CN105733065B - Anisotropic thermal polymer composites and preparation method thereof - Google Patents
Anisotropic thermal polymer composites and preparation method thereof Download PDFInfo
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- CN105733065B CN105733065B CN201410733881.8A CN201410733881A CN105733065B CN 105733065 B CN105733065 B CN 105733065B CN 201410733881 A CN201410733881 A CN 201410733881A CN 105733065 B CN105733065 B CN 105733065B
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Abstract
Anisotropic thermal polymer composites and preparation method thereof.The conductive performance of polymer matrix composite includes not only the structure of matter, thermal conductivity, electric conductivity, optical property, size with the property of filler itself, exterior appearance, geometry etc. is related, and has close relationship with filler dispersity in a polymer matrix and structurally ordered degree.Composition of the invention includes: polymer and heat filling, the polymer is as basis material, the polymeric matrix material mass fraction is 50 ~ 99.9%, the heat filling is with magnetic responsiveness high thermal conductivity inorganic particulate, and the magnetic responsiveness high thermal conductivity inorganic particulate additive amount that has is 0.1 ~ 50wt.%.The present invention is used for heat-conducting polymer field.
Description
Technical field:
The present invention relates to a kind of anisotropic thermal polymer composites and preparation method thereof.
Background technique:
The development of modern science and technology is higher and higher to the performance requirement of material, in addition to good mechanical performance, the function of material
Change has become focus concerned by people.Using method physically or chemically, into polymer, addition has the nothing of functional characteristic
Machine filler, can by high molecular light, easy processing, it is anticorrosive the advantages that and inorganic matter functionality be effectively combined together.
Particle (metal class, carbons, ceramic-like etc.) with thermal conductive resin, is widely used thermally conductive composite wood as heat filling
In the preparation of material, meets the needs of fields such as electrical motor, Electronic Packaging, aerospace, military affairs are to Heat Conduction Material.
The conductive performance of polymer matrix composite includes not only the structure of matter with the property of filler itself, thermal conductivity, leads
Electrical property, optical property, size, exterior appearance, geometry etc. is related, and the dispersity with filler in a polymer matrix
And structurally ordered degree has close relationship.Under conditions of polymeric matrix and filler have determined, in the base to filler
Order degree be adjusted for composite material comprehensive performance design provide more extensive space.With ordered structure
Material organic electronic device, molecular filtration, in terms of be with a wide range of applications, preparation structure Ordered Materials
Have become a hot spot of present material research field.Ordering arrangement can pass through additional physics to filler in a polymer matrix
It is realized as power source, additional physical field can make it occur to be orientated along outer field direction in a polymer matrix or regular row
Column, additional physical field mainly have electric field, magnetic field, mechanical field of force etc..
Carbons inorganic filler especially graphene and graphite nanosheets are received with its good heating conduction much to be ground
The concern for the person of studying carefully, Y Shibayama have studied the orientation texture in polymeric matrix and generate significantly to composite material conductive performance
Influence (Shibayama Y, Sato H, Enoki T, et al. Disordered magnetism at the metal-
insulator threshold in nano-graphite-based carbon materials[J]. Physical
Review letters, 2000,84 (8): 1744.).In recent years, many scientific workers have done greatly the magnetic phenomenon of graphite
Theoretical research is measured, it is found that magnetic performance is mainly derived from defect, magnetic impurity and the electronic state hesitated to move forward of structure, wherein stone
Fault of construction present in ink sheet layer is the main reason for causing nano-graphite to have magnetic responsiveness.However, about external magnetic field
On the orientation behavior of Carbon materials and its on polymer composites heating conduction influence research and patent there is not been reported and
Application.
Summary of the invention:
The object of the present invention is to provide a kind of anisotropic thermal polymer composites and preparation method thereof.
Above-mentioned purpose is realized by following technical scheme:
A kind of anisotropic thermal polymer composites, composition includes: polymer and heat filling, the polymerization
Object is as basis material, and the polymeric matrix material mass fraction is 50 ~ 99.9%, and the heat filling is with magnetic
Responsiveness high thermal conductivity inorganic particulate, the magnetic responsiveness high thermal conductivity inorganic particulate additive amount that has is 0.1 ~ 50wt.%.
The anisotropic thermal polymer composites, the polymeric matrix material be low density polyethylene (LDPE),
Linear low density polyethylene, polypropylene or combinations thereof.
