CN103467895A - Preparation method of flower-shaped nano-microstructure zinc oxide filled composite with high heat conductivity - Google Patents
Preparation method of flower-shaped nano-microstructure zinc oxide filled composite with high heat conductivity Download PDFInfo
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Abstract
The invention relates to a preparation method of a flower-shaped nano-microstructure zinc oxide filled composite with high heat conductivity. The preparation method comprises the following steps of preparing flower-shaped nano-microstructure zinc oxide with a zinc source, an alkali source, an end capping reagent and a solvent through high-temperature and high-pressure reaction, mixing filling and a matrix by a solution blending method, settling a polymer, drying, tabletting, and obtaining the binary composite. According to the preparation method, flower-shaped nano-microstructure zinc oxide composited by a template-free hydrothermal method serves as the filling; polyvinylidene fluoride serves as the matrix; an SEM (scanning electron microscope) test shows the prepared filling has a flower-shaped micrometer structure constructed by nano units, and has larger specific surface area and larger contact area in the matrix in comparison with spherical zinc oxide with the same size; and a heat conduction test indicates that flower-shaped nano-microstructure zinc oxide can form a heat conduction threshold seepage network more easily in the matrix, so that the composite has a better heat conduction property than a zinc oxide filled composite with the same content.
Description
Technical field
The invention belongs to the high-heat-conductive composite material technical field, be specifically related to the preparation method of the flower-shaped nano-micro structure zinc oxide of a kind of high heat conduction filled composite materials.
Background technology
The develop rapidly of and package technique integrated along with microelectronics, the volume of electronic devices and components and logical circuit is more and more less, simultaneously, operating frequency sharply increases, cause semi-conductive envrionment temperature to change to the high temperature direction, for guaranteeing the long-time reliable operation of electronic devices and components, heat-sinking capability just becomes the restraining factors of length in its in work-ing life in time.In addition, many production such as electrical equipment and electrical, LED illumination, aerospace, military equipment and high-tech area are also in the urgent need to having the material of excellent heat conductivity performance.Macromolecular material has mechanics, calorifics and the processing characteristics of unique insulating property, excellence, and has certain performance property changed by structure control and modification, because have the incomparable advantage of other materials.Yet general macromolecular material is all hot poor conductor, its thermal conductivity is generally lower than 0.5Wm
-1k
-1, preparation has the highly thermally conductive polymeric material of excellent comprehensive performance and extensively concerned.
The filled-type thermally conductive polymer composites is by heat conductive filler (carbon system, metal system, pottery are three major types) and polymeric matrix, compound through disperseing, lamination is compound and form after the mode such as surperficial heat conducting film is processed the heterogeneous composite heat-conducting system formed.The ceramic-like filler as zinc oxide, aluminum oxide, silicon-dioxide, boron nitride, boron nitride etc., owing to having excellent intrinsic insulation characterisitic, is subject to extensive concern in the high heat conductive insulating material development.Yet boron nitride, boron nitride cost are higher, are difficult at present realize industrialization; Aluminum oxide, silicon-dioxide intrinsic thermal conductivity a little less than, higher the deteriorated of mechanics and processing characteristics that cause of corresponding matrix material filler content.Zinc oxide is a kind of semiconductor material of uniqueness, there is characteristic and the higher thermal conductivitys such as pressure-sensitive, thermoelectricity, simultaneously, it has structure the abundantest in all material, as spherical, bar-shaped, banded, fibrous, spirrillum, pectination, the high-heat-conductive composite material for the processability excellence such as flower-shaped provides may.
Summary of the invention
The object of the invention is to overcome the deficiency that above-mentioned prior art exists, the preparation method of the flower-shaped nano-micro structure zinc oxide of a kind of high heat conduction filled composite materials is provided, the method prepares flower-shaped nano-micro structure zinc oxide with zinc source, alkali source, end-capping reagent sodium oxalate and reaction medium by high-temperature high-voltage reaction, and be filled into PVDF (that is: polyvinylidene difluoride (PVDF)) matrix by the method for solution blending, make the binary heat-conductive composite material of heat conductivility excellence.
