CN114736431A - MXene/nickel nanowire conductive filler and preparation method and application thereof - Google Patents

MXene/nickel nanowire conductive filler and preparation method and application thereof Download PDF

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CN114736431A
CN114736431A CN202210373625.7A CN202210373625A CN114736431A CN 114736431 A CN114736431 A CN 114736431A CN 202210373625 A CN202210373625 A CN 202210373625A CN 114736431 A CN114736431 A CN 114736431A
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mxene
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nickel nanowire
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杨哲一
崔锦文
王弘喆
崔雄华
张磊
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Xian Thermal Power Research Institute Co Ltd
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Abstract

The invention discloses an MXene/nickel nanowire conductive filler which is formed by compounding a nickel nanowire and MXene, wherein the nickel nanowire is attached to and grows on the MXene, the mass fraction of the nickel nanowire is 35% -70%, and the mass fraction of the MXene is 30% -65%. The invention also discloses a preparation method and application of the conductive filler; the preparation method comprises the following steps: preparing a silver nitrate alcohol solution; pretreating MXene powder; preparing a template agent alcohol solution; preparing ferric trichloride alcohol solution; mixing the three solutions, adding the pretreated MXene powder, heating in a water bath, and mechanically stirring and mixing; pouring the mixed solution into a reaction kettle, placing the reaction kettle in an oven, preserving heat in an alternating high-intensity magnetic field environment, and cooling to obtain a reacted material; and cleaning and drying the reacted materials to obtain the MXene/nickel nanowire conductive filler. The conductive filler has excellent conductive performance and can be used for preparing an anti-corrosion coating with excellent anti-corrosion performance.

Description

MXene/nickel nanowire conductive filler and preparation method and application thereof
Technical Field
The invention relates to the technical field of anticorrosive surface coating materials, in particular to MXene/nickel nanowire conductive filler, a preparation method and application in preparation of an anticorrosive coating.
Background
The corrosion of metal materials not only causes great loss to national economy, but also causes serious harm to the environment. At present, the most direct and common method for corrosion protection of metal materials is to apply an anti-corrosion coating on its surface. The addition of functional anti-corrosive fillers is an effective means of further improving the anti-corrosive properties of the coating, and generally comprises lamellar fillers for improving the shielding properties and fillers for inhibiting the corrosion of metals.
The graphene, boron nitride and other two-dimensional nanosheets have excellent mechanical properties, thermal conductivity, wear resistance, barrier property and hydrophobicity, and have a huge application prospect in the field of metal corrosion protection. Several production lines in China have produced graphene in quantity, but application outlets are still lacked, and the main problem is that the efficient dispersion technology of the graphene is lacked. Compared with graphene, the boron nitride nanosheet is an insulator, does not have a corrosion promoting effect, but lacks a high-efficiency stripping method of the boron nitride nanosheet; the surface of the boron nitride nanosheet is free of any functional group, and the compatibility with resin is poor; and the boron nitride nanosheets are easy to agglomerate, and a proper and efficient dispersing agent is needed. It follows that the two-dimensional materials described above still do not find good application in corrosion protection coatings due to the problem of dispersibility.
Two-dimensional transition metal carbide, nitride and carbonitride (MXene) is an emerging two-dimensional layered nanomaterial. MXene has good application prospect in the aspects of coating corrosion resistance, energy storage, electromagnetic interference shielding, transparent conductors, photoelectricity and the like due to the characteristics of high conductivity, many active sites, large specific surface area and the like. The MXene material can exert optimal performance in the application field by adjusting the transition metal species, different terminal groups, doping types and second composition in the MXene material. Compared with two-dimensional materials such as graphene and the like, the graphene-based composite material has low cost and good dispersibility, so that the graphene-based composite material is more in line with the requirements of practical application.
