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ANDERSEN Jens E.T., 2001-03-06

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Jens E. T. Andersen est chercheur au Département de Chimie de la Technical University of Denmark à Lyngby. Dès 1992, il utilise une technique inaugurée par Dieter Kolb et Richard Nichols un an auparavant : le microscope à effet tunnel en milieu liquide, appelé également « STM in situ » ou « microscopie électrochimique à balayage » (SECM pour Scanning ElectroChemical Microscopy). À partir de 1995, Jens E. T. Andersen a étendu la gamme de ses usages du STM in situ de l’électrochimie à la biologie, en imageant des protéines adsorbées sur des surfaces. Il a organisé trois conférences sur la technique du STM in situ en 1994, 1996 et 2000.

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Pour citer l’entretien :

« Entretien avec Jens E.T. Andersen », par Arne Hessenbruch, 6 mars 2001, Sciences : histoire orale,

Lieu : Danish Technical University, Lyngby, Danemark.

Support : enregistrement cassette.

Transcription : Arne Hessenbruch.

Édition en ligne : Sacha Loeve

ARNE HESSENBRUCH (AH) : Could you give us an overview of your academic career ?

JENS E.T. ANDERSEN (JA) : I studied chemistry and physics. I majored in chemistry and got a bachelor’s degree in physics at the University of Copenhagen in 1987. I did the Danish equivalent of the PhD for three years in surface science at Preben Juul Møller’s laboratory at the University of Copenhagen, doing metal on insulator surfaces. I finished in 1991, after which I got a post-doc at the University of Cambridge, with Dr. Richard Lambert - he is now a professor at the Chemical laboratory. I worked for a year and a half on a catalytic effect denoted as NEMCA, Non-Faradic Electrochemical Modification of Catalytic Activity (figure 1). We wanted to investigate this effect, invented by a Greek scientist in the late 80’s, and we wished to check this under UHV conditions. Then I saw this advertisement for a Danish position to implement a technique called in situ STM. Not just STM, but in situ STM, or electrochemical STM. You see in 1990, as far as I recall, or 1991, Prof. Kolb (University of Ulm) and Richard Nichols (University of Liverpool) found that you were able to operate an STM while the atoms were submerged in a conducting liquid, in an electrolyte, like water. This was a sensation. We used LEED (Low Energy Electron Diffraction) imaging to study electronic details of electronic diffraction, but it was very difficult, especially because we needed UHV conditions. It seemed absolutely sensational that one could image something like that under ambient conditions in air in a liquid, just by electrochemical control of the STM tip. That was brilliant, and this really aroused some interest in me. I took this position. I applied with Per Møller at the Institute of manufacturing and engineering here at the Danish Technical University in 1992 to get the job and I was successful. We continued for two years developing the instrument together with DME. So the purpose with this project...

Figure 1. Non-faradic electrochemical modification of catalytic activity (NEMCA) Principle.

AH : So when you started out with surface science, did you know about STM in the late 80s. It was not of very great interest ?

JA : Well it was interesting as such, because we all speculated : is this technique really able to image atoms. What is it that we really see in the images ? Are these blobs really atoms ? But I think in the mid 80’s it became evident that you could image a silicon 7x7 reconstruction, and this convinced me that this was some kind of atomic resolution. So it was all a technique that was developing.

AH : So you even knew about the STM in the early 80’s. You’d heard about Binnig and Rohrer and you kept an eye on it, but you were not convinced. The blobs had to be...

JA : Had to be something to do with metal conduction bands and the band structure of metals. Semiconductor structures, and maybe more subtle to interpret. But with the silicon 7 x 7 reconstruction it seemed sort of convincing.

AH : And was this common in surface science, or maybe even in chemistry ?

JA : I think it’s more or less a part of the education that you keep an eye on some of the new techniques. You see, the question always arises : what is an atom in reality ? At that time Transmission Electron Microscopy was the prominent technique of atomic studies. But it has become less prominent in the light of STM, because the latter is fairly easy to use and also less expensive. But then again one asks, is it really atoms ? At that time lots of people were speculating and still there is not a convincing theory describing all the details of the tunneling experiments.

