CN111629575A - MXene-based nano composite wave-absorbing material and preparation method thereof - Google Patents
MXene-based nano composite wave-absorbing material and preparation method thereof Download PDFInfo
- Publication number
- CN111629575A CN111629575A CN202010302281.1A CN202010302281A CN111629575A CN 111629575 A CN111629575 A CN 111629575A CN 202010302281 A CN202010302281 A CN 202010302281A CN 111629575 A CN111629575 A CN 111629575A
- Authority
- CN
- China
- Prior art keywords
- mxene
- metal salt
- absorbing material
- wave
- nano composite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/081—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing particle radiation or gamma-radiation
- B01J19/082—Gamma-radiation only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/081—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing particle radiation or gamma-radiation
- B01J19/085—Electron beams only
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Electromagnetism (AREA)
- Plasma & Fusion (AREA)
- Hard Magnetic Materials (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
- Soft Magnetic Materials (AREA)
Abstract
The invention discloses a preparation method of an MXene-based nano composite wave-absorbing material, which comprises the following steps: mixing MXene prepared by an etching method with metal salt, pretreating, irradiating the pretreated mixed solution, and performing post-treatment to obtain the MXene-based nano composite wave-absorbing material. The preparation method provided by the invention is simple, low in preparation cost, high in practicability and small in environmental pollution in the preparation process, and the magnetic nanoparticles are introduced to be uniformly loaded on the surface of the MXene material, so that the impedance matching property of the composite material is improved, and the MXene-based nano composite wave-absorbing material has excellent wave-absorbing performance.
Description
Technical Field
The invention relates to a wave-absorbing material, in particular to a preparation method of an MXene-based nano composite wave-absorbing material.
Background
MXene is a class of two-dimensional inorganic compounds consisting of a transition metal carbide, nitride or carbonitride of several atomic layer thicknesses. It is usually obtained by removing the mesophase of the MAX phase ceramic. MAX phase refers to Mn+1AXn(n ═ 1, 2 or 3), wherein M denotes a transition metal, A denotes a group III or IV element (mainly Al, Ga, In, Ti, Si, Ge, Sn, Pb), and X denotes carbon, nitrogen or carbon-nitrogen. Since n can be 1, 2, 3, the corresponding structure is M2X，M3X2Or M4X3The thickness of the two-dimensional sheet layer is 3 layers, 5 layers and 7 layers, only MXene with oxygen, hydrogen and fluorine as ends exists in nature, pure MXene cannot exist, MXene has good hydrophilicity and dispersibility due to various functional groups on the surface, can be stably fused with various organic solvents in aqueous solution, and MXene material also has a special two-dimensional layered structure and ultrahigh conductivity (the conductivity can reach 7.3 × 10)4S/m), can be widely applied to the wave-absorbing field.
The absorption of MXene to electromagnetic wave is mainly through the effect of dielectric loss, and in order to enhance the wave absorbing performance, MXene is often compounded with other magnetic materials (such as iron and nickel) to improve the magnetic permeability and impedance matching characteristic of the materials. The preparation method comprises a chemical reduction method, a hydrothermal method, an electrodeposition method and the like.
Compared with the method, the high-energy radiation (comprising high-energy electron beams and gamma rays) has the advantages that (1) solvated electrons have very high reduction potential (-2.9V), the use of toxic reducing agents (such as hydrazine and sodium borohydride) is avoided, and the method is environment-friendly; (2) the operation is simple, and the industrialization is convenient to realize; (3) the irradiation process can be carried out at room temperature, and the energy consumption is low; (4) the radiation processing technology condition is controllable, and products with different structures and performances can be synthesized easily by adjusting the irradiation condition. But no report on the preparation of MXene-based nano composite wave-absorbing material by radiation technology exists at present.
Disclosure of Invention
Based on the technical background, the inventor of the invention has made a keen effort, and as a result, the MXene-based nano composite wave-absorbing material prepared by using MXene and a metal salt through an irradiation method has the advantages of simple preparation method, low preparation cost, high practicability, small environmental pollution in the preparation process, uniform loading of the introduced magnetic material on the surface of the MXene material, and excellent wave-absorbing performance of the MXene-based nano composite wave-absorbing material, thereby completing the invention.
The first aspect of the invention provides a preparation method of an MXene-based nano composite wave-absorbing material, which is prepared from MXene and metal salt by an irradiation method;
the metal salt is selected from one or more of organic salt and inorganic salt containing iron, cobalt and nickel; the mass ratio of the metal salt to MXene is (15-20): 1.
