Obtaining Titanium

Developing your Web presence: On Titanium, Thermite, the Bronze Age and... Drywall!
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Developing your Web presence

The exercise of power is determined by thousands of interactions between the world of the powerful and that of
the powerless, all the more so because these worlds are never divided by a sharp line: everyone has a small part
of himself in both - Vaclav Havel
SUNDAY, OCTOBER 19, 2008 About Me
On Titanium, Thermite, the Bronze Age and... Name:

Drywall! Gert
Location:
Yorkshire, United Kingdom
The process for extracting metals from their ores dates back to the
Bronze Age. Despite many modifications, the Bronze Age method to
A chemical enthusiast serving the
extract copper and tin from their oxides, is basically still in use today for
chem and pyro community with
chemicals, professionally,
the mass-production of a wide variety of metals and alloys. In the step-
competitively and courteously...
by-step guide below I describe a method that allows to extract metallic
titanium from white pigment, in your own backyard and using over-the- View my complete profile
counter materials! Where does the drywall come into it? Read on! And it
works too, I've made nuggets of titanium in this way many times before.
Previous Posts
Homemade Titanium Metal from OTC materials in a Thermite
Response to 9/11 was 'huge
Reaction:
overreaction' - ex-MI5 ...
Why Pat Condell is an obnoxious
One of the most used
idiot
methods of extracting
metals from their ores Troopergate: the full timeline
(usually oxides) is the Palin's McMob: the Ohio vids...
chemical reduction of these
Cleese on Horn Shammity
oxides by means of a
Olmert: Israel must hand back
reducing agent, often carbon
land for peace with ...
or another metal. This
principle has been put to
I'm in love with Naomi Klein...
industrial use basically since Econo-comic relief with Red State
the Bronze Age. Among Update...
these pyrometallurgical McCain's debate ploy
reductions, as they are
McCain: Make Health Care more
known in chemical
like Banking
metallurgy, reductions with aluminium, referred to as aluminothermy,
occupy a prominent class. Best known among these is what is colloquially
referred to as Thermite reactions. The term Thermite (etymologically
probably a contraction between thermal and dynamite, on account of the
almost violent generation of lots and lots of heat during the process)
actually originally specifically refers to the reaction of iron oxide with
aluminium powder during which liquid iron and liquid alumina (aluminium
http://developing-your-web-presence.blogspot.ro/2008/10/on-titanium-thermite-bronze-ag... 10-Sep-16
Developing your Web presence: On Titanium, Thermite, the Bronze Age and... Drywall! Page 2 of 24
oxide) are formed in a most spectacular fashion (see the many interesting
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Iron oxide + Aluminium ---> liquid Iron + liquid Aluminium Oxide
(Alumina)
The convenient fact that both reaction products are generated in the
molten state (thus allowing to obtain lump metal or even castings) is due
to the fact that the reaction is accompanied by massive heat generation,
sufficient to heat the reaction products to well above their respective
melting points (3,730 F for alumina and 2,800 F for iron).
Today, iron is industrially hardly ever produced by aluminothermy but a
whole array of more exotic metals and alloys is. And due to linguistic
erosion, all aluminothermic processes (even those where iron plays no
part) are now commonly referred to as thermite reactions or thermite
reductions.
Metals (understood here as chemical elements) as diverse as vanadium,

niobium, manganese, cobalt and chromium are industrially produced
using aluminothermy. Alloys (binary or complex) of these but involving
also iron, molybdenum, tungsten, tantalum, osmium and others can be
produced similarly. Many other elements, including copper, silicon, boron,
lead, tin, scandium, nickel, zinc and a whole raft of others are not usually
prepared industrially in this way but can be (and have successfully been)
produced by backyard scientists (like me).
Where does that leave the so far auspiciously absent titanium? Well,
aluminothermic production of titanium metal is a slightly harder nut to
crack (industrially the metal is prepared not from its oxide but from the
tetrachloride, by means of reduction with magnesium - and not
aluminium, in a process known as the Kroll process) because the reaction:
Titanium dioxide + Aluminium ---> Titanium + Alumina
does not generate enough heat for the reaction products to heat to above
their respective melting points (the MP of titanium is 3,034 F), leaving the
experimenter with a sintered mass of solid alumina, with solid, powdered
titanium metal locked into the alumina matrix. Only melting the whole
thing to well above 3,730 F, the MP of alumina, would make the recovery
of lump titanium metal possible.
Like chemistry? Like photos? Visit labphoto.tumbler (click) for

exquisite chemphotos by Kristof Hegedϋs…
There is of course a remedy to this problem and it's known in

pyrometallurgical circles as heat boosting. Heat boosting is the technique
whereby extra reaction heat is pumped into the reacting mix by running a
second much hotter reaction simultaneously with the main reduction
reaction, in the same reactor. In the case of aluminothermy, most usually
a heat booster reaction is chosen that involves the oxidation of extra
amounts of added aluminium powder with a powerful oxidiser. The
worded reaction of the heat booster reaction is simply:
Oxidiser + Aluminium ---> Alumina + by-product
Oxidisers capable of oxidising aluminium with great generation of heat are
a plenty (in fact, all the metal oxides suitable for thermite reductions are
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its own).
Commercially used heat booster oxidisers include chlorates, perchlorates,
nitrates and sulphates (there are others, less frequently used).
Interested in chemistry or pyrotechnics? We supply hobbyists with fine

chemicals at excellent prices and low cost postage (FREE to UK
customers). Oxford ChemServe online (click here!)
The oxidiser chosen for this particular method of backyard

