CN111673086A - Porous fiber liquid absorption core with surface in-situ grown carbon nano tube and preparation method - Google Patents
Porous fiber liquid absorption core with surface in-situ grown carbon nano tube and preparation method Download PDFInfo
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- CN111673086A CN111673086A CN202010462471.XA CN202010462471A CN111673086A CN 111673086 A CN111673086 A CN 111673086A CN 202010462471 A CN202010462471 A CN 202010462471A CN 111673086 A CN111673086 A CN 111673086A
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- nano tube
- liquid absorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/002—Manufacture of articles essentially made from metallic fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3733—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon having a heterogeneous or anisotropic structure, e.g. powder or fibres in a matrix, wire mesh, porous structures
Abstract
The invention discloses a porous fiber liquid absorption core with a surface in-situ grown carbon nano tube and a preparation method thereof; cutting continuous long fibers from a stainless steel rod by using a multi-tooth turning tool; cutting the long fiber into short fiber and pressing the short fiber into a mold; putting the mould into a vacuum sintering furnace for solid-phase sintering; after the sintering furnace is cooled to room temperature, taking out the stainless steel fiber sintered porous material; cleaning and pickling the surface of the porous fiber liquid absorption core; putting the porous fiber liquid absorption core into an atmosphere sintering furnace, and growing the carbon nano tube in situ by adopting thermal CVD; after the composite porous fiber liquid absorption core is cooled to room temperature, the composite porous fiber liquid absorption core has a three-dimensional net-shaped porous structure with a carbon nano tube with high thermal conductivity attached to the surface, and has the advantages of high specific surface area, good boiling heat exchange performance, simple manufacturing process, low cost and the like.
Description
Technical Field
The invention relates to the field of heat exchange enhancement and liquid absorption cores, in particular to a porous fiber liquid absorption core with a surface in-situ grown carbon nano tube and a preparation method thereof.
Background
Microelectronics, optoelectronics, and the like have become the core technologies of the current high-tech and information industries. Along with the development of microelectronic and optoelectronic chips towards high integration and high performance, microelectronic and optoelectronic products are also continuously developing towards miniaturization, high integration and portability. High heat flux density is associated with high performance microelectronic devices, placing higher demands on heat dissipation. The heat flow density of the high-performance microprocessor at the present stage can reach 100W/cm2, and the heat flow density of the high-power LED chip can reach 200W/cm 2. Excessive operating temperatures can adversely affect the reliability and useful life of microelectronic chips. The conventional heat dissipation method with low heat dissipation efficiency has been gradually unable to meet the current and future heat dissipation requirements of electronic devices, and the efficient heat dissipation scheme of electronic components is becoming urgent.
The heat pipe is a high-efficiency phase-change heat transfer element, has the characteristics of extremely high heat conductivity, small volume and light weight, and can strengthen heat transfer of all parts without additional electric drive. These excellent thermal properties and high heat transfer efficiency make micro heat pipes ideal for heat dissipation in high heat flux microelectronic devices.
According to different liquid absorption core preparation methods, the micro heat pipe can be divided into a groove type, a powder sintering type, a silk screen sintering type, a fiber sintering type and the like, and has good isothermal property. Different types of wicks have different characteristics, such as small groove-type backflow resistance, but small capillary force; the powder sintered type has a large capillary force but also a large reflow resistance. The fiber sintered type wick has more balanced performance compared with the former two wicks.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings of the prior art and provides a porous fiber liquid absorbing core with a carbon nano tube growing on the surface in situ and a preparation method thereof. The liquid absorption core has the characteristics of high heat transfer efficiency and good capillary performance. The preparation method has simple process and does not need to additionally add a catalyst.
The invention is realized by the following technical scheme:
a preparation method of a porous fiber liquid absorbing core with a surface in-situ grown carbon nano tube comprises the following steps:
the method comprises the following steps: preparing stainless steel fiber by a turning method;
step two: cutting stainless steel fiber with diameter of 70-150 μm to length of 8-10 mm; cleaning stainless steel short fiber with 5-10% NaOH solution for 5-10min, cleaning with deionized water, and placing in dilute HC with volume concentration of 5-10%1Soaking in the solution for 3-5 min; then taking out, cleaning and drying for later use to obtain stainless steel short fibers;
step three: filling stainless steel short fibers into a die cavity of a die and pressing the stainless steel short fibers; then putting the mixture into a sintering furnace for solid phase sintering;
step four: the solid phase sintering temperature is 1100-1300 ℃, and the sintering process adopts a heating mode of sectional heating: when the temperature in the sintering furnace is lower than 750-800 ℃, the heating rate is 5 ℃, when the temperature in the furnace reaches 750-800 ℃, the heating rate is 3 ℃, and the sintering time is 60-120 min, so as to obtain the stainless steel short fiber porous material;
step five: taking out the stainless steel short fiber porous material after solid phase sintering from the mold, cleaning, drying, then putting into a CVD tubular furnace to grow carbon nano tubes, and firstly introducing N2Entering a CVD tube furnace and heating to 650-700 ℃; when the furnace temperature reaches 650-700 ℃, H is introduced2And C2H2The mixed gas starts to grow the carbon nano tube, and the growth time is 15-30 mins;
and cooling the carbon nano tube to room temperature along with the furnace after the growth of the carbon nano tube is finished, and taking out the sample to obtain the porous fiber liquid absorption core with the carbon nano tube growing in situ on the surface.
