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Master: To .Pcsisinf Inaisq
Master: To .Pcsisinf Inaisq
by
Pisant Ratanapupech
Date Transmitted:
tO .Pcsisinf inaisq
* ;:od 11 . , .
---- —----------------------------------------- DISCLAIMER---------------------------------------------------
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warranty, express or implied, or assumes any legal liability or responsibility for the accuracy,
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necessarily state or reflect those of the United States Government or any agency thereof.
DISTRIBUTION OF THIS DOCUMENT IS UNLIMITED
Mfriv
DISCLAIMER
D IS C L A IM E R
DISCLAIMER___________
This book was prepared as an account of work sponsored by an
agency of the United States Government. Neither the United
States Government nor any agency thereof, nor any of their
employees, makes any warranty, express or implied, or as
sumes any legal liability or responsibility for the accuracy,
completeness or usefulness of any information, apparatus, pro
duct, or process disclosed, or represents that its use would not
infringe privately owned rights. Reference herein to any specific
commercial product, process, or service by trade name, trade
mark, manufacturer, or otherwise, does not necessarily con
stitute or imply its endorsement, recommendation, or favoring
by the United States Government or any agency thereof. The
views and opinions of authors expressed herein do not neces
sarily state or reflect those of the United States Government or
any agency thereof.
by
Pisant Ratanapupech
MASTER OF SCIENCE
Approved:
For __ _ ollege
1980
iv
TABLE OF CONTENTS
Page
ABSTRACT . vi
I. INTRODUCTION 1
II. THEORY 4
IV. EQUIPMENT 12
B. Heating Equipment 13
V. EXPERIMENTAL PROCEDURE 29
VIII. CONCLUSIONS 52
IX. REFERENCES 54
X. ACKNOWLEDGMENTS 57
A. Iron 58
B. Nickel 59
V
ABSTRACT
method. The temperatures of the samples and the blackbody hole were
liquid iron, liquid nickel, and liquid iron-nickel alloys were found to
for liquid iron, from 1729 K to 1823 K for liquid nickel, and from
en^ = 0.340 + 0.007. For the iron-nickel alloys, the results can be
where en^ is the normal spectral emissivity and X^ is the mole fraction
2
of nickel. The coefficient of determination, R , for this regression is
0.9607.
differ in two ways. The first is that the values of the normal spectral
vii
I. INTRODUCTION
blackbody. The blackbody is one that absorbs all the radiation which
The measurements of the radiant flux of a sample are usually made with
and for any wavelength interval than a blackbody of the same size and
liquid nickel, and liquid iron-nickel alloys over the complete range
of these alloys.
4
II. THEORY
2ttC^
e\b = ~ C /XT (1)
X (e -1)
wavelength X
\ = wavelength (cm)
-13 2
= Planck's first constant, 5.9544 x 10 (W*cm )
e Vxb (2)
X
27TC-
ex = ,5 , VXTa (3)
X (e ■1)
5
'X e
Xb
c2/xt
e
c2/wa (4)
e -1
exp (C2/XT) » 1 .
= e (5)
true and brightness temperatures. These are the two temperatures which
were measured in this work and Equation (5) was used to calculate the
suffix when the surface condition has to be specified. Since the clean
had been calibrated by the Bureau of Standards was used for true
Bidwell [9] was the first to determine the normal spectral emissivity
(X = 660 nm) of liquid nickel by using the method described under liquid
(X = 650 nm) of liquid nickel by using the method described under liquid
respect to composition.
enlarged 7 times and their data were read from the enlargement. The
Wien's equation. The results for each composition are shown in Figure 1.
