The thesis describes the relaxation properties of bituminous binders determined in dynamic shear rheometer (DSR). Paving bitumen, polymer modified bitumen (PMB) and crumb rubber modified bitumen (CRmB) were chosen for comparison. In order to describe the effects of ageing on asphalt binders relaxation properties, the laboratory simulation of ageing using RTFOT and 3xRTFOT method was performed. For each binder were simultaneously conducted tests of needle penetration, softening point and elastic recovery. Selected bitumens were used for the production of asphalt mixtures. The low-temperature properties tests (TSRST) were performed for these mixtures, when the results were compared to the relaxation properties of binders determined in the DSR.

The theoretical part of this thesis describes the rheology of bituminous binders, aging of asphalt binders and laboratory methods simulating short and long term aging. The following describes an empirical tests (needle penetration, softening point ring ball method) and functional tests (complex shear modulus and phase angle, dynamic viscosity), which are performed in the dynamic shear rheometer. At the end of this section, laboratory aging of bituminous binders using method RTFOT and method RTFOT + PAV is described in more detail. In the practical part of this thesis, the results of all tests performed on the binders aged using RTFOT + PAV are introduced and compared with results of properties of non-aged binders and binders aged by 3xRTFOT.

During the pressing of powder mixtures to make cemented carbide tools, the degree to which the powder spreads to fill the die and to which it compacts is uncertain. This leads to inconsistent dimensions and densities in the finished product. This performance changes with the composition of the powder, including the amount of pressing agent in the mixture, the particle size distribution and particle shape. One way to quantify the degree to which powder will spread to fill the mold evenly is using the property called 'flowability'. There are several techniques by which flowability can be measured, and each technique does not always give results that are consistent with other techniques. It is, therefore, important to know what technique(s) predict(s) the final behavior of the powder in this application before it is used in quality assurance or to design a process. Additionally, powder size distribution and shape metrics are measured using dynamic image analysis to investigate if there is any relationship between key values of these properties and compaction behavior. In this study, static Angle of repose, Tap Density, Hall flow time and Powder rheometry were benchmarked against each other and against the dimensions of presses and liquid phase sintered tool inserts to understand which technique had the strongest dependence on the compactability, which was defined as the ratio of the tallest dimension in the insert to the smallest. After the study, the results showed that a more extensive particle size distribution improves the compaction properties and that the powders with a higher resistance to a rotating blade tend to have better compaction properties. On the other hand, a clear pattern for the results of all measurement methods and the correlation between the compaction behavior of the carbide tools could not be discerned. In conclusion, the study showed that it is possible to determine a relationship between the results of measurement methods and the compaction behavior of powders. By using simple tests to predict the compactability properties, both money and time can be saved on the research of new, improved powder. Furthermore, the implementation of this study can lead to even better pressing and compactibility properties in the future for cemented carbide tools. / Vid pressning av pulverblandningar för tillverkning av hårdmetallverktyg är det osäkert i vilken grad pulvret sprider sig för att fylla matrisen och i vilken grad det komprimeras. Detta leder till inkonsekventa dimensioner och densitet i den färdiga produkten. Denna prestanda förändras med pulvrets sammansättning, inklusive mängden bindemedel som finns i blandningen, partikelstorleksfördelningen och partikelformen. Ett sätt att kvantifiera i vilken grad pulvret sprids för att fylla formen jämnt är att använda den egenskap som kallas "flytbarhet". Det finns flera tekniker för att mäta flytbarhet, och varje teknik ger inte alltid resultat som överensstämmer med andra tekniker. Det är därför viktigt att veta vilken eller vilka tekniker som förutsäger pulvrets slutliga beteende i denna tillämpning innan den används i kvalitetssäkring eller för att utforma en process. Vidare mäts pulvrets partikelstorleksfördelning och form med dynamisk bildanalys för att undersöka om det finns något samband mellan nyckelvärden för dessa egenskaper och komprimeringsbeteendet. I den här studien jämfördes statisk rasvinkel, tappdensitet, hallflödestid och pulverreometri samt med dimensionerna på pressar och sintrade verktygsinsatser i vätskefas för att förstå vilken teknik som hade det starkaste beroendet på kompatibiliteten, vilket definieras som förhållandet mellan den högsta dimensionen i insatsen och den minsta. Efter studien visade resultaten att en mer omfattande partikelstorleksfördelning förbättrar komprimeringsegenskaperna och att pulver med högre motståndskraft mot ett roterande blad tenderar att ha bättre komprimeringsegenskaper. Vidare kunde inte ett tydligt mönster för resultaten för alla mätmetoder och sambandet på komprimeringbeteendet för hårmetallverktygen urskiljas. Sammanfattningsvis visade studien på att det går att använda sig av mätmetoder för att kunna urskilja ett samband mellan resultaten på mätmetoderna och pulvers kompaktibillitetsegenskaper. Genom att använda sig av enkla mätningar för att kunna förutsäga kompaktibilitetsegenskaper samt komprimeringsbeteende kan både pengar respektive tid sparas. Vidare kan genomförandet av denna studie i framtiden leda till ännu bättre pressnings- samt kompaktibilitetsegenskaper för hårdmetallverktyg.