The anisotropic thermal polymer composites, the high thermal conductivity inorganic particulate be graphene, graphite flake,
Graphite nanosheets, carbon fiber, carbon nanotube or they and graphene, graphite flake, graphite nanosheets, carbon nanotube, carbon fiber
Dimension, aluminium oxide, boron nitride, in carbon black, silicon nitride, aluminium oxide, magnesia, zinc oxide, silicon carbide, copper powder, aluminium powder, magnesium powder
At least one combination.
A kind of preparation method of the anisotropic thermal polymer composites, the method steps are as follows:
Composite material is prepared using melt-blending process, by polymer thermoplastic matrix, heat filling in selected polymer matrix
Body carries out melt blending composite material in the above decomposition temperature of fusing point temperature below by a certain percentage, will be mixed multiple
Condensation material compression moulding under vulcanizing press obtains composite material.
Induced by magnetic field conductive particle orientations, composite material and mold are put into magnetic field generator, and adjustment magnetic head is extremely
It compresses sample and mold temperature set is the above decomposition temperature of fusing point of selected polymeric matrix hereinafter, protecting under high-intensity magnetic field intensity
Hold certain time, erasing head temperature reduces magnetic induction intensity to zero, and take out sample, obtain after specimen temperature reaches room temperature
To the thermal conductive polymer composite material of anisotropic structure.
The preparation method of the anisotropic thermal polymer composites, the melt-blending process prepare composite wood
Equipment involved in expecting has one of rheometer, extruder, plastics processing mill, vulcanizing press or their combination.
The preparation method of the anisotropic thermal polymer composites, the high-intensity magnetic field intensity are 1T or more.
A kind of preparation method of the anisotropic thermal polymer composites, prepares composite material: by 4g first
Graphene platelet and 40g nano alumina powder (Al2O3, 20-30nm) and it is put into ball milling 2h in planetary ball mill, obtain composite powder
Body, by composite granule and 60gLLDPE in torque rheometer, 135 DEG C of temperature, 45 turns/s of revolving speed, melt blending to torque perseverance
It is fixed, obtain composite material；Composite material is further mixed in open type plastic purificating set, 125 DEG C of temperature；It will be mixed compound
Material compression moulding under the conditions of 150 DEG C, 10MPa in vulcanizing press, obtains composite sample；By composite sample and
Epoxy resin mould is put into together between the magnetic head of steady magnetic field generator, and magnetic head temperature is set as 150 DEG C；Magnetic head is adjusted to compression
Sample and mold；Adjustment pole coil electric current makes magnetic induction intensity reach 1.5T, keeps 30min；Erasing head temperature, to sample
After temperature reaches room temperature, magnetic induction intensity is reduced to zero, obtains composite material after the processing of magnetic field；Using Sirion200 type surface sweeping
Electron microscopic study has determined the orientation behavior of graphite nanosheets in composite material, passes through TC-7000H type laser thermal constant
The thermal diffusion coefficient of tester test sample；After magnetic field is handled, when GNP loading is 4.0wt.%, composite material thermal diffusion
Coefficient improves 13.4%.
The preparation method of the anisotropic thermal polymer composites, it is described prepare first composite material be by
0.4g graphene platelet and 40g nano alumina powder (Al2O3, 20-30nm) and it is put into ball milling 2h in planetary ball mill, it is answered
Powder is closed, by composite granule and 60gLLDPE in torque rheometer, 135 DEG C of temperature, 45 turns/s of revolving speed, melt blending to torque
It is constant, obtain composite material；Composite material is further mixed into (125 DEG C) in open type plastic purificating set；It will be mixed compound
Material compression moulding under the conditions of 150 DEG C, 10MPa in vulcanizing press, obtains composite sample；By composite sample and
Epoxy resin mould is put into together between the magnetic head of steady magnetic field generator, and magnetic head temperature is set as 150 DEG C；Magnetic head is adjusted to compression
Sample and mold；Adjustment pole coil electric current makes magnetic induction intensity reach 1.5T, keeps 30min；Erasing head temperature, to sample
After temperature reaches room temperature, magnetic induction intensity is reduced to zero, obtains composite material after the processing of magnetic field；Using Sirion200 type surface sweeping
Electron microscopic study has determined the orientation behavior of graphite nanosheets in composite material, passes through TC-7000H type laser thermal constant
The thermal diffusion coefficient of tester test sample；After magnetic field is handled, when GNP loading is 0.4wt.%, composite material thermal diffusion
Coefficient improves 7%.
