LPM – Material Preparation Lab
The Materials Preparation Laboratory (LPM) offers infrastructure and equipment for the chemical synthesis of molecular materials and the preparation of devices with organized structure, even at the nanometer scale, for their purification through chromatographic and crystallization techniques, and for subsequent basic characterization, both in solution and in the solid state. The Laboratory therefore allows not only for specific and novel syntheses but also for the manipulation of existing materials to improve their performance, processability, or chemical-physical properties.
- These are some of the activities that can be conducted in the Laboratory:
- synthesis and purification of organic, inorganic, and hybrid materials;
- spectroscopic characterization of materials;
- preliminary characterization of materials through X-ray techniques;
- microscopic characterization (optical, electronic, etc.);
- electrochemical, thermal, and rheological characterization of materials or their precursors;
- preparation of organic, inorganic, and composite membranes;
- assembly of different materials into various types of devices that exploit the functional properties of the materials: preparation of thin and thicker films, monolayers, depositions of films of materials using different techniques.
| Apparatus | Description | |
| Dynamic Light Scatter | The Dynamic Light Scattering instrument allows to measure the size of molecules, nanoparticles, or colloids, typically in the range 0.3 nm – 10 μm. Furthermore, working in Static Light Scattering mode, the instrument allows to estimate the average molecular weight of polymers, between 980 and 2107 Daltons. The available instrumentation includes, in addition to the DLS station, the software and hardware for data acquisition and processing. | |
| Dynamic-Mechanic Analyzer | The dynamic-mechanical analyzer is used to study the mechanical properties of solid materials, in particular polymer films and membranes (materials with moduli from 10E3 to 10E12 Pa). It allows measurements in a temperature range from -150 °C to 500 °C, frequency range 0.01-200 Hz, and force range from 0.0001 to 18 N (amplitude range from ±1 to ±6,000 microns). It has a displacement resolution of 1 nanometer over the entire measurement range (25 mm). | |
| DSC | The Differential Scanning Calorimetry (DSC) instrument allows measurement of the heat flow between the sample under test and a reference sample. The available instrumentation includes a double-furnace oven, two heating systems (from -90°C to 550°C using a non-liquid nitrogen intracooler, and one from room temperature to 725°C), a capsule closing press, and software and hardware for data acquisition, processing, and display. | |
| Galvanostat | The Galvanostat/Potentiostat is a compact and modular electrochemical station. The available instrumentation includes a Galvanostat, software, and hardware for data acquisition, processing, and display in paper and digital format. The instrument features a maximum current of ±2 A and a maximum voltage of ±30 V, with an accuracy of ±0.2% on the potential and ±0.2% on the current measurement. Furthermore, it is integrated with a fast acquisition card and an analog linear ramp generator up to 250 KV/second. | |
| Kelvin Probe | The Kelvin probe is used to measure the work function of surfaces. The available instrumentation includes a chamber shielded from environmental electromagnetic interference, software and hardware for data acquisition, a motorized sample translator, a manual translator, a monitor, and a color video camera. The nominal resolution of the work function measurements is less than 5 meV. | |
| Porosimeter | The iQ MP – XR porosimeter is dedicated to microporous and ultramicroporous materials (whose pores can be determined up to 2.9 Å) thanks to the high degree of vacuum (10-8 torr, turbomolecular pump) and the accuracy of the pressure transducer (full scale 0.1 torr). In addition to automatically managing measurements, data acquisition and processing, the instrument has a vast library of specific models for materials with different chemical nature and pore morphology. | |
| Benchtop X-ray Diffractometer | The benchtop X-ray powder diffractometer (D2 Phaser, Bruker) is capable of analyzing polycrystalline materials sequentially for qualitative and quantitative analysis, both for industrial and research purposes, as well as for structural determinations of new materials. It is a compact, fast, and mobile system, easy to install and ideal for rapid screening and purity checks, even for materials for industrial use. | |
