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EN
This study evaluated the structural changes of Al-Ni-(Fe,Cr,Cu)-Y alloys induced by different cooling states. The aim was to determine the role of Fe, Cr, and Cu addition as well as cooling rate on the structure, hardness and anticorrosion properties of crystalline and nanocrystalline Al-Ni-Y alloys. The impact of the preparation method on the structure of alloys was observed by the broadening of the X-ray diffraction peaks of the alloys in the form of plates, which indicated structure fragmentation at a high cooling rate. The TEM images showed the formation of a structure composed of homogeneously dispersed α-Al nanograins. Phase analysis performed using X-ray diffraction method and Mossbauer spectroscopy revealed that the slowly cooled master alloys were mainly composed of Al23Ni6Y4, Al10Fe2Y, and α-Al phases. The Al10Fe2Y structure was the main Fe-bearing phase in all investigated master alloys. A crystallization mechanism was proposed based on the DTA heating and cooling curves. The pitting corrosion type was identified based on morphology observations after electrochemical tests. Rapid solidification and the addition of chromium and copper improved the microhardness as well as corrosion resistance. The high increase of hardness (289 HV0.1) and corrosion resistance[...]
EN
This article explores the possibility of using the vermiculite-lizardite granular product with 30% of vermiculite content for the potential agronomic application. The vermiculite-lizardite product was obtained by beneficiation of phlogopite mining waste (Kovdor, Murmansk region, Russia). The beneficiation scheme included a hydro separator, a spiral separator, and concentrating tables. The output of vermiculite-lizardite product was about 35%. The effect of roasting temperature on the hydrophysical and agrochemical properties of the vermiculite-lizardite material and the mono-mineral vermiculite was studied. Heat treatment of materials was performed in the laboratory shaft furnace. Based on the differential thermal analysis results, a temperature of 700℃ was selected as the upper limit and the temperature of 400℃ - as the lower limit of the temperature range in order to obtain an expanded vermiculite-reached product containing lizardite. For samples obtained in this temperature range with a step of 25℃, a set of data such as bulk density, water saturation, surface area, volume and average pore diameter, Eh, pH suspensions in water and KCl solution, chemical resistance in ammonium acetate solution buffered at pH 4.65 were obtained. The temperature range of 500-600℃ of the vermiculitelizardite granular product was determined as favorable for agronomic application.
EN
In the work, after preliminary discussion of the complexity of the phenomenon of melting chemical compounds, two basic research methods are presented: calorimetric methods and thermooptical method. The physical basis of the five main calorimetry techniques is now detailed (adiabatic calorimetry, differential thermal analysis – DTA, differential scanning calorimetry with heat compensation – DSC heat compensated, differential scanning calorimetry with heat flow – DSC heat flux and differential scanning calorimetry with temperature modulation – MDSC) and thermo-optical techniques used in phase transitions investigations. The advantages and disadvantages of these methods are shown in numerous examples and the accuracy attainable by the individual measuring techniques is compared.
PL
Żużel wielkopiecowy Calumite jest wykorzystywany w przemyśle szklarskim od dawna. Przyspiesza topienie zestawu, zwiększając tym samym wydajność agregatu topliwego i poprawia ekonomikę wytwarzania szkła. Badania DTA/TG wykonywane dla zestawu szklarskiego o różnej zawartości Calumitu miały na celu poznanie mechanizmu jego działania poprzez określenie zmian, jakie wywołuje w przebiegu kolejnych reakcji pomiędzy komponentami.
EN
Calumite blast furnace slag has been used in the glass industry for a long time. Accelerates the melting of the set, thereby increasing the efficiency of the hot melt aggregate and improving the economy of glass production. The studies of the thermal analysis of the set with different content of Calumite were aimed at learning the mechanism of its operation, by identifying the changes caused by its different presence in the course of subsequent reactions between the components of the set and understanding the essence of its beneficial effects.
PL
Zagadnienie sekwestracji CO2 w betonie w procesie karbonatyzacji nabiera w ostatnim czasie coraz większego znaczenia. Wynika to z faktu, iż coraz częściej zarówno konstrukcja, jak również zastosowane materiały są analizowane pod kątem ich całkowitego śladu węglowego. W artykule przedstawiono wyniki badań procesu karbonatyzacji betonu SCC C30/37 w formie gruzu betonowego frakcji 8 – 31,5 mm w komorze karbonatyzacyjnej przez okres 56, 112 i 168 dni. Próbki zostały poddane analizie spektrofotometrycznej FTIR (Fourier Transformation Infrared Spectroscopy). Następnie próbki badane przez 168 dni poddane zostały analizie termicznej TG/DTA (Thermogravimetric/Differential Thermal Analysis) w celu określenia ilości zaabsorbowanego CO2. Otrzymane wyniki zostały odniesione do maksymalnej teoretycznej ilości zaabsorbowanego CO2 wg normy PN-EN 16757-07.