The second aspect of the invention provides a preparation method of an MXene-based nano composite wave-absorbing material, which comprises the following steps:
step 1, etching MAX phase to obtain MXene;
step 3, irradiating the pretreated mixture;
and 4, finally, carrying out post-treatment to obtain the MXene-based nano composite wave-absorbing material.
The preparation method provided by the invention and the product prepared by the method have the following advantages:
(1) the preparation method of the MXene-based nano composite wave-absorbing material adopts an irradiation technology, and has the advantages of simple method, low preparation cost, high practicability and high preparation efficiency;
(2) the MXene-based nano composite wave-absorbing material is an organic combination of a magnetic material and MXene, so that on one hand, the introduction of the magnetic material endows the material with high magnetic conductivity, and the improvement of the impedance matching characteristic of the composite material is facilitated; on the other hand, the load of the magnetic material and the formation of a small number of structural defects of MXene in the irradiation process effectively reduce the conductivity and the dielectric constant of the composite material, and further improve the impedance matching characteristic of the material. All the materials show excellent wave-absorbing characteristics.
Drawings
FIG. 1 shows that MXene-Ni wave-absorbing material and Ti are prepared3AlC2And XRD spectrum of MXene;
fig. 2 shows a transmission electron micrograph of MXene;
FIG. 3 shows a transmission electron microscope photograph of the prepared MXene-Ni wave-absorbing material;
fig. 4 shows a graph of the reflection loss of the prepared MXene-Ni wave-absorbing material and the frequency change.
Detailed Description
The present invention will be described in detail below, and features and advantages of the present invention will become more apparent and apparent with reference to the following description.
The invention provides a preparation method of an MXene-based nano composite wave-absorbing material, which is prepared from MXene and metal salt by an irradiation method, wherein the MXene is prepared by etching MAX phase.
The MAX phase is a new processable ceramic material of great interest (preparation, structure and performance of MAX phase are detailed (zheng yali, zhou yan chun, von shihai, preparation, structure, performance and development trend of MAX phase ceramics, aerospace materials technology, 2013, 6 th, pages 1-23)). In the present invention, the MAX phase is preferably Ti3AlC2。Ti3AlC2Is M(n+1)AXnOne of the most representative materials in the type ternary compound, Ti3AlC2Having both the characteristics of metal and ceramic, Ti3AlC2CrystalThe atomic bond in the structure comprises three bond types of metallic bond, covalent bond and ionic bond, Ti3AlC2The ceramic characteristics are mainly due to the combined action of ionic bonds and covalent bonds, such as high yield strength, oxidation resistance, high modulus, high melting point and the like, while the metallic bonds are Ti3AlC2Exhibit good metal characteristics such as high electrical conductivity, high elastic modulus, high shear modulus, and machinability, etc., and are useful in the present invention due to their unique physical properties as described above. However, since MXene itself is nonmagnetic, it is necessary to introduce a magnetic material into MXene to obtain a material having excellent wave absorption properties.
MXene materials are a class of metal carbide and metal nitride materials with a two-dimensional layered structure that resemble a chip of potato stacked on top of one another.
In the invention, the special structure of MXene material is utilized, and magnetic substance is introduced into the special structure to prepare the MXene-based nano composite wave-absorbing material, so that the MXene-based nano composite wave-absorbing material has the excellent dielectric loss characteristic of MXene and the magnetic loss of the magnetic substance. Preferably MXene is Ti3C2。
In the invention, the metal salt is selected from one or more of organic salt and inorganic salt containing iron, cobalt and nickel; preferably, the metal salt is selected from one or more of organic salt and inorganic salt containing nickel; more preferably, the magnetic material is (CH)3COO)2Ni·4H2O。
The adding mass ratio of the metal salt to MXene is (15-20): 1, preferably the adding mass ratio of the metal salt to MXene is (16-19): 1, and more preferably the adding mass ratio of the metal salt to MXene is (17-18): 1.
The MXene-based nano composite wave-absorbing material prepared by the invention has the advantages that the magnetic material is uniformly loaded on the surface of MXene, the maximum value of the reflection loss of a sample of the MXene-based nano composite wave-absorbing material is-28 dB, and the absorption bandwidth is 2.65 GHz.
The Mxene wave-absorbing composite material is prepared by the method comprising the following steps:
step 1, etching MAX phase to obtain MXene;
step 3, irradiating the pretreated mixture;
and 4, finally, carrying out post-treatment to obtain the MXene-based nano composite wave-absorbing material.
