An Improved Method for the Production of Metals and Alloys.
Year: 1896

page_text: Date of Application, 28th July, 1896
Complete Specification Left, 27th Apr., 1897-Accepted, 12th June. 1897
PROVISIONAL SPECIFICATION.
An Improved Method for the Production of Metals and Alloys.
I, CLAUDE VAUTIN, of 42 Old Broad Street, in the City of London, United
Kingdom of Great Britain, Metallurgist do hereby declare the nature of this
invention to be as follows:-
If metalline compounds, for instance oxides, sulphides, and chlorides, are heated
with aluminum the respective metal is separated; and if the aluminum has been
used in excess there is formed an alloy. If different metals are reduced at a time
there is obtained an alloy of these metals, and said method may, if desired, be
employed for the production of an alloy of a metal or metals with a metalloid or
metalloids. The aluminum must, however, be very finely pulverized, if the result
is to be a success, and when the mixture of the pulverized aluminum and the
compound to be reduced is heated up to the point of fusion there occurs a very
energic reaction. In consequence of the vehemence of the latter a certain quantity
of the material is thrown out of the crucible before the reduction is finished, and
that quantity, as well as the fuel consumed for heating the same, is lost for the
useful effect of the process.
The purpose of my invention is to overcome said loss, and I attain that object
by causing the reaction to set in not throughout the whole mass at a time, but only
at a point or place of the mass; in other words, I initiate the reaction at a certain
point or place of the mass, and cause it then to proceed from the respective portion:
of the mass to the other or main portion of the same.
Said initiating of the reaction may be performed, for instance, by igniting the.
mixture of pulverized aluminum and one or the other of the compounds afore.
mentioned (or, more precisely, a small portion of that mixture) by means of a blow-
flame directed against that portion, or by means of a piece of sheet magnesium
that is put into that portion, and is then ignited. 1 prefer, however, to make use
of a special igniting-mass for causing the initiating of the reaction, and I employ:
for that purpose mixtures of aluminum with such combinations or compounds that
generate a great heat on being reduced. Such combinations or compounds must,.
therefore, be easily reducible, aud I name as examples oxide of lead and baric.
peroxide, but similar oxides and peroxides may be used as well.
The igniting-mass may either be loosely strewn upon the material or mixture.to
be put in reaction, and may be ignited by a magnesium-band or by a match, or it
may be formed into balls or similar bodies by means of pressure or by aid of a
suitable cementing-medium, and a magnesium-band may then be put into each of
said balls. The latter are slightly pressed down upon, and into, the material or
mixture to be put in. reaction, and when ignited they transfer their own reaction
easily upon said material or mixture. The reaction of the latter may be caused to.
continue by adding fresh material to that contained in the crucible, and I prefer to
compress said fresh inaterial into the shape of cubes, prisms, and the like.
The aluminum may well be replaced by a mixture or an alloy of aluminum and
magnesium.
By making use of the improved method afore described I am enabled to produce.
refractory metals, such as chromium, manganese, and the like, in large quantities
and on a commercial scale; and I can produce also alloys of refractory metals, as

