CN108485514A - A kind of polymer matrix composite and preparation method thereof for capacitor - Google Patents
A kind of polymer matrix composite and preparation method thereof for capacitor Download PDFInfo
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
- C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C09D179/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C09D181/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur, with or without nitrogen, oxygen, or carbon only; Coating compositions based on polysulfones; Coating compositions based on derivatives of such polymers
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
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- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The polymer matrix composite and preparation method thereof that the present invention provides a kind of for capacitor, the composite material parts by weights meter are composed of the following components：60 parts~70 parts of polymeric matrix；20 parts~30 parts of the tin titanium oxide nanofiber of dopamine cladding；5 parts~10 parts of auxiliary agent；Wherein, auxiliary agent is the mixture of aminopropyl silane triol and vinyltrimethoxysilane, and the two mass ratio is (3~8):1.Polymer matrix composite of the present invention coordinates the nanofiber with nucleocapsid, can make polymer matrix composite while having both high-termal conductivity, high-k and low-dielectric loss, have good painting film uniformity by adding auxiliary agent.
Description
Technical field
Technical field of electronic components of the present invention is related to a kind of polymer matrix composite for capacitor and its preparation
Method.
Background technology
Buried capacitor printed circuit board is one kind of integrated original paper plate, by one, U.S. PCB companies Zycon in 1992
It is proposed (Buried Capacitor) at first.But at that time since SMT capacitances price, performance etc. can adapt to integrate
The development of circuit technology, Embedded capacitance long period do not obtain the special attention of PCB industries.The progress of electronic technology, PCB
Densification had quickly previously developed, buried capacitor can preferentially improve printed circuit board interconnection density and improve performance, at
For an importance of HDI plates of new generation development.For making the dielectric substance of buried capacitors, it is needed to have
There is low processing temperature to match with the manufacture craft with pcb board, at the same need dielectric substance have high dielectric constant (with
Reduce usable floor area, be conducive to device miniaturization), low dielectric loss (reduce energy loss and reduce generate heat) and high thermal conductivity
(heat dissipation).
The method of the common dielectric substance for preparing buried capacitors is to prepare height using the method for Material cladding at present
Dielectric constant polymer based composites.Ceramic/polymer composite (such as barium titanate/epoxy resin) and conductive filler/poly-
It is two major classes high dielectric constant polymer base composite wood most studied in recent years to close object (such as silver/polyimides) composite material
Material, but they are often difficult to take into account three high-k, high-termal conductivity and low-loss performances.
CN 104893187A disclose a kind of high energy storage density and the polymer composite film and preparation method thereof of efficiency,
The laminated film is made of the nanofiber of Kynoar matrix and the nucleocapsid being dispersed in Kynoar matrix；Core
The stratum nucleare of the nanofiber of shell structure is ceramic fibre, shell coated with silica layer.But due to the dielectric constant of ceramic fibre
High but thermal conductivity is low, and then the thermal conductivity for resulting in the polyalcohol group compound film being prepared is also low.
For conductive filler/polymer (such as silver/polyimides) composite material, common metal filler such as copper powder, silver powder and
Nickel powder has the thermal conductivity that high-termal conductivity can improve polymeric matrix, and due to seep effect, metal/polymer composite wood
Material also shows very high dielectric constant when tenor approaches and is no more than percolation threshold, but the high conductivity of metal makes gold
The dielectric loss of category/polymer composites is very big.In addition, some insulating properties high heat conduction filler such as aluminium nitride and alumina powder
End, although its thermal conductivity is high, dielectric loss is small, dielectric constant is also low, causes aluminium nitride/polymer and aluminium oxide/polymer
Composite material dielectric constant is relatively low.Meanwhile the film of aluminium nitride/polymer and aluminium oxide/polymer composites etc. is uniform
Property is also to be improved.
Therefore, there is an urgent need for developing one kind having both high-termal conductivity, high-k and low-dielectric loss, and it is equal with good film
The polymer matrix of even property is the demand of industry development.
Invention content
It is normal for high-termal conductivity, high dielectric can not be had both existing for the existing polymer matrix composite for capacitor
Number and low-dielectric loss, and the problems such as film lack of homogeneity, the present invention provides a kind of polymer matrix for capacitor is compound
Material and preparation method thereof.Polymer matrix composite of the present invention coordinates receiving with nucleocapsid by adding auxiliary agent
Rice fiber, can make polymer matrix composite while having both high-termal conductivity, high-k and low-dielectric loss, have
Good painting film uniformity.
