CN114031934A - Polyamide composite material with high thermal conductivity coefficient and preparation method thereof - Google Patents
Polyamide composite material with high thermal conductivity coefficient and preparation method thereof Download PDFInfo
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- CN114031934A CN114031934A CN202111533040.9A CN202111533040A CN114031934A CN 114031934 A CN114031934 A CN 114031934A CN 202111533040 A CN202111533040 A CN 202111533040A CN 114031934 A CN114031934 A CN 114031934A
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- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention belongs to the technical field of composite materials, and relates to a polyamide composite material with high heat conductivity coefficient, which comprises the following components in percentage by mass: polyamide: 40-80 wt%; one-dimensional heat-conducting filler: 10 to 50 wt%; modified second phase polymer: 10-20 wt%; wherein the modified second phase polymer is a mixture of the second phase polymer and the two-dimensional heat-conducting filler, and the second phase polymer is a polymer material incompatible with polyamide. By introducing an incompatible second phase into polyamide and improving the heat-conducting property of the second phase, a heat-conducting enrichment phase is formed, and a one-dimensional heat-conducting filler is introduced to construct an effective heat-conducting network, so that the heat-conducting coefficient and the mechanical property of the polyamide are greatly improved.
Description
Technical Field
The invention belongs to the technical field of composite materials, and relates to a polyamide composite material with high heat conductivity coefficient and a preparation method thereof.
Background
With the continuous development of modern industry, various electronic devices such as LED lamps are continuously developed toward miniaturization and integration. The smaller space and the concentrated heat generation increase the temperature of the electronic device during operation, which not only can reduce the working efficiency and stability of the electronic device, but also can obviously reduce the service life of the electronic device, thereby increasing the cost. The traditional electronic device packaging material is metal or ceramic, which has high heat conductivity coefficient, but the specific gravity of the two materials is often high, and the two materials have certain forming difficulty. The polymer composite material has obvious advantages in many aspects, such as small specific gravity, easy molding, low cost, excellent mechanical property and the like, and is gradually replacing metal and ceramic to become common electronic device packaging materials. However, the thermal conductivity of the polymer is generally low, and it is difficult to meet the requirement of the electronic component on the operating temperature. Therefore, the polymer composite material with higher thermal conductivity coefficient is developed on the basis of keeping the advantages of the polymer.
The advantage of easy modification of the polymer gives the polymer a multifunctional possibility, and the addition of the heat-conducting filler in the aspect of heat-conducting property can improve the heat-conducting coefficient of the polymer composite material to a certain extent, which is also the most common strategy. According to the difference of the thermal conductivity coefficient, the morphology and the like of the used filler, the thermal conductivity coefficient of the final composite material also has a certain difference. In addition, when the amount of the thermal conductive filler added is small, the thermal conductivity of the polymer is not greatly improved, and when the thermal conductive filler is added in a high proportion, the thermal conductivity starts to increase relatively quickly because the fillers are in contact with each other to form a thermal conductive path having a high thermal conductivity. However, the higher thermal conductive filler tends to reduce the advantages of the polymer itself, such as the processing and forming properties, partial mechanical properties, etc., and a strategy with higher efficiency of improving the thermal conductivity coefficient needs to be developed.
In recent years, many studies have been conducted to more effectively increase the thermal conductivity of polymers. For example, fillers of various sizes are used, and the size synergy between the fillers is utilized, namely, the fillers with large sizes provide a heat conduction network, and the fillers with small sizes fill gaps, so that a complete heat conduction network is formed. There are also various forms of fillers used, such as synergistic effects between plate-like and rod-like fillers, to compensate for possible anisotropy of the fillers. However, the improvement of the thermal conductivity of these polymers cannot meet the requirement of high thermal conductivity of electronic components, and therefore, there is a need to further develop a polymer composite material having excellent thermal conductivity and mechanical properties.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a polyamide composite material, which is characterized in that a heat conduction enrichment phase is formed by introducing an incompatible second phase into polyamide and improving the heat conduction performance of the second phase, and an effective heat conduction network is constructed by introducing a one-dimensional heat conduction filler, so that the heat conduction coefficient and the mechanical property of the polyamide are greatly improved.
