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WO2004112997A1 - Procede et appareil permettant de produire des nanoparticules metalliques - Google Patents

Procede et appareil permettant de produire des nanoparticules metalliques Download PDF

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Publication number
WO2004112997A1
WO2004112997A1 PCT/IN2004/000067 IN2004000067W WO2004112997A1 WO 2004112997 A1 WO2004112997 A1 WO 2004112997A1 IN 2004000067 W IN2004000067 W IN 2004000067W WO 2004112997 A1 WO2004112997 A1 WO 2004112997A1
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WO
WIPO (PCT)
Prior art keywords
electrode
electrodes
nanoparticles
wire
explosion
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/IN2004/000067
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English (en)
Inventor
Prasenjit Sen
Joyee Ghosh
Prashant Kumar
Abdullah Q. Alquadami
Vandana
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JAWAHAR LAL NEHRU UNIVERSITY
Original Assignee
JAWAHAR LAL NEHRU UNIVERSITY
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.)
Filing date
Publication date
Application filed by JAWAHAR LAL NEHRU UNIVERSITY filed Critical JAWAHAR LAL NEHRU UNIVERSITY
Priority to US10/562,641 priority Critical patent/US20070101823A1/en
Publication of WO2004112997A1 publication Critical patent/WO2004112997A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/056—Submicron particles having a size above 100 nm up to 300 nm
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites

Definitions

  • the present invention relates to a novel process for producing metal nanoparticles by electro-explosion of wires. More particularly, the present invention provides a process for the production of nanoparticles comprising exploding wires into small fragments by application of suitable voltages, at low voltages in order to supply energy to the wires such that the nanoparticle size depends upon various controlling parameters such as applied voltages and current densities.
  • the present invention provides a simple, repeatable process to achieve large production volumes for nanoparticles. Background of the invention
  • Nanoparticles have been a source of great interest due to their novel electrical, optical, physical, chemical, magnetic etc. properties. They have significant potential for a wide range of applications including catalysis, magnetic recording media, optoelectronic materials, magnetic fluids, composite materials, fuel cells, pigments and sensors. Their uniqueness arises from their high ratio of surface area to volume (aspect ratio), as these materials have diameters of 100 nm or less.
  • Nanoparticles prepared by physical methods such as vapour deposition and sputtering have high quality, i.e. clean surfaces and uniform particle size distribution.
  • industrial applications for such particles are limited due to the low production rates and high cost.
  • Alternative chemical production methods, such as thermal decomposition and precipitation are currently being studied for the preparation of a wide range of nanoparticles.
  • Chemical methods can provide large quantities of ceramic particles for industrial applications.
  • chemical methods are generally not applied to the production of metallic nanoparticles.
  • the main object of the present invention is to provide a novel process for producing metal nanoparticles by electro-explosion of wires, which obviates the above drawbacks.
  • Another object of the present invention is to produce nanoparticles from conducting parent materials shaped in the form of a wire / plate and are used as electrodes, whereby both electrodes produce the particles.
  • Yet another object of the present invention is to generate nanoparticles through the dominant mechanism of spark explosion, which is an adaptation of the phenomena called electro-explosion of wires.
  • Still another object of the present invention is to use low voltages between 12V-50V DC, while also having the possibility of employing AC voltages for the purpose, thereby reducing the energy costs involved in production of nanoparticles.
  • Still another object of the present invention is to provide for the use of various dense liquids as medium of explosion, irrespective of their dielectric property.
  • Still another object of the present invention is to provide a method by which capping is achieved of the nanomaterials with a suitable layer of an inert material produced around the nanomaterial due to a reactive step in the environment of the medium present.
  • the present invention provides a novel process for the production of metallic nanoparticles based on the electro-explosion of wires in a suitable medium.
  • the present invention relates to a novel process for the production of metallic nanoparticles by way of controlled explosion of the metal in a suitable medium applying voltages of about 12V and above, to two electrodes, one in the form of a wire and another in the form of a plate, so as to achieve a spark between the electrodes, thereby simulating a situation where the wire cross-section is pinched or reduced and whereby high current densities are achieved along the length of the wire, instantaneously exploding the electrodes by sending shock waves through the bulk of the material, melting them and dispersing them to form small fragments which are then collected by a suitable medium in which the process is initiated, not only for efficient recovery of the material but also to form a protective layer around the now highly reactive nanomaterial so to prevent the nanomaterials from coalescing into large particles by forming a cap, wherein the capping efficiency is determined by the combination
  • the present invention provides a process for the production of metallic nanoparticles by the controlled electro-explosion of a metallic wire in a suitable medium comprising: i. applying a voltage of greater than 12V to a first electrode and a second electrode, both said first and said second electrodes being formed of the metal whose nanoparticles are desired, said first electrode being in the form of a plate, and said second electrode being in the form of a wire, so as to achieve a spark between the said first and second electrodes, thereby simulating a situation where the second electrode cross-section is pinched or reduced and whereby high current densities are achieved along the length of the second electrode, ii.
  • the present also provides an apparatus for the production of metallic nanoparticles by the controlled electro-explosion of a metallic wire in a suitable medium which comprises a reaction vessel containing said medium, a first and second electrodes mounted inside said vessel, submerged in said medium, said first and second electrodes being formed of a metal whose nanoparticles are desired, said first electrode being in the form of a plate, and said second electrode being in the form of a wire, so as to achieve a spark between the said first and second electrodes, thereby simulating a situation where the second electrode cross-section is pinched or reduced and whereby high current densities are achieved along the length of the second electrode, said electrodes being connected to a power source so that current is passed through said electrodes, instantaneously exploding both said first and second electrodes by sending shock waves through the bulk of the material, thereby melting the electrodes and dispersing them to form said nanoparticles of said metal.
  • said first electrode is mounted wherein said first electrode is mounted perpendicular to the base of said reactor.
  • said first electrode is mounted in said reaction vessel through stainless steel slides on an insulating block
  • said insulating block is a plastic block.
  • said second electrode is mounted in said reaction vessel through a guide.
  • the guide is preferably, an "L" shaped glass tube, mounted through an insulating mounting means fixed in said reaction vessel.
  • the "L" shaped glass tube is mounted on said insulating mounted means such that it collimates said second electrode, passing therethrough to strike said first electrode along its normal.
  • the nanomaterials that have been realized are independent particles, comparable in size to other nanomaterials reported in the prior art literature.
  • the process is very energy intensive since only relatively low voltages are applied, and also results in high volumes of nanoparticles being produced since both electrodes are consumed.
  • the present invention provides a novel process for producing metal nanoparticles by electro-explosion of wires which comprises placing a wire and a plate of the same material in a dense medium, preferably water, in such a manner so as to guide the wire in a straight line to make contact with the plate intermittently.
  • a potential difference of 12V - 48V DC, preferably 36V DC, is apphed between the plate and the wire so as to produce explosion when brought into contact with each other to achieve the desired nanoparticles.
