Effect of Normalization and Temper Heat

Treatment on P91 Weldment Properties

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Technical Report
Effect of Normalization and Temper
Heat Treatment on P91 Weldment
Properties

1004915

Interim Report, December 2003

EPRI Project Managers

A. McGehee
K. Coleman

EPRI • 3412 Hillview Avenue, Palo Alto, California 94304 • PO Box 10412, Palo Alto, California 94303 • USA
800.313.3774 • 650.855.2121 • askepri@epri.com • www.epri.com
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CITATIONS

This report was prepared by

EPRI Fossil Repair Applications Center

1300 W.T. Harris Blvd.
Charlotte, NC 28262

Principal Investigators
A. McGehee
K. Coleman

This report describes research sponsored by EPRI.

The report is a corporate document that should be cited in the literature in the following manner:

Effect of Normalization and Temper Heat Treatment on P91 Weldment Properties, EPRI, Palo
Alto, CA: 2003. 1004915.

iii
PRODUCT DESCRIPTION

During the manufacture of components for high-temperature service, a normalize and temper
(N&T) heat treatment is often required to restore properties of the component. This occurs most
when components are fabricated with longitudinal seams but can occur when fabrication
practices damage the base material, as is the case when the lower critical temperature is exceeded
during post-weld heat treatment (PWHT) operations or during hot forming. Weld metals are
formulized to provide adequate service in the subcritical PWHT condition. Long-term properties
for weld metal subjected to this elevated temperature heat treatment are not available. This
project seeks to develop data for this application.

Results & Findings

Coupons were prepared using SA 387-Grade 91 material (9Cr-1Mo-V) welded with the shielded
metal arc welding (SMAW) process and subjected to normalization heat treatment of 1900ºF
(1038ºC) and tempering at 1400ºF (760ºC) in a heat-treatment oven. Residual-hardness
measurements were performed to determine how much softening of the weld metal, heat-affected
zone (HAZ), and base metal was achieved. Coupons were subjected to tensile, toughness, and
rupture testing to determine serviceability of the different heat treatments. Full microstructural
characterization was performed on the ruptured samples to determine failure location.
Toughness, tensile properties, and rupture life were improved for the weld metal and the area
where the HAZ was located prior to normalization heat treatment as compared to a standard
subcritical post-weld heat treatment at 1400ºF (760ºC).

Challenges & Objectives

This report was written to provide plant managers, maintenance managers, and power plant
engineers with an understanding of the effects of an N&T heat treatment on the long-term
properties of weldments. This research is aimed at answering three questions:

1. What effect does an N&T process have on the residual hardness of B9 weld metal and
Grade 91 base metal?

2. How does the N&T process affect the mechanical properties of the weldment and HAZ
location?

3. How does the N&T process compare to a subcritical PWHT in fitness for service?
Following the methods developed in this report can allow the service life of installed components
to be estimated and premature failures to be minimized.

v
Applications, Values & Use
P91 and higher-strength ferritic alloys will continue to see more use in new power plants as
temperatures and pressures are increased to gain higher efficiency. Data derived from this project
will provide utility personnel information as to how the mechanical properties of weldments
conducted with typical B9 fillers will perform following a normalization and tempering heat
treatment.

EPRI Perspective
EPRI has been very instrumental in the development of the Grade 91 alloy in power plants.
Investigations of material properties (TR-103617, P91 Steel for Retrofit Headers – Material
Properties), manufacturing techniques (TR-106856, Properties of Modified 9Cr-1Mo Cast Steel,
and TR-1004702, Optimal Hardness of P91 Weldments), and repair technologies (TR-1006590,
Guideline for Welding P(T)91 Materials) have been conducted. Continued work is ongoing to
provide utilities with a better-performing material that will enable higher-efficiency power plants
and reduce replacement costs.

Keywords
P91
Weld
Hardness
Pipe
Header

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ACKNOWLEDGMENTS

EPRI would like to acknowledge the support of Böhler Thyssen Welding USA for the
contribution of welding consumables utilized in this project.

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CONTENTS

1 INTRODUCTION.................................................................................................................. 1-1
Requirement for Heat Treatment ........................................................................................ 1-1
Avoidance of Temperatures Exceeding AC1 ........................................................................ 1-2
Normalization and Tempering Heat Treatments.................................................................. 1-2
Normalization ................................................................................................................. 1-3
Tempering...................................................................................................................... 1-5
Manufacturing Practices Requiring N&T ............................................................................. 1-6
Cold Forming with Large Strains .................................................................................... 1-6
Hot Swaging or Forming Operations, Including Resizing and Bending ........................... 1-6
Localized Heating for Alignment of Tubing During Installation........................................ 1-7
Manufacture of Longitudinal Seamed Piping .................................................................. 1-7
Hot Bends in Pipe Made Up of Multiple Pipe Pieces ...................................................... 1-8
Material Heated Mistakenly Above the AC1 During PWHT............................................... 1-8
Concerns for Performing N&T on Weld Metal ..................................................................... 1-8
Proper N&T Utilization ........................................................................................................ 1-9

2 TEST PROGRAM ................................................................................................................ 2-1

Test Materials ..................................................................................................................... 2-1
Base Material ................................................................................................................. 2-1
Weld Metal ..................................................................................................................... 2-2
Mockup Fabrication ............................................................................................................ 2-2
Normalize and Temper Heat Treatment.............................................................................. 2-3
Hardness Testing................................................................................................................ 2-4
Tensile Testing ................................................................................................................... 2-5
CVN Testing ....................................................................................................................... 2-6
Creep Rupture Testing ....................................................................................................... 2-6

