WO2005123272A2 - Liquid feed flame spray modification of nanoparticles - Google Patents

Liquid feed flame spray modification of nanoparticles Download PDF

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Publication number
WO2005123272A2
WO2005123272A2 PCT/US2005/006481 US2005006481W WO2005123272A2 WO 2005123272 A2 WO2005123272 A2 WO 2005123272A2 US 2005006481 W US2005006481 W US 2005006481W WO 2005123272 A2 WO2005123272 A2 WO 2005123272A2
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WIPO (PCT)
Prior art keywords
particles
alumina
metal oxide
preformed
phase
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/US2005/006481
Other languages
English (en)
French (fr)
Other versions
WO2005123272A3 (en
Inventor
Richard M. Laine
Julien Marchel
Jose Azurdia
Roy Rennensund
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.)
University of Michigan System
University of Michigan Ann Arbor
Original Assignee
University of Michigan System
University of Michigan Ann Arbor
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Publication date
Application filed by University of Michigan System, University of Michigan Ann Arbor filed Critical University of Michigan System
Priority to EP05787515A priority Critical patent/EP1718421A4/en
Priority to JP2007500814A priority patent/JP2007534586A/ja
Priority to CA2557832A priority patent/CA2557832C/en
Publication of WO2005123272A2 publication Critical patent/WO2005123272A2/en
Anticipated expiration legal-status Critical
Publication of WO2005123272A3 publication Critical patent/WO2005123272A3/en
Ceased legal-status Critical Current

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    • C01B13/14—Methods for preparing oxides or hydroxides in general
    • C01B13/34—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of sprayed or atomised solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/02—Processes for applying liquids or other fluent materials performed by spraying
    • B05D1/08—Flame spraying
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Definitions

  • the present invention is directed to modification of metal oxide particles by injection into a flame of moderate temperature by liquid feed flame spray techniques.
  • Particles have been supplied into high temperature plasma or flames, i.e. above 2000° C, to melt or even vaporize the particles for use in preparing coatings.
  • phase may be altered, for example a crystalline phase or an amorphous phase, or both, or whereby hollow or core/shell particle morphology may be created from particles in the micron range, and preferably those of nanometer size, while retaining their particulate nature.
  • the literature also describes the injection of preformed particles, or occasionally their precursors, into a plasma or related high temperature flames, typically > 2000° C, such that the particles are vaporized or fully melted to subsequently produce coatings such as thermal barrier coatings.
  • the particles are 10-5Q ⁇ m diameter which are, in some instances, formed from nanosized particles in the range of 6-70 nm.
  • the larger particles or precursors are typically injected off-axis into a plasma arc, and generally result in relatively smooth coatings, as the molten particles "splat" onto the substrate.
  • a similar process has been used for many years to produce boules of alumina (sapphire, ruby).
  • Solution injection of precursors may also be used to prepare particles and/or coatings.
  • rapid evaporation of solvent initially forms more concentrated admixtures which then, under the high temperature pyrolysis conditions, further undergo such processes as breakup, precipitation, and/or gelation, followed by pyrolysis, sintering, and if the flame is hot enough, fusion.
  • the fused particles are much larger than the particles initially formed, as the result of forming agglomerates prior to fusion.
  • the process is also useful for forming thermal barrier coatings.
  • their particulate nature is substantially lost.
  • Alumina, alumina/zirconia and also alumina/titania mixtures are used commonly for the formation of such thermal barrier coatings.
  • the alumina formed is the gamma phase with small amounts of alpha.
  • the invention pertains to injection of nano-, ultrafine- and micron-sized ceramic oxide particles into low temperature (400-2000° C) oxidizing, reducing or neutral flames individually, in combination with each other, or coinjected coincidentally or serially downstream, optionally also with chemical precursors, and as a result, their phases, particle sizes and size distributions, phase compositions and physical and chemical properties significantly modified by exposure to the flame and to the coinjected or serially injected materials.
  • novel and unexpected particle morphologies and size distributions can be generated through the use of combinations of particles, or combinations of particles and precursors coinjected, or serially injected downstream from the initial liquid feed flame spray combustion unit.
