京都大学 / 0048 / 新制・課程博士 / 博士(工学) / 甲第20361号 / 工博第4298号 / 新制||工||1666(附属図書館) / 京都大学大学院工学研究科マイクロエンジニアリング専攻 / (主査)教授 安達 泰治, 教授 小寺 秀俊, 教授 田畑 修 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DFAM

The air intake manifold is an integral part of modern internal combustion engines. Currently manufactured in glass fibre reinforced PA66, inquiries have been raised regarding a change of material to glass fibre reinforced PP. A new engine project is the purpose for which this proposed material is evaluated. The thermochemical environment in the air intake system puts high demands on the material. Ageing treatments and tensile testing was conducted on samples of the new material, as well as on the currently used PA66 to evaluate mechanical response of each material to treatments made to simulate the air intake environment. Furthermore, understanding of the chemical setup is lacking and needs to be studied. Experiments was performed to study the chemistry of the intake environment. Results indicated that PP can retain sufficient mechanical rigidity and strength when subjected to parameters made to simulate the air intake. Moreover, results regarding the chemical environment in the air intake system provided limited information.

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PET har under lång tid använts för flasktillverkning eftersom den är lätt, har goda barriäregenskaper och kan enkelt bearbetas industriellt. På senare tid har miljömedvetenheten ökat i samhället och därmed efterfrågan på återvunnet material, däribland PET-flaskor. Redan idag tillverkas flaskor med helt återvunnen PET.  Återvunnen PET har dock kvalitetsproblem. Därför uppstår frågan hur materialegenskaperna hos 100% återvunna PET-flaskor påverkas av upprepade återvinningscykler.  I den här rapporten undersöks hur den kemiska strukturen och egenskaperna förändras hos materialen allt eftersom fler återvinningscykler genomförs. Tre olika återvunna PET-material används för att ge ett bredare undersökningsunderlag och dessa tre material jämförs sedan sinsemellan samt med jungfrulig PET (icke-återvunnen PET) som referens.  Egenskaperna analyseras med DSC för att ge information om termiska egenskaper, ATR-FTIR utförs för att detektera nedbrytning och förändring i den kemiska strukturen, dragprovning görs för att se hur återvinningen påverkar de mekaniska egenskaperna hos materialen och slutligen analyseras även den inneboende viskositeten hos de återvunna materialen.  Examensarbetet visar på en markant minskning av inneboende viskositet med antalet återvinningscykler. Dessutom kan viss nedbrytning hos den kemiska strukturen ses via ATR-FTIR fastän inte så tydligt. Även en tendens till minskad kristallinitet med återvinning kan ses med DSC. En minskning i kristallinitet möjliggör produktion av mer transparenta flaskor, vilket ofta är eftertraktat. Emellertid får materialet försämrade barriäregenskaper. Dock krävs mer forskning för att kunna dra några slutsatser gällande materialegenskaper i industriell skala. / PET has been used in bottle production for a long time since it is lightweight, easily processable and has good barrier properties. In recent years, the awareness of environmental issues has increased and thereby the demand for recycled materials, including PET bottles. Already today PET bottles with 100% recycled PET are produced. However, recycled PET bottles have quality problems. Thereby, the question arises how the material properties of 100% recycled PET bottles are affected when subjected to multiple recycling loops.  In this report the changes in chemical structure and material properties of the materials are investigated as more recycling loops are performed. Three different recycled PET materials are used to give a broader base of information. These materials are compared to each other and to virgin PET (not recycled PET) as a reference.  The materials are analysed with DSC to give information about the thermal properties, ATR-FTIR to detect changes in the chemical structure, tensile testing to see how the recycling affects the mechanical properties of the material and finally the intrinsic viscosity is analysed for the recycled materials.  In this master thesis a clear decrease in intrinsic viscosity with increasing number of recycling loops can be observed. In addition, some degradation of the chemical structure can be seen through ATR-FTIR, although not very clearly. Also, a decrease in crystallinity with the number of recycling loops can be seen from DSC. A decrease in crystallinity enables production of more transparent bottles, which is often desired, although the material will have reduced barrier properties. However, more research is required to draw any conclusions regarding the material properties on an industrial scale.

