Rapid Solidification Via Melt Spinning:

Equipment and Techniques

R. W. Jech, T. J. Moore, T. K. Glasgow, and N. W. Orth

SUMMARY
One of the simpler methods available to accomplish rapid solidification
processing is free jet melt spinning. With only a modest expenditure of time,
effort, and capital, an apparatus suitable for preliminary experimentation
can be assembled. Wheel and crucible materials, process atmospheres, cruci-
ble design, heating methods, and process parameters and their relationship
to melt composition are described. Practical solutions to processing problems,
based on "hands-on" experience, are offered. Alloys with melting points up
to 3000°F have been rapidly solidified using the techniques described.
INTRODUCTION
Rapidly solidified alloys exhibit unique microstructure, decreased
segregation, very fine grain size, and potentially, improved properties. The
Chill Block Melt Spinning (CBMS) process is one of several in the category
of rapid solidification processing and lends itself to both research sample
preparation and commercial quantity production at high rates (-60 ft/s).
Unique product forms, such as tool steel ribbon, can be made by CBMS
without laborious rolling and annealing cycles. Figure 1 shows a melt-spun
ribbon of nickel-base superalloy 0.002 in. thick and 118 in. wide. Total
continuous length exceeded 60 ft.
The potential of the process is of sufficient interest that NASA's Lewis
Research Center, General Electric CR&D, the National Bureau of Stand-
ards and others are conducting research on materials produced by CBMS.
Metglas Products Division of Allied Chemical, Marko Metals, and Transmet
Corporation, among others, are producing materials in commercial quantity.
To our knowledge, only NASA Lewis, GE CR&D and Marko Metals are
Figure 1. Melt-spun nickel superalloy rib-
intensively evaluating high-temperature alloys. The other organizations bon 2 mils thick, 1/8 in. wide, continuous
are interested in metallic glasses (e.g., as brazing or magnetic materials) length up to 60 ft.
or reinforcement fibers. The purpose of this article is to introduce CBMS to
those unacquainted with the process and describe some of the innovative
equipment and techniques found useful and necessary at Lewis for
processing high-temperature alloys.
Wheel and crucible materials, heating methods, atmosphere control and
instrumentation will be described. Our experience to date with a "first
generation" apparatus will be described. Many of these innovations will be
incorporated into a more advanced, instrumented, CBMS apparatus currently
under construction at Lewis. A CBMS apparatus is an extremely versatile
and valuable facility and requires a modest expenditure of time, effort,
and capital.
GENERAL EQUIPMENT
A chill block melt spinning apparatus installed in an atmosphere cham-
ber is shown in Figure 2. Its main features are an induction coil to heat
the charge, a crucible equipped with a nozzle and pressurization cap, and a
wheel mounted on a variable speed motor (Volkmann Variable Speed
Drive).
After the charge is melted and superheated in the crucible it is ejected
through the nozzle by gas pressure onto the surface of the rotating wheel.
A puddle of molten metal is formed on the wheel and, as solidification
begins, ribbon is expelled into the chamber or catching device.
Figure 2 shows the apparatus in the "free-jet" variation of CBMS.
There is a gap of from 112 to 3/4 in. between the nozzle and the puddle.
The diameter of the nozzle determines the ribbon width. a 0.04-in. nozzle
produces ribbon about 118 in. wide. A larger nozzle would produce wider
ribbon, but because of surface tension effects, superalloy melts would run
out of the crucible. A slot would also produce wider ribbon, but the molten
stream becomes unstable, resulting in width variations along the ribbon
length. .

JOURNAL OF METALS • April 1984 41

 In the "planar flow" variation of CBMS the crucible is positioned with a
gap of about 0.025 in. between crucible and wheel. The nozzle is typically
in the form of a slot with its long dimension parallel to the wheel axis.
When metal is ejected, the puddle is constrained between the wheel and
flat bottom of the crucible. In the "planar flow" variation, wide ribbon can
be produced because the width of the ribbon is determined by the major
dimension of the crucible slot. We will limit our discussion to the "free
jet" mode of operation, although many of the observations are applicable
to "planar flow" as well.