For this purpose, the present invention uses following technical scheme：
In a first aspect, the present invention provides a kind of polymer matrix composite for capacitor, the composite material is pressed
Weight point meter is composed of the following components：
60 parts~70 parts of polymeric matrix；
20 parts~30 parts of the tin titanium oxide nanofiber of dopamine cladding；
5 parts~10 parts of auxiliary agent；
Wherein, auxiliary agent is the mixture of aminopropyl silane triol and vinyltrimethoxysilane, and the two mass ratio is
(3~8):1, such as 3:1、4:1、5:1、6:1 or 8:1 etc., it is not limited to cited numerical value, in the numberical range other
Unrequited numerical value is equally applicable.
The parts by weight of the polymeric matrix can be 60 parts, 62 parts, 64 parts, 66 parts, 68 parts or 70 parts etc., but simultaneously not only limit
It is equally applicable in other unrequited numerical value in cited numerical value, the numberical range；The tin titanyl of the dopamine cladding
The parts by weight of object nanofiber can be 20 parts, 22 parts, 24 parts, 26 parts, 28 parts or 30 parts etc., it is not limited to cited number
Value, other interior unrequited numerical value of the numberical range are equally applicable；The parts by weight of the auxiliary agent can be 5 parts, 6 parts, 7 parts, 8 parts, 9
Part or 10 parts etc., it is not limited to cited numerical value, other unrequited numerical value are equally applicable in the numberical range.
In the present invention, the auxiliary agent is with the quality of aminopropyl silane triol and the mixture of vinyltrimethoxysilane
Than for (3~8):1 effect that reaches is preferable, and with mass ratio for (3~5):Effect is optimal when 1.The auxiliary agent and dopamine packet
The tin titanium oxide nanofiber interaction covered, improves the compatibility of tin titanium oxide nanofiber and polymeric matrix,
And tin titanium oxide nanofiber contributes to the further promotion of the comprehensive performance of material.
It is used as currently preferred technical solution below, but not as the limitation of technical solution provided by the invention, passes through
Following technical scheme can preferably reach and realize the technical purpose and advantageous effect of the present invention.
As currently preferred technical solution, the composite material parts by weights meter is composed of the following components：
63 parts~66 parts of polymeric matrix；
25 parts~28 parts of the tin titanium oxide nanofiber of dopamine cladding；
6 parts~8 parts of auxiliary agent.
Preferably, the composite material parts by weights meter is composed of the following components：
65 parts of polymeric matrix；
27 parts of the tin titanium oxide nanofiber of dopamine cladding；
8 parts of auxiliary agent.
As currently preferred technical solution, aminopropyl silane triol and vinyl trimethoxy silicon in the auxiliary agent
The mass ratio of alkane is (3~5):1.
Preferably, the composite material parts by weights meter is composed of the following components：
65 parts of polymeric matrix；
27 parts of the tin titanium oxide nanofiber of dopamine cladding；
8 parts of auxiliary agent；
Wherein, the mass ratio of aminopropyl silane triol and vinyltrimethoxysilane is (3~5) in the auxiliary agent:
1。
As currently preferred technical solution, the polymeric matrix is polyimides and/or polyether sulfone.
As currently preferred technical solution, the described method comprises the following steps：
(1) the tin titanium oxide nanofiber of the dopamine of formula ratio cladding and auxiliary agent are placed in organic solvent, ultrasound
Dispersion, forms stable suspension；
(2) polymeric matrix of formula ratio is added into step (1) described suspension and stirs and is completely dissolved to it, obtains
Mixed solution；
(3) mixed solution described in step (2) is poured and is cast from substrate and after natural levelling, then through evaporating solvent, Re Chu
Reason and cooling obtain polymer matrix composite.
