CN113976880B - Method and device for preparing carbon-coated metal nanoparticles by electric arc in liquid nitrogen - Google Patents
Method and device for preparing carbon-coated metal nanoparticles by electric arc in liquid nitrogen Download PDFInfo
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Abstract
The invention discloses a method and a device for preparing carbon-coated metal nanoparticles by electric arc in liquid nitrogen, which comprises the following steps: contacting one end face of the metal rod with one end face of the graphite rod and immersing the metal rod into liquid nitrogen; the metal rod is connected with one electrode of a direct current power supply, and the graphite rod is connected with the other electrode of the direct current power supply; separating the graphite rod and the metal rod to an experimental separation distance, generating an electric arc between the graphite rod and the metal rod, maintaining the electric arc in liquid nitrogen or in a gas atmosphere introduced into the liquid nitrogen until the experimental required time is reached, and obtaining liquid nitrogen containing carbon-coated metal nanoparticles, wherein the end face of one end of the graphite rod and the end face of one end of the metal rod are always positioned below the liquid level of the liquid nitrogen; and adding a collecting agent into the liquid nitrogen containing the carbon-coated metal nano-particles, and drying the collecting agent after the liquid nitrogen is volatilized to obtain the carbon-coated metal nano-particles. The invention has the advantages of simpler operation, high production efficiency and lower cost.
Description
Technical Field
The invention belongs to the field of nano material manufacturing, and particularly provides a method and a device for preparing carbon-coated metal nano particles by electric arc in liquid nitrogen.
Background
In recent years, carbon-coated metal nanoparticles have attracted extensive attention of researchers as a core-shell structured nanomaterial, and have great application prospects in functional magnetic materials, biomedicine, wave-absorbing materials, quantum devices, fuel cells and the like.
In the field of magnetic recording media, the magnetic recording density of the magnetic recording media is greatly improved as the particle size of the carbon-coated metal nano material is improved from micron level to nanometer level. In the biomedical field, carbon-coated metal nanoparticles have good compatibility with biological tissues by virtue of the nanoscale particle size, and carbon coating is used as a safe and nontoxic coating material, so that adverse effects of the metal nanoparticles on tissue cells can be effectively avoided. In the field of fuel cells, carbon-coated nanomaterials can serve as good anode materials. The need for carbon-coated metal nanoparticles is therefore increasing.
The preparation method of the carbon-coated metal nano-particles mainly comprises an electric explosion method, a ball milling method, a gas arc method, a hydrothermal method, a chemical vapor deposition method, an ion beam method, a laser method and the like. Chinese patent CN2019109480083 discloses a method for preparing carbon-coated metal nano-materials by enclosing ferric nitrate nonahydrate, an organic carbon source and ethylene glycol in a ball milling tank and performing high-energy ball milling. Patent CN201810379138.5 discloses a method for preparing ultrathin carbon-coated metal nanoparticles by heating small-molecule metal organic salts at high temperature.
The existing preparation methods such as a gas arc method and an electric explosion method need complicated vacuum equipment, the process parameters of a ball milling method are difficult to regulate and control, the number of prepared byproducts is large, a hydrothermal chemical vapor deposition method, a laser method, an ion beam method and the like need expensive experimental equipment, the yield is low, the preparation method is only suitable for laboratory preparation, and the practical application has great limitation.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method and a device for preparing carbon-coated metal nanoparticles by electric arc in liquid nitrogen, which solve the problems of complex operation, high requirement on preparation equipment, high cost and low yield of the conventional preparation method of carbon-coated metal nanoparticles.
In order to achieve the purpose, the invention provides the following technical scheme: a method for preparing carbon-coated metal nanoparticles by electric arc in liquid nitrogen comprises the following steps:
contacting one end face of the metal rod with one end face of the graphite rod and immersing the metal rod into liquid nitrogen;
the metal rod is connected with one electrode of a direct current power supply, and the graphite rod is connected with the other electrode of the direct current power supply;
separating the graphite rod and the metal rod to an experimental spacing distance, generating an electric arc between the graphite rod and the metal rod, and maintaining the electric arc in liquid nitrogen or in a gas atmosphere introduced into the liquid nitrogen until the experimental required time is reached to obtain liquid nitrogen containing carbon-coated metal nanoparticles, wherein the end face of one end of the graphite rod and the end face of one end of the metal rod are always positioned below the liquid level of the liquid nitrogen;
and adding a collecting agent into the liquid nitrogen containing the carbon-coated metal nano-particles, and drying the collecting agent after the liquid nitrogen is volatilized to obtain the carbon-coated metal nano-particles.
