WO2021056851A1 - 一种MXene/金属复合气凝胶、其制备方法、用途及包含其的热界面材料 - Google Patents
一种MXene/金属复合气凝胶、其制备方法、用途及包含其的热界面材料 Download PDFInfo
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
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- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/048—Elimination of a frozen liquid phase
- C08J2201/0484—Elimination of a frozen liquid phase the liquid phase being aqueous
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- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08K3/10—Metal compounds
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Definitions
- This application belongs to the technical field of thermally conductive materials, and specifically relates to a MXene/metal composite aerogel, its preparation method, application and thermal interface material containing the same.
- Thermal interface material is a general term for a class of materials that are used to reduce the contact thermal resistance between the heat dissipating device and the heating device.
- the thermal conductivity of air is very small, which will cause a large contact thermal resistance between the interfaces.
- the use of thermal interface materials can fill this gap well and improve heat dissipation. performance.
- Thermal interface materials are widely used in thermal interface materials due to their good flexibility, low cost and good processability.
- the intrinsic thermal conductivity of polymers is generally too low, and it is difficult to achieve effective heat transfer effects when used alone in practical applications. For this reason, it is usually necessary to add thermally conductive fillers (for example, ceramics, metals, and carbon materials) to the polymer.
- MXene is a two-dimensional material with an accordion-like morphology.
- the composition is a carbide or nitride of a transition metal. It is mainly prepared by etching MAX (such as Ti 3 AlC 2 ), where "M” represents a transition metal element, and "A” Represents an element of the third or fourth main group, and "X" represents carbon or nitrogen.
- MAX such as Ti 3 AlC 2
- the ice template method to prepare aerogels is a very effective way.
- the principle of the ice template method is that the solvent water in the aqueous solution crystallizes into ice during the freezing process.
- the two-dimensional flake filler dispersed in it also forms an orderly network structure with the growth of ice crystals. This frozen structure is It is sublimated and dried in a vacuum to remove ice crystals to obtain a two-dimensional aerogel.
- Li Yecan et al. used silver nanoparticles and graphene oxide as raw materials to prepare a three-dimensional graphene/silver nanoparticle aerogel by the ice template method, and studied its electrical conductivity ("Three-dimensional graphene/silver nanoparticle aerogel” The construction of glue", Li Yecan et al., Journal of Qingdao University of Science and Technology, Volume 39 Supplement 1). Based on the structure of the three-dimensional graphene/silver nanoparticle aerogel, it is speculated that it may have a certain thermal conductivity, but the silver nanoparticles in this aerogel are only adsorbed on the surface of the graphene, and its thermal conductivity is limited.
- the purpose of this application is to provide a MXene/metal composite aerogel, its preparation method, application and thermal interface material containing the same.
- the MXene/metal composite aerogel has good thermal conductivity, structural stability and thermal conductivity, and can be used as a thermally conductive filler. Compared with thermally conductive fillers such as graphene, it has a wider range of application to polymer substrates.
- the present application provides an MXene/metal composite aerogel, including an MXene framework and a metal, and the MXene framework is cross-linked into a network structure through the metal.
- MXene two-dimensional materials have excellent intra-layer thermal conductivity, but because the layers are separated from each other, the overall thermal conductivity is limited.
- This application uses metal to "weld" the MXene sheets to improve the heat transfer efficiency between the MXene sheets, so that the MXene/metal composite aerogel forms a complete heat conduction path, so the obtained MXene/metal composite Aerogel has high thermal conductivity, can be used as a thermally conductive filler, and the required amount of addition is low; moreover, because the metal network has a supporting effect on the MXene framework, the obtained MXene/metal composite aerogel has good properties
- the structural stability and thermal conductivity of MXene are stable; in addition, compared with two-dimensional materials such as graphene, the compatibility between MXene and organic polymer materials is better. Therefore, when the MXene/metal composite aerogel provided in this application is used as a filler , It has a wider application range for polymer substrates and stronger
- the metal is selected from one or a combination of at least two of silver, iron, nickel, or copper, and more preferably silver.
