CN110952014A - Preparation method of low-melting-point metal-carbon nanotube-diamond composite material - Google Patents
Preparation method of low-melting-point metal-carbon nanotube-diamond composite material Download PDFInfo
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- 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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- 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
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1886—Multistep pretreatment
- C23C18/1889—Multistep pretreatment with use of metal first
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- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/52—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating using reducing agents for coating with metallic material not provided for in a single one of groups C23C18/32 - C23C18/50
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- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C2026/002—Carbon nanotubes
Abstract
A preparation method of a low-melting-point metal-carbon nanotube-diamond composite material belongs to the field of phase-change composite materials. Firstly, preparing a carboxylated carbon nanotube by treating a certain mass of carbon nanotubes with mixed acid, then sequentially carrying out sensitization and activation treatment on the carboxylated carbon nanotube, and finally carrying out indium modification on the carbon nanotube to obtain the indium-plated carbon nanotube. Mixing the prepared indium-plated carbon nano tube and diamond according to a certain proportion, carrying out ultrasonic dispersion in absolute ethyl alcohol, carrying out suction filtration, placing the mixture in a crucible, and sintering the mixture under a vacuum condition and a certain temperature to obtain the diamond particles with the surface modified with the carbon nano tube. Mixing the diamond modified by the carbon nano tube and the low-melting-point metal powder according to a certain proportion, placing the mixture in a stainless steel mold, and sintering the mixture at low pressure and low temperature under a vacuum condition to finally obtain the low-melting-point metal-carbon nano tube-diamond composite phase-change material.
Description
Technical Field
The invention relates to a preparation method of a low-melting-point phase-change material, in particular to a low-melting-point metal composite material and a preparation method thereof.
Background
As with moore's law prediction results, chips are evolving toward high levels of integration. Under the driving of a microelectronic product with high performance and high efficiency, the working temperature rise of each component is also greatly improved. The heat is difficult to diffuse out effectively, which causes the stability, reliability and durability of the electronic components to be seriously reduced, and greatly reduces the service life of the electronic components. Therefore, in the field of thermal management of electronic products, how to improve the heat dissipation efficiency is a key technology. Traditional air cooling cannot meet the requirements, particularly in the field of narrow spaces. The heat sink mainly has an active type and a passive type. The passive radiator has unique use advantages under certain conditions due to stable performance. Passive heat sinks often use phase change materials as the medium. Common phase change materials include organic phase change materials and inorganic phase change materials, and the organic phase change materials belong to solid paraffin and are most widely applied. However, the thermal conductivity of paraffin wax is only-0.2W m-1K-1This is a disadvantage of organic phase change materials, while the volume phase change latent heat of organic phase change materials is small. Recently, researchers have conducted a great deal of research into the heat dissipation properties of low melting point metal phase change materials. Compared with the organic phase change material, the thermal conductivity and the volume phase change latent heat of the metal phase change material are dozens to hundreds of times of those of the organic phase change material, and the metal phase change material has huge potential in the field of thermal management.
Meanwhile, composite materials mainly composed of low-melting-point metals or alloys have also been extensively studied, and it has been found that the composite materials exhibit good characteristics. With the research trend, the invention develops a novel preparation method of the low-melting-point metal composite material.
Disclosure of Invention
The present invention aims to modify the surface of a carbon nanotube and then compound the carbon nanotube with a low-melting metal and diamond. Firstly, modifying carbon nano tubes by a chemical modification method, modifying the carbon nano tubes on the surfaces of diamonds by a sintering method, then mixing prepared low-melting-point metal micro powder and modified diamond particles according to a certain proportion, and sintering the low-melting-point metal composite material by a micro-pressure liquid phase method, thereby developing a novel low-melting-point metal-carbon nano tube-diamond phase-change composite material, further improving the heat conductivity of the low-melting-point phase-change metal and enabling the low-melting-point phase-change metal to play a role in a heat management system.