| Glove Box | The instrument allows working in an inert atmosphere (Nitrogen) to prepare samples that cannot be prepared or treated in the presence of oxygen and humidity. The presence of a spincoater integrated into the system allows the production of samples also through this technique. The instrument is also equipped with activated carbon filters that allow the removal of solvent residues, even particularly aggressive, used during preparation to prevent the contamination of the samples or of the instrument purification system. Furthermore, different feed-throughs allow the passage of cables and other types of connections to instruments used inside the glove-box: hotplates, stirrers, scales, and pure gas guns necessary for sample preparation. The glove box endows the users of the infrastructure with the availability of an environment where materials sensitive to oxygen and / or humidity can be prepared, analyzed, modified or simply stored for short periods in a controlled atmosphere. This may be of particular importance, for example, for materials used in the fields of photonics and optoelectronics, or for archaeological finds to be investigated on the STAR beam-lines. | |
| Combined TGA- GC/MS-FT/IR Analytical Workstation | This instrumentation consists of a combination of 3 instruments: TGA (thermal analysis through thermogravimetry), IR spectroscopy (FT-IR) and finally Mass spectroscopy (GC-MS). Among other things, the unique combination of these three instruments (which can also work independently) allows a quick analysis in a single run of any possible thermal degradation of sample of the users of the STAR source. In fact, during beam line analysis, under irradiation, overheating of the sample could compromise its integrity. Not only will the TGA make it possible to immediately determine the thermal stability of the sample, the simultaneous IR and GC-MS analysis on the gases developed during thermal degradation allow to quickly draw conclusions about the exact nature of the decomposition products. With the help of the members of the Materials Preparation and Characterization Laboratory (LPM), it is possible to propose to the users possible modifications to be made to improve the thermal stability of the sample itself. Another important factor is the high compatibility of this instrumentation with the μTomo source, also dedicated to surveys on cultural heritage. In fact, through the analysis of a very small amount of substance (about 2 mg), it is possible to obtain information, in a short time, on the chemical composition of the material under examination and then correlate the latter to the observations obtained from the μTomography, thus obtaining a complete picture both in terms of morphology and of constituents, allowing to propose suitable treatments for the restoration of cultural heritage. The combined TG-MS-IR analysis allows to analyze many types of substances (soils, drugs, glues, rubbers, plastics ...). In fact, during thermal degradation, the gases emitted are analyzed both by IR and GC-MS. The comparison between the obtained spectra and databases allows to identify with high probability the different components of the material under examination, and also to quantify their proportion within the material under study. This also allows the LPM to offer services for third parties. In short, the triad of instruments is perfectly integrated with the LPM laboratory dedicated to the characterization of the materials and their preparation, allowing to determine the thermal properties of the materials, a rapid quality control of the materials prepared by the user and expanding the range of possible analysis services on behalf of third parties. | |
| Contact Angle and Surface Tension Meter | The device is a contact angle and surface tension meter that utilizes the sessile drop and hanging droplet techniques. It consists of a system for measuring out the volume of the drops (up to 4 different liquids) on solid surfaces, in air or in other liquids. The device allows ordinary measurements with drops of 1-16 microliters; in different configuration it can operate on tiny surfaces, up to about 10-3-10-4 mm2, irregular or curved, like single microfibres, hair, etc., with drops up to 20 picolitres, thanks to sample holders and dedicated optics. Static and dynamic contact angle measurements (advancement and recession) can be carried out by swelling and emptying the drop on the flat surface, or by tilting the sample with the drop thanks to a motorized table. This device can support those users of the infrastructure interested in deepening their knowledge of the adhesion characteristics and surface tension of their materials, in sectors such as electronics and composite materials in general. Of particular relevance is the possibility of performing measurements on very limited surfaces, even if not flat, which makes the device particularly useful for samples inhomogeneous in shape and composition. | |
| Film Deposition | The instrument is able to satisfy a wide variety of requests concerning the preparation of samples/devices requiring the deposition of thin films through PVD. The simultaneous presence in the same deposition chamber of thermal type sources and sources that operate through the bombardment of special targets with ion currents (sputtering), allows the deposition of up to 4 different materials in a single operating cycle, with a high saving in terms of machine time and wear of those parts of the instrument responsible for creating the high vacuum required to have a good homogeneity and purity of the films. In addition, the presence of a sophisticated control software allows the automation of the processes that can be carried out overnight or even with remote control. This instrumentation, through the possibility of depositing layers of various materials (metals, oxides, inorganic salts, semiconductors) on objects and supports of various kinds, provides an important support for the manufacture and modification of devices to those STAR users active in the sectors of electronics, optics, photonics, optoelectronics, devices for flexible electronics and photovoltaics, coatings. | |
