US1248648A - Alloy and process of producing the same. - Google Patents

Description

JES 1B. GRENAGLE, 0F CATONSVILLJE, MARYLAND.

ALLUY nine.

Ito Drawing.

prises as a new article an alloy comprising zirconium and iron, said alloy containing advantageously between and 90 per cent. of zirconium with the residue mainly iron, or an iron group metal, and said alloy also advantageously comprising a certain amount of titanium and also comprising in certain cases a small amount of aluminum or other metal; and it also comprises a filament or other luminescent body composed of said al- 10y and it further comprises a method of producing such alloys wherein zirconium and iron compounds are co-reduced in the presence' of sufiicient titanium compounds to produce certain advantageous efiects and to insure the entry of 'asmall amount of metallic titanium into the alloy produced; all as more fully hereinafter set forth and as claimed.

Numerous attempts have been made to obtain alloys of zirconium which could be worked up into forms commercially useful,

but such attempts have been heretofore largely unsuccessful. Zirconium itself is a hard, brittle substance existing in several allotropic forms, all of which are easlly fractured and possess little or no ductillity or malleability. These properties have also characterized practically all the alloys or metal mixtures heretofore produced in which zirconium was present in more than comparatively small proportions. Moreover it' has been found extremely dificult to alloy zirconium with other metals by direct addition of the one metal to the other with production of uniform and homogeneous ductile and malleable alloyed products;

products which are susceptible of being treated by metal-working processes such as drawing, forging, rolling, casting and the like. The physical and chemical properties of these dlrectly produced alloys prevent such manipulation.

Accordin to the present invention true alloys of zirconiumwith .iron, or another Specification oi Letters Patent.

\ PROCESS OF PRODUCING THE SE.

]Patented Dec. d, it 5..

Application filed December 7, 1915. Serial Ito. 55,555.

metal of the iron family, are produced by the simultaneous reduction of the constituent metals from compounds containing them. Under these conditions the zirconium and the iron group metals readily unite .to form homogeneous alloys of varying composltlon depending upon the relativequantities of the materials employed and the conditionsof reduction. The alloys thus produced are of a type hitherto unknown among metalhc zlrconium combinations- They exhibit practically no tendency to oxidize and are highly resistant to most chemical reagents. In appearance they are truly metalllc, and they can be produced in compact bodies which upon grinding and polishing, exhibit bright metallic surfaces of a silvery steel-like luster. Alloys may be produced'which are tough and are malleable They possess a remarkably high degree of luminescence at relatively low filament tem-- peratures andare thus very efficient sources of light. While other metals of the iron group than iron itself, such as nickel, cobalt,- or manganese, or alloys or mixtures thereof, are capable of use in the present invention, they are not in practice as desirable as iron. For the present purposes, iron is by far the most satisfactory metal of the iron group.- The relative proportions of iron and zirconium in alloys under the present invention may vary widely. For most purposes it is desirable to have proportions w ich will give alloys which are malleable and ductile, or have good tensile strength. For binary zirconium-iron alloys, the proportion of zirconium should not fall much below, say 40 per cent. or thereabout, since with lower percentages of this metal the advantageous properties of the alloys are not suiiiciently in evidence. ,Higher percentages of zirconium in such binary alloys are still more desirable for various reasons; and the alloys of from approximately 60 to 90 per cent.- zirconium content with to 10 per cent. of iron are particularly advantageous.

The excellence of these zirconium alloys may be considerably enhanced and many desirable properties attained by the inclusion of a small amount of titanium in the alloy, either by co-reduction of titanium with the other constituents, or by separate addition of titanium to a preformed alloy. The allowable amount of titanium so present is not rigidly restricted, but very small quantities prove efiicacious in practice. As little as 0.10 per cent. serves the present purpose in some instances, and it is seldom necessary in alloys for most purposes that the titanium content shall exceed 2 or 3 per cent. These small amounts of titanium give enhanced strength and toughness to the zirconium alloys, and also increase their electrical properties. The ductility and malleability are also more pronounced. Furthermore in the manufacture of these alloys by co-reduction of the component metals, the presence of the titanium compounds in the mixture reduced has a useful effect in preventing the undesirable retention of oxygen and oxygen compounds in the alloy or resultant melt. The presence of titanium also operates to exclude nitrogen, carbon and other metalloids from the alloy produced. Oxygen and other metalloids have an undesirable effect on malleability, ductility and texture. Ternary alloys containing a certain amount of titanium with preponderating proportions of zirconium and iron have certain decided advantages over the simple binary alloys for many purposes. Finally, the addition of small amounts of other metals such as aluminum, tantalum, columbium, (niobium), etc., give quaternary and still more complex zirconium-iron alloys which for some purposes ofi'er particular advantages and in them the relative proportions of zirconium and iron may often, with advantage, vary more widely than in the simple binary zirconium iron alloys. It is to be understood, however, that in all these alloys under the present invention the combined zirconium iron content preponderates over the other metals. Typical analyses of quaternary alloys of the present invention comprising zirconium, iron, titanium, and aluminum are as follows: zirconium 65.78%, 8.43%, 32.97%, iron 26.39%, 90.97%, 49.21%, titanium, 0.12%, 0.13%, 0.42%, aluminum 7.71%, 0.47%, 17.40%.

