Palladium Nanoparticles and Bimetal Palladium Layers for Enhanced Hydrogenation Properties by Manika Khanuja Depa 比ment of Physics Submitted in fulfillment of the requirement of the Doctor of Philosophy to the INDIAN INSTITUTE OF TECHNOLOGY DELHI NEW DELHI-110016, INDIA February 2009
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Palladium Nanoparticles and Bimetal Palladium Layers for Enhanced
Hydrogenation Properties
by
Manika Khanuja Depa比ment of Physics
Submitted
in fulfillment of the requirement of the Doctor of Philosophy to the
INDIAN INSTITUTE OF TECHNOLOGY DELHI NEW DELHI-110016, INDIA
February 2009
I would like to dedicate my thesis to
Sameer, myfamily and my in-laws
Certifficate
We approve that the thesis of M面ka 助如可a entitled "Palladium Nanoparticles
and B血etal Palladium L習ers for Enhanced Hydrogenation Prope市es" is
worthy of consideration for the award of the degree of Doctor of Philosop畑加d is a
record of original and bonaffide research work carried out by her under our
supervision. OEe results contained in it have not been submitted in part or full to any
other university or institute for awards of any degree/diploma.
Date: c ・え・ユ。。へ
Prof. B. R Mehta
OEmn Film Laboratory
Department of P取sics
Indian Institute of Technology Delhi
New Delhi-i 10016
India
Prof. S. M. Shivaprasad
Chemistry&Physics of Materials Unit (CPMU),
Jawaharlal Nehru Centre for Advance Scientiffic
Research (JNCASR), Jakkur-P.O.
Bangalore-560064
India
Acknowledgement This research started in November 2003 and this thesis is the result of ffive years of
work whereby I have been accompanied and supported by many people. It is a
pleasant aspect that I have now the opportunity to express my gratitude for all of
them.
Prof B. R. Mehta, my supervisor. I would like to express my gratitude for
his continuous support. His enthusiastic and integral view on research and his
mission for undertaking 'only high-quality work and not less', has made a deep
impression on me. I owe him lots of gratitude for initiating me into this fleld of
化se町ch.
Prof. S. M. Shiv叩rasad, my supervisor for being supportive and encouraging in
my research work. His valuable inputs always helped me, both in XPS analysis
and paper publication. His wisdom, knowledge and commitment always inspired
and motivated me.
Dr F. E. Kruis, Institute for Nano Structures Technique 但ST), University of
Duisburg-Essen, Duisburg Campus, Germany, for inviting me at Duisburg
University as a Guest Scientist and supporting me to cany out part of my research
work at Germany.
Dr. D. K. Awasthi, Senior Scientist, Inter-University Accelerator Center (IUAC),
New Delhi, India and Mr. P. K. Kulriya for fruitful collaboration in carrying out
experiments related to in-situ X-ray diffraction measurements
CSIR (Council of Scientiffic and Industrial Research) India for their ffinancial
support in the form of "Junior Research Fellowship" and "Senior Research
Fellowship".
'''
. Dr. Deepak Varandani and Dr. I. Aruna for their continuous guidance, support and
motivation during my experimental and thesis work.
. Dr. V. N. Singh for providing support by carrying out TEM&HRTEM
measurements.
. Special thanks to Shubhra Kala for her support in Synthesis of Size selected
nanoparticles.
. Pragya Agar, Dr. Vandana, Mandeep Singh, Himani Shanna, Rupali Nagar and
Mukesh for being supportive d面ng my research work and thesis writing.
・ K. Gopinathan, Kanwal Preet Bhatti, Mandeep Singh, Sangeeta Handuja, and
Cham Dube for lending their support during XRD analysis. Mr. Vinod Khanna for
TEM measurements.
National Physical Laboratory 国PL) for providing me inifiastructure where I have
done XPS studies and Dr. Govind, Dr. Amish Joshi, Dr. Mahesh Kum叫 Dr.
Him面 Sharma, Praveen, Manoj and Jithesh for backing me up in numerous
ways.
Mr. Balraj Khatri, Mr. Nagendra Chaudhary and members ofIDDC, lIT Delhi, for
providing technical help during modiffication ofthe experimental set up.
. My school and college teachers Ms. Poonam Tandon, Ms. U. Chugh and Dr.斑ta
Chandra for providing me their valuable guidance and motivation to pursue higher
studies.
Dr. Sujeet chaudhary for allowing me to use conductivity measurement set up.
Suchitra, Sudesh and K. Gopinathan for helping me carrying out these
measuremenis.
I would like to appreciate support provided 句 my lab-mates Suneet Arora,
1.1 Palladium .............................................................................................................................. i
i.2 Hydrogen .............................................................................................................................. i i .3 Palladium-Hydrogen ..................。. ......................................................................................... 2
Chapter 5. StructuraI Properties of Palladium Nanoparticle Layers and Thin Films ....... 83 5.1 Introduction ......................................................................................................................... 83 5.2 Hydrogenation of Pd Thin Film and Nanoparticle Layers...................................................83 5.3 Effect of Temperature ...........,............................................................................................. 86 5.4 Effect of Hydrogen Partial Pressure (PH)............................................................................94 5.5 Conclusions. ....................................................................................................................... 99
Chapter 8. Conclusions and Scope for further study ......・.・・……■. ..........・、’ '.・・・・・・ー・・・..・・・…… 1 31 8.1 Conclusions of the present research work ....................................................................... I 31 8.2 Scope for further study .................................................................,................................... 135