Hollow phosphorus-nickel-based carbon nanocomposite derived from MOFs and preparation method thereof

Abstract

The application provides a MOFs derived hollow nickel phosphide-based carbon nanocomposite material and a preparation method thereof, relates to the field of electromagnetic microwave absorption, and mainly takes nickel-based material as a metal source, takes MOFs as a metal-organic framework, synthesizes a Ni / CNs intermediate, and then performs phosphorization treatment on the Ni / CNs intermediate to obtain a hollow Ni / Ni2P / CNs; the preparation method of the hollow nickel phosphide-based carbon nanocomposite material mainly comprises S1, preparation of the hollow Ni / CNs, S2, preparation of the hollow Ni / Ni2P / CNs. The hollow structure of the Ni / Ni2P / CNs composite material of the application promotes impedance matching, the phosphorization improves the wave absorption performance, has great potential to become a high-performance electromagnetic microwave absorption material, and the construction of a Schottky heterojunction also provides a reference for the research on a deep-level electromagnetic wave loss mechanism.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of electromagnetic microwave absorbing materials, and particularly relates to a MOFs-derived hollow nickel phosphide-based carbon nanocomposite material and a preparation method thereof. BACKGROUND

[0002] With the rapid development of communication technology and electronic technology, electromagnetic waves as the carrier of information transmission have penetrated into all aspects of life, although they have brought great convenience to people's life, but also brought serious electromagnetic pollution. Therefore, it is urgent to develop high-efficiency electromagnetic wave absorbing materials. Metal-organic frameworks (MOFs) have attracted much attention due to their porous structure and adjustable microstructure, and have been widely used in catalysis, sterilization, batteries and other fields.

[0003] High-performance electromagnetic microwave absorbing materials depend largely on the impedance matching characteristics and electromagnetic wave attenuation ability of the materials, and they are closely related to the size, microstructure and composition of the materials. Of course, in addition to the inherent impedance matching characteristics and attenuation characteristics of the materials, the micro-morphology of the materials is also a factor affecting the wave absorption performance. In order to improve the electromagnetic microwave absorption performance, it is also a common method to reasonably design wave absorbing materials with special microstructure. In addition, researchers have made a lot of achievements in designing and controlling materials with special structures, such as porous structure, multi-level structure, core-shell structure and hollow structure, especially the hollow structure with large internal void and low density has attracted widespread attention of researchers. The hollow structure not only can reduce the density of the material to achieve lightweight standards, but also can adjust the electromagnetic parameters to promote impedance matching, and such internal voids are also beneficial to the multiple reflection and scattering of electromagnetic waves inside the hollow structure. Huang et al. used ZIF-8 as a template and grew hollow HZIF-CoMo on the surface of ZIF-8 by a solvothermal method. ZIF-8 was rapidly pyrolyzed to form a hollow structure at 900℃, and the surface HZIF-CoMo was converted into Co / MoC2@HNCP. The hollow structure greatly enhances the impedance matching and multiple scattering, and the Co and MoC2 nanoparticles are uniformly distributed in the carbon shell, providing a rich multi-heterojunction. Therefore, the minimum reflection loss of CoMo@HNCP is 44.8 dB, and the effective bandwidth is 6.56 GHz. Su et al. prepared ZIF-67@MoSe2 composite materials by hydrothermal reaction using ZIF-67 as a template, and obtained hollow Co / C@MoSe2 composite materials after high-temperature annealing. Experimental results prove that the designed hollow structure is beneficial to optimizing the electromagnetic parameters and improving the electromagnetic wave absorption performance, and the minimum reflection loss is 42 dB, and the effective bandwidth is 5.1 GHz, which meets the design requirements of excellent wave absorbing materials. Although the hollow structure can significantly improve the electromagnetic microwave absorption performance of the material, it is still necessary to explore a convincing electromagnetic wave attenuation mechanism.

