Contradictions on grain size and soak time

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I recently read through the 5 hour O1 soak thread on here, and the Verhoeven text: "Metallurgy of Steel for Bladesmiths & Others who Heat Treat and Forge Steel".

On page 68, it shows a chart in which grain size growth is directly correlated to increased soak times and temperatures.

Can anyone explain the contradicting viewpoints?
 
Please quote an exact comment on the soak thread that confuses you. Grain growth is far more dependant on temperature than time .As that graph shows the temperature scale is linear and the time scale is logarithmic !
 
I'm sorry, could you explain your last sentence? I don't understand it.

In any case, my point was that according to that graph, increased time in the soak does cause grain growth. Specifically, for 1060 steel, grain size increased from approx. ASTM size 5.5 to 7 when time was increased from 6 minutes to two hours.

I'm not disputing that temperature has a much larger impact then time, however I'm suggesting that perhaps the claims that a 5 hour soak for 01 with no increased grain size might have been wrong. There is grain growth for increased times for 1060, but at least to the naked eye I believe it would be undetectable.
 
I have never proposed soaking for long times like 5 hours. What is important is that you understand [and apparently you do] that temperature has far more effect than time....It's like the three bears -there's 'too much', 'too little' and then there's 'just right' .
 
Ghost Squire:
I love it when someone reads and questions what they read with knowledge.
The quote was about grainb size 5.5 to 7, that is pretty coarse, then consider that the finer the grain, the easier it is to grow.
Thanks
 
I have never proposed soaking for long times like 5 hours.

I wasn't saying you did, just that the claims that were made in the 5 hour 01 soak thread may have been a bit hasty. I'm anxious to hear more about this, especially from Kevin Cashen, he will have some insight into this matter.

I love it when someone reads and questions what they read with knowledge.
The quote was about grainb size 5.5 to 7, that is pretty coarse, then consider that the finer the grain, the easier it is to grow.

As do I, and its a thinker. I didn't know that the finer the grain the easier it is to grow, in fact I thought the opposite was true, that the finer the grain, the easier it is for tinier grains to grow along the borders, because there is more surface area available? Although this probably wasn't what you were referring to.

Thanks for replying mete and Mr. Fowler!
 
ghost squire said:
I wasn't saying you did, just that the claims that were made in the 5 hour 01 soak thread may have been a bit hasty. I'm anxious to hear more about this, especially from Kevin Cashen, he will have some insight into this matter.


Howdy ghost squire,

I'm the one who did the 5 hour soak with O1. When I said there was no grain growth I meant any grain growth that was visible to my untrained eye. :D A microscope might reveal more.
I've over heated steel before and seen huge crystals result. This was nothing like that. Like wise, the steel that had massive grain growth was very easy to break. This O1 sample took some healthy whacks before it broke, and this was with a notch and without tempering.
I would never soak a knife for 5 hours. I was simply proving something to myself. For most steels, 5 to 15 minutes is probably enough.
You really shouldn't take my word for it though. Do you have an oven? If you do, I suggest you do the experiment yourself with whatever steel you want.
I wouldn't blame you for not believing my "claims". It sounded far-fetched to me, that's why I tried it. Now I'm convinced.
 
How coincidental the timing of this thread is, as I began metallography work on Mr. Patton’s, 5 hour soaked O1 today. One person’s word is never good enough for us to go on for proof, however let me reiterate the facts that not only did Mr. Patton’s experiment yield the predicted results, but I mentioned others who have done the same with 52100, I have done extended soak times with O1 (not as extreme as 5 hours, since it is well beyond the realm of usefulness). Ray Kirk is no slouch in the knifemaking field and he told us that he went as far as to soak 52100 for 24 hours with the same results.

I am confident that any others repeating the experiment will get the same results, since any metallurgical text will confirm the concept. The case is looking pretty good on this one folks.

