DOD STTR 24.A BAA

Active
No
Status
Closed
Release Date
November 29th, 2023
Open Date
January 3rd, 2024
Due Date(s)
February 21st, 2024
Close Date
February 21st, 2024
Topic No.
N24A-T021

Topic

Synthetization of Refractory/Transition Metal Diboride & Carbide Precursors for Chemical Vapor Infiltration (CVI) of Ceramic Composites

Agency

Department of DefenseN/A

Program

Type: STTRPhase: Phase IYear: 2024

Summary

The Department of Defense (DOD) is seeking proposals for the synthesis of refractory/transition metal diboride and carbide precursors for Chemical Vapor Infiltration (CVI) of ceramic composites. This research topic aims to develop stable and scalable routes for new precursors to support the integration of metal diborides into Ceramic Matrix Composites (CMCs) using CVI. The goal is to develop precursors suitable for evaporation in a CVI system, which can be used for coating extreme applications with high melting temperatures, high hardness, and excellent thermal oxidation resistance. The Phase I of the project involves demonstrating the synthesis route and basic precursor properties, while Phase II focuses on optimizing the process, conducting deposition studies, and initiating infiltration studies. In Phase III, the project aims to continue infiltration studies and determine optimal conditions for densification of fiber preforms. The potential impacts of this research include advancements in Ultra High Temperature CMC processing, commercial access to space components, and high-temperature applications in the energy and materials processing communities. The project duration is not specified, but interested parties can find more information and submit proposals on the Defense SBIR/STTR Opportunities website.

Description

OUSD (R&E) CRITICAL TECHNOLOGY AREA(S): Hypersonics

 

OBJECTIVE: Develop a stable, scalable synthesis route for a refractory diboride precursor suitable for evaporation in a Chemical Vapor Infiltration (CVI) system.

 

DESCRIPTION: Properties of refractory/transition metal diborides have attractive coating options for extreme applications with melting temperatures above 3200°C, high hardness, and excellent thermal oxidation resistance. Metal diborides such as hafnium, zirconium, tantalum, iridium, etc. have no commercially available single source CVI precursor. Depositing metal diboride via chemical vapor deposition routes such as CVI offer a viable method of integration into Ceramic Matrix Composite (CMCs) with respect to protective interface coatings. Commercial availability of refractory metal boride precursors to support epitaxial deposition is non-existent and development efforts are scarce. This STTR topic aims to develop stable, repeatable and scalable routes for new precursors for integration into existing large scale CVI systems. This research is critical for domestic development of key precursors identified to have the potential for significant advancements in Ultra High Temperature CMC processing.

 

PHASE I: Demonstrate synthesis route and basic precursor properties (vapor pressure, melting/freezing temperature, density, etc.) using modeling, characterization and experimentation. Determine repeatable and projected scalability of formulation.

 

PHASE II: Optimize process and demonstrate repeatability. Determine projected scalability of compound formulation. Begin Chemical Vapor Deposition (CVD) deposition studies. Evaluate deposition temperature range for amorphous and crystalline coatings and associated data showing crystallinity, grain size and stoichiometry. Initiate infiltration studies.

 

PHASE III DUAL USE APPLICATIONS: Continue infiltration studies, modelling the infiltration process to determine optimal conditions (T, P, flow) to optimize densification of fiber preforms. Determine methods and measures to ensure reproducibility for scaling to larger preform sizes. Dual use activities could include commercial access to space components, as well as other high temperature applications in the energy and materials processing communities.

 

REFERENCES:

Coltelli, Maria Beatrice and Lazzeri, Andrea. “Chemical vapour infiltration of composites and their applications.” Chemical Vapour Deposition (CVD): Advances, Technology and Applications, CRC Press, July 2019, p. 363. https://www.routledge.com/Chemical-Vapour-Deposition-CVD-Advances-Technology-and-Applications/Choy/p/book/9780367780111#
Aguirre, Trevor G.; Lamm, Benjamin W.; Corson L. Cramer, Corson L. and Mitchell, David J. “Zirconium-diboride silicon-carbide composites: A review.” Ceramics International, Volume 48, Issue 6, 15 March 2022, pp. 7344-7361. https://doi.org/10.1016/j.ceramint.2021.11.314

 

KEYWORDS: Precursors, coatings, chemical vapor deposition, chemical vapor deposition, organometallics, ceramic matrix composites