Precipitation Hardening Related terms:
Aluminum Alloys,
Austenite, Heat Treatment,
Microstructure, Hardness,
Alloying Element
Precipitation hardening is a strengthening mechanism in alloys with special
characteristics (two phase or multiphase, in which the solubility limit is
increased with temperature) to form small particles in the range of ~100nm
which have three stages: solution treatment (ST), quenching, and aging.
From: Severe Plastic Deformation, 2018
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Precipitation Hardening
REE, Smallman, A.H.W. Ngan, in Modern Physical Metallurgy (Eighth Edition), 2014
13.4.1 The signif cance of particle deformability
The strength of an age hardening alloy is governed by the interaction of moving dislocations and precipitates. The
‘obstacles in precipitation hardening alloys which hinder the motion of dislocations may be either (i) the strains
around GP zones, (i) the zones or precipitates themselves, or both. Clearly, if itis the zones themselves which are
important, it will be necessary for the moving dislocations either to cut through them or go round them. Thus,
merely from elementary reasoning, it would appear that there are at least three causes of hardening, namely: (i)
coherency strain hardening, (i) chemical hardening, ie. when the dislocation cuts through the precipitate or (ii)
dispersion hardening, ie. when the dislocation goes round or over the precipitate.
The relative contributions will depend on the particular alloy system but, generally there is a critical dispersion at
which the strengthening is a maximum, as shown in Figure 13.7. In the small-particle regime the precipitates, or
particles, are coherent and deformable as the dislocations cut through them, while in the larger-particle regime
the particles are incoherent and non-deformable as the dislocations bypass them. For deformable particles, when
the dislocations pass through the particle, the intrinsic properties of the particle are of importance and alloy
strength varies only weakly with particle size. For non-deformable particles, when the dislocations bypass the
particles, the alloy strength is independent of the particle properties but is strongly dependent on particle size and
dispersion strength decreasing as particle size or dispersion increases. The transition from deformable to non-
deformable particle-controlled deformation is readily recognized by the change in microstructure, since the
‘laminar’ undisturbed dislocation f bw for the former contrasts with the turbulent plastic f bw for non-deformable
particles. The latter leads to the production of a high density of dislocation loops, dipoles and other debris which
results in a high rate of work hardening, This high rate of work hardening is a distinguishing feature of al
dispersion-hardened systems.Gaseous processes for low temperature surface hardening
of stainless steel
MAJ. Somers, T.L. Christiansen, in Thermochemical Surface Engineering of Steels, 2015
15.5.3 Precipitation hardening stainless steel
Precipitation hardening stainless steels are steels that are subjected to an annealing treatment in order to improve
‘mechanical properties (strength). The amount of bulk hardening depends on annealing timejtemperature (and
degree of deformation). The temperature/time applied for low temperature surface hardening can coincide with
the temperature/time for maximum bulk hardness which makes it possible to carry out simultaneous bulk
hardening and surface hardening in a single process step. The microstructures of nitrided Sandvik Nanof bx® and
carburised Uddeholm Corrax® are depicted in Figure 15.21 [38]. Nitriding of Nanof kx gives a layer thickness of
more than 20 um. The surface layer actually consists of two zones, nitrogen expanded austenite, Yy, and nitrogen
expanded martensite dy. The applied nitriding potential determines the phases formed; a high nitriding potential
favours the formation of Yj, while a low nitriding potential favours the formation of @'y. The formation of @’y is
likely to occur prior to the formation of Yw. At some threshold nitrogen content, the @'y transforms into Vw due to
the strong austenite stabilising ef ft of nitrogen. This nitrogen threshold value is only reached for high nitriding
potentials. A similar transformation mechanism prevails during carburising, which is clearly observed for
carburising of Corrax (Figure 15.21(b)). The bulk hardness of Nanof Ex yields a signif tant increase from an as-
delivered hardness of 400 HV to 684 HV after nitriding; this increase in bulk hardness is caused by the
simultaneously occurring precipitation hardening of the bulk during the nitriding treatment. The bulk hardness of
Corrax increases from the as-delivered hardness of 330 HV to 540 HV as a result of precipitation hardening
during carburising.