AH : I presume that by the time Binnig and Rohrer had gotten the Nobel prize in 1986, then there was no doubt that these blobs were atomic resolution. Everyone agreed about this. But there was still not commercial STM’s on the market, you couldn’t have used STM’s yourself.

JA : I’m not really sure, the Nanoscope, was that in 1980 ?

AH : Late 80’s. Digital Instruments was only founded after the Nobel prize.

JA : But when they received the Nobel prize I presume they invented Atomic Force Microscopy in the same year ?

AH : 1986, right. But you would have had to build one yourself, and Joergen Garnaes over there [across the road] in the early 90’s he was building his own. And he could only buy one off the shelf in 1992, and there was no longer a point in building one.

JA : In 1991 DME was putting the instrument on the market, but I think Digital Instruments, they were much earlier. I think Besenbacher, who was the Danish pioneer, built his own instruments in the early 80’s, mid 80’s. He’s recognized as a real scientist of developing STM also to convince scientists that this is really a technique of the future. I think he made a really impressive contribution there. So I think he did that in the mid-80’s, he must have because I started out doing surface science in 1987, and he was well known in the field at that time. [Actually, Besenbacher, Lægsgaard, and Stensgaard built their first STM in 1987.]

AH : So in your own work in 1987, what tools did you use, what characterizing tools did you use ?

JA : I used the most common tools, low energy electron diffraction and electron spectroscopy, Auger electron spectroscopy, electron deposition for building up atomic layers, and high resolution EELS (Electron Energy Loss Spectroscopy).

AH : The whole palette ?

JA : Not x-rays. X-rays is a common surface technique of elemental analysis, but we analyzed by AES (Auger Electron Spectroscopy). I think I was also one of the only ones in Denmark doing high-resolution ELS and analyzing surface optical phonons on insulators. This is a fairly difficult technique, and Preben Juul Møller, I think, was the only one who had the instrument at the time. And together with 2 Chinese guys we made it work properly. So we got some interesting surface optical phonon studies of metallic insulator surfaces. The interface of insulators and metals.

AH : Would you describe how that works ? The instrument, and what you had to do to get it work.

JA : The difficulty is, that it is a very narrow electron beam of low energy and you have to focus it delicately - it’s a very delicate focusing problem. You have to optimize with an electrometer where you measure all the currents at the equipment and then you try to focus into the detector, which is a fairly difficult process, and the manufacturer couldn’t really tell you how to do it. Just told us optimize, use optimizing procedures. And we were three people, working on this for three months, and then we made it work by a systematic optimizing approach. You can never do anything by trial and error. Optimizing by statistical methods, experimental planning basically. We used the instrument for a fortnight each, and we did as well as we could, a sort of competitive method of achieving the best signals, and suddenly we got the same signals as the manufacture’s best signal. But I think it’s quite a struggle, and too much of a struggle in comparison to the information you get out of it. But it was fun trying to make this very delicate instrument working. This is interesting for low energy electron studies, when you can do spectroscopy of something like phonons, that’s quite interesting I think. And one of the Chinese guys, Guo Qinlin he’s now a professor in China with a group of 30 people, and the other one, Dr. Wu Mingcheng, he went to the States and was employed in Texas A&M, College Station and he is still living there. So he did quite a good job and produced very exciting results, it was really good experimentally, brilliant. But then the technique you can study surface optical phonons, and overtones of these optical phonons, it can give you an idea about the electronic structure of the surface of insulators.

AH : So, is this a common thread for you to use new techniques try to stay abreast in most recent technology and use them to find out about surfaces ?

JA : In the sense that they can give us new information inside of how Nature is working, then it’s interesting. Some new techniques emerged, I think, that are not that much of a help to something that we know already. When it’s complementary, they can be the sort you need to advance only slightly. Some of the really new exciting technologies can do something that was not possible before, such as the in situ STM, where you can study atoms in an electrolyte medium.

