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TECHNICAL
LIBRARY
AMMRC TR 81-29

MELT PURIFICATION VIA FILTRATION

June 1981

D. APELIAN, R. MUTHARASAN, and C. R0MAN0W5K1

College of Engineering
Drexel University
Philadelphia, Pennsylvania 19104

INTERIM REPORT Contract No. DAAG46-79-C-0052

Approved for public release; distribution unlimited.

Prepared for

ARMY MATERIALS AND MECHANICS RESEARCH CENTER

Watertown, Massachusetts 02172
The findings in this report are not to be construed as an official
Department of the Army position, unless so designated by other
authorized documents.

Mention of any trade names or manufacturers in this report

shall not be construed as advertising nor as an official
indorsement or approval of such products or companies by
the United States Government.

DISPOSITION INSTRUCTIONS

Destroy this report when It is no longer needed.

Do not return it to the originator.
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./\MMRC TR 81-29
4. TITLE (and Subtitle) 5. TYPE OF REPORT 4 PERIOD COVERED
Interim Report -
MELT PURIFICATION VIA FILTRATION 1 Jan 81 - 1 Apr 81
6. PERFORMING ORG. REPORT NUMBER

7. AUTHORfa; 8. CONTRACT OR GRANT NUMBERfsJ

D. Apelian, R. Mutharasan, and C. Romanowski DAAG46-79-C-0052

9. PERFORMING ORGANIZATION NAME AND ADDRESS 10. PROGRAM ELEMENT, PROJECT, TASK
AREA 4 WORK UNIT NUMBERS
College of Engineering ,
Drexel University D/A Project: 1L162105AH84
Philadelphia, Pennsylvania 19104 AMCMS Code: 612105.H840011
11. CONTROLLING OFFICE NAME AND ADDRESS 12. REPORT DATE

Army Materials and Mechanics Research Center June 1981

ATTN: DRXMR-.'XP 13. NUMBER OF PAGES

Watertown, Massachusetts 02172 42

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18. SUPPLEMENTARY NOTES

19. KEY WORDS CConf/nue on reverse side it r^ecessary and identity by block number)

Filtration Steel
Liquid metals Superalloys
Aluminum Purification
20. ABSTRACT CConHnue on reverse side il necessary and Identify by block number)
Background on the mechanisms and kinetics of filtration is discussed and the
Drexel mathematical model is further elaborated and updated to encompass filtra-
tion at the higher temperatures encountered in steels and superalloys. A novel
mathematical analysis of inclusion trajectory is also presented.
The aluininum-TiB2 study has been extended to evaluate a ceramic foam filter.
A low temperature model study of liquid inclusion filtration is described and
discussed.
Reference is made to ongoing work in superalloy and steel filtration,
DD 1 JAN 73 1473 EDITION OF 1 NOV 65 IS OBSOLETE
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 UNCLASSIFIED
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Block No. 20

counter-current gas filtration, filter characterization and flow

visualization.

UNCLASSIFIED
SECURITY CLASSIFICATION OF THIS PACiE.(i>^»n Dmim Eitlcrtd)
 •" ri^'',^\i-- '•

ABSTRACT

Background on the mechanisms and kinetics of filtration is discussed

and the Drexel mathematical model is further elaborated and updated to

encompass filtration at the higher temperatures encountered in steels and

superalloys. A novel mathematical analysis of inclusion trajectory is also

presented.

The aluminum-TiB study has been extended to evaluated a ceramic foam

filter. A low temperature model study of liquid inclusion filtration is

described and discussed.

. Reference is made to ongoing work in superalloy and steel filtration,

counter-current gas filtration, filter characterization and flow visualization.

 FOREWORD

This is the third semi-annual report prepared by Drexel University.

It summarizes the progress made during the period July 1st 1980 to

December 31st 1980 on assessing the feasibility of inclusion removal from

molten metal systems. The contract DAAG46-79-C0052 is administered under

the direction of Mr. Arthur Ayvazian, of the U. S. Army Materials and

Mechanics Research Center, Watertown, Massachusetts.

 TABLE OF CONTENTS

INTRODUCTION

2. BACKGROUND

3. PROPOSED KINETIC MODEL

4. PROGRESS TO DATE

4.1 Aluminum filtration

4.2 Steel filtration
4.3 Inclusion trajectory in a converging
flow geometry
4.4 Low temperature model study to simulate
the filtration of liquid inclusions.

5. RESULTS AND DISCUSSIONS

5.1 Aluminum filtration

5.2 Steel filtration
5.3 Inclusion trajectory in a converging
flow geometry

6. FUTURE WORK
6.1 Aluminum filtration
6.2 Steel filtration
6.3 Superalloy filtration
6.4 Low temperature modeling
1. INTRODUCTION

The objective of this work is to characterize, improve and develop molten

metal filtering techniques, with particular reference to the feasibility of

purifying aluminum, steel and metal based superalloys.

Filtering liquid metals removes impurities present in the melt either as

solid or liquid particles. The presence of these particles is known to reduce

the fluidity of the melt, cause internal porosity in castings, reduce mechanical

strength, ductility and fatigue resistance of the product and also result in poor

machinability, surface finish, etc. (1-8).

Until very recently the technology to filter at the elevated temperatures

required for gteel and superalloys has not been available; however, advances in

ceramics, in combination with the need for greater product confidence, has

generated a strong interest in the feasibility of such melt purification. This

interest is largely confined to superalloys and high cost special steels, e.g.,

razor blade steel; however, the prospect of developing a low cost filtration

process for normal high tonnage carbon steels has certain technological and

economic advantages. One of these advantages is the elimination of tundish nozzle

clogging in the continuous casting process: a phenomenon whereby the alumina

spout, which conducts metal from the tundish to the mold, progressively plugs,

restricting flow and necessitating replacement. The plugging is associated with

alumina inclusions in the steel (a product of deoxidation) which sinter to the

nozzle walls. In effect, therefore, the nozzle is acting as a crude melt

purification process, indicating that at these high temperatures filtration is

not only feasible, but will also be effective due to the rapidity of the kinetics.

