CN102702652A - High-dielectric constant low-loss metal/polymer composite and preparation method thereof - Google Patents
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Abstract
The invention relates to a high-dielectric constant low-loss metal/polymer composite and a preparation method thereof. According to the invention, self-passivating metal Al powder with average particle size of 800 nm is treated by a silane coupling agent, then uniformly mixed with N, N-dimethylacetamide (DMAC) solution of polyvinylidene fluoride (PVDF) by magnetic stirring and ultrasonic dispersion, coated on clean glass plates to form films, and then dried in vacuum at 80 degrees centigrade for 2 h to remove solvent so as to obtain Al/PVDF composites with thickness of 30-80 microns; wherein dosage of Al is 10-50% of PVDF by volume percent. The Al/PVDF composite provided by the invention has a dielectric constant higher than 58 under a frequency of 1 kHz at room temperature, and a dielectric loss lower than 0.02; the dielectric constant is linearly increased along with increment of Al content, so that the dielectric constant can be randomly regulated within certain range according to the need; at the same time, the dielectric constant is good in temperature and frequency stability.
Description
Technical field
The invention belongs to the dielectric composite preparing technical field, particularly the specific inductivity height, loss is low, combined temp is low, the simple a kind of high-k low-loss metal/polymer composites of preparation technology and preparation method thereof.
Background technology
In the dielectric substance field, single component material often is difficult to satisfy the requirement of hyundai electronics industry to the material over-all properties.For example the ferroelectric ceramic(s) dielectric properties are excellent, and specific inductivity is generally all more than 2000, but need high temperature sintering, and fragility is big; The polymer materials good processability, mold temperature is low, snappiness good, dielectric strength is high, but its specific inductivity is generally lower, generally between 2 ~ 10.For this reason; The scientific worker adopts the material composite methods; Exploitation has the polymer matrix composite of good dielectric properties and processing characteristics concurrently, and this type material can be adapted in organic printed circuit board, make the low temperature moulding technology of buried capacitors, thereby has received extensive concern in recent years.
It is the most popular method that obtains the high-k polymer composites, wherein barium titanate (BaTiO that the high-dielectric-constant ceramics powder is filled in the polymeric matrix
3) powder obtained suitability for industrialized production, because of its great variety of goods, specific inductivity is high and do not contain poisonous lead element becomes the most frequently used ceramic powder.Present BaTiO
3/ epoxy resin and BaTiO
3This type of/polyimide high-k matrix material has obtained practical application in buried capacitors.But work as BaTiO
3Content is 50% when following, and the specific inductivity of this type material is generally all below 50.The BaTiO of patent documentation (CN 101955621 A) report for example
3When/PVDF matrix material was 50% when the ceramic volumetric degree, its specific inductivity was 40.75 under room temperature 1 kHz; (Xu is another for Zhu Baoku, Xie Shuhui, Xu Zhikang, functional materials, 2005,4, the 546-549) BaTiO of preparation for Zhu Baoku etc.
3/ composite polyimide material specific inductivity under identical ceramic content and test condition is merely 35.Although improve BaTiO
3Loading level can further increase the specific inductivity of matrix material, but too high pottery is filled the mechanical property often sharply reduce matrix material, causes the material inefficacy of in use breaking.