AH : And you started using the in situ STM when you got here in 1994 ?

JA : 1992.

AH : But you had an interlude in Cambridge, and you didn’t work on the STM in Cambridge. What tools did you use then ?

JA : Mainly mass spectrometry and Auger. I think we may have used electron energy loss spectrometry. Oh yes, we also used thermal desorption spectrometry together with the mass spectrometer to study molecules desorbing off a surface. This was quite an interesting project and we had a close collaboration with the Greek group who invented this technique.

AH : In Athens ?

JA : It may have been the University of Athens. Constantinos Vayenas was the head of the group. And Ioannis Yentakakis was our collaborator at the time. He went to Cambridge and we started this phenomenon under UHV conditions. We succeeded and I was happy to see what was going on, and we went as far as we could interpreting their method. They have brilliant articles in many famous journals where they show how this effect was working. When we got it running under UHV conditions it was not a significant effect, we could not be convinced that this was as brilliant, as they told us it should have been. To this day, a lot of work is going on to study what exactly this NEMCA effect is. So we didn’t really finish the project completely because I left for another position, but I got enough information as to decide not to build a career on it. It was something really exciting, a new science and a new idea, a new and novel effect you can study in detail and resolve all the chemical mechanisms. But I think it was fairly simple. It was an increase in oxygen production by the material that was used for the electrochemistry - it was sort of solid state electrochemistry. And a zirconium dioxide ionic conductor where you can pass oxygen ions through a material by electrochemical potential differences. You can also desorb oxygen off the surface, and of course if you got an oxygen consuming process at the surface you will consume the oxygen produced by the material. And in my mind it was all coming from the material, but my colleagues were not quite convinced, so we disagreed a little.

AH : So you agreed to disagree in the end.

JA : Yes.

AH : How did you get to work in Cambridge in this period ?

JA : Well I had been working with Dr. Preben Juul Møller at University of Copenhagen in surface science and it was sort of a natural continuation of the career. You have to apply for vacant positions abroad, and I was maybe overdoing it a little applying for a position at Cambridge. Richard Lambert knew Preben Juul Møller very well. He was familiar with his work on insulators. So I had been working on insulators and metallic surfaces contacts for 3 years and I knew what it was about. And I think also very quickly, within half a year, we constructed the necessary UHV improvements to study this NEMCA effect together with Ian Harkness, a scottish PhD student who made a brilliant job of constructing this electrochemical cell for UHV conditions. It’s not trivial to make this sort of system, but we did it within half a year. And then we got a whole year of studying the NEMCA effect which worked quite well. But of course I was extremely surprised and happy that I could get this post-doc position at Cambridge.

AH : The laboratory life at Cambridge is very similar to that of the University of Copenhagen ?

JA : Yes.

AH : Same kinds of equipment same level of funding ?

JA : The funding is better at Cambridge. More students available for the studies, but equipment is similar. The level of science is also basically similar, teaching is probably a little better at Cambridge. I haven’t followed the graduate courses, but to my knowledge some of the people there were really brilliant. The young PhD students were really brilliant scientists.

AH : Were you a member of a college ?

JA : No, I was not affiliated through the colleges. I did try to become a member of some of the colleges, but as a post-doc you are not supposed to interfere with college life.

AH : So the people you talked to were people in your field, in your lab.

JA : Yes it was a highly professional and competitive working environment and I think a very good time.

AH : Was it also a lot of fun ?

JA : Well, it was hard work – I am not sure about fun. I had my family with our daughter aged six months. Also my wife was not too happy, it was one of the reasons why we left a little early. We were supposed to stay for 2 years, we left after 1.5 years. My wife also wanted to go back because it was tough when I was working from 9am until late in the evening. She didn’t really have anything to do apart from taking care of our daughter. And she has a Masters in music and rhetoric and wanted to use her education. It was a little too boring for her, I think. But for me it was excellent.

