The production of fine filaments using the melt spinning process needs considerable effort. A thermoplastic melt is stretched from the spinneret under a constant take-up speed. The high performance thermoplastic PEEK is solidified in the melt spinning process in a small distance and short time. Therefore, the fine PEEK filaments in the fibre formation zone underwent a high deformation and cooling rate. To make the melt spinning process stable and to produce the fine PEEK filaments, material properties and material behaviour are examined using on-line and off-line measurements. The fibre speed measured using Laser Doppler Anemometry and simultaneous temperature measured using infrared thermography enable both the strain rate and consequently the apparent extensional viscosity to be estimated. This provides the apparent extensional viscosity over the spinning line, which can itself show the structural development of PEEK fibres in the fibre formation zone, i.e. necking and solidification phenomena. The one-dimensional fibre formation model must include both procedural and material parameters. The heat transfer coefficient was estimated using the filament temperature measurement and showed a relatively high contribution of radiation and free convection in comparison to forced convection near the spinneret. The improved model of PEEK fibre formation gave a good agreement to both temperature and speed measurements, and also confirmed the high deformation rate effect on the extensional viscosity, which could be simulated with a properly generalised Newtonian constitutive equation. The end properties of the fibres, such as as-spun filament fineness, orientation (expressed using total birefringence) and total crystallisation (examined using DSC) are investigated in relation to different spinning conditions, i.e. take-up speed, throughput and the draw down ratio. The tensile test diagram results, measuring phenomena such as the elongation at break, tenacity, and the Young modulus of elasticity are also analysed in order to complete the correlation of the above-mentioned spinning conditions to the structural properties of as-spun fine PEEK filaments. The melt spinning of fine PEEK fibres under different spinning conditions is examined with the purpose of finding the optimum take-up speed and throughputs. Other spinning conditions, such as the temperature of melt processing, and the arrangement and diameter of the spinneret holes, are changed in order to make the process more stable. The recommendations for further study can be used to further examine some aspects of this work; however, this work presents a new concept for fine PEEK melt spinning supported by spinnability examinations under different spinning conditions and the improved model of fibre formation, which is also relevant for typical industrial processing applications.

The production of fine filaments using the melt spinning process needs considerable effort. A thermoplastic melt is stretched from the spinneret under a constant take-up speed. The high performance thermoplastic PEEK is solidified in the melt spinning process in a small distance and short time. Therefore, the fine PEEK filaments in the fibre formation zone underwent a high deformation and cooling rate. To make the melt spinning process stable and to produce the fine PEEK filaments, material properties and material behaviour are examined using on-line and off-line measurements. The fibre speed measured using Laser Doppler Anemometry and simultaneous temperature measured using infrared thermography enable both the strain rate and consequently the apparent extensional viscosity to be estimated. This provides the apparent extensional viscosity over the spinning line, which can itself show the structural development of PEEK fibres in the fibre formation zone, i.e. necking and solidification phenomena. The one-dimensional fibre formation model must include both procedural and material parameters. The heat transfer coefficient was estimated using the filament temperature measurement and showed a relatively high contribution of radiation and free convection in comparison to forced convection near the spinneret. The improved model of PEEK fibre formation gave a good agreement to both temperature and speed measurements, and also confirmed the high deformation rate effect on the extensional viscosity, which could be simulated with a properly generalised Newtonian constitutive equation. The end properties of the fibres, such as as-spun filament fineness, orientation (expressed using total birefringence) and total crystallisation (examined using DSC) are investigated in relation to different spinning conditions, i.e. take-up speed, throughput and the draw down ratio. The tensile test diagram results, measuring phenomena such as the elongation at break, tenacity, and the Young modulus of elasticity are also analysed in order to complete the correlation of the above-mentioned spinning conditions to the structural properties of as-spun fine PEEK filaments. The melt spinning of fine PEEK fibres under different spinning conditions is examined with the purpose of finding the optimum take-up speed and throughputs. Other spinning conditions, such as the temperature of melt processing, and the arrangement and diameter of the spinneret holes, are changed in order to make the process more stable. The recommendations for further study can be used to further examine some aspects of this work; however, this work presents a new concept for fine PEEK melt spinning supported by spinnability examinations under different spinning conditions and the improved model of fibre formation, which is also relevant for typical industrial processing applications.

