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ICES-2020-40
Nanotechnology for Beyond Earth Water Treatment Tanya K.
Rogers1
Rice University, Houston, TX 77005
Pratiksha D. Dongare3, Alessandro Alabastri2 and Naomi J. Halas4
Rice University, Houston, TX 77005
Jordin Metz5, Jacques Mathieu6 and Pedro Alvarez7
Rice University, Houston, TX 77005
Layne Carter8 NASA Marshall Spaceflight Center, Huntsville, AL
35182
Michael S. Wong9 and Rafael Verduzco10
Rice University, Houston, TX 77005
NASA has embarked on a journey to enable human exploration on
the Moon by 2024 and Mars by 2030. These long duration missions
beyond low earth orbit (LEO) will require advanced water treatment
and reuse technologies for life support systems to support crew and
system needs. Resupply to deep space destinations is not desirable
and sustained human presence in a lunar environment increases the
necessity for robust and reliable systems. To reduce propulsion
costs and transit space allocations, mass, power, and volume must
be minimized for all systems. Additionally, a beyond LEO water
treatment system process must be able to tolerate both operational
and dormant periods. Herein, we present nanotechnologies developed
by the Nanotechnology-Enabled Water Treatment (NEWT) center as
advanced solutions to meet the aforementioned requirements. This
survey of fit-for-purpose modular technologies includes room
temperature nanocatalysis, nanophotonics, nano-selective scalant
control, quorum sensing, and nano-bacteriophages for biofilm
mitigation and mono-and multivalent ion control.
Ca2+ = Calcium CB = Carbon Black CSN = Calcium Selective
Nanocomposite HX = Heat Exchanger In-Pd/C = Indium on Palladium ISS
= International Space Station LED = Light Emitting Diode LEO = Low
Earth Orbit Na+ = Sodium NASA = National Aeronautics and Space
Administration
NESMD = Nanophotonics Solar Membrane Distillation NEWT =
Nanotechnology Enabled Water Treatment NH4+ = Ammonium NO3- =
Nitrate NP = Nanoparticle PNC = Phage-nanocomposite-conjugate PVDF
= polyvinylidene difluoride UV-C = Ultraviolet-C WRS = Water
Recovery System
1 PhD Candidate, Chemical and Biomolecular Engineering,
[email protected] 2 Research Assistant Professor, Electrical
Engineering, 6100 S. Main St, Houston, TX 3 Postdoctoral Research
Associate, Electrical and Computer Engineering, 6100 S. Main St,
Houston, TX 4 Professor, Electrical and Computer Engineering, 6100
S. Main St, Houston, TX 5 PhD Candidate, Chemistry Department, 6100
S. Main St, Houston, TX 6 Research Scientist, Civil and
Environmental Engineering, 6100 S. Main St, Houston, TX 7 Professor
and NEWT director, Civil and Environmental Engineering, Houston, TX
8 Space Station Water System Lead, NASA MSFC ES62 9 Department
Chair and Professor, Chemical and Biomolecular Engineering,
Houston, TX 10 Professor and Project Lead, Chemical and
Biomolecular Engineering, Houston, TX
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I. Nanotechnology for Water Management The
Nanotechnology-Enabled Water Treatment (NEWT) center is an
interdisciplinary, multi-institution
nanosystems-engineering research center and the first national
center to develop next-generation mobile, modular, high-performance
water treatment systems enabled by nanotechnology. NEWT’s goal is
to facilitate access to clean water by developing efficient water
treatment systems that can tap unconventional sources to provide
humanitarian water or emergency response. NEWT develops systems to
treat and reuse challenging wastewaters in remote locations,
focusing on sustainable and energy-efficient outcomes in regard to
its water footprint. Three research thrusts, each representing a
key component of the core systems, plus cross-cutting
sustainability and safety theme guide fundamental research and
development of novel water treatment processes and advanced
materials (Figure 1). Owing to the unique physiochemical and
surface properties of materials at the nanoscopic level,
nanotechnology-based approaches offer new solutions to terrestrial
and beyond earth water treatment.
Figure 1. Core focus groups for NEWT research and technology
advancement
II. Biofilm Mitigation The International Space Station (ISS) is
a hermetically closed environment inhabited by microorganisms.
