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Front Title

From Editor's Desk : An Announcement

Chatterjee, Achintya K

Bari, Md. Washimul

Chaudhury, Asit K

Class Transitions of Compact Objects Cygnus X-1 and Cygnus X-3

Indian J. Phys. 82 (12), 1749 (2008) 
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Foreword

De, Udayan

Venkatesh, Manisha

Shaikh, Mehzabin S

Venkataramani, B

Indian J Pins 82 (3), 259-263 (2008) 
Study of elemental composition in some II-VI oxides by 
atomic absorption spectroscopy 
Udayan De1*, Manisha Venkatesh ,^ Mehzabin S Shaikh'' and B Venkataramani' 
Variable Energy Cyrlotron Centre DAE 1/AF Bidhanndgar Kolkata 700 064 India 
-Analytical Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400 085 India 
E mail udec/ veccal ernet in 
Abstract There has been an increasing number of measurements in various oxides of significant physical 
property changes ascribed to non-stoichiometry But there has hardly been any direct measurement of the exact 
composition to find the degree of non-stoichiometry For our well studied cadmium oxide problem for example 
DSC (differential scanning calonmetry) showed an unexplained exothermic peak at 270 C Metal content has 
been estimated here by Atomic Absorption Spectroscopy (AAS) for cadmium oxide magnesium oxide and zinc 
oxide Some of these 11-VI compounds have electronic and other applications In this work metal at % has thus 
been determined (at room temperature) from AAS for as supplied metal oxide and after 36 hour firing at different 
temperatures With increase of the firing temperature, we observe a sudden fall in AAS determined Cd at % at 
270 C and then a steady increase of much larger magnitude Our findings are new matching our new DSC and 
RBS data and of significant importance in view of the incompleteness of the Cd O phase diagram available in the 
literature 
Keywords il-VI semiconductors, Atomic Absorption Spectroscopy non-stoichiometry, CdO MgO, DSC 
PACS Nos 71 55 Gs 78 40 -q, 65 40 Ba 
1. Introduction 
Electronics with Il-VI and lll-V compound semiconductors are the natural follow ups, in 
seach of better electronic materials, of the widely used Ge and Si based electronics 
Various R & D in ll-V and Il-VI semiconductors in recent years [1-7] aim at their 
improvement for practical applications, mainly through substitution and doping, as well as, 
at an atomic level understanding of their semiconductivity. Partial substitution in a Il-VI 
semiconductor like zinc oxide, of the group II metal by a suitable element to generate p-
or n- type carriers and to tailor the band gaps is a very competitive field of research in 
view of the potential of these engineered materials (a) as electronic materials for making 
I J rt 
Corresponding Author 
©2008 1ACS 
260 Udayan De, Manisha Venkatesh, Mehzabm S Shaikh and B Venkataramam 
devices like p-n junctions and transistors, and (b) as TCO in solar cells Such material 
modification by 3rd element addition is needed, for example, to meet the requirement thaf 
the layer of a TCO or Transparent Conducting Oxide over a solar cell must be transparent 
to sunlight and yet act as the conducting electrode of the solar cell 
However, possible non-stoichiometry in the ll-VI host, as concluded by some of us for 
differently heat treated cadmium oxide [8-11], magnesium oxide and zinc oxide [11-12] 
causes doping without adding a 3rd element Our work [8-13] had been more elaborate ir 
cadmium oxide, observing new features that hint at significant composition changes, and 
this has been followed up here by composition characterization by Atomic Absorption 
Spectrometry [14] or AAS In view of self-doping due to non-stoichiometry, that may even 
be unintentional, the reality of our suspected non-stoichiometry must be fully known before 
further theories and more importantly, before taking up any impurity-doping project 
Significant differences in electrical resistivity [8,9,13], optical [8] and thermal [10] properties 
due to different heat treatments led us to suspect that these firings changed the actual 
relative compositions / e M O of the oxides of the group II metals, M = Mg, Zn or Cd ir 
this work For our well-studied cadmium oxide problem, DSC (differential scanning 
calonmetry) showed [10] an unexplained exothermic peak at 270°C, flanked by two 
endothermic dips at 230°C and 382°C, one of the new features observed in differently fired 
cadmium oxide XRD, X-ray Photoelectron Spectroscopy (XPS), Rutherford Backscatterinc, 
(RBS), DSC, TGA, TOF-SIMS have been tried in our earlier work [8-13] to characterize 