On the other hand, the filtration of molten aluminum and its alloys has

been a commercial reality for many years and has traditionally been associated

with products such as aluminum foil. More recently, however, the increasing
 use of aluminum in thin walled beverage cans, computer memory discs, demanding

aerospace applications and utilization in decorative products, such as automotive

trim, etc., has placed a renewed emphasis on melt cleanliness.

The particles present in molten metal prior to casting are an inevitable

feature of the production route and may be characterized as:

(i) Exogeneous inclusions: these are either unavoidly present, such

as refractory particles, or maybe inadvertently added such as
coarse clusters of grain refiner, etc.

(ii) Fluxes and salts suspended in the melt as the result of a prior
metal treatment process.

(iii) Deoxidation products as the result of a prior metal treatment process,

e.g., A1„0„ (solid) or SiO„ (liquid) deoxidation products in steel.

(iv) Oxide of the melt which is both suspended on top of the melt and is entrapped
within it due to tuburlence, e.g., A1„0_ in aluminum melts.

It has been found from industrial observation that the majority of the above

particles which are deleterious to product quality lie in the range of 1-30

microns and are dilutely suspended. Removal of these non-metallic inclusions

may be accomplished by filtration. Early advances in melt refining technology

were made by Brondyke and Hess of Alcoa and Brant, Bone and Emley of

British Aluminum.

Since then a number of techniques have been developed and are now well

established. In this program we have concentrated on two types of filter which

have wide scale industrial application; the deep bed filter and the ceramic foam

filter.

The deep bed filter consists of a packed bed of refractory particles

(usually tabular alumina) through which the molten metal flows. The inclusions

deposit onto the grains of the filter medium due to diffusion, direct interception,

gravity, and/or surface forces. Mechanical entrapment has been obser\'ed to be

responsible for filtration of inclusions larger than SOym; whereas, it is believed

that surface forces are responsible for the retention of inclusions smaller than 30pm.

- 2 -
The primary mode of transport of inclusions smaller than SOym to the grain

surface of the filter medium is due to flow dynamics, while surface forces are

responsible for the retention of the inclusion in the case of lower temperature

systems, e.g. aluminum, while in the case of high temperature systems, e.g.

steels, the inclusion sinters to the filter medium . In a depth filter the

inclusions are dispersed through part or all of its volume (depth). It thus has

the advantage of having a large surface area for entrapment and can trap particles

much smaller than the pores of the filter bed. Industrially, therefore, a deep

bed filter has an extended life and is ideally suited to continuous casting

operations. At the end of its life, however, it does have the disadvantage of

being slow and costly to refurbish.

The ceramic foam filter on the other hand consists of a sheet of open pore

ceramic foam approximately 5cm (2 inch) thick. Typically it would have 85%

volume void fraction, an average pore size of 1mm, with approximately 30 pores

per linear inch. It is manufactured by impregnating an open cell polyurethane

foam with a ceramic slurry. The excess slurry is squeezed out so that only the

filaments of the foam remain coated. The resulting body is then dried and fired

at elevated temperatures. The polyurethane foam decomposes to leave a positive

ceramic replica of the original organic foam. A ceramic foam filter can be

installed prior to the casting station with minimal capital expenditure and merely

requires preheating before use. In contrast to deep bed filters, however, it

only has a limited life, the exact value of which depends on the filter area and

melt cleanliness: inclusions in the melt rapidly forming a filter cake on the

surface which increases in depth and progressively restricts flow. The filter

is thus good only for the single drop applications; however the foam slab is

relatively inexpensive, quick to change and does not require constant heating.

- 3 -
 The goals of the current phase of this work may therefore be itemized

as follows:

Evaluate the feasibility of filtering steels and

nickel based superalloys.

Evaluate various filter media for steel and superalloys.

Determine, compare and contrast the fundamental bed

parameters of various filters with an aim to filter
optimization.

By low temperature modeling simulate the removal of liquid

inclusions by filtration.

2. BACKGROUND

In order that a rigorous, systematic study of liquid metal filtration

(both ferrous and non-ferrous) could be performed, the necessary experimental

apparatus and expertise had to be developed. From the experimental viewpoint

the filtration of aluminum was the least difficult of the three proposed alloy

systems, hence it was the first task to be addressed. A large number of depth

filtration trials were made using the aluminum-titanium diboride system. Using

the experience gained from this work a steel filtration apparatus was designed,

completed and commissioned.

A theoretical model was proposed and compared with the results from the

first phase of this investigation. Good correlation was noted and conclusions

were drawn as to the inclusion removal rate and efficiency as a function of

melt flow rate. This work was extended to encompass variations in deep bed

filter characteristics such as porosity, length of bed, filter area, etc. By

understanding the effect of these fundamentals on inclusion capture behavior

and capture kinetics it was possible to begin establishing the criteria for

optimization.

- 4 -
 To further characterize the above parameters, a low temperature model

study was performed using a calcium carbonate/hydrocarbon system, with results

which reinforced the conclusions of the aluminum/TiB„ system. All this initial

work has been fully detailed in the preceeding reports (A^MRC TR-80-160 and

TR-80-49).

Since this initial work, the aluminum/titanium diboride study has been

extended to evaluate an open pore ceramic filter and a system for introducing

counter-current gas flow (an industrial practice) into the deep bed filters,

has been designed.

In the steel filtration field there has been considerable activity: in

fully characterizing the inclusions formed on deoxidation in our apparatus and

also the mathematical modeling of inclusion flow trajectory in an accelerated

flow field has been performed (using the profile of a tundish nozzle as a

reference).

