Sciencemadness Discussion Board

Carbon Foam Refractory Made From Bread

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j_sum1 - 7-11-2016 at 12:37

Quote: Originally posted by unionised  
Quote: Originally posted by j_sum1  


As for an inert gas, I think CO2 is inert enough in this case.

I don't
C + CO2 --> 2 CO

Duh.
I hate it when I overlook the obvious.

unionised - 7-11-2016 at 12:43

Quote: Originally posted by BOD513  
Soaking the bread in a ferric chloride solution before carbonizing it would probably increase the degree of graphitization, and you could then just wash the iron ii,iii oxide off with hcl. This might make electroplating it easier.

I think that two wrongs have made a right here.
If you heat Fe oxides to a high temperature you end up with a remarkably insoluble mixed oxide- it's only slowly acted on by acids.

However if you heat them under strongly reducing conditions- such as you would get on a carbon foam, you will get metallic iron which is much easier to dissolve in acid.

aga - 7-11-2016 at 14:05

On to some actual Science ...

Is there a reaction that only works appreciably well with the presence of a catalyst that could be used as a test for this stuff ?

To be clear, a reaction that would be useable to do a Scientific test of this burnt toast.

For example: bread baked with FeCl3 and then pyrolised might catylise chlorinination of toluene, as anhydrous FeCl3 is said to do. On an effectively 'activated' carbon support, it might do it quicker.

That may be a really bad example, i dunno.

Some reaction where the effectiveness of the catalyst can be measured, also using things an amateur chemist might have available/on-hand.

BOD513 - 7-11-2016 at 17:10

Unionised,
I've seen papers describing "catalytic graphitization" which uses transition metal salts to lower the temperature at which pyrolytic carbons start to graphitize- this increases conductivity of the finished carbon beyond just impregnating it with a metal or oxide, and the metals can be washed/etched off afterwards with hcl. The temperatures used are still high enough to probably require a kiln, though.
Googling "catalytic graphitization" will give a bunch of results but here are a few

This paper describes using nickel nitrate and wood
http://authors.library.caltech.edu/47220/1/_JMR_JMR26_01_S08...

This one uses iron (paywall)
http://pubs.rsc.org/en/Content/ArticleLanding/2015/GC/c4gc01...

Video where a guy does it with toilet paper and ferric chloride solution
https://youtu.be/xQKpK1pEAjk

Edit- spelling

[Edited on 8-11-2016 by BOD513]

j_sum1 - 7-11-2016 at 17:28

Quote: Originally posted by aga  
Catalytic reaction converting CO2 directly to ethanol ?

Now we're talking business.

https://www.ornl.gov/news/nano-spike-catalysts-convert-carbo...


This seems exciting. But I perceive drawbacks.
The feedstock is CO2 dissolved in water.
The CO2 is converted to ethanol at an efficiency of 63%
So the product is a slightly fizzy and slightly alcoholic liquor. Now that sounds like it might have some applications [burp] but not in the field of making fuel -- unless there can be discovered a way of concentrating the ethanol in a highly energy efficient manner.


aga - 8-11-2016 at 01:11

Quote: Originally posted by j_sum1  
a way of concentrating the ethanol in a highly energy efficient manner.

Solar distillery ?

Robert Murray-Smith once again shows us that there's nothing new under the Sun.

Interesting that the addition of ferric chloride reduces the temperature required to achieve graphitisation.

BOD513 - 8-11-2016 at 04:55

He used to have a bunch of good videos on carbon foams but it looks like most of them are private now, which is a shame. I have a small kiln I can try this out with this weekend, but I have to find a canister that will fit- I've found out the hard way that al foil doesn't do much of a job at excluding air past 500C

Morgan - 8-11-2016 at 05:05

There's this tool wrap foil but it's relatively expensive.
http://www.use-enco.com/CGI/INPDFF?PMPAGE=854&PARTPG=INL...

How is Tool Wrap used?
"It is used in the heat treating process when a controlled vacuum furnace is not available. It saves time by allowing the hardening process to be done on the premises, without time lost due to parts being sent out for heat treatment. The tool, die or part to be heat treated is placed in an envelope formed by folding a sheet of Tool Wrap in half and carefully sealing the open ends of the envelope. This Tool Wrap envelope locks out the air and imitates the results which could be obtained from a vacuum furnace."

"Must the Tool Wrap package be air tight throughout the entire heating & hardening process?
Usually, if the Tool Wrap envelope is not airtight, the heat draws in excess oxygen which causes pitting and scaling on the surface of your part. However, if it is an odd shaped piece, you may need a vent during the pre-heat process. It is also important to note that there is no difference in uniformity of hardness between loosely or tightly wrapped pieces."

"The average operating temperature for our Type 321 Stainless Tool Wrap is 1850 degrees F, but it can work in temperatures up to 2000 degrees F. Overall operating temperature for Tool Wrap is very hard to state specifically because these temperatures are contingent upon the length of time in the furnace. At 1850 degrees F Tool Wrap can stay in a furnace without degrading for more than four hours. At 2000 degrees F Tool Wrap can perform successfully up to four hours. Of course, these are just estimates and users also need to be sure their furnaces are calibrated correctly. Other elements which can effect operating temperatures and overall Tool Wrap performance are contaminants within the envelope and improper sealing. So, there is no direct answer to what temperature Precision Brand Tool Wrap works at. Before responding to the operating temperature, the heating times need to be known."
http://precisionbrand.com/faq/tool-wrap/

[Edited on 8-11-2016 by Morgan]

Jstuyfzand - 8-11-2016 at 08:16

Quote: Originally posted by aga  
Quote: Originally posted by j_sum1  
a way of concentrating the ethanol in a highly energy efficient manner.

Solar distillery ?

Robert Murray-Smith once again shows us that there's nothing new under the Sun.

Interesting that the addition of ferric chloride reduces the temperature required to achieve graphitisation.


Does anybody have a source for at what temperature graphitization normally occurs without addition of catalysts?
The Wiki mentions 2000C for carbon fiber, but that seems a stretch :)

Morgan - 8-11-2016 at 09:22

Here's one company's outline for graphitization.
http://www.graphiteconcept.com/content/view/33/27/

Tidbit
http://www.nature.com/nature/journal/v177/n4501/abs/177239a0...

[Edited on 8-11-2016 by Morgan]

Jstuyfzand - 8-11-2016 at 10:25

Quote: Originally posted by Morgan  
Here's one company's outline for graphitization.
http://www.graphiteconcept.com/content/view/33/27/

Tidbit
http://www.nature.com/nature/journal/v177/n4501/abs/177239a0...

[Edited on 8-11-2016 by Morgan]


Thank you.

That video mentioned that with a metal salt graphitiziation occured at 800C, quite an improvement.
I wonder how the conductivity will hold up when he washes the iron out though.

unionised - 8-11-2016 at 13:29

Quote: Originally posted by BOD513  
Unionised,
I've seen papers describing "catalytic graphitization" which uses transition metal salts to lower the temperature at which pyrolytic carbons start to graphitize- this increases conductivity of the finished carbon beyond just impregnating it with a metal or oxide, and the metals can be washed/etched off afterwards with hcl. The temperatures used are still high enough to probably require a kiln, though.
Googling "catalytic graphitization" will give a bunch of results but here are a few

This paper describes using nickel nitrate and wood
http://authors.library.caltech.edu/47220/1/_JMR_JMR26_01_S08...

This one uses iron (paywall)
http://pubs.rsc.org/en/Content/ArticleLanding/2015/GC/c4gc01...

Video where a guy does it with toilet paper and ferric chloride solution
https://youtu.be/xQKpK1pEAjk

Edit- spelling

[Edited on 8-11-2016 by BOD513]


I didn't check the paywalled one, but there's nothing in the others which shows whether the active catalyst is the metal, an oxide or even (in some cases) a carbonyl.
However, the reality is that it's generally quite easy to reduce Cu,Fe or Ni to the metal and it's generally more difficult to graphitise carbon so, when you have finished and let everything cool, the free metal is a reasonable product, ad that's a lot easier to dissolve in acid.

ave369 - 10-11-2016 at 08:21

Quote: Originally posted by Jstuyfzand  

If its conductive it would be the best electrode for electrolysis on the planet, high surface area and cheap.


I think it's a pretty horrible electrode. Normal graphite electrodes erode and foul the electrolytes with graphite dust. This one, I think, will disintegrate in an instant.

Jstuyfzand - 10-11-2016 at 14:13

Quote: Originally posted by ave369  
Quote: Originally posted by Jstuyfzand  

If its conductive it would be the best electrode for electrolysis on the planet, high surface area and cheap.


I think it's a pretty horrible electrode. Normal graphite electrodes erode and foul the electrolytes with graphite dust. This one, I think, will disintegrate in an instant.


Depends on what you use it for, water electrolysis would be not so tough on them.
I think that carbonized bread would be less useful than for example Wood pieces.

Toady - 15-11-2016 at 11:54

Violet sin-you may wish to hold off on those PARTICULAR mushrooms.