Further, before contacting one end face of the metal rod with one end face of the graphite rod, the method further comprises the following steps:
polishing the surface of the metal rod;
the surfaces of the metal rod and the graphite rod are washed by a cleaning agent.
Furthermore, the metal rod is made of gold, silver, copper, iron, nickel, cobalt, aluminum, magnesium, zinc or titanium.
Furthermore, the current of the direct current power supply is between 10 and 1000A.
Furthermore, the experimental separation distance for separating the graphite rod and the metal rod is 0-30mm.
Further, the gas is helium, neon, argon, xenon, carbon dioxide or methane.
Further, the collecting agent is deionized water, absolute ethyl alcohol or dodecane.
Further, the temperature for drying the collector is 60-100 ℃.
The invention also provides a device for preparing the carbon-coated metal nanoparticles by electric arc in liquid nitrogen, which comprises a container, a quartz tube and a direct-current power supply, wherein the liquid nitrogen is contained in the container, the positive electrode of the direct-current power supply is connected with a lower conductive clamp, the lower conductive clamp is used for clamping a metal rod, the negative electrode of the direct-current power supply is connected with an upper conductive clamp, the upper conductive clamp is used for clamping a graphite rod, and the upper conductive clamp can move under the action of a stepping motor;
the quartz tube is sleeved on the graphite rod, the end face of one end of the quartz tube is of an open structure, the end face of the other end of the quartz tube is sealed and is connected with the graphite rod, the side wall of the quartz tube is communicated with a branch tube, and gas is introduced into the branch tube;
in an initial state, one end face of the metal rod is in contact with one end face of the graphite rod, and in an experimental process, the end face of one end of the metal rod is not in contact with the end face of one end of the graphite rod;
and one end face of the metal rod and one end face of the graphite rod are always positioned in the inner cavity of the quartz tube.
Compared with the prior art, the invention has at least the following beneficial effects:
the invention provides a method for preparing carbon-coated metal nanoparticles in liquid nitrogen by electric arc, which adopts a metal rod and a graphite rod as electrodes, gas is introduced into the liquid nitrogen or the liquid nitrogen, the metal rod and the graphite rod ablate a positive electrode and a negative electrode in a contact arcing mode in a gas atmosphere, carbon particles and metal particles in electric arc plasma escape from a high-temperature growth region under the action of extremely high temperature gradient, the carbon particles and the metal particles are rapidly condensed and nucleated, and finally the carbon-coated metal nanoparticles are formed. Meanwhile, an extremely cold environment created by liquid nitrogen is adopted, so that an extremely high temperature gradient can be created around the electric arc, the produced nano particles can rapidly escape from a high-temperature growth area, the continuous expansion of the particle size of the nano particles is avoided, and the particle size distribution of the produced carbon-coated nano particles is narrow. The preparation method of the invention can avoid adopting special equipment to create and maintain the vacuum environment in the liquid nitrogen, thereby saving the high cost of creating and maintaining the vacuum environment and having lower manufacturing cost. The preparation method can be used for continuously preparing in liquid nitrogen for a long time, avoids the defect that the more common metal wire electric explosion method needs to replace the metal wire and frequently deflate the metal wire, and has simpler operation and high production efficiency.
Furthermore, before the metal rod and the graphite rod are contacted, the metal rod and the graphite rod are treated, so that the oil stain oxidation layer on the surfaces of the metal rod and the graphite rod is prevented from generating adverse effects on the preparation process.
Furthermore, the type of the metal rod can be used for preparing various metal nano particles, and the application range is wide.