Purpose of the present invention is achieved through the following technical solutions: the preparation method of the flower-shaped nano-micro structure zinc oxide of a kind of high heat conduction filled composite materials comprises the steps:
The preparation of the flower-shaped nano-micro structure ZnO of step (1) filler
Take 0.1～1.0g inorganic zinc salt and 0.1～1.0g sodium oxalate under 25～75 ℃, the condition that stirs, be dissolved in 10～100mL solvent, obtain the solution A of homogeneous; Separately take 0.1～1.0g alkali under 25～75 ℃, the condition that stirs, be dissolved in 10～100mL solvent, obtain the solution B of homogeneous; Described solution A and solution B are mixed, transfer in 50～500mL tetrafluoroethylene inner liner stainless steel high pressure vessel after stirring 1～10h, under 100～200 ℃, react 1～24h; After reaction finishes, separate, obtain precipitated product, and respectively wash 2～3 times with ethanol and deionized water, 50～100 ℃ of lower vacuum-drying 12～24h, obtain flower-shaped nano-micro structure ZnO filler;
The preparation of step (2) ZnO/PVDF matrix material
Take the described flower-shaped nano-micro structure ZnO filler of 0.1～1.0g, be scattered in 10～100mL solvent, be designated as solution C; Add 0.1～1.0g PVDF in described solution C, disperse 1～10h, obtain solution D; Described solution D is poured in 0.1～1.0L solvent, separate, obtain the polymkeric substance precipitation, then described polymkeric substance is deposited in to vacuum-drying 12～24h under 25～75 ℃ of conditions, by this dried polymkeric substance precipitation hot pressing, obtain the binary heat-conductive composite material of filler content 9.0～90.9wt% again.
Preferably, in step (1), described inorganic zinc salt is one or more the mixing in zinc acetate, zinc chloride, zinc nitrate, zinc sulfate and zinc oxalate.
Preferably, in step (1), described alkali is one or more the mixing in potassium hydroxide, sodium hydroxide, lithium hydroxide, ethamine, diethylamine, triethylamine and quadrol.
Preferably, in step (2), the method that described dispersion adopts and stirs, ultrasonic or it combines; Preferred, the described ultrasonic time is 1～10h; Described ultrasonic temperature is 25～75 ℃.
Preferably, the method that in step (1) and step (2), that described separation adopts is centrifugal, vacuum filtration, normal pressure filter or topple over.
Preferably, the actual conditions of described hot pressing is: hot pressing 10～30min under 100～200 ℃, 10～100MPa.
Preferably, in step (1) and step (2), described solvent is water, methyl alcohol, ethanol or dimethyl formamide.
Compared with prior art, the present invention has following beneficial effect:
1, flower-shaped nano-micro structure zinc oxide of the present invention, have by the nanometer primitive and build and form high stage structure, from the SEM image, learns, its spherical zinc oxide with respect to comparable size has more bigger serface, and in matrix, contact area is larger;
2, flower-shaped nano-micro structure zinc oxide filled composite materials of the present invention, from the heat conductivility test, learn, ooze network because high stage structure zinc oxide more easily forms threshold in matrix, with respect to the spherical zinc oxide composite of same equal size, there is more excellent heat conductivility.
The accompanying drawing explanation
By reading the detailed description of non-limiting example being done with reference to the following drawings, it is more obvious that other features, objects and advantages of the present invention will become:
The XRD spectra that Fig. 1 is flower-shaped ZnO of the present invention.
The SEM image that Fig. 2 is flower-shaped ZnO filler of the present invention.
The SEM image that Fig. 3 is the flower-shaped ZnO/PVDF matrix material of 40wt%.
The graph of a relation that Fig. 4 is the flower-shaped ZnO/PVDF thermal conductivity of composite materials of different content of the present invention and temperature.
