Laboratory of Inorganic Synthesis
Synthesis and characterisation of inorganic materials with applications in energy, optics, ecology and biomedicine. This includes low- and high-temperature syntheses, solid-state processes and analytical methods such as TXRF for elemental analysis and the evaluation of materials for environmental applications.
Description of Activities
Description of the Service
• Development of methods for the synthesis of target materials for various purposes, based on the available equipment.
• Synthesis of materials at atmospheric and high pressure, as well as under vacuum, using a procedure developed for the specific material.
• Efficient dispersion and homogenisation of high-viscosity reaction mixtures (up to 5 000 mPas).
• Solid-state synthesis, as well as calcination/sintering of materials, in the temperature range 20 – 1300 °C under a controlled atmosphere (nitrogen, argon, oxygen, air) using a variety of temperature regimes.
• Multi-element analysis of impurities in samples in the form of liquids and suspensions, for elements with an atomic number above 20 (macro- and microelements, and traces at ppm level).
Equipment
1. Laboratory Reactor for Synthesis under Pressure
The reactor is a Berghof BR-100 (Germany), made of stainless steel, with a maximum operating temperature of 230°C (when using Teflon vessels) and a pressure of up to 200 bar. The reactor is equipped with Teflon reaction vessels with volumes of 100, 150 and 200 ml. It allows synthesis to be carried out both without stirring and with stirring at a controlled speed. It allows synthesis to be carried out over a period of 17 days without changing the input parameters. It is fitted with an attachment for injecting and withdrawing liquids at operating pressure (i.e. during the actual process). It is equipped with a computer system and dedicated software for operation, control and data recording.
2. Laboratory Reactor System
The system comprises the following modules:
a) 2 laboratory synthesis reactors (LR 1000 control System, IKA®-Werke GmbH &Co. KG, Germany);
b) Vacuum pump with an ultimate pressure of 2 mbar (IKA VACSTAR control), enabling synthesis under vacuum;
c) Refrigerated circulating thermostat (RC 2 basic, IKA®-Werke GmbH &Co. KG, Germany) with a temperature range from minus 20 °C to room temperature;
d) Disperser (T 25 digital ULTRA – TURRAX) with various dispersing attachments;
All modules can operate either independently or as a system. The equipment offers manual and software control and recording of the synthesis parameters. The laboratory reactor system offers a wide range of functional capabilities, such as:
– synthesis in the temperature range between 5 and 120 °C with precise control of the temperature, the pH of the medium and the stirring speed;
– synthesis in various gas atmospheres and under vacuum;
– operation with various dispersing tools, ensuring the stirring and homogenisation of highly viscous reaction mixtures;
3. Temperature-Programmable Furnaces
The laboratory has three programmable high-temperature furnaces:
3.1. Muffle furnace with a maximum temperature of 1400 °C (LHTC 3/14 C450, Nabertherm GmbH);
Internal dimensions of the heating chamber (width x depth x height, in cm): 12 x 21 x 12 cm; volume: 3 l. Time to reach the maximum temperature: up to 40 min. The furnace is equipped with a C450 electronic controller, allowing up to 10 programs with up to 20 steps per program to be set.
3.2. Tube furnace with a maximum temperature of 1300 °C (R 50/500/13 C450, Nabertherm GmbH, Germany)
The furnace is connected for operation in various atmospheres; it is also equipped for operation under vacuum;
It operates with work tubes with an outer diameter of up to 50 mm and a length of 670 mm, and has a heating zone 50 cm long; the heating zone in which the temperature is controlled to within ± 5°C of the set value is 15 cm long. The furnace is equipped with a C450 electronic controller, allowing up to 10 programs with up to 20 steps per program to be set.
3.3. Tube furnace with a maximum temperature of 1200 °C (R 50/500/12 C450, Nabertherm GmbH, Germany).
The furnace operates with work tubes with an outer diameter of up to 50 mm and a length of 670 mm, and has a heating zone 50 cm long; the heating zone in which the temperature is controlled to within ± 5°C of the set value is 15 cm long. The furnace is equipped with a C450 electronic controller, allowing up to 10 programs with up to 20 steps per program to be set.
4. X-ray Fluorescence Spectrometer
The total reflection X-ray fluorescence (TXRF) spectrometer, model S2 PICOFOX 400 (Bruker, Germany), is a modern, high-quality spectrometer operating under atmospheric conditions for the qualitative and quantitative elemental analysis of samples with various matrices. The instrument’s X-ray source (X-ray tube) has a Mo anode with a power of 50 W. Cooling is by air. The X-ray optics include a multilayer monochromator, and the detector is an SDD with Peltier cooling. The system is equipped with an autosampler for quartz and acrylic discs with a diameter of 30 mm.
This instrument is used for the multi-element analysis of impurities in samples in the form of liquids and suspensions. It is suitable for elements with an atomic number above 20 (macro- and microelements, and traces at ppm level) and covers the concentration range from 10 ppb to 10% for the elements measured. Simple calibration with an internal standard is possible. The method is applied in the analysis of samples of various origins – water, soil, ash, solutions, graphite powders, biological fluids, etc.
Access to the Laboratory of Inorganic Synthesis
The Laboratory of Inorganic Synthesis is part of the research infrastructure of the National Centre of Excellence “Mechatronics and Clean Technologies” and is located on the Geo Milev campus. Requests for access and for joint research are therefore handled centrally — see Contact. In addition, a full overview of the Centre’s other laboratories is available on the Infrastructure and Laboratories page.
The inorganic synthesis equipment was set up under project BG16RFPR002-1.014-0006, funded by the Research, Innovation and Digitalisation for Smart Transformation Programme 2021–2027, co-funded by the European Union through the European Regional Development Fund.