The National University of Science and Technology MISIS (Moscow) for several decades implements research programs in nanotechnology and trains specialists, including, for the nanotechnology industry. It is no coincidence that nanotechnologies and new materials are designated as one of the priorities in the University Development Programme in 2009-2017. MISIS puts greater focus on improving the technological infrastructure for the R&D and educational activities, in particular, new laboratories are established. A number of remarkable projects to develop research and educational laboratories in MISIS were accomplished in partnership with Tokyo-Boeki.
Теги: boron nitride electron microscope nanostructures probe microscope spark plasma sintering зондовый микроскоп искровое плазменное спекание наноструктуры нитрид бора электронный микроскоп
A number of remarkable projects to develop research and educational laboratories in MISIS were accomplished in partnership with Tokyo-Boeki, a supplier of the measurement and process equipment of JEOL, Sps, Yamato, Rigaku, Ulvac. Among their number, the Japanese JEOL electron microscopes have been used successfully in advanced research of inorganic nanomaterials as well as for the educational process.
Inorganic nanomaterials laboratory
In 2010, the government adopted a decree on measures to attract leading scientists to Russian universities, according to which on a competitive basis the grants of up to 150 million roubles each are appropriated for research. One of these grants was allocated for MISIS to set up a research laboratory to study boron nitride nanostructures under the supervision of one of the most prominent professionals in this field, director of the Nanotubes Group of the Center for Materials Nanoarchitectonics (MANA) of the National Institute for Materials Science (NIMS), Professor of the University of Tsukuba (Japan) Dmitry Golberg.
The nanostructures of boron nitride are characterized by a high chemical stability and durability. In contrast to carbon nanotubes, which begin to oxidise at 500-600°C, the boron nitride nanotubes can withstand heating up to 1100-1200°C, so they can be used at high temperatures. Some more advantages of the boron nitride nanostructures, which can be in demand, e.g. in the production of electronic and optical components are the electrical insulation properties, high thermal conductivity and low optical density.
The Inorganic Nanomaterials Laboratory in MISIS started operate in October 2012. According to the Laboratory Head Professor Dmitry Shtansky, the main scope of researches is related with obtaining high-strength ultralight structural materials by reinforcement of aluminium alloys by boron nitride nanostructures. A synthesis of nanostructures is performed by chemical vapour deposition techniques (CVD) in reactors specially designed and manufactured for the laboratory. During the synthesis, the nanostructures of different morphologies are obtained, from nanotubes, nano-spheres and graphene-like plates to complex geometric shapes.
The samples of composite materials are produced by hot pressing, pulsed plasma sintering or casting from the melt. After obtaining a sample, its structure and mechanical properties will be studied. Already first experiments showed that the strength of the composite materials reinforced by boron nitride nanotubes is considerably higher than the strength of the base aluminium alloy. With the improvement of composites, their strength reached 350 MPa, which is comparable to the strength of the low-carbon steel, at the same time the new material is three times lighter. But, according to the laboratory staff, this value can be significantly improved.
A new area of researches of the laboratory is the use of different types of boron nitride nanostructures in life science. In particular, it is considered very promising to use nanospheres with the medicines for the treatment of cancer. D.Shtansky: "The problem of biocompatibility of boron nitride nanostructures is still relatively poorly researched but there is evidence that such compatibility can be achieved. It is important that boron nitride nanospheres meet the requirements in respect of size of the objects that can be absorbed by the cancer cells".
The laboratory puts special emphasis on developing technologies for the synthesis of boron nitride nanostructures, which would ensure their production in large quantities. A solution to this problem is one of the necessary pre-conditions for the widespread industrial use of boron nitride nanostructures in metallurgy, medicine and other fields.
The inorganic nanomaterial laboratory has the state-of-the-art metallurgical, measuring and analytical equipment for the synthesis of nanostructures. For a morphological analysis of nanostructures and composites samples is used the Field Emission Scanning Electron Microscope JEOL JSM 7600F. The device can be operated with an accelerating voltage of 0.5 kV to 30 kV and provides a resolution of less than 1 nm (1.0 nm at an accelerating voltage of 15 kV). The attachment for energy-dispersion microanalysis JED-2300F allows carrying out a qualitative and quantitative analysis of the solid-state structures.
"The laboratory needed an electron microscope that would provide rapid screening of a large number of objects with high resolution and depth of field", says Dmitry Shtansky. "Practice has shown that we have made the best choice. Thanks to the high speed of analysis in JEOL JSM 7600F, we daily control the results of several syntheses, that run in parallel. We have quickly mastered the basic functions of the microscope; the instrument is run by several operators who constantly exchange experiences with each other".
A study of boron nitride nanoobjects with an electron microscope do not require any complicated sample preparation procedures or techniques. However, they can not be called routine, in particular, problems with surface charging arise. The latters are resolved by the Gentle Beam mode, which improved the resolution at an extremely low accelerating voltage.