Utilizing seep effect conductive filler materials such as filler metal powder, carbon black, carbon nanotube or electrically conductive polyaniline in polymkeric substance is another domestic method of obtaining the high-k polymer composites.When the volume percent content of conductive filler material during near the seepage flow threshold value, the specific inductivity of matrix material increase sharply tens times even several magnitude.(Rao Y such as Rao for example; Wong C P; IEEE Polytronic 2002 Conference, 2002,196-200) flake silver powder with 20 μ m is filled in the epoxy resin; Under room temperature 10 KHz when the specific inductivity of content matrix material when being 10.4 vol.% of silver up to 2000, loss is 0.24; (Dang Z M, Lin Y H, Nan C W, Adv. Mater. such as Dang Zhimin; 2003,15,1625-1629) Ni powder and the PVDF with 5 μ m is compound; The Ni volume(tric)fraction is 0.17 o'clock under room temperature 100 Hz, and the matrix material specific inductivity is 400, and loss is 0.2.But the specific inductivity of this type material and the relation of filler content have very strong non-linear; Have only when conductive filler material content and just can represent high-k during fully near its seepage flow threshold value; And often corresponding higher loss (> 0.1 when obtaining the specific inductivity peak value), thus this type material also can't be practical.At present; High-k polymer composites research field is badly in need of the exploitation specific inductivity and is higher than 50; Loss is lower than 0.1, and the packing volume degree is less than the preparation method and the technology of 50% polymer matrix composite, to satisfy electrical condenser high-capacitance, undersized growth requirement.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, low-loss metal/polymer composite material of a kind of high-k and preparation method thereof is provided.
The preparation method of the low-loss metal/polymer composite material of a kind of high-k of the present invention is characterized in that:
(1) said high-k low-loss polymer matrix material has following material to form: self-passivating metal Al powder and polymeric matrix PVDF; The volume percent content of described Al powder in matrix material is 10 ~ 50%; Said polymeric matrix PVDF content is 50 ~ 90%; Described self-passivation Al powder median size is 800 nm, and it is the Al of 2 ~ 3 nm that there is one deck thickness that oxidation forms in air on the surface
2O
3Zone of oxidation, the Al powder uses after silane coupling agent is handled, and wherein the mass ratio of Al powder and silane coupling agent is 100:1; Described polymeric matrix PVDF fusing point is 167 ℃, and median size is 25 μ m.
(2) surface treatment method of Al powder is: make it in absolute ethyl alcohol, form suspension-s through ultra-sonic dispersion and stirring in the Al powder under the room temperature, add coupling agent (γ-An Bingjisanyiyangjiguiwan) back then and continue to stir 10 ~ 30 minutes; Add deionized water subsequently, at 40 ~ 60 ℃ of following ultra-sonic dispersion and stirred 15 ~ 60 minutes; The spinning powder, use absolute ethanol washing 1 ~ 3 time then after, 60 ~ 120 ℃ of following vacuum-dryings 2 ~ 5 hours, use after naturally cooling to room temperature;
(3) preparation method of Al/PVDF matrix material is: take by weighing the silane coupler modified Al powder that obtains in the step (1); Making its volumn concentration in matrix material is 10 ~ 50%; According to the Al/DMAC weight ratio is 1/10 ~ 1/1 to take by weighing corresponding D MAC, and Al powder ultra-sonic dispersion in DMAC is obtained dispersion liquid a; According to polymeric matrix PVDF volumn concentration is 50% ~ 90% to take by weighing the PVDF powder, is 1/20 ~ 1/4 to take by weighing DMAC according to the PVDF/DMAC weight ratio, and PVDF is dissolved among the DMAC under 50 ℃, obtains solution b behind the cool to room temperature; Then dispersion liquid a and solution b are mixed, after 15 ~ 60 minutes, obtain the mixing suspension of Al and PVDF through ultra-sonic dispersion 10 ~ 30 minutes and magnetic agitation; To mix suspension-s casting film-forming on clean sheet glass,, obtain the Al/PVDF composite material film 80 ℃ of following vacuum-dryings 2 hours.
The present invention has following beneficial effect:
The specific inductivity of this Al/PVDF matrix material increases with the increase of Al content is linear, and when the long-pending degree of Al powder was 50%, up to 58.34, loss was merely 0.019 to the specific inductivity of matrix material under room temperature 1 kHz; The specific inductivity of matrix material can be regulated arbitrarily between 12 ~ 58 through the content that changes Al; The specific inductivity of matrix material has good frequency and temperature stability, guarantees material stable performance in use; Composite material preparation process is simple, and is with low cost.