Återvinning och insamling av PET-flaskor startade redan 1994 i Sverige och är en av de grundläggande återvinningsindustrierna.Teknologin har ständigt utvecklas sedan dess och vi har nu nya återvinningsmetoder som kan säkerställa PET-material som uppnår livsmedelskvalitet. Dessutom produktionsmetoder så som Solid-State polymerisation, vilket möjliggör flaska-till-flaska mantrat som genomsyrar Returpack.Med den globala klimatutmaningen vi har framför oss så är intresset i återvinning minskning i användning av fossila bränslen väldigt intressant i många industrier.PET-industrin är en av dessa, där både dryck företag och flasktillverkare vill tillverka flaskor med högre andel återvunnet PET-material. Detta kan redan noteras ute på marknaden, där det finns flaskor tillverkade från 100% återvunnen PET. I denna avhandling har vi undersökt effekten av halten återvunnet material har på både mekaniska och kemiska egenskaper. Effekten av antalet återvinnings-cykler har också blivit undersökt.En labb-version av den återvinningsprocess som används kommersiellt i Sverige av Veolia PET utfördes. Fyra cykler av återvinningsprocessen genomfördes på Virgin PET, vilket resulterade i satserna, krPET-1 till krPET-4. Från varje sats tillverkades hundbens-replikat via formsprutning med olika fraktioner: 25, 50 och 100% återvunnen PET. Alla replikat karakteriserades med instrument och metoder så som dragprovning, FT-IR, DSC och inre viskositet.Från en miljösynpunkt finns det definitiva och redan konstaterade fördelar med en ökning av rPET fraktionen i PET-flaskor. Problem under tillverkningen av replikat ledde till små samplingsstorlekar. Som ett resultat gick det ej att dra några slutsatser från de potentiella nackdelarna som en högre rPET fraktion skulle kunna innebära. / The recycling and collection of PET bottles has a long tradition in Sweden dating back to 1994 and is one of the staple recycling industries.Technology has advanced since then, with new recycling processes to assure food grade certified recycled PET and manufacturing processes such as Solid-State polymerization to enable the bottle-to-bottle mantra. Amidst global warming and climate crisis, the interest in recycling and reducing the use of fossil fuel to manufacture new bottles is ever-growing. As a result, manufacturers and breweries want bottles manufactured with higher fractions of recycled PET, and there are already bottles out on the market made from 100% recycled PET. In this thesis, the effect that the fraction of recycled PET may have on the mechanical and chemical properties of the final product was tested. Also, the effect that several recycling cycles may have on the product was tested.A lab-scale version of the recycling process used commercially in Sweden by Veolia PET were carried out. Four cycles of the process were carried out on virgin PET material, resulting in material batches krPET-1 to krPET-4. Dog bone samples from each recycled batch were manufactured via injection moulding with 25, 50 and 100% rPET fractions. All samples were characterized with various instruments and methods such as FT-IR, Tensile testing, DSC, and intrinsic viscosity testing.From an environmental standpoint, there are clear advantages to an increase in rPET fraction in PET-bottles. Due to issues with manufacturing and the production of samples, only a small sample size was acquired. All the analyses suffered, as a result, making it hard to draw any definite conclusions regarding potential disadvantages with a higher rPET fraction.

