Some important points I would like to write about, showing the public how science works. I don't think most people are getting the stories about these aspects of science.
I got these from reading Jim Baggott's wonderful book: "Perfect Symmetry: The Accidental Discovery of Buckminsterfullerene".
1) buckyballs, which are chemistry, were discovered by astronomers looking at OBSERVATIONS of phenomena in the real world. Interstellar dust or molecules made inside machines and soot, rather than the organic chemists theorizing for decades about abstract shapes.
(later we got data that buckyballs very likely are in interstellar space and cause the some of the diffuse interstellar bands (spectra) that the original discoverers of buckyballs were wondering about):
2) Kroto came and visited Smalley's lab, where he had two grad students. When the students revved up their machine to make interstellar organic dust, they found such preposterous results that they were afraid to show them to their supercisor, Smalley for fear he would think they broke his machine or something. But Kroto would hang out with them and that easy going relationship encouraged them to show him their crazy C60 results which then got the ball rolling.
3) some of the investigators were really on a good track to finding the stuff, but they were stymmied by poor funding and malfunctioning machinery delaying their results.
4) fascinating tension between investigators sharing enough info between labs to ask if they were on the right track, edge each other on, but trying not to share too much so that the other lab would discover it first!
5) the nitty gritty details of the techniques the different investigators had to learn in order to get results. Many were working outside the fields they had trained in.
6) the role of grad students had to play, in trying goofy things that ultimately led to new results.
7) how having ALL the different kinds of labs in 1 intercommunicating space/culture at IBM allowed them to put results together so quickly, in the end.
8) caution the investigators displayed in not wanting to publish wild results until they were tested solidly in a few different ways, using different techniques and theories. that is how science becomes more certain of their results and builds a solid foundation.
BUT HERE IS THE DEAL, THIS IS WHY WE THINK OF C60 AS ***REAL*** SO MANY LABS FROM SO MANY ANGLES GET RESULTS THAT JIVE: mass spec, specific signal at 60 70, geometry, huckel theory, La in cages, suggestive uv spec, producing it from laser ablation and cooling, from carbon arc to soot, laser ablation... IR spec, tons of calculations from diff ideas, chem and sublimation purification, raman spec, NMR of 60 and of 70, crystalization, electron diffraction to get spheres, scanning tunneling microscope to get spheres...
AND AFTER 300 YEARS OF KNOWING HOW EASY IT IS TO BE FOOLED, THESE RESULTS ARE DONE OVER AND OVER AGAIN BY DIFF PEOPLE WITH SLIGHTLY DIFF TECHNIQUES CO9NSTANTLY CHECKING EACH OTHER SO YOU KNOW YOU ARE NOT CHASING WILD GOOSE
ALSO TO REALISE THIS ISN'T SUCH AN ARTIFICIAL SPECIALIZED STATE OF MATTER BUT IT CAN FORM QUITE EASILY IN A NUMBER OF DIFFERENT ENVIRONS...
9) how LONG science takes to do.
10) should we redesign things to work like IBM labs so things happen quicker or is it ALL RIGHT that science proceeds at the pace it does. Or even, did things ultimately depend on the fact that enough different investigators were working independantly?
11) Interstellar dust, buckminsterfullerenes, the detection of them... is really cool science.
12) the role that communication of ideas, results, conversation, conferences, critique, plays in science. the community of conversation is, in my opinion, what defines modern science. There were at least 6 different teams interacting on this over a period of about 15 years.
i think these are all important aspects of science that the public is ignorant of, but should really know about.
ok, i need to grokk these notes
review: from Baggott
1927 darcy thomson shows radiolaria produce cages with hexagons but need pentagons too
of course a ton of soot chem
1966
David Jones publishes a whimsy as Daedalus that he can make giant graphite gasbags by adding defects to the graphite and it would be a new state of matter density between gas and condensed
1982
after reading thompson, he elaborates and uses euler formula to show he needs introduce only 12 pentagons
NO ONE NOTICES?
1952
fullers domes were first constructed
1960
Roger Bacon grows graphite whiskers in carbon arc at union carbide pub in jnl applied physics, from elec mic and xray diff decided these were spirally scrolled graphite sheets into micron wide cm long whiskers
NOT FOLLOWED UP?