- silver is the best thermal conductor, and its nanoparticles can be melted at about 200°C, and the "welding" temperature is relatively low. Therefore, in this application, the metal in the MXene/metal composite aerogel can be selected as silver.
- the mass percentage of the metal in the MXene/metal composite aerogel is 0.5%-10%; for example, it can be 0.5%, 0.6%, 0.8%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, 9.5% or 10% Wait.
- the crosslinking degree of the MXene/metal composite aerogel will be lower, and the thermal conductivity will decrease; if the metal content is too high, the mechanical properties of the aerogel will be Will fall.
- the apparent density of the MXene/metal composite aerogel is 0.9-3 kg/m 3 ; for example, it may be 0.9 kg/m 3 , 1 kg/m 3 , 1.2 kg/m 3 , 1.5 kg/m 3 , 1.8kg/m 3 , 2kg/m 3 , 2.2kg/m 3 , 2.5kg/m 3 , 2.8kg/m 3 or 3kg/m 3, etc.
- this application provides a method for preparing the above-mentioned MXene/metal composite aerogel, which includes the following steps:
- step (2) freeze-dry the dispersion obtained in step (1) to obtain MXene/metal nanoparticle composite aerogel
- step (3) Anneal the MXene/metal nanoparticle composite aerogel obtained in step (2) to melt the metal nanoparticles in the MXene/metal nanoparticle composite aerogel. After the annealing is completed, the MXene/metal composite aerogel.
- This application uses the suspended bonds of titanium and oxygen contained on the surface of MXene to reduce the metal ions into metal nanoparticles in situ, and then uses the ice template method to grow the MXene/metal nanoparticle composite material to form an ordered network structure (water is in the freezing process). Crystallize into ice, and the dispersed MXene/metal nanoparticle composite material also forms an ordered structure with the growth of ice crystals). After freeze-drying, this network structure is temporarily fixed to form MXene/metal nanoparticle composite gas.
- the melting temperature at this size is much lower than the melting point of the metal, so in step (3), the MXene is treated by annealing.
- the metal nanoparticles on the flakes are heated and melted, so that the MXene flakes are "welded" to form an MXene/metal composite aerogel.
- the metal layer in MAX is etched away with a mixed solution of hydrochloric acid and lithium chloride to form accordion-like MXene.
- the etched sample is collected by washing and centrifugation, and then the obtained sample is dispersed in deionized water and mechanically shaken for 5 minutes.
- the sample is peeled off into thin slices, centrifuged at 3500 rpm for 30 minutes, and the supernatant is collected, which is the MXene dispersion;
- the MAX powder in a hydrofluoric acid solution for etching, wash the etched sample and collect it by centrifugation, and then disperse it in a solution of cetyltrimethylammonium bromide and shake it mechanically for 5 minutes to make the sample Peel into thin slices, centrifuge at 3500 rpm for 30 minutes, and collect the supernatant, which is the MXene dispersion.
- the temperature of the reaction in the step (1) is -5 to 80°C, for example, -5°C, -2°C, 0°C, 2°C, 5°C, 8°C , 10°C, 15°C, 20°C, 23°C, 25°C, 30°C, 35°C, 40°C, 45°C, 50°C, 55°C, 60°C, 65°C, 70°C, 75°C or 80°C etc.
- the temperature of the reaction in step (1) is more preferably -5-50°C.
- the reaction time in step (1) is 10-30 min; for example, it can be 10 min, 12 min, 15 min, 18 min, 20 min, 22 min, 25 min, 28 min, or 30 min.
- reaction in step (1) is carried out under ultrasonic oscillation conditions.
- the annealing temperature in step (3) is 150-500°C, for example 150°C, 160°C, 170°C, 180°C, 190°C, 200°C, 210°C, 220°C, 250°C, 280°C, 300°C, 320°C, 350°C, 380°C, 400°C, 420°C, 45°C, 480°C or 500°C, etc.; time is 0.5-3h, such as 0.5h, 0.8h, 1h, 1.2h , 1.5h, 1.8h, 2h, 2.2h, 2.5h, 2.8h or 3h etc.