metal production is calcium sulphate, more commonly known
as plaster of Paris, gypsum or... drywall or wall filler! The
worded booster reaction is:
Calcium Sulphate + Aluminium ---> Calcium Sulphide +
Alumina + much, much heat!
The mixture of calcium sulphide and alumina is usually
referred to as the slag.
By combining the main reduction reaction (titanium dioxide +
aluminium) with the booster reaction in the correct ratios, the
required reaction temperature can be increased to almost any
level, including that where all three reaction products (titanium
metal, calcium sulphide and alumina) are produced above their
melting points. From the post-reaction, hot, molten metal/slag
mixture, the metal then coalesces out; much like oil separates
out from an oil/vinegar salad dressing. After cooling, the metal
(the most dense component of the mix) is then found at the
bottom of the crucible, nicely protected by the slag from
oxidation by air during the cooling step.
How to calculate these ratios is outside the scope of this guide
but is usually referred to as a thermochemical calculation,
which takes into account all the reaction enthalpies and the
heat capacities of the reaction products and their abundance in
the slag/metal mix and allows a precise calculation of the end-
temperature of the post-reaction mixture.
So, in a nutshell, by combining the right amounts of titanium
dioxide, calcium sulphate and aluminium and by igniting this
mixture in a fire proof crucible solid titanium can be obtained
(after cooling of the assembly, of course). So far, so good...
Formulation:
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in gram):
Titanium dioxide ........................... 30.0
Drywall ........................................ 25.5
Aluminium powder ........................ 27.0
Ground fluorite ............................. 17.5
For different batch sizes, first calculate the batch factor (BF).
For a batch of, say, 300 g, BF = 300 / 100 = 3. Now multiply
the individual weights with the BF: 30.0 x 3 = 90.0 g, 25.5 x 3
= 76.5 g and so on. Finally check the result by adding the
weights up: 90.0 + 76.5 + 81.0 + 52.5 = 300 g.
Fluorite here is the ingredient so far not discussed. Its role is
that of a slag fluidiser. Where above I made the analogy of the
metal coalescence from the molten slag/metal mix and the
separation of oil and vinegar in a salad dressing, please note
that this analogy is in fact very fair and quite accurate. To
promote the separating of the metal from the molten
sulphide/alumina mixture, it's beneficial to greatly improve its
fluidity (reduce its viscosity in other words), as the coalescing
metal droplets will find it much easier to sink through the
molten cauldron and meet up.
Fluorite (chemically calcium fluoride) has a much lower melting
point (2,555 F) than both alumina and calcium sulphide and is
at those temperatures highly mobile, thereby lowering the
viscosity of the melt considerably and keeping it fluid also
somewhat longer. It's also completely chemically inert in these
conditions, as aluminium is incapable of reducing this
particular fluoride.
Weighing and dry-mixing of the formulation
Weigh the ingredients to at least three significant digits: for
example 2.56 g, 10.3 g or 315 g.
Dry-mix the powders in a roomy container, typically a
hermetically closed food container or similar, by shaking it. I
like to include a couple of marbles in the container during
mixing, as their sloshing about greatly improves mixing
efficiency. Mix until a thoroughly homogeneous dry-mix is
obtained, a few minutes should do the job, depending on batch
size.
Wearing a dust protection mask during weighing and dry-
mixing is probably advisable (although truth be told I never
do).
Fit-for-purpose ingredients
Titanium dioxide:
A good quality grade of titanium dioxide, in the form of fine
flour, of good, clean white colour is advisable. Exact
granulometry isn't critical. If lumpy, sieve it with a tea strainer
or such like. The lumps can later be recovered by gently
grinding in a mortar and pestle.
Calcium sulphate:
Use a no-frills wall filler, the cheaper the better. High-end of

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somewhat detrimental to the thermite process.
The wall filler needs to be thoroughly dried to drive off
inevitable crystal water (this would otherwise be driven off
during the reaction and that could lead to spattering or a
porous slag metal mix) and to ensure it's made up mostly of
anhydrous calcium sulphate. Dry at high heat for about two
hours by spreading the product in an oven proof dish or
stainless steel pan. Drying can be carried out (completely
safely, wall filler isn't toxic) either in a kitchen oven (use max
setting) or on the hob in a steel or copper pan on medium-high
heat. The wall filler will probably darken slightly in colour: this
is normal. After drying and cooling, store it in a dry,
hermetically closed container (e.g. a rubber sealed pickling
jar), where it will keep dry indefinitely. It is not particularly
hygroscopic but will, if exposed, slowly pick up moisture from
the air.
Aluminium powder:
The grade isn't critical. I would advise against too finely
ground grades, about 200 - 400 mesh is what I use. Higher
mesh (finer powder) may lead to too fast reactions and too
high temperatures and hence a formulation adjustment may
be required (see trouble shooting). And really coarse
aluminium (shavings or turnings) would probably still work
fine, provided really large (1 kg or more of mix) batches are
used and you can get the bugger to ignite.
Interested in chemistry or pyrotechnics? We supply hobbyists

with fine chemicals at excellent prices and low cost postage
(FREE to UK customers). Oxford ChemServe online (click
here!)
Some pyrotechnical grades of aluminium powder, like German Black, contain

