WO2015074161A1 - Système et procédé continu basé sur une décharge d'arc non immergé, sous atmosphère contrôlée, pour la production d'un matériau nanométrique - Google Patents

Système et procédé continu basé sur une décharge d'arc non immergé, sous atmosphère contrôlée, pour la production d'un matériau nanométrique Download PDF

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Publication number
WO2015074161A1
WO2015074161A1 PCT/CL2014/000056 CL2014000056W WO2015074161A1 WO 2015074161 A1 WO2015074161 A1 WO 2015074161A1 CL 2014000056 W CL2014000056 W CL 2014000056W WO 2015074161 A1 WO2015074161 A1 WO 2015074161A1
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WO
WIPO (PCT)
Prior art keywords
electric arc
material according
production
nanometric material
controlled atmosphere
Prior art date
Application number
PCT/CL2014/000056
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English (en)
Spanish (es)
Inventor
Manuel Francisco MELÉNDREZ CASTRO
Paulo Andrés FLORES VEGA
Carlos Andrés MEDINA MUÑOZ
Eduardo Gerardo PÉREZ TIJERINA
Original Assignee
Universidad de Concepción
Priority date (The priority date 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 date listed.)
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Application filed by Universidad de Concepción filed Critical Universidad de Concepción
Publication of WO2015074161A1 publication Critical patent/WO2015074161A1/fr

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    • 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
    • B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • B82B3/0009—Forming specific nanostructures
    • B82B3/0033—Manufacture or treatment of substrate-free structures, i.e. not connected to any support
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
    • C01G1/02—Oxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/02—Oxides; Hydroxides
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
    • B01J2219/0822—The electrode being consumed
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
    • B01J2219/0824—Details relating to the shape of the electrodes
    • B01J2219/0826—Details relating to the shape of the electrodes essentially linear
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
    • B01J2219/0837—Details relating to the material of the electrodes
    • B01J2219/0841—Metal
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0869—Feeding or evacuating the reactor
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0881—Two or more materials
    • B01J2219/0886—Gas-solid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44—Carbon
    • C09C1/48—Carbon black
    • C09C1/485—Preparation involving the use of a plasma or of an electric arc