The invention provides a polyamide composite material with high thermal conductivity, which comprises the following components in percentage by mass:
polyamide: 40-80 wt%;
one-dimensional heat-conducting filler: 10 to 50 wt%;
modified second phase polymer: 10-20 wt%;
wherein the modified second-phase polymer is a mixture of the second-phase polymer and the two-dimensional heat-conducting filler.
Preferably, the second phase polymer is a polymeric material that is incompatible with the polyamide.
Preferably, the second phase polymer is one or more of POE-g-MAH, PE-g-MAH, EPDM-g-MAH, PP-g-MAH, PPO-g-MAH and PE-g-MAH.
Preferably, the two-dimensional heat-conducting filler is one or more of two-dimensional flaky boron nitride, two-dimensional flaky alumina, two-dimensional flaky aluminum nitride, two-dimensional flaky silicon nitride and two-dimensional MXene.
Preferably, the mass ratio of the second-phase polymer to the two-dimensional heat-conducting filler is (2-4): (1-3).
Preferably, the modified second phase polymer is obtained from a preparation process comprising the steps of: and dispersing the second-phase polymer in an organic solvent, heating, refluxing and stirring, then adding the two-dimensional heat-conducting filler, continuing heating, refluxing and stirring, finally pouring the mixture into the second solvent, filtering and drying to obtain the modified second-phase polymer.
The organic solvent is tetrahydrofuran and the like, and the second solvent is ethanol, water, diethyl ether, acetone, toluene and the like.
Preferably, the modified second phase polymer is obtained from a preparation process comprising the steps of: and mixing the second-phase polymer and the two-dimensional heat-conducting filler, and adding the mixture into a screw extruder for melting and granulation to obtain the modified second-phase polymer.
Preferably, the one-dimensional heat-conducting filler is one or two of glass fiber and whisker.
Preferably, the whisker is one or more of magnesium oxide whisker, zinc oxide whisker, aluminum nitride whisker, aluminum oxide whisker, boron nitride whisker and silicon carbide whisker.
The second aspect of the invention provides a preparation method of a polyamide composite material with high thermal conductivity, which comprises the following steps:
mixing polyamide, one-dimensional heat-conducting filler and modified second-phase polymer, adding the mixture into a screw extruder, and extruding and granulating to obtain the polyamide composite material with high heat conductivity coefficient.
Compared with the prior art, the invention has the following beneficial effects:
1. the two-dimensional heat-conducting filler and the second-phase polymer are mixed in advance to form a mixture of the two, then the mixture and polyamide are mixed and extruded, the second-phase polymer forms a second phase in a polyamide matrix under the action of orientation and phase separation during extrusion processing, and the two-dimensional heat-conducting filler is uniformly dispersed in the second phase to form a heat-conducting enrichment phase; one-dimensional heat-conducting filler is added along with the modified second-phase polymer, and can be used as a bridge for connecting heat-conducting aggregation phases in the extrusion processing process to connect heat-conducting enrichment phases to form a heat-conducting path, so that the heat-conducting coefficient of the polymer is greatly improved.
2. The second-phase polymer introduced by the invention can also improve the comprehensive performance of the polyamide composite material and improve the feasibility of industrialization.
3. The modified second-phase polymer can be obtained by a simple solution mixing or extrusion mixing method, the modified second-phase polymer can obtain the heat-conducting enrichment phase in the process of blending and extruding with polyamide, and the preparation method of the heat-conducting enrichment phase is very simple.
4. The preparation method of the polyamide composite material with high thermal conductivity coefficient is very simple, can be realized by extrusion processing, and is very suitable for industrial production.
