Sciences : histoire orale

HIRAO Kazuyuki, 2002-08-29

Sophie Jourdin — 2011-11-04T13:08:55Z

Kazuyuki Hirao.

—

HERVE ARRIBART (HA) : In which discipline did you take your degree and your Ph.D.?

KAZUYUKI HIRAO (KH) : I was trained in Inorganic Chemistry.

BERNADETTE BENSAUDE-VINCENT (BBV) : Why did you decide to go into Glass Science ?

KH : Well, you know, the Chemistry Department of Kyoto University is very old, 100 years old. When I had to select a laboratory, I was interested in inorganic chemistry. I belonged to the Chemistry Department but only one division of chemistry was Glass or Ceramics related to inorganic chemistry.

BBV : Did you publish books in inorganic chemistry ?

KH : Yes, I published two textbooks on Inorganic Chemistry intended for undergraduates. One of the textbooks was translated but another one I wrote myself in Japanese.

BBV : Do you have to teach inorganic chemistry ?

KH : Yes at the undergraduate level.

BBV : And do you have to teach a course in Materials Science ?

KH : Yes I have 3 courses a week : one of them is Glass Science, the second is Advanced Materials, and the 3rd one is Inorganic Chemistry. Inorganic Chemistry for undergraduate students, Glass science and Advanced Materials for graduate students.

BBV : There is no department of Materials Science at Kyoto University ?

KH : Materials Science partly belongs to chemistry. My department is called Department of Materials Chemistry. But Materials also belongs to Metallurgy. They have a department of Materials Science which is totally separated from us. We have no common class between Materials Science for chemists and Materials Science for metallurgy. We have to collaborate in the future. The Department of Materials Science also belongs to the Department of Mechanics. Chemistry and Mechanics are totally different. Polymer Chemistry is also separated. We still have to build up the new class of Materials Science. In Japanese universities, it is not usual to have interdisciplinary Materials Centers. It is usually divided. It is not good for research. Because equipment is shared.

HA : What kind of instruments ?

KH : TEM, SEM, X Ray, spectroscopy. At least in nanotechnology we ignore the boundaries between polymer science, metals, ceramics and glass. It will be possible to develop the new materials perspective.

BBV : Do you think that this traditional university system prevents you from doing Materials Science ?

KH : It is difficult to change. If you want to change anything, you will have to obtain agreements from all the professors in our departments. University professors are very conservative.

HA : Still, Professor Soga did endeavor to change the system while he was here.

KH : Yes, but in Japan if one single professor is against the change, then there will be no change at all. We don't usually have a majority decision making system.

BBV : Are the students more attracted by Materials Science in general or by Chemistry and Physics ?

KH : The entrance examination is about Industrial Chemistry. Almost 250 students are admitted. After one year, in the 2nd grade, they will be distributed into three different courses. Three classes divided mechanically. In the 4th grade they chose to enter into one the laboratories of the department. Four graduate students choose to enter in my laboratory every year. Kyoto University is a very big university. We have almost 47 chemistry professors for 250 students. 150 graduate students. Two Nobel Prizes came out from this department. It is a prestigious department.

HA : Could we come back to your PhD subject ? How did you choose it ? Was it Professor Soga who proposed it ?

KH : Yes it was about Glass Science. Thermal properties of glass.

HA : From your list of publications I can see that you have worked on many, many fieldswhile working in Professor Soga's laboratory.

KH : Yes I have been mainly interested in computer simulation of making glass structure and predicting optical properties of glass. I started computer simulation early in the 1980s. It was too early. The computer capacity was very small in the 1980s. Now we have a big project on computer simulation program and we get $5 million over five years from the government for it. Owing to the progress of computers, we can make glass structure containing 10,000 atoms.

HA : Then why did you move to non-linear optics instead of mechanical properties or low temperature behavior ?

KH : It is a good point. One major advantage of glass is transparency. Its major disadvantage is brittleness. Optical fibers are a very important because electrical wires are very limited in speed.

HA : So by the end of the 1980s you guessed that the future of glass for a large application would be optical glasses.

KH : Now we are very lucky. We are also interested in the mechanical properties of glass at the nanolevel. We are dealing with elimination of the nanobubbles. It is very important for industrial companies.

HA : So you got in to the glass making process ?

KH : Yes.

BBV : Was it industrial demand that prompted you to work on optical properties in the 1980s ? Or was it your own initiative, your choice ?

KH : In this period the optical properties were not important for glass industry. Now many glass companies are interested. So now we have a lot of industrial contacts. Before next year we intend to produce 3 commercial optical glasses called photonic glasses. For this, we need connections with venture business.

BBV : Do you mean that you conducted all these researches on optical properties without industrial support ?

KH : No, only in the beginning. Now we get a lot of industrial support. But now I get a lot of budgets from three kinds of government projects, not only from industry. We have 3 projects. One is computer simulation. One is on photoactive glass in cooperation with foreign countries. So we have a lot of post-docs in my laboratory. The third one is the nanoglass project.

HA : Could you tell us about this nanoglass project ?

KH : The government launched a nanotech program that covers a variety of projects : nanometals , nanopolymers, carbon nanotubes, nanocoatings, nanoparticles, nanosimulation and the nanoglass project. For the latter, we get $30 million for 5 years approximately.

HA : How do you spend this amount of money.

KH : Most people involved in the glass project are coming from industry, from Asahi Glass, Hoya, Nippon Electric Glass, Central Glass, Okamoto Glass, Nippon Yamamura Glass, Hitachi, ... 11 companies sent us 15 researchers whose salaries are paid by the project.

HA : How many people are working in your nanoglass project ?

KH : 100 people including the supporters. They join in Tsukuba consortium, from Osaka Institute and several university professors also support us.We have some large equipment.

HA : When did this project start ?

KH : We had a preliminary year and the project itself started in 2001.We have got a number of results. For instance CVD deposition. We also succeed in making very low optical loss glasses. We have reached 0.005dB/cm. This glass will be very useful for making waveguides. In Tsukuba we use two kinds of femtosecond lasers working at 1 kHz and 200 kHz. By using these femtosecond lasers, we not only write in waveguides but also we make crystals from glass, for example silicon crystals from amorphous silica.

HA : Last time you mentioned that you also have a laboratory in China working on crystal growth.

KH : That is right. And we have also made a lot of semiconductors, single crystals in glasses by using this material and we made photonic crystals, which can be used as optical filters.

HA : Where does the money for this nanoglass project come from ?

KH : From NEDO. It is part of METI (Ministry of Economy, Trade and Industry). No connection with AIST although METI also supports AIST. We also made a very tough glass whose strength is very high, 2 times that of standard glass. With the femtosecond laser we made very small dots, nanosize dots, that stop the cracks. We have already succeed.

HA : Was it enough to make these tiny holes on the surface ?

KH : They are under the surface. Also by using the interference technique we have made a lot of dots.

HA : I understand, it is beautiful glass but too costly for bottle makers.

KH : Of course it is not for bottle makers ! Also we have found a cheap process to make AWG (array wave-guide grating) by using the femtosecond laser. AWG are very useful for optical telecommunications. Until now, they were very expensive to make. We also managed to make a nanoglass thin film for CD. The storage medium can be a cobalt oxide-based glass, for example. When we apply a nanoglass coating on this recording material the blue beam is shrinked to ¼. This is a lens effect. We have now this optical disk standardized by Hitachi. So you know that Shuji Nakamura ; a Japanese researcher, has discovered the blue laser diode. In my case by using this blue laser diode, the recording capacity is approximately increased by a factor 4, because the beam is much smaller. And in the field of optoelectronics, we have made 3 dimensional devices including both electrical and optical circuits. We use gold containing glasses that crystallize under laser beam. Three dimensional wires can be obtained, together with optical waveguides in the same device.

HA : So this program seems to be essentially telecommunication oriented.