| Probe MAS-NMR | The multinuclear CPMAS-NMR probe H-X is an advanced accessory for high resolution Nuclear Magnetic Resonance Spectroscopy (NMR) on solid-state materials such as powders, crystalline materials, membranes, etc. It is used in order to investigate structural aspects on an atomic/molecular scale. This accessory represents an important enhancement of a very sophisticated machine (Bruker AVANCE 500 NMR spectrometer) equipped with a superconducting magnet, with resonance frequency of the 1H nucleus of 500 MHz, already present in a III level laboratory (chemistry) of the infrastructure. This equipment is of great help to all those users of the infrastructure interested in receiving detailed structural and dynamic information regarding materials used in various sectors, including mesoporous solids, glass, cements, ceramics, semiconductors, polymers, resins, bones, archaeological finds and biological materials. |
The Laboratory was designed to serve a dual purpose: on the one hand, it serves as the site where samples to be transported to the beamlines receive initial screening and where samples can be prepared, modified, and analyzed in real time, in synergy with the results obtained on the beamlines. This is clearly intended to optimize machine time and assist users who lack the necessary skills and equipment. Furthermore, this laboratory will also offer users the potential for developing materials regardless of their use of the core infrastructure. This is of considerable interest, especially for small and medium-sized users, but it is beneficial to all users given the time saving resulting from developing activities on a single site.
| Service | Description | |
| Measurement of the dimensions of macromolecules or particles | The DLS (Dynamic Light Scattering) technique allows for measuring the dimensions of macromolecules, micelles, and nanoparticles dispersed in solution, also obtaining a quantitative distribution in the case of dispersions of particles of various sizes. In the case of polymers, the determination of the average molecular weight is possible. The areas of application for this type of measurement include all technologies and nanotechnologies that involve the use of polymers or particles. | |
| Service for STAR | The LPM laboratory is the site where samples to be transported to the beamlines receive an initial screening and where samples are prepared/modified in real time, in synergy with the results obtained on the beamlines. This is clearly intended to optimize machine time and assist users who lack the necessary skills/equipment. Furthermore, this laboratory will also be able to offer users the potential for developing materials beyond the core infrastructure alone, an aspect of considerable interest, especially for small to medium-sized users. | |
| Dynamic-mechanical analyses | The dynamic-mechanical analyzer is used to study the mechanical properties of solid materials, particularly polymer films and membranes (materials with moduli from 103 to 1012 Pa). It allows measurements over a temperature range from -150 °C to 500 °C, a frequency range of 0.01-200 Hz, and a force range of 0.0001 to 18 N (amplitude range from ±1 to ±6,000 microns). It has a displacement resolution of 1 nanometer across the entire measuring range (25 mm). The instrumentation allows mechanical analyses to be performed in all conventional deformation modes (bending, tension, shear, and compression), with the possibility of working by immersion with standard solutions. The instrument is managed by software that includes all possible tests (creep, stress relaxation, dilatometry, tensile, compression tests, etc.) and a package for analyzing the collected data, including Time-Temperature Superposition (TTS), as well as the prediction of material relaxation (creep) over time. | |
| Calorimetry | The DSC (Differential Scanning Calorimetry) technique allows for the characterization of the thermal properties of molecular, polymer, metallic, and/or ceramic materials. In particular, it allows for the determination of the enthalpy changes associated with any phase transition (glass transition, mesophase transitions, isotropic transition, melting, crystallization, etc.). The application areas of this type of measurement include all technologies and nanotechnologies that can use liquid crystals, polymers, metals, and/or ceramics. | |
| Thin film deposition | The sputtering technique allows the creation of conductive and non-conductive layers, depending on the type of target used, which can be used in the production of electro-optical devices such as LCD or OLED displays and electrochromic films. The thickness of the deposited layer can vary from a few nm to several microns depending on operating parameters such as the operating gas pressure during the process, the target/sample distance, and the deposition time. In the laboratory, it is also possible to deposit inorganic and volatile organic substances through thermal evaporation. | |
