CN108122870B - Heat dissipation structure, preparation method thereof and heat dissipation device - Google Patents
Heat dissipation structure, preparation method thereof and heat dissipation device Download PDFInfo
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- CN108122870B CN108122870B CN201711437642.8A CN201711437642A CN108122870B CN 108122870 B CN108122870 B CN 108122870B CN 201711437642 A CN201711437642 A CN 201711437642A CN 108122870 B CN108122870 B CN 108122870B
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Abstract
Heat dissipation structure, preparation method thereof and heat dissipation deviceThe preparation method comprises the following steps: sequentially depositing a transition layer and a catalyst layer on a substrate, introducing reducing gas and carbon source gas in a protective gas atmosphere, and keeping the temperature at 700-800 ℃ for 5-30 min to vertically grow a carbon nanotube array on the catalyst layer to obtain a heat dissipation structure; wherein the transition layer is Al2O3The catalyst layer is a metal single layer or an alloy layer of transition metal; the thickness of the catalyst layer is 0.8-10 nm; the volume flow ratio of the introduced reducing gas and the introduced carbon source gas is controlled to be 1: 1-10, and the heat preservation treatment condition is that the temperature is preserved for 5-30 min at 700-900 ℃. The carbon nanotube array prepared by the preparation method is very regular, has a typical graphene structure, does not contain amorphous carbon, and has very few defects; the heat conduction along the growth direction of the carbon nano tube array is quick and effective, so that the heat conduction performance of the prepared heat dissipation structure is obviously improved, and the heat conduction performance is excellent.
Description
Technical Field
The invention relates to the technical field of heat dissipation, in particular to a heat dissipation structure, a preparation method thereof and a heat dissipation device.
Background
With the rapid development of microelectronic technology, the feature size of electronic components has been reduced to nanometer level, and the energy density of the system has been increased continuously, and studies have shown that the power of future chips may reach 510W. The uneven distribution of heat flow on the chip causes 'hot spots' on the chip, so that the local power density of the chip exceeds 1000W/cm2. The problem of thermal management of electronic components becomes quite important. In order to ensure the stable operation of the electronic components, the heat generated in the operation process of the electronic components needs to be rapidly discharged, and the high-temperature severe environment generated when the chip of the electronic components works needs to be ensured to have better stability, and the mechanical pressure, the shearing force and the like during the chip installation and the system packaging can be borne, so that the heat conduction material which has high heat conduction capability and is suitable for the preparation of the electronic components with the micro-nano size needs to be found.
At present, three types of thermal interface materials, such as organic thermal interface materials, low-melting-point alloy solder, phase-change materials and the like, are mainly adopted at home and abroad. Although the organic thermal interface material has high cohesiveness, good flexibility, easy operation and low cost, the heat-conducting property is poor, and the organic matter is easy to degrade, so that the material is modified. The low-melting-point alloy solder has high thermal conductivity and good flexibility, but has the defects of high thermal expansion coefficient, low thermal fatigue strength, easy formation of cavities and the like, and easily causes failure problems of interface delamination and the like. The phase-change material has large heat absorption capacity, but is easy to leak in the installation and working processes, and has poor operability.
Since 1991 the electron microscope expert in basic research laboratory of NEC corporation found carbon nanotubes, the research heat of scientists around the world was developed. As research by research scientists finds that carbon nanotubes have the advantages of good stability, mechanical property, thermal conductivity and the like, but the application of the carbon nanotubes is limited due to factors such as controllability and defects of the preparation of the carbon nanotubes, so that the research on the carbon nanotubes is also gradually silent. At present, the heat conduction research of carbon nanotubes generally adopts the steps of firstly growing a carbon nanotube array on a silicon chip, then transferring the grown carbon nanotube array to a metal copper substrate, and generally using organic glue in order to enable the carbon nanotube array to be well combined with the metal copper substrate, so that the heat conduction performance of the prepared carbon nanotube array heat dissipation structure is poor.
Disclosure of Invention
In view of the foregoing, it is desirable to provide a heat dissipation structure based on a carbon nanotube array and having excellent thermal conductivity, a method for manufacturing the same, and a heat dissipation device.