Figure 1. Composition dependence of normal spectral emissivity
of liquid iron-nickel alloys at X = 650 nm calculated
by using Wien's equation from brightness temperature
versus true temperature figure of Lange and
Schenck [12]
11
0.3 - • ■ • • m + w
34 At % Ni
04 - 6nX =0.2993
uo ^«m
49 At % Ni
e nX
04
cnX=0.3040
NORMAL SPECTRAL EMISSIVITY,
0.3
04 51 At % Ni
6nX =0.3082
0.4 71 At % Ni
enx= 0.3119
• * * a
0.3
04 84 At % Ni
«nX =0.3118
* a a
0.3 •
04 94, 97 At % Ni
«nX = 0.3196
0.3
______ 1______ 1______1______i______i______ i_____ i— _J______1______1_____
1800 1820 1840 I860 1880 1900
TEMPERATURE, K
12
IV. EQUIPMENT
same as that of Stretz and Bautista [15] and Moscowitz et al. [16],
which was modified by Dokko and Bautista [17]. This equipment consists
each other and one rotating screw. One of the positioning screws was
used for focusing and the other for moving the pyrometer horizontally
ranges: 760 to 1229°C (1033 to 1502 K); 1000 to 1758°C (1273 to 2031 K);
13
1500 to 2845°C (1773 to 3118 K); and 2000 to 609O°C (2273 to 6363 K).
A right angle prism was used to bend the optical path perpendicular
to the vertical line. This allowed the sample to be viewed from the
located on the top plate which closed the quartz column, as shown in
Figure 2.
Two shutters were attached to the top plate. The shutters consisted
operating rods. The operating rods extended through the top plate and
were sealed with 0-rings between a flange on the rod and the top of the
top plate. The shutters were designed to protect the quartz window
from condensing metal vapors. These shutters were opened only xvhen
measuring the temperature of the sample and that of the blackbody hole.
B. Heating Equipment
QUARTZ COLUMN
R. F. GENERATOR
COIL ------
WATER INLET
WATER OUTLET
The high frequency generator used was Model #P0.10F SC from the
A.C. line. The line voltage was transformed into high voltage and
concentrator located inside the quartz column was water cooled. The
copper induction coil was wound around the quartz column. This
intensified the electrical field acting on the sample set in the center
the heat generated within the concentrator. When the induction furnace
was on, the high frequency current in the copper coil set up a magnetic
current. The magnetic field was forced to pass through the space which
was not blocked by the concentrator such as the hole in the center which
contained the sample. The magnetic field strength was much stronger
in the sample region with the concentrator present than without the
concentrator [18].
The ten turns 3-1/4 in. (8.255 cm) I.D. copper coil was made of
refrigeration grade soft copper tubing 1/4 in. (6.35 mm) O.D. Heat
shrinkable plastic tubing was put on the copper tubing before it was
TOP VIEW
SOFT SOLDERED
COPPER
UNION
WATER
CHAMBER
I’thick THICK
SCALE
i:2
Two crucibles were used. The inside crucible was made of high
purity Al^O^j and the outside crucible was made of tantalum. Molten
iron and molten nickel react with the Ta crucible. The crucible
to hold the sample was 0.755 in. (1.9177 cm) O.D. and 1.040 in.
(2.6416 cm) long. The Ta crucible was constructed from 0.760 in.
rod was milled to fit the outside of the tube. It was then welded
on the outside of the 3/4 in. (1.905 cm) tantalum tubing. The
blackbody hole has a diameter of 1/16 in. (1.5875 mm) and is 5/8 in.
0.55 [19] and the interior of the hole is left rough to increase the
emittance of the tantalum [5], the blackbody hole used in this work
tube, and stainless steel tubing. The tantalum tube was 0.500 in.
(1.27 cm) O.D. and swaged to 0.400 in. (1.016 cm) O.D. to fit inside
the stainless steel tube. The tantalum tube was 8-1/4 in. (20.955 cm)
long and had a 1/16 in. (1.5875 mm) by 3-1/8 in. (7.9375 cm) slot.
This tube is shown in Figure 5. Tantalum was chosen for the support
18
0.890’
0.796'
0.760'
0.703125'
(18 mm)
To CRUCIBLE
SCALE
2 : I
SLOT
1/16" x 3 1/8 "
8 1/4
SWAGED TO 0.400
SCALE
the Ta crucible. The stainless steel tube had an O.D. of 5/8 in.