In view of the problems and the background, the invention prepares the MXene/NiNWs conductive filler for the high-performance anticorrosion coating by compounding the MXene and the NiNWs with high conductivity and corrosion resistance to form a complex conductive network.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide the MXene/nickel nanowire conductive filler, the preparation method and the application thereof, wherein a complex conductive network is formed between the nickel nanowire and the MXene in the conductive filler, so that the conductive filler has excellent conductive performance; after the conductive filler is applied to the preparation of an anti-corrosion coating, the anti-corrosion performance of the anti-corrosion coating can be improved.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
the MXene/nickel nanowire conductive filler is formed by compounding a nickel nanowire and MXene, wherein the nickel nanowire is attached to and grows on the MXene, the mass fraction of the nickel nanowire is 35-70%, and the mass fraction of the MXene is 30-65%.
The invention further provides a preparation method of the MXene/nickel nanowire conductive filler, which comprises the following steps:
step 1, preparing a nickel nitrate alcoholic solution;
step 2, pretreating MXene powder, including coarsening, sensitizing and activating;
step 3, preparing a template agent alcoholic solution;
step 4, preparing a growth assistant ferric trichloride alcoholic solution;
step 5, fully mixing the solutions obtained in the steps 1, 3 and 4, adding MXene powder treated in the step 2, uniformly stirring, heating in a water bath, and mechanically stirring to fully dissolve and mix;
step 6, pouring the mixed liquid obtained in the step 5 into a reaction kettle, placing the reaction kettle into an oven, preserving heat for a certain time in an alternating high-intensity magnetic field environment, and cooling along with the oven to obtain a reacted material;
and 7, cleaning and vacuum drying the reacted material obtained in the step 6 to obtain the dried MXene/nickel nanowire conductive filler.
Further, in step 1, the specific process for preparing the nickel nitrate alcoholic solution is as follows: mixing Ni (NO)3)2·6H2Mixing O and ethylene glycol, stirring for 10-30 min to dissolve nickel nitrate in the ethylene glycol to obtain a nickel nitrate alcohol solution; wherein Ni (NO)3)2·6H2The mass volume ratio of the O to the ethylene glycol is (4-6 g) to (20-40 ml).
Further, in the step 2, the MXene powder pretreatment specifically comprises the following steps:
step 2.1, weighing MXene powder, pouring the MXene powder into a nitric acid aqueous solution, completely immersing the MXene powder in the nitric acid aqueous solution, and coarsening the MXene powder by using the nitric acid aqueous solution for 30-60 min;
step 2.2, hydrochloric acid and SnCl2Mixing the aqueous solutions to form a sensitization treatment liquid, pouring MXene powder obtained after the treatment in the step 2.1 into the sensitization treatment liquid, completely immersing the MXene powder into the sensitization treatment liquid, and sensitizing the MXene powder by using the sensitization treatment liquid for 30-60 min;
step 2.3, adding Ni (NO)3)2·6H2Dissolving O in water to prepare an activating solution with the concentration of 0.2-0.6 mol/L, pouring MXene powder obtained after the treatment in the step 2.2 into the activating solution, completely immersing the MXene powder in the activating solution, activating the MXene powder by using the activating solution for 1.5-2.5 h, and washing and drying the activated MXene powder to obtain the pretreated MXene powder.
Further, the template agent alcoholic solution in the step 3 is a PVP template agent alcoholic solution; the preparation process of the PVP template agent alcoholic solution specifically comprises the following steps: mixing a template agent PVP and ethylene glycol, and then placing the mixture in an ultrasonic disperser for ultrasonic dissolution for 10-20min to obtain a PVP template agent alcohol solution; wherein the mass volume ratio of PVP to ethylene glycol is (0.6-0.9 g): (10-20 ml).
Further, the preparation process of the growth assistant ferric trichloride alcohol solution in the step 4 specifically comprises the following steps: mixing ferric trichloride with ethylene glycol, and stirring to fully dissolve the ferric trichloride to obtain ferric trichloride alcoholic solution; wherein the mass-volume ratio of ferric trichloride to ethylene glycol is (0.001-0.005 g): (10-15 ml).
Further, in the step 5, the water bath heating temperature is 40-60 ℃, and the stirring time is 10-20 min.