- the annealing temperature is 150-300°C;
- the annealing temperature is 300-500°C;
- the annealing temperature is 200-350°C;
- the annealing temperature is 250-400°C.
- the annealing in step (3) is performed in a protective atmosphere.
- the protective atmosphere is an argon atmosphere.
- the preparation method further includes: before the freeze-drying in step (2), mixing the dispersion obtained in step (1) with polyvinyl alcohol.
- step (2) is: mixing the dispersion obtained in step (1) with polyvinyl alcohol, and then freeze-drying to obtain MXene/metal nanoparticle composite aerogel.
- polyvinyl alcohol may not be added in step (2), but the obtained MXene/metal nanoparticle composite aerogel has an unstable structure and is easy to collapse; adding polyvinyl alcohol can play a role in connecting the MXene skeleton and improve Stability of MXene/metal nanoparticle composite aerogel.
- the added polyvinyl alcohol will be thermally decomposed and removed during the annealing process in step (3).
- the preparation method includes the following steps:
- step (2) Mix the dispersion obtained in step (1) with the polyvinyl alcohol solution, add it to a mold, place it on a copper column immersed in liquid nitrogen for freezing, and then place it in a freeze dryer for drying to obtain MXene/ Metal nanoparticle composite aerogel;
- the MXene/metal nanoparticle composite aerogel obtained in step (2) is annealed at 150-500°C for 0.5-3h to make the metal in the MXene/metal nanoparticle composite aerogel The nanoparticles are melted, and after the annealing is completed, the MXene/metal composite aerogel is obtained.
- this application provides a use of the MXene/metal composite aerogel described in the first aspect, where the MXene/metal composite aerogel is used as a thermally conductive filler.
- the present application provides a thermal interface material.
- the thermal interface material includes a polymer substrate and the MXene/metal composite aerogel described in the first aspect of the application.
- the volume percentage of MXene/metal composite aerogel in the thermal interface material is 3-40%; for example, it can be 3%, 3.5%, 4%, 4.5%, 5% , 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, 9.5%, 10%, 12%, 15%, 18%, 20%, 22%, 25%, 28 %, 30%, 32%, 35%, 38% or 40% etc. More optional is 10-15%.
- the polymer substrates can be selected from epoxy resins, polyimides, and polyesters.
- the MXene/metal composite aerogel can be immersed in the precursor solution of the polymer substrate, cured after deaeration, and polished into a thin sheet of the desired thickness. , To obtain a thermal interface material; or dissolve the polymer substrate in a solvent, infiltrate the MXene/metal composite aerogel, then dry to remove the solvent, and polish into a thin sheet of the desired thickness to obtain the thermal interface material.
- This application uses the suspended bonds contained on the surface of MXene to reduce metal ions into metal nanoparticles in situ, and uses the ice template method to grow MXene/metal nanoparticle composites to form an orderly network structure.
- the melting temperature of metal nanoparticles is lower.
- the properties of MXene sheets are "welded" at low temperatures to obtain a MXene/metal composite aerogel with a metal cross-linked MXene network structure inside.
- the resulting MXene/metal composite aerogel has high thermal conductivity;
- the supporting effect of the metal network, the structure and thermal conductivity of the MXene/metal composite aerogel provided in this application are stable.
- the MXene/metal composite aerogel provided in this application can be used as a thermally conductive filler. Compared with thermally conductive fillers such as graphene, it has better compatibility with organic polymer materials, and has a wider application range for polymer substrates. Less addition is required for the same thermal conductivity, and the thermal conductivity of the thermal interface material prepared therefrom can be as high as 2.8W m -1 K -1 .
- Figure 1 is a low-resolution transmission electron micrograph of the MXene/silver composite aerogel provided in Example 1 of the application;
- Figure 2 is a high-resolution transmission electron micrograph of the MXene/silver composite aerogel provided in Example 1 of the application;
- Fig. 3 is a scanning electron micrograph of the thermal interface material provided in Application Example 1 of this application.
- This embodiment provides an MXene/silver composite aerogel, which includes an MXene skeleton and silver, and the MXene skeleton is cross-linked by silver to form a network structure.