Today, the focus lies on the state of the environment and how we can choose more sustainable alternatives to oil based materials. One material of interest is microfibrillated cellulose (MFC).The microfibril exhibits interesting properties, which one is its excellent barrier properties, that is expected to come in good use for the conversion to a more sustainable society. It is believed that the use of biobased barriers will increase with these new materials and MFC is showing promising results. But in order to develop the material to its full potential, it is important to investigate how MFC behaves in different situations, which can be examined with rheological measurements. The aim of the thesis is to examine how the rheological properties of suspensions containing MFC are affected by temperature and time storing and how the learning from this work can be used for influencing dispersion properties. Four samples were investigated, containing different amounts of MFC and modified waxy maize starch. The samples were analyzed with a dynamic rotational rheometer (Kinexus Pro +) with a splined cup and bob. The following steps were included in the method development used in this work: sample preparation, the repeatability, rest time and statistical analysis. An oscillatory shear and steady shear measurement was performed on the samples, and selected samples were studied with microscopy. The results show that the temperature has affected the samples. The shear viscosity of all samples decreased with increasing temperature and the samples followed the temperature dependence of Arrhenius' equation. For samples containing MFC, the structure was affected, and the initial viscosity was not recovered. The complex viscosity did also decrease at the beginning to then suggestively increase, creating a stronger network at higher temperatures. With the raised temperature the bonding between the fibrils became weaker, which in turn made the dispersion less viscous. Then, depending on the applied force, the shear viscosity and complex viscosity acted differently. To conclude, both the shear viscosity and the complex viscosity in these dispersions containing MFC are dependent on the temperature and time storing. By the learnings from this work, a method has been developed to understand how to use temperature and storing time to lower the shear viscosity and lower, or increase, the complex viscosity. / Idag ligger det ett stort fokus på miljöns tillstånd och hur vi kan välja mer hållbara alternativjämfört med oljebaserade material. Ett material av intresse är mikrofibrillerad cellulosa (MFC).Denna mikrofibrill besitter intressanta egenskaper, varav en är enastående barriäregenskaper,som förväntas komma till god användning i omställningen till ett mer hållbart samhälle. Det tros att biobaserade barriärer kommer att användas mer i dessa nya material och här visar MFC lovande resultat. Men för att kunna utveckla materialet till sin fulla potential är det viktigt att undersöka hur MFC beter sig i olika situationer, som kan undersökas genom reologiska mätningar. Syftet med arbetet är att undersöka hur de reologiska egenskaperna för suspensioner innehållande MFC påverkas av temperatur och lagringstid samt hur lärdomen från det här arbetet kan användas för att påverka dispersionsegenskaper. Fyra prover undersöktes,innehållande olika mängd MFC och modifierad majsstärkelse. Proverna analyserades med en dynamisk rotations reometer (Kinexus Pro +) med räfflad kopp och bob. Följande steg ingick i metodutvecklingen som användes i detta arbete: provberedning, repeterbarhet, vilotid och statistisk analys. En oscillerande skjuvning och jämn skjuvmätning utfördes på de olika proverna samt att utvalda prover studerades med mikroskopi. Resultatet visade att temperaturen hade påverkat proverna. Skjuvviskositeten för alla prover minskade med en ökande temperatur och proverna följde temperaturberoendet av Arrhenius ekvation. För prover innehållande MFC påverkades strukturen och startviskositeten återficks inte. Den komplexa viskositeten minskade också till en början för att sedan suggestivt öka, vilket skapade ett starkare nätverk vid högre temperaturer. Med en högre temperatur blev bindningarna mellan fibrillerna svagare, vilket bidrog att dispersionerna blev mindre viskösa. Beroende på den applicerade kraften, verkade skjuvviskositeten och den komplexa viskositeten olika. Slutsatsen var att både skjuvviskositeten och den komplexa viskositeten i dessa prover innehållande MFC beroende av temperaturen och lagringstid. Från lärdomen av arbetet har en metod tagits fram för att kunna använda temperatur och lagringstid för att sänka skjuvviskositeten och sänka, eller öka, den komplexa viskositeten.