Drawings
FIG. 1 is a schematic diagram of the preparation of a polyamide composite material with high thermal conductivity according to the present invention;
FIG. 2 is a flow chart of a method for preparing a high thermal conductivity polyamide composite material according to the present invention;
FIG. 3 is a schematic diagram of the preparation of a polyamide composite material of comparative example 1.
Detailed Description
Hereinafter, embodiments will be described in detail with respect to the high thermal conductivity polyamide composite material of the present invention and the method of preparing the same, however, the embodiments are exemplary and the present disclosure is not limited thereto. And the drawings used herein are for the purpose of illustrating the disclosure better and are not intended to limit the scope of the invention.
The polyamide composite material with high thermal conductivity provided by some embodiments of the invention comprises the following components in percentage by mass: polyamide: 40-80 wt%; one-dimensional heat-conducting filler: 10 to 50 wt%; modified second phase polymer: 10-20 wt%; wherein the modified second phase polymer is a mixture of the second phase polymer and the two-dimensional heat-conducting filler, and the second phase polymer is a polymer material incompatible with polyamide.
The preparation schematic diagram of the polyamide composite material with high thermal conductivity is shown in figure 1: the two-dimensional heat-conducting filler and the second-phase polymer are mixed in advance to form a mixture of the two, then the mixture and the polyamide are mixed and extruded, the second-phase polymer forms a second phase in a polyamide matrix under the action of orientation and phase separation during extrusion processing, the two-dimensional heat-conducting filler is uniformly dispersed in the second phase to form a heat-conducting enrichment phase, and the introduction of the second phase can also improve the comprehensive performance of a polymer base material. The one-dimensional heat conducting filler is added along with the modified second-phase polymer, is in a linear or rod-shaped structure, and is used as a bridge for connecting a heat conducting aggregation phase in the extrusion processing process to connect heat conducting enrichment to form a heat conducting passage, so that the heat conducting coefficient of the polymer is greatly improved.
According to the invention, the second phase, the two-dimensional heat-conducting filler and the one-dimensional heat-conducting filler are introduced, and the heat-conducting property and the mechanical property of the polymer base material are improved by utilizing the orientation and phase separation effects during extrusion processing.
The polyamide in some embodiments of the invention is preferably one or both of PA6, PA 66.
The second phase polymer of the invention is a polymer material incompatible with polyamide, and is preferably one or more of POE-g-MAH, PE-g-MAH, EPDM-g-MAH, PP-g-MAH, PPO-g-MAH and PE-g-MAH.
The one-dimensional heat conductive filler in the present invention refers to a heat conductive filler having a linear, rod-like, tubular structure or the like, and is preferably one or both of glass fiber and whisker. The whisker is further preferably one or more of a magnesium oxide whisker, a zinc oxide whisker, an aluminum nitride whisker, an aluminum oxide whisker, a boron nitride whisker and a silicon carbide whisker.
The two-dimensional heat-conducting filler refers to a flaky heat-conducting filler, and is preferably one or more of two-dimensional flaky boron nitride, two-dimensional flaky alumina, two-dimensional flaky aluminum nitride, two-dimensional flaky silicon nitride and two-dimensional MXene.
The preparation method of the polyamide composite material with high thermal conductivity provided in some embodiments of the present invention, as shown in fig. 2, includes the following steps:
and S1, mixing the second-phase polymer with a two-dimensional heat-conducting filler to obtain the modified second-phase polymer. The mixing means includes solvent mixing and extrusion mixing. The solvent mixing comprises the following steps: and dispersing the second-phase polymer in an organic solvent, heating, refluxing and stirring, then adding the two-dimensional heat-conducting filler, continuing heating, refluxing and stirring, finally pouring the mixture into the second solvent, filtering and drying to obtain the modified second-phase polymer. The organic solvent is tetrahydrofuran and the like, and the second solvent is ethanol, water, diethyl ether, acetone, toluene and the like.
