CN117641869A - Preparation method of heat-conducting wave-absorbing nanocomposite - Google Patents
Preparation method of heat-conducting wave-absorbing nanocomposite Download PDFInfo
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- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims abstract description 7
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 7
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- UYXWTYRQGBBXHB-UHFFFAOYSA-N platinum 1,2,3,4-tetramethylcyclopenta-1,3-diene Chemical compound [Pt].CC1=C(C(=C(C1)C)C)C UYXWTYRQGBBXHB-UHFFFAOYSA-N 0.000 claims description 4
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Abstract
The preparation method of the heat-conducting wave-absorbing nanocomposite material comprises the following steps: 1. respectively taking hydrofluoric acid solutions with mass fractions of 38-40% and 10-12%, respectively adding Ti 3 AlC 2 Powder and magnetically stirring: 2. diluting, filtering, washing and drying to obtain a first MXene material and a second MXene material; 3. mixing the MXene material I and the MXene material II with copper chloride and chlorineReacting ferrous chloride and ferric chloride in a high-temperature high-pressure kettle, cooling, vacuum filtering, washing and drying after the reaction is finished to obtain an MXene composite material; 4. stirring the MXene composite material and deionized water to form a suspension; preparing the MXene aerogel by unidirectional freeze drying under the magnetic field condition; 5. and immersing the composite silicon resin into an MXene skeleton, and curing the silicon resin by ultraviolet irradiation to obtain the heat-conducting wave-absorbing nanocomposite. The heat-conducting wave-absorbing nanocomposite material prepared by the invention has a wider wave-absorbing range and good heat-conducting capacity.
Description
Technical Field
The invention relates to the field of nanocomposite materials, belongs to the field of preparation and application of high-performance nanocomposite materials for electronic equipment, and in particular relates to a preparation method of a heat-conducting wave-absorbing nanocomposite material.
Background
With the continuous improvement of the technical level of the modern electronic industry, particularly when 5G and radar communication technologies are rapidly developed, a plurality of high-intelligent electronic new devices are widely applied to daily life of people. While these electronic devices provide great convenience in the lifestyle of people, a large amount of electromagnetic radiation is also produced. Excessive and strong electromagnetic radiation can not only interfere the normal operation of electronic equipment, but also directly threaten the health of human bodies, and the development of novel broadband, strong-absorption, green, light and thin high-performance wave-absorbing material aiming at the electromagnetic radiation hazard has great application value.
The phenomena of heating and temperature rising of power consumption of electronic elements and generated electromagnetism caused by high frequency and integration of electronic equipment are increasingly serious, and interference caused by electromagnetic radiation not only affects normal operation of instruments, but also leaks important information. The serious heat dissipation problem not only brings adverse effect on the working stability of the system, but also ensures that the device works in a high-temperature environment for a long time, so that the working performance of the electronic device is reduced or even crashed, and the service life of the electronic device is influenced. Along with the integration of the application requirements of the wave absorbing material, the complexity of application scenes and the diversification of application fields, besides the basic functions of absorbing and attenuating electromagnetic waves, the wave absorbing material based on the limited physical space of electronic equipment is insufficient to simultaneously support the existence of wave absorbing plates and heat conducting plates, and heat conduction is considered.
The wave absorbing material can convert electromagnetic waves into heat energy or other forms of energy loss, achieves the aim of reducing electromagnetic radiation, is suitable for microwave absorption in a very wide frequency domain, has stronger absorption capacity for the electromagnetic waves and higher absorption speed for converting the electromagnetic waves, and is also required to have wave absorbing capacity and heat conducting capacity at the same time; most of traditional heat conducting materials are metal materials with good heat conductivity, but the metal materials are not corrosion-resistant and are difficult to be made into multi-element functional materials, so that the application of the multi-element functional materials in the high technical field is limited.
