Research Papers

Impact of Corrosion Test Container Material in Molten Fluorides

[+] Author and Article Information
Luke C. Olson

Savannah River National Laboratory,
Aiken SC, 29808
e-mail: luke.olson@srnl.doe.gov

Roderick E. Fuentes, Michael J. Martinez-Rodriguez, Brenda L. Garcia-Diaz, Joshua Gray

Savannah River National Laboratory,
Aiken SC, 29808

James W. Ambrosek

Woodward Inc.,
1000 East Drake Road,
Fort Collins, CO 80525

Kumar Sridharan, Mark H. Anderson, Todd R. Allen

Department of Engineering Physics,
University of Wisconsin-Madison,
1500 Engineering Drive,
Madison WI, 53711

1Corresponding author.

Contributed by the Solar Energy Division of ASME for publication in the JOURNAL OF SOLAR ENERGY ENGINEERING: INCLUDING WIND ENERGY AND BUILDING ENERGY CONSERVATION. Manuscript received October 8, 2014; final manuscript received September 1, 2015; published online October 15, 2015. Assoc. Editor: Prof. Nathan Siegel.The United States Government retains, and by accepting the article for publication, the publisher acknowledges that the United States Government retains, a non-exclusive, paid-up, irrevocable, worldwide license to publish or reproduce the published form of this work, or allow others to do so, for United States government purposes.

J. Sol. Energy Eng 137(6), 061007 (Oct 15, 2015) (8 pages) Paper No: SOL-14-1286; doi: 10.1115/1.4031682 History: Received October 08, 2014; Revised September 01, 2015

The effects of crucible material choice on alloy corrosion rates in immersion tests in molten LiF–NaF–KF (46.5–11.5-42 mol. %) salt held at 850 °C for 500 hrs are described. Four crucible materials were studied. Molten salt exposures of Incoloy-800H in graphite, Ni, Incoloy-800H, and pyrolytic boron nitride (PyBN) crucibles all led to weight-loss in the Incoloy-800H coupons. Alloy weight loss was ∼30 times higher in the graphite and Ni crucibles in comparison to the Incoloy-800H and PyBN crucibles. It is hypothesized galvanic coupling between the alloy coupons and crucible materials contributed to the higher corrosion rates. Alloy salt immersion in graphite and Ni crucibles had similar weight-loss hypothesized to occur due to the rate limiting out diffusion of Cr in the alloys to the surface where it reacts with and dissolves into the molten salt, followed by the reduction of Cr from solution at the molten salt and graphite/Ni interfaces. Both the graphite and the Ni crucibles provided sinks for the Cr, in the formation of a Ni–Cr alloy in the case of the Ni crucible, and Cr carbide in the case of the graphite crucible.

Copyright © 2015 by ASME
Your Session has timed out. Please sign back in to continue.


