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At least 55 records · Page 3

Effects of Melt Processing on Evolution of Structure in PEEK

We report on the effects of melt processing temperature on structure formation in Poly(ether-ether-ketone), PEEK. Real time Small Angle X-ray Scattering, SAXS, and thermal analysis are used to follow the melting behavior after various stages of processing. Assignment of peaks to structural entities within the material, the relative perfection of the crystals, and the possibility of their reorganization, are all influenced by the melt processing history. With the advent of high intensity synchrotron sources of X-radiation, polymer scientists gain a research tool which, when used along with thermal analysis, provides additional structural information about the crystals during growth and subsequent melting. PEEK is an engineering thermoplastic polymer with a very high glass transition temperature (145 C) and crystal melting point (337 C). PEEK has been the subject of recent studies by X-ray scattering in which melt and cold crystallization were followed in real-time. X-ray scattering and thermal studies have been used to address the formation of dual endothermic response which has been variously ascribed to lamellar insertion, dual crystal populations, or melting followed by re-crystallization. Another important issue is whether all of the amorphous phase is located in interlamellar regions, or alternatively whether some is located in "pockets" away from the crystalline lamellar stacks. The interpretation of scattering from lamellar stacks varies depending upon whether such amorphous pockets are formed. Some groups believe all of the amorphous phase is interlamellar. This leads to selection of a smaller thickness for the crystals. Other groups suggest that most amorphous phase is not interlamellar, and this leads to the suggestion that the crystal thickness is larger than the amorphous layer within the stacks. To investigate these ideas, we used SAXS and Differential Scanning Calorimetry to compare results of single and dual stage melt crystallization of PEEK using a treatment scheme involving annealing/crystallization at T(sub a1) followed by annealing at T(sub a2) where either T(sub a1) < T(sub a2) or T(sub a1) > T(sub a2). We proposed a model to explain multiple melting endotherms in PPS, treated according to one or two-stage melt or cold crystallization. Key features of this model are that multiple endotherms: (1) are due to reorganization/recrystallization after cold crystallization; and, (2) are dominated by crystal morphology after melt crystallization at high T. In other words, multiple distinct crystal populations are formed by the latter treatment, leading to observation of multiple melting. PEEK 45OG pellets (ICI Americas) were the starting material for this study. Films were compression molded at 400 C, then quenched to ice water. Samples were heated to 375 C in a Mettler FP80 hot stage and held for three min. to erase crystal seeds before cooling them to T(sub a1) = 280 C . Samples were held at T(sub a2) for a period of time, then immediately heated to 360 C. In the second treatment samples were held at T(sub a1) = 31 C for different crystallization times t(sub c) then cooled to 295 C and held 15 min. In situ (SAXS) experiments were performed at the Brookhaven National Synchrotron Light Source with the sample located inside the Mettler hot stage. The system was equipped with a two-dimensional position sensitive detector. The sample to detector distance was 172.7 cm and the X-ray wavelength was 1.54 Angstroms. SAXS data were taken continuously during the isothermal periods and during the heating to 360 C at 5 C/min. Each SAXS scan was collected for 30 sec. Since the samples were isotropic, circular integration was used to increase the signal to noise ratio. After dual stage melt crystallization with T(sub a1) < T(sub a2) the lower melting endotherm arises from holding at T(sub a1). During cooling a broad distribution of crystals forms, and the low-melting tail is perfected during T(sub al). Heating to T(sub a2) melts these imperfect crystals and allows others with greater average long spacing to form in their place. After dual stage crystallization with T(sub a1) > T(sub a2), the amount of space remaining for additional growth at T(sub a2) depends upon the holding time at T(sub a1). The long period of crystals formed at T(sub a2) is smaller than that formed at T(sub a1) due to growth in a now-restricted geometry. Perfection of crystals is seen as an increase of the intensity of the population scattering at higher s, while the intensity of the population scattering at lower s stays constant. During heating from below to above the minor endotherm, we see rapid decrease of the intensity of the X-ray scattering corresponding to the population of crystals scattering in the shoulder. Another important observation is that after the sample is annealed at 295 C, the shoulder intensity is restored once again. The population scattering at higher s remains longer before it disappears in the sample treated to the second stage of melt crystallization, compared to the sample crystallized with a single stage. This could be interpreted as an effect of continued perfection of the less perfect population, which is also reflected in the increased melting temperature of the smaller endotherm as the holding time at 295 C increases. In the corresponding DSC scans we see a shift in the area and the peak temperature of the lower melting endotherm with an increase of the annealing time.