Whilst I won't say 'yes eat them' I am more than willing to point towards species that I believe them to be so you can get a proper ID in books.

Some look like those of the Ceps clade, Boletus edulis, B.aereus etc.
The one with the dun-brown cap looks like a potential bay bolete (B.badius recently transferred to the same family as the red cracking bolete, so now B.badius syn. Xerocomus badius, and are excellent eating, as well as are the ceps family. The funnel shaped ones may be chanterelles if so do NOT waste those on trying to carbonize them, the only heat a chanterelle should ever encounter is that of the cook pot and the heat given off by a human body after having been cooked then eaten. So look em up, if you have better pics give 'em over and I'll have a wee look-see, for since a very very early age it seems that mycology was decided from on high, should a higher power actually exist, that it would be, along with the other sciences, one of my autie speshul interests. Mycology and botany were what I started out with, needing relatively few materials a toddler could not obtain.

My living grandfather (mothers side, mother is now dead, dementia, MS) was recounting to me shortly after her death about how when they sought to take me for walks in the wilds it was more me taking them for the walks, on a sort of nature guided tour, pointing out the different species, uses, edibility and poisonous characters. Actually, I taught myself to be able to read, first of all, using Roger Phillips' field guide, which mind you has a few glaring errors such as listing the blackening waxcaps (Hygrocybe nigrescens and H.conica) as edible. They are not, they are toxic although how severely so is as yet uncertain. Mycena pura, listed as edible contains muscarine and has poisoned a fair few people over the years.

But before I entered primary school, this and similar books, plus some herbals and other botanical guides I used, primarily however, Phillips', to teach myself to read. And so I am told, when I entered infant school the school teachers believed I couldn't read. Actually that was not the case, I was a fluent reader already, and being of course, of the emotional age, if not the mental age of a just post-toddler wee nipper, I was ornery as they come, and was REFUSING to read, because of course infant schools have books suited for infants. And they would not and doubtless could not provide books that would have befitted my reading level. Not that they knew, for I could not at that age explain WHY I was not reading, that it was to me, grey, dull, ashen-tasting prechewed swill; for I wanted not 'the cat shat in his hat' but treatises on fungi, botany and herbal&orthodox medical tracts.

I just couldn't explain, and had both a toddler, and frustrated autistic toddler's level of communication. And even if I HAD explained perfectly, most likely, looking back, I would never have been believed and taken seriously.

Anyhow do feel free to come at me with mycology queries and I shall answer them as best I am capable, and where edibles are sighted, I shall point the relevant species out so you can ID them thoroughly in the proper texts, either in deceased tree format or online.

Few things I love better than to go drag myself up at 6am in the spring, when its going to be first light just about the time I finish getting from A to B (where A is my home and B is the destination fields and woodlands) and not return until 2am the evening coming, with a big basket full of supper. If I have favourite edibles, ceps and their closest relatives are high on the list, but absolute favourites of favourites if I had to pick a handful would be giant puffball (Langermannia gigantea) as well as quite a few of the other large puffballs, sulfur polypore/chicken of the woods (Polyporeus sulfureus, delicious as delicious comes prepared like the puffballs, sliced thickly, then dipped in a batter made from eggy bread covered in whipped eggs and batter, brown bread for both then fried in butter, not the oil/butter mixed spreadable muck, but real hard as a brick when cold salted butter, and only butter. And GOOD butter at that:)), as well as parasol mushrooms (Macrolepiota procera), Lactarius deliciosus, the safron milk cap, who's species epithet is well deserved, when slathered with a bit of butter, a sprinkle of sea salt and black pepper then roasted on a spike under the grill or over the gas flame, hedgehog fungi (Hydnum repandum) as well as Camaryllophyllus (sp?) pratensis syn Hygrocybe pratensis, the meadow waxcap, and two other waxcaps, the scarlet hood and the scarlet waxcap. HH.punicea and H.scarlatina respectively, if I remember right, spelling might be a bit off, since I've just had my evening doses of morphia, oxy, clonidine, tizanidine (another imidazoline related to clonidine, less hypotensive, shorter acting, less powerful by weight but much more so in effect, for spasticity due to nerve damage in my leg that by now is decades past the point of ever having a chance to heal, gabapentin (ew) and chlormethiazole, an oddball, unique, with no relatives in the realm of pharmacy, thats a derivative of B1, minus the pyrimidine portion and the resultant thiazole-2-ethanols -OH group replaced with a terminal chlorine atom. Nothing else like it in the realms of the pharmaceutical dispensaries, although easy to make from thiamine (vitamin B1), which shortly I shall post of in the bio section so that I have made my first contribution to the forum rather than solely queried or chimed in with input to the threads of others. Its an old, old old drug, mainly used for alcohol detox since it inhibits alcohol-, although not aldehyde dehydrogenase and thereby preventing abrupt dropoff of the plasma levels of ethanol from an alcoholic's last booze-up and abrupt DTs. Not listed for seizures whatsoever in the BNF but all the same its what I take and it performs with both great rapidity and most admirable and reliable efficacy. Beginnings of a seizure, during the initial part (mine are myoclonic leading into atonic usually although rarely myoclonic alone and sometimes solely atonic, leading to, respiratory control aside, total voluntary muscular paralysis.) Stuff smells funky, its volatile, its a total complete and utter swine to salt and it cannot be stored in plastic containers, although IMO teflon would be alright, or allowed to contact anything made of or with plastic that you care about, because the free base of the stuff eats plastic like donald trump eats faecal matter swarming with flies and writhing with his fellow blowfly maggots:D

violet sin - 16-11-2016 at 22:48

new cooker... Check, just a few min, some rusty scrap and drywall screws.

IMAG8270.jpg - 1.6MB IMAG8281_1.jpg - 340kB IMAG8265.jpg - 1.3MB IMAG8290.jpg - 1.3MB

Been messing around with the first samples I made, soaked one in crude copper sulfamate and got some copper sponge to grow across/through the porous carbon. Its baking now. Third time through. 1) no conductance, 2) meager conductance in several spots, 3) still cooling. Thinking electroplating it slowly at very low amperage after improving the overall conductivity of the sample. Small metal dendrites may be fun.

Decided would try copper doping first as 1, soluble Ni for later and prety much only when needed, 2. Ammonia + Copper salts = soluble cellulose for the next trial.

Piece #2, pre carbonized, is soaking in Ni sulfamate and has been wrapped in thinned out cotton ball material. Tied with a fillament of same twisted to make thread. Thinking of adding a honey glaze or cellulose washes to tighten it up and add an even coating. After reading for a bit came across this VVV :)
________
Facile synthesis of graphene, graphene derivatives and abrasive nanoparticles and their various uses, including as tribologically-beneficial lubricant additives
CA 2857947 A1

https://www.google.com/patents/CA2857947A1?cl=en

" Test 5... In another method of synthesis of nanoparticles,
powdered sugar, hand sanitizer, isopropanol ("99%), baking powder and mineral oil ("Walgreens Mineral Oil Intestinal Lubricant"

... were combined in a flask. The flask was heated with a direct flame to convert the sugar to graphitic carbon. The top of the flask was stoppered and tubing directed the reaction gas stream containing the vapor-exfoliated graphene scales to bubble into a water bath.

A metal spatula... to collect the reaction product .. after being transported by the vapor stream. ... was then wiped against a carbon TEM grid ... was observed using a ... the images. These structures are similar ... to as holey carbon or lacey carbon... shows a fairly large, uniform graphene sheet morphology... shows a large graphene sheet morphology with a tendril ...shows folded multilayer graphene sheets... show thin strands of graphene connecting larger sheet areas... showing a higher magnification of the multiple layers of such a strand.
________________________

Now I didn't add the photos, but good lord that is an easy one eh? Also used were things like honey, high fructose corn syrup, and whole host of sweets, inver sugars, etc.

Other papers I came across were likewise interesting. For instance the carbonization of bacterial cellulose, including acetobacterium(sp?) mat. And one that had freezedried bacterial cellulose backfilled with siloxane of some variety( forget the specifics, was 2am). Heated at some point and made flexible conductors...
http://www.nature.com/am/journal/v4/n6/full/am201234a.html

graphite film from bacterial cellulose
http://scitation.aip.org/content/aip/journal/jap/68/4/10.106...

Carbon aerogels from bacterial cellulose > lithium ion batt electrode
http://pubs.rsc.org/en/content/articlehtml/2014/ra/c3ra47853...
-VS

We did eat those mushrooms, look forward to it each and every year. Been doing so since about 25 yrs ago

[Edited on 17-11-2016 by violet sin]

mayko - 17-11-2016 at 11:54


Someone brought some nasty BlunderBread hamburger buns to my 4th of July cookout and they've been sitting in the fridge since. Finally, a use for them!