Description of drawings
Accompanying drawing 1: the transmission electron micrograph of the self-passivation Al powder that the present invention uses;
Accompanying drawing 2: the scanning electron photomicrograph of the Al/PVDF matrix material section of the present invention's preparation, wherein the long-pending degree of Al powder is 50%;
Accompanying drawing 3: the present invention prepares the process flow sheet of Al/PVDF matrix material;
Accompanying drawing 4: under room temperature and test frequency 1 kHz, relation curve between Al/PVDF matrix material specific inductivity and loss and the Al volume(tric)fraction;
Accompanying drawing 5: the Al/PVDF matrix material of different al volume content is relation curve between specific inductivity and the test frequency at room temperature;
Accompanying drawing 6: relation curve between the Al/PVDF matrix material loss at room temperature of different al volume content and the test frequency;
Accompanying drawing 7: the Al/PVDF matrix material of different al volume content under test frequency 1 kHz, relation curve between specific inductivity and the probe temperature;
Accompanying drawing 8: the Al/PVDF matrix material of different al volume content under test frequency 1 kHz, relation curve between loss and the probe temperature.
Embodiment
Below through combining specific embodiment that the present invention is done further detailed description.Embodiment only is to a kind of explanation of the present invention, and is not construed as limiting the invention.Embodiment is the practical application example, is easy to grasp and checking for those skilled in the art.If on basis of the present invention, make certain change, its essence does not exceed scope of the present invention so.
Embodiment 1
(1) makes it in absolute ethyl alcohol, form suspension-s through ultra-sonic dispersion and stirring in 50 g Al powder under the room temperature, add 0.5 g coupling agent (γ-An Bingjisanyiyangjiguiwan) back then and continue to stir 10 ~ 30 minutes; Add deionized water subsequently, at 40 ~ 60 ℃ of following ultra-sonic dispersion and stirred 15 ~ 60 minutes; The spinning powder, use absolute ethanol washing 1 ~ 3 time then after, 60 ~ 120 ℃ of following vacuum-dryings 2 ~ 5 hours, use after naturally cooling to room temperature;
(2) take by weighing silane coupler modified Al powder 0.8333 g that obtains in the step (1); Making its volumn concentration in matrix material is 10%, is 1/1 to take by weighing corresponding D MAC according to the Al/DMAC weight ratio, and Al powder ultra-sonic dispersion in DMAC is obtained dispersion liquid a; According to polymeric matrix PVDF volumn concentration is 90% to take by weighing PVDF powder 4.9166 g, is 1/7 to take by weighing DMAC according to the PVDF/DMAC weight ratio, and PVDF is dissolved among the DMAC under 50 ℃, obtains solution b behind the cool to room temperature; Then dispersion liquid a and solution b are mixed, after 15 ~ 60 minutes, obtain the mixing suspension of Al and PVDF through ultra-sonic dispersion 10 ~ 30 minutes and magnetic agitation; To mix suspension-s casting film-forming on clean sheet glass,, obtain the Al/PVDF composite material film 80 ℃ of following vacuum-dryings 2 hours.
(3) the silane coupler modified transmission electron micrograph of self-passivation Al powder under different amplification seen accompanying drawing 1, Fig. 2 among the embodiment 1-5; The preparation flow figure of matrix material sees accompanying drawing 3 among the embodiment 1-5; The matrix material that step among the embodiment 1-5 (2) obtains becomes the square sample of 2 cm * 2 cm with blade cuts, specimen dielectric properties behind the coated on both sides conductive silver paste, and test result is seen Fig. 4, Fig. 5, Fig. 6, Fig. 7, Fig. 8 respectively; The specific inductivity of Al/PVDF matrix material under room temperature 1 kHz is 12.83, and loss is 0.012; The specific inductivity of matrix material changes very little in 30 ~ 200 kHz test frequency scopes and 20 ~ 150 ℃ of TRs, and loss is less than 0.1, and the overwhelming majority is below 0.05.