The Mxene is prepared from MAX through an etching method;
the etching agent is LiF/HCl composite solvent;
the mass ratio of MAX to LiF is 3: (5-10), preferably, the mass ratio of MAX to LiF is 3: (7-9), more preferably, the mass ratio of MAX to LiF is 3: 8.
the etching reaction temperature is 30-50 ℃, preferably 35-45 ℃, and more preferably 40 ℃.
The irradiation dose is 40-60 kGy, preferably 45-55 kGy, and more preferably 50 kGy; the irradiation dose rate is 140-180 Gy/min, preferably 150-170 Gy/min, and more preferably 160 Gy/min.
The post-treatment comprises washing, suction filtration and freeze drying.
The second aspect of the invention provides a preparation method of an MXene-based nano composite wave-absorbing material, which comprises the following steps:
step 1, etching MAX phase to obtain MXene;
step 3, irradiating the pretreated mixture;
and 4, finally, carrying out post-treatment to obtain the MXene-based nano composite wave-absorbing material.
Step 1, etching the MAX phase to obtain MXene.
Currently, there are three main methods for preparing MXene, including solution method (immediate etching method), high-temperature fluoride melting method and bottom-up synthesis method. The high-temperature fluoride melting method is to mix MAX phase with metal salt containing fluorine, then introduce inert gas, and generate MXene through high-temperature heating reaction. The bottom-up synthesis method mainly utilizes Chemical Vapor Deposition (CVD) to generate a large-area continuous MXene thin film. Compared with the etching method, the two methods have the defects of high preparation cost, low practicability and immature synthesis process.
In the present invention, the MAX phase is Ti3AIC2MXene is Ti3C2。
In the invention, MXene is prepared by adopting an etching method, and HF and NH are usually adopted in the etching preparation method of MXene4HF2Or LiF/HCl composite solvent as etching agent, but HF has high danger and is difficult to store, while NH4HF2Has high toxicity, is easy to decompose toxic fluoride, nitrogen oxide and ammonia gas in hot water, and has very harsh experimental synthesis conditions.
Therefore, in the invention, LiF/HCl composite solvent is preferably used as the etching agent, which has the advantages of mild synthesis process, small environmental pollution and the like.
LiF and HCl are firstly put into a reactor, and then MAX phase is slowly added into the reactor, wherein the dosage of the hydrochloric acid is not limited.
The mass ratio of the MAX phase to the LiF is 3: (5-10), preferably, the mass ratio of the MAX phase to the LiF is 3: (7-9), more preferably, the mass ratio of the MAX phase to the LiF is 3: 8.
and putting the reactor which is weighed and added with the MAX phase and the LiF/HCl composite solvent into an oil bath pot for oil bath heating, and carrying out magnetic stirring in the reaction process, so that the etching effect of the MAX phase is better.
The etching reaction temperature is 30-50 ℃, preferably 35-45 ℃, and more preferably 40 ℃.
The magnetic stirring time is 40-55 h, preferably 45-50 h, and more preferably 48 h.
And taking the sample after the etching reaction is finished out of the reactor, and washing for multiple times, preferably centrifugal washing, wherein the centrifugal washing is mainly used for removing impurities. And (3) carrying out ultrasonic stripping on the sample from which the impurities are removed, then centrifuging, and taking supernatant fluid to obtain the small-layer MXene.
Filling inert gas into the MXene aqueous solution for refrigeration and preservation for subsequent use.
And 2, mixing and pretreating the metal salt and the prepared MXene.
MXene materials are a class of metal carbide and metal nitride materials with a two-dimensional layered structure, and the structure is similar to an accordion. But the MXene composite material has no magnetic property, in the invention, the special structure of the MXene material is utilized, and the magnetic substance is introduced into the MXene material to endow the composite material with magnetic loss characteristic, improve the impedance matching characteristic and enable the MXene material to have excellent wave absorbing performance.
The metal salt is dissolved in deionized water and then mixed with the MXene aqueous solution.
The metal salt is selected from one or more of organic salt and inorganic salt containing iron, cobalt and nickel; preferably, the metal salt is selected from one or more of organic salt and inorganic salt containing nickel; more preferably, the metal salt is (CH)3COO)2Ni·4H2O。
The metal salt is dissolved in deionized water, and the amount of the deionized water is not particularly limited as long as the metal salt can be completely dissolved.
In order to better dissolve the metal salt in the deionized water, the aqueous solution to which the metal salt is added is stirred, preferably ultrasonically stirred, the time of the ultrasonic stirring is not particularly limited as long as the metal salt is completely dissolved, and the time of the ultrasonic stirring is preferably 1 min.