KH : Yes NEDO asked us to make such devices. Otherwise they would cut the financial support.

BBV : You mean that the budget is according to your practical results.

KH : Yes.

BBV : What kind of connections do you have with venture business ?

KH : For optical properties we have to make such connections. Otherwise we could not do it on university money or government money. Venture business have a lot of demands in optical properties of glasses. For instance some fibermakers make lenses inside optical fibers. With my technique of femtosecond laser we can make lense in fiber. There are many such innovations of interest for business, although optical properties are not directly related to optical devices.

BBV : Do you mean that you only do research and no development ?

KH : Optical properties are synchronized with optical devices. There is no linear sequence from optical properties to technical devices, from basic research to applied science then development. We have to work in synergy.

HA : So do you consider yourself as a materials scientist because you are dealing with devices ?

KH : Yes we have to make connections with venture business and industry. For doing this kind of research we have to build a wide network. So many venture businesses are connected with me and they are eager to be.

HA : Where does the money come from ? From big industrial companies ?

KH : So far my devices did not cost much. If one day we have to develop a costly device, the Japanese governement is able to support us immediately, at least for two or 3 years. The Japanese governement is encouraging this kind of cooperation.

HA : Do you also collaborate with foreign companies ?

KH : With Schott in Germany. They have sent a researcher here. And Corning is also willing to collaborate. In the USA glass professors are not so many in optical devices. Here we have more than 50 professors of Glass Science

BBV : Do you send students to the USA ?

KH : Not right now.

HA : Where do you locate the leading centers in your field ?

KH : I guess Osaka is the center. Glass science originated in Osaka National Center.

HA : You told me last year that you run many laboratories. How many ?

KH : I have 6 laboratories including one in China, one in Osaka, one Tsukuba ... 300 people altogether. There are autonomous and eager to make things because optical devices is a very promising field. So I don't have to be continuously behind them. There are so many things to do such as inkjet using semiconducting cadmium selenide nanoparticles. The color changes depending on particle size.

HA : This is not glass. Is it ?

KH : Yes it is, because nanoparticle CdSe particles are made in micelles and encapsuled by glass using sol-gel chemistry. The fluorescent yield increases nearly 10times using these nanoparticles. Silica sol-gel coating is necessary ; otherwise the semiconductor particles aggregate to each other. Encapsulated particles are then deposited by inkjet to make displays. We do this development by collaborating with venture business.

BBV : So you seem to work as a partner of venture business, as a manager of projects rather than as a traditional scientist supplying science for applications downstream.

KH : Yes my aim is really to make optical devices. This is what we have to do. We teach Glass Science. But in laboratory research we have to make devices. Traditional professors are not interested in devices ; I am. But you see, in Japan I don't have to move to an industrial company to make such devices.

BBV : Is it part of your obligations as a university professor to make devices ?

KH : No, teaching is the only obligation. We just have to teach and take care of the students.

BBV : Does the university system recognize your devices ?

KH : Yes now the government recognizes patents.

HA : So you feel that you are in a better position at the university because you have the freedom of choosing your topics of research and you have the money that you need for them.

KH : Yes I am very lucky.

BBV : How do you select your research projects ?

KH : The keywords are glass and optics. We have a lot of choices. One criterium is to use the femtosecond laser.

HA : You mean that you can use it to change glass composition ?

KH : If we use samarium doped glasses we can change the samarium3+ to samarium2+ with the femtosecond laser. So glass composition is very important for me. Not just to make new glasses and measure their optical properties. If we make a new glass it is to make a new device by using a new technique. We also made electrical lithography by plasma etching for nanodevices, in Osaka.

HA : On our webpage you also mention that you are working on hybrid materials.

KH : Yes usually at the macroscale, it is difficult to combine organic and inorganic components. Nanohybrids work better by using chemical reactions with micelles. Professor Tetsuo Yazawa at Himeji Institute of Technology University made a lot of nanohybrids that can be used for gas filters, for membranes, solid sensors and solid electrolytes. Conductivity is very high in the nanohybrids. Both electronic and ionic conductivities. And hybrids are also useful for glass capsules for drug delivery. So we started that kind of research on hybrids within the nanoglass project.

BBV : Do you try to compete with other materials in your nanoglass project ?

KH : No, glass offers unique advantages. We can overcome polymers. Glass is the only transparent material even at the nanoscale. I forgot ! Athermal glass is very important. We achieved athermal glass-ceramics we have to apply pressure to control the size of the nanoparticles and the growth. So nanoglass is unique and very useful.

HA : I can see that your project works very well. But do you remember any failure in your research career ? It is also instructive for our project on the history of Materials Science.

KH : For the Photoncraft project we are at the middle point so we have to submit. The nanoglass project started one year ago. We have to make an effort, otherwise budget might be cut.

HA : This morning Professor Soga told us that he considers himself as an educator rather than as a glass scientist. Is teaching and training also important for you ?

KH : You cannot separate teaching and research. Education and laboratory work together. In the field of glass, just making optical devices is a good education, a good training. Now we are training a number of students through the nanoglass project.

BBV : Do you mean that the nanoglass project is in itself a kind of training ?

KH : Yes, for graduate students. When I present the results of our nanoglass project to company presidents, they are essentially grateful for our work as educators because we train the researchers from industrial companies. Helping each other is very important.

HA : Does it mean that you are no longer interested in basic research and basic education ?

KH : No. Presently I am making devices but maybe in a few years I write a new textbook of glass science because they are so many new glasses that all conventional glasses are obsolete. This textbook should be written in English.

BBV : You want to write a textbook of Glass Science, not of Materials Science in general ? Are there any Japanese textbooks of Materials Science ?

KH : Yes and we had written one.

BBV : One final question : Do you see differences in the research styles of various countries ?

KH : In Europe originality is important. Here it is rather collaboration and harmony. We are more modest, more humble. Collaborations, mutual help and mutual learning, Interdiscipinary philosophy is my project aim.

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Pour citer l'entretien :

« Entretien avec Kazuyuki Hirao », par Bernadette Bensaude-Vincent et Hervé Arribart, 29 aout 2002 Sciences : histoire orale, https://sho.spip.espci.fr/spip.php?article125.

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Entretien avec Kazuyuki Hirao, par Bernadette Bensaude-Vincent et Hervé Arribart, 29 aout 2002

Lieu : Department of Materials Chemistry, Kyoto University

Support : enregistrement non précisé

Transcription : Bernadette Bensaude-Vincent et Hervé Arribart

Edition en ligne : Sophie Jourdin

BOILOT Jean-Pierre, 2000-12-12

Sophie Jourdin — 2011-10-28T12:00:58Z

Jean-Pierre Boilot worked on b-alumina in the 1970s and subsequently on ionic conductors within the framework of chimie douce.

BERNADETTE BENSAUDE-VINCENT (BBV) : Quel fut votre parcours individuel ?

JPB : Je suis entré au laboratoire Collongues en 1971, étant assistant à l'Ecole de céramique de Sèvres où j'enseignais la chimie. Mon sujet de thèse portait sur l'alumine-b plus exactement sur les gallates. On cherchait à améliorer la conduction ionique en remplaçant l'aluminium par du gallium. On connaissait, bien sûr, les travaux de Yao et Kummer et on savait déjà échanger les ions sodium par d'autres. Mais ceci n'a constitué qu'un chapitre de ma thèse qui devait en avoir 5 ou 6.
Après j'ai eu un rôle très particulier : travailler à l'interface de la physique et de la chimie. Cette expérience de collaboration de la physique et de la chimie du solide, c'était une innovation. Seul Yves Le Car avait commencé avant moi. Lui avait un financement industriel, avec CGE qui est devenu Alcatel. Cette collaboration est issue de discussions entre Robert Collongues et André Guinier qui était responsable d'un groupe de physique du solide à Orsay au bâtiment 510. Le Car a commencé à faire de la diffusion des rayons X, organisation des ions de conduction dans alumine-b. J'ai poursuivi dans cette voie. La collaboration s'est étendue. Je passais 50% de mon temps au labo Collongues et 50% en physique chez Guinier et chez Jérôme, un autre groupe de physique du solide qui faisait de la RMN. Une grande partie de ma thèse concernait des problèmes fondamentaux : comment les ions s'organisent, ordre désordre, stœchiométrie.