Finally, a low temperature model system to simulate liquid inclusions has

been selected, a filtration apparatus has been designed and is at present in

the construction stage. The model system currently under investigation consists

of ditoluyl inclusions in water passing through a filter of spherical glass

packing.

The combined results of the above work have allowed the kinetic model to

be further refined and updated, taking into account the special conditions

encountered at the higher temperature of molten steel and superalloys. This

revised kinetic model is described in the following section.

3. PROPOSED KINETIC MODEL

The model described in the preceding reports (AMMRC TR-80-160 and

TR-80-49) quantified the important variables and parameters affecting the

inclusion removal kinetics and efficiency for comparatively low temperature

melt systems, e.g. molten aluminum, where the retention of inclusions smaller

- 5 -
than SOy is by quasi-permanent surface associated effects. This model agreed

closely with the experimental results obtained in the aluminum-titanium

diboride and low-temperature model systems. The rentention of inclusions at

the higher temperatures necessary for steel and superalloy filtration is by

a permanent sintering mechanism, hence the kinetic model has to be slightly

revised so that it will effectively describe this high temperature case. The

model is, at present, still limited to the short term behavior of the filter,

a situation which reflects the experimental runs. The fundamental mechanisms,

however, remain largely the same throughout the majority of a filter's useful

life and are described below.

When a melt containing inclusions flows past the grains of a filter medium,

the inclusions should deposit on the surface of the grain if the filter is to

be effective. The primary mode of transport to the grain surface for inclusions

smaller than 30y is flow dynamics, while inclusions greater than 30\i have been

observed to experience mechanical entrapment.

The proposed kinetic model is based on an equation which

relates the overall behavior of the filter to the microscopic entrapment

mechanisms as below.

90
= KC (1)
8t
Z

where

a is the volume of entrapped impurity particles per unit filter volume.

t is time

K is the kinetic parameter

C is the concentration of suspended impurity particles in the

bulk liquid.

Z is the distance from the inlet of the filter.

6 -
 The above expression represents the rate of change of entrapped particles

per unit filter volume. The parameter K is generally found to be a function

of a and is expressed as:

K = K f (a) (2)
o

where K is a constant whose value depends on the properties of the fluid, the

size and surface morphology of both the filter medium and the inclusion. In the

aluminum-titanium diboride studies and in the low temperature models the function,

f(a), is generally found that K is a function of a, which is the concentration of

entrapped inclusions, as well as a function of the melt physical properties,

melt flow rates and the shape and size of the inclusions. The functional nature

of K may be expressed as (11)

K = K o II-
I —
am ' (3)

where K is the kinetic parameter coefficient and a is the inclusion retention

o m
capacity of the filter bed. However, in the case of superalloy and steel melts,

the inclusions sinter readily with the surface of the filter media and act as a

site for further entrapment of other inclusions. Thus, it may be observed

that, f(a), will increase with a. Furthermore, it is reasonable to assume that

electrokinetic forces do not contribute to inclusion capture since the melt is

electrically conductive.

Use of the kinetic expression Equation (1) , in conjunction with an inclusion

mass balance over a differential filter results in a first order partial

differential equation (11).

Using the appropriate boundary conditions the solution can be obtained as:

C.
exp ■^ e^ (^ '(9 - n) (4)
C m
c. re: "
exp((|)n) + exp -i e ^ (6 - n) - 1
'm
- 7 -
 where the subscript i refers to the inlet condition and the dimensionless

parameters are:

m , dimensionless time (5)

1

n = — , dimensionless distance (6)

J-j

K L
is = —— , dimensionless kinetic constant (7)
m

in the above expression, e. is the bed porosity, t is time, U is the melt

1 m
approach velocity, L is the height of filter bed and Z is the distance from

the filter entrance.

Equation (4) gives the concentration of inclusions in the melt as a

t function of time and distance along the filter. For a given value of 9, Eq. (4)

describes the axial composition profile. If one is interested in the exit

concentration, then n will be set to unity in Eq. (4) and the resulting

expression gives the outlet inclusion concentration, C as a function of time.

The fundamental parameter which characterizes the performance of a

depth filter is the kinetic parameter K, as given by Eq. (3). However, the

value of K is a function of the magnitude of the coefficient K and the relative

bed retention a la (see Eq. (3)). The coefficient K is a function of the melt
m o
velocity through the filter, U , the inclusion size, d., the filter grain size,
m 1
d , and the melt system. The coefficient K can be experimentally determined
g o
by short time experiments, whereas determination of a would require experiments

of long duration.

A filter having a relatively finite capacity for inclusions, will reach

maximum inclusion retention capacity with extended use. On the other hand.
for a filter having a very large capacity for inclusions, progressive blockage

of melt flow will occur with extended use. To determine the inclusion retention

capacity factor, a , melts in the order of thousands of pounds must be filtered

m
and hence would require pilot-plant scale equipment. In this study the coefficient

K has been experimentally determined and its dependence on melt velocity has

been quantified using a low temperature model, the aluminum-titanium diboride

system (see AMMRC TR-80-160 and TR-80-49) and is currently being extended to

steel filtration and a low temperature model with liquid inclusions. During the

Initial stages of filter use when the filter bed has been exposed to only a

few residence times, the inclusion retention capacity value of the filter is

large compared to the entrapped inclusions, that is,

olo., ->■ 0. Under this condition, it can be shown that

M

^ e. ^ (9-n) ^0. (8)

a
m

The above enables us to simplify equation (3) to

K Z
"1^ = exp ( - ((.n ) = exp ( - -2- ) (9)
i m

At the exit end of the filter, the dimensionless distance, n = 1 and the

above expression reduces to

C K L ,
^ = exp ( - ^ ^ (10)
i m

Experiments can be designed to measure C., C , U and L, and thus K , can be

1 o m o
calculated by the use of Equation (10) . The preferred approach is one in which

data from many experiments can be used collectively to determine the coefficient

- 9 -
K . P.earrangement of Equation (10) gives
0

C.
In ( -T^ ) (11)
U K L ' C
mo o

The above suggests that if K is not a function of the melt velocity, U ,

o m
then a plot of 1/U vs In (C./C ) will yield a straight line with a slope of
m X o
1/K L passing through the origin. From the slope of the graph one can calculate
o
the coefficient K . However, if the assumption that K is independent of the
o o
melt velocity cannot be made, one may express the dependence of K on U to

the first order approximation as a linear function such as

K = K ' + K " U (12)

o o o m

Combining the above with Eq. (9)

