CN112111153A - Oriented heat conduction material and preparation method and application thereof - Google Patents
Oriented heat conduction material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides an oriented heat conduction material and a preparation method and application thereof. The oriented heat conduction material comprises a polymer matrix and anisotropic heat conduction fibers filled in the polymer matrix, wherein the anisotropic heat conduction fibers are oriented in the polymer matrix, and the anisotropic heat conduction fibers are oriented along the direction of the oriented arrangement. The oriented heat conduction material provided by the embodiment of the invention at least has the following beneficial effects: the oriented heat conduction material utilizes the anisotropic heat conduction filler to form the oriented heat conduction fibers, and the heat conduction fibers are also oriented along the arrangement direction on the microscale of the oriented heat conduction fibers, so that the anisotropy of the filler can be utilized to the greatest extent by the oriented heat conduction material, the orientation degree of the filler is greatly improved, the higher heat conduction performance can be realized by the lower proportion of the anisotropic heat conduction filler, and the oriented heat conduction material is further suitable for the heat dissipation requirement brought by the high-speed development of electronic devices.
Description
Technical Field
The invention relates to the technical field of heat management materials, in particular to a directional heat conduction material and a preparation method and application thereof.
Background
With the rapid development of electronic technology and the continuous rise in the fields of 5G communication, the Internet of things, new energy automobile electronics, intelligent wearable equipment and the like, the power density and the integration degree of related electronic devices are increasingly improved. When the electronic device works, a part of power loss is led out as heat, and the dissipation and heating of the electronic device directly cause the rapid temperature rise and the increase of thermal stress of electronic equipment, thereby causing serious threats to the working reliability, the safety and the service life of the electronic device. This has also led those skilled in the art to recognize that the ability to break through thermal management material systems has to some extent determined whether electronic devices can be further developed.
The traditional heat management material system mainly adopts a heat transfer mode of diffusing heat from a generation point to the surface of a radiator, but as the size of an electronic device is continuously reduced, the waviness and the roughness of a contact interface between the heat management material system and a packaging shell are gradually increased, and pores between interfaces under a microscale have great influence on the heat conduction of the heat management material system. In order to reduce the interface thermal resistance as much as possible, a thermal interface material is introduced between the interface of the power component such as a chip and the heat sink to fill the air pores.
In consideration of ensuring the long-term stability of electronic devices, thermal interface materials not only have requirements on thermal conductivity, but also have to meet certain standards for mechanical strength, electrical insulation and other properties. The high molecular polymer material becomes a thermal interface material with the widest application at present due to the characteristics of good electrical insulation performance, corrosion resistance, easy processing, high mechanical strength and the like. However, most polymers have low thermal conductivity, and polymer materials are used as a matrix, and high thermal conductive fillers are added to the matrix to increase the thermal conductivity of the thermal interface composite.
The anisotropic high thermal conductive filler may have a thermal conductivity of several hundreds of W/m · K in the axial direction or in-plane direction, and examples thereof include carbon fibers and carbon nanotubes having a one-dimensional structure, and Boron Nitride (BN), graphite, and graphene having a two-dimensional structure. If these anisotropic, highly thermally conductive fillers can be oriented in a polymer matrix, the thermally conductive material can be made to have a high thermal conductivity in a particular direction. However, the degree of orientation that can be achieved with existing orientation processes is not high, and high thermal conductivity must be achieved with higher filler ratios. Therefore, there is a need for a thermally conductive material that can achieve higher thermal conductivity with a lower filler fraction.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides an oriented heat conduction material capable of realizing higher heat conduction performance by using a lower filler proportion, and a preparation method and application thereof.
In a first aspect, an embodiment of the present invention provides an oriented thermal conductive material, which includes a polymer matrix and anisotropic thermal conductive fibers filled in the polymer matrix, wherein the anisotropic thermal conductive fibers are aligned in the polymer matrix, and the anisotropic thermal conductive fibers are oriented along the direction of the alignment.