As currently preferred technical solution, the tin titanium oxide nanofiber of step (1) the dopamine cladding
Preparation method includes the following steps：
(a) precursor solution of polymer precursor, the precursor solution of tin and titanium is uniformly mixed, obtains electrostatic spinning
Solution；
(b) electrostatic spinning solution for obtaining step (a) carries out electrostatic spinning, obtains polymer nanofibre film；
(c) polymer nanofibre film that step (b) obtains is heat-treated, obtains tin titanium oxide nanofiber；
(d) the tin titanium oxide nanofiber dispersion for obtaining step (c) is in Tris-HCl buffer solutions, through ultrasonic disperse
Afterwards, dopamine is added, 10h~12h is stirred at 30 DEG C~40 DEG C, through being filtered, washed and dried drying, obtains dopamine cladding
Tin titanium oxide nanofiber, wherein whipping temp can be 30 DEG C, 32 DEG C, 34 DEG C, 36 DEG C, 38 DEG C or 40 DEG C etc., but simultaneously not only
It is limited to cited numerical value, other unrequited numerical value are equally applicable in the numberical range；The mixing time can be 10h,
10.5h, 11h, 11.5h or 12h etc., it is not limited to cited numerical value, other interior unrequited numerical value of the numberical range
It is equally applicable.
In the present invention, the electrospinning process is conventional method in this field, is repeated no more to its operating parameter etc..
As currently preferred technical solution, step (a) polymer precursor is polyimides.
Preferably, the presoma of step (a) tin is butter of tin and/or stannous chloride.
Preferably, solvent is absolute ethyl alcohol in the precursor solution of step (a) tin.
Preferably, the presoma of step (a) titanium is butyl titanate.
Preferably, solvent is absolute ethyl alcohol in the precursor solution of step (a) titanium.
Preferably, in step (a) electrostatic spinning solution polymer a concentration of 0.5g/mL~0.8g/L, such as
0.5g/mL, 0.6g/mL, 0.7g/mL or 0.8g/mL etc., it is not limited to cited numerical value, in the numberical range other
Unrequited numerical value is equally applicable；A concentration of 1mol/mL~1.5mol/mL of the presoma of tin, such as 1mol/mL, 1.1mol/
ML, 1.2mol/mL, 1.3mol/mL, 1.4mol/mL or 1.5mol/mL etc., it is not limited to cited numerical value, the numerical value
Other unrequited numerical value are equally applicable in range；A concentration of 0.5mol/mL~1mol/mL of the presoma of titanium, such as
0.5mol/mL, 0.6mol/mL, 0.7mol/mL, 0.8mol/mL, 0.9mol/mL or 1mol/mL etc., it is not limited to listed
The numerical value of act, other interior unrequited numerical value of the numberical range are equally applicable.
As currently preferred technical solution, heat treatment described in step (c) carries out in air atmosphere.
Preferably, the temperature being heat-treated described in step (c) be 300 DEG C~400 DEG C, such as 300 DEG C, 320 DEG C, 340 DEG C,
360 DEG C, 380 DEG C or 400 DEG C etc., it is not limited to cited numerical value, other interior unrequited numerical value of the numberical range are same
Sample is applicable in.
Preferably, the time being heat-treated described in step (c) be 2h~4h, such as 2h, 2.5h, 3h, 3.5h or 4h etc., but
It is not limited in cited numerical value, other unrequited numerical value are equally applicable in the numberical range.
Preferably, in step (d) in Tris-HCl buffer solutions tin titanium oxide nanofiber a concentration of 4mg/mL~
5mg/mL, such as 4mg/mL, 4.2mg/mL, 4.4mg/mL, 4.6mg/mL, 4.8mg/mL or 5mg/mL etc., it is not limited to
Cited numerical value, other interior unrequited numerical value of the numberical range are equally applicable；A concentration of 6mg/mL~8mg/ of dopamine
ML, such as 6mg/mL, 6.5mg/mL, 7mg/mL, 7.5mg/mL or 8mg/mL etc., it is not limited to cited numerical value, it should
Other unrequited numerical value are equally applicable in numberical range.
Preferably, drying temperature is 60 DEG C~80 DEG C in step (d), such as 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C or 80 DEG C etc.,
It is not limited to cited numerical value, other interior unrequited numerical value of the numberical range are equally applicable.
As currently preferred technical solution, the organic solvent described in step (1) is n,N-Dimethylformamide.