Here is related research from the same team, published last year, with an emphasis on supercapacitors:

Deng, J., Xiong, T., Xu, F., Li, M., Han, C., Gong, Y., … Wang, Y. (2015). Inspired by bread leavening: one-pot synthesis of hierarchically porous carbon for supercapacitors. Green Chem., 17(7), 4053–4060. http://doi.org/10.1039/C5GC00523J


Quote:

Hierarchically porous carbons (HPCs) show great potential in energy storage due to their high surface area as well as short ion transport path derived from the interconnected porous framework. However, most existing protocols highly rely on nanocasting and soft-templating, which usually make the use of specific raw materials and thus their industrial application unfeasible. It still remains a big challenge to build HPCs from crude biomass, which is abundant on the earth, through a simple one-pot approach. Inspired by leavening of bread, we design a strategy to fabricate HPCs with three-dimensional (3D) hierarchical pores consisting of macro, meso, and micropores. The “leavening method” is conducted simply by mixing the biomass with KHCO3 followed by elevated temperature treatment. Besides the well-defined hierarchical structure, the as-prepared HPCs also exhibit notably large specific areas (up to 1893 m2 g−1). It is noteworthy that this “leavening” strategy is widely applicable to most of the biomass derivatives and biomass, including glucose, cellulose, chitin, starch, rice straw, bamboo, etc. When evaluated as supercapacitor electrode materials in two-electrode test systems, the as-prepared HPCs exhibit an excellent electrochemical performance: a specific capacitance of 253 F g−1, with almost no capacitance loss after 10 000 cycles.


(yes, I am procrastinating at work by skimming through every issue of Green Chemistry; stop judging me.)

Regarding microwaves, I've never met a form of carbon which doesn't arc and spawn plasma balls when irradiated. The best for this effect is burn newsprint or burn cork, but wood charcoal, pencil graphite, soot, even nanotubes will also work.



Attachment: Inspired by bread leavening- one-pot synthesis of hierarchically porous carbon for supercapacitors.pdf (2.2MB)
This file has been downloaded 482 times

aga - 17-11-2016 at 12:10

Excellent stuff VC !

Burnt Toast is the Future.

elementcollector1 - 19-11-2016 at 07:53

About to try this in a dormitory oven. So far, my procedure is:
-Wrap slices of bread in aluminum foil. I'm going to test the effect of nonuniform thickness (read: that awful end piece of the loaf) versus uniform thickness on mechanical properties.
-Bake wrapped bread at 500 F (260 C) for 1 hour.
-Remove, and test.

Future testing will include attempting to make a carbon reactor chamber for a high-temperature furnace, as the stuff I'm currently using for insulation isn't that great.

The brand I'm using is Schwebel's Giant Bread, which appears to be a knockoff of Wonder Bread.

Results in an hour!

elementcollector1 - 19-11-2016 at 09:29

Well, here they are!

Some photos of the bread, pre-baking:





The slices were individually wrapped in foil packets, as shown:


Once this was done, they were baked at 260 degrees C for exactly one hour. Then, they were taken out of the oven and left to cool. Once cool, they looked like this:




As you can see, the porous structure and general shape is retained. However, a little bit of the volume was lost (it's a bit hard to see in this photo):


The resultant product behaves like a firebrick, in that while it is quite resistant to breaking, it abrades easily. Finally, the two samples were snapped in half to test how they would fracture:


To my surprise, they snap cleanly down the middle! This indicates good structural rigidity of the carbon foam.

Electrical results will follow later, and temparature results may have to wait for now (no access to a blowtorch). Still, this was an extremely easy experiment to carry out, and produces a rather useful material!

EDIT: Electrical results in! This stuff has a resistivity of, at the very least, 3.94 x 10^5 ohms per cm, putting it about on par with cement or limestone in terms of resistivity.

[Edited on 11-19-2016 by elementcollector1]

Jstuyfzand - 19-11-2016 at 10:34

It amazes me that 260C achieved this.

Great work!

aga - 19-11-2016 at 12:04

Superb work there elementcollector1 !

It would be great if anything can be added before/during/after to make an excellent catalyst or something.

violet sin - 19-11-2016 at 13:06

Thought 1) So what if we soaked the once charred bread in epsom salt sol. In a form fitting container, then dosed the lot with ammonia/lye to drop Mg(OH)2 into the carbon scaffolding and re-baked it? Maybe something more structural could be produced for fire brick like material. Just a thought. Also, sodium aluminate, TSP or calcium acetate could be candidates. Would be wonderful to use a conventional oven to make bits for a hobby high temp oven.

2) still working on the cellulose coating project. Dollar store ammonia is WEAK sauce. You can stick your nose right in the jug and barely smell anything = waste of $. So I went to a True Value hardware stor and got "magestic extra strength ammonia cleaner" for 3$... Got home and read MSDS,... A whopping 4% con. in that mix. It's going back today, and I will be buying a jug of janitorial ammonia @ 10% strength. The idea here is to dissolve cotton balls into sol. add the preburnt bread and acidify to drop cellulose in the pores/on the surface. Could potentially add a LOT of surface area if it works.

I'm still away from home so it sux to buy stuff again that is laying around the lab, but darnit I want to know :) the family isn't in town and I have the day off, a bag of briquetts and that new stove ... Gonna get me some answers. Along with some more bread kinds to try. The french bread from safeway was good, but sourdough had huge irregular pockets that made for a dissapointing outcome when sawed into slabs. Check back later today, hopefully with more info than ponderings

Morgan - 19-11-2016 at 13:39

Maybe some water glass would be something to try.

"Water glass was defined in Von Wagner's Manual of Chemical Technology (1892 translation) as any of the soluble alkaline silicates, first observed by Jean Baptist van Helmont circa 1640 as a fluid substance made by melting sand with excess alkali."

Refractory use
Water glass is a useful binder of solids, such as vermiculite and perlite. When blended with the aforementioned lightweight aggregates, water glass can be used to make hard, high-temperature insulation boards used for refractories, passive fire protection and high temperature insulations, such as moulded pipe insulation applications. When mixed with finely divided mineral powders, such as vermiculite dust (which is common scrap from the exfoliation process), one can produce high temperature adhesives. The intumescence disappears in the presence of finely divided mineral dust, whereby the waterglass becomes a mere matrix. Waterglass is inexpensive and abundantly available, which makes its use popular in many refractory applications.
https://en.wikipedia.org/wiki/Sodium_silicate

aga - 19-11-2016 at 13:52

As seen Done, this is the perfect Do-For-Yourself-and-See experiment.

No need to wait on a superior Chemist who has access to advanced materials, such as
Bread, Tinfoil and Fire.

Words play no part in this, as Anyone can try it for themself.

Online words are so easy, compared to actually doing something.

Words after Doing Something are far, far more interesting, as this thread shows.

Nobody on this planet has any valid excuse when it comes to over-toasting bread.

careysub - 19-11-2016 at 15:54

I am glad I dug up that original item about making carbon refractory with kitchen chemistry! It looks like it is going to be one of those long threads.

violet sin - 19-11-2016 at 18:08

I would have to agree. This is accessable, cheap, quick and fun. Not to mention the multitude of variations in feedstock, treatments, and intended uses. Truely seems like you can tailor the stuff to your needs.

Just brewed a batch of coffee and wondered about the leftover grounds... AC perhaps? Same with rice grains or friggn gold fish crackers for that matter. But my travel-with-me hobby stuff is only electronics and tools. So I have no way of testing the actual activation level of the produced carbon. I'm having to buy all my chemicals for this from hardware stores, which is nice as they are low tech and widely available. That can't be said for so many other chemistry topics.

There are some interesting vids on youtoob from individuals with little knowledge, about graphene production, buzzwords galore. Many buy graphite and "intercalate" it with acid, prior to microwave "expansion" or "exfoliation". All the while "few layer graphene" is just on the other side of the blender, as it were. failure = "graphene oxide" when some dont see the conductivity they crave.

Regardless of all the nonsense, microwave heating of the carbon scaffold causes high temps in micro regions during electrical discharge in the 1000℃ area results in graphitic ordering. Those patents with chelatants imbeded to hold metal cations had a microwave step. Causing reduction of the metal salt or oxide, dissolution of carbon and precipitation of graphite on cooling. (One) Reason why graphitization is lowered from >2000℃ to 800℃. Any one have a spare/chem microwave to try. It would still have to be sealed from O2. Perhaps a sacrificial yogurt container flushed with a small amount of volatile hydrocarbon could exclude oxygen. Your carbon could arc its heart out and then be tested for conductivity increase.

Any how back to actually doing the science, not just postulating ideas. I will edit this post later tonight with valuable data from the field. Or.. outstanding failure, either way something will come of it.
_______________
Starting to smell toasty :) got a pile of things crammed into the SS cup this time. Soggy bread with boric acid, same with Mg(OH)2, charred bits with some of each, same bread with nothing on it, couple cotton balls and a couple mystery items to show when its all cooked. Fingers crossed for excellence.

[Edited on 20-11-2016 by violet sin]
_________________
Just a touch over 2 hrs in charcoal briquette fueled heat, choked a good deal by stainless pot cover( thanks thrift store 1.5$). Results are:

control toast.jpg - 914kB Mg toast.jpg - 945kB
B toast.jpg - 926kB bannana.jpg - 1.1MB
cotton ball.jpg - 602kB wasp nest.jpg - 896kB
wasp nest II.jpg - 744kB
Control toast, Mg toast, B toast, bannana, cotton balls, wasp nest, wasp nest II.