A preparation method of a heat dissipation structure comprises the following steps:
sequentially depositing a transition layer and a catalyst layer on a substrate, introducing reducing gas and carbon source gas in a protective gas atmosphere, and preserving heat at 700-900 ℃ for 5-30 min to vertically grow a carbon nanotube array on the catalyst layer to obtain the heat dissipation structure;
wherein the transition layer is Al2O3A layer, the catalyst layer being a metal monolayer or alloy layer of a transition metal; thickness of the catalyst layerThe degree is 0.8-10 nm; the volume flow ratio of the reducing gas to the carbon source gas is 1: 1-10.
The preparation method of the heat dissipation structure comprises the step of depositing Al on a substrate2O3The layer is used as a transition layer, which can not only prevent the catalyst layer from directly contacting with the substrate, but also prevent the transition metals such as iron, cobalt, nickel and the like from being in Al2O3The catalyst has good dispersibility, and can promote the uniform distribution of the catalyst; in addition, due to Al2O3The structure of the catalyst is compact, the catalyst can be well prevented from mutually melting with the metal substrate, the catalyst can not form particles, the uniform distribution of the catalyst is promoted, and the amorphous carbon in the carbon nano tube array can be reduced. Further, by controlling the thickness of the catalyst layer and the growth conditions of the carbon nanotubes, the carbon nanotube array vertically grows on the catalyst layer, and the prepared carbon nanotube array is very regular, has a typical graphene structure, does not contain amorphous carbon and has very few defects; the carbon nanotube array with high thermal conductivity is obtained, and the structure of the preparation method does not contain organic glue with low thermal conductivity, so that the problem that the thermal conductivity is reduced due to the adoption of the organic glue is avoided, and the thermal conductivity of the prepared heat dissipation structure is remarkably improved and excellent.
In one embodiment, the thickness of the transition layer is 3-100 nm.
In one embodiment, the catalyst layer is a metal monolithic layer of iron, cobalt or nickel.
In one embodiment, the carbon source gas is selected from one of acetylene, ethylene, and methane.
In one embodiment, the volume flow ratio of the reducing gas to the carbon source gas is 1: 3-10.
In one embodiment, the heat preservation condition is that the heat preservation is carried out for 8-14 min at 700-900 ℃.
In one embodiment, the method further comprises the step of forming a graphene layer on the carbon nanotube array.
The heat dissipation structure prepared by the preparation method of the heat dissipation structure.
A heat dissipation device comprises the heat dissipation structure.
In one embodiment, the heat dissipation structure comprises at least two heat dissipation structures, wherein the two heat dissipation structures are respectively arranged at two sides of a heat source body, and one side of the heat dissipation structure, where the carbon nanotube array is located, faces the heat source body.
Drawings
Fig. 1 is a structural view of a heat dissipation structure according to an embodiment;
FIG. 2 is a block diagram of a heat sink according to one embodiment;
FIG. 3 is a scanning electron microscope image and a transmission electron microscope image of a carbon nanotube array in the heat dissipation structure manufactured in example 1;
FIG. 4 is a scanning electron microscope image of a carbon nanotube array in a heat dissipation structure according to example 2;
FIG. 5 is a transmission electron microscope image of a carbon nanotube array in a heat dissipation structure according to example 3;
FIG. 6 is a Raman spectrum of a carbon nanotube array in the heat dissipation structure according to example 1;
FIG. 7 is a diagram of a heat dissipation structure according to example 1;
FIG. 8 is an image of a thermal imager at the heat source body of the control group;
fig. 9 is an imaging diagram of a thermal imager at a heat source body tested using the heat sink manufactured in example 1.
Detailed Description
In order that the invention may be more fully understood, a more particular description of the invention will now be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The method for manufacturing a heat dissipation structure according to an embodiment includes the following steps S1 to S3.
Step S1: depositing a transition layer on the substrate, wherein the transition layer is Al2O3And (3) a layer.
The transition layer is important for forming the carbon nanotube array, which can not only prevent the catalyst layer from directly contacting with the substrate, but also prevent the transition metal such as iron, cobalt, nickel and the like from Al2O3The catalyst has good dispersibility, and can promote the uniform distribution of the catalyst; in addition, due to Al2O3The structure of the catalyst is compact, the catalyst can be well prevented from mutually melting with the metal substrate, the catalyst can not form particles, the uniform distribution of the catalyst is promoted, and the growth of the carbon nano tube array is facilitated.
