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 PNNL-13644
Phase 3

Novel Concepts for Damage-Resistant

Alloys in Next Generation Nuclear
Power Systems
Final Report, Project 99-0280

S. M. Bruemmer * P. L. Andresen
E. P. Simonen * L. Young
J. Gan ** G. S. Was
F. A. Garner ** L. Fournier
D. S. Gelles ** B. H. Sencer
D. J. Edwards

* General Electric Global Research & Development

** University of Michigan

December 2002

Prepared for the U.S. Department of Energy

under Contract DE-AC06-76RL01830
 DISCLAIMER

This report was prepared as an account of work sponsored by an agency of the

United States Government. Neither the United States Government nor any agency
thereof, nor Battelle Memorial Institute, nor any of their employees, makes any
warranty, express or implied, or assumes any legal liability or responsibility
for the accuracy, completeness, or usefulness of any information, apparatus,
product, or process disclosed, or represents that its use would not infringe
privately owned rights. Reference herein to any specific commercial product,
process, or service by trade name, trademark, manufacturer, or otherwise does not
necessarily constitute or imply its endorsement, recommendation, or favoring by
the United States Government or any agency thereof, or Battelle Memorial
Institute. The views and opinions of authors expressed herein do not necessarily
state or reflect those of the United States Government or any agency thereof.

PACIFIC NORTHWEST NATIONAL LABORATORY

operated by
BATTELLE
for the
UNITED STATES DEPARTMENT OF ENERGY
under Contract DE-AC06-76RL01830

This document was printed on recycled paper.

(8/00)
 NUCLEAR ENERGY RESEARCH INITIATIVE

NOVEL CONCEPTS FOR DAMAGE-RESISTANT ALLOYS

IN NEXT GENERATION NUCLEAR POWER SYSTEMS

Final Report, Phase 3

Project Number 99-0280

Pacific Northwest National Laboratory

S. M. Bruemmer and E. P. Simonen, Principal Investigators
J. Gan, F. A. Garner, D. S. Gelles and D. J. Edwards

General Electric Global Research & Development

P. L. Andresen, Principal Investigator
L. Young

University of Michigan
G. S. Was, Principal Investigator
L. Fournier and B. H. Sencer

December 27, 2002

Prepared for:

U.S. Department of Energy

Oakland Operations Office
1301 Clay Street
Oakland, CA 94612
Attn: Rebecca L. Richardson, NSPD

U.S. Department of Energy

Office of Nuclear Energy, Science and Technology
19901 Germantown Road
Germantown, MD 20874
Attn: Lisa C. Herrera, NE-50

Pacific Northwest National Laboratory

Richland, Washington 99352
 2

TABLE OF CONTENTS

Executive Summary ……………………………………………………………….. 4

Project Objective ……………….………………………………………………….. 5

Project Approach ………………………………………………….……………….. 6

Project Accomplishments …...…………………………………………………….. 6

Publications ……………………...………………………………….………………. 7

Project Management ……………………………………………………………….. 10

Financial Summary ……………………………………………………………….... 10

Research Summary ………………………………………………………………..... 11

Background …………………………………………………………………….. 11

Research Approach …………………………………………………………….. 15

Research Significance and Benefits ……………..…………………………….. 16

Task Objectives by Phase ………………………………………….………….... 17

Detailed Description of Accomplishments …………………………………….. 18

Oversized Elements ……………………………………………………….………… 20

Materials Processing…………………………………………….….……….…….. 20

Irradiations……………………………………………………..…………….…… 20

Heavy-Ion Irradiation……………………………………………………….... 21

Proton Irradiation………………………………………………………..….... 21

Neutron Irradiation………………………………………………………..…... 24

Characterization of Radiation-Induced Microstructures……….….…………..….. 26

Transmission Electron Microscopy Procedures…………………………..…... 26

TEM Measurements of Defect Microstructures…………………………..…..… 27

 3

Characterization of Radiation-Induced Grain Boundary Segregation……..…..…… 48

Measured Grain Boundary Compositions - Ni++ Irradiation…………..…..…... 48

Measured Grain Boundary Compositions - Proton Irradiations……..…..…..... 54

Discussion of Oversized Element Concept for Radiation-Damage

Resistance ……………………………………..……………….……………...….... 57

Insights on Current Understanding for Oversized Solute………….…….…………. 65

Multiphase Microstructure……………………………………………….……………... 67

Ni-Base Alloy Concept Evaluation……………………………..……….………….. 69

Fe-Base Alloy Concept Evaluation…………………………..………..……………. 73

Ferritic/Martensitic Concept Evaluation…………………..………..………………. 79

Mechanical Behavior and Irradiation-Assisted Stress Corrosion Cracking…….….…… 88

Radiation-Induced Hardening………………………………………………..……… 88

Irradiation-Assisted Stress Corrosion Cracking……………………………..……… 90

Crack-Growth Rate Evaluation of Stress Corrosion Cracking……………..…….……… 97

Background……………………………………………….……………...…….…… 97

Materials and Experimental Procedures………………………………..……..……… 98

Crack Growth Test Results and Discussion………………..…………..….………… 102

Stress Corrosion Cracking of Cold-Worked Stainless Steels………...…….…… 102

Stress Corrosion Cracking of Sensitized and Desensitized Stainless Steels.…… 141

Comparisons and Summary of Stress Corrosion Response..…………..….………… 157

References……………………………………..…………..….……………..….………… 174
 4

Executive Summary

Novel Concepts for Damage-Resistant Alloys

in Next Generation Nuclear Power Systems

S. M. Bruemmer and E. P. Simonen

Pacific Northwest National Laboratory
P. L. Andresen
General Electric Global Research
G. S. Was
University of Michigan

December 27, 2002

This project has elucidated approaches for managing damage evolution through control of matrix
solute and multiphase structures. Radiation microstructures, microchemistries and properties
affected by irradiation were evaluated with the goal of developing damage-resistant alloys for
next generation nuclear power systems. Three complementary experimental approaches
identified key factors for the development of alloys: Ni++ irradiation, proton irradiation and
manipulation of simulated irradiation characteristics in non-irradiated alloys. Specifically, alloys
processed with oversized solute, i.e., Hf, and multiphase alloys show promise for retarding
damage evolution.

The discovery of a damage-resistant alloy based on Hf solute additions (oversized solute) to a

low-carbon 316SS is the highlight of the research. This damage resistance is supported by
characterization of radiation-induced microstructures and microchemistries along with
measurements of environmental cracking. The addition of Hf to a low-carbon 316SS reduced
the detrimental impact of radiation by inhibiting the formation of voids and initiation of cracking
during slow-strain rate environmental tests. Because cracking susceptibility is associated with
several material characteristics, separate effect experiments exploring strength effects using non-
irradiated stainless steels were conducted. These crack growth tests suggest that irradiation
strength by itself can promote cracking in high-temperature reactor water environments.

The concept of using oversized solutes to promote catalyzed defect recombination was a major
thrust of this Nuclear Energy Research Initiative project. The successful demonstration of
damage resistance in the optimized Hf-doped alloy demonstrates promise for developing
damage-resistant alloys for future generation nuclear reactors. Differences between irradiation
responses for Hf-doped and Pt-doped alloys suggest that the influence of the oversized elements
has a significant influence on partitioning of point defects in the development of radiation
damage. However, current theories describing the effect of oversized elements on mutual
recombination do not account for all of the observations. Elimination of void formation to a
dose of 50 dpa (during heavy-ion irradiation) is a significant improvement in material
performance. Samples from these initial alloys were prepared and included in a major multi-
year, neutron-irradiation program as part of collaborative research activities.
 5

The second concept for developing damage-resistant alloys is the use of multiphase alloys to
stabilize the microstructure during irradiation. Three alloys have been tailored for evaluation of
precipitate stability influences on damage evolution. The first alloy is a Ni-base alloy (alloy 718)
that has been characterized after neutron and Ni-ion irradiations. The radiation-induced
dissolution of the nanometer-scale precipitates (γ’ and γ”) alters damage evolution, grain
boundary segregation and decreases alloy strength with increasing dose. Two Fe-base alloys
(PH 17-7 and PH 17-4) that also have nanometer-scale precipitate structures were also evaluated
after Ni-ion irradiations. Fe-base alloys are more practical in light water reactors (LWRs)
nuclear structures because of their lower Ni content and hence lesser transmutation to He. The
PH alloys were much more complex with base multiphase microstructures including delta ferrite
and tempered martensite. As for the alloy 718 case, γ’ particles are unstable with irradiation
while fine carbides slightly coarsen. In all cases, the complex multiphase structures resulted in
damage resistance when compared to the simple base alloy design. In addition to the above
experimental studies, a review was conducted to evaluate multiphase ferritic/martensitic alloys
with oxide-dispersion strengthening. One final multiphase alloy approach was employed by
tailoring precipitate distributions and compositions at grain boundaries in a 300-series stainless
steel. Precipitates were found to reduce intergranular SCC crack growth in cold-worked 304SS.

The successful development of next generation nuclear power systems must address and mitigate
several materials degradation issues that now strongly impact existing LWRs and that will limit
structural materials performance at the more aggressive radiation exposures envisioned for
various advanced reactor concepts. Although previous fast reactor and fusion device programs
have focused on the development of improved structural materials for their relevant conditions,
there has been no comparable effort directed toward the conditions unique to LWRs. In addition,
this work directly links material changes at the nanoscale to bulk behavior. Novel, non-
traditional approaches are necessary to create durable damage-resistant alloys and establish the
foundation for advanced reactor designs.

