Professional Documents
Culture Documents
ABSTRACT
Rather pure electrolytic nickel was further purified by annealing in hydrogen.
A study was made of suitable refractory crucibles and of melting conditions i,>
produce extremely pure compact metal. The ingots finally prepared Were of a
purity of 99.94 per cent.
New
determinations of
many
have been made on the very pure metal thus made available. Data
are given on density, crystal-lattice constant, melting point, electrical resistiviU
magnetic properties, thermal e. m. f., thermal expansion, hardness, tensile
strength, and reflectivity.
of nickel
CONTENTS
I.
II.
III.
IV.
V.
VI.
Pago
1291
1292
1293
1296
1 298
1299
1299
1300
1300
1301
1 302
1304
1304
1305
!306
1306
!306
13 07
Introduction.
Material
Preliminary melting experiments
Melts of pure electrolytic nickel
Mechanical working and preparation of test specimens
Physical properties
1. Density
2. Crystal structure and lattice dimensions
3. Melting point
5.
Electrical resistivity
Magnetic properties
6.
Thermal transformation
7.
Thermoelectromotive force
Thermal expansion
Hardness
4.
8.
9.
VII.
Summary
I.
INTRODUCTION
and
reflectivity.
With the
various sections rf
1
'
Bureau
1292
[Vol.S
of the materials
detailed discussion of the preparation and purity
the present paper as well
is given
determinations
above
the
in
used
of the above work on physical
as a fairly detailed summary of all
certam of the deterThe methods and results involved
properties.
still
described
be,
will
or
are,
nickel
of
minations of the properties
m
m
whom
MATERIALS
II.
The two
of metal,
Ni-l-A
Ni-2-B
Per cent
Per
c
Si
Fe...
Cu
---
Co
cent
0.05
0)
.003
.007
0.03
.005
.007
.005
.004
.013
.07
.01
Some difficulty was experienced in making satisfactory determinations of sulphur in the original cathode nickel, particularly in the
metal of lot Ni-2-B. Some analyses indicated no sulphur in Ni-2-B,
others gave about 0.005 per cent, while still others showed as high as
0.012.
As is shown later, the sulphur found in fused samples of both
Ni-l-A and Ni-2-B melted under conditions which should not introduce sulphur, indicated that the actual sulphur content of both
lots of nickel was of the order of 0.010 per cent.
Table
1.
Effect of
crucibles
on the composition
Ni-2-B
Purity of resulting ingot
Mell
No.
Type
Type
of crucible
of
furnace
Zirconium
do.-_
N-2*
N-3
KK
N-4
N-5
Ziroconium
silicate
O.
same
Bame
New
N-10
N-ll
"ind
sintered MgO:
inside of crucible fused and
under
C P. MgO+Shellac
ommereial
"he ~v-
(alumi-
silicate).
MgO+shellac
P.
k( ''
'
' '"
'V
lot
of
<.01
Si
.59
.009
.015
.016
.008
.31
.24
.005
.011
.008
.079
.01
<.003
.014
.009
.009
.010
.03
.02
.01
.009
.008
.031
.006
do......
-.do
Billimanite porcelain
num
do
518
Fe
do
do
"\~6l5~
.04
.-do
.-do..
High - fre-
""."oliT
.03
"<."66i"
0.017
.027
.004
quency.
Arsem
do
electric arc.
M, crucible charge
was
Cu
Per cent Per cent Per cent Per cent Per cent Per cent
<0.01
0.59
0.015
0.003
Arsem
silicate
mixture
of coarse flakes
and the
liner as received.
0.028
Jordan 1
Swangerj
2!
): ]
(Table 1), was the less pure nickel, Ni-2-B. The first eight melts
were made in an Arsem vacuum furnace (pressures of 5 to H, nun of
mercury) as were also melts N-10 and N-ll. Ingot N-9 was fused
in vacuum (pressure of less than 1 mm of mercury) in the lii-lifurnace induction furnace.
The three melts made in zirconium silicate crucibles were all
contaminated by phosphorus (N-l, N-2, and N-4), although the
zirconium silicate used was the commercial refined grade. Tho
carbon content of ah melts was slightly lower than that of the origin ;ii
cathode nickel. This decarburization was noticeable with all types
of crucibles, although it was very slight in the first melt in a magnesiashellac crucible. 2
The silicon in the nickel increased very noticeably when the metal
was melted in aluminum oxide (N-3) or in zirconium silicate (N-4).