This super cheap white bread is pretty hard without modification, the two test dopings were sub optimally attempted. Room temp saturation of well water by epsom salt and boric acid separately. Test slices were set in plastic liner and doused with each. After soaking, ammonia (10%) was dribbled in Mg sulfate side to ppt. Mg hydroxide in bread pores. No attempt was made to wash, but it was drained. Then both were set in aluminum boats on top of my stainless cover to dry a touch. Probably stupid as it soggied them up too. Pre-charred bits of sourdough were dosed with each dopant in a similar manner, except this time the boric acid was dissolved in MeOH. Both dried with white staining.

The boric acid toast doesnt seem to be noticibly affected structurally. Perhaps a touch softer. The Mg(OH)2 toast seems a touch stronger and the pre-charred seems noticibly stronger/slightly heavy.

The cotton balls are nondescript, charred all through, still feel roughly the same. Nice because they offer a compact/moldable shape(pre fire) and are absorbant. Could be fun on a few levels.

The bannana was on a whim, figured they have a ton of fiber. However shrinkage leads me to believe that freeze dried would be the way to go here. It looks pretty structurally sound, but like water loss defeated this on shrinking as it cracked but bits were strong. It also had a nice blue tinge fading to gold in some areas. Ravens feather if you will. The center was more large pores and the exterior had smaller fiberous areas. Could be really cool if structure was preserved in cooking = freeze dried first. Not in my capability.

And my favorite effort, a portion of a yellowjacket comb stolen from a colony dying back for the season. All empy celled and unattended. I failed to safely cook them. Like an idiot, I pulled the tin out by had when nothing convienient presented it self to aid extraxting it = dropped from 2" up and fell over. ALMOST made it, lol. But the sample survived enough to see structure was preserved, surprisingly strong and dellicate simultaneously and easily catches a breeze.
____________

Thoughts:
dont get your bread soggy trying to dope it with structural modifiers. A single piece of bread weathers poorly in a round tin. Seems reasonable to cook them flat if you want something stackable for a refactory lining. Better yet toast a section of un-sliced bread then quarry you shape from that. It is more practicle to strengthen it after shaping. Only down side is the interior doesnt get coated if all the cells are charred closed. Maybe a normal(edible) toasting followed by an alcoholic suspension of sorts. Still soak into all the pores, but the shape is possibly preserved and quick(er) to be dry- untested as of yet.

Reinforced bread feels like it could be good structurally. Slabs of such might be able to be permanently assembled with a (honey/syrup/starch)
binder if it could be re-fired.

The cotton will have to be toyed with more, but so far I like it. Some of my reading indicated cotton ball cellulose were difficult to dissolve because of more crystalinity. I wonder if that translates into easier to char towards graphite? Metal salts(liquids in general) would deffinitely absorb on them easily. no direct use yet.

Wasp nest thing opens more windows. Hard to come by and delicate, though many other natural shapes are more common and robust. If the back closed portion is sawed off, as I did, the open nature, low air resistance and relative strength in that direction could make effective catalyst support. Cars prove the shape is right. Nowhere near the same force could be supported, but I can see it working in some lab sized model.
______

Next on the to-do list:

1) glue slabs together with sugar, starch etc.
2) attempt to wrap a charred bit with cotton and reinforce with MgO.
3) try just sugar etc. on edible toast as a sealant. (Close the structure off)
4) paste of sugar & graphite powder

Rolling around for later
-sodium aluminate, sodium sillicate and sodium phosphate on char bit.
-Magnesium citrate in alcohol, structural dopant.
-seeding graphite growth with lubricating powder from hardware store
-microwave treatment to test possible increase in conductivity from graphitization
-insects whole, freezedried from pet store.

[Edited on 20-11-2016 by violet sin]

[Edited on 20-11-2016 by violet sin]

probe meter check 1.jpg - 564kBsurprising toast controll 5.jpg - 681kBIMAG8387.jpg - 741kB

aga - 20-11-2016 at 10:15

Awesome efforts there violet sin !

The wasp nest is intriguing in that it managed to retain any shape at all.

Car catalytic converters definitely use the honeycomb pattern.

The idea of toasting then adding X then toasting again is probably a good one.
Dunno why, just 'feels right' somehow.

My last Toast attempt with CaCl2 gave ~20 ohms resistance - maybe that can be improved on.

Density is probably a thing.

Maybe toasting once, powderise (smash up) then compress with a hydraulic jack, then toast again would do something different.

Think i'll try that after the trophies are finished.

Edit:

Was thinking about the cotton + honey thing and BANG the word 'Baclava' arrived !

Wafer thin sheets of wheat-pastry infused with honey !

Dragon's Hair candies too ! (2048 strands of honey & cornflour)

[Edited on 20-11-2016 by aga]

aga - 20-11-2016 at 12:32

Odd. Went looking for carbon in a microwave and found this :
https://www.youtube.com/watch?v=Q176cmHGywo

Ground charcoal in a microwave.

The carbon 'sparked' a bit as reported in the video.

With the pyrolysed bread the arc light was so intense you'd need a welding mask to even look at it for more than a split-second.

violet sin - 20-11-2016 at 14:43

found a fun substance to try this time. Went to the dollar store again to get some little tuppers for doping trays that can seal ammonia in. Had in mind something like homogenous solid or regular enough on the individual particles, that a sugar wash might glue them. Had tapiocca prills in mind. Found green blocks of floral foam. label says "caution: flammable. Keep away from open flames"... googling, I believe they are phenolic foam, a delightfully regular, small pore, easily shaped and cheap materia. Available were one large ish block, four smaller blocks, rings or cones of which I purchased the first two.

All said and done, I have spent less than 50$ with various, and at times unneeded, dopants included. Bread cheap, cooker free, various bits n charcoal and aluminum foil for cooker <10$.

The goal for today is to try and make something actually usefull instead of testing different forms.

holy flying pyrex :) that was a crazy vid. Still wish people would seal the carbon from air while trying this...
------------
Crazy stinky fumes going on. It was quite dense and yellowish. Just stayed up wind. Fume caught fire for a bit, then seems to have subsided. Hope to be past major burn-off at the 1 hr mark now. Shooting for two like before.
-------------
Ahhh dissapointment, I know ye well. As it turns out,... my hopes of greatness were dashed. The stuff went from a block that barely fit in my container to about 1/50th of that. Bummer. My guess is that it got too hot too fast and 2hr may be too long. Reading a couple papers about phenolic foam indicated they use REALLY gradual temp increases, 20℃/hr, not possible for me in this setup. Going up as far as 900℃ like that, then 100℃/hr to max temp of 1,400℃.( the max temp checked, min was around 350℃). But still it reflects a slow transition.

On the bright side it is porous and wettable, so doping is a possibility.

IMAG8391.jpg - 1.7MB IMAG8392.jpg - 1.7MB IMAG8409.jpg - 1.1MB
1) as bought, 2) stuffed in, 3) remains

There was a paper divider which the mass stuck to. It is quite fiberous where it stuck to the walls and paper. Side note, cotton covered in sugar water seems sturdy. This was on the other side of the paper divide. Cotton wrapped around stainless tube, covered in sugar water/sugar. wont come off the tube easily.

Spent the time to carve a nice crucible and lid in preparation for a sucessful outcome. Set back to trying samples with reinforcement to see how to modify it to save my effort. Something to give structure but not close all the pores. Dissolved cellulose maybe?

IMAG8402.jpg - 914kB IMAG8403.jpg - 862kB

Foam test II: another as purchased small block aranged differently. some wire mesh was added like a hammock across opening that keeps the SS cup about 4" above the coals instead of dirrectly on. Coals are dying out some anyway, as the rain starts again. It was also wrapped in foil inside the cup with a bottom spacer.

The crucible I hope to save just fits in the tupper so a dosing is possible. Blue copper/ammonia complex is waiting to eat cotton balls, but I have major doubts I will get an acid wash too deep in the pores. So may just ppt cellulose on outer edges. It may also attack the resin. Unknown as of yet. Small bits will be tested if I can. Running low on charcoal and time.
___________
1 hr residence of second foam block ~4" above coals = no physical changes apparent. Still green and new looking, but the odor isnt plesant. I added the last of my charcoal, lowered the cradle some and set the SS cup against side of cooker leaning on the cradle. So it is closer, like 2-2.5" above coals. Maybe 3" considering the spacer, between foam and coals.

Looks like a narrow window between nothing changing and failure.

Another hour and perhaps 30-45 min elapsed at the lower position. Was raining so left it past the timer. Nada, no change again. Green and new looking. Last of coals burning out and time to put stuff away.

I find this quite frustrating. Most papers on reinforcing phenolic resin foam obviously do it in production, not after the fact. Seems like a usefull product if it would carbonize like bread. First attempt at schweizer's reagent has littile visible effect on cotton or paper towells, nice blue though. Material for second attempt is settling after first rinse. See if it does any better with a stronger sollution in terms of copper present.