The described alloys are substantially iron-zirconium alloys, other metals forming a minor fraction. And, for practical purposes, these alloys may be looked upon as zirconium alloyed with iron or its equivalent, an iron-rich ferrous alloy.

The process of making the described alloys under the present invention is one of coreduction of compounds containing zirconium and iron in such a manner that the two metals are presented to each other in a nascent reactive condition. It is best that this reduction occur in the presence of a titaniferous compound, since as before stated, the inclusion of a small ercentage of titanium in the alloy prod iiced is especially valuable and the presence of titanium during the reduction is desirable for the other reasons stated. A convenient method, especially where it is desired to have aluminum present in the alloy, as is often the case, is to reduce mixed oxids of iron and zirconium by means of finely divided aluminum, the reaction being started With any firing means or materials such as magnesium, barium oxids, etc. In making an alloy of iron and zirconium containin about 44.7 per cent. zirconium the following equation may serve to represent the reaction of reduction by aluminum:

The process of reduction may also be carried out by suitably heating the mixed oxids in a graphite crucible as b means of the oxyacetylene flame, or electrlcally. Or, a mixture of titaniferous oxid of iron, and the mineral zircon, or other zirconium-containing materials, such as zirconia together with suitable amounts of titaniferous minerals such as rutile, ilmenite, sphene, titanic oxid, etc., may be heated as before described. Fluxes and slag forming bodies such as silica, soda, etc., may be employed. The mineral ilmenite is a source of titanium convenient to employ in the present process.

. The alloys thus produced may be mechanically Worked in any suitable way. In making filaments, the alloys, in the form of rods, produced by casting or by otherwise suitably shaping the alloys produced as above described may be heated to the necessary temperature, rolled, drawn, swaged or extruded through dies to size, the alloy rod being conveniently heated by passage of a current therethrough during drawing. With many of the present alloys no special precautions need be taken to avoid oxidation during working, but where necessary or desirable, working may be carried on in vacuo or in an inert atmosphere.

In addition to their utility for incandescent lamp filaments and for glowers, alloys under the present invention may be usefully employed in forming arcs. As stated, the present materials give out more light than is equivalent to their temperature. Being resistant to acids and corrosion, the alloys may be used for various shaped articles for ornamental and other purposes, such as s ark points, etc. Another field of utility for t ese alloys is in the manufacture of transformer elements.

was,

Halogen compounds, such as fluorids, chlorids, etc. of the Various metals may be used in maklng the alloys by co-reduction; but their use ofiers no advantage over the oxidized compounds of the metals as described.

What I claim is 1. As a new article, an alloy comprising not less than about 40 per cent. and not more than about 90 per cent. zirconium together with an iron group metal.

2. As a new article, an alloy comprising not less than about 40 per cent. and not more than about 90 per cent. zirconium together with iron. I

3. As a new article, an alloy comprising approximately between 60 and 90 per cent.

zirconium together with van iron group metal.

4. As a new article, an alloy comprising approximately between 60 and 90 per cent.

- zirconium together with iron.

5. An alloy comprising between 60 and 90 per cent. zirconium, the residue of said alloy being mainly iron, and said alloy being substantially free of oxygen, oxids and metalloids and being malleable and ductile.

6. The process of making an alloy comprising iron and zirconium which comprises admixing materials containing compounds of iron and of zirconium and co-reducing the metals from the mixture as an alloy.

7. llhe process of making an alloy comprising iron and zirconium which comprises admixing materials containing compounds of iron, of zirconium and of titanium and coreducing the metals from the mixture as an alloy.

8. The process of making an alloy comprising iron and zirconium which comprises admixing materials containing compounds of iron and of zirconium with metallic aluminum and igniting the mixture.

In testimon whereof, I afiix my signature in presence 0 two witnesses.

JAMES B. GRENAGLE.

Witnesses:

F. L. MIDDLETON, BENNETT S. Jones.