Project Objective

The objective of the proposed research is to develop the scientific basis for a new class of
radiation-resistant materials to meet the needs for higher performance and extended life in next
generation power reactors. New structural materials are being designed to delay or eliminate the
detrimental radiation-induced changes that occur in austenitic alloys, i.e., a significant increase in
strength and loss in ductility (<10 dpa), environment-induced cracking (<10 dpa), swelling (<50
dpa) and embrittlement (<100 dpa). Non-traditional approaches are employed to ameliorate the
root causes of materials degradation in current LWR systems. Changes in materials design are
based on mechanistic understanding of radiation damage processes and environmental
degradation and the extensive experience of the principal investigators with core component
response. This work was integrated with fundamental research at Pacific Northwest National
Laboratory (PNNL) and with focused international projects at PNNL, General Electric Global
Research (GE) and University of Michigan (UM) led by EPRI. This leveraged approach
facilitated the revolutionary advances envisioned in NERI by creating a multi-faceted effort into
the basic and applied science necessary to drive mechanistic understanding and promote
development of next generation materials. The research strategy capitalized on unique national
 6

laboratory, industry and university capabilities for studies of radiation damage and
environmental cracking response.

Project Approach

This project was accomplished in three distinct tasks over a three-year period as documented in
this report. Accomplishments by task of the project are highlighted in the description of Tasks
A, B, and C as part of the detailed report. In summary, novel alloys were selected on the
mechanistic basis for radiation damage resistance. Although neutron irradiation of large
specimens for materials characterization and mechanical property testing would be desirable, this
three-year program could not accommodate that need. In contrast, the program strategy
emphasized irradiation using rapid Ni++ ion irradiation for damage response. Proton irradiations
were conducted to verify the heavy-ion response and allow selected mechanical properties and
SCC behavior studies. To evaluate the effect of the irradiation damage condition on SCC,
testing of deformation-hardened stainless steels was included in work scope. These high-
strength, non-irradiated samples allowed confirmation that matrix strength similar to that created
by irradiation can promote SCC susceptibility and enable tailored microstructural changes to be
evaluated. Finally, in partnership with an international program, promising alloys are being
neutron irradiated for future evaluation as warranted.

Project Accomplishments

Project research is highlighted by the discovery of superior damage resistance for an optimized
alloy of 316LSS+Hf. The damage resistance was evidenced by no void swelling to high dpa,
restricted dislocation loop growth, no radiation-induced segregation after proton irradiation (at
low dose) and no evidence of environmental cracking after proton irradiation. This is in contrast
to the clear evidence of voids, large diameter loops, radiation-induced segregation, and cracking
found in the base 316LSS alloy without Hf. Samples were prepared and included in an
international neutron-irradiation program to achieve doses from 5 to 70 dpa. In addition, the
influence of strength on environmental cracking was quantified. The key implication is that
strength alone promotes cracking without the influence of radiation-induced grain boundary
segregation, radiation-induced microstructure, hydrogen enhancement, or martensite formation.
Precipitate distribution and stability were demonstrated to alter radiation-induced microstructure,
segregation, hardening and SCC.

Task A: Oversized Elements

The damage-resistant alloy based on Hf solute additions (oversized solute) to a low-carbon
316SS showed promise for development of a damage-resistant austenitic stainless steel.
Characterization of radiation-induced microstructures and microchemistries along with
measurements of environmental cracking supported the promise for this alloy. Radiation
induced loop growth was retarded and void formation was suppressed to a high dose of 50 dpa.

Task B: Multiphase Microstructures

Two multiphase microstructures were evaluated with irradiation and microstructural
characterization and exhibited no void formation to the highest doses tested. The complex
structures inhibited the development of radiation-induced dislocation loops and hence formation
 7

of voids. The concept of using ferritic/martensitic alloys with oxide-dispersion strengthening

was reviewed and strategies for development of these alloys were assessed. Carbide precipitate
distributions at grain boundaries were tailored in 304SS and 316SS along with the local
segregation and depletion of alloying elements.

Task C: Mechanical Behavior and Stress Corrosion Cracking

The dependence of IASCC on irradiation and strength was evaluated using proton irradiation and
in a separate experiment using cold/warm work on non-irradiated specimens. Cracking
susceptibility was demonstrated in the proton-irradiated base 316SS and the 316SS+Pt alloys.
Cracking was not observed in the 316SS+Hf optimized alloy. The dependence of crack growth
rate on alloy strength in non-irradiated SSs was extensively evaluated. The strength effect was
confirmed for contrasting conditions of electrochemical potential, martensite formation and
hydrogen contribution. Grain boundary precipitates were found to reduce the crack growth rate
by up to a factor of ten for an oxidizing environment.

Publications

1. S. M. Bruemmer, D. J. Edwards, B. W. Arey and L. A. Charlot, "Microstructural,

Microchemical and Hardening Evolution in LWR-Irradiated Austenitic Stainless Steel," 9th
International Symposium on Environmental Degradation of Materials in Nuclear Power
Systems - Water Reactors, TMS, 1999, p. 1079.

2. D. J. Edwards, E. P. Simonen and S. M. Bruemmer, "Radiation Hardening in Austenitic

Stainless Steels Irradiated in LWRs," 9th International Symposium on Environmental
Degradation of Materials in Nuclear Power Systems - Water Reactors, TMS, 1999, p. 1007.

3. S. M. Bruemmer, “Heat-to-Heat Variability in Radiation-Induced Microstructure and

Microchemistry for Commercial 300-Series Stainless Steels”, Minutes of the International
Collaborative Group on Environmentally Assisted Cracking, April 2000, Williamsburg, VA,
Paper I13.

4. E. P. Simonen, “Transitions in Stainless Steel Radiation-Induced Microstructures from 270 to

370 ˚C ”, Minutes of the International Collaborative Group on Environmentally Assisted
Cracking, April 2000, Williamsburg, VA, Paper I14.

5. J. Gan, G. Was and R. Stoller, “Microstructure Evolution in Austenitic Stainless Steels

Irradiated Under Conditions Relevant to Light Water Reactor Core,” 20th ASTM
International Symposium on Effects of Radiation on Materials, June 2000, Williamsburg,
VA.

6. P. L. Andresen, T. M. Angeliu, W. R. Catlin, L. M. Young and R. M. Horn, “Effect of

Deformation on SCC of Unsensitized Stainless Steel,” Corrosion 2000, NACE, 2000, Paper
203.

7. D. J. Edwards, E. P. Simonen, F. A. Garner and S. M. Bruemmer, “Microstructural

Evaluation of a Cold-Worked 316SS Baffle Bolt Irradiated in A Commercial PWR,” 10th
 8

Int. Conf. Environmental Degradation of Materials in Nuclear Power Systems - Water

Reactors, NACE, 2002.

8. L. Fournier, J. Gan, E. P. Simonen, S. M. Bruemmer and G. S. Was, “Effect of Oversized

Solute Additions on Irradiation-Assisted Stress Corrosion Cracking of Austenitic Stainless
Steels,” 10th Int. Conf. Environmental Degradation of Materials in Nuclear Power Systems -
Water Reactors, NACE, 2002.

9. J. Gan, D. J. Edwards, E. P. Simonen, G. S. Was and S. M. Bruemmer, “Microstructural

Evolution and Hardening in 300-Series Stainless Steels: Comparisons Between Neutron and
Proton Irradiations,” 10th Int. Conf. Environmental Degradation of Materials in Nuclear
Power Systems - Water Reactors, NACE, 2002.

10. S. M. Bruemmer, “New Issues Concerning Radiation-Induced Material Changes and

Irradiation-Assisted Stress Corrosion Cracking,” Invited Paper, 10th Int. Conf.
Environmental Degradation of Materials in Nuclear Power Systems - Water Reactors,
NACE, 2002.

11. S. M. Bruemmer, D. J. Edwards, V. Y. Gertsman and E. P. Simonen, “Grain Boundary

Modification During Neutron Irradiation at Intermediate Temperatures,” Invited Paper,
Microstructural Processes in Irradiated Materials, Materials Research Society (MRS), 2001,
p. R2.1.

12. E. P. Simonen and S. M. Bruemmer, “The Influence of Submicroscopic Vacancy Clusters

During Neutron Irradiation of Stainless Steel near 300oC,” Microstructural Processes in
Irradiated Materials, MRS, 2001, p. R2.5.

13. S. M. Bruemmer and L. E. Thomas, “Insights into Environmental Degradation Mechanisms

from High-Resolution Characterization of Crack Tips,” Invited Paper, Proc. Symposium on
Chemistry and Electrochemistry of Corrosion and Stress Corrosion, The Minerals, Metals
and Materials Society (TMS), 2001, p. 321.

14. D. J. Edwards, E. P. Simonen and S. M. Bruemmer, “Nature of the Fine-Scale Defects and
Radiation Hardening in Stainless Steel Neutron-Irradiated at 550oK,” Microstructural
Processes in Irradiated Materials, MRS, 2001, p. R2.7.

15. L. E. Thomas, B. H. Sencer and S. M. Bruemmer, “Radiation-Induced Phase Instabilities and

Their Effects on Hardening and Solute Segregation in Precipitation-Strengthened Alloy 718,”
Microstructural Processes in Irradiated Materials, MRS, 2001, p. R1.5.