Preferably, in step (1) ultrasonic disperse time be 30min~50min, such as 30min, 35min, 40min,
45min or 50min etc., it is not limited to cited numerical value, other interior unrequited numerical value of the numberical range are equally applicable.
As currently preferred technical solution, the evaporation solvent is：3h~4h is dried in vacuo at 60 DEG C~70 DEG C,
Wherein drying temperature can be 60 DEG C, 62 DEG C, 64 DEG C, 66 DEG C, 68 DEG C or 70 DEG C etc., it is not limited to cited numerical value, it should
Other unrequited numerical value are equally applicable in numberical range；Drying time can be 3h, 3.2h, 3.4h, 3.6h, 3.8h or 4h etc.,
It is not limited to cited numerical value, other interior unrequited numerical value of the numberical range are equally applicable.
Preferably, described be heat-treated is：At 80 DEG C~100 DEG C heat 1h~2h, wherein heating temperature can be 80 DEG C, 83
DEG C, 85 DEG C, 87 DEG C, 90 DEG C, 93 DEG C, 95 DEG C, 97 DEG C or 100 DEG C etc., it is not limited to cited numerical value, the numberical range
Other interior unrequited numerical value are equally applicable；Heating time can be 1h, 1.3h, 1.5h, 1.7h or 2h etc., it is not limited to
Cited numerical value, other interior unrequited numerical value of the numberical range are equally applicable.
In the present invention, the temperature of heat treatment is unsuitable excessively high, and the tin titanium oxide nanofiber to prevent dopamine cladding occurs
Carbonization.
Compared with prior art, the invention has the advantages that：
The tin titanium oxide coated in polymer matrix composite of the present invention by adding auxiliary agent and dopamine
Nanofiber is interacted using the tin titanium oxide nanofiber of auxiliary agent and dopamine cladding, improves Xi Taiyanghuawuna
The compatibility of rice fiber and polymeric matrix, and tin titanium oxide nanofiber contributes to the further of the comprehensive performance of material
It is promoted, the thermal conductivity of polymer matrix composite at room temperature is allow to reach 2.2W/mK, the dielectric constant under room temperature 1kHz
50 or so can be reached, dielectric loss is only 0.005, and has good painting film uniformity.
Specific implementation mode
For the present invention is better described, it is easy to understand technical scheme of the present invention, below further specifically to the present invention
It is bright.But following embodiments is only the simple example of the present invention, does not represent or limit the scope of the present invention, this
Invention protection domain is subject to claims.
Specific embodiment of the invention part provides a kind of polymer matrix composite for capacitor and its preparation
Method, the composite material parts by weights meter are composed of the following components：
60 parts~70 parts of polymeric matrix；
20 parts~30 parts of the tin titanium oxide nanofiber of dopamine cladding；
5 parts~10 parts of auxiliary agent；
Wherein, auxiliary agent is the mixture of aminopropyl silane triol and vinyltrimethoxysilane, and the two mass ratio is
(3~8):1.
The preparation method of the polymer matrix composite includes the following steps：
(1) the tin titanium oxide nanofiber of the dopamine of formula ratio cladding and auxiliary agent are placed in organic solvent, ultrasound
Dispersion, forms stable suspension；
(2) polymeric matrix of formula ratio is added into step (1) described suspension and stirs and is completely dissolved to it, obtains
Mixed solution；
(3) mixed solution described in step (2) is poured and is cast from substrate and after natural levelling, then through evaporating solvent, Re Chu
Reason and cooling obtain polymer matrix composite.
Wherein, the preparation method of the tin titanium oxide nanofiber of dopamine cladding includes the following steps：
(a) precursor solution of polymer precursor, the precursor solution of tin and titanium is uniformly mixed, obtains electrostatic spinning
Solution；
(b) electrostatic spinning solution for obtaining step (a) carries out electrostatic spinning, obtains polymer nanofibre film；
(c) polymer nanofibre film that step (b) obtains is heat-treated, obtains tin titanium oxide nanofiber；
(d) the tin titanium oxide nanofiber dispersion for obtaining step (c) is in Tris-HCl buffer solutions, through ultrasonic disperse
Afterwards, dopamine is added, 10h~12h is stirred at 30 DEG C~40 DEG C, through being filtered, washed and dried drying, obtains dopamine cladding
Tin titanium oxide nanofiber.