  • This process includes the coating of supports and substrates with combinations of metal oxides and metals for development of new catalysts, photonic materials, sensing materials, thermal barrier coatings, abrasion and corrosion resistant coatings, prosthetic ceramic materials, conducting materials, transparent ceramics, etc.
  • the products may be ⁇ -alumina or combinations of ⁇ -alumina coated with other metal oxides or products of the reaction of ⁇ - or ⁇ -alumina nanoparticles with coinjected or serially injected components including other metal oxide powders or precursors or combinations thereof; are large clay particles transformed to dense spherical or hollow spherical particles that can be coated with alumina or related hard ceramic nanopowders for applications ranging from novel abrasives to insulating packing materials for construction materials; metal oxide coatings on alumina, yttria, YAG, or titania, NiO or other transition, lanthanum or actinide or main group metal oxide such that the coatings can be modified to become catalytically active or electrically conducting, and may be
  • microparticles preferably nanoparticles
  • introduction of microparticles, preferably nanoparticles, into a flame with a temperature of from 400°C to less than 2000°C can produce novel compositions of matter, and may also be used to perform useful phase transformations not previously possible.
  • particles having particles of different composition adhered to their surface may be formed, including metal oxide particles coated with metals.
  • the products have a wide range of uses including the production of dense sintered ceramic materials, novel catalysts, applications in optoelectronics, etc.
  • the present invention is broadly directed to a process for the preparation of particles by the injection of particles of a first composition and morphology into a high temperature zone ("flame") by liquid feed flame spray pyrolysis ("LSP") such that particles having a different composition and/or morphology are thereby obtained.
  • the thusly obtained particles may be collected, or may impinge upon a "target” or “substrate” while in a particulate state such that the particulate character is maintained to a substantial degree; in other words, the particles are not fused to a state where upon impacting the target they "splat” or fuse, forming smooth or somewhat irregular continuous coatings, but instead strongly adhere in the form of discrete particles.
  • the preformed particles are injected into the high temperature zone along with liquid precursor of the same composition or a different composition.
  • particles having a different morphology and/or composition than the initial particles are thereby formed.
  • This different morphology and/or composition may take several forms.
  • the initial particles may be coated with solid derived from the liquid precursor; may comprise but a single phase with its composition derived from both the composition of the preformed particles and from the liquid precursor; may contain two or more distinct phases, e.g. crystalline phases of different composition or crystalline phases of the same composition but different crystal structures; or may contain particles of one or more phases enriched at the surface with elements or compounds derived from the precursor.
  • solvent dispersing media solid particles of similar or identical composition but different morphology may be obtained, and hollow particles may also be obtained.
  • solid particles i.e. particles having a size less than 100 ⁇ m, preferably less than 10 ⁇ m, and most preferably nanoparticles having a size less than 1 ⁇ m, preferably between
  • particles 1 and 100 nm be employed as the initial particles.
  • These particles may be derived from numerous sources. They may, for example, be of natural origin, such as fine clay, diatomaceous earth, finely ground minerals such as bauxite, ash, for example fly ash, rutile, and garnet, or may be of wholly synthetic manufacture, for example particles produced by high temperature flame hydrolysis, liquid feed spray pyrolysis, solution precipitation, etc.
  • Synthetic particles are preferred, most preferably metal oxides or mixed metal oxides prepared by high temperature flame processes, and most preferably metal oxides and mixed metal oxides which exhibit exceptional high temperature stability, such as silicates, and oxides and mixed oxides of transition metals, and especially of silicon, aluminum, and titanium, with or without additional elements such as the main group 1 and 2 elements, carbon, boron, phosphorous, arsenic, etc., the latter group generally in relatively low concentration.
  • carbon may be present in the form of carbides, while phosphorous, arsenic, boron, etc. , may be dopants in a matrix of metal oxide, as also may be transition elements, particularly lanthanides and actinides, for example silica or titania doped with Ce, Pr, Nd, Yb, etc.
  • the concentration of solid particles in the liquid feed to the flame may be any concentration which is sufficiently pumpable and atomizable.