1963 hoard et all find B60 with a B24 inside boron is crazy theres' tons of boron geometry, no?
1966
Wayne Barth and Richard Lawton umich synthesise corannulene with pentagon surrounded by 5 hexagons. is it aromatic? chemists believed aromatic had to be planar, yes it was but xray diff said bowl shape!
Eiji Osawa was wondering about non planar aromatics, and read this and wondered all the way to sphere? saw kids soccer ball, bingo, published an abstract in japanese journal, and then with z. yoshida published ideas in book 1971 he even checked huckel theory, yes it checked. but he and other japanese chemists who read this were thinking of mundane problem: how would you synthesise in ordinary lab procedures. THEY WEREN'T THINKING BIG ENOUGH, BROAD ENOUGH WAS IT A NATURAL FORM OF CARBON?
>>>SO ULTIMATELY THIS DISCOVERY COMES FROM OBSERVATION, OBSERVATIONS OF NATURE, OF CURIOUS SPECTRA IN ASTRONOMY! and kroto, kratchmer, huffman, curl and smaley heath and obrien are NOT orgo chemists!
1968
Goresy, Donnay looking at shiny samples alternating with graphite in meteorite crater suggested new form of carbon called carbyne
whittaker 78 heats graphite to white substance at high temp and imagines carbynes alternating single and triple bonds
1973
Bochvar and Gal'pern also imagine C60 and do the Huckel calculations even imagine a whole new class of such molecules pub in proceedings acad sci ussr
tx english in russian chemical reviews 1984
1980
sumio iijima finds elec micrograph of onion shaped carbon strtucts from carbon deposition at NEC corp fund research div in japan and thinks its graphite laryers around a structure with pentagons.
EXPLORE THIS ROUTE NOT TAKEN
no mention of if he published this till 1987
BY 1991 he discovers nanotubes
1981
Robert Davidson of dupont, delaware also imagines it and calculates, in theoretical chimica acta 1981 obscure
jul1981
Orville chapman visits U. erhlengin and francois diederich decides to synthesis C60 gets national science foundation grant and 5 grad students 81-85 during this time discussing with organic chem community skeptical, he complains orgo chem community is stale turned inward
by 1985 Diederich with rubin, knobler, Robert Whetten, schriver, Houk, Li is synthesizing C18 to C30 but the large rings not stable and turn into some kind of forms of C48 50 60 70 SOME ODD RESULTS DID THEY FINALLY FIGURE OUT WHAT THEY WERE GETTING?
1983
leo paquette et al synthesise dodecahedrane
1985
Anthony haymet ucal berkely doing huckel calcs on C60 INDEPENDANTLY?
1985
bloomfield, geusic (ex student of smalley) freeman and brown at at&t bell labs were working on similar experiments mass specx with ion clusters they got diff pos and neg ion distributions no special C60
1986
Robert Whetten et all of ucla dep chemm biochem solid state also got mass spec with odds and evens and signatures of magic numbers 50 60 70 but thot this was breakup process not special structures
ALOT OF PEOPLE WERE WORKING ON THIS, ONLY SOME GOT ALL THE WAY
MAIN STORY
1975
Harry Kroto is a microwave spectroscopist! looking for interstellar orgo molecs polyenes
production on surfaces or plasmas of red giants
82 microwave spec show c chains up to 11
sees 1963 paper on carbon arc producing C molecules up to C33 hintenberger, franzen, schuy
their graph stops at C33, why did they not continue up to even numbered Cs? QQQ
what are diffuse interstellar bands? found in visible spectrum of starlight, instead of sharp absorption lines found in solar spectrum we have bands, in 30s were shown to be interstellar
Douglas suggests long C molecules by mid 1970s there are 40 unexplained bands associated with dust grains maybe smaller particles on the dust grains
radio astronomy detects molecules with dipoles,
rotations vibrations of long molecules picked up in microwave
1976
Wolfgang Kratschmer physics radiation damage on solids joins Donald Huffman physics spec study of interstellar dust to study spectroscopy of possible interstellar dust analogs
dust is <1%interstellar medium but dimms light by 1/2 every 3000lightyears of travel. by absorption and scattering it preferentially dimms uv, blue, hence reddening
similar to our own atmosphere?