For manufacturing of nanocomposites samples is also used equipment installed in other laboratories of the University, e.g. the spark plasma sintering system Labox 650 produced by the Japanese company Sinter Land. Spark plasma sintering occurs in vacuum at a pressure of up to 6 tons by passing high currents (5000A). There is also a possibility of using an inert gas, and the operational temperature can reach 2400°C. The system provides sintering of similar and dissimilar materials with evaporation of impurities and a minimal grain growth.
International School of Microscopy
Scientific Research Center "International School of Microscopy" (SRCM) was established in 2011 by MISIS in collaboration with Tokyo-Boeki. The Center is a base for scientific research, teaching of University students, and commercial courses on electron and atomic force microscopy.
"The idea of establishing the center appeared in 2008", says the director of the SRCM Dmitry Zhukov. "Deficiency of specialists in electronic and atomic-force microscopy is apparent; so we have developed training courses that allow for mastering both theoretical knowledge and practical skills for a few days. Currently three courses are offered: basics of the scanning and transmission electron microscopy and an advanced course in the scanning electron microscopy. Also almost ready is the course in atomic force microscopy. We educate everyone including those from scratch. After passing intensive basic training courses, operators can work independently on the device meaning that they can obtain and interpret images".
The SRCM has five employees, three of them are trainers. Courses are designed for 40 academic hours of study combining theory and practice, plus 10 hours of self-training and a four-hour exam. Graduates receive a certificate of professional development and the operator’s certificate signed by MISIS and Tokyo-Boeki.
The Center’s key equipment includes the transmission electron microscope JEOL JEM 1400, scanning electron microscope JEOL JSM 6610LV and atomic-force microscope AIST-NT Smart SPM 1000. " We proceeded from the fact that, on the one hand, the devices should allow to perform research, on the other hand, their design should be intelligible for training ", D.Zhukov explains the choice of equipment. "When choosing a supplier, the positive experience in using of JEOL equipment and the partner relationships with Tokyo-Boeki, which had worked in our country since 1959, was taken into account".
The transmission electron microscope JEM 1400 allow to work with accelerating voltage up to 120 kV and high resolution (point image of 0.38 nm and lattice image of 0.2 nm). The minimum diameter of the electron beam is 50 nm, which allows obtaining in the microbeam mode a diffraction pattern from an area of approximately the same diameter.
The scanning electron microscope JSM 6610LV is equipped with electron gun with W or LaB6 cathodes. Due to the unique condenser lens with a variable focal length developed by JEOL, the focus and position of the visual field even at very high magnifications are kept unchanged. The microscope provides a spatial resolution of up to 3 nm. The unit for energy-dispersion microanalysis INCA SDD X-MAX produced by Oxford Instruments and INCA Energy software extends the capabilities of the microscope.
A classroom of the SRCM is equipped with an interactive whiteboard, which displays the same information as the operator sees on the devices in neighbouring premises. Instrument control systems are integrated into a network thus making it possible for the operator to have remote access from anywhere in the world.
"The courses like ours in Russia are rare", says D.Zhukov. "The combination of the theoretical and practical lessons ensures a high efficiency of our courses, and we are pleased to invite to our center all those wishing to become experts in the field of electron microscopy". ■
Inorganic nanomaterials laboratory
In 2010, the government adopted a decree on measures to attract leading scientists to Russian universities, according to which on a competitive basis the grants of up to 150 million roubles each are appropriated for research. One of these grants was allocated for MISIS to set up a research laboratory to study boron nitride nanostructures under the supervision of one of the most prominent professionals in this field, director of the Nanotubes Group of the Center for Materials Nanoarchitectonics (MANA) of the National Institute for Materials Science (NIMS), Professor of the University of Tsukuba (Japan) Dmitry Golberg.
The nanostructures of boron nitride are characterized by a high chemical stability and durability. In contrast to carbon nanotubes, which begin to oxidise at 500-600°C, the boron nitride nanotubes can withstand heating up to 1100-1200°C, so they can be used at high temperatures. Some more advantages of the boron nitride nanostructures, which can be in demand, e.g. in the production of electronic and optical components are the electrical insulation properties, high thermal conductivity and low optical density.
The Inorganic Nanomaterials Laboratory in MISIS started operate in October 2012. According to the Laboratory Head Professor Dmitry Shtansky, the main scope of researches is related with obtaining high-strength ultralight structural materials by reinforcement of aluminium alloys by boron nitride nanostructures. A synthesis of nanostructures is performed by chemical vapour deposition techniques (CVD) in reactors specially designed and manufactured for the laboratory. During the synthesis, the nanostructures of different morphologies are obtained, from nanotubes, nano-spheres and graphene-like plates to complex geometric shapes.
The samples of composite materials are produced by hot pressing, pulsed plasma sintering or casting from the melt. After obtaining a sample, its structure and mechanical properties will be studied. Already first experiments showed that the strength of the composite materials reinforced by boron nitride nanotubes is considerably higher than the strength of the base aluminium alloy. With the improvement of composites, their strength reached 350 MPa, which is comparable to the strength of the low-carbon steel, at the same time the new material is three times lighter. But, according to the laboratory staff, this value can be significantly improved.