these materials So, metal content (Cd at%, Mg at% or Zn at% as the case may be) for 
the as-supplied and differently fired samples has been estimated here (at room temperature) 
by the completely new technique of Atomic Absorption Spectrometry [14], using standard 
Cd / Mg / Zn solutions Here, we discuss AAS methodology for the present compounds 
and AAS results for the differently fired oxides 
2. Experimental outline 
Commercially available pure powders of cadmium oxide (99 99% from Aldrich, USA) 
magnesium oxide (99 9% from E Marck, India) and zinc oxide (99 9% from Loba Chemicals 
India) have been made into pellets of 12 mm diameter and ~ 1 mm thickness, under the 
same palletizing load of 6 ton Different pellets were heat treated at different temperatures 
in air for 36 hours in a Carbolite Furnace with PID temperature controller and then cooled 
in the furnace with the cooling rate set at 200°C/h XRD in a Bruker Diffractometer showed 
the correct phase in each sample 
Atomic Absorption Spectroscopy determines the at % of an element in a sample by 
the spectroscopically observed intensity of the atomic absorption lines of the element A 
critical requirement for getting unmodified atomic absorption lines is atomization in the 
AAS set-up of a solution of the sample. Steps for our AAS were . (1) known weight of 
the metal oxide sample was dissolved completely in nitric acid and diluted to a known 
volume, (2) the w t % of the metal was estimated by Atomic absorption Spectrometry 
using hollow cathode lamp made of the same metal, and repeating the experiment with 
Study of elemental composition in some //- VI oxides by atomic absorption etc 261 
standard metal solutions for calibration. Our atomization was done by a Compressed Air 
- Acetylene Flame. Calculation of at% from wt.% is, then, straightforward. 
3. Results and discussions 
Atomic absorption spectroscopy sample was prepared by dissolving a bulk speck of the 
original sample in an acid. So, it gives true bulk composition, unlike the surface composition 
seen by XPS, EDAX, RBS and some other techniques. Table 1 indicates, atomic percents 
ot Mg, Zn and Cd (if detectable as an impurity) in differently fired Mg- & Zn-oxides. 
Table 1. Impurities and composition for differenly fired magnesium oxide and zinc oxide samples from 
present AAS at room temperature Maximum possible error in AAS itself is 5% of the measured 
concentration A figure like "800" and "1 K" = 1000 in the sample name indicates the temperature in °C at 
,..hich the sample was heat treated for 36 hours before AAS, while "as" implies "as-supplied" or unfired 
sample X-rayed (X) and not x-rayed (NX) MgO samples show same at% values, as expected With no 
standard MO samples available, complete calibration could not be done. Accordingly, these results cannot 
;ivo the absolute values of the composition But the results are reliable for studying the variation of 
.omposition with firing temperature. Samples (marked #) were stored in partially evacuated dry condition 
for 6 months, compared to other (fresh) samples, for which AAS was done within 1 to 3 weeks of 
preparation, with similar storing 
Name 
MgCLasNX 
MgCLasX 
MgO.200# 
MgO„800# 
MgO_1K# 
MgO 1K 
ZnO400# 
ZnO_as# 
Cd(wt ppm) 
<180 
<180 
<180 
wt%<0.3 
<180 
-do-
-do-
-do-
Zn (wt ppm) 
<130 
-do-
-do-
-do-
-do-
-do-
24.65 (at%) 
23 82 (at%) 
Mg (at%) 
38 74 
39 02 
36.85 
42 40 
48.95 
45 98 
wt ppm < 100 
-do-
Figure 1 illustrates graphically our AAS result on Cd at.% in differently fired Cd-Oxide. 
Our cadmium oxide was very pure (99.99%), compared to the magnesium and zinc oxide 
material (99.9%), used here. However, our AAS showed that even in these magnesium 
oxide and zinc oxide samples, contamination, for example, of Cd, is lower than 0.018 
wt.%, except in one old 800°C fired sample "MgO_800#". This could be due to possible 
unintentional contamination during firing. Still, even this sample is OK for our main study 
- its Mg:0 ratio matches well with the values for MgO„200 and MgCMOOO samples. 
Composition variation was not expected in X-rayed (X) and non-X-rayed (NX) samples. 
It is satisfying that AAS data in Table I shows ~ 39 at.% Mg in both of these as-supplied 
magnesium oxide samples. As mentioned in Table I, there may be a scaling factor to 
take care of the unknown factors affecting the calculation of O and metal content. Still, 
different AAS results for different firing temperatures definitely indicate composition changes 
