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Laboratory physico-chemical analysis and material innovations


 

 

Head of laboratory:   Ing. Alberto Viani, Ph.D.

                                        viani@itam.cas.cz

                                        +420 567 225 308

 

Members of laboratory: Mgr. Radek Ševčík, Ph.D.

                                                     Ing. Konstantinos Sotiriadis, Ph.D.

                                                     Mgr. Petra Mácová

                                                     Eva Pažourková

                                                     Ing. Milan Svoboda

Chemical laboratory

 

This laboratory is dedicated to sample preparation and general chemical analysis. It is equipped with instruments for milling, chemical attack, physical characterization (e.g. pH, conductivity, sieving, weighting), titration, microwave digestion, ultrasonic bath, muffle furnace for the synthesis of compounds, etc.

 

 

Bruker D8 Advance diffractometer (Bragg-Brentano theta-theta geometry)

Specifications

·        Ni-filter

·        LYNXEYE Position Sensitive Detector

·        rotating sample stage

·        multi-purpose sample stage for massive samples

·        Euler cradle for microstructural measurements

·        parallel beam optics

Applications

This is the technique of election for investigating solid samples. It’s mainly used with samples in form of powders. Sample preparation can be accomplished with our crushing/milling equipment. Typical use is execution of qualitative analysis: phase identification in polycrystalline samples, identification of minerals in geological samples, detection of polymorphs in pharmaceutical samples, the determination of impurities in a pure phase (down to 0.1 weight %).

More advanced data treatment (Rietveld method) allows also to perform powder diffraction quantitative analysis: Quantification of phases into powdered samples, like minerals in geological samples, in raw materials, in industrial ceramics, refractories, cements, mortars. The technique is suitable for the quantification of non-crystalline component (amorphous) as well.

X-ray Crystallography: investigation of the crystal structure of known and unknown phases.

Crystallite size and residual strain: the determination of mean dimension of diffraction domains (crystallites) allows for the characterisation of samples undergoing thermal or mechanical treatments.

Texture analysis: the reconstruction of the distribution of orientation of the crystallites in polycrystalline samples, allows for the reconstruction of the sample microstructure. Specific orientation of crystallites develops as a result of industrial production processes (as for many metallic parts) or by action of external or internal agents. Examples are the way in which carbonate crystals grow in molluscs shells, the way in which crystal habit develops in rocks subjected to oriented pressure (metamorphism), the way in which crystals grow within processed technical ceramic bodies or metals.

Grazing incidence: with this technique the identification of phases deposited at the surface of solid samples in form of films in the range 10-200nm, and their thickness, can be investigated. Typical field of application are materials for electronics, functional materials.

Peculiar to the last two methods is that they are non destructive, the sample is analysed without preparation with the aid of specific sample stages.

Typical output of Rietveld refinement of X-ray powder diffraction data. On the lower half of the picture, the original spectrum (in blue) and the refined one (in red) together with the difference between the experimental and the calculated (gray line) and markers corresponding to reflection peaks of the phases in the sample, are depicted. Quantification of all the phases including the amorphous (non crystalline) fraction is reported on the bottom right.

 

 

 

SEM FEI Quanta 450 FEG (scanning electron microscope)

Specifications

·        high resolution Schottky field emission emitter

·        accelerating voltage: 200 V to 30 kV

·        magnification: 6 to 1000000x

Detectors

·        Everhardt Thornley SED (secondary electron detector)

        Backscattered electron detector

·        Large Field Low vacuum SED (LFD)

·        Gaseous SED (GSED) (used in ESEM mode)

·        IR camera for viewing sample inside the chamber

·        EDS spectrometer

         Cathodoluminescence detector

         EBSD detector

Main features

The microscope is equipped with the last generation emitter, allowing for a stable flux of electrons and high intensity. This is a versatile instrument that can be used to investigate a wide range of specimens ranging from inorganic to organic. Although the best results are obtained with a superficial conductive coating of few nanometers (usually gold or carbon), it’s possible to characterize even non-conductive samples, avoiding any treatment.

Working under low vacuum and ESEM enables charge-free imaging and analysis of non-conductive and/or hydrated specimens.

Applications

NanoCharacterization: Metals & alloys, oxidation/corrosion, fractures, failure analysis, welds, polished sections, magnetic and superconducting materials. e.g. ceramics, composites, plastics, films/coatings, geological sections, minerals, soft materials (polymers, pharmaceuticals, filters, gels, tissues, plant material), particles, porous materials, cements, fibers.

In situ NanoProcesses: hydration/dehydration; wetting behaviour/contact angle analysis; oxidation/corrosion; tensile (with heat or cooling); crystallization/phase transformation.

