Method of obtaining colloidal solution of nano-sized carbon

FIELD: chemistry.

SUBSTANCE: invention can be used in obtaining coatings, reducing coefficient of secondary electronic emission, growing diamond films and glasses, elements, absorbing solar radiation. Colloidal solution of nano-sized carbon is obtained by supply of organic liquid - ethanol, into chamber with electrodes, injection of inert gas into inter-electrode space, formation of high-temperature plasma channel in gas bubbles, containing vapours of organic liquid. High-temperature plasma channel has the following parameters: temperature of heavy particles 4000-5000K, temperature of electrons 1.0-1.5 eV, concentration of charged particles (2-3)·1017 cm3, diameter of plasma channel hundreds of microns. After that, fast cooling within several microseconds is performed.

EFFECT: simplicity, possibility to obtain nanoparticles of different types.

3 cl, 1 dwg

 

The proposed method of producing stable nano-colloidal solution of carbon relates to the field of nanotechnology.

Preparation and investigation of nanostructured materials is of great interest from the scientific and applied points of view (unique electrical, magnetic, chemical, mechanical properties, catalytic activity, luminescent properties, etc.).

Of fundamental interest is associated with structural features and physico-chemical characteristics of the object (a large amount of free carbon bonds, the compactness of the structure).

Of great interest are the study of such properties of nanofluids, thermal conductivity, density, viscosity, conductivity, optical and magnetic properties.

The unusual properties of nanoparticles is the basis for many areas of applied character:

- new materials technology, pharmacology;

- a unique source of field electron emission;

- metallic and semiconductor characteristics are the most miniature electronic devices;

- surface structure of the object allows it to be used as a container for liquids and gases, in particular hydrogen.

Recently attracted considerable interest of the work associated with obtaining thin films of nanostructured carbon d�I reduce secondary emission coefficients of metals and dielectrics, growing diamond films and glasses, and stable colloidal solutions (solar energy absorber) (Robert Taylor, Sylvain Coulombe, Todd Otanicar, Patrick Phelan, Andrey Gunawan4, Wei Lv4, Gary Rosengarten, Ravi Prasher, and Himanshu Tyagi. Small particles, big impacts: A review of the diverse applications of nanofluids. J. Appl. Phys. 113, 011301 (2013)).

There are various methods (physical, chemical, composite, etc.) of nanoparticles formation:

- electric arc,

- pulsed arc and spark,

- laser ablation in gases and liquids

- deposition of products of chemical reactions

- pyrolysis in the presence of metal catalysts

- electrical explosion of conductors,

- catalytic conversion of composite powders in flames.

However, most of these methods take too much time and costs are complex and typically require the separation of useful products from impurities. The carbon nanostructures represent metastable States of condensed carbon, receiving them is possible only in conditions of deviation from thermodynamic equilibrium. Therefore, great interest in the recent past, a number of works, which is necessary for the synthesis of nanoparticles of carbon, metals, and various compositions used pulsed electric discharge in liquids. Short pulse discharge contributes to the creation of metastable�x carbon phases as a result of atomization of carbon in the high temperature discharge channel and followed by rapid cooling ("quenching").

The method is promising for a number of features:

- simplicity and low cost installations and source materials;

- scaling of the synthesis process;

- the possibility of obtaining nanoparticles of various types;

- the presence of fluid around the plasma limits the possibility of expansion, and contributes to increasing the temperature and pressure that favors the flow of exothermic chemical reactions.

Pulsed electrical discharges in liquids can be realized in two ways. In one case, the pulse energy ≥1 kJ, and the second does not exceed a few joules. The first case requires a rather cumbersome and complicated equipment, the reactor experiences a significant shock load. In addition, the obtained nanoparticles from nanoscale to micron, which requires additional effort on their separation when used in different technologies. A carbon source in such liquids as water are graphite electrodes. In the case of organic liquids supplier of carbon is the liquid itself.

The results of studies on the synthesis of carbon nanoparticles in organic liquids, in particular in ethanol, published by Journal of Physics D: Applied Physics, 43 (32). p.323001. Mariotti, D and Sankaran, RM (2010) Microplasmas for nanomaterials synthesis).

Closest to the proposed method is �], described in the work (Pulsed discharge production of nano - and microparticles in ethanol and their characterization. N. Parkansky, Alterkop V., R. L. Boxman, S. Goldsmith, Barkay Z., Y. Lereah Powder Technology. 2005. T. 150. No. 1. P. 36-41), which uses pulsed arc discharge in ethanol. Into ethanol are placed two electrodes (graphite, Nickel, tungsten, etc.), pulse repetition rate f=100 Hz, the current and voltage I=100-200 A, U=20 V, respectively, the pulse duration τ=30 μs, particles are formed from nanoscale to micron.

The disadvantage of this method is the instability of the colloidal solution (a fairly rapid deposition of sediment), wide size spectrum of particles and a relatively complicated procedure electrical breakdown in ethanol.

The technical result of the invention is simplicity and low cost, the possibility of obtaining nanoparticles of different types. In addition, it should be noted the following advantages of the proposed technical solution:

- multi-electrode high-voltage pulse discharge with injection of inert gas in the interelectrode space allows to form in ethanol ustoichivy nanostructured colloidal solution. There is a certain threshold value of the specific energy deposition (j/cm3) above which the colloidal solution is stable, the property of the solution does not change more than a year. At lower specific energy deposition within 2-3 days occurs in�drop sediment and enlightenment of fluid;

- while heating the solution to boiling temperature and subsequent cooling property of the colloid does not change;

- when current flows through a colloidal solution (electrophoresis) rapid deposition of sediment and fluid enlightenment. Simultaneously, the positive electrode is formed of a nanostructured carbon film;

- the size of the nanoparticles depend on the specific energy deposition. Near the threshold value of the specific energy deposition their size is 5-10 nm, and represent a disordered carbon;

the nanopowder may be separated from the colloidal solution by evaporation or as a result of electrophoresis.