Polyetheretherketone (PEEK) is a designation given to materials of the polyaryletherketone family having a characteristic distribution of ether and ketone groups in the polymer backbone. PEEK materials have high strength and chemical resistance as well as very high melting points and glass transition temperatures. Because of this combination of properties, PEEK materials find use for wear application in extreme environments where they provide a light-weight and corrosion resistant bearing material that often does not require lubrication. An initial study focused on determining the effects of supplier and molecular weight on the wear of particular PEEK materials, in addition to the effect of contact pressure. This work is significant because it highlights the fact that tribologically relevant polymers, such as PEEK materials, vary greatly in terms of their polymer morphology and processing history, and this variation must be recognized by investigators when reporting wear data. Because of their light weight, chemical resistance, and self-lubricating properties, polymers are used in applications ranging from biomedical to aerospace. Some polymers exhibit significant differences in wear resistance based on whether they are in unidirectional or multidirectional sliding. Shear induced polymer chain orientation is believed to be responsible for this behavior. Polyetheretherketone (PEEK) has excellent wear resistance, but its multidirectional sliding behavior has not been thoroughly investigated. A factorial multidirectional pin-on-plate wear study of PEEK was conducted with a focus on molecular weight and sliding path directionality. These factors were studied for their correlation to overall wear performance. Additionally, transfer film thickness was measured at locations along the wear path using white light interferometry. A result of this work has been a greater understanding of PEEK wear mechanisms in various sliding configurations and how they relate to transfer film formation. A major outcome was the development of a quantitative metric to describe transfer film thickness and continuity. It was found that thinner more continuous transfer films form under sliding conditions that change direction rather than overlapping along the same path. The thinner more continuous transfer film was found to also correspond with statistically lower wear behavior. Scanning electron microscope (SEM) investigation of the transfer film and pin wear surface confirmed the relationship between transfer film quality and wear.

ABSTRACT PEEK matrix reinforced by carbon fibers as one thermoplastic composite material is studied. Thermoplastic composites have the advantages of high specific stiffness and strength, longer fatigue life, good resistance to moisture absorption and high temperature condition. The thesis is aimed to investigate the mechanical properties and fracture mechanism of the centrally notched AS-4/PEEK composite laminates subjected to tension-tension fatigue loading at elevated temperature. We use three common types of laminates, such as cross-ply , quasi-isotropic and angle-ply . After centrally notched, we first obtain the base-line data of mechanical properties by tensile tests at five different temperatures, such as 25¢J¡B75¢J¡B100¢J¡B125¢J¡B150¢J. Then, the fatigue tests are conducted, we receive the fatigue strength and life and establish the stress-life curves. The fatigue characteristics and fracture mechanism of a centrally notched composite laminate at elevated temperature are also recorded and observed. The empirical results can be concluded as follows. At the same temperature, the laminate of cross-ply possesses the largest ultimate strength and fatigue strength, quasi-isotropic the second angle-ply the smallest. As for the elastic modulus, the laminate of cross-ply is larger than that of quasi-isotropic. However, the large strain of angle-ply is within the plastic range that is out of the limit of the study. Thus, a further investigation is needed for angle-ply laminates alone. After centrally notched, the net area is reduced of the specimen, and then the elastic modulus is raised and the ultimate strength and fatigue strength of composite materials are lower. As the temperature increasing, the ultimate strength, fatigue strength and elastic modulus are all decreasing.

