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Graphene-based products are already being used by manufacturers, from heat-dissipating helmets to antistatic packaging. However, this wonderful material, as it is often called, still has much to deliver to society. As it is two-dimensional, flexible and excellent conductor of electricity, among other properties, graphene can be the basis of a series of high-performance miniaturized electronic and optoelectronic devices. However, this requires producing, at an industrial scale, a graphene whose network of atoms is free of unwanted impurities, but which contains, besides the carbon inherent in the graphene, small amounts of other elements (doping) in order to control its electronic properties.
In a work totally carried out in Brazil, a scientific team has proposed a process that can help produce large-scale graphene that is suitable for electronic devices. “The process developed in our group allows us to improve and adjust the graphene properties, as well as the removal of contaminants from its surface,” said Professor Claudio Radtke (UFRGS), corresponding author of an article reporting the study, recently published in The Journal of Physical Chemistry C.
The team acquired graphene samples produced by chemical vapor deposition (CVD) and transferred to silicon substrates. This technique is currently one of the most suitable for large-scale production of relatively large area graphene sheets, but it leaves residual impurities and generates defects in the graphene. To remove impurities, it is common to apply a heat treatment in an atmosphere of carbon dioxide (CO2), which is efficient in removing contaminants, but ends up generating new defects in the graphene sheet. The good news is that these defects can be neutralized (passivated).
While looking for strategies to passivate these defects, then PhD student Guilherme Koszeniewski Rolim found a scientific paper from 2011, which pointed to, through theoretical calculations, the possibility of using nitric oxide (NO) to passivate graphene defects with nitrogen atoms, while doping it to modulate its electronic properties (mainly transforming it into a semiconductor material, an essential condition for using graphene in electronic devices).
The team then decided to experimentally verify the theoretical prediction and, after performing the traditional treatment with CO2 at 500 °C, they applied a second heat treatment to the samples, this one in nitric oxide atmosphere and at different temperatures, from room temperature to 600 °C.
After the process, the researchers used various characterization techniques to check the results and gladly confirmed that nitrogen doping had taken place and that it had passivated the defects, thus improving the material’s electronic properties. However, the researchers also noted an unwanted effect of nitric oxide treatment: etching of graphene sheets at some points. After much scientific work, the team was able to determine the cause. During heating, there was a conversion of NO to NO2, which, as it is a much more reactive compound than the former, eventually oxidized the graphene.
However, the Brazilian team found a solution to this problem. The “eureka” moment occurred as the researchers were trying to determine the amount of nitrogen atoms that had been incorporated into graphene using a technique based on the analysis of nuclear reactions triggered by the effect of an ion beam on the graphene samples. In order to apply this technique, the team had to use an isotopically enriched nitric oxide in the heat treatment, which has a purity of 99.9999% instead of 99.9% of the gas previously used.
The analysis did not yield the expected results as it failed to quantify nitrogen, which was below the detection limit. However, the use of the enriched gas eventually brought great satisfaction to the team. Indeed, when the researchers compared the electronic properties of both sample types, they found that graphene treated with enriched gas always had superior properties. “Initially, such a result created much confusion in the interpretation of the results,” says Professor Radtke. “But after a few more experiments, it became one of the most important points of the article, highlighting the importance of gas purity during processing,” he adds. Specifically, the conclusion was that by properly controlling the temperature and purity of the gas during the treatment one can eliminate the problem of oxidative graphene degradation.
Thus, based on solid knowledge and scientific method, as well as some serendipity, the UFRGS team was able to develop a process of waste removal, defect neutralization and graphene doping, which improved the electronic properties of the material without producing deleterious side effects. Because it is a heat treatment in a gas atmosphere, a step that is now part of the industrial production of graphene, the process proposed by the Brazilian team could be easily applied in the production of graphene sheets for devices.
“The insertion of heteroatoms (such as nitrogen) into the graphene network without the degradation of its properties is especially important in the production of optoelectronic devices, high speed transistors, low power electronics and photovoltaic cells,” says Radtke, noting that manufacturing these graphene-based devices may be a reality in years to come. “The Graphene Flagship (European consortium of industries, universities and institutes) has announced the implementation of a pilot plant to integrate graphene at different production stages of devices as early as 2020,” comments the professor from UFRGS.
The study, which was funded by the Brazilian agencies CNPQ (mainly through INCTsNamitec and INES), Capes and Fapergs, was developed within the PhD in Microelectronics by Guilherme Koszeniewski Rolim, held at the UFRGS Graduate Program in Microelectronics and defended in 2018. The experimental work was carried out at the UFRGS Solid Surface and Interfaces Laboratory and the Brazilian National Synchrotron Light Laboratory.