Definitions

  • the technology is oriented to the chemical area, more specifically, it corresponds to a system and a process for the continuous production of nanometric material.
  • the arc discharge generates a plasma at high temperatures that involves highly reactive metal atoms, which in the presence of an oxidizing or reducing gas can react producing growing structures.
  • the principle is simple and is based on generating a short circuit between two precursor materials until plasma generation is controlled at a constant speed, angles and voltage.
  • This method can be used with dry or submerged arc, for the first case it presents as disadvantages that the equipment only has a variable electrode and does not incorporate an accumulation chamber, so the reaction chamber acts as both.
  • the synthesized material is then mixed with the residue of the anode or the cathode that is deposited in the bottom of the reaction chamber (quartz chamber), making its separation difficult. Overheating of the system leads to pressure loss, so it is likely that in the case of the synthesis of oxide nanostructures mixtures of metal and oxidized structures are obtained.
  • the process is not continuous and the thickness of the 00056
  • the anode ends at a point to reduce the operating voltage of the system, when this is carried out, the arc generated splits the tip due to overheating which happens quickly. This is very counterproductive due to the loss of efficiency of the equipment and the poor performance of the reaction.
  • the second case like dry synthesis, is not conditioned a separation of the accumulation chamber with the reaction chamber, which leads to producing mixtures of residue with the synthesized material.
  • the residual material remains in the same solution where the dispersed nanostructures are found, making it difficult to separate them.
  • This system is simple in operation and can be of the compact or integrated type, depending on the purpose for which it is required. It is safe, non-polluting, efficient with a conversion capacity greater than 90% and empowers production from reusable waste. In addition, it allows to expand the field of action since it not only facilitates the elaboration of nanostructures of the nickel, zinc, copper and aluminum type, but also allows the production of nanometric alloys or bimetallic particles and even doped oxides.
  • the safety of the system is based mainly on the fact that it has closed areas and the joints between the reaction chamber and the accumulation are also tightly closed, therefore there are no material leaks in the synthesis process, which makes it safe and secure. non-polluting.
  • the reaction zone that could be considered the most dangerous, since it is where the electric arc discharge occurs, is well conditioned with a robust chamber and electrically isolated from the arc by means of a polymeric connection piece, which would avoid a possible electric shock out of the camera.
  • the system for the continuous production of nanometric material consists of 3 sections: (a) feeding, (b) discharge and reaction, and (c) accumulation and relaxation.
  • Figure 1 shows the parts that make up the different sections of the system, where (a) corresponds to the welders, (b) to the precursor "1", (c) to the precursor "2" , (d) at the gas inlet, (e) at the voltage source, (f) at the flow of oxygen, (g) at the precursor material, (h) at the electric arc, (i) at the nanoparticles, (j ) to the gas inlet that can be of the nitrogen, oxygen or argon type, and (k) corresponds to a vacuum valve.
  • This section is composed of welding equipment (welders) located in parallel, which must be joined by means of starting triggers of both welders to work at the same time, which operate between 30 - 80 amps.
  • This section also includes the gas feeders and their respective system of digital flow controllers that operate up to 500 mlJmin.
  • the thickness of the precursor electrodes is between 1-2 mm, allowing low voltages to be used, which decreases the consumption capacity of the equipment.
  • the reaction chamber made of stainless steel, preferably has a longitudinal shape since it benefits the movement of the particles and better resists internal pressures. It is also provided on the outside by a cooling system that prevents overheating of the reaction and discharge zone, which prevents the chamber from melting.
  • FIG. 2 A detail of the parts that make up the chamber is shown in Figure 2, where: (I) corresponds to copper electrodes where the precursor passes; (m) a stainless steel conveyor gas tube, which is located at least 2 cm from the arc zone to facilitate oxidation of the nanoparticles; (n) corresponds to an insulating polymer having a preferred shape of the cylinder type; (o) is a stainless steel cover, which is screwed into the reaction chamber and supports the electrodes, the insulating polymer and the connectors to the power source (welders); and (p) is the body (cover) of the stainless steel reaction chamber.
  • the feed system of the precursor material and the gases that produce the reaction is formed by the copper extension (I) and the gas injector (m), where the copper extensions (I) are the guides of the precursor material from welding machines.
  • the copper extensions (I) are the guides of the precursor material from welding machines.
  • "ground" wires of the welders are connected in such a way to allow the flow of electric current at the time of the arc discharge.
  • These connections are attached to the cover (o) by means of the polymeric connector (n), which allows the tips to be electrically insulated with the rest of the reaction chamber.