BBV : Quels étaient les modèles théoriques à l'époque ?

JPB : Peu de choses pour comprendre les mécanismes de conduction. C'est venu plus tard. Les physiciens durs ont attaqué le problème plus tard.
J'ai soutenu ma thèse d'Etat en 1975 devant un jury très impressionnant : Jacques Friedel, Jean Rouxel, Michel Fayard, qui est devenu directeur du secteur chimie au CNRS, Jeanine Théry et Robert Collongues. Je me souviens avoir été mauvais, je n'étais pas fier de moi.

BBV : Avez-vous poursuivi sur alumine-b ?

JPB : Oui de 1975 à 82 j'ai travaillé avec Gaston Colin, cristallographe et avec Philippe Colomban qui est arrivé au labo Collongues. Je l'avais eu comme étudiant à l'école de céramique. On a travaillé essentiellement sur deux aspects : alumine-b stœchiométrique et alumine-b''. Même type de base : compréhension, organisation des ions en utilisant les paramètres fondamentaux du solide : répulsion entre ions, transition au désordre etc.

BBV : Y avait-il alors une communauté française de chercheurs sur l'alumine-b ?

JPB : Oui, il y avait des séminaires organisés ici à Polytechnique par Bernard Sapoval->http://pmc.polytechnique.fr/bs/english.html] et Hervé Arribart. Les gens ici ont commencé à travailler sur l'alumine-b avec des porteurs de protons et ils utilisaient la RMN.
Donc si l'on fait le bilan de ces 10 ans, il y a deux caractéristiques propres à ce sujet

- C'étaient les premières recherches fondamentales menées parallèlement à la recherche industrielle car CGE en France, Ford, General Electric aux USA faisaient des recherches plus appliquées sur les accumulateurs sodium-soufre. C'était particulièrement motivant de voir qu'il y avait des possibilités d'application.
- Deuxième caractéristique : c'était la possibilité de travaux à l'interface physique-chimie. Ces deux aspects là se retrouvent plus tard dans les recherches sur les supra-conducteurs au cours des années 90.

BBV : Aviez-vous des contacts avec l'industrie ?

JPB : On avait des contacts avec CGE et on allait parfois à Marcoussis voir M. Dumas de CGE. Mais on faisait de la recherche fondamentale.
Des contacts avec l'industrie, il y en avait sans doute au labo Collongues. Mais je n'étais pas au courant. Par contre, au laboratoire Collongues, Didier Goureyet était plus proche des préoccupations industrielles, tout en étant en recherche fondamentale.

BBV : Avez-vous ressenti un certain pessimisme industriel sur l'alumine-b au cours de ces années ?

JPB : Non, il y eut une effervescence de 1970 à 76. Le pessimisme est venu après. Il y avait peut être des problèmes pour les gens qui ne travaillaient pas sur le sujet. C'est faux de dire qu'il y avait un pessimisme dans les années 70. Pour les années 80, c'est une autre histoire. Plus de problème d'énergie, d'autres problématiques sont arrivées : utiliser des systèmes. On savait que les batteries sodium-soufre ne seraient pas commerciales. Elles ne le seront peut-être jamais. Donc du point de vue industriel, c'était un tout petit peu moins motivant.

BBV : Avez-vous participé aux congrès internationaux des années 70-80 ?

JPB : Bien sûr je pourrai vous donner la liste. C'est un autre aspect important : il y avait une compétition internationale, essentiellement avec les Américains, avec les gens de General Electric - Roth - et les gens de Bell Telephon. J'ai commencé à participer en 1976 Schenectady ; 1979 Lake Geneva (USA), Gatlinburg (Tennessee) en 1981, Grenoble en 1983, Lake Tahoe en 1985 ; Garmisch en 1987. Outre cette série des Solid State Ionics il y avait Rome (1976) et Saint-Andrews en Ecosse, en 1978. A chaque fois on avait des papiers dans ces conférences.

BBV : Y-a-t-il eu une évolution ou réorientation de vos recherches sur cette période ?

JPB : On a pousuivi les mêmes pistes de recherche sur les deux alumines-b.
Philippe Colomban, chimiste, s'est consacré à l'élaboration des mono-cristaux d'alumine-b. Seuls deux groupes au niveau international savaient faire la synthèse des alumines-b : Colomban au laboratoire Collongues et Farrington chez General Electric. C'était un procédé à haute température avec quelques subtilités chimiques pour parvenir à faire l'alumine stoechiométrique. Mais il n'y eut pas de brevets sur les mono-cristaux. L'objectif était purement fondamental car les applications se faisaient sur un milieu polycristallin, céramique.
Parallèlement à partir de 1978, on a commencé à travailler sur d'autres conducteurs ioniques qui pouvaient remplacer l'alumine. Ils faisaient partie d'une série qu'on appelait nasicons : c'étaient des phosphates ou des phospho-silicates avec des ions sodium.
Le choix du sodium repose sur des arguments très simples : il faut un ion monovalent, de la bonne taille. S'il est trop gros il ne diffuse pas facilement ; s'il est trop petit (cas du proton ou du lithium) il vient se coller sur le réseau ; ou on a une interaction trop forte avec les anions (les chimistes disent trop polarisants). Les meilleurs ions sont Na+ et Ag+. Ensuite le choix dépend des applications. A cette époque là le problème était le stockage d'énergie, on visait des accumulateurs de haute puissance pour faire du stockage. Les critères de densité d'énergie massique portaient le choix sur les éléments légers, donc le sodium plutôt que l'argent.

BBV : Est-ce que la crise d'énergie a infléchi les recherches au labo Collongues ?

JPB : Peut-être mais à cette époque j'étais trop concentré sur ma thèse et je n'avais pas de vue d'ensemble. Pour revenir aux applications, les nasicons ont eu moins d'intérêt car ils sont moins stables, ils résistent moins bien au sodium liquide. Ils n'ont pas eu le succès de l'alumine-b mais des gens travaillent encore dessus. Il y a eu beaucoup de travail sur cette famille : diversité de compositions et de phases. Elle présente un intérêt pour la compréhension des paramètres fondamentaux du solide mais moins que l'alumine-b.

BBV : Rétrospectivement considérez vous que ce travail sur les nasicons a été positif ?

JPB : Oui on aurait peut-être pu arrêter un peu plus tôt. On a travaillé là dessus de 1978 à 1984 mais toujours en parallèle avec l'alumine-b. C'est un travail qui se faisait à Polytechnique où je suis venu en 1981. C'est un sujet qu'on a développé ici avec Colomban, toujours en liaison avec les physiciens du solide (Collin) d'Orsay dans le groupe de Robert Gomès qui avait pris la succession de Guinier.
Après on a pris un virage vers les sols-gels. La transition s'est faite par le biais des nasicons. On avait dans l'idée d'élaborer des phases amorphes pour conducteurs ioniques. Elles étaient dérivées du nasicon. On a préparé les premiers verres organo-minéraux en s'inspirant des conducteurs ioniques type nasicons. Notre modèle à nous était le conducteur ionique. Puis on a eu des résultats intéressants sur ces matériaux, sans rapport avec la conduction ionique. Ces hybrides organo-minéraux, à la frontière entre organique et minéral sont faits à température ambiante avec une chimie douce.

BBV : N'est-ce pas un paradoxe que de la chimie à haute température du labo Collongues sorti une chimie à température ambiante ?

JPB : Oui à la même époque Jacques Livage faisait des gels V205.