particle sizes from few nm (uv) to 100nm visible, to small amount of micron (IR)
in interstellar space with 1 atom per cc dust particles might be 100m apart
thyere are 40 diffuse interstellar bands in visible but huffman notes some other features:
some absorption features in 3-9micron in IR, and 217nano feature, he began exploring in spare time, not much FUNDING
this harder than kroto's work on microwave spectra, they are distinctive, this stuff more vague
kratschmer decides start with 9.7micron band, maybe olivines, to get match bombard olivine crystals with high energy to make amorphous
next 3.1micron band: ice? make it amorphous but particles fairly large size, coating dust?
1973
next huffman wants to tackle 217nano feature, thinks graphite, begins carbon evaporation machine to examine soot some match but not good, over years huffman chips away, decides factors of size, crystalinity, shapes of particles play role
could be more than just C, but Huffman wants to keep simple
1982
he and kratcscher and Norbert Sorg begin try make small round graphite particleds in graphite tube evaporator jar, with vacuum pump. controlling pressure seen to be key to particle formation size, but needed some gas to cool the carbon into soot
they didn't quite get the 217nano feature looking for, thot particles clumping too much,
but also: every now and then on smooth curve predicted for soot, they get some humps at 215 265 and 340 nanos
kratschmer dismayed, thot contaminants, huffman intriqued
their IR spectrometer was not great, no good results. ACCESS TO GOOD EQUIPMENT, shift priorities...
they worked at their camel humps but no good results offered ideas. they never raised pressure of gas >20torr
raman scattering spec also showed interesting features in he camel samples
are they thinking carbyne?
they gave up in 83
1984
kroto visits Bob Curl in houston, who had been working with Rick Smalley created wonderful machine to produce and study new molecules of semiconducting materials
this lab was well equipped, smalley developed big lab but kept his fingers on the experiments, specialized in building the machinery, macine was unique cause used lasers to blast stuff into small molecules in a cool enough environment to measure good spectra not too noisy with too many energetic modes
then onto time of flight mass spec
kroto of course wanted to try carbon, as this machine would mimic red giant atmosph, smalley didn't think anything new would be found
1984
Rohlfing, Cox, Kaldor at exon get a mass spec of blasting graphite with laser: find carbon clusters from 2 to 190!
Pat langridge-smith (who had been at smalley lab) found the paper gave it to tony stace (worked with noble element clusters) who gave it to Kroto
Rohlfing et al got a copy of Smalley's AP2 in 82!
first half of spectrum repeats hintenbergers results, alternating peaks in even odd number C atoms some odds being tallest 11 15 19 23 trail off at C33
but then rise again at C38 and show even peaks, capping at C60 and falling again, NO signals from odd Cs
R et al had no explanation for only evens, carbyne? i.e. CzC units
but more measurements could be done, kroto wanted to try
Smalley saw paper, and said nah, don't want to let that team do it.
Kroto is still interested in finding cyanopolyenes cause they are dipoles and can be found in interstellar space
july84
Kaldor presents results at conference, Huffman and Kratschmer see it, they present some results on finding low C chains, find the large cluster results curious but
they didn't mention their camel humps (huffman had thot camel humps carbyne?)
[[SO THIS KEPT THEM INTERESTED?]
nobody remarked upon the C60, 70 signals
aug85
the app2 is finally available for kroto. jim heath and sean o'brien are students with smalley. yuan liu and quing ling zhang also joined.
liu and zhang are able to repeat exon results, they did not report to anyone one run where 60 70 signals out the roof, just recorded in the log
they and heath begin 2 photon resonance spec and find smaller molecules <25 respond, so they can test douglas' ideas of long molecs in red giant clouds
working under smalley was difficult and students feared showing weird results unless they could explain them
they met. kroto: aim for HC33N and measure spec to see if in interstellar space
Kroto begins to gets to know the students high C60 result still hidden in student log
heath and obrien worked the machnine.