Furthermore, the particle size distribution of the nanoparticles can be effectively regulated and controlled by regulating and controlling the direct current power supply, so that the specific requirement of a customer on the particle size of the nanoparticles is met.
Furthermore, the distance separating the graphite rod and the metal rod is beneficial to stably maintaining the electric arc, thereby improving the production efficiency of the nano particles.
The invention also provides a device for realizing the method for preparing the carbon-coated metal nanoparticles by electric arc in the liquid nitrogen, the metal rod and the graphite rod are used as a cathode and an anode, the liquid nitrogen is put into the beaker, the quartz tube is sleeved on the graphite rod, and gas is introduced into the quartz tube, so that the electric arc between the graphite rod and the metal rod is under the protection of the gas, the whole device is simple and convenient, the high equipment cost and the complex experimental device of the traditional method are avoided, and the device is suitable for large-scale production of the carbon-coated metal nanoparticles.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is an XRD pattern of carbon-coated aluminum nanoparticles prepared in example 1;
FIG. 3 is a HRTEM image of the carbon-coated aluminum nanoparticles prepared in example 1;
in the drawings: 1-direct current power supply, 2-step motor, 3-upper conductive clip, 4-branch pipe, 5-quartz tube, 6-graphite rod, 7-liquid nitrogen, 8-carbon-coated metal nanoparticle, 9-lower conductive clip, 10-metal rod, 11-moving part, 12-driving arm and 13-step motor support frame.
Detailed Description
The invention is further described with reference to the following figures and detailed description.
The invention provides a method for preparing carbon-coated metal nano particles in liquid nitrogen by electric arc, which is a method for preparing a carbon-coated metal nano material by creating a gas environment in the liquid nitrogen and arc ablation under the protection of gas.
In this embodiment, the steps of the present invention are as follows:
contacting one end face of a metal rod 10 with one end face of a graphite rod 6 and immersing the metal rod into liquid nitrogen 7;
the metal rod 10 is connected with one electrode of the direct current power supply 1, and the graphite rod 6 is connected with the other electrode of the direct current power supply 1;
separating the graphite rod 6 and the metal rod 10 to an experimental separation distance, generating an electric arc between the graphite rod 6 and the metal rod 10, maintaining the electric arc in liquid nitrogen or in a gas atmosphere introduced into the liquid nitrogen until the experimental required time is reached, obtaining liquid nitrogen containing carbon-coated metal nanoparticles, wherein the end face of one end of the graphite rod 6 and the end face of one end of the metal rod 10 are always positioned below the liquid level of the liquid nitrogen 7;
and adding a collecting agent into the liquid nitrogen 7 containing the carbon-coated metal nano-particles 8, and drying the collecting agent after the liquid nitrogen 7 is volatilized to obtain the carbon-coated metal nano-particles 8.
In this embodiment, the anode is a metal rod 10, wherein the metal rod 10 comprises gold, silver, copper, iron, nickel, cobalt, aluminum, magnesium, zinc, titanium, or the like. The cathode adopts a graphite electrode as a carbon-coated carbon source, the cathode and the anode of the metal rod 10 and the graphite rod 6 are ablated in liquid nitrogen 7 in a contact arcing mode, gas is introduced into the liquid nitrogen 7 to create a gas atmosphere in the liquid nitrogen 7, electric arc is generated under the protection of the gas, carbon ions and metal ions in electric arc plasma escape from a high-temperature growth region under the action of extremely high temperature gradient, the carbon ions and the metal ions are rapidly condensed to form core, and finally carbon-coated metal nano particles are formed.
Preferably, the collector is added to the liquid nitrogen after the arc discharge is finished, and the carbon-coated metal nanoparticles are collected in the collector after the liquid nitrogen 7 is volatilized. The collecting agent is various organic and inorganic solvents, including deionized water, absolute ethyl alcohol or dodecane and the like.
In the present embodiment, the gas is helium, neon, argon, xenon, carbon dioxide or methane; the DC power supply is used as an excitation source to maintain the DC arc, and the arc current is controlled to be 10-1000A.