16. E. P. Simonen, “Definitions of Defect Nanostructures Through Post-Irradiation Annealing”,

Minutes of the International Collaborative Group on Environmentally Assisted Cracking,
April 2001, Kjongju, South Korea, Paper I15.
 9

17. S. M. Bruemmer, “Linking Radiation-Induced Material Changes to IASCC Susceptibility”,

Minutes of the International Collaborative Group on Environmentally Assisted Cracking,
April 2001, Kjongju, South Korea, Paper I11.

18. T. M. Angeliu, P. L. Andresen, E. Hall, J. A. Sutliff, S. Sitzman, Strain and Microstructure

Characterization of Austenitic Stainless Steel Weld HAZs", Corrosion/2000, Paper 00186,
NACE, 2000.

19. P. L. Andresen, T. M. Angeliu, L. M. Young, W. R. Catlin, and R. M. Horn, "Mechanisms

and Kinetics of SCC in Stainless Steels", Proc. Tenth Int. Symp. on Environmental
Degradation of Materials in Nuclear Power Systems – Water Reactors, NACE, 2002.

20. P. L. Andresen, "Perspective and Direction of Stress Corrosion Cracking in Hot Water",
Invited Paper, Proc. Tenth Int. Symp. on Environmental Degradation of Materials in Nuclear
Power Systems - Water Reactors, NACE, 2002.

21. P. L. Andresen, L. M. Young, W. R. Catlin and R. M. Horn, "Stress Corrosion Crack Growth
Rate Behavior of Various Grades of Cold Worked Stainless Steel in High Temperature
Water", Corrosion/02, Paper 02511, NACE, 2002.

22. P. L. Andresen, T. M. Angeliu and L. M. Young, "Effect of Martensite & Hydrogen on SCC
of Stainless Steels", Paper #01228, Corrosion/01, NACE, 2001.

23. P. L. Andresen, "Similarity of Cold Work and Radiation Hardening in Enhancing Yield
Strength and SCC Growth of Stainless Steel in Hot Water", Corrosion/02, Paper 02509,
NACE, 2002.

24. P. L. Andresen, T. M. Angeliu and L. M. Young, "Immunity, Thresholds, and Other SCC
Fiction", Invited Paper, Proc. Staehle Symp. on Chemistry and Electrochemistry of Corrosion
and SCC, TMS, Feb. 2001.

25. G. S. Was, J. T. Busby, T. Allen, E. A. Kenik, A. Jensson, S. M. Bruemmer, J. Gan, D. J.

Edwards, P. M. Scott, and P. L. Andresen, J. Nucl. Mater. Vol. 300, No. 2-3, pp. 198-216,
2002.

26. J. Gan, E. P. Simonen, S. M. Bruemmer, L. Fournier, B. H. Sencer and G. S. Was, “The

Effect of Oversized Solute Additions on the Microstructure of 316SS Irradiated with 5 MeV
Ni++ Ions of 3.2 MeV Protons,” J. Nuclear Materials, in press.

27. D. J. Edwards, E. P. Simonen and S. M. Bruemmer, “Evaluation of Fine-Scale defects in

Stainless Steels Neutron-Irradiated at 275C,” J. Nucl. Materials, in press.

28. D. J. Edwards, E. P. Simonen, F. A. Garner, B. A. Oliver and S. M. Bruemmer, “Sensitivity

of Microstructural Evolution Due To Temperature and Dose Gradients In Neutron-Irradiated
316SS,” J. Nucl. Materials, in press.
 10

29. L. Fournier, B. H. Sencer, G. S. Was, J. Gan, S. M. Bruemmer, E. P. Simonen, E. A. Kenik,

Proceedings of Fontevraud 5 – Contribution of Materials Investigation to the Resolution of
Problems Encountered in Pressurized Water Reactors, French Nuclear Energy Society,
September 2002.

30. G. S. Was, J. T. Busby, M. Hash, R. Dropek, B. H. Sencer, L. Fournier, T. Allen, J. Gan, J.

Cole, E. Kenik, E. P. Simonen and S. M. Bruemmer, “Influence of Oversize Solute Additions
on IASCC of Proton-Irradiated Austenitic Stainless Steels,” 11th Int. Conf. Environmental
Degradation of Materials in Nuclear Power Systems - Water Reactors, American Nuclear
Society, 2003, to be published.

31. P. L. Andresen, L. Young and R. Horn, “Effects of Yield Strength, Potential, Stress Intensity
and Grain Boundary Carbides on Stress Corrosion Cracking,” 11th Int. Conf. Environmental
Degradation of Materials in Nuclear Power Systems - Water Reactors, American Nuclear
Society, 2003, to be published.

Project Management

All milestones were completed on schedule. Irradiation and characterization were accomplished
to 50 dpa using Ni++ ions and to 5 dpa using protons utilizing both microstructural and
microchemical examinations. Solute addition and multiphase alloys were fabricated for the
irradiation experiments. Charged particle irradiations of the solute addition and multiphase
alloys were completed and extended to the optimized alloy for the case of Hf addition.
Demonstration of matrix strength effects on SCC growth rates was achieved. The thesis for
damage modification using misfit solute atoms and multiphase microstructures were confirmed
by analyzing high-dose microstructures and by performing SCC tests on selected proton-
irradiated alloys.

Financial Summary

Spending occurred at a consistent rate meeting projections throughout this 39-month project that
ended September 30, 2002.

1600

1400
Project Cost, $K

1200
1000
800

600
400 Planned Cost
200 Actual Cost

0
0 10 20 30 40
Month
 11

Research Summary

Background

Material degradation is a primary limitation for the safe and economical operation of commercial
nuclear power reactors.1,2 Traditional approaches for alloy development have emphasized minor
modifications in alloys (predominantly austenitic stainless steels) that were developed for use in
non-irradiation environments. As problems were discovered during service, alloy characteristics
or service conditions were adjusted to provide modest improvements in performance and
hopefully achieve adequate component lifetimes.

However, it is now clearly recognized that such minor traditional alterations are not sufficient to
mitigate radiation-induced property degradation (loss in ductility and toughness, void swelling
and embrittlement) and environmental cracking (referred to as irradiation-assisted SCC or
IASCC). Therefore, unconventional metallurgical approaches and alloys outside standard
stainless steels must be adopted to optimize performance in the radiation and corrosive
environments of next generation nuclear reactors.

Radiation-induced degradation is driven by the displacement of atoms from their lattice sites and
the subsequent creation of interstitial and vacancy defects as shown in Figure 1. Defect
recombination, migration and their annihilation at sinks promotes a wide variety of potentially
detrimental material changes including dislocation loop formation that leads to extensive

Interstitial
primary
knock-on
atom

Vacancy

Solute with Large

Size and Mass
Figure 1. Schematic of the damage process for influence from a large size or large mass solute.
The primary knock-on atom can be created with ions, protons or neutrons. Minor additions
(3,000 appm) of massive oversized solute are being explored. Large elements in solution perturb
the cascade production of defects and subsequent irradiation damage.
 12

hardening and limited uniform ductility, segregation of alloying and impurity elements to grain
boundaries and other sinks, and void swelling. These changes are inevitable in standard stainless
steels during LWR irradiation and result in an increasing susceptibility to failure with core
component exposure. Displacement of atoms from irradiation cannot be avoided; they are the
result of fundamental Newtonian mechanics. The path for aggregation of defects into
detrimental microstructures can be avoided. The processes of migration and aggregation of
displacement defects are illustrated in Figure 2. Atoms of large size or mass misfit and fine-
scale precipitate distributions interfere with the processes of recombination, migration and
aggregation.

Displacement events can be created by ion, proton or neutron particles. Heavy ions and protons
have the advantage of producing damage at high rates and therefore are commonly used for
fundamental studies of damage mechanisms. Neutrons have the advantage of producing damage
in bulk materials and therefore have the advantage for studies of bulk properties that are relevant
to assessment of structural integrity. In this research, heavy-ion irradiation is used first as a
screening tool to assess damage microstructures in candidate alloys. Protons are used for
additional microstructural studies and for studies of mechanical behavior and stress corrosion
cracking. Specimens for neutron-induced damage are included in a collaborative research
program using the Bor-60 reactor in Russia. The neutron-irradiated samples will not be
examined under this NERI program. Damage from ions, protons and neutrons can be related

GRAIN
BOUNDARY T LOOP
(INTERSTITIAL AGGREGATION)
GRAIN
BOUNDARY

I-Migration

I MUTUAL V
RECOMBINATION
V-Migration

T
VOID
(VACANCY AGGREGATION)

Figure 2. The fundamental products of displacement damage are interstitials (I) and
vacancies(V). These point defects migrate and collect in components of radiation damage.
Interstitials collect preferentially in interstitial loops and the remaining supersaturation of
vacancies collect in voids. Solute atoms of large size or mass misfit and preciptiates disturb the
migration and aggregation of these point defects and therefore damage evolution is optimized.
Damage can be induced using ions, protons or neutrons and can be characterized using
transmission electron microscopy.
 13

800
Thermal Vacancy Flux-Temperature Regions Used

Irradiation Temperature, C
Formation Dominates for Charged Particle Irradiations

o
600

LWR Peak Protons Ni Ions

400 Flux Region

Radiation-Induced
200 Segregation

Recombination Dominates Due

0 to Limited Vacancy Migration

-8 -5 -4 -2
10 10-7 10-6 10 10 10-3 10
Radiation Flux, dpa/s

Figure 3. Increasing the rate of damage requires using a higher temperature to obtain equivalent
damage microstructures. The lower temperature range is limited by mutual recombination and
the upper temperature range is limited by the energy for vacancy formation. Equivalent ranges
for neutrons, protons and ions are shown.

using a compensation of higher temperature for higher rate processes. The interdependence of
damage rate, temperature and particle type is shown in Figure 3.

