WO2006076534A2 - Procede permettant de preparer de particules composites presentant des caracteristiques de surface sur mesure - Google Patents

Procede permettant de preparer de particules composites presentant des caracteristiques de surface sur mesure Download PDF

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WO2006076534A2
WO2006076534A2 PCT/US2006/001165 US2006001165W WO2006076534A2 WO 2006076534 A2 WO2006076534 A2 WO 2006076534A2 US 2006001165 W US2006001165 W US 2006001165W WO 2006076534 A2 WO2006076534 A2 WO 2006076534A2
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process according
solvent
dispersant
group
metal
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PCT/US2006/001165
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WO2006076534A3 (fr
WO2006076534B1 (fr
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John Oliver Freim
Clint Ronald Bickmore
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Onmaterials, Llc
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Publication of WO2006076534B1 publication Critical patent/WO2006076534B1/fr

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    • 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
    • B22F1/17—Metallic particles coated with metal
    • 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
    • B22F1/18—Non-metallic particles coated with metal
    • 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
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/045—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by other means than ball or jet milling
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Definitions

  • Materials have properties that can be ascribed to either surface or bulk characteristics. These parameters include catalytic activity, electrical and thermal conductivity, optical, electronic, chemical and mechanical properties. Particles with metallic exteriors of tailored compositions and thickness can exploit these properties while providing control over other properties such and density, material cost and particle behavior.
  • zero valent metals may be useful as fillers, such as those for thermal and electrical conductivity, capacitance, charge dissipation and electromagnetic interference and absorbance.
  • Such metals also may be used as magnetic and/or luminescent materials, taggants, pigments, conductive inks and coatings, sensors, dopants, alloys, sintering aids, and catalysis supports such as in fuel cells and batteries, for example.
  • zero valent metals may be useful for infrared missile decoys, for example as chaff or pyrophoric tracers.
  • Electrochemical reactions include those that convert toxic chemical compounds into innocuous products.
  • halogenated chemical compounds such as trichloroethylene and carbon tetrachloride
  • hydrocarbons such as ethane and methane, for example.
  • toxic compounds such as chromium (VI) (Cr +6 ), lead (II) (Pb +2 ) and arsenic (V) (As +5 ), for example, can be converted to compounds having less toxic oxidation states or aqueous solubility.
  • zero valent metals have a wide variety of uses in the field of remediation, such as in ex-situ and in-situ electrochemical reduction, and in ex-situ and in-situ immobilization.
  • the foregoing examples provide only an indication of the wide variety of uses for zero valent metals, such uses being clearly understood and appreciated by any person having ordinary skill within arts utilizing metal particles.
  • a promising in-situ remediation protocol uses zero valent metals that are injected into the subsurface where they react with and destroy the targeted contaminants. It is difficult or impossible to transport coarse microscale particles through the subsoil as the particles settle ⁇ l ⁇ M ⁇ ..&m ⁇ $Mw ⁇ M ⁇ Mfa ⁇ ' MM$ i ⁇ Q r ⁇ c
  • Zero valent metal particles are typically microscale with dimensions greater than one micrometer and these large particles offer a low specific surface area.
  • spray atomized and electrolytic iron particles typically offer dimensions greater than 10 micrometers and have an active surface area of only about 0.1 to 0.2 m 2 /g.
  • Carbonyl iron particles that are produced by condensation from the vapor phase typically offer dimensions of 1 to 10 micrometers and have an active surface area of only about 0.5 to 1 m 2 /g.
  • the large particle size makes this product unsuitable for many applications including in- situ remediation, for example.
  • Nanoscale zero valent metal particles having a surface area in excess of 20 m 2 /g has been produced by various methods.
  • One method involves the electrochemical reduction of a metal salt solution in water. Equation (2) shows the electrochemical reduction of a trivalent iron ion with a borohydride ion.
  • the particles also have residual boron that is undesirable for some applications. These particles also tend to form aggregates of smaller particles. Aggregated particles still provide a high surface area but behave like coarse particles when injected underground and offer less than ideal sub-surface mobility.
  • Another method that is employed to make high surface area zero valent metal involves the thermal reduction of a metal oxide.