In another embodiment of the present invention, as shown in fig. 1, there is also provided an apparatus for performing the above-mentioned steps of a method for preparing carbon-coated metal nanoparticles by arc in liquid nitrogen, comprising a dc power supply 1, a stepping motor 2, an upper conductive clip 3, a branch tube 4, a quartz tube 5, a graphite rod 6, liquid nitrogen 7, a lower conductive clip 9, and a metal rod 10. Specifically, liquid nitrogen 7 is contained in the beaker, the positive electrode of the direct current power supply 1 is connected with a lower conductive clamp 9, a metal rod 10 is clamped by the lower conductive clamp 9, and the metal rod 10 is immersed in the liquid nitrogen 7; a negative electrode of a direct current power supply 1 is connected with an upper conductive clamp 3, a graphite rod 6 is clamped by the upper conductive clamp 3, wherein in an initial state, one end face of a metal rod 10 is in contact with one end face of the graphite rod 6, a rod body of the metal rod 10 in contact with the graphite rod 6 is immersed into liquid nitrogen 7, in an experimental process, a stepping motor 2 is supported by a stepping motor support frame 13, a moving part 11 is driven by the stepping motor 2, the moving part 11 drives the graphite rod 6 to move through a driving arm 12, the metal rod 10 and the graphite rod 6 are pulled open, electric arcs are generated between the metal rod 10 and the graphite rod 6, and an arc striking area of the metal rod 10 and the graphite rod 6 is always maintained below the liquid nitrogen 7 in the protection of gas;
further, the quartz tube 5 is sleeved on the graphite rod 6, one end face of the quartz tube 5 is of an opening structure, the other end face of the quartz tube 5 is of a sealing structure, the other end face of the quartz tube 5 is connected with the graphite rod 6, the side wall of the quartz tube 5 is communicated with the branch tube 4, gas is introduced into the liquid nitrogen 7 through the quartz tube 5 to create a gas atmosphere in the liquid nitrogen 7, and electric arcs are generated under the protection of the gas in the quartz tube 5.
In this embodiment, the quartz tube 5 has a diameter of 20mm,
specifically, the method for preparing the carbon-coated metal nanoparticles by using the device comprises the following steps:
the method comprises the following steps: the metal rod 10 is polished by abrasive paper, then the raw materials of the graphite rod 6 and the metal rod 10 are cleaned, the metal rod is washed by a cleaning agent, oil stains and impurities on the surface of an electrode are washed, and the cleaning agent is washed clean by another cleaning agent.
Step two: clamping a metal rod 10 on the lower conductive clamp 9 to serve as an anode; the graphite rod 6 is clamped on the upper conductive clamp 3 to be used as a cathode, the cathode and the anode and the quartz tube 5 are placed in a beaker filled with liquid nitrogen 7, the contact position of the cathode and the anode is ensured to be below the liquid level of the liquid nitrogen 7, and gas is introduced through a branch tube 4 on the quartz tube 5.
Step three: the direct current power supply 1 is turned on and is kept unchanged in the experiment process. The anode and cathode are pulled apart to the experimental separation distance, and the arc is maintained to be stable for a period of time.
Step four: after the experiment is finished, adding a collecting agent into the liquid nitrogen 7; after the liquid nitrogen 7 is volatilized, the carbon-coated metal nanoparticles 8 remain in the non-volatilized collecting agent, and the absolute ethyl alcohol containing the carbon-coated aluminum nanoparticles 8 is dried in a blast drying oven at the temperature of 60-100 ℃ to obtain a powder sample. The obtained powder sample is determined to be carbon-coated aluminum nano-particles by X-ray diffraction.
Specifically, the experimental separation distance is 0-30mm.
Example 1
Step one, cleaning raw materials, namely a graphite rod 6 and a metal rod 10, washing with absolute ethyl alcohol, washing off oil stains and impurities on the surface of an electrode, and washing the absolute ethyl alcohol clean with deionized water. The graphite rod 6 is a high-purity graphite rod with the diameter of 6mm and the purity of 99.9 percent. The metal rod 10 is an aluminum rod with the purity of 99.7 percent and the diameter of 12mm, and an oxide layer on the surface of the aluminum rod is polished by abrasive paper before cleaning.