(1.5875 cm) and was machined to 1/2 in. (1.27 cm) O.D. at the bottom
and was 6-1/4 in. (15.875 cm) long. A 1/16 in. (1.5875 mm) wide slot
was cut in the wall extending the full length of the tube, and two
set screws were attached for positioning the support tube as shown
3/16 in. (4.7625 mm) O.D. copper cooling coil to dissipate any heat
secured inside the stainless steel tube with two set screws as shown
in Figure 2.
a base plate, and a spacer plate. The quartz column was constructed
from a standard 3 in. (7.62 cm) I.D. column, and was 18-1/32 in.
(45.799 cm) long as shown in Figure 7. The top plate was made of
4-3/4 in. (12.065 cm) O.D. by 1/4 in. (6.35 mm) thick stainless steel
plate containing a 15/16 in. (2.38125 cm) diameter hole through which
the sample was viewed and two 1/4 in. (6.35 mm) diameter holes through
which the shutter shafts enter. The plate is shown in Figure 8. The
base plate was made of 3/4 in. (1.905 cm) thick stainless steel and
was 6-9/16 in. (16.669 cm) O.D. Cooling water inlets and outlets were
21
0.410"* 0.001"
COOLING COIL
SOFT SOLDERED TO
6 1/4" * O.OIO" SUPPORT TUBE
D
1/2"
(PRESS FIT IN BASE PLATE)
SCALE
I: I
18 1/32"
SCALE
1:3
©
2 HOLES
4 3/4
2 HOLES
10-32 N F THREADS
1/4" DEEP
15/16" HOLE
3 HOLES, DRILLED a TAPPED
ALL THE WAY
6-32 THREADS
THROUGH DRILLED a TAPPED
ALL THE WAY THROUGH
1/8“ NTP
0- RING
DRILLED a
GROOVE
TAPPED
1/4" THICK
TOP VIEW
O-RING
GROOVE
15/16" HOLE 3 HOLES,DRILLED a TAPPED
ALL THE WAY 6-32 NF THREADS
THROUGH DRILLED a TAPPED
4 3/4* 0.010
BOTTOM VIEW
SCALE
1:2
drilled into the base plate to provide cooling for the support tube and
(1.27 cm) diameter hole in the center of the base plate provided
support for the crucible support tube and as an outlet to the vacuum
system. The quartz column was closed at the top by the top plate and
closed at the bottom by the base plate. These were secured with
clamping ring and tapered fiber ring as shown in Figures 10 and 11,
respectively. The spacer plate was made of 3/4 in. (1.905 cm) thick
stainless steel and was 9.00 in. (22.86 cm) O.D. It had a 2-3/4 in.
(6.985 cm) diameter hole in the center and eight 5/8 in. (1.5875 cm)
diameter holes every 45° (0.7854 rad) as shown in Figure 12. The
spacer plate was attached on the top of the vacuum system and the
base plate was secured to the top of the spacer plate with four
socket head cap screws. The vacuum system used was a 6 in. (15.24 cm)
4 HOLES DRILLED IN
CENTER OF FLANGE t—r "i—r -
SCALE
2:3
4 3/4*0.010
3 29/32^0.005
304 STAINLESS
STEEL
5/32 HOLES
1/4" THICK
TAPERED TO FIT
FIBER RING
(Da©
©a®
3 11/16 HOLE
TAPERED TO 3 1/2
4 1/8
TAPERED TO
3 7/8 ••
3 15/32
4 1/8
SCALE
l: I
O-RING GROOVE
SCALE
3/4' * 0.005 THICK
I :2 SS 304
V. EXPERIMENTAL PROCEDURE
and the column back-filled with high purity argon gas to prevent the
sample from oxidizing. A clean, unused Al^O^ crucible was loaded with
completely fill the sample crucible. The A^O^ crucible was placed
inside the Ta crucible. The top of the column was removed. The
crucibles were placed inside the column on the sample support tube.