heath and kroto first run, heath curious about arrival times of diff molecs (the mass spec comes from avberageing many runs) heath adds thermalization nozzle to let all particles thermalize together.
slight C60 signal but machine not working well
they meet, trying to imagine why even numbers. smalley discusses dangling edges must be closed, rings?
next they try in H atmosphere the odd len Cs turn to even lengths, so Polyenes! large even signals are a little stronger
kroto wanted to find cyanopolyenes, curl wanted to look for pure carbon molecs
Kroto had graphic art background
they all worked together as team long hours into night having discussions of all sorts of topics
finally they tried N, not interesting!
switched back to He for some reason this time they saw C60 off the scale and C70 following. AH... THIS TIME KROTO WAS WITH THE STUDENTS, SMALLEY STAYS AWAY. KROTO'S REL WITH STUDENTS HELPS SEE THE SIGNAL.
sep3
kroto brings results back to smalley and curl, finally they discuss. why this very peculiar C60, 70 signal?
at this point they try imagine what made C60, 70 so stable, dangling ends must be joined? why would a ring be only stable at 60? a sphere? geodesic dome? they had only VAGUE notionsof the geometry and didn't understand what was needed to curl the graphite hexagon sheet into sphere. kroto has vague memeory of geodesic toy with pentagons
they went back to N and did find cyanopolyenes up to 20, cool
kroto got his result, but they all were intrigued by the C60. the students decided to find out why thge signal was so haphazardly produced
obrien and heath systematically found the C60 signal to be robust and dependent on pressure of He and timing of laser blast and cooling
heath finally found conditions which produced virtually all C60 with a little C70 tagging alonhg
obrien got tired of wondering what structure C60 was wanted to go back to GaAs exps
they decided to publish the cyanopolyene story but reluctant to publish the C60 until they had some notion of struct
heath and wife tried making a C60 from gummies and toothpicks, even tried includiing triangles with hexagons, coulnd't
smalley tried with paper hexagons, no. what? then rememberd kroto had mentioned pentagons, eventually, he found it.
[when did i know what a dodecahedron was? well math book on platonic solids... but i made dodecahedron in boston in 86 AFTER this stuff was published? hmm]
Curl decdided to check if he could make a series of single and double bonds around the thing to satisfy carbon. bingo
a call to the math department told them that they had just built themselves a SOCCER BALL oy duh duh! HOW BLIND WE CAN BE!
***(((QQQQ)))
but also... we already knew boron does this right???
now they were excited!
they published., reviewer suggested they look at Douglas and Huffman's work
they tried Iron in the cage, wouldn't go
NAILING IT
they tried lanthanum (heath favored it) they found it associated with C60 AND other large even numbered molecules, was this a whole FAMILY of cages?
exon group fought the buckyball interpretation
they do stuff, get lots of criticism
they couldn't get spec of C60 tho
exps show odd chains fragment by loosing C3s at a time, but smalley lab showed buckyballs loose C2s each time
apr1987
kroto and smalley split, kroto back to sussex
he got some funding, started with evapo machine, couldn't get a mass spec tho <<<<<<<<<
in 87 homann finds a 60C molec in ordinary soot formation, burning acetylene etc..
then iijima publishes his onion pictures from carbon arc process
by 89 cold fusion fiasco cools the waters and there is still no sample large enouigh to be analyuzed. doubt
1985
lowell Lamb postgrad with background in computers tells huffman about kroto and smalley's C60
Alain Leger u paris stuies polycyclic aromatic hydrocarbons in dust clouds shows kratchmer the 85 C60 article
Kratchmer not to keen on idea, and busy with ESO infrared project
Huffman didn't think he could get funding, so got lamb working on semiconductors but told lamb to fiddle with it in spare time
87
theoreticians trying to approx absorption bands of C60
Larsson, volosov, Arne Rosen chalmers u of tech sweden publish CNDO/S calculations for buckyball for uv spec 340nm, 260, 240, 230 220
Huffman sends this to kratchmer and says, it is suggestive of the camel humps. kratchmer doubtful, these calculations are not accurate.