significant amounts of carbon and may be less suitable.
Ground Fluorite:
Fineness isn't critical either. Something of the consistency of fine sand is
great. There is no such thing as "too fine" Fluorite, as this species doesn't
actually take part in the reactions but merely melts and increases the slag
fluidity.
Reaction assembly
While the entire procedure
has been designed with the
safety of the experimenter
in mind, it has to be noted
that during reaction
temperatures well in
excess of 3,800 F are being
generated, so keeping
one's distance and some
rudimentary insulation
against these excessive
heats are advisable (right
hand photo: a 400 g titanium
thermite assembly - magnesium
ribbon not installed yet).
For this an embedded design is used, which consists of an of-the-shelf

terracotta plant pot (of suitable size) filled with the thermite mixture,
embedded in a larger container (another plant pot for instance) filled with
(this is important) dry sand. Prior to filling the crucible plant pot with
thermite mixture, close over the hole in the bottom with duct tape or
similar. Pictures speak louder than words and here's such an assembly at
work for a silicon thermite (a cache-pot and small steel bucket are used
here).
The dry sand insulates the crucible (the sand will get pretty hot,
depending on batch size) and holds it together during the reaction: the
intense heat inevitably causes the plant pot to crack (but not melt) due to
the extreme thermal shock the material is subjected to.
For smaller reactions, porcelain drinking cups or even egg cups as smaller
crucibles are equally suitable.
Ignition method
Several ignition methods are available, from very safe to slightly riskier,
but all involve locally heating the thermite mixture to very high heat to
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My preferred one I've dubbed ignition mix + magnesium ribbon. It
consists of separately preparing a small amount of a mixture of dried wall
filler and aluminium powder (here the grade of aluminium needs to be
sufficiently fine - 200 mesh or finer) in a weight ratio of wall
filler/aluminium of 136 / 72. Prepare about 20 g or so and keep it in a
safe place, hermetically sealed. This ignition mixture when ignited burns
with sufficient heat to set alight even the most stubborn of thermite
mixtures (some can be hard to light but the titanium/sulphate boosted
thermite has never caused me such problems).
The ignition mix itself requires quite a bit of heat input to get going
(which is why it's safe to store indefinitely) and the best way of doing this
in my opinion is by means of magnesium ribbon. The ignition procedure
thus becomes: after filling the pant pot with thermite mixture, make a
small dent in it at the top and centre and fill this cavity with about 1 small
teaspoon of ignition mix (adjust the amount for much smaller batches).
Stick a 1" long piece of magnesium ribbon in the ignition mix. The
magnesium ribbon can be lit with a small propane blow torch (like a pen
blow torch - the ribbon will also light more easily if you cut a couple of
small 1 mm cuts parallel to the length of the ribbon at the end to be lit).
Caution, once the ribbon is lit, there is no going back: stand well back as
the magnesium fuse will burn down and ignite the ignition mix and the
burning ignition mix will ignite the thermite mixture...
Other experimenters use the potassium permanganate / glycerin ignition
method, others simply take a blow torch straight to the thermite mix or
stick a fireworks sparkler in it. Personally I prefer my own method,
because it allows the experimenter to retreat to a safe distance without a
great hurry and is relatively idiot-proof.
Energy produced
It's intuitive that something that delivers high melting products like
titanium metal and alumina in the molten state must generate lots of
heat. Well, a 500 g reaction mix delivers about 1,500 kJ (kilojoules),
enough to heat about 9 liters of water from room temperature to boiling
point. A domestic 600 W microwave oven would take nearly 45 minutes of
operation on full power to achieve that. Industrial scale thermite reactions
probably generate enough energy to keep a small town supplied with
energy for a few minutes...
Recovery of the metal
Leave the assembly to cool down sufficiently for safe post-reaction

handling. Lift the plant pot out of the sand insulator: the pot is usually
seriously cracked but still held together by a layer of slag sticking to the
inner wall.
Now break open the slag with a hammer: an annealed mixture of
alumina, fluorite and calcium sulphide is pretty hard stuff, so considerable
force may be needed depending on the size of the block of slag.
Inside you should find nuggets of titanium metal. With my sulphate-
boosted reactions, the nuggets (or reguli, if you want to be posh)

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irregularities. A 20 g test batch will usually deliver a few nuggets a couple
of mm across; a 100 g reaction already yields blobs the size of smallish
marbles. Much larger reactions are likely to produce roundish slabs of
metal.
Feel like a real metallurgist and calculate the obtained yield as follows. A
100 g of the mix contains 18.0 g of the metal (but as oxide, of course).
Recover as much of the produced metal as possible, including smaller
reguli and weigh it. The yield is calculated by dividing the weight of the
recovered metal by the weight of the total metal contained in the batch
and multiplying the result by 100 %.
Most
of the
'missing' metal (100 % minus the yield) is in fact present in the slag as
fine, even invisibly small droplets, stuck in some of the early formed slag
that froze when it hit the cold crucible walls, this metal had no
opportunity to settle out from the slag. (Photo left: a fresh 20 g thermite titanium
button, after light buffing with sand paper.)
Yield usually improves greatly with the size of the reaction: for reactions
of, say about 1 kg, I'd expect the yield to be well over 90 %.
Positive identification of the metal as actual titanium
1. Buff it up with sanding paper: removing the surface coating of

oxide reveals the highly shiny, metallic nature of the material. Left
alone the shiny surface will slowly tarnish again, forming a new
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shares that
property with aluminium (and other metals/elements).
2. Check electrical conductivity (press the electrodes against freshly

sanded surface): the material conducts electricity, confirming its
metallic nature.
3. Flame test: press a piece of the metal against a fast spinning

sanding wheel or similar. Small fragments of the metal will be torn
off and burn up spontaneously in the air. Nice to watch and fairly
unique to titanium. Watch a video by my friend Jeffrey on the page
below, using metal from a chlorate boosted reaction (my
formulation). Scroll down to almost the bottom of the page.
4. Chemical identification: for this you'll need strong hydrochloric acid