Misra, A. , and Whittenberger, J. , 1987, “ Fluoride Salts and Container Materials for Thermal Energy Storage Applications in the Temperature Range 973 to 1400 K,” NASA Lewis Research Center, Cleveland, OH, Technical Memorandum No. 89913.
Forsberg, C. , Peterson, P. , and Zhao, H. , 2007, “ High-Temperature Liquid-Fluoride-Salt Closed-Brayton-Cycle Solar Power Towers,” ASME J. Sol. Energy Eng., 129(2), pp. 141–146. [CrossRef]
Greene, S. , Holcomb, D. , Gehin, J. , Carbajo, J. , Cisneros, A. , Corwin, W. , Ilas, D. , Wilson, D. , Varma, V. , Bradley, E. , and Yoder, G. , 2010, “ SMAHTR—A Concept for a Small, Modular Advanced High Temperature Reactor,” Fifth International Conference on High Temperature Reactor Technology (HTR 2010), Prague, Czech Republic, Oct. 18–20, Paper No. 205.
Schmidt, J. , Scheiffele, M. , Crippa, M. , Peterson, P. , Urquiza, E. , Sridharan, K. , Chen, Y. , Olson, L. , Anderson, M. , and Allen, T. , 2011, “ Design, Fabrication and Testing of Ceramic Plate Type Heat Exchangers with Integrated Flow Channel Design,” Int. J. Appl. Ceram. Technol., 8(5), pp. 1073–1086. [CrossRef]
Williams, D. , Toth, L. , and Clarno, K. , 2006, “ Assessment of Candidate Molten Salt Coolants for the Advanced High-Temperature Reactor (AHTR),” Oak Ridge National Laboratory, Oak Ridge, TN, Report No. ORNL/TM-2006/1.
Olson, L. , Ambrosek, J. , Sridharan, K. , Anderson, M. , and Allen, T. , 2009, “ Materials Corrosion in Molten LiF–NaF–KF Salt,” J. Fluorine Chem., 130(1), pp. 67–73. [CrossRef]
Olson, L. , 2009, “ Materials Corrosion in Molten LiF–NaF–KF Eutectic Salt,” Engineering Physics2009, University of Wisconsin-Madison, Madison, WI.
Olson, L. , Sridharan, K. , Anderson, M. , and Allen, T. , 2010, “ Intergranular Corrosion of High Temperature Alloys in Molten Fluoride Salts,” Mater. High Temp., 27(2), pp. 145–149. [CrossRef]
DeVan, J. H. , 1969, “ Effect of Alloying Additions on Corrosion Behavior of Nickel–Molybdenum Alloys in Fused Fluoride Mixtures,” Vol. I, Oak Ridge National Laboratory, Oak Ridge, TN, Technical Document No. ORNl-TM-2021.
Prasad, S. , 2000, “ The Principle Problems of Aluminum Electrowinning: An Update,” Br. J. Chem. Eng., 17(2), pp. 211–218. [CrossRef]
Godding, A. , and DeAntonio, D. , 1991, “ Liquid Carburizing and Cyaniding,” ASM Handbook: Heat Treating, ASM International, Materials Park, OH, pp. 329–347, 793–814.
Becherer, B. , 1991, “ Processes and Furnace Equipment for Heat Treating of Tool Steels,” ASM Handbook: Heat Treating, ASM International, Materials Park, OH, pp. 726–733.
Ozeryanaya, I. , Zalanzinski, G. , Smirnov, M. , Finkel’shtein, S. , and Shamanova, N. , 1975, “ Corrosion of Molybdenum in Molten Sodium Chloride in the Presence of Carbon,” Zashch. Met., 11(1), pp. 66–68.
Ozeryanaya, I. , 1985, “ Corrosion of Metals by Molten Salts in Heat-Treatment Processes,” Metal Sci. Heat Treat., 27(3), pp. 184–188. [CrossRef]
Williams, D. , Wilson, D. , Keiser, J. , Toth, L. , and Caja, J. , 2003, “ Research on Molten Fluorides as High Temperature Heat Transfer Agents,” Global 2003, Session 2A: Coolant/Material Interactions in Advanced Reactor Systems, Embedded Topical Within 2003 American Nuclear Society Winter Meeting, New Orleans, LA, Nov. 16–20.
Poco, 2013, “ AXZ-5Q,” Poco Graphite Inc., Decatur, TX, accessed Dec. 17, 2013, http://www.poco.com/tabid/92/Default.aspx
Sheppard, R. , Mathes, D. , and Bray, D. , 2001, “ Poco Graphite, Inc. Properties and Characteristics of Graphite for Industrial Applications,” Poco Graphite Inc., Decatur, TX, Report No. 60038.
Ludwig, D. , 2008, “ Analysis Techniques for Corrosion Product Detection in Molten Salts: High Temperature Electrochemistry and Neutron Activation Analysis,” Engineering Physics 2008, University of Wisconsin-Madison, Madison, WI.
Jones, D. A. , 1996, Principles and Prevention of Corrosion, 2nd ed., Prentice Hall, Upper Saddle River, NJ.
Tabet, N. , Allam, I. , and Yin, R. , 2003, “ X-Ray Photoelectron Spectroscopy Investigation of the Carburization of 310 Stainless Steel,” Appl. Surf. Sci., 220(1–4), pp. 259–272. [CrossRef]
Detroye, M. , Reniers, F. , Buess-Herman, C. , and Vereecken, J. , 1999, “ AES-XPS Study of Chromium Carbides and Chromium Iron Carbides,” Appl. Surf. Sci., 144–145, pp. 78–82. [CrossRef]
Streicher, M. , 1976, “ Effect of Composition and Structure on Crevice, Intergranular, and Stress Corrosion of Some Wrought Ni–Cr–Mo Alloys,” Corrosion-NACE, 32(3), pp. 79–93. [CrossRef]
Olson, L. , Fuentes, R. , Martinez-Rodriguez, M. , Garcia-Diaz, B. , and Gray, J. , 2014, “ Reducing Agent Effects on Haynes-230 in Molten Halide Salts,” ANS Annual Meeting, Reno, NV, June 15–19, pp. 859–862.