The technical scheme of the invention is as follows:
(1) carrying out mixed acid treatment on the original carbon nano tube to obtain a carboxylated carbon nano tube; the mixed acid is concentrated nitric acid: concentrated sulfuric acid is 1:3, the temperature is 50-80 ℃, and the time is 1-3 h;
(2) weighing 0.01-0.08g of carboxylated multi-walled carbon nanotube and 0.1-0.4g of PVP, and placing in 40-200ml of deionized water for ultrasonic dispersion;
(3) weighing 0.5-2g of stannous chloride, putting the stannous chloride into a beaker, dissolving the stannous chloride with a certain amount of hydrochloric acid, slowly pouring the solution dispersed in the step (2) into the beaker, and performing ultrasonic dispersion on the solution for 30-60 min;
(4) carrying out centrifugal separation on the sensitized multi-walled carbon nano-tubes, repeatedly washing with deionized water, and carrying out centrifugal drying;
(5) weighing 0.02-0.2g of palladium chloride, placing the palladium chloride in a beaker, dissolving the palladium chloride by using a proper amount of hydrochloric acid, placing the sensitized multi-wall carbon nano tube and the dissolved palladium chloride in 40-200ml of deionized water, and carrying out ultrasonic treatment for 30-60 min;
(6) repeatedly cleaning the multi-walled carbon nano-tubes after the activation treatment by using deionized water, and centrifugally drying;
(7) dissolving a certain amount of indium nitrate (0.1-0.5g) in 40-200ml of deionized water, adding the multi-walled carbon nano-tube obtained in the step (6) into the deionized water, ultrasonically dispersing for 5-10min, and then placing the mixture in an oil bath pot for heat preservation (40-80 ℃);
(8) 2-8g of sodium hypophosphite is dissolved in 40-200g of deionized water, and slowly dropped into the solution in the step (7) for reaction for 0.5-3 h;
(9) dissolving the carbon nano tube obtained in the step (8), performing centrifugal dispersion, repeatedly cleaning the carbon nano tube by using deionized water, and performing centrifugal drying;
(10) placing the indium-plated carbon nano tube and the diamond in a certain ratio (5:0.1-5:0.5) in absolute ethyl alcohol for ultrasonic dispersion for 5-10min, performing suction filtration, drying, and modifying the surface carbon nano tube of the diamond at a certain temperature (180-;
(11) uniformly mixing the low-melting-point metal powder and the diamond modified by the carbon nano tube according to a certain proportion (4.9:5.1-4.5: 5.5);
(12) and (3) putting the powder mixed in the step (11) into a stainless steel mold, pressing into a tablet, putting the prefabricated tablet into a mold with a certain size, sealing the prefabricated tablet by using high-temperature silicone adhesive, after the prefabricated tablet is cured, pressurizing the prefabricated tablet by using the pressure of 0.2-2MPa, putting the prefabricated tablet into a tubular furnace, sintering the prefabricated tablet at the temperature of 80-200 ℃ for 5-60min, and then cooling the sintered tablet to room temperature in air.
The invention has the advantages that: 1) developing a preparation process of multi-walled carbon nanotube surface modified indium; 2) preparing carbon nano tube-diamond particles by adopting a sintering mode; 3) preparing the low-melting-point metal-carbon nano tube-diamond composite material.
Drawings
Fig. 1 is a schematic diagram of the low-melting-point metal-carbon nanotube-diamond composite preparation in embodiment 1 of the present invention.
FIG. 2 is an SEM of an indium-plated carbon nanotube obtained in example 1 of the present invention.
Fig. 3 is an SEM of carbon nanotube-modified diamond obtained in example 1 of the present invention.
FIG. 4 is an SEM of the diamond particles connected by carbon nanotubes obtained in example 1 of the present invention.
Detailed Description
The technical solution of the present invention is further explained below with reference to specific embodiments.
Example 1
(1) Preparing indium-plated carbon nanotubes:
sensitization: placing 0.02g of carboxylated carbon nanotube and 0.2g of PVP in 40mL of deionized water, and ultrasonically dispersing for 5 min; 0.5g SnCl was weighed2Placing in a beaker, dissolving with 1ml HCl, slowly adding the dispersed carbon nanotube solution, performing ultrasonic treatment for 30min, cleaning, centrifuging, and drying; and (3) activation: 0.04g of PdCl was dissolved in 0.2mL of HCl2Adding the sensitized carbon nano tube and 40mL of deionized water into the solution, carrying out ultrasonic treatment for 30min, cleaning, centrifuging and drying; indium plating: will be 0.2g, dissolving In (NO3)3 In deionized water, adding the activated carbon nano tube, placing the carbon nano tube In an oil bath pot, and preserving the temperature at 70 ℃; 5g of sodium hypophosphite is dissolved in 50mL of deionized water, slowly added into a carbon nano indium nitrate solution for reaction for 2 hours, and then washed, centrifuged and dried.
