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Thread: Wootz/Pulad Old Recipes

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    Wootz/Pulad Old Recipes

    Hi all

    I'm going to start the ball rolling here... Over the years there are alot of myth's surrounding wootz steels... some are reasonable but others are just simply not true. I feel that its about time to take a chunk out of one belief that the process is a mysterious and lost process. I intend to post as many OLD recipes as i can ( with references !!!! ) ..... ofcourse i'll start with my favourite..
    -- please feel free to add some, if you have

    1)
    " Second Captain Massalski published in Annuaire du Journal des Mines de Russie, 1841,pp.297-308 (plate V, Figs 2,4,5,6,7 and 8) "

    The proportion of elements constituting damascene steel varies according to the quality of the metals used in its preparation. These metals are: iron, cast iron and a little silver. The first should be old, already worked (nails, sheets, etc.), but free from rust. The cast iron is to be chosen from the best qualities of white iron. The steel should be of very high purity. The normal proportion is 1 of cast iron to 3 of iron by weight. "



    it is worth it to get this study because it really goes into detail about the forging and melting process....... fantastic account

    Greg

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    2)

    Islamic Swords in the Middle Ages
    A,R Zaki
    Bulletin de L'Institut d"Egypte
    vol 36
    1953 pg 365-379

    this is a recipe from Al-Tarsussi .... of which he has 9 different recipes

    " take one rotl of iron ( Narmahan ) and half a rotl of male-iron ( shabarqan ). Collect the mixture in a pot and put on it five dirhems of magnesia and a handful of acid pomegranate bark. Let the fire blow on it still the alloy melts, then make an egg of it. Take it out and make a sword "


    interesting to see the ratio of cast iron to iron !

    take care
    Greg

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    Thumbs up

    Male -iron ??? They didn't tell us anything about male and female iron in school !! I better forget about nano stuff and get back to the basics !!..I always wonder how good those old recipies are . From the smith not wanting to give secrets away, to misinterpretations ,to incorrect translations. Thanks Greg thats great food for thought.

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    Hi Robert

    glad you like it.......i've got more to come... i thought i'd post one or two at a shot...

    take care
    Greg

    i'll provide some translation to it as best i can.... for some words..

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    these are a few from the persian steel book by J Allen and B. Gilmour

    1200 AD , Al- Tarsussi

    if it comes from the heads of old nails... 17 dirhems of myrobalan from kabul and the same quantity of belleric, should be cast upon it. The iron should be placed in a pot, which should be cleaned well with water and salt. The above mentioned preparation should be mixed with it, and the whole placed in a crucible , which should be dusted with a dirhem and a half of crushed magnesia ( probably maganese dioxide) . The foundry fire should then be blown upon this until it melts ans is collected as a cake or egg. This is over several days . Then alllow this to cool and make a sword from it: this is a mortal poison.

    I don't have the exact study on me.... but when i go back home for the holidays, i should be able to go to the source


    Next

    1 part male magnesia (manganese dioxide ) , 1 of sunbad ( coral ) I of borax. Break up the whole then set it aside. Take a mann of soft iron filings in the pure state, place them in a crucible , and pour overthem two uqiya of the aforesaid mixture. Blow on the fire to cause it to melt and make it soft enough to take up a round shape in the crucible. Then take 1 part of syrian rue ( peganum hamala), 1 of gall nuts, 1 of acorns, 1 of aloes, together with a quantity of cantharides equal to all these. Make the whole into a powder, and of this mixture cast 2 uqiya on to the mann ( 1 maund = 2 ratl ) of iron, blow on the fire until what appears to be a rainbow rises out of the crucible. When it has reached this state, allow it to cool, then forge it to make what ever you want.

    Greg

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    Fulad Salmani

    also from same book

    cultivated myrobalan, 20 dirhem: magnesia, 7 dirhem: scammony, 5 dirhem. Reduce all to a powder. Cast this preparation onto 3 ratl of shaburqan, and blow the fire to make it melt in a crucible with a lid pierced with a hole so that one can see into it, and examine the iron until it is seen and felt with an iron rod to melt. Then remove it from the furnace, allow the crucible to cool with it, and make of it what you will. And strike a 20 ratl iron bar: with Allah's help it will cut it..