Zugl.: Erlangen, Nürnberg, Univ., Diss., 2008

Shrinking down into nanoscale, materials exhibit huge property advantages over their bulk form. New forms of carbon at nanoscale have occupied the prominent position in modern materials research. With a very long history accompanying our human civilisation, carbon as a wonder material has once again contributed to our technological advances, as evidenced by the discoveries and research attractions in the last a few decades. Research into fullerenes (C60, C70, etc.), carbon nanotubes (CNTs) and graphene has been continued raising, because of the numerous novel properties associated with these new carbon forms1-3. On top of their excellent electronical, physical and chemical properties, CNTs and graphene also exhibit excellent mechanical properties including ultra-high tensile strength, Young’s Modulus, as well as high thermal conductivities. Research into carbon has also promoted the flourish of many new non-carbon nanomaterials, and typical examples include the inorganic fullerene-like tungsten disulphide (IF-WS2) nanoparticles (NPs), numerous oxide NPs and nanowires that also exhibit various remarkable properties, such as high hardness and anti-oxidation stability. To combine the outstanding performances of both carbon and non-carbon nanomaterials by marrying nanoscale carbon with various metal oxide particles, which forms the backbone of my thesis by carrying out the intensive investigations. In my project it have further validated the advantages of the resulting new carbon-coated NPs in different polymeric matrix composites. The main findings are as follows: 1. A home-made rotary chemical vapour deposit (RCVD) system has been modified and this versatile facility has been applied successfully to produce different types of graphitic carbon-coated nanocomposite particles, from micro- down to nano-scale, including IF-WS2, TiO2, ZnO, Y2O3, Cr2O3, CeO2 and ZrO2 etc. The production can be up to 30 g/per batch, which is 10s times more than using a traditional static furnace, by avoiding severe agglomeration. 2. The resulting coating consists of a few layered graphitic carbon with lattice space 0.34 nm. The thickness of the coating is simply controllable between 1-5 nm, depending on the deposition time (10~60 min), precursor injection flow rate (1.2~2.4 ml/L) and heating temperature (700~900 oC). Furthermore, the oxide core of ZnO@C was removed by heating under the H2/Ar atmosphere, and have successfully generated nano- to micro-scale, hollow, closed, and all-carbon structures. 3. The commercial Nylon 12 is applied to fabricate the metal oxide polymer composite. Using ZnO@C-Nylon 12 composite as an example, at 2 wt% content, the composites have achieved with the ultimate tensile strength increased by 27% (from 47.9 to 59.6 MPa), In particular, at 4 wt% content, the ZnO@C showed an impressive improvement in thermal conductivity of nearly 50% (From 0.21 t0 0.31 W∙m-1∙K-1), comparing 16% improvement for ZnO-Nylon 12 composite. 4. Apart from investigations of nylon composite, intensive studies of the Poly ether ether ketone (PEEK), an important high performance engineering thermoplastics polymer, and its nanocomposites reinforced by IF-WS2 and IF-WS2@C have been carried out in this thesis. The IF-WS2/PEEK composites exhibited not only an improvements of 24% (From 77.6 to 96.7 MPa) in the tensile strength (2 wt%), but also showed an extraordinary increase in thermal conductivity by 190%, from 0.248 to 0.719 W∙m-1∙K-1 at 8 wt%, higher onset decomposing temperatures (54 oC) against the plain PEEK. 5. Moreover, owing to the better dispersal capacity of IF-WS2@C NPs, the ternary IF-WS2@C-PEEK nanocomposites produced in this thesis displayed impressive mechanical properties, increased by 51% (From 77.6 to 120.9 MPa, at 2 wt%), and extremely greater thermal conductivity, with 235% (From 0.248 to 0.831 W∙m-1∙K-1 at 8 wt%), and better stability than the comparison IF-WS2-PEEK composites. The parameters influencing the coating quality and thickness have also been investigated. Further, their interface studies based on the FTIR and XPS techniques have verified the formation of chemical bonding (C=S bonding and carbon π-π bonding), rather than physically bonded together. The successful application of the generic RCVD process can be further extended to the processing of many new particles for an ultrathin carbon coating. Considering the vast amount of literature focusing on carbon, the project further processing of carbon-coated materials in composites could easily be tailored to achieve desired surface contacts with different matrices and leading to the better desired performance, as verified in this thesis for the advanced binary and ternary composites. Finally, this research is expecting to expand the application potentials of PEEK-based nanocomposites in critical areas where thermal conductivity and thermal stability are important.

