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HOME-EXAM 3

What is residual stress? Give the definition, the causes and the different problems that can
be encountered. Are there any differences between thermosets and thermoplastics?

Residual stress is a stress is a stress that remains in a material and does not come from applied
load or thermal stress, that is to say it is free of external forces or temperature gradients. For
some cases it can be desirable but in the case of polymer composite manufacturing, it is
necessary to minimize this residual stress because it degrades the strength and in the worst cases
fails prematurely. Residual stress can be considered at four different scales: micro-scale, meso-
scale, macro-scale, and global scale. It can lead to various defects, and it exists several types of
measurements that can be destructive or not.
The number one cause of residual stress is that composites are very anisotropic materials, so
the properties are not the same in the different direction which results of an inhomogeneity. The
mechanical and the thermal properties are significantly different for the fibers and the matrix.
This is a parameter that is uncontrollable since it is what composite are. Then there are other
causes, the different lay-ups have an important impact, also the cure temperature: higher the
temperature cure is, higher the residual stress will be. Mold thermal expansion can also be a
cause since they have their own thermal expansion behavior. Void and fiber content, thermal
gradients, mold surface and cool down rate are also other factors. It is preferable to cool down
slowly to reduce the stress.
Residual stress mostly develops during the step of curing. After that, the composite
manufactured can have different defects or problems. For example, physical effects can be
observed: warpage, especially in thin parts, caused by lay-up and tool interaction, thermal
gradients, uneven heating or cool down rate and distortion, that occurs after curing. A certain
degree of distortion can be allowed. Moreover, if the stress is not allowed to go away, the stress
increases in the material (stress build-up) and this results in matrix microcracking and crack of
the fiber. These problems cause the degradation of mechanical properties and poses a problem
of change of dimensions. And it can also cause of course premature failure as said before. It can
be possible to compensate these phenomena during the design of the parts.
For thermosets, the main source of residual stress is due to the different coefficient of thermal
expansion and the cure shrinkage behavior of the resin and the fibers. However, for
thermoplastics, there is no curing. In this case, the effects are the same, but the shrinkage is not
due to curing but to crystallinity.

What are the measurements techniques for residual stresses? Give one detailed example of a
non-destructive method, and one for a destructive method.

It exists several different techniques in order to measure residual stresses in composites. It can
be noted that it is not possible to measure directly residual stress. Indeed, displacement of the
material or residual strain can be determined and then from that, residual strain can be found.
Sometimes, it can be challenging to determine residual stresses in composite due to the fact that
it can be self-equilibrated meaning that the tensile and the compressive forces are equal and
opposite. The methods can be destructive, non-destructive, invasive, and non-invasive and the
measurements can be done during the process or after. It is also possible to proceed to
verification and validation of the results obtained using predictive models. These methods give
quantitative information and maybe little qualitative.
For the destructive methods, here is a list of different measurements that can be used: first ply
failure, blind-hole drilling, successive grooving technique, layer removal, ring-core method,
slitting method…
The first ply failure method can be detailed. This method is used for cross ply laminate in order
to obtain the transverse residual stress. The aim of this method is to compare the transverse
tensile strength of a cross ply laminate with an embedded stressed ply and an unloaded
reference. The failure occurs when there is an initial crack growth in the matrix and when it
happens at the same strength during the test. Then, it is possible to determine the difference in
failure strengths and so the residual stress which is at the origin of this difference. Unfortunately,
this technique works only for macro-scale residual stress measurement.
For the non-destructive method, it can be used: photoelasticity, cure reference method, Raman
spectroscopy, electrical conductance, embedded methods, warpage analysis, interferometry…
Photoelasticity is a technique based on the relation between stress or strain and changes in
optical properties. It is based on light polarization (polarizing filters or polarized light sources).
This requires a translucent or transparent matrix and works better with semi-crystalline or
crystalline matrices. The two refractive indices of a birefringent material depend on the stress
of the material. So, it is possible with optical measurements, to determine the stress of a loaded
birefringent material. This technique is efficient to show debonding in carbon fiber epoxy
components. It also works well for the micro-scale residual stress. However, this technique is
not possible with cross-ply or woven fabric with high fiber density because there will be not
enough light passing through the sample.

What are the different methods to recycle CFRP?

Three different processes can be used to recycle CFRP and two of them are more interesting.
The first method is the mechanical method. It is based on crushing, shredding, grinding and/or
milling. The CFRP is reduced in particle size, fibrous fragments (rich in fibers) or powdered
CFRP (rich in resin) can be obtained. Then, these can be used in reinforced material for the
fibrous fragments and in filled material for powdered CFRP. The use of this fragment in new
material is however limited. Glass fiber-reinforced composites are more suitable for this
method. The advantage is this technique is that it does not require the use of hazardous materials
and does not product either. But this method is not the best option because the properties of the
material are largely lost, the architecture of the fiber are non-consistent, unstructured, and
coarse and there are not many possibilities to re-manufacture.
The second method is the thermal method. This method includes pyrolysis and fluid bed
process, that are the most used techniques. The principle of the processes is quite simple, the
CFRP is heated up and carbon fiber, resin cut down into pieces and hydrogen or carbon
monoxide are obtained. The temperature is increasing over 350 °C (up to 700°C) with an
absence of oxygen (N2 is often used). In this case, the fibers stay almost inert, and the matrix is
depolymerized. At the end, the matrix is in the form of an oil or a gas. The advantages of this
technique are the no use of chemicals, is it scalable so adaptable and the mechanical properties
are kept. Nevertheless, a deposition of char can occur on fiber surface, some gases are not
environmentally friendly, and the recycled fibers properties are processing dependent.
The last method is the chemical method called solvolysis. This is a technique using a solvent in
order to degrade the resin. The matrix will depolymerize into oligomers. Another important
parameter is that this degradation is done at elevated temperature. The solvent can be a classical
solvent, supercritical fluid (ethanol, acetone, water...) or an acid/base. Catalysts can be added
to have more efficiency and a faster dissolution rate. The advantages of this method are the
good conservation of the mechanical properties and a high potential for material-recovery from
resin. But there are also drawbacks with this technique, the first one is of course the use of
chemicals and a bad environmental impact, a lower adhesion to resins, and a limited scalability.

Explain the Darcy’s law.

This is a physical law that aims to express the flow of a fluid through a porous medium. It is
thanks to the hydraulic conductivity or the coefficient of permeability that the circulation of the
fluid between 2 points can be determined. It is in 1856 that Darcy established this law, after
several experiments, including the famous one of the flow of water through sand. Today this
law is very useful in hydrogeology and underground hydraulics.
Δ𝑝
This law can be expressed for the 1D- case as: 𝑄 = 𝐾𝐴 𝜇𝐿
With Q the filtering volume flow in m3.s-1, K the permeability in m2, A the cross-section area
in m2, p the difference of pressure in Pa, L the length of the sample in m and  the dynamic
viscosity in Pa.s.
Here is a scheme for a fiber:

This law operates under certain conditions or assumptions: the fluid must first be
incompressible (it is almost always the case in composite resin manufacturing) and Newtonian,
that is to say a fluid whose stress-strain rate law is linear. The regime must also be stationary.
Finally, the Reynolds number must be sufficiently low in order to neglect the inertia effects.
𝜌𝑉𝐿
For a unidirectional flow, the expression of the Reynolds number is the following: 𝑅𝑒 = 𝜂
Darcy’s law can be generalized for many different cases and the 3D equations can also be
𝐾
deduced with the permeability tensor which is: 𝑢̅ = − 𝜂 ∇𝑃