262 Udayan De, Mamsha Venkatesh, Mehzabin S Shaikh and B Venkataramam 
due to firings. For zinc oxide, 400°C firing is not enough to change the composition of the 
as-supplied or "as" sample. 
For magnesium oxide (Table I), the set of fresh samples shows that Mg at% increase 
to ~ 46% after 1000°C firing from ~ 39% for as-supplied samples, X or NX. The set of 
three old Mg oxide samples independently show that, with increase of firing temperature, 
Mg at% increases from - 37% to 49%, more than the combined maximum error. For 
cadmium oxide (Figure 1), Cd at% falls slightly at an intermediate firing temperature 
(270°C) and then increases more sharply at higher temperatures. Variation for cadmium 
oxide is sufficiently large with respect to maximum possible error (5%) in AAS - firing at 
800°C giving 19.5 at% higher Cd with respect to the sample fired at 270°C and 12.6 at°0 
higher Cd with respect to the as-supplied sample. This confirms that our AAS-observecl 
composition variation of the bulk to be real. Fall of Cd at% at 270°C can be a case of 
limited Cd-loss and related to above-mentioned exotherm, although further details are not 
clear at the moment. There being no possibility of adding metal atoms to the sample 
during its firing in air in a furnace, this increase of metal fraction actually indicates 0-
loss, the predominant and confirmed process. Present data on compositions of differently 
fired cadmium oxide should help improve the incomplete phase diagram of Cd-O. 
0 45H 
0) 
T3 
'x 
o 0 40 
| 
3 035 
£ 0 30 J 
E 
o 
-*•• 
CO 
3 °25 
" i • 
100 
— I » I — 
200 300 
I ' I — 
400 500 600 
— I — 
700 800 
— I 
900 
Heat Treatment Temperature (C) 
Figure 1. Room temperature atomic absorption spectroscopy result of Cd at% in as-supplied and differently 
fired cadmium oxide samples Heat treatment at the indicated temperatures have always been for 36 h 
practically sufficient to reach the final state. 
4 Conclusion 
A small fall and subsequent large rise of metal at% in the samples as a function of heat 
treatment temperature has been observed by room temperature Atomic Absorption 
Spectrometry, for Cd oxide (Figure 1). This is very much in line with RBS and XPS [9-12] 
observations of similar small fall and subsequent larger rise of metal content as a function 
of heat treatment temperature. For magnesium oxide, an increase of Mg at% for higher 
Study of elemental composition in some ll-VI oxides by atomic absorption etc 263 
temperature is confirmed, while the data is inadequate to decide whether there is a small 
tall of Mg at% at an intermediate firing temperature. With increase of the firing temperature, 
we observe a sudden fall in AAS-determined Cd at.% at 270°C, and then a steady increase 
ot much larger magnitude. Our findings are new, matching our new DSC [10-12] and RBS 
:ii ( 12] data, and of significant importance in view of the incompleteness of the Cd-0 
phase diagram available in the literature. 
Acknowledgment 
One of the authors (UD) thanks Director, VECC, Kolkata, for encouragement, and Shn P 
K Kulnya, lUAC, New Delhi, for help in X-ray diffraction characterization. 
References 
• i ; Z W Pang, Z R Dai and 2 L Wang Science 291 1947 (2001) 
[2] M H Huang, Y Y Wu, H Feick, N I ran, E Weber and P D Yang Science 292 1897 (2001) 
[3] H Rensmo, K K Lindstrom, L N Wang and M Muhammed J Phys Chem B101 2598 (1997) 
i4j C H Liu, W C YIU, F C K AU, J K Ding and C S Lee Appl Phys. Lett. 83 3168 (2003) 
[5] X Liu, C L I , S Han, J Han and C Zhou Appl Phys Lett 82 1 (2003) 
[6] T K Subramanyam, S Uthanna and B Srinivasulu Naidu Mater Lett 35 214 (1998) 
[7| R Ferro and I A Rodriguez Sol Energy Mater Sol. Cells 64 363 (2000) 
[8] Udayan De, M K Chattopadhyay, S Chaudhury, A Sarkar, D Sanyal and T K Dey J Phys Chem 
Solids 61 1955 (2000) 
|9| Udayan De, K C Verma, P Karmakar, A Sarkar, Soma Dey and Sikha Verma Nuclear Instru & 
Methods in Phys Res B212 505 (2003) 
[10] Udayan De and K C Verma Proc of the "15th National Symp on Thermal Analysis", Jaipur (India), 
c/o Indian Thermal Analysis Society 6-8 February (2006) 
111] Udayan De, Rajesh Kumar, Dipak Paramanik, Sikha Verma and Rajendra Prasad International 
Conference on Atomic Collisions in Solids or ICACS, Berlin (Germany), 20-27 July (2006) 
112) Udayan De, Dipak Paramanik, Rajesh Kumar, Rajendra Prasad, P K Kulnya and Sikha Verma 
International Conference on Atomic Collisions in Solids or ICACS, Berlin (Germany), 20-27 July 
(2006) 
[13] K C Verma and Udayan De Indian J. Phys. 79 1075 (2005) 
[14] S B Smith Jr and G M Hieftje Appl. Spectrosc. 37 419 (1983) 


