Laboratory for Additive Technologies, Functional Coatings and Components for Mechatronic Systems

Laboratory for Additive Technologies, Functional Coatings and Components for Mechatronic Systems

The laboratory carries out studies of the corrosion resistance of metals, alloys and coatings under artificial atmospheric and electrochemical conditions, as well as thermal analyses of materials. It is equipped with a chamber for accelerated corrosion testing to international standards, electrochemical analysis systems and instrumentation for differential thermal (TGA-DTA) and differential scanning calorimetry (DSC) analysis.

Description of Activities

  • Corrosion testing of: ferrous and non-ferrous metals, alloys, composites and products made from them; coatings – organic, inorganic, metallic and hybrid; analysis of the results and assessment of the intensity of corrosion damage.
  • Differential thermal analysis (TGA-DTA).
  • Differential scanning calorimetry (DSC)
Workstation with a laptop and a monitor showing graphs, an electrochemical cell with electrodes and a potentiostat
Woman in a purple lab coat pressing buttons on the control panel of a large white test chamber

Description of the Service

Corrosion studies under artificial atmospheric conditions

The laboratory applies both standardised methods and methods developed in-house for accelerated corrosion testing and for testing in model and service environments.

The chamber enables testing of the corrosion resistance of materials and coatings to the following standards: ISO 9227; ISO 6270-2, IEC 60068-2-52; IEC 60068-2-11; ASTM B117.

Electrochemical studies of metals, alloys, composites and coatings

The laboratory also carries out electrochemical corrosion tests, which provide information on the corrosion behaviour of materials within a short period of time. Data are obtained on the main electrochemical characteristics (Ecorr, Ept, Epr, icorr, βa, βc and R), as well as a graphical representation of the results.

Differential thermal analysis (TGA-DTA) involves the simultaneous recording of changes in the mass of a test specimen (TG) and the differential temperature (DTA), accompanied by changes in the rate of the thermal reactions (DTG), for the respective temperature intervals (T) over time.

The following can be determined:

  • The thermal behaviour of the test specimen or a series of test specimens in a programmed operating mode, including data on:
  • the temperature intervals of transformation of the various phases of the test specimen;
  • recording of the intermediate mass losses at the individual stages and of the total mass losses at the end of the thermal decomposition process of the test specimen;
  • calculation of the dependence dm/dT = f(t) (DTG) and determination of the inflection points of the reactions that have taken place;
  • Phase transition temperatures;
  • Thermal stability of the test specimen;
  • The mechanism of the thermal behaviour of the test specimen: dehydration, decomposition, phase transition, reduction and oxidation reactions, etc., depending on the nature of the substances and the choice of specific experimental conditions;
  • The kinetic parameters of the decomposition process of the test specimen;
  • Construction of phase diagrams;
  • Comparative characteristics of the substances.

Differential scanning calorimetry (DSC)

Recording of differences in heat flow as a function of time, ΔH = f(t)

The following can be determined:

  • Amount of heat released (absorbed) during a given process;
  • Heat of reaction;
  • Specific heat capacity of the test specimen;
  • Heat of phase and chemical transformations;
  • Heats of wetting;
  • Kinetic and thermodynamic parameters of phase and chemical transformations.
Two men looking at graphs on a laptop and monitor in a laboratory, with a scientific instrument behind them

Equipment

Cyclic salt fog corrosion test chamber Q-FOG CCT/1100, Q-LAB

• Usable working volume with the lid closed: 800-1200 litres;

• Humidity of the test environment up to 95-100%;

• Programming of cyclic tests with user-defined modes and parameters;

• Built-in salt solution reservoir with a capacity of 120 litres;

• Total load capacity of the chamber (total weight of the test specimens) over 500 kg;

• Maximum atomisation temperature  + 60oC; maximum forced-air drying temperature not less than + 70oC;

• Atomisation pressure control device with a range of not less than (70 – 170) kPa;

• Execution of cyclic tests with temperature setting and control at relative humidity of up to 100%;

