Paulina Wiecinska

Thermal degradation of organic additives used in colloidal shaping of ceramics investigated by the coupled DTA/TG/MS analysis

The paper presents the analysis of thermal decomposition of selected organic additives, which are commonly used in shaping of ceramic materials by colloidal methods. Shaping of ceramics requires using different additives which then are burned out during sintering process. For this reason, the knowledge about thermal degradation of organics used, as well as decomposition products, seems to be very important from the application point of view. The analyzed substances were as follows: diammonium hydrocitrate, citric acid, ammonium salt of acrylic polymer, l-ascorbic acid, N,N,N′,N′-tetramethylethylenediamine, and ammonium persulfate. The thermal analysis has been done on the apparatus coupled with mass spectrometer what allowed to observe what types of gasses are released to the atmosphere during heating. The obtained results showed important differences in thermal degradation of organic additives. It was possible to determine at what temperature regions harmful gases like N2O, NO2, or SO2 are released from the organics and which additives can be treated as environmentally friendly.

Characterization of composites containing NiAl2O4 spinel phase from Al2O3/NiO and Al2O3/Ni systems

This paper focused on the characterization of the composites containing nickel aluminate spinel from Al2O3/NiO and Al2O3/Ni systems. The composites were prepared by die pressing of powders and subsequent sintering of green bodies in air atmosphere. Composites were characterized by XRD, SEM, EDS and DTA/TG/MS analyses. The physical properties of the composites were measured by Archimedes method. Quantitative description of the composites microstructure was made on the basis of SEM images using computer image analysis. The XRD studies and SEM observations of composites confirmed the presence of two phases Al2O3 and NiAl2O4 in the whole volume of samples from both systems. Spinel phase was evenly distributed throughout the volume of the material. Morphology of NiAl2O4 obtained from both systems was characterized by the presence of voids. The DTA/TG/MS measurements showed the characteristics of organic binder decomposition and type of gases released to the atmosphere during thermal treatment. Moreover, the DTA/TG analysis showed the temperature of spinel-phase formation for both systems. It was found that the spinel-phase NiAl2O4 formation retards the process of densification. Therefore, it can be concluded that densification of samples with spinel phase depends mainly on the volume of spinel phase in composite material and does not depend on the substrates used to prepare spinel phase. The values of the selected properties of Al2O3–Ni- and Al2O3–NiO-based materials confirmed that the physical properties depend on the type of substrates used in the fabrication of composites. The type of powder influences the open porosity of samples. For composites produced using NiO powder, open porosity is lower than for samples formed with nickel powder.

Monoacryloyl esters of carbohydrates: Synthesis, polymerization and application in ceramic technology

The article presents the interdisciplinary research among organic synthesis, chemistry of polymers and ceramic technology. It presents the synthesis of monoacryloyl esters of fructose and glucose that is 1-O-acryloyl-D-fructose and 3-O-acryloyl-D-glucose, conditions of their polymerization and application in shaping of advanced ceramic powders by the so called gelcasting method. The paper presents the influence of carbohydrate esters on the viscosity of Al2O3 suspensions and microstructure of final ceramic samples. The results showed that synthesized esters of saccharides can play the role of organic monomers able to polymerize in situ and self-cross-linking compounds in gelcasting. The paper presents the proposed structure of polymeric network which is formed from acryloyl ester of glucose during gelcasting process. The paper describes rheological behaviour of slurries composed of synthesized substances and A2O3 powders, wetting angles of alumina substrate by synthesized compounds, differences in glass transition temperatures of polymers and the microstructure of obtained final ceramic samples.

