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Lab activities and organization

Introduction

The Laboratory of Catalysis and Spectrochemistry (LCS) is a research unit belonging to both ENSICAEN, the University of Caen – Normandy and the CNRS. It was founded in 1978 by the merging of the Laboratory of Catalysis (initiated by François Gault, who had just left Strasbourg) with the Spectrochemistry Laboratory. Jean-Claude Lavalley created from the very beginning the LCS as the French center for infrared spectroscopy in catalysis. In 1990, J. Saussey in the LCS began using IR in situ spectroscopy to study the surface of the catalyst inside the working reactor, an approach that later became known as name of spectroscopy operando .

NMR was added in 2000 to spectroscopic techniques in LCS, and the operando method was rapidly initiated in NMR.

Zeolites have always been an important topic for LCS, but we often relied on other groups to provide samples. In 2009, a major change was made to the scientific scope of the LCS when it was joined by a group specialized in the synthesis of zeolites. This change in the size and scope of LCS research has significantly changed our place and our role in the scientific community. LCS was quickly recognized as one of the leading centers of spectroscopy in catalysis and science of zeolites in France and in Europe.

We have become an important partner of the LABEX EMC3, a structure that organizes joint funding between the main scientific laboratories in Normandy. We have been members of the EPE Energy and Environment Research Federations with CORIA and LOMC in Rouen and Le Havre and with Toxemac, INSERM team) and LABOMAT (coordination of the activities of Materials Laboratories in the North West of France). Since mid-2016, we are also part of the Carnot ESP Institute (Energy and Propulsion System) which should expand our collaborations with companies.

Researchers

Technical staffs

PhD’s et postdocs

Scientific policy

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The main strength of the LCS is its scientific specificity. The LCS has developed a unique expertise and tool at European and international level. We are leaders in the spectroscopy of heterogeneous catalysts under controlled conditions or even in working conditions and at the same time in the controlled synthesis of zeolites. We have become a recognized partner to solve difficult questions of reaction mechanisms in heterogeneous catalysis, and we can provide the industry with new catalysts with optimized particle size at the nanoscale.

The LCS has always attracted world-class scientists who have joined the lab or have established collaborations with us. We organize several important conferences in our two areas of expertise and are invited by the international community to give lectures and write reviews in major journals.

One of the main scientific objectives of the LCS is the understanding and control of heterogeneous catalysis at the molecular level. One of the molecular limits of heterogeneous catalysis is the ability of the reactants to reach the active site and the products to be released into the external phase. This can be controlled with suitable spectroscopic tools optimized and / or controlled by the control of the morphology and shape of the catalyst, which requires a thorough understanding of the synthesis, in particular for the zeolites. In this way, the two areas of expertise, spectroscopy and the synthesis of zeolites are combined for a unique and efficient research. in situ and operando spectroscopy can be the ultimate tool to characterize and understand the diffusion and kinetics, nature and role of active sites (metals, electronic densities…), deactivation. The chemical engineering of the reactor with nanoparticles and transport modeling in our model reactors (operando cells) is a new cross-link between these different concerns of LCS.

The LCS approach to heterogeneous catalysis contributes to a sustainable future for our society in the fields of energy (renewable) (production and rational use), clean chemistry, depollution and environmental control. Our research plays a role at the interface between basic and applied science, with close links to the economy and technology.

In 2012, we changed our organization from a matrix of crossing projects and expertise, to a structure in three scientific themes. As part of the 2012-2016 project, the following three themes were discussed: Surface and Environment (Mr Daturi), Catalysis for Energy and Chemistry (Françoise Maugé) and Porous Materials, Advanced Synthesis and Applications (V. Valtchev). This has been very effective in integrating the synthesis of zeolites into our other older activities. Each theme invited professors, made important scientific contributions and obtained the corresponding recognition of the community.

For the new five-year contract 2017-2021, we want to balance our activities and promote scientific communication on a larger scale. To achieve this, it is important to increase the visibility and simplify the scientific organization of the laboratory. We now regroup our research into two scientific teams, organizing communication and coordination: the ZÉOLITHES team and the SPECTROCAT team . This change in organization will allow us to:

Maintain a long-term scientific direction
Encourage fast response to external calls
Facilitating the exploration of new emerging areas
Encourage interaction within the LCS; Create synergies among complementary areas of expertise.

The Scientific Committee of the LCS is a specific place for the discussion of our scientific policy at the level of the research unit. The annual PhD grants for the LCS within the Doctoral School, the policy of new permanent posts … A program to support new emerging projects (without independent funding) is organized by a joint contribution of all the projects financed .

Activity profile

Our research unit is strongly engaged in industry relations. Many of our research projects are in collaboration with industrial partners. The transition from in situ spectroscopy to operando spectroscopy stems from a recurring question from industrial partners: “we understand your description of the surface of the catalyst, But is it the same under the conditions of reaction? ” Still today we keep the same approach to understanding catalysis, and many of our fundamental questions arise from the concerns of industry or society, environmental and sustainable development issues.