The development of radiation damage microstructures has two primary effects on components:
(1) swelling and (2) mechanical behavior. Swelling is detrimental because the component
dimensions change during service that affect stresses and core component dimensional
tolerances. A primary concern in the present research is the affect on mechanical behavior and
IGSCC. The effect of displacement damage on interstitial loop development, and on the increase
in yield strength, for LWR-irradiated components has been documented. The measured increase
in tensile yield strength is shown in Figure 4.
1000
Measured Tensile Yield Strength, MPa

800

600

304SS Jenssen
304SS Jenssen
304SS Jenssen
400 304SS Jenssen
316SS Jenssen
316SS Jenssen
316SS Jenssen
316SS Jenssen
316SS Bergenlid
304SS Kodama
200 316SS Kodama
347SS Kodama
304/316SS Odette/Lucas
Neutron-Irradiated
300-Series Stainless Steels

0
0 1 2 3 4 5 6 7

Square Root, dpa

Figure 4. Irradiation Dose Effects on Measured Tensile Yield Strength for Several 300-Series
Stainless Steels reported in the literature near 288˚C. Microstructures for several of these alloys
were characterized at PNNL.
 14

A four-fold increase in yield strength occurs over the first few dpa of irradiation. The effect of
this large increase in yield strength on IGSCC is a critical issue examined in this research.

The critical links between damage processes, materials characterization and property
measurements are highlighted in Figure 5. Although the primary components of irradiation
damage (vacancies and interstitials) are simple, their aggregation into the microstructure and
influence on deformation, void swelling and fracture are complex processes requiring a
complementary mix of experiments being conducted on this NERI program.

The above radiation damage mechanisms affect lifetime for components exposed to high
irradiation doses as shown in Figure 6. Recent work has enabled many aspects of IASCC
phenomenology to be explained (and predicted) based on the experience with IGSCC of non-
irradiated stainless steel in BWR water environments. This continuum approach has successfully
accounted for radiation effects on water chemistry and its influence on electrochemical corrosion
potential. However, the specific radiation-induced microstructural and microchemical changes
that promote IASCC susceptibility are largely unknown. Well-controlled IASCC data from
properly irradiated, and properly characterized, materials is sorely lacking due to the affect
experimental difficulties and financial limitations related to working with highly activated
.
Radiation Hardening, Localized Deformation and Creep
Processes Impacting Crack-Tip Micromechanics
oo o o oo
oo
oo
ooo oo

o oo

Crack Tip
oo o o

oo o

Processes
o o oo
o

During IASCC
o oo
o oo ooo

oo o o
o oo o

ooo
o
oo

H
oo

H
H+ Rad iat io n-I nd uce d C ha nge s
GRAIN H+
H H Rea ct or W ate r Ch em ist ry
BOUNDARY O OH-
Corrosion OH- =
H2O2 H2O
Reactions
at Crack Tip
Enrichme nt & Dep letion o f Defect Clusters and
21 Alloy ing & Impu rity Eleme nts 17 Dislocation Loops n
oo
o

16
Chromium Concentration, w t%

Nickel Concentration, w t%

20
15
19 300-Series SS
Chromium LWR Irradiated 14
Cr, to ~2 dpa Ni,
18 13 Radiation Damage
. wt%
FEG-ATEM
Measurement 12
wt%
Vacancy & Interstitial
17
11 Defect Production
Nickel
16
10

15 9
-20 -15 -10 -5 0 5 10 15 20
Distance from Grain Boundary , nm

Rad iat io n-I nd uce d C ha nge s in

Gra in Bounda ry Co mpo sit io n

Figure 5. Schematic illustrating mechanistic issues believed to influence crack advance during
IASCC. Understanding is advanced through alloy design, irradiation experiments (ion, protons
and neutrons, microstructural and microchemical characterization, and measurements of
mechanical and stress corrosion cracking properties. Interstitial aggregation results in loops that
strength, which in turn affects SCC. Concurrent void production (not shown in the schematic)
does not affect IASCC but does affect dimensional stability and component lifetime.
 15

P W R C o n tro l P W R B a ffle
B W R E nd R o d F a ilu re s B o lt F a ilu res PW R E nd
B W R C o re (IA S C C )
o f L ife (IA S C C ) o f L ife
C o m p o n en t
F a ilu res P W R L ife
(IA S C C ) E x ten sio n

10 20 10 21 10 22 10 23
N eu tron Fluence, n/cm 2 (E > 1 M eV ) G eneration IV
Irradiation D ose, dpa M aterial G oals

0.1 1 10 100

Significa nt C hange s O n set o f S ig n ific an t

in G rai n B ound ary V o id S w ellin g
C om position, A lloy an d P o ssib le
Strength & D uctility E m b rittle m e n t

Figure 6. Neutron fluence effects on alloy characteristics and IASCC susceptibility of 304SS in
LWR environments. Dose effects on mechanical behavior and swelling are also shown.

materials. The paramount need to understand and mitigate IASCC led to the formation of an
internationally funded, Cooperative IASCC Research (CIR) project of which PNNL, GE and UM
are participants. Many of the important metallurgical, mechanical and environmental aspects
that are believed to play a role in the cracking process are illustrated in Figure 5. Since only
persistent material changes are required for IASCC to occur, in-core processes such as radiation
creep and radiolysis influence cracking, but are not controlling mechanisms. The current
understanding of persistent material changes (dose affects) that are produced in stainless alloys
during LWR irradiation is elucidated based on the fundamentals of radiation damage from
experimental measurements.

Research Approach

The response of alloys to irradiation has been evaluated using a variety of irradiation
experiments using neutrons, electrons, protons and heavy ions. Each irradiation technique
possesses both advantages and disadvantages. Neutron irradiation is the preferred choice based
on providing the practical environment of engineering interest. Conversely, neutron irradiation
has the disadvantage of requiring expensive resources and many years for materials studies.
PNNL has an extensive history in the conduct and interpretation of neutron and charged-particle
experiments from mechanistic and alloy development efforts for fast-reactor and fusion-energy
programs.

A productive approach for obtaining screening results has been to use charged particle
irradiations for establishing the physical basis for phenomenological interpretation and
mechanism development. Research conducted over the last ten years at PNNL has demonstrated
that quantitative comparisons between Ni++ ion and LWR neutron irradiations can be made for
radiation-induced microstructural (defect clusters, dislocation loops and voids) and
microchemical (grain boundary segregation) evolution. In addition, localized deformation and
hardening behavior has been effectively investigated. Within this irradiation strategy, neutron
irradiations are used to confirm and calibrate models for mechanistic interpretation and
engineering applications.
 16

Proton irradiation techniques have been developed in parallel with heavy-ion irradiation
techniques. Similar advantages and disadvantages occur for both. However, proton penetration
depths are greater than for heavy ions (40 µm vs. 1 µm) making protons a preferred technique for
observing “bulk” irradiation effects and mechanical property behavior. Proton PKA spectra are
softer than heavy ions and neutrons but none-the-less many experimental correlations have
indicated the usefulness of proton irradiation for simulating neutron irradiation effects. Recent
work at UM has demonstrated that radiation microstructures (dislocation loops and voids),
microchemistries (grain boundary segregation), hardening and IASCC susceptibility can be
produced by proton irradiation (at 360oC) in 300-series stainless steels in a nearly identical
fashion as for LWR neutrons (at 280oC).

Standard mechanical property and SCC tests cannot be performed in ion-irradiated specimens
because of the limited depth range of ions. Therefore, a strategy has been adopted based on
using thermo-mechanical heat treatments of non-irradiated alloys to produce similar
microchemistries and mechanical properties as expected in irradiated alloys. A continuum in
SCC behavior has been demonstrated using irradiated and non-irradiated specimens of the same
alloy type. Cold working on non-irradiated 300 series stainless steels is evaluated to demonstrate
if material strengthening can promote enhanced IG crack growth rates without the need for grain
boundary microchemical changes.

Research Significance and Benefits

The present research has the potential to eliminate one of the most significant economic and
safety issues facing current and future nuclear power systems. This work integrates
fundamental and applied science resources to design advanced core component structural
materials with the required resistance to radiation and environmental degradation
mechanisms. Thus, the research benefits a wide range of areas from fundamental science to
applied alloy development. The research strategy and the combination of national laboratory,
industry and university resources enables important NERI objectives to be achieved:

1) Advanced materials concepts are being developed and scientific breakthroughs facilitated
to overcome a principal obstacle facing nuclear fission reactors. The focus on next
generation LWR concepts will promote relatively near-term (within 10 years) benefits for the
safe and economical operation of commercial nuclear power. This is essential considering
the current status of the nuclear power industry worldwide.