1 1 , . ^O ^ + . _ V ^ (13)
m o 1 o

The above suggests that a plot of 1/U vs In (C./C ) will also give a

straight line with an intercept of value ( - K "/K ') and a slope of 1/K 'L.
° o o o
Hence, the two parameters K ' and K " can be calculated from the plot of
o o
1/U vs In (C./C ).
m 10
It can be seen from Eq. (12) that the capture kinetics are a function of

two terms: the first a constant, attributable to the characteristics of the

filter bed, i.e. filter media size and type, bed porosity and tortuosity, flow

geometry, etc.; whilst the second is a variable which modulates the expression

for flow rate.

The model may be rearranged to accommodate an experimental technique

where filtered samples are taken along the length of the filter bed; that

- 10 -
is, Inclusion concentration C, as a function of height, Z is measured.

Equation (10) can be rearranged as

A plot of ln(C./C(Z)) as a function of Z will yield a straight line with a

slope of U /K and passing through the origin. In this approach one need not

make the assumption on the functional dependence of K on the melt velocity U .

o m
Here, a single short-time filtration experiment will enable the determination of

the kinetic parameter K .

o
Of the two experimental approaches described, it is experimentally easier

to use the first method for melt systems in which only the outlet and inlet

samples are monitored. However, the second approach is found to be effective in

the low temperature model system studies.

4. PROGRESS TO DATE

The phase of the work investigating the filtration of the aluminum-titanium

diboride system through deep bed filters has been completed. The study has now

been extended so that the performance of a ceramic foam filter may be compared.

The steel filtration study has been continued; a thorough investigation of the

inclusions formed during deoxidation having been undertaken and completed.

Preliminary filtration runs have also been performed. In tandem with this work

a mathematical model of inclusion trajectory in a converging flow field has been

developed. Using experience gained from the first low temperature model study

another low temperature model is currently under investigation. This work

utilizes ditoluyl inclusions in water to simulate the removal of liquid inclusions

from melt systems, e.g. Silica from steel melts. Each of these activities is

further discussed below.

- 11
4.1 Aluminum Filtration

Using the experience gained during the deep bed filtration stage of the

work the apparatus was modified, so that it would accommodate the ceramic

foam filter, yet still meet the experimental requirements of: sustained heating,

adequate head and metal flow rates in the range of 1 - 17 Kg/(m s) i.e. filter
2
factors of 5 - 90 lbs./in hr. The filter apparatus consisted of a graphite

fixture (Figure 1), in which a two inch thick disc of the ceramic foam filter

material was inserted. A refractory lined steel cylinder was cemented to the

fixture to complete a filtration "module". Five of these "modules" were then

placed in a special resistance furnace, so modified that molten aluminum was

able to enter and exit the assemblies while they were in the furnace, precluding

the freezing of the aluminum.

The size of the orifice at the bottom of the graphite fixture as well as

the metallostatic head within the apparatus regulate the flowrate through each

module. A steel taper placed in the orifice of each module acted as an on/off

valve to control the flow of metal.

The melt to be filtered was prepared exactly as for the deep bed runs

(see AMMRC TR-80-160 and TR-80-A9). A filtration run consisted of pouring

a transfer crucible containing approximately 25 lbs. of aluminum titanium

diboride suspension into the filtration apparatus. Once the proper metallostatic

head had been attained the steel taper was rem^oved from the orifice and the

filtered metal was collected in cast iron molds. Flowrates were manipulated
2
to give filter factors in the range of 5 - 90 (Ib/hr-in ). Samples of the

melt system were taken from the transfer crucible prior to filtration, and

outlet samples were taken periodically from the filter apparatus. The flowrate
3
(cm /s) was measured by collecting the filtrate over a specified period of time

and determining its weight. For the flowrates involved in these experiments

it was not difficult to maintain the required m.etallostatic head (approximately

18.0 in.) and it is estimated that the metallostatic head varied no more than

- 12
±10% over the course of the experiments.

In addition, an experiment was performed to determine the long term

behavior of the ceramic foam filter material. An apparatus similar to that

used in the previously described filtration experiments was used; the only

essential difference being that a smaller filter disc was employed. In contrast

with the other filtration runs, approximately 130 lb. of aluminum was passed

through the foam filter disk in this experiment; while all other procedures

remained the same. All inlet and outlet samples were then chemically and

spectrographically analyzed for TiB^ content. Selected inlet and outlet samples

along with certain infiltrated filter discs were cut, mounted, electropolished

and metallographically examined.

Although the results of this work are still to be fully analyzed, prelimi-

nary results and discussion are presented in Section 5.1.

4.2 Steel Filtration

In the preceding report (AMMRC TR-80-49) details of the steel filtration

apparatus were described. An instrumented load cell attached to the receiving

crucible records the accumulated melt weight instantaneously. Accurate flowrate

measurements are needed to evaluate the filter coefficient, X.

The primary motive here is to identify and quantify the kinetics of

inclusion removal. Experimental determination of the kinetic parameter requires

a number of filtration runs at different flow rates. Measurement of thfe inclusion

(Al^O,) concentration in the inlet and filtered melt at different flowrate

allows one to calculate the kinetic constant K (equation 2), which is a funda-

mental property. The filtration efficiency, n, may then be calculated.