  • the cross-section of wires employed are in the range of 0.4411 x 10 "5 cm 2 - 1.7721 x 10 "5 cm 2 to carry current in the range of 0.96 x 10 6 A/m 2 - 77.6 x 10 6 A/m 2 to obtain the desired nanoparticles after explosion.
  • all metals capable of maintaining a current density of 10 5 A/m 2 or higher is amenable to production of nanomaterials, whose size are in the range of a few nanometers, and whose examples are transition metals such as Fe and Cu, noble metals such as Ag and Group HI metals such as Al.
  • Figure 1 is a depiction of a Z-pinch obtained in a wire due to the self-inductive interactions between the circuit elements resulting in the development of an axial force.
  • Figure 2 is a top view of the wire guide for carrying out the process of the invention.
  • Figure 3 is a front view of the wire guide for carrying out the process of the invention.
  • Figure 4 is a schematic view of the reaction vessel used for carrying out the process of the invention.
  • Figure 5 shows the AFM data collected for nano-crystalline copper particles allowing for the recording of particles in the range 27nm - 72nm.
  • Figure 6 shows the XRD data of bulk and nanoparticles of copper.
  • Figure 7 shows the AFM data collected for nano-crystalline silver particles allowing for the recording of particles in the range 50nm - 200nm.
  • Figure 8 shows the XRD data of bulk and nanoparticles of silver.
  • Figure 9 shows the AFM data collected for nano-crystalline iron particles allowing for the recording of particles in the range lOnm - 50nm.
  • Figure 10 shows the XRD data of bulk and nanoparticles of iron.
  • Figure 11 shows the AFM data collected for nano-crystalline aluminium particles allowing for the recording of particles in the range 40nm - 150nm.
  • Figure 12 shows the XRD data of bulk and nanoparticles of aluminium.
  • the pres'ent invention provides metal nanoparticles made by the novel process of the present invention as detailed below.
  • EEW The exploding wire technique, EEW was basically the guiding principle behind the actual experimental arrangement to synthesise nanopowders of Cu, Fe, Al and Ag metals.
  • the current I should be very large, i.e. very high current density is required for the explosion process, which basically gives rise to some non-linearity in the volt-ampere characteristics.
  • the initial stage of EEW is a Z-pinch which essentially decreases the cross- sectional area of contact to 1/100th of the rest of the conductor, thereby tremendously increasing the current density which is required for explosion to take place, whenever contact was made and broken. • The medium which is to be used for doing the explosion.
  • an inert atmosphere is suitable as a medium, one which does not interact with the plasma formed during the explosion, e.g. butanol, heavy oils, etc.
  • Oxygen or any other active medium is not suitable since with mobile carriers they form compounds.
  • the process of exploding the wire on the plate can take place using a DC current performing an instantaneous connection - disconnection. This is equivalent to . using AC current source at a wide range of frequencies.
  • the present invention also discloses a portable apparatus for carrying out the explosion.
  • the apparatus is both simple and efficient and resulted in production of large quantities of nanoparticles.
  • the wire guide (as shown in Figures 2 and 3) was prepared by the following method
  • a one inch plastic rod of 4cm diameter was cut into two equal halves. Two perpendicular holes were drilled through one and the portion was cut open to fix a 5mm diameter glass bent tube (90° bent) in that place. This served as the wire guide through which the wire can be passed. This collimates the wire to go and strike the metal plate without bending in its way.
  • Glass beaker cutting A wire with its two free ends, each connected to a terminal of the battery was looped around the glass beaker along the mark at which the cut was to be done. Without touching the two ends, they were held tightly - then current was passed through the wire. It became red hot and the glass beaker got cut along that mark.
  • Etching of the metal plate Before the plate could be used for the explosion, its surface should be chemically clean and smooth. For this the plate was etched. Etching was done in nitric acid in case of copper, nitric acid mixed with a few drops of hydrofluoric acid in case of iron and sodium hydroxide solution in case of aluminium. Silver wires of a required diameter were ordered. Nitric acid was poured in a beaker containing water to obtain a dilute solution. Then the plate was immersed in it and after sometime a clean metallic surface resulted. It was rinsed in distil water and dried. The explosion was carried out for a range of voltages from 12 V to 48V. The minimum battery voltage available was 12 volts, so two and three such batteries were connected in series to meet the voltage requirements as needed.
  • the electro-explosion of wires is carried out employing a reaction vessel (1) prepared to house the electrodes (2, 2') and the medium (3) in which the explosion is carried out.
  • the wire (2') is aligned to the correct geometry through the wire guide (5).
  • the voltages required for the purpose of exploding the wire is provided by a bank of batteries (4) operating under the condition of an ideal current source.
  • the plates (2) and wires (2') are cleaned through acid etching and the same method is employed to control the cross-section of the wires.
  • the Al wires and plates were etched with a 10% solution of NaOH.
  • Graneau Graneau 's emphasis that the fractures are tensile in character, whereas pinch forces are compressive and could not cause wire fragmentation of the form observed, but his theoretical account did not explain why the wire breaks into as many as 50 fragments. Each of these fragments is of insufficient length to develop adequate force.
  • the applied emf and the potential drop are no longer in balance. Their difference can be measured experimentally and can account for an axial force in the line of current flow.
  • the positive atomic lattice of the conductor is subject to the full intensity E, as are the electrons, but the electrons has an additional role. They not only act as a catalyst in transferring,/ momentum to the lattice by collisions, but they also transfer momentum to whatever it acts as a store for the energy associated with the magnetic induction process.
  • the field medium is closely coupled with the collective electron action and this field can assert forces in its interaction with charge in matter.
  • the force will be axial force acting between the conductor and the field induced in the observer's reference frame by the electron motion. Such a force can cause rupture of the conductor if the current build up is rapid enough, but it cannot separate the conductor body from the electron population. All that can be expected is that the conductor will disintegrate into elements, which are contained during the explosion within the plasma formed by the current discharge. The reason for this is that the force acting on each positive element of the atomic lattice of the conductor will not, in general, be the same throughout the conductor. The quantitative analysis fully supports this explanation.