We have set up a small organization ( LCS-Valoris ) within the laboratory for the delivery service for Industry: analyzes and measures for local industries, specific measures for industrial companies and first experiments under a large contract of collaboration. This is a very effective way to provide scientific services to the industry without too much time for permanent researchers, while preparing the ground for further collaborations. This partnership research will henceforth be carried out within the framework of the Carnot ESP Institute (Energy and Propulsion System) to which we belong.

Training through research is of course a big part of our commitment: the temporary staff, hired in the laboratory to conduct research with our permanent staff, is currently 18 graduate and undergraduate students, for 17 postdocs: half of our Temporary research staff is therefore student, and half of our time in research can be considered as training through research. Many of our researchers teach at the university or Ensicaen, but we also play an important part in the organization of education in both institutions.

We are also heavily involved in the life of the scientific community (Research Aid). We have members of the LCS in national, international and international scientific panels since 1990 (CNU, CoNRS, FWO in Belgium, chairman of the EU panel …), several members of the LCS have been Zeolites (GFZ), we preside over IZA, the International Association of Zeolites (V.Valtchev) and are members of a commission within the IZA. LCS participates in the Division of Catalysis (DIVCAT) of the French Chimical Society (LCS is also in the DIVCAT, permanent member of the GeCat committee).

Organization and life of the unit

A healthy research unit, both in human and financial resources.

The support of our tutorship institutions is very strong. We have received constant support from CNRS, the University and ENSICAEN for research, teaching and technical support. The age pyramid of researchers and academics on permanent posts in the LCS is therefore fairly balanced. At the time of writing, there were 20 teachers and researchers. We were joined by a new CNRS researcher in September 2015.

The age distribution is different among technical staff. It starts at just 31, meaning that no very young technician has joined the lab recently. Several technicians retired a few years ago and were replaced between 2008 and 2012. The last retirement in 2013 was not, however, replaced by a new recruitment, but by an internal movement at the CNRS (NOEMI), in the Same age bracket. A young technician (glass blower) joined the unit in January 2017.

The scientific scope in the LCS changed in 2009 when the synthesis of zeolites was added to spectroscopy. The technical potential within the laboratory has been reorganized so that the new research focus is not lacking in technical personnel.

Financial resources are also balanced for LCS. In 2014, the annual funding of the laboratory of our tutorship institutions was around 100 k €, the salary of the permanent staff amounting to 1053 k €. The financing of the contracts amounted to about 1300 k €, of which 530 k € came from subsidies from the ANR and 410 k € from purely industrial contracts. This last part is constantly increasing and we have recently succeeded in establishing new collaborative research contracts with the refining industry in the United States. This balanced source of revenue is the only way to pay the laboratory’s operating costs, which we could not afford to subsidize solely at the institutional level. Part of the contractual envelope is based on a common budget for the LCS, which contributes to operating costs or to support emerging or high-risk projects decided by the Scientific Committee.

Age distribution (Jul 2015) among the permanent staff (33 people: 20 teaching and research, 13 technical)

Continuous improvement of the organization and the scientific policy

Since the end of 2016, the LCS is organized in 2 scientific teams: SPECTROCAT (in charge: Arnaud Travert) and ZEOLITHES (in charge: Valentin Valtchev). The functional flow chart is shown above. Within the biggest team, three project-oriented sub-groups are formed around a project manager. Each member of the LCS can have its activity in one of the teams, but also a transversal activity, whenever necessary. Each team organizes internal scientific meetings, proposes invited professors and subjects for new projects to the Scientific Committee. The balance between teams and subgroups is one of the parameters of the decisions of the Scientific Committee. Scientific seminars are held regularly, with presentations by visiting scientists or members of the LCS.
LCS has progressively assembled a remarkable infrastructure for studying catalysis by spectroscopy with 23 IR spectrometers, 1 UV-Vis, 1 Raman, all with in situ; or operando with on-line analysis (flow controllers, MS, GC, computer control …). All experimental configurations are standardized and dedicated to specific types of measurements, and the management and planning of the use of spectrometers is organized by a small team of technicians and support staff. When a researcher plans an experiment or experimental campaign for a project in one of the scientific themes, the first step is to determine the most appropriate configuration and time of year, which is discussed with the research engineer who Is the main organizer for The Platform, Dr. P. Bazin. The platform is very well organized and ensures that the equipment is in good order and that the users work safely. The training of new users is carried out by the permanent researchers, as well as by the staff of the platform.
Other techniques and infrastructure (NMR characterization, catalysis and synthesis in particular) have recently been installed in LCS, and we have organized them with similar approaches. We therefore now have 4 technological platforms in LCS:

VISIO: Infrared spectroscopy and other vibrations (Philippe Bazin)
RMN (Aurélie Vicente)
SYNTHESIS: Preparation of materials and methods of physical characterization (structure / texture) (Valérie Ruaux)
CATALYSIS: Catalytic tests and characterization of catalysis (Karine Thomas)

Each of the platforms receives a financial contribution from general laboratory funding, and other costs are shared between the scientific projects using the platform. A person is responsible for the platform, and must report annually on the performance and expenses in the platform. This organization makes it possible to give well-defined responsibilities to the greatest number of people and to recognize and use their expertise with maximum efficiency.We also have technical support in computer science, glass blowing and mechanical workshop, with a trained staff (the last two shared with the laboratory of organic chemistry – LCMT, UMR 6507). Over the years, glass blowing has been one of the main advantages of our laboratory for the maintenance and design of new experimental facilities for in situ spectroscopy.