Further, in the step 6, the magnetic field intensity of the alternating high-intensity magnetic field environment is 0.5T, the magnetic field direction is changed every 1h, the heat preservation temperature is 150-180 ℃, and the heat preservation time is 5-8 h.
The invention also provides application of the MXene/nickel nanowire conductive filler, and particularly provides the MXene/nickel nanowire conductive filler which can be used for preparing an anti-corrosion coating.
The invention has the beneficial effects that:
MXene with good chemical stability and a nickel nanowire with high conductivity and corrosion resistance are compounded to form a conductive filler with a complex multidirectional conductive network; compared with two-dimensional nanosheets such as graphene and boron nitride, the conductive filler has better dispersibility and lower production cost, and the preparation process is simple and is more beneficial to practical application and large-scale production. Compared with a single MXene material, the conductivity of the conductive filler is improved by 2.2 times.
The conductive filler can be used for preparing an anti-corrosion coating, and the anti-corrosion performance of the anti-corrosion coating is improved by improving the conductivity. When electrochemical corrosion occurs, electrons generated by metal anode reaction are more easily transferred to the surface of the coating through the good conductive effect of the conductive filler, so that cathode reaction is carried out on the surface of the coating, and the anode reaction can be inhibited along with the accumulation of metal ions, so that the purpose of inhibiting metal corrosion is achieved, and the base metal is protected. Moreover, based on the complex multidirectional conductive network of the conductive filler, the coating prepared by the conductive filler has excellent conductivity along all directions, and the anti-corrosion performance of the coating can be obviously improved.
The preparation method of the MXene/NiNWs conductive filler adopts Ni (NO)3)2As an activating agent, the activating point is applied on the surface of MXene particles, thereby not only optimizingThe preparation process reduces the production cost and heavy metal ions in the waste liquid. In addition, the preparation method of the invention obtains the alternating magnetic field by regularly changing the direction of the magnetic field, is more beneficial to the growth of NiNWs, and forms a more complex conductive network by interweaving MXene and NiNWs, thereby improving the conductivity and the corrosion resistance of the composite conductive filler.
Drawings
Fig. 1 is an XRD pattern of MXene/nickel nanowire conductive filler of example 3 of the invention.
Fig. 2 is an SEM image of MXene/nickel nanowire conductive filler of example 3 of the invention.
Fig. 3 is a graph comparing the conductivity of an MXene/nickel nanowire conductive filler of example 3 of the present invention to a single MXene material.
Detailed Description
The following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the invention easier to understand by those skilled in the art, and thus will clearly and clearly define the scope of the invention.
The invention provides MXene/nickel nanowire conductive filler which is formed by compounding a nickel nanowire and MXene, wherein the nickel nanowire is attached to and grows on the MXene, the mass fraction of the nickel nanowire is 35-70%, and the mass fraction of the MXene is 30-65%.
The preparation method of the MXene/nickel nanowire conductive filler comprises the following steps:
step 1, preparing a nickel nitrate alcoholic solution; the specific process is as follows: mixing Ni (NO)3)2·6H2Mixing O and ethylene glycol, stirring for 10-30 min to dissolve nickel nitrate in the ethylene glycol to obtain a nickel nitrate alcohol solution; wherein Ni (NO)3)2·6H2The mass volume ratio of the O to the ethylene glycol is (4-6 g) to (20-40 ml).
Step 2, pretreating MXene powder, including coarsening, sensitizing and activating; the method comprises the following specific steps:
step 2.1, weighing MXene powder, pouring into a certain amount of nitric acid aqueous solution, completely immersing the MXene powder in the nitric acid aqueous solution, and utilizing the nitric acid aqueous solutionThe solution is used for coarsening MXene powder for 30-60 min; quality of MXene powder and Ni (NO) in step 13)2·6H2The addition amount ratio of O is (0.5-1.5 g): (4-6 g); the nitric acid aqueous solution is prepared by mixing nitric acid and water according to the volume ratio of 1: 1-5, and uniformly mixing.