I have looked over pg. 68 of the excellent writing to which we are referring and there are no contradictions at all, it entirely supports previous conversations as well as the experiments we have mentioned. Then entire section deals with why temperature control is important. On that chart the 2 hour growth rate parallels the 6 minutes and they are continuously increasing in temp, clearly showing how irrelevent time is in comparison to temperature. Also be aware that the only part of this graph that would be within the range of proper heat treating would be the lower left section below 1500F. Allow me to quote the text that is right next to that chart:

“Note that raising the temperature of the 6 min. hold from 1400F to 1700F nearly triples the grain size, from 33 to 94 microns. Like most metallurgy rate processes, grain growth is more sensitive to temperature than time…”

I strongly recommend further reading in the same book, pages 74 through 76 will clearly describe how substitutional solutes will cause the 5 hour soak with O1 to be entirely possible. The same chapter also goes into the work of R.A. Grange back in 1966 where he shows the refinement of grain to ASTM size 15. Isn't forty years is a long time for something to be ground breaking or “theoretical”? Mr. Verhoeven also goes on to explain how the same process can be done with no hammering at all.

I could go on for some time quoting how this book entirely supports Phillip’s findings, or I could point to any number of others. One that I just found on my shelf and had forgotten about is “Vanadium Steels and Irons”, which explain on every other page how undissolved vanadium carbides will stop grain enlargement.

Finally the chart in question uses 1060 steel. 1060, 1070, 1080, 1084 will all grow grains much more readily than O1, W2, 52100 etc… Without rehashing the other thread entirely, most should see a difference between these steels.

O.K. one more time…

Simple iron carbides will take some time to dissolve but will indeed eventually fall to the process of diffusion. Austenite grains form and grow by pulling this carbon into solution. If you are working with a simple carbon eutectoid* steel, or close to it, at room temperature the steel will consist entirely of pearlitic grains with no left over material in the grain boundaries. When you heat this steel the segregated carbon will very easily go back into solution with nothing to stabilize the grain boundaries when it is all used up, so extended soaks with such a steel will produce larger grains over time. However with proper temperature control this is still nothing to worry about.

Steels with stronger carbide formers, vanadium, chromium, tungsten etc… will have plenty of very tenacious carbides that take much more diffusive power to dissolve. In the above mentioned Vanadium book it explains tests done on steels that had vanadium in excess of the necessary carbon levels for proper hardening. Such steels had to be heated to temperatures in excess of 1850F before they would show any hardening from quenching. Why? Because below these temps all the carbon was locked up in V-carbides and could offer nothing to the martensite. You can take it to the bank that there was zero grain growth regardless of how long they soaked that stuff, unless they heated it over 2000F.

To say that it is easier to grow grains when they are finer is inaccurate. All the same rules still apply, just the temperature at which grain boundaries can move gets lower. So if we simply lower our austenitizing temperatures, time once again becomes impotent in comparison. It still all comes down to control. Folks that have limited precision in controlling temperatures need to worry about grain growth, those who have precise controls have nothing to fear from it and can even soak for ludicrous lengths of time.
We covered a lot of this in Dan’s question about over soaking his 154CM, there as well we were overlooking the most important part the temperature, in both cases we are over 300 degrees hotter than you ever go in heat treating simple steels. At these temperatures grain growth will happen when solution is complete.

I hope I never gave the impression that grain growth was impossible from time, it is just not a problem compared to temperature. We don't need a microscope, just put two and two together, if the rate that we are presuming grains to grow in a couple of minutes were applied to 5 hours, we should darn well see those suckers with the naked eye!

I have Phillip's 5 hour O1 in my posession now and I can independantly verify His observations. I have yet to get my tools to precisely measure ASTM grain size worked out from my microscopes to my computer, and Phillip’s samples are not in a good phase to see grain boundaries, but in comparing it to my samples soaked for only 10 minutes I see no difference is structure size at 400X. I do see some other things however…;)


*Eutectoid: carbon content of approx. .8%
 
Phillip, I have prepped a couple of specimens from your steel so far and the story it is telling is quite fascinating, but rather hard to pin down. On the first etch I did, I hit just the right time to reveal both fine spheroidal carbides (yep they are still there), as well as some super-fine black structures that I was very interested in, as well as some other odds and ends that I need some data from you to interpret better.

What brand or type of O1 was this? I am trying to work out a possible chemistry for it.

How was the steel treated after the soak? Was it quenched? Quenched and tempered? If so, how hot? I ask this because I am seeing structures that would indicate more than just pure untempered martensite.