huffman gets idea that if his apparatus is producing C60, he should patent it this gets him going
eaerly 88 lamb reproduces the 83 heidelberg results with new evaporator and got camel humps, but not very reproducible
gave up in feb
later aftert a conrference in july huffman convinced kratchmer to try again. kratchmer got a neophyte undergrad student Bernd Wagner to do it. got irreproducible camel hjumps
THEN the student for the hell of it raised the pressure from 20torr to 100torr AND this time kratchmer had access to high quality IR spec, the new samples had stronger camel humps but bamm 4 sharp lines in IR
geometry says C60 should have only 4 modes vibratioon
calculations run from 1429 1183 577 527 to 1655, 1374 551 491
kratchmer calculated from hight of his lines that they must have got 1%yield which seemed phenomenal this blew the AP2 out of the water
lamb also eventually thot to raise pressure and got better camel humps but had no IR machine
Wagner went back to school vaguely aware that he had done something.
next comes grad student Konstantinos Fostiropoulos. he and kratchmer checked forf every possible sorce of contaminants, couldn't find one.
by know the spectre of the cold fusion fiasco was making people wary of reporting hasty results...
couldn't riase yield or he didn't know if he could extract...
finally convo with huffman said, use C13 and see if you get the 4 lines to shift by predicted amount for heavier nucleii
C13 came in dust form, they tried various methods to get it into cylinders for the evaporator, not yet.
conference season came around and they decided to report their results at the summer interstellar dust conference
mike jura attended and sent abstract to kroto...
summer 89
Kroto had tried this but didn't have enough equipment. he couldn't beleive the reported yields. decided he'd have to try again
he managed to get some sort of funding and student jonathan Hare all these people are PHYSICS people not orgo chem! and simon Balm, balm left then amit sarkar, they got the 4 lines! but still weak and not robustly reproducible, then machine broke but they got funding to fix it
meanwhile fostiropoulos was trying all kinds of things to make the 13dust solid, was not supposed to be possible. finally he got a lab to compress it under heat, and he built a new evaporator and by
feb 90
he got results, and measured the four lines they all shifted close to average .963, the predicted value was 0.9625, this was pretty damm convincing
***
at this point they are in contest kratchmer with kroto group, giving each other just enough info of results to show each other they are on the right track but not enough to show exactly how far ahead each is *****
mar90
Hare presented his 4lines at astro conference. by now he was better at getting strong reproducible lines, distance of collector to carbon rods was crucial,,. by now people are more interested, a second repetition of very specific results, BUT STILL WHAT WAS THIS STUFF
[[BAR COULD YOU CONTINUE WORKING ON SUCH A PROJECT FOR 7 YEARS?]]
in between kroto asked hare and balm to analyse spectra from halley comet from giotto space craft [ALWAYS KEEPING FOOT IN REALITY OF OBSERVATION] not bad idea as they now decided what they needed to do was keep reproducing the experiment and collecting soot so get big enough sample C60
mar90
francois diederich assoc of orville chapman and his group at ucla was working on long chain syntheses
they got C18CO6 synthesized then used laser desorption mass spectrometry to lift the molecules off of surface and gently heat off the CO to synthesise first ever C18 ring in sep 89
then they synthesized C24CO8 and C30CO10 these were 4 sided and 5 sided rings of 6 carbon carbyne groups, when they tried desorption of them, they got odd results
from C18CO6 they got signals of C18, 36, 50, 60, 70!
from C24 they got weak 24, but strong 48, 50, 60, strongest 70
from c30 they got NO C30 but huge C60, with following of 70
WHAT was happening? they showed kroto, they didn't think they had buckyballs but kroto was worried they'd get large quqantities so back to work!
Hare took sample of soot tried NMR, MACHINE FAULTY! NO GOOD RESULT, went on holiday and gave some to grad student ala'a abdul sala, try mass spec:
got 60 and 70!!!! but then MASS SPEC MACHINE BROKE couldn't repeat!
SEEMS THE BRITTISH TEAM HAS THE CRAPPIEST EQUIPMENT AND FUDING!!!!
IN FEB 90 ebert and frenklach put article in chem engineering news comparing buckyball research to cold fusion!
6jul90
fostiropoulos and kretchmer publish their C12 and C13 results on camel humps and 4 IR lines shifted
then they noticed weaker lines and remembered C70 follows C60!
the race is on to isolate a sample of C60 but they were not chemists!!!
