I think maybe you could try lead in a powder form and mix in the Sulfur powdered to get it to integrate better, and maybe have a stronger heat source, like a Bunsen burner.
Sadfully Lead(II) sulfide (PbS) isn't made that easy! You have to give hydrogen sulfide to a solution of lead salt (e.g. lead nitrate) or you can try a solution of lead salt + sulfide salt but I don't know exactly which salts to use (the sulfide must push away a weaker "acid" out of the lead salt. There will also be problems with purification of the lead sulfide and a crystallisation. If you burn or melt lead and sulfur together (under atmospheric conditions you'll most likely end up with lead(II) sulfate (PbSO4) (Oxygen is very sneaky 😅) If you have a p/o box or company address I'll send you a whole bunch, the crystalls are cheap as fk where I live 😅
@Christian-lh7ux Thank you for the information. I guess I had to learn the hard way. I appreciate the offer of the galena, but it's around here, I am just being lazy (and you shouldn't encourage my laziness!) 😉
@Christian-lh7ux Come to think of it, my school had a press, and for a demo they would put lead powder in a die, then squeeze it until it squirted out the end like hot toothpaste. Mix sulfur in there and I would wager it would work. I'm just 50 years too late.
@@tsbrownie Than get your a$$ up and go and collect some rocks! Just kidding 😅 I'm just a hobby chemist but I made some thoughts about it. Do you have a source of noble gas e.g. nitrogen, helium etc? Fill a test tube with your (mostly) stoichiometric mixture of sulfur and lead and press it in the end of the tube with asbestos wool(🤔 I guess you dont have such so use stone wool) (use bb pellets or fishing weights, solderwick has often times flux in it or was yours without? But even silver/tin is not so good. You want to have somewhat of pure PbS if you want to use it as a semiconductor especial if you don't crytallize it/ more byproducts = harder to crystallize) Fill a balloon with nitrogen or helium, mount a glass tube on its opening (a tube with tap would be perfect. It would also be good if it has an angle/is formed like a "L") Hold the test tube upside down in a waterbath, suck out the air until the water line reaches almost the rock wool. Use a plug with a hole in the middle at the other end of the glass tube to be able to close the test tube. Fill the test tube with your gas and displace as many water as possible preferably everything and close the test tube with the plug. Now you should have an inert/noble gas atmosphere where you can do the reaction without making PbSO4. That would be my setup if I would try to do it!
I dated a girl who's brother wrote a book on Union Park in Dubuque. We desided to see if we could find the old mine that was in the park and I did! The power company had blown up the entrance to keep people out many decades ago. I discovered a couple of small entrances into the old mine and we found even the old wooden stairs were still intact once we crawled inside the narrow opening. Most of the lead within reach had been taken by visitors back when Union Park still let people into the mine. I could see small deposits high up and out of reach on the ceiling but didn't know about crystal radios back in the late 80's. Not too far across the river from Dubuque there's Galena Illinois and you can probably guess how that city got it's name. Galena is a great town to eat and shop in with a few wineries too. That keeps the women interested. I also liked the various civil war cannons in and around the park there. Since civil war era Grant was from Galena there's also a museum dedicated to him. There's a few old mine museums too but you would have to hang out with the locals to find out how to get in any old mines that might still have openings there. Are you familiar with metal charging? They use a metal rod with a metal cup like yours attached to the end. The chemical they want to charge is packed into these cups. Once the metal to be charged is molten they plunge the charger to the bottom of the molten metal so it can interact with the metal just before pouring.
@@tsbrownie The process of adding the chemicals during charging is sometimes called fluxing and degassing and is often used even on a hobby level to cast aluminum and brass or bronze.
There are many small gem and minerals shows around the country. My wife has a small chunk of galena that she bought for about $5. Unfortunately she won't let my sticky fingers near it for fear it finds its way into a radio. I guess I'll just have to go to a gem and minerals show with her and get my own. 😂
I got some galena a number of years ago from a store called Black Market Minerals in Hilton Head, SC. IIRC they have a website too and sell stuff online.
Elmer Osterhoudt said a pea size piece of lead with a little sulfur and optionally some silver shavings. I couldn’t get that to work. I had the lead from old pre-ban fishing sinkers.
I think I read somrplace that the doping of galena with sulfur is less than its common natural form, for a better radio diode. Other possible minerals might be corrundum (aluminum oxide), and silicon carbide (carborundum), but then again, the amount of doping will also determine performance.