Step 2.2, mixing the raw materials in a volume ratio of 1-5: 1 reacting hydrochloric acid and SnCl2Mixing the aqueous solutions to form a sensitization treatment liquid, pouring MXene powder obtained after treatment in the step 2.1 into the sensitization treatment liquid, completely immersing the MXene powder into the sensitization treatment liquid, and carrying out sensitization treatment on the MXene powder by using the sensitization treatment liquid for 30-60 min;
step 2.3, adding Ni (NO)3)2·6H2Dissolving O in water to prepare an activating solution with the concentration of 0.2-0.6 mol/L, pouring MXene powder obtained after the treatment in the step 2.2 into the activating solution, completely immersing the MXene powder in the activating solution, activating the MXene powder by using the activating solution for 1.5-2.5 h, and washing and drying the activated MXene powder to obtain the pretreated MXene powder.
Step 3, preparing a PVP template agent alcoholic solution; the specific process is as follows:
mixing a template agent PVP and ethylene glycol, and then placing the mixture in an ultrasonic disperser for ultrasonic dissolution for 10-20min to obtain a PVP template agent alcohol solution; wherein the mass-volume ratio of PVP to ethylene glycol is (0.6-0.9 g): (10-20 ml).
Step 4, preparing a growth assistant ferric trichloride alcoholic solution; the specific process is as follows:
mixing solid ferric trichloride with ethylene glycol, and stirring to fully dissolve the solid ferric trichloride to obtain ferric trichloride alcoholic solution; wherein the mass-volume ratio of ferric trichloride to ethylene glycol is (0.001-0.005 g): (10-15 ml).
Step 5, fully mixing the solutions obtained in the steps 1, 3 and 4, adding MXene powder treated in the step 2, uniformly stirring, placing in a water bath, heating in a water bath to 40-60 ℃, and mechanically stirring for 10-20min to fully dissolve and mix;
step 6, pouring the mixed solution obtained in the step 5 into a polytetrafluoroethylene reaction kettle, placing the reaction kettle into a drying oven, placing two magnets on two sides of the reaction kettle, wherein the magnetic field intensity is 0.5T, the magnetic field direction is changed every 1 hour, the temperature is 150-180 ℃, the heat preservation time is 5-8 hours, so as to ensure that Ni nanowires fully grow and coat MXene, and then cooling to room temperature along with the furnace to obtain a reacted material;
step 7, firstly, cleaning the reacted materials in the step 6 by using 2-3 times of volume of acetone solution, centrifuging the materials in a centrifuge of 7000-9000 r/min for 5-10 min, pouring off the yellow ethylene glycol impurity solution on the upper layer, adding deionized water for centrifugal cleaning, and repeating the steps for 3-4 times to remove the redundant ethylene glycol, PVP and other impurities; and finally, drying the cleaned solid and liquid in an oven at the temperature of 80-120 ℃ for 4-10 h to obtain the MXene/nickel nanowire conductive filler.
The invention also provides application of the MXene/nickel nanowire conductive filler, and particularly relates to the MXene/nickel nanowire conductive filler which can be matched with an organic carrier to prepare an anti-corrosion coating.
Example 1
The preparation method of the MXene/nickel nanowire conductive filler comprises the following steps:
step 1, preparing a nickel nitrate alcoholic solution; the specific process is as follows: weighing 4g of Ni (NO)3)2·6H2And O is placed in a beaker, 20ml of ethylene glycol is measured and added into the beaker, and a mechanical stirrer is adopted to fully stir for 10min, so that nickel nitrate is dissolved in the ethylene glycol to obtain nickel nitrate alcohol solution.