Wheels
Wheels for CBMS have been made from a variety of materiais. There is
generally a preferred wheel material for a particular melt composition.
Wheel materials are listed in Table I along with operating parameters
which have been used with success at NASA Lewis. These are not necessari-
ly the optimum combinations, but are considered as "starting points" from
which to expand.
The relationship between melt and wheel material and ribbon quality
and microstructure are the subject of on-going research. Primarily, the aim
is to select a wheel which will extract heat from the ribbon as quickly as
possible while allowing the puddle to wet the wheel and form ribbon. An
uncooled wheel acts as a heat sink and is suitable for casting times of only
a few seconds duration. Cooled wheels are desirable for longer runs such
Figure 2. General view of melt spinning as would be encountered in commercial operations.
apparatus for use in vacuum or gas Cooled wheel designs can become complex when the wheel is to be used
atmosphere. inside an atmosphere chamber. Uncooled wheels are much easier to install
and change. For uncooled wheels, quick change Transtorque bushings allow
rapid wheel replacement while maintaining axiality within acceptable limits.
Wheel surface texture and cleanliness influence both product quality and
form. The wheel side of vacuum cast ribbon is almost an exact replica of
the wheel surface. Arrow-shaped marks on the wheel surface are used to
indicate wheel rotation. These arrows are reproduced on the wheel side of
the ribbon and are a great aid in determining the head and tail of the
ribbon. .
Smooth wheel surfaces, e.g., 32 microinches, are appropriate for casting
continuous ribbon of nickel-base superalloys. Rougher surfaces, e.g., 150
microinches, result in discontinuous or flake-like product.
Melt wetting of the wheel contributes greatly to the success of CBMS.
Great care must be exercised to prevent vacuum pump oil, lubricants, or
other contaminants from contacting the wheel and disrupting wetting. The
wheel should be abrasively cleaned and washed with acetone or alcohol
within the shortest practical time prior to actual use.

Crucibles
Selection of a crucible should be based on chemical compatibility with
the melt, temperature resistance, thermal shock resistance, low thermal
conductivity, and low porosity (gas permeability).
Figure 3a shows a crucible made by dipping a wax mandrel in commer-
cial shell mold refractory slurry. Repeated dippings build the crucible wall
to the required thickness. Intricate nozzle geometries may be molded in
wax and duplicated in the shell mold. Simple nozzles may be molded in or
Figure 3. Crucibles used for melt spinning, machined later. Alumina shell mold crucibles are thermal shock resistant,
(a) shell molded, (b) dense alumina, and have low thermal conductivity, and are compatible with most engineering
(c) quartz. alloys, including high-temperature nickel- and iron-base alloys. The major

eM 1
o I 2 ~
o , c J

a b c

42 JOURNAL OF METALS· April 1984

disadvantage of the shell mold crucible is that it is hot fully dense and is
therefore permeable to the pressurizing gases.
A dense alumina crucible is shown in Figure 3b. These are commercially
available, but nozzles must be machined in the closed end of the crucible.
We have used ultrasonic abrasive machining, a process which allows the
drilling of multiple and/or angled holes; As shown in Figure 4, the resulting
hole (0.020-0.040 in. diameter) is circular, clean, and has sharp edges. The
stability of the molten metal jet is dependent upon the shape and uniformi-
ty of the nozzle.
Dense alumina crucibles are compatible with many alloys, are gas tight,
and are useable to temperatures in excess of 3000°F. Their major disadvan-
tage is susceptibility to cracking when internally heated at a high rate. L......J
This can be minimized by using a susceptor to heat the crucible externally, 0. 01"
or by jacketing the crucible to reduce the thermal gradient. When this is
done the dense crucibles survive repeated use. Figure 4. Ultrasonically drilled nozzle in
dense AI 2 03 crucible.
Quartz crucibles, Figure 3c, are useful for temperatures below 2500"F.
They are thermally shock resistant, relatively cheap, and can be purchaSed
with nozzles in place. Temperature limitations and possible reactivity with
the melt are the major disadvantages.
Heating Methods
Radio frequency (RF) induction heating has been the usual method for
heating the charge in the crucible. This can be done by direct coupling to
the melt or by using a susceptor.
Direct coupling is most effective when used with crucibl(!s which are
good thermal insulators, have good thermal shock resistance, and are
opaque, such as the alumina shell mold crucibles described earlier.
Opaqueness is especially important to prevent heat loss by radiation.
Susceptor heating is useful when the resistivity of the charge is very
high (silicon) or very low (copper). Using a susceptor, heat can be intro-
duced to the charge by radiation through the crucible walls. In some cases
it is possible to use a nonreactive susceptor inside the crucible. An exam-
ple of this is the melting of copper or copper alloys using a tungsten
su8ceptor.
Electrical resistance heating elements are useful in place of RF induc-
tion heating for low-melting alloys or for heating charges with very high
or very low resistivity. CBMS of lead, .tin, and lead/tin alloys was done
using resistance heaters surrounding a quartz crucible. The heaters were
commercially available Ni-Cr band heaters I)ormally used to heat plastic
injection molding nozzles. Temperatures to 1200°F were attained in this
way.
Temperature Measurement
Temperature me~surement for purposes of fuonitoring or control may be
done using immersion thermocouples or radiation pyrometry. Care must be
exercised when using thermocouples in an RF field. The thermocouple
wires must be smaller than a certain critical diameter so that they are not
heated by the induction field. The critical size is related to the frequency;
higher frequencies require finer diameter thermocouple wires. Thermocou-
ple w.i res 0.010 in. or less in diameter have been used successfully in a 450
kHz RF field. A two-color infrared radiation pyrometer has been used for
higher melting point (2700°F) alloys.
Ejection Pressurization
Ejection of the melt from the crucible is accomplished by gas
pressurization. An inert gas is usually used, but any gas which is compati-
ble with the melt is suitable. Pressures of 2-20 psi have been used, depend-
ing upon the desired melt delivery tate.
Ejection of the melt by gas pressurization in a vacuum chamber is
complex. Figure 5 is a diagram of the system used as NASA Lewis.
Ejection is accomplished by creating a pressure in the gas supply line
which is higher than the chamber pressure. The heart of the system is the
three-way valve (2) which is used to control crucible pressurization. During
heat-up the valve assures that the pressure in the crucible and the cham-
ber are equal. 'this prevents premature ejection of the melt due to pressure
buildup by gas entrapped in the crucible.
At ejection, the three-way valve (2) is actuated, isolating the vacuum
chamber, pressurizing the crucible, and ejecting the melt. The desired
ejection pressure (2-12 psi) is regulated by setting the vacuum pressure
regulator (4) which serves as a leak valve. The vacuuni pump (3) main-
tains a pressure of flowing gas at less than atmospheric pressure in the
gas supply line. The same piping is used for ejection of the melt into a