English

Study of Elemental Composition in Some II-VI Oxides by Atomic Absorption Spectroscopy

Chowdhury, S

Choudhury, A

Optical and Structural Studies of SHI Irradiated SiO<SUB>2</SUB> Coated IV-VI Semiconductor Quantum Dots

Indian J Phvs 82 (3), 359-362 (2008) 
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Notes for Contributors

Roy, Amit

Indian J. Phys. 82 (5), 497-504 (2008) 
Use of low energy accelerators 
Amit Roy 
Inter-University Accelerator Centre, New Delhi-110 067, India 
E-mail roydriuac emet res in 
I first thank the organisers of the PANE conference for giving me the opportunity to talk to 
you. I feel privileged to give the Bipinpal Das Memorial Lecture of the conference. Prof. 
Das was an eminent educationist of high intellectual calibre known for his idealism and 
selfless sacrifice. If the teachers and students today need a role model Prof. Bipinpal 
Das would be an ideal candidate. 
For nearly a century ion beams have been accelerated to different energy regimes to 
tackle variety of problems in physics. The entire energy range can be broadly divided in 
three regions: Low, Medium and High energies. We shall assign the values of energies 
to these regions as follows: 
Low Energy 0 - 1 MeV 
Medium Energy 1-1000 MeV(1 GeV) 
High Energy > 1 GeV 
Accelerators of higher and higher energies have been built over the years to probe first 
into the structure of the nucleus, then that of the nucleons. Many ground-breaking 
discoveries in particle and nuclear physics, astrophysics, atomic and molecular physics, 
condensed matter physics, biomedical physics, medicine, biology, and industrial processing 
testify the impact of the accelerator developments. In this lecture some of the current 
work in physics with ion beams at low and medium energies will be reviewed. 
Why do we need high energies? High energies act in two ways. One is their ability to 
impart energy to the system under study and excite various degrees of freedom, and 
second is that they provide a snapshot of the inside of the system with resolution depending 
on their energy in analogy to studying objects with a microscope. The spatial resolution 
that can be achieved depends on the momentum of the particle through the de Broglie 
wavelength associated with the particle. The wavelength associated with an electron and 
a proton is given in Table 1 as a function of the particle energy. 
©2008IACS 
498 Amit Roy 
Table 1 The associated wavelengths of electron and proton at various energies 
Energy 
eV 
MeV 
GeV 
TeV 
Wavelength of an 
2 x 1010 m 
14 x 1013 m 
2 x 1016 m 
6 x 1018 m 
electron 
i 
Wavelength of a proton 
44 x 1012 m 
44 x 1015 m 
11 x 1016 m 
2 x 1019 m 
Particles accelerated to high energies are required to explore the dynamics of systems 
with high binding energies Energies associated with chemical reactions are usually a few 
meV, with atoms in the range of few eV to few keV, with nuclei in the range of MeV and 
with "elementary particles' in the range of GeV 
All accelerators use electric fields in which charged particles are accelerated The 
electric fields are used over most of the available frequency range from static fields to ac 
magnetic fields oscillating at 50 -60 Hz and extending to RF fields in the MHz to GHz 
range New ideas are being developed to use laser beams to generate even higher electric 
fields for particle acceleration 
Every accelerator has a particle source or injector followed by the main accelerator 
The sources for positive ions are usually one of the following glow discharge, ECR plasma 
and sputter source The goal for heavy ions is to maximise the charge state before 
injection into the main accelerator Electrons are commonly generated from a heated 
filament or an indirectly heated cathode Very short pulses of electrons can be generated 
using a powerful laser directed at a photocathode Anti-particle beams are generated 
through the interaction of high-energy particles with energy » 2mc2, where m is the rest 
mass of the particle The flux, / e, the number of particles incident per unit area of 
particles depends on the yield of the ion source and the emittance of the beam Since 
the flux decides the type of physics problems that can be addressed, considerable effort 
has been given for increasing this quantity by beam cooling techniques 
Then comes the main accelerator, which could be of several types, both electrostatic 
or electromagnetic The different categories of accelerators are shown in figure 2 
Electromagnetic field in vacuum does not accelerate particles directly There are two reasons 
for this, (i) E vector of the plane wave in free space is normal to the direction of propagation 
and (n) the wave velocity is c, thus even if we could turn E vector in the direction of 
