Normalization and Temper Heat Treatment

on P91
INTRODUCTION
Grade 91 (9Cr-1Mo-V, referred to in this document as P91 for pipe and T91 for tubing) has
seen use in replacement headers and tubing during the last few 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.
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.
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.
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 810C. Weld metal AC1is generally lower than base
metal because it has higher nickel to develop toughness in the weld. Most filler metal
produced by various manufacturers has an AC1 above 780C. However, weld metal may have
an AC1 as low as 760C.
PWHT between 704 and 760C is required by the American Society of Mechanical Engineers
(ASME) Section B31.1. ASME Section requires PWHT of Grade 91 to be carried out at a
minimum of 704C. 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 normalizing treatment, Additions of alloying elements such as Cr, Ni, and Mo
can shift the various phase boundaries. For the sake of simplicity, look at the iron-iron
carbide phase diagram for steels given in Figure 1.

Figure 1 Iron-Iron Carbide Phase Diagram

Normalization
Critical temperatures (AC1, AC3, and ACM) are the temperatures where a material undergoes
a phase change. As steels are heated, they encounter their first critical temperature at
approximately 732C, 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 fieldthat 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 38C above the upper critical 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 2. Martensite is formed during nonequilibrium 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. The Ms
is around 200C and the Mf could be at room temperature or lower. 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.

Figure 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.
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 56C
above the AC3 temperature and for the material in this project was performed at 1038C. 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 788C.
Manufacturing Practices Requiring N&T
Manufacturing practices require a normalization heat treatment to restore properties 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
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 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.

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.
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 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, 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.
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
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 . It is unknown whether these subtle changes
have an effect on the properties of the weld metal after N&T heat treatment.