I grew up in Missouri. I bought some galena and pyrite about a year ago -- and, yes, it damn expensive for a lima bean sized piece. When I was a kid I could get baseball sized for almost nothing. I really don't understand the hugh price increase. I had a hugh pyrite collection as a kid and threw it away as I though it was worthless. Would have been thousands of dollars to day -- no kidding. What the hell happened?
The real question is, why aren't you and I out digging through the old mine tailings? ;) Our family drove on a trip and we passed through SE Ks and NE Ok. There were HUGE tailing piles.
That is exactly what I have been thinking. Though as an adult hauling away sacks of rocks is probably going to get some unwelcome attention.@@tsbrownie
you should just melt lead and sprinkle sulfur over it untilsurface is covered wigh crystals, the stuff looks horrible but actually works fine. I have discussed with an old Elmer, he said to use a cut of brass casing fir melting in and fill with lead till justc1mm from top then sprinkle sulfur until you get a layer of that gunk. it is what they did to make some of thosev"steel galena" detectors back in the day, this was from someone that worked as radio engineer in kate 1920s untill late 1980s, and he was REALLY interested in crystal radios. it was well discussed on the old Crystal radio forum, looong lost by now can't even find it on wayback or similar, i yhink we had a shorter discussionon Theradioboard forum, but that is also lost, luckily most of the Ben Tounge crystal radio articles are on wayback. they are REALLY worth a serious study.
@@tsbrownie do that, I have made DX competition sets for decades, i was one of first dozen members of Dave schmarders theradioboard. As for the fake galena, I live nortern Sweden and have caught DX from Portugal and Turkey on such crystal, true, i have 1000+ litz wire on custom polystyrene foam formers, silver plated copper capacitors with minimal steatite insulation... One such radio cost me just shy of 1500€ and that was without the refurbished RCA big can balanced armature headphones and audio matching transformers... Saying I have been serious in pursuit of perfection is an understatement
@@najroe WOW! That's some serious stuff. I thought putting $25 USD in a radio was expensive. You should be teaching and making videos! I've been to Sweden many times on business. Stockholm, Orebro, Linkoping, and a few other places where I have no idea where I was. Met your Minister of Health and his administration. Spent Christmas there once. Good food, great country full of wonderful people.
teaching? we did that on crystal radio forum and theradioboard, we had a great FAQ on most subjects (antenna, antenna tuning,, impedance matching (a,ntenna, coils, detector, headphones),loose coupling of coils, High Q benefits... it could be summed to, antenna as high and long as practical (over 160m high tower is beyond most so antenna is likely too short), match everything as well as possible, everything as low loss (high Q) as possible. how to get there is no easy task. just getting good teflon served 1050x48 lits with correct twist is hard, then getting a good thin wall styrofoam coil former with grooves cut to space the bifilar winding with right separation between turns (0.45-0.7 of single wire diameter depending on frequency, wire thickness, total inductance...) you still have proximity and skin effect as wellas eddy currents and other losses, even with litz. you want unloaded Q as high as possible as you will have to liad it down with things like antenna, detector... to extract audio from the signal and thenhigher Q the more you can liad ut without tuning becoming wide enough to hear several stations at same time when trying to tune
You were successful just not at making a large crystal. Requires different "environmental conditions." You need same set up that is used for growing large quartz. It's simply not feasible at home scale. But if you are only interested in semiconductors, there are tons of papers on growing atomic layers on electrodes or glass.
If there's a chemist out there who knows if this process can be made to work, please comment! (I know it can be done with other chemistry.)
I think maybe you could try lead in a powder form and mix in the Sulfur powdered to get it to integrate better, and maybe have a stronger heat source, like a Bunsen burner.
Sadfully Lead(II) sulfide (PbS) isn't made that easy!
You have to give hydrogen sulfide to a solution of lead salt (e.g. lead nitrate) or you can try a solution of lead salt + sulfide salt but I don't know exactly which salts to use (the sulfide must push away a weaker "acid" out of the lead salt.
There will also be problems with purification of the lead sulfide and a crystallisation.