(2) Modifying the carbon nano tube on the surface of the diamond:
putting diamond and indium-plated carbon nano tube into 40mL alcohol according to the ratio of 5:0.1, performing ultrasonic dispersion for 10min, performing suction filtration, drying, putting into a crucible, and preserving heat at 200 ℃ for 30min under a vacuum condition.
(3) Preparing a low-melting-point metal-carbon nanotube-diamond composite material:
uniformly mixing the metal micro powder of the field and the carbon nano tube modified diamond according to the ratio of 4.9:5.1, placing the mixture in a stainless steel mold, setting the sintering temperature to be 120 ℃, the sintering pressure to be 530KPa and the sintering time to be 30min, and then cooling to room temperature.
Example 2
(1) Preparing indium-plated carbon nanotubes:
sensitization: placing 0.04g of carboxylated carbon nanotube and 0.4g of PVP in 100mL of deionized water, and ultrasonically dispersing for 10 min; 0.9g of SnCl is weighed out2Placing in a beaker, dissolving with 1.5ml HCl, slowly adding the dispersed carbon nanotube solution, performing ultrasonic treatment for 60min, cleaning, centrifuging, and drying; and (3) activation: 0.04g of PdCl was dissolved in 0.2mL of HCl2Adding the sensitized carbon nano tube and 100mL of deionized water into the solution, carrying out ultrasonic treatment for 60min, cleaning, centrifuging and drying; indium plating: dissolving 0.1g of In (NO3)3 In deionized water, adding the activated carbon nano tube, placing the carbon nano tube In an oil bath pot, and preserving the temperature at 60 ℃; dissolving 3g of sodium hypophosphite in 50mL of deionized water, slowly adding the sodium hypophosphite into the carbon nano indium nitrate solution, reacting for 2h, washing, centrifuging and drying.
(2) Modifying the carbon nano tube on the surface of the diamond:
putting diamond and indium-plated carbon nano tube into 40mL alcohol according to the ratio of 5:0.2, performing ultrasonic dispersion for 30min, performing suction filtration, drying, putting into a crucible, and preserving heat at 180 ℃ for 60min under a vacuum condition.
(3) Preparing a low-melting-point metal-carbon nanotube-diamond composite material:
uniformly mixing the metal micro powder of the field and the carbon nano tube modified diamond according to the ratio of 4.8:5.2, placing the mixture in a stainless steel mold, setting the sintering temperature to be 150 ℃, the sintering pressure to be 530KPa and the sintering time to be 15min, and then cooling to room temperature.
Embodiment 3
(1) Preparing indium-plated carbon nanotubes:
sensitization: placing 0.03g of carboxylated carbon nanotube and 0.2g of PVP in 60mL of deionized water, and ultrasonically dispersing for 5 min; 0.7g of SnCl is weighed out2Placing in a beaker, dissolving with 1ml HCl, slowly adding the dispersed carbon nanotube solution, performing ultrasonic treatment for 50min, cleaning, centrifuging, and drying; and (3) activation: 0.02g of PdCl was dissolved in 0.1mL of HCl2Adding the sensitized carbon nano tube and 50mL of deionized water into the solution, performing ultrasonic treatment for 50min, cleaning, centrifuging and drying; indium plating: dissolving 0.1g of In (NO3)3 In deionized water, adding the activated carbon nano tube, placing the carbon nano tube In an oil bath pot, and preserving the temperature at 50 ℃; dissolving 4g of sodium hypophosphite in 60mL of deionized water, slowly adding the sodium hypophosphite into the carbon nano indium nitrate solution, reacting for 1h, washing, centrifuging and drying.
(2) Modifying the carbon nano tube on the surface of the diamond:
putting diamond and indium-plated carbon nano tube into 40mL alcohol according to the ratio of 5:0.3, performing ultrasonic dispersion for 30min, performing suction filtration, drying, putting into a crucible, and preserving heat at 210 ℃ for 20min under a vacuum condition.
(3) Preparing a low-melting-point metal-carbon nanotube-diamond composite material:
uniformly mixing the metal micro powder of the field and the carbon nano tube modified diamond according to the ratio of 4.7:5.3, placing the mixture in a stainless steel mold, setting the sintering temperature to be 90 ℃, the sintering pressure to be 640KPa and the sintering time to be 30min, and then cooling to room temperature.