It is present invention typical case but non-limiting embodiment below：
Embodiment 1：
Present embodiments provide a kind of preparation method of the tin titanium oxide nanofiber of dopamine cladding, including following step
Suddenly：
(a) by the anhydrous second of polymer precursor polyimides, the ethanol solution of butter of tin and butyl titanate
Alcoholic solution is uniformly mixed, and obtains electrostatic spinning solution, a concentration of 0.6g/mL of polymer, the concentration of butter of tin in the solution
For 1.3mol/mL, a concentration of 0.7mol/mL of butyl titanate；
(b) electrostatic spinning solution for obtaining step (a) carries out electrostatic spinning, obtains polymer nanofibre film；
(c) it carries out the polymer nanofibre film that step (b) obtains to carry out heat treatment 3h at 340 DEG C~360 DEG C, obtain
To tin titanium oxide nanofiber；
(d) the tin titanium oxide nanofiber dispersion for obtaining step (c) is in Tris-HCl buffer solutions, through ultrasonic disperse
Afterwards, dopamine is added, a concentration of 4.6mg/mL of tin titanium oxide nanofiber in solution, a concentration of 7mg/ of dopamine are made
ML stirs 10h~12h at 30 DEG C~40 DEG C, through being filtered, washed and dried drying, obtains the Xi Taiyanghuawuna of dopamine cladding
Rice fiber.
Embodiment 2：
Present embodiments provide a kind of preparation method of the tin titanium oxide nanofiber of dopamine cladding, the method ginseng
According to the step in embodiment 1, differ only in：
A concentration of 0.52g/mL of polymer in step (a) solution, a concentration of 1.1mol/mL of butter of tin, metatitanic acid four
A concentration of 0.53mol/mL of butyl ester；
The heat treatment temperature of step (c) is 300 DEG C~320 DEG C, time 4h；
A concentration of 4.1mg/mL of tin titanium oxide nanofiber in step (d) solution, a concentration of 6.2mg/ of dopamine
mL。
Embodiment 3：
Present embodiments provide a kind of preparation method of the tin titanium oxide nanofiber of dopamine cladding, the method ginseng
According to the step in embodiment 1, differ only in：
A concentration of 0.78g/mL of polymer in step (a) solution, a concentration of 1.5mol/mL of butter of tin, metatitanic acid four
A concentration of 0.98mol/mL of butyl ester；
The heat treatment temperature of step (c) is 380 DEG C~400 DEG C, time 2h；
A concentration of 5mg/mL of tin titanium oxide nanofiber in step (d) solution, a concentration of 7.9mg/mL of dopamine.
Embodiment 4：
Present embodiments provide a kind of polymer matrix composite and preparation method thereof for capacitor, the composite wood
Expect that parts by weights meter is composed of the following components：
65 parts of polymeric matrix；
27 parts of the tin titanium oxide nanofiber of dopamine cladding；
8 parts of auxiliary agent；
Wherein, the mass ratio of aminopropyl silane triol and vinyltrimethoxysilane is 4 in the auxiliary agent:1.
The preparation method of the polymer matrix composite includes the following steps：
(1) by the tin titanium oxide nanofiber and formula ratio of dopamine cladding obtained in the embodiment of formula ratio 1
Auxiliary agent is placed in n,N-Dimethylformamide, and ultrasonic disperse 40min forms stable suspension；
(2) polymeric matrix of formula ratio is added into step (1) described suspension and stirs and is completely dissolved to it, obtains
Mixed solution；
(3) mixed solution described in step (2) is poured and is cast from substrate and after natural levelling, the vacuum at 60 DEG C~70 DEG C
Dry 3h~4h, heating 1h~2h and cooling obtain polymer matrix composite at 90 DEG C.
Embodiment 5：
Present embodiments provide a kind of polymer matrix composite and preparation method thereof for capacitor, the composite wood
Expect that parts by weights meter is composed of the following components：
63 parts of polymeric matrix；
25 parts of the tin titanium oxide nanofiber of dopamine cladding；
6 parts of auxiliary agent；
Wherein, the mass ratio of aminopropyl silane triol and vinyltrimethoxysilane is 3 in the auxiliary agent:1.