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3 RESULTS ............................................................................................................................ 3-1

Hardness ............................................................................................................................ 3-1
Tensile Data ....................................................................................................................... 3-1
CVN Data ........................................................................................................................... 3-2
Rupture Data ...................................................................................................................... 3-3
Failure Characterization...................................................................................................... 3-5

4 CONCLUSIONS................................................................................................................... 4-1
Subcritical PWHT Versus N&T of P91 Weldments.............................................................. 4-1

5 REFERENCES..................................................................................................................... 5-1

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LIST OF FIGURES

Figure 1-1 Iron-Iron Carbide Phase Diagram........................................................................... 1-3

Figure 1-2 Continuous Cooling Transformation Diagram for P91 Steel.................................... 1-5
Figure 1-3 Hot Bending Operations ......................................................................................... 1-7
Figure 2-1 Weld Plate Preparation .......................................................................................... 2-3
Figure 2-2 Cross-Section Removal for Hardness Evaluation ................................................... 2-4
Figure 2-3 Typical Hardness Indentation Sites on Cross Section ............................................ 2-5
Figure 2-4 Test Specimen Removal ........................................................................................ 2-6
Figure 3-1 LMP-Versus-Stress Results for N&T and PWHT Weldments (Base Metal
Failures Removed) .......................................................................................................... 3-4
Figure 3-2 General Microstructure Associated with the N&T Treatment for the Base
Metal and Weld Metal Sides of the Composite Rupture Sample ...................................... 3-6

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LIST OF TABLES

Table 1-1 Comparison of “Grade 91 Modified” Weld Metal Compositions................................ 1-9

Table 2-1 Chemistry of Base Metal ......................................................................................... 2-1
Table 2-2 Mechanical Properties of Base Metal ...................................................................... 2-1
Table 2-3 Weld Metal Chemistry ............................................................................................. 2-2
Table 2-4 Mechanical Properties of Weld Metal From Certification.......................................... 2-2
Table 2-5 Test Matrix .............................................................................................................. 2-7
Table 3-1 Cross Section at 50% Thickness Hardness Results of 1400°F (760°C) PWHT
and N&T .......................................................................................................................... 3-1
Table 3-2 Results of Cross-Weld Tension Tests...................................................................... 3-2
Table 3-3 Results of Charpy V-Notch Impact Test of Post-Weld Heated P91 Plates ............... 3-2
Table 3-4 Rupture Hours Data................................................................................................. 3-3

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1
INTRODUCTION

In the ever-increasing competitive environment that utilities are faced with today, an effort to
save costs by using thinner section components has driven the utility industry to use
higher-strength materials. Additional benefits are achieved through the use of these stronger
materials, including lighter-weight support structures, smaller hangers, and more flexible
systems, which are less susceptible to thermal and mechanical fatigue.

One of the alloys currently being utilized in retrofit applications and new installations is
Grade 91 (9Cr-1Mo-V, referred to in this document as P91 for pipe and T91 for tubing). This
material has seen use in replacement headers and tubing during the last 20 years and is starting to
be the material of choice for headers, piping, and tubing in new fossil and combined-cycle plants.

One area of concern with this alloy continues to be what is the proper heat treatment for
weldments in this alloy. During fabrication of components, it is sometimes required to perform
normalization and temper heat treatment on completed welds. The effects of this heat treatment
are evaluated in this report.

Requirement for Heat Treatment

Two of the more commonly used heat treatments employed during the manufacture of Cr-Mo
components are subcritical post-weld heat treatments (PWHT) and normalize and temper (N&T)
heat treatments. Most Grade 91 base materials, pipes, and plates are supplied in the N&T
condition because this heat treatment develops the required service properties in the material.
Weldments generally receive a subcritical PWHT to temper and soften the weld metal and
heat-affected zone (HAZ).

Grade 91 demonstrates substantial hardenability when welded. Although the hardness of the base
material is around 220 Hv, hardness of weld metal prior to PWHT can reach 450 Hv. This large
difference in hardness results in substantial strength differences between the base material and
the weld metal, which can lead to fatigue notches for equipment loaded by cyclic forces.
Additionally, weld metal with hardness of this level generally does not exhibit adequate
toughness to resist crack initiation or propagation. High hardness welds may also be susceptible
to stress corrosion cracking (SCC) in aqueous environments.

To provide good service, the weldment hardness values should be similar to the base metal
values. A subcritical PWHT is normally performed to minimize the hardness mismatch between
the weld and base metal. This PWHT is performed after completion of the weld and before the
component is placed into service.

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Introduction

Avoidance of Temperatures Exceeding AC1

There is also a concern that the lower critical temperature (AC1) is not exceeded during the
PWHT operation. The AC1 temperature has been shown to vary with the nickel and manganese
content of Grade 91 alloy. For P91 base materials, the AC1 depends on composition and is
commonly around 1490ºF (810ºC). Weld metal AC1is generally lower than base metal because it
has higher nickel to develop toughness in the weld. Most filler metal produced by domestic
manufacturers has an AC1 above 1436ºF (780ºC) [1]. However, weld metal may have an AC1 as
low as 1400ºF (760ºC).

PWHT between 1300 and 1400ºF (704 and 760ºC) is required by the American Society of
Mechanical Engineers (ASME) Section B31.1. ASME Section І requires PWHT of Grade 91 to
be carried out at a minimum of 1300ºF (704ºC). Exceeding the lower critical temperature can
substantially reduce the material properties. One method to restore properties to materials that
have been heated above the AC1 temperature is to perform an N&T heat treatment.