[Paper: Chemical Doping and Etching of Graphene: Tuning the Effects of NO Annealing. G. K. Rolim, G. V. Soares, H. I. Boudinov, and C. Radtke. J. Phys. Chem. C, 2019, 123, 43, 26577-26582. https://doi.org/10.1021/acs.jpcc.9b02214.]
In 2004, three young chemistry graduates from the Brazilian Federal University of São Carlos (UFSCar) created a nanotechnology-based materials company. Today, Nanox has about 30 products developed, a technological platform consisting of seven patents (three worldwide, one in Europe, one in the United States) and over 200 clients, not only in Brazil, but also in 13 other countries.
Nanox’s business is to develop, produce and market nanotechnology-based materials whose properties (bactericidal, fungicidal, repellent, anti-sweat, antiallergic…) add value to a particular product (packaging, flooring, carpet, t-shirt…). Thus, Nanox provides its customers (companies in various segments) nanomaterials that can be easily incorporated into their products, which bring tangible benefits to end consumers.
Today Nanox’s flagship products are silver-based antimicrobial additives. The company has developed a series of such products within three broad lines: solution additives (liquid), powder additives (solid), and additives already mixed with polymeric materials.
As shown by the ratio between the number of products launched and the company’s years of existence (about 30 innovations in 15 years), innovation is part of everyday life at Nanox. Generally, the process is as follows. In its contacts with the market, the Nanox team identifies latent demands that can be met by applying the technologies that the company has mastered. The team then validates their innovation ideas with potential customers and begins to work on product development.
At its 500 m2 headquarters, located in the city of São Carlos (state of São Paulo, Brazil), Nanox has about 150 m2 of internal laboratories for research and development and quality control. There are three physicochemical laboratories, one for materials engineering and one for microbiology, in which the team performs bactericidal and fungicidal efficiency tests. The company has two researchers (one master’s and one doctor) dedicated to R&D activities, but, depending on the project and the development phase, the team may include up to five people. In addition, Nanox partners with external research laboratories to perform activities where there is no internal expertise and for those requiring expensive equipment such as electron microscopy or X-ray characterization of materials.
History and cases
It all started at a UFSCar research center supported by the São Paulo Research Foundation (Fapesp), the Multidisciplinary Center for the Development of Ceramic Materials (CMDMC), today the Center for the Development of Functional Materials (CDMF). There, under the guidance of Professor Elson Longo, friends André Luiz de Araujo (who worked at the company until 2011 and to date remains a shareholder), Daniel Tamassia Minozzi (current COO) and Luiz Gustavo Pagotto Simões (current CEO) were doing their undergraduate and master´s research.
In 2004, at the behest by the Brazilian home appliance company Multibrás to CMDMC, the trio saw an opportunity for entrepreneurship in the nanotechnology-based materials segment, which at that time had few products and very few companies in Brazil.
The project consisted of developing nanostructured films to protect metallic surfaces. To make it possible, Nanox obtained funding from Fapesp’s Pipe program, dedicated to supporting innovation research in small companies. This would be the first of seven fundings for Nanox from the Pipe program to support various phases of technology and product development, among other Brazilian public federal fundings.
In 2005, Nanox sold a product for the first time. It was a titanium dioxide nanoparticle film applied in the filters of hair dryer used in beauty salons, manufactured by the Brazilian company Taiff. The bactericidal and fungicidal effect of the nanomaterial guaranteed more salon hygiene and consumer health. The product earned Nanox a Brazilian award (Finep Innovation Award) in 2007, as well as widespread publicity and visibility.
In 2006, realizing that there was plenty of room for Nanox innovations in plastic products, the partners decided to start developing nanomaterials in the form of additives that could be incorporated into various polymers. Through partnerships with companies (Nanox customers), these innovations have reached end-consumers. An example is PVC films (those used in the home environment to pack cut fruits and other foods) with antibacterial shield. In 2014, the Brazilian company AlpFilm launched a line of films with additives from Nanox, whose antibacterial and antifungal effect allows conserving packaged foods longer by avoiding their degradation. Another Nanox case is a packaging that doubles the validity of fresh milk thanks to the antibacterial effect of the additive. The world’s first bactericidal milk bottle began to be used by the Brazilian agro-industry Agrindus in 2015, and was the headline for food and packaging industry websites and magazines in several countries.
