CN102775705A - Polymer-matrix composite material and preparation method thereof - Google Patents
Polymer-matrix composite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a polymer-matrix composite material and a preparation method thereof, which belong to the technical field of preparation of electronic composite materials. The composite material is prepared from metal passivation fillers and polymer materials with different shapes, wherein the fillers are metal passivation particles and fibrous or platy metal with two grain sizes, which are matched with each other at a certain proportion, and according to the formula, the volume ratio of polymer is that the metal filler accounts for 1%-50% and the polymer accounts for 50%-99%. The composite material prepared from the metal passivation fillers with the different shapes and the polymer matrix has the advantages of high heat conductivity, low dielectric constant, low dielectric loss and the like. The preparation method has the characteristics of low heat treatment temperature, low cost and environment friendliness, and also has the characteristics of being simple to operate and suitable for industrial production.
Description
Technical field
The invention belongs to the electron recombination technical field of material, particularly a kind ofly adopt difform metal as polymer matrix composite of filler and preparation method thereof.
Background technology
Thermally conductive material is widely used in fields such as heat exchange engineering, heating engineering, Electronics and Information Engineering.For a long time, the general choice metallic substance uses as thermally conductive material.Owing to the corrosion resistance difference of metallic substance has limited its range of application.In order to improve the resistance to corrosion of metal, adopted alloy technology, corrosion protection coating technology etc., but greatly reduce its capacity of heat transmission.In the last few years, field that some can have higher requirements to material thermal conductivity such as heat exchange engineering, electromagnetic shielding, electronic information, friction materials etc. were base material with the thermal conductive polymer, had caused investigator's attention.But the thermal conductivity of polymkeric substance is little, expand its application in the heat conduction field, and improving heat conductivility is key problem in technology.
Metallic substance filled polymer base heat-conductive composite material has good heat-conducting.Many in the world major companies, research institution, as: du pont company, IBM Corporation, the University of Pennsylvania, Mitsubishi main body chemical company, German BASF AG etc. have all carried out the research and the product development of this respect, and have obtained remarkable progress.
Retrieve through document; Do not find to have document and the patent that duplicates with the present invention as yet; Document that some that retrieve are relevant with the present invention and patent; Mainly be that aluminium powder with surface passivation layer is the report of the dielectric properties of the compound raising material of filler, find to change any report that the metallic stuffing shape improves matrix material thermal conductivity and dielectric properties.Below be reference and the patent relevant that the applicant retrieves with the present invention:
1.J.W.Xu,C.P.Wong,Appl.Phys.Lett.87,082907(2005)；
2. Wang Hong, Zhou Yongcun, to cutting edge of a knife or a sword, Li Kecheng, analogy section, Chen Huiru, polymer matrix composite and preparation method thereof, application number: 201110054346.6 application publication numbers: CN 102181168A.
Summary of the invention
The object of the present invention is to provide a kind of polymer matrix composite and preparation method thereof, this method is through changing thermal conductivity and the dielectric properties that the filler shape has improved prepared polymer matrix composite.
For achieving the above object, the present invention has adopted following technical scheme.
A kind of polymer matrix composite; This matrix material by volume mark is made up of 1～50% metallic stuffing and 50～99% polymeric matrix; Said metallic stuffing comprises metal passivation particle and fibrous metal or sheet metal, and the mass ratio of metal passivation particle and fibrous metal or sheet metal is 1: 1.
Said metal passivation particle comprises the metal passivation particle of micron grain size and the metal passivation particle of nanometer particle size; The metal passivation particulate volume ratio of the metal passivation particle of micron grain size and nanometer particle size is 5～30: 1; The metal passivation particulate diameter of micron grain size is 1～19 μ m; The metal passivation particulate diameter of nanometer particle size is 10～90nm, and the length of fibrous metal is that 3mm, diameter are 50 μ m～1mm, and the area of sheet metal is that 3～5mm * 3～5mm, thickness are 1～9 μ m.
Said metal passivation particle is to be prepared from after the powder with the metal with excellent propertys such as passivation properties and heat conduction, conductions such as Al, Fe, Cr, Mo, Ni, Co, Ta, Nb or W etc. utilizes strong oxidizer oxidation style or the passivation of air heating oxidation style; Strong oxidizer is the vitriol oil, nitric acid, chloric acid, acid iodide, SRM 935a or potassium permanganate etc., and fibrous metal or sheet metal adopt aluminium, copper, iron or silvery to be equipped with.