- the specific preparation method is as follows:
- step (2) Take 200 mL of the MXene dispersion obtained in step (1), drop in 1 mL of silver nitrate solution with a concentration of 0.5 mol/L, and after fully stirring, the mixture is ultrasonically shaken in an ice bath for 30 minutes to reduce the silver ions Form silver nanoparticles, centrifuge, and remove the supernatant to obtain a high-concentration dispersion of MXene/silver nanoparticle composite materials;
- step (3) Take 16 mg of the dispersion obtained in step (2) and disperse it in 4 mL of 30 mg/mL polyvinyl alcohol aqueous solution, and pour it into a square polytetrafluoroethylene mold (the mold runs through the top and bottom, and the lower surface is made of aluminum Tape sealing), then place it on the surface of a copper column immersed in liquid nitrogen for freezing, and use a freeze dryer for drying to obtain MXene/silver nanoparticle composite aerogel;
- step (3) The MXene/silver nanoparticle composite aerogel obtained in step (3) is annealed in an argon atmosphere at 250°C for 2 hours to melt the silver nanoparticles, weld the MXene sheet, and cool down to obtain the MXene/silver composite gas Gel (with XPS test, the silver content is 0.5wt%).
- FIGs. 1 and 2 are transmission electron micrographs of MXene/silver nanoparticle composites at low resolution and high resolution, respectively. From Figure 1, we can observe the Ag particles deposited on the surface of MXene. The diameter of these particles is about 20-50nm; from Figure 2, the lattice spacing of silver (the black circular area in the center of Figure 2) is 0.235nm, MXene ( The lattice spacing of the area except silver in Figure 2 is 0.215nm, which matches the JCPDS card. The results prove that Ag NPs are successfully modified on the surface of MXene.
- This embodiment provides an MXene/silver composite aerogel, which includes an MXene skeleton and silver, and the MXene skeleton is cross-linked by silver to form a network structure.
- the specific preparation method is as follows:
- step (2) Take 200 mL of the MXene dispersion obtained in step (1), drop 1 mL of silver nitrate solution with a concentration of 1 mol/L, and after fully stirring, the mixture is ultrasonically shaken in an ice bath for 30 minutes to reduce the silver ions to Centrifuge the silver nanoparticles to remove the supernatant to obtain a high-concentration dispersion of MXene/silver nanoparticle composites;
- step (3) Take 16 mg of the dispersion obtained in step (2) and disperse it in 4 mL of 30 mg/mL polyvinyl alcohol aqueous solution, and pour it into a square polytetrafluoroethylene mold (the mold runs through the top and bottom, and the lower surface is made of aluminum Tape sealing), then place it on the surface of a copper column immersed in liquid nitrogen for freezing, and use a freeze dryer for drying to obtain MXene/silver nanoparticle composite aerogel;
- step (3) The MXene/silver nanoparticle composite aerogel obtained in step (3) is annealed in an argon atmosphere at 150°C for 3 hours to melt the silver nanoparticles, weld the MXene sheet, and cool down to obtain the MXene/silver composite gas Gel (using XPS test to obtain a silver content of 0.8 wt%).
- This embodiment provides an MXene/silver composite aerogel, which includes an MXene skeleton and silver, and the MXene skeleton is cross-linked by silver to form a network structure.
- the specific preparation method is as follows:
- step (2) Take 200 mL of the MXene dispersion obtained in step (1), and drop 1 mL of silver nitrate solution with a concentration of 2 mol/L. After fully stirring, the mixture is ultrasonically shaken in an ice bath for 30 minutes to reduce the silver ions to Centrifuge the silver nanoparticles to remove the supernatant to obtain a high-concentration dispersion of MXene/silver nanoparticle composites;
- step (3) Take 16 mg of the dispersion obtained in step (2) and disperse it in 4 mL of 30 mg/mL polyvinyl alcohol aqueous solution, and pour it into a square polytetrafluoroethylene mold (the mold runs through the top and bottom, and the lower surface is made of aluminum Tape sealing), then place it on the surface of a copper column immersed in liquid nitrogen for freezing, and use a freeze dryer for drying to obtain MXene/silver nanoparticle composite aerogel;
- step (3) The MXene/silver nanoparticle composite aerogel obtained in step (3) was annealed in an argon atmosphere at 200°C for 2.5 hours to melt the silver nanoparticles and weld the MXene sheet layer, and after cooling to obtain the MXene/silver composite gas Gel (using XPS test to obtain a silver content of 1.6 wt%).