propagation, the particles would not remain in phase with the wave The wave changes its 
phase as it overtakes the particle and the net effect is zero There are two ways of 
getting around this difficulty One solution is to slow down the electromagnetic wave in a 
suitable structure or medium and let the particles go in a straight line The second solution 
is to bend the particles and let the electromagnetic wave travel as in free space All 
accelerators can be classified into one of these categories 
In the linear electrostatic machines, the electric field is provided by the high voltage is 
generated either using a cascade multiplier circuit or a belt/pellet charging system 
L 
Use of low energy accelerators 499 
Among the RF machines we have one group that can be classified as resonant system 
and the other non-resonant. Linear accelerators using resonant cavities, cyclotrons and 
synchrotrons come under this category. Linear induction accelerators and circular betatrons 
can be classified as non-resonant RF accelerators. 
Before we proceed further, let us take a look at the limits of these machines and the 
reasons for the limits. The energy gain in linear accelerators is determined by the electric 
field and the length of the accelerator. The maximum voltage reached in electrostatic 
machines is 25-30 MV, determined by the breakdown limit of insulation gas medium. For 
resonant cavities, the field limit is set by the field emission of electrons and is close to 
-100 MV/m. This limit has nearly been reached in laboratory tests for superconducting 
niobium cavities operating in the GHz region. However, no existing accelerator as yet 
operates at this limiting accelerating fields. Thus for the length scales of few km we 
expect the energy gain in linacs to be in the range of 100 GeV. In cyclic accelerators, 
the energy gain is determined by the magnetic fields required to keep the particles in 
orbit and the size of the machine is governed by the radius. As we reach the regime of 
relativistic energies, the energy available in the centre of mass system increases only as 
the square root of the beam energy for stationary targets. This is where the colliders 
score over fixed target machines. For a collider, the energy available is the sum of the 
energies of the two particles. With superconducting magnets and a radius of -10 km the 
highest energy achievable is ~ 1000 TeV. But emission of synchrotron radiation limits the 
useful energy for electrons to ~ 100 GeV and for protons to ~ tens of TeV. The highest 
energy lepton accelerator was the 100 GeV electron- positron collider at CERN(LEP) and 
for hadrons the 1 TeV proton-antiproton collider at Fermilab(Tevatron) provides the highest 
energy. The 7 TeV large hadron collider(LHC) at CERN is the highest energy accelerator 
to be built so far, and will be commissioned at the end of 2007. The next high energy 
machine being planned is the International Linear Collider, in which electrons and positrons 
will be accelerated to 500 GeV each first and then upgraded to 1 TeV each. 
The ever-increasing size of accelerators has now reached both the physical and financial 
limits. Thus, totally revolutionary concepts in generating high electric fields are required. 
Would it be possible to use the high crystal fields ( 1017 eV/cm or 1010 GeV/m) present 
in solids although they exist over very small distances? Hopes for the future have come 
from the investigations being carried out in laser-plasma interactions. Extremely high fields 
( 100 GeV/m ) has been generated over lengths of few mm in relativistic plasma waves 
driven Raman forward scattering instability induced by short, high-intensity laser pulses. 
Accelerated electrons upto 44 MeV have been detected from early experiments in this 
field at Rutherford Appleton laboratory[2]. Other laser driven plasma accelerator schemes 
are the Plasma Wakefield accelerator and the Plasma Beatwave accelerator. 
Where are we in India in the accelerator scenario? All our accelerators address the 
low energy regime. Currently the accelerator facilities in India include, 
H U D Pelletron at TIFR, Mumbai with superconducting booster Linac [3] 
15UD Pelletron at NSC, Delhi, with superconducting booster Linac [4] 
500 AmitRoy 
K=140 Variable Energy Cyclotron at Calcutta and the K = 500 superconducting 
cyclotron [5] 
700 MeV electron synchrotron feeding a 450 MeV storage ring INDUS-I at RR CAT 
Indore and a 2 5 GeV storage ring INDUS-II [6] 
3UD Pelletrons at Bhubaneswar [7] and 3 MV Tendctron at Hyderabad [8], 
1 7 MV Tandetrons at, I IT, Kanpur [9] and Kalpakkam [10], 
7 MeV cyclotron at Chandigarh [11] 
5 5 MV Van de Graaff at BARC converted into a 7 MV folded tandem [12], 
8 MeV electron microtrons at Pune [13] and Mangalore [14] 