The height of the sample support tube was adjusted to place the
sample for approximately 1-1/2 hours before the run was started. The
high frequency generator was shut off and the sample cooled to room
driven out of the metal and the crucibles. Thirty minutes before
starting the run, the temperature controller for the gas purification
furnace was turned on to heat the titanium sponge to 898 K. The argon
gas first passed through the molecular sieves to remove any moisture
and then passed through the titanium sponge in the furnace to remove
any oxygen which might be present in the gas and in the stainless steel
30
pipe line. The vacuum system was closed and the column back-filled
with purified argon gas. Both lower and upper shutters were then
opened and the pyrometer was carefully aligned with the blackbody hole
located at the rim of the Ta crucible. Then both shutters were closed.
The high frequency generator was turned on to heat the sample. The
within the column between the current field concentrator and the
was placed around the quartz column under the copper coil to blow air
on the column. The cooling ring was constructed from 1/2 in.
_2
(1.27 x 10 m) O.D. polyethylene tubing which had 1/16 in.
-3 -2
(1.5875 x 10 m) holes drilled every 1 in. (2.54 x 10 m) on the I.D.
of the cooling ring. Forty psi (2.7579 x 10^ Pa) air pressure were
argon from the top of the column at a pressure of about 1.27 atmosphere
blackbody temperature, the effect of the quartz window and the prism
in the optical path was taken into consideration. The corrections were
N.B.S. test No. 174783, with the automatic optical pyrometer by first
focusing on the lamp through the window and prism and then focusing
can be expressed as
temperature.
^2 1 1
e , = exp [-— (— - —)] (5)
n\ ^LXTT
a
These oxide films were observed on almost all liquid iron samples.
of oxide floating near the blackbody hole. It was found that increasing
the power input to the copper coil caused the film of oxide to move. The
increase in power input to the copper coil increased the magnetic flux
flowing between the concentrator and the sample [18]. This caused the
top layer of liquid sample to flow. Since the copper coil has a
circular shape, the flow direction of the top layer was radial from
temperature at a point near the blackbody hole was higher than the
made was less than 100 K due to the high melting point of iron (1809 K)
spectral emissivity data are presented in Figure 13. The results are
€nX
NORMAL SPECTRAL EMISSIVITY, = 0.3461 0.007
1830 1840
TEMPERATURE, K
Figure 13. Experimental data on the normal spectral emissivity of liquid iron at X = 645 nm
35
compared with other literature values in Table 1 and in Figure 14. Two
distinct differences can be found from the comparison. The first is that
constant as it is for liquid Y, Nd, and Gd [15], La, Ce, and Pr [16],
emissivity values than the present work. These differences may be due
to: (i) the wavelength of radiation; (ii) the quality of the blackbody
hole; (iii) the presence of oxide films or other impurities; (iv) the
accuracy of the equipment for measuring the temperatures; and (vi) the
of radiation used for the present work was 645 nm, while the others were
650 nm or 660 nm. The quality of the blackbody hole used in the
present work had more than 99% blackness from the criteria of Devos [20].
The brightness temperature of iron for the present work was measured
work were taken in a dark room. The present work used a Leeds and
the Leeds and Northrup Co. against their standards which have been
BIDWELL
e nx (1914)
0.500
NORMAL SPECTRAL EMISSIVITY,
DASTUR
0.450 GOKCEN
(1949)
0.400
BONNELL
ET AL.
— (1972) '
d'ENTREMONT (1963)
PRESENT WORK
0.250
>00 1950 2000 2050
TEMPERATURE, K
Figure 14. Comparison of the reported values of the normal spectral emissivity of liquid iron
at around \ = 650 nm
38
pyrometer output.