Embodiment 2
(1) process of surface treatment of Al powder is with embodiment 1;
(2) take by weighing silane coupler modified Al powder 1.9212 g that obtain in the step (1); Making its volumn concentration in matrix material is 20%, is 1/1 to take by weighing corresponding D MAC according to the Al/DMAC weight ratio, and Al powder ultra-sonic dispersion in DMAC is obtained dispersion liquid a; According to polymeric matrix PVDF volumn concentration is 80% to take by weighing PVDF powder 5.0382 g, is 1/9 to take by weighing DMAC according to the PVDF/DMAC weight ratio, and PVDF is dissolved among the DMAC under 50 ℃, obtains solution b behind the cool to room temperature; Then dispersion liquid a and solution b are mixed, after 15 ~ 60 minutes, obtain the mixing suspension of Al and PVDF through ultra-sonic dispersion 10 ~ 30 minutes and magnetic agitation; To mix suspension-s casting film-forming on clean sheet glass,, obtain the Al/PVDF composite material film 80 ℃ of following vacuum-dryings 2 hours.
(3) specific inductivity of Al/PVDF matrix material under room temperature 1 kHz is 21.02, and loss is 0.012; The specific inductivity of matrix material changes very little in 30 ~ 200 kHz test frequency scopes and 20 ~ 150 ℃ of TRs, and loss is less than 0.1, and the overwhelming majority is below 0.05.
Embodiment 3
(1) process of surface treatment of Al powder is with embodiment 1;
(2) take by weighing silane coupler modified Al powder 3.5103 g that obtain in the step (1); Making its volumn concentration in matrix material is 30%, is 1/2 to take by weighing corresponding D MAC according to the Al/DMAC weight ratio, and Al powder ultra-sonic dispersion in DMAC is obtained dispersion liquid a; According to polymeric matrix PVDF volumn concentration is 70% to take by weighing PVDF powder 5.3701 g, is 1/5 to take by weighing DMAC according to the PVDF/DMAC weight ratio, and PVDF is dissolved among the DMAC under 50 ℃, obtains solution b behind the cool to room temperature; Then dispersion liquid a and solution b are mixed, after 15 ~ 60 minutes, obtain the mixing suspension of Al and PVDF through ultra-sonic dispersion 10 ~ 30 minutes and magnetic agitation; To mix suspension-s casting film-forming on clean sheet glass,, obtain the Al/PVDF composite material film 80 ℃ of following vacuum-dryings 2 hours.
(3) specific inductivity of Al/PVDF matrix material under room temperature 1 kHz is 31.81, and loss is 0.017; The specific inductivity of matrix material changes very little in 30 ~ 200 kHz test frequency scopes and 20 ~ 150 ℃ of TRs, and loss is less than 0.1, and the overwhelming majority is below 0.05.
Embodiment 4
(1) process of surface treatment of Al powder is with embodiment 1;
(2) take by weighing silane coupler modified Al powder 5.8214 g that obtain in the step (1); Making its volumn concentration in matrix material is 40%, is 1/1 to take by weighing corresponding D MAC according to the Al/DMAC weight ratio, and Al powder ultra-sonic dispersion in DMAC is obtained dispersion liquid a; According to polymeric matrix PVDF volumn concentration is 60% to take by weighing PVDF powder 5.7248 g, is 1/8 to take by weighing DMAC according to the PVDF/DMAC weight ratio, and PVDF is dissolved among the DMAC under 50 ℃, obtains solution b behind the cool to room temperature; Then dispersion liquid a and solution b are mixed, after 15 ~ 60 minutes, obtain the mixing suspension of Al and PVDF through ultra-sonic dispersion 10 ~ 30 minutes and magnetic agitation; To mix suspension-s casting film-forming on clean sheet glass,, obtain the Al/PVDF composite material film 80 ℃ of following vacuum-dryings 2 hours.