Kratchmer sends his C13 paper to Leger, who contacted Werner schmidt at polycyclic aromatic research group, schimdt tells kratchmer: try sublimate the C60 out of the soot around 800 900K in vacuo or i think C60 should be soluble in orgo solvent! don't use benzene poisonous
fostiro not being chemist tried sublimation, and got a sublimate! put it in uv and bingo! camel humps without background of soot! first to see uv spectrum of C60 he and kratchmer kept at it and got the IR spec
they sent to huffman, huffman and lamb repeated the results!
fostiro washed the slides with benzene, readily soluble so attempted to isolate more C60 with benzene in centrifuge, got deep red solution! evaporated it and the dark powder still had the spec properties of C60! they even watched crystals of 'fullerite' form under microscope!
now they had to do analytical work, again they are the wrong people to do it, not chemists, but they wanted to be the discoverers
first they did mass spec and got messy results. HUH!
from crystals with help of werner kuhlbrand from nearby molec bio lab they got some poor electron diffraction patterns but at least gave characteristic spacing of one nm, this could be a match to calculated 0.7nm diam of C60 + 0.3nm thickness of graphene sheet
next they needed xray diffrac to show characteristic spacings of C atoms to show really buckyball struct
1987
Don Bethune, new phd student ucal berkely goes to IBM, hears smalley give lecture on bucky balls and watches...
1989
decides to try something new with that research. he had no knowlege of astro community and didn't see kratchmer's Capri presentation.
may 1990
he and heinrich hunziker, Mattanjah de Vries, Gerard Meijer begin work, using laser desorption etc... device similar to AP2 but gentler lasers. first they repeat the 1984 exon results. but what new could they do?
bethune contacted Rohlfing from the exon group for ideas. rohlfing joked just try to find it in carbon soot! ibm teem thot well if its suppose to be so stable, why not?
they knew nothing of soot chem! so they made soot in the clumsiest of manners! they put the soot in their laser desorption machine and got carbon clusters. eventually they found burning plastic or acetylene gave good pure carbon clusters but still too much contamination
19jun1990
so they went back for laser vaporization of graphite under 500torr argon and collect the soot 1cm away directly, bingo C60, 70 and higher signals, that easy.
at in house seminar july they decided they needed to do the C13 nmr to get the 1line signal. but how much C60 would they need to collect? they were gtetting better yeilds than had so far been publlished but still only 0.1 microgram.
Nino Yannoni suggests 0.1 to 1gram, get cracking then robert johnson says i can do it with 300micrograms but also ibm is big, they had raman spectroscopists even use scanning tunneling microscope on the film!
7aug
they published they preliminary work journal of chem physics
26jul
Hare reads kracchmers paper on C13 shift and realizes lets get going. he remembers enough chem to try dissolve the soot sample in benzene. sits like a lump soot not soluble [[WHAT IS SOOT]] goes home for weekend. comes back: slight red color in solution!! filters off solids, evaporates adn deep red. C60?
tries mass spec, machine still cranky BAD MACHINERY!
jun
huffman and lamb take fullerite sample and gtet xray diff: definitely new form of crystaline carbon but still need bigger crystals to get struct
they got big crystals. dissapointment! xray diffract not clean signal. this happens with cobolt. maybe spheres pack disorderly, maybe C70 disrupts structure... damm
mention something vague about frostiro visiting another lab learning he could use chromatography to seperate hexane sol into bands, but doesn't follow up? ***
then the lab people say: you should do nmr on C13, but he doen't understand importance of that either!
WOW, SO THESE RESEARCHERS ALL HAD HUGE GAPS IN THEIR KNOWLEGE OF WHOLE WEALTH OF ALL THE SCIENCE PARTS, EACH GROUP IS SEEING THIS PROJECT THROUGH PARTICULAR LENSES!
jul
huffman and kratchmer finally decided they had enough might as well publish but huffman wanted to renew patent! green light they publish, phillip ball gets paper 7 aug
ball sent to kroto 10aug
kroto: damm they did it! now what?
kroto tells ball to send to bob curl as second ref
oddly huffman and kratchmer didn't have mass spec data! their machine sucked. so someone else ought to try. kroto hare and abdul sala had mass spec before machine broke
Curl referee report: paper should include mass spec and NMR
***
OH: h AND k HAD MASS SPE RESULT THAT A COLLEGE MADE BUT DIDN'T INCLUDE IT CAUSE COLLEGUE WANTED NAME ON PAPER.