The aqueous solution of metal salt and the aqueous solution of MXene are mixed, and ultrasonic dispersion is preferable for more uniform dispersion of MXene and metal salt. The ultrasonic dispersion time is likewise not limited.
The adding mass ratio of the metal salt to MXene is (15-20): 1, preferably the adding mass ratio of the metal salt to MXene is (16-19): 1, and more preferably the adding mass ratio of the metal salt to MXene is (17-18): 1. If the added metal salt is too little, the metal salt introduced into the MXene surface is less, the wave absorbing performance of the finally prepared MXene-based nano composite wave absorbing material is not greatly improved, if the added metal salt is too much, the metal salt can be gathered on the MXene surface, and the wave absorbing performance of the finally prepared MXene-based nano composite wave absorbing material is also not greatly improved.
After ultrasonic dispersion, dropwise adding alkali solution to adjustThe pH value is between 9 and 10 so as to avoid solvation electrons generated by irradiation in a solvent system from being H+While the pH is not too high, otherwise Ni will be caused2+With OH-Combined formation of Ni (OH)2And (4) precipitating.
Subsequently, an oxidative radical scavenger is added to the solution to avoid oxidative radicals generated by irradiation in the solvent system from affecting the Ni2+In the present invention, the oxidizing radical scavenger is selected from one or two of isopropyl alcohol and ethanol; the oxidizing radical scavenger is preferably isopropanol, more preferably isopropanol at a concentration of 2 mol/L.
And dispersing the mixed solution, preferably performing ultrasonic dispersion, wherein the ultrasonic dispersion time is 20-40 min, preferably 30 min. The dispersion of the mixed solution is preferably carried out by placing a beaker containing the mixed solution in an ice-water mixture so as to avoid MXene from being oxidized in the air and influencing the performance of the finally prepared product.
And 3, carrying out irradiation reaction on the pretreated mixture.
And (3) moving the mixed liquid subjected to ultrasonic dispersion in the step (2) into an irradiation tube, and introducing nitrogen into the irradiation tube into which the mixed liquid is moved before the irradiation reaction, so as to discharge air in the irradiation tube, thereby avoiding influencing subsequent irradiation reaction, influencing the reduction degree of magnetic ions and influencing the performance of the finally prepared product. After the nitrogen gas was introduced, the irradiation tube was sealed.
The time for introducing the nitrogen is 25-35 min, and only other air in the irradiation tube needs to be exhausted, so that other side reactions are prevented from being generated in the irradiation reaction, and the performance of the finally prepared product is influenced. The nitrogen gas is preferably introduced for 30 min.
In the invention, the irradiation reaction is carried out in a cobalt source chamber, and the irradiation dose is 40-60 kGy, preferably 45-55 kGy, and more preferably 50 kGy. Too high irradiation dose rate and dose can cause too much loaded magnetic particles and too large size to generate agglomeration, and too low irradiation dose rate and dose can cause too low loaded magnetic particles and too small size, thereby causing the material to have poor impedance matching and wave absorption characteristics due to low magnetic permeability.
The irradiation dose rate is 140-180 Gy/min, preferably 150-170 Gy/min, and more preferably 160 Gy/min.
And 4, finally, carrying out post-treatment to obtain the MXene-based nano composite wave-absorbing material.
The post-treatment includes washing, suction filtration and freeze drying, and the washing is preferably carried out with deionized water, mainly for the purpose of removing unreacted substances.
And (3) carrying out suction filtration on the cleaned sample, dispersing the filter cake after suction filtration in deionized water, wherein the deionized water is used only for dispersing the filter cake.
And then freeze-drying the filter cake dispersed in the deionized water to finally obtain a powder sample, namely the MXene-based nano composite wave-absorbing material.
The freeze drying time is 40-55 h, preferably 48 h.
The MXene-based nano composite wave-absorbing material prepared by the preparation method can be applied to radar stealth of airplanes, tanks, ships and missiles and can also be applied to electromagnetic shielding of electronic elements in communication, electronic and other equipment.
The invention has the following beneficial effects:
(1) the preparation method of the MXene-based nano composite wave-absorbing material adopts a radiation technology, and has the advantages of simple method, high efficiency, low requirement on equipment, low preparation cost, high practicability, low environmental pollution and low risk;
(2) the MXene-based nano composite wave-absorbing material disclosed by the invention organically combines a magnetic material and MXene, so that on one hand, the introduction of the magnetic material endows the material with high magnetic conductivity, and the improvement of the impedance matching characteristic of the composite material is facilitated; on the other hand, the load of the magnetic material and the formation of a small number of structural defects of MXene in the irradiation process effectively reduce the conductivity and the dielectric constant of the composite material, and further improve the impedance matching characteristic of the material. All the materials show excellent wave-absorbing characteristics.
