CN112708401A - Processing system and method for graphene film with micro thermal structure pattern - Google Patents
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Abstract
The invention relates to a processing system of a graphene film with a micro thermal structure pattern, which comprises a filter cup, a suction filtration liquid collection bottle, a vacuum pump, a fixing clamp for holding a filter membrane, an ultrasonic water tank and a pattern processing device, wherein the filter cup is arranged on the upper surface of the filter cup; the filter cup and the suction filtration liquid collection bottle are buckled up and down, the filter membrane is arranged between the filter cup and the suction filtration liquid collection bottle, and the vacuum pump is communicated with the suction filtration liquid collection bottle; the suction filtration liquid collection bottle is arranged in the ultrasonic water tank; the pattern processing device is used for processing a thermal structure pattern on the graphene film. The invention overcomes the trend that the heat dissipation structure can not follow the electronic manufacturing to manufacture the minimized multifunctional device; the requirements of simple equipment, easy operation, low cost, high precision, high flexibility and the like are further met.
Description
Technical Field
The invention relates to the technical field of graphene, in particular to a system and a method for processing a graphene film with a micro thermal structure pattern.
Background
Heat energy is very common in life, and brings convenience to human society and simultaneously solves problems which are difficult to overcome. Electronic devices generate heat during operation, while electronic components are generally temperature sensitive, and some electronic components have thermal characteristics that change rapidly with temperature changes during operation, such as the thermal performance of a chip package encapsulation module changes with temperature changes. The service life and reliability of the electronic element are reduced along with the increase of the working temperature, the key for improving the service life and reliability of the electronic element is to solve the heat dissipation problem, effective heat dissipation has a close relation to higher reliability and longer service life of the electronic element, and therefore the effective treatment of the heat effect problem is crucial to the further research and development of the electronic element. Thermal management is increasingly becoming a non-negligible important component of electronic packaging.
In recent years, with the rapid development of electronic technology, electronic devices are not only applied to military fields such as airplanes, satellites, space shuttles, naval vessels and submarines, but also widely applied to civil fields such as industrial production, communication systems and personal computers. Along with the development of society, the contradiction in the development of electronic equipment is increasingly sharp, on one hand, the electronic equipment is small in size, has multiple functions, is high in portability, and has wide adaptability and development requirements on the environment, and the problem of heat control of the equipment is more and more difficult due to heat constraint. The current trend in electronic components is to manufacture powerful devices in a minimum size, which puts a great strain on the heat dissipation requirements of the electronic device package, where the performance and life cycle of the device is critical. Therefore, controlling the temperature of these components is the best way to increase the lifetime of electronic products. Therefore, efficient heat dissipation of electronic equipment is very important, and the heat dissipation performance directly determines the service life of the equipment.
At present, the common heat dissipation methods of electronic components include natural cooling, energy dispersion and the like. For example, a heat dissipation method for a computer generally utilizes a heat sink and a fan. While the heat sink is typically made of a material with a high heat capacity, such as aluminum and copper, in order to absorb more heat at a lower temperature rise. By adopting a metal heat dissipation mode, when a circuit board is designed, the thickness of a heat dissipation copper foil is specially increased, or a large-area power supply and a ground copper foil are used, or more heat conduction holes are used.
However, these heat dissipation methods are not directed to local heat dissipation, and the heat dissipation efficiency of this heat dissipation method increases with the increase of the space occupied by the device. The leading trend in electronics manufacturing is to produce multifunctional devices with minimized size, and current heat dissipation approaches are not satisfactory. Therefore, there is a need to develop a new method with smaller size, lighter weight and higher pertinence to effectively guide and shield the heat on the electronic component, and satisfy the development of the electronic component toward being small, light and portable while realizing thermal protection.
Graphene has very good thermal conductivity, is one of the highest known materials, has very good toughness, can be bent, and is expected to be used for thermal protection of electronic components.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a system and a method for processing a graphene film with a micro thermal structure pattern, which can realize thermal protection and meet the requirements of small size, light weight and portability of electronic elements.