Examples of nitrided and nitrocarburised austenitic precipitation hardening stainless steel A286 (see Table 15.1)
are shown in Figure 15.22 [39]. The precipitation hardening temperature for this material is 720°C, which is
considered far beyond the temperature range for low temperature surface hardening. Indeed, simultaneous bulk
and surface hardening at 720°C resulted in development of CrN at grain boundaries, albeit modest [39].
Nevertheless, the presence of the strong nitride formers (as compared to Cr) Ti, Al and V, makes this 2 most
interesting material, as N atoms will be ‘bound’ preferably by the strong nitride forming elements rather than Cr.
Prolonged nitriding at temperatures as high as 500°C and low ammonia contents in the gas produced expanded
austenite zones without the presence of CrN.
It should be noted that low temperature surface hardening of stainless steels is a surface engineering treatment in
its infancy as compared to nitriding, nitrocarburising and carburising. For the latter treatments nitriding and
carburising steels were designed which have an optimal response towards the performance improvement that can
be achieved with thermochemical treatment. No such optimisation of the steel composition has so far been
initiated for stainless steels that are to be surface hardened. Rather, more or less standardised treatments are
applied to commercially available steels. It is anticipated that alloy development in parallel with further process
optimisation of low temperature surface hardening will pave the way for wider applicability of this promising
family of surface engineering treatments. For this purpose gaseous processes are preferred as they have the
largest exibility
[Poe bok |Strengthening of metal alloys
In Introduction to Aerospace Materials, 2012
4.4.5 Precipitation hardening
Precipitation hardening is a strengthening process involving the formation of hard precipitate particles in the host
alloy and these restrict dislocation slip. Precipitation-hardened alloys are used extensively in aircraft structures and
engines, and include aluminium, magnesium, titanium and nickel alloys as well as several types of steel.
Precipitation hardening is a remarkably ef €ctive strengthening process; for instance, the strength of aluminium
alloy can be increased from about 150 to over 500 MPa (or more than 300%).
Precipitation hardening is achieved by heat treating the metal alloy to form a di
impede the movement of dislocations. Heat treatment involves the following stages:
persion of f he precipitates that
1. Heating the metal at high temperature within the single-phase region to dissolve and disperse the alloying
‘elements in the matrix of the host metal. This stage is known as solution treatment.
2. Rapid cooling using a cool solution (e.g. water, oil) from the solution treatment temperature to obtain a
supersaturated solid solution of alloying elements in the host metal. This is known as quenching.
3. Reheating to an intermediate temperature to convert the supersaturated solid solution to finely dispersed
precipitate particles. This is called the age-hardening stage.
The heat-treatment temperatures depend on the composition of the metal alloy and the desired amount of
strengthening, For example, solution treatment of aluminium alloys used in aircraft is usually performed in the
range 450-500 °C, quenched and then age-hardened at 160-220 °C. Titanium alloys are solution treated at about
750 °C, quenched and aged at 450-650 °C.
Precipitation hardening is only possible when one or more of the alloying elements is completely soluble in the
host metal at elevated temperature (i.e. solution treatment) and their solubility decreases when the metal is
cooled. As the solubility falls with temperature, the host matrix rejects the excess of atoms of the alloying element
from the lattice sites. These atoms cluster into small precipitate particles that induce high lattice strains that resist
dislocation slip and thereby increase strength,
Precipitation hardening involves a complex series of physical transformations in the metal alloy at the atomic and
microstructural levels that induces dif Grent strengthening mechanisms over time. Figure 4.22 shows the
hardening mechanism with each successive transformation in the age-hardening process. The mechanisms
change with increasing age-hardening time in the order: solid-solution strengthening (SSS), Guinier-Preston (GP)
strengthening, coherent precipitate strengthening, and f nally incoherent precipitate strengthening.