Specifically, the transition layer is deposited by adopting an atomic layer deposition technology.
Preferably, the thickness of the transition layer is 3-100 nm. More preferably, the thickness of the transition layer is 20 nm.
Further, the substrate is a metal substrate. Specifically, the substrate is made of copper, nickel, aluminum, or the like.
Further, when the substrate is a metal substrate, a pretreatment step for the substrate is further included before step S1. The pretreatment step of the substrate includes a cleaning step and an annealing treatment.
The cleaning steps are as follows: polishing a substrate, ultrasonically removing impurities in an organic solvent, washing with water, soaking in a hydrochloric acid solution to remove a surface oxide layer, and sequentially cleaning with water and ethanol. Wherein the organic solvent used for ultrasonic treatment is acetone; the surface oxide layer was removed by soaking in a 5 wt% hydrochloric acid solution for 10 seconds.
The annealing treatment step comprises the following steps of putting the substrate into a chemical vapor deposition chamber, and carrying out annealing treatment on the substrate in a hydrogen-argon ratio of 400: anneal for two hours in an atmosphere of 400 sccm.
Step S2: depositing a catalyst layer on the transition layer, wherein the catalyst layer is a metal single layer or an alloy layer of transition metal; the thickness of the catalyst layer is 0.8-10 nm.
The thickness of the catalyst layer in step S2 is too small, and the catalyst particles are too sparse, so that the vertically grown carbon nanotube array cannot be obtained in step S3; the thickness of the catalyst layer is too large, so that the carbon nanotube array is prepared, and the larger the tube diameter of the carbon nanotube is, the more the tube wall number of the carbon nanotube is, thus being not beneficial to heat conduction. Therefore, the thickness of the catalyst layer is selected to be 0.8-10 nm, and the carbon nano tube prepared in the range vertically grows on the catalyst layer, is in a carbon nano tube array structure, is very neat and has no amorphous carbon.
More specifically, the catalyst layer is deposited on the transition layer using electron beam evaporation (EB L).
Optionally, the catalyst layer is an iron-zinc alloy layer, a cobalt-nickel alloy layer, an iron metal layer, a cobalt metal layer, or a nickel metal layer. Preferably, the catalyst layer is an iron metal layer, a cobalt metal layer or a nickel metal layer.
Step S3: and introducing reducing gas and carbon source gas in the protective gas atmosphere, and preserving the heat at 700-900 ℃ for 5-30 min to vertically grow the carbon nanotube array on the catalyst layer to obtain the heat dissipation structure.
Wherein the volume flow ratio of the introduced reducing gas to the carbon source gas is 1: 1-10, and the heat preservation treatment condition is that the temperature is preserved for 5-30 min at 700-900 ℃. The research finds that the length of the carbon nanotube array under the condition is mainly influenced by time, the carbon nanotube array generated when the heat preservation time is less than 5min is very irregular and is not beneficial to heat conduction, and the length of the carbon nanotube array generated when the heat preservation time is more than 30min is too long, so that the heat conduction transmission path is too long and is not beneficial to heat conduction. The carbon nano tube array prepared in the range has the best heat-conducting property.
Step S3 is to control the length of the formed carbon nanotube array by controlling the volume flow ratio of the introduced reducing gas and the carbon source gas, and the temperature and time of the heat-preserving treatment. The research shows that the length of the carbon nano tube prepared under the condition is 5-276 mu m. The prepared heat dissipation structure has excellent heat dissipation effect.
According to the preparation method of the heat dissipation structure, the transition layer and the catalyst layer are sequentially deposited on the substrate, and then the carbon nanotube array vertically grows on the catalyst layer, so that the prepared carbon nanotube array is very regular, has a typical graphene structure, does not contain amorphous carbon and has very few defects; the heat conduction along the growth direction of the carbon nano tube array is quick and effective, and the preparation method does not need to use organic glue, so that the problem of reduction of the heat conduction performance caused by the adoption of the organic glue is avoided, and the heat conduction performance of the prepared heat dissipation structure is remarkably improved and excellent.