Patent CN108264358A discloses a preparation method of flexible SiC/Si3N4 composite nanofiber with electromagnetic wave broadband strong absorption, based on a polymer-converted ceramic method, and combined with an electrospinning technology, the flexible SiC/Si3N4 composite nanofiber with high electromagnetic absorption strength and wider electromagnetic wave absorption band is prepared, but the material is not improved in heat conduction performance;
at present, a polymer-based heat-conducting wave-absorbing nanocomposite which has the comprehensive properties of good heat-conducting wave-absorbing performance, light weight, wide frequency band, thin thickness and multifunction and is based on electromagnetic wave protection does not exist. Solves the problem of electromagnetic wave radiation pollution which is more prominent in the current problem, and promotes the wide application of the polymer-based heat-conducting and wave-absorbing material in electronic, communication, medical equipment and the like.
Disclosure of Invention
The invention aims to solve the problems of the background technology and provides a preparation method of a heat-conducting wave-absorbing nanocomposite.
The aim of the invention can be achieved by the following technical scheme:
a thermally conductive wave-absorbing nanocomposite comprising the steps of:
step one, taking hydrofluoric acid solution with the mass fraction of 38-40%, and adding Ti 3 AlC 2 Powder, reacting under magnetic stirring; taking hydrofluoric acid solution with mass fraction of 10-12%, adding Ti 3 AlC 2 Powder, reacting under magnetic stirring;
step two, diluting, filtering, washing and drying the reacted solution to obtain a first MXene material and a second MXene material;
thirdly, adding the MXene material I and the MXene material II into deionized water, performing ultrasonic stirring to form uniform suspension, adding copper chloride powder, and performing magnetic stirring; adding ferrous chloride and ferric chloride, stirring uniformly to obtain a mixed solution, transferring the mixed solution into a high-temperature high-pressure kettle for reaction, cooling to room temperature after the reaction is finished, and washing and drying by deionized water and absolute ethyl alcohol after vacuum suction filtration to obtain an MXene composite material;
adding the MXene composite material into deionized water, and stirring to form a suspension; the suspension is placed in a magnetic field and frozen into solid at the temperature of liquid nitrogen in such a way that the bottom of the suspension contacts a cold source, and then the suspension is placed in a freeze dryer for freeze drying to obtain the MXene aerogel;
and fifthly, uniformly mixing copper oxide powder, silicon resin and vinyl silicone oil, adding a trimethyl (methyl-cyclopentadiene) platinum catalyst to obtain composite silicon resin, immersing the composite silicon resin into MXene aerogel, and using an ultraviolet light source to irradiate so as to cure the silicon resin and obtain the heat-conducting wave-absorbing nanocomposite.
Further, hydrofluoric acid solution with mass fraction of 38-40% and Ti 3 AlC 2 The mass ratio of the powder is 50-55:1-1.1, stirring at 30-40 ℃ for 24-36h;
hydrofluoric acid solution with mass fraction of 10-12% and Ti 3 AlC 2 The mass ratio of the powder is 200-220:1-1.1, stirring temperature is 10-15 ℃ and time is 8-12h.
Further, the drying temperature of the oven is 55-65 ℃ and the drying time is 4-6h.
Further, the mass ratio of the first MXene material to the second MXene material to the copper chloride powder to the ferrous chloride to the ferric chloride is 1-1.5:1-1.5:4-8:1-1.5:2-4.
Further, the rotation speed of the magnetic stirring is 400-600rpm, the temperature is 35-45 ℃, and the stirring time is 18-24h.
Further, the set temperature of the high-temperature high-pressure kettle is 200-210 ℃, and the reaction time is 11-13h.
Further, the magnetic field strength is 100-120mT, the drying temperature of the freeze dryer is 208.15K-213.15K, the pressure is 10-11pa, and the freeze drying time is 68-74h.
Further, the mass ratio of the copper oxide powder to the silicone resin to the vinyl silicone oil is 1-1.5:3-4:4-6.
Further, the ultraviolet light source has a wavelength of 355-365nm and an illumination intensity of 45-50mW/cm 2 The irradiation time is 8-10min.