(HCl 20 w% or more - 30 w% is better) and some pharmacy or
hair dye grade hydrogen peroxide (H2O2, a few w%). Crush up
some of the metal with a hammer (due to contamination with

oxygen and nitrogen it's rather brittle) and put it in a test tube or
otherwise suitable glass container and immerse it in the acid for 24
h or so. As small amounts of hydrogen sulphide (rotten eggs gas -
see below) will be formed, store the assembly in a well ventilated
place, away from your living quarters.
Although titanium is well known and desired for its excellent
corrosion resistance, strong hydrochloric acid does attack it
noticeably but slowly even at ambient temperatures, with the
ubiquitous evolution of hydrogen gas. Titanium (III) chloride
(TiCl3) is formed, which, depending on concentration has a
beautiful, amethyst-like purple hue. After the overnight soak in

HCl, carefully add a few drops of the hydrogen peroxide to the
solution: a beautiful deep red, caused by a very characteristic red
colour from a titanium (IV) peroxo complex being formed. A more
detailed explanation can be found here.
Below, from left to right three test tubes: titanium starting to react with
strong HCl with bubbles of hydrogen starting to form (left), after some
time of reaction the typical Amethyst purple of TiCl3 appears (middle),
after adding H2O2 to some liquid from the middle tube the deep red colour
of the titanium (IV) peroxo complex confirms the presence of titanium

(right).
Why does it smell slightly of rotten eggs?

The explanation is simple: the slag contains calcium sulphide and
inevitably the metal (which in industrial circumstances would be de-
slagged by re-melting under argon or in vacuum) contains small amounts
of slag inclusions. Calcium sulphide, like most other sulphides, is prone to
hydrolysis (it's attacked by water or moisture from the air) and this
causes hydrogen sulphide (H2S) to be formed according to:
Calcium Sulphide + Water (or acid) ---> Calcium Hydroxide (or Calcium
salt) + Hydrogen Sulphide
To keep specimens of the metal without resorting to de-slagging, storage
in hermetically sealed glass containers or ampoules is recommended, to
allow admiring the metal without experiencing the faint but unmistakable
smell of rotten eggs.
It's also advisable to dispose of the slag and broken crucible by either
putting it in some disposable sealed container or wrapping it amply in bin
bags, before disposing of it in a domestic bin, to avoid the lingering smell
of rotten eggs around the house.
Trouble shooting
I'll assume that in the case
of problems, weighing,
mixing and ignition were all
carried out correctly, the
correct ingredients were
used and the thermite
burned right through but
that no metal or very poor
quality metal was formed
(right hand photo: the post-
reaction melt of a 400 g titanium
thermite reaction).
The most likely cause of poor metal production is not that the metal didn't
form but that it didn't coalesce out of the slag/metal mix. The most likely
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this should be rectifiable by adjusting the overall formulation slightly.
Too cold: symptoms include:
• slag didn't collect well at bottom of crucible, contains considerable

voids
• no metal can be found or metal is too intertwined with solid slag

mass and cannot be broken away from slag. Excessive sticking of
the metal to the solidified slag (good metal breaks away clean and
easily).
This is indicative of too low reaction temperature, leading to too high slag
viscosity. This problem should be remediable by increasing the amount of
booster reaction. For the 100 g batch described above, increase the
amount of dried wall filler to 30.6 g and the aluminium powder to 29.6 g
(the total batch weight then becoming 107.7 g) and try again.
Too hot: symptoms include:
• highly porous slag, numerous bubble-like voids, an indication that

something had started to volatilise
• no metal can be found or metal is too intertwined with solid slag

mass and cannot be broken away from slag
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some extent regulates reaction speed and very fast reactions tend to lose,
proportionately speaking, less heat to the environment and this can lead
to overheating. At very high temperatures, even the most high boiling
substances gain some degree of volatility. This evaporation can interfere
with the metal coalescence, a bit like it would be hard for the oil in an
oil/vinegar salad dressing to separate out, if the dressing was actually
boiling.
Try and remedy this by reducing the amount of booster reaction. For the
100 g batch, use 20.4 g of dried wall filler (instead of 25.5 g) and 24.4 g
of aluminium powder (instead of 27.0 g), making the total batch weight
92.3 g and try again.
Related posts written by me:
Chlorate-boosted Titanium thermite
Manganese thermite
A sulfur-free silicon thermite
Copper thermite
Good luck!
posted by Gert @ 1:33 PM 60 comments links to this post
60 Comments:
At 5:58 AM, cyphercube said...

I would like to attempt something useful with this method, would it be
OK with graphite crucible/mold and argon atmosphere?
At 6:14 PM, Gert said...

Yes, absolutely...
At 11:53 PM, Richard F. said...

How much Titanium would you get per 100grams of the mixture you
put into the pot?
Hi Richard,
analiza traficul.18
Theoretically Dacă
gram.folosiți acest
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some sunteți
remains stuckde
onacord cusoutilizarea cookie-urilor.
the slag,
in real terms yield is always lower than 18 g of metal per 100 g of mix.
It's explained in the article.
At 2:28 AM, BRIAN said...