An extensive literature survey was conducted which revealed that the

refractories Al^O^, MgO, Zr02 and Cr^O^ are good candidates for filter material.

At present AI2O2 filter material is being studied. To determine the effectiveness

13 -
 of the filtration process, alumina inclusions were intentionally formed in

the melt in the same manner as was done by Braun et. al (12). Approximately

the first 20 filtration runs were made using electroytic iron as starting

material. The oxygen content of this electrolytic iron was very high -

approximately 1200 to 1800 ppm. Several runs were made to determine the

nature of inclusions formed when cooling the melt in the furnace, or quenching

on a steel plate. In runs (//21 to #27), the melt was contained in an alumina

crucible. Samples from each run were sent out for expert inclusion analysis

by a specialist in the field. The results show the electrolytic iron which

was used in earlier experiments contained oxygen greater than 580 ppm, thus

resulting in hercynite formation when aluminum was added. Addition of suitable

amount of carbon reduces the initial oxygen level of the melt and further

addition of aluminum then results in alumina precipitation without hercynite

m formation. In light of practical problems, alumina removal is far more important

than hercynite removal. Hence, a 60 pound ingot containing C - 0.012%, 0-13

to 22 ppm, Ni < 0.04%, was obtained.

Using this low oxygen content iron three filtration runs were made. The

oxygen level of the melt was brought up to 400 ppm by appropriate addition of

Fe„0„. Deoxidation was carried out with 0.1% aluminum. Samples of unfiltered

and filtered melt are currently being analyzed. Microscopy of cut samples

from these runs show that there is a significant reduction in inclusion count

in the filtered metal; however, to determine filtration efficiency, chemical

analysis is needed.

The inclusion observations and discussion are presented in Section 5.2

together with some results from the preliminary scoping filtration experiments.

- 14 -
"^•3 Inclusion trajectory in a converging flow geometry: A study of
the nozzle clogging phenomenon.

Singh (13) experimentally showed that the blockage of tundish nozzles by

aluminum-killed steels was caused by an agglomeration of primary alumina inclusions

due to aluminum deoxidation. Since inclusions are being removed during clogging

of tundish nozzles, this may be fundamentally viewed as a melt purification

process. To better understand the mechanism of tundish nozzle blockage and to

investigate its relationship to melt purification, a mathematical model was

developed by applying a force balance to an inclusion. This force balance was

then integrated to obtain the trajectory of the inclusion through the tundish

nozzle. The specific nozzle used in Singh's studies can be thought of as a

channel having a converging geometry (see Figure 2). An understanding of the

inclusion trajectory within the converging channel as well as the capture mode

of the inclusion in the channel is complementary to the kinetic model which deals

with the kinetics of inclusion capture in filters.

A computer program was written to use the Runga Kutta method of inte-

gration to find inclusion trajectories for various initial positions in the

nozzle. The trajectory which terminates exactly at the end of the nozzle wall

is called the limiting trajectory (see Figure 3). All trajectories to the wall

side of the limiting trajectory contact the nozzle and result in inclusion

collection. In contrast, trajectories lying on the other side of the limiting

trajectory (i.e., towards the nozzle center) pass through unimpeded. Thus,

knowledge of the limiting trajectory allows one to calcualte the fraction of

inclusions which contact the nozzle wall - the collection efficiency.

The effect of the different terms in the force balance equation (force

balance applied to an inclusion moving through the nozzle) on' collection

efficiency was evaluated. The steady state drag force balance is:

du (m - m) TV C, R ^P„ u|u| (15)

m— = ^ ^ g -2 d p £ M

- 15 -
Equation (15) is termed the steady state drag force balance because it applies

to an inclusion moving at steady state (not being accelerated) an infinite

distance away from any solid boundaries. In equation (15) M is the mass

of the Inclusion. U is the inclusion velocity relative to the fluid, t is

time, m^ is the fluid mass displaced by the inclusion, g is the acceleration

of gravity, C is the drag force coefficient, R is the inclusion radius, and

u P
p^ is the fluid density. A collection efficiency of 1.71% was found by using

equation (15) and utilizing industrial operating condition values.

Subsequently, the increase in drag force due to inclusion motion close

to a solid boundary was considered. Inclusion motion towards the nozzle wall

is impeded by the added energy required to drain fluid out from between the

inclusion and the nozzle wall. The force balance equation, which takes into

account this drainage effect is

dU _ (. TD —m -1 Cr - (11/2^0
R2p^u|u|
m—
— =
= (m^-m)g - -^^^ ''-—^ ^6)

where the constant k is a function of geometry and i is the distance of the

inclusion from the nozzle wall. Using equation (16) a collection efficiency

of 1.65% was obtained. This is less than the efficiency found previously

(equation 15) because the acceleration on an inclusion towards the nozzle

center is increased as it approaches the nozzle wall.

To take into consideration the effect of acceleration on the trajectory

of an inclusion, two additional terms are considered and subsequently included

in the force balance. The first term to be included is the added mass term,

which accounts for the acceleration of the f;luid adjacent to the inclusion.

The force balance then becomes ■

dU , , ^./^yp^^Pjl^I'M c, m, dU (17) ■
m ^ = (m^-m)g - kl ^ ^ dl

16 -
where C is the added mass coefficient. When this equation was used in the

computer program it was found that 2.9% of the inclusions passing through the

tundish nozzle are collected. This is an increase over the previous cases

because the added mass term decreases the inclusion's acceleration towards

the nozzle center.

The second term to be added to the force balance equation is the history

term which takes into account the dependence of the instantaneous drag force

on the state of development of the boundary layer around the inclusion. In

this case, the force balance equation is

2 I ,

'^ni KO^'' J'i2 • dT

/t-1

where C is the history coefficient and T is a dummy variable of integration.

By the use of eq. (18), a 5.2% collection efficiency is obtained. This is

larger than the collection efficiency found in all the preceding cases since

the history term increases the inclusion acceleration towards the nozzle wall.