(3) specific inductivity of Al/PVDF matrix material under room temperature 1 kHz is 44.96, and loss is 0.018; The specific inductivity of matrix material changes very little in 30 ~ 200 kHz test frequency scopes and 20 ~ 150 ℃ of TRs, and loss is less than 0.1, and the overwhelming majority is below 0.05.
Embodiment 5
(1) process of surface treatment of Al powder is with embodiment 1;
(2) take by weighing silane coupler modified Al powder 8.2137 g that obtain in the step (1); Making its volumn concentration in matrix material is 50%, is 1/1 to take by weighing corresponding D MAC according to the Al/DMAC weight ratio, and Al powder ultra-sonic dispersion in DMAC is obtained dispersion liquid a; According to polymeric matrix PVDF volumn concentration is 50% to take by weighing PVDF powder 5.3849 g, is 1/9 to take by weighing DMAC according to the PVDF/DMAC weight ratio, and PVDF is dissolved among the DMAC under 50 ℃, obtains solution b behind the cool to room temperature; Then dispersion liquid a and solution b are mixed, after 15 ~ 60 minutes, obtain the mixing suspension of Al and PVDF through ultra-sonic dispersion 10 ~ 30 minutes and magnetic agitation; To mix suspension-s casting film-forming on clean sheet glass,, obtain the Al/PVDF composite material film 80 ℃ of following vacuum-dryings 2 hours.
(3) specific inductivity of Al/PVDF matrix material under room temperature 1 kHz is 58.34, and loss is 0.019; The specific inductivity of matrix material changes very little in 30 ~ 200 kHz test frequency scopes and 20 ~ 150 ℃ of TRs, and loss is less than 0.1, and the overwhelming majority is below 0.05.
Claims (2)
1. high-k low-loss metal/polymer composites is characterized in that: said high-k low-loss polymer matrix material has following material to form: self-passivating metal Al powder and polymeric matrix PVDF; The volume percent content of described Al powder in matrix material is 10 ~ 50%; Said polymeric matrix PVDF content is 50 ~ 90%; Described self-passivation Al powder median size is 800 nm, and it is the Al of 2 ~ 3 nm that there is one deck thickness that oxidation forms in air on the surface
2O
3Zone of oxidation, the Al powder uses after silane coupling agent is handled, and wherein the mass ratio of Al powder and silane coupling agent is 100:1; Described polymeric matrix PVDF fusing point is 167 ℃, and median size is 25 μ m.
2. the preparation method with high-k and low-loss polymer composites is characterized in that, comprises the steps:
(1) surface treatment of Al powder: make it in absolute ethyl alcohol, form suspension-s through ultra-sonic dispersion and stirring in the Al powder under the room temperature, add then and continue behind the coupling agent γ-An Bingjisanyiyangjiguiwan to stir 10 ~ 30 minutes; Add deionized water subsequently, at 40 ~ 60 ℃ of following ultra-sonic dispersion and stirred 15 ~ 60 minutes; The spinning powder, use absolute ethanol washing 1 ~ 3 time then after, 60 ~ 120 ℃ of following vacuum-dryings 2 ~ 5 hours, use after naturally cooling to room temperature;
(2) compound: take by weighing the silane coupler modified Al powder that obtains in the step (1), making its volumn concentration in matrix material is 10 ~ 50%, is 1/10 ~ 1/1 to take by weighing DMAC according to the Al/DMAC weight ratio, and Al powder ultra-sonic dispersion in DMAC is obtained dispersion liquid a; According to polymeric matrix PVDF volumn concentration is 50% ~ 90% to take by weighing the PVDF powder, is 1/20 ~ 1/4 to take by weighing DMAC according to the PVDF/DMAC weight ratio, and PVDF is dissolved among the DMAC under 50 ℃, obtains solution b behind the cool to room temperature; Then dispersion liquid a and solution b are mixed, after 15 ~ 60 minutes, obtain the mixing suspension of Al and PVDF through ultra-sonic dispersion 10 ~ 30 minutes and magnetic agitation; To mix suspension-s casting film-forming on clean sheet glass,, obtain the Al/PVDF composite material film 80 ℃ of following vacuum-dryings 2 hours.