Normalization and Tempering Heat Treatments

To understand what actually takes place during a normalizing treatment, one must become
familiar with the representative phase diagram for the material being heat-treated. Additions of
alloying elements such as Cr, Ni, and Mo can shift the various phase boundaries. For the sake of
simplicity, we shall look at the iron-iron carbide phase diagram for steels given in Figure 1-1 [2].

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Introduction

Figure 1-1
Iron-Iron Carbide Phase Diagram

Normalization

An understanding of the critical temperatures (AC1, AC3, and ACM) is warranted in discussing
temperature boundaries associated with heat treating. Critical temperatures are the temperatures
where a material undergoes a phase change. As steels are heated, they encounter their first
critical temperature at approximately 1350ºF (732ºC), where, depending on composition, the
material begins to transform to austenite. Normalization is the thermal process by which steel is
heated into the austenite phase field—that is, above the Ac3 for hypoeutectoid (<0.77% carbon)
steels and above the Acm for hypereutectoid (0.77% <carbon <2.1%) steels. Materials are
typically heated to temperatures approximately 100ºF (38ºC) above the upper critical

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Introduction

temperature and allowed to stabilize so that complete transformation from ferrite to austenite will
occur throughout the thickness of the material. Once uniform temperature is obtained, carbon
and other alloying additions that are soluble in the austenite phase begin to redistribute
themselves throughout the austenitic phase. This homogenization serves to redistribute the solute
elements throughout the matrix to provide a more uniform dispersion upon cooling than what
was imparted during welding and subsequent solidification.

After temperature uniformity has been obtained and sufficient time has been given for
homogenization to occur, the material is allowed to cool in a uniform manner to room
temperature. When the material is cooled, it passes two more critical temperatures, ms and mf.
These are the martensite start and martensite finish temperatures, which are typically represented
on a continuous cooling transformation (CCT) diagram, as shown in Figure 1-2 [3].

Martensite is formed during non-equilibrium conditions. When an air-hardenable material such

as Grade 91 is heated above the lower critical temperature (AC1) and allowed sufficient time for
partial reaustenitization to occur, transformation to untempered martensite at the ms temperature
is expected. Oak Ridge National Laboratory is currently performing tests to determine the
corresponding temperature for the ms and mf for P91 materials. Early results indicate that the ms
is around 400ºF (200ºC) and the mf could be at room temperature or lower [4]. Another
significant aspect of heating above the AC1 temperature is that if a P91 material is not cooled low
enough to completely transform the austenite to martensite, some retained austenite could remain
in the microstructure. This could lead to problems later during the heat-treating process, where
upon cooling to room temperature, regions of untempered martensite could form and cause
undesirable material properties.

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Introduction

°C = (°F - 32) * 5/9

Figure 1-2
Continuous Cooling Transformation Diagram for P91 Steel

Tempering

Because of the increased hardenability of Grade 91, a tempering treatment is commonly

performed for these materials. Tempering provides relief to some of the thermal stresses that
may have been imparted upon cooling from normalizing temperatures and is performed primarily
to increase ductility and toughness. This is accomplished through the precipitation of the
carbides and carbonitrides that occur during exposure to the elevated tempering temperature.
Precise control of the precipitants are governed by the time and temperature in which tempering
is performed.

Normalization and tempering can be performed to produce a vast array of mechanical properties
by controlling normalizing temperatures, time at temperatures, and cooling rates. Tempering
following normalizing can also be used to further refine the mechanical properties. Specific
procedures must be followed to achieve precise mechanical properties for the Grade 91
materials.

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Introduction

One way to restore properties to Grade 91 materials that have been heated in the intercritical
range is to perform a normalization heat treatment. This is normally performed at least
100°F (56°C) above the AC3 temperature and for the material in this project was performed at
1900°F (1038°C). This results in a fully austenitic microstructure. The material is then air cooled
down to room temperature to transform the austenite to martensite. The material is now in the
condition we want to give us our high-temperature creep strength, but it is hard and brittle. To
gain toughness and soften the metal some, it is then tempered at 1450°F (788°C).

Manufacturing Practices Requiring N&T

The question arises: What manufacturing practices require a normalization heat treatment to
restore properties? Several instances are listed below:
• Cold forming with large strains
• Hot swaging or forming operations, including resizing and bending
• Localized heating for alignment of tubing during installation
• Manufacture of longitudinal seamed piping
• Hot bends in pipe made up of multiple pipe pieces
• Material mistakenly heated above the AC1 during PWHT

Any of the fabrication practices above can result in deterioration of long-term high-temperature
properties of Grade 91 material.

Cold Forming with Large Strains

It has been known for over 50 years that large strains deteriorate properties of austenitic tubing.
Construction codes, including codes from the ASME, have rules that allow only low amounts of
strain, generally below 15%, before heat treatment is required. Industry experience with T91
tubing has shown that this material suffers from loss of long-term properties. This phenomenon
is being studied under a separate project by EPRI [5].

Hot Swaging or Forming Operations, Including Resizing and Bending

Tubes for superheat and reheat pendants are frequently hot- or cold-bent. Tubes, depending on
material, can only be cold-bent down to a certain radius. Below that radius, damage to the tube
will occur if it is bent cold. To further reduce the radius, a tube must be heated to a temperature
in the transition range. Because of the strength of piping and the force required to make bends,
most piping is bent hot. Hot bending requires an N&T heat treatment after the forming operation
to restore properties. An example of a hot-bent hairpin tube is shown in Figure 1-3.