This doctoral thesis consists of a literature review, presented in two papers, and another six papers describing experimental studies of the influence of different kinds of wax and polyphosporic acid on bitumen and asphalt concrete mixture properties. The literature review should give an extensive description of the field of knowledge concerning wax in bitumen. Effects of wax in crude oil, bitumen and asphalt concrete as well as test methods for studying these effects are described. Theories behind possible mechanisms are also discussed, and commercial wax as additive to bitumen for different purposes included. The experimental parts comprise laboratory studies involving totally five 160/220 penetration base bitumens from different sources, two isolated bitumen waxes, five commercial waxes and one polyphosphoric acid. Asphalt concrete slabs, containing base or modified bitumen were prepared and tested. Binder properties were evaluated using different types of laboratory equipment, such as dynamic shear rheometer (DSR), bending beam rheometer (BBR), differential scanning calorimeter (DSC), force ductilometer, as well as equipment for determining conventional parameters like penetration, softening point, viscosity, and Fraass breaking point. Fourier Transform Infrared (FTIR) spectroscopy and Thin Layer Chromatography (TLC-FID) were used for chemical characterization. The binders were aged by means of the rolling thin film oven test (RTFOT) and pressure ageing vessel (PAV) in combination. Asphalt concrete properties were evaluated at low temperatures using the tensile strain restrained specimen test (TSRST) and creep test at -25°C. Dynamic creep testing was performed at 40°C, as well as complex modulus tests between 0 and 20°C. Binder test results indicated that the magnitude and type of effect on bitumen rheology depend on the bitumen itself, type of crystallizing fraction in the bitumen and/or type and amount of additive used. Bitumen composition was found to be of decisive importance. Adding polyethylene wax or polyphosphoric acid, especially to a non-waxy 160/220 penetration grade bitumen, showed no or positive effects on the rheological behaviour at low temperatures (decrease in stiffness) as well as medium and high temperatures (increase in complex modulus and decrease in phase angle). However, the corresponding positive effects could not be shown in dynamic creep testing (at 40°C) of asphalt concrete mixtures containing these modified binders. Adding FT-paraffin decreased the physical hardening index for all bitumens. Also polyethylene wax and montan wax showed this effect for some bitumens. Slack wax showed a large increasing effect on physical hardening, and polyphosphoric acid none or a minor negative effect. No correlation between physical hardening index (PHI) and wax content by DSC was found in this study, involving both natural bitumen wax and commercial wax. Addition of the commercial waxes used showed no or marginally positive influence on bitumen ageing properties for the bitumens and test conditions used. Comparing asphalt mixture test results to the corresponding binder test results, the effects on asphalt mixtures from adding commercial wax or polyphosphoric acid were less evident. Significant binder physical hardening by BBR could not be confirmed by TSRST. / QC 20101006

Dissertation thesis is focused on rheological properties of asphalt binders and on changes of their performance during the lifetime in road structures. Aging processes of asphalt binders and methods of laboratory aging are described in the theoretical part of the thesis. Furthermore, basic rheological models and related test methods for the evaluation of asphalt binders are described. In the practical part, properties of asphalt binders are investigated after aging process and their performance is evaluated by empirical and functional test methods. The various methods of aging are compared with each other and a relationship between real conditions and laboratory aging is researched. In the next section, vacuum flashed cracked residue (VFCR) is added to the selected asphalt binders and their influence on rheological properties during description of aging of asphalt binders is investigated. The results were used in publication of two certified methodology under the title „The methodology for the evaluation of paving bitumen in terms of susceptibility to thermal oxidative aging“ and „The methodology describes laboratory aging of asphalt mixtures“. The results of the thesis are listed in the conclusion.