BBV : Qu'est-ce qui a motivé votre virage vers les verres ?

JPB : Du point de vue industriel, l'alumine-b c'était moins motivant et, du point de vue fondamental, on avait fait le tour. De plus, je démarrais un groupe ici à Polytechnique, c'était le moment de passer à un nouveau projet.

BBV : Est-ce que ce virage vers les verres organo-minéraux a changé votre place dans la recherche ?

JPB : Au niveau du CNRS, non, car on appartient toujours à la famille chimie du solide. Mais on a eu des contacts industriels nouveaux avec Saint-Gobain (Silor). Bien sûr pendant deux ans, on a eu un peu de ralentissement dans la production de publications. Mais le virage se fait bien.

BBV : Quelles sont les activités de votre laboratoire actuellement ?

JPB : Actuellement on est toujours sur la chimie douce. En plus des hybrides organo-minéraux, on travaille sur des objets nanométriques. On part de molécules et on essaie de construire des solides à partir de ces molécules. Ce sont essentiellement des matériaux pour l'optique : lasers ou stockage de l'information optique.

BBV : Quelles sont les techniques que vous utilisez ? Sont-elles totalement différentes de celles qu'on utilisait au laboratoire de Collongues ?

JPB : C'est de la chimie classique avec des béchers mais pas de haute température. C'est bien différent des labos d'alumine où on avait des fours à 2000°C. Le labo Collongues était surtout tourné vers l'élaboration de matériaux alors que maintenant on fait surtout de la caractérisation. Comme maintenant on dispose de nombreuses techniques, on peut faire des thèses sur la caractérisation avec peu de chimie.
Ce que m'a appris l'alumine-b c'est qu'il faut faire de la chimie. C'est le matériau qui est intéressant. C'est le message le plus important. Toutes les avancées qu'on a eues au laboratoire Collongues, c'est parce qu'on a su faire de la synthèse de matériaux avant et mieux que les autres. Notre premier travail est de faire de l'innovation en matériaux, mais on a beaucoup de collaboration en physique.
Notre troisième thème est la pile à combustible. Il est arrivé avec un ancien du laboratoire de Collongues : Philippe Barboux. Il travaillait sur les films minces de céramique et prépare maintenant des membranes conductrices ioniques pour les piles à combustibles. C'est donc un retour à la tradition d'origine.
Mais il y a un lien entre les verres, les particules nanométriques et les piles à combustibles. Ce sont toujours des procédés à basse-température. On travaille sur la diffusion de molécules comme autrefois on travaillait sur la diffusion des ions.

BBV : Combien de personnes travaillent dans votre groupe ?

JPG : Actuellement notre groupe de chimie du solide comprend 10 personnes et il est l'une des composantes de l'UMR-CNRS intitulée Laboratoire de Physique de la matière condensée qui comprend 50 personnes.

BBV : Quels sont vos liens avec l'étranger ?

JPB : Nous avons gardé des relations avec Bruce Dunn de UCLA (nous avons ici un chercheur permanent qui a fait son post-doc là bas). Nous avons également une collaboration avec un laboratoire allemand. Pas de programme européen, c'est trop de paperasses.

BBV : Comment voyez-vous la chimie du solide française sur la scène internationale ? Est-ce qu'elle n'a pas d'une certaine manière fait obstacle à l'essor d'une science des matériaux en France ?

JPB : C'était suite au démarrage de la physique du solide. Il y a avait a deux pôles de chimie du solide en France, celle de Hagenmuller à Bordeaux et celle de Collongues à Paris. L'une plus mandarinale que l'autre. Des gens comme Rouxel, je les mets dans la famille Hagenmuller. En fait, si on prend les labos actuels de chimie du solide, ce sont tous des descendants d'Hagenmuller ou des descendants de Collongues.
Les deux écoles sont tournées vers la science fondamentale plus que vers les applications. C'est totalement différent de l'approche science des matériaux aux USA. Elle n'existe pas en France. L'approche Materials Science est plus tournée vers les applications. En France, il y a eu beaucoup de recherche fondamentale. L'originalité française n'est pas dans la collaboration avec l'industrie mais dans l'approche physique, dans la collaboration entre chimistes et physiciens du solide. Je défends l'approche française. Si les gens avaient été très proches du milieu industriel, je ne crois pas qu'on aurait été aussi forts en chimie du solide.

BBV : Peut-on associer une coloration politique à cette discipline ?

JPB : Traditionnellement en France, les physiciens sont plutôt à gauche et les chimistes plutôt à droite. Quant à la couleur de ces deux écoles de chimie du solide, je dirais que Hagenenmuller était un gaulliste bon teint ; il serait plutôt proche de Pasqua aujourd'hui ; Collongues, lui, était plutôt centre droite, bon vivant.

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« Entretien avec Jean-Pierre Boilot », par Bernadette Bensaude-Vincent, 12 décembre 2000 Sciences : histoire orale, https://sho.spip.espci.fr/spip.php?article121.

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Entretien avec Jean-Pierre Boilot, par Bernadette Bensaude-Vincent, 12 décembre 2000

Lieu : Ecole polytechnique, Palaiseau, France

Support : non communiqué

Transcription : Bernadette Bensaude-Vincent

Edition en ligne : Sophie Jourdin

ARRIBART Hervé, 2001-02-19, 05-29, 02-20

Sophie Jourdin — 2011-06-16T07:31:17Z

Hervé Arribart is the Scientific Director of Saint-Gobain Recherche, an international company of French origin with an emphasis on glass manufacture. He took his PhD from the Ecole Polytechnique in Paris in the mid-1970s and subsequently researched ionic transport using nuclear magnetic resonance. In the late 1970s he worked with Jean Rouxel's group at the University of Nantes. In 1981 he joined the company Elf to work in research and development. In 1985 he moved to Saint-Gobain, where at first a large portion of his research was closely related to the practical problems of production. In 1990 he started a laboratory (a joint venture of Saint-Gobain and the CNRS) on the basic science of glass surfaces, using a diverse set of tools and especially the Atomic Force Microscope. In 1999 he moved to the more managerial position of Scientific Director. Hervé is also on the staff of this project.

2001-02-19 :

HERVE ARRIBART (HA) : I studied at the École Polytechnique in Paris. The selection to the school is done mainly on mathematics. But during my studies I learnt to appreciate physics in particular. I decided to pursue research in solid-state physics. It was a good place to study physics. While in my last year as an undergraduate I did a Diplome d'Étude Approfondie in parallel (an intermediary between an M.Sc. and a PhD typically done for a year before starting one's PhD studies). In Orsay, near the École Polytechnique, there is a very famous place in solid state physics, a lab started by Jacques Friedel - a great name in solid-state physics. I followed this course and afterwards I did the PhD at the École Polytechnique in the field of condensed matter physics. In principle I ought to have started with a topic distant from materials science. I extracted spin-polarized electrons from semiconductors. This was in 1974.

ARNE HESSENBRUCH (AH) : How did one extract spin-polarized electrons in 1974 ?

