ODP 868 makes possible the analysis of samples beyond the limits of classical dilatometry.
Result of over twenty years of R&D of optical instruments for the study of the thermo-mechanical behavior of materials, ODP 868 makes possible the analysis of samples beyond the limits of classical heating microscopy. Its versatility makes of ODP 868 the most innovative tool for production and R&D laboratories for the optimization of all the industrial processes that involve thermal cycles.
The Heating Microscope mode uses a 5Mpix high resolution camera to study the physical behavior of the materials during the industrial firing cycles.
With the Morphometrics applicative it is possible, in real-time during the analysis, to automatically calculate and visualize different characteristic temperatures and parameters selectable by the user.
Capable to analyze samples in a wide range of shapes and sizes (for example a 3mm sample and simultaneously a 10mm sample), ODP 868 can simultaneously analyze up to 8 samples of ISO standard size.
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The HORIZONTAL DILATOMETER mode has 2 HiRes videocameras and is used to study expansion and shrinkage of samples 30 to 60mm long. It is possible to easily determine the most significant parameters like linear thermal expansion, coefficient of thermal expansion (CTE), glass transition temperature (Tg) and the dilatometric softening temperature.
Used to study the sintering of materials without significant vitreous phases, can follow contractions of up to 50% with heating rates up to 100°C/min. For samples that melt, a disposable holding plate is provided.
The whole measuring system is thermostated and thermally isolated from the furnace chamber.
The VERTICAL DILATOMETER mode has 2 HiRes videocameras and is used to study expansion and shrinkage of samples less than 20mm, placed vertically in the furnace chamber. It is possible to follow the sintering process of materials that present contractions up to 100% with heating rates up to 100°C/min. The development of vitreous phases does not interfere with the test result because the top of the samples is free to move though its lower base interacts with the sample holding plate.
FLEXIMETER and ABSOLUTE FLEXIMETER modes, through 3 high resolution independent cameras, enable non-contact bending measurements simulating real industrial heat treatments in order to optimize manufacturing processes of ceramic products as well as have a better and deeper understanding of the materials.
In absolute fleximetry mode the 3 cameras allow to measure simultaneously the sample position in three different points (TA patent), removing the need of a correction curve.
The bending experiments can be carried out on samples 80-85mm or 25-30mm long and it is possible to:
- analyze bending caused by the difference in thermal expansion between coupled materials (i.e.: body and a glaze)
- determine coupling temperature (formerly done with a Steger tensiometer);
- measure bending caused by the difference in sintering behaviour between several coupling materials (i.e.: glaze, engobe and ceramic body);
- measure bending during cooling, caused by the volume variation of the glassy phases;
- study pyroplastic deformation and speed of deformation occurring in the material at high temperature due to its weight;
measure bending caused by absorption of water on one face of the green material.
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ODP 868 |
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| Optical measuring system | Optical bench with 4 independent optical measuring systems, each equipped with a high-resolution camera and fully automated focus |
| Operating modes | Heating microscope, optical dilatometer both vertical and horizontal, optical fleximeter and absolute fleximeter |
| International Standards | ASTM D1857, CEN/TR 15404, BS 1016:Part 15, CEN/TS 15370-1, DIN 51730, IS 12891, ISO 540, NF M03-048 |
| Sample displacement | Bidimensional |
| Sample number | From 1 up to 8, depending upon samples sizes |
| Temperature range on specimen | RT – 1650 °C |
| Temperature resolution | 0,2 °C |
| Heating rate | 0,1 – 100 °C/min 200 °C/sec in Flash mode |
| Resolution | 3ppm with ISO Standard sample |
| Sample number | Up to 8 simoultaneously with ISO standard size |
| Sample dimensions: | Up to 85mm (depending upon operating mode) |
| Morphometrics | Height, Width, Contact angle, Height/Width Ratio, Perimeter, Area, Roundness, Eccentricity, Center of mass. More and freely user-selectable also possible |
| Atmosphere | air, oxidizing, reducing, quasi-inert |
| Light source | LED |
| Software | Misura 4 Thermal Analysis software |
With Misura 4 Thermal Analysis software it is possible to define, easily and intuitively, analytical methods comprising an unlimited number of segments of unlimited duration and complexity.
Structured in “Apps”, Misura 4 Thermal Analysis software includes instrument control and data analysis for all the five different operating modes.
HSM App allows to run tests of heating microscopy.