  • the novelty and inventive step of the process of the patent resides in making metal nanoparticles dispersed in a dense medium through the electro-explosion of wires.
  • a reaction vessel for preparation of nanomaterials employing the exploding wire technique was constructed out of glass with an arrangement for mounting a copper metal plate (electrode 1) perpendicular to the base of the reactor.
  • a wire guide arrangement is placed so that a copper wire (electrode 2), while passing through the guide, approaches the plate along its normal.
  • the metal plate and the wire form the two electrodes which is connected to a battery bank allowing for supply of voltages starting at 12 V and going up to 48V in incremental steps of 12 V.
  • the reactor vessel is filled up with a suitable dense medium so as to completely immerse electrode 2 and 66% of electrode 1.
  • Electrode 2 is brought into contact with electrode 2 to achieve an explosion, following which the current naturally falls to zero. This signals the start of a new explosion sequence whereby the process is repeated.
  • the exploded metal particles remain suspended in the dense medium which is collected in the following manner.
  • An initial centrifuge of the suspension at 5000 RPM separates the fluid from the solid mass. While the former is rejected, the solid mass is dispersed in electronic grade acetone for further AFM analysis.
  • AFM analysis was carried out in the contact mode employing a silicon ultralever having a force constant of 0.2 N/m. The contact force was set at 10.4 nN for all topography data collected with the AFM.
  • the nanoparticles dispersed in acetone was spread on single crystalline silicon (100).
  • Figure 5 shows the AFM data collected for nano-crystalline copper particles allowing for the recording of particles in the range 27nm - 72nm.
  • a reaction vessel for preparation of nanomaterials employing the exploding wire technique was constructed out of glass with an arrangement for mounting a silver metal plate (electrode 2) perpendicular to the base of the reactor.
  • a wire guide arrangement is placed so that a silver wire (electrode 2'), while passing through the guide, approaches the plate along its normal.
  • the metal plate and the wire form the two electrodes which is connected to a battery bank allowing for supply of voltages starting at 12 V and going upto 48 V in incremental steps of 12 V.
  • the reactor vessel is filled up with a suitable dense medium so as to completely immerse electrode 2 and 66%> of electrode 1.
  • Electrode 1 connected to the positive terminal of the battery and electrode 2 to the negative terminal. Electrode 2' is brought into contact with electrode 2 to achieve an explosion, following which the current naturally falls to zero. This signals the start of a new explosion sequence whereby the process is repeated.
  • the exploded metal particles remain suspended in the dense medium which is collected in the following manner.
  • An initial centrifuge of the suspension at 5000 RPM separates the fluid from the solid mass. While the former is rejected, the solid mass is dispersed in electronic grade acetone for further AFM analysis.
  • AFM analysis was carried out in the contact mode employing a silicon ultralever having a force constant of 0.2 N/m. The contact force was set at 10.4 nN for all topography data collected with the AFM.
  • the nanoparticles dispersed in acetone was spread on single crystalline silicon (100).
  • Figure 7 shows the data collected for nano-crystalline silver particles allowing for the recording of particles in the range 50nm - 200nm.
  • a reaction vessel for preparation of nanomaterials employing the exploding wire technique was constructed out of glass with an arrangement for mounting an iron metal plate (electrode 2) perpendicular to the base of the reactor.
  • a wire guide arrangement is placed so that an iron wire (electrode 2'), while passing through the guide, approaches the plate along its normal.
  • the metal plate and the wire form the two electrodes which is connected to a battery bank allowing for supply of voltages starting at 12 V and going upto 48 V in incremental steps of 12 V.
  • the reactor vessel is filled up with a suitable dense medium so as to completely immerse electrode 2 and 66% of electrode 1.
  • Electrode 1 connected to the positive terminal of the battery and electrode 2 to the negative terminal. Electrode 2 is brought into contact with electrode 1 to achieve an explosion, following which the current naturally falls to zero. This signals the start of a new explosion sequence whereby the process is repeated.
  • the exploded metal particles remain suspended in the dense medium which is collected in the following manner.
  • An initial centrifuge of the suspension at 5000 RPM separates the fluid from the solid mass. While the former is rejected, the solid mass is dispersed in electronic grade acetone for further AFM analysis.
  • AFM analysis was carried out in the contact mode employing a silicon ultralever having a force constant of 0.2 N/m. The contact force was set at 10.4 nN for all topography data collected with the AFM.
  • the nanoparticles dispersed in acetone was spread on single crystalline silicon (100).
  • Figure 9 shows the data collected for nano-crystalline iron particles allowing for the recording of particles in the range lOnm - 50nm.
  • a reaction vessel for preparation of nanomaterials employing the exploding wire technique was constructed out of glass with an arrangement for mounting an aluminium metal plate (electrode 2) perpendicular to the base of the reactor.
  • a wire guide arrangement is placed so that an aluminium wire (electrode 2'), while passing through the guide, approaches the plate along its normal.
  • the metal plate and the wire form the two electrodes which is connected to a battery bank allowing for supply of voltages starting at 12 V and going upto 48 V in incremental steps of 12 V.
  • the reactor vessel is filled up with a suitable dense medium so as to completely immerse electrode 2 and 66% of electrode 1.
  • Electrode 1 connected to the positive terminal of the battery and electrode 2 to the negative terminal. Electrode 2 is brought into contact with electrode 1 to achieve an explosion, following which the current naturally falls to zero. This signals the start of a new explosion sequence whereby the process is repeated.
  • the exploded metal particles remain suspended in the dense medium which is collected in the following manner.
  • An initial centrifuge of the suspension at 5000 RPM separates the fluid from the solid mass. While the former is rejected, the solid mass is dispersed in electronic grade acetone for further AFM analysis.
  • AFM analysis was carried out in the contact mode employing a silicon ultralever having a force constant of 0.2 N/m. The contact force was set at 10.4 nN for all topography data collected with the AFM.
  • the nanoparticles dispersed in acetone was spread on single crystalline silicon (100).
  • Figure 11 shows the data collected for nano-crystalline aluminium particles allowing for the recording of particles in the range 40nm - 150nm.
  • Nanoparticles from conducting parent materials which can be shaped in the form of a wire/plate can be used. In this case both electrodes produce the particles.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