HA : It is true of all solids, but in semiconductors it is especially interesting that when light falls upon a surface there is a coupling between the spin of photons (in classical physics : the polarization of light) and the spin of electrons. Electrons in the upper layer absorb light photons depending upon the spin. If by some technique you can extract electrons from the conduction band of the semiconductor, you can find ways to select electrons of specific spins. This was quite important at the time because at big-science institutions such as LEP [Large Electron Positron collider] or SLAC [Stanford Linear Accelerator Center], there was a need for spin-polarized electrons. And of course you then needed solid-state physics to do it. But the man who in principle was my supervisor decided to do something else. His name is Claude Weisbuch, and he is now a good friend of mine. For a few years he was the scientific director of the French Department of Defense. He is still working in solid-state physics, in the optics of semiconductors. But he decided to do something else and Bernard Sapoval, another professor at the lab, proposed that I work on new materials. At that time there was little contact between solid-state physics and solid-state chemistry. The idea was to link up with chemists. This is why very early on in my career I had contact with chemists. We worked with Parisian solid state chemists on a new material. We found a new way to draw single crystals of an already existing material. It was very nice because we could examine transport and NMR phenomena. And the material, a copper vanadium sulfide exhibited astonishing properties : a large spread of conductivity that one can measure in a standard experiment. We suspected that this was due to mixed conduction properties. Mixed conductivity refers to conductivity by both electrons and ions. The experiment appeared to verify our a priori suspicion. This gave me the possibility to present a model for mixed conduction in this material and to understand the influence of ion transport and electron transport. I also used NMR in order to understand which ions moved. It turned out that the copper ions moved. So, this was the subject of my first thesis. At the time, in France, there were two theses. The first one was called "thèse de troisième cycle". The second was the "Docteur es sciences". This degree does not exist any longer. The thesis that is done now is shorter.

I decided to continue to work with chemists. I decided to combine NMR and transport measurements. I changed my collaborators, turning to two different groups. In my PhD there had been two chapters on NMR. But I wanted to study proton transport. I had two reasons. One was that protons give a strong NMR signal. The second reason was that two reasons had been given for proton transport. In one, protons move in individual jumps. In the other the proton is a part of a more complex molecule such as the ammonium ion (NH4+) or hydroxonium (H30+). In the former case we can see the transport phenomenon as a result of molecule rotation and proton jump. The molecule would turn and the proton jumps to the neighboring molecule, which again turns and so on. This was called the rotation-jump model. The second model was for the whole complex ion to jump. This was called the vehicle model because the whole molecule acts as a vehicle. So I worked with one group of chemists in Nantes, at the Institut de Matériaux de l'Université de Nantes. It had just been created by Jean Rouxel, a chemist. With them I worked on a substance called antimony acid - a solid. I was able to show using NMR that transport occurred in this case with rotation-jump. Protons used H30+ as a complex rotator. I was also able to show that the jump was due to quantum mechanics within a certain temperature range. It was not the usual ion transport of classical mechanics.

AH : A tunneling effect ?

HA : Yes, this is one aspect of protons, because protons are very light ions allowing for this quantum effect. The other material I studied was ammonium beta alumina. This was the standard beta aluminium in which the sodium had been ion exchanged with ammonium. This material was very interesting from the perspective of NMR. All kinds of ionic motion took place at different temperatures. At the lowest temperatures, that of liquid helium (1-4K), there was rotational quantum motion. As the temperature increases the motion becomes classical.

AH : If I may make a comparison with Stanley Whittingham here. You were working on some of the same materials, you were using some of the same tools (NMR), but you were asking very different questions, right ?

HA : Yes, that is true. I was not at all involved in the application. For two reasons : French chemists were interested in materials and did not look to the application. And chemists were between me and the application, so I had no contact with attitudes such as Whittingham's. I was very happy working on the solid-state physics problems.

AH : And we are talking about the late 1970s now ?

HA : Yes, I began the proton transport research, I think, in 1976.

AH : And it went on for how long ?

HA : For five or six years.

AH : And you lived in Nantes ?

HA : No, I remained in Paris while collaborating with the Nantes group.

AH : Were you employed in Nantes ?

HA : No, not at all. At the beginning I was employed at the Ecole Polytechnique as a research assistant, and then I was hired by the CNRS - in 1977.

AH : So, the CNRS paid your salary, you were able to do basically whatever you wanted, and you collaborated with Jean Rouxel and coworkers because you found it interesting ?

HA : Yes. It was a chance to work with an outstanding chemist. French chemists were really very good. The problem, as we just said, was that there was little interest in application.

AH : What did you do next ?

HA : After my PhD thesis, I found it interesting to go to industry.

AH : I imagine that there were many advantages and disadvantages to leaving academia for industry. For instance, where was status greater, what paid better, where were working conditions better ?

HA : First of all, it was rare, even more so than today, for CNRS people, or people within the public system, to go to industry. I cannot give you a clear answer about my motivation - it was not even clear to myself at the time. I did get a higher salary in industry. I also had personal reasons for leaving Paris and going to the Elf company. I went to an Elf research lab in the Southwest of France, in a very nice place in the Pyrénées. I had small children at the time and it was much better for them to grow up in the countryside and in a very nice climate. I was also curious. So the decision involved many elements. And anyway, it was not irreversible. The CNRS allowed me to take a three-year leave after which I could have gone back. With regard to the working conditions : I was of course less free than I had been at the CNRS, but I found it more stimulating because there were a lot of different problems on the horizon, arriving almost every day. We could easily get the necessary equipment at the CNRS and at Elf, so there were no differences there.

AH : The restrictions at Elf had to do with what you were allowed to study ?

HA : Yes.

AH : What did Elf want you to do ?

HA : In principle I was hired to work on solid-state sensors. Because it was not in the direct line of my previous work I proposed that I work on solid-state sensors and ion conduction. We developed a family of sensors named ISFETs (Ion Sensitive Field Effect Transistors). It was a new kind of transistor at the time but now it is very common. You control the electrode using field effects, opening and closing the circuit between the two other electrodes. This is the way the transistor works. My idea - not an original one - was to replace this way of controlling the electrode, the gate, to replace it with a membrane, selective to such and such an ion. If you put the device in a solution containing the ion for which you have designed the system, the membrane will be charged. This charge will change the state of the solid-state transistor. It worked all right for protons. We could use the device to measure pH and afterwards we just had to change the nature of the membrane, choosing a different solid electrolyte, such as calcium fluoride.

AH : Your toolkit remained the same and you still used NMR ?

HA : Not NMR, but yes. You need large samples in order to do NMR. So it was mainly electrochemistry and surface analysis. This was between 1982 and 1985. But as I told you, in industry new projects can arrive almost every day. I had developed some skills in electronics using instrumentation at the École Polytechnique. Elf applied for a patent for a medical analysis system, a small instrument to be sold to private practitioners, as opposed to hospitals. This had nothing to do with solid-state ionics. But the people working on this project needed someone who knew about electronics, and so I got progressively more involved. After one or two years it had become my main project. This worked very well. I was very proud to design an electronic system that required no manual setting. It was set in the factory forever. This was a critical issue, because we thought that doctors could not be expected to deal with electronics - and I am sure that we were right in this. So there was nothing to check or calibrate - the system was self-calibrating. So it worked very well, and after only two or three years Elf built a plant and people were hired. But in 1984 and 1985 there were big changes in chemistry. And there was a great redistribution of all chemical industries. And Elf, that had been an oil company, in this period expanded to become also a chemical company. As a result a lot of the more diversified lines of business lost in importance. Many projects like ours were discontinued. But because we were already quite advanced we found a way to keep going. In fact it was Dupont de Nemours that found that our system was complimentary to some of theirs. The result was that Elf shipped the patent and everything else to Dupont. For a few months I considered following the project to Dupont and to the United States. In the end I decided against. I still wanted to work in solid-state physics and not to work completely in the instrument making business. But for one or two years I continued as a consultant.

2000-05-29 :

HA : For both personal and professional reasons, I decided to stay in Paris, and then Saint-Gobain offered me a position, working in a new research field : polymer adhesion on glass and other materials. It was a new topic for me too. At the time adhesion was not even considered a science. It was before Pierre-Gilles de Gennes's Nobel Prize in polymer adhesion [1991]. It was rather considered an art. Even though I had no background in the field I was interested. What interested me in the Saint-Gobain proposal was that real breakthroughs were to be expected in the science of adhesion when two materials are brought into contact. In fact this was my first real industrial experience. Of course CNRS had not been an industrial experience at all, and even at Elf I was always in the research lab. As I explained, my work at Elf had nothing to do with the industrial activities. I never visited factories. At Saint-Gobain I had to do this, at least in the beginning.