Guinier—Preston zone strengthening
Precipitation hardening in the age-hardening stage of the heat-treatment process starts with the formation of
GuinierPreston (GP) zones. The formation of GP zones which occurs fistly by GP1 zones and then GP2 zones is
illustrated in Fig. 4.23. After solution treatment and quenching, the alloying elements are dissolved and dispersed
4 a supersaturated solid solution in the host metal. The material in this condition is relatively soft with
strengthening achieved by solid solution hardening. Upon age hardening the supersaturated solid solution
undergoes a transformation with the alloying atoms dif fising through the host lattice to form solute-rich clusters.
The driving force for this process is the concentration of the alloying elements in solid solution being higher than
their equilibrium solubility limit. Atomic dif fision and clustering of the alloying elements is assisted by vacancies
in the lattice. The dif Gision process is accelerated by heat treating the metal at elevated temperature; this is called
thermal age hardening, The process occurs at a slower rate at room temperature with some metal alloys, and thisis known as natural ageing.
The atoms of the alloying elements form a large number of tiny clusters (up to 10! per em®) that are 10-50 nm
long and only one or two atomic planes thick. These clusters are called GP zones. Figure 4.24 shows copper-rich
GP zones in an aluminium alloy used in aircraft structures. The solute-
ich GP zones are coherent with the crystal
structure of the host metal. In other words, the arrangement of alloying atoms in the GP zone and matrix phase
match at the interface plane and the two lattices are continuous across the interface. GP zones induce high strain
in the surrounding lattice thus impeding dislocation slip. Dislocations are able to shear through GP zones,
although the lattice strain imposes resistance against slip which strengthens the metal.
Coherent precipitate strengthening
The formation of coherent precipitate particles is the next step in the sequence of age-hardening processes. The
GP zones transform into coherent precipitates in the matrix phase. Coherent precipitates also form by
heterogenous nucleation at lattice defect sites such as grain boundaries and dislocations. A precipitate develops
when the concentration of alloying elements clustered within a small region gives the composition of another
phase. For example, copper in aluminium forms precipitate particles with a dif €rent composition (Al,Cu) to the
matrix phase. When precipitation fist occurs, the particles are coherent with the host lattice (Fig. 4.25). That is, the
lattice planes to the precipitate particles are continuous with the planes to the matrix, and there is no distinct
interface between the particles and matrix. An abrupt change in composition occurs across the precipitate-matrix
interface, but there is no change to the crystal structure. For instance, coherent Al;Cu precipitates have an fec
ceystal structure similar to the host aluminium metal
Coherent precipitates distort the surrounding matrix which resists dislocation slip. Once the dislocation has
‘overcome the lattice strain in the matrix and reached the precipitate, it can move through the particle because the
slip planes are coherent with the matrix. However, the particles resist the slip process, thus increasing strength.
‘The strength gained by coherent precipitates increases with time during the ageing process as their population
increases and they become larger.
Incoherent precipitate strengthening
The fal transformation in the age-hardening process is the formation of incoherent precipitate particles. These
particles are created by coherent precipitates changing their crystal structure such that the lattice planes are no
longer continuous with the planes of the host metal lattice. Incoherent precipitates are truly distinct second-phase
particles with their own crystal structure and separated from the surrounding matrix by 2 well-def ned interface
(Fig. 4.26)
Incoherent precipitates are ef €ctive obstacles against dislocation slip because the large distortion of the matrix
surrounding the particles interacts strongly with the stress f eld of the dislocations. The precipitates also obstruct
dislocation movement because slip cannot occur across the particle-matrix interface owing to the change in
ceystal structure. Strengthening by incoherent precipitates occurs by the Orowan hardening mechanism whereby
dislocations must bend and loop around the particles (Fig. 4.21). The combination of high lattice strain and
Orowan hardening results in incoherent precipitates being very ef €ctive in strengthening age-hardenable alloys.