Because of Misura 4’s advanced morphometrical applicative for the image analysis, during the sintering process it is possible to automatically detect: characteristic temperatures (sintering beginning, softening, sphere, half-sphere and melting / fusion), flattening curve, contact angle curve, sample area variation curve, ratio curve between width and height, bloating effects, combustion, theoretical glass viscosity (V.F.T. equation) and, optionally, surface tension (glasses) using the Young-Laplace equation.
The recognition of shapes can be done accordingly to a wide range of international standards or to user-defined parameters and concepts.
All the results, the complete series of original frames and the sample shapes are stored in a database together with analytical parameters in a non-proprietary format file. To validate the integrity of the results, the output file is cryptographically validated and signed.
Through the browser-based interface it is possible to access test files and view all the configuration options, analysis results and archived images and:
- print graphs of single tests;
- export images selecting single or multiple frames;
- generate customized, interactive PDF reports;
- export all images in movie format (.AVI) usable in presentations or video reports;
- re-define standard methods to recognize automatically the characteristic temperatures;
- input key data as glass transition temperature (Tg), dilatometric softening temperature softening temperature, hemisphere temperature in order to calculate theoretical viscosity of materials according to V.F.T. equation;
- store analysis and related data without overwriting the original data;
- validate cryptographically the original data.
Files can be opened in a graphic module providing printing and advanced mathematical functionalities.
Multiple tests can be overlapped on the same graph, and all the curves can be displayed or printed separately or overlapped to other curves, also related to tests performed with other thermal techniques.
It is possible to view all the measured parameters characterizing the softening and melting behavior and the fusibility according to international standards.
Graphs can import data from a large variety of formats (CSV, FITS, NPY, QDP, HDF) and drawn in Misura data sets.
All the graphs have quality and resolution necessary to be edited and to be exported in PNG raster format, PDF or SVG vectorial format.
Furthermore it is possible to open directly and automatically the data archive related to each analysis.
Related graphs
Thermal expansion and CTE curves of aluminium compared to the same curves of steel
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Optimization of the firing cycle of a stoneware body, given a fixed body formulation. The best firing temperature is the temperature at which the given body composition is able to achieve full densification, with no bloating in the minimum time (in this case 1220°C). Firing above this temperature results in a drastic fall of the mechanical properties and arising of deformations, due to bloating caused by bubbles growth inside the body.
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Analysis of coal ashes according to ISO 540 norm.
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A piece of zirconia implant subjected to its industrial sintering cycle; the sample shows an isotropic shrinkage (densification) but no changes in shape.
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Frit for enamel analysed according to ISO 540 norm. The characteristic points of deformation, sphere, hemisphere and flow are automatically detected.
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Flattening curves of ceramic frits. Black curve represents a glassy frit, while red curve represents a crystallizing frit for monoporosa application. After the sintering phase, this curve shows a long plateau indicating that a crystallization is taking place inside the material. As the temperature increases, the material does not behave like a glass but melts with the typical behaviour of a crystalline material.
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Analysis of a fuel ash sample according to DIN 51730 norm. This test is important in power plants, because the maximum temperature of the combustion chamber must be regulated to be always lower than the softening temperature of the ash.
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Thermal expansion of a palladium – silver alloy for dental implants and C.T.E. calculation.
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Thermal expansion and CTE curves of a glaze. The glass transition temperature (Tg) is determined with the tangents method, while the softening temperature (Ts) is identified in correspondence of the peak in the curve. The expansion curve obtained with an optical dilatometer has a wide rising section above the glass transition temperature because the sample is not subject to any pressure. The sharp fall beyond Ts demonstrates that the ends of the sample are rounding off, even though the volume of the material continues to increase as a consequence of thermal expansion, but its length reduces as a result of surface tension.
Related graphs
The ceramization curve of a glass ceramic material is characterized by an initial expansion, followed by a first little shrinkage and the plateau of nucleation of a crystalline phase. After a descending segment in which the glass undergoes an apparent contraction caused by the reduction of the viscosity and a resulting softening of the sample, there is a phase of clear swelling. Crystallization phenomena within the vitreous mass makes the material rigid again.
Related graphs
The state of tension between glaze and body depends essentially on two factors: the relation between their thermal expansion curves and their coupling temperature. The bending curve on a fired glazed piece of tile is fundamental to identify the coupling temperature and also reveals the qualitative level of stress between body and glaze. Combining the flexion curve of the glazed tile with the thermal expansion curves of body and glaze allows a complete quantitative study of the residual stresses. In this case the glaze results under compression.