AH : Did you not say that your development of the medical analysis system resulted in the setting up of a plant ?

HA : Yes. I did participate in the design of the plan, in order to make it efficient. But I had no role in the plant itself after construction. It was also a small plant for high-tech activity.

AH : You had nothing to do with the fabrication side of it, situated in the plant – merely the R&D before the plant became functional ?

HA : Yes, exactly. Saint-Gobain of course has many plants all over France and Europe, and even the United States. But at that time, the company was still franco-français [French through and through] in its general spirit and culture, despite the many factories in other countries. There were only French directors and the system was based on the French system of education. There is a hierarchy from the École Polytechnique through the École des Mines and the École Centrale to lesser schools, and you carry the status of your school within you for the rest of your life. I remember that I strongly felt the weight of tradition when I first joined the company. It is true that winds of change were already blowing then, but they were barely noticeable and needed a couple of years before really expressing themselves. But eventually the company changed its culture, and now the company considers itself an international one. I think a deep change has taken place during my 15 years with the company.

So, anyway, this was the first time I gained experience of the industrial aspect of research. My first task was to examine and synthesize different kinds of adhesion in Saint-Gobain's products and processes. I decided to simultaneously pursue fundamental reflection and a practical approach, helping the factories improve their processes. This was a very instructive experience. I learnt many things although I am not sure that I helped the factories all that much. I certainly learnt for myself that I preferred to stay within R&D and not to progress into production. On the fundamental side, I developed a network of contacts in public labs in France and the US. This became useful later on. After three years in the field, and having created a small research lab, I decided to gain some distance from the practical aspect of my work. It was also obvious to me that fundamental research was required first. Progressively the idea came to me to propose the creation a special laboratory dedicated to the basic aspects of polymer adhesion - and of course also to related issues such as the surface science of glass. But I knew that Saint-Gobain was not ready to have a laboratory for basic science by itself, so my idea was to set up a lab jointly with the CNRS. This was in 1988. From the administrative point of view this was feasible : a number of such joint ventures already existed, an example of which is Rhône-Poulenc. Of course I had to convince both Saint-Gobain and the CNRS of the utility of the project which was not straightforward. Although I managed to convince Saint-Gobain in a manner of hours, CNRS needed more prompting.

AH : Would you explain the nature of Saint-Gobain's research before your proposed laboratory ?

HA : It was a quite common kind of R&D geared towards problem solving. Helping the development of new products and solving problems within production.

AH : So the research agenda was driven by questions arising out of production ?

HA : Yes, and my idea was to get a more fundamental understanding of the questions which would enable us to help with such questions in a much better way.

Figure 1. Saint-Gobain Recherche, Paris

At Saint-Gobain I had to sell the idea primarily to the Vice-President of R&D. He took the decision just before retiring. The CNRS process was more complex. It has a democratic organization where decisions are taken by committees. The members consist of both elected researchers and individuals named by the Ministry of Research. They are divided up into different scientific sections. So here I had to convince a diverse group of people, and not just one person, as at Saint-Gobain. As I mentioned, I had developed a network of relationships in the fields of adhesion and surface science and now this turned out to be useful. I knew that many people approved of my research agenda. My project was accepted without much fanfare, but it still took a while because of the administrational hoops that a proposal has to jump through within the CNRS. They meet only twice a year, and every decision has to be validated by the CNRS directors and so on. It took maybe 12 months. The laboratory started on January 1, 1990. But there was only a building and neither instruments nor people.

Figure 2. Joint lab : Saint-Gobain Recherche & CNRS

The three yellow arrows point to the units of the joint lab within the Saint-Gobain Recherche building.

In the meantime I conferred with scientists in many other labs trying to recruit people. Of course the CNRS could not order people to go, so I had to entice scientists away. I estimated that I needed three scientists from the CNRS in addition to three scientists from Saint-Gobain. Two of the latter had already worked with me, and they followed me to the new project. A further researcher came from somewhere else – it was a young Chinese woman. We also had two or three technicians and some PhD students. Altogether, it took a year or so to gather everyone together. We also had to buy instruments and the process of getting the laboratory shipshape lasted altogether something like 2 years. We began to actually do some research in late 1990. And from then on the activities progressed rapidly. In two to three years we reached a plateau of 20 people, a level that had been stipulated by the CNRS. A third of the people had come from the CNRS, a third from Saint-Gobain, with PhD students constituting the last third.

AH : Where did they come from ?

HA : The latter were doing industrial PhDs (Contrat à Durée Déterminée) with Saint-Gobain, and their salary came jointly from the French Ministry of Research and from Saint-Gobain. Of the entire staff, about half each came from chemistry and physics. It was crucial that we develop knowledge and expertise in both these fields. Later we also developed an interest in mechanical problems.

Figure 3. The SPM from Park Scientif Instrument

AH : What was the instrumentation ?

HA : There was a conjunction of the beginning of our lab with the very early days of scanning probe microscopy. This new kind of instrumentation offered a very exciting opportunity. There was a risk in this. We purchased the first Atomic Force Microscope (AFM) ever in France. We bought it from Park Scientific Instruments. Later we built the first AFM for UHV purposes. There were many people then who thought the instrument had no future, so it was a risk to invest time and money in it.

AH : Why did people think it had no future ?

HA : The objection was that it was not clear that atomic resolution could actually be achieved with the AFM. It was not until 1993 that Binnig showed true atomic resolution.

AH : Well, yes, but before he had claimed to achieve atomic resolution. In 1993 he only claimed that so far he had been mistaken and only in 1993 did he achieve true resolution. Is that not right ?

HA : Yes. But in 1993 the community was convinced. The reason I did not hesitate was that atomic resolution was not actually the big issue for our purposes. Even a resolution of 1 nanometer amounted to a great deal. Much could be done with such a resolution in the field of adhesion, and also in fracture mechanics and surface chemistry.

AH : I have the impression that since 1995 or so many people argue that atomic resolution is not really that important, and that in the early 1990s it was still considered the holy grail. So you were unusual in that you had this attitude so early ?

HA : You are right that atomic resolution had a special ring to it in those days.

AH : Did you emphasize the issue of atomic resolution in your application to the CNRS ?

HA : I am not sure. Even today, nobody has achieved atomic resolution in glass. So it would have been a hard sell, also then. The same goes for polymers. And those two were our substances under investigation.
There is a difference between STM and AFM. They obey two different logics. The STM has remained a tool of basic research, in surface science. The AFM, even early on (and this would be interesting to discuss with Calvin Quate or Gerd Binnig), there was a hope that it could be useful, for example in other fields of science, such as mine, or in technology, such as process control, microelectronics, semiconductors, and so on. Generally speaking, in early phases there are always many people who think that a novelty will never become common. We have to remember that in 1987 or 1988 solid probe microscopes were still big and unwieldy instruments. Of course miniaturization had set in by 1990, but it was a novelty. Only very few people were convinced that the AFM would become so common. Calvin Quate is one of the few. The STM has revolutionized basic research on metals and semiconductors. There was a reaction against it, because surface science was done using diffraction techniques working in reciprocal space. Surface scientists were formed in this mode of research. They resisted the change, feeling that newcomers would enter their field without the kind of abstraction that had hitherto been key to access to the field. Working in ordinary space was too easy ! Of course it has not actually become easy because the instrument has brought its own problems, and there are still people working with diffraction and in reciprocal space. The two complement each other.

AH : So this is the background against which your decision has to be seen. You went out on a limb.

HA : Yes. The beginning of my lab coincided with the first commercial scanning probe microscopes (SPMs). We had to grasp the opportunity.

AH : How did you know about the AFM ? Was it a very visible instrument at the time ?