    1 ratl = 12 uqiya ounces= 144 dirhams =.75lbs =.3kg
    1 mann= 2 ratl


    take care
    Greg

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    .

    Greg, thanks for starting this post.

    . These metals are: iron, cast iron and a little silver. The first should be old, already worked (nails, sheets, etc.), but free from rust. The cast iron is to be chosen from the best qualities of white iron. The steel should be of very high purity. The normal proportion is 1 of cast iron to 3 of iron by weight. "

    Last night I tried the above recipe. It should work the next time. The reason for the failure is:
    I make my own crucibles (one can only afford a finite quantity of comercial crucibles only to see them destroyed ), they are dried and fired in the forge (slowly over charcoal) until they are at least cherry red. These crucibles resemble an ordinary coffee cup, two are used to make a crucible and cover. The halves are luted together with a commercial fire brick mortar.
    My mistake was firing the lip of one of the crucible halves too high and creating a glassy edge thus a poor surface for bonding with the mortar. As I am firing in a charcoal furnace I end up rocking the thing back and forth while pushing charcoal under it with the poker. Just at the time I was getting liquid (about 1 hr +15 min into the process) the two halves came appart.
    Some time this week I plan to do it again.
    Jan
    Last edited by Jan Ysselstein; 12-10-2006 at 06:37 PM. Reason: hit wrong key and was not done

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    Hi Jan

    home made crucibles are tough... I've tried several times... I just don't have the talent to make them work dependably..

    did you see Vasilli's site... he has a small tutorial about mid way...
    http://playground.sun.com/~vasya/Bulat.html

    i emailed him and he's a very honest and informative..

    he gave me a translation which i posted here... for the crucible ingredients
    http://p222.ezboard.com/fprimalfires...icID=219.topic


    Good luck
    Greg

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    Greg:

    Thanks very much, I did see the articles by Vasilli (probably posted by you in the past). They are very clear and if my method fails me, I will follow his suggestions ( I like his method tamping the clay mix into the shape ).

    My crucibles are made with a clay mixture roughly as suggested bythis site [ http://users.ticnet.com/mikefirth/crucible.htm ]. I have done some major substitution with the assistance of a local ceramics supply store.
    To stay as faithful to the "old" recipies, I add some charred rice hulls and form the crucibles around a male form onto which some burlap or cheese cloth has been wrapped (this allows the clay shape to be pulled off) , once they are somewhat firm I shape the inside with a teaspoon (thereby eliminating the cloth imprint found on the inside of some crucibles of the past, variable? ) and let them dry. The clay mix has to be extremely well mixed, assuming people are using a proper mix, a lack of mechanical mixing is probably the cause of most failures.

    Slowly but slowly I will get the easy part (making an egg) under control. Now I am beginning to look at a quick way of finely dividing the "pure" iron
    (like a cold saw or a rotating rasp) and dealing with the desirable impurities.

    A recipe on the horizon is cast iron and iron ore, (it works well because an impatient one using a $35 crucible (gone!) has a gassy egg with a very nice fine dentritic structure. My problem is finding out if the oxygen will be carried away as CO or CO2 or what the ratio will be.

    Jan

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    Greg have your opened up a can of worms which I am going to have to slither after ? A few things for people to note: as you mentioned Massalski's text is important (as it is) but also because it illustrates that Bukhara, Uzbekistan was still producing pulad in the mid 1800's! (not importing it from India). Right there it illustrates that the technology was never "lost" (from there it went to Anosov etc).

    I have a whole compliation of recipies, and I am still looking for more!

    Something else for people to consider....the materials put into the crucible charge were also highly symbolic. For example, Pomagranates represented immortality etc...what more would you want in a blade?

    Robert, male and female iron is a very common "Eastern" concept. Male iron is hard while female iron is soft. Furnaces also have a sex.
    Dr. Ann

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    Hi Ann
    that is fantastic... I hope to encourage everyone to jump in on it.. I should have a couple more once i get back home.. to that other stack of paper

    yes.. i love that Massalski account... I had voysey and barker account but i misplaced them in the move... and luckily kept the Massalski... as it was in my brief case.. .. I'll have to reapply for my interlibrary loans again to see if i can get the old ones back... what a pain in the butt..