[0004] Researchers have explained the electromagnetic microwave loss mechanism from the perspective of metal-semiconductor heterojunctions. Based on differences in semiconductor type and work function, metal-semiconductor heterojunctions are classified into ohmic contacts and Schottky contacts. Ohmic contacts form a thin superconducting layer on the semiconductor surface, which is beneficial for improving conduction loss. Schottky contacts, due to the presence of the Schottky barrier, result in a large interfacial resistance, which helps accumulate charge at the interface. In an alternating electric field, the positive and negative charges at the interface are forced to rearrange, forming a local dipole electric field, which converts electromagnetic energy into heat energy through polarization. Qiu et al. designed abundant Co@C@MnO heterojunctions using etching and pyrolysis processes. By adjusting the Co content, they enhanced the interfacial polarization loss, and the composite material exhibited a minimum reflection loss of -64.4 dB. Xu et al. used MnO3 nanorods as templates to grow a series of FeOOH nanoarrays on their surface. Then, using a polymerization-etching strategy, they simultaneously etched MnO3 and coated the FeOOH surface with a layer of PDA. After annealing, they obtained hollow Fe / Fe3O4 / C nanocomposite materials. This unique structure, composed of abundant heterogeneous interfaces, can induce strong interfacial polarization losses. Due to its hierarchical hollow structure, abundant electromagnetic heterogeneous interfaces, and highly dispersive magnetic particles, the prepared Fe / Fe3O4@C exhibits excellent electromagnetic wave absorption performance, with a maximum reflection loss of [value missing]. The effective absorption bandwidth is 4.2 GHz, with a spectral density of 55.4 dB. High-temperature annealing of MOFs generates numerous heterojunctions between metals and nitrogen-doped carbon. Analyzing the electromagnetic microwave loss mechanism of MOF-derived composites from the perspective of metal-semiconductor contacts is a worthy research topic. Summary of the Invention

[0005] (a) Technical problems to be solved

[0006] To address the shortcomings of existing technologies, this invention provides a MOFs-derived hollow nickel phosphide-based carbon nanocomposite material and its preparation method, which solves the problem of low electromagnetic microwave absorption performance.

[0007] (II) Technical Solution

[0008] To achieve the above objectives, the present invention provides the following technical solution:

[0009] The first technical objective of this invention is to disclose a MOFs-derived hollow nickel-phosphated carbon nanocomposite material, which mainly uses nickel-based materials as the metal source and MOFs as the metal-organic framework to synthesize Ni / CNs intermediates, and then phosphating the Ni / CNs intermediates to obtain hollow Ni / Ni2P / CNs.

[0010] The second technical objective of the present application is to disclose a preparation method of MOFs-derived hollow nickel phosphide-based carbon nanocomposite material, specifically comprising the following steps:

[0011] S1, preparation of hollow Ni / CNs

[0012] The hollow Ni-MOF precursor is prepared by using nickel nitrate as a metal source, using trimesic acid as an organic ligand, using DMF and water as solvents, and using polyvinylpyrrolidone (PVP) as a stabilizer. The hollow Ni-MOF precursor is weighed, and the hollow Ni / CNs are prepared after high-temperature annealing under a nitrogen atmosphere.

[0013] S2, preparation of hollow Ni / Ni2P / CNs

[0014] The hollow Ni / CNs are weighed in a porcelain boat and placed downstream of a tube furnace. NaH2PO2·H2O is weighed in a porcelain boat and placed upstream of the tube furnace. The final product Ni / Ni2P / CNs is prepared after high-temperature annealing under a nitrogen flow.

[0015] Preferably, the high-temperature annealing in S1 and S2 is specifically operated as follows: the temperature is increased to 700-900℃ at a rate of 2℃ / min from room temperature, and then the temperature is decreased to room temperature after 2h of holding.

[0016] Preferably, the high-temperature annealing temperature is 800℃.

[0017] Preferably, the specific method for synthesizing the hollow Ni-MOF precursor is as follows: nickel nitrate, trimesic acid, and polyvinylpyrrolidone are stirred in a mixed solvent of DMF and water for 30-40min, then kept at 140-160℃ for 8-16h, and then the green precipitate obtained by centrifugation after cooling to room temperature is the hollow Ni-MOF precursor.

