the terminating lamella a s elsewhere on the i n t e r f a c e l e a d s to Eq. [7].

REFERENCES
'R. F. Mehl and W. C. Hagel: Prog. Metal Phys., 1956, vol. 6, pp.

'W. H. Brandt: AlME Trans., 1946, vol. 167, p. 405; J . A p p l . Phys., 1945, vol. 16, p. 139. 'J. Scheil: 2. Metallk., 1946, vol. 37, p. 123. 'M. Hillert: Jernkontorets Ann., 1960, vol. 144, p. 520. 'C. Zener: AlME Trans., 1946, vol. 167, p. 550. 6K.A. Jackson and B. Chalmers: to be published.

74-134.

Filtering and Fluxing Processes for Aluminum Alloys

K. J. Brondyke and P. D. Hess
Two processes have been developed for improving the quality of molten -aluminum allovs before casting. The Filtration Process. which involves passing molten metal through a packed bed of granular filter material, is a rapid menns of r e moving finelv divided pnrticles. It has the most potential in those instances where removal of inclusions is of primnry importance. The Combination Filtration -Inert Gas Fluxing Process in uolzles introduction of an inert gas so that it will diffuse countercurrent to metal flow through the filter bed of gvanular material. Dissolved hydrogen i s removed from the metal in addition to removal of finelv dzvided particles. The Combination Process i s most useful where both inclusion removal and attainment of cotuistently low -hydrogen -content metal are important. Metal treated by the Combination Process is of higher and more uniform quality than heretofore attainable with prolmged chlorine fluxing. Costs of the Combination Process can, for the most part, be offset bv sacings derived from high recoveries and increased production of superior -quality products
The development of ultrasonics f o r m e a s u r e m e n t of internal quality, tightening of quality controls, and the application of the aluminum alloys t o new o r different c o m m e r c i a l fields have been responsible f o r an e v e r increasing demand for improvement of quality of both c a s t and fabricated products. T h i s demand f o r high quality has not been r e s t r i c t e d to any single type of product. On the contrary, the demand encompasses about the e n t i r e variety of products including those for fabrication, those to be machined, buffed, o r finished f o r decorative purposes, and those f o r c r i t i c a l applications where both s u r f a c e and internal quality is of utmost importance. In many instances products acceptable in the 40's would now be scrapped a s unacceptable by these higher present-day standards. With t h i s e v e r increasing demand for higher quality, i t became apparent a t Alcoa that conventional means of melt treatment w e r e inadequate in many instances and new approaches w e r e n e c e s s a r y . Consequently the r e s e a r c h program w a s intensified with attention focused on metal treatment d u r ing t r a n s f e r in o r d e r to r e d u c e the furnace processing t i m e to a minimum in a n effort to attain the d e s i r e d r e s u l t s a t a minimum of additional expense. As a r e s u l t of this intensive r e s e a r c h program which covered numerous variations and adaptations of conventional methods in addition to new methods of melt treatment, s e v e r a l new p r o c e s s e s w e r e developed, two of which will b e described h e r e . The f i r s t of these, a method of melt filtration, was patented in February, 1959.l The second p r o c e s s involving combination filtration-inert g a s fluxing w a s patented in June, 1 9 6 ~ Other melt-treatment .~ p r o c e s s e s developed during t h i s period of investigation w e r e patented as l i ~ t e d . ~ FILTRATION PROCESS General Description. The Filtration P r o c e s s , which involves passing molten metal through a packed bed of g r a n u l a r f i l t e r m a t e r i a l , i s a rapid method of effectively removing finely divided p a r ticles. It i s an impingement-type f i l t e r ; hence the s i z e of the p a r t i c l e s removed f r o m the metal a r e considerably s m a l l e r than the i n t e r s t i c e s of the
VOLUME 230, DECEMBER 1964-1553