- This embodiment provides an MXene/silver composite aerogel, which includes an MXene skeleton and silver, and the MXene skeleton is cross-linked by silver to form a network structure.
- the specific preparation method is as follows:
- step (2) Take 200 mL of the MXene dispersion obtained in step (1), and drop 1 mL of silver nitrate solution with a concentration of 4 mol/L. After fully stirring, the mixture is ultrasonically shaken in an ice bath for 30 minutes to reduce the silver ions to Centrifuge the silver nanoparticles to remove the supernatant to obtain a high-concentration dispersion of MXene/silver nanoparticle composites;
- step (3) Take 16 mg of the dispersion obtained in step (2) and disperse it in 4 mL of 30 mg/mL polyvinyl alcohol aqueous solution, and pour it into a square polytetrafluoroethylene mold (the mold runs through the top and bottom, and the lower surface is made of aluminum Tape sealing), then place it on the surface of a copper column immersed in liquid nitrogen for freezing, and use a freeze dryer for drying to obtain MXene/silver nanoparticle composite aerogel;
- step (3) The MXene/silver nanoparticle composite aerogel obtained in step (3) is annealed in an argon atmosphere at 250°C for 2 hours to melt the silver nanoparticles, weld the MXene sheet, and cool down to obtain the MXene/silver composite gas Gel (using XPS test to get a silver content of 2.4 wt%).
- This embodiment provides an MXene/silver composite aerogel, which includes an MXene skeleton and silver, and the MXene skeleton is cross-linked by silver to form a network structure.
- the specific preparation method is as follows:
- step (2) Take 200 mL of the MXene dispersion obtained in step (1), and drop 1 mL of silver nitrate solution with a concentration of 8 mol/L. After fully stirring, the mixture is ultrasonically shaken in an ice bath for 30 minutes to reduce the silver ions to Centrifuge the silver nanoparticles to remove the supernatant to obtain a high-concentration dispersion of MXene/silver nanoparticle composites;
- step (3) Take 16 mg of the dispersion obtained in step (2) and disperse it in 4 mL of 30 mg/mL polyvinyl alcohol aqueous solution, and pour it into a square polytetrafluoroethylene mold (the mold runs through the top and bottom, and the lower surface is made of aluminum Tape sealing), then place it on the surface of a copper column immersed in liquid nitrogen for freezing, and use a freeze dryer for drying to obtain MXene/silver nanoparticle composite aerogel;
- step (3) The MXene/silver nanoparticle composite aerogel obtained in step (3) is annealed in an argon atmosphere at 300°C for 1 hour to melt the silver nanoparticles and weld the MXene sheets. After cooling, the MXene/silver composite gas is obtained Gel (using XPS test to obtain a silver content of 3.2 wt%).
- This embodiment provides a MXene/iron composite aerogel, including MXene framework and iron, the MXene framework is cross-linked by iron into a network structure; the specific preparation method differs from that in Example 1 in that the nitric acid in step (2) The silver is replaced with the same molar amount of ferrous chloride, and the annealing temperature in step (4) is 400° C. and the time is 2 h.
- This embodiment provides a MXene/nickel composite aerogel, which includes a MXene skeleton and nickel.
- the MXene skeleton is cross-linked by nickel to form a network structure; the specific preparation method differs from that in Example 1 in that the nitric acid in step (2)
- the silver is replaced with the same molar amount of nickel nitrate, the annealing temperature in step (4) is 250° C., and the time is 2 h.
- This embodiment provides an MXene/copper composite aerogel, which includes an MXene framework and copper.
- the MXene framework is cross-linked by copper to form a network structure; the specific preparation method differs from that in Example 1 in that the nitric acid in step (2) The silver is replaced with copper sulfate of the same molar amount, and the annealing temperature in step (4) is 350° C. and the time is 2 h.