Could just be a dead end for my equipment as I still need to find the sweet spot temp wise even if I do manage to strengthen the stuff. Low temp decomp of additive, prior to foam failure is required. That will be some stinky science to undertake. papers suggest phenolic foam may be stable to 200℃ so a long roasting around 150 with starch is an option. Prob need that just to drive off the water that put it there. Could also just lead to a condensed wad of crud as they shrink together. Fast and cheap is the goal here, not mind numbingly time consuming and frustrating. Then again, if something this consistant and available can be mastered, it will make a nice refactory. (Maybe just use poundcake and forget this mess)



[Edited on 21-11-2016 by violet sin]

Morgan - 20-11-2016 at 17:48

Perhaps of interest although not a foam.
https://www.youtube.com/watch?v=ki1aCdkMSeo
Maybe it would be possible to make flexible carbon foam fiber hybrid of some sort.

DrP - 23-11-2016 at 06:33

Hi aga - I would try the pyrolysis under an inert gas like Argon or Nitrogen. The article suggests that and I would expect that it would stop the disintegration from oxidation. Maybe that will give a more sturdy and flexible char?

I might try this out myself.

DrP - 23-11-2016 at 06:34

Sorry - long time since I visited this site - I just realised I posted this suggestion without reading the entire thread. lol. sorry.

I still might try it under N2.

aga - 23-11-2016 at 12:49

violet sin is currently at the Cutting Edge on this one, and it wasn't even my idea to begin with.

All so very easy to do if you can make Fire and have access to Bread.

Access to inert gasses are entirely optional.

Ability to exert Effort and actually do this simple-1-hour-thing is mandatory, or your bread remains just bread.

Without the Effort required to try it with and without an inert gas, we will never know if it makes a difference to the outcome.

[Edited on 23-11-2016 by aga]

aga - 23-11-2016 at 12:54

@violet sin:

The green stuff is called 'Oasis' and is used in flower-arranging.

A bit of googling and it seems that 'Oasis' is a 'phenolic foam' which can be a bit of a mix of stuff.

MSDS copied here : https://gorgeousandgreen.wordpress.com/2011/08/16/msds-flora...

Maroboduus - 23-11-2016 at 16:50

Phenols are awfully stable. Could be a lot of the structure just de-polymerizes and gets emitted as vaporized phenol.

This is a guess.

However making phenol by potassium fusion at around 300C used to be a common organic chemistry class lab assignment, so the stuff really holds together at high temperatures.

Don't know what vaporized phenol smells like, but if memory serves phenol can corrode flesh without causing much pain, so be careful.

The MSDS for this stuff doesn't look too bad, but they're not really addressing destructive distillation.

BTW: You have impressive foam carving skills. On first glance at that picture i thought, "Where did she buy THAT?"

j_sum1 - 23-11-2016 at 16:56

Quote: Originally posted by Maroboduus  
BTW: You have impressive foam carving skills. On first glance at that picture i thought, "Where did she buy THAT?"

"She" has very manly hands. (As well as an impressive beard IIRC.)
But I concur. Nice work all round VS.

Maroboduus - 23-11-2016 at 17:10

Quote: Originally posted by j_sum1  
Quote: Originally posted by Maroboduus  
BTW: You have impressive foam carving skills. On first glance at that picture i thought, "Where did she buy THAT?"

"She" has very manly hands. (As well as an impressive beard IIRC.)
But I concur. Nice work all round VS.


Yes, I noticed the manly hands, but wasn't sure if that meant a man or a woman who might be sensitive about her masculine meat-hooks.
Sorry for the gender confusion, violet sin.

Thanks j_sum1.

violet sin - 24-11-2016 at 00:58

Yes sir, I have a nice size beard. But of course no ofence was taken. Not much time today, I did get charcoal and a cheap angel food cake.

Today's charcoal was the lump mesquite natural kind. Just chared wood bits of various size. Harder to estimate fuel use and heat and still its pretty easy to eyeball a comfortable hot but not blazing temp. For any one keeping track I bet single press lump stuff would be easier to record.

The first run was 2hr usual but had a slower start as the cup went in right when the fire started, no preheat. Results were actually quite strong where it didn't stress crack under strain. Kinda spawling off shallow flakes were noticed.
angelfood 1b.jpg - 59kB angelfood 1c.jpg - 181kB angelfood 1d fractures.jpg - 103kB


The second run, I considered why not for a shorter duration. Wanted to take it down to one hour and see if I could still get stiff carbon without breaking, but went for the safer half hour. If it were only partially carbonized then maybe a 10-15min break might ease strain. But it was already carbonized, with less cracks on first inspection. Have not had a chance to cut either yet or any other testing.
angelfood 2_1.jpg - 224kB IMAG8443.jpg - 1002kB

Pretty regular, shrinks a noticable amount. Not too bad. More work will have to wait. Cooking a chunk of bolete stem, check tomorrow.

IMAG8447.jpg - 2.1MB IMAG8448.jpg - 1.9MB
1) two hour angel food top, one half hour bottom
2) close up of knot of bolete stem above the half hour angel food cake

So the fungus bit makes it aparent that nature is far better at this than a baker. I have one in mind to fell
IMAG8431.jpg - 1.6MB
Happy thanksgiving everyone! Enjoy family, friends and fond memories.


[Edited on 24-11-2016 by violet sin]

DrP - 24-11-2016 at 02:17

OK - I was wondering what the inclusion of some powdered Ammonium Polyphosphate added to the bread mix would give in your resultant char. It should promote further crosslinking in the char. Whether this will make it less flexible or stronger and more flexible I do not know - but it should improve over all charring - we use it as a catalyst to cross linking in chars.

Some kind of gassing agent could help you play around with cell structure and final size of the foam. With some APP and a suitable blowing agent I recon that char would swell to a few times it's size.... maybe.

I think the APP would need to be what is sold in industry as Phase II - which I think has polymer chains around 1000 to 2000 units long. The theory is that it reacts with -OH groups and cross links via a condensation. With the systems I use we add pentaerythritol to provide further carbon source and the -OH groups, but there might be enough functionality in all the bready proteans to act as cross linking sites anyway.

Violet - can you get hold of APP?

3DTOPO - 4-12-2016 at 17:43

I wonder if carbonizing wool might work better than bread?

(please spare me the lecture Aga)

violet sin - 4-12-2016 at 19:05

Cotton fiber chars right up nicely. Iv'e been busy with work and fam, had to settle for reading this last week. Had no phosphoric acid, so bought ospho corrosion stopper. 45% phosphoric acid + dichromate, the green stuff. Also bought concentrated sulfuric drain opener( remembering the sugar demo from middle school)... It does not play nice with fungal tissue, leaves a liquid suspension instead of preserving any form.

I did manage to fell that massive bolete, froze the cap and stem separately. Trying to find a way to freeze dry the some'bitch. But it will take a large pressure cooker to take the cap whole, and my vac is weak. Gonna ha e to keep that in the freezer untill arangements are made.

Super time crunch right now, check back in later with other thoughts, tests and results not listed.
--------

it was noted that you said wool. I drew a correlation to cotton as also being thin and dainty material. yet it carbonizes nicely.

[Edited on 5-12-2016 by violet sin]

3DTOPO - 4-12-2016 at 19:09

P.S. I said wool, but what I really meant was felt (wool or acrylic fibers). I think acrylic might carbonize very well (based on my experience with burning out acrylic SLA 3d prints).

Unlike a lot of plastic and foams - acrylic doesn't melt - so it should hold its form...

[Edited on 5-12-2016 by 3DTOPO]

DrP - 6-12-2016 at 02:48

Looking forward to seeing what the phosphoric acid does. :-)

aga - 19-12-2016 at 09:40

Lidl have finally decided to stock a stainless steel carbohydrate pyrolysis kit with 2 reactors for €8.99 (just need to drill holes in the lid).

They also sell the raw chemical feedstock (bread!)

tins.JPG - 92kB treated.JPG - 72kB

The jar on the left has about 6 slices of a Bimbo bread analogue in it, the smaller one on the right has 2 slices soaked in a Zn(NO3)2 solution.

smoke.JPG - 78kB

Simply stuffed both tins into a charcoal fire.

Overloaded i know, as the tiny barbie is way too small for both tins.

flames.JPG - 94kB

After about 30 mins the smoke coming out of the tins caught fire and burned for around another 15 mins.

after.JPG - 93kB

The result of the untreated bread is pretty much as expected - ceramic-sounding bent carbon tiles.

Oddly the resistance is in the 1~2 kilo-ohm range per cm.
On the first go it was at 20 ohms. Damned flukes !

The zinc nitrate treated bread gives a much finer and powdery carbon.

Bashed it up and added HCl to dissolve out the zinc.

Currently filtering/washing a lot to remove the HCl and zinc chloride.

JJay - 19-12-2016 at 13:14

Every time I read about this, I'm surprised that the product is such a poor conductor of electricity. Does the bread still bend if you pyrolyze stale bread?

violet sin - 19-12-2016 at 20:28

I have to say in this one thread specifically, doing is friggn easy and leads to FAR more productive afterthoughts. I don't see why people keep bitching about being nudged to throw in and participate. You will not get exactly how to improve or substitute unless you have done it.