in the quality of molten-aluminum alloys i s s e c u r e d generally through the u s e of s o m e fluxing practice in a crucible, holding furnace, o r ladle involving e i t h e r gaseous o r solid fluxing media. Typical fluxing agents may include the g a s e s nitrogen, argon, o r chlorine used either singly o r a s mixtures and the solids aluminum chloride o r hexachloroethane. R e g a r d l e s s of the fluxing m e a n s used, the p r i m a r y objectives a r e the adequate removal of both metallic and nonmetallic inclusions and reduction of hydrogen content to an acceptably low level. The ultimate goal i s to produce ingots and c a s t products of high quality f r e e f r o m inclusions and porosity.
K. J. BRONDYKE, Member AIME, and P. D. HESS are v Assistant Chief and Research Enaineer, r e s ~ e c t i v e,l . .Fabricating Metallurgy Division, ~ l c o a e i e a r i h ~ Laboratories, Aluminum Co. of America, New Kensington, Pa. Manuscript submitted January 21, 1964. EMD TRANSACTIONS OF THE METALLURGICAL SOCIETY OF AlME

IMPROVEMENT

bed. The unit is normally placed in a t r a n s f e r system s o that the metal is treated just p r i o r t o casting. The filter unit consists essentially of a heated r e f r a c t o r y container equipped with a vertical baffle to direct the metal through the bed of granular filt e r material. The baffle is offset s o that the inlet side housing the filter bed is l a r g e r than the outlet. The filter unit illustrated in Fig. 1 r e p r e s e n t s a type commonly used in a t r a n s f e r system f r o m furnace to casting station. This design, in which the filter bed is continually submerged by the metal, p e r m i t s either continuous o r intermittent operation without impairing either efficiency of filtration o r flow capacity. Complete submersion of the bed is essential to the attainment of d e s i r e d results. The unit is normally maintained a t a temperature slightly higher than casting temperature. The granular bed of the filter may be made up of any r e f r a c t o r y of high melting point, i n e r t to molten aluminum with a specific gravity g r e a t e r than molten aluminum s o the granules will sink to the bottom, and of sufficient hardness s o a s to p r e vent powdering during use. Of the r e f r a c t o r i e s possessing these qualities, Tabular Alumina (synthetic corundum) i s preferred. The refractoryparticle sizing may be in the range of - 3 + 14 mesh U.S. Standard. The depth of the filter bed may v a r y f r o m a minimum of 6 in. to any maximum practically convenient. Since filtration o c c u r s in depth, the flow capacity of this filtration p r o c e s s is not affected to the extent associated with r e f r a c t o r y plate-type f i l t e r s o r s c r e e n s where filtration o c c u r s principally on the leading surface. As shown in Fig. 1, the f i l t e r bed i s supported on a layer of Tabular Alumina balls. The latter s e r v e s both a s a plenum chamber t o provide uniform metal flow through the bed and a s a b a r r i e r against washing r e f r a c t o r y particles into the t r a n s f e r system and ultimately into the castings. Metal flow through the unit i s related to an overflow principle in which flow r a t e is a function of f i l t e r c r o s s section and metal head (the difference

,lNiET

TIIOUGU

PUTLET

TROUGH

i;

Fig. 1 -Filtration-process

unit with off-set baffle.