The thermal conductivity that Fig. 5 is ZnO/PVDF matrix material in flower-shaped ZnO/PVDF matrix material of the present invention, prior art and the relation of filler content.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.Following examples will contribute to those skilled in the art further to understand the present invention, but not limit in any form the present invention.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make certain adjustments and improvements.These all belong to protection scope of the present invention.
embodiment 1
The present embodiment relates to the preparation method of the flower-shaped nano-micro structure zinc oxide of a kind of high heat conduction filled composite materials, comprises the steps:
The preparation of the flower-shaped nano-micro structure ZnO of step (1) filler
Take 0.5g Zinc diacetate dihydrate and 0.5g sodium oxalate, be dissolved in the 50mL deionized water under 50 ℃, obtain solution A; The another 0.5g sodium hydroxide that claims, be dissolved in 50mL ethanol under 50 ℃, obtains solution B; Above-mentioned two uniform solution are mixed, transfer in 100mL tetrafluoroethylene inner liner stainless steel high pressure vessel after stirring 1h, react 24h under 150 ℃; Centrifugation product after reaction finishes, and respectively wash 3 times with ethanol and deionized water, 100 ℃ of lower vacuum-drying 12h obtain flower-shaped nano-micro structure ZnO filler;
The preparation of step (2) ZnO/PVDF matrix material
Take 0.1g ZnO (flower-shaped or prior art), ultrasonic 1h is scattered in 50mL DMF, is designated as solution C; Take 0.5g PVDF and add solution C, ultrasonic dispersion 1h under 50 ℃, obtain solution D; Solution D is poured in 0.5L ethanol, and normal pressure filters the 50 ℃ of vacuum-drying 24h of solid product that obtain; By abundant desciccate hot pressing 10min under 150 ℃, 50MPa, obtain filler content 50wt% binary heat-conductive composite material.
embodiment 2
The present embodiment relates to the preparation method of the flower-shaped nano-micro structure zinc oxide of a kind of high heat conduction filled composite materials, comprises the steps:
The preparation of the flower-shaped nano-micro structure ZnO of step (1) filler
Take 0.7g zinc chloride and 1.0g sodium oxalate, be dissolved in the 100mL deionized water under 50 ℃, obtain solution A; The another 0.7g potassium hydroxide that claims, be dissolved in 10mL ethanol under 25 ℃, obtains solution B; Above-mentioned two uniform solution are mixed, transfer in 100mL tetrafluoroethylene inner liner stainless steel high pressure vessel after stirring 3h, react 15h under 100 ℃; High speed centrifugation separated product after reaction finishes, and respectively wash 2 times with ethanol and deionized water, 90 ℃ of lower vacuum-drying 15h obtain flower-shaped nano-micro structure ZnO filler;
The preparation of step (2) ZnO/PVDF matrix material
Take 0.2g ZnO (flower-shaped or prior art), ultrasonic 10h is scattered in 100mL DMF, is designated as solution C; Take 0.3g PVDF and add solution C, ultrasonic dispersion 3h under 25 ℃, obtain solution D; Solution D is poured in 0.1L ethanol into to 50 ℃ of vacuum-drying 12h of the solid product that vacuum filtration obtains; By abundant desciccate hot pressing 20min under 100 ℃, 100MPa, obtain filler content 9wt% binary heat-conductive composite material.