Excellent titanium making method, Gert.Just asking how pure was the
titanium after forging (do crystals form in the titanium metal from the
other chemicals), and is the metal that you get from this process able
to be forged or machined??? Thanks

Hi Brian,
The metal hereby obtained hasn't been refined, deslagged or forged in

any way yet. The crude material does contain some 10 - 15 % acid
insoluble residue, presumably slag micro droplets that didn't manage
to 'escape' upon solidification.
Various measures could be taken to reduce that slag content. Metal

obtained this way would normally be deslagged, prior to casting,
followed by further refining. As Theo stated: this is not really
intended as the road to your $ 700 titanium scissors business. High
quality Ti metal obtained via the Kroll process would remain the grade
of choice for any commercial venture, it isn't that expensive either.
But the homemade Ti is definitely a useful material for those

enthusiasts that would want to put it to good use.
At 5:22 PM, BRIAN said...
Well i don't have plans for a commercial venture, i just wanted to

make a small titanium plate, or dish from your method, and was
wondering if the metal material generated from this process could be
forged into the shape of a plate, and does it require further refining
(which i now understand that it does). Do you have any ideas on how
to deslag the material or refine it??? Thanks again Gert

Well, further refining will make the metal purer of course and thus
more 'true' to its 'theoretical' properties (corrosion resistant, very high
strength to density ratio, etc). Inevitably, refining here means melting
in inert atmosphere and scraping of the so-called 'dross' (slag and
assorted metal insoluble impurities) from the melt.
As regards mechanically forging (not casting) the crude metal into

useful objects, again heating to close to it's melting point, in the
absence of air (in vacuum or under argon atmosphere to avoid
oxidation or even fire) is really the only way. It is this that, as Gray
points out, contributes greatly to the cost of manufactured titanium
items.

As regards making a cookie-uri
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sufficiently hard cutting tool, or so I'd imagine.
In principle the coalescing metal could also be cast straight in to a

mold, for the production of 'blanks' (subjected to post-casting
machining to obtain finished items).
At 4:04 AM, Maestro said...

Would CaCO3 work? It would seem to me that the properties and uses
of that vs. Fluorite are very similar (Calcium Carbonate is used in Iron
processing) but it is infinitely cheaper and thus easier to make the
Titanium.
At 9:40 AM, Gert said...

Maestro:
I've played with CaO (w/o good results) but never with CaCO3. Worthe
trying!
At 7:53 PM, bigdumbchicken said...
Were do you get ground fluorite? Is there anything you can use instead
of fluorite?

Your best bet is a good quality pottery (materials) shop. Minerals and
gems shops will probably sell 'off-grade' fluorite (mine does), but you'd
have to grind that yourself. It grinds down easily in a granite mortar
and pestle.
At 6:29 AM, tankman said...
2 things. Have you ever considered creating a crucible from portland

cement and vermiculite/perlite? I think the ratio is 1/5 cement to
vermiculite. I know this is what I am planning on using in my forge and
it should be able to withstand 4000 degree + temps. I would think
making a pot or crucible from this would be fairly easy.
Also, have you ever played around with Barium Nitrate? I know Ba
(NO3)2 is used in military thermite and in some explosives (flash
powder). Would this work instead of the plaster of paris?

Hi Tankman:
1. I've never made a crucible from a Perlite/cement composite but I

did use this classic mixture for making a small charcoal fired furnace,
see here. Perlite/firecement (NOT Portland) is the 'poor man's
refractory'.
It would be possible to make a crucible from Perlite/firecement,

provided cookie-uri
you have proper ways ofpentru a oferi
'firing' the servicii,
crucible. Such pentru
cruciblesa personaliza anunțuri și pentru a
analiza
wouldtraficul.
be very Dacă folosiți
resistant acest site,
to temperature andsunteți de acord
quite refractory butcu
notutilizarea cookie-urilor.
very strong or long lasting. Worth doing though, IMHO.
2. All powerful oxidisers of Aluminium work. Originally I started

making backyard titanium using potassium chlorate (KClO3) as an
oxidiser, see here. I've also used sodium nitrate (NaNO3) and of course
calcium sulfate (CaSO4). Barium nitrate (Ba(NO3)2), with its high
nitrate content would work a treat, I'm positively sure of it. Of
course the amount of barium nitrate would need to be adjusted to
meet the stoichiometric requirements of the booster reaction. If
uncertain about this, please ask me (its an important point!)
At 1:59 PM, stole said...

i was wondering if there is a way to make titanium which will be
resistant to oxidizing??? i am interested in making my own forge, and
as a fan of medival weapons i would like to try and forge some. i
intend to use titanium instead of carbon steel, having in mind that
titanium blade is much more resiliant and hard than carbon steel one.
so if not posible to make that kind grade of titanium, is it possible
during the thermite process to somehow cause chemical reaction to
mix the titanium with the steel for aditional hardness of the steel ??
thank you.
Stole:
Titanium is very resistant to corrosion, that's one of its attractive

features.
The metal, however, is very difficult to forge by a hobbyist because

forging titanium requires an inert atmosphere (argon blanket), at high
temperatures titanium combines with air oxygen very readily. Also,
thermite titanium is not ductile because it's contaminated with
oxygen. It'd be like trying to gorge cast iron: it can't really be done;
too brittle.
Adding small amounts of titanium to steel will of course affect the

steel's properties, notably hardness and corrosion resistance.
This would be done by adding calculated amounts of so-called

titanium master alloy to molten steel (so it's only possible if you can
actually reach about 1800 C and melt the steel).
The titanium master alloy can itself be prepared quite easily by means
of a thermite reaction: by co-reducing iron oxide and titanium dioxide
with aluminium powder. If the iron oxide/titanium oxide ratio is high
enough, this thermite doesn't require a booster system because the
highly exothermic reduction of iron oxide provides the required heat.
This way, master alloys containing up to about 40 % titanium can be
obtained. I've done it and it works.

analiza traficul.
The master Dacă
alloys are folosiți
known asacest site, sunteți
'ferrotitanium' deindustrially
and are acord cu utilizarea cookie-urilor.
prepared by thermite route.
At 12:02 AM, stole said...

so by those means i can produce titanium enriched steel which i can
then forge in let's say blade ??? and it will be the better choice from
any carbon steel with the same fold / layers ? thx for the answer again

Stone:
If you have the capability to make a decent ferrotitanium master alloy

(by means of a thermite reaction) and disperse calculated quantities
of it in molten carbon steel, then yes, you should be able to create a
titanium enhanced carbon steel. Whether this can easily be forged I
don't know.
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At 6:31 PM, Richard said...