The oriented heat conduction material provided by the embodiment of the invention at least has the following beneficial effects:
the oriented heat conduction material utilizes the anisotropic heat conduction filler to form the oriented heat conduction fibers, and the heat conduction fibers are also oriented along the arrangement direction on the microscale of the oriented heat conduction fibers, so that the anisotropy of the filler can be utilized to the greatest extent by the oriented heat conduction material, the orientation degree of the filler is greatly improved, the higher heat conduction performance can be realized by the lower proportion of the anisotropic heat conduction filler, and the oriented heat conduction material is further suitable for the heat dissipation requirement brought by the high-speed development of electronic devices.
According to some embodiments of the present invention, the anisotropic thermal conductive fibers are made of a raw material including anisotropic thermal conductive fillers, and the raw material may specifically include:
(a) an anisotropic thermally conductive filler;
(b) at least one of thermosetting resin, silicon rubber and phase change material.
The anisotropic heat-conducting filler refers to a one-dimensional or two-dimensional heat-conducting filler with anisotropy, the one-dimensional heat-conducting filler can be, but is not limited to, a carbon nanowire, a carbon nanotube and the like, and the two-dimensional heat-conducting filler can be, but is not limited to, lamellar boron nitride, lamellar graphene, expanded graphite and the like. In order to further improve the properties of the anisotropic heat conductive filler, such as adhesion property, thermal stability, etc., the anisotropic heat conductive filler may be subjected to surface modification treatment, such as by chemical grafting, coupling agent treatment, ultrasound, microwave treatment, and acid-base treatment. The thermosetting resin may be, but is not limited to, phenolic resin, epoxy resin, amino resin, unsaturated polyester, etc., the silicone rubber is mainly composed of silicone segments containing methyl groups and a small amount of vinyl groups, and the phase change material may be, but is not limited to, paraffin, fatty acid-alcohol, high density polyethylene, polyethylene glycol, etc. The thermosetting resin and the silicon rubber contained in the anisotropic heat conducting fibers can ensure the electrical insulation of the heat conducting material, and the phase change material can strengthen the heat conducting property to a certain extent.
The oriented heat conduction material according to some embodiments of the invention has the mass fraction of the anisotropic heat conduction filler of 5-20% based on the total mass of the anisotropic heat conduction fibers. Because the oriented heat conduction material has extremely high orientation, the anisotropic heat conduction filler in the material can obtain higher heat conductivity with lower content, and the material cost is reduced. Of course, it is obvious that if the content of the thermally conductive filler is higher, the oriented thermally conductive material will necessarily bring about higher thermal conductivity.
According to some embodiments of the present invention, the polymer matrix is prepared from the following raw materials:
(c) a particulate thermally conductive filler;
(d) at least one of thermosetting resin and silicone rubber.
The oriented heat conduction material takes thermosetting resin and/or silicon rubber as a support material of a main body so as to ensure that the oriented heat conduction material has enough mechanical strength. Wherein, can also add graininess heat conduction filler to make the whole of directional heat conduction material can both have certain heat conductivity along anisotropic heat conduction fibre's axial, radial, circumference, make the holistic heat conductivity of directional heat conduction material promote to some extent. The particulate thermally conductive filler may be an optional thermally conductive filler in particulate form, including but not limited to alumina, silica, aluminum nitride, silicon nitride, zinc oxide, and the like.
The oriented heat conduction material according to some embodiments of the invention has the mass fraction of the granular heat conduction filler of 5-80% based on the total mass of the polymer matrix. The above-mentioned amount of the particulate heat conductive filler is mixed in the polymer matrix in view of improvement of the overall heat conductivity of the oriented heat conductive material.
The oriented heat conduction material according to some embodiments of the invention has a volume fraction of the anisotropic heat conduction fibers of 20-70% based on the total volume of the oriented heat conduction material. The anisotropic heat conduction filler on the microscopic scale in the anisotropic heat conduction fiber has good orientation, so that the axial heat conductivity of the anisotropic heat conduction fiber is greatly improved, and therefore, higher heat conduction performance can be realized at a lower proportion.