Said polymeric matrix is the polymer materials with good dielectric properties; Like PVDF (PVDF) or its multipolymer ([P (VDF-TrFE)]; [P (VDF-TrFE-CFE)]), Vestolen PP 7052 (PP), Vilaterm (PE); Vestolen PP 7052 methyl acid methyl esters (PMMA), epoxy resin (Epoxy) or polyimide (PI) etc.
The complex method of said metallic stuffing and polymeric matrix comprises admixture of powder method, solution method or pressure sintering etc.
A kind of method for preparing above-mentioned polymer matrix composite may further comprise the steps:
Step 1: metal-powder is broken for micron metal powder and nano metal powder respectively;
Step 2: utilize the air heating oxidation style to carry out passivation respectively micron metal powder and nano metal powder, obtain the metal passivation particle of micron grain size and nanometer particle size;
Step 3: adopting mechanical cutting to prepare length is that 3mm, diameter are the fibrous metal of 50 μ m～1mm or to prepare area be that 3～5mm * 3～5mm, thickness are the sheet metal of 1～9 μ m;
Step 4: immerse the metal passivation particle of micron grain size and nanometer particle size in the organic solvent respectively; The coupling agent that adds organic solvent quality 1～2.5% then; Supersound process makes the metal passivation particle surface coat one deck coupling agent uniformly after adding coupling agent, carries out dry evaporative removal organic solvent after the supersound process;
Step 5: through after the step 4 with the metal passivation particle of micron grain size and nanometer particle size according to 5～30: 1 volume ratio mixing takes by weighing fibrous metal or sheet metal with quality such as mixed metal passivation particle;
Step 6: through after the step 5 with mixed metal passivation particle and polymeric matrix mix mixture, mixture and fibrous metal or sheet metal are put into the hot-forming polymer matrix composite that promptly makes of mould after compound.
Said metal-powder is the powder of aluminium, chromium, nickel, iron or molybdenum, and the step of said air heating oxidation style is: aerating oxygen in metal-powder, and following dry 3～5 hours in 120 ℃ then.
Said organic solvent is an absolute ethyl alcohol, and coupling agent is a silane coupling agent.
The volume(tric)fraction of polymeric matrix is 50% in the said polymer matrix composite.
Said hot-forming condition is: temperature is 200 ℃, and pressure is 50MPa, and the time is 25 minutes.
The invention has the beneficial effects as follows:
The present invention improves polymer matrix composite thermal conductivity and dielectric properties through changing the filler shape.In the practical implementation; The utilization oxidation style realizes the surface of metal particles passivation; Thereby form the fine and close metal oxide film of one deck, this metal passivation particulate micron powder and nanoscale powder are mixed with the metal passivation powder that size is arranged in pairs or groups, it is mixed with polymeric matrix material; Fibrous or the sheet metal of quality such as adding and hybrid metal passivation powder adopts recombining process to prepare the matrix material of polymer-based carbon then.
The present invention makes that as filler the thermal conductivity of matrix material and specific inductivity are improved significantly through using difform metal; And the dielectric loss of matrix material still remains on lower level, makes the thermal conductivity of matrix material and dielectric properties obtain complex optimum; The preparation method preparation technology of polymer matrix composite according to the invention is simple, ripe, and cost is low, and processing parameter is convenient to control, realizes by the laboratory small-scale production to big industrial transition easily.
Description of drawings
Fig. 1 is the Photomicrograph of Al passivation particle/PVDF composite sample of the adding sheet metal Al of embodiment 1 preparation;
Fig. 2 is the Changing Pattern (test frequencies: 0.1kHz-1MHz) of the composite sample dielectric properties of embodiment 1 preparation with frequency;
Fig. 3 compares for the average thermal conductivity value of the matrix material of different shapes filler preparation.
Embodiment
Below in conjunction with embodiment the present invention is further described.It is pointed out that according to technical scheme of the present invention, the present invention is not limited to following embodiment, those skilled in the art can make some nonessential improvement and adjustment to the present invention according to following content, all can reach the object of the invention.