(2) The effective integration of national laboratory (PNNL), industry (GE) and university
(UM) team members focuses their scientific research and development infrastructures on
nuclear energy issues and fosters a leveraged approach to address basic and mission-oriented
research. Industry partners and collaborators ensure that radiation material science
breakthroughs are effectively transferred to advance the state of nuclear technology.
International cooperation and U.S. leadership in the research is ensured by the collaborative
experimental activities as part of two separate multi-national projects led by EPRI. Principal
investigators play an important role in the oversight of these projects and foster continuous
interactions to transfer novel materials concepts into engineering application.
Another Random Scribd Document
with Unrelated Content
 The narrow ways were lined with shops and bazaars, offering
the shopper a wide variety of commodities.
“But most of the things they sell you don’t want,” smiled Bob,
glancing at a counter laden with coarse native food.
The youths noticed that certain streets were devoted to the
selling of certain products. For instance, one avenue was lined with
shops displaying brassware.
“It ought to be easy to find what you want,” grinned Joe. “Just
walk down one street and you will have a large choice of the same
thing.”
The boys spent nearly a half-hour in the native quarter. Finally
Bob suggested that they get back to the hotel, and his friend was
also in favor.
In a short time they were back in the hostelry and proceeded to
go to their rooms. But they were scarcely at the doors when the
sound of footsteps came to their ears. The next moment Dr. Kirshner
came into view.
“Hello,” greeted Bob, and then his jaw dropped.
That something was wrong was evidenced by the frown that
was on the archæologist’s face. His usual smile was absent.
“There’s been a wreck,” he said in an anxious voice. “The train
has been wrecked. I guess we can’t get to Wargla so soon after all.”
 CHAPTER IV
Lured to Danger

B OB and Joe gasped in astonishment.

“The train wrecked!” muttered Bob and then started. “What
caused it?”
“I imagine you’re thinking the same as I,” the archæologist said
quietly. “That those thieves were responsible for it to prevent us from
getting to Wargla at once.”
Joe’s face glowed with anger.
“The dirty beggars!” he cried. “Was anyone hurt?”
“No. It happened that no one was. But the locomotive was
derailed and lodged in a ravine, and the work of getting it back on
the track and repairing it won’t start any too soon in this country. It
may be two or three days before order will be restored. It looks like
those robbers have won out after all.”
They walked on into the room, where they were met by the
boys’ fathers and Fekmah.
“Is there anything wrong?” asked Mr. Holton, as he noticed the
sober faces of his friends.
The situation was explained, and the men frowned. Fekmah
especially was agitated.
“May the black monsters of Tidihet feast on them!” he
exclaimed, running his fingers through his white hair. “Allah will
punish them—they will not go free!”
“But that won’t help us any,” said Mr. Lewis dryly. “We’ve got to
figure out some way to stop them, if it’s at all possible. The question
is, what will it be?”
 “There’s no way of telegraphing,” said Dr. Kirshner, gazing
thoughtfully at the floor. “If we had any idea where they went—that
is, what route they took—we might overtake them on fast
dromedaries. But the chances even then would be slight.”
“We might——” began Joe but was interrupted by a knock at the
door.
For a moment the adventurers looked at one another in surprise.
Then Mr. Holton moved over and cautiously opened the door.
The figure that stood in waiting was a tall, powerful Arab, with
dark, piercing eyes that were none too pleasant to look at. He
towered several inches above Mr. Holton, who was himself nearly six
feet. Around the man’s shoulders and reaching nearly to the floor
was a white gown, and on his head was the conventional hlafa.
For several moments he stood looking at the occupants of the
room, as though forming a rapid opinion of the situation. Then he
again turned to Mr. Holton and muttered something in the native
tongue.
That Bob’s father understood was evidenced by the look of
surprise that came on his face. A moment later he turned to his
friends.
“He says Fekmah is wanted by a friend,” Mr. Holton said. “Won’t
say any more. I don’t know what to make of it.”
“A friend?” Fekmah gasped. “Why, I know no person here. What
could it mean?”
Again the stranger said something in Arabic and motioned for his
objective to come out.
For a moment Fekmah was thoughtful. Then he decided to
investigate.
“I will be back in short minutes,” he said and walked toward the
door.
“Wait a minute,” called Dr. Kirshner. “I’m going with you.”
“And I, too,” cried Bob, getting up from his chair.
Joe also put in a request, but the archæologist shook his head.
 “Two more are enough,” he said quietly, as he and Bob followed
the Arab down the hall.
“Be careful,” warned Mr. Lewis, as they reached the stairs.
“There’s no telling what that fellow may want.”
They reached the street and were directed around the corner
and up a narrow byway, the stranger remaining several yards in the
van.
“Keep a ready hand on your automatic,” whispered Dr. Kirshner
to Bob. “Something may happen in a short time now.”
“Do you believe Fekmah is really wanted by friends?” the youth
asked, glancing about as if he expected any minute to be confronted
by a band of desperate characters.
“Beyond me,” was the reply. “But I believe it would be safer to
say no than yes. But there is a possibility that he met someone and
has forgotten about it.”
“What could they want of him? It all seems funny to me.”
On they went, now upward by a gently sloping street that was
so crooked it seemed to have no outlet.
Suddenly the street stopped at a narrow, winding stairway that
led almost straight up. All about were crowded houses of clay, dirty
and weather-beaten and suggesting that only the very poorest of
Arabs lived there.
Having made sure that the others were following him, the
stranger led the way up the stairs. At the head was a small door, and
this was opened for them to go inside.
But they hesitated.
“Ask him what he wants,” directed Bob. “There could be
anything in there.”
Dr. Kirshner turned to the Arab and in a stern voice put the
question before him.
The latter surveyed the American closely, then said in the native
tongue:
 “I wish nothing of you. It is Fekmah who is wanted. But if you
and your friend must intrude, you may come in.”
The man’s attitude did not win the friendship of the explorers,
but chiefly because they were at a loss to know what to do next they
followed him inside.
A moment later the door was closed and they found themselves
in a sort of twilight.
As soon as their eyes became accustomed to the dim light, they
made out four figures sitting in the corner of the room. The bare
floor alone served the place of chairs, and the men seemed
comfortable. Bob at once formed the conclusion that these Arabs
were of the same type as the stranger who escorted them here, and
felt a bit uneasy. He would have felt much better with a hand on his
gun, but this would have aroused the suspicions of the natives.
Nevertheless he kept on guard for any treachery. If it came to a
fight, he knew that it would be two to five, for Fekmah was, in his
age, not capable of taking part.
None of the Arabs was able to speak English, evidently, but Dr.
Kirshner knew the native language from his previous visits to North
Africa. And he promised to translate occasionally to Bob.
But a moment later it was plain that there was little translating
to be done, for one of the Arabs said something to Fekmah and
motioned for him to come into the next room. The Americans were
to remain where they were.
“I don’t like this,” muttered Dr. Kirshner, as he and Bob were told
to be seated on the floor. “Anything may happen to him in there.”
“Suppose we go with him,” suggested Bob.
The archæologist nodded. He arose from his chair and started to
follow, but one of the Arabs gently pushed him back.
“It is Fekmah who is wanted,” the fellow said in a queer bass
voice. “You will wait here. It will only be a moment.”
Dr. Kirshner had half a notion to push through and follow his
Arab friend, but he changed his mind and sat down with Bob on the
floor.
 “What’s the big idea of all this?” the youth asked in a puzzled
voice. “They trying to double-cross us or something?”
The archæologist did not answer, for he felt all too sure that
something serious was wrong. But what was there to do?
There was no conversation between the archæologist and the
natives, for each seemed busy with his thoughts. Bob was extremely
grave, and he wondered what was taking place in the adjoining
room. Perhaps the Arabs wished to sell Fekmah something and did
not wish to be thwarted by the whites. Or perhaps they wanted to
engage themselves as guides on the coming expedition and knew
they would have a better chance with Fekmah than with the
Americans. But whatever it was, Bob felt uneasy. If their friend did
not return before long he would go after him, the youth thought.
“We’ll wait a few more minutes,” said Dr. Kirshner. “Then——”
“Listen!” commanded Bob. “What was that?”
“I didn’t hear anything. What——”
“There it is again. Sounds like a muffled cry for help. It’s—it’s
Fekmah!”
 CHAPTER V
A Fight for Freedom