With superconducting booster upgrades at Mumbai and Delhi, Superconducting Cyclotron 
at Calcutta and the INDUS-II at Indore we shall continue to address low energy physics 
problems in Nuclear and Atomic Physics, Condensed Matter and Materials Science 
World-wide the scenario for Nuclear Physics is moving towards research with radioactive 
ion beams and relativistic heavy ion collisions High brightness synchrotrons are being 
used for condensed matter and atomic physics research Many smaller accelerators have 
now entered the industries and there is a growing market for these machines In the 
higher energy regime efforts are being put to develop high current GeV proton machines 
for applications for energy production, radioactive waste transmutation and spallation neutron 
sources 
Let us now take a look at the impact of accelerators on fundamental research first 
and then we shall turn our attention to the applications in industry and medicine 
Particle Physics 
The development of particle physics has been intimately connected with the availability of 
particle accelerators of high energy Some of the important milestones associated with 
accelerators are 
Discovery of antiproton at Berkeley Bevatron in 1955 
Two neutrinos at AGS, Brookhaven in 1962 
Discovery of CP violation in K decay at Brookhaven, 1964 
Neutral current at CERN proton synchrotron, 1972 
Discovery of J/s at AGS, Brookhaven and Stanford Linear Collider, 1974 
Discovery of b quark, Fermilab, 1977 
Discovery of W and Z with SPS collider, CERN, 1983 
Discovery of top quark, Fermilab and LEP, CERN, 1995 
Now accelerators are probing structures of matter with ever-increasing resolutions 
L 
Use of low energy accelerators 501 
Nuclear Physics 
As we have noted earlier, the accelerators were first built to study the nucleus and these 
nave been an essential tool ever since the first machines were built They have been 
used to probe structure of nuclei at different energy and angular momentum states and 
far from the lines of stability. The energy levels of a large number of nuclei have been 
determined showing a rich variety of phenomena from backbending, superdeformation, 
shape coexistence, etc. The question of how the strong force binds nucleons together in 
nuclei is fundamental to the very existence of the universe. From the first few minutes of 
the "Big Bang", the mutual interactions of nucleons to form nuclei and their further accretion 
to form heavier nuclei, has been crucial in shaping the world we live in Recent experiments 
with accelerators at Berkeley and Dubna have shown evidence for the unusual stability of 
superheavy nuclei. Manifestations of subnucleonic degrees of freedom in nuclei are being 
searched using medium energy electron and proton accelerators Relativistic heavy ions 
are being used to probe the possible quark-gluon-plasma phase of matter 
Vaul t 
nnlv i KM M ft n 
Atomic Phy«l«« 
Material* S c i e n c e 
CJJDA 
„Sv*tttrinft Chamber 
B*j«n HoJl 
•j < h i n > I \ » | ja t * 
Figure 1. Schematic of the 15 UD Pelletron accelerator facility at IUAC with 7 beam 
The facilities available for nuclear physics research are Gamma Detector Array, Recoil-
distance device, Mini-orange spectrometer, Charged-particle array, Neutron Array, Heavy 
Ion Reaction Analyser, Hybrid Recoil Analyser, Indian National Gamma Array, Light 
Radioactive Ion Beam(e.g, 7Be). The schematic of the accelerator system at IUAC is 
presented in Figure 1 and the first module of superconducting linac booster in Figure 2. 
Cosmology and Astrophysics 
Accelerators with higher and higher energies are providing information about the state of 
matter in the universe at early epochs At 100 GeV equivalent of energy the time scale is 
1010 s from the origin in a hot "big bang" model of the universe. Results obtained with 
502 Amit Roy 
Figure 2. Eight Quarter Wave Nb resonators mounted in the first linac module at lUAC 
accelerators on nuclear reaction cross sections allow the observed H/He ratio to be 
explained. The determination of the rates of nuclear reactions occurring inside stars and 
supernova are crucial for understanding of the synthesis of elements. In the coming years 
the advent of radioactive ion beams are going to provide direct measurement of the relevant 
cross sections. 
Atomic Physics 
The mechanism of atomic collisions and ionisation processes is still not sufficiently 
understood. Accelerators are being used in many laboratories towards measurement of 
electron and photon emissions, charge exchange cross sections, energy loss processes 
in atomic collisions. Many of these phenomena are important in understanding of plasma 
processes in tokamaks and dynamics of stellar atmosphere. Radiation from synchrotrons 
is also used for atomic and molecular studies. These types of studies are also important 
