Neel Nadpara

MSE 4003
10/16/2016

Investigating the Quench Sensitivity of 2219 Aluminum

Transmission Electron Microscopy (TEM) Summary:

Sometimes it is necessary to resolve features that are too small to be resolved in light
microscopy. In these cases it is necessary to use transmission electron microscopy. Electron microscopes
produce images of samples at significantly greater magnification and resolution than light microscopes
are capable of. There are three key differences that allow TEM to produce images at higher
magnification and resolution than light microscopy. First, the beam is comprised of electrons rather than
0.61𝜆
light. If one considers the wavelength (𝜆) in the Rayleigh criterion (𝑅 = 𝑁𝐴
), the smaller the
wavelength the greater the resolution when one uses light the shortest wavelength of light (Violet) is
about 400nm while a electron’s wavelength is about 10,000 times shorter. Thus, while the resolution
limit for VLM is about 200nm, for TEM it is about 0.1 nm which allows much smaller features to be
resolved such as dislocations in a microstructure. Secondly, the lenses are electromagnetic or electro
static rather than simple or complex lenses. These magmatic lenses focus moving electrons from the
electron gun though a series of magnetic lenses onto the sample. Since the magnetic lens are essentially
electromagnets they can be controlled using power allowing for greater and more variable magnification
than with traditional lens (between 500X and 500,000X is possible in TEM). Third, the environment is
much more controlled in TEM over VLM since the system is under high vacuum which allows the
electrons to be focused without interruption by air molecules.

A TEM is comprised of four primary components: an electron gun, an image production system,
an image capturing system, and a vacuum system as can be seen in Figure 1. The electron gun produces
the electron beam by using either a thermionic gun which heats up a filament to cause electron
emission or a field-emission gun which employs a high electric field to eject electrons. In thermionic
guns there are two types of filaments used. One is a tungsten filament which is heated to 2700-3000K
and lasts for about 25 hours. The alternative is a LaB6 filament which is indirectly heated to 1850K which
lasts for over 500 hours but it requires a higher vacuum and gentler handing. In field-emission sources,
electrons are stimulated by an electrostatic field. The two main types of field-emission sources are
thermal field emission (which works at 1600K) and cold field emission (works at 300K). After the
electron beam is generated, it passes through a condenser system which subsequently focuses the
beam onto the sample. Additionally, there is an image production system that contains the objective
electromagnetic lenses, an indexing specimen fixture system, and intermediate as well as projector
lenses. The image production system guide electrons which pass through the thin (less than 100nm)
sample and form a highly magnified electron image. This electron image is processed into a visible image
by the image capturing system which contains a fluorescent viewing screen as well as a high quality
camera that allows digital images to be captured and reviewed. Additionally, since the beam consists of
electrons the system must be under high vacuum to prevent interactions between the electron beam
and air which would prevent the beam from generating images as the molecules within the air would
interfere with the electrons in the path. Also, there are three key apertures that an operator can control
the condenser aperture, the objective aperture, and the field-limiting aperture. The condenser aperture
defines angular convergence/divergence of the illumination which limits effects of aberrations at the
loss of intensity. The objective aperture defines the portion of the focal plane which contributes to
either a bright field or dark field image. There is also the field-limiting aperture that is used to determine
the area of the sample that will be used to form the diffraction pattern (used in SAD mode).

Figure 1: TEM Major Component Diagram

Moreover, it is important to note that TEM has three primary imaging modes which are mass-
density contrast, diffraction contrast, and phase contrast. Mass-density contrast is amplitude contrast in
bright field images due to differences in incoherent scattering from one location to another within a
sample (used in biological/strained samples). Diffraction contrast is amplitude contrast in bright field
and dark field images due to differences in coherent elastic scattering from one location to another
within a sample (used in crystalline/stained samples). Phase contrast is contrast in multi-beam images
due to differences in phases of the direct and Bragg diffracted beams (used for high resolution images
crystalline solids and nanostructures). Selected area diffraction is another technique that can be used in
TEM which provides a series of spots (each spot relates to a fulfilled diffraction condition of the sample’s
crystal structure, and if the sample is tilted different diffraction conditions will actuate and some spots
will lite up or be hidden). SAD allows one to find and examine crystal defects similar to what is done with
XRD, however in a much smaller scale. Kikuchi lines can also be found in SADPs , they are pairs of
parallel lines one bright and the other dark and arise due to elastic scattering of inelastically scattered
intensity in thicker TEM samples.