In order to achieve the purpose, the invention adopts the following technical scheme:
a processing system of a graphene film with a micro thermal structure pattern comprises a filter cup, a suction filtration liquid collection bottle, a vacuum pump, a fixing clamp for holding a filter membrane, an ultrasonic water tank and a pattern processing device; the filter cup and the suction filtration liquid collection bottle are buckled up and down, the filter membrane is arranged between the filter cup and the suction filtration liquid collection bottle, and the vacuum pump is communicated with the suction filtration liquid collection bottle; the suction filtration liquid collection bottle is arranged in the ultrasonic water tank; the pattern processing device is used for processing a thermal structure pattern on the graphene film.
A method of using a processing system for graphene thin films having a micro thermal structure pattern, comprising the steps of:
fixing a filter membrane between a filter cup and a suction filtration liquid collecting bottle;
step two, preparing uniform carbon fiber turbid liquid and graphene turbid liquid;
pouring the carbon fiber suspension into a filter cup, starting a vacuum pump, and depositing a carbon fiber precursor on the upper surface of the filter membrane;
pouring the graphene turbid liquid into a filter cup, starting a vacuum pump, and depositing graphene in the carbon fiber precursor to obtain a graphene film;
step five, pasting the filter membrane on the glass substrate, and putting the glass substrate into a vacuum drying oven for drying;
taking out the filter membrane, cooling, and stripping the graphene film from the filter membrane;
processing a pattern with a micro thermal structure on the graphene film, and removing the graphene film except the micro thermal structure pattern;
and step eight, distributing the graphene film with the micro thermal structure pattern in an area needing to specifically realize thermal management by adopting a method of covering or embedding the circuit board.
In a further elaboration, said step seven of patterning the micro thermal structure using photolithography, comprises the steps of,
step S71, transferring the obtained complete graphene film to a PET film and attaching the complete graphene film to a glass substrate;
step S72, carrying out photoetching process on the graphene film and leaving a mask plate with a target pattern on the surface of the graphene film, introducing O2 plasma for surface treatment, introducing O2, keeping the pressure at 70kPA and the temperature at 60 ℃ for 30S, and removing the part of the graphene film which is not protected by the mask plate;
step S73: removing the photoresist mask on the surface of the graphene film in the spraying reaction medicine chamber to obtain the graphene film with the micro thermal structure pattern;
step S74: and introducing Ar into the obtained graphene film with the micro thermal structure pattern at 300 ℃ for annealing for 60 min.
In a further aspect, the seventh step of patterning the micro thermal structure using a laser etching method includes the steps of,
step S81: transferring the obtained complete graphene film to a PET film and fixing the complete graphene film on a laser workbench;
step S82: removing the part of the graphene film except the target pattern to obtain the graphene film with the thermal control function;
step S83: and bending one corner of the PET film towards the side without the graphene, and peeling the graphene film from the PET film.
More specifically, the wavelength of the laser is 355mm, the laser power is 10W, the current range is 50% -75%, and the laser is irradiated until the target pattern is etched.
Further, when the carbon fiber suspension is prepared in the second step, deionized water is poured into a beaker filled with carbon fibers with the length of 1-5mm, and the mass ratio of the deionized water to the carbon fibers is 3000-5000: 1, and sonicated for 30 minutes.
Further, when the graphene turbid liquid is prepared in the second step, deionized water is poured into a beaker filled with flash-evaporated graphene, and the mass ratio of the deionized water to the carbon fiber is 3000-4000: 1, and sonicated for 30 minutes.
More specifically, the step five is baked at the temperature of 55-65 ℃ for 50 minutes.
Further, in the third step and the fourth step, the ultrasonic treatment is performed on the processing system in the vacuum filtration process.
In a further aspect, the pattern of step seven includes a combination of patterns that perform heat shielding, heat spinning, or heat focusing functions.