One thing is for certain, it was not protected entirely from the Oxygen for all those hours- the decarb is spectacular! Huge ferrite fingers reaching in from the surface, if it wasn't the kiss of death for a blade, I would say it is lovely. This is afterall the down side to longer soaks, more time for decarburization. Samples that I have of 1095 austenitized with a torch has a good ammount (nothing like that 5 hour stuff;)), but my O1 samples that I did in my salts has none of it- no oxygen under the surface of salts;).
 
Mr. Cashen, firstly thank you for responding. Quickly, those super fine black structures you're seeing are a type of carbide if I'm not mistaken. Reading "Cryogenic Quenching of Steel Revisited" by Zbigniew Zurecki, he observes that in some of the cryogenically frozen samples of A2 steel, super fine black carbides were found to have appeared. Probably nothing special in the chemistry, simply that the longer soak times for your samples likely allowed these carbides to form for whatever reason. A definite upside to the longer soak times.

In response to your entire first post, I already confirmed that I do indeed realize that temperature is more important then time. However, are you denying that increasing time spent at temperature (above 1400 to be specific, although I'm not sure where it starts) does grow grains? I absolutely am not denying the benefits of a longer soak. But its hard to say that grain growth cannot be expected.

I looked through that entire section of the text again, and lo if I did not see that in every chart provided on the matter, regardless of the steel there were in fact increases in grain size. I did read it thoroughly before and I know how much the grains grow is highly dependant on the steel, due to varying alloy content. But increased time spent at temperatures, (regardless if your lowering temperature by 50 degrees or so for austenitizing) seems to always result in the same thing. Its a tradeoff. Personally I think for many applications it's worth it, since you're getting all those lovely fine carbides which result in higher hardness and such. But the steel will likely suffer a bit as a result.
 
Kevin R. Cashen said:
Phillip, I have prepped a couple of specimens from your steel so far and the story it is telling is quite fascinating, but rather hard to pin down. On the first etch I did, I hit just the right time to reveal both fine spheroidal carbides (yep they are still there), as well as some super-fine black structures that I was very interested in, as well as some other odds and ends that I need some data from you to interpret better.

What brand or type of O1 was this? I am trying to work out a possible chemistry for it.

How was the steel treated after the soak? Was it quenched? Quenched and tempered? If so, how hot? I ask this because I am seeing structures that would indicate more than just pure untempered martensite.

One thing is for certain, it was not protected entirely from the Oxygen for all those hours- the decarb is spectacular! Huge ferrite fingers reaching in from the surface, if it wasn't the kiss of death for a blade, I would say it is lovely. This is afterall the down side to longer soaks, more time for decarburization. Samples that I have of 1095 austenitized with a torch has a good ammount (nothing like that 5 hour stuff;)), but my O1 samples that I did in my salts has none of it- no oxygen under the surface of salts;).


Interesting stuff. Thanks for doing this analysis.
Sadly, I don't know much about the O1. I got it off ebay. It was 1 1/4" round bar, so it required a lot of forging to get it to the size you have, so that may be where (some, at least) of the decarb came from. I didn't grind it at all after forging.
After the soak, I cut the envelope open and dumped it into Shell H201 quenching oil (almost identical to Texaco type A) which had been preheated to around 150 F. The O1 kind of got stuck in the foil trying to get it out, so it took longer to get it in the quench than I would have liked. So if you find some pearlite, that's why. :o
It was not tempered at all. Why don't you do a Rockwell test on it? I'd like to know how hard it got.
Can you tell how thick the decarb is?
I have more of the same bar of O1. If you want to know what's in it, I can send it off and have it tested. (If the guy is still willing.)
BTW, Kevin, did you see the thread I started about some samples i sent in? If you've wondered what's in Admirals L6, you can find out there. ;)
Last year I started building a high temp salt pot. I'm gonna have to finish it soon. Sounds like heaven. No decarb and no warping. :)

Ghost squire, this is your thread, if you want, I can start another one about the O1 sample.
 
ghost squire said:
Mr. Cashen, firstly thank you for responding. Quickly, those super fine black structures you're seeing are a type of carbide if I'm not mistaken.

Ghost squire, to satisfy my curiosity would you mind sharing your real name with us?