AH : And so you went back to the in situ STM ?

JA : Yes, I started with the STM when I arrived back in Denmark. I had never worked with the STM before.

AH : But you had kept an eye on STM all the while.

JA : Oh yes, as a surface scientist you always look out for interesting techniques that are competitive to what you have in your field. And when I saw this atomic resolution in an electrolyte, I couldn’t believe it, because you can’t imagine the struggles you have to go through to make a metallic surface clean under UHV conditions. And once it’s clean you have only approximately half an hour to make all your studies because it adsorbs all the gases even under UHV conditions. Approximately one hour you can keep your surface clean under UHV conditions. By contrast, with the arrival of the STM you suddenly were able to study atoms under brilliant conditions (ambient conditions) with a low cost instrument and you can even deposit atoms electrochemically. You can study the metallic overlayer at atomic resolution while it is being constructed atom by atom. I just couldn’t believe my own eyes. My colleagues and the PhD students had a good laugh and they said : “So, you’re going into in situ STM submerged surfaces. Well, you will need a diving suit.” I assured them that “No, no, no, it’s atomic resolution.” They didn’t believe me. We discussed the article and I have to say that even Richard Lambert was really surprised that this was possible.

AH : So you were one of the people that convinced others that this was possible, that this was real.

JA : Well it seemed real. If there is a paper in Physical Review Letters my attitude is always to take it seriously ? And you can study also the references in the particular paper by Richard Nichols. You can see in the references that they had been struggling with various modifications of STM to get this result. So it seemed very convincing to me.

AH : But if someone like Lambert was critical, he must have had a good reason. And you say that...

JA : It’s so difficult to get a clean metallic surface and it’s so highly reactive towards gases in the background and it will destroy the clean surface in a matter of minutes and then suddenly you can have water on top of the metal adsorbing to the metallic surface and you can still observe your atoms. At first nobody really understood, and they said okay it was an aqueous monolayer or something like that, we observed under liquid conditions. Of course this is not what Nichols told us - It’s really metallic atoms deposited electrochemically, you can see atom by atom building up. No doubt !

AH : So Richard Lambert didn’t develop a new STM really, he just used it ?

JA : Well he did acquire an STM for UHV studies at a later stage. Maybe he got it while I was there, but he was convinced that this was a technique he also had to consider for catalytic studies.

AH : But he didn’t build his own STM. You take an STM off the shelf and use it for new studies.

JA : But it wasn’t much off the shelf for UHV conditions. I think there was one Swiss company building UHV equipment for the STM.

AH : So a UHV chamber with an STM inside as a package ?

JA : Yes.

AH : And the job here was advertised for in situ STM you said ?

JA : It was advertised in a Danish union journal. Magisterbladet, I think. Or maybe it was in Ingeniøren.

AH : So the people here, they must have trusted the new technique also.

JA : Well you see, Danish Micro-Engineering produced the instrument already before I arrived. I think they sold 10 or 20 air STM equipments around Europe. So they wished to develop the STM. They considered this to be a minor problem and they employed me to do the job. As a matter of fact, Per Møller who advertised this position wasn’t really familiar with science as such, but the purpose of implementing this technique was to use it for bulk electrochemical studies. So he would more easily be able to study corrosion processes under the real conditions in an electrolyte. He also wanted to use the instrument to automate electrochemical deposition. You know, he is an expert in plating. So we would like to optimize plating processes, let’s say pulse plating and things like that. We wanted to study such things with the instrument. He also wanted to build small metallic machinery, something like submarines swimming about in your veins, depositing medicals at the right spots.

AH : Nanomachines ?

JA : Nanomachines. Within 10 months we got the desired atomic resolution and we finished development of the instrument. I’m saying we because Carl-Erik Foverskov, an instrument maker at the institute, he made the design for a bi-potentiostat. Actually, I must mention that I visited Richard Nichols. I think that without his help we would have taken much longer.

AH : Where was Richard Nichols ?