The invention has the beneficial effects that: according to the invention, the pattern with the heat manipulation function is processed on the graphene film, the pattern can be transformed and distributed in the area needing to realize heat management pertinently according to different use environments or heat flow control area changes, heat shielding, heat rotation and heat collection of a specific area can be realized, heat flow manipulation is realized, pertinence of heat flow manipulation and accuracy of heat flow manipulation are improved, and flexibility of random transformation along with the heat flow control area is enhanced; the graphene is adopted to control heat flow, so that the trend that a heat dissipation structure cannot follow electronic manufacturing to manufacture minimized multifunctional devices is overcome; the requirements of simple equipment, easy operation, low cost, high precision, high flexibility and the like are further met, the device can be applied to electronic elements which are small in size, light in weight, sensitive to heat and need high targeted protection, and the device can meet the requirement that the electronic elements have a large development space in the directions of being small, light and portable while realizing thermal protection.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a schematic overall structure of one embodiment of the present invention;
FIG. 2 is a schematic structural diagram of one embodiment of the present invention;
FIG. 3 is a flow chart of one embodiment of the present invention;
fig. 4 is a schematic structural diagram of an embodiment of the present invention.
Wherein: the device comprises a filter cup 1, a fixing clamp 2, a base 3, a suction filtration liquid collecting bottle 4, a filter membrane 5, a pattern processing device 7, a vacuum pump 8, a pumping pipe 9, a heating area 10, a first heat sensitive electronic element placing area 11, a second heat sensitive electronic element placing area 12 and an ultrasonic water tank 14.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
As shown in fig. 1-2, a processing system of a graphene film with a micro thermal structure pattern comprises a filter cup 1, a suction filtration liquid collection bottle 4, a vacuum pump 8, a fixing clamp 2 for holding a filter membrane 5, an ultrasonic water tank 14 and a pattern processing device 7; the filter cup is vertically buckled with the suction filtration liquid collection bottle 4, the filter membrane 5 is arranged between the filter cup and the suction filtration liquid collection bottle 4, and the vacuum pump 8 is communicated with the suction filtration liquid collection bottle 4; the suction filtration liquid collecting bottle 4 is arranged in the ultrasonic water tank 14; the pattern processing device 7 is used for processing a thermal structure pattern on the graphene film.
Filter cup 1 and be used for holding carbon fiber turbid liquid and graphite alkene turbid liquid, suction filtration collecting bottle 4 and vacuum pump 8 are used for suction filtration carbon fiber turbid liquid and graphite alkene turbid liquid, and wherein vacuum pump 8 links to each other with suction filtration collecting bottle 4 through taking out pipe 9. Filter membrane 5 is used for deposiing carbon fiber precursor and graphite alkene, and suction filtration liquid collecting bottle 4 sets up in the supersound basin 14, supersound basin 14 just can be at the in-process vibrations that keep suction filtration liquid collecting bottle 4 of suction filtration, make the even deposit of carbon fiber turbid liquid and graphite alkene turbid liquid of straining. After the complete graphene film is prepared, the required thermal structure pattern is processed by using the pattern processing device 7, and the whole system is simple and convenient and is easy to operate. Ultrasonic wave is exerted to ultrasonic water tank 14 at the in-process of suction filtration, makes the turbid liquid more even, deposits out the graphite alkene film of thickness unanimity. In order to stabilize the stability of the filter membrane 5 in the operation process, the fixing clamp 2 holds the filter membrane 5, and more preferably, a base 3 is arranged between the suction filtration liquid collecting bottle 4 and the filter cup 1 and used for placing the filter membrane 5.
As shown in fig. 3, a method of using a processing system of a graphene thin film having a micro thermal structure pattern includes the steps of:
firstly, fixing a filter membrane 5 between a filter cup and a suction filtration liquid collecting bottle 4;
step two, preparing uniform carbon fiber turbid liquid and graphene turbid liquid;
pouring the carbon fiber suspension into the filter cup 1, starting the vacuum pump 8, and depositing a carbon fiber precursor on the upper surface of the filter membrane 5;
pouring the graphene turbid liquid into a filter cup 1, starting a vacuum pump 8, and depositing graphene in the carbon fiber precursor to obtain a graphene film;
step five, pasting the filter membrane 5 on the glass substrate, and putting the glass substrate into a vacuum drying oven for drying;
taking out the filter membrane 5, cooling, and stripping the graphene film from the filter membrane 5;
processing a pattern with a micro thermal structure on the graphene film, and removing the graphene film except the micro thermal structure pattern;
and step eight, distributing the graphene film with the micro thermal structure pattern in an area needing to specifically realize thermal management by adopting a method of covering or embedding the circuit board.