The preparation method of the polymer matrix composite is differed only in reference to the preparation method in embodiment 4：
The tin titanium oxide nanofiber that dopamine used in step (1) coats is obtained in embodiment 2, ultrasonic disperse
30min；Step (3) heat treatment temperature is 80 DEG C.
Embodiment 6：
Present embodiments provide a kind of polymer matrix composite and preparation method thereof for capacitor, the composite wood
Expect that parts by weights meter is composed of the following components：
66 parts of polymeric matrix；
28 parts of the tin titanium oxide nanofiber of dopamine cladding；
7 parts of auxiliary agent；
Wherein, the mass ratio of aminopropyl silane triol and vinyltrimethoxysilane is 5 in the auxiliary agent:1.
The preparation method of the polymer matrix composite is differed only in reference to the preparation method in embodiment 4：
The tin titanium oxide nanofiber that dopamine used in step (1) coats is obtained in embodiment 2, ultrasonic disperse
50min；Step (3) heat treatment temperature is 100 DEG C.
Embodiment 7：
Present embodiments provide a kind of polymer matrix composite and preparation method thereof for capacitor, the composite wood
Expect that parts by weights meter is composed of the following components：
61 parts of polymeric matrix；
22 parts of the tin titanium oxide nanofiber of dopamine cladding；
5 parts of auxiliary agent；
Wherein, the mass ratio of aminopropyl silane triol and vinyltrimethoxysilane is 7 in the auxiliary agent:1.
The preparation method of the polymer matrix composite is with reference to the preparation method in embodiment 4.
Embodiment 8：
Present embodiments provide a kind of polymer matrix composite and preparation method thereof for capacitor, the composite wood
Expect that parts by weights meter is composed of the following components：
70 parts of polymeric matrix；
29 parts of the tin titanium oxide nanofiber of dopamine cladding；
9 parts of auxiliary agent；
Wherein, the mass ratio of aminopropyl silane triol and vinyltrimethoxysilane is 8 in the auxiliary agent:1.
The preparation method of the polymer matrix composite is with reference to the preparation method in embodiment 4.
Comparative example 1：
This comparative example provides a kind of polymer matrix composite and preparation method thereof for capacitor, the composite wood
For material other than not adding auxiliary agent, other compositions are in the same manner as in Example 4 with consumption proportion.
Preparation method is with reference to method in embodiment 4.
Comparative example 2：
This comparative example provides a kind of polymer matrix composite and preparation method thereof for capacitor, the composite wood
Expect in addition to the mass ratio of aminopropyl silane triol and vinyltrimethoxysilane is 1 in auxiliary agent:Outside 1, other compositions and use
Amount proportioning is in the same manner as in Example 4.
Preparation method is with reference to method in embodiment 4.
Comparative example 3：
This comparative example provides a kind of polymer matrix composite and preparation method thereof for capacitor, the composite wood
Expect in addition to the mass ratio of aminopropyl silane triol and vinyltrimethoxysilane is 10 in auxiliary agent:Outside 1, other compositions and use
Amount proportioning is in the same manner as in Example 4.
Preparation method is with reference to method in embodiment 4.
Comparative example 4：
This comparative example provides a kind of polymer matrix composite and preparation method thereof for capacitor, the composite wood
Expect other than the tin titanium oxide nanofiber in the tin titanium oxide nanofiber for coating dopamine replaces with ceramic fibre,
Other compositions are in the same manner as in Example 4 with consumption proportion.
The preparation method of ceramic fibre is with reference to the preparation in CN 104893187A in the ceramic fibre of the dopamine cladding
Method coats dopamine after ceramic fibre is prepared using method described herein.
The preparation method of the polymer matrix composite is with reference to method in embodiment 4.
Comparative example 5：
This comparative example provides a kind of polymer matrix composite and preparation method thereof for capacitor, the composite wood
The composition of material and consumption proportion are in the same manner as in Example 4.
Preparation method is differed only in reference to method in embodiment 4：Heat treatment temperature in step (3) is higher, is
300℃。
Polymer matrix composite obtained in embodiment 4-8 and comparative example 1-5 is tested for the property, test result is such as
Described in table 1.