B OB was on his feet in an instant and dashed toward the door to

the next room. But two of the Arabs were there first. With a catlike
quickness they drew knives and advanced on the Americans. The
other two natives came at them from the side.
“What does this mean?” demanded Dr. Kirshner, looking from
one to the other, his black eyes snapping with anger.
“You are going to die!” was the grim answer from an evil-
looking, flat-nosed fellow. He moved forward a step or two.
Bob did not understand the man but sensed that something
sinister was to take place. He noticed the look of anger and anxiety
on the scientist’s face.
With a sudden movement he drew out his automatic, at the
same time stepping back several feet. His action was so quick that
the Arabs were taken by surprise and stood for several moments
trying to grasp the true meaning of it all.
“Now get back!” he commanded, flashing the shining pistol in
their faces. “Take away their knives,” he said to Dr. Kirshner. “I’ve got
them covered. Tell them I’ll shoot the first man who makes a forward
move.”
The scientist did as directed and found that, beyond a vicious-
looking knife, they were unarmed.
“You stay here and guard them,” said Bob. “I’m going in and see
what’s happened to Fekmah.”
He moved over to the door and opened it. Holding the pistol in
readiness, he walked slowly in the room. One glance told him that no
one was in sight. But there was a door leading into a large alcove,
and it was possible that he could find someone there. Perhaps the
Arabs were in hiding, having sensed that they were in danger.
Tiptoeing as quietly as possible, Bob made his way to the closed
door. He stood for several moments wondering what to do next.
Then he decided to make a bold move.
Clutching his tiny automatic tightly, he took hold of the knob and
with a sudden twist threw open the door.
The next instant he shrank back, for a tall Arab was almost upon
him. The man held a vicious-looking knife in his uplifted right hand
and was apparently ready to open the door when Bob did so first.
During the next few seconds Bob’s brain was in a whirl. He had
half a mind to shoot the fellow outright and take no chances. But a
moment later he thought better of it. He did not want to be guilty of
murdering even this cruel Arab. If he had been as good a shot with a
pistol as he was with a rifle, he would have shot the knife from the
fellow’s hand. But as it was, he knew this could not be done.
Suddenly the Arab lowered the knife and, scowling cruelly, he
rushed at the youth furiously.
Realizing that he must act quickly, Bob aimed at the man’s leg
and fired. But his hand was unsteady from the terrific strain, and the
bullet missed and lodged itself in the wall.
With a hoarse bellow the Arab came forward with terrific force,
muttering angrily. He had the knife in readiness now, and was about
to plunge it into the youth’s body when something unexpected
happened.
Seeing a good chance, Bob pushed his foot forward with all his
strength, bringing the man down with a thud that resounded through
the little room. The Arab was taken completely unawares, and the
knife went sliding across the floor.
The next instant he was on his feet, and, showing his black
teeth wickedly, he darted toward his young enemy, his large hands
ready to grip anything they might rest on.
Now was the time to act, Bob thought. Leaping forward, he sent
his fist crashing into the Arab’s nose with all the strength in his
powerful young body.
The man reeled, backed up, and then fell against the wall.
Another victim of the youth’s boxing ability had gone to his fate.
Perspiration was dripping from the boy’s brow. His leg ached
from the twist he gave it in bringing the Arab to the floor. Every
muscle in his body seemed fatigued. For a brief moment a sensation
of nothingness crept over him, and he felt slightly numb.
With a start he regained his composure and, with one glance at
the still limp Arab, he dashed through the door, the shining automatic
still in his possession. One thought stood out in his mind above all
others. He must find Fekmah.
No one was in the alcove, but another door led out into a sort of
hallway, and casting aside all thoughts of personal danger, Bob
passed through it.
The next instant he found himself in a narrow passageway, with
no windows or other means to admit light. The semidarkness was
tantalizing, overcoming, but the boy went bravely on. Occasionally he
stopped to listen. But no sound reached his ears. Could it be possible
that Fekmah had been....
The thought was not a pleasant one, and Bob dismissed it from
mind. Here was a door. Perhaps this would reveal something.
As quietly as possible he turned the latch and peeped in the
room.
In the darkness he could make out no one at first. Then his eyes
almost burst from his head as he saw, lying on the floor in the
corner, tightly bound and gagged—Fekmah!
For a moment Bob stood spellbound. Then he rushed over to the
unfortunate man.
“Fekmah,” he cackled gently and then bent over and felt of the
Arab’s heart. It was still beating, and with a swift motion of a small
knife Bob cut the ropes that bound the man. Then he removed the
gag and stood back to see if his friend had been injured.
The Arab’s eyes opened, and he sat up with a start. A moment
later the look of fear vanished from his face as he saw Bob.
 “Praise be to Allah!” he murmured, getting feebly to his feet.
“Are you hurt?” the youth asked.
“No—not yet,” was the grim reply. “But the evil-doers were going
to come back and kill me if I not tell where to find treasure. It is time
now that they come. Let us go in haste, or they will stab us.”
“Treasure?” cried Bob. “You mean they wanted you to tell where
the hidden riches in the desert are?”
“Yes. They were going torture me if I not tell. They are demons.
Allah curse them!”
“But how did they know?” demanded Bob. “How did they find
out about it? They’re not the same ones who wrecked the train, are
they?”
Fekmah shook his head.
“How they find out, I not know,” he said.
Cautiously they made for the door and opened it. Satisfied that
there was no one in sight, they walked through the hallway and into
the alcove.
“Now we must be careful,” Bob warned. “I knocked a man out a
while ago, and he may have come to by now.”
But when they reached the place, they found the fellow still
limp.
At sight of the Arab, Fekmah looked at Bob with admiration. It
was evident that the youth had gone beyond his expectations.
In a short time they reached the door into the first room and
found that Dr. Kirshner was still guarding the Arabs. The scientist
looked up in relief when he again saw Bob and Fekmah.
“I feared something had happened to you,” the scientist said. “I
shouldn’t have allowed you to go in there,” he said to Bob. “But I see
you’ve done your duty and brought back Fekmah.”
“But what shall we do now?” Bob asked. “Are there any officers
to take charge of these crooks?”
“Yes,” the archæologist returned. “You and Fekmah stay here
and guard these men and I will go after them. It is best not to take
them down to the police station for fear of attracting too much
attention. Other Arab friends might charge us in a large band.”
The next moment he was gone, after having promised that he
would be back with officers in a few minutes.
“There ought to be some way to get the fellow I knocked out in
here,” Bob thought, as he guarded the Arabs closely. “But I’d better
not risk letting Fekmah have the gun. I’ll trust the fellow is still out of
his senses when Dr. Kirshner and the officers arrive.”
The Arabs whom the youth was guarding were silent, but their
evil faces suggested what they would do if given the chance.
Bob was in a position where he could also watch the door in the
next room. He was taking no chances on an attack from behind.
“I bet Dad and the others are worried,” the boy thought. “We’ve
been gone a long time.”
Inside of ten minutes Dr. Kirshner was back with three native
policemen, who handled the crooks roughly. Each man was
handcuffed and made to walk in front of the officers.
“Now,” said Dr. Kirshner, “suppose we get back to the hotel
room. Our prolonged absence has probably caused a great deal of
anxiety among our friends.”
“Yes,” Bob returned. “We——” He stopped suddenly and then
dashed into the next room for the crook whom he had previously
knocked out.
But he was not surprised to find the man gone. An opened door
revealed that he had escaped.
“No use looking for him,” the youth thought, as he retraced his
footsteps back to his companions.
Bob was forced to explain to Dr. Kirshner, who was puzzled at
the youth’s sudden dashing away. When he had finished, the scientist
regarded him admiringly but warned him against taking unnecessary
chances.
“Those fellows would think nothing of stabbing you to death,” he
said, shaking his head gravely.
 They went on up the street and arrived in a short time at the
hotel in which were their friends. Up at Fekmah’s room they were
given a hearty welcome.
“What kept you so long?” asked Mr. Holton, seeing at a glance
that something was wrong.
Dr. Kirshner related the details of the previous happenings,
laying stress on the pluck and bravery of Bob.
The naturalists and Joe listened closely, eager to get an account
of everything. They did not seem unduly surprised, for at the start
they felt that something was wrong. But that their friends would be
in such grave danger was not in the least anticipated.
“It’s lucky that you’re here to tell it,” said Mr. Lewis, with a
shaking of his head. “Such desperate characters know nothing else
but to rob and kill.”
“But as it is,” smiled Joe, “you came out all right, and had an
unusual experience at that.” Secretly he was sorry he had not taken
part in it.
“And that is the second time Bob brought in criminals,” said Mr.
Lewis, recalling an incident that happened the summer before.
“I’d rather you wouldn’t take such risks, though,” urged Mr.
Holton. “If one taxes good fortune too much, he is sure to come to a
tragic end some time.”
There was a short silence. Then Joe ventured to touch upon the
matter that concerned them before the abrupt interruption of a short
time ago.
“What will be our next move?” he inquired.
“Hmm,” hesitated Dr. Kirshner, “that is hard to say at present. I
suppose, though, that the logical thing to do is wait and take a train
to Wargla as soon as possible. When the track will be cleared is hard
to say. It might be a day, or it might be several. I can see no other
way of getting to Wargla, can you, Fekmah?”
“No,” replied the Arab. “Of course there are good roads part of
way, and might ride automobile some of way, but train could get
there sooner, even if we wait.”
 “I guess you’re right,” agreed Joe, thoughtfully. “There’s no use
wasting time trying to do a thing that can’t be done. Have you made
inquiries as to about when we can expect the train to be ready?”
“Yes,” answered Dr. Kirshner. “The station agent said inside of
two days, but it probably won’t be that soon.”
“Let’s hope it will,” said Bob. “I’m anxious to get started into the
desert. How long will it probably be before we reach our destination,
once we get started on camelback?”
“That all depends,” replied the archæologist. “If we see fit to use
dromedaries, or the one-hump camel, we will make much better
time. They can travel from ninety to a hundred miles a day with
ease, and if forced, can do much better than that.”
“But the jolting is most uncomfortable,” Mr. Lewis reminded him,
and Fekmah nodded.
“Soon get used to it, though, don’t you?” asked Joe.
Fekmah laughed.
“No, never,” he said. “But not feel it so bad after many days of
riding.”
“But getting back to your question,” resumed the archæologist,
speaking to Joe, “if we have good luck we should cover the thousand
miles to the Ahaggar Mountains inside of two weeks, considering, of
course, stops at oases, small towns, and the like. Then how soon we
can find the hidden riches would be a mere guess, because without
the map Fekmah will probably have much more difficulty in
recognizing various landmarks.”
“But you must remember that our main object was to work for
the good of science,” Bob’s father said. “Mr. Lewis and I were to get
specimens of any animal life that exists in the far reaches of the
desert, and you were to look up the remains of ancient civilizations.
Incidentally, though, we’ll search for the hidden riches.”
“And Joe and I were to take motion pictures when we get
started on camelback,” said Bob proudly.
“Speaking of animal life,” began Mr. Lewis, “suppose in the
morning we get out in the open country and see if we can collect any
specimens. From what I’ve read and heard, I guess it is necessary to
go at least as far as Arba before we would find a region that is worth
hunting in.”
“I’m with you,” said Mr. Holton. “We’ll engage an automobile to
take us the fourteen miles or so to Arba, and then foot it from there.
It will be funny if we can’t bag a few worth-while specimens, at
least.”
“Of course Joe and I can go, can’t we?” grinned Bob.
“You bet. And Dr. Kirshner and Fekmah, if they care to.”
But those persons announced that they would remain in Algiers
and further discuss the coming expedition.
“Then too,” the archæologist remarked, “I’d like to keep posted
on the progress made in getting the train ready for the journey to
Wargla.”
It was well past noon, and the explorers now realized for the
first time that they were extremely hungry. The strain of the eventful
morning had stimulated their appetites to a high degree, and they
felt they could devour almost anything in the way of food.
“Lead me to the café and watch what happens,” said Joe,
making for the door.
The others followed, and although not as emotional they were
no less hungry.
The meal tasted good, despite the fact that they were ignorant
of its composition. Fekmah tried to explain one of the dishes, but the
foodstuffs used in its preparation were unknown to the Americans,
and they were as much in the dark after he had finished the
explanation as before he had begun it.
“We’ll trust there isn’t anything repulsive in its make-up,” smiled
Mr. Holton.
“At any rate the taste isn’t so bad,” came from Bob. “I’ve seen
stuff much worse.”
“Referring to the delicacies of the South American Indians, I
suppose,” laughed Mr. Lewis, and the boys nodded.
 “We were forced to eat almost anything for a while,” reflected
Joe. “Getting lost in the Brazilian jungle was a serious thing, and we
realized it. Then when we got in with those savages, we accepted
their offer of food at once, even though we weren’t sure it was all
right.”
“That was a great adventure, boys,” remarked Mr. Holton, his
thoughts going back to the countless days of river traveling in
unknown South America. “The more I think of it the more convinced
I am that we should be extremely proud of that exploit. Mr. Lewis
and I have had many adventures in unknown lands while collecting
specimens for the museum, but none surpasses that one.”
“I’d like to go there some time,” said Dr. Kirshner. “But so far, my
work as an archæologist has not called me into that region. When it
will, if ever, I do not know.”
After the bountiful meal the explorers took it easy in the hotel,
and Fekmah returned to his room.
“Since we haven’t anything in particular to do, we might as well
rest up for the hunting trip tomorrow,” said Mr. Lewis, as he and the
others sat in the lobby of their hotel. “We’ve had a hard day of it and
deserve to be idle for a while.”
The others agreed, and the remainder of the day was spent in
quiet.
But early the next morning the boys and their fathers were
busily preparing for the hunting expedition. By seven o’clock they
had their rifles and other necessities in readiness, and with a farewell
to Dr. Kirshner, who wished to talk over the Sahara journey with
Fekmah, they left the hotel.
Mr. Lewis had earlier made arrangements for a car to take them
to Arba, whence they would go on foot into the forests and desert.
The automobile was parked in a small garage not far away, and they
reached the place in but a few minutes. It was a low, dirty structure,
with few windows.
A swarthy native came out to meet them and at once recognized
Mr. Lewis. He led the way through a small door and into a room that
served as the garage.
“Here we are,” said Joe’s father, as they rounded a corner.
He pointed to something that at once caused Bob and Joe to
burst out with laughter.
 CHAPTER VI
Through Unknown Forests