The goal of this research is to aid the development of large-scale additive manufacturing of jointless underbody hulls for the Army Ground Vehicle Systems by 1) generating an improved mechanical and metallurgical database and 2) understanding the Additive Friction Stir Deposition (AFSD) process. AFSD is a solid-state additive manufacturing process that is a high strain rate and a hot working process that deforms material onto a substrate and builds a component layer by layer. This unique, solid-state additive manufacturing process has the potential for scalability into ground vehicle applications on the extra large-scale due to its solid-state nature. Two different aluminum alloys were investigated: Al-Mg-Si (6061) and Al-Zn-Mg-Cu (7075). AFSD builds were evaluated in the transverse or through layer direction (Z) and the 6061 material was also evaluated in the longitudinal direction (X). Uniaxial tensile testing was performed to generate mechanical property data while fractography, and metallography were used to better understand the metallurgical implications of this process. This research determined that the refinement of the grain size caused by the AFSD process had little or no strengthening effect on the mechanical properties of either alloy. Instead, the as-deposited condition in both alloys were soft with good ductility due to the dissolution of the strengthening particles. After heat treatment, the elongation and fracture mode of the 6061 alloy was dependent on the layer direction. Failure often initiated at interfaces and affected the materials' elastic-plastic behavior. For the 7075 alloy, the strength and failure mechanism of the material were affected by the presence of the graphite lubricant used during processing. The use of graphite increased the variability of the mechanical properties results and caused premature failure in numerous samples. In both alloys, the heat treatment caused grain coarsening to varying degrees which can affect the mechanical behavior. From these results, it was found that a precipitation strengthening heat treatment is required for material deposited with AFSD to achieve the minimum mechanical property standards for a forging. Recommendations and future work include 1) investigating the effect of residual stresses on AFSD components, 2) determining the fatigue properties of AFSD materials, 3) continuing to increase the database of mechanical properties for AFSD materials, and 4) developing additional lubricants for the AFSD process. / Master of Science / The results of this research will be used to help generate design requirements for large-scale additively manufactured parts such as underbody tank hulls. This research generated and expanded on the mechanical and metallurgical understanding of solid-state additively manufactured aluminum. The solid-state additive process used was Additive Friction Stir Deposition. Like its name, this process uses a rotating tool head to apply friction to a solid bar of aluminum that then generates heat which makes the metal soft enough to stir and deposit into a layer. Another layer is then deposited on top and repeated layer by layer until the final part is completed. Other metal additive manufacturing processes that involve melting and then rapidly cooling the material degrade the quality of the metal material. The first part of this research investigated the mechanical properties in different layer directions either pulling along the build direction or against the layers. The results showed that a heat treatment was required to improve the strength of the aluminum to meet current standards of quality. However, the ability of the aluminum to elongate depended on the orientation of the layers. The second part of this research investigated the effect that a graphite lubricant used on the aluminum feedstock to help prevent the material from sticking in the tool head affected the mechanical properties. The results show that the graphite lubricant did not dissolve or disappear into the metal and caused a reduction in the elongation of the aluminum. Recommendations for extra large-scale metal additive manufacturing are to design parts to apply the highest stress along the layer direction and to eliminate the use of the graphite lubricant.