Step two, clamping the aluminum bar on the lower conductive clamp 9 as an anode; a graphite rod 6 was held on the upper conductive holder 3 as a cathode.
Step three, introducing argon gas into the liquid nitrogen through a quartz tube 5; the cathode and the anode and the quartz tube 5 are placed in a beaker filled with liquid nitrogen 7, and the contact position of the cathode and the anode is ensured to be below the liquid level of the liquid nitrogen.
And step four, setting the current of the direct current power supply 1 to be 10A, and keeping the current unchanged in the experimental process. The cathode and the anode are pulled apart by a certain distance of 5mm, and the arc is maintained to be stable for 60min.
And step five, after the experiment is finished, adding a collecting agent absolute ethyl alcohol into the liquid nitrogen 7, and after the liquid nitrogen 7 is volatilized, leaving the carbon-coated aluminum nanoparticles 8 in the unvaporized absolute ethyl alcohol. And drying the absolute ethyl alcohol containing the carbon-coated aluminum nano particles 8 in an air-blast drying oven at 60 ℃ to obtain a powder sample. The obtained powder sample is determined to be carbon-coated aluminum nano-particles by utilizing X-ray diffraction.
As shown in fig. 2, the XRD patterns of the carbon-coated aluminum nanoparticles prepared under the above conditions show that the diffraction peaks of aluminum are 38.5 ° (111), 44.76 ° (200), 65.1 ° (220), 78.23 ° (311), 82.42 ° (222), and 26.57 ° (002), respectively, demonstrating the presence of metallic aluminum and carbon in the product. Fig. 3 shows HRTEM of carbon-coated aluminum nanoparticles prepared under the above conditions, demonstrating the presence of a carbon coating on the outer layer of the aluminum nanoparticles.
Example 2
Step one, cleaning raw materials, namely a graphite rod 6 and a metal rod 10, washing with absolute ethyl alcohol, washing off oil stains and impurities on the surface of an electrode, and washing the absolute ethyl alcohol clean with deionized water. The graphite rod 6 is a high-purity graphite rod with the diameter of 6mm and the purity of 99.9 percent. The metal rod 10 is a copper rod with the purity of 99.7 percent and the diameter of 12mm, and an oxide layer on the surface of the copper rod is polished by sand paper before cleaning.
Secondly, clamping the copper bar on the lower conductive clamp 9 to be used as an anode; a graphite rod 6 was held on the upper conductive holder 3 as a cathode.
Thirdly, introducing helium into the liquid nitrogen 7 through the quartz tube 5; the cathode and the anode and the quartz tube 5 are placed in a beaker filled with liquid nitrogen 7, and the contact position of the cathode and the anode is ensured to be below the liquid level of the liquid nitrogen.
And step four, setting the current of the direct current power supply 1 to be 100A, and keeping the current unchanged in the experimental process. The cathode and the anode are pulled apart by a certain distance of 7mm, and the arc is maintained to be stable for 30min.
And step five, after the experiment is finished, adding a collecting agent deionized water into the liquid nitrogen 7, and after the liquid nitrogen 7 is volatilized, remaining the carbon-coated copper nanoparticles in the non-volatilized deionized water. And drying the deionized water containing the carbon-coated aluminum nanoparticles in an air-blast drying oven at the temperature of 80 ℃ to obtain a powder sample. The obtained powder sample is determined to be carbon-coated copper nanoparticles by X-ray diffraction.
Example 3
Step one, cleaning raw materials, namely a graphite rod 6 and a metal rod 10, washing with absolute ethyl alcohol, washing off oil stains and impurities on the surface of an electrode, and washing the absolute ethyl alcohol clean with deionized water. The graphite rod 6 is a high-purity graphite rod with the diameter of 6mm and the purity of 99.9 percent. The metal rod 10 is an iron rod with the purity of 99.7 percent and the diameter of 12mm, and the surface of the iron rod is polished by abrasive paper before cleaning.
Step two, clamping the iron rod on the lower conductive clamp 9 to be used as an anode; a graphite rod 6 was held on the upper conductive holder 3 as a cathode.