Thermoanalytical studies of the ceramic-metal composites obtained by gel-centrifugal casting

Composite material with a gradient concentration of the metallic phase was prepared by the novel gel-centrifugal casting method. This method combines the consolidation of powders by the centrifugal force with the reaction of radical polymerization of an organic monomer which simultaneously proceeds within the composite slurry. The combination of the centrifugal casting with gel-casting permits production of ceramic–metal composites, including materials with a gradient distribution of metallic particles in a ceramic matrix. Special attention was paid to the thermal analysis of the composite Al2O3–Ni green bodies and the binder used in the fabrication of the material. The experiments were performed on the simultaneous thermal analyzer coupled with the mass spectrometer. The measurements were carried out in air and the inert atmosphere (argon) what allowed to determine the effects characteristic for organic binder decomposition and type of gases released to the atmosphere during thermal treatment. The measurements allowed also to establish the sintering program of the green composite samples and evaluate whether harmful gases are released to the atmosphere. The thermal experiments were complemented with physical and structural measurements, including X-ray diffraction and scanning electron microscopy.

Colloidal processing of Al2O3 and BST materials: Investigations of thermal stability and decomposition of green bodies

The paper presents the analysis of thermal stability and decomposition of Al2O3 and (Ba,Sr)TiO3 green bodies as well as commercially available organic additives which are used in shaping of ceramics by colloidal processing. The first analyzed ceramic material was Al2O3 green body obtained by gelcasting. The second examined material was elastic ceramic–polymer composite based on ferroelectric powder Ba0.8Sr0.2TiO3 with NiO obtained by tape casting method. This flexible and durable material is characterized by high value of dielectric constant and finds the application in devices operating at very high frequencies up to sub-THz. Most organic additives are indispensable just in forming step but must be then eliminated in order to obtain pure ceramic phase, additionally some of them have to be stable in a wide temperature range. The analyzed organic substances were as follows: 2-carboxyethyl acrylate, SYNTRAN 8250, DURAMAX D-3005, DURAMAX B-1000. The DTA/TG measurements coupled with mass spectrometry allowed to gain new knowledge concerning degradation of selected organic additives, thermal stability of ceramic–polymer composite and type of gases released from samples during thermal treatment.

Colloidal processing of Al2O3 and BST materials

The paper presents the analysis of thermal stability and decomposition of Al2O3 and (Ba,Sr)TiO3 green bodies as well as commercially available organic additives which are used in shaping of ceramics by colloidal processing. The first analyzed ceramic material was Al2O3 green body obtained by gelcasting. The second examined material was elastic ceramic–polymer composite based on ferroelectric powder Ba0.8Sr0.2TiO3 with NiO obtained by tape casting method. This flexible and durable material is characterized by high value of dielectric constant and finds the application in devices operating at very high frequencies up to sub-THz. Most organic additives are indispensable just in forming step but must be then eliminated in order to obtain pure ceramic phase, additionally some of them have to be stable in a wide temperature range. The analyzed organic substances were as follows: 2-carboxyethyl acrylate, SYNTRAN 8250, DURAMAX D-3005, DURAMAX B-1000. The DTA/TG measurements coupled with mass spectrometry allowed to gain new knowledge concerning degradation of selected organic additives, thermal stability of ceramic–polymer composite and type of gases released from samples during thermal treatment.

Al2O3/Ni functionally graded materials (FGM) obtained by centrifugal-slip casting method

The fabrication and the characterization of Al2O3/Ni composites with a gradient distribution of the Ni particles are reported. The composites have been obtained by centrifugal-slip casting and subsequent sintering and had the shape of a hollow cylinder. TG/DTA analysis was done for the nickel powder with the addition of the dispersant used in centrifugal-slip casting as well as for the composite green body. The measurements were performed in two atmospheres: argon and the mixture of argon and hydrogen (1:1). Additionally, coupling the thermobalance with the mass spectrometer allowed to determine type of gases released from the samples during thermal treatment. The morphology and chemical composition of the produced composites were analyzed using a scanning electron microscope equipped with an EDS detector. Interface between alumina and nickel was described. Moreover, the X-ray diffraction was made. The stereological analysis confirmed that the nickel particles are distributed in the composite in a gradient way.