(3) The invention realizes the uniform distribution of the magnetic material on MXene by the accurate control of the radiation condition, and avoids the agglomeration phenomenon.
(4) The MXene-based nano composite wave-absorbing material sample has the maximum value of reflection loss of-28 dB and the absorption bandwidth of 2.65GHz, and can achieve excellent wave-absorbing performance under the condition of lower thickness, so that the material has bright application prospect in the field of stealth coatings.
Examples
The invention is further illustrated by the following specific examples, which are intended to be illustrative only and not limiting to the scope of the invention.
Example 1
4g LiF and 50mL concentrated HCl were placed in a reactor, and 1.5g Ti was slowly added3AIC2The reactor was placed in a 40 ℃ oil bath and reacted for 48h with magnetic stirring. Taking out the sample, centrifuging and washing with deionized water for 3 times to remove impurities, ultrasonically stripping, centrifuging again, and collecting supernatant to obtain Ti with less layer3C2。
Example 2
4g LiF and 50mL concentrated HCl were placed in a reactor, and 1.5g Ti was slowly added3AIC2The reactor was placed in a 40 ℃ oil bath and reacted for 48h with magnetic stirring. Taking out the sample, centrifuging and washing with deionized water for 3 times to remove impurities, ultrasonically stripping, centrifuging again, and collecting supernatant to obtain Ti with less layer3C2. Mixing Ti3C2Filling inert gas into the aqueous solution, and refrigerating for storage.
Dissolving 3.5g nickel acetate in 42mL deionized water, ultrasonically stirring for 1min, adding 17mL Ti with concentration of 11.7mg/mL3C2Ultrasonic treatment for 1min to obtain Ti3C2And nickel acetate are uniformly dispersed. And (3) dropwise adding ammonia water to adjust the pH value to be 9-10, adding isopropanol of which the oxidizing free radical scavenger is 2mol/L, ultrasonically treating a beaker containing the mixed solution in an ice-water mixture for 30min, transferring the ultrasonically dispersed liquid into an irradiation tube, introducing nitrogen for 30min, sealing, and placing the irradiation tube in a cobalt source chamber for irradiation. The irradiation dose is 50kGy, and the irradiation dose rate is 160 Gy/min.
The irradiated sample was washed 3 times with deionized water to remove unreacted materials. Dispersing the filter cake obtained by the third suction filtration in 100mL of deionized water, and freeze-drying for 48h to obtain a powder sample, which is recorded as Ti3C2-Ni。
Examples of the experiments
Experimental example 1X-ray diffraction Pattern analysis
For Ti3AlC2、Ti3C2And the produced Ti3C2XRD performance test is carried out on the-Ni wave-absorbing material, and the result is shown in figure 1.
As can be seen from FIG. 1, with Ti3AlC2Comparison of spectra, Ti3C2The characteristic absorption peak of medium Al disappears, and it can be seen that Ti is present3C2The (002) peak in the spectrum was shifted to a small angle, indicating successful etching. Comparative Ti3C2With Ti3C2Spectrum of-Ni at Ti3C2In the spectrum of-Ni, Ni and Ni (OH) can be clearly observed2The characteristic peaks of (A) prove that Ni and Ni (OH)2Has been loaded to Ti3C2The above.
Experimental example 2 Transmission Electron microscopy test
Respectively to Ti3C2And the produced Ti3C2The transmission electron microscope test of the-Ni wave-absorbing material is respectively shown in the figure 2 and the figure 3.
As can be seen from FIG. 2, Ti3C2Is a flat sheet, and it can be seen from FIG. 3 that particulate matter is supported on Ti after modification3C2The surface is uniform in distribution, and the agglomeration phenomenon is avoided. And from the above XRD analysis, it can be seen that the Ti is loaded3C2The surface material should be Ni and Ni (OH)2。
Experimental example 3 wave-absorbing Property test
The obtained Ti3C2-Ni material mixed with paraffin wax in a mass ratio of 17:50 for Ti of different thicknesses3C2the-Ni material is subjected to a wave absorbing performance test, and the test result is shown in FIG. 4.