  • the metal oxide particles are heated in a reducing atmosphere (typically hydrogen or carbon monoxide) to produce zero valent metal.
  • a reducing atmosphere typically hydrogen or carbon monoxide
  • An example is provided in equation (3) and involves the reaction of hematite (Fe 2 ⁇ 3) with hydrogen gas.
  • Another method for producing zero valetit metal particles involves the chemical precipitation of zero valent iron onto the surface of an inert carrier particle, as described in U.S. Patent No. 6,689,485.
  • Using iron salt and borohydride precursors in water and a reaction similar to that shown in equation (2) produces nanocrystalline iron deposits on the carrier surface.
  • This procedure also offers the disadvantages of expensive chemical precursors and difficulties in scaling the process.
  • the present invention is a cost-effective and scalable technique for producing sub- micrometer and nanocrystalline zero valent metal particles and particle suspensions by depositing metal onto the surface of a carrier particle.
  • the particles typically offer a surface area of greater than 5 m 2 /g and can be inexpensively produced on a large scale. Moreover the particles have reactivity superior to currently available microscale metal particles.
  • Figure l(a) depicts a carrier particle (010) prior to mixing with metal.
  • Figure 1 (b) depicts a carrier particle (010) with a metal surface layer (Oil).
  • Figure 2 is a scanning electron microscope (SEM) picture of particles produced by mechanical attrition of coarse iron particles.
  • Figure 3 is a scanning electron microscope (SEM) picture of particles produced according to the methods disclosed herein.
  • Figure 4 is a scanning electron microscope (SEM) picture of particles produced by thermal reduction.
  • Equation (6) depicts the corrosion of a zero valent metal (M) to produce a metal ion (M + , valence of x) and x electrons (e " ).
  • RX halogenated compounds
  • Equations (9) through (11) illustrate the transfer of electrons from a zero valent metal to an aqueous solution containing an ion with hexavalent chromium (Cr +6 ).
  • the net product includes the less toxic Cr +3 ion and the oxidized metal ion (M +3 ).
  • Electrons supplied by the reduction of zero valent metals can accomplish the electrochemical reduction of not only halogenated and metal containing substances but also other chemical substances that include but are not limited to arsenates, phosphates, sulfates, chromates, mercurates, perchlorates, and nitrates.
  • r ⁇ rt compounds are often located underground.
  • Commercially available zero valent metal varies in particle size from about 1 micrometer to about 1 millimeter or larger.
  • the large particle size and coarse morphology make it difficult and expensive to transport the zero valent metal particles through the sub-surface as the particles are strained or filtered by soil. Smaller particles can more easily fit within and pass though the interstices of the soil particles.
  • the ability to make sub-micrometer (primary particle dimension less than about 1 micrometer) and nanocrystalline (primary particle dimension less than about 100 nm) particles can help alleviate the problems associated with transporting the zero valent particles to the targeted compounds.
  • reaction rates generally scale with surface area that is inversely proportional to particle size. Because of the high surface area, smaller sub-micrometer and nanoscale particles are typically preferred for applications where reactivity and catalytic activity are required.
  • Aqueous phase halogenated compounds are electrochemically reduced by zero valent metals.
  • Reaction products vary and depend upon several variables that include metal composition and particle size. Considering the electrochemical reduction of carbon tetrachloride for example, reaction products can include partially halogenated substances (i.e., chloroform and dichloromethane), halogen free hydrocarbons (i.e, methane), and carbon dioxide gas.
  • the partially dehalogenated hydrocarbons are still toxic and usually are more thermodynamically stable than the parent compound.
  • Current zero valent metal particles often provide reaction pathways that produce these partially dehalogenated hydrocarbons. Zero valent metal particles that minimize or eliminate the formation of partially dehalogenated hydrocarbons are instead preferred.
  • carrier particles and metal source particles are combined with a dispersant and solvent and the mixture is then mechanically agitated such that the metal is deposited onto the carrier particle material.
  • Carrier particle materials may be nanoscale to microscale particles and include oxide ceramics, or mixtures of one or more oxide ceramics, such as aluminum oxide, iron oxide, titanium oxide, silicon oxide, titanates, zircon, tricalcium aluminate, and ilmenite, for example.