The extrusion mixing comprises the following steps: and mixing the second-phase polymer and the two-dimensional heat-conducting filler, and adding the mixture into a screw extruder for melting and granulation to obtain the modified second-phase polymer. The rotation speed of the screw extruder is preferably 200-500 rpm, the temperature of the screw extruder from a feed port is 210-230 ℃, 230-245 ℃ and the head temperature is 230-240 ℃.
S2, mixing the polyamide, the one-dimensional heat-conducting filler and the modified second-phase polymer, and adding the mixture into a screw extruder for extrusion and granulation to obtain the polyamide composite material with high heat conductivity coefficient. The rotation speed of the screw extruder is preferably 200-500 rpm, the temperature of the screw extruder from a feed port is 210-230 ℃, 230-245 ℃ and the head temperature is 230-240 ℃.
The technical solutions of the present invention are further described and illustrated by the following specific embodiments and the accompanying drawings, it should be understood that the specific embodiments and the accompanying drawings described herein are only for better illustrating the present disclosure, and do not limit the scope of protection. The raw materials used in the examples of the present invention are those commonly used in the art, and the methods used in the examples are those conventional in the art, unless otherwise specified.
Example 1
The polyamide composite material with high thermal conductivity coefficient comprises the following components in percentage by mass: PA 6: 40 wt%, magnesium oxide whisker: 45 wt%; modified POE-g-MAH: 15 wt%, wherein the modified POE-g-MAH is a mixture of POE-g-MAH and two-dimensional flaky boron nitride, and the mass ratio of the POE-g-MAH to the two-dimensional flaky boron nitride is 2: 3.
The modified POE-g-MAH is obtained by the following preparation method:
and dispersing the POE-g-MAH in tetrahydrofuran, heating at 50 ℃, refluxing and stirring, adding two-dimensional flaky boron nitride, continuously heating, refluxing and stirring, finally pouring the mixture into ethanol, filtering and drying to obtain the modified POE-g-MAH.
The polyamide composite material with high thermal conductivity coefficient is obtained by the following preparation method:
PA6, magnesium oxide whiskers and modified POE-g-MAH are mixed and then added into a double-screw extruder for extrusion and granulation, so that the polyamide composite material with high thermal conductivity coefficient is obtained. The rotation speed of the double-screw extruder is 300r/min, and the temperatures of the double-screw extruder from the feed inlet are 225 ℃, 240 ℃ and the head temperature is 240 ℃.
Example 2
The polyamide composite material with high thermal conductivity coefficient comprises the following components in percentage by mass: PA 6: 40 wt%, magnesium oxide whisker: 50 wt%; modified POE-g-MAH: 10 wt% of modified POE-g-MAH, wherein the modified POE-g-MAH is a mixture of POE-g-MAH and two-dimensional flaky boron nitride, and the mass ratio of POE-g-MAH to two-dimensional flaky boron nitride is 2: 3.
The preparation method of the modified POE-g-MAH and the preparation method of the polyamide composite material with high thermal conductivity are the same as those of the embodiment 1.
Example 3
The polyamide composite material with high thermal conductivity coefficient comprises the following components in percentage by mass: PA 6: 40 wt%, magnesium oxide whisker: 40 wt%; modified POE-g-MAH: 20 wt%, wherein the modified POE-g-MAH is a mixture of POE-g-MAH and two-dimensional flaky boron nitride, and the mass ratio of the POE-g-MAH to the two-dimensional flaky boron nitride is 3: 2.
The preparation method of the modified POE-g-MAH and the preparation method of the polyamide composite material with high thermal conductivity are the same as those of the embodiment 1.