Example 4
(1) Preparing indium-plated carbon nanotubes:
sensitization: placing 0.02g of carboxylated carbon nanotube and 0.1g of PVP in 40mL of deionized water, and ultrasonically dispersing for 15 min; 0.4g SnCl is weighed2Placing in a beaker, dissolving with 1ml HCl, slowly adding the dispersed carbon nanotube solution, performing ultrasonic treatment for 30min,cleaning, centrifuging and drying; and (3) activation: 0.02g of PdCl was dissolved in 0.1mL of HCl2Adding the sensitized carbon nano tube and 40mL of deionized water into the solution, carrying out ultrasonic treatment for 30min, cleaning, centrifuging and drying; indium plating: dissolving 0.1g of In (NO3)3 In deionized water, adding the activated carbon nano tube, placing the carbon nano tube In an oil bath pot, and preserving the temperature at 70 ℃; dissolving 2g of sodium hypophosphite in 50mL of deionized water, slowly adding the sodium hypophosphite into the carbon nano indium nitrate solution, reacting for 2h, washing, centrifuging and drying.
(2) Modifying the carbon nano tube on the surface of the diamond:
putting diamond and indium-plated carbon nano tube into 40mL alcohol according to the ratio of 5:0.1, performing ultrasonic dispersion for 30min, performing suction filtration, drying, putting into a crucible, and preserving heat at 190 ℃ for 20min under a vacuum condition.
(3) Preparing a low-melting-point metal-carbon nanotube-diamond composite material:
uniformly mixing the metal micro powder of the field and the carbon nano tube modified diamond according to the ratio of 4.9:5.1, placing the mixture in a stainless steel mold, setting the sintering temperature to be 120 ℃, the sintering pressure to be 530KPa and the sintering time to be 30min, and then cooling to room temperature.
Claims (7)
1. The carbon nano tube modification is characterized by comprising the following preparation steps:
firstly, mixing sensitizing solution, dispersing agent and carbon nano tube according to a certain proportion, then carrying out ultrasonic dispersion for a certain time, centrifuging, cleaning and then drying; mixing the activating solution, the dispersing agent and the sensitized carbon nano tube according to a certain proportion, then ultrasonically dispersing for a certain time, centrifuging, cleaning and drying; mixing the activated carbon nano tube with indium plating solution, then carrying out indium plating treatment on the surface of the carbon nano tube at a certain temperature and for a certain time, centrifuging, cleaning and drying to obtain the indium-plated carbon nano tube.
2. Modifying the surface of the diamond with carbon nanotubes, and the preparation steps are as follows:
mixing diamond and indium-plated carbon nano tubes according to a certain proportion, placing the mixture into absolute ethyl alcohol for ultrasonic dispersion, then carrying out suction filtration on the mixture, drying the mixture, placing the dried mixture into a crucible, carrying out heat preservation on the mixture for a certain time at a certain temperature under a vacuum condition, and then cooling the mixture along with a furnace to obtain the diamond particles modified by the carbon nano tubes.
3. The preparation method of the low-melting-point metal-carbon nanotube-diamond composite material comprises the following preparation steps:
the composite material is prepared by adopting a low-temperature low-pressure sintering mode, the low-melting-point metal powder and the diamond modified by the carbon nano tube are uniformly mixed according to a certain proportion, then the mixture is placed in a stainless steel mold, and the low-melting-point metal-carbon nano tube-diamond composite material is prepared under the vacuum condition and under certain temperature, pressure and time.
4. The carbon nanotube modification of claim 1, wherein the carbon nanotubes are multi-walled carbon nanotubes having a length of 10-50 μm, and the indium plating solution comprises indium nitrate and sodium hypophosphite.
5. The diamond surface modified carbon nanotube as claimed in claim 2, wherein the diamond grains have a size of 45-400 μm, the diamond content in the composite material is 10-50%, the carbon nanotube content is 1-5%, the sintering temperature is 180-220 ℃, and the sintering time is 10-60 min.
6. The method for preparing a low melting point metal-carbon nanotube-diamond composite according to claim 3, wherein the sintering temperature is 80-200 ℃ and the sintering time is 5-60 minutes.
7. The low melting point metal according to claim 3, wherein the base material is mainly an indium-based low melting point metal having a melting point of 57 to 80 ℃.
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