embodiment 3
The present embodiment relates to the preparation method of the flower-shaped nano-micro structure zinc oxide of a kind of high heat conduction filled composite materials, comprises the steps:
The preparation of the flower-shaped nano-micro structure ZnO of step (1) filler
Take 1.0g zinc nitrate and 0.7g sodium oxalate, be dissolved in the 10mL deionized water under 50 ℃, obtain solution A; The another 0.3g lithium hydroxide that claims, be dissolved in 100mL ethanol under 75 ℃, obtains solution B; Above-mentioned two uniform solution are mixed, transfer in 50mL tetrafluoroethylene inner liner stainless steel high pressure vessel after stirring 5h, react 10h under 200 ℃; Reaction finishes final vacuum suction filtration separated product, and respectively washs 3 times with ethanol and deionized water, and 80 ℃ of lower vacuum-drying 18h obtain flower-shaped nano-micro structure ZnO filler;
The preparation of step (2) ZnO/PVDF matrix material
Take 0.5g ZnO (flower-shaped or prior art), ultrasonic 5h is scattered in 10mL DMF, is designated as solution C; Take 0.8g PVDF and add solution C, ultrasonic dispersion 5h under 75 ℃, obtain solution D; Solution D is poured in 1.0L ethanol, and normal pressure filters the 25 ℃ of vacuum-drying 20h of solid product that obtain; By abundant desciccate hot pressing 30min under 200 ℃, 10MPa, obtain filler content 20wt% binary heat-conductive composite material.
embodiment 4
The present embodiment relates to the preparation method of the flower-shaped nano-micro structure zinc oxide of a kind of high heat conduction filled composite materials, comprises the steps:
The preparation of the flower-shaped nano-micro structure ZnO of step (1) filler
Take 0.3g zinc sulfate and 0.1g sodium oxalate, be dissolved in the 50mL deionized water under 50 ℃, obtain solution A; The another 0.1g triethylamine that claims, be dissolved in 50mL ethanol under 50 ℃, obtains solution B; Above-mentioned two uniform solution are mixed, transfer in 500mL tetrafluoroethylene inner liner stainless steel high pressure vessel after stirring 7h, react 5h under 150 ℃; Normal pressure filtering separation product after reaction finishes, and respectively wash 2 times with ethanol and deionized water, 70 ℃ of lower vacuum-drying 20h obtain flower-shaped nano-micro structure ZnO filler;
The preparation of step (2) ZnO/PVDF matrix material
Take 0.7g ZnO (flower-shaped or prior art), ultrasonic 1h is scattered in 50mL DMF, is designated as solution C; Take 1.0g PVDF and add solution C, 50 ℃ of lower dispersed with stirring 8h, obtain solution D; Solution D is poured in 0.5L ethanol, toppled over and discard liquid, 75 ℃ of vacuum-drying 15h of the solid product obtained; By abundant desciccate hot pressing 10min under 150 ℃, 50MPa, obtain filler content 70wt% binary heat-conductive composite material.
embodiment 5
The present embodiment relates to the preparation method of the flower-shaped nano-micro structure zinc oxide of a kind of high heat conduction filled composite materials, comprises the steps:
The preparation of the flower-shaped nano-micro structure ZnO of step (1) filler
Take 0.1g zinc oxalate and 0.3g sodium oxalate, be dissolved in the 50mL deionized water under 50 ℃, obtain solution A; The another 1.0g quadrol that claims, be dissolved in 50mL ethanol under 75 ℃, obtains solution B; Above-mentioned two uniform solution are mixed, transfer in 100mL tetrafluoroethylene inner liner stainless steel high pressure vessel after stirring 10h, react 1h under 150 ℃; High speed centrifugation separated product after reaction finishes, and respectively wash 3 times with ethanol and deionized water, 50 ℃ of lower vacuum-drying 24h obtain flower-shaped nano-micro structure ZnO filler;
The preparation of step (2) ZnO/PVDF matrix material
Take 1.0g ZnO (flower-shaped or prior art), stir 1h and be scattered in 50mL DMF, be designated as solution C; Take 0.1g PVDF and add solution C, ultrasonic dispersion 10h under 50 ℃, obtain solution D; Solution D is poured in 0.5L ethanol into to 50 ℃ of vacuum-drying 18h of the solid product that vacuum filtration obtains; By abundant desciccate hot pressing 10min under 150 ℃, 50MPa, obtain filler content 90.9wt% binary heat-conductive composite material.
implementation result
The XRD spectra that Fig. 1 is flower-shaped ZnO of the present invention, Fig. 2 is flower-shaped ZnO filler SEM image of the present invention, Fig. 3 is the flower-shaped ZnO/PVDF matrix material of 40wt% SEM image, known according to Fig. 1, Fig. 2 and Fig. 3, flower-shaped nano-micro structure zinc oxide of the present invention, have by the nanometer primitive and build the high stage structure formed, and from the SEM image, learns, its of the prior art spherical zinc oxide with respect to comparable size has more bigger serface, and in matrix, contact area is larger.