EN
Issue of CO2 sequestraion in the carbonation process has become a crucial problem. This is due the fact, that construction and applied materials are analyzed in the terems of their total carbon footprint. Resutls of research on carbonation of SCC (Self-Compacting Concrete) C30/37 in the form of concrete rubble, in fraction 8 – 31,5 mm, kept for 56, 112 and 168 days have been presented in the paper. Samples were investigated with FTIR (Fourier Transformation Infrared Spectroscopy) analysis. Next, samples kept for 168 days were analyzed with thermal analysis TG/DTA (Thermogravimetric/Differential Thermal Analysis) to determine the amount of absorbed CO2. The obtained results were referred to the formula for the maximum theoretical CO2 uptake according to PN-EN 16757-07.
EN
The results of studies on the thermal decomposition of potassium chlorate(VII) (PP) and the catalytic effects of copper, iron, nickel, titanium, magnesium, chromium and manganese oxides on the process are presented in this paper. The investigated oxides are ranked according to the magnitude of their catalytic effect; of these, CuO and МnО2 show the best catalytic performance. These oxides reduce the PP decomposition temperature from 919.3 K down to even 825.2 K. The share of the catalytic additive in the composition, required to achieve a desirable thermal decomposition profile, was found to be no more than 0.5 wt.%. The activation energy of the decomposition process was determined, using the modified Freeman and Carroll method for both neat PP and PP supplemented with MnO2; the addition of the catalyst produced a 48.8% decrease in the activation energy of thermal decomposition.
EN
With the use of the differential thermal analysis (DTA), studies of the phase transitions were conducted for 90 of alloys from the quaternary Bi-In-Sn-Zn system and for the constant ratio of Bi:In and Bi:Sn. The studies were conducted for the alloys prepared from the purity metals (Bi, In, Sn, Zn = 99.999 mas. %) by way of melting in a graphite crucible in a glove-box filled with Ar, in which the impurities level was less than 0.1 ppm. After melting and thorough mixing, the liquid alloys were poured out into a graphite test mold. The phase transition temperature data obtained from the DTA investigations were next confronted with those determined from the calculations based on the binary and ternary optimized thermodynamic parameters available in the literature. It was found that the experimental and the calculated phase transition temperatures were in good agreement.
PL
W artykule przedstawiono wyniki badań wpływu naturalnych warunków klimatycznych na destrukcję chemiczną (utlenianie) oraz destrukcję fizyczną powłok poliuretanowych w postaci: pękania, wzrostu chropowatości oraz wykruszania się materiału powłokowego. Oceny procesów starzenia badanych powłok dokonano na podstawie termicznej analizy różnicowej (DTA). Zmiany w wyniku starzenia klimatycznego powłok przyczyniły się do obniżenia wartości temperatury początku ich rozpadu termicznego o około 3,2% w porównaniu do powłoki niestarzonej. Degradację powłok dokumentowała również analiza rentgenograficzna (EDS). Warstwy nawierzchniowe starzonych powłok wykazywały zwiększony stopień utlenienia, co skutkowało wzrostem chropowatości ich powierzchni. Destrukcyjny wpływ naturalnych czynników klimatycznych oraz środowiskowych, na warstwy nawierzchniowe powłok polimerowych potwierdziły również badania mikroskopowe.
EN
The paper presents results of investigations of natural weathering influence on polyurethane coating chemical (oxidation) and physical (cracks, increased roughness, chipping) destruction. An evaluation of coatings aging processes was based on differential thermal analysis (DTA). Changes caused by natural weathering of coatings contributed to decrease of their thermal decomposition onset temperature by 3,2% in comparison with not aged coating. Likewise, X-ray analysis (EDS) documented degradation of the coatings. Surface layers of the aged coatings showed increased oxidation degree which caused their surface roughness increase. Also microscopic examination confirmed destructive effect of natural climatic factors on the surface layers of polyurethane coatings.