The invention has the beneficial effects that:
(1) The heat-conducting wave-absorbing nanocomposite material prepared by the invention has a wider wave-absorbing range, and a three-dimensional conductive network is constructed by aerogel technology, so that the wave-absorbing performance of the material is further improved; in the arrangement of the heat conducting filler, the copper oxide and the ferroferric oxide compound are prepared, the heat conducting filler is directionally arranged under the action of a magnetic field to form a heat conducting network, copper oxide powder is added into silicon resin, and the copper oxide powder is cooperated with the heat conducting network while filling the gaps of the MXene aerogel, so that the heat conducting property of the material is improved, and the material is light in weight, has the thickness formulated by an aerogel framework and is high in selectivity due to the great reduction of the filler; the resin after uv light curing further improves the flexibility and physical strength of the material.
(2) The invention improves the wave-absorbing range of the material by preparing two MXene materials with wave-absorbing frequency bands and mixing the MXene materials, and adds CuCl 2 The powder is such that Cu 2+ Is inserted between MXene material layers, increases the interlayer spacing of MXene sheets, is beneficial to the formation of single-layer MXene nano sheets, leads the MXene nano sheets to be more prone to relatively orderly stacking during vacuum filtration, and simultaneously leads Cu to be more favorable 2+ And Fe added 2+ 、Fe 3+ Better interacts with MXene nano-sheets under the condition of high temperature and high pressure kettle, is tightly combined together, and reacts and oxidizes to generate CuO and Fe 3 O 4 The compound can be used as a heat conducting filler to enhance the heat conducting capacity of the MXene material.
(3) The invention introduces Fe into the heat conductive filler 3 O 4 To make the heat conductive filler CuO and Fe 3 O 4 The composite has rearranged magnetic moment under the action of external magnetic field, so that the composite of the heat conducting filler CuO and Fe3O4 is directionally arranged to form a heat conducting network, and the heat conducting capability of the material is improved; meanwhile, the three-dimensional conductive network structure constructed by the MXene nano-sheets is further improved in electromagnetic wave loss capacity by adopting a one-way freeze drying method to prepare the MXene aerogel, and the wave absorbing capacity of the material is improved; the porous structure also effectively improves the impedance of the composite materialMatching, so that the material is lighter; the material has anisotropic mechanical property and wave absorbing property due to directional freezing.
(4) According to the invention, silicon resin is used for filling the gaps of the MXene aerogel, and phonon scattering in the heat transmission process is increased by air existing in the gaps, so that the interface thermal resistance is increased, and the heat transmission is not facilitated; meanwhile, effective contact between the fillers is weakened, and the construction of a heat conduction path is not facilitated. The silicon resin is used for filling the gaps of the MXene aerogel, so that the air in the gaps can be removed, and after the curing, the flexibility and the physical strength of the MXene aerogel can be increased, so that the composite material can be suitable for various field requirements, and meanwhile, the copper oxide filler is added into the silicon resin and matched with the heat conduction filler in the MXene aerogel, so that the heat conduction capability of the composite material is further enhanced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the attached tables in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A preparation method of a heat-conducting wave-absorbing nanocomposite material comprises the following steps:
step one, preparing an MXene material I: 25g of 38% hydrofluoric acid solution is added with 0.55g of Ti 3 AlC 2 Magnetically stirring the powder at 30 ℃ for 24 hours;
preparation of MXene Material II: 100g of hydrofluoric acid solution with the mass fraction of 10% is taken and added with 0.55g of Ti 3 AlC 2 Magnetically stirring the powder at 10 ℃ for 8 hours;
the high-purity MXene prepared by 38-40% of HF has high concentration and complete etching, the prepared MXene material has an accordion structure, separation layers are mutually parallel, and macroscopic performance is obvious in low-frequency band (2-13 GHz); the high-purity MXene prepared by 10-12% of HF is low in HF concentration and is not thoroughly etched, and the prepared MXene material II is granular and has fewer layer stripes, and macroscopic appearance is high in absorption loss intensity in a high frequency band (5-18 GHz). So that the MXene material I and the MXene material II are prepared and mixed to improve the wave absorbing performance of the composite material;
and step two, respectively adding deionized water into the two cups of solution after the reaction is finished for dilution, respectively filtering the solution, washing the MXene material I and the MXene material II obtained after the filtering by deionized water and absolute ethyl alcohol until the materials are neutral, putting the materials into a 55 ℃ oven, drying for 4 hours, and collecting the materials for later use.