The relation that Fig. 4 is the flower-shaped ZnO/PVDF thermal conductivity of composite materials of different content of the present invention and temperature, the thermal conductivity that Fig. 5 is ZnO/PVDF matrix material in the flower-shaped ZnO/PVDF matrix material of the present invention and prior art and the relation of filler content, known according to the heat conductivility test of Fig. 4 and Fig. 5, flower-shaped nano-micro structure zinc oxide filled composite materials of the present invention, ooze network because high stage structure zinc oxide more easily forms threshold in matrix, with respect to the of the prior art spherical zinc oxide composite of same equal size, there is more excellent heat conductivility.
Above specific embodiments of the invention are described.It will be appreciated that, the present invention is not limited to above-mentioned specific implementations, and those skilled in the art can make various distortion or modification within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (9)
1. the preparation method of the flower-shaped nano-micro structure zinc oxide composite of high heat conduction, is characterized in that, comprises the following steps:
Step 1, flower-shaped nano-micro structure ZnO filler preparation
Take 0.1～1.0g inorganic zinc salt and 0.1～1.0g sodium oxalate under 25～75 ℃, the condition that stirs, be dissolved in 10～100mL solvent, obtain the solution A of homogeneous; Separately take 0.1～1.0g alkali under 25～75 ℃, the condition that stirs, be dissolved in 10～100mL solvent, obtain the solution B of homogeneous; Described solution A and solution B are mixed, transfer in 50～500mL tetrafluoroethylene inner liner stainless steel high pressure vessel after stirring 1～10h, under 100～200 ℃, react 1～24h; After reaction finishes, separate, obtain precipitated product, and respectively wash 2～3 times with ethanol and deionized water, 50～100 ℃ of lower vacuum-drying 12～24h, obtain flower-shaped nano-micro structure ZnO filler;
Step 2, the preparation of ZnO/PVDF matrix material
Take the described flower-shaped nano-micro structure ZnO filler of 0.1～1.0g, be scattered in 10～100mL solvent, be designated as solution C; Add 0.1～1.0g PVDF in described solution C, disperse 1～10h, obtain solution D; Described solution D is poured in 0.1～1.0L solvent, separate, obtain the polymkeric substance precipitation, then described polymkeric substance is deposited in to vacuum-drying 12～24h under 25～75 ℃ of conditions, by this dried polymkeric substance precipitation hot pressing, obtain the binary heat-conductive composite material of filler content 9.0～90.9wt% again.
2. preparation method according to claim 1, is characterized in that, in step 1, described inorganic zinc salt is one or more the mixing in zinc acetate, zinc chloride, zinc nitrate, zinc sulfate and zinc oxalate.
3. preparation method according to claim 1, is characterized in that, in step 1, described alkali is one or more the mixing in potassium hydroxide, sodium hydroxide, lithium hydroxide, ethamine, diethylamine, triethylamine and quadrol.
4. preparation method according to claim 1, is characterized in that, in step 2, and the method that described dispersion adopts and stirs, ultrasonic or it combines.
5. preparation method according to claim 4, is characterized in that, the described ultrasonic time is 1～10h.
6. preparation method according to claim 4, is characterized in that, described ultrasonic temperature is 25～75 ℃.
7. preparation method according to claim 1, is characterized in that, the method that in step 1 and step 2, that described separation adopts is centrifugal, vacuum filtration, normal pressure filter or topple over.
8. preparation method according to claim 1, is characterized in that, the actual conditions of described hot pressing is: hot pressing 10～30min under 100～200 ℃, 10～100MPa.