- Example 1 The difference from Example 1 is that steps (2) and (4) are not performed, and the MXene dispersion obtained in step (1) is directly mixed with an aqueous polyvinyl alcohol solution, and step (3) is performed to obtain MXene aerogel.
- the apparent density and thermal conductivity of the MXene/metal composite aerogel provided in Examples 1-8 and the MXene aerogel provided in Comparative Example 1 were tested.
- the test methods are as follows:
- Example 1 Example 2
- Example 3 Example 4
- Example 5 Metal content (wt%) 0.5 0.8 1.6 2.4 3.2 Apparent density (g/m 3 ) 1.1 1.2 1.5 1.6 1.8
- Test items Example 6
- Example 7 Example 8 Comparative example 1 To Metal content (wt%) 0.3 0.32 0.36 0 To Apparent density (g/m 3 ) 0.92 0.94 0.98 0.9
- To Metal content (wt%) 0.3 0.32 0.36 0
- Apparent density (g/m 3 ) 0.92 0.94 0.98 0.9
- the preparation method is as follows: hexahydrophthalic anhydride (curing agent), epoxy resin (E-54) and N,N-dimethylbenzylamine (catalyst) at 10:10: The mass ratio of 1 is mixed to form an epoxy resin matrix, the MXene/silver composite aerogel provided in Example 1 is poured, and then placed in a vacuum oven at 40°C for 3 hours to remove all bubbles, and then placed in the oven. It was cured at 120°C for 1 hour, then at 160°C for 2 hours, and finally at 200°C for 2 hours. After natural cooling, it was polished to obtain a thermal interface material (MXene/silver composite aerogel content 12vol%).
- the morphology of the thermal interface material provided in Application Example 1 was characterized by using a scanning electron microscope, and the result is shown in FIG. 3. It can be seen from Figure 3 that the epoxy resin adheres well to the MXene/Ag composite aerogel skeleton, and there is no obvious interface peeling and blistering in the thermal interface material. In addition, the 3D framework structure of the MXene/Ag composite aerogel is well maintained, which is conducive to effective heat transfer.
- a thermal interface material is provided.
- the preparation method is as follows: Stir polyethylene terephthalate uniformly at 80°C, pour the MXene/silver composite aerogel provided in Example 1, and then cure it in an oven at 100°C for 6 hours , And polished after curing to obtain a thermal interface material (MXene/silver composite aerogel content 12vol%).
- a thermal interface material is provided.
- the preparation method is as follows: dissolve methyl methacrylate in azobisisobutyronitrile, heat and stir uniformly in a water bath, and pour the slurry into the MXene/silver composite aerogel provided in Example 1. It was placed in an oven at 40°C for low-temperature polymerization for 10 hours, then cured at 100°C for 1.5 hours, and slowly cooled to room temperature to obtain a thermal interface material (MXene/silver composite aerogel content 12vol%).
- a thermal interface material is provided separately.
- the difference between the preparation method and application example 1 is that the MXene/silver composite aerogel provided in Example 1 is replaced by the MXene/metal composite aerogel provided in Examples 2-8. And the content of MXene/metal composite aerogel is different (the specific content is shown in Table 2).
- a thermal interface material is provided.
- the difference between the preparation method and Application Example 1 is that the MXene/silver composite aerogel provided in Example 1 is replaced with the MXene aerogel provided in Comparative Example 1.
- the thermal interface material prepared by the MXene/metal composite aerogel provided by this application has higher thermal conductivity at the same addition amount, indicating that the metal has a higher thermal conductivity.
- the cross-linked structure reduces the interface contact thermal resistance between the MXene sheets.