Related graphs
Enlargement of the most interesting zone of the LTCC sintering curve. An initial shrinkage phase, due to the binder burnout, starts at 292°C and ends at 347°C. After it, the material undergoes a process of low thermal expansion, up to 626°C. This temperature identifies the onset of actual sintering.
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Thermal expansion and CTE curves of Invar. Invar is a Ni-Fe alloy characterized by an extremely low thermal expansion coefficient from room temperature up to 200°C.
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Multi-layer ceramic chip capacitors are the most widely used passive components in electronics. The shrinkage control is very important; the sintering curve of each layer must match in order to avoid delaminating problems.
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The fusibility of continuous casting powders strongly depends on the thermal cycle applied: here is shown the effect of the heating rate on the melting behaviour.
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Fusibility test on a 99.99% gold wire.
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Comparison between raw materials. Each type of clay shows its own characteristic behaviour of thermal expansion, sintering and swelling.
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Sinter-crystallization process of a piece of iron rich glass-ceramic containing slags of steel industry. The sample was pre-treated at 800°C in order to enhance crystal formation, then subjected to 2h dwell at 1080°C. The sintering curve makes clear the densification kinetic and measures a -0.57% contraction at the end of the 2h.
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Sintering study of a single anode layer consisting of Ni-YSZ CerMet (125 microns thick) and on a YSZ electrolyte layer (10 microns thick).
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Analysis of a RDF ashes sample and study of the influence of the heating rate applied (flash heating, 8°C/min, 80°C/min).
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Analysis of a waste ash sample according to ASTM 1857 norm.
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Sintering curves of different mixtures ceramic body (porcelain like)-austenitic stainless steel 316L in oxidizing atmosphere.
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Fusion test on a welding allow. Determination of the melting point and measurement of the contact angle on stainless steel sample holder.
Optical Contact-less Measurement
Optical Contact-less Measurement
The sample is allowed to freely expand/shrink without any interference due to mechanical contact. This results in a more precise determination of specimen’s behaviour when heated/cooled, as well as of the temperature at which the events are detected. Also, the lack of any load on the sample due to the contact with a measuring system enables to extend the analysis well beyond softening point into the melt, and also analyze soft samples that would otherwise be impossible to test.he HiRes CCD videocamera frames the sample up to 14 times a second, enabling an extremely refined image analysis software to automatically determine the characteristic shapes and temperatures necessary to optimize processing parameters for the production of ceramics as well as the processing of metals or the combustion parameters in power plants.
Morphometrix software
Morphometrix software
The evolution of Misura 3 Image Analysis application, Morphometrics can capture up to 14 frames per second making it possible to automatically determine and visualize, in real-time during the analysis, sample’s characteristic shape’s temperatures. The recognition of shapes can be performed accordingly to a wide range of international standards or also by user-defined parameters and concepts.
All the results, the complete series of original frames and the sample shapes are stored in a database together with analytical parameters in a non-proprietary format file.
Thermostatted Optical Bench Housing
Thermostatted Optical Bench Housing
To ensure the ultimate reproducibility and prevent any short-to-mid term drift, regardless of possible temperature fluctuations due to changed environmental conditions, the housing of the optical bench is actively thermostatted with temperature control in three points. The resulting temperature stability within the housing is +- 1°C.
As a further measure, the support of the optical bench is made of thermally stable materials.
High-performance LED source
High-performance LED source
The LED illumination system operates in the blue range. This significatively improves the resolution as it lowers the limit posed by scattering. As a result it is possible to appreciate smaller changes in shape hence determine with a higher level of accuracy the temperatures of characteristic shapes
Fully Motorized Kiln Operation
Fully Motorized Kiln Operation
For completely automated, error-free operations ODP 868’s furnace rests on a motorized stage ensuring the maximum safety for the user
Flash Mode
Flash Mode
Designed to reproduce the industrial processing conditions, it allows to increase the furnace temperature to a set temperature and then to automatically introduce the specimen in the kiln.
So to heat the sample in a few seconds with heating rates of up to 200°C/sec like in standard manufacturing processes
100 ° C / min Temperature Heating Rates
100 ° C / min Temperature Heating Rates
Up to the temperature range, ODP 868 allows to program heating rates of up to 100°C, enabling users to study the behavior of materials in conditions virtually identical to those used in today’s most demanding manufacturing processes
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