Its clearly one thing to imagine wrapping some bread in foil, its another to see it try to fold and wad up. It sounds really easy but there are lessons to learn. Some members first run may be 1000% more sophisticated than your first run, no matter. We all have diff heat, wrap and bread.

Every batch of toast I tried to fint in several things and mods at once. After each run, I'd sum up observations and plan again. Plenty of "ideas" were basically garbage, because of impratical methods, numerous steps, poorly behaving materials and all mamer of issues. You don't want to spend all the time and 14 steps to get to nothing... But if no one does a 14 step optimization we will never know if there is a pot-o-gold at the end of the rainbow. There is NO gauranteed paycheck/prize/material there unless you a) find one through experimentation b) poorly copy some one elses hard work.

I have plenty of ideas, now waiting on ancilary equipment/chems to be made. I also tried a bunch of diff materials to get a feel for the process. Can only plan a little farther than you can see. Not everyone has the time or space to set up distillation equipment etc. Required from serious experiments. Amlost no one has a cop out excuse for putting an already owned food material in a commonly used food wrapping in an existing piece of machinery in an already functional setting. ( horrible sentance, I know, but functional in a sense). buck up, aga's got a point. This has been super fun, despair not.

** And I am not aiming to seriously chastize any one. just a reminder it's not a slap in the face to be nudged into activity **

[Edited on 20-12-2016 by violet sin]

3DTOPO - 19-12-2016 at 21:02

Quote: Originally posted by violet sin  
I have to say in this one thread specifically, doing is friggn easy and leads to FAR more productive afterthoughts.

Personally, I have professional carbon foam boards with a graphite hot face for my vacuum furnace, and don't have a need for any more carbon insulation at this point. But it is still a subject that I find interesting, so are you suggesting that people like me not chime in with ideas?

Like I offered the suggestion of using acrylic felt, is that so wrong?

violet sin - 20-12-2016 at 04:57

Well, I'm glad you have the use of some real tools, thats awesome :) From my tests, bet acrylic felt would have a tight window to retain any form. Would likely be hard to control temp well enough with out a lot of trial and error, or a nicer setup than coals. Lol. Bare minimum a hotplate, stainless pot and lid with Al foil to spare. Maybe a toaster oven. But your nice vac furnace would make simple work of finding the best temp. So for someone with only charcoal to work with, probably a bad idea to expect much to work out. Not a bad idea to try, or suggest though.

Start out toasting bread, end up looking all over the place for new materials and processes. The issue being any one can toast bread, not everyone has all the tools to go further. Freezedrying would be usefull, as would the adjustable temp. The more varried your toolchest, the more diverse feedstock you can coax into submission.

Im not saying thought in absense of action is totally useless. Just saying it would be better to see ways in which you want to improve the outcome. If you remember this is usefull for more than just refactory. So there are quite a few attributes possible. Well its 4:54am, time for bed.

unionised - 21-12-2016 at 03:34

It's not strictly relevant to the thread but trying to measure the "resistance" of a carbon foam like these by stabbing the two probes from an ohm meter into it just isn't going to work properly.
The contact resistance will dominate the reading.
You need to use something like this
https://en.wikipedia.org/wiki/Four-terminal_sensing


aga - 26-12-2016 at 10:26

Quote: Originally posted by unionised  
... trying to measure the "resistance" of a carbon foam ... by stabbing the two probes from an ohm meter into it just isn't going to work properly.

Agreed, but's it's fun to see low resistances on a bit of bread by any method.

The Bimbo bread pyrolysis method reliably gets lower readings no matter where the probes are prodded : 200 ~ 400 ohms rather than several kilo-ohms with pyrolysed wood.

To lower the resistance, today i tried to coat a bit of pyrolysed bread with chemically-made copper powder and then zap it with a focussed beam of sunlight (fresnel lens). Made absolutely no perceivable difference.

Then i wondered if copper would electro-plate onto it. After wondering for 0.6 seconds, i tried it.

Saturated copper sulphate solution with a few drops of sulphuric acid in a 250ml disposable plastic cup, 1.5V AA battery, bit of 15mm copper pipe. (i spilt the blue contents setting up for the photo)

rig.JPG - 47kB

The piece of pyrolysed bread had an aligator clip<sup>1</sup> on it, making sure that the clip did not touch the solution. The current was 26mA when first measured.

This surface was facing the copper pipe and now (unsurprisingly) measures Zero ohms at all points where the copper has adhered.

top.JPG - 45kB

I forgot to measure the resistance of the bottom surface.

This shot shows how far through the carbon material the copper had penetrated after ~1 hour.

bottom.JPG - 48kB

Not sure what this means/could mean.

The range of materials that can be plated is huge, so it could hold wonderful possibilites.

In terms of batteries/supercaps, maybe this could make the best current collector ever, seeing as the copper is deposited atom-by-atom making better contact with the substrate than 'calendering' ever could.

Have to try soldering a wire to the copper plating tomorrow.


<sup>1</sup> found a bag of metal 'curtain clips' in the chinese shop. 15 for a euro.

aga - 26-12-2016 at 14:42

Quote: Originally posted by aga  
... compress with a hydraulic jack, then toast again would do something different.

Tried the 'press with hydraulic jack' part today with all the carbons made so far and it seems pointless.

It was a bottle jack that is commonly used for car tyre replacement and a home-built jig.

Just makes a disc of very fragile carbon that falls to bits when touched.

Maybe it needs a ton of heat while pressed to do anything different.

[Edited on 26-12-2016 by aga]

aga - 27-12-2016 at 04:07

A bit of toast with a wire soldered to it.

soldered.JPG - 45kB

elementcollector1 - 29-12-2016 at 14:42

Well, it's that time of the year again. Time for bread science!

Today, I decided I would try an entire furnace made out of bread. Specifically, a loaf of rosemary bread because that was the only one the local grocery store sold that was big enough.


Size comparison with my hand:


This stuff's pretty easy to shape - I just carved out the insides with a kitchen knife. The only problem was the occasional void inside the bread, which could be fixed by stuffing cut-out pieces into it until it regained structural integrity.

I already packed in the kanthal heating wires, which are going to be present during the bake in the oven just to make sure they have enough space. Here's the ends poking out on opposite sides of the central chamber:

(^This one's a bit hard to see - it's the black wire in the very center of the picture.)


Probably going to bake this for 2 hours instead of 1, just because of the sheer volume of bread that needs to get carbonized. Wish me luck!

[Edited on 12-29-2016 by elementcollector1]

aga - 29-12-2016 at 14:52

The 'wire' looks like rosemary to me ...

It will not retain any absolute dimensions during pyrolysis, so just carve it up afterwards.

Such a HUGE piece will give an awesome result !

violet sin - 29-12-2016 at 16:49

Aga: YES YES YES!!! You frigging soldered to your coppered bread foam!! I love this

Ec1: awesome, best of luck with form holding up through baking. Really cool to see some one use nichrome wire in the thing pre bake. After a few of my experiments, I also wanted to do a whole loaf, but never got around to it with holiday season.

Not as fun to take a back seat and watch others do all the fun... But progress is still awesome. Thanks for keeping a guy going. I'll try to get actual chores done so I can participate again soon

aga - 30-12-2016 at 01:20

Just had a thought: that recent paper about making ethanol from carbon dioxide and a 'deposited copper on n-doped graphene nanotube spike' catalyst might be an application of this toast thing.

Bread slices dampened with ammonia, then pyrolysed, then very briefly copper plated might work.

The resulting 'tile' will be both conductive and porous, so two of them could be used for the electrodes.

If they were arranged horizontally, like this '=' with the CO2 (or air) bubbled in from underneath, the gas will pass over a huge surface area of 'catalyst', twice !

TODO List += 'EtOH from Air and Toast'.

aga - 1-1-2017 at 04:56

Seems that a steel 'form' can help get the resulting toast flatter.

Probably better to just lay the bread horizontally and put a plate of steel on top.

flatter.JPG - 64kB

Certainly gets hotter in those tins than i ever imagined !

hot tin.JPG - 84kB 718.JPG - 71kB

Edit:
Tried the horizontal steel plate.
6 circles of bread separated by a circle of steel plate with holes in it. Some big nuts on top to weigh it all down. Whole lot pyrolysed.

sepstack.JPG - 53kB discs.JPG - 59kB thin.JPG - 52kB round.JPG - 62kB

[Edited on 1-1-2017 by aga]

Jstuyfzand - 1-1-2017 at 09:28

I wonder, what if you electrolyse the carbon in a solution of Manganese sulphate, depoisiting MnO2, and use it as a catalyst for in the Ostwald Nitric Acid thread. A paper has been posted which showed potential.

aga - 1-1-2017 at 10:04

Unfortunately this batch has come out with random point-resistances in the mega-ohm range instead of the usual few hundred ohm range, so electrolytically depositing stuff on them won't work.

Not sure why that happened.