Table 1：The performance test table of embodiment 4-8 and comparative example 1-5
It can be seen that based on the above embodiments with comparative example and pass through addition in polymer matrix composite of the present invention
The tin titanium oxide nanofiber of auxiliary agent and dopamine cladding utilizes the tin titanium oxide Nanowire of auxiliary agent and dopamine cladding
Dimension interaction, improves the compatibility of tin titanium oxide nanofiber and polymeric matrix, and tin titanium oxide Nanowire
Dimension contributes to the further promotion of the comprehensive performance of material, and the thermal conductivity of polymer matrix composite at room temperature is allow to reach
Dielectric constant under 2.2W/mK, room temperature 1kHz can reach 50 or so, and dielectric loss is only 0.005, and with good
Apply film uniformity.
Applicant declares, and the present invention illustrates the detailed applications method of the present invention by above-described embodiment, but the present invention is simultaneously
It is not limited to above-mentioned detailed applications method, that is, does not mean that the present invention has to rely on above-mentioned method detailed and could implement.Affiliated skill
The technical staff in art field is it will be clearly understood that any improvement in the present invention, to the equivalence replacement and auxiliary of products material of the present invention
The addition of ingredient, the selection etc. of concrete operations condition and mode, all fall within protection scope of the present invention and the open scope.
Claims (10)
1. a kind of polymer matrix composite for capacitor, which is characterized in that the composite material parts by weights meter by with
The following group is grouped as：
60 parts~70 parts of polymeric matrix；
20 parts~30 parts of the tin titanium oxide nanofiber of dopamine cladding；
5 parts~10 parts of auxiliary agent；
Wherein, auxiliary agent be aminopropyl silane triol and vinyltrimethoxysilane mixture, the two mass ratio be (3~
8):1。
2. polymer matrix composite according to claim 1, which is characterized in that the composite material parts by weights meter by
Following components forms：
63 parts~66 parts of polymeric matrix；
25 parts~28 parts of the tin titanium oxide nanofiber of dopamine cladding；
6 parts~8 parts of auxiliary agent；
Preferably, the composite material parts by weights meter is composed of the following components：
65 parts of polymeric matrix；
27 parts of the tin titanium oxide nanofiber of dopamine cladding；
8 parts of auxiliary agent.
3. polymer matrix composite according to claim 1 or 2, which is characterized in that aminopropyl silicon in the auxiliary agent
The mass ratio of alkane triol and vinyltrimethoxysilane is (3~5):1；
Preferably, the composite material parts by weights meter is composed of the following components：
65 parts of polymeric matrix；
27 parts of the tin titanium oxide nanofiber of dopamine cladding；
8 parts of auxiliary agent；
Wherein, the mass ratio of aminopropyl silane triol and vinyltrimethoxysilane is (3~5) in the auxiliary agent:1.
4. according to claim 1-3 any one of them polymer matrix composites, which is characterized in that the polymeric matrix is
Polyimides and/or polyether sulfone.
5. a kind of preparation method of polymer matrix composite according to any one of claims 1-4, which is characterized in that described
Method includes the following steps：
(1) the tin titanium oxide nanofiber of the dopamine of formula ratio cladding and auxiliary agent are placed in organic solvent, ultrasonic disperse,
Form stable suspension；
(2) polymeric matrix of formula ratio is added into step (1) described suspension and stirs and is completely dissolved to it, is mixed
Solution；
(3) mixed solution described in step (2) is poured and is cast from substrate and after natural levelling, then through evaporate solvent, heat treatment and
Cooling obtains polymer matrix composite.
6. preparation method according to claim 5, which is characterized in that the tin titanyl of step (1) the dopamine cladding
The preparation method of object nanofiber includes the following steps：
(a) precursor solution of polymer precursor, the precursor solution of tin and titanium is uniformly mixed, it is molten obtains electrostatic spinning
Liquid；
(b) electrostatic spinning solution for obtaining step (a) carries out electrostatic spinning, obtains polymer nanofibre film；
(c) polymer nanofibre film that step (b) obtains is heat-treated, obtains tin titanium oxide nanofiber；
(d) the tin titanium oxide nanofiber dispersion for obtaining step (c) is in Tris-HCl buffer solutions, after ultrasonic disperse,
Dopamine is added, 10h~12h is stirred at 30 DEG C~40 DEG C, through being filtered, washed and dried drying, obtains the tin of dopamine cladding
Titanium oxide nanofiber.