Step 2, pretreating MXene powder, including coarsening, sensitizing and activating; the method comprises the following specific steps:
step 2.1, weighing 0.5g of MXene powder, pouring the MXene powder into a certain amount of nitric acid aqueous solution, completely immersing the MXene powder in the nitric acid aqueous solution, and coarsening the MXene powder by using the nitric acid aqueous solution for 30 min; wherein, the nitric acid aqueous solution is obtained by uniformly mixing nitric acid and water in a volume ratio of 1: 1;
step 2.2, mixing the raw materials in a volume ratio of 1:1 reacting hydrochloric acid and SnCl2Mixing the aqueous solutions to form a sensitized layerPouring MXene powder obtained after the treatment in the step 2.1 into the sensitizing treatment liquid, completely immersing the MXene powder in the sensitizing treatment liquid, and sensitizing the MXene powder by using the sensitizing treatment liquid for 30 min;
step 2.3, adding Ni (NO)3)2·6H2Dissolving O in water to prepare an activating solution with the concentration of 0.2mol/L, pouring MXene powder obtained after the treatment in the step 2.2 into the activating solution, completely immersing the MXene powder in the activating solution, activating the MXene powder by using the activating solution for 1.5h, washing the activated MXene powder with water, and drying to obtain the pretreated MXene powder.
Step 3, preparing a PVP template agent alcoholic solution; the specific process is as follows:
weighing 0.6g of template PVP into a beaker, weighing 10ml of ethylene glycol, adding into the beaker, and then placing into an ultrasonic disperser for ultrasonic dissolution for 10min to obtain the PVP template alcohol solution.
Step 4, preparing a growth assistant ferric trichloride alcoholic solution; the specific process is as follows:
0.001g of solid ferric trichloride is mixed with 10ml of ethylene glycol, stirred for 5min by a glass rod, and fully dissolved to obtain ferric trichloride alcoholic solution.
Step 5, fully mixing the solutions obtained in the steps 1, 3 and 4, adding MXene powder treated in the step 2, uniformly stirring, placing in a water bath, heating in a water bath to 40 ℃, and mechanically stirring for 10min to fully dissolve and mix;
step 6, pouring the mixed solution obtained in the step 5 into a polytetrafluoroethylene reaction kettle, placing the reaction kettle into an oven, placing two magnets on two sides of the reaction kettle, wherein the magnetic field intensity is 0.5T, changing the magnetic field direction every 1 hour, the temperature is 150 ℃, the heat preservation time is 5 hours, so as to ensure that Ni nanowires fully grow and coat MXene, and then cooling the mixture to the room temperature along with a furnace to obtain a reacted material (MXene/NiNWs powder mixed solution);
step 7, firstly, cleaning the reacted materials in the step 6 by using 2 times of volume of acetone solution, centrifuging for 5min in a 7000r/min centrifuge, pouring off the upper yellow glycol impurity solution, adding deionized water for centrifugal cleaning, and repeating for 3 times to remove redundant glycol, PVP and other impurities; and finally, drying the cleaned solid and liquid in an oven at the temperature of 80 ℃ for 4 hours to obtain the MXene/nickel nanowire conductive filler.
Example 2
The preparation method of the MXene/nickel nanowire conductive filler comprises the following steps:
step 1, preparing a nickel nitrate alcoholic solution; the specific process is as follows: weighing 6g Ni (NO)3)2·6H2And O is placed in a beaker, 40ml of ethylene glycol is measured and added into the beaker, and a mechanical stirrer is adopted to fully stir for 30min, so that nickel nitrate is dissolved in the ethylene glycol to obtain nickel nitrate alcohol solution.
Step 2, pretreating MXene powder, including coarsening, sensitizing and activating; the method comprises the following specific steps:
step 2.1, weighing 1.5g of MXene powder, pouring the MXene powder into a certain amount of nitric acid aqueous solution, completely immersing the MXene powder in the nitric acid aqueous solution, and coarsening the MXene powder by using the nitric acid aqueous solution for 60 min; wherein, the nitric acid aqueous solution is obtained by uniformly mixing nitric acid and water in a volume ratio of 1: 5;
step 2.2, hydrochloric acid and SnCl are added according to the volume ratio of 5:12Mixing the aqueous solutions to form a sensitization treatment liquid, pouring MXene powder obtained after the treatment in the step 2.1 into the sensitization treatment liquid, completely immersing the MXene powder in the sensitization treatment liquid, and sensitizing the MXene powder by using the sensitization treatment liquid for 60 min;
step 2.3, adding Ni (NO)3)2·6H2Dissolving O in water to prepare an activating solution with the concentration of 0.6mol/L, pouring the MXene powder obtained after the treatment in the step 2.2 into the activating solution, completely immersing the MXene powder in the activating solution, performing activating treatment on the MXene powder by using the activating solution for 2.5 hours, and washing and drying the activated MXene powder to obtain the pretreated MXene powder.