Step three, adding 1g of the first MXene material and 1g of the second MXene material into deionized water, ultrasonically stirring to form a uniform suspension, and adding 4g of CuCl 2 The powder was then magnetically stirred for 18h (rotation speed 400rpm, temperature 35 ℃); then adding 1g of ferrous chloride and 2g of ferric chloride, stirring uniformly, transferring the mixed solution into a high-temperature high-pressure kettle, keeping the temperature at 200 ℃ for 11 hours, cooling to room temperature after the reaction, carrying out vacuum filtration, washing with deionized water and absolute ethyl alcohol for multiple times, and drying to obtain the MXene composite material;
the MXene material has a layered structure, cu 2+ Can be inserted into the MXene material layered structure, so that the MXene material tends to have a few-layer and single-layer structure, and the surface area and the functionality of the MXene material are improved; iron ions generate Fe through hydrothermal reaction under the conditions of high temperature and high pressure 3 O 4 ，Fe 3 O 4 For Cu 2+ Has adsorption effect, and the surface of MXene is usually provided with hydroxyl (-OH) or oxide functional groups, cu 2+ The ions react with the functional groups on the surface of MXene under the conditions of high temperature and high pressure to generate CuO and Fe 3 O 4 Forming a complex.
And step four, preparing the MXene aerogel by adopting a unidirectional freeze drying method. Adding the MXene composite material into deionized water and stirring to form a suspension, placing the suspension in a magnetic field with the magnetic field strength of 100mT, enabling copper oxide and ferroferric oxide composite in the composite material to be directionally arranged in the magnetic field, freezing for 10 minutes at the temperature of liquid nitrogen in a way that the bottom of the suspension contacts a cold source, and then placing the suspension in a freeze dryer (208.15K, 10 Pa) for freeze drying for 68 hours to obtain the MXene aerogel.
The MXene aqueous suspension is frozen at the temperature of liquid nitrogen, and only the bottom is contacted with a cold source, so that ice crystals vertically grow in the suspension, and CuO and Fe are simultaneously grown under the action of a magnetic field 3 O 4 The formed compound can be aligned to form a better heat conduction network, and the heat conduction network is fixed under the action of freeze drying.
Fifthly, mixing copper oxide powder, silicone resin and vinyl silicone oil according to a proportion of 1:3:4, adding a trimethyl (methyl-cyclopentadiene) platinum catalyst to obtain composite silicon resin, immersing the composite silicon resin into a skeleton of the MXene aerogel, wherein the wavelength is 355nm, and the illumination intensity is 45mW/cm 2 And (3) irradiating the silicon resin for 8min by using an ultraviolet light source to cure the silicon resin, thereby obtaining the heat-conducting wave-absorbing nanocomposite.
Because the skeleton pores in the MXene aerogel are smaller, vinyl silicone oil is required to dilute the silicone resin, so that the interior of the MXene skeleton is filled with the silicone resin, and the flexibility and the physical strength of the composite material are improved; meanwhile, copper oxide powder is added into the resin, so that the pores of the MXene skeleton are filled with heat conducting filler, and the heat conducting filler is matched with the copper oxide/ferroferric oxide composite material in the MXene skeleton to jointly form a heat conducting network, so that the heat conducting capacity of the composite material is improved.