Individual carbon nanotubes have been theoretically and experimentally proven to be the strongest and stiffest materials discovered to date with tensile strengths ranging from 1-5 TPa and elastic modulus values as high as 150 GPa. In this work, the recent development of continuous sheets of CNTs, produced by Nanocomp Technologies Inc ., are investigated for their potential as reinforcement in polymer matrix composite (PMC) materials. The potential of these nanotube-based PMC materials have been reported by researchers at Florida State University (FSU). Through the use of mechanical stretching procedures to increase the alignment of the nanotubes within the CNT sheets, the tensile strength and Young's modulus of the composites in the FSU study averaged 3081 MPa and 350 GPa, respectively. These values are for composites fabricated from 40% stretched CNT sheets and are 48% and 107% improvements over composites fabricated from the pristine, unstretched CNT sheets. However, the test specimens used in the FSU study consisted of a single CNT ply and each coupon was individually stretched and cured for testing. Therefore, the process used to generate the coupons which exhibited these high mechanical properties would be difficult to scale to a usable size for aerospace structural components. In the current study, a scalable process has been developed in which 2-ply, 3" x 3" panels of CNT and resin composites are fabricated. An apparatus and methodology for mechanically stretching the CNT sheets used in these composite panels has also been developed. After initial testing was conducted with the CNT composites and the coupons exhibited significant elongation at failure, along with the absence of a linear elastic region, conventional test standards for material testing were deemed impractical. For this reason, new mechanical testing methodologies have been developed to determine the mechanical properties of specific strength and specific modulus of CNT-polymer composites. In order to obtain the maximum benefits of a fiber in any matrix in terms of stiffness and strength, it is preferable to align the high strength and stiffness fibers in the direction of loading. Given that these CNT sheets essentially consist of billions of short, discontinuous CNTs of 2-3mmin length, the process of mechanical stretching is used in an attempt to align these tubes in the direction of the applied tensile load. Here we have explored methodologies for stretching, fabricating, and mechanical testing. Having identified a process which seems viable, an examination into the effect of the mechanical stretching to increase the alignment of the nanotubes within the CNT sheets, and thus to increase the material properties of the 2-ply composites constructed from them, is conducted. In order to correlate the enhancements in the mechanical properties with the increased alignment of the CNTs, polarized Raman spectroscopy techniques have been used. Lastly, Scanning Electron Microscopy (SEM) is used to examine the effect of stretching on the pristine CNT sheet, as well as examine the fracture surfaces of failed test coupons to better characterize the failure modes. In this report, polarized Raman spectroscopy has been used to confirm the enhancedalignment of nanotubes within the CNT sheets through the used of a nematic order parameter. Unstretched sheets exhibit an order parameter of 0.07 and 0.09 for untreated and Acetone treated sheets, respectively. Upon stretching the untreated sheets to 45%, the order parameter increases to 0.1409 and, when stretched to 30%, Acetone treated sheets have an order parameter of 0.1518. During the mechanical testing of 2-ply composites fabricated from stretched CNT sheets, the effect of this increased alignment is made apparent. Untreated CNT sheets are used to fabricate 2-ply composites after being stretched and are compared to baseline values of panels fabricated using sheets which are not stretched. In the panels fabricated with PEI resin and 43% stretched, untreated CNT sheets, a 137% increase in average specific strength and a 44% increase in average specific modulus over the baseline panel is observed. For panels fabricated with BMI and 33% stretched, untreated CNT sheets, a 169% increase in average specific strength and 105% increase in average specific modulus is observed when compared to the baseline panel. These increases are evidence for the potential of mechanical stretching to align the nanotubes within the CNT sheets and bolster the mechanical properties of resulting CNT-polymer composites. / Master of Science

Additive manufacturing (AM), also known as 3D printing, is a concept and method of a manufacturing process that builds a three-dimensional object layer-by-layer. Opposite to the conventional subtractive manufacturing, it conquers various limitations on component design freedom and raises interest in various fields, including aerospace, automotive and medical applications. This thesis studies the mechanical behavior of thin-walled component manufactured by a common AM technique, laser powder bed fusion (LPBF). The studied material is Hastelloy X, which is a Ni-based superalloy, and it is in connection to a component repair application in gas turbines. The influence of microstructure on the deformation mechanisms at elevated temperatures is systematically investigated. This