Submitted by Maria Medeiros (maria.dilva1@ufcg.edu.br) on 2018-07-12T11:42:41Z No. of bitstreams: 1 GEIZA FERREIRA DA SILVEIRA - DISSERTAÇÃO (PPGCEMat) 2015.pdf: 1911970 bytes, checksum: 11453fabee54145719137019d8d1d030 (MD5) / Made available in DSpace on 2018-07-12T11:42:41Z (GMT). No. of bitstreams: 1 GEIZA FERREIRA DA SILVEIRA - DISSERTAÇÃO (PPGCEMat) 2015.pdf: 1911970 bytes, checksum: 11453fabee54145719137019d8d1d030 (MD5) Previous issue date: 2015-08-31 / Na odontologia os implantes dentários osseointegráveis têm sido a melhor opção para o tratamento da perda dental. Estes permitem a recuperação estética e funcional, como a capacidade de mastigação. Atualmente vem se introduzindo a utilização de polímeros para fabricação de implantes osseointegráveis em substituição aos convencionais de titânio, a exemplo do poli-éter-éter-cetona (PEEK). Dessa forma, o objetivo deste trabalho é avaliar as propriedades do PEEK para aplicações odontológicas a partir das caracterizações morfológica, química e físicas, na perspectiva de uso como implante. As amostras foram analisadas através de Microscopia Eletrônica de Varredura – MEV com Espectroscopia por Energia Dispersiva de raios X – EDS, Difração de raios-X (DRX), Espectroscopia na Região de Infravermelho com Transformada de Fourier (FTIR), Calorimetria Exploratória Diferencial (DSC) e Molhabilidade por Ângulo de Contato. O resultado de MEV apresentou característica de um material de superfície lisa e densa. O EDS exibiu os elementos químicos oxigênio e carbono, característicos do polímero. No DRX observou-se que o PEEK tem comportamento de material semicristalino. Os espectros de FTIR revelaram as bandas típicas de absorção do PEEK. Na análise térmica realizada por calorimetria exploratória diferencial do PEEK, observou-se a presença de um pico endotérmico em 344,68° C, com início em aproximadamente 320° C e final em 349° C. De acordo com os resultados, verifica-se que o PEEK apresenta medidas de ângulo de contato menor que 90°, indicando hidrofilicidade. No ensaio mecânico, percebeu-se que tanto o módulo elástico quanto a resistência à tração do PEEK é mais próximo ao osso que o titânio. Conclui-se que o PEEK apresenta propriedades compatíveis para ser utilizado como biomaterial / In odontology, the dental osseointegrated implants have been the best option for the treatment of total dental loss. These allow a functional and esthetical recovery, such as the ability of chewing. Nowadays, the use of polymers to fabricate osseointegrated implants has been introduced in replacement to the titanium’s conventionals, as for example the polyether ether ketone (PEEK). Therefore, the purpose of this work is to evaluate the properties of polyether ether ketone (PEEK) to use in dental applications, describing it physically, chemically and morphologically, in the use perspective as implant. The samples have been analyzed through a Scanning Transmission Electron Microscope (STEM), Energy Dispersive x-ray Spectroscopy (EDS), X-ray Diffraction, (XRD), Fourier Transform Infrared (FTIR), Differential Scanning Calorimeter (DSC), Wettability by contact Angle. The result of the STEM showed a characteristic of a flat and dense surface material. The EDS displayed the chemical elements oxygen and carbon, typical of a polymer. On the XRD, the PEEK was observed to behave as a semi crystalline material. The spectrums of the FTIR revealed typical bands of PEEK’s absortion. On the thermical analysis by PEEK’s differential scanning calorimeter, it was observed the presence of an endothermic peak in 344,68˚C, initiating approximately with 320˚C and ending in 349˚ C. According to the results, it is verified that the PEEK presents measures of contact angle less that 90˚, indicating hydrophilicity. On the mechanic test, it was perceived that the elastic module and PEEK’s traction resistence is the closest to the bone rather than the titanium. The conclusion therefore is that the PEEK shows compatible properties to be used as a biomaterial.

No description available.

No description available.

