CN102993751A - High-thermal-conductivity and high-strength insulating PPS (polyphenylene sulfite) composite material and preparation method for same - Google Patents
High-thermal-conductivity and high-strength insulating PPS (polyphenylene sulfite) composite material and preparation method for same Download PDFInfo
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Abstract
The invention discloses a high-thermal-conductivity and high-strength insulating PPS (polyphenylene sulfite) composite material and a preparation method for the same. The high-thermal-conductivity and high-strength insulating PPS composite material disclosed by the invention is composed of polyphenylene sulfite resin, carbon fibres, an inorganic filler subjected to plasma surface activating treatment, high-thermal-conductivity Si3N4 and a thermal stabilizer. The preparation method comprises the following steps of: 1) cleaning the inorganic filler and performing surface activating treatment; 2) performing oxidation thermal crosslinking treatment on polyphenylene sulfite resin; 3) placing the inorganic filler, the polyphenylene sulfite resin, the high-thermal-conductivity Si3N4 and the thermal stabilizer in a high-speed stirrer and uniformly mixing with a high speed; and 4) mixing the mixed material aforementioned with carbon fibres in a double-screw extruder, performing melt extrusion and granulating. The PPS composite material prepared by the scheme disclosed by the invention has the advantages of high thermal conductivity, high insulativity and high mechanical strength; and moreover, the production process is simple, easy to realize, and capable of being widely applied to the technical fields of electronic and electric components, machinery, automotive parts and the like.
Description
Technical field
The present invention relates to technical field of polymer composite materials, relate in particular to a kind of high conductive high strength insulation PPS matrix material and preparation method thereof.
Background technology
Flourish along with the new industry such as the progress of polymer science technology and information in recent years, macromolecular material is proposed new performance requriements, macromolecular material begins to become the good conductor of heat, has played the part of the key player in heat conduction field, has overturned traditional heat insulation concept of plastics macromolecular material.Heat-conductive composite material is compared with metallic substance, and following several large advantage is specifically arranged: the first, and lightweight; The second, design freedom is high; The 3rd, machine-shaping is convenient; The 4th, good insulation preformance; The 5th, need not secondary processing, more environmental protection.
Polyphenylene sulfide (PPS) claims again polyphenylene sulfide, poly-inferior (inferior) aralkyl sulfid, a kind of lightweight, high performance material, application in electronics, automobile, precision optical machinery and aerospace, military equipment just more and more comes into one's own, and especially uses at advanced composite material to have potential quality.The link configuration unit of PPS is very simple, firm monomer is given at high temperature very high intensity, rigidity retention rate of material, stronger crystallization trend and larger degree of crystallinity are arranged, yet, simultaneously also because on the PPS main chain a large amount of phenyl ring are arranged, and degree of crystallinity is very high, makes its elongation at break low, and toughness, shock resistance are also relatively poor; On the other hand, the PPS thermal conductivity is lower, is the poor conductor of heat.These shortcomings have limited its application to a certain extent.Therefore, it is carried out study on the modification imperative.
Prior art mostly concentrates on the research of PPS matrix material and uses fiber reinforced material, such as glass and carbon fiber, also has the mineral filler of coupling agent treatment, nitride or oxidate nano particulate such as various high thermal conductivity, make the structure of PPS matrix material obtain enhancing, performance makes moderate progress, and has also produced following counter productive: a. and has added the insulativity that too much carbon fiber can affect the PPS matrix material, adding glass then can cause product surface irregularity to occur, jagged phenomenon; B. adopt the mineral filler of coupling agent treatment because agglomerate easily appears in surface-area effects, strengthened the preparation difficulty of product, performance also has been subject to impact; C. the common mineral filler of the employing of high fill-ratio has improved the thermal conductivity of PPS matrix material, has but reduced its physical strength.