A carbide indeed, but none of the elusive creatures often mentioned in cryo research, as I would need a bit more than 1000X to catch them. My questions about Phillip's subsequent treatments were to see if there had been enough post quench heating to produce tempering carbides (dark) large enough to make out at that magnification.

ghost squire said:
In response to your entire first post, I already confirmed that I do indeed realize that temperature is more important then time. However, are you denying that increasing time spent at temperature (above 1400 to be specific, although I'm not sure where it starts) does grow grains?

Kevin R. Cashen said:
I hope I never gave the impression that grain growth was impossible from time, it is just not a problem compared to temperature...

I looked through that entire section of the text again, and lo if I did not see that in every chart provided on the matter, regardless of the steel there were in fact increases in grain size.

Fig. 8-3, Fig.8-9, Fig. 8-10, Fig. 8-12 would be the ones that could deal with this matter. Of these the only one that deal with holding at a constant temperature is 8-12, and that temperature is 1850F:eek: and still it takes six hours for the richer steel to enlarge one grain size at 350F degrees hotter than Philips temperature.

All the other charts deal, not with constant soaks, but increasing temps. from 1400F or 1600F to well over 2000F. Fig 8-10 gives no time at all just very high temperatures yet the text includes- "As the figure shows, these particles are able to effectively pin the austenite grain boundaries at temperatures up to 2000F."

Fig. 8-9 shows the difference between soaking a fine grained (aluminum killed) steel for 6 minutes and 2 hours in a range from 1400F to over 2200F, and it can be noted that the range from 1400F to 1600F there is no difference. I hope we are reading the same book here.

It is undeniable that diffusive processes are both time and temperature dependant and in almost every post I have made I have been careful to mention that in great enough amounts time can affect these processes, but we are now using examples of 6 hours at 1850F moving grain boundaries a few measly microns, I believe that would qualify as what I often refer to as "hair splitting", on a point that I never disagreed with.

I do believe that I see your point though. It would indeed be very irresponsible of us to lead anybody to believe that any soak longer than that recommended for the steel would be beneficial. Most simple steels have a recommended time of 30 minutes or less. It is entirely correct to say that to go beyond this is not good for the steel. If one avoids grain growth, I would consider the decarb issues to be a much worse problem. 5 hour soaks are ludicrous in knife cross sections for anything other than to prove a point with an extreme example.

Please folks, do not interpret this test as a recommendation of heating any steel for 5 hours, to get some magic result that the spec sheets overlooked. Soaking for longer than necessary is not beneficial. But having tight control over the temperatures at which you do soak is always a plus.
 
Phillip Patton said:
...Why don't you do a Rockwell test on it? I'd like to know how hard it got...
I will do that as soon as I am done harvesting samples, I didn't want to grind any of the surfaces until I was done with them.

I saw the thread about the analysis, it was VERY interesting.

and I agree...
Phillip Patton said:
...Ghost squire, this is your thread, if you want, I can start another one about the O1 sample.
So I will cover more of my findings in another thread when I can get a consistent etch and produce images.
 
Ghost squire, this is your thread, if you want, I can start another one about the O1 sample.

No no this is fine.

Ghost squire, to satisfy my curiosity would you mind sharing your real name with us?

A carbide indeed, but none of the elusive creatures often mentioned in cryo research, as I would need a bit more than 1000X to catch them. My questions about Phillip's subsequent treatments were to see if there had been enough post quench heating to produce tempering carbides (dark) large enough to make out at that magnification.

Oh ok, sorry I couldn't help with that. My name is Eric Gullicksen BTW.

Understand that I am playing the devil's advocate here. I don't want there to be increased grain size for these marginally longer soak times that are beneficial, such as 10-30 minutes which you mentioned.

I believe you misinterpreted figure 8-3, I'm not the sciencey one, but if you take a look at it again on page 68, I believe they used more then two samples to make that chart. I think every square on the two lines is where they took the sample out and took a grain size reading. If I'm correct on this, then in the 1400-1500 F range, there is almost a full grain size of difference between the two samples.

BUT, I believe I understand you now, that you never advocated such long soak times, and that 10-30 minutes was more then sufficient, correct? And also that in alloyed steels the time difference would make no practical difference in grain size because of the effects on limiting grain growth that alloys have?
 