According to the oriented heat conduction material of some embodiments of the invention, the radius of the anisotropic heat conduction fiber is 10-500 μm, and the length-diameter ratio of the anisotropic heat conduction fiber is not less than 10. The length-diameter ratio of the heat conducting fibers is set to be more than 10, so that the high orientation of the one-dimensional or two-dimensional filler in the anisotropic heat conducting fibers can be effectively ensured, the larger the length-diameter ratio is, the better the orientation effect of the one-dimensional or two-dimensional filler on a microscopic scale is, and the better the axial heat conductivity of the oriented heat conducting material is. The micron-diameter heat-conducting fibers can ensure that high polymers such as thermosetting resin, silicon rubber, phase-change materials and the like in the heat-conducting fibers have good forming orientation effect, are the same as the orientation of the filler, and bring higher orientation to the whole heat-conducting fibers.
In a second aspect, an embodiment of the present invention provides a method for preparing an oriented thermal conductive material, the method comprising the steps of:
s1: filling the first slurry into the through holes which are arranged in the template in an oriented mode, and solidifying the first slurry in the through holes to obtain anisotropic heat conducting fibers;
s2: removing the template, coating the second slurry on the anisotropic heat conduction fibers, and curing to obtain the oriented heat conduction material;
the first slurry comprises anisotropic heat-conducting filler, the second slurry comprises polymer matrix material, the diameter of the through hole is 10-500 mu m, and the length-diameter ratio of the through hole is not less than 10.
The preparation method of the oriented heat conduction material provided by the embodiment of the invention at least has the following beneficial effects:
the method adopts a template method to prepare the heat conduction material, uses a template with through holes with large length-diameter ratio to obtain a large amount of highly oriented anisotropic heat conduction fibers, and then cures the fibers and second slurry containing a polymer matrix material to form the oriented heat conduction material. The small diameter and high aspect ratio through hole can promote the orientation of the anisotropic heat conducting filler, and at the same time, the polymer material used therein can generate a certain orientation, which may result in the requirement of a larger pressure during the filling of the slurry, but on the other hand, the whole heat conducting material can also have a higher orientation, and a higher heat conductivity can be obtained at a lower filler ratio compared with the existing heat conducting material.
According to the preparation method of the oriented heat conduction material, when the template is removed, the anisotropic heat conduction fibers are fixed between the upper cover plate and the lower cover plate of the mold. Since the through holes for obtaining the anisotropic heat conduction fibers in the embodiment have a high length-diameter ratio, the fibers may be bent without being supported, and therefore, the anisotropic heat conduction fibers need to be oriented in the template without being bent by fixing the upper cover plate and the lower cover plate, and then the step of filling the second slurry is performed.
According to the preparation method of the oriented heat conduction material, the template used in the preparation method can be prepared by selecting materials such as ice, anodized aluminum, silicon dioxide, polycarbonate or polyester according to actual use requirements.
In a third aspect, an embodiment of the present invention provides an electronic device comprising the oriented thermal conductive material described above. The electronic device adopts the oriented heat conduction material to dissipate heat or assist in dissipating heat. Because the directional heat conduction material has higher axial heat conductivity, the temperature rise of the directional heat conduction material can be effectively controlled when the directional heat conduction material is used in an electronic device, and the influence of overhigh long-term temperature on the working reliability, safety and service life of the electronic device is avoided.
Drawings
Fig. 1 is a side view of a mold used in the method of making an oriented thermal conductive material of example 1 of the present invention.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
Example 1
The present embodiments provide an oriented thermal conductive material that includes a polymer matrix and anisotropic thermal conductive fibers filled in the polymer matrix. The polymer matrix comprises 40 wt% of spherical alumina and 60 wt% of silicone rubber, and the anisotropic thermal conductive fibers comprise 5 wt% of carbon fibers and 95 wt% of paraffin wax. The volume fraction of the anisotropic heat-conducting fibers in the total volume of the oriented heat-conducting material is 30%. The anisotropic heat conducting fibers are oriented in the polymer matrix, and the anisotropic heat conducting fibers are oriented along the direction of the oriented arrangement.