WOW******
20aug
Bethune at Ibm is shown huffman etal july paper and lets get snapping, just do a makeshift graphite arc and collect soot and laser desorb it. ok C60 signal they even called huffman and huffman said we have paper in 10aug but no mass spec, go publish mass spec
so bethune et all send report to chem physical letters 24aug, smalley editor.
tyhen kept collecting soot till 20milligrams and tried sublimating C60 out, got it with C70
Kroto lab, they thot fast, consulted with chemists Roger Taylor and Jim Hansen and decided to put the stuff through alumina packed collumn in hexane. BINGO separated out 3 bands, with another lab's help, they got mass spectra one band C60, other C70, third mixed FINALLY PURE SAMPLE OF C60!
end of aug
fuckit, Curl called huffman and said forget about my qualms, publish your paper! they published with Zscheeg and Natuour's mass spec, they first send the preprints do many scientists
7sep
bethune et al publish raman spectrum with rosen and Tang, of sublimed C60/70 mix the 273 cm^-1 line was most conclusive of squqashing/bouncing vibration of ball struct. next they set to get nmr 1line
Smalley decided to get Kratchmer to a conference in germany to announce their C60 results 12Sep, meanwhile he gets HIS lab cracking on producing C60 using the Heidelberg techniques
[[RIGHT! SMALLEY AND KROTO SPLIT! WHAT ****WAS**** THE SPLIT OVER? MAYBE THAT KROTO GOT TOO FRIENDLY WITH THE GRAD STUDENTS AND IT WAS REALLY KROTO'S REL WITH THEM THAT GOT THE RESULTS?
ANYWAY THIS ISOLATED KROTO AND HE HAD LESS ACCESS TO PEOPLE AND MACHINES AND FUNDS?]]
***
ALL IN ALL THEY PUSHED EACH OTHER JUST ENOUGH TO KEEP THE BALL ROLLING!
>>>>
BUT DID THE SCIENCE NEED THEM TO ALL DO IT SO ****FAST**** DID THE CONTEST HELP ANYTHING IN THE LONG RUN?
IN ALL, THE PROCESS TOOK FROM 83 TO 90. BUT IT HAD STARTS IN 60S AND IT LANGUISHED FOR 25 YEARS WOULD YOU SAY ****THAT**** IS TOO SLOW? ONCE THE CONNECTIONS STARTED HAPPENING IT ALL ZOOMED TOGETHER IN 5 YEARS REALLY.
BUT WAIT... THERE'S MORE IT'S NOT THAT IT WOULD HAVE TAKEN 25 YEARS BUT IT MIGHTA TAKEN WAY MORE THAN THAT, ONE PEICE AT A TIME WITH LONG GAPS... WITHOUT THE POSITIVE FEEDBACK FRENZY
SOME PIECES OF SCIENCE TAKE 150 YEARS. ***THAT*** IS TOO SLOW.
Krotolab
Hare brings solutions to Gerry Lawless and Tony Avent to do NMR, they get the single line for the magenta solution! then the red solution, predicted 5 lines, some confusion, back to chromatography, almost misinterpret because one line is close to the hexane solvent line but finally yes conclusive: the 5 lines are what we expect for C70! David Walter long time colleague of kroto convinced him this is the data that nails it.
3 sep now they get started on writing up results while Taylor kept at the chromotography to purify the C70 sample enough to get clean NMR 5 spikes.
kroto decides to visit kratchme4r to thank them for suggestions and show nmr results of separated 60/70
10sep
Taylor succeeds with nmr of purified 70 and they send paper to chemical communications jnl
3sep
Whetten meets Stace at a conference and stace tells him about fullerene results and whetten tells diederich.