A new area of researches of the laboratory is the use of different types of boron nitride nanostructures in life science. In particular, it is considered very promising to use nanospheres with the medicines for the treatment of cancer. D.Shtansky: "The problem of biocompatibility of boron nitride nanostructures is still relatively poorly researched but there is evidence that such compatibility can be achieved. It is important that boron nitride nanospheres meet the requirements in respect of size of the objects that can be absorbed by the cancer cells".
The laboratory puts special emphasis on developing technologies for the synthesis of boron nitride nanostructures, which would ensure their production in large quantities. A solution to this problem is one of the necessary pre-conditions for the widespread industrial use of boron nitride nanostructures in metallurgy, medicine and other fields.
The inorganic nanomaterial laboratory has the state-of-the-art metallurgical, measuring and analytical equipment for the synthesis of nanostructures. For a morphological analysis of nanostructures and composites samples is used the Field Emission Scanning Electron Microscope JEOL JSM 7600F. The device can be operated with an accelerating voltage of 0.5 kV to 30 kV and provides a resolution of less than 1 nm (1.0 nm at an accelerating voltage of 15 kV). The attachment for energy-dispersion microanalysis JED-2300F allows carrying out a qualitative and quantitative analysis of the solid-state structures.
"The laboratory needed an electron microscope that would provide rapid screening of a large number of objects with high resolution and depth of field", says Dmitry Shtansky. "Practice has shown that we have made the best choice. Thanks to the high speed of analysis in JEOL JSM 7600F, we daily control the results of several syntheses, that run in parallel. We have quickly mastered the basic functions of the microscope; the instrument is run by several operators who constantly exchange experiences with each other".
A study of boron nitride nanoobjects with an electron microscope do not require any complicated sample preparation procedures or techniques. However, they can not be called routine, in particular, problems with surface charging arise. The latters are resolved by the Gentle Beam mode, which improved the resolution at an extremely low accelerating voltage.
For manufacturing of nanocomposites samples is also used equipment installed in other laboratories of the University, e.g. the spark plasma sintering system Labox 650 produced by the Japanese company Sinter Land. Spark plasma sintering occurs in vacuum at a pressure of up to 6 tons by passing high currents (5000A). There is also a possibility of using an inert gas, and the operational temperature can reach 2400°C. The system provides sintering of similar and dissimilar materials with evaporation of impurities and a minimal grain growth.
International School of Microscopy
Scientific Research Center "International School of Microscopy" (SRCM) was established in 2011 by MISIS in collaboration with Tokyo-Boeki. The Center is a base for scientific research, teaching of University students, and commercial courses on electron and atomic force microscopy.
"The idea of establishing the center appeared in 2008", says the director of the SRCM Dmitry Zhukov. "Deficiency of specialists in electronic and atomic-force microscopy is apparent; so we have developed training courses that allow for mastering both theoretical knowledge and practical skills for a few days. Currently three courses are offered: basics of the scanning and transmission electron microscopy and an advanced course in the scanning electron microscopy. Also almost ready is the course in atomic force microscopy. We educate everyone including those from scratch. After passing intensive basic training courses, operators can work independently on the device meaning that they can obtain and interpret images".
The SRCM has five employees, three of them are trainers. Courses are designed for 40 academic hours of study combining theory and practice, plus 10 hours of self-training and a four-hour exam. Graduates receive a certificate of professional development and the operator’s certificate signed by MISIS and Tokyo-Boeki.
The Center’s key equipment includes the transmission electron microscope JEOL JEM 1400, scanning electron microscope JEOL JSM 6610LV and atomic-force microscope AIST-NT Smart SPM 1000. " We proceeded from the fact that, on the one hand, the devices should allow to perform research, on the other hand, their design should be intelligible for training ", D.Zhukov explains the choice of equipment. "When choosing a supplier, the positive experience in using of JEOL equipment and the partner relationships with Tokyo-Boeki, which had worked in our country since 1959, was taken into account".
The transmission electron microscope JEM 1400 allow to work with accelerating voltage up to 120 kV and high resolution (point image of 0.38 nm and lattice image of 0.2 nm). The minimum diameter of the electron beam is 50 nm, which allows obtaining in the microbeam mode a diffraction pattern from an area of approximately the same diameter.
The scanning electron microscope JSM 6610LV is equipped with electron gun with W or LaB6 cathodes. Due to the unique condenser lens with a variable focal length developed by JEOL, the focus and position of the visual field even at very high magnifications are kept unchanged. The microscope provides a spatial resolution of up to 3 nm. The unit for energy-dispersion microanalysis INCA SDD X-MAX produced by Oxford Instruments and INCA Energy software extends the capabilities of the microscope.
A classroom of the SRCM is equipped with an interactive whiteboard, which displays the same information as the operator sees on the devices in neighbouring premises. Instrument control systems are integrated into a network thus making it possible for the operator to have remote access from anywhere in the world.
"The courses like ours in Russia are rare", says D.Zhukov. "The combination of the theoretical and practical lessons ensures a high efficiency of our courses, and we are pleased to invite to our center all those wishing to become experts in the field of electron microscopy". ■
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