[0018] Preferably, the volume ratio of DMF to water is (1-5):1.

[0019] The third technical objective of the present application is to provide an application of MOFs-derived hollow nickel phosphide-based carbon nanocomposite material or a preparation method of MOFs-derived hollow nickel phosphide-based carbon nanocomposite material, which can apply the above-mentioned composite material or preparation method to the field of electromagnetic microwave absorption.

[0020] (Three) beneficial effects

[0021] The present application provides a MOFs-derived hollow nickel phosphide-based carbon nanocomposite material and a preparation method thereof. Compared with the prior art, the present application has the following beneficial effects:

[0022] The present application prepares a hollow Ni / Ni2P / CNs composite material through high-temperature annealing and phosphating strategies. The hollow structure not only reduces the material density to achieve lightweight standards, but also facilitates the improvement of impedance matching characteristics and the increase of decay constant, allowing more electromagnetic microwaves to enter the material interior and consuming electromagnetic microwave energy through multiple reflections and scattering. The highly dispersed metal nickel nanoparticles form a dense magnetic coupling network, and the Ni2P produced after phosphating not only improves the impedance matching characteristics of the material, but also improves the electromagnetic microwave absorption performance of the material. A large number of Schottky heterojunction interfaces are generated between the metal Ni and the semiconductor Ni2P, which facilitates the improvement of polarization loss due to the formation of internal dipole electric field by the Schottky barrier, and converts electromagnetic energy into heat energy through interface polarization.

[0023] The hollow structure of the Ni / Ni2P / CNs composite material of the present application promotes impedance matching, and phosphating improves the wave absorption performance. Under a filler content of 20 wt%, the minimum reflection loss of the Ni / Ni2P / CNs composite material is-72.1 dB, and the effective bandwidth is 5.8 GHz. The results show that the Ni / Ni2P / CNs composite material has great potential to become a high-performance electromagnetic microwave absorption material, and the construction of the Schottky heterojunction interface also provides a reference for the research of deep electromagnetic wave loss mechanism. BRIEF DESCRIPTION OF DRAWINGS

[0024] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings needed to be used in the embodiments or prior art description. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can also be obtained by those skilled in the art without creative labor.

[0025] Figure 1 Figures (a) (b) (c) (d) (e) (f) are SEM images of Ni-BTC, H-Ni-BTC, Ni / CNs, Ni / Ni2P / CNs-1, Ni / Ni2P / CNs-2 and Ni / Ni2P / CNs-3, respectively, (g) is a TEM image of Ni / Ni2P / CNs, and (h) is a HRTEM image of Ni / Ni2P / CNs.

[0026] Figure 2 Figure is a flowchart of the preparation method of the Ni / Ni2P / CNs composite material in the embodiments of the present application.

[0027] Figure 3 Figure is a comparison diagram of the minimum reflection loss of Ni / Ni2P / CNs-2, Ni / CNs and Ni / C in the embodiments and comparative examples of the present application.

[0028] Figure 4A schematic diagram of minimum reflection loss of Ni / Ni2P / CNs-1, Ni / Ni2P / CNs-2 and Ni / Ni2P / CNs-3 in the embodiments of the present application is shown. DETAILED DESCRIPTION

[0029] In order to make the objectives, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application are described clearly and completely. Obviously, the described embodiments are part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0030] The embodiments of the present application provide a MOFs-derived hollow nickel phosphide-based carbon nanocomposite material and a preparation method thereof, solve the problem of low electromagnetic microwave absorption performance at present, the hollow structure of the hollow Ni / Ni2P / CNs composite material promotes impedance matching, phosphating improves the wave absorption performance, has great potential to become a high-performance electromagnetic microwave absorption material, and the construction of the Schottky heterojunction also provides a reference for the research of deep electromagnetic wave loss mechanism.