    Hi Jan
    thank you very much for that link... I will link it to primal, forsure...
    - if you can do the crucibles... wow.. thats great ! Its not something i was ever successful at... I just use the clay graphite crucibles and really watch out for the carbon uptake to the charge...

    oh... I also try to have my charge completely clean.... no rust or scale on it... I find that does contribute to gassy ingots...

    -- also.. you have to melt the charge and keep it melted for awhile ... the steel will bubble furiously... and note how high it climbs up in the crucible... be patient and keep the fire to it..... when you see the steel sit right down in the bottom of the crucible... ... the level will go much lower... ... this is the sweet spot when the bubbles are out of the steel... .. now you can slow cool the charge and make a nice wootzy ingot..

    ofcourse i wear welding goggles to gaze at the charge... and be safe.. i've burnt my eyebrows, nose hairs, eye lashes in just one puff

    take care
    Greg

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    Greg, Ann, please don't stop... PLEASE !!
    Please forgive my english.

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    Greg, I managed to get my hands on several pounds of top-quality wrought iron. Some of it's designated for hilts but would you be interested in a bit for a smelt?

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    Hi Carlo
    glad you like the post... we will most certainly continue..
    - posting maybe abit spotty as i'm back in the northland for the holidays..

    Hi Al
    -- thanks for the generous offer.. definitely sounds like a good idea ! Wrought with cast would make a splendid wootz !!



    take care
    Greg

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    just saw this link... heres a modern product used to desulphurize the charge....
    -- and its made of magnesium..
    -if you look... some recipes use a magnesium salt...

    http://www.magnesium-elektron.com/ma...ions.asp?ID=16


    very interesting stuff

    Greg

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    just saw this link... heres a modern product used to desulphurize the charge....
    -- and its made of magnesium..
    -if you look... some recipes use a magnesium salt...

    Greg,

    Sounds like an effective solution to sulphur (though it seems too dangerous for the home shop). The finely divided silver is going to take care of that. I hope no one is counting the spoons around here.

    Three more crucibles (clay) are assembled and will be tested this week. An experience with cast iron and iron ore was posted on the Wootz Questions thread. The result was, too great a fluxing effect of iron oxide on the clay. The next test will not have iron oxide in the crucibles (just cast iron and iron) and they will be placed in a gas furnace to eliminate having to manipulate the delicate item.

    Jan

  17. #17
    Major thanks Greg! All this talk about Wootz is starting to fuel my interest in it more and more I still know far from enough to start making my own, but every piece of information is very helpfull. I do have a pretty good understanding of furnaces and crucibles, so at least that's a good start. What sort of temperatures are actually required for the process? I know pure iron melts at 1538°C, but I assume that the iron will dissolve in the liquid cast iron well below that temperature?

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    Hi Jeroen

    for myself, i prefer to have a furnace that runs hot ... hot enough to melt plain iron by itself. My reasons are that my fuel source is mostly propane in a 30lbs tank. With this fuel limitation in mind, its abit of a race to get the furnace bore to high temp.... then a hold time... Even though your furnace bore is close to temp, the charge seems to be cool and it takes time to completely melt... my first run will take at least 40-45 min to be completely liquid (and the start of slow cooling )
    -- ofcourse i can get there much quicker but... i like to take the bore up slowly in temperature at first.
    -each crucible after takes much less time to melt...

    you are very correct that the cast iron melts at a very low temp... I imagine that for the iron plates to dissolve in the cast iron would take longer times than what i typically run at..

    another problem.... the clay graphite crucibles i use contribute carbon to the melt the longer it is at liquid... so you have to watch this aswell not to add too much..

    once you can melt iron.... you'd be very surprised how easy it is to make wootz ingots... however, forging is another thing..

    there are so many ways to make it... you just have to find a method that gives you the greatest success


    Hi Jan

    I read awhile back a post, where one fella used a charge that was mostly iron oxide... it produced an ingot with alot of porosity... and this was also my experience.. this is why i clean my iron and cast iron clean of all rust ....
    -- i do think the rust will reduce.... eventually.... but it will take some time for the steel to be killed..
    -- i think its all about getting a repeatable formula and sticking with it... making steel has so many variables that can pop up...