study aims for a fundamental and universal study that can apply to different material grades with FCC crystallographic structure. It is common to find elongated grain and subgrain structure caused by the directional laser energy input in the LPBF process, which is related to the different printing parameters and brands of equipment. This thesis will start with the study of scan rotation effect on stainless steel 316L in an EOS M290 equipment. The statistic texture analysis by using neutron diffraction reveals a clear transition when different level of scan rotation is applied. Scan rotation of 67° is a standard printing parameter with intention to lower anisotropy, yet, the elongated grain and cell structure is still found in the as-built microstructure. Therefore, the anisotropic mechanical behavior study is carried out on the sample printed with scan rotation of 67° in this thesis. Thin-walled effects in LPBF are investigated by studying a group of plate-like HX specimens, with different nominal thicknesses from 4mm down to 1mm, and a reference group of rod-like sample with a diameter of 18mm. A texture similar to Goss texture is found in rod-like sample, and it becomes <011>//BD fiber texture in the 4mm specimen, then it turns to be <001> fiber texture along the transverse direction (TD) in the 1mm specimen. Tensile tests with the strain rate of 10−3 s−1 have been applied to the plate-like specimens from room temperature up to 700 ℃. A degradation of strength is shown when the sample becomes thinner, which is assumed to be due to the overestimated load bearing cross-section since the as-built surface is rough. A cross-section calibration method is proposed by reducing the surface roughness, and a selection of proper roughness parameters is demonstrated with the consideration of the calculated Taylor’s factor and the residual stress. The large thermal gradient during the LPBF process induces high dislocation density and strengthens the material, hence, the LPBF HX exhibits better yield strength than conventionally manufactured, wrought HX, but the work hardening capacity and ductility are sacrificed at the same time. Two types of loading condition reveal the anisotropic mechanical behavior, where the vertical and horizontal tests refer to the loading direction being on the BD and TD respectively. The vertical tests exhibit lower strength but better ductility that is related to the larger lattice rotation observed from the samples with different deformation level. Meanwhile, the elongated grain structure and grain boundary embrittlement are responsible for the low horizontal ductility. A ductile to brittle transition is traced at 700 ℃, so a further study with two different slow strain rates, 10−5 s−1 and 10−6 s−1, are carried out at 700 ℃. Creep damage is shown in the slow strain rates testing. Deformation twinning is found only in the vertical tests where it forms mostly in the twin favorable <111> oriented grain along the LD. The large lattice rotation and the deformation twinning make the vertical ductility remain high level under the slow strain rates. The slow strain rate tensile testing lightens the understanding of creep behavior in LPBF Ni-based superalloys. In summary, this thesis uncovers the tensile behavior of LPBF HX with different variations, including geometry-dependence, temperature-dependence, crystallographic texture-dependence and strain rate-dependence. The generated knowledge will be beneficial to the future study of different mechanical behavior such as fatigue and creep, and it will also enable a more robust design for LPBF applications. / Additiv tillverkning, eller 3D-utskrifter, är tillverkningsmetoder där man skapar ett tredimensionellt objekt genom att tillföra material lager for lager. Till skillnad från konventionella avverkande tillverkningsmetoder elimineras många geometriska begränsningar vilket ger större designfrihet och metoderna har därför väckt stort intresse inom en rad olika områden, inklusive flyg-, fordons- och medicinska tillämpningar. I denna avhandling studeras mekaniska egenskaper hos tunnväggiga komponenter tillverkade med en vanligt förekommande laserbaserad pulverbädds-teknik, laser powder bed fusion (LPBF). Det studerade materialet är Hastelloy X, en Ni-baserad superlegering som är vanligt förekommande for både nytillverkning och reparation av komponenter för gasturbiner. Inverkan av mikrostruktur på deformationsmekanismerna vid förhöjda temperaturer undersöks systematiskt. Detta arbete syftar till att ge grundläggande och generisk kunskap som kan tillämpas på olika materialtyper med en kubiskt tätpackad (FCC) kristallstruktur. Det är vanligt att man hittar en utdragen kornstruktur orsakad av den riktade tillförseln av laserenergi i LPBF-processen, vilket kan relateras till olika processparametrar