Step 3, preparing a PVP template agent alcoholic solution; the specific process is as follows:
weighing 0.9g of template agent PVP in a beaker, weighing 20ml of ethylene glycol, adding into the beaker, and then placing in an ultrasonic disperser for ultrasonic dissolution for 20min to obtain the PVP template agent alcohol solution.
Step 4, preparing a growth auxiliary agent ferric trichloride alcohol solution; the specific process is as follows:
0.005g of solid ferric trichloride is mixed with 15ml of ethylene glycol, stirred for 10min by a glass rod, and fully dissolved to obtain ferric trichloride alcoholic solution.
Step 5, fully mixing the solutions obtained in the steps 1, 3 and 4, adding MXene powder treated in the step 2, uniformly stirring, placing in a water bath, heating in a water bath to 60 ℃, and mechanically stirring for 20min to fully dissolve and mix;
step 6, pouring the mixed solution obtained in the step 5 into a polytetrafluoroethylene reaction kettle, placing the reaction kettle into an oven, placing two magnets on two sides of the reaction kettle, wherein the magnetic field intensity is 0.5T, changing the magnetic field direction every 1 hour, the temperature is 180 ℃, the heat preservation time is 8 hours, so as to ensure that Ni nanowires fully grow and coat MXene, and then cooling the mixture to the room temperature along with a furnace to obtain a reacted material (MXene/NiNWs powder mixed solution);
step 7, firstly, cleaning the reacted materials in the step 6 by using 3 times of acetone solution, centrifuging the materials in a centrifuge of 9000r/min for 10min, pouring off the yellow ethylene glycol impurity solution on the upper layer, adding deionized water for centrifugal cleaning, and repeating the steps for 4 times to remove the redundant ethylene glycol, PVP and other impurities; and finally, drying the cleaned solid and liquid in a 120 ℃ drying oven for 10 hours to obtain the MXene/nickel nanowire conductive filler.
Example 3
The preparation method of the MXene/nickel nanowire conductive filler comprises the following steps:
step 1, preparing a nickel nitrate alcoholic solution; the specific process is as follows: weighing 5g Ni (NO)3)2·6H2And O is placed in a beaker, 30ml of ethylene glycol is measured and added into the beaker, and a mechanical stirrer is adopted to fully stir for 20min, so that nickel nitrate is dissolved in the ethylene glycol to obtain nickel nitrate alcohol solution.
Step 2, pretreating MXene powder, including coarsening, sensitizing and activating; the method comprises the following specific steps:
step 2.1, weighing 1.0g of MXene powder, pouring the MXene powder into a certain amount of nitric acid aqueous solution, completely immersing the MXene powder in the nitric acid aqueous solution, and coarsening the MXene powder by using the nitric acid aqueous solution for 40 min; wherein, the nitric acid aqueous solution is obtained by uniformly mixing nitric acid and water in a volume ratio of 1: 2;
step 2.2, hydrochloric acid and SnCl are added according to the volume ratio of 3:12Mixing the aqueous solutions to form a sensitization treatment liquid, pouring MXene powder obtained after the treatment in the step 2.1 into the sensitization treatment liquid, completely immersing the MXene powder in the sensitization treatment liquid, and sensitizing the MXene powder by using the sensitization treatment liquid for 40 min;
step 2.3, adding Ni (NO)3)2·6H2Dissolving O in water to prepare an activating solution with the concentration of 0.4mol/L, pouring MXene powder obtained after the treatment in the step 2.2 into the activating solution, completely immersing the MXene powder in the activating solution, activating the MXene powder by using the activating solution for 2.0 hours, washing the activated MXene powder with water, and drying to obtain the pretreated MXene powder.