The EBSD detector, allows for accomplishing micro-diffraction on the specimen’s surface, thus, identify the nature of crystalline phases within the sample and perform texture analysis: the reconstruction of the distribution of orientation of the crystallites in polycrystalline samples, allows for the reconstruction of the sample microstructure. Specific orientation of crystallites develops as a result of industrial production processes (as for many metallic parts) or by action of external or internal agents. Examples are the way in which carbonate crystals grow in molluscs shells, the way in which crystal habit develops in rocks subjected to oriented pressure (metamorphism), the way in which crystals grow within processed technical ceramic bodies or metals. The EDS detector allows for investigating the chemical composition with high spatial resolution.

 

 

Examples from our SEM investigations: top left: spherical particle in fly ashes from combustion of coal; top right: detail of crack failure in steel; bottom left: glass fibres in fibre cement composite construction material; bottom right: EBSD pattern of silicon wafer.

 

ICP - OES Spectroblue

Applications

ICP-OES is a widely used analytical technique for the determination of major and trace elements. The ICP-OES technique has been applied to the analysis of a large variety of agricultural and food materials, like trace metals in beer and wine; trace elements in biological systems.

ICP-OES has become an important tool in the area of biological and clinical applications. Determinations by ICP-OES of essential, toxic and therapeutic trace elements are important in the medical research laboratories as well as in the clinical and forensic lab environments.

Geological applications of ICP-OES involve determinations of major, minor and trace compositions of various rocks, soils, sediments, and related materials.

Environmental analysis, analysis of drinking and waste water, soils, sludge, plants, foods.

ICP-OES is used widely for the determination of major, minor and trace elemental constituents in metals and related materials. The technique is used for analysis of raw materials, production control, and quality control for final products as well as in the developmental lab environment.

Analysis of organic solutions by ICP-OES is important not only for analysing organic-based materials such as petroleum products but also for a wide variety of other applications. lubricating oils for trace metal content is one of the more popular applications for organics analysis by ICP-OES. Some other applications include determination of lead in gasoline; determination of Cu, Fe, Ni, P, Si and V in cooking oils; analysis of organophosphates for trace contaminants; and determination of major and trace elements in antifreeze.

Standard sample preparation procedure is accomplished with a microwave digestion unit allowing for excellent reproducibility.

 

IEC (Ion Exchange Chromatography) DIONEX

Specifications

autosampler with 49 positions

anions – fluoride, chloride, bromide, nitrite, nitrate, phosphate, sulphate

cations – lithium, sodium, ammonium, potassium, magnesium, calcium

Applications

Ion chromatography system is designed to perform analysis of specific anions and cations in liquid samples. Common applications are: qualitative and quantitative determination of water soluble salts from a wide range of solid samples, such as bricks, mortars, cements and chemical analysis of water samples.

DXR Raman microscope

Specifications

the wide spectral range with measurements down to  50cm-1

objectives Olympus: 10x, 20x, 50x, 100x

lasers: 532 nm (10 mW, solid-state, diode-pumped); 633 nm (8 mW, HeNe); 780 nm (24 mW, high brightness diode)

 

Applications

This spectroscopic technique allows for identification of specific compounds within a wide range of specimens, organic and inorganic. With the aid of the optical microscope the laser beam can be focused down to 0,6 µm, thus, onto very small particles. Typical applications include: identification of particulate contaminants, high-resolution depth profiling and subsurface analysis on transparent and semi opaque samples, characterization of coatings, multi-layer laminates, thin films, inclusions and subsurface defects.

Good representation of carbon and silicon molecular backbones provides great differentiation of pharmaceutical and mineral polymorphs as well as differentiation of amorphous and crystalline forms of silicon and different carbon nanomaterials.

Surface areas and subsurfaces can be investigated producing x-y area maps and x-z maps. Measurements can be accomplished through glass and plastic packaging.

 

The figure reports a spectrum obtained using point measurement mode on the elongated crystal depicted in the inset picture. Peaks correspond to Raman bands of aragonite (CaCO3).

 

Infrared Nicolet iN10 microscope with Nicolet iZ10 FT-IR module

Specifications

room temperature DTGS and liquid nitrogen-cooled MCT detectors

transmission, ATR and DRIFT techniques

ATR with diamond crystal inside

DTGS detecto

Applications

This spectroscopic technique allows for identification of specific compounds within a wide range of specimens, organic and inorganic. Measurements can be performed in transmission mode (producing a small pellet containing few mg of powder sample) or in reflection mode (in which the sample surface is simply investigated). Typical applications include: microspectroscopy with identification of compounds and contaminants inside the sample, particle analysis, study of inclusions, investigation of packaging and laminate, coatings, failure analysis. Maps with compound distribution can be produced.

Example of outputs of FT-IR using Micro ATR technique. The chemical map (on the left) show the distribution of calcite (red areas with high concentration of calcite (CaCO3), blue area without calcite) in the selected area of the sample depicted on the right. On the bottom left a typical spectrum showing peaks of calcite is reported.

 

Thermal Analysis (STA 504)

The method is based on the measurement of changes in mass (TG) and heat flow (DTA) simultaneously, as function of temperature. This can be accomplished in the temperature range -160 – 700°C or from room temperature to 1100°C.