Embodiment 1:
What present embodiment provided is matrix with PVDF; To be shaped as flaky metal and metal passivation granules prepn filler, preparation polymer matrix composite, metallic stuffing and PVDF in the matrix material; Weigh according to each 50% conversion of volume(tric)fraction, its preparation comprises the following steps:
1) gets the metallic aluminium powder particle, for pure aluminium powder simple substance, do not contain other impurity, the metallic aluminium powder particle is broken into the nano level two kind powders of particle diameter about micron order about 10 μ m and 50nm respectively through the XRD test;
2) get micron order metal-powder 10g after the fragmentation, feed behind an amount of oxygen 120 ℃ dry 3 hours down, cross 120 mesh sieves the metal-powder of dry back caking disperseed, obtain micron order metallic aluminium powder passivation of uniform size powder;
3), obtain the metallic aluminium powder passivation powder of nanoscale size with step 2;
4) the metal aluminium flake is made into 5mm * 5mm, thickness is about the sheet of 5 μ m;
5) coupling agent treatment: the absolute ethyl alcohol of other aluminium powder passivation powder of two kinds of grain-size grades being put into 10g respectively; Add the silane coupling agent KH550 of absolute ethyl alcohol quality 2.5% then and under ultrasonic power 500W, handled 1 hour; Make aluminium powder passivation powder surface coat one deck coupling agent uniformly, carry out drying with the evaporative removal absolute ethyl alcohol in 80 ℃ after the supersound process;
6) will (micron order: volume ratio nano level=20: 1) mixes according to 20: 1 through other aluminium powder passivation powder of two kinds of levels of coupling agent treatment; The flaky aluminum metal (5mm * 5mm, thickness are about 5 μ m) of weight such as weighing and mixed aluminium powder passivation powder then;
7) through step 6); Mixed aluminium powder passivation powder and PVDF are mixed into uniform powder, the flaky aluminum metal of powder and weighing is compound according to the 2-3 composite structure, insert mould hot pressing on press then; Hot pressing temperature is 200 ℃; Pressure is 50MPa, and the time is 25 minutes, can obtain adding the matrix material of 2-3 composite structure of the Al/PVDF of aluminium flake after hot-forming.
Present embodiment is a coupling agent with KH550, and as solvent, selecting aluminium powder and being shaped as flaky metal is filler with absolute ethyl alcohol, and selection PVDF is a polymkeric substance, prepares the matrix material of the 2-3 composite structure of flaky aluminum metal/aluminium powder passivation powder filler/PVDF.
The micrograph of this composite sample is as shown in Figure 1, and the dielectric properties of matrix material and the relation of frequency are as shown in Figure 2.
The relative permittivity of the material of this sheet metal Al passivation/PVDF 2-3 composite structure is 24.5 (1MHz), and dielectric loss tan δ appears stable, is about 0.015 (1MHz).And the thermal conductivity peak is up to 11.81W/ (mK), far above the thermal conductivity 3.258W/ (mK) of Al powder/PVDF matrix material.It is thus clear that the thermal conductivity and the dielectric properties of matrix material obviously are improved behind the adding sheet metal.
Embodiment 2:
What present embodiment provided is matrix with PVDF; To be shaped as fibrous aluminum metal and metal passivation granules prepn filler, preparation polymer matrix composite, metallic stuffing and PVDF in the matrix material; Weigh according to each 50% conversion of volume(tric)fraction, its preparation comprises the following steps:
1) gets the metallic aluminium powder particle, for pure aluminium powder simple substance, do not contain other impurity, the metallic aluminium powder particle is broken into the nano level two kind powders of particle diameter about micron order about 10 μ m and 50nm respectively through the XRD test;
2) get micron order metal-powder 10g after the fragmentation, feed behind an amount of oxygen 120 ℃ dry 4 hours down, cross 120 mesh sieves the metal-powder of dry back caking disperseed, obtain micron order metallic aluminium powder passivation of uniform size powder;
3), obtain the metallic aluminium powder passivation powder of nanoscale size with step 2;
4) the metal aluminium flake is made into diameter 1mm, length is about fibrous (bar-shaped) of 3mm;
5) coupling agent treatment: the absolute ethyl alcohol of other aluminium powder passivation powder of two kinds of grain-size grades being put into 10g respectively; Add the silane coupling agent KH550 of absolute ethyl alcohol quality 1% then and under ultrasonic power 500W, handled 1 hour; Make aluminium powder passivation powder surface coat one deck coupling agent uniformly, carry out drying with the evaporative removal absolute ethyl alcohol in 80 ℃ after the supersound process;
6) will (micron order: volume ratio nano level=20: 1) mixes, then the fibrous aluminum metal of weight such as weighing and mixed aluminium powder passivation powder according to 20: 1 through other aluminium powder passivation powder of two kinds of levels of coupling agent treatment;
7) through step 6); Mixed aluminium powder passivation powder and PVDF are mixed into uniform powder, the fibrous aluminum metal of powder and weighing is compound according to the 1-3 composite structure, insert mould hot pressing on press then; Hot pressing temperature is 200 ℃; Pressure is 50MPa, and the time is 25 minutes, can obtain adding the matrix material of 1-3 composite structure of the Al/PVDF of aluminium bar after hot-forming.