Example 2
A preparation method of a heat-conducting wave-absorbing nanocomposite material comprises the following steps:
step one, preparing an MXene material I: 27.5g of hydrofluoric acid solution with the mass fraction of 40% is taken and added with 0.5g of Ti 3 AlC 2 Magnetically stirring the powder at 40 ℃ for 36h;
preparation of MXene Material II: 110g of hydrofluoric acid solution with the mass fraction of 10-12% is taken and added with 0.5g of Ti 3 AlC 2 Magnetically stirring the powder at 15 ℃ for 12 hours;
and step two, respectively adding deionized water into the two cups of solution after the reaction is finished for dilution, respectively filtering the solution, washing the MXene material I and the MXene material II obtained after the filtering by deionized water and absolute ethyl alcohol until the materials are neutral, putting the materials into a 65 ℃ oven, drying for 6 hours, and collecting the materials for later use.
Step three, adding 1.5g of the first MXene material and 1.5g of the second MXene material into deionized water, ultrasonically stirring to form a uniform suspension, and adding 8g of CuCl 2 The powder was then magnetically stirred for 24h (rotation speed 600rpm, temperature 45 ℃); then adding 1.5g of ferrous chloride and 4g of ferric chloride, stirring uniformly, transferring the mixed solution into a high-temperature high-pressure kettle, keeping the constant temperature at 210 ℃ for 13 hours, cooling to room temperature after the reaction, carrying out vacuum suction filtration, washing with deionized water and absolute ethyl alcohol for multiple times, and drying to obtain the MXene composite material;
and step four, preparing the MXene aerogel by adopting a unidirectional freeze drying method. Adding the MXene composite material into deionized water and stirring to form a suspension, placing the suspension in a magnetic field with the magnetic field strength of 120mT, enabling copper oxide and ferroferric oxide composite in the composite material to be directionally arranged in the magnetic field, freezing for 10 minutes at the temperature of liquid nitrogen in a way that the bottom of the suspension contacts a cold source, and then placing the suspension in a freeze dryer (213.15K, 11 Pa) for freeze drying for 74 hours to obtain the MXene aerogel.
Fifthly, copper oxide powder, silicone resin and vinyl silicone oil are mixed according to the proportion of 1.5:4:6, adding a trimethyl (methyl-cyclopentadiene) platinum catalyst to obtain composite silicon resin, immersing the composite silicon resin in MXene aerogel, wherein the wavelength is 365nm, and the illumination intensity is 50mW/cm 2 And (3) irradiating for 10min by using an ultraviolet light source to solidify the silicon resin, thereby obtaining the heat-conducting wave-absorbing nanocomposite.
Comparative example 1
The only difference from example 1 is that MXene material two was not prepared and used.
Comparative example 2
The only difference from example 1 is that step three is: adding copper oxide powder, stirring and mixing.
Comparative example 3
A commercially available heat conducting and wave absorbing material of the type TIF900B-30 is available in the megalogy of ziitek.
The following table shows the wave-absorbing and heat conducting properties of the 5mm thick nanocomposites of the examples and comparative examples;
from the above table, the effective absorption bandwidths of example 1 and example 2 are 6.32GHz and 6.18GHz, which are greater than those of comparative example 1 and comparative example 2, and it is demonstrated that the combined use of the first and second MXene materials can effectively improve the absorption bandwidth of the composite material; the maximum reflection loss of example 1 is-31.14 dB, the maximum reflection loss of example 2 is-30.26 dB, which are smaller than those of comparative examples 1, 2 and 3, and the absorption performance of example 1 and example 2 on electromagnetic waves is good; the embodiment 1 and the embodiment 2 of the invention can achieve both wider effective absorption bandwidth and smaller maximum reflection loss, and the comparative example 3 has larger effective absorption bandwidth, but has higher maximum reflection loss, and the comprehensive wave absorption capacity is not as good as that of the embodiment 1 and the embodiment 2; the thermal conductivity of example 1 was 7.3W/mK, the thermal conductivity of example 2 was 7.1W/mK, and the thermal conductivities of comparative example 1, comparative example 2 and comparative example 3 were all superior, and the thermal conductivities were excellent.
The foregoing describes one embodiment of the present invention in detail, but the description is only a preferred embodiment of the present invention and should not be construed as limiting the scope of the invention. All equivalent changes and modifications within the scope of the present invention are intended to be covered by the present invention.