PL
Analiza termiczna, jako grupa metod analitycznych, umożliwia pomiar zmian szeregu właściwości fizycznych i chemicznych materiałów w funkcji temperatury i czasu. Dzięki różnorodności jej odmian stanowi niezwykle przydatne narzędzie badawcze oraz znajduje szerokie zastosowanie w wielu dziedzinach nauki, a w szczególności w analizie chemicznej substancji.
EN
Thermal analysis is a group of analytical methods which are capable of measuring changes in a number of physical and chemical properties of materials as a function of temperature and time. Because of the diversity of its variety it is an extremely useful research tool and it can find broad applications in many fields of science, and in particular in the chemical analysis of substances.
PL
Analiza termiczna - jako grupa metod analitycznych - umożliwia pomiar zmian szeregu właściwości fizycznych i chemicznych materiałów w funkcji temperatury i czasu. Dzięki różnorodności jej odmian stanowi niezwykle przydatne narzędzie badawcze oraz znajduje szerokie zastosowanie w wielu dziedzinach nauki, a w szczególności analizie chemicznej substancji.
EN
Thermal analysis is a group of analytical methods which are capable of measuring changes in a number of physical and chemical properties of materials as a function of temperature and time. Because of the diversity of its variety is an extremely useful research tool and it can find broad applications in many fields of science, and in particular in the chemical analysis of substances.
EN
This paper shows preliminary thermal analysis of 6 polymer materials which are commonly used or can be used as models for precision casting. Thermal analysis was carried out with use of derivatograph and allowed to determine two fundamental properties of examined materials - their phase transition during heating to the temperature of 800⁰C and mass of dry residue after burning which can be used to evaluate polymer residues remaining in the casting mould cavity. The subject of this paper is related to increasing participation of rapid prototyping methods in casting with use of printed models. Determination of changes in materials, in particular their linear and cubical expansion and analysis of dry residue after burning in casting mould cavity is extremely important for the construction of form crust and surface quality of casting. A problem is to design a polymer-based casting model which allows non-residue burning and simultaneously causes no cracking of ceramic form during heating.
EN
Thermo-physical properties are the critical input parameters in computational models of solidification and casting simulations. In thermodynamics, the enthalpy is quotient of thermodynamic potential of a system, which can be used to calculate the useful work obtainable from a closed thermodynamic system under constant pressure. Differential thermal analysis has been used to study melting and solidification paths in the cobalt based superalloy FSX-414. The temperature enthalpy curve was determined from differential thermal analysis curves obtained from solidification curves. A solidification simulation of a cobalt base multi-component alloy casting was carried out to predict cooling and shrinkage porosity in the casting of a turbine engine vane segment. The effect of latent heat on the heat transfer calculation was considered by enthalpy method.
PL
Do badania zachowania się różnych substancji podczas ogrzewania stosuje się metody termoanalityczne, a w szczególności różnicową analizę termiczną (DTA), różnicową kalorymetrię skaningową (DSC) i termograwimetrię (TG). Metody analizy termicznej są niezastąpione jako cenne źródło informacji o temperaturach przemian fazowych, temperaturach rozkładu i o produktach rozkładu, podczas gdy inne metody kalorymetryczne umożliwiają pomiar ilości ciepła biorącego udział w tych przmeianach. Metody termoanalityczne dostarczają ponadto informacji m.in. o zmianie masy próbki, jej rozszerzalności cieplnej lub o innych właściwościach fizycznych badanej substancji, ulegających zmianie podczas ogrzewania.
EN
For the study of reactions of different substances during heating thermoanalytical methods are used, especially differential thermal analysis (DTA), differential scanning calorimetry (DSC) and thermogravimetry (TG). The methods of thermal analysis are indispensable as sources of knowledge on temperatures of phase transitions, temperatures of degradation and on degradation products, whereas calorimetric methods enable measurement of amount of heat taking part in these transformations. Moreover the thermoanalytical methods provide among others, the information on change of a sample mass, its thermal expansion or other physical properties of a studied substance, which are changed under heating,
16
Content available remote The effect of copper concentration on the microstructure of Al-Si-Cu alloys
EN
In the metal casting industry, an improvement of component quality depends mainly on better control over the production parameters. In order to gain a better understanding of how to control the as-cast microstructure, it is important to understand the evaluation of microstructure during solidification and understanding how influence the changes of chemical concentration on this microstructure. In this research, the effect of Cu content on the microstructure and solidification parameters of Al-Si-Cu alloys has been investigated. Thus, the thermal analysis of the alloys is used to control of aluminum casting process. The effect of different Cu content on solidification parameters such: aluminum dendrites nucleation temperature (TLiq, Liquidus temperature), á+â eutectic nucleation temperature (TE(Al+Si)N), Cu-rich eutectic nucleation temperature (TAl+Cu), solidus temperature (Tsol), solidification range (ÄTs) has been studied in liquidus region. Influence of Cu content on the microstructure has been carried out. The principle observation made from this work ware that as copper concentration is increased the liquidus and solodius temperature decried. In addition to this it was observed that increase a Cu content from 1 to 4 wt % caused reduce of the secondary dendrite arm spacing and increase the grain size.
