Details of the proposal
Scientific Case/ background (Give a brief description of scientific study)
The severity of oil spills has posed significant challenges to environmental protection and marine
ecosystems, necessitating the development of efficient methods for oil-water separation.
Superhydrophobic materials, which exhibit a high-water contact angle have gained considerable attention
for their potential in addressing this issue, and can effectively separate oil from water due to their ability
to repel water while selectively adsorbing oil, making them ideal candidates for use in oil spill
remediation.
In this study, we focus on the development of a superhydrophobic sponge material designed for enhanced
oil-water separation by modifying the surface of a hydrophilic sponge substrate with a hydrophobic
hydrocarbon-based material. The resulting surface exhibits properties that are favorable for oil adsorption
while maintaining resistance to water, allowing for selective oil absorption from water.
Present objective (Give objective of present experiments using Indus beamline)
To characterize the surface chemistry and composition of the coated material, we employ X-ray
Photoelectron Spectroscopy (XPS), a powerful surface analysis technique. XPS will provide valuable
insights into the chemical bonding and elemental composition of the surface, helping to confirm the
success of the superhydrophobic coating and assess its stability and durability in real-world applications.
Experimental plan/requirements (e.g. Mode of experiments)
Cutting and mounting of sample onto the conductive stub, avoiding contamination. As the sponge is
highly porous, measurements need to be taken at different depths or different areas to get a representative
sample.
Radiation source: Al Kα (1486.6 eV) or Mg Kα (1253.6 eV) as the X-ray source. Al Kα is commonly
used for organic materials and provides better sensitivity for surface analysis.
Energy Resolution: Resolution of 0.5 eV for high-quality core-level peaks, particularly for elements such
as C, O, and S, which are important for your superhydrophobic surface analysis. 50–100 eV of energy to
pass the sample is typically good for a balance between resolution and acquisition time.
Scan Mode: Wide-range survey scan (binding energy range: 0–1200 eV) to determine the overall
elemental composition of the surface. Performing high-resolution scans for specific elements (C1s, O1s,
N1s, S2p) to study the chemical states in detail.
Angle of Detection: Low take-off angle (15–45°) to improve surface sensitivity of sponge.
Sample Charge Compensation to prevent charging effects as sample is non-conductive. Depth profiling
for analyzing the depth of the coating or any interactions between the hydrocarbon and the sponge
surface.
Safety Considerations (if any) (Such as use of hazardous gases, radioactive material etc)
No such safety considerations, however, proper precautions to be taken when handling the sample to
avoid surface contamination. Clean handling would ensure the sample is free from fingerprints, oils, and
other extraneous material. Also, since the material is non-conductive, maintaining a stable charge
compensation system is critical for accurate measurements.
Local Support Requested (Accommodation, Travel etc. ) Yes
Expected Outcome of the Proposed Experiments
The expected outcome of your XPS experiment is to gain detailed insights into the surface chemistry of
the superhydrophobic sponge. The XPS data will provide the elemental composition of the surface
(predominantly carbon with minor oxygen depending on the coating), the chemical states of the elements
(especially carbon), helping to understand the nature of the coating and any functional groups present, an
understanding of the surface modifications and the effectiveness of the hydrophobic coating in providing
the desired oil-water separation properties.
By comparing the XPS results with the desired characteristics of a superhydrophobic surface, we will be
able to assess how well the hydrocarbon coating has been applied and whether it is suitable for oil spill
remediation applications.
References (if any)
Dashairya, Love, M. Gopinath, and Partha Saha. "Synergistic effect of Zr/Cl dual-ions mediated pyrrole
polymerization and development of superhydrophobic melamine sponges for oil/water separation."
Colloids and Surfaces A: Physicochemical and Engineering Aspects 599 (2020): 124877.
Lei, Zhiwen, et al. "Surface modification of melamine sponges for pH-responsive oil absorption and
desorption." Applied Surface Science 416 (2017): 798-804.
Niu, Haifeng & Qiang, Zhe & Ren, Jie. (2021). Durable, magnetic-responsive melamine sponge
composite for high efficiency, in-situ oil-water separation. Nanotechnology. 32.
10.1088/1361-6528/abef2e.
Zhao, Y.; Zhang, Y.; Li, R.; Wang, Z.; Lou, Z.; Li, Y. Facile Synthesis of Ultralight and Porous
Melamine-Formaldehyde (MF) Resin-Derived Magnetic Graphite-Like C3N4/Carbon Foam with
Electromagnetic Wave Absorption Behavior. Crystals 2020, 10, 656.
https://doi.org/10.3390/cryst10080656.
Deryło-Marczewska, J. Goworek, S. Pikus, E. Kobylas, and W. Zgrajka. Characterization of
Melamine−Formaldehyde Resins by XPS, SAXS, and Sorption Techniques. Langmuir 2002 18 (20),
7538-7543. DOI: 10.1021/la0202172
Zhang, Ying, et al. "A superhydrophobic and elastic melamine sponge for oil/water separation." New
Journal of Chemistry 43.16 (2019): 6343-6349.
UNDERTAKING
I hereby ___________________________________(Principal Investigator) undertake followings:
(1) The principal investigator/s will submit an experimental report to concerned beamline scientist/in-
charge within three months of the utilization of his/her beamtime.
(2) The principal investigator/s will inform the concerned beamline scientist/in-charge about any
publications/ reports based on the data taken using Indus synchrotron beamlines.
(3) Proper acknowledgement will be given for the RRCAT, Indore as an institute for extending its
facilities, concerned beamline scientist/s or any other RRCAT staff members for their involvement/
help extended during the experiment (if any).
(4) We accept the RRCAT Disclaimer that “ALL EFFORTS ARE MADE AT THE INDUS
BEAMLINES TO PROVIDE THE MOST ACCURATE DATA TO ITS USERS. HOWEVER,
INDUS BEAMLINES ARE NOT CERTIFYING AGENCIES, AND HENCE NO
BLAME/LIABILITY CAN EITHER BE ATTACHED OR NO LEGAL RECOURSE CAN BE
TAKEN IN THE EVENT OF ANY CONTROVERSY."
(5) Funding declaration:
This research received no specific grant from any funding agency in the public, commercial,
or not-for-profit sectors.
The proposed research work is supported by __________________________________
Date:___________ Signature:___________________
Place:_______________ (Principal Investigator)