Lastly, sample preparation makes TEM a more difficult characterization technique as the sample
must be extremely thin at less than 100nm. For most samples there needs to be a pre-thinning stage
where the sample is cut to less than 1mm and a final thinning stage where the sample is cut down
further until it is less than 100nm. Pre-thinning can be completed by hand grinding or dimple grinding;
while finial thinning is carried out by electro-polishing (makes the sample into an anode and uses
current to dissolve it), ion milling (uses beams of ions to sputter atoms from the sample), or ultra-
microtomy (cut sample to thin size using a diamond blade).

Application to Analysis of 2219 Aluminum Alloy:

Often times one needs materials that provide a number of useful features such as 2219
aluminum alloy. 2219 aluminum alloy is a special alloy used in aerospace and defense applications sue
to its good weldability, machinability, specific strength, and corrosion resistance. In order to maximize
the mechanical properties of the alloy, three steps of solution treatment, quenching, and artificial aging
are employed. Quenching is the key step for ensuring good mechanical properties as inadequate
quenching leads to poor performance following aging (known as quench sensitivity). 2219 aluminum
alloy is known for its high quench sensitivity and it is unable to be strong if the quenching rate is lower
than the critical cooling rate. The quench sensitivity is typically assessed using the temperature-time-
property (TTP) curve and temperature-time-transformation (TTT) curve; however there is little data for
these curves for 2XXX series aluminum alloys. Thus, in this experiment, the time-temperature-
transformation (TTT) curve and time-temperature-property (TTP) curve of 2219 aluminum alloy were
computed by an interrupted quench technique.

The material used in the experiment was sectioned out of a large 2219 aluminum alloy forging.
Simples of specific dimensions were prepared and solution treated at 535°C for one hour then shifted to
a salt water bath and isothermally held at different temperatures from 280°C to 500°C for periods of
time. After this, they were quenched in cold water and artificially aged at 175°C for 18 hours. A
conductivity measurement was used to find the TTT curve while a hardness measurement was used to
find the TTP curve as seen in Figure 2 below.
 Figure 2: Left TTT curve, Right TTP Curve

While one can use these diagrams to determine quench sensitivity, one cannot quantify quench
sensitivity in terms of what actually happens within the microstructure without the use of TEM. Thus,
TEM was employed to probe into the precipitation behavior at the nose temperature. It can be seen in
Figure 3 that the Bright Field TEM image of the as solution threated samples shows that there is a fairly
pure matrix with a few rod shaped precipitates which are most likely copper since it is a 2XXX series
aluminum alloy.

Figure 3: As quenched sample TEM image

Figure 4: As quenched sample held at 440°C TEM image

In this sample it can be seen that holding the temperature at 440°C lead to more rod shaped theta
phase precipitates forming also leading to a loss of solutes and a loss of age hardening ability. From this
it was determined that the quench cooling rate for the alloy should be increased as high as possible to
achieve good mechanical properties. This would have been difficult to determine without the use of
TEM in order to see what actually occurred in terms of precipitates.

Citation:

Wang, H., Yi, Y., & Huang, S. (2016). Investigation of quench sensitivity of high strength 2219 aluminum
alloy by TTP and TTT diagrams. Journal of Alloys and Compounds, 690, 446-452. DOI:
http://dx.doi.org/10.1016/j.jallcom.2016.08.160