The mold used in the process of making the oriented thermal conductive material is shown in fig. 1, and referring to fig. 1, is a side view of the mold according to one embodiment of the present invention. The mold is of a cylindrical structure and comprises a lower cover plate 101, a side wall 102 is fixed along the outer edge of the lower cover plate 101, the side wall 102 wraps a template 110, and the height of the template 110 is slightly lower than that of the side wall 102, so that after a cavity defined by the side wall 102 and the lower cover plate 101 is loaded with the template 110, the upper part of the cavity still forms a cavity 120. At the upper end of the side wall 102, an upper cover plate 103 may be in contact therewith and extend into the cavity 120 to seal it. The template 110 is provided with uniformly distributed cylindrical through holes 111, the diameter d of the through holes 111 is 200 μm, and the length L of the through holes 111 in the extending direction thereof is 3cm, which is perpendicular to the plane of the lower cover plate 101. The sum of the cross-sectional areas of the through-holes 111 is 20% of the cross-sectional area of the template 110. The template 110 is an anodized aluminum template, and the upper cover plate 103, the sidewall 102, and the lower cover plate 101 are made of stainless steel. The upper cover plate 103 and the lower cover plate 101 are detachable, and sealing rings (not shown) are further arranged on the upper cover plate 103 and the lower cover plate 101 to ensure air tightness.
The preparation method of the oriented heat conduction material comprises the following steps:
step 1: mixing paraffin and carbon fiber subjected to surface pretreatment by a coupling agent KH550 into first slurry according to the proportion, and mixing silicon rubber and spherical alumina subjected to surface treatment by the coupling agent KH550 into second slurry according to the proportion;
step 2: keeping the temperature of the first slurry above the phase-change point temperature of the paraffin, injecting the first slurry into the cavity 120, installing the upper cover plate 103, vacuumizing and pressurizing to enable the first slurry to enter the through hole 111 of the template 110 and fill the through hole 111;
and step 3: removing the redundant first slurry on the surface of the template 110, attaching the upper cover plate 103 to the upper surface of the template 110, and cooling to solidify paraffin to obtain anisotropic heat-conducting fibers;
and 4, step 4: dismantling the side wall 102 of the mold, soaking the upper cover plate 103, the lower cover plate 101 and the template 110 of the mold in a sodium hydroxide solvent, dissolving and removing the template 110, cleaning the anisotropic heat-conducting fibers fixed between the upper cover plate 103 and the lower cover plate 101 by using ethanol and deionized water, and drying under a vacuum condition;
and 5: completely soaking the upper cover plate 103, the lower cover plate 101 and the anisotropic heat conduction fibers fixed between the upper cover plate 103 and the lower cover plate 101 into the second slurry, mounting the side wall 102 within the range of the upper cover plate 103 and the lower cover plate 101 again, coating the second slurry replacing the template 110 around the anisotropic heat conduction fibers in the mold, taking out the mold, and heating to completely cure the second slurry;
step 6: the side walls 102 and the upper and lower cover plates 103, 101 are removed to obtain the oriented heat conducting material.
The small-diameter and high-length-diameter through holes of the template adopted in the embodiment can promote the anisotropic heat-conducting filler to be axially oriented along the through holes in macroscopic and microscopic scales in the pressurizing process, and meanwhile, the high polymer materials in the anisotropic heat-conducting filler can be oriented to a certain degree through the small-diameter and small-diameter through holes, so that the whole orientation of the heat-conducting material is higher, and higher heat conductivity can be obtained under the condition of lower filler proportion compared with the existing heat-conducting material.