page_text: well as of a refractory metal with aluminum, and also of a refractory metal or
metals with an alkali-metal or metals, an earth alkali metal or metals, a rare earth
or earths, and so on.
CLAUDE VAUTIN,
By Cassell & Co.,
22 Glasshouse Street, Regent Street, London,
Agents for the Applicant.
An Improved Method for the Production of Metals
АПОУЗ.
I, CLAUDE VAUTIN, of 42, Old Broad Street City of London United
Kingdom of Great Britain Metallurgist do hereby declare the nature of this
invention, and in what manner the same is to be performed, to be particularly
described and ascertained in and by the following statement:--
If metallic compounds containing oxygen, sulphur, or chlorine, for instance
oxides, sulphides, and chlorides, are heated with aluminium, the metal of the
compound is separated out. When the aluminium is employed in excess an alloy
of aluminium and the metal of the compound is obtained. If different metals are
reduced at the same time an alloy of these metals is obtained. This method may
also be employed for the production of an alloy of a metal or metals with a
metalloid or with metalloids, as silicium, arsen and so on.
The aluminium should be employed in a finely pulverized state if good results
are to be obtained, and it is necessary to heat only a little portion of the whole
mixture to the temperature of reaction. After having brought this little portion
to reaction by the heat of a flame, of a burning piece of magnesium or by
electricity, the adjacent parts of the mixture are ignited successively and auto-
matically by the parts being already in reaction; by this method a very soft
reaction without explosions is gained.
When the whole mixture of the pulverized aluminium and the compound to be
reduced is heated to the point of fusion, by an exterior source of heat, such an
energetic reaction takes place, that by its vehemence a certain quantity of the
material is ejected and thrown out of the crucible before the reduction of the
compound is fully effected so that the said quantity of material and the fuel
consumed for heating the same are wasted as far as the operation is concerned.
Now it is the object of my invention to remedy this defect or loss and to this
end I cause, as already mentioned, the reaction, instead of taking place simul-
taneously throughout the whole mass, to take place at one point or place only of
the mass; in other words I initiate the reaction at a certain point or place in the
mass, and then cause it to proceed or spread from this portion of the mass to the
remaining portion of the same.
To start the reaction I may, for instance, ignite the mixture of pulverized
aluminium and of one or the other of the compounds above mentioned in a finely
pulverized state, (or, more precisely, a small portion of that mixture) by means of
a blow pipe-flame directed against it, or by means of a piece of sheet- or band-
magnesium which is inserted into that portion of the mixture and is then ignited.
I prefer, however, to make use of a special igniting-mass for starting the reaction,
such igniting mass being composed of a similar mixture to that to be treated but
which generates greater heat and gives rise to a more intense reaction on being
reduced. The combination or compound forming the mixture must, therefore, be
easily reducible, and I may mention as examples of such a mixture oxide of lead

page_text: and baric peroxide with aluminium, but other similar oxides and peroxides may be
used, if desired, in combination with aluminium.
The igniting mass may either be loosely strewn upon the material or mixture to
be treated, and may be ignited by a magnesium-band or by a match, or it may be
formed into balls or similar bodies by pressure, or by means of a suitable cement,
and a magnesium-band may then be put into each of the said balls or bodies.
The latter are slightly pressed down upon, and into, the material or mixture to be
treated and when ignited they start the reaction of the said material or mixture.
The reaction may be continued by adding fresh material to that contained in the
crucible, and I prefer to press the said fresh material into the shape of cubes,
prisms and the like.
The aluminium may be replaced by a mixture or an alloy of aluminium and
magnesium.
By making use of the improved method above described I am enabled to produce
refractory metals, such as chromium, manganese, and the like, in large quantities
and on a commercial scale; and I can also produce alloys of refractory metals, as
well as of a refractory metal with aluminium, and also of a refractory metal or
metals with an alkali metal or metals, with a metal or metals of the alkaline earths,
with the metals of a rare earth or earths, and so on.
The metals are gained perfectly free from carbon, silicium and other impurities
and that is a great advantage of this method.
In the following examples I give all the necessary details in executing my
method.
To gain the metal of chromium I mix for example equivalent parts of the oxide
of chromium (Cr,O,) with aluminium (Al,). The inixture is brought into a
crucible provided at the inside with a cover of magnesia (MgO) which is spread
in a moist state on the inside of the crucible and afterwards dried in the usual
manner.
Upon the mixture in the crucible is then laid a little cartridge consisting of a
ball of half an inch diameter.. The cartridge is composed of equivalent parts of
finely powdered peroxide of barium and aluminium, intimately mixed and
compressed to a solid body. To this body is fixed a thin piece of magnesium.
The whole arrangement of the apparatus is shown in cross-section in the
accompanying drawing.
I ignite the piece of magnesium in the well-known manner and when burning
down it ignites the cartridge and by the aluminium contained in it the reduction of
the peroxide of barium takes place. By this reaction a sufficient heat is produced,
so that successively the igniting of the whole mass takes place. Of course, I may
add new masses to the burning mixture and the transferring of the reaction will
take place in the same manner to the added masses.
The reaction is as follows:
Al, Cr,O, A₁₂O3 + Cг.
=
Bo,O 3 Cu,O + 2 Al, = 2 Al₂O, + Bo₂ + 3 Cu₂.

