；
Fig. 4 is the boron nitride of embodiment one preparation and the high heat conduction high dielectric polyimide laminated film of aluminium nitride codope
N element mapping；
Fig. 5 is the boron nitride of embodiment one preparation and the high heat conduction high dielectric polyimide laminated film of aluminium nitride codope
C element mapping；
Knowable to Fig. 2～Fig. 5, the high heat conduction high insulation polyamides of the boron nitride of embodiment one preparation and aluminium nitride codope is sub-
In amine laminated film, B, Al, N, C element are evenly distributed, and prove that layered nitride boron and spherical aluminium nitride have been carried out and gather first
Imido be successfully combined, secondly prove that the two is uniformly distributed in the base.
Fig. 6 is the boron nitride of embodiment one preparation and the high heat conduction high dielectric polyimide laminated film of aluminium nitride codope
Thermal property figure, the heat conductivity of the Kapton that A is prepared for comparative example in Fig. 6, B be embodiment one preparation
The heat conductivity of the high heat conduction high dielectric polyimide laminated film of boron nitride and aluminium nitride codope, C is prepared for embodiment two
Boron nitride and aluminium nitride codope high heat conduction high dielectric polyimide laminated film heat conductivity, D makes for embodiment three
The heat conductivity of the high heat conduction high dielectric polyimide laminated film of standby boron nitride and aluminium nitride codope, E is example IV
The heat conductivity of the high heat conduction high dielectric polyimide laminated film of the boron nitride of preparation and aluminium nitride codope, F is embodiment
The heat conductivity of the high heat conduction high dielectric polyimide laminated film of the boron nitride of five preparations and aluminium nitride codope；
As can be seen from Figure 6, in doping stratiform boron nitride and spherical aluminium nitride, prepared boron nitride and the nitridation of proper ratio
The heat conductivity of the high heat conduction high dielectric polyimide laminated film of aluminum codope is greatly enhanced.Heat conductivity improves
68%～330%.
Fig. 7 is the boron nitride of embodiment one preparation and the high heat conduction high dielectric polyimide laminated film of aluminium nitride codope
Mechanical property figure；The tensile strength of the Kapton that A is prepared for comparative example in Fig. 7, B is embodiment one preparation
The tensile strength of the high heat conduction high dielectric polyimide laminated film of boron nitride and aluminium nitride codope, C is prepared for embodiment two
Boron nitride and aluminium nitride codope high heat conduction high dielectric polyimide laminated film tensile strength, D makes for embodiment three
The tensile strength of the high heat conduction high dielectric polyimide laminated film of standby boron nitride and aluminium nitride codope, E is example IV
The tensile strength of the high heat conduction high dielectric polyimide laminated film of the boron nitride of preparation and aluminium nitride codope, F is embodiment
The tensile strength of the high heat conduction high dielectric polyimide laminated film of the boron nitride of five preparations and aluminium nitride codope；
As can be seen from Figure 7, in stratiform doping boron nitride and the spherical aluminium nitride of proper ratio, prepared boron nitride and nitrogen
Change the getable reinforcement of mechanical property of the high heat conduction high dielectric polyimide laminated film of aluminum codope, tensile strength improves
1%～31%.
Fig. 8 is the boron nitride of embodiment one preparation and the high heat conduction high dielectric polyimide laminated film of aluminium nitride codope
Resistivity properties block diagram；In Fig. 8, A is the boron nitride of embodiment one preparation and the high insulation of high heat conduction of aluminium nitride codope gathers
The volume resistance of acid imide laminated film, B is the boron nitride of embodiment two preparation and the high insulation of high heat conduction of aluminium nitride codope
The volume resistance of polyimide composite film, C is the boron nitride of embodiment three preparation and the high heat conduction of aluminium nitride codope is high absolutely
The volume resistance of edge polyimide composite film, the boron nitride that D is prepared for example IV and the high heat conduction of aluminium nitride codope are high
The volume resistance of dielectric polyimide laminated film, E is the boron nitride of embodiment five preparation and the high heat conduction of aluminium nitride codope
The volume resistance of high dielectric polyimide laminated film；
As it can be observed in the picture that in stratiform doping boron nitride and the spherical aluminium nitride of proper ratio, prepared boron nitride and nitrogen
The insulation resistance changing the high heat conduction high dielectric polyimide laminated film of aluminum codope increases substantially, and insulation resistance improves
0.8 times～4.1 times.