Example 2
The present embodiments provide an oriented thermally conductive material comprising: a polymer matrix and anisotropic heat conducting fibers filled in the polymer matrix. The polymer matrix comprises 50 wt% of spherical silicon oxide and 50 wt% of silicon rubber, and the anisotropic heat-conducting fiber comprises 10 wt% of boron nitride and 90 wt% of silicon rubber. The volume fraction of the anisotropic heat-conducting fibers in the total volume of the oriented heat-conducting material is 30%. The anisotropic heat conducting fibers are oriented in the polymer matrix, and the anisotropic heat conducting fibers are oriented along the direction of the oriented arrangement.
The preparation method of the oriented heat conduction material comprises the following steps:
step 1: mixing silicon rubber and boron nitride treated by a coupling agent KH550 into first slurry, and mixing the silicon rubber and spherical silicon oxide treated by the coupling agent KH550 into second slurry;
step 2: adding the first slurry into an upper cavity of a mold loaded with an anodized aluminum template, installing an upper cover plate, vacuumizing and pressurizing to enable the first slurry to enter through holes of the template and fill the through holes;
and step 3: removing the redundant first slurry on the surface of the template, enabling the upper cover plate to be attached to the upper surface of the template, heating to semi-cure the silicon rubber (facilitating re-softening during heating in the subsequent step 5 and carrying out cross-linking reaction with the polymer matrix material for combination), and obtaining the anisotropic heat-conducting fiber;
and 4, step 4: removing the side wall of the mold, soaking the mold and the template in a sodium hydroxide solution, removing the template, cleaning with ethanol and deionized water, and vacuum-drying;
and 5: completely soaking the upper cover plate, the lower cover plate and the anisotropic heat-conducting fibers fixed between the upper cover plate and the lower cover plate into the second slurry, mounting the side walls in the second slurry within the range of the upper cover plate and the lower cover plate, taking out the mold, and heating to completely cure the polymer matrix;
step 6: and (4) removing the side wall, the upper cover plate and the lower cover plate to obtain the oriented heat conduction material.
Thermal conductivity test
Comparative example 1
The comparative example provides a thermally conductive material comprising a polymer matrix and thermally conductive fibers, the polymer matrix and thermally conductive fibers being in a volume ratio of 4: 1, the polymer matrix comprises 40 wt% of spherical alumina and 60 wt% of silicone rubber, and the heat conducting fiber comprises 5 wt% of carbon fiber and 95 wt% of paraffin wax. The preparation method of the heat conduction material is to simply and uniformly mix the raw materials and then solidify and shape the mixture.
Comparative example 2
The comparative example provides a thermally conductive material comprising a polymer matrix and thermally conductive fibers, the polymer matrix and thermally conductive fibers being in a volume ratio of 4: 1, the polymer matrix comprises 50 wt% of spherical silicon oxide and 50 wt% of silicone rubber, and the heat conducting fiber comprises 10 wt% of boron nitride and 90 wt% of silicone rubber. The preparation method of the heat conduction material is to simply and uniformly mix the raw materials and then solidify and shape the mixture.
The method for measuring the axial thermal conductivity of the oriented thermal conductive material along the anisotropic thermal conductive fiber by adopting a steady state method comprises the following specific steps: the directional heat conduction material is placed between instrument bars of the resistance and conductivity measuring instrument, after stable heat flow is established, the temperature in the electric meter bar is measured at two or more than two points along the axial direction of the electric meter bar, and the temperature difference is calculated, so that the thermal conductivity of the directional heat conduction material along the axial direction of the directional heat conduction material is determined.
The thermal conductivity was measured by the above method using the thermally conductive materials prepared in examples 1 to 2 and comparative examples 1 to 2, respectively, and the results are shown in table 1.
TABLE 1 measurement of thermal conductivity
| Example 1 | Example 2 | Comparative example 1 | Comparative example 2 | |
| Thermal conductivity (W/m.k) | 15.6 | 12.3 | 3.7 | 2.4 |
From the above results, compared with comparative examples 1 and 2, the oriented heat conduction material provided by the embodiment of the invention achieves a good orientation effect, and the axial heat conductivity is remarkably improved.