The above proposed model is compared with the experimental results obtained

by Singh (13) in Section 5.3.

4.4 Low Temperature Model System to Simulate the Filtration of Liquid Inclusions

To simulate the removal of liquid inclusions from melt system.s e.g., SiO_

in steel or halide salts (a product of reactive gas "cleaning") in aluminum,

a low temperature model system consisting of an emulsion of 0.01% 3-3 dimethyl-

diphenyl in distilled water has been developed. The emulsion has the following

unique properties: (i) the suspension is very stable over several days with

- 17 -
liquid inclusions in a narrow size range of 2 to 4ym; (ii) the density

difference between water and ditoulyl is essentially zero thus enabling

the determination of kinetics of filtration free of settling effects:

(iii) the difference in refractive index between water and ditoulyl is high,

thus enabling easy visualization.

An apparatus to study filtration in this system is currently under

construction. It will consist of five evenly spaced beds of glass beads

each of 5cm height, contained within a 6.3cm diameter plexiglas column.

Sample ports will be placed at the inlet and after each bed.

It is envisaged that an experimental run will proceed as follows: first,

the model melt system will be prepared. This will be an emulsion of 0.01%

3-3 dimethy1-diphnyl in distilled water which will be left overnight to

stabilize droplet size. Scoping experiments with this emulsion have shown

that the droplets range from 2 to 5y; as 3-3 dimethyl-diphenyl has a density,

similar to water, the emulsion formed is stable for several days without the

addition of surfactants. The emulsion will be pumped upwards through the

column and samples will be taken between every 1-2 residence time periods until

the filter appears to be saturated. The samples will then be immediately diluted

with an equal weight of ethanol , in which both of the emulsion components are

soluble. This will allow for spectrophotometric analysis of 3-3 dimelthyl-

diphenyl concentration, although some further dilution may be necessary to bring

the solution into the absorbance range (0-9 p.p.m for ditoulyl) of the spectro-

photometer.

There are three variables in the experiment: velocity,grain size and inter-

facial tension. It is proposed to vary the velocity between 0.015 cm (A range

of industrial interest) for a combination of grain size (glass bead size) and inter-

facial tension. Flow and logistic considerations would dictate glass beads of 3mm

and 5mm diameter, while their interfacial tension can be varied by baking a film

of silicone oil onto the surface. This changes the glass surface from one not

wetted by the diphenyl, to one which is partially wetted.

- 18 -
 5. RESULTS AND DISCUSSION

5.1 Aliimlrunn fi"1 tratinn: Thp_rpraTm'p fnam filfpx.

The results of the filtration experiments are presented in Table 1

and graphically represented in figures 4 to 10, Figure 4 shows the

filtration efficiency is represented by n,, where n is the function of

inclusions removed, i.e.

Ci - %
(19)
Ci

As can be seen from the figure at low melt velocities the efficiency

of titanium diboride inclusion removal approaches 100%, while at higher

velocities (greater than 0.5 cm/sec), the efficiency of inclusion removal

levels off to a value between 40% and 60%.

Figure 5 shows a plot of ln(C-L/CQ) vs l/Uj^, which as predicted by

m the proposed kinetic model, is of a linear nature. It may also be seen

that the line clearly does not intercept the origin, hence the filter

behavior will fall into the regime where the kinetic parameter, K , is

a function of the melt approach velocity, U^. Figure 6 shows the de-

pendence of KQ on the melt velocity, where it can be seen that the func-

tionality may be analyzed by use of equation (12). Analysis of the K^

function yields Kg = 0.018 + 0.062 Um, the first term being the value

of the intercept and hence reflects the intrinsic characteristics of the

filter, whereas the second term is the slope and is related to the flow

rate dependency of the filter.

Figure 7 shows the filtration coefficient, A, (see AMMRC TR-80-160

and TR-80-49) as a function of melt velocity. It can be seen that the

value of X initially drops rapidly with increasing velocity, levelling

19 -
off, however, after about 0.40 cm/sec. This would indicate that to

maintain good filter performance the melt velocity has to be low, or

if production constraints necessitate a higher velocity, then a longer

filter length would be required. This information is reinterpreted in

figure 8 which shows the relationship of A to melt velocity. It can be

seen that A, the depth of filter required to remove 63% of the incoming

inclusions (see AMMRC TR-80-16 and TR-80-49), increases with increasing

melt velocity.

As outlined in the introduction, the longer term behavior of a ce-

ramic foam filter is expected to be substantially different to that

observed in the short term. This disparity in behaviors would be expected

due to the rapid build up of a filter "cake" on the top surface of the

foam. An experiment to monitor this cake formation was performed. The

superficial melt velocity was measured as a function of time, the results

are presented in Figure 9. It can be seen that the melt approach velocity,

Um) initially remained fairly constant, then abruptly dropping and leveling

off to a value much lower than the initial melt approach velocity. A plot

of At/AV as a function of V, Figure 10, where AV is the increment of fil-

trate collected over a time period At, and V which is (V-[_ + V2)/2 of each

increment of filtrate volume, indicates that the ceramic foam filter in

this run exhibits behavior characteristic of a cake filter where dt/dV =

CK-|_/P)V + (K2/P) for constant pressure cake filtration, i.e., where the

metallostatic head remains constant; (K^/P), (K2/P) constants for a partic-

ular filtration system. A plot of the cumulative filtrate volume, i.e.,

the total volume of aluminum melt passed through the apparatus, as a

function of time indicates that the 1.0" diameter

- 20 -
ceramic foam filter disk used in the long term filtration run progressed

from an initial packed bed mode of filtration, where the flow rate re-

mains essentially constant, to a cake filtration mode, after approximately

8500 cm^ of aluminum had passed through the system. This analysis is

based on the fact that as the cake forms and builds up, the pressure (AP)

required to force metal through the cake increases; however, since this

was a constant pressure operation where AP = pgh, h being the metallo-

static head, the driving force decreases, resulting in a steadily de-

creasing flow of metal through the system, which was in fact observed.