Far too many possible things to try with this toasted bread for 1 person to try in 1 lifetime.

Give it a go yourself and see what you get.

Jstuyfzand - 3-1-2017 at 13:31

I finally got my head out of my arse and made my foundry, first thing to throw in was a piece of bread.

Flames are spewing out so results might not be amazing but i'm one step closer to muh homemade graphite anodes, although many steps need to be taken still.

[Edited on 3-1-2017 by Jstuyfzand]

1483479172638-2098594357.jpg - 491kB

Erm, the foil melted?

This is the first piece of toasted bread that is toasted at higher temperatures though, I wonder if this will graphitize it more increasing conductivity.
I don't have an OhmMeter, unfortunately, but I do have a PSU which can measure current and voltage, so I can get the resistance, but if its in the mega ohm range I'm affraid I wont see any current.

[Edited on 3-1-2017 by Jstuyfzand]


Edit:
After half an hour of toasting, I pulled out the bread which fell apart, I took a small piece to the PSU.

CONDUCTIVITY!
Arcs spawned around the piece at 10 volts, 2 -3 Amps was measured but it fluctuated alot. The structure feels very crispy but fragile, it draws like graphite though.

I quickly submerged it into some water with NaCl, 1 amp with the tip of it submerged and very poor electrical contact from my aligator clips.
Tomorrow I will solder a wire to it and put something bigger in the furnace and test that out as an anode and the conductivity when submerged.

Looks like diy anodes are pretty close after all!

A youtube video:
https://youtu.be/DZ8PJsRpl_U


[Edited on 3-1-2017 by Jstuyfzand]

20170103_230330.jpg - 1.8MB

[Edited on 3-1-2017 by Jstuyfzand]

aga - 3-1-2017 at 15:05

Awesome Jstuyfzand !

The sparking in the video is exactly like it does in a microwave, just it does it all over.

Soldering a wire to the pyrolysed bread requires plating it with Copper first.

1.5V AA battery, bit of copper tube connected to the +ve terminal, copper sulphate solution, bit of e-Toast connected to the -ve terminal, dunk 'em in the solution, leave it overnight. (make sure the wire to the toast does not touch the liquid)

Super awesome that yours came out with low resistance as well.

I tried the discs thing using some ammonium sulphate crystals, and that made e-Toast with resistance in the 30+ mega-ohm range, basically an insulator.

Get yourself a multimeter !

Gonna be a long and fun road from here on in.

Edit:

Sorry i lied about the "Not sure why that happened" thing earlier.

Having proved yourself an Actual Amateur Chemist i'll not withold data from you again.

[Edited on 3-1-2017 by aga]

Jstuyfzand - 3-1-2017 at 15:32

I have some copper acetate laying around so I can start plating first thing tomorrow, I will plate a small part on the top to solder a wire to it and then test it for electrolysis.

I am experimenting to get some anodes for Hydrogen production and chlor alkali, however, there are mixed interests in this thread.
Is there anything you would like me to try with this conductive toast?
Please do realize that my supply of reagents is depressing, but I if you suggest something I'll gladly find a way.

aga, don't worry about it, just keep throwing pieces of bread into fire!

I used a piece of baguette by the way, it shrinked to 25% of its original volume, tomorrow I am pyrolizing a different kind of bread, I hope the results won't change too much.

Jstuyfzand - 4-1-2017 at 10:56

The second piece came out conductive as well, with a very sturdy structure.
It was a very weird shape though, and plating was inconsistent.

I will try carbonizing the square white wonderbread type, I hope it will form something flat like sheets, so that the plating process is easier.
I will also try bread dough, I`ll leave it in longer and see if I get something resembling a graphite rod.

aga - 4-1-2017 at 12:27

The bread tends to curl.

Stick some steel on top to hold it in shape.

Getting a Shape has proved to be hard with this process.

elementcollector1 - 17-1-2017 at 09:12

Just a thought, has anyone tried making carbon pancakes? Seems like they'd be better than regular bread in terms of pore size distribution and mechanical properties. Might also make a good ceramic heating plate.

gatosgr - 18-1-2017 at 08:34

That's just yummy I suddendly have an appetite for donuts, there is another research that used the maillard reaction to make carbon foam but it didn't use dough, I remember it used NH4Cl to make ammonia bubbles. Nitrogenous compounds emit toxic stuff when pyrolyzed, take care.

[Edited on 18-1-2017 by gatosgr]

elementcollector1 - 21-1-2017 at 21:20

Just tried the Bread Furnace again - this time, with homemade bread!

Recipe was doubled from this source, with regular flour substituting for rye flour:
http://www.foodnetwork.com/recipes/emeril-lagasse/homemade-r...

Results of 1.5 hours of baking at 500 F, next to a 1000 mL beaker for scale. Apologies for the horrible pic, I really need a camera that's not my phone.


Here's a closeup of the kanthal wires inside the furnace.


Does anyone have any ideas about insulating these from the metal crucible? Maybe more breadmix in between? I'm just worried about space - the crucible I intend to use is pretty wide, and I misjudged the size of the cavity in the center - the bread expanded while baking and shrank it. : /


[Edited on 1-22-2017 by elementcollector1]

elementcollector1 - 23-1-2017 at 19:38

Have since made a mix of flour and water, and coated the kanthal wires with it before baking the whole thing. I had to widen the cavity inside the main furnace block to fit everything in, but now all the wires are electrically insulated. As soon as I receive my stainless steel reactor again, I'm going to bake the inner insulation until it burns to carbon. Hopefully that way this furnace won't light on fire when I power it. : /

aga - 24-1-2017 at 12:29

Quote: Originally posted by elementcollector1  
Just tried the Bread Furnace again - this time, with homemade bread!

Cool ! Looks like a Huge chunk of carbon material there.

Quote: Originally posted by elementcollector1  
any ideas about insulating these from the metal crucible?

There's a Huge chunk of carbon material somewhere around that might be cut up and used as a hi-temp insulator ;)

(alternatively, rock wool insulation)

Edit:
A while ago i tried mixing a type of building plaster with sand to make a pourable insulation material for a home-made heating mantle.

It worked as far as the pouring-on-the-coiled-wire-and- setting-hard part went, but smoked horribly when i tried to heat it with the kanthal wire to dry it - eventually it broke to bits.

Maybe heating it that was was silly, possibly i just used the wrong material. Maybe a high-sand cement mix would work better.

[Edited on 24-1-2017 by aga]

wg48 - 7-2-2017 at 05:36

Here is some carbon foam made from a malt loaf when I defrosted it in a microwave oven accidentally on full power. A malt loaf is probably very similar to bread but with a lot of sugar. It held its shape and does appear to be well carbonised. Its crispy and has a glass like sound when tapped though it reads open circuit even on the 20mohm range of a multimeter.

Be warned it produced an acrid smoke that stung my eyes and throat. It took a more than an hour to clean the microwave oven and it along with the kitchen and half the house still smell like a wood fire.


malt-loaf.jpg - 306kB

aga - 7-2-2017 at 08:34

Shame it came out high-resistance.

Mixing in zinc nitrate before baking might have worked, but i wouldn't suggest repeating the microwave experiment in the house !

Jstuyfzand - 30-4-2017 at 11:05

Got the bloody kiln working, but the damn bread caught on fire and now there is soot on my ytong "refractory".

Got a multimeter, results in an hour or so.

The piece of bread is a custom baked slab of hard bread resembling a plate, to continue with my ongoing search for a cheaper alternative to SS for Hydrogen production and consumable carbon/graphite electrodes. Which is also the reason I cant mix in chemicals like zinc nitrate.




PS: When making your own kiln, make it square. This pentagon thing looks good on paper but making the angles with a handsaw is a pain in the bum.
25$ got me pretty far though (excluding pid)



20170430_210406.jpg - 1MB

[Edited on 30-4-2017 by Jstuyfzand]

Jstuyfzand - 30-4-2017 at 11:44

7 ohms per centimetre, damn.

Brittle though! I think it was in too long.

ferrousexplosive - 18-7-2017 at 17:27

is it suitable for electrolysis?

Brominated Potato - 12-10-2017 at 06:58

About graphitization, I found this article about graphitization of charcoal using rare earth metals:
http://pubs.acs.org/doi/abs/10.1021/acs.langmuir.6b02000
The abstract seems relevant but I can't afford 40 dollars.

NEMO-Chemistry - 13-10-2017 at 13:57

Quote: Originally posted by Brominated Potato  
About graphitization, I found this article about graphitization of charcoal using rare earth metals:
http://pubs.acs.org/doi/abs/10.1021/acs.langmuir.6b02000
The abstract seems relevant but I can't afford 40 dollars.


save your money and enjoy

although i think your are supposed to ask in references, so grab quick incase the file has to be removed. Ask a admin for access to ref i will plonk a copy there incase

Attachment: wang2016.pdf (6.1MB)
This file has been downloaded 476 times


aga - 13-10-2017 at 14:33

Beaten-up carbon, no matter what the starting compounds were, nor the process, is likely to become an entire field of physics/chemistry in itself.

chironex's exploits got me interested in the whole Carbon Quantum Dot thing (CQD/QD/CD).