Inevitably, microbes accumulate in the onboard Water Recovery
System (WRS), resulting in biofouling from bacteria growth/regrowth
that obstructs flow paths, reduces overall system performance,
limits functionality, and reduces system life and reliability. For
the past decade, biofilm growth in WRS system components has been
an ongoing issue. Heterotrophic biomass is consistently detected in
the stationary bowl of the distillation assembly, system plumbing,
and inlet valves. Biofouling at gas/liquid interfaces in the waste
hygiene unit and rotary water separator has restricted flow. The
accumulated release of biofilm from the water processor waste tank
has clogged downstream solenoid valves, resulting in the costly
replacement of the mostly liquid separator (MLS) and process pump.
Define on first use(NASA) has implemented multiple methods to
address these issues, including tank recycling, micron filters,
reduced organic content, and regular flushes with iodinated water,
but has declared biofouling as an ongoing critical challenge that
needs a more effective solution, especially for long-duration
planetary missions with anticipated dormant periods and limited
resupply flight windows1.
A multi-pronged treatment approach that prevents biofilm
formation without impacting system operation, destroys existing
films, and kills suspended cells while preventing regrowth is an
ideal solution. The principal determinants of bacterial rich
environments are temperature and humidity, presence of
disinfectants, and organic and inorganic constituents. Strategies
to effectively control biological environments should target these
factors and
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nanotechnology-based approaches offer opportunities to enhance
conventional technologies. Surface coatings and interruptions in
quorum sensing can limit biofilm attachment. Nanoparticles of a
variety of materials, from chitosan to silica, can kill existing
microbes. Bacteriophages can selectively destroy bacteria, and
coupled with nanoparticles, can penetrate a biofilm for bottom-up
eradication in a way that traditional chemical disinfectants often
cannot. Researchers at NEWT have developed many of these
technologies and have the experience and expertise to conduct
further testing in an applied system for space applications.
A. Nano-silica for Side Emitting UV-C Disinfection Ultraviolet-C
(UV-C) light emitting diodes (LEDs) are a disinfection tool that
uses short-wavelength UV-C
to kill or inactive microorganisms. A major technology barrier
of LED disinfection is the amount of irradiation emitted, limited
by LED surface area. As a result, reactors require a
disproportionate amount of LED arrays for effective disinfection
and produce high amounts (>85% of LED energy output) of
undesired heat. To overcome the surface area barrier, NEWT
researchers developed a nanotechnology-based solution to achieve
side-emission of UV-C in optical fibers, increasing the irradiation
area of LEDs by >100x (Figure 2). This is achieved by coating an
optical fiber with modified silica nanoparticles (NP) that create
light-scattering centers on the surface of the fiber. The coated
fiber is overlaid with transparent polymer and prevents
nanoparticle release into water and allows germicidal light to
permeate. A proof-of-concept investigation demonstrated 2.9 log
inactivation of Escherichia coli at a delivery dose of 15 mJ/cm2
using the silica-NP enhanced side-emitting fiber2.
Figure 2. Schematic diagram of side-emitting optical fibers
enhanced with scattering centers enabled by silica
nanoparticles
B. 200nm Bacteriophage as a Dormant Biocide Bacteriophages
(phages) are the most abundant biological entities in the biosphere
and exclusively prey on
bacteria. Average phage diameters range between 24 - 200 nm,
though some filamentous phages can exceed 800 nm in length. Phages
autonomously absorb to receptors on the cell surfaces of
susceptible bacteria and infect the host cells by injecting their
genomes through the cell membrane. While most characterized phages
are considered species or strain-specific, recent efforts have
demonstrated the widespread existence of broad host-range
(polyvalent) phages that can infect multiple bacterial species.
NEWT has developed broad-spectrum polyvalent
phage-nanocomposite-conjugates (PNCs) to target multiple bacterial
species in biofilms using bottom-up eradication3. For this method,
magnetic iron oxide nanoparticles were coated with chitosan and
treated to bind phages to the nanoparticle surface. A weak magnetic
field was applied to the PNCs, which facilitated biofilm
penetration and subsequent phage proliferation and propagation
within the biofilm. The biofilm removal efficiency was 98.3 ± 1.4%
for dual species biofilm (i.e., Escherichia coli and Pseudomonas
aeruginosa) and 92.2 ± 3.1% for multi-species biofilm (i.e., E.
coli, P. aeruginosa, and non-hosts Bacillus subtilis and Shewanella
oneidensi) (Figure 3).