Subsequent metallographic examination of the filter disk used in

the long term filtration run clearly showed that a cake had formed on

the top surface. Although inlet and outlet samples were taken during

this run they cannot be used to estimate a , the available capture

volume of the filter because: (i) the filter enters a cake filtration

mode which is not encompassed by the proposed kinetic model; (ii) the

samples are analyzed only for titani'om diboride content, hence there is

no information as to the total volume and number of inclusions present

in the melt.

It should also be noted that the results obtained from spectro-

photometric analysis provide only quantitative information about the

titanium diboride content; they give no indication of a qualitative

nature, i.e. the effect of filtration on inclusion size distribution is

unknown. It is believed that inclusion particle size is an important

factor in determining filter performance, however particle size anal-

ysis is a slow, costly and specialized procedure; hence the effect of

this variable in all the experiments has been minimized by using a con-

21 -
 sistent titanium diboride master alloy, systematic stirring, etc.

5. 2 Sj:eel FIT tration

To date 31 filtration runs have been made. Many of those were

scoping experiments to debug the apparatus and to verify the nature of

the deoxidation products which were being "manufactured". The inclu-

sion observations are summarized in Table 2. In some runs Fe-10% Ni

alloy was used as the starting material, rather than pure iron. The

purpose of this was to assist in etching the structure, hence better

delineating the portion of the inclusions in relation to the solidifi-

cation structure. Table 3 summarizes the successful filtration experi-

ments. In both runs numbers 5 and 10 the Al 0 was reduced approxi-

mately seven-fold (from 0.0784 to 0.0116 and 0.1945 to 0.0264, respec-

m tively), whereas the total oxygen was reduced between 2 to 4 times.

It is expected that as the apparatus has now beeii debugged and

standardized, filtration runs will proceed apace, resulting in the

following contributions:

(1) The major mechanism by which particles are entrapped in the

filter m.edium will be identified.

(ii) The functional nature of the particle capture kinetics in

steel melts Xv'ill be developed.

(iii) The kinetic parameter, KQ, and the filtration coefficient, X,

will be experimentally determined.

(iv) The effect of the important operating (process) variables on

the performance characteristics of the filters will be deter-
mined .

22 -
5.3 Inclusion Trajectory in a Converging Flow Geometry
(12)
The proposed model may be compared to Singh's experimental

results. Singh reported that flow through the nozzle shown in Figure

2 became greatly reduced after 21 minutes. The inclusion trajectory

model proposed here predicts that at Singh's casting conditions, 1.5%

of the inclusions passing through the nozzle will be collected. THis

value of 1.5% collection gives a total volume of collected inclusions

of 21 cm^ which is more than enough to reduce the flow through Singh's

nozzle. The bottom section of Singh's nozzle has a volume of approxi-

mately 40 cm^. Since alumina inclusions readily sinter together there

is a great deal of void space in the bulk agglomerated alumina at the

nozzle exit. Thus, the total volume of the agglomeration is much more

than 21 cm^ and the inclusion trajectory model successfully explains

the tundish nozzle blockage phenomenon.

The important result of this phase of the program is the similarity

of the mechanism of nozzle blockage to the inertial impaction mechanism

(14)
of impurity removal in depth filtration . This indicates the high

potential of depth filtration as a viable process for melt purification.

- 23 -
6. FUTURE WORK

Work is planned in several different areas:

6.1 Aluminum Filtration

• The performance of the deep bed and ceramic foam filters will
be compared and contrasted with reference to the kinetic model.

• The industrial practice of passing counter current gas flow

through a deep bed filter will be evaluated.

A series of filtration experiments will be conducted using a

ceramic filter, the tortuosity and surface area of xvhich are
readily definable.

6.2 Steel Filtrati_on_

• The efficiency of filtration will be evaluated initially using

A1„0_ tabular beds.

6 .3 Superalloy ^Filtration

Evaluation of filtration efficiency initially using Al 0 tabular

beds. Work is currently in progress to design modifications to
the steel filtration apparatus for superalloy work.

6.4 Low TemperatureJModeling.

The current work extending the original diesel/calcium carbonate,

solid inclusions system, to the liquid inclusion system will be
continued. It is expected that the model will elucidate the
effect of factors such as velocity, grain size and interfacial
tension on the performance of a filter removing liquid inclusions.

This work may be extended to include a flow visualization study

which will pictorially record and illustrate the capture, satura-
tion and subsequent release phenomena of liquid inclusion in
packed beds.

- 24
 REFERENCES

1. F.R. Mollard, N. Davidson, "Ceramic Foam - A unique Method of

Filtering Molten Aluminum in the Foundry", presented at the 1978
AFS Conference, Detroit, Michigan.

2. R.B. Miclot, Technical Report No. 67-1507, Rock Island Arsenal,

June 1967.

3. L.A. Alekseev, I.B. Kumanin, Izv. Vyssh. Uchebr. Zaved. Tseutn.

Metall., Vol. 11, No.l (1968), pp. 155-159.

4. D. Apelian, ScD. Thesis, MIT, 1972.

5. H.E. Miller, Aluminum (1972), pp. 368-371.

6. Dj. Hedjazi, G.H.J. Bennett, V. Kondic, Metals Technology, Dec.

C1976) pp. 537-541.

7. A.I. Kemppinen, G.D. Schnittgrund, Light Metals, Vol. 2 (1969),

pp. 721-732.