page_text: The importance of my novel method and the particular effect of the same
becomes best obvious from the fact that the metal or alloy is not obtained in small
particles that are distributed through the mass resulting from the reaction, but the
by far greatest part of the metal or alloy is gained as a distinct or separate body, i.e.
a compact regulus.
Having now particularly described and ascertained the nature of my said inven-
tion, and in what manner the same is to be performed, I declare that what I
.claim is :-
1. The method of producing metals from metallic compounds containing oxygen,
sulphur or chlorine alone, or two of, or all these substances, by the reducing action
of aluminium, such method consisting in heating a small portion of a mixture
of aluminium with the metallic compound to the temperature of reaction and
transferring this temperature and reaction successively and automatically to the
adjacent parts of the mixture and thus igniting the whole mass by the parts being
already in reaction, as set forth.
2. The method of producing alloys from metallic compounds containing oxygen,
sulphur or chlorine, aloue or two of or all these substances, by the reducing action
of aluminium, such method consisting in heating a small portion of a mixture
of aluminium with the metallic compound to the temperature of reaction and
transferring this temperature and reaction successively and automatically to the
adjacent parts of the mixture and thus igniting the whole mass by the parts being
already in reaction, as set forth.
3. The method of producing metals from metallic compounds containing oxygen,
sulphur or chlorine alone, or two of or all these substances, by the reducing action
of aluminium, such method consisting in heating a small portion of a mixture of
aluminium and magnesium to the temperature of reaction and transferring this.
temperature and reaction successively and automatically to the adjacent parts of
the mixture and thus igniting the whole mass by the parts being already in
reaction, as set forth.
4. The method of producing alloys from metallic compounds containing oxygen,
sulphur or chlorine alone, or two of or all these substances, by the reducing action
of aluminium, such method consisting in heating a small portion of a mixture of
aluminium and magnesium to the temperature of reaction and transferring this
temperature and reaction successively and automatically to the adjacent parts of
the mixture and thus igniting the whole mass by the parts being already in reaction,
as set forth.
5. The method of producing metals from metallic compounds containing oxygen,
sulphur or chlorine alone, or two of or all these substances by the reducing action of
aluminium, such method consisting in heating a small portion of a mixture of
aluminium with the metallic compound in a finely powdered state to the temperature
of reaction and transferring this temperature and reaction successively and
automatically to the adjacent parts of the mixture and thus igniting the whole mass
by the parts being already in reaction, as set forth.
6. The method of producing alloys from metallic compounds containing oxygen,
sulphur or chlorine alone, or two of or all these substances by the reducing action
of aluminium, such method consisting in heating a small portion of a mixture of
aluminium with the metallic compound in a finely powdered state to the temperature
of reaction and transferring this temperature and reaction successively and
automatically to the adjacent parts of the mixture and thus igniting the whole mass
by the parts being already in reaction, as set forth.
7. The method of producing metals from metallic compounds containing oxygen,
sulphur or chlorine alone, or two of or all these substances, by the reducing action
of aluminium, such method consisting in heating a small portion of a mixture of
aluminium, or aluminium and magnesium with the metallic compound in a finely
powdered state, to the temperature of reaction and transferring this temperature
and reaction successively and automatically to the adjacent parts of the mixture

page_text: and thus igniting the whole mass by the parts being already in reaction, as-
set forth.
8. The method of producing alloys from metallic compounds containing oxygen,.
sulphur or chlorine alone, or two of or all these substances, by the reducing action:
of aluminium, such method consisting in heating a small portion of a mixture of
aluminium, or aluminium and magnesium with the metallic compound in a finely
powdered state, to the temperature of reaction and transferring this temperature
and reaction successively and automatically to the adjacent parts of the mixture
and thus igniting the whole mass by the parts being already in reaction, as.
set forth.
9. The described method of producing metals and alloys from metallic compoun Is.
containing oxygen, sulphur or chlorine alone, or two of or all; such method
consisting in finely pulverizing the compound, mixing it with finely pulverized.
metallic aluminium or aluminium and magnesium, heating a small portion of the
mixture to start its reaction and afterwards adding the remaining or main portion,
Eo as to heat it from the heat of reaction of the first portior, whereby the reaction.
automatically spreads throughout the whole mass, substantially as set forth.
10. The described method of producing metals and alloys from metallic compounds-
containing oxygen, sulphur or chlorine alone, or two of or all; such method.
consisting in finely pulverizing the compound, mixing it with finely pulverized.
metallic aluminium or aluminium and magnesium, covering a small portion of the
said mixture with a small portion of a mixture similar to the first mixture, but
coming more easily in reaction; and heating the added mixture so as to start its-
reaction which then spreads to the main portion of the first mixture, being:
maintained by the heat developed by the initial reaction, as set forth.
DocL 1... SA11007
CLAUDE
VAUTIN,
By Cassell & Co,
Agents for the Applicant..