HA : No. I knew about it from publications, but in order to actually see an instrument, I had to travel to California - although I guess I could have seen one at IBM Zurich. There was an STM at Marseille, because two physicists there (Salvan and Humbert) had worked at IBM Zurich, and they had brought one back with them. But they had no experience with the AFM. So I went to the US and visited the very few labs with AFM, both academic labs and the start-up companies of PSI [Park Scientific Instruments] and DI [Digital Instruments]. At Stanford University I met Calvin Quate and at UC Santa Barbara I met Paul Hansma.

AH : Was there a relationship between Paul Hansma and DI ?

HA : I don't remember. But at any rate it was not as close as the one between Quate and Park. I think Park was a former student of Quate's.

AH : So you purchased an AFM from Park. What about the other kinds of instrumentation you purchased for your lab ?

HA : Yes, we had to get other instruments, partly because it took a long time for the AFM to arrive. I had to go to the US to compare the DI and the Park instruments, and I discussed it with the physicists and chemists in our lab before ordering, and then we had to wait for the delivery – maybe 4 months or so. We got a 40% discount, because we were the first French customers, and they hoped that we would open the French market for them. I had very good discussions with Quate, and I think he trusted me to be a good advertisement for him in France. I think we paid 400,000 French Francs, so that the catalogue price was in the order of 800,000 French Francs [approximately US$100,000].

We bought also an infra-red spectrometer, in order to study molecular grafting on oxides. This we used as a complement to the AFM. And as I said in a previous part of the interview, our approach was to combine the traditional surface science (very clean surfaces) with “true surfaces” interacting with the environment. The infra-red spectrometer, XPS (X-ray Photoelectron Spectroscopy), and LEED (Low-Energy Electron Diffraction) were good tools for the traditional surface science approach working in UHV Ultra-High Vacuum). And also HR-EELS (High-Resolution Electron Energy Loss Spectroscopy). Our choice was risky, but it turned out to be correct. Our decision to build bridges between the two approaches was taken in 1992 or 1993. Quite early on in our project we built a surface force apparatus (SFA). It is not at all an AFM – there is no concept of high resolution, but it is similar in that you can get a direct measurement of the force interacting between two objects only a few Ångstroms apart. The idea is to make the measurement quantitative in order to study whether the interaction is due to van der Waals or electrostatic forces. In fact this project took six years – not for technical reasons but simply because we had to get the right people.

AH : Each instrument had its strengths and weaknesses in terms of resolution and the scale of the surface analyzed. And each instrument required special skills. The AFM, for example, requires quite some expertise to disentangle signal from instrumental artifacts, right ?

HA : Yes, artefacts were a real concern at the beginning, when we all had very limited experience. We had to pay much attention in order to ascertain the results.

AH : Can you explain how one separates signal from artefact ?

HA : There are different kinds of artefact. One that now seems quite natural but was hard to understand then is the tip effect. If the surface under examination has sharper topographic features than the tip, then the tip will be imaged rather than the surface. We had trouble with this kind of artefact. In fact, when studying tin oxide deposits on some substrate we got very nice images that we at first interpreted as small crystals having the similar orientation. We were very excited to find a growth mechanism of specific orientations on isotropic surfaces such as glass. I decided to present this result at a small meeting in Davos, Switzerland. The topic there was in fact “The AFM for Technological Applications”. Famous scientists attended, including Calvin Quate, Jim Gimzewski, and Heinrich Rohrer. There were only some 10 people there, because this was very early, maybe 1991. The night before my presentation, I began to wonder that the result was really too beautiful to be true. I telephoned my lab and asked people there to turn the sample by some angle and do the experiment again. That way, the features should have changed if they belonged to the surface. But they did not, and so we knew that the features belonged to the tip. So I did not present that particular slide in my talk.

AH : So rotating the sample by some degree is one way of identifying artefacts.

HA : Yes, that will eliminate this kind of artefact, the tip effect. There are also adhesion artefacts, some of which have been solved in the meantime thanks to new recording techniques such as the tapping mode.

AH : Digital Instruments has a patent for the tapping mode, right ?

HA : Yes.

AH : So the Park instrument that you bought did not have the tapping mode ?

HA : No it did not. The tapping mode did not become available until 1993 or so. Later on, Park Scientific Instruments did do something similar, but they may not call it tapping mode. The DI patent covers the name. And in the straightforward contact mode many artefacts were possible ; for example when looking at soft materials and polymers surface scratches easily occur. If you do that you image the substrate only. One way to identify this effect is to scan again with a smaller tip-surface interaction. In some cases you will find miniature small squares where the surface had been damaged in the course of the first scan. Some artefacts are very common, others are quite specific and harder to identify.

AH : In what you have explained, the identification of artefacts is internal to the instrument itself. It is not that you can go and compare the results of an AFM scan with those from a different instrument ?

HA : You can change the tip, and you should identify artefacts unless you are very unlucky to get the same tip. Everybody understood that the AFM has great potential not just as an imaging instrument but also to measure adhesion, hardness and so on.

AH : Using force-distance curves ?

HA : Yes, force-distance curves. This turned out to be very useful for us. For instance in order to understand the electrostatic interaction between oxide and a silicon nitride tip under water. This was original work. For example, in polymer adhesion we checked if it stayed on the substrate and what scratching would do. Of course such ideas were floating around at the time.

AH : Were you important to the subsequent spread of the AFM in France ?

HA : Yes, people came to our lab. Another lab, at the Institut Curie, that got an AFM at almost the same time. For a while we were a small community but then gradually we grew larger and larger. Yes, we were the pioneers. It was exciting.

2001-02-20 :

HA : I went with one of my sons who was 11 years old at the time to see Park Scientific Instruments. There were no more than 10 people working there, in fact I think it was more like three. It was very small and familial. We discussed and had tea. I enjoyed discussing with these people. It was nothing like an established company.

AH : What did it look like ? Did they work out of a garage ?

HA : Something like between a home and a garage. It was a small house. Even Digital Instruments started out like this. Already in those days DI, and especially Virgil Elings, was much more commercially aggressive, but they were very small too at the time.

AH : Did you stay in touch with some of these guys ?

HA : I stayed in touch with Calvin Quate for five or six years, until 1996. After that I lost the contact but he will probably remember me because we had many discussions. It was curious to see his impact upon materials science. In fact it was very difficult for him to get the first paper on the AFM accepted in Physical Review Letters. Some of it was considered just a pure mechanical profilometer. It had good resolution but it was not really anything new. His project now is very interesting from what I can tell reading his articles in the scientific journals. And he really is a very nice person. Maybe the last time I saw him is when I invited him to give a talk at Saint-Gobain Recherche.

AH : So you stayed in touch with him in the early 1990s, while you were developing your own AFM. I guess the use of the AFM changed the project from what you had originally envisaged ? Did you continue using all the other tools or did you focus exclusively on the AFM ?

HA : We used the other tools.

AH : What did you buy for your laboratory ?

HA : Infrared spectrometer, XPS, HR-EELS (High Resolution Electron Energy Loss Spectrometer), LEED. Quite quickly we had three AFMs. I wanted to develop a PSTM working in the infrared but unfortunately that particular project died because the physicist we had working on it left.

AH : What journals show the history of these instruments best ?

HA : In the beginning it was mainly in the general physics journals such as Applied Physics, Applied Physics Letters, Physical Review Letters, Surface Science. Now there are specialized journals. A journal like Journal of Scientific Instruments is not so important in this respect. Langmuir is also important for soft matter.

AH : Do any of these journals have review articles ?

HA : I am almost sure that all of them do.

AH : We were talking about the various instruments you had in your lab. How did you apply them to your research project ?

HA : The idea was to have two parallel approaches. We were mainly interested in adhesion, molecular grafting and so on. One approach is the classical view of surface science, the ideal surface approach. The other is the REAL surface approach, taking the environment as a part of the system.

AH : Not working in Ultra-High Vacuum (UHV) ?

HA : Yes. But we were trying to make the two approaches meet.

AH : So when you started working with the AFM in UHV, the point was to simplify the experiment ?