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Figure 3. Simulation and experimental results of biofilm removal
following treatment by free phages and different sized PNCs. The
dual species biofilm before treatment (A) and after treatments with
(B) free phages, (C) large PNCs, (D) medium PNCs, and (E) small
PNCs for 6 hours. The left panels are simulated cross-section of
dual species biofilm of E. coli (red cell) and P. aeruginosa (green
cell). The blue cells represent phage-infected bacteria that have
not lysed yet. Each grid represents 0.5 × 0.5 μm. The right panels
are microscopic images of the surface of residual biofilms stained
with SYTO 9.
The use of bacteriophages over common chemical disinfectants and
biocides offers several advantages. While chemicals cannot easily
penetrate and eradicate biofilms, some phages possess depolymerases
which enhance biofilm penetration and degradation. Phage
populations can also evolve to circumvent the development of
resistance within bacterial populations. Furthermore, phages are
innocuous to human health and do not require downstream removal
unlike traditional chemical disinfectants. Additionally, unlike
antibiotics or biocides, whose concentration decreases with time
after repeated dosage, phages may continue to self-replicate and
infect the target bacteria, eventually disappearing with their
hosts in a typical predator−prey relationship. Moreover, a diverse
library of phages can be maintained with minimal weight and space
requirements. These factors, and bacteriophages ability to be
stored in ambient conditions for extended periods of time, make
phages an ideal technology for on-line and dormant water systems
during long-duration missions.
C. Porous Nanocarriers to disrupt quorum sensing Quorum sensing
is a cell-to-cell communication mechanism that functions through
chemical signaling and
regulates gene expression in response to bacterial population
densities. It plays a major role in biofilm formation, influencing
each step in the process from establishment to maturity. Disruption
of bacterial quorum sensing has shown promise for controlling
biofilms. If cell-to-cell signaling can be interfered with, biofilm
formation may be delayed, or the biofilm may not be as robust and
therefore more susceptible to removal by various treatments. We
have identified divalent metal quorum sensing inhibitors (nickel
and cadmium) and demonstrated cell signaling disruption through a
porous nanocarriers delivery method4 (Figure 4).
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Figure 4. biofilm attachment (B) of Burkholderia multivorans
17616 in the presence of nickel, measured by absorbance at 24 h.
Each bar represents the average of five experiments with a minimum
of four replicates per experiment
III. Mono-and Multivalent Ion and Nutrient Control
D. Capacitive Deionization for Selective Removal of Scalant Ions
NEWT has developed a chemical-free, membrane-free, and regenerable
technology to remove inorganic
constituents prone to cause scaling from wastewater streams.
This technology, known as capacitive deionization, is electrically
driven by a low energy applied voltage. An electric potential (~1.0
V) is supplied to an anode and cathode resulting in charged species
adsorbing onto the electrode surfaces. Once the electrodes reach
saturation, a reverse potential or zero charge state is applied and
the ions desorb resulting in a regenerated surface. Selective
removal of targeted ions can be achieved by altering the electrode
surfaces with unique nanomaterials (Figure 5). In order to achieve
calcium selective removal, we developed a calcium-selective
nanocomposite coating (CSN) of nano-sized calcium chelating resins
with aminophosphonic groups in a sulfonated polyvinyl alcohol
hydrogel matrix, which accomplished a Ca2+-over-Na+ selectivity of
3.5–5.4 at Na+:Ca2+ equivalent concentration ratio from 10:1 to
1:1, 94 – 184% greater than the uncoated electrode. The CSN coated
electrode exhibited complete reversibility in repeated
operation5.
Figure 5. Schematic Diagram of Capacitive Deionization
continuous-flow reactor with calcium-selective nanocomposite
electrode
E. Ambient Temperature Nanocatalysis for Selective Conversion of
Nitrogen Containing Species to Desired products
Urine waste streams are rich with nitrogen containing species
such as urea (13,400 mg/L) and ammonium nitrate (756 mg/L),
contributing to pH shifts resulting in divalent ion precipitation
and hydrolysis to toxic NH4+/NH3. NEWT has developed a method to
selectively transform N-species to innocuous dinitrogen using novel
“designer”
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bimetallic nanocatalysts (5-7 nm). Tunable atomic configuration,
metal-on-metal loading, and metal nanoparticle size are customized
to influence the catalytic performance and reaction pathway. We
have demonstrated that surface-tuned deposited Pd nanoparticles
with indium deposits (“In-on-Pd NPs”) shows room-temperature
nitrate catalytic reduction towards dinitrogen gas.