| Porosimetry | The technique allows the characterization of ultra-microporous materials (zeolites, carbonaceous molecular sieves, etc.) using the models (NLDFT, GCMC, QSDFT) best suited to the probe molecule, the nature of the material, and the shape and size of the pores. It is suitable for the use of numerous probe molecules (e.g., H2, N2, CH4, CO2, Ar, Kr, Xe, SF6, etc.), vapors (water, alcohols, aliphatic and aromatic hydrocarbons, etc.), up to 1 bar, at any temperature between 20 and 323 °K. | |
| X-ray diffractometry | X-ray diffraction on microcrystalline powders is a non-destructive analytical method useful for characterizing and studying the structure-property relationships of various classes of chemical compounds, such as molecules of pharmaceutical interest, metal complexes used as catalysts or sensors, and precursors to nanostructured materials. Studying the structure-property relationships of chemical compounds is of fundamental importance in the design phase of molecules with specific chemical-physical properties, or to explain the reactivity observed in similar classes of molecules. Areas of potential use include the pharmaceutical, chemical, biomedical, biotech, composite materials, construction and ceramics, photovoltaic, and cultural heritage sectors. | |
| Substance manipulation in inert atmosphere | Working in an inert atmosphere (nitrogen) to synthesize substances and produce samples that cannot be prepared or processed in the presence of oxygen and humidity is often necessary in various sectors, including photonics and optoelectronics, or to process archaeological finds. The glove box in the LPM laboratory allows this to be done efficiently, thanks also to the approximately 2 cubic meters of available space. The presence of an integrated spincoater in the system also allows samples to be prepared using this technique. The instrument is also equipped with activated carbon filters that allow the removal of solvent residues, even particularly aggressive ones, used during preparation to prevent contamination of the samples or the instrument's purification system. Thanks to the feed-throughs, it is also possible to bring cables and other types of connections inside the glove box for the use of plates, stirrers, scales, pure gas guns and anything else necessary for sample preparation. | |
| Measurement of contact angle and surface energy | The contact angle and surface tension measurement device provided by the laboratory can support those users of the infrastructure interested in deepening their knowledge of the adhesion characteristics and surface tension of their materials, in sectors such as electronics and composite materials in general. Of particular importance is the ability to perform measurements on very small surfaces, even non-flat ones, which makes the device particularly useful for samples with heterogeneous shapes and compositions. | |
| Chemical analysis | In addition to the basic instrumentation for chemical analysis, the laboratory has a combined analytical system consisting of three instruments that can operate individually or in sequence to perform: TGA (thermal analysis by thermogravimetry), infrared spectroscopy (FT-IR), and finally mass spectrometry (GC-MS). The unique combination of these three instruments allows for rapid analysis in a single run. Not only does TGA allow for immediate determination of the thermal stability characteristics of the sample, but the simultaneous IR and GC-MS analysis performed on the gases produced during thermal degradation allows for quick conclusions regarding the exact nature of the decomposition products. By analyzing a very small quantity of substance (approximately 2 mg), information on the chemical composition of materials can be obtained quickly. Combined TG-MS-IR analysis allows for the analysis of a wide range of substances (soil, drugs, glues, rubber, plastics, etc.). During thermal degradation, the gases emitted are analyzed by both IR and GC-MS. Comparison of the obtained spectra with databases allows for the high-probability identification of the various components of the material under examination, as well as the quantification of their proportion within the material. This also allows LPM to offer third-party services. |
| 2025 |
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| 2024 |
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| 2023 |
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Service Laboratories
- LCM – Material Characterization Lab
- LMSV – Modeling Simulation and Visualization Lab
- LPCB – Biological Sample Preparation Lab
- LPF – Physical Prototyping Lab
- LSAM – Advanced Spectroscopy and Microscopy Lab
LPM – Material Preparation Lab
Polo Tecnologico Unical, via Tito Flavio, 87036 Rende (CS)
Attilio GOLEMME
Responsabile scientifico LPM
Professore di II Fascia
Dipartimento di Fisica
a.golemme@unical.it