JOURNAL OF METALS· April 1984 43

 CRUCIBLE~ CRUCIBLE~
GAS Components GAS
1. Vacuum chamber with crucible and wheel
2. 3-way valve
CHAMBER 3. Vacuum pump CHAMBER
4. Vacuum regulator
5. Gas supply

(a) Heat-up. (bl Ejection.

o CD
Figure 5. Schematic of crucible pressuriza- variety of gas atmospheres in the chamber except that the vacuum pump
tion system showing three-way valve posi- and vacuum pressure regulator are isolated from the system.
tion during (a) heat-up and (b) melt
ejection. Chamber Atmosphere
CBMS may be carried out in vacuum, air, inert gas, or reactive gas
deperlding upon the chemical and physical properties of the charge. Alloys
susceptible to oxidation may be processed in vacuum or inert gas. The
latter is usually used for alloys subject to both oxidation and alloying
element loss due to vaporization. Some alloys such as lead, tin, or bismuth,
need no protection and may be processed in air.
Chamber atmosphere influences ribbon quality with respect to surface
and edge quality. Many alloys cast in vacuum have regular, smooth edges
and wheel side surfaces which are almost exact replications of the wheel
surface. The same alloys cast in helium may have edges with a rough
"saw tooth" appearance and wheel side surfaces with pits and irregularities.
Casting in argon aggravates the condition. The pits and surface irregulari-
ties are thought to be due to gas entrapment under the ribbon during
solidification, but the situation must be more complicated since some alloys
cast in air are perfectly smooth and regular.
Process Variables
Process variables involved in CBMS are primarily wheel composition,
surface speed, temperature, and surface condition. Major variables for the
melt are temperature and ejection pressure.
Generally, increasing the wheel speed results in thinner ribbon. For
example, a nickel-base superalloy (Inconel 713 LC) cast on a mild steel
wheel rotating at a surface speed of 30 ftls produced ribbon 0.0038 in.
thick. When the speed was increased to 90 ftls the ribbon was 0.0018 in.
thick. Generally we have used a wheel speed of 65 ft/s.
Increasing the ejection pressure, within the range 2-20 psi, increased
the ribbon thickness, since more material per unit time was delivered to
the wheel. Increased pour temperature had an opposite effect. There is
some indication that the slight increase in melt fluidity at higher
temperature, along with the increased heat content, allows the ribbon to
spread more before solidification. The practice at Lewis has been to cast at
a superheat 50 - lOO°F above the liquidus temperature of a given alloy.
Process variables also influence alloy microstructure. Under optimum
conditions cooling rates on the order 105 _10 6°/s may be attained. At these
rates equilibrium solid solution limits can be exceeded and alloys not
obtainable by conventional solidification techniques can be formed.
Metals and alloys which have been successfully processed by CBMS at
NASA Lewis range from pure lead and pure tin to superalloys and
44 JOURNAL OF METALS· April 1984
 Table I: Typical Alloys and Operating Parameters Used for Chill Block Melt Spinning (CBMS) at NASA Lewis
Casting Wheel Ejection
Temperature, Wheel Speed Pressure,
Alloy Crucible OF Com~osition ftls Atmos~here psi
Nickel-base
superalloy Dense Ab03, 2500-2700 1020 steel 65 Vacuum 5
shell mold (Ab03)
Tool steel Dense Ab03, 2800 1020 steel 65 Vacuum 5
shell mold (Ab03)
Copper Dense AbOa 2100 OFHC copper 65 Vacuum 10
N il Al intermetallic Dense Ab Oa 3000 304 stainless 65 Argon 10
steel
Fel Al intermetallic Dense AbOa 3000 304 stainless 65 Argon 10
steel
Tin Quartz 495 1020 steel 65 Air 12
Lead Quartz 665 1020 steel 65 Air 12
Bismuth Quartz 555 1020 steel 65 Air 12