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Introduction

Figure 1-3
Hot Bending Operations

Localized Heating for Alignment of Tubing During Installation

One forming method that has resulted in some failures is heating of tubing during fit-up with a
torch to correct minor alignment problems. This has been done for many years on low-alloy
tubing without experiencing problems. This practice cannot be performed on advanced ferritic
alloys like T91 without deteriorating the material. During installation, the field engineer should
watch for boilermakers performing this operation, because most do not know the consequences
of heating this material above the AC1.

Manufacture of Longitudinal Seamed Piping

Since the failures of longitudinal seamed hot reheat piping in the mid 1980s, EPRI has developed
an extensive database on material properties for P22 materials. This database indicates that
normalized longitudinal seamed piping demonstrates better service lives than subcritical
PWHT piping. Reasons for using a N&T heat treatment include:
• The strength of weld metal is reduced closer to that of base metal.
• Type IV failure location is eliminated.
• Better reduction is achieved in the residual stresses than with PWHT operations.

The same data have not been developed for P91 weldments, but many manufacturers are using
normalized P91 piping.

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Introduction

Hot Bends in Pipe Made Up of Multiple Pipe Pieces

Due to availability of piping, fabricators have welded several short pieces of piping together
prior to performing hot-bending operations. This places circumferential welds either in the bends
or in the tangent ends. Subsequent N&T heat treatments to restore properties to the piping base
metal may deteriorate the weld metal in the circumferential welds.

Material Heated Mistakenly Above the AC1 During PWHT

Material mistakenly heated above the AC1 during PWHT frequently occurs due to equipment
failure or incorrect placement of thermocouples. If thermocouples that are controlling the heating
pads break loose and are measuring the temperature of the air under the insulating blanket, the
controllers may drive the pads to too high of a temperature. Control thermocouples for one area
may also be wired to the wrong controller. Insufficient number of thermocouples may also lead
to overshooting set points. Sometimes the controllers are programmed incorrectly or the set point
is set too high. Additionally, on large horizontal pipes, if thermocouples are located on the
bottom of the pipe, the actual temperature on the top may be higher than what is measured on the
bottom.

Concerns for Performing N&T on Weld Metal

When a material is incorporated into a code (ASME or other international code), there are
specific test that are required. These tests include room-temperature tests (toughness, tensile, and
so on) and elevated-temperature tests (rupture tests) on several heats of material. Minimal
information is required on the weld metal, and the information that is provided is generally based
on weldments that have been optimally heat-treated. Data do not exist on weld metal subjected to
heat treatments out of the norm. EPRI and others have accumulated considerable data on B3
fillers used in the N&T condition as a result of many longitudinal seam weld failures that have
occurred on power plant hot reheat piping. These data do not exist for Grade 91 base and B9
filler materials.

One of the reasons for concern is that the B9 weld fillers are formulated to be used in the
subcritical heat-treated condition (PWHT). It is formulated to have adequate toughness, strength,
and ductility after this type of heat treatment. Although carbon is kept to the high end of the
specification in the base metal for strength and nickel is kept low, filler metal generally has
carbon at the low end of the specification for weldability, and nickel is varied to control
toughness and AC1 temperature. Other elements that are different from the base metal to the weld
metal are highlighted in Table 1-1 [1]. It is unknown whether these subtle changes have an effect
on the properties of the weld metal after N&T heat treatment. This concern is addressed in the
current project.

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Introduction

Table 1-1
Comparison of “Grade 91 Modified” Weld Metal Compositions

P/T91 Gr. 91 Gr. 91 Gr. 91 Gr. 91 Gr. 91

Element Steel AWS A5.28-96 AWS A5.23-97 AWS A5.5-96 BS EN 1599:1997 EN 12070:1996
ASME/ASTM ER90S-B9 EB9 E901X-B9 ECrMo91B CrMo91**

Process N/A GTAW SAW SMAW SMAW GTAW

C 0.08/0.12 0.07/0.13 0.07/0.13 0.08/0.13 0.06/0.12 0.07/0.15

Mn 0.30/0.60 1.25 1.25 1.25 0.40/1.50* 0.4/1.5*

P 0.020 0.010 0.010 0.01 0.025 0.020

S 0.010 0.010 0.010 0.01 0.025 0.020

Si 0.20/0.50 0.15/0.30 0.30 0.30 0.60 0.6

Cr 8.00/9.50 8.00/9.50 8.00/10.00 8.00/10.50 8.0/10.5 8.0/10.5

Mo 0.85/1.05 0.80/1.10 0.80/1.10 0.85/1.20 0.80/1.20 0.80/1.20

Ni 0.40 1.00 1.00 1.00 0.40/1.00* 0.4/1.0*

V 0.18/0.25 0.15/0.25 0.15/0.25 0.15/0.30 0.15/0.30 0.15/0.30

N2 0.03/0.07 0.03/0.07 0.03/0.07 0.02/0.07 0.02/0.07 0.02/0.07

Nb 0.06/0.10 0.02/0.10 0.02/0.10 0.02/0.10 0.03/0.10 0.03/0.10

Single values are maximums

* Ni + Mn <1.5
** Draft in Review
SMAW = shielded metal arc welding
GTAW = gas tungsten arc welding
Note: Major differences between base metal and weld metal are highlighted in bold type

Proper N&T Utilization

When an N&T treatment is necessary, it is critical to understand the limitations by which correct
utilization of the process can be conducted on these advanced ferritic type of materials. For
example, suppose a temperature excursion occurs during the installation or repair of a Grade 91
component during a subcritical PWHT, which may have partially reaustenitized the weld/base
metal or caused sufficient over tempering, which may have resulted in a substantial loss in
strength of the component and potentially degraded other physical material properties.
Performing an in situ N&T treatment would not be an option because the heat source (mats,
induction coils, and so on) produces two more transition regions where the heat source ends on
the component, therefore creating essentially the same problem again. There have been
numerous recorded failures citing improper thermal treatments as the root cause.