Claims (9)
1. The preparation method of the heat-conducting wave-absorbing nanocomposite is characterized by comprising the following steps of:
step one, taking hydrofluoric acid solution with the mass fraction of 38-40%, and adding Ti 3 AlC 2 Powder, reacting under magnetic stirring; taking hydrofluoric acid solution with mass fraction of 10-12%, adding Ti 3 AlC 2 Powder, reacting under magnetic stirring;
step two, diluting, filtering, washing and drying the reacted solution to obtain a first MXene material and a second MXene material;
thirdly, adding the MXene material I and the MXene material II into deionized water, performing ultrasonic stirring to form uniform suspension, adding copper chloride powder, and performing magnetic stirring; adding ferrous chloride and ferric chloride, uniformly stirring to obtain a mixed solution, transferring the mixed solution into a high-temperature high-pressure kettle for reaction, cooling to room temperature after the reaction is finished, and washing and drying by deionized water and absolute ethyl alcohol after vacuum suction filtration to obtain an MXene composite material;
adding the MXene composite material into deionized water, and stirring to form a suspension; the suspension is placed in a magnetic field and frozen into solid at the temperature of liquid nitrogen in such a way that the bottom of the suspension contacts a cold source, and then the suspension is placed in a freeze dryer for freeze drying to obtain the MXene aerogel;
and fifthly, uniformly mixing copper oxide powder, silicon resin and vinyl silicone oil, adding a trimethyl (methyl-cyclopentadiene) platinum catalyst to obtain composite silicon resin, immersing the composite silicon resin into MXene aerogel, and using an ultraviolet light source to irradiate so as to cure the silicon resin and obtain the heat-conducting wave-absorbing nanocomposite.
2. The method for preparing a heat-conducting and wave-absorbing nanocomposite according to claim 1, wherein in the first step, the hydrofluoric acid solution with the mass fraction of 38-40% and Ti 3 AlC 2 The mass ratio of the powder is 50-55:1-1.1, stirring at 30-40 ℃ for 24-36h; the mass fraction of hydrofluoric acid solution and Ti is 10-12 percent 3 AlC 2 The mass ratio of the powder is 200-220:1-1.1, stirring temperature is 10-15 ℃ and time is 8-12h.
3. The method for preparing a heat-conducting wave-absorbing nanocomposite according to claim 1, wherein in the second step, the drying temperature is 55-65 ℃ and the drying time is 4-6h.
4. The method for preparing a heat conduction wave-absorbing nanocomposite according to claim 1, wherein in the third step, the mass ratio of the first MXene material to the second MXene material to the copper chloride powder to the ferrous chloride to the ferric chloride is 1-1.5:1-1.5:4-8:1-1.5:2-4.
5. The method for preparing a heat-conducting and wave-absorbing nanocomposite according to claim 1, wherein in the third step, the rotation speed of the magnetic stirring is 400-600rpm, the temperature is 35-45 ℃, and the stirring time is 18-24 hours.
6. The method for preparing the heat-conducting wave-absorbing nanocomposite according to claim 1, wherein the high-temperature autoclave is set at 200-210 ℃ and the reaction time is 11-13h.
7. The method for preparing a heat-conducting and wave-absorbing nanocomposite according to claim 1, wherein in the fourth step, the magnetic field strength is 100-120mT, the drying temperature of the freeze dryer is 208.15K-213.15K, the pressure is 10pa, and the freeze drying time is 68-74h.
8. The method for preparing the heat conduction wave-absorbing nanocomposite according to claim 1, wherein in the fifth step, the mass ratio of the copper oxide powder to the silicone resin to the vinyl silicone oil is 1-1.5:3-4:4-6.
9. The method for preparing a heat-conducting wave-absorbing nanocomposite according to claim 1, wherein in the fifth step, the ultraviolet light source wavelength is 355-365nm, and the illumination intensity is 45-50mW/cm 2 The irradiation time is 8-10min.
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