As can be seen from FIG. 4, when the reflection loss value of the material is less than-10 dB, the absorption rate of the material to electromagnetic waves is greater than 90%, and the use requirement of the wave-absorbing material is met. When the thickness of the sample is 1.43mm, the reflection loss value is-28 dB, and the width of the absorption band is 2.65GHz, which shows that the wave-absorbing material prepared by the invention can achieve excellent wave-absorbing performance under the condition of lower thickness. The thickness and weight of the coating are closely related, and in some military applications, the thinner the thickness of the coating is, the better the coating thickness is on the premise of keeping certain wave absorption performance in order to reduce the weight of the coating and increase the loading capacity as much as possible. The material has bright application prospect in the field of stealth coatings.
The invention has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to be construed in a limiting sense. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, which fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
Claims (10)
1. The MXene-based nano composite wave-absorbing material is characterized in that the wave-absorbing composite material is prepared by MXene and metal salt through an irradiation method, and the MXene is prepared by etching MAX phase.
2. The MXene-based nanocomposite wave-absorbing material of claim 1, characterized in that,
the metal salt is selected from one or more of organic salt and inorganic salt containing iron, cobalt and nickel;
the mass ratio of the metal salt to MXene is (15-20): 1.
3. The MXene-based nanocomposite wave-absorbing material of claim 1, characterized in that,
the metal salt is selected from one or more of organic salt and inorganic salt containing nickel;
the addition mass ratio of the metal salt to MXene is (16-19): 1.
4. The MXene-based nanocomposite wave-absorbing material of claim 1, characterized in that,
the magnetic material is loaded on the surface of MXene, the maximum value of the reflection loss of the MXene-based nano composite wave-absorbing material sample is-28 dB, and the absorption bandwidth is 2.65 GHz.
5. The MXene-based nanocomposite wave-absorbing material of claim 1, prepared by a method comprising the steps of:
step 1, etching MAX phase to obtain MXene;
step 2, mixing and pretreating metal salt and the prepared MXene;
step 3, irradiating the pretreated mixture;
and 4, finally, carrying out post-treatment to obtain the MXene-based nano composite wave-absorbing material.
6. A preparation method of an MXene-based nano composite wave-absorbing material comprises the following steps:
step 1, etching MAX phase to obtain MXene;
step 2, mixing and pretreating metal salt and the prepared MXene;
step 3, irradiating the pretreated mixture;
and 4, finally, carrying out post-treatment to obtain the MXene-based nano composite wave-absorbing material.
7. The production method according to claim 6, wherein, in step 1,
the MAX phase is etched by adopting concentrated HCl and LiF, and the mass ratio of the MAX phase to the LiF is 3: (5-10);
the etching temperature is 30-50 ℃;
the etching is carried out under magnetic stirring, and the stirring time is 40-55 h;
and centrifugally washing, ultrasonically stripping and centrifuging the etched product to obtain MXene.
8. The production method according to claim 6, wherein, in step 2,
prior to mixing, dissolving the metal salt in deionized water, the dissolving being carried out with stirring;
mixing an aqueous metal salt solution and an aqueous MXene solution, the mixing being carried out under ultrasound;
the addition mass ratio of the metal salt to MXene is (15-20) to 1;
the pretreatment comprises the steps of dropwise adding ammonia water into a mixed solution of metal salt and MXene, and adjusting the pH value to 9-10;
adding an oxidizing free radical scavenger, preferably isopropanol, thereto; the mixture is then subjected to ultrasonic dispersion, preferably in an ice-water mixture.
9. The production method according to claim 6, wherein, in step 3,
transferring the mixture dispersed in the step 2 into an irradiation tube, introducing nitrogen into the irradiation tube, and sealing;
the irradiation reaction is carried out in a cobalt source chamber, and the irradiation dose is 40-60 kGy, preferably 45-55 kGy, and more preferably 50 kGy;
the irradiation dose rate is 140-180 Gy/min, preferably 150-170 Gy/min, and more preferably 160 Gy/min.