  • oxide ceramics such as aluminum oxide, iron oxide, titanium oxide, silicon oxide, titanates, zircon, tricalcium aluminate, and ilmenite, for example.
  • Also useful as carrier particle materials calcium carbide, boron carbide, aluminum carbide, silicon nitride. Other useful materials are phosphates, sulfates, and carbonates, for example.
  • Suitable carrier particle materials also include clays and minerals such as aluminosilicates, for example, and mixtures thereof.
  • carrier particle materials include, but are not limited to polymers and plastics such as polycarbonates and nylon for example.
  • suitable carrier particle materials include intermetallic compounds such as TiAl, and metals and metal alloys, for example.
  • Carrier particle materials may be comprised of combinations of any of the foregoing exemplary compounds. There are few restrictions on carrier particle material composition other than it should not react with or change the targeted properties or function of the metal surface layer.
  • the carrier particle is present in the range of about 25 to about 99 volume percent, more preferably about 80 to about 99 volume percent of the composite particle.
  • compositions produced according to the methods of the invention reduce the propensity for rapid exothermic reactions since a lesser quantity of reactive metal is present and the metal is stored in a non-reactive medium.
  • Another advantage of these methods is the ability to produce a lightweight material, since in most cases the specific gravity of the carrier particle is lower than that of the metal particle. Lightweight materials result in compositions having lower overall product mass and more stable suspensions, as the particle settling rates are proportional to the solid particle's specific gravity.
  • Suitable metals include Li, Al, Na, K, Si, Mg, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, Rb, Sr, Y, Zr, Nb, Mo, Pd, Ag, In, Sn, Sb, Cs, Ba, La, Ta, W, Pt, Au, Pb, Bi, Ce, and U and alloys and combinations thereof.
  • the metal material is present in the range of about 1 to about 75 volume percent , more preferably about 1 to about 20 volume percent of the composite particle.
  • the solvent preferably should exhibit a relatively high flash point and autoignition temperature (flash point greater than about 75°C and autoignition temperature greater than about 150 0 C, for example ) and a National Fire Protection Agency (NFPA) flammability rating of 0 or 1.
  • flash point greater than about 75°C and autoignition temperature greater than about 150 0 C, for example
  • NFPA National Fire Protection Agency
  • the solvent system should offer low toxicity and be biodegradable, particularly when used in in-situ remediation applications where some of the solvent is introduced into the subsurface and can enter aquifers.
  • solvents with a NFPA health rating of greater than about 1 are considered unsuitable.
  • the solvent system should offer a low viscosity of less than about 100 centipoise, for example.
  • the glycol ethers offer the lowest viscosity and therefore result in the most fluid suspensions.
  • the solvent system should be water miscible, particularly when used for in-situ remediation applications where the material is mixed with water and introduced into groundwater.
  • the solvent system additionally should be inexpensive and available in quantity.
  • Initial processing trials employed a mixture according to the foregoing criteria containing aluminum oxide powder, 2 mm diameter spherical steel ball bearings and diethylene glycol monoethyl ether as the solvent. The trials involved adding the solvent and ball bearings into a small media disc mill. After starting the mill, powder was added incrementally. Additions up to about 15 volume percent powder produced fluid slurries, but greater volume fraction slurries unexpectedly produced a very viscous sludge or paste-like product.
  • the slurry required dilution to about 10 volume percent powder to lessen the viscosity enough for the composite particle product to be separated from the steel ball bearings.
  • the presence of metal was verified by adding a few drops of dilute hydrochloric acid to the slurry. This induced the rapid evolution of hydrogen gas bubbles and a lightening of the slurry color as the metal was depleted and the white aluminum oxide particle surface was exposed. Reactivity was evaluated by mixing the aluminum oxide/iron composite particles with an aqueous solution containing chlorinated hydrocarbons. The chlorinated hydrocarbon concentrations were reduced, evidencing the ability of the composite particles to accomplish electrochemical reduction reactions.
  • Dispersants also known as surfactants
  • surfactants are chemical substances, often polymers or oligomers that adhere to particle surfaces.
  • the presence of the dispersant provides repulsive forces (electrostatic or steric) that maintain interparticle separation and prevent agglomeration thereby dramatically reducing slurry viscosity.