JA : Richard Nicols was employed at Schering, in Berlin. Schering is a pharmaceutical company, and they were taken over by a French company, Atotech. He stayed in Berlin for a number of years doing in situ STM. But he helped me out with some of the problems. I visited him in Berlin and he participated in our conferences. He was invited to help us out, and he also delivered some of the gold samples that were necessary to obtain atomic resolution. So he was very helpful. Within 10 months, we improved the DME instrument, got atomic resolution, and it was ready for distribution, ready for sale. They needed maybe six more months before they were ready to sell the instrument.

AH : What was the connection between the Danish Technical University and the DME in your job ? You said there was a DME that started the job how did they influence the DTU ?

JA : The connection was Per Møller, the center leader. He was head of the Center for advanced electroplating at the DTU. In Denmark, such a center must be a collaboration between DTU and a company. I think there must be something like 3 institutions involved. I don’t know which was the third, but I think it’s Danish Plating Industry, something like that. So it was a joint venture. I think we succeeded. But I remember that Møller wasn’t too happy about the outcome, because he wasn’t really interested in the scientific achievements. And we even made this instrument work for pulse plating, varying electrochemical potentials up and down very quickly. This influences the instrument, so you lose the imaging, but we could maintain the imaging while doing pulse plating.

AH : What did you do next ?

JA : Then I was employed with Professor Ulstrup, who’s a bioinorganics scientist. I never expected to be involved in bio-something. But then suddenly I found myself in the imaging of proteins. I still don’t know what a protein is. [Laughter] Today I do know a little about this field. We started a joint venture with Per Møller, and we applied for the [Danish] National Technical Science Foundation and got a three-year project. We were supposed to image proteins, and yet we uncertain about what we saw in the STM images (figure 2). But we knew some other group in Europe was grappling with proteins because if you can image proteins, you can image the molecule of life. That’s really a big thing. It took quite a while but we succeeded.

Figure 2. In situ STM image of azurin adsorbed on gold(111).

From Esben P. Friis, Jens E. T. Andersen, Yu. I. Kharkats, A. M. Kuznetsov, R. J. Nichols, J.-D. Zhang, and Jens Ulstrup, 1999, « An approach to long-range electron transfer mechanisms in metalloproteins : In situ scanning tunneling microscopy with submolecular resolution », Proceedings of the National Academy of Sciences of the United States of America, vol. 96, n° 4, pp. 1379-1384 (figure 7). Quoting the paper : « individual molecules and a submolecular central feature of brighter contrast are clearly visible ». Copyright © 1999, The National Academy of Sciences.

AH : Which groups ?

JA : Professor Kolb in Ulm. Well, he is working not on proteins as such. Dr. Davis at Oxford and his group. Prof Allen Hill, also Oxford. They are the prime investigators in Europe I think. They have come up with some of the best results, including the imaging of proteins. So we’ve been working in parallel towards the same goal and we arrived there sort of simultaneously.

AH : And when did you succeed ?

JA : 1996 I think.

AH : Were in touch with Hansma ?

JA : Not as such, but I asked him for some preprints, and he sent me some piles of preprints and said "I’m happy you’re working in this important field." He encouraged us very much and we invited him to our conference last year in 2000, but he was not able to attend. But he’s done very good work and I think encouraged us to continue what we were doing.

AH : So these workshops. How did they start. Who took the initiative ?

JA : That’s professor Ulstrup. 100%. He took all the initiative. When he saw this instrument and that we were able to image proteins he became very excited because he’s a theoretician doing electrochemistry on metalloproteins. He has developed protein electrochemistry together with Allen Hill but from a more theoretical point of view. And then he’s got me and the group to do the experiments. This way he could develop his theory. He took the initiative and then we’ve got lists of Danish companies and foundations who supported the first workshop. It’s no problem to obtain funding for this purpose, I think. We even got funding from the Danish National Research Foundation. You know the Carlsberg Foundation in Copenhagen, they’ve got a house of science, the Royal Danish Academy of Science and Letters. And they supported us so we could use the premises of their Foundation. There was I think 60 people attending the workshop, in 1994.