Zhi et al came across QDs while trying to purify them.

Turns out that many abused carbon materials contain them.

Anyone ever seen some brown/black tarry goo after an OC experiment ?

Guess what's in there.

Sticking stuff in a microwave seems to be the easiest route to QDs, so i'll give that a try, seeing as the results have already been documented.

Attachment: yang2013.pdf (395kB)
This file has been downloaded 473 times

mayko - 15-10-2017 at 19:04

Another Brominated Potato request

Attachment: Iron-catalyzed graphitization of biomass.pdf (2.3MB)
This file has been downloaded 415 times

MrHomeScientist - 27-12-2017 at 14:00

It was a rainy day off work today so I thought I'd give this a shot. I bought a quart-size metal paint can and punched two holes in the lid for gas exhaust. I loaded this with 3 slices of honey wheat bread.

1.jpg - 310kB

This was placed in my charcoal chimney "furnace" and heated for about 50 minutes. About 20 minutes in, the smoke coming from the holes in the lid caught fire and burned for a while, as was noticed by others.

2.jpg - 305kB

After cooling down here's what it looked like. The bread had shrunk considerably and is somewhat brittle, but I did get one nice tiny slice intact. Neat!

3.jpg - 254kB



I made good use of the coals afterward.

4.jpg - 431kB

aga - 27-12-2017 at 14:02

Awesome !

Measure the resistance of the product - obviously not the sausages.

MrHomeScientist - 28-12-2017 at 18:14

Stabbing the bread with probes 1cm apart, I got several readings. The average for the large piece (pictured) was about 15 ohms. The other pieces had values around 80, 30, and even just 8 ohms.

80 ohms over 1cm corresponds to 0.8 ohm*m, and looking up a table of resistivities of various materials (here) that's about 300x less conductive than graphite measured along the plane of the sheets. The 8 ohm measurement would then be 30x less conductive. Assuming I have my facts straight.

I made somewhat conductive bread!

5.jpg - 435kB

elementcollector1 - 28-12-2017 at 20:35

Perhaps you should be looking at it another way: Given a resistivity of 3.5 x 10-5 ohm*m for amorphous carbon, your bread is approximately 23,000 times more conductive than regular ol' burnt bread.

aga - 29-12-2017 at 00:02

Excellent stuff MrHomeScientist !

The confirmation that it is also measurably conductive with a meter is very encouraging.

Has anyone tried burning some bread in air to see what resistance that ends up with ?

violet sin - 29-12-2017 at 00:26

I've been really wanting to get back into this... But the time has been imaginary thus far. Ever since my better half handed me a solid black lump of a potato found in back of oven, it's been on my mind.

Dollar store had bags of prilled Styrofoam. Basically just not stuck to one another, sold as decorative snow. I imagined making several potatoes into mash and mixing in the wee Styrofoam orbs. If done right with super low temperature start and ramped up final temp, it could make great insulation. Though I bet weak unless stabilized, chopped up fiberglass insulation? Hopefully that will be my next test. Need a good container for this one, going to check the thrift stores when I get a chance.

Radium212 - 1-1-2018 at 06:52

That really is quite amazing.

aga - 1-1-2018 at 08:15

Today i baked a loaf and pyrolysed the resulting bread.

My half-baked (pun intended) idea was to add 10% sulphur powder to the mix, right at the start, in some vague hope that the yeast might utilise it somehow and cross-link the gluten bits.

All it made was a smelly yellow loaf and a fairly nasty pyrolysis smell.

The end result is no non-conductive that it is effectively an insulator :(

NEMO-Chemistry - 1-1-2018 at 17:35

Dunno if this is any help.

Salicylic Acid and 4-Nitroaniline Removal from Water Using Magnetic Biochar: An Environmental and Analytical Experiment for the Undergraduate Laboratory
DOI: 10.1021/acs.jchemed.6b00154 J.

I wanted the paper for something else, but i figure if its magnetic then it might help with the conductivity of Bio Char. I also think there is a copy of the supporting material in refs.

aga - 2-1-2018 at 14:52

The reason for adding Sulphur to the bread is all down to a nagging suspicion about Bread itself.

Our species evolved without 'manna', IF we are the species we think we are.

Currently i think it likely that we are derivatives of ancient aliens not that it makes any great difference in the scheme of things.

Probably a cross-breed kinda thing.

Now, going back into antiquity, some tens of thousands of years, we suddenly see what we assume are Humans abandon hunter-gatherer techniques (which worked fine for millenia) and begin to Farm Barley, domesticate animals and build Cities - all in a very short time.

Looks more like meddling to me than 'natural' progression.

Anyway, that's Sumeria.

A bit of research found that Sulphur is available in large deposits in the zone once known as Akkadia, which appears to have had a close relationship with Sumeria.

A place currently called Mishraq in Iraq has some sulphur deopsits, as do other places in Iran, so it was locally available back in Sumerian times.

Fundamentally it is a HUGE shift for a hunter-gatherer to begin to predominantly Farm instead of hunting/gathering.

To create Bread is also a HUGE leap. 2 step-changes so fast is supicious, hence suspecting that sulphur and bread were related.

Edit:

Also that some people say the 'Annuki' got humans to mine Gold, which is also yellow.

[Edited on 2-1-2018 by aga]

DrP - 3-1-2018 at 03:27

Quote: Originally posted by aga  
My half-baked (pun intended) idea was to add 10% sulphur powder to the mix, right at the start, in some vague hope that the yeast might utilise it somehow and cross-link the gluten bits.




For better crosslinking in your char try Ammonium PolyPhosphate rather than sulphur. Preferably a fine powdered phase II grade. It is the industry standard charring aid and cross linker.

MrHomeScientist - 19-1-2018 at 08:08

Stumbled across this the other day: https://www.youtube.com/watch?v=Wex_yKfrTo4

He makes his bread in a welded steel chamber filled with argon, and shows how resistant it is to heat by melting aluminum on it with a thermocouple underneath. Neat!

aga - 19-1-2018 at 11:14

It was stumble-able right back on page 1 of this thread.

Quote: Originally posted by aga  
Odd.

I watched a utoob vid a while back by AvE (probably no relation to ave) doing exactly this with sliced bread.

https://www.youtube.com/watch?v=Wex_yKfrTo4

MrHomeScientist - 19-1-2018 at 11:56

Damn! I should have practiced what I preach and read the thread.

aga - 19-1-2018 at 13:28

It happens.

There is a rumour that even i posted without reading the thread (blush).

At least you didn't start a new thread based on a post in an existing thread, which leads to my next post ...

aga - 18-2-2018 at 11:05

An attempt today using just a wood fire and aluminium foil didn't turn out too well.

Looks like i made a high-temperature dog poo.

turd.jpg - 30kB

Chemetix - 18-2-2018 at 13:28

I don't have the time to go and try this so don't crucify me. But has anyone tried, or would like to try, dipping their bread refractory foam in a thin mix of plaster and see what happens. Or sodium silicate perhaps, just something to shield the carbon from getting oxidised.

aga - 18-2-2018 at 13:42

Dipping a chunk of bread in some plaster slip would be very easy to do.

Nice idea Chemetix.

I tried a tin can today with very little Al foil as a cover.

Stupid really - the teeny amount of foil disintegrated.

Should just have turned the can upside down and used the floor as the seal. maybe with a brick on top to hold it down.

[Edited on 18-2-2018 by aga]

elementcollector1 - 18-2-2018 at 13:54

Quote: Originally posted by Chemetix  
I don't have the time to go and try this so don't crucify me. But has anyone tried, or would like to try, dipping their bread refractory foam in a thin mix of plaster and see what happens. Or sodium silicate perhaps, just something to shield the carbon from getting oxidised.


I'm eventually hoping to get up to 2000 C thermal resistance, meaning that even plaster would melt at those temperatures, but hopefully graphite and/or amorphous carbon would stand up. Also, store-bought plaster of Paris is incredibly prone to cracking unless you stabilize it with a fairly precise mix of either cement and sand, or perlite and other stuff.

Dipping the bread, though, is probably a good idea. I've never worked with sodium silicate before, nor can I think of any liquid-coating solutions at the moment, but what if one were to 'squeeze' bread between two lubricated steel containers, one larger than the other, and create a roughly-container shaped piece of shielded bread that can then be charred?

I've also been wondering whether it's worth trying to make one's own bread for use in this experiment, instead of relying on store-bought versions. Pizza dough comes to mind as a very formable, smooth-walled version, and it can be made pretty easily. Form it around a metal, cup-shaped object and make your own 'graphite' crucible, maybe?

aga - 18-2-2018 at 14:04

I made my own bread for the last few attempts.

Making bread is really easy.

happyfooddance - 18-2-2018 at 14:09

Quote: Originally posted by aga  
I made my own bread for the last few attempts.

Making bread is really easy.


I feel like this is the only way to go, and be scientific, with this project. Most breads have a lot of salt, which I can only imagine would mess with conductive properties, especially with adsorbed moisture.


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