I am new to thermite (was taught how to make black iron oxide
thermite in a pyrotechnics class this spring). Can the heat booster you
used here be used to increase the heat in a black iron oxide thermite
to above the melting temperature of titanium?

Richard:
I assume it could but would imagine that it’s quite dangerous to do so.
Classic Thermite ® is already extremely hot burning, so adding extra
heat becomes dangerous.
If you’re gonna try this, then add only small amounts of the heat
booster package to start with and ramp up slowly if it works for you.
At some point your mixture will become a ‘flash powder’…
At 7:22 PM, rose said...

Nice titanium making method, Gert.Just asking how pure was the
titanium after forging (do crystals form in the titanium metal from the
other chemicals), and is the metal that you get from this process able
to be forged or machined,Thanks.
SARONG
At 9:14 PM, Faizan said...

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At 3:55 AM, Hari said...

Hey, great blog about your experience with reducing titanium dioxide!
I was looking into doing this so I could use the titanium to electroplate
steel (similar to a TiN coating, but anodize-able). I was wondering
about the feasibility of using the titanium nuggets to do this. If they
were cleaned and prepared by washing in HCl or NaOH (I'm not sure
whish would be better, but NaOH wouldn't react), could they be used?
Also, instead of using CaF2 to make the metal more fluid, couldn't
NaCl be used? It also melts at a lower temperature than the reaction
(~800°C), and is a salt. I'm not sure if CaF2 has some other properties
that are necessary for making the titanium liquid more fluid. Also,
would doing this under argon help? What about just CO2 or nitrogen?
Acest site very
Thanks folosește
much! Icookie-uri pentru
appreciate any a you
advice oferican
servicii,
give me!pentru a
personaliza anunțuri și pentru a
Hi Hari,
The nuggets can be polished quite easily and be used as such.
To electroplate you need the metal as a solution of one of its salts.

TiOSO4 for instance or TiCl3 but solutions of these salts tend to be
very acidic, attacking the substrate you want to coat.
NaCl cannot be used as a flux because it is FAR TOO volatile: this

reaction exceeds 2,500 C end temperature. Only CaF2 or Na3AlF6
(Cryolite) are suitable fluxes: both are inert and have very high boiling
points but sufficiently 'low' melting points to cause slag fluidisation.
Hope this helps.
At 3:37 AM, Hari said...

I understand, NaCl would be too volatile. I'm not sure I can get any of
the salt forms of titanium, but I was hoping to use titanium as the
cathode and conduct the electroplating in a molten salt environment
(such as NaCl).

That would be highy innovative!
At 6:48 PM, Hari said...

Well, I guess I will go ahead and try this then! Thank you *very* much
for answering my questions quickly and with useful information. I truly
appreciate the help. Thank you!
At 4:48 PM, Winter said...

I was wondering if this process could be used to make a ballistic plate?
My thought was to make a large batch of the titanium thermite mix in
a large flower pot. That way when it cools it would form a large disk
at the bottom of the pot. My plan was to clean up the disk and use it
as a reactive, bullet proof, target.
http://www.accurateshooter.net/Blog/lvtargets2x350.jpg
I guess my questions are will the titanium form into a single disk if
done in a large enough pot and also will there be so many impurities
that the resulting metal is highly brittle?

Hi Winter,
While it would be entirely possible to make a disc that way (even

other shapes would be possible with so-called 'drop-casting'), the
unrefined metal is quite brittle and would probably not survive bullet
impacts.
analiza traficul.
To refine Dacăitfolosiți
the metal acest
would have site,
to be sunteți
nelted deatmosphere
in inert acord cu utilizarea cookie-urilor.
(most of the impurities then simply float and can be skimmed off).
Considering the high MP of titanium, I'd say 'good luck with that' at the
hobbyist level!

Ooops, 'melted' of course ;-)

That makes since.
Earlier in addressing a question from stole you talked about making a
titanium master alloy by combined iron and titanium thermites. If I
was to refine the resultant alloy, hopefully without it spontaneously
combusting with the air, could that possibly be strong and hard
enough?
by the way thanks for the help
Aha, very interesting point: use titanium alloying to further harden

termite iron!
I’ve actually made ferrotitanium (about 50/50 Fe/Ti), so I know it’s

perfectly possible to make such alloys; it requires no heat boosting
(the Fe2O3 acts as heat booster!), just light the straight
Fe2O3/TiO2/Al/CaF2 mix.
An FeTi alloy with lower Ti content would still be considerably harder

than Fe alone, yet have an MP closer to steel, so easier to forge. No
refining would be needed, IMHO. But whether such an alloy is
sufficiently hard for your purpose is something only experimentation
can show.
I'm looking at making an alloy of 35%Fe to 65%Ti. That should have a

nice low melting point of around 1065C. I'm not sure if that will be
enough iron thermite to generate the heat needed. What equations
are you using to calculate the end temperature. I know a little bit
about thermodynamics so words like entropy and gibbs free energy.
Also where are you getting your supplies from and what grade are
they?
Thanks again for all your help