  • This connector (n) corresponds to an insulating polymer of the acetal type with a cylindrical shape, capable of withstanding the high temperatures that occur inside the reaction chamber, and whose purpose is the aligned maintenance of the precursor material feed system.
  • the cover (o) and the tube-shaped gas injector (m) are made of stainless steel and M10 bolts are attached, in order to avoid leaking nanoparticles to the outside.
  • Said tube (m) has a perforation of between 20-30 mm at the end where the reaction chamber ends, to guide the flow of the nanoparticles to the accumulation chamber, in addition to preventing an overpressure of the system, allowing its operation in the form keep going.
  • the precursor materials from the feed section are directed to the interior of the reaction chamber at a speed between 1 - 13 m / min, in addition a gas flow that can be the type 0 2 , N 2 is introduced or Ar, which operates at atmospheric pressure and at a flow between 50-500 mL / min that enters through the gas injector (m).
  • a gas flow that can be the type 0 2 , N 2 is introduced or Ar, which operates at atmospheric pressure and at a flow between 50-500 mL / min that enters through the gas injector (m).
  • the precursors are introduced horizontally and continuously to the electric arc reaction chamber.
  • the equipment is empowered for continuous production and 90% efficiency, where the reaction occurs through pulses to prevent the electrodes from burning.
  • the pulses operate in a 2: 1 ratio for on (power on) and off (power off), with a maximum of up to 20 seconds on, c- Accumulation and relaxation section:
  • the synthesized nanostructures are transported with a constant gas flow to the accumulation and relaxation section by means of a quartz tube (transparent and resistant) that has a diameter that varies between 8-12 cm, which is located from the end of the reaction chamber to the accumulation chamber, through a surface charge acceleration system (ASC) to prevent radiation leakage.
  • This acceleration system corresponds to a conventional furnace, which operates between 10 - 1000 watts of power, and which is conditioned in the lateral areas by two holes with a diameter between 8 - 12 cm, and which is located perpendicular to the magnetron of microwave.
  • the microwave is placed in a box of carbon fibers and the holes must be sealed with a special epoxy resin type material, which blocks the microwaves.
  • the ASC also has a security system based on 2 microwave leak detectors, which provide an alarm when leaks are greater than 2 watt / m 2 .
  • a detail of the ASC system is shown in Figure 4, where (q) corresponds to the connector to the reaction chamber; (r) is the connector to the accumulation chamber; (s) represents the quartz tube; (t) corresponds to microwave detectors; (u) is a microwave blocking mesh; (v) is the carbon fiber box; and (w) corresponds to the microwave.
  • the nanostructures remain in the accumulation and relaxation chamber for 30-60 min.
  • This section physically corresponds to a chamber commonly referred to as a glove box, made of materials with particularities such as transparency and resistance, such as acrylic.
  • This chamber is fitted on its sides with cavities provided with neoprene gloves in order to facilitate the manipulation of the nanostructures at the time of extraction.
  • the system is provided with conventional microwave magnetrons with variable power. They correspond to an intermediate passage where the quartz tube passes through the inside of a perforated microwave before reaching the accumulation chamber.
  • the feeding section allows the continuity of the equipment to be supplied by supplying the precursor material.
  • the precursor material is conducted inside an insulating conduit to the discharge chamber, the conveyor tube is electrically isolated from the material and connected to the power source.
  • zinc oxide nanoparticles (Zn02) were obtained, according to the following reaction:
  • the precursor wire used had a purity of 99.99% (Sulzel metco) with a diameter of 2.0 mm, and the precursor gas was supplied by Linde.
  • the wire speed was adjusted in 1.5 m / minutes and the gas flow was 500 mL / min.
  • the power source (welders) was adjusted to a voltage of 40 -60 V.
  • the wire was introduced into the adjusted and synchronized welding machine, so that its passage was not interrupted at the time of the arc. .
  • the terminal points where the electric arc is made were adjusted to the electrodes to prevent them from moving during the reaction process.
  • the surface charge acceleration system was connected and turned on.
  • the accumulation chamber was previously cleaned and sealed to prevent the nanometric dust from being lost.
  • the system was tuned for the reaction (wire speed, gas flow, controllers and welding machines on, accelerator and microwave leak detectors on).
  • the reaction chamber operated at room temperature at the beginning of the arc reaction, which was carried out by pulses of 10 seconds and resting pulses of 5 seconds for a total of 100 seconds. After the electric arc, the interior of the chamber increased the temperature to 500 ° C, which was controlled by the heat exchange cooling system that the walls of the reaction chamber possess, where water was used as a refrigerant.
  • Figure 3 shows two views of the zinc oxide nanoparticles obtained, where the size of these was distributed between 20-40 nm.
  • the non-reactive material and the nanometric material produced was heavy, obtaining a conversion rate of 95%.
  • 100 seconds of reaction 37 grams of metallic Zn were used and 33.3 grams of particularized nano zinc oxide were obtained.