Embodiment 3:
What present embodiment provided is matrix with PI; To be shaped as flaky metal and metal passivation granules prepn filler, preparation polymer matrix composite, metallic stuffing and PI in the matrix material; Weigh according to each 50% conversion of volume(tric)fraction, its preparation comprises the following steps:
1) gets the metallic aluminium powder particle, for pure aluminium powder simple substance, do not contain other impurity, the metallic aluminium powder particle is broken into the nano level two kind powders of particle diameter about micron order about 10 μ m and 50nm respectively through the XRD test;
2) get micron order metal-powder 10g after the fragmentation, feed behind an amount of oxygen 120 ℃ dry 5 hours down, cross 120 mesh sieves the metal-powder of dry back caking disperseed, obtain micron order metallic aluminium powder passivation of uniform size powder;
3), obtain the metallic aluminium powder passivation powder of nanoscale size with step 2;
4) the metal aluminium flake is made into 5mm * 5mm, thickness is about the sheet of 5 μ m;
5) coupling agent treatment: the absolute ethyl alcohol of other aluminium powder passivation powder of two kinds of grain-size grades being put into 10g respectively; Add the silane coupling agent KH550 of absolute ethyl alcohol quality 2.5% then and under ultrasonic power 500W, handled 1 hour; Make aluminium powder passivation powder surface coat one deck coupling agent uniformly, carry out drying with the evaporative removal absolute ethyl alcohol in 80 ℃ after the supersound process;
6) will (micron order: volume ratio nano level=20: 1) mixes according to 20: 1 through other aluminium powder passivation powder of two kinds of levels of coupling agent treatment; The flaky aluminum metal (5mm * 5mm, thickness are about 5 μ m) of weight such as weighing and mixed aluminium powder passivation powder then;
7) through step 6); Mixed aluminium powder passivation powder and PI are mixed into uniform powder, the flaky aluminum metal of powder and weighing is compound according to the 2-3 composite structure, insert mould hot pressing on press then; Hot pressing temperature is 200 ℃; Pressure is 50MPa, and the time is 25 minutes, can obtain adding the matrix material of 2-3 composite structure of the Al/PI of aluminium flake after hot-forming.
Embodiment 4:
What present embodiment provided is matrix with PVDF; To be shaped as flat tinsel and metal passivation granules prepn filler, preparation polymer matrix composite, metallic stuffing and PVDF in the matrix material; Weigh according to each 50% conversion of volume(tric)fraction, its preparation comprises the following steps:
1) gets the metallic aluminium powder particle, for pure aluminium powder simple substance, do not contain other impurity, the metallic aluminium powder particle is broken into the nano level two kind powders of particle diameter about micron order about 10 μ m and 50nm respectively through the XRD test;
2) get micron order metal-powder 10g after the fragmentation, feed behind an amount of oxygen 120 ℃ dry 3 hours down, cross 120 mesh sieves the metal-powder of dry back caking disperseed, obtain micron order metallic aluminium powder passivation of uniform size powder;
3), obtain the metallic aluminium powder passivation powder of nanoscale size with step 2;
4) the metal aluminium flake is made into 3mm * 3mm, thickness is about the tabular of 5 μ m;
5) coupling agent treatment: the absolute ethyl alcohol of other aluminium powder passivation powder of two kinds of grain-size grades being put into 10g respectively; Add the silane coupling agent KH550 of absolute ethyl alcohol quality 1.5% then and under ultrasonic power 500W, handled 1 hour; Make aluminium powder passivation powder surface coat one deck coupling agent uniformly, carry out drying with the evaporative removal absolute ethyl alcohol in 80 ℃ after the supersound process;
6) will (micron order: volume ratio nano level=20: 1) mixes according to 20: 1 through other aluminium powder passivation powder of two kinds of levels of coupling agent treatment; The tabular aluminum metal (3mm * 3mm, thickness are about 5 μ m) of weight such as weighing and mixed aluminium powder passivation powder then;
7) through step 6); Mixed aluminium powder passivation powder and PVDF are mixed into uniform powder, the tabular aluminum metal of powder and weighing is compound according to the 2-3 composite structure, insert mould hot pressing on press then; Hot pressing temperature is 200 ℃; Pressure is 50MPa, and the time is 25 minutes, can obtain adding the matrix material of the 2-3 composite structure of the dull and stereotyped Al/PVDF of aluminium after hot-forming.