 

Applications

Typical applications include: identification of compounds following their thermal decomposition/transformation with temperature (e.g. phases of hydration in mortars nad concrete), and their quantification; determination of decomposition temperatures, glass transition temperature in polymers, calculation of specific heat capacity. Engine oil volatility measurements, filler content, flammability studies, measurement of volatiles (e.g. water, oil), oxidative stabilities, thermal stabilities, catalyst and coking studies, melting/crystallization behavior. The technique is particularly suitable for the analysis of construction, ceramic and geological materials.

In this image, corresponding to a sample of CaCO3, a phase transition is shown as an exothermic peak (up) at about 450°C and the decomposition as an endothermic peak (down) with a weight loss at 750°C. These results allows to determine and quantify the composition of the sample.

 

 

MECHANISM OF DAMAGE OF QUASI-BRITTLE SURFACE LAYER – THE CASE OF PLASTERS FROM THE FAÇADE OF VALTICE CASTLE

CHARACTERISATION OF HYSTORIC MATERIALS- THE CASE OF TAQ-I-KISRA PALACE (IRAQ)


MINERALOGICAL, CHEMICAL-PHYSICAL CHARACTERIZATION OF MINERAL FIBERS AND THEIR INTERACTION WITH THE HUMAN BODY.
 

REACTION KINETICS OF MAGNESIUM PHOSPHATE CEMENTS
 

Determination of optimal burning temperature ranges for production of natural hydraulic limes. (Published paper)
 

ACCURACY OF INTERNAL AND EXTERNAL STANDARD METHOD IN QUANTITATIVE ANALYSIS BY X-RAYS POWDER DIFFRACTION .
 

LONG TERM COMPOSITON OF ALTERNATIVE CEMENTITIOUS BINDERS PRODUCED BY RECYCLING THE PRODUCT OF THERMAL TRANSFORMATION OF CEMENT-ASBESTOS. (Conference extended abstract).
 

INVESTIGATION OF CONTAMINANTS IN STAINLESS STEEL CORRUGATED TUBES

 

Testing of treatment effects of nano sols on selected porous historic materials and link it to the paper

 

Study on mechanical properties of lime-based pastes with additions of metakaolin and brick dust

Laboratory porosimetry

Laboratory studies the structure of porous materials , identifying physical characteristics and behavior of materials, particularly materials of historic structures.

Mercury porosimeter Autopore IV 9500

  • Characterizes a material’s porosity by applying various levels of pressure to a sample immersed in mercury. The pressure required to intrude mercury into the sample’s pores is inversely proportional to the size of the pores. This is called mercury porosimetry, or often, “mercury intrusion.”
  • Measurements in the pressure range from 0-228 MPa
  • Range: pore diameter 5nm - 360 micron

 

Helium pycnometer AccuPyc II 1340

  • Determination of density
  • Sample is inserted into the chamber of known volume, helium with certain pressure is admitted into the reference chamber and then into the measuring chamber, where it simultaneously measures the pressure of peer pressure ratio and volume to calculate the density matrix of material.
  • Sample size of 0,01 to 350 cubic centimeters

 

Asap 2020

  • Determination of surface area and distribution of pore size of solid materials

  • Device uses the principle of physical adsorption to obtain adsorption and desorption isotherms and to obtain information about the nature of the investigated material

  • Two fully automated degassing systems with controlled heating time

  • Twelve gas supply lines, which are automatically adjustable

  • Software with great flexibility of measured data

 

 

Preparation of samples

Table lapping equipment BROTLAB 1.03.26

  • Using for finishing machining, with this device it´s possible to achieve a high accuracy of dimensions and geometrical shape and surface of the lowest roughness

 

Grinder / Polisher ECOMET PRO 250-300 and 250-300 automatic head Automet

  • Fully programmable grinder / polisher

  • Touch control panel on the console , the possibility of programmed procedures and the Zaxis ( can substitute time for step rate of material removal )

Automatic press for pressing samples SimpliMet 1000

  • Electro - hydraulic system that allows you to define the pressure , temperature of heating and cooling time

  • Molds for pressing for sizes from 25 mm to 50 mm

  • Short cycle time for sample preparation

 

The system for thin slices (saw) Petro Thin

 

 

Device for watering samples in vacuum CAST N' VAC 10000

  • Equipment for simultaneous infiltration and embedding of larger number of samples
  • Includes a vacuum pump with a stable vacuum tank , built-in synchronous motor , pouring equipment , manometer , filter for absorbing moisturei

 

 

Microscopic laboratory

Petrographic polarizing microscope BX41 with transmitted and reflected light

  • Description of the components of the material , size, shape , distribution of individual components, the mineralogical composition

 

Videomicroscopes Hirox KH 7700 with transmitted and reflected light

  • Digital microscope for observation with a large depth of field when placed on a tripod or hand-held
  • Morphology of untreated surfaces
  • Petrographic analyzes of the through - polarized light

 

Stereo Microscope SZX -7

  • Microscope designed for materials science with magnification up to 120x