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Abstract
Description
测试项目 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 |
金属含量(wt%) | 0.5 | 0.8 | 1.6 | 2.4 | 3.2 |
表观密度(g/m 3) | 1.1 | 1.2 | 1.5 | 1.6 | 1.8 |
测试项目 | 实施例6 | 实施例7 | 实施例8 | 对比例1 | |
金属含量(wt%) | 0.3 | 0.32 | 0.36 | 0 | |
表观密度(g/m 3) | 0.92 | 0.94 | 0.98 | 0.9 |
Claims (11)
- 一种MXene/金属复合气凝胶,其中,所述MXene/金属复合气凝胶包括MXene骨架和金属,所述MXene骨架通过所述金属交联成网络结构。
- 根据权利要求1所述的MXene/金属复合气凝胶,其中,所述金属占所述MXene/金属复合气凝胶的质量百分比为0.5%-10%,可选为1-3.2%。
- 根据权利要求1或2所述的MXene/金属复合气凝胶,其中,所述MXene/金属复合气凝胶的表观密度为0.9-3kg/m 3;可选地,所述金属选自银、铁、镍或铜中的一种或至少两种的组合,可选为银。
- 一种如权利要求1-3任一项所述的MXene/金属复合气凝胶的制备方法,其中,所述制备方法包括如下步骤:(1)将MXene分散液与金属盐溶液混合,反应,使金属离子还原成金属纳米颗粒,得到MXene/金属纳米颗粒复合材料的分散液;(2)将步骤(1)得到的分散液冷冻干燥,得到MXene/金属纳米颗粒复合气凝胶;(3)对步骤(2)得到的MXene/金属纳米颗粒复合气凝胶进行退火,使所述MXene/金属纳米颗粒复合气凝胶中的金属纳米颗粒熔融,所述退火完成后,得到所述MXene/金属复合气凝胶。
- 根据权利要求4所述的制备方法,其中,所述步骤(1)中所述反应的温度为-5~80℃,可选为-5~50℃;可选地,步骤(1)中所述反应的时间为10-30min;可选地,步骤(1)中所述反应是在超声振荡条件下进行。
- 根据权利要求4或5所述的制备方法,其中,所述制备方法还包括:在步骤(2)中所述冷冻干燥之前,将步骤(1)得到的分散液与聚乙烯醇混合;可选地,步骤(3)中所述退火的温度为150-500℃,时间为0.5-3h;可选地,步骤(3)中所述退火是在保护气氛下进行。
- 根据权利要求4-6任一项所述的制备方法,其中,所述制备方法包括如下步骤:(1)将MXene分散液与金属盐溶液搅拌混合,在超声振荡条件下,在-5~50℃下反应10min~30min,使金属离子还原成金属纳米颗粒,得到MXene/金属纳米颗粒复合材料的分散液;(2)将步骤(1)得到的分散液与聚乙烯醇溶液混合,加入模具中,放置在浸泡于液氮中的铜柱上进行冷冻,然后置于冷冻干燥机中进行干燥,得到MXene/金属纳米颗粒复合气凝胶;(3)在保护气氛下,将步骤(2)得到的MXene/金属纳米颗粒复合气凝胶在150-500℃下退火0.5-3h,使所述MXene/金属纳米颗粒复合气凝胶中的金属纳米颗粒熔融,所述退火完成后,得到所述MXene/金属复合气凝胶。
- 一种如权利要求1-3任一项所述的MXene/金属复合气凝胶的用途,其中,所述MXene/金属复合气凝胶用作导热填料。
- 一种热界面材料,其中,所述热界面材料包括聚合物基底和如权利要求1-3任一项所述的MXene/金属复合气凝胶。
- 根据权利要求9所述的热界面材料,其中,所述热界面材料中MXene/金属复合气凝胶的体积百分含量为3-40%,可选为10-15%。
- 根据权利要求9或10所述的热界面材料,其中,所述聚合物基底选自 环氧树脂、聚酰亚胺、聚酯、聚二甲基硅氧烷、聚氨酯、聚偏氟乙烯、丙烯腈-丁二烯-苯乙烯共聚物、聚氯乙烯、聚乙烯、聚苯乙烯、聚丙烯、天然橡胶、丁苯橡胶、硅橡胶、顺丁橡胶、异戊橡胶、氯丁橡胶、聚甲基丙烯酸甲酯、聚酰胺、聚甲醛、聚碳酸酯、乙烯基硅油或二甲基硅油中的一种或至少两种的组合。
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