The alumina crucible, however, contained some commercial alundum
cement (No. 518), which was probably considerably higher in silica
than the
alundum. Increase of silicon in the melt took place
crucibles (N-6 and N-7) but appeared
after some melts in C. P.
to be not necessarily characteristic of all melts in this refractory
(N-8, N-9, and N-10). Melts N-7 and N-8 were, respectively,
the second and third melts of fresh charges of cathode nickel in the
same magnesia crucible. In these cases the solidified ingot did not
wet or stick to the magnesia crucible and could be removed after
cooling to room temperature by gentle tapping and without injury
The remelts were made to determine if appreciable
to the crucible.
purification of the refractory occurred on continued use, particularly
as indicated by an increase in the sulphur content of the nickel ingot
The most serious contamination in any of these trial melts
RR
MgO
the
In all of the preliminary melts, N-l to N-10, regardless of
was
nature of the crucible, the sulphur content of the resulting ingot
of the original
practically 0.01 to 0.02 per cent, whereas the analysis
OOo per
cathode nickel of lot Ni-2-B had shown generally not over
to
doubt
reason
be
may
there
before
cent sulphur. As has been noted
obtained even with
the accuracy of the analytical values for sulphur
the case of this cathode
great pains in the analytical procedure,
,
in a.crucible oi
A final melt of this lot of nickel (N-ll) was made
inside surface of thM
commercial electrically sintered magnesia. The
the crucible *hilejm
crucible was fused and glazed by spinning
.
The
magnesia-shellac
cn^^made
^ riiS^M
No.
281; 1925.
as described
by R-
J-
-s
and
s
P Sn
"
T,rl "
'
i,h>
1294
Bureau
ivoi.s
Jordan 1
Swanger]
go
5|ii
s*
o-sss
2?
11
So
22
aoocv
W*J
"3 so
|S
_=
1
I
OO
4? tca;s
as,
S
'2
*********
12!).-)
1296
IV.
Bureau
ivoi. s
Ni-l-A
resistance furnace.
A stream of dry purified hydrogen was passed
through the tube during the heating. The temperature actually
[cached was somewhat higher than had been intended and the nickel
sample fused. As might be expected, the silicon content of this
fused nickel button was high, namely, 0.14 per cent (NH-1, Table
2), but the sulphur was gratifyingly low.
It was less than 0.002 per
C(MH.
01
* S^^SSSfflfsi.VpaS;
actories for
'
Jordan
swangerj
2) )7
content
(less
'
mm
than 1
of mercury.
The magnetic stirring of the liquid
metal in this furnace very effectively cleaned out all remaining visiblo
traces of magnesia films.
The complete analysis of the resulting ingot (N-19) showed that
carbon, manganese, phosphorus, and silicon were not detectable.
The sulphur content was 0.004 per cent, which was believed to he
Copper appeared to h.
sufficiently low to give a malleable nickel.
increased over that present in the original cathode nickel, namely,
from 0.004 to 0.016 per cent. Cobalt was also 0.0 Hi per cent, about
the same as in the original material. Iron had increased noticeably,
ant,
to 0.024 per cent, and a small amount of magnesium, 0.0<
less
was
present.
larger ingot of nickel was prepared
b]
icedure.
Ingots N-20 and N-21, each weighing about 160 g, were cleaned,
remelted in the Arsem to give ingot N-22, and a final remell in the
high-frequency furnace was designated as N-23. This ingol
approximately the same puritv as N-19, containing 0.005 per cent
and
carbon, 0.004 sulphur, 0.006 silicon, 0.03 iron, 0.006 copper,
no!
were
magnesium
and
phosphorus,
0.016 cobalt. Manganese,
>nt.
detected and a direct determination of nickel gave 99.94
Bhowed
thisingol
in
nitrogen
and
hydrogen,
Later analyses for oxygen,
and nitrogen
the presence of only 6.001 percent oxygen and hydrogen,
per cent.
totaled
100.008
thus
analysis
complete
The
not detected
Bureau
1298
[Vol.
&cm
Table
3.
Hardness of nickel
Hardness
Temperature
half
As
cold
Rockwell
worked
63-C8
52-59
51-59
35-52
fi50.
760
B50
U50
Too
Rockwell
(15-18)
Scleroscope
12-19
8-13
8-13
7-11
4-6
B measurements.
Jordan ]
Swanger]
Properties of Pure
\ichl
(as
heatin-s
enter the
annealing
0.65
and
cm
<
8-2
8-/
Of
C-/
B-3
or
C-3
Of*
S- +
8-f
C-+
Cf
or
or
cm
e#9
Figure
2.-
Serf+4
4*
//
(./+
C#7
C*y
cs*
PHYSICAL PROPERTIES
VI.
1.
DENSITY
(By E.
L. Peffer
Table
4.