With few exceptions, almost all of the liquid nickel samples had
near the blackbody hole was higher than the temperature at the center
results are compared with the literature values given in Table 2 and
shown in Figure 16. Again, two distinct differences can be found from
the comparison. The first is that the value of the normal spectral
normal spectral emissivity values than the present work. These differences
NICKEL
LlJ
1
1
|
< 1
cr 1
1
o 0.2
UJ 1
CL 1
CO 1
1
1
_l 1
I o.i
QC
O *
1
1720 1730 1740 1750 1760 1770 1780 1790 1800 1810 1820 1830
TEMPERATURE, K
Figure 15. Experimental data on the normal spectral emissivity of liquid nickel at X = 645 nm
40
0500
0.200
Figure 16. Comparison of the reported values of the normal spectral emissivity of liquid
nickel at around X = 650 nm
WEIGHT PERCENT Ni
10 20 30 40 50 60 70 80 90
0.059
CURIE
TEMP 4>
N)
rl042‘
CURIE TEMP 885'
.0.625
LiiiUiiiJ X f\j j
Figure 17. phase diagram of binary Fe-Ni system [24] with permission of the publisher
43
pure iron and pure nickel metal pieces. To obtain a homogeneous alloy
higher than the melting point of iron and left at that temperature about
was made. The solidified alloy No. 5 was selected to be segmented and
was cut into pieces as shown in Figure 18 using a Sparkatron spark cutter
The method used for the composition analysis of iron-nickel alloy [25]
for alloy No. 5 are shown in Figure 18. The results of composition
was observed for the normal spectral emissivities of these liquid iron-
summarized in Table 3.
67.5 at. 7o Ni. It then increases to e , = 0.340 for pure nickel. The
n\
least-square method shows that this result can be represented by the
Figure 18. Sections of the solidified sample No. 5 segmented
by a Sparkatron spark cutter for chemical analysis
and the results of composition analysis
45
Figure 19. Experimental data on the normal spectral emissivity
for liquid iron-nickel alloys at \ = 645 nm
47
T T
RUN Xf I -14.61 At % Ni
04 enX 1 0.333 ± 0.007
M-m.
0.3
RUN Xt 2-2090 At % Ni
0.4 «nX =0.312 ± 0.005
RUN# 8-29.94 At % Ni
04 «nX '0.304 ± 0.007
0.3 r^-
04 RUN #11-51.43 At % Ni
«nX =0.270i 0008
03
j* m # ^
RUN #5-66.47 At % Ni
0.3 «nX =0246 t 0.007
»—•
0.2
RUN # 12 -72.25 At % Ni
0.3 enX =0.250 * 0.004
*--f» »» » * *---- #»■
0.2
RUN #7-90.70 At % Ni
04 <nx =0 314 ♦ 0007
0.3
J_ _ _ _ _ _ I_ _ _ _ _ _ I_ _ _ _ _ _ I_ _ _ _ _ _ I_ _ _ _ _ _ I_ _ _ _ _ _ I_ _ _ _ _ _ I_ _ _ _ _ _ I_ _ _ _ _ _
1820 1840 I860 1880 1900
TEMPERATURE, K
48
ATOMIC % Ni
51
equation,
cobalt [12] alloys showed that they monotonically change with respect
plateau near the pure cerium side and then went through a maximum at
about 67 at. % Cu, followed by a drastic drop to that for pure copper.
67.5 at. 7, Ni. The normal spectral emissivity then increased to that
for pure nickel. Smith and Chipman's [14] results are higher and Lange
These differences may be explained in the same way as in the case of iron.
52
VIII. CONCLUSIONS
the automatic optical pyrometer onto the liquid sample surface. The
sighting the automatic optical pyrometer onto the blackbody hole. The
quality of the blackbody hole used in this work has more than 99%
of liquid iron, liquid nickel, and liquid iron-nickel alloys over all
by the equation
regression is 0.9607.
Two distinct differences can be found from the comparison. The first
53
showed higher normal spectral emissivity values than the present work.
For some of the runs, the experiments could only be made over a
IX. REFERENCES
22. Tarapore, Erach Dorab. 1977. Fluid flow and mass transfer in
induction melting furnaces. Ph.D. Thesis. University of
California, Berkeley. University Microfilms, Ann Arbor, Mich.
(Diss. Abstr. Int. 77-15878).
25. American Society for Testing and Materials. 1973. Annual Book of
ASTM Standards. Part 32. American Society for Testing and
Materials, Philadelphia, Pa.
56
27. Lustman, B., and F. Kerze, Jr. 1955. The metallurgy of zirconium.
1st ed. McGraw-Hill Book Company, New York, N. Y.