Beneficial effects of the present invention:
For the present invention using polymer as matrix, high thermal conductivity inorganic particulate is heat filling composition with anisotropic structure
Polymer composites are continuously applied magnetic field steady strong magnetic field in the process with hot-forming in composite material melting, make thermally conductive fill out
Material is arranged of preferred orient in the same direction under high-intensity magnetic field induction, forms the anisotropic structure of polymer matrix composite,
Under the additive amount of same heat filling, composite material is effectively improved in the heating conduction in orientations direction.Polymer is compound
Material mechanical performance is good.This High thermal-conductivitypolymer polymer composite material has wide in heat-conducting polymer field and practical application
Prospect.
Detailed description of the invention:
Attached drawing 1 is composite material profile scanning electron microscope.
Attached drawing 2 is profile scanning electron microscope after the processing of composite material magnetic field.
Specific embodiment:
Embodiment 1:
A kind of anisotropic thermal polymer composites, composition includes: polymer and heat filling, the polymerization
Object is as basis material, and the polymeric matrix material mass fraction is 50 ~ 99.9%, and the heat filling is with magnetic
Responsiveness high thermal conductivity inorganic particulate, the magnetic responsiveness high thermal conductivity inorganic particulate additive amount that has is 0.1 ~ 50wt.%.
Embodiment 2:
According to anisotropic thermal polymer composites described in embodiment 1, the polymeric matrix material is low
Density polyethylene, linear low density polyethylene, polypropylene or their combination.
Embodiment 3:
According to anisotropic thermal polymer composites described in embodiment 1, the high thermal conductivity inorganic particulate is stone
Black alkene, graphite flake, graphite nanosheets, carbon fiber, carbon nanotube or they and graphene, graphite flake, graphite nanosheets, carbon
Nanotube, carbon fiber, aluminium oxide, boron nitride, carbon black, silicon nitride, aluminium oxide, magnesia, zinc oxide, silicon carbide, copper powder, aluminium
The combination of at least one of powder, magnesium powder.
Embodiment 4:
The preparation method of anisotropic thermal polymer composites described in a kind of one of embodiment 1-3, this method step
It is rapid as follows:
Composite material is prepared using melt-blending process, by polymer thermoplastic matrix, heat filling in selected polymer matrix
Body carries out melt blending composite material in the above decomposition temperature of fusing point temperature below by a certain percentage, will be mixed multiple
Condensation material compression moulding under vulcanizing press obtains composite material.
Induced by magnetic field conductive particle orientations, composite material and mold are put into magnetic field generator, and adjustment magnetic head is extremely
It compresses sample and mold temperature set is the above decomposition temperature of fusing point of selected polymeric matrix hereinafter, protecting under high-intensity magnetic field intensity
Hold certain time, erasing head temperature reduces magnetic induction intensity to zero, and take out sample, obtain after specimen temperature reaches room temperature
To the thermal conductive polymer composite material of anisotropic structure.
Embodiment 5:
According to the preparation method of anisotropic thermal polymer composites as described in example 4, the melt blending
Method, which prepares equipment involved in composite material, one of rheometer, extruder, plastics processing mill, vulcanizing press or their group
It closes.
Embodiment 6:
According to the preparation method of anisotropic thermal polymer composites as described in example 4, the high-intensity magnetic field is strong
Degree is 1T or more.
Embodiment 7:
The preparation method of the anisotropic thermal polymer composites, by 4g graphene platelet and 40g nano oxygen
Change aluminium powder (Al2O3, 20-30nm) be put into ball milling 2h in planetary ball mill, obtain composite granule, by composite granule with
60gLLDPE is in torque rheometer, and 135 DEG C of temperature, 45 turns/s of revolving speed, melt blending to constant torque obtains composite material；
Composite material is further mixed into (125 DEG C) in open type plastic purificating set；By mixed composite material in vulcanizing press
150 DEG C, compression moulding under the conditions of 10MPa, obtain composite sample.Composite sample and epoxy resin mould are put together
Between the magnetic head for entering steady magnetic field generator, magnetic head temperature is set as 150 DEG C；Magnetic head is adjusted to compression sample and mold；Adjust magnetic
Polar curve loop current makes magnetic induction intensity reach 1.5T, keeps 30min；Erasing head temperature, after specimen temperature reaches room temperature, drop
Low magnetic induction intensity obtains composite material after the processing of magnetic field to zero.It is determined using Sirion200 type Scanning Electron microscopic study
The orientation behavior of graphite nanosheets, passes through the heat of TC-7000H type laser thermal constant tester test sample in composite material
Diffusion coefficient.After magnetic field is handled, when GNP loading is 4.0wt.%, composite material thermal diffusion coefficient improves 13.4%.