So is that a Ti/Fe eutectic or something? Because 1065 C sounds low.
W/o calculation my guess is that 35 % Fe + 65 % Ti would generate

more than enough heat (to about 2500 - 3000 C end temp.).
Calculation is done by calculating the Reaction Enthalpy for each

reaction, then usingcookie-uri
NIST Shomatepentru a oferi
equations servicii,
for ΔH for the pentru
reactiona personaliza anunțuri și pentru a
analiza traficul.
products Dacă end
to estimate folosiți acest site,
temperature sunteți
(basically de acord
ΔHreaction cu utilizarea cookie-urilor.
products
= n x Cp,reaction products x ΔT, with n the moles of reaction
products). It must be assumed that the assembly loses no heat to the
environment, as estimating a loss factor is difficult. For fast and
furious reactions this adiabatic requirement is more or less true
because heat needs time to transfer.
It’s best to do everything in moles, then convert to masses.
Say you reacted 1 mol of TiO2 and x mol of Fe2O3:
TiO2 + 4/3 Al === > Ti + 2/3 Al2O3

x . (Fe2O3 + 2Al === > 2 Fe + Al2O3)
So you’ll need 1 mol TiO2, x mol Fe2O3, (4/3 + 2x) mol Al and obtain 1
mol Ti, 2x mol Fe and (2/3 + x) mol Al2O3. From it the reaction
enthalpy can be derived easily. Then work out what temperature
increase this causes for 1 mol Ti, 2x mol Fe and (2/3 + x) mol Al2O3. If
you’re any good with basic algebra you can just leave x in there as
such and obtain a general expression: ΔT = f(x).
Don’t forget to account for CaF2: that absorbs some of the heat too…
And don’t bank on leaving it out either: as a slag fluidiser it greatly
improves yield.

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At 6:04 AM, ZippoLag said...

Awesome and detailed post! Hats off to you sir!
I'm particularly interested in the possibility of making a damascus with

some FeTi in there, altough I'm not sure that the benefits (in
performance and aesthetics) will be worth the trouble, or if it will
even hold toghether! Any thoughts?
PS: too bad your comments got quite spammed by adbots :/
Hi Zippol,
analiza traficul.
Not sure what Dacă folosiți
you mean acest site,FeTi
by a 'damascus'? sunteți
is wellde acord
worth cuand
doing utilizarea cookie-urilor.
easy too.

Ah, a type of steel, right?
The FeTi would then be used as a masterbatch to seed the steel with a
desired amount of Ti, to modify its properties like hardness, corrosion
resistance etc.
At 4:17 PM, ZippoLag said...

Yes, damascus steel in a nutshell is just -slightly- various plaques of
different types of steel packed toghether and then folded to stack in
layers. It's used mostly for aesthetics but it also shields nice
performance if done properly. It has been discovered that much of it's
impressive edge-holding capabilities come from the formation of
carbon nanotubes, this has been found on pieces centuries old.
If you use 2 steels with different carbon content (let's say a hard one
and a soft one) during the proccess carbon migration occurs and the
resulting damascus will have an overall homogeneous carbon content.
Now, I'm not very familiar with the theory (I only know basic
chemistry, mild physics and hobbyst blacksmithing.. and soap opera
english, so sorry for my mistakes BTW '^^) but I wonder if a similar
phenomenon would occur if I put a plaque of FeTi on the mix.
Moreover, what would happen if I try alloys with different components
as well. Of course, 2 adjacent plaques need to be fairly similar to be
compatible enough to weld properly, but the possibilities intrigue me.
Lastly, speaking of possibilities, the big problem here is oxidation of

the titanium, right? I was wondering if I could design a -hermetically-
closed pottery container in wich I would place a cilinder in the center,
suspended above ground level, with a hole in it's bottom, capped with
a small piece of iron. I would then use combustion to exahust the
oxigen in said container, simultaneous with the ignition of a self-
oxidizing fuse that would eventually ignite the thermite. As the metal
liquifies, it would melt the iron cap and flow to a case, obtaining a
bar shape. I'm thinking I would have to set a pool to collect slag as a
middle step, but perhaps I should look up how this is done in
metalurgy and not trying to reinvent the wheel.
My question is then, once it cools down, assuming everything went as

planned I would have a somewhat pure and non contaminted bar of
titanium or whatever alloy I had calculeted, correct? If so, if I wanted
to use said ingot as forge material, I would still have to do it in
another inert atmosphere? Or that's a problem only with titanium
alone, but not ferrotitanium alloys?
Acest
PS:site folosește
damn, cookie-uri
sorry for the pentru a oferi servicii, pentru a personaliza anunțuri și pentru a
long commet!
Hello again!
”Lastly, speaking of possibilities, the big problem here is oxidation of

the titanium, right? I was wondering if I could design a -hermetically-
closed pottery container in wich I would place a cilinder in the
center, suspended above ground level, with a hole in it's bottom,
capped with a small piece of iron. I would then use combustion to
exahust the oxigen in said container, simultaneous with the ignition
of a self-oxidizing fuse that would eventually ignite the thermite. As
the metal liquifies, it would melt the iron cap and flow to a case,
obtaining a bar shape.”
Remarkable! What you’re suggesting is called ‘drop casting’ and it’s