SammanfattningSyfteSyftet med föreliggande studie är varär att med en finita elementanalys (FEA) undersöka hållfastheten i implantatförankrade treleds-brounderkonstruktioner av materialet PEEK beroende på konnektordimension och belastningsvinkel med hjälp av finita elementmetoden (FEM) genom att analysera spänningskoncentration, displacering och töjning. i implantatförankrade treleds-brounderkonstruktioner i materialet PEEK beroende på konnektortjocklek och belastningsvinkel med hjälp av finita elementmetoden (FEM). Material och MetodTre Ddigitala implantatförankrade brokonstruktioner 44-46 i PEEK respektive zirkconia med konnektordimensionerna konnektorarean 12 mm2, 14 mm2 och 16 mm2 f framställdes i ett CAD-program. Grupperna med konnektordimensionen 16 mm2 utgjorde intern (P-16) respektive extern (Z-16) kontrollgrupp. Därefter Dessa belastades dessa med hjälp av med en programvara för FEM FEA på ponticen med kraften 500 N i vinklarna axiell (0°) och vinklad ( 30°) riktning. Värdena för spänningskoncentration, displacering och töjning visualiserades och analyserades.ResultatResultaten visade att högst spänningsvärden uppstod i PEEK-konstruktionen med konnektorarean 12 mm2 under en vinklad belastning, samt att lägst spänningsvärden uppstod i PEEK-konstruktionen med konnektorarean 14 mm2 under axiell belastning. Endast i kontrollgrupperna, PEEK respektive zirkonia 16 mm2P-16 respektive Z-16 uppstod den maximala spänningskoncentrationen ocklusalt istället för vid konnektorn, även om höga spänningsvärden fortfarande kunde utläsas cervikalt på konnektorn. Högre displacerings- och töjningsvärden kunde iakttas i samtliga PEEK-grupper jämfört med zirkonia-grupperna, oavsett konnektortjocklek konnektordimension och belastningsvinkel.SlutsatsInom ramen för följande föreliggande studiesrs begränsningar kan följande slutsatser dras:•En underdimensionerad konnektor har en negativ inverkan på hållfastheten i implantatförankrade treleds-brounderkonstruktioner av PEEK då de maximala spänningskoncentrationernas lokalisering förflyttas till mer kritiska områden i konnektorområdet. •En vinklad belastning ökar spänningarna, displaceringen och töjningen i implantatförankrade brounderkonstruktioner oavsett material eller konnektortjocklekkonnektordimension. •Spänningsvärden och spänningsfördelning är likartade i implantatförankrade treleds-underkonstruktioner av PEEK och zirkonia, men är mer kritiska för PEEK.•Displacerings- och töjningsvärden är högre i PEEK- än i zirkonia-implantatförankrade treleds-underkonstruktioner. / AbstractPurposeThe aim of the study was is to examine the strength ofin three-unit implant-supported frameworks made of PEEK, depending on connector dimension and loading direction utilizing via a finite element analysis-method (FEAM) by analyzing the stress concentration, displacement and strain. in three-unit implant-supported frameworks made of PEEK, depending on connector dimension and loading direction utilizing a finite element-method (FEM).Material and methodImplant-supported frameworks, 44-46, of PEEK and zirconia with connector dimensions area 12 mm2, 14 mm2 and 16 mm2 was produced by CAD. Via FEAM-software the pontic was loaded with 500 N angled at 0° and 30°. Values for stress, displacement and strain were analyzed.ResultsMaximum stress values ​​occurred in PEEK with the connector area 12 mm2 under angled loading and minimum stress​​ in PEEK with 14 mm2 under axial loading. In the control groups, P/Z 16 mm2, maximum stress arose occlusally, but high stress remained in the cervical connector area. Higher displacement and strain values for displacement and strain waswere observed in all PEEK-groups compared to zirconia, regardless of connector dimension and load angulation of the load.ConclusionWithin the limitations of this the study, the following conclusions were made:•An under-dimensioned connector have a negative impact on the strength of three-unit implant-supported frameworks made of PEEK since the location of the maximum stress appears in more critical areas – the connector areas.•Inclined loading increases stress, displacement and strain in three-unit implant-supported frameworks regardless of material or connector dimension.•Stress values and stress distribution are similar in three-unit implant-supported frameworks made from of PEEK as well as zirconia, but affects PEEK more critically.•Higher displacement and strain values were observed in three-unit implant-supported frameworks of PEEK compared to zirconia.