Abstract

Système à arc électrique sous atmosphère contrôlée fonctionnant en mode continu pour la production d'un matériau nanométrique, comprenant les éléments constitutifs suivants: (a) une section d'alimentation formée par des dispositifs de soudage, des électrodes précurseurs et des distributeurs de gaz; (b) une section de décharge et de réaction dans laquelle se déroule la réaction d'arc électrique, constituée par une enceinte de réaction en acier inoxydable et de forme longitudinale pour favoriser le déplacement des particules; et (c) un système d'accélération de charge superficielle (ASC); et (d) une section d'accumulation et de relaxation où se termine le processus de nucléation et de croissance des nanostructures, et qui est constituée par une enceinte présentant sur les côtés des ouvertures pourvues de gants et d'un élément de jonction en quartz. L'invention concerne en outre le procédé d'obtention d'un matériau nanométrique à partir dudit système à arc électrique.
PCT/CL2014/000056 2013-11-21 2014-10-22 Système et procédé continu basé sur une décharge d'arc non immergé, sous atmosphère contrôlée, pour la production d'un matériau nanométrique WO2015074161A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CL2013003340A CL2013003340A1 (es) 2013-11-21 2013-11-21 Sistema con arco electrico en atmosfera controlada, que comprende una seccion de alimentacion, una seccion de descarga y reaccion, seguida de un sistema de aceleracion de carga superficial, que conduce a una seccion de acumulacion y relajacion; y proceso continuo para la produccion de material nanometrico en dicho sistema.
CL3340-2013 2013-11-21

Publications (1)

Publication Number Publication Date
WO2015074161A1 true WO2015074161A1 (fr) 2015-05-28

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PCT/CL2014/000056 WO2015074161A1 (fr) 2013-11-21 2014-10-22 Système et procédé continu basé sur une décharge d'arc non immergé, sous atmosphère contrôlée, pour la production d'un matériau nanométrique

Country Status (2)

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CL (1) CL2013003340A1 (fr)
WO (1) WO2015074161A1 (fr)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6638403B1 (en) * 2000-07-07 2003-10-28 Hitachi, Ltd. Plasma processing apparatus with real-time particle filter
US6794599B2 (en) * 2001-03-01 2004-09-21 Sony Corporation Device and method for manufacture of carbonaceous material
JP3803757B2 (ja) * 2003-09-24 2006-08-02 独立行政法人物質・材料研究機構 超微粒子作製装置
US7153398B2 (en) * 2001-06-01 2006-12-26 Euronano Spa Method for producing fullerene-containing carbon and device for carrying out said method
US7306503B2 (en) * 2002-10-18 2007-12-11 Canon Kabushiki Kaisha Method and apparatus of fixing carbon fibers on a substrate using an aerosol deposition process
US7666381B2 (en) * 2003-06-10 2010-02-23 Plasmet Corporation Continuous production of carbon nanomaterials using a high temperature inductively coupled plasma
US8071906B2 (en) * 2002-05-09 2011-12-06 Institut National De La Recherche Scientifique Apparatus for producing single-wall carbon nanotubes

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6638403B1 (en) * 2000-07-07 2003-10-28 Hitachi, Ltd. Plasma processing apparatus with real-time particle filter
US6794599B2 (en) * 2001-03-01 2004-09-21 Sony Corporation Device and method for manufacture of carbonaceous material
US7153398B2 (en) * 2001-06-01 2006-12-26 Euronano Spa Method for producing fullerene-containing carbon and device for carrying out said method
US8071906B2 (en) * 2002-05-09 2011-12-06 Institut National De La Recherche Scientifique Apparatus for producing single-wall carbon nanotubes
US7306503B2 (en) * 2002-10-18 2007-12-11 Canon Kabushiki Kaisha Method and apparatus of fixing carbon fibers on a substrate using an aerosol deposition process
US7666381B2 (en) * 2003-06-10 2010-02-23 Plasmet Corporation Continuous production of carbon nanomaterials using a high temperature inductively coupled plasma
JP3803757B2 (ja) * 2003-09-24 2006-08-02 独立行政法人物質・材料研究機構 超微粒子作製装置

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