“T HAT a car—an automobile?” asked Bob, holding back his

laughter.
“You don’t mean to say that thing will take us fourteen miles!”
cried Joe, no less moved than his chum.
The naturalists smiled. They had apparently not expected this.
“It’s about the best we can do here,” confessed Mr. Lewis. “Of
course there are better automobiles, but none of them seems to be
for hire. You see, this drive-yourself idea doesn’t appear to be very
popular here. I suppose it’s because there is so much danger of
being attacked by bands of nomads who would think nothing of
robbing the occupants and stealing the car. But this car, although not
beautiful to look at, has a good motor and good tires, and that’s
about all we could expect. Remember, we’re not in America now.”
The object of their remarks was indeed not anything to be
especially proud of. A well-known American make, it had undoubtedly
been of great service in its time, and was still capable of covering
many more miles. It had no top, and nothing to show that one had
been present, but the seats were in fair condition, and a well-shined
windshield promised to keep away the formidable dust of the desert.
“Well, I suppose we could do much worse,” sighed Joe, taking
his place in the back seat.
After a few more remarks with the keeper of the garage, the
adventurers started the motor and pulled out into the street, Mr.
Lewis at the wheel. The chug of the engine was almost deafening,
but, as Bob remarked, they would probably get used to it.
 “Ought to be some new springs,” said Joe, with a wink at his
chum.
“And there could be new upholstering,” added Bob. “Of course it
needs new——”
“All right, boys,” smiled Mr. Holton, cutting off their capricious
suggestions. “If you don’t like it, you know what you can do.”
“I guess we’d better shut up,” grinned Bob. “We may get thrown
out on our ear.”
Mr. Lewis had studied the map of Algiers and had no difficulty in
finding his way out of the city and to Maison Carrée, which might
almost be called a suburb of the metropolis. From here they went
almost straight south and soon came to a narrow river, which was
spanned by a small bridge.
“Scarcely any curves from here on,” said Mr. Lewis, as he
increased the speed of the car.
The road remained good, and in a short time they reached Arba,
their destination. Here for the first time they caught a glimpse of a
camel caravan, for they are never seen as far as Algiers. It was
composed of about ten dromedaries, with only three riders. Strapped
on the brutes’ backs were packs containing probably dates and other
products of the desert.
Bob and Joe took in the scene with intense interest, for soon
they would be fitted out in a like manner for the long desert journey.
The youths were particularly anxious to observe the manner in which
the brutes are ridden. They had heard that to straddle a camel and
be able to bounce freely along was an art that came only of long
practice. Whether this was true they did not know but resolved to
find out sooner or later from Fekmah.
“I’ll bet it’s harder than it looks, though,” remarked Joe.
A little later they saw other caravans of donkeys, the usual beast
of burden used near the coast.
“The Arab, unlike other natives, never carries his load,”
explained Mr. Holton. “I guess he thinks it lowers himself too much.”
 They drove on into the town and had more trouble finding good
streets than in Algiers.
Luckily it was Wednesday, and the market was in full swing.
Traders were swarming everywhere, buying and selling the queer
native goods and foodstuffs.
“Suppose we park the car where we can and look about a bit,”
suggested Joe. “It’s no special hurry to begin the hunt, is it?”
The others were more than willing, and as soon as possible the
automobile—if it could be called that—was stopped at a convenient
corner.
“Sure feels good to get out and stretch,” smiled Bob, taking
advantage of the opportunity to relax his cramped legs.
They left the car and made for the business center of the town,
intent upon spending a half-hour or so in watching the busy scene of
interest.
It was soon discovered that except for the large market there
was little of interest to be seen. In many respects the town
resembled Algiers, although on a much smaller scale and not nearly
as modern. The streets were narrow and, in many cases, curving,
and the houses were far from attractive. But the hustle and bustle of
the natives clearly indicated that Arba was of considerable
importance commercially.
This was especially noted in the city market, where every article
imaginable was for sale. Bakers, vegetable dealers, butchers,
shoemakers, wine venders, and many others did their best to
convince the buyer of the worth of their products.
“And over there in that tent is a physician,” pointed out Mr.
Lewis. “How good he would be considered in the United States is
hard to say, but the Arabs seem to have confidence in him. Look at
the patients going in.”
“For my part, I’d rather trust nature to cure my illness,” smiled
Bob, as he noted the rather blank expression of the native physician.
The explorers spent nearly a half-hour in the city, taking in the
various sights so strange and interesting to a visitor from a far-away
land. At last Mr. Holton moved that they go back to the car and get
their rifles and begin the hunt, and the others were in favor of doing
so.
Their lunch, cartridges, binoculars, and other hunting necessities
were packed in lightweight ruck sacks, which required but a minute
to strap on their backs.
The car was to be left where it was, as probably no better
parking place could be found.
“Guess we’re ready,” said Mr. Lewis, picking up his rifle.
It required but a short walk to reach the edge of the town, and
one glance revealed that the country here was wild and uncultivated.
Mountains were but a short distance away, and some of the peaks
were rather impressive.
“Those forests look like there might be anything in them,”
observed Joe, directing his glance at the towering wooded slopes.
“We’ll see in a short time,” said his father, fumbling his rifle.
The foothills over which they were passing were, for the most
part, bare and devoid of heavy vegetation. But a little later they
came to a region that gradually sloped upward, and less than an
hour’s traveling brought them to the base of a high, sloping
mountain, which was covered with a dense forest.
With renewed efforts they began the task of climbing, keeping a
sharp lookout for any wild animals that might dart out in front of
them.
“About all the wild animals to be found here are rabbits, jackals,
hyenas, panthers, and a very few lions,” said Mr. Holton, as they
trudged up the hill.
Luckily there were no sharp cliffs to be scaled. Instead, the way
was gradual, unbroken.
“I’d like to get a glimpse of one of those queer creatures that
have been reported to exist in these woods,” remarked Mr. Holton
with a smile.
“What’s that?” asked Joe.
 “Another Arabian myth, most likely. At any rate I know of
nobody who has ever been fortunate enough to see one. It is
supposed to be about the size of a badger and is a very peculiar
combination of six or more well-known animals. The face, eyes, tail,
abdomen, and other body regions are supposed to be taken from
other creatures; and all the details are very accurate and convincing,
to hear the Arab tell it. Again arises the question of where such
queer conceptions get into his head.”
As they hiked on, Bob and Joe began to get behind their elders.
There was much to be seen in the way of odd plants and colorful
flowers, and their attention was continually diverted from one thing
to another.
“I suppose when we get as seasoned in the art of exploring as
our dads we’ll not notice such minorities,” said Bob. “But right now
——”
He stopped suddenly as he caught sight of something that made
his blood turn cold.
Not five feet away was a huge wild boar, showing its terrible
tusks savagely as it prepared to rush at the youths.
 CHAPTER VII
Good News