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| CN102660096A (en) * | 2012-05-28 | 2012-09-12 | 南昌航空大学 | Preparation method of Al/PVDF (Al and polyvinylidene fluoride) superhydrophobic surface with wettability adjustable for aqueous alcohol |
| CN103087449A (en) * | 2013-01-16 | 2013-05-08 | 南昌航空大学 | Preparation method of polymer nanometer composite material with high heat conduction, high dielectric and low loss |
| CN103506621A (en) * | 2013-10-11 | 2014-01-15 | 南京理工大学 | Preparation method for fluororubber cladding nanometer aluminum powder composite particles |
| CN103694748A (en) * | 2013-12-17 | 2014-04-02 | 北京北矿锌业有限责任公司 | Surface modification method of metallic pigment |
| CN109251514A (en) * | 2018-08-15 | 2019-01-22 | 山东大学 | A kind of APU-Al high frequency high-dielectric and low-loss material and preparation method thereof |
| CN109909494A (en) * | 2019-03-14 | 2019-06-21 | 昆山市中迪新材料技术有限公司 | A kind of high thermal conductivity powder and its preparation method and application |
| CN110157021A (en) * | 2019-06-20 | 2019-08-23 | 湘潭大学 | A method of improving Kynoar heat dissipation performance |
| CN111825936A (en) * | 2019-04-17 | 2020-10-27 | 南京理工大学 | Aluminum powder/polytetrafluoroethylene composite material and preparation method thereof |
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| CN102660096A (en) * | 2012-05-28 | 2012-09-12 | 南昌航空大学 | Preparation method of Al/PVDF (Al and polyvinylidene fluoride) superhydrophobic surface with wettability adjustable for aqueous alcohol |
| CN103087449A (en) * | 2013-01-16 | 2013-05-08 | 南昌航空大学 | Preparation method of polymer nanometer composite material with high heat conduction, high dielectric and low loss |
| CN103506621A (en) * | 2013-10-11 | 2014-01-15 | 南京理工大学 | Preparation method for fluororubber cladding nanometer aluminum powder composite particles |
| CN103694748A (en) * | 2013-12-17 | 2014-04-02 | 北京北矿锌业有限责任公司 | Surface modification method of metallic pigment |
| CN109251514A (en) * | 2018-08-15 | 2019-01-22 | 山东大学 | A kind of APU-Al high frequency high-dielectric and low-loss material and preparation method thereof |
| CN109251514B (en) * | 2018-08-15 | 2020-04-03 | 山东大学 | APU-Al high-frequency high-dielectric low-loss material and preparation method thereof |
| CN109909494A (en) * | 2019-03-14 | 2019-06-21 | 昆山市中迪新材料技术有限公司 | A kind of high thermal conductivity powder and its preparation method and application |
| CN109909494B (en) * | 2019-03-14 | 2021-05-04 | 昆山市中迪新材料技术有限公司 | High-thermal-conductivity powder and preparation method and application thereof |
| CN111825936A (en) * | 2019-04-17 | 2020-10-27 | 南京理工大学 | Aluminum powder/polytetrafluoroethylene composite material and preparation method thereof |
| CN111825936B (en) * | 2019-04-17 | 2021-12-28 | 南京理工大学 | Aluminum powder/polytetrafluoroethylene composite material and preparation method thereof |
| CN110157021A (en) * | 2019-06-20 | 2019-08-23 | 湘潭大学 | A method of improving Kynoar heat dissipation performance |
| CN110157021B (en) * | 2019-06-20 | 2021-05-14 | 湘潭大学 | Method for improving heat dissipation performance of polyvinylidene fluoride |
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Application publication date: 20121003 |