    take care
    Greg

  19. #19
    Quote Originally Posted by Greg T. Obach View Post
    Hi Jeroen

    for myself, i prefer to have a furnace that runs hot ... hot enough to melt plain iron by itself. My reasons are that my fuel source is mostly propane in a 30lbs tank. With this fuel limitation in mind, its abit of a race to get the furnace bore to high temp.... then a hold time...
    I didn't realize you can reach that temperature with a propane furnace. I thought the flame temperature was around 1400C. I can reach up to 1300C in a charcoal furnace, perhaps 1400C if I really push it. But then it will have to be a very well insulated furnace system. Traditional clay crucibles also won't survive more then 1400C (at least, that's the highest recommended firing temp. on the high-temp clays), so that's pretty much my limit. So melting pure iron (without carburizing it) is not an option for me, unless I go for modern materials and fuels.

    another problem.... the clay graphite crucibles i use contribute carbon to the melt the longer it is at liquid... so you have to watch this aswell not to add too much..
    I use graphite free crucibles, so that shouldn't be a problem.

    once you can melt iron.... you'd be very surprised how easy it is to make wootz ingots... however, forging is another thing..
    I've got experience in cold working bronze, which is probably even worse. Not that I can do that reliably yet, but at least I'm all to familiar with hitting cracks

    there are so many ways to make it... you just have to find a method that gives you the greatest success
    I don't expect to get around to it in the near future (to many other plans for the moment), but I'll definately keep reading on the subject. It's definately on my list of things to do.

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    Greg:

    I am glad you brought up the cleaning of the metal prior to melting. I am not sure I can do that unless I tumble in sand or do an acid wash, as I am using smashed bits of cast iron.
    I am using bloomery iron, and bloomery cast iron, some iron oxides will be in the melt. I think holding just below 2100 Deg F with a reducing atmosphere (about an hour or so) will help eliminate surface oxides.
    Based on what I have read and experienced, I think historically, the crucibles were ramped up to the 1440 Deg C range very very slowly.

    A knife maker I am not but I do enjoy the learning curve I am experiencing.
    I will attempt to attach some pics. to this reply. It may not work but in case it does. They are pictures of:
    . a broken (failed crucible)
    . a crucible assembly exterior
    . a tatara furnace in use last night
    . the resulting tamahagane ( mostly cast but some soft spots)
    this was my first time using this new furnace, I was shooting for all
    cast iron but I will take what I got

    Jan
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    Last edited by Jan Ysselstein; 01-03-2007 at 09:12 PM. Reason: Wrong temperature scale

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    Hi
    If you look at the iron/carbon diagram
    http://www.sv.vt.edu/classes/MSE2094...es/kimcon.html

    it looks like 1400c would be fine... for a 1.5% carb charge... also the other alloys in the steel would lower that abit more..

    one other thing.... my furnace is typically run with a closed crucible and a glass flux to provid another barrier to furnace atmosphere.... so i tend not to worry about reducing atmospheres.... and run it as hot as i can get it...

    why as if you use charcoal... that produces some monoxide...and that would definitely help to reduce the charge..

    the ancient smith used charcoal... and they did it well... so its very possible


    Nice tatara !

    when i clean my cast and iron charge... i just use a wire wheel, and get to the metal ...... no pickling... just wire it down to the grey metal.... any little bits that i miss, should get cleaned off by the glass flux ....

    if you use clay crucibles..... do you include rice husks and some grog ? i have a study back home bout that ... that should help to give it a higher work temp...

    clay crucibles is really an area that i've had the least success with... I'm definitely not a good ceramist ... thats why i use the clay graphites..

    take care
    Greg

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    if you use clay crucibles..... do you include rice husks and some grog ? i have a study back home bout that ... that should help to give it a higher work temp...

    Greg:
    Thanks for the temperature suggestion and the iron carbon phase diagram. I have no way of measuring the temp and initially it will have to be guess work based on assumed composition and a steel rod.