The filter membrane 5 is provided with a layer of PDMS, and the PDMS is not adhered to graphene, the graphene membrane is adhered to the filter membrane 5 together after vacuum filtration because moisture exists, and after vacuum drying and cooling, the graphene membrane is not adhered to the filter membrane 5 and is directly in a separated state; if the small area is adhered, the glass sheet is held to slightly knock the side surface, and the graphene film can slide down. And then processing a thermal operation pattern on the graphene film, so that the graphene film with the micro thermal structure pattern can be manufactured by the method.
The thermal structure pattern is composed of three basic micro thermal structure patterns, including a thermal rotation pattern, a thermal aggregation pattern and a thermal shielding pattern, the corresponding patterns are arranged according to the needs of the electronic elements, the thermal shielding pattern is arranged around the heat sensitive electronic elements, the thermal rotation pattern is arranged around the heating elements, and the rest part is composed of outward diffusion conduction curves. The pattern can be changed correspondingly according to different relative positions of various electronic elements, and each electronic element with different distribution types can be accurately protected, so that the flexibility is high.
As shown in fig. 4, the processed graphene film has a preset heat-generating region 10, a first heat-sensitive electronic element placing region 11, a second heat-sensitive electronic element placing region 12, and lines between the three regions, and because different materials with different thermal conductivity coefficients alternately implement energy dispersion, the heat emitted by the elements in the heat-generating region 10 is less likely to affect the first heat-sensitive electronic element placing region 11 and the second heat-sensitive electronic element placing region 12, or the heat emitted by the elements in the heat-generating region 10 is more likely to affect the first heat-sensitive electronic element placing region 11 and the second heat-sensitive electronic element placing region 12.
From a two-dimensional view, the patterned graphene sheets and air alternate with each other, that is, two materials with large thermal conductivity coefficient difference alternate with each other, and thus the thermal device formed in this form has a thermal manipulation function.
The covering is to directly adhere the patterned graphene sheet to the surface of the electronic component substrate, such as the surface of a circuit board; embedding is the cutting of the substrate into two pieces and then sandwiching the patterned graphene sheets between them.
In a further elaboration, said step seven of patterning the micro thermal structure using photolithography, comprises the steps of,
step S71, transferring the obtained complete graphene film to a PET film and attaching the complete graphene film to a glass substrate;
step S72, carrying out photoetching process on the graphene film and leaving a mask plate with a target pattern on the surface of the graphene film, and introducing O2Plasma surface treatment with introduced O2Removing the part of the graphene film which is not protected by the mask plate under the pressure of 70kPA and the temperature of 60 ℃ for 30 s;
step S73: removing the photoresist mask on the surface of the graphene film in the spraying reaction medicine chamber to obtain the graphene film with the micro thermal structure pattern;
step S74: and introducing Ar into the obtained graphene film with the micro thermal structure pattern at 300 ℃ for annealing for 60 min.
The method comprises the steps of transferring the graphene film to a PET film and attaching the graphene film to a glass substrate to facilitate a photoetching process, wherein a layer of positive photoresist is coated on the surface of the graphene in a spin coating mode, and then the graphene film is exposed to ultraviolet raysA light for exposing the thermal structure pattern through the mask and covering the rest part, wherein the ultraviolet irradiation part is a thermal operation pattern part; and adding a developing solution after the exposure is finished, dissolving the photoresist in the unexposed area in the developing solution, and leaving a layer of mask plate with a thermal operation pattern formed by the photoresist on the surface of the graphene film. Then introducing O2And etching a pattern by using a plasma, removing the residual photoresist mask, and performing an annealing process to obtain the graphene film with the micro thermal structure pattern.
