The Micro-FUEL CELL™ is a spherical particle composed of
layers of polymers (plastics) which are organic materials
and high energy fuels and oxygen sources (oxidizers) which
can be either organic or inorganic (salt-like) chemicals.
The only way to make an MFC™ is by "growing" it, layer by
layer, in a solvent, as shown in the diagram on the left,
Figure 1. But the MFC™ is composed of a variety of
chemicals, some of which are very similar, and others of
which are very different.
Conventional solvents strictly fall into two
classes, those (such as alcohol or paint thinner) in which
organic chemicals are very soluble, and those (such as
water) in which inorganic chemicals are very soluble. On
the other hand, each class of solvent is not very
specific. For instance, water will solubilize many
different inorganic chemicals simultaneously, but there is
no way to selectively choose one of these solubilized
chemicals, and specifically make that one chemical
insoluble, leaving all the rest in solution.
The MFC™ particle is made of both kinds of chemicals -
organic and inorganic - each of which are soluble in very
different kinds solvents. Furthermore, each layer of a
MFC™ may contain chemically similar chemical ingredients
to an underlying layer. Once a layer is formed on the
particle, the act of "growing" the next successive layer
cannot solubilize chemical components of the layer
previously "grown" on the particle. From the requirements
of manufacturing MFC™s, it is clear that conventional
solvents are not suitable, they are not
selective enough in what they solubilize. Yet an
MFC™ must be "grown" in a solvent or solvent system in the
manner illustrated in the above illustration.
One further limitation for using conventional
solvents in the manufacture of MFC™s is related to
their inability to make the ultra-thin (1 micron or less),
defect-free barrier layer which is required to separate
the high energy fuel layer in the MFC™ from the oxygen
source (oxidizer) core of the MFC™. This is due to the
inalterable fact that you cannot remove conventional
solvent from a conventional solvent deposited
layer without tearing the very thin layer apart, thereby
destroying the layer. Thus, conventional solvents
cannot be used to make "protective" defect-free layers
less than 15 microns in thickness - yet the MFC™
propellant particle needs a defect-free inner plastic
barrier layer only 1 micron thick!
SPS therefore needed a "new" process technology for
manufacture of the MFC™s, one that could be tuned to
"grow" layered particles with highly specific and tailored
chemical compositions for each layer. This new technology
must also be suitable for production of the ultra-thin,
defect-free plastic barrier layers required in the MFC™s.
This process technology is further suitable for
manufacture of large volumes of propellant at production
rates consistent with industry standards. The process
exhibits the ability to meet the exacting standards
required for production of MFC™s with consistent
performance in use as solid rocket propellants.
Matter commonly exists in any of three distinct states.
Matter can be in the form of a liquid, a solid, or a gas.
Supercritical fluids (SCF) are materials that exist in a
different state, a fourth state of matter. In this fourth,
supercritical, state, materials simultaneously take on the
properties of both a liquid and a gas. It is not one, nor
the other, but both - in a way it is similar to a dense
fog. (See illustration at right)
Both organic and inorganic materials are highly
soluble in supercritical fluids. However, in supercritical
fluids, a small change in temperature or pressure (the
process variables) can result in these solubilized
materials becoming instantaneously and totally insoluble.
This feature of SCF processing is illustrated in an
animation sequence in Figure 2.
Further, a supercritical solution containing many
different solubilized materials can be made to completely
desolubilize specific ingredients, or even combinations of
ingredients, by a small change in temperature or pressure.
This feature of SCF was discussed in figure 2, above. In
this illustration, three different materials are made
soluble in SCF, by changing pressure and temperature until
all three become soluble. All three components can
similarly be made insoluble, or two of the three can be
made insoluble, by similar changes in pressure and
temperature. This high degree of control of the solubility
of chemicals in SCF makes the 'growth' of multi-layered
MFC™s with specific layer compositions possible, without
damaging the underlying layers in any way.
Particle "growth" in SCF is also uniquely suited for the
production of MFC™s. With a slight change in pressure and
temperature, the solubilized material instantaneously
becomes totally insoluble. This rapid change in solubility
results in the formation of a uniform "fog" of super small
nanoparticles. Mutual attraction between the particles
results in the formation of centers where the
nanoparticles collect, forming larger particles. These
particles can be "grown" to any desired size by
controlling of amount of chemical originally solubilized
in the SCF. When the concentration of nanoparticles is
exhausted, the particle stops "growing".
Particle "growth" is extremely fast, and millions of
particles can be simultaneously "grown", all of which are
the same size, and made of the same materials.
Introduction of a second solubilized material under
conditions where the previously "grown" particles are
insoluble, followed by a change in conditions to a state
where the new material is made insoluble, allows formation
of a uniform layer of the new material on the previously
"grown" particle. This process is continued until the
multilayer MFC™ propellant particle is completely
formed.
In a similar manner, two or more different materials
can be "grown" into a particle and/or deposited as layers,
all without re-solubilizing any components of the
previously "grown" particle. Since the particles are
"grown" from a uniform fog of nanoparticles, the natural
shape of the MFC™ is spherical. This process is
demonstrated in the accompanying animation, Figure 3.
Since SCF solvents simultaneously possesses the
properties of a gas and a liquid, extremely thin layers of
material, such as those required for the ultra-thin inner
plastic barrier of the MFC™, can be deposited without
incorporating defects. This was discussed in Figure 2.

The perfection of these SCF processed barrier layers can
be seen in the electron micrograph immediately left
(Figure 4), and the atomic force micrograph immediately
below (Figure 5). The barrier coating is less than 1
micron (0.00004 inches) in thickness. Overview of the
whole particle in Figure 4 shows no visible defects,
while Figure 5, below, uses atomic force microscopy
(AFM) to highly magnify (zoom in on) an extremely minute
surface region of this coating. This magnification is so
great that individual pieces of the plastic barrier
molecules can be seen in the image. Only at this high
magnification can any surface variations be seen.
The right hand portion of the image below (Figure 5b,
with the x-axis labelled "Lateral Force") more clearly
shows the molecular fragments, while the left hand portion
of this image (titled "Topography") measures the variation
in surface height (unevenness) of the coating. We can see
from this image that the variation in surface height is
only about 17 nanometers, or about 2% of the thickness of
the 1 micron barrier layer.
Both these graphics clearly demonstrate the high
uniformity and defect-free nature of the layers formed
using SPS's "Fourth State of Matter"™ MFC™ production
process. Chemical analysis of this barrier layer, which is
composed of three different ingredients simultaneously
layered on the core particle, demonstrates that complex
multi-component defect-free layers of uniform thickness
can be "grown" on core particles to a precise thickness
using this innovative production technology.
The patent pending Supercritical Fluids based "Fourth
State of Matter"™ MFC™ Propellant Particle production
technology has been seen to possess all the required
features for successful, cost effective, manufacture of
SPS Corporation's patented MFC™ Solid Rocket Propellants,
and in high enough volume to meet all projected industry
demands for solid rocket propellants within the
foreseeable future.