used for making ingots of crude Niobium for example. There is no
need to eliminate oxygen: the slag protects the hot metal (Ti or FeTi)
perfectly. The mould is placed under the crucible. As you said, a steel
or iron membrane is used to prevent the charge from falling into the
mould prior to ignition. After ignition the molten alloy melts through
it and the metal then fills up the mould cavity. Very similar to
‘thermit welding’ (tram rails and such like).
Try and search for it in this book (niobium drop casting):
http://books.google.co.uk/books?
id=6n7Uy2kodZgC&pg=PA343&source=gbs_toc_r&cad=4#v=onepage&q&f=false
Pure titanium needs an inert atmosphere for casting or forging

because it is too reactive towards oxygen. For alloys of Ti, especially
at fairly low Ti content (20 w% or less, at a guess) this may no longer
be true.
You can buy my extensive report on ‘all things Thermite’ here:
http://www.amazon.co.uk/The-Thermite-Report-Goldschmidt-
Aluminothermy/dp/B0086FZR8G/ref=sr_1_1?
ie=UTF8&qid=1338661723&sr=8-1
It includes calculations for desired FeTi compositions.
Also on eBay (most countries) or directly from me (using PayPal).

Buy from me and get a discount!
Best regards.
At 8:05 PM, ZippoLag said...

Thanks Gert!
That pretty much solves my doubts :D

analiza traficul.
Although, Dacă
do you havefolosiți acestonsite,
any thoughts howsunteți
to make de acord cu utilizarea cookie-urilor.
a -preferrably
cheap- crucible that won't crack like pottery for this process? I'm even
concidering pre-heating the pottery before ignition, but I have no clue
if that would prevent the thermal shock enough.. (I'm looking at that
book you linked, but there are some page's not available for viewing,
so I don't know what I'm missing)
BTW, I'd gladly buy your book, but sadly I have no means of making an
electronic payment ATM.

Check or bank transfer are also accepted.
Don't try and make your own crucibles. Honest advice!
Preheating? Unless you pre-heat to near 1,000 C most things will

thermally shock, apart from high melting alloys. It's not worth doing,
at least not for that purpose. Large terracotta pots are cheap as chips.
So you throw them away post-reaction, so what?
At 1:11 AM, ZippoLag said...

Heh, just the habit of wanting to reuse and recycle things (I make
software for a living '^^).
Alright then, thanks or the advices! I believe I won't be trying this for
*a while* yet, but I'll be sure to post results when I do ;)
OK, so long... :-)
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Developing your Web presence: On Titanium, Thermite, the Bronze Age and... Drywall!

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Developing your Web presence

SUNDAY, OCTOBER 19, 2008 About Me

On Titanium, Thermite, the Bronze Age and... Name:

Metals (understood here as chemical elements) as diverse as vanadium,

Like chemistry? Like photos? Visit labphoto.tumbler (click) for

There is of course a remedy to this problem and it's known in

Interested in chemistry or pyrotechnics? We supply hobbyists with fine

The oxidiser chosen for this particular method of backyard

Use a no-frills wall filler, the cheaper the better. High-end of

Interested in chemistry or pyrotechnics? We supply hobbyists

Some pyrotechnical grades of aluminium powder, like German Black, contain

hand photo: a 400 g titanium

thermite assembly - magnesium

ribbon not installed yet).

For this an embedded design is used, which consists of an of-the-shelf

Recovery of the metal

Leave the assembly to cool down sufficiently for safe post-reaction

boosted reactions, the nuggets (or reguli, if you want to be posh)

button, after light buffing with sand paper.)

1. Buff it up with sanding paper: removing the surface coating of

2. Check electrical conductivity (press the electrodes against freshly

3. Flame test: press a piece of the metal against a fast spinning

4. Chemical identification: for this you'll need strong hydrochloric acid

some of the metal with a hammer (due to contamination with

beautiful, amethyst-like purple hue. After the overnight soak in

of the titanium (IV) peroxo complex confirms the presence of titanium

Why does it smell slightly of rotten eggs?

reaction melt of a 400 g titanium

• slag didn't collect well at bottom of crucible, contains considerable

• no metal can be found or metal is too intertwined with solid slag

Too hot: symptoms include:

• highly porous slag, numerous bubble-like voids, an indication that

• no metal can be found or metal is too intertwined with solid slag

Related posts written by me:

Chlorate-boosted Titanium thermite

A sulfur-free silicon thermite

posted by Gert @ 1:33 PM 60 comments links to this post

At 5:58 AM, cyphercube said...

At 6:14 PM, Gert said...

At 11:53 PM, Richard F. said...

At 5:15 PM, Gert said...

At 2:28 AM, BRIAN said...

At 3:54 PM, Gert said...

The metal hereby obtained hasn't been refined, deslagged or forged in

Various measures could be taken to reduce that slag content. Metal

But the homemade Ti is definitely a useful material for those

At 5:22 PM, BRIAN said...

Well i don't have plans for a commercial venture, i just wanted to

At 9:02 PM, Gert said...

As regards mechanically forging (not casting) the crude metal into

Acest site folosește

In principle the coalescing metal could also be cast straight in to a

At 4:04 AM, Maestro said...

At 9:40 AM, Gert said...

At 7:53 PM, bigdumbchicken said...

At 8:21 PM, Gert said...

At 6:29 AM, tankman said...

2 things. Have you ever considered creating a crucible from portland

At 2:31 PM, Gert said...

1. I've never made a crucible from a Perlite/cement composite but I

It would be possible to make a crucible from Perlite/firecement,

2. All powerful oxidisers of Aluminium work. Originally I started