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Introduction

To evaluate the effect of a normalization heat treatment, a test program using normalized weld
coupons was developed. The program was divided into three main tasks:

1. What effect does an N&T process have on the residual hardness of B9 weld metal and Grade
91 base metal?

2. How does an N&T process affect the mechanical properties of the weldment and HAZ
location?

3. How does an N&T process compare to a subcritical PWHT in fitness for service?

The evaluation was performed on 1.5-inch (3.8-cm) thick coupons heat treated in an oven.
Properties of base metal, weld metal, and HAZs were evaluated. Hardness measurements were
taken with laboratory and field-testing equipment to evaluate the residual hardness. Finally, the
coupons were subjected to rupture testing to determine serviceability of the weldments. Results
were compared to data for standard subcritical heat-treated coupons to see if any advantages
exist in performing an N&T heat treatment over a subcritical post-weld heat treatment.

The test matrix and weldment fabrication is discussed in Section 2, “Test Program.” The test
results, discussions, and conclusions are documented in Section 3, “Results,” and “Conclusions”
in Section 4.

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2
TEST PROGRAM

Test Materials

Base Material

The base metal used for the program was 1.5-inch (3.8-cm) thick American Society for Testing
and Materials (ASTM) A387 Gr 91 CL 2 manufactured by Bethlehem Lukens Plate. The
material was heat treated at the producing mill (normalized 1900°F [1038°C] for 62 minutes air
cooled and tempered 1450°F [788°C] for 109 minutes AC). Table 2-1 shows the chemistry for
the base material [1]. The heat number was C1472. The identification of the plates’ rolling
direction was maintained for proper fabrication of the weld coupon to minimize any lamination
effect on the mechanical properties. The mechanical properties for the plate are shown in Table
2-2 [1]. Note that only one heat of base metal and weld metal was used for this evaluation. The
base metal that was utilized for this project was the same that was utilized in the project
described in EPRI report 1004702, Optimal Hardness of P91 Weldments [6].
Table 2-1
Chemistry of Base Metal

Element (%)
Base
Material
C Mn P S Cu Si Ni Cr Mo V Al Cb N

ASME/ 0.08- 0.30– 0.020 0.010 NS 0.20– 0.40 8.00– 0.85– 0.18– NS 0.06– 0.03–
ASTM 0.12 0.60 0.50 9.50 1.05 0.25 0.10 0.07

Plate 0.11 0.48 0.011 0.003 0.13 0.27 0.28 8.36 0.98 0.217 0.016 0.078 0.046

Table 2-2
Mechanical Properties of Base Metal

Tensile Strength (ksi [MPa]) 0.2% Yield Strength (ksi [MPa]) % Elongation

102.0 [703] 78.4 [540] 22.0

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Test Program

Weld Metal

All B9 filler materials for this investigation were supplied courtesy of Böhler Thyssen Welding
USA. The shielded metal arc welding (SMAW) filler used for the investigation was 0.125-inch
(0.318-cm)-diameter E9015-B9 H4. The chemistry for the filler material is given in
Table 2-3.
Table 2-3
Weld Metal Chemistry

Dia. Element (%)

(in.
[cm]) C Si Mn P S Cr Mo Ni V Al N Nb Sn As Sb Cu

0.125 0.09 0.24 0.73 0.007 0.008 8.55 1.05 0.37 0.17 0.004 0.022 0.054 0.004 0.006 0.001 0.03
[0.318]

The mechanical properties of the weld metal as indicated on the material certification supplied
with the filler metal are given in Table 2-4. The properties of the weld metal were determined
following a normal subcritical PWHT at 1400°F (760°C) for two hours.
Table 2-4
Mechanical Properties of Weld Metal From Certification

Electrode Diameter Tensile Strength 0.2% Yield Strength % Elongation

(in. [cm]) (ksi [MPa]) (ksi [MPa)

0.125 [0.318] 104.0 [717] 85.0 [586] 19.9

Mockup Fabrication

The mockup consisted of a P91 butt-welded plate using a 10° to 40° bevel with the 10° bevel
occurring approximately 2/3 the thickness from the face of the weld plate as shown in
Figure 2-1. This was done for easy removal of the rupture samples and Charpy V-Notch samples.
The welding was conducted utilizing an electrode with a diameter of 0.125 inches (0.318 cm).
The mockup was preheated to 450°F (232°C), and a 550°F (288°C) interpass temperature was
maintained using the SMAW process. The weld direction was 90° to the rolling direction of the
base metal. Welding was performed using stringer bead in the flat position.

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Test Program

Figure 2-1
Weld Plate Preparation

Normalize and Temper Heat Treatment

Normalization of steel is often conducted to obtain certain microstructural and mechanical

characteristics. There are several reasons whereby normalizing a material might be considered.
During normalization of a Grade 91, weldment grain refinement and homogenization of the
microstructure occur. This not only serves to relieve the residual stresses of the weldment but
also breaks down the dendritic structure of the weld and eliminates the HAZ microstructure. This
is beneficial because the fine-grained portion of the HAZ present in all subcritical PWHT
Grade 91 components is the typical failure location (Type IV) in long-term service. Careful
temperature selection, control, time at temperatures, and cooling rates are required to achieve the
desired results for these high-hardenability Grade 91 materials. Because of the Grade 91’s high
hardenability, a tempering cycle must be completed following the normalizing treatment to
obtain the desired combination of strength and ductility. The 1400ºF (760C) subcritical PWHT
temperature investigated in EPRI report 1004702 [6] was shown to provide better tensile, charpy,
and rupture strength results than heat treatment at 1200ºF (649ºC) or 1300ºF (704ºC). Based on
these results, a 1400ºF (760ºC) tempering temperature was selected for comparison of the N&T
treatment proposed in the current research.