8. J.J. Farber, F.M. Rupp, Light Metals, Vol. 2 (1979), pp. 733-740.

9. K.J. Brondyke, P.D. Hess, Trans. TMS-AIME (1964), Vol. 230, pp.
1553-1556.

10. M.V. Brant, B.C. Bone and E.F. Emley, Journal of Metals, March (1971)
Vol. 23, pp. 48-53.

11. D. Apelian, R. Mutharasan, "Filtration, a Melt Refining Method",

Journal of Metals, September (1980), Vol. 32, No. 9, pp. 14-19.

12. T.B. Braun, J.F. Elliot, and M.C. Flemings: Met. Trans. Vol. lOB,
June 1979, pp. 171-184.

13. S.N. Singh: I & SM Journal, June 1979, pp. 40-46.

14. L.A. Spielman: Ann. Rev. Fluid Mech., 9:297, 1977.

- 25 -
 TABLE 1

Summary of Filtration Results

Ci-Co
Sample UmCcm/s) 1/Um Cl(ppm) Co(ppm) ''^- Cl
ST201 0.22 4.53 979.2 382.5 0.61

ST202 0.22 4.53 979.2 489.6 0.50

ST301 0.153 6.54 750.0 351.9 0.53

ST302 0.153 6.54 750.0 183.6 0.76

ST401 0.075 13.32 1040.0 168.0 0.84

ST501 0.056 17.92 581.4 137.7 0.76

ST603 0.451 2.22 45.2 22.9 0.49

ST701 0.775 1.29 26.8 16.8 0.37

 <:
w
XI
U
•H
B
OJ
3

n
S-i
3
OJ

en
•H
3
•H
OJ
01

O
<4H
3
3
•H
O
3

X
en
01
U
3
O
3
o
o

>
O
•H
o
C
en

X3
en
>
3
4J

QJ

01
(-1
■H
3
4-1

CJ
3
0)

-i3

1
>?

c3

•H

SH
4-1

CU
Melted at 1600°C, melt is held Duplex inclusion SEM study

m
%

^ -H
C X
rH
flH -H

w -H
O 3
u r-i
3
O B
3
0)
OJ 3

rH 3
for 30 min. at 1600°C, solid shows the presence of Fe,

>, 3 6
O
U ^
•H 3 <U
U 0 U
O -H OJ

O
a
_^
3
4-1
CO

ca
M
•
aluminum (0.09 wt%) is dropped Al and 0 in inclusions.

o a A

SO
in the melt. The induction Size of inclusion: 2-40ym.
power was shut off after 5 min. Near crucible wall clusters
of aluminum addition. of inclusions were present.

Spherical inclusions of

CM
(N
Electrolytic iron melted No Al or Fe203 was added. The
at 1600°C in alumina sample was held as 1600°C for size 2-10 pm were present.
crucible in argon 11/2 hrs, and then furnace SEM study shows the presence
atmosphere. cooled. of Fe and 0 in inclusions.

eg
Electrolytic iron + Melted in vacuum ('^ 10 microns) The sample was very clean.
0.0 25 % C in alumina and then furnace cooled after Negligible amount of small
crucible in argon holding at 1600°C for 30 min. inclusions 1 to 5 ym were
atmosphere. present.
 TABLE 3

Summary of Filtration Experiments

Wt % AI2C 3 Wt % Oxygen
Run No. Inlet to filter Outlet Inlet to filter Outlet

5 0.0784 0.0116 0.0365 0.0114

8 0.2644 0.0019 0.1800 0.1000

10 0.1945 0.0264 0.1700 0.0600

20 0.1210 0.0180 0.0914 0.0203

28

29
analysis unavailable at the time of ^inriting this report .
30

31
 Al > lK)CLU5\Ok)

STEEL TUBE
RESISTANCE
FURNACE

GRAPH\TE FlXTliRE
7 ■^'
5ELEE RLTER

^-^-^
TT

FILTRATE
/

M0UDC5)

Figure 1. A schematic of the Ceramic Foam Filtration Apparatus used in

the investigation of short-term filter behavior.
 5 cm

10 cm

Figure 2. Schematic diagram showing dimensions of the converging nozzle

geometry studied by Singh (13)
 R (cm)
2.0 2.5 3.0

5.5

5.0

4.5

E
-^ 4.0 —

3.5

3.0

2.5
Figure 3,
Limiting trajectory computed from the model (equation 9) shown at'
the exit side of the converging nozzle. Z indicates the height
from the nozzle exit, and R is the radial distance from the lozzie
center.
 1.0

o.a

a6

I a4 -•

cxx ••

U^C-id'^-^)

c - c
Figure 4. TiB2 inclusion removal efficeincy, n = _J; o , as a function
of tke melt approach velocity, Umo i
 3 -■

^ ■■

U(%)

U„ (Vc-)

Figure 5, In — as a function of the reciprocal of the melt approach

velocity, U .
 ao7--

0.0* ■•

o.os ■•

K.

aca ■•

0.01 ■•

aoi -■

Figure 6. Kinetic parameter, K , as a function of the melt approach

velocity, V^^.
 A
O.3S0 .

0,^00 ■ \
A \
A

0.2SO ■ • \

X CcV) \
0.Z0O -
\ A
^ A

O.ISO - ■ d
A
-^.^ A

0.100 - ■
A

0.05O — 11 t > 1

10 20 30 40 50 60 70 80

U.
'M
Mo"'-?)

K
figure 7. A, i.e. T^,asa function of the melt approach, velocity, Xl^.
U
m
 Figure 8. Depth of ceramic foam required to remove 63% of TiB2 inclusions,
A, as a function of the melt approach velocity, U^.

•
 (•i6'^-^)

Figure 9. Melt approach velocity, Uj^, as a function of time for the

long tenn filtration experiment, i denotes the time at which
an outlet sample was taken.
 a4 ..

as ..
At {5/C^)
AV
o.i ..

O.I •.

140C

VOLUME (cW), V

Figure 10. The reciprocal of the increment of filtrate volixme collected

over a period of time, AV/At, as a function of V, which is
(Vi + V2)/2 of each increment of filtrate volume.
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