Example 4
The polyamide composite material with high thermal conductivity coefficient comprises the following components in percentage by mass: PA 6: 80 wt%, glass fiber: 10 wt%; modified PE-g-MAH: 10 wt%, wherein the modified PE-g-MAH is a mixture of PE-g-MAH and two-dimensional flaky alumina, and the mass ratio of the PE-g-MAH to the two-dimensional flaky alumina is 4: 1.
The modified PE-g-MAH is obtained by the following preparation method:
and mixing the PE-g-MAH and the two-dimensional flaky alumina, and adding the mixture into a screw extruder for melting and granulation to obtain the modified PE-g-MAH. The rotation speed of the double-screw extruder is 300r/min, and the temperatures of the double-screw extruder from the feed inlet are 225 ℃, 240 ℃ and the head temperature is 240 ℃.
The preparation method of the polyamide composite material with high thermal conductivity is the same as that of example 1.
Example 5
The polyamide composite material with high thermal conductivity coefficient comprises the following components in percentage by mass: PA 6: 50 wt%, magnesium oxide whisker: 20 wt%; glass fiber: 10 wt%; modified POE-g-MAH: 20 wt%, wherein the modified POE-g-MAH is a mixture of POE-g-MAH and two-dimensional flaky boron nitride, and the mass ratio of the POE-g-MAH to the two-dimensional flaky boron nitride is 7: 3.
The preparation method of the modified POE-g-MAH and the preparation method of the polyamide composite material with high thermal conductivity are the same as those of the embodiment 1.
Comparative example 1
The polyamide composite material of comparative example 1 comprises the following components in percentage by mass: PA 6: 50 wt%, magnesium oxide whisker: 20 wt%; glass fiber: 10 wt%; POE-g-MAH: 20 wt%. Mixing PA6, magnesium oxide whisker, glass fiber and POE-g-MAH, adding into a double-screw extruder, and extruding and granulating to obtain the polyamide composite material. The speed of rotation of the twin-screw extruder and the temperatures in the zones were the same as in example 1.
Comparative example 2
The polyamide composite material of comparative example 2 comprises the following components in percentage by mass: PA 6: 50 wt%, magnesium oxide whisker: 20 wt%; glass fiber: 10 wt%; POE-g-MAH: 14 wt%; two-dimensional lamellar boron nitride: 6 wt%.
Mixing PA6, magnesium oxide whiskers, glass fibers, POE-g-MAH and two-dimensional flaky boron nitride, adding the mixture into a double-screw extruder, and extruding and granulating to obtain the polyamide composite material. The speed of rotation of the twin-screw extruder and the temperatures in the zones were the same as in example 1.
Comparative example 3
The polyamide composite material of comparative example 3 comprises the following components in percentage by mass: PA 6: 50 wt%, magnesium oxide whisker: 20 wt%; glass fiber: 10 wt%; POE-g-MAH: 14 wt%; two-dimensional lamellar boron nitride: 6 wt%.
Dispersing POE-g-MAH in tetrahydrofuran, heating at 50 ℃, refluxing and stirring, adding two-dimensional flaky boron nitride, magnesium oxide whisker and glass fiber, continuing heating, refluxing and stirring, finally pouring the mixture into ethanol, filtering and drying to obtain a mixture;
and mixing the PA6 with the mixture prepared above, and adding the mixture into a double-screw extruder for extrusion granulation to obtain the polyamide composite material. The speed of rotation of the twin-screw extruder and the temperatures in the zones were the same as in example 1.
The polyamide composite materials of examples 1 to 5 and comparative examples 1 to 3 were subjected to a thermal conductivity test, and the results of the test are shown in Table 1. The thermal conductivity was tested using the hot TPS2500S, with reference to GB/T32064-.