  • the weight percentage will of course vary with the density of the particles. With respect to alumina particles, the lower range is not technically limited, but for economic reasons is preferably at least 0.1 weight percent.
  • the upper limit is partially dependent on particle surface area, and for particles of low specific surface area, may range as high as 80% by weight. Ranges of 1 weight percent to 70 weight percent are more preferable, with weight percentages in the range of 5 to 20 weight percent being more preferred, each integral range between 1 % and 80% being considered to be disclosed herein.
  • the flame temperature must be such that the desired particle morphology is obtained.
  • the temperature will be within the range of 400 to 2000°C, more preferably 600 to 1800°C, and most preferably from about 800°C to 1300 or 1400°C.
  • the high temperature zone may be provided by any convenient method. Such methods are well known to those skilled in the art.
  • the flame may be created by an oxyhydrogen torch, by combustion of liquid or gaseous fuels such as alkanes, alcohols, ketones, etc. in oxygen or oxygen diluted with air or nitrogen, may be provided by electrical discharge, for example an arc flame, or by any suitable procedure.
  • the flame is produced by burning of a combustible fuel, with or without hydrogen, in oxygen or oxygen diluted with air, nitrogen, inert gas, water, etc.
  • the flame stoichiometry may be adjusted to provide an oxidizing or reducing atmosphere, or may be neither oxidizing nor reducing.
  • Additional elements or compounds may be fed to the flame so as to incorporate additional elements into the particles or to modify the particles composition and/or morphology by their presence.
  • additional elements include halogens, metal halides, tin compounds, chalcogenides, and the like. Injection of such components may take place at any time, for example concurrently with particle introduction and/or subsequent thereto.
  • the process is capable of producing coatings on substrates such as metal, glass, ceramics, and even high melt temperature thermoplastics, which are durable and abrasion resistant.
  • Particles can be injected into a low temperature (400 - 2000 °C) flame and their properties significantly modified by exposure to the flame and to materials coinjected with the particles. Novel particle size distributions may be created through the use of combinations of particles, or combinations of particles and precursors may be coinjected or injected serially downstream from the initial liquid feed flame spray combustion unit.
  • This process includes the coating of supports and substrates with combinations of metal oxides for development of new catalysts, photonic materials, sensing materials, thermal barrier coatings, abrasion and corrosion resistant coatings, prosthetic ceramic materials, conducting materials, transparent ceramics, etc.
  • the current invention demonstrates that the concepts espoused in the earlier patent often do not occur and, furthermore, different and unusual events occur that are inconsistent with what is suggested.
  • LF-FSP of pure Cr(O 2 CCH 2 CH 3 ) 3 precursor (0.5 wt. % Cr 2 O 3 solids loading) dissolved EtOH gives simple green nanopowders of Cr 2 O 3 (40 nm average particle size by BET) with the XRD pattern exactly that expected for ⁇ -phase Cr 2 O 3 .
  • LF-FSP of a 92:08 mixture of particulate ⁇ -alumina:Cr 2 O 3 as Cr(O 2 CCH 2 CH 3 ) 3 precursor in EtOH results in the production of very slightly off-white nanopowders with a size distribution ranging from nanosized to micron sized.
  • XRD line broadening analysis indicates that the agglomerates actually consist of nanopowder particles 60 nm in diameter. Thus, efforts were made to break up the agglomerates.
  • the larger particles are readily separated from the fine particles by simple sedimentation in water after 2 minutes.
  • the larger particles appear to be only lightly agglomerated because they can be suspended in EtOH and sonicated (800 Watts/lh). After sonication, the agglomerates are broken up and the resulting powder now remains suspended in EtOH for lengthy periods where before ultrasonication it did not. Sedimentation of the powders after sonication gives top and bottom fractions.
  • the top fraction turned slightly green and the bottom fraction slightly red as the Cr 2+ ions were oxidized to Cr 3+ ions.
  • the red color is common for Cr 3+ , attributable to d-d transitions, as seen in ruby where Cr 3+ ions are part of the ⁇ -alumina lattice.