Ghost Squire, as I suspected, your last post has confirmed that we did a lot of typing just to find out that we totally agree. What I am doing in my studies is in fact to find the shortest soak time to get the best results for my practices. Time in austenitizing is time that could be spent on other pursuits, and uses up fuel and electricity for me. It is all worth it if I can produce a better product, but how much is enough? That is what I am looking for. This is also why I was eager to get my hands on Phillip's steel, then I wouldn't have to waste, time, energy and materials to have a look at the extremes of such an outrageous soak time.

Now if I can only get around the polishing issues and get a good look at the samples:( . Perhaps I may find time this weekend. There was a difference in the amount of carbides, but there were still a good number of them there. This tells me that a good area to study now is to see how fine I can make them and where I can put them in the whole scheme of things. A 65HRC as-quenched with loads of very fine carbides evenly scattered throughout the martensite would be very nice.:D
 
Considering "fuel and electricity" ? I thought that was done only by us guys with industrial background !! "Very fine carbides evenly scattered" and you could call it something like CPM ! ...... They are building a new bridge here in town and it's curved ! As I photograph the construction and the curved beams I think of blade makers - just invent a new style knife with a curved blade , that will take care of the warping !
 
mete said:
Considering "fuel and electricity" ? I thought that was done only by us guys with industrial background !!

mete it was, until fuel prices went to a level that would break the bank from an hour worth of use...:( now even the one man shop has to be as efficient as possible to see a profit.

new bridge here in town and it's curved ! As I photograph the construction and the curved beams I think of blade makers - just invent a new style knife with a curved blade , that will take care of the warping !
Hey! You may be onto something, blades made specifically for left or right handed people!:)
 
Kevin R. Cashen said:
It is all worth it if I can produce a better product, but how much is enough? That is what I am looking for.

that's not that "good enough" thing is it, reminding of that other thread :D
it also reminds me of using helium to get to colder temps for quenching but is it worth it?
but in turn , is it? in the pursuit of the best :D
I know,, I'm toying with fire here :D

We covered a lot of this in Dan’s question about over soaking his 154CM, there as well we were overlooking the most important part the temperature, in both cases we are over 300 degrees hotter than you ever go in heat treating simple steels. At these temperatures grain growth will happen when solution is complete.

Kevin you mentioned my long soak with 154cm
so I did get grain growth from my soak time because of the temp needed for this steel, solely because of time( 2 hours in my goof), temp and grain being grain
specifically the temperature having to be over 1600F?

All the other charts deal, not with constant soaks, but increasing temps. from 1400F or 1600F to well over 2000F. Fig 8-10 gives no time at all just very high temperatures yet the text includes- "As the figure shows, these particles are able to effectively pin the austenite grain boundaries at temperatures up to 2000F

I'm still not sure if I got my question answered?
when this happened to me with the 154CM the steel was hard as hell
the only thing different was the soak time, 1 3/4 hours over my normal soak time of 15 min's at temp..
and then I had to use a higher temper temp to bring it back to workable for a knife edge.( ease of sharpening).
again, I had the spots in the finish on this one blade.

to sum up
I would enjoy the hardness that I got from the over soaking on the 154cm barring break strength if in-deed this was grain growth I was seeing in the finish , other than the inability to polish the blade.:grumpy:
this brings me to.
is it worth extra time in the oven just to have to bring the blade back in Rockwell at a still higher temperature in the temper,
waste of heat in both ovens to get the same rock..with spots :D

twisted morel of the story, watch the heat and timers:confused: :D
I may have to delete this post to make sence..
 
You're seeing spots before your eyes ? Like that Bugs Bunny cartoon ? Did you end up with continuous carbide in the grain boundary ? One place where you can see large grain is in sheet metal that has been bent or drawn and you get a texture on the surface called "orange peel" .
 
Ghost Squire, as I suspected, your last post has confirmed that we did a lot of typing just to find out that we totally agree. What I am doing in my studies is in fact to find the shortest soak time to get the best results for my practices. Time in austenitizing is time that could be spent on other pursuits, and uses up fuel and electricity for me. It is all worth it if I can produce a better product, but how much is enough? That is what I am looking for. This is also why I was eager to get my hands on Phillip's steel, then I wouldn't have to waste, time, energy and materials to have a look at the extremes of such an outrageous soak time.

:) It was worth it for me though because I learned a lot from this thread.

PS are those carbides the ductility enhancing carbides mentioned in the Verhoeven document?
 
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