Optionally, the carbon source gas is selected from one of acetylene, ethylene, and methane.
Specifically, when the carbon source gas is ethylene, the volume flow ratio of the reducing gas to the carbon source gas is controlled to be 1: 2-10. When the carbon source gas is methane, controlling the volume flow ratio of the introduced reducing gas to the carbon source gas to be 1: 3-10. Further preferably, the volume flow ratio of the reducing gas to the carbon source gas is controlled to be 1: 3-10.
Preferably, the heat preservation treatment condition is that the heat preservation is carried out for 8-14 min at 700-900 ℃. Researches show that the length of the carbon nano tube prepared under the condition is 30-100 mu m, and the prepared heat dissipation structure has better heat dissipation effect.
In one embodiment, the method further comprises the step of forming a graphene layer on the carbon nanotube array.
Specifically, the step of forming a graphene layer on the carbon nanotube array includes: and coating organic glue on the graphene sheet as a support, transferring the graphene sheet with the organic glue onto the carbon nanotube array, dissolving the organic glue by using an organic solvent, and annealing for 1-3 hours at 250-500 ℃ in an oxygen-free environment. It is understood that the method of forming the graphene layer on the carbon nanotube array is not limited thereto, and may be implemented by a dry transfer method or the like.
Specifically, the graphene sheet takes a copper sheet as a substrate, single-layer graphene is grown by a CVD method, the method further comprises the step of removing the copper sheet, and after organic glue is coated, the graphene sheet with the organic glue is placed in ferric chloride solution, and copper is removed. Specifically, the organic glue is PMMA glue; the organic solvent used for dissolving the glue is alcohol or acetone and the like.
Annealing not only can remove residual glue, but also can strengthen the combination of the graphene sheet and the carbon nanotube array. Preferably, annealing is carried out for 2-10 hours in an oxygen-free environment at 250-500 ℃.
When the heat dissipation structure is used, the carbon nano tube array is in contact with the heat source body to conduct heat, and the heat is conducted to the substrate through the transition layer in sequence. Research shows that when the carbon nanotube array is contacted with a heat source body for heat conduction, the heat source body may generate heat unevenly and the carbon nanotube array has relatively weak heat conduction in a plane, thereby causing local hot spots in the heat dissipation process, which may lead to inconsistent heat conduction rate on the carbon nanotube array. Therefore, in order to uniformly conduct the energy of the heat source body, the layered graphene structure with one layer of high heat conduction performance is further formed on the carbon nanotube array, so that the heat conduction of the heat source in the horizontal direction of the surface of the carbon nanotube array is enhanced, the heat is firstly conducted to the graphene layer and then conducted to the carbon nanotube array, and the heat dissipation performance of the whole structure is greatly improved. The resulting heat dissipation structure is shown in fig. 1.
Referring to fig. 1, the heat dissipation structure manufactured by the method for manufacturing a heat dissipation structure according to an embodiment is based on a carbon nanotube array and has excellent heat conductivity.
Referring to fig. 2, a heat dissipation device according to an embodiment includes the heat dissipation structure.
The heat dissipation device adopting the heat dissipation structure has excellent heat conduction performance.
In one embodiment, the heat dissipation device comprises at least two heat dissipation structures. The two heat dissipation structures are respectively arranged at two sides of the heat source body, and one side of the heat dissipation structure, where the carbon nano tube array is located, faces the heat source body. Preferably, the heat dissipation structure is in direct contact with the heat source body at the side where the carbon nanotube array is located to conduct heat. It is understood that in other embodiments, there may be one heat dissipation structure, or three or more heat dissipation structures.
Wherein the side of the carbon nanotube array is referred to the catalyst layer.
Specifically, when the heat dissipation structure does not include the graphene layer, the heat dissipation structure directly conducts heat with the heat source body by the carbon nanotube array. When the heat dissipation structure contains the graphene layer, the heat dissipation structure conducts heat directly through the graphene layer and the heat source body.