Summary of the invention
The object of the invention is to overcome above-mentioned shortcoming of the prior art and provide a kind of thermal conductivity good, high-insulation, high mechanical strength, PPS matrix material that manufacture craft is simple, specious, be easy to realize and preparation method thereof.
For achieving the above object, the technical solution adopted in the present invention is:
A kind of high conductive high strength insulation PPS matrix material is characterized in that, consists of by mass percentage:
Described polyphenylene sulfide is the modified linear polyphenylene sulfide, and molecular weight is greater than 100000.
Described carbon fiber is chopped strand, and chopped length is 5-12nm.
The mineral filler of described plasma surface activation treatment refers to process the mineral filler that obtains through dielectric barrier discharge.
Described dielectric barrier discharge is treated to sparking voltage 500-10000V, treatment time 10-40min.
The mixture that the mineral filler of described plasma surface activation treatment is comprised of nano aluminum nitride powder and inorganic crystal whisker.
Described nano aluminum nitride powder, by sheet and particulate state nano aluminum nitride powder by volume 1:6 mix, wherein the major diameter of sheet aluminium nitride powder is 100-300nm, the particle diameter of particulate state nitrogenize aluminium powder form is 5-20nm.
Described inorganic crystal whisker is one or more the mixture in silicon carbide whisker, calcium sulfate crystal whiskers, barium sulfate crystal whisker, magnesium sulfate crystal whisker, calcium carbonate crystal whisker, the magnesium carbonate whisker, and whisker length is 10-25 μ m.
Described high thermal conductivity Si
3N
4Be to add the seed particles that order orientation is arranged in material powder, form the fibrous silicon nitride with oriented structure, its particle diameter is 5～20 μ m.
Described thermo-stabilizer is one or both the mixture in Fatty Alcohol(C12-C14 and C12-C18) polyoxy vinylbenzene ether phosphate salt and the trisnonyl phenyl phosphite.
PPS composite manufacture method of the present invention comprises the steps:
(1) takes by weighing the mixture of nano aluminum nitride powder and inorganic crystal whisker, put into acetone and clean and soak 10min to remove surface contaminants, clean with distilled water after taking out and remove residual acetone, be placed on clean open spaces and dry;
(2) powder processing is put in the mineral filler of step (1) being processed gained, slowly passes into helium, carries out dielectric barrier discharge, and sparking voltage is 500-10000V, and the treatment time is 10-40min, is stored in the helium stand-by after being disposed;
(3) the poly-p-phenylene sulfide ether resin is made heat of oxidation crosslinking Treatment, and treatment temp is controlled at 250-280 ℃, the crosslinked 2-4 of the heat of oxidation hour;
(4) take by weighing by mass percentage mineral filler that the dielectric barrier discharge of above-mentioned steps gained processes and the polyphenylene sulfide of heat of oxidation crosslinking Treatment, put into homogenizer, add high thermal conductivity Si
3N
4And thermo-stabilizer, high-speed mixing is even;
(5) above-mentioned compound is mixed with carbon fiber in twin screw extruder, through melt extruding, granulation obtains high conductive high strength insulation PPS matrix material.
Compare with prior art, characteristics and beneficial effect that the present invention possesses are:
(1) introduces chopped carbon fiber, realized that following effect: a. increases the directed capacity of heat transmission; B. increase intensity and the toughness of material; C. product surface is relatively smooth, attractive in appearance, can not occur surface irregularity, jagged phenomenon as the matrix material that has added glass fibre;
(2) mineral filler had both reduced surface energy through the plasma surface activation treatment, avoided agglomerate, had improved again wettability and adhesivity, had improved its dispersiveness and binding property in resin matrix; The compound inorganic stuffing combination of long drives and drop shots of selecting is had complementary advantages, and efficient enhancing and toughening effect have been played in the combination of material, gives good physical strength and the shock-resistance of PPS matrix material that the present invention makes, and has improved processing characteristics; Sheet and particulate state nano aluminum nitride powder mix combines closely mutually afterwards, allows form maximum degree of piling up between filler, makes the heat conduction network in the system form to the full extent high heat conductive body system, thereby realizes effective thermal conduction;
(3) the high thermal conductivity Si that adopts
3N
4In material powder, add seed particles, and the arrangement of seed particles order orientation, form the filamentary structure with orientation, make Si
3N
4Thermal conductivity present anisotropy, thermal conductivity is 120W/mK on structural approach, is common Si
3N
43 times, be equivalent to the thermal conductivity of steel, greatly improved the heat-conducting effect of PPS matrix material.