‘The maximum improvement in strength gained by precipitation hardening occurs immediately upon the
coherent precipitates transforming into incoherent particles. During the ageing process the particle size increases
with a corresponding reduction in the particle spacing over time, as shown in Fig. 4.27. The spacing increases
because the precipitates grow via a process called particle coarsening. The precipitates are not all the same size at
any point during the ageing process; instead they occur over a range of sizes. Larger particles and particles located
at high energy lattice sites (e.g. grain boundaries) are thermodynamically more stable than small particles located
in the core of the grain. As ageing proceeds, the smaller, less stable particles dissolve and thereby release the
solute atoms back into the matrix. These atoms migrate through the lattice to the larger particles, thus expanding,
their size. As a result, the particles become larger but fewer in number and therefore more widely spaced.
Incoherent precipitates are more ef Ective than coherent particles at resisting dislocation slip because they createhigher lattice strains and promote Orowan hardening. Strengthening by Orowan hardening is most ef Gctive
when the particles are closely spaced; a high density of tightly packed incoherent particles being the best
condition to resist the bending and looping of dislocations. When the spacing increases, the particles are more
‘easily by-passed by moving dislocations, and therefore the strengthening ef €ct diminishes. For these reasons,
maximum strengthening occurs with closely spaced incoherent precipitates. The strengthening ef €ct diminishes
with prolonged ageing because the incoherent particles coarsen and thereby Orowan hardening becomes less
cf Ective. The age-hardenable alloys used in aircraft structures are usually heat-treated to close to maximum
strength. More information on the age hardening of aerospace alloys is provided in later chapters.
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Failure of 17-4PH stainless steel components in of shore
platforms
Sérgio S.M. Tavares, .. Juan M. Pardal, in Handbook of Materials Failure Analysis with Case Studies from the Oil
and Gas Industry, 2016
Abstract
Precipitation hardening is a strengthening mechanism very common in many classes of metallic materials, from
Aland Cu alloys to high-strength steels. In special, precipitation hardening (PH) stainless steels may allow
corrosion resistance and mechanical strength desired to special applications. Despite this, there are many cases of
failures involving PH stainless steels reported in the literature. Incorrect material selection or wrong heat
treatment procedures are usually associated to these cases of failure. This chapter is focused on three cases of
failure of 17-4 PH steel, a common precipitation hardenable martensitic stainless steel used in oil and gas
production and ref ning industries.
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Mj
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Microstructure control in creep-age forming of aluminium
panels
L. Zhan, ... D. Balint, in Microstructure Evolution in Metal Forming Processes, 2012
11.4.4 Finite element (FE) modelling of precipitation hardening
Precipitation hardening is a key feature of CAF. The evolution of precipitates af €cts not only the creepjstress
relaxation behaviour, but also the achievement of the material's Fnal strength. As discussed before, CAF is based
on a complicated combination of stress relaxation, creep and age hardening. Creep deformation takes place at lowstress levels, and the amount of plastic deformation is directly related to the ageing temperature and time. This is
signif eantly dif €rent from other metal forming processes, where elastic-plastic deformation of the material is
dominant. For industrial applications, numerical studies on springback and precipitation hardening in CAF need
to be available.
For the past 20 years, most of the fhite element (FE) methods for simulation or numerical calculation have taken
only macroscopic parameters, such as stress relaxation, creep strain, springback and so on, into consideration.
‘The research carried out has concentrated mainly on the prediction of springback in CAF processes using simple
creep or stress relaxation models. The coupling of ageing or precipitation hardening and creep or stress relaxation
has not been considered.
Stress-ageing and creep-ageing phenomena in aluminium alloys have been understood further in recent years,
and industry needs to be able to know and predict the mechanical-property distribution of creep-age-formed
aircraft wing parts. Thus Ho et al (2004) proposed a set of mechanism-based unif ed creep-ageing constitutive
equations for AA7010, which were implemented into ABAQUS through the user-def ned subroutine CREEP. In
addition to creep deformation and stress relaxation, the precipitate growth during ageing and the evolution of the
yield stress increment during CAF were predicted. Similar work has also been done by Zhan et al. (20116) for
AATOSS at 120°C, which will be discussed below.
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