Furthermore, one of the substrates is provided with a first cooling water inlet and a second cooling water outlet, and the other substrate is provided with a first cooling water outlet and a second cooling water inlet, so that the substrates are cooled and radiated by the two pieces of cooling water.
The following are specific examples.
Example 1
Pretreatment of the copper substrate: polishing a copper substrate with the thickness of 3 mu m, ultrasonically removing impurities in acetone, washing with water, soaking in a 5 wt% hydrochloric acid solution for 10s to remove a surface oxide layer, and sequentially washing with water and ethanol. And then putting the copper substrate into a chemical vapor deposition chamber, wherein the ratio of hydrogen to argon is 400: anneal for two hours in an atmosphere of 400 sccm.
Depositing Al with the thickness of 20nm on a copper substrate by adopting an atomic layer deposition technology2O3Transition layer of Al2O3And an iron metal layer with the thickness of 2nm is evaporated and evaporated by adopting an electron beam on the transition layer to be used as a catalyst layer. And placing the cut metal substrate on a quartz glass slide, then placing the cut metal substrate in the center of a furnace tube, sealing the furnace tube, and starting heating when the air in the tube is completely exhausted after argon is introduced for five minutes. After heating from room temperature to 560 ℃, hydrogen was introduced to prevent the catalyst from being oxidized. And when the temperature reaches 750 ℃, introducing acetylene, controlling the volume flow ratio of the introduced hydrogen to the introduced acetylene to be 1:8, and carrying out heat preservation treatment for 30min to vertically grow the carbon nanotube array on the catalyst layer.
Coating a layer of PMMA glue on a copper sheet of a graphene sheet grown by CVD (chemical vapor deposition), placing the copper sheet into a ferric chloride solution to remove copper, transferring the graphene sheet with the PMMA glue onto the carbon nanotube array, dissolving PMMA in alcohol, and placing the graphene sheet in an oxygen-free environment for annealing at 400 ℃ for 2 hours so as to remove residual glue and strengthen the combination of the graphene sheet and the carbon nanotube array.
Example 2
The procedure of example 2 was substantially the same as in example 1, except that the incubation treatment time for vertically growing the carbon nanotube array on the catalyst layer was 10 min.
Example 3
The procedure of example 3 was substantially the same as in example 1 except that the thickness of the iron metal layer as the catalyst layer was 0.8 nm.
Example 4
Depositing Al with the thickness of 100nm on a nickel substrate by adopting an atomic layer deposition technology2O3Transition layer of Al2O3And adopting a cobalt metal layer with the thickness of 5nm as a catalyst layer on the transition layer by electron beam evaporation and vapor deposition, and then introducing hydrogen and ethylene in an argon atmosphere for heat preservation treatment so as to vertically grow a carbon nano tube array on the catalyst layer. Controlling the volume flow ratio of the introduced hydrogen and the introduced ethylene to be 1:2, and keeping the temperature for 14min at 700 ℃.
Coating a layer of PMMA glue on a copper sheet of a graphene sheet grown by CVD (chemical vapor deposition), placing the copper sheet into a ferric chloride solution to remove copper, transferring the graphene sheet with the PMMA glue onto the carbon nanotube array, dissolving PMMA in alcohol, and placing the graphene sheet in an oxygen-free environment at 250 ℃ for annealing for 10 hours so as to remove residual glue and strengthen the combination of the graphene sheet and the carbon nanotube array.
Example 5
Depositing Al with the thickness of 3nm on a nickel substrate by adopting an atomic layer deposition technology2O3Transition layer of Al2O3And (3) evaporating and evaporating a nickel metal layer with the thickness of 10nm by adopting an electron beam on the transition layer to serve as a catalyst layer, and introducing hydrogen and methane in an argon atmosphere to carry out heat preservation treatment so as to vertically grow a carbon nano tube array on the catalyst layer. Controlling the volume flow ratio of the introduced hydrogen and the introduced methane to be 1:10, and keeping the temperature of 900 ℃ for 5min under the condition of heat preservation treatment.
