Source: http://www.google.com/patents/US7828998?dq=5527183
Timestamp: 2015-04-20 02:02:56
Document Index: 555279469

Matched Legal Cases: ['Application No. 200800008', 'Application No. 200700583', 'Application No. 200701830', 'Application No. 200700583', 'Application No. 200700296', 'Application No. 200700583', 'Application No. 200680038963', 'Application No. 200580030660']

Patent US7828998 - Particles of a ceramic mineral material having a metal oxide dopant are ... - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inAdvanced Patent SearchPatentsDisclosed is a method for making a material having a controlled microstructure, the method including providing particles of a ceramic mineral material, the particles having a metal oxide dopant therein. The particles of the ceramic mineral material are consolidated into larger aggregates of a size relevant...http://www.google.com/patents/US7828998?utm_source=gb-gplus-sharePatent US7828998 - Particles of a ceramic mineral material having a metal oxide dopant are consolidated into larger aggregates of a size relevant to application; heating, chemical reducing,sintering, oxidizing; shell/core; gradient of voids; well fracturingAdvanced Patent SearchPublication numberUS7828998 B2Publication typeGrantApplication numberUS 11/775,671Publication dateNov 9, 2010Filing dateJul 10, 2007Priority dateJul 11, 2006Fee statusPaidAlso published asUS20080015103, WO2008008828A2, WO2008008828A3Publication number11775671, 775671, US 7828998 B2, US 7828998B2, US-B2-7828998, US7828998 B2, US7828998B2InventorsWalter G. Luscher, John R. Hellmann, Barry E. Scheetz, Brett A. WilsonOriginal AssigneeCarbo Ceramics, Inc.Export CitationBiBTeX, EndNote, RefManPatent Citations (101), Non-Patent Citations (79), Referenced by (2), Classifications (18), Legal Events (4) External Links: USPTO, USPTO Assignment, EspacenetParticles of a ceramic mineral material having a metal oxide dopant are consolidated into larger aggregates of a size relevant to application; heating, chemical reducing,sintering, oxidizing; shell/core; gradient of voids; well fracturing
US 7828998 B2Abstract
8. The method of claim 1 wherein said aggregated particles are heated in said reducing atmosphere to a temperature in the range of 800-1800� C.
heating said aggregated particles having said islands formed therein in air, so as to cause at least a portion of the reduced metal forming said islands in the interior of said aggregated particles to be taken up by said aggregated particles creating voids therein and to consolidate the islands of said metal on the surface of said aggregated particles so as to at least partially form a shell thereupon. Description
This application claims priority of U.S. Provisional Patent Application Ser. No. 60/807,012, filed Jul. 11, 2006, entitled �Dopant Enhanced Densification of Aluminosilicate Aggregate� which is incorporated herein by reference.
According to certain embodiments of the present invention, the ceramic mineral material can include oxides of aluminum, oxides of silicon, aluminosilicates and combinations thereof. In some embodiments, the ceramic mineral material can include kaolinite, bauxite, fly ash and combinations thereof. In some embodiments, the metal oxide dopant can include an oxide of a polyvalent transition metal and in some embodiments can include oxides of iron, and/or oxides of titanium, chromium, manganese, or others, and combinations thereof. In one embodiment, the dopant includes hematite. In some embodiments, the amount of metal oxide dopant can range from approximately 0.1 to 30 weight percent of the particles. In some embodiments, the aggregates can have a sieve size in the range of 12-20 to 20-40 mesh and at least one of the heating steps includes a temperature in the range of 1100-1800� C. In some embodiments, larger or smaller aggregate size ranges are used. When heated within this temperature range under a controlled oxygen fugacity, the liquid phase forms a metastable eutectic with the ceramic mineral material, thereby promoting sintering. Post sintering thermal treatment under an alternative oxygen fugacity causes the formation of voids within the aggregates.
In one specific group of embodiments of the process of the present invention, starting mineral ores of kaolinite and bauxite were ground to a fine powder (approximately 30 micron) and doped with up to ten weight percent of hematite (Fe2O3) each. The powders were spheroidized in an industrial mixer and size classified by sieving to isolate aggregates in the size range of 12-20 to 20-40 mesh. The resultant mixtures were then heated in a rotary kiln at a temperature in the nominal range of 1400-1600� C. under a forming gas atmosphere (N2/H2 mixture). The oxygen partial pressure was below 0.05 atm, and it was noted that during the sintering process the Fe2O3 was initially reduced to FeO, which forms a metastable eutectic mixture with alumina, silica, and aluminosilicates at a temperature of approximately 1148� C. The formation of this eutectic mixture promoted the sintering of the mineral material at a relatively low temperature. Capillary forces aided in the passage of the iron-rich aluminosilicate liquid through the particulate material, thereby redistributing solids and minimizing porosity through solution precipitation reactions between the liquid and the solid.
As the reduction process proceeded, the iron-rich aluminosilicate liquid was further reduced to form elemental iron. Elemental iron does not readily wet ceramic materials, and hence the liquid phase in the interior portions of the aggregate formed pockets or islands while the liquid phase at the exterior segregated to the surface to form islands thereupon. This process resulted in formation of a ceramic sphere having islands of metal dispersed on the outer surface thereof, and further containing metal islands therein. This material could be used as is for a catalyst, and appropriate catalytic activity could be selected by an appropriate choice of metal oxide dopants. FIG. 1 shows a scanning electron micrograph of a cross section of a bauxite-derived aggregate doped with 10% hematite after being heated in the nominal range of 1400-1600� C. under the forming gas. FIG. 2 is a higher magnification of the circled region in FIG. 1. As shown in these two figures, the aggregate is relatively dense and includes significant amounts of iron on the surface thereof.
Next, the thus-produced particles were heated in an oxidizing atmosphere, which in this embodiment was comprised of air at atmospheric pressure. Heating was again carried out in a rotary kiln at temperatures in the nominal range of 1400-1600� C. This heating process caused the internal islands of elemental iron to be taken back up by the solid matrix material. The iron dissolved into the matrix and/or reacted with surrounding crystal phases, as for example to produce iron titanates. The take-up of the metal produced a number of voids in the sintered aggregate via oxidative decomposition of less stable metal oxides and further served to densify and consolidate the outer metal shell/layer, as shown in FIGS. 3 and 4.
The materials thus produced exhibited a structure which combined high strength together with a controlled density. An example of the experimental parameters used in the above-described process are listed below in Table 1. In addition, Table 2 provides properties of particles produced according to the present invention wherein the characteristic strength, specific gravity and specific strength are compared with current state of the art materials CARBOHSP� and CARBOPROP� with a 20-40 mesh size, manufactured by CARBO Ceramics of Irving, Tex. As shown by Table 2, particles of this type have improved properties in terms of a reduction of specific gravity while maintaining strength and an increase in specific strength (i.e. the ratio of strength to density). compared to current state of the art materials and have significant utility as proppant materials.
1.00 � 10−8 Step 2
0.21 (air)
Typical reduction reactions will be carried out at a temperature range sufficiently high to promote the formation of the transient: metastable liquid phase, and this range will typically be 800-1800� C. In some embodiments, the temperature range will be 1100-1800� C., and in other embodiments the temperature range will be 1400-1600� C. Reaction times will depend upon the temperature and the nature of the materials employed, but it is anticipated that most commercially feasible processes will utilize reaction times for the reduction step in the range of 20-120 minutes. The oxidation reaction will typically be carried out under time and temperature conditions similar to those for the reduction step.
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