Fig. 9 is the boron nitride of embodiment one preparation and the high heat conduction high dielectric polyimide laminated film of aluminium nitride codope
Inverter fed motor life-span block diagram, in Fig. 9 A be the boron nitride of embodiment one preparation and aluminium nitride codope the high insulation of high heat conduction poly-
The Inverter fed motor time of acid imide laminated film, B is the boron nitride of embodiment two preparation and the high heat conduction of aluminium nitride codope is high absolutely
The Inverter fed motor time of edge polyimide composite film, C is the boron nitride of embodiment three preparation and the high heat conduction of aluminium nitride codope
The Inverter fed motor time of high dielectric polyimide laminated film, boron nitride and the height of aluminium nitride codope that D is prepared for example IV
The Inverter fed motor time of heat conduction high dielectric polyimide laminated film, E is boron nitride and the aluminium nitride codope of embodiment five preparation
High heat conduction high dielectric polyimide laminated film the Inverter fed motor time.
As can be seen from Figure 9, the boron nitride of embodiment one preparation and the high dielectric polyimide of high heat conduction of aluminium nitride codope are multiple
The Inverter fed motor life-span closing thin film has obtained substantial lifting, and Inverter fed motor life-span improves 8.1 times～36.1 times.
Claims (10)
1. the preparation method of the high heat conduction of a kind of boron nitride and aluminium nitride codope high dielectric polyimide laminated film, its feature
It is that the method completes according to the following steps：
First, prepare ultrathin boron nitride powder：
1., boron nitride powder and oxide are added in concentrated acid, then are 100r/min～300r/ in ice-water bath and mixing speed
Stirring reaction 60min～120min under min, obtains mixture A；Mixture A is heated to 50 DEG C, then is 50 DEG C and stir in temperature
Mixing speed is stirring reaction 60min～180min under 100r/min～300r/min, is cooled to room temperature, then in mixture A
The hydrogen peroxide solution that mass fraction is 30% is instilled with the rate of addition of 1mL/min, obtains mixture B；Under ice-water bath, to mixed
Add deionized water in compound B, obtain mixture C；Again by mixture C under centrifugal speed 6000r/min～8000r/min from
The heart separates 5min～15min, removes centrifugal liquid, obtains the presoma of thin layer boron nitride；Hydrochloric acid first by 0.5mol/L is clear
Wash the presoma 3 times of thin layer boron nitride, reuse the presoma 5 times～8 times that deionized water cleans thin layer boron nitride, cleaned
The presoma of thin layer boron nitride afterwards；
Step one 1. described in concentrated acid for mass fraction be 98% concentrated sulphuric acid or mixed acid；Described mixed acid divides for quality
The concentrated sulphuric acid for 98% for the number, mass fraction are 85% phosphoric acid and the mixed liquor of nitric acid that mass fraction is 98%；Described is mixed
Close the concentrated sulphuric acid that mass fraction in acid is 98%, mass fraction is 85% phosphoric acid and the volume of nitric acid that mass fraction is 98%
Than for 1:1:5；
Step one 1. described in the volume ratio of the quality of boron nitride powder and concentrated acid be (4g～8g):400mL；
Step one 1. described in the volume ratio of the quality of oxide and concentrated acid be (20g～40g):400mL；
Step one 1. described in concentrated acid and mass fraction be 30% volume ratio of hydrogen peroxide solution be 400:(5～10)；
Step one 1. described in the volume ratio of concentrated acid and deionized water be 400:(300～400)；
2., the presoma of the thin layer boron nitride after cleaning is vacuum dried 12h～24h at temperature is 80 DEG C～100 DEG C, obtains
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 ultrasonic 12h～24h under 100W～500W, obtains the precursor solution of thin layer boron nitride；In centrifugal speed it is
Precursor solution centrifugation 5min～10min to thin layer boron nitride under 3000r/min, then take upper strata centrifugal liquid, surpassed
Thin layer nitrogenizes B solution；Superthin layer nitridation B solution is carried out vacuum filtration, then by the solid matter obtaining after sucking filtration in temperature