“W HAT is it?” cried Joe, as he noticed the look of anxiety on

his chum’s face.
For answer, Bob pointed to the wild boar, and as Joe glanced
around he shrank back in consternation.
“Quick!” he cried. “It’s going to charge!”
There was no time to lose. The animal, angered because
cornered, was getting ready to stand its ground savagely. And the
boys had heard of the wild boar’s terrible ferocity.
Almost in unison the youths raised their rifles and took careful
aim. The guns were of only twenty-two caliber, not any too powerful
for the occasion, but the chance had to be taken.
“Now,” murmured Bob, holding his rifle in a steady position.
Bang! Bang! Two shots rang out, and each found the mark.
But the small bullets did not stop the beast’s charge, and it came
on with horrible atrocity.
“Run!” cried Bob, his nerve completely gone. “Let’s go up a
tree!”
As the youths darted to one side, a shot rang out; another; and
still another. A moment later the wild boar sank to the ground in a
crumpled mass, gave a convulsive twitch, and then lay still.
Mr. Lewis and Mr. Holton came running up, on their faces a look
of apprehension.
“A narrow escape!” said Joe grimly. “It’s a good thing you came
across with those high-speed bullets. They sure did the job, all right.”
 “We just happened to glance around in time,” explained his
father. “We didn’t know you boys were so far behind. Why didn’t you
bring larger rifles?”
“Weren’t expecting to meet such a creature as this,” replied Bob.
“I had an idea that this was a tame country, but I see I’m wrong,”
with a glance at the wild boar.
“You certainly are,” smiled Mr. Holton, shaking his head. “And
this incident may be the beginning of a series of adventures with wild
animals. Where there’s one of a thing there’s likely to be another. So
stick close, boys. I’d hate to have to rely on those twenty-twos
again.”
The wild boar was shattered by the bullets and was no good as
a specimen. The naturalists especially wanted one of these terrible
beasts and were put out to think that this one had been made
worthless by the rifles, but they were thankful that they had been
able to come to the rescue of their sons.
With one last look at the creature they resumed the hike, this
time keeping a closer lookout for any other formidable beast.
As they penetrated deeper into the forest, signs of life began to
increase in numbers. Small rodents darted out, only to be brought
down by the guns of the naturalists; lizards of grotesque and ugly
shapes were all about; birds of many colors flew overhead, their
plumage showing brightly in the sunlight. It was a sight that the
youths never grew tired of.
Suddenly a jackal ran out, and Mr. Holton lost no time in firing at
it. It was carefully but quickly skinned and placed in the burlap bag
for the specimens.
“This forest certainly is untrodden,” observed Mr. Lewis, unable
to discern the faintest traces of human tracks. “It has probably been
a long time since anyone broke into its fastness.”
“Which is all the better for us,” said Joe. “Animals here probably
have never heard the sound of a gun before.”
Along toward noon they picked out a small grassy area and got
out the kit of lunch. The sandwiches were spread on a paper, and
thermos bottles of cold lemonade were opened. To the tired
adventurers it promised to be a feast fit for a king.
“No meal in the most luxurious café tastes better than a
bountiful lunch in the heart of a forest,” said Mr. Lewis.
Bob’s father nodded.
“It has been said that no one but an explorer really knows what
an appetite is,” he remarked. “And in times when I’m working in the
museum at home and not doing any strenuous work I can fully
realize the truth of it.”
They ate the lunch in quiet contentment, taking it easy on the
soft grass. It seemed good to be out on the trail again, feasting on
the wonders of nature. Bob and Joe were impressed by the stillness
of the great forest.
“This is about the only kind of a woods you can get through,”
remarked Bob, his eyes on the numerous cork-oak trees. “A tropical
jungle has so much undergrowth and vines that it keeps you busy
cutting them away with a machete.”
An hour or two after the repast was spent in resting their tired
limbs and chatting merrily. Then Mr. Lewis suggested that they
continue the hunt.
“We won’t have so very much time left,” he said. “And we’d like
to get several more specimens.”
A little later they came to a narrow valley between two high
mountains. A tiny spring trickled from beside a large rock, and they
welcomed the taste of the refreshing liquid. It was quite cold,
showing that it probably came from an underground stream.
“Drink all you want,” said Mr. Lewis. “It’s likely the last water
we’ll see till we get back to Arba.”
All the remainder of that afternoon the explorers trudged on,
bringing down several small animals and birds. None of them
happened to be dangerous, however.
The hunters had described a wide circle that took them by
sundown within a mile or two from Arba, and the accuracy of the
naturalists’ calculations was greatly appreciated, for they were very
tired and did not feel that they would care to have to hike a great
distance to get to the automobile.
“Wonder if the old car’s still there,” mused Bob, as they came to
the limits of Arba.
“Don’t know why it shouldn’t be,” returned his chum. “Nobody’d
want it for anything.”
It required but a short time to reach the main part of the town.
Then they turned off on the street where the car was parked.
“It’s there!” cried Joe, making out its ancient shape in the
distance.
The others shared in his enthusiasm. They had had an uneasy
feeling about its safety all day, despite the fact that the ignition had
been locked.
In a short time the explorers were in the seats, and Joe, who
had asked to drive, began the task of starting the engine. It finally
responded to the sluggish self-starter.
“Now let’s hurry and get back to Algiers,” urged Mr. Holton. “We
don’t want to be out after dark, for there’s no telling how good these
lights are.”
During the next half-hour Joe pulled the throttle as far down as
possible, and then complained because he could only do forty-five.
However, it was not long before they saw the lights of Algiers in the
distance.
“Now to get something to eat,” said Mr. Holton, sitting up in the
seat in anticipation. “It will be good to see the old hotel again, won’t
it?”
“Sure will,” replied Bob. “I’ll bet Dr. Kirshner expected us long
before this.”
“He’s probably conversing with Fekmah,” was the opinion
expressed by Mr. Lewis. “You know,” he went on, “that Arab is a
strange contrast to these worthless fellows around here. It all goes
to show what anyone can do if he wants to.”
“He’s educated, too, isn’t he?” inquired Joe.
 “Yes, highly,” the naturalist replied. “Was graduated from the
University of Algiers and received a degree. What he doesn’t know
isn’t worth knowing.”
“Where is his home?” asked Bob. “He doesn’t live in Algiers,
does he?”
“No. He lives in Oran; that’s about a hundred and twenty-five
miles or so west of here. Quite a prosperous city, I guess.”
“But,” questioned Bob, thoroughly puzzled, “what is he doing
here in Algiers?”
“It all goes back to Dr. Kirshner’s conversation with him on the
ship,” Mr. Holton explained. “You see, Tom”—referring to the
archæologist—“met him on the last day of the voyage and
recognized him to be a very intellectual man. As soon as Fekmah
found that he could trust Kirshner, he confided this secret about the
hidden riches. Well, then, when he found that we would accept his
proposition and make it one of the objects of the expedition to
search for this treasure, Fekmah put up at a hotel in Algiers in order
to accompany us into the Sahara. See?”
“Sure. I don’t know now why I didn’t before.”
They were now among the lights of Algiers, and Joe headed
straight for the business section, where the car was to be returned to
the garage.
They reached the place in a short time and left the automobile.
Then they hurried around to their hotel.
When they came to their room, they found Dr. Kirshner and
Fekmah in earnest conversation. When the two heard their friends in
the hall, they arose, wreathed in smiles.
“We have good news for you,” announced Dr. Kirshner joyously.
“The train is leaving for Wargla in the morning.”
 CHAPTER VIII
Off for the Sahara

“H URRAH!” burst out Joe, overwhelmed with delight. “We’ll get

ahead of those crooks after all.”
“When did you find out?” asked Mr. Holton, as overjoyed as the
youth.
“Late this afternoon,” was the response. “We intended to make
frequent trips to the railroad station in order to know as soon as
possible. The agent there informed us that the track had been
cleared last night and the locomotive repaired this morning. He didn’t
give the impression that there are other trains on this route, but I
suppose there are.”
“That’s fine!” exclaimed Mr. Lewis, as excited as a boy. “We’ll get
a meal at once and then complete preparations for the journey. Have
you two eaten?”
“Yes,” returned Fekmah. “It is getting late. Six, seven o’clock.”
The naturalists and their sons made their way to the café and
did full justice to a delicious meal. Then they went back to their room
and finished packing their possessions.
“Do you know,” remarked Joe that night just before retiring, “we
were, in a sense, responsible for that train wreck?”
Bob looked up in surprise.
“If it hadn’t been for our proposed expedition, those two Arabs
would have had no cause to wreck the train,” Joe explained.
“Oh. Indirectly, huh? Well, you’re right.”
Very early the next morning the explorers were up making last-
minute preparations. The train was to leave for Wargla at eight
o’clock, giving them three hours or so to use to best advantage.
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