[0031] To solve the above technical problems, the general idea is that the present application prepares a hollow Ni / Ni2P / CNs composite material through high-temperature annealing and phosphating strategy. The hollow structure not only reduces the material density to achieve the lightweight standard, but also is beneficial to the improvement of impedance matching characteristics. The highly dispersed metal nickel nanoparticles form a dense magnetic coupling network, and the Ni2P produced after phosphating not only improves the impedance matching characteristics of the material, but also improves the electromagnetic microwave absorption performance of the material. A large number of Schottky heterojunctions are produced between the metal Ni and the semiconductor Ni2P, and the electromagnetic energy is converted into heat energy through interface polarization. The hollow structure promotes impedance matching, and the phosphating improves the wave absorption performance. Under the condition of 20 wt% filler content, the minimum reflection loss of the Ni / Ni2P / CNs composite material is-72.1 dB, and the effective bandwidth is 5.8 GHz. The results show that the Ni / Ni2P / CNs composite material has great potential to become a high-performance electromagnetic microwave absorption material, and the construction of the Schottky heterojunction also provides a reference for the research of deep electromagnetic wave loss mechanism.

[0032] In order to better understand the above technical solutions, the above technical solutions will be described in detail in combination with the drawings of the specification and the specific embodiments.

[0033] Embodiment 1:

[0034] The MOFs-derived hollow phosphatized nickel-based carbon nanocomposite material takes a nickel-based material as a metal source, takes MOFs as a metal-organic framework, synthesizes a Ni / CNs intermediate, and then performs phosphatization treatment on the Ni / CNs intermediate to obtain the hollow Ni / Ni2P / CNs.

[0035] The preparation method of the MOFs-derived hollow phosphatized nickel-based carbon nanocomposite material, as shown in Figure 2 , specifically includes the following steps:

[0036] S1, 432 mg of Ni(NO3)2·6H2O, 150 mg of H3BTC, and 1.5 g of PVP are weighed and dissolved in a solution of 10 mL of water and 20 mL of DMF, stirred for 30 min, and then kept at 150℃ for 15 h. After cooling to room temperature, centrifugation is performed to obtain a green precipitate, which is dried to obtain a hollow Ni-MOF precursor;

[0037] 500 mg of the hollow Ni-MOF precursor is weighed in a crucible, heated to 800℃ at a rate of 2℃ / min under a nitrogen atmosphere, and then cooled to room temperature after being kept at 800℃ for 2 h to obtain the hollow Ni / CNs.

[0038] S2, 100 mg of Ni / CNs is weighed in a porcelain boat and placed downstream of a tube furnace. 1000 mg of NaH2PO2·H2O is weighed in a porcelain boat and placed upstream of the tube furnace. Heating is performed at a heating rate of 2℃ / min to 800℃ under a nitrogen flow, and then kept at 800℃ for 2 h. After the temperature is reduced to room temperature, the final sample Ni / Ni2P / CNs-2 is obtained.

[0039] As shown in Figure 3 (c) (f) or Figure 4 (b) (e), the minimum reflection loss of the hollow Ni / Ni2P / CNs-2 obtained above is 71.8 dB, and the effective absorption bandwidth EAB is 5.8 GHz.

[0040] Example 2:

[0041] The MOFs-derived hollow phosphatized nickel-based carbon nanocomposite material takes a nickel-based material as a metal source, takes MOFs as a metal-organic framework, synthesizes a Ni / CNs intermediate, and then performs phosphatization treatment on the Ni / CNs intermediate to obtain the hollow Ni / Ni2P / CNs.

[0042] The preparation method of the MOFs-derived hollow phosphatized nickel-based carbon nanocomposite material, as shown in Figure 2 , specifically includes the following steps:

[0043] S1, 432 mg of Ni(NO3)2·6H2O, 150 mg of H3BTC and 1.5 g of PVP were weighed and dissolved in a solution of 10 mL of water and 20 mL of DMF, stirred for 30 min, and then kept at 150°C for 15 h. After cooling to room temperature, centrifugation was performed to obtain a green precipitate, which was dried to obtain a hollow Ni-MOF precursor;

[0044] 500 mg of the hollow Ni-MOF precursor was weighed into a crucible, heated to 800°C at a rate of 2°C / min under a nitrogen atmosphere, and then cooled to room temperature after being kept at 800°C for 2 h to obtain hollow Ni / CNs.