And step five, cleaning, namely using deionized water and absolute ethyl alcohol in sequence, and performing ultrasonic cleaning for 10 min.
The carbon nano tubes are arranged in a disordered mode, the thickness of the carbon nano tubes is 50-100 mu m, and the surface coverage rate is larger than 90%.
Compared with the prior art, the invention has the following advantages and effects:
the invention uses a multi-tooth lathe tool to cut continuous long fiber from a stainless steel bar; cutting the long fiber into short fiber and pressing the short fiber into a mold; putting the mould into a vacuum sintering furnace for solid-phase sintering; after the sintering furnace is cooled to room temperature, taking out the stainless steel fiber sintered porous material; cleaning and pickling the surface of the porous fiber liquid absorption core; putting the porous fiber liquid absorption core into an atmosphere sintering furnace, and growing the carbon nano tube in situ by adopting thermal CVD; and cooling to room temperature, and taking out the composite porous fiber liquid absorption core. By adopting the preparation process, the surface appearance of the liquid absorption core is richer, and the surface of the fiber liquid absorption core has a nano-scale tubular/filamentous structure after the carbon nano tubes grow on the surface. The rich surface structure can increase the capillary performance of the liquid absorption core without greatly increasing the reflux resistance; the carbon nano tubes on the surface are added with catalyst in a disordered way, so that the bonding force with the substrate is stronger;
the axial heat conductivity coefficient of the carbon nano tube covered on the surface of the liquid absorption core can reach 2000W/m-1K-1The thermal conductivity of the copper is more than 5 times that of the copper, and the heat transfer efficiency is greatly improved.
After the stainless steel liquid absorption core for growing the carbon nano tube is applied to the liquid absorption core of the heat pipe, the temperature distribution is more uniform, the local overheating is prevented, and therefore the ultimate power of the heat pipe is effectively improved.
The porous fiber liquid absorption core with the carbon nano tubes growing in situ on the surface has a three-dimensional net-shaped porous structure with the carbon nano tubes with high thermal conductivity attached to the surface, and has the advantages of high specific surface area, good boiling heat exchange performance, simple manufacturing process, low cost and the like.
Drawings
FIG. 1 is an SEM image of a stainless steel fiber porous wick without carbon nanotubes grown thereon according to the present invention;
FIG. 2 is an SEM image of a stainless steel fiber porous wick after carbon nanotubes have grown in accordance with the present invention.
Fig. 3 is a schematic view of the structure of a mold used in the manufacturing process of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
The preparation process of the porous fiber liquid absorbing core with the surface in-situ grown carbon nano tube comprises the following steps:
and (3) preparing the stainless steel fiber by a turning method. Firstly, cleaning a stainless steel bar by using an alkaline degreasing agent, and cutting and removing surface oxide skin after clamping the stainless steel bar on a lathe. Then a multi-tooth cutter with a large blade inclination angle is changed, and the stainless steel fiber is cut on a lathe. The cutter is made of superhard high-speed steel.
Cutting the stainless steel fiber with the diameter of about 70-150 mu m to the length of about 10 mm; cleaning stainless steel short fiber with 5-10% NaOH solution for 5-10min, cleaning with deionized water, and placing in dilute HC with volume concentration of 5-10%1Soaking in the solution for 3-5 min; then taking out, cleaning and drying for later use to obtain the stainless steel short fiber. The cleaning and drying process can be carried out by rinsing with tap water and then drying with a drying oven.
And (3) molding the stainless steel porous fiber liquid absorption core. Weighing a certain amount of stainless steel short fibers according to different porosities (the smaller the porosity, the more the stainless steel short fibers are, which can be determined according to the actual application requirements), filling into a cavity of a die and compacting; then putting the mould into a sintering furnace for solid-phase sintering;
the structure of the mold used in the present invention is shown in fig. 3. The die comprises a bolt 1, an upper pressing plate 2, a die cavity plate 3, a lower pressing plate 4, a die cavity boss 5 and a die cavity 6. Stainless steel short fibers are placed in the die cavity 6, and the upper pressing plate 2 and the lower pressing plate 4 are locked through the bolts 1 so as to tightly press and compact the stainless steel short fibers in the die cavity 6.