Im Rahmen der vorliegenden Arbeit wurden verschiedene duroplastische Formmassen laboranalytisch hinsichtlich der rheologischen und thermischen Eigenschaften untersucht. Es wurde u.a. gezielt die absolute Materialfeuchte gesteigert, um den Einfluss dieser auf das Fließ­ Härtungsverhalten zu charakterisieren. Anschließend wurden die Materialien auf einer hochinstrumentierten Spritzgussmaschine mit einem Fließspiralenwerkzeug untersucht. Dabei konnte ein direkter Zusammenhang zwischen dem Rückfluss und dem Plastifizierdrehmoment in Abhängigkeit der Materialfeuchte und der Prozessparameter detektiert werden . Des Weiteren wurden über die Differenzdruckmessung im Fließspiralenwerkzeug die scheinbaren Viskositäten über den Fließweg ermittelt. Hierbei konnten unterschiedliche Aufschmelzeffekte über die Fließweglänge in Abhängigke it der duroplastischen Formmasse, der absoluten Materialfeuchte und der Prozessparameter detektiert werden . Durch Schererwärmung konnte die Formmassentemperatur teilweise die Werkzeugtemperatur übersteigen. Hinsichtlich der mechanischen Eigenschaften (Schlagzähigkeit, Biegefestigkeit) konnten keine signifikanten Einflussgrößen detektiert werden. Hinsichtlich des Tg konnten systematischen Unterschiede detektiert und begründet werden. Die beste Möglichkeit zur Ermittlung des Tg lieferte die TMA. Die thermischen Glasübergänge korrelieren mit den in der DSC ermittelten Aushärtegraden , wobei mit steigender Materialfeuchte ein geringer Aushärtegrad detektiert wird. / Within this paper, the rheologieal and thermie eharaeteristies of different thermosetting molding eompounds were investigated using lab analysis methods. Among others, the absolute moisture eontent was inereased purposefully to investigate its influenee on the flow-euring behavior. Subsequently, the materials were analyzed using a highly instrumented injeetion-molding maehine and a flow spiral tool. A direet link between the baekflow and the plastifieation torque dependent on the moisture eontent and proeess parameters was deteeted . Furthermore, a measurement of the differential pressure was eondueted within the flow spiral to deteet the apparent viseosity over the flow path. Within this proeess, different melting effeets over the flow eurve length depending on the molding eompound, the absolute moisture eontent and proeess parameters were deteeted. The shear heating lead to a material temperature inerease of the molding eompound, whieh was partly higher than the tool temperature . Coneerning the meehanieal eharaeteristies (impaet strength, flexural strength), no signifieant influeneing faetors eould be deteeted. In eontrast, systematie differenees of the glass transition temperature were deteeted and their eause eould be explained. The best way to determine the glass transition is the TMA. The glass transition temperatures eorrelate with the degree of eure determined with the DSC, whereas an inereasing moisture eontent is assoeiated with a lower degree of eure.

Subject of this diploma thesis is to describe the effect of adding different amount of aged binder recovered from RAP on the change of properties of polymer modified bitumen. The RAP containing unmodified bitumen and the RAP where we can expect bitumen modification are used to recover binder. The binder obtained from RAP is dosed into the virgin binder in amount of 15 %, 30 % and 50 %. The methods of recycling of flexible pavements, extraction and regeneration of asphalt binders, rejuvenating of their properties and methods of empirical and functional laboratory tests are described in the theoretical part. The practical part deals with evaluating and comparison of the results mixed binders properties.

Additive manufacturing with the use of metals have been a steadily increasing field, being able to create products with a higher degree of complexity than traditional processing techniques. SLM is a popular AM process that uses metal powder as feedstock, and one of the key components of this process is the powder rheology. In recent years the use of a powder rheometer has been shown to be a good way of evaluating powder rheology of metal powders used within AM processes, but there is a clear lack of standardised tests and methods. In this study the Compressibility, Permeability, and Aeration test for 316L powders used within SLM processes was evaluated with a FT4 powder rheometer. 15 powders that had undergone printing in SLM processes were studied. This showed that the compressibility test had the best results in differentiating the bad preforming powders, thereafter the Aeration test. The Permeability test wasn’t able to differentiate the bad preforming powders with the settings used. This study demonstrates that some tests with a powder rheometer can evaluate the powder performance in SLM processes, but further research to evaluate the tests and standardise the settings are needed for clearer test results. / Additiv tillverkning med metall är ett område som stadigt ökat i intresse, främst på grund av möjligheten att producera produkter med en mycket högre grad av komplexitet i jämförelse med traditionella processmetoder. SLM är en populär AM process som använder metallpulver som råmaterial, och en av huvudkomponenterna för processen är pulvrets reologi. Under senare år har användningen av en pulver-reometer visat sig ett bra sätt att utvärdera pulver-reologi för metallpulver som används inom AM, men det finns en klar avsaknad av standardiserade test och metoder. I denna studie utvärderas Kompressabilitet, Permeabilitet, och Aerabilitet testen för 316L pulver producerade för SLM processer med en FT4 pulver-reometer. 15 pulver som genomgått SLM printing studerades. Studien visar att kompressabilitets testets utfall bäst överensstämde med det som setts under SLM processen, och bäst urskilde pulvren som fungerat dåligt att printa med, därefter Aerations testet. Permeabilitets testet kunde inte urskilja de sämre pulvren med de inställningarna som användes. Studien demonstrerar att vissa test och index samlade med ett pulver reometer är mer tillförlitliga än andra när det gäller för att utvärdera pulvrets prestanda inom SLM processer, men vidare forskning och studier krävs för att utvärdera testen och standardisera inställningar baserat på pulvret som testas.