[0045] S2, 100 mg of Ni / CNs was weighed into a porcelain boat and placed downstream of the tube furnace, and 500 mg of NaH2PO2·H2O was weighed into a porcelain boat and placed upstream of the tube furnace. The temperature was raised to 800°C at a rate of 2°C / min under a nitrogen flow, and then kept at 800°C for 2.5 h. After the temperature was reduced to room temperature, the final sample Ni / Ni2P / CNs-1 was obtained.

[0046] As shown in (a) and (d), the minimum reflection loss of the hollow Ni / Ni2P / CNs-1 obtained above is Figure 4 44.2 dB, and the effective absorption bandwidth EAB is 3.8 GHz.

[0047] Example 3:

[0048] The hollow nickel phosphide-based carbon nanocomposite material derived from MOFs uses a nickel-based material as a metal source, uses MOFs as a metal-organic framework, synthesizes a Ni / CNs intermediate, and then performs phosphating treatment on the Ni / CNs intermediate to obtain a hollow Ni / Ni2P / CNs.

[0049] The preparation method of the hollow nickel phosphide-based carbon nanocomposite material derived from MOFs, as shown in (a) and (d), specifically includes the following steps: Figure 2

[0050] S1, 432 mg of Ni(NO3)2·6H2O, 150 mg of H3BTC and 1.5 g of PVP were weighed and dissolved in a solution of 10 mL of water and 20 mL of DMF, stirred for 30 min, and then kept at 150°C for 15 h. After cooling to room temperature, centrifugation was performed to obtain a green precipitate, which was dried to obtain a hollow Ni-MOF precursor;

[0051] 500 mg of the hollow Ni-MOF precursor was weighed into a crucible, heated to 800°C at a rate of 2°C / min under a nitrogen atmosphere, and then cooled to room temperature after being kept at 800°C for 2 h to obtain hollow Ni / CNs.

[0052] ​​S2, 100 mg of Ni / CNs was weighed in a porcelain boat and placed downstream of the tube furnace, 1500 mg of NaH2PO2·H2O was weighed in a porcelain boat and placed upstream of the tube furnace. The heating rate was 2℃ / min under nitrogen flow to 800℃, and the temperature was kept for 3h. The final sample Ni / Ni2P / CNs-3 was obtained when the temperature dropped to room temperature.

[0053] As shown in Figure 4 (c) (f) shows the hollow Ni / Ni2P / CNs-3 obtained above. The minimum reflection loss is 51.6 dB, and the effective absorption bandwidth EAB is 6.0 GHz.

[0054] Comparative Example 1:

[0055] The preparation method of the MOFs-derived hollow nickel-based carbon nanocomposite material specifically comprises the following steps:

[0056] 432 mg of Ni(NO3)2·6H2O, 150 mg of H3BTC and 1.5 g of PVP were weighed and dissolved in a solution of 10 mL of water and 20 mL of DMF, stirred for 30 min, and then kept at 150℃ for 15h. After cooling to room temperature, the green precipitate was centrifuged and dried to obtain a hollow Ni-MOF precursor;

[0057] 500 mg of the hollow Ni-MOF precursor was weighed in a crucible and heated to 800℃ at a rate of 2℃ / min under a nitrogen atmosphere. After keeping the temperature for 2h, the hollow Ni / CNs was obtained when the temperature dropped to room temperature.

[0058] As shown in Figure 3 (b) (e) shows the hollow Ni / CNs obtained above. The minimum reflection loss is 30.7 dB, and the effective absorption bandwidth EAB is 3.4 GHz.