Density of nickel
Speci-
Form
men
of
Condition
specimen
>ity
No.
g/rm*
or
B-4
C-4
B-4
C-4
"As
do
Rod
do
do
18296 30
cast"
Cold swaged
...
and density.
Bureau
1300
ivoi. b
3
The maximum density 8.907 g/cm was obtained in the very
had received no mechanical
which
metal
ingot
crystalline
coarsely
working. The density of the worked metal was slightly less, about
3
8.901 g/cm either as annealed or after a 30 per cent reduction in
area by cold working.
6
The International Critical Tables give the density of nickel as
3
The average density of commercial nickel, of
8.90 g/cm at 20 C.
3 7
purity of about 99.2 per cent, has been given as 8.85 0.03 g/cm
.
2.
jr. 8 )
lattice
3.
MELTING POINT
Wm.
F. Roeser )
is
ol
Lp,
TJ.. i,
p. KM
104.
.
^If
:;
wM Book co
^^B^^^:^^^^
'
Am.
'
*l E- 88;
1929.
m4
Jordan 1
SwangerJ
Table 5. Melting
Specimen
No.
Number
of
determinations
Freezes
N-19
N-23
1301
i.
Hire
C.
9
11
Table
6.
<!<
termina-
SaP le
Condition
Oxygen
Hydrogen
Nitrogen
Per cent
Per cent
Per cent
0.001
.008
.001
.015
Not
0.0002
(')
(0
0.0002
(')
(')
(')
o.ow
detected.
4.
ELECTRICAL RESISTIVITY
(By
F.
Wenner and
F. R. Caldwell ")
Specimens B-4 and C-4 of N-23, after being used for density
determinations and magnetic measurements, were cold-rolled until
long enough to handle with ease in the swaging machines and were
then cold swaged to wire 0.079 inch in diameter. This wire was cold
drawn to 0.0385-inch diameter through a steel draw nlat-. except For
Dunn- this
the last three passes which were through sapphire dies.
workino- the metal was annealed in an oxy-hydroiren flame bet*
-insuccessive passes through the grooved rolls or through
d
the
drawuig
through
passes
dies and annealed after every two
diameter
Lengths of 120 cm of approximately 1 mm (0.0386-inch)
measureresistivity
the
for
used
were
wire of specimens B-4 and C-4
sapphire dies from
ments, first as cold-drawn through the last two
been annealed.
after
having
then
and
0.0435 to 0.0385 inch diameter,
annealed at about
The single strand wire, suspended in still air. was
v uiv.
800
means of an electric current passed t hrough the
C by
13
pyromctry section.
resistance and assistant physicist,
Respectively, chief, section of electrical
of Standards Journal of Research
Bureau
1302
[Vol. 6
Table
7.
Temperature
Specimen
No.
B-4
C-4
B-4
C-4
N-19
N-19
N-23
The
and
Resistivity
Condition of metal
at 20
coefficient
of resistance
0 to 100
Microhm-
Ohms per C.
per ohm at
cm
0 C.
7.289
7.292
7.235
7.237
do
do
Before M. P. determination
After M. P. determination
do
0.00667
.00667
.00658
.00674
.00672
14
resistivity of nickel has been given as low as 6.5 microhm-cm
microhm-cm 15 at 0 C. This latter value is from Fleming's
6.9
MAGNETIC PROPERTIES
(By R.
L. Sanford
i)
Specimen C-2 both as cold worked and after annealing was used
for determinations of normal induction, residual induction, and coercive force.
The effect of annealing on the normal induction is shown
in
Figure
3.
"
>.
Am.
R
Electrolytic Nickel, Proc. Roy.
(London),
Mh'SSX
f ^
.ix %2X5
UH-rimental
Researches on Cobalt and Nickel, Ann Chem. Phys.,
S S Ivity '
kunde.'
17,^
" Chief
of
?St; 1925!
magnetic section.
Soc.
Liem P l
Electric
Measurements on Metals
of
High Purity,
Jordan
Swanger}
"j
annea
al[bed by
per
timeter were
Fischer. 20
made with
For
ma^netism."
2o
40
60
tO
/co
/eo
/so
'to
/<A>
zee *ao
**o
**o
x/o
too
/HA6#T/Z/"6
Figure
3.
Normal induction
of pure nickel
The temperature
TM
u
F. Fischer. Apparatus
lafe'.
L^a^K^^
B. B. Jour.
K-n*. 2 (HP
B. S
>;
1~
of Standards
Bureau
1304
Journal of Research
[Vol. 5
THERMAL TRANSFORMATION
6.