  • t OI! ⁇ .4'4 J ffihe' distiieiiSaK ⁇ t i 'also role in the manufacturing processes described herein.
  • the metal particles are substantially larger than the composite particles of the finished product, which comprise metal particles deposited on a carrier particle support.
  • the metal source particles must be separated from the product.
  • Settling velocity has been found to be inversely proportional to viscosity and roughly proportional to the square of particle size.
  • the dispersant reduces slurry viscosity, often dramatically, and this allows for the larger metal particles to be separated from product by settling for a short time period.
  • HLB hydrophile-lipophile balance
  • Dispersant solubility may be tested in the selected solvent by any appropriate routine experimentation readily apparent to any person having ordinary skill in the art. For example, 2 mass percent dispersant additions may be mixed with solvent and poured into glass vials. Where the solvent is transparent, dispersant containing solutions that maintain a transparent appearance may be considered soluble with the solvent. Dispersants producing an opaque or translucent solution may be eliminated from consideration.
  • dispersants should adhere to the particle surfaces.
  • Particle surfaces have both positive and negative point charges.
  • a negatively charged dispersant molecule typically an anionic dispersant, will adhere to the particle surface at the location of a positive point charge.
  • a positively charged dispersant molecule typically a cationic dispersant, will adhere to the particle surface at the location of a negative point charge.
  • %% ⁇ b anionic or cationic will be effective for a particular particle system, in practice performing experiments is the most pragmatic and best way to identify and screen candidate dispersants.
  • the dilute suspensions are mixed and agitated, they are poured into capped glass vials and a subjective analysis is used to determine dispersant compatibility with the solvent/particle system.
  • a good suspension exhibits distinct characteristics.
  • One favorable characteristic is the presence of a bluish tint or Tyndall Effect that is indicative of the scattering or reflection of light provided by only small, dispersed particles.
  • Another favorable characteristic is the formation of a thin, uniform sheet of liquid suspension that cascades down the inner surface of the capped glass vial surface when shaken.
  • poorly dispersed systems do not exhibit a bluish appearance and exhibit clumping or a non-uniform distribution of particles on the glass vial surface.
  • Dispersants meeting the foregoing criteria are exemplified by but not limited to Disperbyk ® 111 and Disperbyk ® 180, proprietary polymeric dispersants made by Altana Chemie (Wessel, Germany). Similar compatibility tests may be used in addition and/or in the alternative to the foregoing example, such tests being readily apparent to any person having ordinary skill in the art.
  • Viscosity is measured and the concentration MtpiJbMia@ife is identified. Concentrations between about 2.0 and about 3.0 mg dispersant per square meter of surface area provide a suitably low viscosity with a minimum at about 2.5 mg dispersant per meter square. Similar tests may be used in addition and/or in the alternative to the foregoing example, such tests being readily apparent to any person having ordinary skill in the art.
  • compositions comprised components meeting all of the criteria described herein. The compositions were stored, as typical, in closed plastic containers.
  • the Disperbyk ® 180 containing slurry maintained the initial gray color of the harvested material.
  • the Disperbyk ® 111 containing slurry experienced a color change and had assumed a brownish, rust-colored appearance after about 3 days. It was suspected that the Disperbyk ® 111 possessed acidic characteristics that initiated a reaction with the metal and caused corrosion. This is unacceptable if metallic characteristics are desired in the product, as is the case for enabling electrochemical reactions, for example.
  • Disperbyk ® 180 containing slurry was tested for presence of metal by adding a few drops of dilute hydrochloric acid. Unexpectedly, few hydrogen gas bubbles were evolved when compared to prior material that was made without dispersant. This was despite the fact that metallic powder color clearly indicated the presence of a metal fraction. Perplexed by this observation, the ability of this material to accomplish the electrochemical reduction of aqueous phase chlorinated hydrocarbons was tested. Unlike prior material made without dispersant, the material accomplished little or no electrochemical reduction despite its metallic color. f ⁇ 'ti ' B ' #ijU fepllSMicMW tEe non-reactive nature of the dispersant- containing particles. While several theories accounting for this observation have been set forth, none are determinative of the problem. Ultimately this unforeseen problem has now been solved using a surprisingly unique processing approach.