Example 3
This embodiment provides an electronic device including a chip and a heat sink arranged in this order, with a thermal transfer adhesive interposed between the chip and the heat sink, the thermal transfer adhesive including the oriented thermal conductive material of embodiment 1. By utilizing the directional heat conduction material, the heat generated by the chip in the working process can be rapidly transferred to the radiator to be dissipated, and the temperature rise of the chip is effectively slowed down.
The present invention has been described in detail with reference to the embodiments, but the present invention is not limited to the embodiments described above, and various changes can be made within the knowledge of those skilled in the art without departing from the gist of the present invention. Furthermore, the embodiments of the present invention and the features of the embodiments may be combined with each other without conflict.
Claims (10)
1. The oriented heat conduction material is characterized by comprising a polymer matrix and anisotropic heat conduction fibers filled in the polymer matrix, wherein the anisotropic heat conduction fibers are aligned in the polymer matrix in an oriented mode, and the anisotropic heat conduction fibers are oriented along the direction of the aligned mode.
2. The oriented thermal conductive material of claim 1, wherein the anisotropic thermal conductive fiber is prepared from:
(a) an anisotropic thermally conductive filler;
(b) at least one of thermosetting resin, silicon rubber and phase change material.
3. The oriented heat conduction material according to claim 2, wherein the mass fraction of the anisotropic heat conduction filler is 5-20% based on the total mass of the anisotropic heat conduction fibers.
4. The oriented thermal conductive material of claim 1, wherein the polymer matrix is prepared from materials comprising:
(c) a particulate thermally conductive filler;
(d) at least one of thermosetting resin and silicone rubber.
5. The oriented thermal conduction material according to claim 4, wherein the mass fraction of the granular thermal conductive filler is 5-80% based on the total mass of the polymer matrix.
6. The oriented heat conduction material according to any one of claims 1 to 5, wherein the volume fraction of the anisotropic heat conduction fibers is 20-70% based on the total volume of the oriented heat conduction material.
7. The oriented heat conduction material according to any one of claims 1 to 5, wherein the radius of the anisotropic heat conduction fiber is 10 to 500 μm, and the aspect ratio of the anisotropic heat conduction fiber is not less than 10.
8. The preparation method of the oriented heat conduction material is characterized by comprising the following steps of:
s1: filling first slurry into through holes which are arranged in a template in an oriented mode, and curing the first slurry in the through holes to obtain anisotropic heat conducting fibers;
s2: removing the template, coating the anisotropic heat conduction fibers with second slurry, and curing to obtain an oriented heat conduction material;
the first paste comprises anisotropic heat conduction filler, the second paste comprises polymer matrix material, the diameter of the through hole is 10-500 mu m, and the length-diameter ratio of the through hole is not less than 10.
9. The method as claimed in claim 8, wherein in the step S2, the anisotropic thermal conductive fiber is fixed between an upper cover plate and a lower cover plate of the mold when the template is removed.
10. An electronic device comprising the oriented thermal conductive material of any one of claims 1 to 7.
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| CN115181551A (en) * | 2022-07-07 | 2022-10-14 | 深圳市鸿富诚新材料股份有限公司 | Anisotropic heat conduction phase change material and preparation method thereof |
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| CN113461989A (en) * | 2021-08-06 | 2021-10-01 | 扬中市华龙橡塑电器有限公司 | Anisotropic heat conduction composite material and preparation method thereof |
| CN115181551A (en) * | 2022-07-07 | 2022-10-14 | 深圳市鸿富诚新材料股份有限公司 | Anisotropic heat conduction phase change material and preparation method thereof |
| CN115181551B (en) * | 2022-07-07 | 2023-12-12 | 深圳市鸿富诚新材料股份有限公司 | Anisotropic heat conduction phase change material and preparation method thereof |
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