in metal level a s measured on the inlet and outlet sides of the baffle). With a 5-in. metal head, a filter bed of 8 in. depth is capable of passing 200 l b of metal per h r p e r sq in. of filter a r e a normal to metal flow. Capacities a t g r e a t e r depths of filter bed a r e correspondingly l e s s . During prolonged operation, the filter bed will become clogged progressively by inclusions removed; consequently metal flow r a t e will d e c r e a s e if the metal head is kept constant. Installations a r e therefore designed with e x c e s s capacity and with provision for ample variation in metal head a s required. Results. No methods a r e available f o r auantitative d i r e c t measurements of either the number o r size of inclusions in molten-aluminum alloys. Because of the problem of taking a representative sample, there is no reliable method for oxide determination applicable to the low concentrations normally encountered in aluminum melting. Consequently, the effectiveness of the filtration proc e s s h a s been established by plant and laboratory evaluations of machining and tool-wear t e s t s . In each evaluation the filtration p r o c e s s w a s compared to the standard method of melt treatment normally used. In the casting field, machining-test evaluations included determination of number of visible d r o s s inclusions, determination of incidence of hard spots, tool life, and tool wear based on radioactive measurements. Since in most instances the castings a r e machined only by the customer, machining t e s t s w e r e devised using spectrographic disk samples c a s t f r o m the molten-aluminum alloy to represent melt quality. Visual examination of machined surfaces showed a decreased incidence of inclusions in metal treated by the Filtration P r o c e s s . Typical r e s u l t s a r e shown in Table I . This beneficial effect of filtration was a l s o observed in examinations for d r o s s inclusions and hard spots of those castings roughly machined in our plants. Coincident with these r e s u l t s was a n improvement in the life of the lathe tool used in these rough-machining operations. Radioactive tool-wear t e s t s on die castings showed a 50 pct d e c r e a s e in tool wear when machining castings which had been poured f r o m filtered metal. Coincident with the r e s u l t s of these evaluations, a substantial improvement by filtration was observed in densities of vacuum g a s t e s t samples taken f r o m the molten metal. Regardless of the density of the vacuum g a s t e s t sample of the untreated metal, densities of vacuum g a s test s a m ples after filtration approached the theoretical density of the alloy sampled when the hydrogen content was sufficiently low. In spite of these inc r e a s e s in density, there was no evidence of measurable hydrogen removal by the Filtration a s ~ P r o c e s s using either the ~ e l e ~ instrument o r the solid-extraction method5 for hydrogen determinations. Since hydrogen was not removed by f i l tration, it is now concluded that the increased
TRANSACTIONS OF THE METALLURGICAL SOCIETY OF AlME

1554-VOLUME 230, DECEMBER 1964

densities of the vacuum g a s test samples were indicative of efficient removal of inclusions which serve a s nuclei for bubble formation during solidification. This phase of the subject i s described in detail in our companion paper entitled "Interpretation of Vacuum Gas Test Results for Aluminum ~llo~s".~ COMBINATION FILTRATION-INERT FLUXING PROCESS GAS

Table I. Inclusions in Spectrographic Disc Samples

Test No. Sample Source Gas-fired crucible furnace Gas-fired crucible furnace Gas-fired crucible furnace Ingot Molten metal Filtered molten metal Unfiltered molten metal Filtered molten metal Metal Charge Incidence of Inclusions, Pct

4.1
18.5

General Description. The Combination FiltrationInert Gas Fluxing Process provides a rapid method both for removing inclusions and for reducing hydrogen content. Since hydrogen i s the only g a s appreciably soluble in aluminum, other gases a r e not considered in the discussion in this paper. The importance of attaining low concentrations of hydrogen in aluminum alloys lies in the drastic difference in hydrogen solubility between the liquid and the solid metal at the freezing temperature. Because of this reduced solubility a t the freezing point, there is rapid precipitation of the gas during solidification with the result that gas porosity often forms in the cast metal. Voids thus formed become discontinuities upon subsequent fabrication a s the g a s press u r e s developed prevent healing. In castings the voids a r e undesirable from the standpoint of potential leakers, reduced available c r o s s section, lower strengths, and s o forth. The basic unit of the Combination P r o c e s s i s identical to that described for the Filtration Proc e s s . However, in the Combination Process, provision i s also made to introduce the i n e r t gas so that it will pass countercurrent to metal flow. Dissolved atomic hydrogen in the aluminum diff u s e s into the inert gas and i s thus removed. Tabular Alumina i s preferred for the filter-bed material a s in the Filtration P r o c e s s . In the Combination Process, the inert gas passes upwardly through the filter bed on the inlet side. Argon i s preferred a s the fluxing gas a s it i s substantially inert to aluminum. However, nitrogen may also be employed in the treatment of those aluminum-base alloys where nitride formation can be tolerated. The efficiency of hydrogen removal i s comparable to that when using argon. Chlorine i s unsuitable because of chloride formation with a tendency toward rapid clogging of the filter bed. The procedure for charging the unit of the Combination P r o c e s s is similar to that for the Filtration Process, except that the diffuser for introducing the inert gas should also be placed in position. Because of the countercurrent flow of the inert fluxing gas, metal flow capacity o the Combination f unit is not a s great a s f o r a Filtration unit of the same size. Results. The lack of quantitative methods for determination of filtration efficiencies discussed for the Filtration P r o c e s s also applied to the Combination Filtration-Inert Gas Fluxing Process. Efficiencies of hydrogen reduction, however, were
TRANSACTIONS O F THE METALLURGICAL SOCIETY O F AlME