Embodiment
Preparation method of the present invention is as follows:
(1) takes by weighing the mixture of nano aluminum nitride powder and inorganic crystal whisker, put into acetone and clean and soak 10min to remove surface contaminants, clean with distilled water after taking out and remove residual acetone, be placed on clean open spaces and dry;
(2) powder processing is put in the mineral filler of step (1) being processed gained, slowly passes into helium, carries out dielectric barrier discharge, and sparking voltage is 500-10000V, and the treatment time is 10-40min, is stored in the helium stand-by after being disposed;
(3) the poly-p-phenylene sulfide ether resin is made heat of oxidation crosslinking Treatment, and treatment temp is controlled at 250-280 ℃, the crosslinked 2-4 of the heat of oxidation hour;
(4) take by weighing by mass percentage mineral filler that the dielectric barrier discharge of above-mentioned steps gained processes and the polyphenylene sulfide of heat of oxidation crosslinking Treatment, put into homogenizer, add high thermal conductivity Si
3N
4And thermo-stabilizer, high-speed mixing is even;
(5) above-mentioned compound is mixed with carbon fiber in twin screw extruder, through melt extruding, cooling granulation obtains high conductive high strength insulation PPS matrix material.
In order to deepen the understanding of the present invention, the invention will be further described below by embodiment.Described embodiment only technical scheme of the present invention does not consist of the restriction to rights protection scope of the present invention for illustrating.
Embodiment 1
(1) takes by weighing the mixture of nano aluminum nitride powder and silicon carbide whisker, barium sulfate crystal whisker, put into acetone and clean and soak 10min to remove surface contaminants, clean with distilled water after taking out and remove residual acetone, be placed on clean open spaces and dry.
(2) powder processing is put in the mineral filler of step (1) being processed gained, slowly passes into helium, carries out dielectric barrier discharge, and sparking voltage is 1000V, and the treatment time is 35min, is stored in the helium stand-by after being disposed.
(3) the poly-p-phenylene sulfide ether resin is made heat of oxidation crosslinking Treatment, and treatment temp is controlled at 250 ℃, crosslinked 4 hours of the heat of oxidation.
(4) take by weighing 15kg mineral filler that the dielectric barrier discharge of above-mentioned steps gained processes and the polyphenylene sulfide of 74kg heat of oxidation crosslinking Treatment, put into homogenizer, add 8kg high thermal conductivity Si
3N
4With the mixture of 1.3kg Fatty Alcohol(C12-C14 and C12-C18) polyoxy vinylbenzene ether phosphate salt and trisnonyl phenyl phosphite, high-speed mixing is even.
(5) above-mentioned compound is mixed with the 10kg carbon fiber in twin screw extruder, through melt extruding, cooling granulation obtains high conductive high strength insulation PPS matrix material.
Embodiment 2
(1) takes by weighing the mixture of nano aluminum nitride powder and calcium sulfate crystal whiskers, magnesium sulfate crystal whisker, magnesium carbonate whisker, put into the acetone cleaning and soak 10min to remove surface contaminants, clean the removal residual acetone with distilled water after taking out, be placed on clean open spaces and dry.
(2) powder processing is put in the mineral filler of step (1) being processed gained, slowly passes into helium, carries out dielectric barrier discharge, and sparking voltage is 3000V, and the treatment time is 30min, is stored in the helium stand-by after being disposed.