10. The production method according to claim 6, wherein, in step 4,
the post-treatment comprises cleaning, suction filtration and freeze drying, and the cleaning is carried out by using deionized water;
the freeze drying time is 40-55 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010302281.1A CN111629575B (en) | 2020-04-16 | 2020-04-16 | Preparation method of MXene-based nano composite wave-absorbing material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010302281.1A CN111629575B (en) | 2020-04-16 | 2020-04-16 | Preparation method of MXene-based nano composite wave-absorbing material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111629575A true CN111629575A (en) | 2020-09-04 |
| CN111629575B CN111629575B (en) | 2022-11-11 |
Family
ID=72260636
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010302281.1A Active CN111629575B (en) | 2020-04-16 | 2020-04-16 | Preparation method of MXene-based nano composite wave-absorbing material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111629575B (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113316379A (en) * | 2021-05-26 | 2021-08-27 | 湖南工程学院 | Nano composite structure wave absorber material, preparation method and application |
| CN113316378A (en) * | 2021-04-21 | 2021-08-27 | 东南大学 | MoS2/MXene composite aerogel wave-absorbing material and preparation method thereof |
| CN113840529A (en) * | 2021-11-02 | 2021-12-24 | 浙江优可丽新材料有限公司 | NiCo2O4@ agaric carbon aerogel composite material and preparation method and application thereof |
| CN114058328A (en) * | 2021-08-27 | 2022-02-18 | 东华大学 | Wave-absorbing composite material and preparation method thereof |
| CN114423269A (en) * | 2022-01-24 | 2022-04-29 | 同济大学 | Nitrogen-doped MXene @ HCF electromagnetic composite wave-absorbing material and preparation method thereof |
| CN114471646A (en) * | 2021-12-22 | 2022-05-13 | 湘潭大学 | Preparation method and application of single-atom iron-series metal loaded on surface of titanium carbide |
| CN114906850A (en) * | 2022-06-24 | 2022-08-16 | 湖南大学 | Method for improving stability of MXene aqueous solution |
| WO2022259775A1 (en) * | 2021-06-10 | 2022-12-15 | 株式会社村田製作所 | Magnetic material, electromagnetic component, and method for manufacturing magnetic material |
| CN116446177A (en) * | 2023-03-15 | 2023-07-18 | 天津工业大学 | Preparation method of MXene/metal nanoparticle multifunctional coating composite material |
| CN117641872A (en) * | 2023-11-27 | 2024-03-01 | 山东省地质科学研究院 | Hollow manganese dioxide nanotube loaded MXene material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105854913A (en) * | 2016-04-07 | 2016-08-17 | 河南理工大学 | Two-dimension carbide loaded metal simple substance nano-powder, and preparation method and application thereof |
| CN108751995A (en) * | 2018-07-10 | 2018-11-06 | 中国科学院宁波材料技术与工程研究所 | Nanoparticle in-stiu coating MXenes composite materials, its preparation method and purposes |
| CN110124529A (en) * | 2019-05-28 | 2019-08-16 | 北京理工大学 | A kind of preparation method and application of graphene oxide/MXene composite membrane |
| CN110499142A (en) * | 2019-09-25 | 2019-11-26 | 深圳大学 | A kind of high-efficiency shielding electromagnetic interference MXene/ metal ion composite material and preparation method |
-
2020
- 2020-04-16 CN CN202010302281.1A patent/CN111629575B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105854913A (en) * | 2016-04-07 | 2016-08-17 | 河南理工大学 | Two-dimension carbide loaded metal simple substance nano-powder, and preparation method and application thereof |
| CN108751995A (en) * | 2018-07-10 | 2018-11-06 | 中国科学院宁波材料技术与工程研究所 | Nanoparticle in-stiu coating MXenes composite materials, its preparation method and purposes |
| CN110124529A (en) * | 2019-05-28 | 2019-08-16 | 北京理工大学 | A kind of preparation method and application of graphene oxide/MXene composite membrane |
| CN110499142A (en) * | 2019-09-25 | 2019-11-26 | 深圳大学 | A kind of high-efficiency shielding electromagnetic interference MXene/ metal ion composite material and preparation method |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113316378A (en) * | 2021-04-21 | 2021-08-27 | 东南大学 | MoS2/MXene composite aerogel wave-absorbing material and preparation method thereof |
| CN113316378B (en) * | 2021-04-21 | 2023-03-10 | 东南大学 | MoS 2 /MXene composite aerogel wave-absorbing material and preparation method thereof |
| CN113316379B (en) * | 2021-05-26 | 2022-09-02 | 湖南工程学院 | Nano composite structure wave absorber material, preparation method and application |
| CN113316379A (en) * | 2021-05-26 | 2021-08-27 | 湖南工程学院 | Nano composite structure wave absorber material, preparation method and application |
| WO2022259775A1 (en) * | 2021-06-10 | 2022-12-15 | 株式会社村田製作所 | Magnetic material, electromagnetic component, and method for manufacturing magnetic material |