I1

Reverberatory holding furnace Reverberatory holding furnace

0.0

determined by measurements using both the Telegas and solid-extraction method of determining absolute hydrogen contents. Vacuum gas test samples were also taken to determine relative gas content and indicate melt cleanliness. These tests were supplemented by dye-penetrant examinations and ultrasonic tests of both ingots and forgings. Material for forging stock and forgings was selected for these evaluations, a s quality requirements for these products a r e high and metal of low hydrogen content i s desired. The effectiveness of the Combination P r o c e s s on melt quality was established by a comparison of samples taken both before and after the unit in the metal-transfer system. Since there was interest in either reducing furnace fluxing time in some instances, or altogether eliminating furnace fluxing with chlorine in others, numerous evaluations were made to determine the effectiveness of the process either with o r without prior chlorine fluxing. In each instance results of the evaluations were compared with those of the then existing practices involving only furnace fluxing with chlorine. The improvement in densities of vacuum gas test samples produced by the use of the Combination Process was, in all cases, equivalent to or better than that attained by long-time chlorine fluxing. Because of the simultaneous removal of both hydrogen and inclusions, the densities of vacuum gas t e s t samples were consistently high, always approaching the theoretical density of the alloy under test. Hydrogen removal by the Combination Process i s dependent on metal flow rate, inert-gas flow rate, and the hydrogen content of the incoming metal. As in any gas-removal process, increased inert-gas flow r a t e s a r e necessary either when operating with increased metal flow r a t e s o r when treating metal of higher hydrogen contents. Under proper operating conditions, hydrogen contents after the Combination Process a r e in the proximity of 0.1 ml per 100 g. Hydrogen reductions typical of the Combination Process under plant conditions a r e given in Table II. One will observe that the same low final hydrogen content was attained regardless of initial hydrogen content or metal flow rate. I t appears that the only
VOLUME 230, DECEMBER 1964-1555

-~

-.

-~

Table II. Typical Hydrogen Reduction with Combination Filtration-Inert Gas Fluxing Process
. -

Alloy

Metal Flow, l b per hr

-

Argon Flow, (CFH) 40 40 50 50 130 280 40 40 165 50

~

Hydrogen, ml per 100 g t Before 0.16 0.18 0.21 0.24 0.41 0.33 0.29 0.28 0.25 0.34 After 0.08 0.09 0.12 0.12 0.12 0.08 0.10 0.14 0.07 0.13

Hydrogen Reduction, Pct 50 50 43 50 71 76 66 50 72 65

2014 2014 6061 6061 6061 6061 7075 7075 7075 7079

3,700 4,200 4,150 8,300 8,300* 28,000* 3,600* 6,200* 38,000 6,200

'No prior C1, flux. + ~ ~ d r o determinations - by T e l e g a s instrument described in ~ e n

8ElORC .,,ER COYBlNlTON conslNnrlow PROCESS PROCE55

J.

Inst. Metals, 1938, vol. 86, pp. 212-19.

