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II.
~re
of great
imrort~nce
suh~t~nces
~olid
state physics
2
Super cooling of mol ten metal etc. is regula ted
NaN0
etc.
3
carefully leading to growth of single crystals.
Tammanns Method
( ii)
...
( iv)
( llJ. )
( v)
(vi)
(vii)
(viii)
-(R)
techniau~
pota~-sium.
(ii)
'Nhisker grov.rth
This technique of Sears (!953, !955) have been
(iv)
(v)
+ 3H 2 = 6HC1 + W
furn~ce
The
Static method
This was devised hy Reynolds and Czyzak (1950)
TIJis charge
Ji'lS
resistance furnace.
deposition.
( ix)
26.
(x)
Epitaxial Growth.
Hergenrother et al. (1960) have shown that SiC
The most
It can be
The following
suoersat~~t~y
on a laboratily scale.
Evaporat-ion at
inducin~
In the
~-
comroon lahoratnry
v~rsion
of th;_s techniaue is
ROT/>.TING
CYLINDER
METI-JOD
~
I
I
'\
'
~ ' ~ 'lui!!'.
,,,,t,[hc.t"" , . . . ,
----
---~~----""'
be rotated slowly.
by slow cooling.
was used and the whole was placed in a large vessel of water
f\OT!ITING
r----J
CRYST~L
METHOD (!9.15)
r'---~
of capacity
The crysta-
speed.
A rod
A wi.th
which form on the surface drop down to the bottom and do not
affect the growing cr'/Stnl.
Kruger
and
Finke
Method
The bag
r2
r2
be~t
.30 to .5 0
31
;
The saturated
CuS~
sulphuric acid,
a saturated solution of the pentahydrate with solid carbon dioxide and Poulenc (1894) obtained it from a solution of cupric
fluoride in concentrated sulphuric acid.
Graham (1835) obtained the monohydrate by heating the
pentahydrate in
vacuum at
38 -
vide infra.
Hodgkinson
in a current
of dry air for a week and Krafft (1907) 60 hrs. over sulphuric
acid in vacuum.
Etard ( 1887) obtained the trihydrate by heating a
saturated solution of cupric sulphate in a sealed tube at
108 - 110 for 48
hours.
alco~ol,
- 20.3 0 ,
Fes~.7H o
sulphate.
cuso4 5H2o It is evident from the above account that the anhydrous
cupric sulphate and the hydrated sulphates other than the
pentahydrate are not obtained under
It is
33
crystals from the solution were tried :
and
1.
2.
Evaporation Method.
r..
'
'
'
'
--.._
];
. v_/ c
~
"'0
'!;
..rv
tc.J
'
C)
're.....,p~"~""t"'rL.
\b'
'lcmp<r<'l.tu re
- ---
. ---
A' represents
saturation
C1
to
i~
at the
solution so
34
''
seeded
prepare
the
4o.o
28.5
180
80.2
75.4
75.4
s
s
s
=
=
&
26.5 + 0.3700 0
&
:: 45 0 -
029 3 0
"
"
.. TABLE- 2
------------------,----------------------,-----------;---,------,
II Temperature
! 0 ! 10 !: 20 Il 30 Il 4o lI 50!I 60 i' 10 i 80 lI 90!J 100 JI
in C
1
I
, i
I
L100
gms
pe
c. c. of
1'
C\IIC\11'
1 1:', 0
, C\1 , ..:t
1"1 I .....,': co
0
i 0:.
I co'
'I "'
1:'-
1:'-
l \()
I '
t
I 1"1a- :'"'I
-o
,...
..:t
!
I
I
lj
.,.~,:r.'
I 't3 1 ~
~ , :i , ~ i S R I a> 'b'
~
I
L~~:~.:_c ______ j_ ___ j ____ j_ ___ j____ i __ l __ j ___ j_ __ j ___ j_~_j__: ___ J
~
1~
Preparation of the Saturated Solution 585.0 gms of the salt (supplied by E.Merck) were
5 minutes.
B.r
the
solution deposits its excess solid and the bottom in the form of
crystals, ( These crystals are twinned together irregularly and
are not single crystals.)
solution.
2.5
5o 0 c
!.-'
\
,
The bell jars were slightly tilted in order to
in
J'l
37
of solvent by
off and the seed crystals were gently washed with distilled
water, dried with blotting papers and were
preserved in
This
These sections
latter
experiments.
2.7
Mounting of the seedsIn earlier experiments the tiny seeds were glued to
thin glass rods when it was found that the solution creeped
on the supporting rods itself.
Minimising creep
Spurious
... ,
j(,
Growth by evaporation -
cork.
Fig. 2. 7( f) the
complete apparatus
with solution &
growing seeds.
.. 39.
only
The
of dimention
The three
'.
l
! '
'.',
..
~b)
~ {11.,1
-----------
~-'II)
The
o~
"
.,,
2.10
---:---~l
RubbH
Cork
l'opp<:l'
\.hre
.Sdk
Fibre
( 't
(b)
(a)
~~. 110 , ..,
I'
1J(r
K.ibra t:'lf
wtrtt
Cr
<15)
crystals
'' and 2.
"
r~
.
"'
'" .
'l -
th~
of the crystal -
rr---,
As shown in fig.
2.1~
the
'!-
%for
The size
d~minished
with increas-
ing r.p.m. but the milky inclusions (due to air) were minimised.
It made no difference whether the vanes are kept below or above
the growing seed.
Work on similar lines has been done by Matuserich
( 1960 ) on the same substance.
NiS~, FeS~,
and
CoS~-
NiS~
5 %,
10
%and
20
%respectively.
found to
of the
crystals.
2. 13
. In Fig, 2. ~3
supply A. C. voltage,
de..,.,c;\ly
place
on the supporting rod (ii) size of the crystal was not much
different than that without passing current and (iii) milky
inclusions ( of air ) were absent.
When the experiment was repeated in the same manner
with D. c. current of the same magnitude it was noticed that
( i) No spurious growth occured on the surface of the solution (ii) The crystal was somewhat more transparent and
(iii) The size of the crystal was approximately larger by
about 10 %.
.. 2.14
Arrangement for cutting the crystal lt'or the measurement of electrical conductivity in
The
even
This method
The following
l4.tL
r.p.m.
The
The crystal is
on to a heavy table.
The sections of the crystal thus obtained are then
ground first on a wet cotton pad then on ground glass surface.
Photographs of the above arrangement and that of the crystal
sections are given below.
lj '
'.10
RBF.IiRBNCBS Alan Holden and Phylis singer, "Crystals and Crystal Growing"
Indian Etlition 1968, Wakils, Feffer And Simons
Private Ltd. Bombay. P. 101.
Bridgman P.S.,(1925), Proc. Am. Acad. Arts Sciences, 60,
303 - 383.
Cohen, li:., and Crouunelin ( 1903), Zeitschrift Fur &l.ektrochemic
9, 431.
Cohen, E., F. D. Chattaway et al, ( 1907), Ziet. Phys. Cham. ,
60' 713
Czochralski J., (1918),
z.
de Copett, 1.
c.,
de Lodyguine, (1893),
u. s.
Patent.,
575,ooo.
A.,
Foote, H.
w.,
Herrick,
York.
'+35.
w.
s.,
Kyropoulos
(1926),
z.
34, 1802.
z.
c.
and
s.
(1960), J. Appl.
Sears, G.
w.
Phys~
Rev.?9, 543;
31, 94.
and Swenson,
P. 26.
Z~
z.
Krist.,