[0059] Comparative Example 2:

[0060] The preparation method of the MOFs-derived solid nickel-based carbon nanocomposite material specifically comprises the following steps:

[0061] 432 mg of Ni(NO3)2·6H2O, 150 mg of H3BTC and 1.5 g of PVP were weighed and dissolved in a solution of 10 mL of water and 20 mL of DMF, stirred for 30 min, and then kept at 150℃ for 15h. After cooling to room temperature, the green precipitate was centrifuged and dried to obtain a hollow Ni-MOF precursor;

[0062] 500 mg of the hollow Ni-MOF precursor was weighed in a crucible and heated to 800℃ at a rate of 2℃ / min under a nitrogen atmosphere. After keeping the temperature for 2h, the hollow Ni / CNs was obtained when the temperature dropped to room temperature.

[0063] like Figure 3 As shown in (a) and (d), the minimum reflection loss of the solid Ni / C obtained above is 24.3 dB, with an effective absorption bandwidth (EAB) of 3.4 GHz.

[0064] Figure 1 (a), (b), (c), (d), (e), and (f) are SEM images of Ni-BTC, H-Ni-BTC, Ni / CNs, Ni / Ni2P / CNs-1, Ni / Ni2P / CNs-2, and Ni / Ni2P / CNs-3, respectively; (g) is a TEM image of Ni / Ni2P / CNs; and (h) is an HRTEM image of Ni / Ni2P / CNs.

[0065] pass Figure 3 Analysis of the electromagnetic parameters and reflection loss diagram of the samples reveals that phosphating significantly enhances the electromagnetic wave absorption capability of the material based on the hollow structure. Building upon the improved impedance matching characteristics and attenuation constant of the hollow structure, the Ni / Ni2P / CNs-2 produced after phosphating not only exhibits a larger attenuation constant but also improved impedance matching characteristics, resulting in optimal electromagnetic microwave absorption performance.

[0066] pass Figure 4 It was clearly observed that the Ni / Ni2P / CNs-2 sample exhibited the best electromagnetic microwave absorption capability. Figure 4 The minimum reflection loss of Ni / Ni2P / CNs-1 in (a) and (d) is 44.2 dB, with an effective absorption bandwidth (EAB) of 3.8 GHz. Figure 4 In (b) and (e), the minimum reflection loss of Ni / Ni2P / CNs-2 is optimal. 71.8 dB, with an effective bandwidth of 5.8 GHz. In Figure 4 In (c) and (f), the minimum reflection loss of Ni / Ni2P / CNs-3 is optimal. The effective bandwidth is 6.0 GHz, with a strength of 51.6 dB. Comparison with the electromagnetic microwave absorption performance of Ni / CNs shows that phosphating improves the electromagnetic microwave absorption performance of the sample. However, with increasing phosphating degree, the electromagnetic microwave absorption performance of the sample first increases and then decreases.

[0067] In summary, compared with existing technologies, it has the following beneficial effects:

[0068] 1、The application prepares a hollow Ni / Ni2P / CNs composite material through high-temperature annealing and phosphating strategies. The hollow structure not only reduces the material density to achieve lightweight standards, but also is beneficial to the improvement of impedance matching characteristics and the increase of decay constant, allowing more electromagnetic microwaves to enter the material interior and consuming electromagnetic microwave energy through multiple reflections and scattering. The highly dispersed metal nickel nanoparticles form a dense magnetic coupling network, and the Ni2P produced after phosphating not only improves the impedance matching characteristics of the material, but also improves the electromagnetic microwave absorption performance of the material. A large number of Schottky heterojunctions are generated between the metal Ni and the semiconductor Ni2P, which is beneficial to the improvement of polarization loss due to the formation of internal dipole electric field by the Schottky barrier, and the electromagnetic energy is converted into heat energy through interface polarization.

[0069] 2、The hollow structure of the Ni / Ni2P / CNs composite material of the application promotes impedance matching, and phosphating improves the wave absorption performance. Under a filler content of 20 wt%, the minimum reflection loss of the Ni / Ni2P / CNs composite material is-72.1 dB, and the effective bandwidth is 5.8 GHz. The results show that the Ni / Ni2P / CNs composite material has great potential to become a high-performance electromagnetic microwave absorption material, and the construction of the Schottky heterojunction also provides a reference for the research of deep electromagnetic wave loss mechanism.