Mechanistically, In-on-Pd bimetallic catalysts first oxidizes
indium(spell out) in order to reduce NO3− to NO2−. Next, a series
of surface reactions occur with hydrogen adatoms to further reduce
the nitrite that has surface diffused to neighboring Pd sites.
Selectivity in excess of 95% to nontoxic N2 was observed6 (Figure
6).
Figure 6. Concentration−time curves of NO3−, NO 2 −, NH 4+, and
N2. Reaction conditions: 40 sc% In-on-Pd NPs with 0.553 mg/L In in
reactor, 600 rpm stirring rate, 1 atm pressure, ambient
temperature
F. Nanophotonics for Distillation Driven by Localized Heating
Nanophotonics regards the interaction of light with nanostructures.
The use of nanophotonics for solar energy
driven vapor generation was initially demonstrated by Neumann
et.al.7 at Rice University and has since been implemented by
various research groups around the world. Researchers have
demonstrated the use of different nanoparticles, such as
carbon-based materials, metallic nanoparticles, semiconductor
nanoparticles to achieve broadband maximum light absorption from
incident sunlight by tuning their material and shape8-22. Hogan
et.al.18 demonstrated that depending on nanoparticle scattering and
absorption cross sections, incident light interacts differently
with the nanoparticle solution and as the nanoparticle
concentration increases, light gets absorbed and scattered closer
to the illumination surface as shown in Figure 7a. As a result, for
an optimal concentration, nanoparticle temperature increase can
efficiently convert water to vapor at the liquid/air interface
without increasing the bulk water temperature. Based on this light
absorption localization phenomenon, NEWT researchers developed a
nanophotonics-enabled solar membrane distillation (NESMD) system19,
employing light absorbing carbon black (CB) nanoparticles coupled
with a relatively thin ~100 microns polyvinylidene difluoride
(PVDF) hydrophobic membrane. In NESMD, saline and purified water at
ambient temperature flow on opposite sides of this photothermal
membrane (Figure 7b.). The incident sunlight is absorbed on the
nanoparticle-coated surface, generating a temperature and vapor
pressure gradient across the membrane. The vapor pressure
difference results in water vapor flowing from the feed side
through the membrane to the distillate side, where it condenses
(Figure 7c.). Salts and other pollutants are left behind at the
input side of the membrane. This is a highly efficient process
because only the few-microns-thick volume of water at the
photothermal membrane surface is heated by the sun, leading to an
effective layer-by-layer vaporization process. The solar-driven
localized heating in NESMD maintains a positive temperature
difference across the membrane even for larger modules and makes it
a highly scalable process
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Figure 7. Light localization in nanoparticles enables surface
heat generation. (a) Modifying light absorbing nanoparticle
concentration allows heat localization at liquid/air interface. (b)
Schematic of nanophotonics-enabled solar membrane distillation
(NESMD), where saline feed and purified distillate flow on two
sides of a nanoparticles coated hydrophobic membrane. (c) Incident
sunlight gets absorbed in few microns thick nanoparticle layer on
top of the membrane and the resultant heat creates a temperature
gradient across the membrane. This temperature difference creates a
vapor pressure gradient, pushing water vapor from feed to
distillate through the membrane, leaving salts behind and thus
purifying water.
After a successful proof-of-concept NESMD demonstration with a
lab scale system operating at ~20% efficiency19 and > 99% salt
rejection, NEWT research efforts have been directed towards scaling
up the system and increasing its performance. To facilitate NESMD
scale-up, we have developed a spray-based method which can coat
membranes of any size. One way to increase the efficiency of a
solar driven distillation process is to use solar concentrators to
illuminate the device with higher solar power. However, solar
concentrators are bulky, costly and need extensive tracking
infrastructure, limiting the system design flexibility and
applicability. The water evaporation efficiency increases with
solar power because the water vapor pressure is an exponential
function of temperature and the temperature is a nearly linear
function of the incident solar intensity. With this understanding,
we modified the illuminated surface of the light absorbing membrane
with lens arrays to create high intensity hot-spots (Figure
8a,b)20. While the input solar power in the system is unchanged,
its spatial distribution is now related to the lenses focusing
properties. Due to the exponential dependence of flux on intensity,
the increase in flux at the high intensity focal spots exceeds the
reduction in flux in the rest of the device, resulting in a higher
average flux. Purified water flux from a 4 inch × 8 inch module
with 1 inch and 2 inch diameter lens arrays resulted in
enhancements of ~38% and ~58% respectively. The corresponding water
flux enhancements for a 4 inch × 16 inch module were ~22% and ~30%
respectively. Over a period of 9 hours, adding 2 inch diameter lens
array to a 4 inch × 16 inch module casting 5 mm focusing spots
resulted in 27% water production increase from the same solar power
input, without using any bulky light concentrators (Figure 8c).