• Mode control software – Q-Lab Virtual Strip Chart 3.1

Large white Q-FOG test cabinet with its lid open in a laboratory, with a cylindrical tank beside it
Control panel with display and buttons on an open Q-FOG cyclic corrosion test chamber

Potentiostat for the electrochemical study of corrosion characteristics PGSTAT 204, Metrohm Autolab

Technical specifications of the potentiostat:

  • Potential range +/- 20 V;
  • Maximum current +/ – 400 mA;
  • Option to add at least one expansion module for impedance measurement and/or a rotating disc electrode;
  • Corrosion test measuring cell kit – 1 litre, containing an Ag / AgCl reference electrode and standard steel electrodes;
  • Control and data acquisition software – NOVA 2.1.8
AUTOLAB potentiostat connected to a glass electrochemical cell with electrodes on a laboratory bench

A. Simultaneous thermal analyser (TGA-DTA and TGA-DSC-Cp) STA 449 F3 Jupiter® for analyses in the temperature range from room temperature to 1650°C. Standard single-phase power supply – voltage 230 ± 10 V, 50 Hz

  • The basic system includes a (digital) microbalance with maximum loading at a resolution of 0.1 µg, maximum sample load / measuring range 35 g.
    Proteus basic 8 measurement and analysis software for STA 449 F3 for data acquisition, storage and evaluation under MS WINDOWS. Includes TGA-BeFlat as well as AutoEval for DSC and TGA. Proteus basic 8 media: 1 DVD-ROM. Perpetual licence for Proteus basic 8;
  • Furnace holder with lift;
  • Rhodium furnace, temperature range from room temperature to 1650°C;
  • TG-DTA sample holder/sensor with radiation shield and type S thermocouples, including two Al2O3 99.7 sample crucibles, 0.3ml, temperature range 25 … 1650°C;
  • TG-DSC – Cp sample holder/sensor, also for Cp determination, complete with radiation shield and type S thermocouples. Two sample crucibles GB399205 (PtRh) with lids GB399860 for the temperature range 25 … 1500°C, for Cp determination up to 1500°C, 2 sample crucibles GB399972 (Al2O3) with lids GB399973 for the temperature range 25 … 1650°C;
  • OTS system for the elimination of side oxidation processes by means of a system for trapping traces of oxygen from gases such as argon and helium, creating an ultra-pure inert atmosphere in the working chamber;
  • Cp extension of the Proteus basic 8 software for the determination of specific heat capacity;
  • Proteus basic 8 extension “Advanced DSC-BeFlat for Proteus 8” for DSC correction and high DSC baseline stability;
  • Software (extension of Proteus basic 8) for precise determination of the area of overlapping DSC/DTA peaks and TG mass steps;
  • NETZSCH “Kinetics Neo” kinetics software, academic version for universities and research institutes only. Includes licence – two serial numbers for installation on 2 computers;
  • Proteus basic 8 analysis software extension for the display and evaluation of measurement data from the Aeolos® Quadro mass spectrometer;
  • MFC unit installed inside the instrument for gas control – three gases, with controllable flow rates from 0 to 250 ml/min and a resolution of 1ml/min.

B. Gas analyser module:

  • QMS 403 Aëolos Quadro mass spectrometer for evolved gas analysis, mass range 1-300 amu, power supply 230V, 50 / 60Hz;
  • NIST 17 library for the mass spectrometer;
  • Multichannel temperature controller for temperature regulation (RT … 300°C);
Two analytical instruments connected by a hose on a laboratory table, next to a desk with a laptop and monitor

Gallery

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Access to the Laboratory for Additive Technologies

The Laboratory for Additive Technologies 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 processed centrally — see Contact. In addition, a full overview of the Centre’s other laboratories is available on the Infrastructure and Laboratories page.

The additive technologies equipment was established under project BG16RFPR002-1.014-0006, funded under the Research, Innovation and Digitalisation for Smart Transformation Programme 2021–2027, co-funded by the European Union through the European Regional Development Fund.