In a further aspect, the seventh step of patterning the micro thermal structure using a laser etching method includes the steps of,
step S81: transferring the obtained complete graphene film to a PET film and fixing the complete graphene film on a laser workbench;
step S82: removing the part of the graphene film except the target pattern to obtain the graphene film with the thermal control function;
step S83: and bending one corner of the PET film towards the side without the graphene, and peeling the graphene film from the PET film.
More specifically, the wavelength of the laser is 355mm, the laser power is 10W, the current range is 50% -75%, and the laser is irradiated until the target pattern is etched.
The wavelength is fixed 355nm, the power is 10W, the energy of the laser is adjusted by adjusting the current, the current range is 50% -75%, and the repetition frequency is two times or more, so long as the purpose of etching is achieved, the continuous repetition is not needed.
When the current is below 50%, the unnecessary part cannot be quickly and effectively etched, and the time, the labor and the efficiency are low because the processing is repeated all the time; when the current is increased to more than 75%, the thermal influence and the beam quality are also increased, the requirement of superfine line width cannot be met, and the residual graphene is easily damaged.
Further, when the carbon fiber suspension is prepared in the second step, deionized water is poured into a beaker filled with carbon fibers with the length of 1-5mm, and the mass ratio of the deionized water to the carbon fibers is 3000-5000: 1, and sonicated for 30 minutes.
The carbon fiber is 1mm-5mm, the longer the carbon fiber in the range, the better the network toughness built by the longer carbon fiber, but the longer the carbon fiber is, the more difficult the carbon fiber is to be uniformly dispersed in water, the deposited carbon fiber layer is not uniform, and the performance of each position of the graphene film is not uniform.
Further, when the graphene turbid liquid is prepared in the second step, deionized water is poured into a beaker filled with flash-evaporated graphene, and the mass ratio of the deionized water to the carbon fiber is 3000-4000: 1, and sonicated for 30 minutes.
Joule heat flash graphene is selected because of its advantages of being mass processable and low cost.
More specifically, the step five is baked at the temperature of 55-65 ℃ for 50 minutes.
60 ℃ is an optimum temperature found experimentally. The more holes in the graphene sheet, the better the heat conduction, when the graphene sheet is evaporated to dryness, a large amount of water in the graphene sheet escapes in a water vapor mode, holes are left in the graphene sheet, the holes generated by the escape of water vapor have no more high temperature when the temperature is lower, and if the temperature is too high, the defects of cracks and the like can occur on the surface of the graphene film. Baking until insufficient moisture is present in the graphene film to allow the graphene film to cool and continue to adhere to the filter membrane 5.
Further, in the third step and the fourth step, the ultrasonic treatment is performed on the processing system in the vacuum filtration process.
The concentration of the graphene turbid liquid is suddenly increased in the suction filtration process, and the aggregated graphene is easily generated in the mixed solution and is uniformly dispersed by adopting ultrasound. The sonication is stopped while the graphene film is shaped.
In a further aspect, the pattern of step seven includes a combination of patterns that perform heat shielding, heat spinning, or heat focusing functions.
The pattern described herein is a combination pattern, which is a basic pattern of heat shielding, heat rotation and heat aggregation, and is a design pattern flexible according to the relative position of electronic components or the heat manipulation required by the electronic components, for example, a heat shielding pattern is provided around a thermosensitive component requiring heat protection; the heat generating element needs heat dissipation, and a heat shield is arranged on one side close to the thermosensitive element, and a heat aggregation pattern is arranged on the other side.
The above description is only a preferred embodiment of the present invention, and for those skilled in the art, the present invention should not be limited by the description of the present invention, which should be interpreted as a limitation.
Claims (10)
1. A system for processing a graphene film with a micro thermal structure pattern is characterized in that: comprises a filter cup, a suction filtration liquid collection bottle, a vacuum pump, a fixing clamp for holding a filter membrane, an ultrasonic water tank and a pattern processing device; the filter cup and the suction filtration liquid collection bottle are buckled up and down, the filter membrane is arranged between the filter cup and the suction filtration liquid collection bottle, and the vacuum pump is communicated with the suction filtration liquid collection bottle; the suction filtration liquid collection bottle is arranged in the ultrasonic water tank; the pattern processing device is used for processing a thermal structure pattern on the graphene film.