L'invention concerne un procédé et un appareil permettant de produire des nanoparticules métalliques par électro-explosion de fils. L'invention consiste à placer un fil et une plaque du même matériau dans un milieu dense, de préférence de l'eau, pour qu'elles fassent office d'électrodes, à guider le fil dans une ligne droite et à appliquer à ces électrodes une tension supérieure à 12V afin de provoquer l'explosion du fil en nanoparticules.
PCT/IN2004/000067 2003-06-25 2004-03-22 Procede et appareil permettant de produire des nanoparticules metalliques Ceased WO2004112997A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US10/562,641 US20070101823A1 (en) 2003-06-25 2004-03-22 Process and apparatus for producing metal nanoparticles

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IN840/DEL2003 2003-06-25
IN840DE2003 2003-06-25

Publications (1)

Publication Number Publication Date
WO2004112997A1 true WO2004112997A1 (fr) 2004-12-29

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US (1) US20070101823A1 (fr)
WO (1) WO2004112997A1 (fr)

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WO2005080030A3 (fr) * 2004-02-20 2006-11-16 Maciej Pike-Biegunski Colloide, procede de fabrication d'un colloide ou de ses derives et ses applications
WO2007024067A1 (fr) * 2005-08-26 2007-03-01 Korea Electro Technology Research Institute Procede de fabrication de poudre nanostructuree par explosion electrique dans un liquide et dispositif de fabrication associe
WO2010024474A1 (fr) * 2008-08-25 2010-03-04 University Of Ulsan Foundation For Industry Cooperation PROCÉDÉ DE PRODUCTION DE POUDRE COMPOSITE DE WC-Co
EP2402389A2 (fr) 2010-07-02 2012-01-04 Eckart GmbH Mousse rigide de polystyrène comprenant des pigments revêtus contenant de l'aluminium , procédé pour sa pröparation et son utilisation.
US8361505B1 (en) * 2006-06-28 2013-01-29 Perry Stephen C Method and apparatus for producing a stable sub-colloidal nano-phase silver metal hydrosol
CN103097588A (zh) * 2010-07-19 2013-05-08 莱顿大学 一种制备金属纳米颗粒或金属氧化物纳米颗粒的方法
WO2017164802A1 (fr) * 2016-03-22 2017-09-28 Sht Smart High-Tech Ab Procédé et appareil permettant la fabrication de nanoparticules à grande échelle

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