to chemistry and biology, not only in understanding of reaction processes, but also in 
determination of structures. 
Condensed Matter and Materials Science 
Condensed matter and materials science also benefited enormously from accelerators 
Synchrotron radiation from electron machines has become a major tool for determination 
of structure of materials using the technique EXAFS. Neutron diffraction studies have 
taken a giant leap forward with intense beams being available from spallation neutron 
sources driven by GeV protons. Ion beams are used in a host of techniques with acronyms 
like RBS(Rutherford Backscattering), ERDA(Elastic Recoil Detection Analysis), PIXE(Proton 
Induced X-ray Emission), NRA(Nuclear Reaction Analysis), SIMS(Secondary Ion Mass 
Use of low energy accelerators 503 
spectrometry), PDMS(Particle Desorption Mass Spectrometry), AMS(Accelerator Mass 
Spectrometry). 
Use of swift heavy ions (SHI) from heavy ion accelerators in material modification is 
throwing new light on relaxation mechanisms in solids in time scales of nanosec to 
picosec Large changes in critical currents have been observed in high temperature 
superconductors on SHI impact The transition temperature is significantly modified for 
materials showing Colossal magnetoresistance 
The facilities available for materials science research are UHV Scanning Tunnelling 
Microscope, Elastic Recoil Detection Analysis, Three-axis Goniometer, In-situ X-ray 
reflectivity, In-situ photoluminescence, Atomic Force Microscope, Low Temp Cryostat with 
8T magnet, In-situ X-ray Diffractometer The in-situ XRD set-up at IUAC is presented in 
Figure 3 
Figure 3 In-situ XRD set up in beam line after the booster linac 
Accelerator produced ion beams are increasingly being used for studying Single Event 
Upset mechanisms for electronic circuits These studies are extremely important for space 
missions, where the circuitry used is subject to bombardment of particle radiation in 
space 
Radiation Biology 
Heavy ions are being increasingly used for radiation therapy. They are highly ionizing and 
the Linear Energy Transfer (LET) for heavy ions are large Also due to the nature of 
504 AmitRoy 
energy loss in materials, most of the energy of a heavy ion is transferred to the medium 
at the end of its range. This is the Bragg peak region in energy loss of ions. This 
property is utilized for heavy ion therapy to target specifically tumour cells which can be 
selectively destroyed with minimum collateral damage to the healthy tissue surroundinn 
it. 
The process of interaction of high LET radiation with living cells is far from understood 
and the studies undertaken in this area are apoptasis, DNA damage and repair. The 
modifications of genetic material under bombardment of heavy ions are also being pursued 
at different labs. 
Some of the areas of science where important contributions have emerged from 
accelerator based research in India are, (i) in Nuclear Physics, fusion fission reactions 
with heavy ions, role of angular momentum in sub-barrier fusion and delineation of the 
equilibration time for angular momentum degree of freedom in fission reactions 
Spectroscopy of high spin states and the role of p-n residual interactions in nuclei, neutron 
emission in pre-equilibrium reactions, (ii) in Atomic Physics, the measurement of inner-
shell ionisation and recoil ion spectroscopy, (iii) in Materials Science, flux pinning in high-
temperature superconductors, change of transition temperature in Colossal Magnetic 
Resistance materials. 
Among the application of accelerators, the notable ones are: Medical applications, 
such as diagnosis and treatment of cancer, Mineral and oil prospecting, using neutrons 
produced with small accelerators, Charged particle beams for processing semiconductor 
chips, Intense sources of X-rays for sterilization of medical equipment and food products 
Charged particle beams for materials sciences analysis and radioisotope production 
Radiocarbon dating and trace element analysis using ion beam induced radiation techniques 
References 
[1] T Tajima and J M Dawson Phys. Rev. Lett 43 267 (1979) 
[2] I Blumenfeld et al Nature 445 741 (2007); S P D Mangles et al, Nature 431 535 (2004); C G P 
Geddes et al, Nature 431 538 (2004); J Faure et al, Nature 431 541 (2004) 
[3] TIFR website : www.tifr.res.in 
[4] IUAC website : www.iuac.ernet.in 
[5] VECC website : www.veccal.ernet.in 
[6] RRCAT website : www.ernet.in 
[7] IOP website : www.iop.res.in 
[8] CCCM website : www.ccmindia.org 
[9] IITK website : www.iitk.ac.in 
[10] IGCAR website : www.igcar.ernet.in 
[11] PU website : www.puchd.ac.in 
[12] BARC website : www.barc.ernet.in 
[13] Univ Pune website : www.unipune.emet.in 
[14] Mangalore website : www.mangaloreuniversity.ac.in 