  • the metal source particles are still easily separated from the powder fraction slurry product by settling.
  • the powder produced using the this process may be evaluated by adding a few drops of dilute hydrochloric acid to the slurry; metal content is evidenced by the rapid evolution of hydrogen gas bubbles. The ability to enable electrochemical reduction may be evidenced by the rapid elimination of halogenated hydrocarbons in an aqueous solution.
  • metal constituents, solvent and dispersant a wide variety of materials may optionally be included, the benefits of which are readily apparent to anyone having ordinary skill in the art.
  • Particularly beneficial optional ingredients include, but are not limited to metals more noble than the host metal such as Pd, Pt, Au, Cu, and Ni for example.
  • More noble metals are easily added to the host metal surface using an electrochemical reaction.
  • Other additives can include micronutrients such as phosphorus, for example, and non- metals such as carbon and sulfur, for example.
  • any person having ordinary skill in the art would be capable of determining the types of additives that would be beneficial.
  • Suitable devices include, but are not limited to stirred media mills having a vertical mixing chamber such as an attritor mill for example.
  • Other devices include stirred media mills having a horizontal mixing chamber such as a sand mill for example.
  • the stirred media mill can be operated in batch or continuous mode.
  • tumbling mills such as jar mills and ball mills, for example, are suitable.
  • Additional examples include vibratory mills such as a SWECO ® mill, ultrasound 3 and lapping. If a smaller or larger mixing chamber is used, the mass of each constituent is proportionally increased or decreased.
  • the mixtures are mechanically agitated until the slurry assumes the desired metallic color.
  • Water may be pumped through a cooling jacket, for example, in order to maintain a -iOffyf® er ⁇ £f ⁇
  • the mixtures are agitated in air, nitrogen, oxygen, forming gas, vacuum, or other suitable atmospheres that are readily apparent to anyone having ordinary skill in the art.
  • the processing temperature should be maintained between the freezing and boiling temperatures of the selected solvent system.
  • the resulting slurry is typically decanted into another vessel.
  • the coarse and high density metal source particles rapidly settle to the bottom of the vessel.
  • the suspended product may be pumped or decanted, for example, into another container.
  • the particles are typically configured of a carrier particle material with metal deposited thereon, such as a core and shell. Some free, non-supported metal and non-metal particles may also be produced by the process and mixed within the core and shell particles.
  • the resulting particles typically resemble the initial size of the carrier particles.
  • reduction of the initial particle size may occur as the metal particles can act as media to break down the carrier particles.
  • the process is capable of producing very small particles, in the nanoparticle regime.
  • the process is also capable of producing larger microscale particles. This versatility is enabling since the particle size can be tailored to meet the requirement of the targeted application.
  • the preferred particle size is typically small if reactivity and catalytic activity are desired; for other applications larger particles may be preferred.
  • sub-micrometer particles are often preferable to nanoparticles. As the particle size is decreased the particles are more susceptible to agglomeration. Accordingly, using slightly larger but discrete sub-micrometer particles can provide better underground mobility.
  • the resulting particles typically resemble the shape of the initial carrier particles. In some cases shape change may occur if the carrier particles are broken down during the synthesis process. Therefore, several particle morphologies including but not limited to equiaxed, acicular, and platelet shapes are possible if carrier particles of these geometries can be obtained-
  • the composite particle suspensions are typically stored in closed airtight containers or in an inert atmosphere. Stable suspensions can be maintained for days or weeks using the solvent and dispersant used for particle synthesis.
  • Almatis, Pittsburgh, PA Almatis, Pittsburgh, PA
  • Powder surface area was measured at about 12 m 2 /g.
  • the mill speed was set to 3200 RPM and was operated at a constant temperature of 20 0 C in a nitrogen atmosphere. About 450 g of roughly spherical aluminum oxide (P730) was added in stages. After 3 hr., slurry color was metallic gray. The mill speed was reduced to 1500 RPM and 4.2 g of dispersant (Disperbyk ® 180) was added to reduce viscosity and enable separation of zinc source particles by settling.