Georgiev, Georgi↗

Interpenetrating polymer network approach to tougher and more microcracking resistant high temperature polymers. I - LaRC-RP40

Interpenetrating polymer networks in the form of the LaRC-RP40 resin, prepared by the in situ polymerization of a thermosetting imide prepolymer and thermoplastic monomer reactants, are presently used to obtain toughness and microcracking resistance in a high-temperature polymer. Attention is presently given to the processing, physical, and mechanical properties, as well as the thermooxidative stability, of both the neat resin and the resin as a graphite fiber-reinforced matrix. Microcracking after thermal cycling was also tested. LaRC-RP40 exhibits significant resin fracture toughness improvements over the PMR-15 high-temperature matrix resin.

Pater, Ruth H.↗

A review of high-temperature adhesives

The development of high temperature adhesives and polyphenylquinoxalines (PPQ) is reported. Thermoplastic polyimides and linear PPQ adhesive are shown to have potential for bonding both metals and composite structures. A nadic terminated addition polyimide adhesive, LARC-13, and an acetylene terminated phenylquinoxaline (ATPQ) were developed. Both of the addition type adhesives are shown to be more readily processable than linear materials but less thermooxidatively stable and more brittle. It is found that the addition type adhesives are able to perform, at elevated temperatures up to 595 C where linear systems fail thermoplastically.

St.clair, A. K.↗

An investigation of physical properties of thermoplastic polyimides

Thermoplastic polyimides are a class of promising high temperature polymers for aerospace applications. NASA-developed LARC-TPI is a prominent member of this family of polymers. Its physical characteristics have been measured as a function of its curing schedule. The results and their possible interpretations are discussed.

Singh, Jag J.↗

New high-temperature flame-resistant resin matrix for RP/C

The processing parameters of graphite composites utilizing graphite fabric and epoxy or other advanced thermoset and thermoplastic resins as matrices are discussed. The evaluated properties include anaerobic char yield, limiting oxygen index, smoke evolution, moisture absorption, and high-temperature mechanical properties. It is shown that graphite composites having the highest char yield exhibit optimum fire-resistant properties.

Kourtides, D. A.↗

Castable Amorphous Metal Mirrors and Mirror Assemblies

A revolutionary way to produce a mirror and mirror assembly is to cast the entire part at once from a metal alloy that combines all of the desired features into the final part: optical smoothness, curvature, flexures, tabs, isogrids, low CTE, and toughness. In this work, it has been demonstrated that castable mirrors are possible using bulk metallic glasses (BMGs, also called amorphous metals) and BMG matrix composites (BMGMCs). These novel alloys have all of the desired mechanical and thermal properties to fabricate an entire mirror assembly without machining, bonding, brazing, welding, or epoxy. BMGs are multi-component metal alloys that have been cooled in such a manner as to avoid crystallization leading to an amorphous (non-crystalline) microstructure. This lack of crystal structure and the fact that these alloys are glasses, leads to a wide assortment of mechanical and thermal properties that are unlike those observed in crystalline metals. Among these are high yield strength, carbide-like hardness, low melting temperatures (making them castable like aluminum), a thermoplastic processing region (for improving smoothness), low stiffness, high strength-to-weight ratios, relatively low CTE, density similar to titanium alloys, high elasticity and ultra-smooth cast parts (as low as 0.2-nm surface roughness has been demonstrated in cast BMGs). BMGMCs are composite alloys that consist of a BMG matrix with crystalline dendrites embedded throughout. BMGMCs are used to overcome the typically brittle failure observed in monolithic BMGs by adding a soft phase that arrests the formation of cracks in the BMG matrix. In some cases, BMGMCs offer superior castability, toughness, and fatigue resistance, if not as good a surface finish as BMGs. This work has demonstrated that BMGs and BMGMCs can be cast into prototype mirrors and mirror assemblies without difficulty.

Hofmann, Douglas C.↗

LARC-TPI: A multi-purpose thermoplastic polyimide

A linear thermoplastic polyimide, LARC-TPI, was characterized and developed for a variety of high temperature applications. In its fully imidized form, this material can be used as an adhesive for bonding metals such as titanium, aluminum, copper, brass, and stainless steel. LARC-TPI was evaluated as a thermoplastic for bonding large pieces of polyimide film to produce flexible, 100 void-free laminates for flexible circuit applications. The development of LARC-TPI as a potential molding powder, composite matrix resin, high temperature film and fiber is also discussed.