(By H. C. Cross
**)
mm
mv
Table
Determined by
8.
thermal analysis
Temperature
Specimen
No.
of transformation
Cooling
Heating
Maximum
Ending
Beginning
C.
B-3
353
359
355
C-3
351
357
357
7.
C.
Maximum
Ending
c.
and
351
|
332
351
a
316
342
THERMOELECTROMOTIVE FORCE
(By F. R. Caldwell
*>)
Table
9.
Table
9.
Temperature of hot
junction
C.
100
200
300
400
500
800
E.m.f.a
Pt-Ni
Millivolts
1.485
3. 105
Temperature of hot
junction
C.
4.590
5.450
700
800
900
1,000
165
1,100
<;.
E.m.f."
Pt-Ni
Millivolts
8.105
9.350
695
12. 130
13. 625
10.
7. (Mi)
mi
I
viMrNo'^r
:
freeman,
5S
physicist,
J
.
.,
jr.,
Use
of a
pyrometry
section,
Method
for
of
Thermal Analysis, B.
S.
Thermal Analyses, B.
S.
Jordan
Swav.ger.
8.
L305
THERMAL EXPANSION
(By P. nidr-
of ingot
N-23.
1',
Si
2
d
b!
//
/
/
/
1
/
)
K>
2 >0
* 30
5 DO
6 00
7 90
B >0
10 00
II
JO
Figure
4.
c.
Thermal
m. I
of the
to 900
near 350 C.
expansivity.
Associate physicist, section of thermal
(
'.
and
30
nmal
from Pt to Ni.
in
the n
an
of Standards Journal of Research
Bureau
1306
Table
10.
Average
Temperature
per
(in C.)
Average
Temperature
coefficient
range
[Vol.6
coefficient
range
C.
per
(in C.)
X10
C.
X10
25
25
25
25
to
to
to
to
100
300
600
900
13.3
14.4
15.5
16.3
400
500
600
700
500
600
700
800
15.9
16.9
17.1
17.7
100
200
300
350
to
to
to
to
200
300
350
400
14.4
15.4
17.2
16.4
800 to 900
300 to 600
600 to 900
18.6
16.5
17.8
9.
to
to
to
to
HARDNESS
tions
shown by the
figure in parentheses.
Table
11.
Hardness of nickel
Hardness No.
Specimen
No.
Baby
Brinell
B-3
C-3
10.
Rockwell
Scleroscope
68(4)
78(4)
100
kg
inch ball
5.0 (3)
5.0 (3)
42
44
TENSILE PROPERTIES
11.
Measurements
REFLECTIVITY
specimen of this
have been made and already reported by
obentz and Stair
and compared with the reflectivity of elec<ropl, rd Qickel and of
commercial refined nickel.
Their results
are I. illy recorded in lugure
5, the curve designated as "C & S vacuum
pure nickel (I)-i
fig
l)
31
S 'z\ K
,.
'
;!!};
\\^}
QnecVmg Power
of Beryllium,
Chromium, and
Jordan ]
Swanger}
SdS^p^.
The
"*"
lire
thereSUltS bt;UmMl
VII.
L307
SUMMARY
summarized in Table 12
Tins metal was
in vacuum and contained not over 0.001
per
electrolytic bkkel
cent oxygen
Nickel
-aHagen
>
300
350
Figure
Table
5.
12.
400
450
Summary
of properties of nickel
As cast.
Worked and annealed.
8.907g/cm3at23C.-
.901.
Density.
.8.917..
of side of unit
cube
(face
centered).
Melting or freezing point
Electrical resistivity
Temperature
coefficient of electrical
resistance.
Thermal
e.
m.
f.
in-
of
3.525
Angstrom
6,150 gausses..
mv at 100 C...
mv at 500 C...
mv at 1,000 C.
X 10-o~
X 10- _
X 10-
X 10--
1.485
6.165
12.130
thermal ex---
units.
1,455 C
7.236 microhm-cm at 20 C...
0.0067 ohms per C. per ohm
at 0 C.
370 to 380
350 C
vs. Pt.
Average coefficient
pansion
600 m>*
pure nickel
Numerical value
Property
Length
550
BOO
Ultra-violet reflectivity of
13.3
14.4
16.5
17.8
Annealed.
From
0 to 100 O.
By magneton
By thermal an
l\iekel
th< rriKM'lectrieally
is
to
platinum.
25 to 100
i C.
800 to 601
600 to 900 0.
Hardness:
Baby BrinelL
68 to 78.
--
Scleroscope...
5.0.
Rockwell
42 to 44.
46,400 lbs./in..
Tensile strength..
Reflectivity
Washington, October
See Figure
3,
5...
1930.
100
kg k
men
only.
ncg-