Step 3, preparing a PVP template agent alcoholic solution; the specific process is as follows:
weighing 0.8g of template PVP into a beaker, weighing 15ml of ethylene glycol, adding into the beaker, and then placing into an ultrasonic disperser for ultrasonic dissolution for 15min to obtain the PVP template alcohol solution.
Step 4, preparing a growth assistant ferric trichloride alcoholic solution; the specific process is as follows:
0.002g of solid ferric trichloride is mixed with 12ml of ethylene glycol, stirred for 8min by a glass rod, and fully dissolved to obtain ferric trichloride alcoholic solution.
Step 5, fully mixing the solutions obtained in the steps 1, 3 and 4, adding MXene powder treated in the step 2, uniformly stirring, placing in a water bath, heating in a water bath to 50 ℃, and mechanically stirring for 15min to fully dissolve and mix;
step 6, pouring the mixed solution obtained in the step 5 into a polytetrafluoroethylene reaction kettle, placing the reaction kettle into an oven, placing two magnets on two sides of the reaction kettle, wherein the magnetic field intensity is 0.5T, the magnetic field direction is changed every 1 hour, the temperature is 160 ℃, the heat preservation time is 6 hours, so as to ensure that Ni nanowires fully grow and coat MXene, and then cooling the mixture to the room temperature along with a furnace to obtain a reacted material (MXene/NiNWs powder mixed solution);
step 7, firstly, cleaning the reacted materials in the step 6 by using 3 times of volume of acetone solution, centrifuging for 8min in a centrifuge of 8000r/min, pouring off the upper layer of yellow glycol impurity solution, adding deionized water for centrifugal cleaning, and repeating for 4 times to remove redundant glycol, PVP and other impurities; and finally, drying the cleaned solid and liquid in a drying oven at 100 ℃ for 8h to obtain the MXene/nickel nanowire conductive filler.
The XRD pattern of MXene/nickel nanowire conductive filler obtained in example 3 of the invention as shown in figure 1; as can be seen from FIG. 1, besides the MXene diffraction peak, the NiNWs diffraction peak can be observed obviously, which indicates that the MXene/nickel nanowire composite conductive filler is prepared successfully, and besides, no other impurity peak is detected.
An SEM image of MXene/nickel nanowire conductive filler obtained in example 3 of the invention as shown in fig. 2; as can be seen from fig. 2, MXene and NiNWs are interwoven together to form a conductive network in multiple directions, which is beneficial to improving the conductivity. Figure 3 is a graph comparing the conductivity of MXene/nickel nanowire conductive filler obtained from example 3 of the present invention with that of a single MXene. As can be seen from fig. 3, the conductivity of the MXene/nickel nanowire conductive filler of the present invention is significantly higher than that of a single MXene; compared with a single MXene material, the conductivity of the MXene/nickel nanowire conductive filler is improved by 2.2 times, and the conductive filler is a conductive filler for an anti-corrosion coating with good application prospect.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.

Claims (9)

1. The MXene/nickel nanowire conductive filler is characterized by being formed by compounding a nickel nanowire and MXene, wherein the nickel nanowire is attached to and grows on the MXene, the mass fraction of the nickel nanowire is 35-70%, and the mass fraction of the MXene is 30-65%.
2. The preparation method of the MXene/nickel nanowire conductive filler as claimed in claim 1, comprising the steps of:
step 1, preparing a nickel nitrate alcoholic solution;
step 2, pretreating MXene powder, including coarsening, sensitizing and activating;
step 3, preparing a template agent alcoholic solution;
step 4, preparing a growth assistant ferric trichloride alcoholic solution;
step 5, fully mixing the solutions obtained in the steps 1, 3 and 4, adding MXene powder treated in the step 2, uniformly stirring, heating in a water bath, and mechanically stirring to fully dissolve and mix;
step 6, pouring the mixed liquid obtained in the step 5 into a reaction kettle, placing the reaction kettle into an oven, preserving heat for a certain time in an alternating high-intensity magnetic field environment, and cooling along with the oven to obtain a reacted material;
and 7, cleaning and vacuum drying the reacted material obtained in the step 6 to obtain the dried MXene/nickel nanowire conductive filler.