"
\

2 2

, [7
2

CII

L R L . PO14 A L L O Y - 3 1 0 0 NO C1? FURNACL FLUX

Le5 < H e

m
L-

m L

W -

,
CII

[IID C L E V E L I N D

C L ~ V ~ L A H WORK5 - X2214 D ALL^^ ! P O 0 0 1 8 5 ,nP, NO C12 FURNACL F L U X

WORK5 - 7 0 7 9 A L L ~ y 3 9 0 0 L B S IHR, P R l O R CI2 F U R N I C E FLU*

%
m C
W

2 4

0 4

0
2 5

Q ,

m
0 u

O 3

t
W

5
3
0

2.6

5
u 0 z
W 0

0.2

s a m p l e s and hydrogen determinations, was reflected in examination of ingots and fabricated products produced therefrom. In each evaluation, these ingots exhibited increased soundness, with isolated inclusions virtually absent. This improved quality resulted in fewer rejections by ultrasonic inspection a t the ingot stage, during fabrication, and a t final inspection. This reduction in rejections r e sulting f r o m the improved ingot quality h a s been realized in fabricated products in the fields of forging, rolling, and extrusion. SUMMARY

7
E

2 7

0.1

0
~3

LT
2.8
I

0
1 2

Cu

F
0
I

Fig. 2-Average hydrogen and vacuum gas test density improvement with Combination Filtration-Inert Gas Fluxing P r o c e s s .

restriction to the minimum hydrogen content attainable by the Combination P r o c e s s is one related to environmental conditions prevailing a t the time of operation. The ability to f u r t h e r reduce hydrogen content when the Combination P r o c e s s supplemented chlorine furnace fluxing was duplicated in every evaluation r e g a r d l e s s of alloy. Data illustrating this effect a r e depicted in Fig. 2, a b a r graph of a v e r age vacuum g a s t e s t densities and hydrogen contents of metal processed a t the Laboratories and a t Alcoa's Cleveland Works. F r o m this graph and Table I1 i t is apparent that the Combination P r o c e s s will produce: 1) high final densities of vacuum g a s t e s t s a m ples r e g a r d l e s s of whether the metal is previously chlorine fluxed; 2) s i m i l a r final hydrogen contents over a wide range of metal flow r a t e s ; 3) lower hydrogen contents than metal fluxed in the furnace; 4) substantial additional reduction in the hydrogen content of metal fluxed in the furnace. The improvement in melt quality by the Combination P r o c e s s , as measured by vacuum g a s t e s t
1556-VOLUME 230, DECEMBER 1964

Improved metal quality can be attained by use of either the Filtration P r o c e s s o r the Combination Filtration-Inert G a s Fluxing P r o c e s s . The F i l t r a tion P r o c e s s has the most potential i n those instances where removal of inclusions is of p r i m a r y importance. The combination P r o c e s s is most useful where both inclusion removal and attainment of consistently low-hydrogen-content metal a r e important. Material treated by the Combination P r o c e s s is of a higher and m o r e uniform quality than heretofore attainable with prolonged chlorine fluxing. C o s t s of the Combination P r o c e s s can, f o r the most p a r t , b e offset by savings derived f r o m high r e c o v e r i e s and increased production of superior-quality products. Use of the p r o c e s s e s h a s improved the internal integrity of Alcoa products. This i s especially significant by today's standards with the demand f o r maximum reliability of equipment f o r both defense and commercial applications. REFERENCES
'U.S. Patent No. 2,863,558. 'U.S. Patent No. 3,039.864. '~Ju.. patents N o s . 2,840,463 and 3,006,473. . 'C. E. Ranslev.. D. E. 1 Talbot, and H. C. Barlow: .I. Inst. Metals, . 1958, vol. 86, part 5. '1. L. Brandt and C. N. Cochran: .I. Metals, 1956, vol. 8, no. 12, pp. 16762-74. K. J . Brondyke and P . D. H e s s : S e e companion paper T r o n s . Met. Soc. AIME, 1964, vol. 230. pp. 1542-46.

TRANSACTIONS O F THE METALLURGICAL SOCIETY O F A I M E