In 2009 there was another milestone in the history of Nanox. A presentation the company prepared for a General Electric team in Brazil ended up at the company’s Mexican branch and generated so much interest that, 15 days later, Nanox was undertaking its first export, which consisted of plastic additives to make refrigerator boxes in Mexico. From that moment on, Nanox began to look towards the foreign market, starting a strategy that includes investments in international fairs, representatives in several countries and training the team to deal with bureaucratic issues inherent to the export process and the introduction of products in different countries. This journey is currently reflected in exports that represent 12% of the company’s revenues, with recurring sales to Argentina, Chile, Colombia and Mexico; halfway toward the US market, and distributors in countries from Latin America, Eastern Europe and Asia. In addition, this year Nanox participated in a business acceleration program for Plug and Play Tech Center, a Silicon Valley-based innovation platform that has hosted companies such as Dropbox and PayPal. Nanox was one of 15 companies selected from 1,000 companies worldwide.
See our interview with Luiz Gustavo Pagotto Simões, PhD (2009) in Chemistry from UNESP, co-founder and current CEO of Nanox.
B-MRS Newsletter: What were the most important factors that allowed Nanox to develop in its various phases?
Gustavo Simões: It was a sum of factors. Financial resources, both public and venture capital – the latter from 2006 on, when the company became a Ltd., as well as the work of entrepreneurs and the team to validate products and bring them to market. We always use the resources of Fapesp and Finep to lower capital acquisition costs for development, especially at some crucial moments of the company. For example, at a time when we had a technology but its scale was too small, we got a Pipe phase 3 that allowed us to scale up production. The investor was also important; it improved the administrative and commercial structure of the company. The most important thing was to validate everything we thought could be a Nanox product, and you can’t do it without money or personnel. In addition, we must thank Professor Elson Longo, who accompanied Nanox in all its phases as a supporter, scientific advisor, partner, promoter…
B-MRS Newsletter: What were the main difficulties Nanox has faced thus far?
Gustavo Simões: In fact, trading nanotechnology in Brazil is not easy. At that time, many people said they wanted to have nanotechnology, but very few took a chance on this. We were very lucky to have some key partners like Taiff and IBBL. These companies decided, in a market as competitive as Brazil, to differentiate themselves and add a product like ours into their product. So the difficulty of getting customers has always been among the greatest issues. And also to survive this madness that is Brazil for entrepreneurship. The exchange rate variations, for example, have a direct impact on the company, and we have to get around such situations, this requires creativity and flexibility. It is rare to plan and get out what you have planned.
B-MRS Newsletter: Nanox is recognized worldwide and exports its products to various countries. Tell us a little about Nanox’s internationalization and what it is like for this Brazilian company to compete in foreign markets.
Gustavo Simões: Latin American markets are similar to Brazil’s market. They are less regulated, which increases the possibility of competition because there may always be a local player that competes with you. On the other hand, these markets are easier to access than the more regulated markets, such as the US, where you need multiple regulatory agency registrations and licenses, which require a number of expensive studies and tests. Not everyone is willing to do this. So, higher regulation creates a barrier to enter the market which decreases the number of competitors. We’re in the process of getting licenses to be able to sell our products in the United States, and we’ve already obtained some. In some products, we will only have three competitors in the United States.
In addition to this regulatory issue, other factors that hinder export are cultural issues, such as language. In Latin America, Brazil is the only Portuguese-speaking country. In Brazil there are also some bureaucracies, for example in banks, which hinder exports and may also make a business line not worth it. This has to change.
So, internationalization is quite expensive. You have to attend fairs abroad and have a team trained in the export bureaucracy and regulation of the markets you want to reach. However, I believe that in products like ours, more technology intensive and less labor intensive, Brazil is very competitive. We even have incentives to export. If you export, you do not pay some taxes and the product has a more competitive price abroad. Exports account for approximately 12% of Nanox’s revenues, but this percentage is expected to grow. After the last international fair in which we participated (in the plastics segment) we received orders from Iran, India, Pakistan…
B-MRS Newsletter: What do you think is Nanox’s main contribution to society?
Gustavo Simões: A contribution is the training of human resources, always with very good interaction here. A lot of people have worked here and today they are doing really well working in multinational companies. Moreover, I believe it’s important to share through media, lectures, etc. our experience from the point of view of entrepreneurship, to show that there is a different way of working, besides working in a private company or as a Professor. It is important to show that there is a possibility and that there are incentives and support in the country, perhaps not as many as we would like, but much more than in other places. In addition, the other contribution we make is our products for food safety and better quality of life. But, as Elson [Longo] says, if I can leave a line in the literature, that’s a lot; now, if I can motivate a person to undertake and run a project, this is very important.