[0070] It should be noted that, in this paper, relational terms such as first and second are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "contain" or any other variants thereof are intended to cover non-exclusive inclusion, so that the process, method, article or equipment including a series of elements not only includes those elements, but also includes other elements not explicitly listed or inherent to such process, method, article or equipment. Without more limitations, the element defined by the statement "including a" does not exclude the presence of additional identical elements in the process, method, article or equipment including the element.

[0071] The above examples are only used to illustrate the technical solutions of the application, but not to limit it; although the application has been described in detail with reference to the foregoing examples, those skilled in the art should understand that they can still modify the technical solutions recorded in the foregoing examples, or make equivalent replacement for part of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the application.

Claims

1. A method for preparing MOFs derived hollow nickel phosphide-based carbon nanocomposite material, characterized in that, The MOFs derived hollow phosphatized nickel-based carbon nanocomposite material mainly uses a nickel-based material as a metal source, uses MOFs as a metal-organic framework, synthesizes a Ni / CNs intermediate, and then performs phosphatization treatment on the Ni / CNs intermediate to obtain the hollow Ni / Ni2P / CNs; The prepared hollow Ni / Ni2P / CNs is an electromagnetic microwave absorption material; The preparation method specifically includes the following steps: S1. Preparation of the hollow Ni / CNs The hollow Ni-MOF precursor is weighed, annealed under a nitrogen atmosphere, and then the hollow Ni / CNs is prepared; S2. Preparation of the hollow Ni / Ni2P / CNs The hollow Ni / CNs is weighed in a porcelain boat and placed downstream of a tube furnace, NaH2PO2·H2O is weighed in a porcelain boat and placed upstream of the tube furnace, and then the final product Ni / Ni2P / CNs is prepared after high-temperature annealing under a nitrogen flow; The content of NaH2PO2·H2O is 500 mg-1500 mg. The high-temperature annealing temperature is 700-900℃.

2. The method for preparing MOFs derived hollow nickel phosphide-based carbon nanocomposite material according to claim 1, characterized in that, The high-temperature annealing in the S1 and the S2 is specifically operated as follows: the temperature is increased to 700-900℃ at a rate of 2℃ / min from room temperature, and then the temperature is decreased to room temperature after 2h of holding.

3. The method for preparing MOFs derived hollow nickel phosphide-based carbon nanocomposite material according to claim 2, wherein, The high-temperature annealing temperature is preferably 800℃.

4. The method for preparing MOFs derived hollow nickel phosphide-based carbon nanocomposite of claim 1, wherein, The preparation method of the hollow Ni-MOF precursor in the S1 is as follows: using nickel nitrate as a metal source, using trimesic acid as an organic ligand, using DMF and water as solvents, and using polyvinylpyrrolidone (PVP) as a stabilizer to react to generate the hollow Ni-MOF precursor.

5. The method of producing MOFs-derived hollow nickel phosphide-based carbon nanocomposite of claim 4, wherein, The specific method for synthesizing the hollow Ni-MOF precursor is as follows: nickel nitrate, trimesic acid, and polyvinylpyrrolidone are stirred in a mixed solvent of DMF and water for 30-40min, then kept at 140-160℃ for 8-16h, cooled to room temperature, and then centrifuged to obtain green precipitate, which is the hollow Ni-MOF precursor.

6. The method of producing MOFs derived hollow nickel phosphide-based carbon nanocomposite of claim 4, wherein, The volume ratio of the DMF to water is (1-5):

1.

7. The MOFs derived hollow phosphatized nickel-based carbon nanocomposite material of claim 1 or the preparation method of the MOFs derived hollow phosphatized nickel-based carbon nanocomposite material of any one of claims 2-6 is applied to the field of electromagnetic microwave absorption.

Images