Use of Low Energy Accelerators

Soibam, Ibetombi

Phanjoubam, Sumitra

Sharma, H Basantkumar

Sarma, H N K

IwlMi'J. P/j.yi-.82(5),6n-6J4(2(X)8) 
Synthesis of lithium zinc ferrite powders by citrate precursor 
gel formation method 
Ibetombi Soibam*, Sumitra Phanjoubam, H Basantkumar Sharma 
and H N K Sarma 
Department of Physics, Manipur University. 
Canchipur-795 003, Manipur, India 
E-mail ibetombi j3hys(r/'rediffmail com 
Abstract • A nitrate-citrate gel was prepared from metal nitrates and citric acid, inorder to synthesize lithium 
zinc ferrites The nitrate-citrate gel so prepared exhibits self-propagating combustion behaviour After combustion 
the synthesized powder is densified at a temperature of 900°C for 3 hours. In this method of synthesis, the 
sintering temperature is lower than that in ceramic process and calcination is not required 
Keywords . Soft Ferrites, Cilrate piccuisoi method, Ndnopui tides 
PACS No. 75.50.Gg 
1. Introduction 
New development and innovative ideas in the area of material processing have often led to 
the discovery of new materials with interesting and useful properties. Lithium and substituted 
lithium ferrites have been found to be very good materials in microwave devices due to 
their low costs, high resistivity and low eddy current loss. In the preparation of lithium 
based ferrites low temperature sintering is desirable to suppress lithium volatility and 
oxygen loss during firing [1], which have detrimental effect on their various properties. In 
order to prepare ferrites at low temperature usually liquid phase agents such as bismuth 
oxide are added. The additives tend to form glassy phase at grain boundaries enhancing 
densification [1,2]. However, they may tend to deteriorate some of the properties of certain 
ferrites [3]. Therefore, low temperature sintered ferrites without additives are a hot topic of 
research. This has been found to be achieved by using active ultra fine powders, which 
can be synthesized by wet chemical methods like the citrate precursor synthesis, which 
has been proved to be very simple and economic, and the particles are of the order of 
Corresponding Author 
© 2008 IACS 
612 IbetombiSoibam, Sumitra Phanjoubam, HBasantkumarSharmaandHNKSarma 
nanoscale [3-5]. Nanostructured material hold promises for dramatic changes in future 
research direction. 
In the present work lithium zinc ferrites has been synthesized by using citrate precursor 
method. The idea behind this technique is a thermally induced anionic redox reaction 
where the exothermic reaction between oxidant and reductant is high enough to form the 
desirable phase within a short time. 
2. Experiment 
Lithium zinc ferrites with compositional formula ^ 5^
 5xZnxFe2 ^  5 x 0 4 where x = 0.0,0 2,0 4 
were prepared by a citrate precursor method. The starting chemicals used in this studv 
were lithium hydroxide, iron nitrate, zinc nitrate and citric acid. 
Appropriate amount of lithium hydroxide was dissolved in dilute nitric acid. This was 
added to a beaker containing stoichiometric amount of zinc nitrate and iron nitrate i he 
solution was made to mix properly and citric acid was added to it. The ratio of meta1 
cations to citric acid is 1:1. The solution was homogenously mixed with the help of a 
magnetic stirrer using a magnetic agitator until a transparent clear solution occurs. Ammonia 
solution was added drop by drop until the pH becomes 7. During this process change r 
colouration occurs, passing through 3 colour stages. After controlling pH at 7 it was 
refluxed at 40°C with continuous stirring for about half an hour. The solution was then put 
in oven at 100°C. Viscosity and colour changed as sol turned into a brown puffy porous 
dry gel. The dried gel then gets ignited, undergoing a strong auto combustion process 
with evolution of large amount of gases, which started in the hottest zone of the beaker 
and propagated from the bottom to the top like the eruption of a volcano, giving rise to 
dark grey voluminous product with structure similar to a branched tree, as shown in 
Figure 1 for x = 0.2 and 0.4. The ash-synthesized product so obtained is the typK a 
(a) (b) 
Figure 1. Picture of a branched voluminous product obtained from auto combustion for (a) x = 0.2 and 
(b) x = 0.4 
Synthesis of lithium zinc ferrite powders etc 613 
spinel structured lithium ferrite powder with nanocrystallite size. The synthesized powder 
was mixed with polyvinyl alcohol as binder and pressed into pellets with 50 kilo Newton 
pressure. All the three samples were sintered at 900°C for 3 hours in air. 
3. Results and discussion 
XRD pattern of the prepared samples confirmed the spinel structure and are shown in 
Figure 2. It has been reported by earlier workers that the spinel phase is generally formed 
m the ash prepared powder. 
ifl 
c 
TO 
(311) 
(220) 
JWrv^*».^,< v'™.*«^. 
( 4 0 0 )
 ^99i511)(440) 
(422) 2n=0 4 
Zn=0.2 
20 30 40 50 60 
20(Degrees) 
Zn=0 0 
70 
Figure 2. XRD pattern for x = 0 0, 0 2 and 0 4 
From an analysis of the XRD data, the average crystallite size of the synthesized 
powder was estimated using Debye Scherrer equation and is found to be 21 nm, 21 nm, 
29nm for x = 0.0,0.2,0.4 respectively. It is therefore observed that citrate precursor is a 
simple method to synthesize highly homogenous lithium zinc ferrite with nanosized 
crystallites. This process has various advantages over the other methods of preparation. 
The process is based on aqueous system and, therefore, it neither requires expensive 
chemicals as alkoxide based sol gel process nor special equipment like autoclaves for 
combustion synthesis. Another advantage is that the ash burnt powder does not require 
calcination at high temperature as in the conventional ceramic process, to transform into 
final powder with expected crystal structure. The phase is generally formed right at he 
moment of auto combustion. Thus the synthesized powder can be sintered at a 
comparatively low temperature, thereby reducing the loss of lithia at the time of preparation. 
Acknowledgment 
The authors would like to thank DRDO, Delhi for financial support, and Dr. L Radhapiyari 
SSPL, Delhi for getting the XRD of the samples. 
614 Ibetombi Soibam, Sumitra Phanjoubam, H Basantkumar Sharma and HNK Sarma 
References 
[1] P D Baba, Gil M Argentina, William E Courtney, Gerald F Dionne and Donald H Temme IEEE 
Transactions on Magnetics Vol. 8 (1) 83 (1972) 
(2) J-H Hsu, W-S Ko, H-D Shen and C-H Chen IEEE Transactions on Magnetics, 30 4875 (1994; 
[3] Zhenxing Yue, Ji Zhou, Xiaohiu Wang, Zhilun Gui and Longtu Li J. European Ceramic Society 23 
189 (2003) 
[4] Xiwei Qi, Ji Zhou, Zhenxing Yue, Zhilun Gui and Longtu Li J. Magnetism Magnetic Materials 251 
316 (2002) 
[5] C Cannas, A Falqui, A Musinu, D Peddis and G Piccaluga J. Nanoparticle Research 8 255 (200C> 


Synthesis of Lithium Zinc Ferrite Powders by Citrate Precursor Gel Formation Method

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