Coating a layer of PMMA glue on a copper sheet of a graphene sheet grown by CVD (chemical vapor deposition) by using a glue throwing machine, then placing the copper sheet into a ferric chloride solution to remove copper, then transferring the graphene sheet with the PMMA glue onto the carbon nanotube array, dissolving PMMA by using alcohol, and then placing the graphene sheet in an oxygen-free environment for annealing at 500 ℃ for 4 hours so as to remove residual glue and strengthen the combination of the graphene sheet and the carbon nanotube array.
Example 6
The preparation procedure of example 6 is substantially the same as that of example 1, except that the step of transferring the graphene layer therein, i.e., the heat dissipation structure does not contain the graphene layer, is omitted.
Comparative example 1
The procedure of comparative example 1 was substantially the same as in example 1 except that the thickness of the iron metal layer as the catalyst layer was 20 nm.
Comparative example 2
Comparative example 2 was prepared by substantially the same procedure as in example 1 except that the thickness of the iron metal layer as the catalyst layer was 0.5 nm.
Comparative example 3
The preparation procedure of comparative example 3 was substantially the same as in example 1 except that the incubation treatment time for vertically growing the carbon nanotube array on the catalyst layer was 10 min.
Comparative example 4
The preparation procedure of comparative example 4 was substantially the same as in example 1 except that the incubation treatment time for vertically growing the carbon nanotube array on the catalyst layer was 35 min.
The carbon nanotube arrays in the heat dissipation structures prepared in examples 1 and 2 were subjected to Scanning Electron Microscopy (SEM), transmission electron microscopy (SEM) and raman testing for micro-morphology and structural characterization.
Fig. 3 shows a scanning electron microscope image and a transmission electron microscope image of the carbon nanotube array in the heat dissipation structure obtained in example 1, where a is a scanning electron microscope image magnified 120 times, b is a scanning electron microscope image magnified 50000 times, and c is a transmission electron microscope image. As can be seen from FIG. 3, the prepared carbon nanotube array has a regular structure, does not contain amorphous carbon, and has a height of 276 μm, a tube diameter of 31.5nm, and a number of tube walls of about 15.
Fig. 4 is a scanning electron microscope image of the carbon nanotube array in the heat dissipation structure prepared in example 2, wherein the magnification is 5000, the prepared carbon nanotube array has a regular structure, does not contain amorphous carbon, has a height of 64.8 μm, a tube diameter of 30nm, and the number of tube walls is about 15. From this, it is known that the height, i.e., the length of the carbon nanotube array is different depending on the growth time.
As shown in fig. 5, which is a transmission electron microscope image of the carbon nanotube array in the heat dissipation structure prepared in example 3, the prepared carbon nanotube array has a regular structure, does not contain amorphous carbon, has a height of 50 μm, a tube diameter of 12.7nm, and has about 10 tube walls. From this, it can be seen that the tube diameters of the carbon nanotube arrays are different depending on the thickness of the catalyst layer.
The carbon nanotube array in the heat dissipation structure prepared in example 4 has a regular structure, does not contain amorphous carbon, and has a height of 100 μm. The carbon nanotube array in the heat dissipation structure prepared in example 5 was neat and free of amorphous carbon, and the height thereof was 30 μm.
FIG. 6 shows a Raman spectrum of a carbon nanotube array in the heat dissipation structure prepared in example 1, where the abscissa of the Raman spectrum is the Raman shift in cm-1The ordinate is intensity in au. From these results, the defect rate of the carbon nanotube array was found to be 0.64 ID/IG. Namely, the grown carbon nanotube array has good structural integrity, a typical graphene structure and few defects.
Fig. 7 is a physical diagram of the heat dissipation structure manufactured in example 1, and a heat dissipation device is assembled by two identical heat dissipation structures in fig. 7 according to fig. 2. And testing the heat conducting performance of the assembled heat radiating device, and heating the heat source body under fixed power during testing. The traditional indium welding method is adopted as a control group for testing, and the difference of the traditional indium welding method and the heat dissipation device is that metal indium replaces a carbon nano tube array and a graphene layer in the heat dissipation device. The experimental environment was performed in the same relatively closed environment. And monitoring the temperature of the heat source body by adopting a thermal infrared imager.