The N&T treatment was carried out in a laboratory furnace with thermocouples attached to the
surface of the weld test plate to ensure uniform material temperature. The furnace was brought
up to 1900°F (1038ºC [normalizing/austenitizing temperature]) at approximately 360°F/hr
(182°C/hr) to protect against overshoot. Once up to temperature, the plates were held for
45 minutes and then allowed to still-air cool to room temperature to allow full transformation of
the material from austenite to martensite to occur. The plates were then heated at the same rate as
was utilized for the normalizing thermal cycle to 1400°F (760ºC) and held for 2 hours and
allowed to cool to room temperature to temper the hardened structure that resulted from the

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Test Program

normalization treatment. Tempering following normalization is utilized primarily to increase

ductility and provide increased toughness.

Hardness Testing

After all heat treatment was complete, room-temperature hardness testing was performed to
evaluate the differences in hardness between a N&T heat treatment versus a subcritical PWHT.
In EPRI report 1004702, Optimal Hardness of P91 Weldments [6], evaluations were conducted
to thoroughly characterize the resulting weldment, HAZ, and base metal hardnesses of a
subcritical 1400°F (760°C) PWHT. These evaluations contained the results of hardness testing
performed with laboratory instruments as well as results obtained from various field-testing
equipment. The results from the earlier investigation will be utilized to provide a basis for
comparison of the hardness resulting from the N&T treatment conducted in this project.
Figure 2-2 below shows the typical section removed from the test plate for hardness testing.

Figure 2-2
Cross-Section Removal for Hardness Evaluation

In the present effort, hardness evaluations were conducted on cross-sectioned samples that had
been ground on a surface grinder to approximately a 0.29-µm surface finish and etched with
Villellas Reagent to reveal the weld and fusion zone. Hardness tests were performed in the weld
metal and along the base metal side of the fusion zone where the HAZ existed prior to the grain
refinement that takes place during the normalization treatment. Figure 2-3 shows typical
Rockwell hardness test indentation sites conducted on the cross section of the weldment.

Hardness values were recorded using Rockwell and Micro-hardness testing equipment. The
hardness values were converted from their unique scales to Rockwell B scale so that
comparisons could be made.

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Test Program

Figure 2-3
Typical Hardness Indentation Sites on Cross Section

Tensile Testing

Tensile tests coupons were removed from the center thickness in the 10º bevel portion of the
weld test plate for testing. The fusion line of the weldment was centered in the gage section.
Figure 2-4 shows typical sample removal from the weld coupon. Tensile and yield strength along
with percent elongation and reduction in the area were evaluated and compared against the
results obtained from similar testing performed on the subcritical 1400ºF (760ºC) PWHT weld
coupon.

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Test Program

Figure 2-4
Test Specimen Removal

CVN Testing

Charpy impact tests were removed from the N&T plates and machined with notch placement in
the weld metal and adjacent to the fusion line of the weldment (which would be in the HAZ
location of a subcritical heat-treated weldment). These results were then compared to the results
obtained from the samples removed from the subcritical PWHT test plate evaluated in EPRI
report 1004702 [6].

Creep Rupture Testing

A test matrix for rupture testing was chosen to develop rupture trends associated with the affect
of the N&T treatment. Larson-Miller parameters (LMPs) were calculated and plotted versus
stress. Table 2-5 shows the preliminary test matrix for the N&T plates as well as the subcritical
PWHT plates.

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Test Program

Table 2-5
Test Matrix

PWHT N&T(1900°F/1400°F, Subcritical PWHT @ 1400°F

1038°C/760°C) (760°C)

Test 1050°F 1100°F 1150°F 1050°F 1100°F 1150°F

temperatures (566°C) (593°C) (621°C) (566°C) (593°C) (621°C)

σ to produce 500 500 500 500 500 500

rupture hrs

σ to produce 1000 1000 1000 1000 1000 1000

rupture hrs

σ to produce 2000 2000 2000 2000 2000 2000

rupture hrs

Test temperatures were kept below the 1400°F (760°C) tempering temperatures. The test
temperatures and stresses were chosen to match the range of the LMP-versus-stress plot that was
investigated in EPRI report 1004702 [6].

Composite test samples were removed from the center thickness in the 10º bevel portion of the
weld test plate for testing, as shown in Figure 2-4. The fusion line of the weldment was centered
in the gage section. Postmortem investigation of the ruptured samples was conducted to provide
information as to the rupture location (base metal or weld metal).

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3
RESULTS

Hardness

The results of the hardness testing for the 1400°F (760°C) subcritical PWHT from EPRI report
1004702 [6] and the results of the hardness tests taken on the N&T plates are shown in
Table 3-1. The hardness values presented are values obtained on cross-sectioned samples at mid
thickness of the weldment, which is where the rupture samples were removed. The first number
of each cell represents the average hardness from the sub critically PWHT weldment while the
second number is the result from the N&T plate. All hardness values were converted from their
measured scale to Rockwell B scale for comparison.
Table 3-1
Cross Section at 50% Thickness Hardness Results of 1400°°F (760°°C) PWHT and N&T

PWHT (1400°F, 760°C)/N&T(1900°F/1400°F, 1038°C/760°C)

Instrument
Base Metal HAZ Location Weld Metal

Rockwell 95/90 96/95 97/91

TeleBrineller* 98/91 94/93 96/91

Micro-Hardness* 95/94 97/92 100/93

*All hardness values were converted from their measured scale to Rockwell B scale for comparison.