9. preparation method according to claim 1, is characterized in that, in step 1 and step 2, described solvent is water, methyl alcohol, ethanol or dimethyl formamide.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105215347A (en) * | 2015-09-07 | 2016-01-06 | 济南大学 | A kind of zinc oxide and gold nano grain composite and preparation method thereof |
| CN106186044A (en) * | 2016-07-26 | 2016-12-07 | 陕西科技大学 | A kind of preparation method of flower shape zinc oxide nanometer sheet cluster |
| CN106277027A (en) * | 2016-07-26 | 2017-01-04 | 陕西科技大学 | A kind of preparation method of flower shape zinc oxide nanometer rods cluster |
| CN108251072A (en) * | 2018-03-05 | 2018-07-06 | 北京科技大学 | A kind of preparation method of liquid metal composite phase-change material |
| CN109825112A (en) * | 2019-03-22 | 2019-05-31 | 河南大学 | A kind of perfluorocarboxylic acid modification zinc oxide nanoparticle and its preparation method and application |
| CN109897312A (en) * | 2019-04-04 | 2019-06-18 | 鹤壁汽车工程职业学院 | A kind of dendritic flower-shape ZnO heat-conductive composite material of PVDF- and preparation method thereof |
| CN113999469A (en) * | 2021-11-11 | 2022-02-01 | 中国科学院兰州化学物理研究所 | Flower-like binary hydroxide modified polytetrafluoroethylene-based friction material and preparation method and application thereof |
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- 2013-08-23 CN CN2013103743995A patent/CN103467895A/en active Pending
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| WEI WU ET AL.: "Novel Three-Dimensional Zinc Oxide Superstructures for High Dielectric Constant Polymer Composites Capable of Withstanding High Electric Field", 《THE JOURNAL OF PHYSICAL CHEMISTRY C》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105215347A (en) * | 2015-09-07 | 2016-01-06 | 济南大学 | A kind of zinc oxide and gold nano grain composite and preparation method thereof |
| CN105215347B (en) * | 2015-09-07 | 2017-03-29 | 济南大学 | A kind of Zinc Oxide and gold nano grain composite and preparation method thereof |
| CN106186044A (en) * | 2016-07-26 | 2016-12-07 | 陕西科技大学 | A kind of preparation method of flower shape zinc oxide nanometer sheet cluster |
| CN106277027A (en) * | 2016-07-26 | 2017-01-04 | 陕西科技大学 | A kind of preparation method of flower shape zinc oxide nanometer rods cluster |
| CN108251072A (en) * | 2018-03-05 | 2018-07-06 | 北京科技大学 | A kind of preparation method of liquid metal composite phase-change material |
| CN108251072B (en) * | 2018-03-05 | 2020-08-25 | 北京科技大学 | Preparation method of liquid metal composite phase-change material |
| CN109825112A (en) * | 2019-03-22 | 2019-05-31 | 河南大学 | A kind of perfluorocarboxylic acid modification zinc oxide nanoparticle and its preparation method and application |
| CN109897312A (en) * | 2019-04-04 | 2019-06-18 | 鹤壁汽车工程职业学院 | A kind of dendritic flower-shape ZnO heat-conductive composite material of PVDF- and preparation method thereof |
| CN109897312B (en) * | 2019-04-04 | 2020-12-29 | 鹤壁汽车工程职业学院 | PVDF (polyvinylidene fluoride) -dendritic flower-shaped ZnO heat-conducting composite material and preparation method thereof |
| CN113999469A (en) * | 2021-11-11 | 2022-02-01 | 中国科学院兰州化学物理研究所 | Flower-like binary hydroxide modified polytetrafluoroethylene-based friction material and preparation method and application thereof |
| CN113999469B (en) * | 2021-11-11 | 2022-11-15 | 中国科学院兰州化学物理研究所 | Flower-like binary hydroxide modified polytetrafluoroethylene-based friction material and preparation method and application thereof |
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Application publication date: 20131225 |