2. The method of using the system for processing a graphene thin film having a micro thermal structure pattern according to claim 1, comprising the steps of:
fixing a filter membrane between a filter cup and a suction filtration liquid collecting bottle;
step two, preparing uniform carbon fiber turbid liquid and graphene turbid liquid;
pouring the carbon fiber suspension into a filter cup, starting a vacuum pump, and depositing a carbon fiber precursor on the upper surface of the filter membrane;
pouring the graphene turbid liquid into a filter cup, starting a vacuum pump, and depositing graphene in the carbon fiber precursor to obtain a graphene film;
step five, pasting the filter membrane on the glass substrate, and putting the glass substrate into a vacuum drying oven for drying;
taking out the filter membrane, cooling, and stripping the graphene film from the filter membrane;
processing a pattern with a micro thermal structure on the graphene film, and removing the graphene film except the micro thermal structure pattern;
and step eight, distributing the graphene film with the micro thermal structure pattern in an area needing to specifically realize thermal management by adopting a method of covering or embedding the circuit board.
3. The method for processing a graphene thin film with a micro thermal structure pattern according to claim 2, wherein: said seventh step of patterning the micro thermal structure using photolithography, comprises the steps of,
step S71, transferring the obtained complete graphene film to a PET film and attaching the complete graphene film to a glass substrate;
step S72, carrying out photoetching process on the graphene film and leaving a mask plate with a target pattern on the surface of the graphene film, introducing O2 plasma for surface treatment, introducing O2, keeping the pressure at 70kPA and the temperature at 60 ℃ for 30S, and removing the part of the graphene film which is not protected by the mask plate;
step S73: removing the photoresist mask on the surface of the graphene film in the spraying reaction medicine chamber to obtain the graphene film with the micro thermal structure pattern;
step S74: and introducing Ar into the obtained graphene film with the micro thermal structure pattern at 300 ℃ for annealing for 60 min.
4. The method for processing a graphene thin film with a micro thermal structure pattern according to claim 2, wherein: and a seventh step of patterning the micro thermal structure using a laser etching method, including the steps of,
step S81: transferring the obtained complete graphene film to a PET film and fixing the complete graphene film on a laser workbench;
step S82: removing the part of the graphene film except the target pattern to obtain the graphene film with the thermal control function;
step S83: and bending one corner of the PET film towards the side without the graphene, and peeling the graphene film from the PET film.
5. The method for processing a graphene thin film with a micro thermal structure pattern according to claim 4, wherein: the wavelength of the adopted laser is 355mm, the laser power is 10W, the current range is 50% -75%, and the laser irradiates until the target pattern is etched.
6. The method for processing a graphene thin film with a micro thermal structure pattern according to claim 2, wherein: when carbon fiber turbid liquid is prepared in the step two, pouring deionized water into a beaker filled with 1-5mm long carbon fibers, wherein the mass ratio of the deionized water to the carbon fibers is 3000-5000: 1, and sonicated for 30 minutes.
7. The method for processing a graphene thin film with a micro thermal structure pattern according to claim 2, wherein: when the graphene turbid liquid is prepared in the step two, pouring deionized water into a beaker filled with flash-evaporated graphene, wherein the mass ratio of the deionized water to the carbon fibers is 3000-4000: 1, and sonicated for 30 minutes.
8. The method for processing a graphene thin film with a micro thermal structure pattern according to claim 2, wherein: and baking the obtained product at the temperature of 55-65 ℃ for 50 minutes in the step five.
9. The method for processing a graphene thin film with a micro thermal structure pattern according to claim 2, wherein: and in the third step and the fourth step, carrying out ultrasonic treatment on the processing system in the vacuum filtration process.
10. The method for processing a graphene thin film with a micro thermal structure pattern according to claim 2, wherein: the pattern of step seven includes a combination of patterns that perform heat shielding, heat rotation, or heat aggregation functions.
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CN109742019A (en) * | 2019-01-21 | 2019-05-10 | 广东工业大学 | A method of utilizing hard mask plate in ultraviolet laser processing dry etching |
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