(3) the poly-p-phenylene sulfide ether resin is made heat of oxidation crosslinking Treatment, and treatment temp is controlled at 280 ℃, crosslinked 2 hours of the heat of oxidation.
(4) take by weighing 17.2kg mineral filler that the dielectric barrier discharge of above-mentioned steps gained processes and the polyphenylene sulfide of 54kg heat of oxidation crosslinking Treatment, put into homogenizer, add 7.6kg high thermal conductivity Si
3N
4With 0.9kg Fatty Alcohol(C12-C14 and C12-C18) polyoxy vinylbenzene ether phosphate salt, high-speed mixing is even.
(5) above-mentioned compound is mixed with the 12kg carbon fiber in twin screw extruder, through melt extruding, cooling granulation obtains high conductive high strength insulation PPS matrix material.
Embodiment 3
(1) takes by weighing the mixture of nano aluminum nitride powder and calcium carbonate crystal whisker, magnesium carbonate whisker, put into acetone and clean and soak 10min to remove surface contaminants, clean with distilled water after taking out and remove residual acetone, be placed on clean open spaces and dry.
(2) powder processing is put in the mineral filler of step (1) being processed gained, slowly passes into helium, carries out dielectric barrier discharge, and sparking voltage is 5000V, and the treatment time is 20min, is stored in the helium stand-by after being disposed.
(3) the poly-p-phenylene sulfide ether resin is made heat of oxidation crosslinking Treatment, and treatment temp is controlled at 270 ℃, crosslinked 3.2 hours of the heat of oxidation.
(4) take by weighing 25kg mineral filler that the dielectric barrier discharge of above-mentioned steps gained processes and the polyphenylene sulfide of 67kg heat of oxidation crosslinking Treatment, put into homogenizer, add 9kg high thermal conductivity Si
3N
4With the 1kg trisnonyl phenyl phosphite, high-speed mixing is even.
(5) above-mentioned compound is mixed with the 8.7kg carbon fiber in twin screw extruder, through melt extruding, cooling granulation obtains high conductive high strength insulation PPS matrix material.
Embodiment 4
(1) takes by weighing the mixture of nano aluminum nitride powder and barium sulfate crystal whisker, put into acetone and clean and soak 10min to remove surface contaminants, clean with distilled water after taking out and remove residual acetone, be placed on clean open spaces and dry.
(2) powder processing is put in the mineral filler of step (1) being processed gained, slowly passes into helium, carries out dielectric barrier discharge, and sparking voltage is 7000V, and the treatment time is 13min, is stored in the helium stand-by after being disposed.
(3) the poly-p-phenylene sulfide ether resin is made heat of oxidation crosslinking Treatment, and treatment temp is controlled at 265 ℃, crosslinked 4 hours of the heat of oxidation.
(4) take by weighing 31.5kg mineral filler that the dielectric barrier discharge of above-mentioned steps gained processes and the polyphenylene sulfide of 58kg heat of oxidation crosslinking Treatment, put into homogenizer, add 8.4kg high thermal conductivity Si
3N
4With the mixture of 0.8kg Fatty Alcohol(C12-C14 and C12-C18) polyoxy vinylbenzene ether phosphate salt and trisnonyl phenyl phosphite, high-speed mixing is even.
(5) above-mentioned compound is mixed with the 7.5kg carbon fiber in twin screw extruder, through melt extruding, cooling granulation obtains high conductive high strength insulation PPS matrix material.
Embodiment 5
(1) takes by weighing the mixture of nano aluminum nitride powder and silicon carbide whisker, magnesium sulfate crystal whisker, put into acetone and clean and soak 10min to remove surface contaminants, clean with distilled water after taking out and remove residual acetone, be placed on clean open spaces and dry.