For being vacuum dried 12h～24h at 80 DEG C～100 DEG C, obtain superthin layer boron nitride powder；
Step one 2. described in the quality of presoma of dried thin layer boron nitride and organic solvent volume ratio be (1g～
3g):100mL；
2nd, prepare the thick polyamic acid solution containing superthin layer boron nitride and aluminium nitride：
1., by step one 2. in the superthin layer boron nitride powder that obtains be dissolved in organic solvent, then low whipping speed is 100r/
Stir 10min～30min under min～300r/min, then be 10min～30min ultrasonic under 100W～300W in ultrasonic power, then
Add aluminium nitride powder, then be 20min～40min ultrasonic under 100W～300W in ultrasonic power, obtain nitrogenizing containing superthin layer
Boron and the solution of aluminium nitride；
In the 1. described solution containing superthin layer boron nitride and aluminium nitride of step 2, the mass fraction of superthin layer boron nitride is
0.5%～7.5%, the mass fraction of aluminium nitride is 0.5%～7.5%；
2., diamidogen is added in the solution containing superthin layer boron nitride and aluminium nitride, then is ultrasonic under 300W in ultrasonic power
Process 2h～4h, then the condition for 100r/min divides 4 times～5 times addition dianhydrides in ice-water bath and mixing speed, then in stirring speed
Spend for stirring 12h～24h under 100r/min～300r/min, then be placed in the vacuum drying oven of room temperature standing 2h～6h, obtain
The thick polyamic acid solution containing superthin layer boron nitride and aluminium nitride；
3rd, prepare laminated film：
1., by step 2 prepare thick containing superthin layer boron nitride and aluminium nitride polyamic acid solution curtain coating, spin coating or
Plastic film mulch is dried 12h～24h on clean glass plate, then by glass plate at 80 DEG C, obtains 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 naturally cool to room temperature, the last demoulding, obtain the high insulation of high heat conduction of boron nitride and aluminium nitride codope
Polyimide composite film.
2. the high heat conduction high dielectric polyimide THIN COMPOSITE 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 N-Methyl pyrrolidone or N- dimethyl formyl
Amine.
3. the high heat conduction high dielectric polyimide THIN COMPOSITE 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 diamidogen be 4，4′-diaminodipohenyl ether.
4. the high heat conduction high dielectric polyimide THIN COMPOSITE 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；Described connection
Benzene-type dianhydride is 3,3', 4,4'- biphenyl tetracarboxylic dianhydride；Described equal benzene-type dianhydride is pyromellitic acid anhydride.
5. the high heat conduction high dielectric polyimide THIN COMPOSITE 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 heat conduction high dielectric polyimide THIN COMPOSITE 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 high heat conduction high insulation polyamides
The thickness of imines laminated film is 30 μm～50 μm.
7. the high heat conduction high dielectric polyimide THIN COMPOSITE 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 one 1. described in oxide be potassium permanganate or potassium ferrate.
8. the high heat conduction high dielectric polyimide THIN COMPOSITE 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 one 2. described in organic solvent be N-Methyl pyrrolidone, dimethylformamide
Or dimethyl acetylamide.
9. the high heat conduction high dielectric polyimide THIN COMPOSITE of a kind of boron nitride according to claim 1 and aluminium nitride codope
The preparation method of film is it is characterised in that superthin layer nitrogen in the 1. described solution containing superthin layer boron nitride and aluminium nitride of step 2
The mass fraction changing boron is 0.5%～1.5%, and the mass fraction of aluminium nitride is 0.5%～1.5%.
10. the high dielectric polyimide of high heat conduction of a kind of boron nitride according to claim 1 and aluminium nitride codope is combined
The preparation method of thin film is it is characterised in that superthin layer in the 1. described solution containing superthin layer boron nitride and aluminium nitride of step 2
The mass fraction of boron nitride is 1.5%～7.5%, and the mass fraction of aluminium nitride is 1.5%～7.5%.
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