  • the phases present in these samples were mainly ⁇ and ⁇ * Al 2 O 3 while no Cr species were observed.
  • the relative amounts of each Al 2 O 3 phase were, for the top and bottom respectively 68% and 56% v-Al 2 O 3 . If a Cr 2 O 3 coating had formed, one would expect the same dark green color, and the XRD should easily have shown 8 wt. % ⁇ -Cr 2 O 3 on alumina.
  • the absence of a Cr 2 O 3 coating, yet the obvious oxidation to Cr 3+ ions indicates that the chromium precursor decomposes during LF-FSP and becomes incorporated into the alumina to some depth but not to the point where it cannot be oxidized.
  • a further important change was the observation of ⁇ -alumina. In all previous studies that generated alumina nanoparticles, the only phases observed are ⁇ -alumina or ⁇ -alumina.
  • XRDs show the starting Degussa ⁇ -alumina to be > 70% ⁇ -Al 2 O 3 , the remaining material being ⁇ -Al 2 O 3 .
  • the resulting powders have surface areas of 60 m 2 /g and APS of 40-60 nm. SEMs of these materials show essentially no features.
  • the as-produced treated powders contain some fraction of larger particles, which can be separated by simple sedimentation, or because they are soft agglomerates, can be broken down by ultrasonication as above. Sedimentation provides rather uniform particles. However, by controlling the conditions, it is possible to produce products where no large particles are obtained.
  • the method of injection of the nanopowders into the flame does not have to be by coinjection. It can also be done by serial injection, but with control of the flame temperature at the point of injection so that it is between about 400° and about 2000°C. Furthermore, it could also be done through use of a second flame directly after the initial LF-FSP production of either the ⁇ -alumina or ⁇ -alumina powders.
  • the FTIR data for the particles indicates that the treated particles are more crystalline.
  • FTIR also shows v O-H vibrations for the Degussa ⁇ -alumina, which are typical of a highly hydrated surface and mostly physisorbed water.
  • the LF-FSP treated materials have only small amounts of isolated chemisorbed OH groups.
  • the product would have contained the anatase phase nearly exclusively.
  • the product consists of a mixture of ⁇ -alumina and a poorly crystalline titania phase.
  • Typical SSAs of clay samples after LF-FSP at temperatures > 1500°C are:
  • splat droplets By placing surfaces in or near the flame, they can be coated with nanopowders without formation of splat droplets.
  • a sample of 316 SS was placed near a flame containing coinjected ⁇ -alumina particles. After just a few seconds the piece of steel was removed and cooled. The sample had an iridescent coating of particles as shown by SEM images. These coatings could not be removed by rubbing with abrasive media. The thickness and quality of the coatings depend on the conditions used. Longer times will give thicker but uneven coatings. The particles can be distinctly seen, however, without the formation of a continuous coating.
  • Titanatrane isopropoxide or Tyzor TE (Me 2 CHOTi(OCH 2 CH 2 ) 3 N)] was purchased from Dupont. Ethanol was purchased from standard sources and used as received. Gamma alumina powders were received from Degussa and ⁇ -alumina powders were prepared from the LF-FSP of alumatrane,
  • LF-FSP methods The systems used in the production of coated or coreacted or coinjected or serially reacted nanopowders or micron sized powders, are unique.
  • the powders once suspended must be pumped and subsequently aerosolized using a pump system that will not be abraded by the suspended particles through an aerosolizer that can be an ultrasonic atomizer or a bernouli mister or other similar misters that can mix the powder suspension with oxygen or air or even an inert gas such that droplets less than about 50 microns are generated.
  • the powders and/or precursors can be serially injected as a liquid or air suspension into the flame.
  • the combustion process can use the suspending medium as fuel which can include oxygenates such as methanol, ethanol, propanol, or other linear or branched alcohol or tetrahydrofuran or dimethoxyethane or dimethoxydiethyleneglycol or other fuel that has a low viscosity, lower than about 300 cp at temperatures less than about 200°C.
  • Fuel can be used as a co-suspending medium or as the sol-medium.