Step three, introducing carbon dioxide into the liquid nitrogen 7 through a quartz tube 5; the cathode and the anode and the quartz tube 5 are placed in a beaker filled with liquid nitrogen 7, and the contact position of the cathode and the anode is ensured to be below the liquid level of the liquid nitrogen.
And step four, setting the current of the direct current power supply 1 to 1000A, and keeping the current unchanged in the experimental process. The cathode and the anode are pulled apart by a certain distance of 5mm, and the arc is kept stable for 1min.
And step five, after the experiment is finished, adding dodecane serving as a collecting agent into the liquid nitrogen 7, and after the liquid nitrogen 7 is volatilized, remaining the carbon-coated copper nanoparticles in the unvolatile dodecane. And drying dodecane containing carbon coated copper nanoparticles in an air drying oven at 100 ℃ to obtain a powder sample. The obtained powder sample is determined to be carbon-coated iron nano-particles by X-ray diffraction.
Example 4
Step one, cleaning raw materials, namely a graphite rod 6 and a metal rod 10, washing with absolute ethyl alcohol, washing off oil stains and impurities on the surface of an electrode, and washing the absolute ethyl alcohol clean with deionized water. The graphite rod 6 is a high-purity graphite rod with the diameter of 6mm and the purity of 99.9 percent. The metal rod is a zinc rod with the purity of 99.7 percent and the diameter of 12mm, and the surface of the zinc rod is polished by sand paper before cleaning.
Secondly, clamping a zinc bar on the lower conductive clamp 9 to serve as an anode; a graphite rod 6 was held on the upper conductive holder 3 as a cathode.
Thirdly, introducing neon into the liquid nitrogen 7 through the quartz tube 5; the cathode and the anode and the quartz tube 5 are placed in a beaker filled with liquid nitrogen 7, and the contact position of the cathode and the anode is ensured to be below the liquid level of the liquid nitrogen.
And step four, setting the current of the direct current power supply 1 to 1000A, and keeping the current unchanged in the experimental process. The cathode and the anode are pulled apart by a certain distance of 30mm, and the arc is maintained to be stable for 10min.
And step five, after the experiment is finished, adding dodecane serving as a collecting agent into the liquid nitrogen 7, and after the liquid nitrogen is volatilized, leaving the carbon-coated zinc nanoparticles in the unvolatile dodecane. And drying dodecane containing the carbon-coated zinc nanoparticles in an air drying oven at 100 ℃ to obtain a powder sample. The obtained powder sample is determined to be carbon-coated zinc nano-particles by utilizing X-ray diffraction.
Example 5
Step one, cleaning raw materials including a graphite rod 6 and a metal rod 10, washing with absolute ethyl alcohol, washing off oil stains and impurities on the surface of an electrode, and washing the absolute ethyl alcohol clean with deionized water. The graphite rod 6 is a high-purity graphite rod with the diameter of 6mm and the purity of 99.9 percent. The metal rod is a zinc rod with the purity of 99.7 percent and the diameter of 12mm, and the surface of the zinc rod is polished by sand paper before cleaning.
Step two, clamping the aluminum bar on the lower conductive clamp 9 as an anode; a graphite rod 6 was held on the upper conductive holder 3 as a cathode.
And step three, placing the cathode and the anode in a beaker filled with liquid nitrogen 7, and ensuring that the contact position of the cathode and the anode is below the liquid level of the liquid nitrogen.
And step four, setting the current of the direct current power supply 1 to be 30A, and keeping the current unchanged in the experimental process. The cathode and the anode are pulled apart by a certain distance of 5mm, and the arc is kept stable for 1min.
And step five, after the experiment is finished, adding a collecting agent absolute ethyl alcohol into the liquid nitrogen 7, and after the liquid nitrogen is volatilized, leaving the carbon-coated zinc nanoparticles in the unvaporized absolute ethyl alcohol. And drying dodecane containing the carbon-coated zinc nanoparticles in an air drying oven at 100 ℃ to obtain a powder sample. The obtained powder sample is determined to be carbon-coated zinc nanoparticles by X-ray diffraction.
