In-situ synthesis of carbon nanotubes filled with metallic nanoparticles using arc discharge in solution
View Patent ↗A novel method for simultaneously forming and filling and decorating carbon nanotubes with palladium nanoparticles is disclosed. Synthesis involves preparing a palladium chloride (PdCl 2 ) solution in a container, having two graphite electrodes, then immersing the graphite electrode assembly, into the PdCl 2 solution; connecting the graphite electrodes to a direct current power supply; bringing the electrodes into contact with each other to strike an arc; separating the electrodes to sustain the arc inside the solution; putting the container with electrode assembly in a water-cooled bath; and collecting Pd-nanoparticles encapsulated in carbon nanotubes and carbon nanotubes decorated with Pd-nanoparticles. The temperature at the site of the arc-discharge is greater than 3000° C. At these temperatures, the palladium is ionized into nanoparticles and the graphite electrodes generate layers of graphene (carbon), which roll away from the anode and encapsulate or entrap the Pd-nanoparticles. The unique nanotube structures have significant commercial potential as gas sensors or as a means for hydrogen storage.
1. A method of preparing a composition of matter wherein carbon nanotubes are simultaneously formed and filled with metallic-nanoparticles prepared by in-situ arc discharge in solution comprising the steps of:
a) selecting a cylindrical reactor cell consisting of
i) a double walled glass with 2 cm thickness, on two sides of a cylindrical cell having an inner diameter of 10 cm, for flowing of cold water at 7° C. to cool the cell;
ii) a cell cavity with a pair of inlets and a pair of outlets, wherein a first inlet is paired with a first outlet connected to the volume between the double glass walls for the flow of chilled water, and a second inlet is used for filling the cell with a solution for the arc-discharge reaction and is paired with a second outlet for filtering out the encapsulated and decorated carbon nanotubes formed in the cell;
iii) a first stainless steel plate covering the top of the cylindrical reactor cell that connects to an anode and a second stainless steel plate covering the bottom of the cylindrical reactor cell that connects to a cathode; and
iv) a direct current power supply system connecting to both the anode and the cathode that are immersed in the solution for the arc-discharge reaction;
b) preparing a metallic compound solution comprising a metallic compound powder, de-ionized water, and hydrochloric acid in a container;
c) using the second inlet to fill the cell cavity with the metallic compound solution;
d) immersing a graphite electrode assembly, having two graphite electrodes, wherein the electrode assembly consists of one electrode acting as a cathode and another electrode acting as an anode, into the metallic compound solution;
e) connecting the graphite electrodes to a direct current power supply;
f) bringing the electrodes into contact with each other to strike an arc and create an in-situ arc-discharge, wherein the temperature at the site of the arc-discharge is greater than 3000° C.;
g) vaporizing the metallic compound solution to leave a residue of a plurality of metallic-nanoparticles;
h) separating the electrodes to sustain the arc inside the solution;
i) forming graphene layers that roll away from the electrodes thereby forming graphitic carbon nanotubes that simultaneously encapsulate the metallic-nanoparticles;
j) flowing chilled water at a temperature of approximately 7° C. through the first inlet of the cell to facilitate cooling; and
k) collecting metallic-nanoparticles entrapped in carbon nanotubes.
2. The method of preparing a composition of matter in claim 1 , wherein the metallic compound solution for the in-situ arc discharge reaction includes a solution selected from at least one of metallic chlorides, metallic oxides, metallic sulfides, metallic carbides and metallic nitrides, for synthesizing carbon nanotubes filled with metallic nanoparticles.
3. The method of preparing a composition of matter in claim 2 , wherein the solution for the in-situ arc discharge reaction includes palladium chloride for synthesizing carbon nanotubes filled with palladium nanoparticles.