  • combustion must be promoted through use of a combustible gas or easily volatilized organic such as natural gas or methane, ethane, propane, butane, hexanes, methanol, ethanol, tetrahydrofuran etc. or mixtures thereof.
  • a combustible gas or easily volatilized organic such as natural gas or methane, ethane, propane, butane, hexanes, methanol, ethanol, tetrahydrofuran etc. or mixtures thereof.
  • hydrogen can be combusted.
  • Combustion in systems with less than about 50 vol % fuel used as the suspending medium may require co-combustion of combustible gas and/or hydrogen.
  • Flow rates of suspended particles in a combustible medium can be controlled to control the flame temperature to about 400° to less than 2000°C.
  • Flow rates of suspended particles in a noncombusting medium can be controlled by both the flow rate of the suspending medium and the amount of combustible gas metered into the combustion system.
  • the temperature is usually adjusted so as to avoid fusion of the particles, although in some cases, fusion may be desired, as long as the resulting particles solidify prior to collection.
  • particles and/or precursors can be entrained in separate gas flows and injected tangentially, but at temperatures between about 400° and 2000°C.
  • the powder can be introduced separately into the flame via entrainment in a gas. Combustion occurs at temperatures ⁇ 2000°C producing selected products as described in the Examples below, and gaseous byproducts.
  • the powders are collected downstream in electrostatic precipitators (ESPs) or a bag house or cyclone filter.
  • ESPs electrostatic precipitators
  • a 1 wt. % suspension of 40 g ⁇ -alumina with particle sizes of 20-40 nm and surface areas of 60 m 2 /g in 4 1 of EtOH/ButOH 50/50 is subjected to LF-FSP at rates of 4L/h.
  • the resulting powder is converted to mixtures of ⁇ - and ⁇ -alumina.
  • Alpha alumina powders (15 g) were mixed with Tyzor TE to make a composition of 80 mol% alumina-20 mol% titania. 400 ml of EtOH were added and the solution was ultrasonically dispersed for 5 min, and then 2500 ml of EtOH was added with stirring at 20°C for at least 30 min. Following LF-FSP, the resulting particles consisted of ⁇ -alumina coated with rutile.
  • Delta alumina powders (15 g) were mixed with Tyzor TE to make a composition of mol% alumina-20 mol% titania. 400 ml of EtOH were added and the solution was ultrasonically dispersed for 5 min, and then 1250 ml of nBuOH and 1250 ml of EtOH were added with stirring at 20° for at least 30 min. Following LF-FSP, the resulting particles consisted of ⁇ -alumina and a nondescript titania doped phase. Example 6.
  • Delta alumina powders (2 g) were mixed with Tyzor TE to make a composition of mol% alumina-85 mol% titania. 400 ml of EtOH were added and the solution was ultrasonically dispersed for 5 min, and then 1250 ml of nBuOH and 1250 ml of EtOH were added with stirring at 20° for at least 30 min. The products analyzed by XRD were found to be only alumina doped titania very similar to that produced solely by LF-FSP of precursors without nanopowder coinjection.
  • Alpha alumina nanopowder produced as above (75 wt. % phase pure) 15 g was dispersed in 4 1 of a 50/50 (volume) EtOH/nBuOH solution. 125 g of yttrium propionate (4 wt. % ceramic) was added. The total ceramic loading was 0.5 wt. % with a ratio of 75 wt. % v-Al 2 O 3 :25 wt. % Y 2 O 3 as yttrium proprionate.
  • This mixture was processed through LF-FSP at the rate of 20 g/h.
  • the XRD shows that the resulting powder is mostly monoclinic Al 2 Y 4 O 9 (YAM), although YAlO 3 I, Cubic Y 2 O 3 are also observed in smaller quantities. This suggests a reaction between the alumina particle surface and the yttrium ions in the flame, forming a YAM coating around an alumina core. The nanoparticles are lightly agglomerated.