7. preparation method according to claim 6, which is characterized in that step (a) polymer precursor is that polyamides is sub-
Amine；
Preferably, the presoma of step (a) tin is butter of tin and/or stannous chloride；
Preferably, solvent is absolute ethyl alcohol in the precursor solution of step (a) tin；
Preferably, the presoma of step (a) titanium is butyl titanate；
Preferably, solvent is absolute ethyl alcohol in the precursor solution of step (a) titanium；
Preferably, in step (a) electrostatic spinning solution polymer a concentration of 0.5g/mL~0.8g/mL, the presoma of tin
A concentration of 1mol/mL~1.5mol/mL, a concentration of 0.5mol/mL~1mol/mL of the presoma of titanium.
8. the preparation method described according to claim 6 or 7, which is characterized in that heat treatment is in air atmosphere described in step (c)
Middle progress；
Preferably, the temperature being heat-treated described in step (c) is 300 DEG C~400 DEG C；
Preferably, the time being heat-treated described in step (c) is 2h~4h；
Preferably, in step (d) in Tris-HCl buffer solutions tin titanium oxide nanofiber a concentration of 4mg/mL~5mg/mL,
A concentration of 6mg/mL~8mg/mL of dopamine；
Preferably, drying temperature is 60 DEG C~80 DEG C in step (d).
9. according to claim 5-8 any one of them preparation methods, which is characterized in that the organic solvent described in step (1)
For N,N-dimethylformamide；
Preferably, the time of ultrasonic disperse is 30min~50min in step (1).
10. according to claim 5-9 any one of them preparation methods, which is characterized in that the evaporation solvent is：60 DEG C~
3h~4h is dried in vacuo at 70 DEG C；
Preferably, described be heat-treated is：1h~2h is heated at 80 DEG C~100 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115029049A (en) * | 2022-07-19 | 2022-09-09 | 宁波科鑫腐蚀控制工程有限公司 | Epoxy composite coating containing dopamine modified fiber and preparation method and construction process thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004011672A1 (en) * | 2002-07-26 | 2004-02-05 | Ntera Limited | Porous nanostructured film sensor |
| US20050189240A1 (en) * | 2004-02-26 | 2005-09-01 | Tamkang University | Method and chemical sensor for determining concentrations of hydrogen peroxide and its precusor in a solution |
| CN102504449A (en) * | 2011-11-01 | 2012-06-20 | 清华大学 | Polymer matrix composite membrane with high energy density and preparation method thereof |
| CN103803490A (en) * | 2014-02-27 | 2014-05-21 | 北京化工大学 | Carbon nanofiber material and preparing method and application of carbon nanofiber material |
| CN104194020A (en) * | 2014-08-03 | 2014-12-10 | 北京化工大学 | Method for preparing flexible inorganic/polymer composite film with high dielectric property |
| CN105295263A (en) * | 2015-11-11 | 2016-02-03 | 同济大学 | Polymer matrix composite and preparation method thereof |
-
2018
- 2018-03-29 CN CN201810285623.6A patent/CN108485514B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004011672A1 (en) * | 2002-07-26 | 2004-02-05 | Ntera Limited | Porous nanostructured film sensor |
| US20050189240A1 (en) * | 2004-02-26 | 2005-09-01 | Tamkang University | Method and chemical sensor for determining concentrations of hydrogen peroxide and its precusor in a solution |
| CN102504449A (en) * | 2011-11-01 | 2012-06-20 | 清华大学 | Polymer matrix composite membrane with high energy density and preparation method thereof |
| CN103803490A (en) * | 2014-02-27 | 2014-05-21 | 北京化工大学 | Carbon nanofiber material and preparing method and application of carbon nanofiber material |
| CN104194020A (en) * | 2014-08-03 | 2014-12-10 | 北京化工大学 | Method for preparing flexible inorganic/polymer composite film with high dielectric property |
| CN105295263A (en) * | 2015-11-11 | 2016-02-03 | 同济大学 | Polymer matrix composite and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115029049A (en) * | 2022-07-19 | 2022-09-09 | 宁波科鑫腐蚀控制工程有限公司 | Epoxy composite coating containing dopamine modified fiber and preparation method and construction process thereof |
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