Finally, it should be noted that: the above-mentioned embodiments are only specific embodiments of the present invention, which are used for illustrating the technical solutions of the present invention and not for limiting the same, and the protection scope of the present invention is not limited thereto, although the present invention is described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: any person skilled in the art can modify or easily conceive the technical solutions described in the foregoing embodiments or equivalent substitutes for some technical features within the technical scope of the present disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the embodiments of the present invention, and they should be construed as being included therein. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (8)
1. A method for preparing carbon-coated metal nanoparticles by electric arc in liquid nitrogen is characterized by comprising the following steps:
one end face of the metal rod (10) is contacted with one end face of the graphite rod (6) and is immersed in liquid nitrogen (7);
the metal rod (10) is connected to one electrode of the direct current power supply (1), and the graphite rod (6) is connected to the other electrode of the direct current power supply (1);
separating the graphite rod (6) and the metal rod (10) to an experimental spacing distance, generating electric arc between the graphite rod (6) and the metal rod (10), introducing gas into liquid nitrogen through a quartz tube (5), maintaining the electric arc in the gas atmosphere introduced into the liquid nitrogen until reaching the experimental required time, and obtaining liquid nitrogen (7) containing carbon-coated metal nanoparticles, wherein the end face of one end of the graphite rod (6) and the end face of one end of the metal rod (10) are always positioned below the liquid level of the liquid nitrogen (7);
adding a collecting agent into liquid nitrogen (7) containing the carbon-coated metal nanoparticles (8), and drying the collecting agent after the liquid nitrogen (7) is volatilized to obtain the carbon-coated metal nanoparticles (8);
the gas is helium, neon, argon, xenon, carbon dioxide or methane.
2. The method for preparing carbon-coated metal nanoparticles by arc in liquid nitrogen according to claim 1, further comprising the following steps before contacting one end face of the metal rod (10) with one end face of the graphite rod (6):
polishing the surface of the metal rod (10);
the surfaces of the metal rod (10) and the graphite rod (6) are washed by a cleaning agent.
3. The method for preparing carbon-coated metal nanoparticles through electric arc in liquid nitrogen according to claim 1, wherein the metal rod (10) is made of gold, silver, copper, iron, nickel, cobalt, aluminum, magnesium, zinc or titanium.
4. The method for preparing carbon-coated metal nanoparticles in liquid nitrogen through electric arc according to claim 1, wherein the current of the direct current power supply (1) is 10 to 1000A.
5. The method for preparing carbon-coated metal nanoparticles in liquid nitrogen through electric arc according to claim 1, wherein the experimental separation distance between the graphite rod (6) and the metal rod (10) is 0-30mm.
6. The method of claim 1, wherein the collector is deionized water, absolute ethanol, or dodecane.
7. The method for preparing carbon-coated metal nanoparticles through electric arc in liquid nitrogen according to claim 1, wherein the temperature of the drying collector is 60-100 ℃.
8. The device for realizing the method for preparing carbon-coated metal nanoparticles by arc in liquid nitrogen according to any one of claims 1 to 7 is characterized by comprising a container, a quartz tube (5) and a direct current power supply (1), wherein the container contains liquid nitrogen (7), the positive pole of the direct current power supply (1) is connected with a lower conductive clamp (9), the lower conductive clamp (9) is used for clamping a metal rod (10), the negative pole of the direct current power supply (1) is connected with an upper conductive clamp (3), the upper conductive clamp (3) is used for clamping a graphite rod (6), and the upper conductive clamp (3) can move under the action of a stepping motor (2);
the quartz tube (5) is sleeved on the graphite rod (6), one end face of the quartz tube (5) is of an open structure, the other end face of the quartz tube (5) is sealed and is connected with the graphite rod (6), the side wall of the quartz tube (5) is communicated with a branch tube (4), and gas is introduced into the branch tube (4);
in an initial state, one end face of the metal rod (10) is in contact with one end face of the graphite rod (6), and in an experimental process, one end face of the metal rod (10) is not in contact with one end face of the graphite rod (6);
and one end face of the metal rod (10) and one end face of the graphite rod (6) are always positioned in the inner cavity of the quartz tube (5).
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