  • YAM monoclinic Al 2 Y 4 O 9
  • Example 8 Degussa ⁇ -alumina, 15 g was dispersed in 4 1 of a 50/50 (volume)
  • XRD of resulting powder indicates that the powder is almost phase pure YAlO 3 I with minor amounts of YAM and ⁇ -alumina. This indicates a reaction between the yttrium ions in the flame and the alumina particles. Contrary to the above example, the production of YAlO 3 I indicates better mixing than obtained with ⁇ -alumina, likely a combination of the higher thermal stability of this alumina phase and the higher surface area/smaller particle size of the ⁇ -alumina as indicated by the Y/Al ratio of YAlO 3 1.
  • Delta alumina nanopowder, 15 g was dispersed in 4 1 of a 50/50 (vol)
  • EtOH/nBuOH. 41.3 g of yttrium propionate (12 wt. % ceramic) was added. The total ceramic loading was 0.5 wt. % at a 75 wt. % v-Al 2 O 3 :25 wt. % Nd 2 O 3 as neodymium proprionate ratio. This mixture was LF-FSP processed at 20 g/h. The product appears to be pure NdAlO 3 .
  • Core shell powders were produced by mechanically mixing a 12% ceramic wt. Ni propionate precursor with 15 g of ⁇ * -Al 2 O 3 powders followed by LF-FSP. A sample with a slight blue-green cast was produced. The sample was dispersed using an ultrasonic horn (800 W for 1 h) and left to sediment for 12 h after which the top fraction of the dispersed solution was separated from the bottom fraction. These were then dried at 80 °C for 24 h and analyzed using XRD.
  • Clay suspension precursors were prepared by placing 25 g of clay in a 250 mL PVP bottle, with 180 ml EtOH and 100 g of alumina milling media. Each precursor was then milled for 48 h and filtered. The resulting suspension was diluted with EtOH to give 4L batches of suspension.
  • the apparatus used for FSP consists of an aerosol generator, a combustion chamber and an electrostatic powder collection system.
  • the precursor solution is pumped through an aerosol generator at a rate of 100 mL/min.
  • the solution is atomized with O 2 to form an aerosol and ignited by two methane/oxygen pilot torches, while the pressure in the system was kept at 7.5 psi. Combustion produces temperatures of about 400-2000°C.
  • the particles are collected in ESPs.
  • the production rate was typically ca. 30 g/h.
  • Clay suspension precursors were prepared by placing 25 g of clay in a 250 mL PVP bottle, with 180 ml of 50:50 EtOH:H 2 O and 100 g of alumina milling media as above.
  • the precursor solution is pumped through an aerosol generator at a rate of 100 mL/min.
  • the solution is atomized with O 2 to form an aerosol and ignited by two methane/oxygen pilot torches, while the pressure in the system was kept at 7.5 psi. Combustion produces temperatures > 800 ° C and the particles are collected in ESPs.
  • Clay suspension precursors were prepared by placing 25 g of clay in a 250 mL PVP bottle, with 180 ml of 50:50 MeOH:H 2 O and 100 g of alumina milling media. FSP. The precursor solution is pumped through an aerosol generator at a rate of 100 mL/min. The solution is atomized with O 2 to form an aerosol and ignited by two methane/oxygen pilot torches, while the pressure in the system was kept at 7.5 psi. Combustion produces temperatures > 800 ° C and the particles are collected in ESPs. The particles are predominately hollow spheres.
  • Clay suspension precursors were prepared by placing 25 g of clay in a 250 mL PVP bottle, with 180 ml of 25:75 MeOH:H 2 O and 100 g of alumina milling media.
  • the precursor solution is pumped through an aerosol generator at a rate of 100 mL/min.
  • Clay suspension precursors were prepared by placing 25 g of clay in a 250 mL PVP bottle, with 180 ml of 25:75 MeOH:H 2 O and 100 g of alumina milling media.
  • the precursor solution is pumped through an aerosol generator at a rate of 100 mL/min.
  • Example 15
  • Coatings of nanoparticles on glass, ceramic, and metal components can be made by exposing the required substrate to the product stream from Example 1 or any other Example above, such that the temperatures are sufficient to cause particle adhesion to the substrate surface without significantly altering its properties.
  • the resulting coatings can be abrasion resistant, catalytically active, corrosion resistant, adhesive to second coating materials or for joining dissimilar materials.

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