och kan variera mellan utrustningar frän olika leverantörer. Denna avhandling inleds med studien av effekten av scanningsstrategi vid tillverkning av rostfritt stål 316L i en EOS M290-utrustning. En statistisk texturanalys med hjälp av neutrondiffraktion påvisar en tydlig övergång mellan olika mikrostrukturer när olika scanningsstrategier tillämpas. En scanningsrotation på 67 mellan varje lager är en typisk standardinställning med avsikt att sanka anisotropin i materialet, dock finns den utdragna kornstrukturen oftast kvar. I denna avhandling studeras därför de anisotropa egenskaperna hos material tillverkade med 67 scanningsrotation. Effekten av tunnväggiga strukturer i LPBF undersöks genom att studera en uppsättning platta HX-prover, med olika nominella tjocklekar från 4 mm ner till 1 mm, samt en referensgrupp med cylindriska prov med en diameter på 18 mm. Kristallografisk textur som liknar den av Goss-typ återfinns i de cylindriska proverna vilket gradvis övergår från en fibertextur med <011> i byggriktningen for 4mm-proven till en fibertextur med <001> i tvärriktningen for 1mm-proven. Dragprovning med en töjningshastighet på 10−3 s−1 har utförts på de platta provstavarna från rumstemperatur upp till 700 ℃. En sänkning av styrkan uppvisas när proven blir tunnare, vilket kan antas bero på att det lastbarande tvärsnittet överskattas på grund av den grova ytan. En metod för tvärsnittskalibrering föreslås genom att kompensera for ytråheten, och valet av lämplig ytfinhetsparameter motiveras med hänsyn till den beräknade Taylor-faktorn och förekomsten av restspänningar. Den stora termiska gradienten som uppstår for LPBF-processen inducerar en hög dislokationstäthet vilket höjer materialets styrka och följaktligen uppvisar LPBF HX högre sträckgräns an konventionellt tillverkad, smidda HX, men förmågan till deformationshårdnande samt duktiliteten i materialet sänks samtidigt. Tester utförda i två olika belastningsriktningar, vertikalt respektive horisontellt mot byggriktningen, demonstrerar det anisotropiska mekaniska beteendet. De vertikala testerna uppvisar lägre hållfasthet men bättre duktilitet vilket kan relateras till en större benägenhet for kristallstukturen att rotera när deformationsgraden ökar. Samtidigt är den utdragna kronstukturen ansvarig for den lägre duktiliteten for de horisontella proverna. En övergång från ett duktilt till ett mer sprött beteende noterades vid 700 ℃, och därför initierades ytterligare en studie där tester med två lägre töjningshastigheter, 10−5 s−1 och 10−6 s−1, utfördes vid 700 ℃. Det kan noteras att krypskador återfinns i tester med en långsam deformationshastighet och deformationstvillingar uppstår endast i de vertikala provstavarna där det främst bildas tvillingar i korn orienterade med <111> riktningen längs belastningsriktningen. Den stora förmågan till rotation i kristallstrukturen och deformationstvillingarna bidrar till att den vertikala duktiliteten förblir hög även i testerna med en låg deformationshastighet. Testerna med en långsam draghastighet bidrar därför till en bättre förståelse av krypbeteendet i LPBF Nibaserade superlegeringar. Sammanfattningsvis så bidrar denna avhandling till bättre förståelse av de mekaniska egenskaperna hos LPBF HX i olika utföranden och förhållanden, inklusive geometriberoende, temperaturberoende, deformationshastighetsberoende samt inverkan av kristallografisk textur. Den genererade kunskapen kommer att vara till stor nytta vid fortsatta studier av olika mekaniska egenskaper som utmattning och kryp, samt bidrar till att möjliggöra en mer robust design for LPBF-tillämpningar.

The main purpose of this thesis is to investigate the ductility and application of titanium alloys, like titanium 6Al-4V, when used in aerospace fasteners compared to more conventional stainless steel aerospace fasteners such as A286. There have been concerns raised about the safe usability of titanium 6-4 in the aerospace industry due to its lack of strain hardening. However, there is a lack of data pertaining to this concern of safe usage which this thesis aims to address. Tensile tests were conducted to find the ductility indexes of these fasteners which quantify the amount of plastic to elastic elongation. From the tests conducted it was found that the two materials yield and tensile strengths were very similar, though the ductility index of A286 is on average ten times greater than that of titanium 6-4. This thesis includes joint diagram examples that analyze typical joints using both materials. It was found from joint diagram examples that the lower ductility index of the titanium alloy will only be detrimental to use at higher preloads. However, the titanium alloy can be used safely in place of A286 in most loading situations just with narrower safety margins in these controlled examples.