TABLE 1 thermal conductivity and mechanical data for the polyamide composites of examples 1-5 and comparative examples 1-3
FIG. 3 is a schematic diagram of the preparation of the polyamide composite material of comparative example 1, and it can be seen that the thermal conductivity of comparative example 1 is greatly reduced by using the unmodified POE-g-MAH and not forming the thermal conductivity-rich phase, and the thermal conductivity is only 0.671W/(m.K). Comparative example 2 all the raw materials were mixed together and extruded for granulation, and the heat conductive rich phase was not efficiently formed in the polyamide composite material, as shown in comparative example 2 having a lower heat conductivity than that of example 5. All the heat-conducting fillers in the comparative example 3 are mixed with POE-g-MAH to form modified POE-g-MAH, the modified POE-g-MAH is formed by mixing and extruding PA6, the modified POE-g-MAH can form a heat-conducting enrichment phase in PA6, but the heat-conducting enrichment phase cannot be connected due to the lack of the bridging effect of the one-dimensional heat-conducting fillers, and the heat conductivity coefficient of the comparative example 3 is lower.
Finally, it should be noted that the specific examples described herein are merely illustrative of the spirit of the invention and do not limit the embodiments of the invention. Various modifications, additions and substitutions for the embodiments described herein will occur to those skilled in the art, and all such embodiments are neither required nor possible. While the invention has been described with respect to specific embodiments, it will be appreciated that various changes and modifications may be made without departing from the spirit and scope of the invention, as defined by the appended claims.
Claims (10)
1. The polyamide composite material with high thermal conductivity is characterized by comprising the following components in percentage by mass:
polyamide: 40-80 wt%;
one-dimensional heat-conducting filler: 10 to 50 wt%;
modified second phase polymer: 10-20 wt%;
wherein the modified second-phase polymer is a mixture of the second-phase polymer and the two-dimensional heat-conducting filler.
2. The high thermal conductivity polyamide composite material according to claim 1, wherein the second phase polymer is a polymer material incompatible with polyamide.
3. The high thermal conductivity polyamide composite material according to claim 2, wherein the second phase polymer is one or more of POE-g-MAH, PE-g-MAH, EPDM-g-MAH, PP-g-MAH, PPO-g-MAH, PE-g-MAH.
4. The high thermal conductivity polyamide composite material according to claim 1, wherein the two-dimensional thermal conductive filler is one or more of two-dimensional boron nitride flakes, two-dimensional aluminum oxide flakes, two-dimensional aluminum nitride flakes, two-dimensional silicon nitride flakes, and two-dimensional MXene.
5. The polyamide composite material with high thermal conductivity according to claim 1, wherein the mass ratio of the second phase polymer to the two-dimensional heat-conducting filler is (2-4): (1-3).
6. The high thermal conductivity polyamide composite material according to claim 1, wherein the modified second phase polymer is obtained by a preparation method comprising the steps of: and dispersing the second-phase polymer in an organic solvent, heating, refluxing and stirring, then adding the two-dimensional heat-conducting filler, continuing heating, refluxing and stirring, finally pouring the mixture into the second solvent, filtering and drying to obtain the modified second-phase polymer.
7. The high thermal conductivity polyamide composite material according to claim 1, wherein the modified second phase polymer is obtained by a preparation method comprising the steps of: and mixing the second-phase polymer and the two-dimensional heat-conducting filler, and adding the mixture into a screw extruder for melting and granulation to obtain the modified second-phase polymer.
8. The high thermal conductivity polyamide composite material according to claim 1, wherein the one-dimensional thermal conductive filler is one or both of glass fiber and whisker.
9. The high thermal conductivity polyamide composite material according to claim 8, wherein the whiskers are one or more of magnesium oxide whiskers, zinc oxide whiskers, aluminum nitride whiskers, aluminum oxide whiskers, boron nitride whiskers, and silicon carbide whiskers.
10. A method for preparing the high thermal conductivity polyamide composite material according to claim 1, comprising the steps of: mixing polyamide, one-dimensional heat-conducting filler and modified second-phase polymer, adding the mixture into a screw extruder, and extruding and granulating to obtain the polyamide composite material with high heat conductivity coefficient.
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