If you burn or melt lead and sulfur together (under atmospheric conditions you'll most likely end up with lead(II) sulfate (PbSO4) (Oxygen is very sneaky 😅)
If you have a p/o box or company address I'll send you a whole bunch, the crystalls are cheap as fk where I live 😅
@Christian-lh7ux Thank you for the information. I guess I had to learn the hard way. I appreciate the offer of the galena, but it's around here, I am just being lazy (and you shouldn't encourage my laziness!) 😉
@Christian-lh7ux Come to think of it, my school had a press, and for a demo they would put lead powder in a die, then squeeze it until it squirted out the end like hot toothpaste. Mix sulfur in there and I would wager it would work. I'm just 50 years too late.
@@tsbrownie Than get your a$$ up and go and collect some rocks!
Just kidding 😅
I'm just a hobby chemist but I made some thoughts about it.
Do you have a source of noble gas e.g. nitrogen, helium etc?
Fill a test tube with your (mostly) stoichiometric mixture of sulfur and lead and press it in the end of the tube with asbestos wool(🤔 I guess you dont have such so use stone wool) (use bb pellets or fishing weights, solderwick has often times flux in it or was yours without? But even silver/tin is not so good. You want to have somewhat of pure PbS if you want to use it as a semiconductor especial if you don't crytallize it/ more byproducts = harder to crystallize)
Fill a balloon with nitrogen or helium, mount a glass tube on its opening (a tube with tap would be perfect. It would also be good if it has an angle/is formed like a "L")
Hold the test tube upside down in a waterbath, suck out the air until the water line reaches almost the rock wool.
Use a plug with a hole in the middle at the other end of the glass tube to be able to close the test tube.
Fill the test tube with your gas and displace as many water as possible preferably everything and close the test tube with the plug.
Now you should have an inert/noble gas atmosphere where you can do the reaction without making PbSO4.
That would be my setup if I would try to do it!
I dated a girl who's brother wrote a book on Union Park in Dubuque. We desided to see if we could find the old mine that was in the park and I did!
The power company had blown up the entrance to keep people out many decades ago.
I discovered a couple of small entrances into the old mine and we found even the old wooden stairs were still intact once we crawled inside the narrow opening.
Most of the lead within reach had been taken by visitors back when Union Park still let people into the mine.
I could see small deposits high up and out of reach on the ceiling but didn't know about crystal radios back in the late 80's.
Not too far across the river from Dubuque there's Galena Illinois and you can probably guess how that city got it's name.
Galena is a great town to eat and shop in with a few wineries too. That keeps the women interested. I also liked the various civil war cannons in and around the park there. Since civil war era Grant was from Galena there's also a museum dedicated to him. There's a few old mine museums too but you would have to hang out with the locals to find out how to get in any old mines that might still have openings there.
Are you familiar with metal charging? They use a metal rod with a metal cup like yours attached to the end. The chemical they want to charge is packed into these cups. Once the metal to be charged is molten they plunge the charger to the bottom of the molten metal so it can interact with the metal just before pouring.
I had to look up places named Galena:
Galena - Washington
Galena - Virginia
Galena - South Dakota
Galena - Oregon
Galena - Ohio
Galena - New York
Galena - Missouri
Galena - Mississippi
Galena - Maryland
Galena - Kansas
Galena - Indiana
Galena - Illinois
Galena - Idaho
Galena - Colorado
Galena - Arkansas
Galena - Arizona
Galena - Alaska
I don't know about metal charging. Is that like Bessemer converters?
@@tsbrownie I didn't realize there were so many. I wonder if they all had lead mines like we have here in Dubuque and Galena Illinois?
@@tsbrownie The process of adding the chemicals during charging is sometimes called fluxing and degassing and is often used even on a hobby level to cast aluminum and brass or bronze.
@@tenlittleindians OK, I understand. Thanks.
There are many small gem and minerals shows around the country. My wife has a small chunk of galena that she bought for about $5. Unfortunately she won't let my sticky fingers near it for fear it finds its way into a radio. I guess I'll just have to go to a gem and minerals show with her and get my own. 😂
I will have to watch for a show. Thanks.
I got some galena a number of years ago from a store called Black Market Minerals in Hilton Head, SC. IIRC they have a website too and sell stuff online.
@@stamasd8500 OK, thanks. I'll check on it.
Elmer Osterhoudt said a pea size piece of lead with a little sulfur and optionally some silver shavings. I couldn’t get that to work. I had the lead from old pre-ban fishing sinkers.
As every ebgineer will tell you, there's a difference between theory and reality. If you could vacuum out all the O2, it might work.