Embodiment 8:
The preparation method of the anisotropic thermal polymer composites referring to described in embodiment 7 is thin by 0.4g graphene
Piece and 40g nano alumina powder (Al2O3, 20-30nm) and it is put into ball milling 2h in planetary ball mill, composite granule is obtained, it will be compound
Powder and 60gLLDPE are in torque rheometer, and 135 DEG C of temperature, 45 turns/s of revolving speed, melt blending to constant torque obtains compound
Material；Composite material is further mixed into (125 DEG C) in open type plastic purificating set；By mixed composite material in compression molding
150 DEG C in machine, compression moulding under the conditions of 10MPa, obtain composite sample.By composite sample and epoxy resin mould one
With being put between the magnetic head of steady magnetic field generator, magnetic head temperature is set as 150 DEG C；Magnetic head is adjusted to compression sample and mold；It adjusts
Whole pole coil electric current makes magnetic induction intensity reach 1.5T, keeps 30min；Erasing head temperature reaches room temperature to specimen temperature
Afterwards, magnetic induction intensity is reduced to zero, obtains composite material after the processing of magnetic field.It is ground using Sirion200 type Scanning Electron microscope
Study carefully and the orientation behavior of graphite nanosheets in composite material has been determined, passes through TC-7000H type laser thermal constant tester test specimens
The thermal diffusion coefficient of product.After magnetic field is handled, when GNP loading is 0.4wt.%, composite material thermal diffusion coefficient is improved
7%。
Claims (2)
1. a kind of preparation method of anisotropic thermal polymer composites, it is characterized in that: this method is specifically to press following step
Suddenly it completes: preparing composite material first, the nano alumina powder of 4g graphene platelet and 40g20-30nm is put into planetary
Ball milling 2h in ball mill, obtains composite granule, by composite granule and 60gLLDPE in torque rheometer, 135 DEG C of temperature, and revolving speed
45 turns/s, melt blending to constant torque obtains composite material；Composite material is further mixed in open type plastic purificating set,
125 DEG C of temperature；By mixed composite material, compression moulding under the conditions of 150 DEG C, 10MPa in vulcanizing press, is obtained compound
Material sample；Composite sample and epoxy resin mould are put into together between the magnetic head of steady magnetic field generator, magnetic head temperature
It is set as 150 DEG C；Magnetic head is adjusted to compression sample and mold；Adjustment pole coil electric current makes magnetic induction intensity reach 1.5T, protects
Hold 30min；Erasing head temperature reduces magnetic induction intensity to zero, obtains multiple after magnetic field is handled after specimen temperature reaches room temperature
Condensation material；The orientation behavior of graphene platelet in composite material has been determined using Sirion200 type Scanning Electron microscopic study,
Pass through the thermal diffusion coefficient of TC-7000H type laser thermal constant tester test sample；After magnetic field is handled, work as graphene platelet
When loading is 4.0wt.%, composite material thermal diffusion coefficient improves 13.4%.
2. a kind of preparation method of anisotropic thermal polymer composites, it is characterized in that: this method is specifically to press following step
Suddenly it completes: preparing composite material first, the nano alumina powder of 0.4g graphene platelet and 40g20-30nm is put into planet
Ball milling 2h, obtains composite granule in formula ball mill, by composite granule and 60gLLDPE in torque rheometer, 135 DEG C of temperature, turns
45 turns/s of speed, melt blending to constant torque obtain composite material；By composite material in open type plastic purificating set in 125 DEG C into
The mixing of one step；By mixed composite material, compression moulding under the conditions of 150 DEG C, 10MPa in vulcanizing press, is obtained compound
Material sample；Composite sample and epoxy resin mould are put into together between the magnetic head of steady magnetic field generator, magnetic head temperature
It is set as 150 DEG C；Magnetic head is adjusted to compression sample and mold；Adjustment pole coil electric current makes magnetic induction intensity reach 1.5T, protects
Hold 30min；Erasing head temperature reduces magnetic induction intensity to zero, obtains multiple after magnetic field is handled after specimen temperature reaches room temperature
Condensation material；The orientation behavior of graphene platelet in composite material has been determined using Sirion200 type Scanning Electron microscopic study,
Pass through the thermal diffusion coefficient of TC-7000H type laser thermal constant tester test sample；After magnetic field is handled, work as graphene platelet
When loading is 0.4wt.%, composite material thermal diffusion coefficient improves 7%.
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