AH : Was it a conference on STM in general ?

JA : No it was on in situ STM, electrochemical STM, also called scanning electrochemical microscopy. Allen Bard at the University of Texas, Austin, invented a similar method, and he denoted it as SECM - scanning electrochemical microscopy. So there are various denotations of this technique. We say in situ because we image while it’s occuring.

AH : What sort of people came in 1994 ? What fields did they come from ?

JA : Well we invited people to display their results in STM in general and we did get some contributions that were not really in situ. It’s definitely not under water, it is not in an electrolyte. We accepted more or less a wide range of contributions because there were overlaps also with in situ in many fields : solid state depositions by vacuum evaporation can also be considered as in situ, and can be made as comparison to some of our in situ experiments. But the purpose was to promote in situ STM. We still believe that in situ STM is superior to regular STM. The availability, information, methods, and scientific results you can obtain are more varied, there are many things you can do. So we would like to promote this technique and of course you can also image proteins in air, but we would like to image molecules in their own environment, which is electrolyte environments. And I’ve also considered to image viruses and things like that. At the present stage we have imaged proteins satisfactorily, and we have been promoting in situ STM also in the year 2000 to make people understand that this is really something worthwhile.

AH : Have you had a conference every year since 1994 ?

JA : No, only in 1994, 1996, and 2000.

AH : Were the people who came in 1996 all in situ STM people ?

JA : Almost yes.

JA : It was absolutely the most important groups in Europe represented at this congress and some invited speakers from the States also present. I think there were a couple of students from Japan, but no speakers from there.

AH : How many people came in ’96 ?

JA : There was around 60 people – same as in 1994.

AH : And in 2000 ?

JA : The same

AH : Any change in composition of attendees in 2000 ?

JA : No, the same groups were represented. The focus was more bio-oriented in 2000 because now the issue was protein superstructures. Bio-inorganic imaging, that was the purpose, so there were some new groups.

AH : Is that because you are now more involved in the bio-side, or because the field in general has moved towards bio.

JA : I don’t think the field in general has moved towards bio. The prime investigations are still made in superstructures and under-potential deposition, which is mono-layer studies, because in situ STM is the only technique where you can obtain atomic resolution. Subatomic resolution can be obtained even with other techniques than in situ STM. Some groups may consider imaging of proteins as subatomic. It’s not really atomic resolution. Superatomic I’d say, not really at a higher resolution but at a lower resolution than atomic resolution. And they don’t consider this very interesting because you get some difficulties in STM theory : how does it work when you see a protein ? People are a little anxious that they may be studying artifacts rather than real molecules.

AH : Yes of course.

JA : There are a number of artifacts in STM, it’s known for artifacts.

AH : Can we back up a little ? I have difficulties imagining just how you would scan something like a protein where you don’t have a surface, right ? You have something more unwieldy - how does it work ?

JA : It’s a little surprising when you try to study large features with STM because the tunneling distance is some 10 Ångstroms, and a protein is at least 40 Ångstroms in diameter. Obviously, the tunneling current itself ought to deform the protein completely. And something like the deformation of a protein is observed : it’s flattened considerably. The measured thickness of a protein is approximately 20 Ångstroms so it’s probably flattened while in scanning. But it needs to be immobilized at a surface, otherwise you cannot get the image.

AH : How do you do that ?

JA : We choose specific enzymes and proteins where you have a sulfide bridge to a gold surface. If you react sulfides or thiols with gold you form a covalent bond that is relatively strong. Sulfides react readily with gold surfaces, and our problem in the first instance was to show that we were able to image proteins that were immobilized properly and the question was : Is one sulfide bridge from the protein to the gold surface sufficient linkage for imaging ? And it turned out it was adequate. There was just one molecular bond to the gold surface from the protein, through this sulfide bridge.

AH : Thank you !

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