B-MRS Newsletter: What is your goal/dream for Nanox?
Gustavo Simões: We want to consolidate internationalization, and we want to place ourselves as global players. We are making a very strong move, even though the dollar is crushing us because we are earning in reais [Brazilian currency] and spending in dollars. Over the next 5 years, we expect to have a larger international market share in revenues, so much that we have opened an office in the United States and are talking to investors to get funds over there.
B-MRS Newsletter: Leave a message for people who are considering entrepreneurship.
Gustavo Simões: I would say that entrepreneurship is worthwhile and necessary. I believe that the technical knowledge we receive in Brazil in our undergraduate courses, for example in Materials, leaves nothing to be desired elsewhere in the world. We have to convert knowledge into wealth, and there is only one way to do that – which is through entrepreneurship.
I think this issue of university-business interaction and spin-offs is the future for us to create a differentiated value-added economy in a country where we have a huge consumer market. If we can use all these financial and human resources, these extremely well-trained people, and generate products and services for the economy, I think it will be a very promising future.
Professor Andrea Simone Stucchi de Camargo (IFSC-USP), B-MRS member and elected scientific director of the Society for the 2020-2021 period, is one of the coordinators of an international event for women in science to be held in Rio de Janeiro from February 12 to 14, 2020, with support from the Brazilian Academy of Sciences (ABC).
The event will bring together the “World Forum for Women in Science” and the “4th International Conference for Women in Science without Borders: Energy, Water, Health, Agriculture and Environment for Sustainable Development.”
Event website: http://www.abc.org.br/en/evento/wfwsbr20/
Forty-nine (49) proposals were submitted by the international scientific community within the XIX B-MRS Meeting + IUMRS ICEM symposium call. The number of submissions is one of the largest in the history of B-MRS events. “We received proposals from 18 different countries,” says Professor Gustavo Dalpian, chair of the event.
The organizing committee is already working on the analysis of the proposals, in order to solve cases of thematic overlap and to ensure the symposia are adequate to the structure of the event. When necessary, the committee will contact the authors of the proposals. The final list of symposia will be announced during December on the event website, B-MRS website, B-MRS Newsletter and social media. In February 2020, the abstract submission will be opened.
About the event
The event, which will be held from August 30 to September 3, 2020 at the Rafain Palace Hotel in Foz do Iguaçu (Brazil), will bring together the nineteenth edition of B-MRS annual meeting and the seventeenth edition of the international conference on electronic materials organized every two years by IUMRS.
In addition to symposia oral and poster presentations, the program will include plenary lectures by leading scientists such as Alex Zunger (University of Colorado Boulder, USA), Edson Leite (LNNano, Brazil), Hideo Hosono (Tokyo Institute of Technology, Japan), John Rogers (Northwestern University, USA), Luisa Torsi (Università degli Studi di Bari “A. Moro”, Italy) and Tao Deng (Shanghai Jiaotong University, China).
The event is coordinated by professors Gustavo Martini Dalpian (UFABC) in the general coordination, Carlos Cesar Bof Bufon (LNNANO) in the program coordination and Flavio Leandro de Souza (UFABC) as general secretary. At the international committee, the event features scientists from America, Asia, Europe and Oceania.
B-MRS’s Board of Directors created, in October of this year, the José Arana Varela Award. This new honor from B-MRS pays tribute to Professor José Arana Varela, a prominent Brazilian materials scientist and former president of B-MRS, who passed away in 2016.
This is an annual award that will be bestowed to a leading researcher in Brazil, who will deliver one of the plenary lectures at B-MRS Meeting. In 2020, the recipient will be Edson Roberto Leite, full professor at UFSCar and scientific director of the Brazilian Nanotechnology National Laboratory (LNNano).
About Professor José Arana Varela
Born in Martinópolis, São Paulo State (Brazil), on April 11, 1944, José Arana Varela graduated in Physics from the University of São Paulo (USP) in 1968. In 1975, he obtained his Master’s degree in Physics from the Technological Institute of Aeronautics (ITA). He completed his doctorate in ceramic materials (1977 to 1981) at the University of Washington (United States).
Arana Varela was a Full Professor at the Paulista State University Júlio de Mesquita Filho (Unesp), where he began his academic career in 1969. He was also a Professor at the Federal University of São Carlos (UFSCar), where he worked since 1985, mainly in the graduate programs in Chemistry and Materials Science and Engineering.
As a researcher, Arana Varela worked in the field of ceramic materials, making important international contributions to electroceramics and ceramic thin films, and their applications in varistors, ferroelectric memories and chemical sensors.