| CN114058328A (en) * | 2021-08-27 | 2022-02-18 | 东华大学 | Wave-absorbing composite material and preparation method thereof |
| CN113840529A (en) * | 2021-11-02 | 2021-12-24 | 浙江优可丽新材料有限公司 | NiCo2O4@ agaric carbon aerogel composite material and preparation method and application thereof |
| CN114471646A (en) * | 2021-12-22 | 2022-05-13 | 湘潭大学 | Preparation method and application of single-atom iron-series metal loaded on surface of titanium carbide |
| CN114423269A (en) * | 2022-01-24 | 2022-04-29 | 同济大学 | Nitrogen-doped MXene @ HCF electromagnetic composite wave-absorbing material and preparation method thereof |
| CN114906850A (en) * | 2022-06-24 | 2022-08-16 | 湖南大学 | Method for improving stability of MXene aqueous solution |
| CN114906850B (en) * | 2022-06-24 | 2024-01-30 | 湖南大学 | Method for improving stability of MXene aqueous solution |
| CN116446177A (en) * | 2023-03-15 | 2023-07-18 | 天津工业大学 | Preparation method of MXene/metal nanoparticle multifunctional coating composite material |
| CN116446177B (en) * | 2023-03-15 | 2024-05-28 | 天津工业大学 | Preparation method of MXene/metal nanoparticle multifunctional coating composite material |
| CN117641872A (en) * | 2023-11-27 | 2024-03-01 | 山东省地质科学研究院 | Hollow manganese dioxide nanotube loaded MXene material and preparation method thereof |
| CN117641872B (en) * | 2023-11-27 | 2024-06-11 | 山东省地质科学研究院 | Hollow manganese dioxide nanotube loaded MXene material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111629575B (en) | 2022-11-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111629575B (en) | Preparation method of MXene-based nano composite wave-absorbing material | |
| CN109712769B (en) | MXene-magnetic metal composite material and preparation method thereof | |
| US20220274844A1 (en) | Core-shell structure type wave absorbing material, preparation method therefor, and application | |
| CN112251193A (en) | Composite wave-absorbing material based on MXene and metal organic framework and preparation method and application thereof | |
| CN112375541B (en) | Nitrogen-doped graphene nickel ferrite composite wave-absorbing material and preparation method thereof | |
| CN108587159A (en) | One type graphene carbonitride/ferroso-ferric oxide/polyaniline nano composite wave-suction material and preparation method thereof | |
| CN110041885A (en) | A kind of preparation method of redox graphene/stannic oxide nanometer composite wave-suction material | |
| CN115491177B (en) | MOF-derived carbon-based magnetic nano composite electromagnetic wave absorbing material and preparation method thereof | |
| CN101521046B (en) | Graphite sheet surface load magnetic alloy particle wave-absorbing material and preparation method thereof | |
| CN112225950B (en) | Preparation method of environment-friendly Fe @ C composite wave-absorbing material | |
| CN113816620B (en) | Dielectric fiber composite wave-absorbing material coated with molybdenum disulfide/iron-cobalt alloy/carbon on surface and preparation method thereof | |
| CN115092910A (en) | Method for preparing MXene-graphite ring stacked carbon nanotubes by low-temperature vacuum CVD (chemical vapor deposition) | |
| CN113438883B (en) | Preparation method and application of binary heterostructure wave-absorbing material molybdenum oxide-molybdenum phosphide | |
| CN114520419A (en) | Preparation method of cobalt-based metal organic framework derivative wave absorbing agent with nano composite structure | |
| CN112939083A (en) | Molybdenum disulfide/ferroferric oxide/graphene nanosheet composite wave absorber and preparation method thereof | |
| CN112980389A (en) | Preparation method of functionalized graphene wave-absorbing material | |
| CN111234776A (en) | Solid Fe3O4@ C superstructure microsphere wave-absorbing material and preparation method and application thereof | |
| CN114479762B (en) | Magnetic metal/metal oxide/carbon nanocomposite material, preparation method and application thereof | |
| CN113423255B (en) | Core-shell structure Ti 4 O 7 Magnetic metal composite absorbent and preparation method thereof | |
| CN113708085B (en) | Preparation method of nano porous carbon coated magnetic nanoparticle compound | |
| CN114614272A (en) | MXene/Co/C composite wave-absorbing material derived from MOF and preparation method thereof | |
| CN114073919B (en) | Carbon-magnetic metal dispersion type hollow composite microsphere and preparation method and application thereof | |
| CN117229756B (en) | Preparation method of MXene-based nano composite wave-absorbing material with adjustable interlayer spacing | |
| CN112280533A (en) | Preparation method of ternary composite wave-absorbing material with hollow structure | |
| CN108165008A (en) | 1,1- diacetyl ferrocene chirality polyShiff bases salt/graphene composite wave-suction material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |