Reactive matrix infiltration of powder preforms
| Title: | Reactive matrix infiltration of powder preforms |
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| Patent Number: | 11565,318 |
| Publication Date: | January 31, 2023 |
| Appl. No: | 17/011316 |
| Application Filed: | September 03, 2020 |
| Abstract: | A reactive matrix infiltration process is described herein, which includes contacting a surface of a preform comprising reinforcement material particles with a molten infiltrant comprising a matrix material, the matrix material comprising an Al—Ce alloy, whereby the infiltrant at least partially fills spaces between the reinforcement material particles by capillary action and reacts with the reinforcement material particles to form a composite material form, the composite material comprising the matrix material, at least one intermetallic phase, and, optionally, reinforcement material particles. A composite material form also is described, which includes a plurality of reinforcement material particles comprising a metal alloy or a ceramic, a matrix material at least partially filling spaces between the reinforcement material particles; and at least one intermetallic phase surrounding at least some of the reinforcement material particles. The reinforcement material particles and intermetallic phase together may form a gradient core-shell structure. |
| Inventors: | Rios, Orlando (Knoxville, TN, US); Bridges, Craig A. (Knoxville, TN, US); Elliott, Amelia M. (Knoxville, TN, US); Henderson, Hunter B. (Livermore, CA, US); Kesler, Michael S. (Knoxville, TN, US); Sims, Zachary (Knoxville, TN, US); Weiss, David (Manitowoc, WI, US) |
| Assignees: | UT-Battelle, LLC (Oak Ridge, TN, US), University of Tennessee Research Foundation (Knoxville, TN, US), Eck Industries Incorporated (Manitowoc, WI, US) |
| Claim: | 1. A composite material form, comprising: a plurality of reinforcement material powder particles comprising a metal alloy or a ceramic, the reinforcement material powder particles having an aspect ratio of from 1 to 2; a matrix material at least partially filling spaces between the reinforcement material powder particles, the matrix material comprising Al and Ce; and at least one intermetallic phase surrounding one or more of the reinforcement material powder particles, the intermetallic phase including one or more elements of the reinforcement material powder particles, Al, and Ce, and wherein, the reinforcement material powder particle is ceramic, an average diameter of the ceramic reinforcement material powder particles is within a rnage of from 65 μm to 250 μm. |
| Claim: | 2. The composite material form of claim 1 , wherein the reinforcement material comprises a Ti-Al-V alloy. |
| Claim: | 3. The composite material form of claim 1 , wherein the reinforcement material comprises a first metal M1, and the reinforcement material powder particles and the intermetallic phase together comprise a gradient core-shell structure comprising: a gradient core comprising M1, Al, and Ce, and a plurality of intermetallic phases, the gradient core having a compositional gradient with a first average M1 concentration and a first average Ce concentration at a first average distance from a center of the gradient core, a second average M1 concentration and a second average Ce concentration at a second, further average distance from the center, wherein the second average M1 concentration is less than the first average M1 concentration; and a shell surrounding the gradient core, the shell comprising an average Ce concentration at least 5 -fold greater than the second average Ce concentration. |
| Claim: | 4. The composite material form of claim 3 , wherein M1 comprises Ti. |
| Claim: | 5. The composite material form of claim 1 , wherein the reinforcement material powder particles are spherical. |
| Claim: | 6. A composite material form, comprising: a plurality of spherical reinforcement material powder particles comprising a metal alloy or a ceramic; a matrix material at least partially filling spaces between the spherical reinforcement material powder particles, the matrix material comprising Al and Ce; and at least one intermetallic phase surrounding one or more of the spherical reinforcement material powder particles, the intermetallic phase including one or more elements of the spherical reinforcement material powder particles, Al, and Ce. |
| Claim: | 7. A method, comprising: contacting a surface of a preform comprising a plurality of reinforcement material powder particles having an initial average diameter and an aspect ratio of from 1 to 2 with a molten infiltrant at a temperature T 1 , wherein T 1 is greater than a melting point of the molten infiltrant and less than a melting point of the reinforcement material powder particles, the molten infiltrant comprising an aluminum-cerium (Al-Ce) alloy and the reinforcement material powder particles comprising a metal alloy or a ceramic, whereby the molten infiltrant at least partially fills spaces between the reinforcement material powder particles by capillary action and reacts with the reinforcement material powder particles to form a composite material form, the composite material form comprising a matrix material comprising the Al-Ce alloy and at least one intermetallic phase comprising at least one element of the reinforcement material powder particles, Al, and Ce, the matrix material at least partially filling the spaces between the reinforcement material powder particles and the at least one intermetallic phase surrounding one or more of the reinforcement material powder particles; and cooling the composite material form to a temperature T 2 less than a melting point of the molten infiltrant, and wherein, when the reinforcement material powder particle is ceramic, an average diameter of the ceramic reinforcement material powder particles is within a range of from 65 μm to 250 μm. |
| Claim: | 8. The method of claim 7 , wherein the composite material form further comprises reinforcement material powder particles having a final average diameter, wherein the final average diameter is less than the initial average diameter. |
| Claim: | 9. The method of claim 7 , wherein the preform is maintained at a temperature greater than the melting point of the molten infiltrant while contacting the surface of the preform with the molten infiltrant. |
| Claim: | 10. The method of claim 7 , wherein the preform is a bonded powder preform comprising the reinforcement material powder particles and a binder, the method further comprising: heating the bonded powder preform to a temperature T 3 , wherein T 3 is effective to decompose the binder and T 3 is less than a melting point of the reinforcement material powder particles and less than a melting point of the molten infiltrant, thereby decomposing the binder and producing the preform, the preform having spaces between the reinforcement material powder particles; and subsequently contacting the surface of the preform with molten infiltrant at the temperature T 1 . |
| Claim: | 11. The method of claim 10 , further comprising forming the preform using binder jet technology. |
| Claim: | 12. The method of claim 7 , wherein contacting the surface of the preform with the molten infiltrant comprises dipping the surface of the preform into the molten infiltrant. |
| Claim: | 13. The method of claim 7 , further comprising subsequently heating the composite material form to a temperature T 4 , whereby the matrix material reacts further with the reinforcement material powder particles to form additional intermetallic. |
| Claim: | 14. The method of claim 7 , wherein the Al-Ce alloy comprises from 5 wt % to 20 wt % Ce with the balance being Al. |
| Claim: | 15. The method of claim 7 , wherein the reinforcement material powder particles constitute 50% (v/v) of the preform. |
| Claim: | 16. The method of claim 1 , wherein when the reinforcement material powder particle is metal alloy, an average diameter of the metal alloy reinforcement material powder particles is within a range of from 20 μm to 250 μm. |
| Claim: | 17. The method of claim 7 , wherein the reinforcement material powder particles comprise a first metal M1, and the composite material form comprises one or more gradient core-shell structures, the gradient core-shell structure comprising: a gradient core comprising M1, Al, and Ce, and a plurality of intermetallic phases, the gradient core having a compositional gradient with a first average M1 concentration and a first average Ce concentration at a first average distance from a center of the gradient core, a second average M1 concentration and a second average Ce concentration at a second, further average distance from the center, wherein the second average M1 concentration is less than the first average M1 concentration; and a shell surrounding the gradient core, the shell comprising an average Ce concentration at least 5-fold greater than the second average Ce concentration. |
| Claim: | 18. The method of claim 7 , wherein the reinforcement material powder particles comprise a metal alloy. |
| Claim: | 19. The method of claim 18 , wherein the metal alloy comprises a titanium alloy, a nickel alloy, a copper alloy, an iron alloy, steel, an aluminum alloy, a high-entropy alloy, or any combination thereof. |
| Claim: | 20. The method of claim 19 , wherein the metal alloy is a Ti-Al-V alloy. |
| Claim: | 21. A method, comprising: contacting a binder jet preform comprising a plurality of reinforcement material powder particles and a binder with an infiltrant comprising an Al-Ce alloy, the reinforcement material powder particles comprising a metal alloy and having an aspect ratio of from 1 to 2; heating the binder jet preform to a temperature greater than a decomposition temperature of the binder, wherein the temperature is less than a melting point of the infiltrant, thereby decomposing the binder and producing a preform having spaces between the reinforcement material powder particles; increasing the temperature to a temperature greater than a melting point of the infiltrant, whereby the infiltrant fills the spaces between the reinforcement material powder particles by capillary action and reacts with the reinforcement material powder particles to produce a composite material form comprising a matrix material comprising the Al-Ce alloy and at least one intermetallic phase comprising at least one element of the reinforcement material powder particles, Al, and Ce, the matrix material at least partially filling the spaces between the reinforcement material powder particles and the at least one intermetallic phase surrounding one or more of the reinforcement material powder particles; and cooling the composite material form to a temperature less than a melting point of the infiltrant. |
| Claim: | 22. The method of claim 21 , wherein the reinforcement material comprises a Ti-Al-V alloy. |
| Claim: | 23. The method of claim 21 , wherein heating the binder jet preform to the temperature greater than the decomposition temperature of the binder is performed under a non-reactive gas. |
| Claim: | 24. The method of claim 21 , further comprising subsequently heating the form to an effective temperature for reaction of the infiltrant with the reinforcement material powder particles. |
| Patent References Cited: | 5224533 July 1993 Kantner et al. 5509555 April 1996 Chiang et al. 10760148 September 2020 Plotkowski et al. 20090263277 October 2009 Pandey 20110142710 June 2011 Kondoh 20180237893 August 2018 Rios et al. 20190085431 March 2019 Rios et al. 20190169725 June 2019 Rios 102011012142 January 2012 1 525 330 July 2003 WO 2017/007908 January 2017 |
| Other References: | Arslan et al., “Quantitative X-ray diffraction analysis of reactive infiltrated boron carbide-aluminium composites,” Journal of the European Ceramic Society, 2003, 23:1243-1255. cited by applicant Dobrzański et al., “Composite Materials Infiltrated by Aluminium Alloys Based on Porous Skeletons from Alumina, Mullite and Titanium Produced by Powder Metallurgy Techniques,” Powder Metallurgy—Fundamentals and Case Studies 2017, Chapter 5, pp. 95-137, published by InTech, Croatia. cited by applicant Sims et al., “High Performance Aluminum-Cerium Alloys for High-Temperature Applications,” accepted manuscript, 12 pages, published in Materials Horizons, Aug. 1, 2017, vol. 6. cited by applicant Yadav et al., “Binder Jetting 3D Printing of Titanium Aluminides Based Materials: A Feasibility Study,” Adv. Eng. Mater., May 15, 2020, 2000408, 7 pages. cited by applicant Yu et al., “Effect of Ti Addition on the Microstructure and Mechanical Properties of SiC Matrix Composites Infiltrated by Al—Si (10 wt.%)—xTi Alloy,” Materials, Jan. 21, 2019, 12, 318, 12 pages. cited by applicant |
| Primary Examiner: | Wang, Xiaobei |
| Attorney, Agent or Firm: | Klarquist Sparkman, LLP |
| Accession Number: | edspgr.11565318 |
| Database: | USPTO Patent Grants |
| Language: | English |
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