Embodiment 5:
What present embodiment provided is matrix with PVDF; To be shaped as fibrous steel fiber and metal passivation granules prepn filler, preparation polymer matrix composite, metallic stuffing and PVDF in the matrix material; Weigh according to each 50% conversion of volume(tric)fraction, its preparation comprises the following steps:
1) gets the metallic aluminium powder particle, for pure aluminium powder simple substance, do not contain other impurity, the metallic aluminium powder particle is broken into the nano level two kind powders of particle diameter about micron order about 10 μ m and 50nm respectively through the XRD test;
2) get micron order metal-powder 10g after the fragmentation, feed behind an amount of oxygen 120 ℃ dry 3 hours down, cross 120 mesh sieves the metal-powder of dry back caking disperseed, obtain micron order metallic aluminium powder passivation of uniform size powder;
3), obtain the metallic aluminium powder passivation powder of nanoscale size with step 2;
4) metallic aluminium is made into diameter 50 μ m, length is about the fibrous of 3mm;
5) coupling agent treatment: the absolute ethyl alcohol of other aluminium powder passivation powder of two kinds of grain-size grades being put into 10g respectively; Add the silane coupling agent KH550 of absolute ethyl alcohol quality 2.0% then and under ultrasonic power 500W, handled 1 hour; Make aluminium powder passivation powder surface coat one deck coupling agent uniformly, carry out drying with the evaporative removal absolute ethyl alcohol in 80 ℃ after the supersound process;
6) will (micron order: volume ratio nano level=20: 1) mixes, then the fibrous aluminum metal of weight such as weighing and mixed aluminium powder passivation powder according to 20: 1 through other aluminium powder passivation powder of two kinds of levels of coupling agent treatment;
7) through step 6); Mixed aluminium powder passivation powder and PVDF are mixed into uniform powder, the fibrous aluminum metal of powder and weighing is compound according to the 1-3 composite structure, insert mould hot pressing on press then; Hot pressing temperature is 200 ℃; Pressure is 50MPa, and the time is 25 minutes, can obtain adding the matrix material of 1-3 composite structure of the Al/PVDF of fibrous aluminium after hot-forming.
Referring to Fig. 3; Three kinds of filler shapes are respectively single ball-type filler (A among Fig. 3); Be added with the ball-type filler (B among Fig. 3) of fibrous metal; Be added with the ball-type filler (C among Fig. 3) of sheet metal, the thermal conductivity of its matrix material increases successively, increases to 9.883W/ (mK) by 3.258W/ (mK).Very big by the visible filler selection of Fig. 3 to the thermal conductivity influence of matrix material.The present invention improves the performances such as thermal conductivity of matrix material through the approach of the composite structure of change matrix material; Particularly fibrous and flake shape filler forms the heat conduction network of matrix material effectively; Thereby the thermal conductivity of matrix material is obviously improved, and performances such as dielectric, physical strength also are significantly improved simultaneously.
The foregoing description can also be enumerated a lot; Here do not provide one by one, so long as in scope disclosed by the invention, promptly difform metal is prepared the metal/metal oxide structured packing; Grain diameter is in the scope of micron and Nano grade; And organic solvent, the coupling agent of the selection of preparation process, in the process parameters range that the preparation method provides, all can be prepared into the polymer matrix composite of different shapes metal as filler.