  • dispersant Dispersant
  • Dispersant Dispersant ® 180
  • the solvent was a mixture of diethylene glycol monoethyl ether (80 m/m%), propylene glycol (10 m/m%) and polyethylene glycol 400 (10 m/m%).
  • the solvent/dispersant mixture was pumped through a disc mill (Union Process DM-20 Delta Mill, Akron, OH) with a 20 liter volume horizontal mixing chamber.
  • the water-cooled mixing chamber was filled to 85% of net volume with US-280 Ultrasoft Shot steel particles.
  • Example 8 As the solvent/dispersant mixture was pumped through the Delta Mill, 350 kg of the aluminum oxide (Almatis PlOF) was added incrementally to maintain a fluid suspension. The slurry was re- circulated through the mill operating at a tip speed of 2500 feet per minute and back into the stirring tank. The initially white slurry darkened into a metallic color with increasing time. After 8 hours the slurry was pumped into the mixing tank and the remaining iron remained in the mixing chamber and can be used for another run. [0075] Example 8
  • Coarse reference powders (electrolytic iron North American Hoganas AC325 grade and carbonyl iron BASF OM grade, Mount Olive, NJ) were also evaluated.
  • the work used an 8.4 pH buffered 200 ⁇ M carbon tetrachloride solution.
  • About 175 g of the carbon tetrachloride solution was transferred to a 240 mL bottle to which 2.2 g (1.5 g powder basis) of the composite particle slurry was added.
  • the reference materials used 1.5 g of dry powders. These powders were tested straight out of the container and no attempt was made to remove any oxide surface layer.
  • the bottles were not shaken or agitated during the testing period.
  • Chemical composition was measured by injecting headspace gas into a gas chromatograph over a 2 day period. Table 1 shows the measured carbon tetrachloride concentration for each compound.
  • Table 2 shows the measured chloroform concentration for each compound.
  • Example 8 demonstrated the ability of the carrier particle supported zero valent metals to accomplish the electrochemical reduction of dilute carbon tetrachloride (200 uM, 30.8 mg/L) solutions. The ability of the carrier supported metal particles to accomplish the electrochemical reduction of more concentrated solutions was also demonstrated.
  • This experiment employed aluminum oxide carrier particles supporting a mixture of zero valent iron and zero valent aluminum.
  • Microscale reference powders electrolytic iron North American Hoganas AC325 grade and carbonyl iron BASF HS grade, Mount Olive, NJ were also evaluated.
  • the work used an 8.4 pH buffered 9.37 mM (1250 mg/L) 1,1,1 trichloroethane solution. About 175 g of the carbon tetrachloride solution was transferred to a 240 mL bottle to which 1.4 g slurry (1.0 g powder basis) of the composite particle slurry was added. The reference materials used 1.0 g of dry powders. These powders were tested straight out of the container and no attempt was made to remove any oxide surface layer. Mixing was accomplished by slowly rolling the rolling the bottles. Chemical composition was measured by injecting headspace gas into a gas chromatograph over a 2 day period. Table 3 shows the measured 1,1,1 trichloroethane composition for each compound. Table 3: 1,1,1 trichloroethane (C 2 H 3 Cl 3 ) concentration
  • the experimental data showed that the carrier particle supported aluminum/iron particles enabled the rapid electrochemical reduction of the near-saturated 1,1,1 trichloroethane solution; the concentration was reduced by approximately 50% in less than two days. Reaction products included ethane gas and 1,1 dichloroethane. The reference iron powders showed negligible reactivity in the time period studied under these processing conditions .

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Abstract

Cette invention concerne un procédé permettant de produire des particules composites contenant du métal, et des suspensions de particules composites. Ce procédé est polyvalent et permet de produire des particules de diverses tailles et de diverses compositions. Pour certaines applications, les particules composites métalliques peuvent offrir la fonctionnalité de particules entièrement métalliques, comprenant des configurations dans lesquelles le métal est situé à la surface de la particule. De tels métaux ont des applications dans un large éventail de domaines, notamment dans la réduction électrochimique et la catalyse.
PCT/US2006/001165 2005-01-12 2006-01-11 Procede permettant de preparer de particules composites presentant des caracteristiques de surface sur mesure WO2006076534A2 (fr)

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