In Brazil, he led the development of these research lines, beginning in 1988 with the founding, together with other professors of UFSCar, of the Interdisciplinary Laboratory of Electrochemistry and Ceramics (LIEC), which was the seed of the Multidisciplinary Center for the Development of Ceramic Materials (CMDMC), which created the Center for the Development of Functional Materials (CDMF).
Professor Varela supervised or co-supervised at least 30 master’s and over 40 doctoral works. He co-authored more than 600 articles published in international journals, with more than 20,000 citations. He also authored patents and participated in various projects interacting with the industry.
A strong supporter of international collaboration as a driver of scientific and technological advancement, Arana Varela maintained such cooperation throughout his career with research groups from the United States, France, Spain, Portugal, Slovenia and Italy, as well as Brazil.
In parallel to his distinguished career as a researcher and professor, José Arana Varela had a broad performance in management or advisory positions. At the São Paulo State Research Foundation (Fapesp), he was the director-president of the Technical-Administrative Council from 2012 to 2016 and vice-president of the Superior Council from 2007 to 2010. At Unesp, he was the first Pro-Rector of Research (2005-2009), as well as founder and director of the Unesp Innovation Agency (2009-2012). He was also a member of the Superior Council for Innovation and Competitiveness of the Federation of Industries of the State of São Paulo (Fiesp), member of advisory committees of the National Council for Scientific and Technological Development (CNPq) and director at the Brazilian Association of Metallurgy and Materials (ABM) and the Brazilian Ceramic Association (ABCeram). Finally, starting in 2015, he was a board member of the Ceramic and Glass Industry Foundation, the arm of ACerS (The American Ceramic Society), dedicated to developing professionals for the global ceramic and glass industry.
Arana Varela was a fellow of ACerS and a member of The World Academy of Ceramics and the Materials Research Society (MRS). Professor Varela was also a member of several Brazilian scientific societies, such as the Brazilian Academy of Sciences (ABC), the São Paulo State Academy of Sciences and the Brazilian Society of Physics (SBF).
At B-MRS, the scientist was a founding member, part of the founding board, and served as chief financial director from 2004 to 2005, and as president from 2010 to 2011.
Arana Varela was a member of the editorial board of the journals Ceramics International, Science of Sintering, Cerâmica, and Materials Research. He received more than twenty national and international awards and distinctions, such as the Premio Épsilon de Oro (2003) of the Sociedad Española de Cerámica y Vidrio, the Scopus Capes-Elsevier Award (2006) for his scientific production, and two awards from the American Ceramic Society, the Global Star Award (2013) and the Bridge Builder Award (2014).
José Arana Varela passed away on May 17, 2016, at the age of 72, after battling cancer for three years.
A team of students from the Brazilian Federal University of ABC (UFABC) created the twelfth unit of B-MRS’s University Chapters (UCs) program. The new UC is made up of 4 Master’s degree students in Materials Science and Engineering and 6 Master’s students in Nanosciences and Advanced Materials, in addition to the group advisor, Professor Márcio Gustavo Di Vernieri Cuppari.
“We hope to bring together the students of the two postgraduate programs, as well as undergraduate students,” says Isabela Coutinho, president of UC – UFABC. “We hope that these meetings, in the form of scientific events, will facilitate the dissemination of the materials area among students of the ABC community. We also hope to enrich the education of undergraduate and graduate students through the influence of B-MRS,” adds the Master’s student in Materials, who won one of the Bernhard Gross Awards at the XVIII B-MRS Meeting, held from 22 to 26 September of this year in Balneário Camboriú.
To this end, the team plans to invite internal and external researchers to lectures and workshops and to hold scientific outreach meetings and exchange experiences. In addition, says the president, the team would like to receive suggestions for activities that have been successfully performed in other UCs and which can be carried out by the UFABC group.
The UC – UFABC, which was created on August 1st of this year, has a Facebook page (https://www.facebook.com/UCUFABC/) where it has already started to promote its activities.
Within the UCs program, B-MRS has 12 teams of students from federal, state and community universities located in the five Brazilian regions. These groups develop complementary activities to their academic development.
Learn about the B-MRS UCs Program and the units created so far: http://sbpmat.org.br/en/university-chapters/
The current president of B-MRS, Professor Osvaldo Novais de Oliveira Junior (IFSC-USP), is part of the triple list sent to the governor of the State of São Paulo to select the new scientific director of the São Paulo Research Foundation (FAPESP). The list was defined by the Superior Council of FAPESP after the election, which had 13 candidates.