The results of the hardness testing indicate that the material responded well to the N&T heat
treatment. The spread in hardnesses of the weld metal-HAZ-base metal interface following N&T
is reduced. This in turn tends to ease the metallurgical notch effect of a higher hardness weld
metal relative to the base metal. Micro-hardness tests revealed a slight decrease in hardness
directly adjacent to the fusion zone of the weldment following N&T. This may be indicative of
carbon migration from the higher-carbon base metal to the lower-carbon weld metal, which
resulted in a decarburization effect on hardness of the base metal. Further research would be
necessary to address this question.

Tensile Data

Tensile tests were conducted on samples removed from the subcritical PWHT and N&T weld
plates. The results are listed in Table 3-2.

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Results

Table 3-2
Results of Cross-Weld Tension Tests

Specimen 0.2% Offset Yield Ultimate Tensile % Elongation % R.A.

Strength, ksi (MPa) Strength, ksi
(MPa)

N&T 62.6 [432] 90.2 [622] 21.7 66.6

N&T 65.0 [448] 92.2 [636] 19.8 66.2

1400ºF (760ºC) 61.2 [422] 83.4 [575] 16.0 70.3

PWHT

1400ºF (760ºC) 64.6 [445] 87.4 [603] 18.0 69.0

PWHT

The N&T tensile strengths show a slight increase over the standard subcritical PWHT, while the
yield strengths are approximately the same. The elongation values are also slightly increased for
the N&T samples versus the PWHT. By renormalizing and tempering the weldment, an increase
in strength and ductility was realized most likely as a result of homogenization of the transition
from weld metal to HAZ to unaffected base metal.

CVN Data

Charpy impact tests were removed from the weld metal and HAZs of the subcritical PWHT and
N&T weld plates. The results are given in Table 3-3.
Table 3-3
Results of Charpy V-Notch Impact Test of Post-Weld Heated P91 Plates

Identification Notch Specimen Size Impact Strength, Ft.-Lbs. Avg

Location (in. [cm]) [Joules]
Spec 1 Spec 2 Spec 3.

N&T HAZ 0.394x0.394 126.0 [170.9] 130.3

(1900ºF/1400ºF, [1x1] 133.0 [180.3]
1038°C/760°C) 132.0 [179.0]

N&T Weld 0.394x0.394 113.0 [153.2] 116.3

(1900ºF/1400ºF, [1x1] 126.0 [170.9]
1038°C/760°C) 110.0 [149.2]

1400ºF (760ºC) HAZ 0.394x0.394 147.5 [200.0] 136.7

PWHT [1x1] 135.5 [183.7]
127.0 [172.2]

1400ºF (760ºC) Weld 0.394x0.394 67.0 [90.9] 62.6

PWHT [1x1] 67.0 [90.9]
54.0 [73.2]

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 EPRI Licensed Material

Results

The results of the CVN testing reveal that the base metal HAZ (subcritical PWHT) and fusion
zone (N&T) values are similar. The weld metal values for the N&T plate are approximately
double that of the subcritical PWHT plates. This is most likely due to the homogenization that
occurred during the normalization treatment, which eliminated any grain boundary phase or
retained austenite that may have inhibited the weld metal toughness.

Rupture Data

As of the writing of this report, the rupture data available and/or currently running are given in
Table 3-4. Test specimen loading conditions were developed based on the rupture data gathered
from tests conducted in EPRI report 1004702 [6]. Loading conditions were developed as ruptures
occurred for the N&T weld test plate. The rupture data are plotted in Figure 3-1, which shows
the LMP versus the applied stress of the loading condition.
Table 3-4
Rupture Hours Data

Loading Condition Rupture Hrs. N&T Rupture Hrs. Subcritical

(ºF @ ksi (1900ºF/1400ºF, PWHT (1400ºF, 760ºC)
[ºC @ MPa]) 1038°C/760°C)

1050 @ 35.0 16.4 -

[566 @ 241]

1050 @ 30.0 169.7 324.6

[566 @ 207]

1050 @ 28.0 - 1583.8

[566 @ 193]

1050 @ 27.5 584.3 2684.7

[566 @ 190]

1100 @ 27.0 - 77.9

[593 @ 186]

1100 @ 25.0 103.3 -

[593 @ 172]

1100 @ 22.5 - 484.6

[593 @ 155]

1100 @ 22.0 - 732.6

[593 @ 152]

1100 @ 21.0 - 2387.0

[593 @ 145]

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Results

Table 3-4 (cont.)