intermetallic compounds. The alloys and typical conditions under which

they have been processed are listed in Table I. Figure 6 shows the micro-
structure of a CBMS ribbon of Fe-6.5 Si. All of the alloys listed are very
fine polycrystalline materials in the as solidified condition. The same tech-
niques and equipment may be used to cast other compositions which form
metallic glasses.
CONCLUSION
It has been our intention to introduce CBMS processing to those
unacquainted with the process and describe equipment and techniques
found useful at NASA Lewis. More detailed information and answers to
specific questions about this laboratory research faci lity may be obtained
from the references or by contacting the authors.
Figure 6_ Microstructure of melt spun Fe-6.S
Bibliography 51 alloy.
1. R. L. Ashbrook, Editor, Rapid S olidification Technology Source Book, ASM 1983.
2. H. H. Vincent, et aI. , "A Study of the Melt Spinning Process," in Continuous Casting of Sma ll Sections.
edited by Y. V. Murty and F. R. Mallard, The Metallurgical Society of AIME, 1981.
3. H. H. Liebermann, et aI. , "Process and Structural Aspects of Melt Spun Nickel Base Superalloy Ribbons," Me t.
Trans., 14A, September 1983, p. 1817.
4. Annan., "Amorphous and Metastable Microcrysta lline Rapidly Solidifed Alloys: Status and Potential," Report
NMAB-358, National Materi als Advisory Board, Washington , D.C., 1980.
5. R. Mehrabian, B. H. Kear. and M. Cohen, editors, R apid Solidification Processes: Princlpais and Technoiogles,
Claitor's Publishing Division, Baton Rouge, Vol. I, 1978, Vo l. II, 1980.

ABOUT THE AUTHORS

Robert W. Jech, Metal- Thomas K. Glasgow,

lurgist, Processing Sci- Metallurgist, Processing
ence Section, Lewis Re- Science Section, Lewis
search Center, Cleveland, Research Center.
Ohio. Mr. Glasgow received
Mr. Jech received his his SS and MS in metal-
SMetE from Ohio State lurgy from Case Western
University. He has been Reserve University. He
at NASA since 1958 joined NASA in 1968
working in the fields of powder metallurgy, and since then hes worked on powder metal-
fiber composites, and most recently, processing lurgy products, mechanical alloying, oxide dis-
science. persion strengthening, and physical metallur-
gy of super alloys. He is a member of The
Thomas J. Moore, Metal- Metallurgical Society of AIME.
lurgist, Processing Sci-
ence Section, Lewis Re- Norman W. Orth, Techni-
search Center. cian, Processing Science
Mr. Moore received his Section , Lewis Research
SS in welding engineer- Center.
ing from Ohio State Uni- Mr. Orth has been at
versity and his MS in NASA since 1954. He
metallurgical engineer- has been concerned with
ing from University of Pennsylvania. He joined the design and construc-
NASA in 1963 and has worked in the areas tion of innovative equip-
of diffusion welding and brazing. He is ment for the production of metal powders,
currently working on rapid solidification mechanical alloying, and dispersion strengthen-
processing of copper- and iron-base alloys. ing . His efforts in these areas have resulted
in three patents for such equipment.

JOURNAL OF METALS· April 1984 45