EN
Glasses with composition 50 GeO2-(45 - x)PbO-5 PbF2-x LnF3 (Ln = Nd or Sm, x = 0.2 and 2 mol%) were synthesised in the bulk form. Phase profiles and temperature characteristics were measured by differential thermal analysis (DTA); glass transition temperature Tg, as well as the b-PbF2 Tb and oxide glass crystallisation Tc temperatures have been derived for each individual system. A study of optical properties (absorption, emission) of the PbF2-Nd3+ and PbF2-Sm3+ was carried out. The oscillator strengths were obtained for several optical transitions and they have been used to calculate phenomenological intensity parameters W2, 4, 6. The probabilities of radiative transitions from fluorescent levels of Nd3+ and Sm3+ ions, as well as branching ratios and radiative lifetimes, were estimated on the basis of the Judd-Ofelt framework. The fluorescence dynamics of studied systems was measured. Experimental lifetimes were compared and discussed with those obtained with the Judd-Ofelt theory.
18
Content available remote Compatibilty studies of explosives using MAKRODTA 550-EX apparatus
EN
The most common method for compatibility determination of explosives is so called Reactivity Test performed using Vacuum Stability Test device. This method does not allow neither gaining of detailed information about the origins of possible incompatibilities of studied mixtures nor determination of volatile substances. For the above mentioned reasons utilization of device that would be able to measure samples of tens or even hundreds of miligrams appears as a good idea. One of such devices is DTA 550-Ex developed at our site.
PL
Metody termiczne umożliwiają badanie przebiegu ważnych procesów, jakim mogą podlegać podczas ogrzewania ciał stałe : reakcji rozkładu utleniania, redukcji oraz topnienia, krystalizacji i innych przemian fazowych.
20
Content available remote Badania termiczne związków kompleksowych
PL
W części pierwszej niniejszej pracy przedstawiono w skrócie metody termoanalityczne stosowane w badaniach związków kompleksowych: termograwimetrię (TG), termiczną analizę. różnicową (DTA), różnicową kalorymetrię skaningową (DSC), termomagnetometrię, termodylatometrię, termodyfraktometrię, a także niektóre metody łączone analizy termicznej, stosowane w badaniach gazowych i stałych produktów reakcji rozkładu termicznego. W części drugiej omówiono, w oparciu o dane literaturowe, czynniki wpływające na trwałość termiczną związków kompleksowych, a w szczególności wpływ metalu centralnego, ligandów i kationów sfery zewnętrznej kompleksu. W części trzeciej podano przykłady zastosowania reakcji rozkładu termicznego związków kopleksowych w analityce, np. do wyznaczenia charakterystycznych temperatur suszenia lub prażenia osadów w grawimetrycznych metodach oznaczania, a także do ilościowego oznaczania pierwiastków, w szczególności metali alkalicznych pojedynczo bądź obok siebie. Przedstawiono też możliwości stosowania rozkładu termicznego kompleksów do otrzymywania związków chemicznych, których synteza na innej drodze jest trudna lub niemożliwa.
EN
In the first part of the publication the thermoanalytical methods used in the studies of the complex compounds are presented: thermogravimetry (TGA), differential thermal analysis (DTA), differential scanning calorimetry, thermomagnetometry, thermodilatometry and some simultaneous methods of thermal analysis applied in studies of gaseous and solid products of the thermal decomposition reactions. In the second part, effect of central metal atoms, ligands and outer sphere cations on thermal stability of complex compounds is discussed. In the third part, several applications of the thermal decomposition reactions of the complex compounds in the chemical analysis are summarised, for instance, the determination of the characteristic temperatures of drying or roasting in the gravimetric methods of determination, as well as the quantitative determination of some elements, especially alkali metals. Also, possible applications of thermal decomposition of complexes to obtain chemical compounds which synthesis in the other way is difficult or impossible, are described.
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