The technical result is achieved in that a method of obtaining a colloidal solution of nanosized carbon is as follows, the organic liquid is fed into a chamber with electrodes, Inuktitut inert gas in the interelectrode space, form a high temperature plasma channel in the gas bubbles, through the atomization of carbon atoms followed by rapid cooling.

In excess of the specific energy deposition in the liquid threshold form a stable colloidal solution. As the organic liquid may be used ethanol.

The drawing shows a device for obtaining a colloidal solution.

We offer m�TOD obtain a stable colloidal solution of nanosized carbon-based implementation of a pulsed high-voltage discharge in bubbles of inert gas, injected into the organic liquid (ethanol). As noted above, a feature of pulsed discharges in ethanol is atomization of carbon in channel with high temperature followed by rapid cooling. Using high voltage multi-electrode discharge device with injection of gas in the interelectrode space due to the specificity of the formation of the plasma channel and its cooling opens up new possibilities for the formation of nanostructures, carbon nanofluids.

Used dielectric chamber 1, a multi-electrode discharge device 3 with the injection of gas in the interelectrode space, located inside the chamber, placed in ethanol 2, which partially fills the chamber. Camera 1 is provided with a device for injection of gas, the fill system and flow through the organic liquid (ethanol). When the discharge device is connected to the high voltage pulse generator 12. The device comprises a pulse generator 5, the Rogowski coil 6, the voltage divider 7, the spectrograph 8, the optical waveguide 9, the nozzles for pumping the fluid 10, the outlet for removal of gas 13.

The device operates as follows.

In a discharge device 3 through the pipe 4 is injected inert gas. To remove it from the reactor is used the pipe 13. After that, the reactor 1 is partially zapalne�Xia liquid, so discharging device 3 was entirely in her. The extreme electrodes of the discharge device, high voltage is applied a predetermined value (U≤20 kV) and pulse frequency (f≤100 Hz). In the case of reactor operation in running mode, the connectors 10 provide the necessary fluid flow. The gas bubbles 11 filled with alcohol vapor, the interelectrode space through the openings 5, pulse discharge occurs. In each of the interelectrode gaps is formed of high temperature plasma channel with a duration of several microseconds with the following parameters: temperature of heavy particles T=4000-5000 K, the electron temperature Te=1-1. 5 eV, the concentration of charged particles n=(2-3)·1017cm3the diameter of the plasma channel hundreds of microns. The energy invested in the discharge during one pulse, ≤2-3 J.

In the plasma channel occurs atomization of carbon atoms. After the termination of the current pulse is rapid expansion of the plasma channel, which leads to rapid cooling ("quenching") and the formation of nonequilibrium nanostructures of carbon, thereby defining characteristics, properties of colloidal solution. The characteristic time of cooling of the discharge channel units, tens of microseconds. Dynamics of heating and cooling of the plasma channel significantly affects the parameters of nanoparticles.

Determining� to obtain a colloidal solution is the specific energy deposition in the treated liquid. In the absence of flow regime specific energy deposition of γ is defined as follows:

γ=WftV,

W is the energy deposited in the discharge during one pulse, f is the pulse frequency, V is the volume of the liquid, t is the time of the treatment fluid.

In the case of flow-through mode:

λ=WfU,

U is the liquid flow rate per unit time (cm3/C). With increasing time of the treatment fluid (specific energy density), the liquid darkens, resulting in the formation of nanoparticles of carbon and when it exceeds a certain threshold value of the specific energy deposition forms a stable colloidal solution (precipitate falls more than one year). At lower values of specific energy deposition within a day or two comes falling out of carbon on the bottom of the vessel, the liquid is illumined.

The parameters of the nanoparticles were investigated by various methods: Raman (Raman scattering), DLS (dynamic light scattering), x-ray diffraction, electron microscopy, elemental composition, etc.

Note that by heating the colloidal solution to a temperature close to the temperature �andsinging, followed by cooling the solution remains stable. The threshold value of the specific energy deposition depends on the material of the electrodes.

The elemental composition of the powder of the nanoparticles obtained by evaporation of the colloidal solution is as follows: C - 79,05%; O - 19,57%, other detected elements are Si; K; Ti; Cr; Fe. The presence of oxygen is the result of its adsorption from the air.

The results can be used for various applications, in particular for producing coatings of metal carbon film to reduce the coefficient of secondary electron emission in the technology of growing diamond films and glass, to create elements that absorb solar radiation, etc.

1. A method of producing a colloidal solution of nano-sized carbon, characterized in that the organic liquid is fed into a chamber with electrodes, Inuktitut inert gas in the interelectrode space, form a high temperature plasma channel in the bubbles of gas containing vapors of the organic liquid, with the following parameters: temperature of heavy particles T=4000-5000K, the electron temperature Te=1-1. 5 eV, the concentration of charged particles n=(2-3)·1017cm3the diameter of the plasma channel hundreds of microns, while atomization of carbon atoms followed by rapid cooling by dlitelnosti a few microseconds.

2. A method according to claim 1, characterized by the fact that in excess of the specific energy deposition in the liquid threshold form a stable colloidal solution.

3. A method according to claim 1 or 2, characterized in that as the organic liquid is ethanol.



 

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