Grahic Jump Location
Fig. 1

Gibbs free energy of fluoride formation per F2 molecule of metals present in the salt and materials at 850 °C. The more negative the Gibb’s free energy of formation an alloy constituent is in comparison to the salt constituents, the less stable it will likely be in the molten salt.

Grahic Jump Location
Fig. 2

Gibbs free energy of carbide formation per C atom for elements present in the alloys at 850 °C. Favorable reactions have more negative Gibb’s free energy of formations.

Grahic Jump Location
Fig. 3

Schematic illustration of one corrosion capsule apparatus used in the present study for testing corrosion performance of alloys in molten FLiNaK salt at 850 °C for 500 hrs. Dimensions are in centimeters. This design utilized graphite or Incoloy-800H for the crucible material.

Grahic Jump Location
Fig. 4

Sketch of corrosion cells used in research

Grahic Jump Location
Fig. 5

SEM of Cr-rich film on graphite fixturing rod from Incoloy-800H containing crucible tests

Grahic Jump Location
Fig. 6

SEM on graphite central fixturing rod from (a) Incoloy-800H corrosion experiments with a ∼15 μm thick carbide layer. EDS X-ray mapping of elemental (b) Cr and (c) Fe, show the elements are concentrated on the surface and do not penetrate into the graphite.

Grahic Jump Location
Fig. 7

XRD data showing identifying peaks for graphite and Cr7C3 from the Cr film present on the graphite fixturing rod from the Incoloy-800H containing crucible

Grahic Jump Location
Fig. 8

XPS data from the Cr rich film found on the graphite rod that was used to fixture the Incoloy-800H coupons. The sample was progressively sputtered with Ar, followed by sampling of the electron binding energy, leading to a decreasing peak from C contamination and increasing peaks from the graphite rod and carbide.

Grahic Jump Location
Fig. 9

RBS data from the graphite crucible’s bottom and side that held Hastelloy-X coupons during the FLiNaK exposure test

Grahic Jump Location
Fig. 11

Schematic of nonelectric transfer described by Ozeryanaya, as applied to the Fe–Ni–Cr/graphite/FLiNaK system

Grahic Jump Location
Fig. 10

EDS line scan taken from the Ni crucible containing a single Incoloy-800H coupon. The mounting material identified in the SEM image is located on the salt exposed side of the Ni crucible wall.



Some tools below are only available to our subscribers or users with an online account.

Related Content

Customize your page view by dragging and repositioning the boxes below.

Related Journal Articles
Related eBook Content
Topic Collections

Sorry! You do not have access to this content. For assistance or to subscribe, please contact us:

  • TELEPHONE: 1-800-843-2763 (Toll-free in the USA)
  • EMAIL: asmedigitalcollection@asme.org
Sign In