(2) nano aluminum nitride powder of step (1) being processed gained is put into powder processing, slowly passes into helium, carries out dielectric barrier discharge, and sparking voltage is 10000V, and the treatment time is 10min, is stored in the helium stand-by after being disposed.
(3) the poly-p-phenylene sulfide ether resin is made heat of oxidation crosslinking Treatment, and treatment temp is controlled at 275 ℃, crosslinked 3.5 hours of the heat of oxidation.
(4) take by weighing 34kg mineral filler and the 64kg polyphenylene sulfide that the dielectric barrier discharge of above-mentioned steps gained is processed, put into homogenizer, add 8kg high thermal conductivity Si
3N
4With the 1.1kg trisnonyl phenyl phosphite, high-speed mixing is even.
(5) above-mentioned compound is mixed with the 14kg carbon fiber in twin screw extruder, through melt extruding, cooling granulation obtains high conductive high strength insulation PPS matrix material.
Embodiment 6
(1) takes by weighing the mixture of nano aluminum nitride powder and calcium carbonate crystal whisker, put into acetone and clean and soak 10min to remove surface contaminants, clean with distilled water after taking out and remove residual acetone, be placed on clean open spaces and dry.
(2) powder processing is put in the mineral filler of step (1) being processed gained, slowly passes into helium, carries out dielectric barrier discharge, and sparking voltage is 500V, and the treatment time is 40min, is stored in the helium stand-by after being disposed.
(3) the poly-p-phenylene sulfide ether resin is made heat of oxidation crosslinking Treatment, and treatment temp is controlled at 255 ℃, crosslinked 2.5 hours of the heat of oxidation.
(4) take by weighing 41kg mineral filler that the dielectric barrier discharge of above-mentioned steps gained processes and the polyphenylene sulfide of 45kg heat of oxidation crosslinking Treatment, put into homogenizer, add 10.6kg high thermal conductivity Si
3N
4With 1.2kg Fatty Alcohol(C12-C14 and C12-C18) polyoxy vinylbenzene ether phosphate salt, high-speed mixing is even.
(5) above-mentioned compound is mixed with the 11.3kg carbon fiber in twin screw extruder, through melt extruding, cooling granulation obtains high conductive high strength insulation PPS matrix material.
Embodiment 1～6 prepared product is carried out performance test, and the result is as shown in the table:
Comprehensively upper table obtained experimental data as can be known: the PPS matrix material that adopts scheme of the present invention to make has advantages of high heat conduction, high-insulation and high mechanical strength, and manufacture craft is simple, be easy to realize, can be widely used in the technical fields such as electrical and electronic component, machinery, auto parts machinery.The present invention accomplishes the end in view.
Claims (11)
1. a high conductive high strength insulation PPS matrix material is characterized in that, consists of by mass percentage:
2. high conductive high strength insulation PPS matrix material according to claim 1 is characterized in that, described polyphenylene sulfide is the modified linear polyphenylene sulfide, and molecular weight is greater than 100000.
3. require described high conductive high strength insulation PPS matrix material according to right 1, it is characterized in that, described carbon fiber is chopped strand, and chopped length is 5-12nm.
4. high conductive high strength insulation PPS matrix material according to claim 1 is characterized in that, the mineral filler of described plasma surface activation treatment refers to process the mineral filler that obtains through dielectric barrier discharge.
5. according to claim 1 or 4 described high conductive high strengths insulation PPS matrix materials, it is characterized in that, described dielectric barrier discharge is treated to sparking voltage 500-10000V, treatment time 10-40min.
6. according to claim 1 or 4 described high conductive high strengths insulation PPS matrix materials, it is characterized in that the mixture that the mineral filler of described plasma surface activation treatment is comprised of nano aluminum nitride powder and inorganic crystal whisker.
7. high conductive high strength according to claim 6 insulation PPS matrix material, it is characterized in that, described nano aluminum nitride powder, by sheet and particulate state nano aluminum nitride powder by volume 1:6 mix, wherein the major diameter of sheet aluminium nitride powder is 100-300nm, and the particle diameter of particulate state nitrogenize aluminium powder form is 5-20nm.