Before the experiment, firstly, the thermal infrared imager is calibrated. For the results of the experiment to be obvious, the power for heating the heat source body was added to 1125 watts. To ensure the accuracy of the experiment, the heating process was measured for half an hour. The control was tested using a conventional indium welding method, where the heat source imaged a red spot in the thermal imager, showing a temperature of 51.9 ℃, as shown in fig. 8. When the heat dissipation device is used for half an hour under the same condition, the temperature displayed by the thermal imager in an imaging mode is 35.3 ℃, as shown in fig. 9. Therefore, the heat dissipation structure and the heat dissipation device have excellent heat dissipation performance.
The heat dissipation devices assembled by the heat dissipation structures prepared in comparative examples 1 to 4 according to fig. 2 were subjected to heat conduction performance tests by the above method, and the results show that the heat dissipation performance of the heat dissipation devices is significantly lower than that of the heat dissipation structure prepared in example 1.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (6)
1. The preparation method of the heat dissipation structure is characterized by comprising the following steps of:
sequentially depositing a transition layer and a catalyst layer on a substrate, introducing reducing gas and carbon source gas in a protective gas atmosphere, and preserving heat at 700-900 ℃ for 8-14 min to vertically grow a carbon nanotube array on the catalyst layer to obtain the heat dissipation structure; wherein the substrate is a metal substrate;
wherein the transition layer is Al2O3A layer, the thickness of the transition layer being 3-100 nm; the thickness of the catalyst layer is 0.8-10 nm, and the catalyst layer is a metal single layer of iron, cobalt or nickel; the volume flow ratio of the reducing gas to the carbon source gas is 1: 3-10; the reducing gasThe body is hydrogen; the carbon source gas is selected from one of acetylene, ethylene and methane; the length of the carbon nano tube is 30-100 mu m;
the preparation method further comprises the step of forming a graphene layer on the carbon nanotube array: the method comprises the steps of coating organic glue on a graphene sheet as a support, transferring the graphene sheet with the organic glue onto a carbon nano tube array, dissolving the organic glue by using an organic solvent, and annealing the heat dissipation structure containing the carbon nano tube array and the graphene layer for 1-3 hours at 250-500 ℃ in an oxygen-free environment.
2. The method of manufacturing a heat dissipation structure as defined in claim 1, wherein the transition layer has a thickness of 20 nm.
3. The method of claim 1, wherein the substrate is made of copper, nickel, or aluminum.
4. A heat dissipation structure, characterized by being produced by the method for producing a heat dissipation structure according to any one of claims 1 to 3.
5. A heat dissipating device comprising the heat dissipating structure according to claim 4.
6. The heat dissipating device according to claim 5, comprising at least two heat dissipating structures, wherein two heat dissipating structures are respectively disposed on two sides of a heat source body, and the graphene layer of the heat dissipating structure is in direct contact with the heat source body.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948105A (en) * | 2010-08-25 | 2011-01-19 | 上海理工大学 | Method for preparing vertical array of high-purity single-walled carbon nanotubes |
| CN102651961A (en) * | 2012-05-29 | 2012-08-29 | 邱璟 | Heat-conduction heat-dissipation interface material and manufacturing method thereof |
| CN106281257A (en) * | 2016-08-12 | 2017-01-04 | 曹蕊 | A kind of thermal interfacial material with Graphene and preparation method thereof |
| CN107059004A (en) * | 2017-04-19 | 2017-08-18 | 江苏联科纳米科技有限公司 | A kind of high radiant rate heat radiating metal paper tinsel and preparation method and application |
-
2017
- 2017-12-26 CN CN201711437642.8A patent/CN108122870B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948105A (en) * | 2010-08-25 | 2011-01-19 | 上海理工大学 | Method for preparing vertical array of high-purity single-walled carbon nanotubes |
| CN102651961A (en) * | 2012-05-29 | 2012-08-29 | 邱璟 | Heat-conduction heat-dissipation interface material and manufacturing method thereof |
| CN106281257A (en) * | 2016-08-12 | 2017-01-04 | 曹蕊 | A kind of thermal interfacial material with Graphene and preparation method thereof |
| CN107059004A (en) * | 2017-04-19 | 2017-08-18 | 江苏联科纳米科技有限公司 | A kind of high radiant rate heat radiating metal paper tinsel and preparation method and application |
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