3. The method for preparing the MXene/nickel nanowire conductive filler according to claim 2, wherein in the step 1, the specific process for preparing the nickel nitrate alcoholic solution comprises the following steps: mixing Ni (NO)3)2·6H2Mixing O and ethylene glycol, stirring for 10-30 min to dissolve nickel nitrate in the ethylene glycol to obtain a nickel nitrate alcoholic solution; wherein Ni (NO)3)2·6H2The mass volume ratio of the O to the ethylene glycol is (4-6 g) to (20-40 ml).
4. The method for preparing the MXene/nickel nanowire conductive filler according to claim 2, wherein in the step 2, the MXene powder is pretreated by the specific steps of:
step 2.1, weighing MXene powder, pouring the MXene powder into a nitric acid aqueous solution, completely immersing the MXene powder in the nitric acid aqueous solution, and coarsening the MXene powder by using the nitric acid aqueous solution for 30-60 min;
step 2.2, hydrochloric acid and SnCl2Mixing the aqueous solutions to form a sensitization treatment liquid, pouring MXene powder obtained after treatment in the step 2.1 into the sensitization treatment liquid, completely immersing the MXene powder into the sensitization treatment liquid, and carrying out sensitization treatment on the MXene powder by using the sensitization treatment liquid for 30-60 min;
step 2.3, adding Ni (NO)3)2·6H2Dissolving O in water to prepare an activating solution with the concentration of 0.2-0.6 mol/L, pouring MXene powder obtained after the treatment in the step 2.2 into the activating solution, completely immersing the MXene powder in the activating solution, activating the MXene powder by using the activating solution for 1.5-2.5 h, and washing and drying the activated MXene powder to obtain the pretreated MXene powder.
5. The method for preparing the MXene/nickel nanowire conductive filler according to claim 2, wherein the templating agent alcohol solution in the step 3 is a PVP templating agent alcohol solution; the preparation process of the PVP template agent alcoholic solution specifically comprises the following steps: mixing a template agent PVP and ethylene glycol, and then placing the mixture in an ultrasonic disperser for ultrasonic dissolution for 10-20min to obtain a PVP template agent alcohol solution; wherein the mass-volume ratio of PVP to ethylene glycol is (0.6-0.9 g): (10-20 ml).
6. The method for preparing the MXene/nickel nanowire conductive filler according to claim 2, wherein the preparation process of the growth assistant ferric trichloride alcoholic solution in the step 4 specifically comprises the following steps: mixing ferric trichloride with ethylene glycol, and stirring to fully dissolve the ferric trichloride to obtain ferric trichloride alcoholic solution; wherein the mass-volume ratio of ferric trichloride to ethylene glycol is (0.001-0.005 g): (10-15 ml).
7. The method for preparing the MXene/nickel nanowire conductive filler according to claim 2, wherein in the step 5, the water bath heating temperature is 40-60 ℃, and the stirring time is 10-20 min.
8. The preparation method of the MXene/nickel nanowire conductive filler according to claim 2, wherein in the step 6, the magnetic field strength of the alternating high-intensity magnetic field environment is 0.5T, the magnetic field direction is changed every 1h, the heat preservation temperature is 150-180 ℃, and the heat preservation time is 5-8 h.
9. The use of the MXene/nickel nanowire conductive filler of claim 1, wherein the MXene/nickel nanowire conductive filler is used to prepare an anti-corrosion coating.
CN202210373625.7A 2022-04-11 2022-04-11 MXene/nickel nanowire conductive filler and preparation method and application thereof Pending CN114736431A (en)

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