This performance improvement was comparable to enhancements in
other solar driven distillation systems obtained with solar
concentration. This strategy can be applied to increase performance
of other photothermal processes with supralinear light dependence
like phase separations16 and chemical reactions.
Evaporation based thermal distillation processes like NESMD are
essential to treat high-salinity water, but the extraction and
collection of vapor occurs through an energy intensive phase change
process and has intrinsically low thermodynamic efficiency20. Thus,
recovering the heat utilized for vaporization represents an obvious
path towards highly efficient thermal desalination systems. To
achieve that, we combined NESMD system with a heat exchanger (HX)
system to effectively recover vaporization energy from the
condensed vapor to preheat the feed before entering the NESMD
system (Figure 8. c,d)21. After rigorous experiments and
theoretical calculations, we found that a NESMD+HX coupled system
can act as a thermal oscillator, where evaporation-condensation and
recovered latent heat can be maximized by dynamically matching feed
and distillate flow rates. Additionally, it was found that, through
real time modification of matched flow rates (i.e. dynamic flow
control, DFC), the production rate could be furtherly optimized
depending on light intensity, system size and losses. Through flow
rates optimization, the thermal energy in the system is
recirculated multiple times, oscillating between NESMD and HX
regions. Following these thermal recovery strategies, we obtained a
thermal efficiency of ~150% with a fresh water flux of ~1.1
L/(m2.h) under 0.475 Suns utilizing LED light sources. We
numerically predicted water production of 20.5 L/m2 for an
optimized system operating under varying ambient solar illumination
during a typical sunny day in Alamogordo, NM. These advancements
point towards nanophotonics-enabled desalination as a promising
technology for space applications. In fact, NESMD is driven by
vapor pressure gradients as opposed to gravity driven convective
flow based conventional distillation processes, making it a
potential solution for water treatment in space missions.
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Figure 8. Schematics and mechanism of NESMD with multilens array
and NESMD with heat exchanger. (a) Saline feed and purified water
flow on top and bottom respectively of a carbon black coated PVDF
membrane in countercurrent flow. The carbon black nanoparticles
absorb incident solar radiation and lead to heat localization on
top of the membrane. The heated feed evaporates on top of the
membrane and condenses on the bottom in the purified water leaving
salts and pollutants behind. Modification of the top surface of
NESMD with multilens array leads to focusing incident sunlight in
smaller regions with higher feed temperature rise (b) which lead to
higher water vapor flux in smaller regions and overall improved
performance. (c) Calculated flux production from 4 in. × 16 in.
NESMD with 2-in.-diameter lens array with 5-mm focal spots (orange
area) and bare NESMD (dark-gray area) under varying solar intensity
(dashed blue line) for more than 9 h. (d) Heat exchanger (HX)
coupled to NESMD allows to transfer heat from the exiting purified
water to the incoming saline feed. (e) As the water vapor condenses
in the purified input distillate it transfers its energy of
condensation in the distillate making the distillate output warmer
than input. This heat can be transferred to the input saline feed
before entering NESMD with an HX with metallic layer (Copper or
Aluminum) in between the top and bottom water stream. (f)
Comparison of flux production from NESMD with 10 HX layers during a
9 hour day with (orange) and without (grey) dynamic flow control
(right axis). Solar intensity variation in blue (right axis).
IV. Conclusions This survey paper highlighted nanotechnologies
for water treatment applications in beyond earth systems.
We have described groundbreaking research efforts that enable
high-surface area UV-C disinfection, dormant treatment of bacterium
using autonomous nanophages, bottom-up eradication of biofilms and
cell-to-cell signaling disruption through porous nanocarrier
delivered quorum sensing inhibitors, selective removal of calcium
scalant using nanocomposite layered capacitive deionization, room
temperature nanocatalysis of nitrogen containing species to
innocuous products, and nanophotonics for distillation driven by
localized heating. Future work will further evaluate implementation
considerations for beyond earth water systems.
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Acknowledgements The authors of this work wish to acknowledgment
the many professors and graduate students that have
contributed to this overall effort. This work was partially
funded by the National Science Foundation (EEC-1449500) Nanosystems
Engineering Research Center on Nanotechnology-Enabled Water
Treatment.
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