Rupture Hours Data

Loading Condition Rupture Hrs. N&T Rupture Hrs. Subcritical

(ºF @ ksi (1900ºF/1400ºF, PWHT (1400ºF, 760ºC)
[ºC @ MPa]) 1038°C/760°C)

1100 @ 19.0 3476.1* -

[593 @ 131]

1150 @ 18.0 568.1 -

[621 @ 1214]

1150 @ 15.0 1581.8 609.7, 906.3

[621 @ 103]

1150 @ 12.5 3476.0* 2355.5

[621 @ 86.2]

* = Still in progress
Italicized = base metal failures

1 ksi = 6.89 MPa

Figure 3-1
LMP-Versus-Stress Results for N&T and PWHT Weldments (Base Metal Failures Removed)

It is apparent from the LMP-versus-stress rupture trend shown in Figure 3-1 that the N&T plate
begins to exceed the rupture strength of a subcritical PWHT weldment below approximately
20 ksi (138 MPa). From the trend it is estimated that the service life of a component welded with
a similar filler material as was employed in this evaluation and operating at 10 ksi (69 MPa) and
1000ºF (538ºC) would provide three times the life expectancy when it has been N&T over a

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Results

subcritical PWHT weldment. This is based on the limited number of data points conducted for
this examination and is not meant to serve as an absolute life expectancy for welded and N&T
Grade 91. Nevertheless, this may be an indication of how much remaining life a subcritical
heat-treated weldment may be losing when it fails in a Type IV fashion.

Failure Characterization

Because of the grain refinement that occurs during the normalization treatment, the typical HAZ
that is prevalent following welding is eliminated. Conducting accelerated rupture testing to
extrapolate long-term properties can sometimes mask what happens under actual operating
conditions and long-term service. Thermal and mechanical stresses can affect the microstructure
and rupture characteristics differently in various test regimes. It was discovered that
incorporating the results obtained from failures that occurred in the base metal of the subcritical
PWHT weldments altered the LMP trendline results. These failures occurred at high stress
loading conditions that are not applicable to the material in normal lower stress operating
regimes. Therefore, the tests that were determined to have failed in the base metal rather than in
the Type IV were eliminated from the trend analysis.

Post rupture evaluation of the tested samples revealed that all of the N&T composite rupture
sample failures occurred in the weld metal with the exception of one, which was at low stress
and long term. Failure for this sample occurred in the base metal and is shown in the 10X picture
of the stress rupture specimen (Figure 3-2). Two other tests, which are still running, may show
that under loading conditions that approach actual service conditions, N&T weldments provide
increased life over welds made with similar fillers employed in this investigation that exceed the
typical Type IV failures of subcritical PWHT weldments.

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Results

Figure 3-2
General Microstructure Associated with the N&T Treatment for the Base Metal and Weld
Metal Sides of the Composite Rupture Sample

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4
CONCLUSIONS

Subcritical PWHT Versus N&T of P91 Weldments

The following conclusions are given concerning the differences observed in performing a
subcritical PWHT versus an N&T treatment. The conclusions are provided to address the three
main industry questions presented at the end of Section 1, “Introduction.” The following
conclusions address the effect that N&T has on the residual hardness of the weld and base metal:
• The N&T heat treatment performed in this research produced hardness values slightly lower
in the HAZ/fusion zone locations compared to the subcritical PWHT:
– HAZ hardness after a 1400ºF (760ºC) PWHT averaged 97 RB as measured by
micro-hardness.
– Base metal hardness directly adjacent to the fusion zone for the N&T weldment
averaged 92 RB as measured by micro-hardness (readings were taken in the base
metal because there is no HAZ after an N&T heat treatment).
• Measurable differences in the hardness of weld metal resulted from the different heat
treatments:
– Weld metal hardness after a 1400ºF (760ºC) PWHT averaged 97 RB as measured
with the Rockwell instrument.
– Weld metal hardness of the N&T weldment averaged 93 RB as measured with the
Rockwell instrument.

Various mechanical tests were conducted to provide insight on how an N&T treatment affects
the mechanical properties of a Grade 91 material welded with B9 filler. The following
conclusions are offered not to be an all inclusive description of the mechanical behavior but
rather to give some idea of how the weldment responds to N&T:
• The N&T heat treatment produced rupture trends superior to that of a subcritical PWHT
weldment operating below 20 ksi (138 MPa)—approximately three times greater at 1000ºF
(538ºC) and 10 ksi (69 MPa) based on the small number of tests run in this program.
• The N&T rupture samples showed evidence that the failure location possibly changes over
from weld metal to base metal at longer test durations and lower stresses.
• The tensile strength and elongation of the N&T weldment are higher than the subcritical
PWHT weldments.
• The yield strengths are approximately equal for the N&T and PWHT weldments.

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Conclusions

• The N&T weld metal CVN impact strengths at room temperature are higher as compared to
the subcritical PWHT weldments.
• The HAZ (PWHT) and fusion zone (N&T) CVN impact strengths at room temperature are
approximately the same.
• Based on the tests run in this examination, all mechanical properties after an N&T heat
treatment were equal to or surpassed those following a 1400ºF (760ºC) subcritical heat
treatment.

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5
REFERENCES

1. Guideline for Welding P(T)91 Materials, EPRI, Palo Alto, CA: 2001. 1006590.

2. Metals Handbook Volume 2: Heat Treating Cleaning and Finishing, 8th Edition, ASM
International, Metals Park, Ohio. 1985.

3. The T91/P91 Book. Vallourec & Mannessmann Tubes, 1999.

4. M. Santella et al., “Martensite Transformation, Microsegregation, and Creep Strength of

9Cr-1Mo-V Steel Weld Metal,” EPRI Conference on 9Cr Materials Fabrication and Joining
Technologies, July 2001, Myrtle Beach, SC.

5. Effect of Cold-Work and Heat Treatment on the Elevated Temperature Rupture Properties of
Grade 91 Material, EPRI, Palo Alto, CA: 2003. 1004703.

6. Optimal Hardness of P91 Weldments, EPRI, Palo Alto, CA: 2003. 1004702.

5-1
Program:
Fossil Materials and Repair
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