Claims (10)
1. polymer matrix composite; It is characterized in that: this matrix material by volume mark is made up of 1～50% metallic stuffing and 50～99% polymeric matrix; Said metallic stuffing comprises metal passivation particle and fibrous metal or sheet metal, and the mass ratio of metal passivation particle and fibrous metal or sheet metal is 1: 1.
2. according to the said a kind of polymer matrix composite of claim 1; It is characterized in that: said metal passivation particle comprises the metal passivation particle of micron grain size and the metal passivation particle of nanometer particle size; The metal passivation particulate volume ratio of the metal passivation particle of micron grain size and nanometer particle size is 5～30: 1; The metal passivation particulate diameter of micron grain size is 1～19 μ m; The metal passivation particulate diameter of nanometer particle size is 10～90nm, and the length of fibrous metal is that 3mm, diameter are 50 μ m～1mm, and the area of sheet metal is that 3～5mm * 3～5mm, thickness are 1～9 μ m.
3. according to the said a kind of polymer matrix composite of claim 1; It is characterized in that: said metal passivation particle is to be prepared from after the powder with Al, Fe, Cr, Mo, Ni, Co, Ta, Nb or W utilizes strong oxidizer oxidation style or the passivation of air heating oxidation style; Strong oxidizer is the vitriol oil, nitric acid, chloric acid, acid iodide, SRM 935a or potassium permanganate, and fibrous metal or sheet metal adopt aluminium, copper, iron or silvery to be equipped with.
4. according to the said a kind of polymer matrix composite of claim 1, it is characterized in that: said polymeric matrix is PVDF or its multipolymer, Vestolen PP 7052, Vilaterm, Vestolen PP 7052 methyl acid methyl esters, epoxy resin or polyimide.
5. according to the said a kind of polymer matrix composite of claim 1, it is characterized in that: the complex method of said metallic stuffing and polymeric matrix comprises admixture of powder method, solution method or pressure sintering.
6. one kind prepares the method for polymer matrix composite according to claim 1, it is characterized in that: may further comprise the steps:
Step 1: metal-powder is broken for micron metal powder and nano metal powder respectively;
Step 2: utilize the air heating oxidation style to carry out passivation respectively micron metal powder and nano metal powder, obtain the metal passivation particle of micron grain size and nanometer particle size;
Step 3: adopting mechanical cutting to prepare length is that 3mm, diameter are the fibrous metal of 50 μ m～1mm or to prepare area be that 3～5mm * 3～5mm, thickness are the sheet metal of 1～9 μ m;
Step 4: immerse the metal passivation particle of micron grain size and nanometer particle size in the organic solvent respectively; The coupling agent that adds organic solvent quality 1～2.5% then; Supersound process makes the metal passivation particle surface coat one deck coupling agent uniformly after adding coupling agent, carries out dry evaporative removal organic solvent after the supersound process;
Step 5: through after the step 4 with the volume ratio mixing of the metal passivation particle of micron grain size and nanometer particle size according to 5～30:1, take by weighing fibrous metal or sheet metal with quality such as mixed metal passivation particle;
Step 6: through after the step 5 with mixed metal passivation particle and polymeric matrix mix mixture, mixture and fibrous metal or sheet metal are put into the hot-forming polymer matrix composite that promptly makes of mould after compound.
7. according to the said a kind of method for preparing polymer matrix composite of claim 6; It is characterized in that: said metal-powder is the powder of aluminium, chromium, nickel, iron or molybdenum; The step of said air heating oxidation style is: aerating oxygen in metal-powder, and following dry 3～5 hours in 120 ℃ then.
8. according to the said a kind of method for preparing polymer matrix composite of claim 6, it is characterized in that: said organic solvent is an absolute ethyl alcohol, and coupling agent is a silane coupling agent.
9. according to the said a kind of method for preparing polymer matrix composite of claim 6, it is characterized in that: the volume(tric)fraction of polymeric matrix is 50% in the said polymer matrix composite.
10. according to the said a kind of method for preparing polymer matrix composite of claim 6, it is characterized in that: said hot-forming condition is: temperature is 200 ℃, and pressure is 50MPa, and the time is 25 minutes.
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