HA : Yes.

Figure 4. UHV Chamber et AFM in UHV Chamber

If a probe were to be introduced directly into the UHV chamber, it would take days of pumping to achieve UHV. Instead, it is first introduced into an antechamber, whereupon a vacuum is produced there. Only then can walls be opened without reducing the UHV too much. By pushing the rods labelled 1 and 2, the sample is transported in successive stages into the central chamber. Several instruments are attached to the chamber, including an XPS. On the right, an AFM can be discerned in the UHV chamber.

AH : How did the various instruments complement each other ?

HA : The spectrometers provided structural information. They give a chemical signature. One point of interest was silver on magnesium oxide. In order to have a simple model of glass we chose to study this problem within pure single crystal. We had the probe in situ in the same UHV chamber where we had the instruments to add the deposition techniques. In the case of silver it was just thermal evaporation. We wanted in situ real-time studies of the atoms arriving upon the substrate, the oxide surface. There were two models in this problem. One was that the atoms remain isolated or form small islands, so that the growth process is two-dimensional, so that you first get a perfect monolayer before a second layer is started upon. The other is that growth is three-dimensional with occasional collapses into flatness. To study this it is of course useful both to look directly and to use diffraction techniques. But in order to understand the process you need to grasp the interaction between the silver and the oxide. And only spectroscopic techniques will help here. We always tried to look at a problem from two differing points of view – in this case geometrical and chemical.

AH : You make it sound easy. You just use one tool and you get the topography, and then you use another and you get the chemical composition.

HA : Well of course it is not at all easy. It was very difficult because for instance, the STM works very well when you have a smooth surface but when you have corrugation it becomes much more difficult, because this corrugation interferes with the instrument. In spectroscopy you integrate over the size of the beam which is much larger than the surface scanned by the AFM. So you have to do many different experiments to see what effect the temperature has and so on. You also have to model the interaction. This was a little known problem. What is the mechanism of very small silver clusters on magnesium oxide with other silver clusters in the neighborhood ? It was a new problem. So it took time to understand the system.

AH : What is the measure of success ? It was partly CNRS, so you were under pressure to publish ?

HA : Yes.

AH : And since it was partly Saint-Gobain you had to get patents ?

HA : We had to do both. It was an interesting exercise in communication. In my position as head of the lab, I could not use the same words, the same way of presenting things when addressing different audiences. From time to time it was necessary to gather the scientific and the industrial people together under one roof.

AH : And what language did you speak then ?

HA : Fortunately everyone was happy with this lab, so it was not quite so difficult. The conditions were good. Nonetheless your question is quite correct. It was interesting.

AH : How did you convince Saint-Gobain that this would have a pay-off ? And how did you negotiate long- and short-term goals ?

HA : The short term was a problem. It was not straightforward to plan a new product for the company. The pay-off was very diffuse and difficult to identify. One way of motivating the directors was the argument that we trained very good PhD researchers for Saint-Gobain. And this was not expensive for Saint-Gobain, because they shared all the expenses with CNRS. Up until now this has not been a problem.

AH : Stanley Whittingham told me that in the last 15 years or so there has been a tremendous shift in company planning towards the short term in industry. Partly this was due to the MBA education and the fanning out of this new generation of business administrators into all nooks and crannies of industry. As a result the long-term disappeared, because everything had to fit into the financial year so that you have something to show to your shareholders.

HA : It is true that this has taken hold in industry. We had the good fortune that it was not very developed in Saint-Gobain. But also, the time required for the development of new glass materials just is acknowledged to be greater than that in electronics or informatics. When we start new projects, we are simply not able to show a product six months later. So we are less exposed than people in other fields, but the general development that you alluded to certainly has taken place. Maybe our situation will also change in the future. We may be excessive.

AH : Has the accountancy changed for you ? Did you have to write annual reports ? And has it changed over the last ten years ?

HA : In general ?

AH : Well, for the CNRS I can sort of imagine it. In academia you would specify the number of publications that you have produced and that is the measure. End of story. And that is very simple accountancy. But if you account to a company, keeping in mind the increasing influence of MBAs : did you have to account for your expenses in ever greater detail ?

HA : I do not think there has been such a change in the last decade.

AH : And do you write annual reports ?

HA : Bi-annual. But I am not in this lab anymore ; I left two years ago.

AH : Okay, so during the 1990s up until two years ago you wrote biannual reports to the company and in that period the structure of the reports did not change.

HA : That is correct.

AH : Did you have to specify just how much money you spent ?

HA : Yes, but also there, no change took place. And I always reported to the same person within Saint-Gobain. He was basically content with what we did, so it was never critical. It is true, it might have changed with a different person in charge.

AH : So, how did the instrumentation change throughout the 1990s ? The AFM became commercially available to an ever greater extent, you were able to buy many more things off the shelf. Is that true also of all the other instruments ?

HA : Yes, there are different aspects to your question. We used to build many instruments ourselves, and this was of great use for training. And this has changed. A reason the French PhD has been shortened is that equipment is being bought and not made in-house. That is a general trend. Science is changing as a result, because using a commercial instrument is not the same. When you develop an instrument yourself you know exactly how to get the result. In the specific case of AFM/STM : probably the AFM has been developed much more than the STM. In the STM the major breakthrough was with the driver and that was quite early. I think it was possible to purchase an STM driver already by 1992. Variable temperature was a little more difficult, but it was certainly available by 1994. Different ways of scanning and acquiring information were developed. Otherwise the evolution was purely technical : cheaper, and more diverse (such as an STM expressly for electrochemical research). By contrast the AFM has developed rapidly. Tapping mode and other modes where you measure not only the distance but also hardness, conductivity, adhesion, chemistry. It has become possible to map all these parameters. This explains why more and more people use the AFM.

AH : It has also become cheaper, right ?

HA : Yes.

AH : It has certainly become more user-friendly, adaptable to different circumstances.

HA : Yes. For the STM : there have very beautiful studies made of the coupling between tunneling and modulation. You might modulate the tunneling current with light for instance. You can even leverage the spin of the tunneling electrons. So you can do beautiful physics. But this contributes little to the democratization of the technique.

AH : I have the sense that Calvin Quate, by contrast, is working hard to increase throughput.

HA : Yes, that is right. There can be two reasons for doing that. To make the investigated part of the surface larger – of use in the semiconductor industry. And to shorten the time required for a scan. He is trying to use the system technologically.

AH : Okay. Two years ago you left your lab. Your own lab. Why ?

HA : I wanted to try something new and I was lucky to find someone who was well capable of taking over and for whom I have a lot of respect. He is from a different background. So now it is a different group. I became the Scientific Director of Saint-Gobain Recherche. There are two parts to the job ; one is to be the scientific manager, the other is to establish contacts in the outside world, and to promote innovations within the company, for instance with the marketing people.

AH : You were promoted ?

HA : Yes.

AH : And you have become slightly removed from lab work ?

HA : Yes, completely, I am now involved in organizational work.

AH : In fact, our project resembles your job in the sense that we stand back and look at the scientific research and try to gain a perspective ?

HA : Yes, you could say that.

Fin de l'enregistrement

Pour citer l'entretien :

« Entretien avec Hervé Arribart », par Arne Hessenbruch, 19 février, 29 mai et 20 février 2001, Sciences : histoire orale, /spip.php ?article47.

Pour citer l'entretien :

« Entretien avec Hervé Arribart », par Arne Hessenbruch, 19 février, 29 mai et 20 février 2001, Sciences : histoire orale, https://sho.spip.espci.fr/spip.php?article47.

Lieu : dans le salon (les 19 février et 29 mai 2001) et dans la petite salle de réunion (le 20 février 2001) du Dibner Institute, Etats-Unis.

Support : enregistrement sur cassette.

Transcription : Arne Hessenbruch.

Édition en ligne : Sophie Jourdin, Sacha Loeve.