In January 2010, we created a service for industry (especially SMEs) by recruiting V. Blasin-Aube, former Postdoc at the LCS. It has created LCS-Valoris and offers analyzes and on-demand experiments to local or national private companies. These contracts are not as demanding as a full collaborative agreement and may be less costly for the company than a longer collaborative search. Moreover, there is no share of intellectual property and ownership belongs to society. These on-demand science services allow for new relationships with industry, and can often lead to more conventional and broader research collaboration. LCS-Valoris also gives greater visibility to our laboratory in the industrial world. This is a way for us to ensure that our technical equipment is used optimally at all times. The financial resource created is sufficient for the wage costs incurred and even generates some benefits for the LCS, contributing to the overall costs and funding of scientific projects.

We continually develop communication and our common policy by organizing regular meetings of the laboratory board and using internal communication through our Intranet site as much as possible. The laboratory board is the place where all matters concerning everyday life and organization in the LCS are discussed, and where the director may have the laboratory’s advice for all important decisions. The Annual General Meeting is an opportunity to comment on what has happened over the past year, to present the main events planned for next year and to organize a general vote on the key points Of the life of the research unit. The scientific committee meets regularly with an official mission in the laboratory. This committee advises the Director in areas such as the awarding of doctoral scholarships to scientific projects, the policy of new permanent posts and the priority between scientific projects. Scientific calls (EU, LABEX, ANR …) are discussed at the Scientific Committee and meetings are held on a monthly basis. Particular attention is given to health and safety. Each newcomer to the laboratory must pass the H&S available on a specific web page on our intranet. A financial envelope is decided each year for expenditure H & amp; S, resulting in continuous improvements in working conditions. A specific procedure has been introduced to come to the laboratory outside working hours on weekends, and authorization is required in order to avoid isolated workers and to ensure the supervision of scientists trained at all times. Two H&S (Prevention Assistants) were designated (one for each of the LCS buildings) as well as one trained for Radiation Protection and several academic and permanent researchers trained for emergency response. Health and safety training is included in the continuing education and laboratory training plan. Constant care is taken to improve the quality and comfort of offices and common places in the LCS. A comfortable pause area has been created which gives the lab members a pleasant space to eat their lunch, take a coffee break or arrange small meetings that do not require a formal meeting area. Communication and storage of information Are also well supported. The website has been established as an important external and internal communication tool. Each member of the laboratory can have his personal page to show his scientific activities and his production. The H&S is hosted on the website. Information on seminars and scientific news is also posted on the lab homepage, and important news is published on a twitter account. Information and data security is ensured by secure network access and secure data backup procedures.

Highlights

Very important results have been obtained in LCS in recent years. This has allowed us to reach a leading position in our scientific community and to give high visibility to our two new scientific axes.

- Our mastery of the synthesis of nanozeolites without organic structuring agent was recognized by the journal Science as one of the 10 major scientific achievements for the whole of science in the year 2011. This was then a line of Research was very important in LCS and was followed by an article in Nature Material in 2014 for nano zeolites of industrial interest. A very important industrial interest was raised by this achievement, and a major collaboration agreement was established with a large company in the United States. This also led to the award of the first Cronstedt Prize to S. Mintova and V. Valchev, followed by the Breck Prize and the “Research” magazine award.
- Since 1990, we have been designing new and very efficient reactor cells for operando studies. This activity has become increasingly strong over the years. Whatever the experimental conditions, a new cell can be designed and implemented to achieve unprecedented and relevant results by IR spectroscopy. We can even perform operando spectroscopy on a real part of a catalyst monolith. This was recognized by the assignment of CNRS CRISTAL to the Research Engineer in charge of our IR platform, P. Bazin. Our methodological advances cover all our fields of work, and we now have a working facility for hyperpolarized Xenon NMR to study porous systems in solids.

These are just a few examples of the striking facts that have occurred in LCS over the last 5 years. One of the important results of these achievements is our established position in our field of science. Many LCS researchers received the Catalytic Division award from the French Society of Chemistry (DIVCAT), and the last one was awarded to Arnaud Travert in 2012. We have been invited to contribute to several very important work (6 reviews in ChemSocRev and 1 in Chemical Reviews), and in 2015 we organize four major scientific events: the 2nd Euro-Asia Zeolite Conference in Nice in January, the internationally recognized Zeolite Workshop in Caen in April, the 5th Conference Internationale Operando in May in Deauville and the 5th International Symposium on advanced micro- and mesoporous materials in Bulgaria in September.