When solid-phase sintering is carried out, the temperature is 1100-1300 ℃, a heating mode of sectional temperature rise is adopted in the sintering process, when the temperature in a sintering furnace is lower than 800 ℃, the temperature rise rate is 5 ℃, when the temperature in the furnace reaches 800 ℃, the temperature rise rate is 3 ℃, and the sintering time is 60-120 min (determined according to the thickness and the size of a sintered workpiece), so as to obtain the stainless steel short fiber porous material;
the final process is to grow carbon nanotube by CVD process. Taking out the solid-phase sintered stainless steel short fiber porous material from the mold, cleaning, drying (sequentially cleaning with deionized water and anhydrous ethanol for 10min, drying), placing into a CVD tube furnace to grow carbon nanotubes, and introducing N2Entering a CVD tube furnace and heating to 700 ℃; when the furnace temperature reaches 700 ℃, H is introduced2And C2H2The mixed gas starts to grow the carbon nano tube, and the growth time is 15-30 mins.
The carbon nano tubes are arranged in disorder, the thickness is 50-100 mu m, and the surface coverage rate is more than 90%.
In conclusion, the invention discloses a manufacturing process for in-situ growth of carbon nanotubes on the surface of a porous fiber liquid absorption core taking stainless steel as a matrix. Cutting continuous long fibers from a stainless steel rod by using a multi-tooth turning tool; cutting the long fiber into short fiber and pressing the short fiber into a mold; putting the mould into a vacuum sintering furnace for solid-phase sintering; after the sintering furnace is cooled to room temperature, taking out the stainless steel fiber sintered porous material; cleaning and pickling the surface of the porous fiber liquid absorption core; putting the porous fiber liquid absorption core into an atmosphere sintering furnace, and growing the carbon nano tube in situ by adopting thermal CVD; after the composite porous fiber liquid absorption core is cooled to room temperature, the composite porous fiber liquid absorption core has a three-dimensional net-shaped porous structure with a carbon nano tube with high thermal conductivity attached to the surface, and has the advantages of high specific surface area, good boiling heat exchange performance, simple manufacturing process, low cost and the like.
The embodiments of the present invention are not limited to the above-described embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and they are included in the scope of the present invention.
Claims (4)
1. A preparation method of a porous fiber liquid absorbing core with a surface in-situ grown carbon nano tube is characterized by comprising the following steps:
the method comprises the following steps: preparing stainless steel fiber by a turning method;
step two: cutting stainless steel fiber with diameter of 70-150 μm to length of 8-10 mm; cleaning stainless steel short fiber with 5-10% NaOH solution for 5-10min, cleaning with deionized water, and placing in dilute HC with volume concentration of 5-10%1Soaking in the solution for 3-5 min; then taking out, cleaning and drying for later use to obtain stainless steel short fibers;
step three: filling stainless steel short fibers into a die cavity of a die and pressing the stainless steel short fibers; then putting the mixture into a sintering furnace for solid phase sintering;
step four: the solid phase sintering temperature is 1100-1300 ℃, and the sintering process adopts a heating mode of sectional heating: when the temperature in the sintering furnace is lower than 750-800 ℃, the heating rate is 5 ℃, when the temperature in the furnace reaches 750-800 ℃, the heating rate is 3 ℃, and the sintering time is 60-120 min, so as to obtain the stainless steel short fiber porous material;
step five: taking out the stainless steel short fiber porous material after solid phase sintering from the mold, cleaning, drying, then putting into a CVD tubular furnace to grow carbon nano tubes, and firstly introducing N2Entering a CVD tube furnace and heating to 650-700 ℃; when the furnace temperature reaches 650-700 ℃, H is introduced2And C2H2The mixed gas starts to grow the carbon nano tube, and the growth time is 15-30 mins;
and cooling the carbon nano tube to room temperature along with the furnace after the growth of the carbon nano tube is finished, and taking out the sample to obtain the porous fiber liquid absorption core with the carbon nano tube growing in situ on the surface.
2. The method for preparing the porous fiber wick with the surface in-situ grown with the carbon nanotubes according to claim 1, wherein the method comprises the following steps: and step five, cleaning, namely using deionized water and absolute ethyl alcohol in sequence, and performing ultrasonic cleaning for 10 min.
3. The method for preparing the porous fiber wick with the surface in-situ grown with the carbon nanotubes according to claim 1, wherein the method comprises the following steps: the carbon nano tubes are arranged in a disordered mode, the thickness of the carbon nano tubes is 50-100 mu m, and the surface coverage rate is larger than 90%.
4. A porous fiber wick with a surface on which carbon nanotubes are grown in situ, characterized in that it is obtained by the method of any one of claims 1 to 3.
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Cited By (1)
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| CN115654980A (en) * | 2022-10-27 | 2023-01-31 | 西安交通大学 | High-temperature heat pipe nano-structure liquid absorption core, preparation method and performance test method |
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