11sep
not knowing how much work had already been going on, bethune reports on his work, preempting kratchmers talk the next day. kratchmer urges him to publish the raman spectra
[[THE IBM LAB GOT IN LATE AND SUCCEEDED REALLY FAST BECAUSE OF ITS INTERDISCIPLINARY RESCOURCES!]]]
12sep
kratchmer gives his report his photos of crystals and xray diffraction made audience realize something amazing in carbon science had happened
then smalley gave his talk on the original 85 work and La enclosed fullerenes
then whetten told group that he knew kroto had isolated 60 and 70 and got 1line nmr on 60 and 5 on 70
Whetten agrees to visit kratchmer lab maybe think ideas for better xray diffrac
smalley was amazed that the ibm team had been able to collect so much C60 from soot from laser evaporation where he and heath had spent year and gave up. [[did they have it all along?]]
15sep
bethune returns to usa and Meijer greets him at airport and rushes jetlagged bethune to the lab: photo of scanning tunneling micrograph of layer of buckyballs on gold surface! with a few c70s thrown in. then also: the single line NMR spec.
WHAT YOU CAN DO WITH SINGLE INTERDISCIPLANRY LAB WITH LOTS OF MONEY AND GOOD MACHINERY!
BUT HERE IS THE DEAL, THIS IS WHY WE THINK OF C60 AS ***REAL*** SO MANY LABS FROM SO MANY ANGLES GET RESULTS THAT JIVE: mass spec, specific signal at 60 70, geometry, huckel theory, La in cages, suggestive uv spec, producing it from laser ablation and cooling, from carbon arc to soot, laser ablation... IR spec, tons of calculations from diff ideas, chem and sublimation purification, raman spec, NMR of 60 and of 70, crystalization, electron diffrac to get spheres, scanning tunneling microscope to get spheres...
AND AFTER 300 YEARS OF KNOWING HOW EASY IT IS TO BE FOOLED, THESE RESULTS ARE DONE OVER AND OVER AGAIN BY DIFF PEOPLE WITH SLIGHTLY DIFF TECHNIQUES CO9NSTANTLY CHECKING EACH OTHER SO YOU KNOW YOU ARE NOT CHASING WILD GOOSE
ALSO TO REALISE THIS ISN'T SUCH AN ARTIFICIAL SPECIALIZED STATE OF MATTER BUT IT CAN FORM QUITE EASILY IN A NUMBER OF DIFFERENT ENVIRONS...
diederich and whetten work with Kratchmer to separate 60 from 70 publish some results in jnl phys chem oct 3
they were eventually able to get 14% yeild in their own carbon evaporator!!
smalley group built a fullerene generator with spring loaded carbon sticks that got 10% yield on 10 grams in a few hours! they begin to do fullerene CHEMISTRY!
DEC 13
ibm stm image is published along with an image by jeffrey wragge chamberlin and white from fullerite obtranied ffrom kratchmer lab
STILL WANTED XRAY DIFFRAC to nail the carbon carbon distances and really show its buckyball
finally ibm gets solid nmr spec not make sense! HOW DID THEY DEDUCE IT'S BECAUSE THE BALLS ARE ROTATING? anyway by cooling the solid they get the spectrum to broaden as it should showing that the room temp balls ARE spinning, that's why no one could bet dcent xray diffrac nor did the stm image show any atomic detail, just fuzzy balls
the balls spin 10billion times a second, cool it enough and get ratchet phase balls click one atom at a time, till cool it to stillnes
at about the same time bell labs gets similar results
ibm then used C13 enriched cooled C60 to get interatomic distances. two sets: 0.140 and 0.145nm the shorter distance in the pentagons, all together it makes the 0.71nm buckyball
bethune's colleage bob johnson then used another nmr technique to nail interatom distances in C70 that yield the 5 spike signal. johnson's result also showed that the C13s are incorporated randomly into the ball suggesting that they are being incorporated into the ball during discharge in the gas phase atom by atom, not from peices of the graphite.
finally joel hawkins et al 91 pin some molecules to the bucky balls in the same places and get them to stop spinning and crystalize orderly, and get xray diffrac and get the two c-c distances: 0.1386, 0.14324 match!
buckyballs is a molecule!
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