8. high conductive high strength according to claim 6 insulation PPS matrix material, it is characterized in that, described inorganic crystal whisker is one or more the mixture in silicon carbide whisker, calcium sulfate crystal whiskers, barium sulfate crystal whisker, magnesium sulfate crystal whisker, calcium carbonate crystal whisker, the magnesium carbonate whisker, and whisker length is 10-25 μ m.
9. high conductive high strength insulation PPS matrix material according to claim 1 is characterized in that described high thermal conductivity Si
3N
4Be to add the seed particles that order orientation is arranged in material powder, form the fibrous silicon nitride with oriented structure, its particle diameter is 5～20 μ m.
10. high conductive high strength according to claim 1 insulation PPS matrix material is characterized in that, described thermo-stabilizer is one or both the mixture in Fatty Alcohol(C12-C14 and C12-C18) polyoxy vinylbenzene ether phosphate salt and the trisnonyl phenyl phosphite.
11. a method for preparing high conductive high strength insulation PPS matrix material claimed in claim 1 is characterized in that, comprises the steps:
(1) takes by weighing the mixture of nano aluminum nitride powder and inorganic crystal whisker, put into acetone and clean and soak 10min to remove surface contaminants, clean with distilled water after taking out and remove residual acetone, be placed on clean open spaces and dry;
(2) powder processing is put in the mineral filler of step (1) being processed gained, slowly passes into helium, carries out dielectric barrier discharge, and sparking voltage is 500-10000V, and the treatment time is 10-40min, is stored in the helium stand-by after being disposed;
(3) the poly-p-phenylene sulfide ether resin is made heat of oxidation crosslinking Treatment, and treatment temp is controlled at 250-280 ℃, the crosslinked 2-4 of the heat of oxidation hour;
(4) take by weighing by mass percentage mineral filler that the dielectric barrier discharge of above-mentioned steps gained processes and the polyphenylene sulfide of heat of oxidation crosslinking Treatment, put into homogenizer, add high thermal conductivity Si
3N
4And thermo-stabilizer, high-speed mixing is even;
(5) above-mentioned compound is mixed with carbon fiber in twin screw extruder, through melt extruding, cooling granulation obtains high conductive high strength insulation PPS matrix material.
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| CN104788955A (en) * | 2015-04-17 | 2015-07-22 | 广西藤县通轩立信化学有限公司 | Heat-conducting resin composition |
| CN107011658A (en) * | 2017-04-07 | 2017-08-04 | 中国科学院兰州化学物理研究所 | It is a kind of suitable for polyphenylene sulfide base self-lubricating nano composite material of diesel fuel lubricity and preparation method thereof |
| CN109294128A (en) * | 2018-09-28 | 2019-02-01 | 安徽省永欣织带有限公司 | A kind of thermally conductive ribbon of flexible insulation |
| CN110066577A (en) * | 2019-04-30 | 2019-07-30 | 中国船舶重工集团公司第七二五研究所 | Titanium alloy and carbon fibre composite bonding insulating coating and its adhering method |
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| JPWO2021246268A1 (en) * | 2020-06-02 | 2021-12-09 |
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| CN104788955A (en) * | 2015-04-17 | 2015-07-22 | 广西藤县通轩立信化学有限公司 | Heat-conducting resin composition |
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| C14 | Grant of patent or utility model | ||
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Address after: 529728 Jiangmen City, Heshan Province, Republican Town, Xianghe Road, No. H, building, 326 Patentee after: Heshan Tongfang Lighting Technology Co., Ltd. Address before: 529728 Jiangmen City, Heshan Province, Republican Town, Xianghe Road, No. H, building, 326 Patentee before: Heshan Lide Electronic Industry Co., Ltd. |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20141217 Termination date: 20191203 |