57
X. ACKNOWLEDGMENTS
and Mr. Gary Austin are thanked for composition analysis. The author
also wishes to acknowledge the fellowship from the Royal Thai Navy,
Thailand and the research support from the Ames Laboratory under
WPAS-KC-02-03.
58
The iron and nickel samples used in this work both analyzed
electrode arc melting method [2?]. The metal was first etched
before being put in the arc melter and melted into buttons. These
buttons were then beam melted into large.fingers approximately 3/4 in.
(1.905 cm) O.D., and 4 in. (10.16 cm) long. The beam melting helped
remove the gases trapped in the metal. The finger was then swaged
to 11/16 in. (1.74625 cm) O.D. after which it was machined down to
5/8 in. (1.5875 cm) O.D. The metal finger was cut into pieces. The
pieces of metal were weighed to the amount which when melted would
completely fill the sample crucible. Then they were cleaned by the
proper method.
A. Iron
forceps and a flexible lead. The sample was submerged in the cold
electrolyte with the current still flowing and rinsed briskly in absolute
prevent staining from the acid after warming from the 203 K temperature
characteristics.
B. Nickel
-3
cooled to room temperature before addition of 1.2 gm (1.2 x 10 kg)
quickly removed from the solution, rinsed with distilled water, then
-3
Transfer 1 g (1 x 10 kg) of the sample (10 percent of iron or over),
-3
or 3 g (3 x 10 kg) (under 2 percent iron), from which iron has been
3
removed, to a 400-ml (400 cm ) covered beaker. Add 10 to 25 ml
3
(10 to 25 cm ) of 70 percent HCIO^. Heat to dense white fumes to
Add NH^OH slowly, while stirring, until the precipitate formed slowly
3
dissolves. Then quickly add about 25 ml (25 cm ) of NH^OH and
-3
2 g (2 x 10 kg) of (NH^)2S20g. Boil a few minutes, filter through
precipitate the iron with NH^OH and (NH^)2S20g as before. Filter and
manganese is present.
3
Dissolve the precipitate with 15 to 25 ml (15 to 25 cm ) of hot
HCl (1+4) and wash the filter thoroughly with hot water. Heat the solution
to boiling. Add SnC^ solution drop by drop, while stirring, until the
1 3 3
HCl (i+j) means the mixture of i m of HCl and j m of ^0.
61
color of the ferric iron is discharged, and then add 1 or 2 drops more.
Wash down the inside of the beaker and quickly cool the solution to
3
room temperature. Add, all at once, 10 ml (10 cm ) of saturated HgC^
solution, stir, again wash down the inside of the beaker, and allow the
3
solution to stand for 2 to 3 minutes. Add 15 ml (15 cm ) of the
end point.
of the sample,
62
of the blank,
The pyrometer output data for the run on liquid iron, liquid
are then corrected for the effect of absorption of light by the quartz
window and the prism. After this correction, the observed blackbody
temperature in C.
The sample calculation given below is for the first point in run
output:
mv - mv.
(T) (T. .. - T.) + T. (9)
obs mv. n - mv. i+l i i
i+l i
43.03 - 43.00
(1488 - 1486) + 1486
43.07 - 43.00
= 1486.86°C .
pyrometer output:
= 1350.57°C .
Correction of temperatures:
temperatures:
v [ r (t - 5-)]
a
1.4388
= exp [
-4 (v1809.19 1665.14 )]
0.645 x 10
e = 0.344
n\
65
Pyrometer Pyrometer
Run output3 Run output3
# B S # B S
mv mv mv mv
Pyrometer Pyrometer
Run output3 Run output3
# B S # B S
mv mv mv mv
3 41.20 36.42
41.39 36.66
41.39 36.67
41.42 36.74
41.44 36.70
41.49 36.67
41.49 36.80
41.50 36.75
Pyrometer Pyrometer
Run output3 Run 4. a
# B S # B S
mv mv mv mv
Table 6. (Continued)
Pyrometer Pyrometer
Run output5 Run : ______ output5
# B S # B S
mv mv mv mv
Table 6. (Continued)
Pyrometer
Run output3
# B S
mv mv
Table 7. (Continued)
Table 7. (Continued)