I think I read somrplace that the doping of galena with sulfur is less than its common natural form, for a better radio diode. Other possible minerals might be corrundum (aluminum oxide), and silicon carbide (carborundum), but then again, the amount of doping will also determine performance.
I grew up in Missouri. I bought some galena and pyrite about a year ago -- and, yes, it damn expensive for a lima bean sized piece. When I was a kid I could get baseball sized for almost nothing. I really don't understand the hugh price increase. I had a hugh pyrite collection as a kid and threw it away as I though it was worthless. Would have been thousands of dollars to day -- no kidding. What the hell happened?
The real question is, why aren't you and I out digging through the old mine tailings? ;) Our family drove on a trip and we passed through SE Ks and NE Ok. There were HUGE tailing piles.
That is exactly what I have been thinking. Though as an adult hauling away sacks of rocks is probably going to get some unwelcome attention.@@tsbrownie
@@tsbrownie60 miles from NYC there are old lead mines that have lots of galena, and pyrites to a lesser extent.
@franzliszt3195 On the other hand, many of those places are EPA sites and the owners might turn a blind eye to people "cleaning" up the site. ;)
@trs80model14 When I was in grade school the playground had lots of pyrite. We filled our pockets until the teacher explained it was fool's gold.
you should just melt lead and sprinkle sulfur over it untilsurface is covered wigh crystals, the stuff looks horrible but actually works fine. I have discussed with an old Elmer, he said to use a cut of brass casing fir melting in and fill with lead till justc1mm from top then sprinkle sulfur until you get a layer of that gunk.
it is what they did to make some of thosev"steel galena" detectors back in the day, this was from someone that worked as radio engineer in kate 1920s untill late 1980s, and he was REALLY interested in crystal radios. it was well discussed on the old Crystal radio forum, looong lost by now can't even find it on wayback or similar, i yhink we had a shorter discussionon Theradioboard forum, but that is also lost, luckily most of the Ben Tounge crystal radio articles are on wayback. they are REALLY worth a serious study.
@@najroe I am going to try again. We shall see how it goes.
@@tsbrownie do that, I have made DX competition sets for decades, i was one of first dozen members of Dave schmarders theradioboard.
As for the fake galena, I live nortern Sweden and have caught DX from Portugal and Turkey on such crystal, true, i have 1000+ litz wire on custom polystyrene foam formers, silver plated copper capacitors with minimal steatite insulation... One such radio cost me just shy of 1500€ and that was without the refurbished RCA big can balanced armature headphones and audio matching transformers... Saying I have been serious in pursuit of perfection is an understatement
@@najroe WOW! That's some serious stuff. I thought putting $25 USD in a radio was expensive. You should be teaching and making videos! I've been to Sweden many times on business. Stockholm, Orebro, Linkoping, and a few other places where I have no idea where I was. Met your Minister of Health and his administration. Spent Christmas there once. Good food, great country full of wonderful people.
@@tsbrownie interesting to hear
teaching? we did that on crystal radio forum and theradioboard, we had a great FAQ on most subjects (antenna, antenna tuning,, impedance matching (a,ntenna, coils, detector, headphones),loose coupling of coils, High Q benefits...
it could be summed to, antenna as high and long as practical (over 160m high tower is beyond most so antenna is likely too short), match everything as well as possible, everything as low loss (high Q) as possible. how to get there is no easy task.
just getting good teflon served 1050x48 lits with correct twist is hard, then getting a good thin wall styrofoam coil former with grooves cut to space the bifilar winding with right separation between turns (0.45-0.7 of single wire diameter depending on frequency, wire thickness, total inductance...) you still have proximity and skin effect as wellas eddy currents and other losses, even with litz. you want unloaded Q as high as possible as you will have to liad it down with things like antenna, detector... to extract audio from the signal and thenhigher Q the more you can liad ut without tuning becoming wide enough to hear several stations at same time when trying to tune
i have an idea , if you can use a heating element instead of flame , then try it in a sealed container or vacuumed housing and flood it with Argon gas
There's another comment that has a detailed description on how to do that. It makes sense, but it's probably way beyond the average experimenter!
You were successful just not at making a large crystal. Requires different "environmental conditions."
You need same set up that is used for growing large quartz. It's simply not feasible at home scale. But if you are only interested in semiconductors, there are tons of papers on growing atomic layers on electrodes or glass.