    Yes I have added some charred rice hulls (probably tooo much), I crush them before mixing with the clay. I bought some soft broken high temp brick (2600 Deg F)from our supplier for $ 1.00 a piece, I crushed them for grog. Basically it is 40% fire clay 60% other ( grog,rice hulls calcined kaolin).

    Tonight I ended my attempts at working with two small crucibles luted together. An improvised furnace was made and worked very well and seems to be durable enough for 5-6 runs. The crucible was quite hot, the 1lb of cast iron was liquid, I was adding 3" length of wrought iron (alternating with bits of wood soaked in lighter fluid ( may your lamp burn brightly ) the iron pieces were slowly sinking.....and the the kiln shelf support (crucible stand) gave way on one side and the two crucible halves came appart when I was fishing with a rod to straighten it out.
    Tomorrow I will mix a new batch of clay, easy on the rice hulls (if any). Make a form for a crucible capable of holding 1 kg of steel (no more adding stuff to a 2500 Deg F container).


    A couple of observation which surprised me.

    The perfectly formed egg had 3/8 dia. rod pieces frozen in the top. Though these had onle been in cast iron for a minute or two, the spark indicates very high carbon (not just at the surface).

    When I pulled the top half of the crucible off, the molten liquid was acting as a big sparkler (was I seeing a boil and if so does the boil toss up Fe as well as FeO)

    Jan

  23. #23
    Quote Originally Posted by Greg T. Obach View Post
    if you use clay crucibles..... do you include rice husks and some grog ? i have a study back home bout that ... that should help to give it a higher work temp...
    It doesn't do anything to the melting temperature, just makes it more resistant to thermal stresses. The crucibles I use for bronze casting consist of clay pre-mixed with grog, to which I add 40-50% of silica sand, and sometimes a small amount of horsedung. The less clay in the crucible, the better it handles temperature differences without cracking. The clay I use is a 1280C clay though, so not the highest temperature clay. So I get quite a bit of glazing, and once in a while a partially molten crucible (usually only with small crucibles). But the clay is quite suitable for bronze casting, and easy to fire. High temp clays won't harden until much higher firing temperatures).

  24. #24
    It seems like the magnesium would definitely be a bit too exciting for use by most of us. I did some looking around and discovered that the reaction of magnesium with sulfur when used in the purification of an iron melt is described as "violently exothermic". This didn't sound good to me. I also looked into the silver additive, and I have some doubts about its efficacy. It looked to me like silver sulfide breaks down at high temperatures, possibly into a couple different poisonous gases. This says to me that either it will break down within the melt and leave both the silver and sulfur in the steel, or it will come to the top and poison everyone in the area.

    I looked a little further and found that calcium is also an effective desulfurizer, and has been in use for purifying steel melts for a loooonnnggg time. Most wootz formulas call for some kind of calcium ingredient for the slag topping, as does the formula that Pendray uses. It probably isn't as effective as the magnesium, but it also won't be as exciting!

    Peter
    http://www.fallinghammerproductions.com
    http://www.dragonsbreathforge.com/wootz.htm

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    Most wootz formulas call for some kind of calcium ingredient for the slag.

    Peter:
    Thank you for the tips and the cautions.
    I have had four samples of the iron I am using tested for composition. The sulphur levels were:

    1) .004%, 2).015% 3) .004% 4) .004%

    Sample two had .85% C while 1,3 and 4 were at .01% carbon. I assume the cast iron I am making (and have not yet had tested) is at about .015% Sulphur. I am not going to concern myself with Sulphur at this time. Once I get some melted samples tested and if Sulphur is a concern, I will add some lime.
    I just want to make a cake (the easy part) in a clay crucible, using my iron.

    I recall some discussion (which you were participating in) regarding W-2, and wootz on another thread. Did you melt some W-2 yourself or were you working manufactured bar stock? I would think just melting W-2 in a reducing environment will give a dentritic cake with some key trace metals,while kicking up the Carbon content a little. Before I realized files were not made of W-2, I tried this in a crucible (sphere) made of rammed refractory. All my earlier trials were failures due to impatience, but I did fuse a pile of file fragments together (none had deformed, the textures were still clearly visible, but wherever they touched they had fused) .

    Jan
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