St.clair, A. K.↗

Reinforcing of thermoplastic polycarbonate and polysulfone with carbon fibers: Production and characteristics of UD-compound objects

The production and characteristics of the carbon fiber reinforced thermoplastics polycarbonate and polysulfone are described. The production of prepregs from defined polymer solutions is emphasized along with methods of optimizing the production of compounds. The characteristics of unidirectionally reinforced thermoplastics, such as shear strength, bending strength, and impact resistance are compared with regard to fracture behavior, the influence of intermediate layers, and the behavior under cryogenic conditions and under slightly elevated temperatures. The problem of adhesion between high strength carbon fibers and thermoplastics is examined, taking into account the effect of moisture on the shear strength and the impact resistance.

Fitzer, E.↗

Fiber reinforced thermoplastic resin matrix composites

Polyimide polymer composites having a combination of enhanced thermal and mechanical properties even when subjected to service temperatures as high as 700.degree. F. are described. They comprise (a) from 10 to 50 parts by weight of a thermoplastic polyimide resin prepared from 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane and (b) from 90 to 50 parts by weight of continuous reinforcing fibers, the total of (a) and (b) being 100 parts by weight. Composites based on polyimide resin formed from 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane and pyromellitic dianhydride and continuous carbon fibers retained at least about 50% of their room temperature shear strength after exposure to 700.degree. F. for a period of 16 hours in flowing air. Preferably, the thermoplastic polyimide resin is formed in situ in the composite material by thermal imidization of a corresponding amide-acid polymer prepared from 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane. It is also preferred to initially size the continuous reinforcing fibers with up to about one percent by weight of an amide-acid polymer prepared from 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane. In this way imidization at a suitable elevated temperature results in the in-situ formation of a substantially homogeneous thermoplastic matrix of the polyimide resin tightly and intimately bonded to the continuous fibers. The resultant composites tend to have optimum thermo-mechanical properties.

Jones, Robert J.↗

A multi-purpose thermoplastic polyimide

A linear thermoplastic polyimide, LARC-TPI, has been characterized and developed for a variety of high-temperature applications. In its fully imidized form, this new material can be used as an adhesive for bonding metals such as titanium, aluminum, copper, brass, and stainless steel. LARC-TPI is being evaluated as a thermoplastic for bonding large pieces of polyimide film to produce flexible, 100% void-free laminates for flexible circuit applications. The further development of LARC-TPI as a potential molding powder, composite matrix resin, high-temperature film and fiber will also be discussed.

Saint Clair, A. K.↗

A multi-purpose thermoplastic polyimide

A linear thermoplastic polyimide, LARC-TPI, has been characterized and developed for a variety of high-temperature applications. In its fully imidized form, this new material can be used as an adhesive for bonding metals such as titanium, aluminum, copper, brass, and stainless steel. LARC-TPI is being evaluated as a thermoplastic for bonding large pieces of polyimide film to produce flexible, 100% void-free laminates for flexible circuit applications. The further development of LARC-TPI as a potential molding powder, composite matrix resin, high-temperature film and fiber is also discussed.

Saint Clair, A. K.↗

High performance thermoplastics: A review of neat resin and composite properties

A review was made of the principal thermoplastics used to fabricate high performance composites. Neat resin tensile and fracture toughness properties, glass transition temperatures (Tg), crystalline melt temperatures (Tm) and approximate processing conditions are presented. Mechanical properties of carbon fiber composites made from many of these thermoplastics are given, including flexural, longitudinal tensile, transverse tensile and in-plane shear properties as well as short beam shear and compressive strengths and interlaminar fracture toughness. Attractive features and problems involved in the use of thermo-plastics as matrices for high performance composites are discussed.

Johnston, Norman J.↗

Development of a composite geodetic structure for space construction, phase 1A

The development of a geodetic beam and beam builder for on orbit construction of large truss type space structures is discussed. The geodetic beam is a lightweight, open lattice structure composed of an equilateral gridwork of crisscrossing rods. The beam provides a high degree of stiffness and minimizes structural distortion, due to temperature gradients, through the incorporation of a new graphite and glass reinforced thermoplastic composite material with a low coefficient of thermal expansion. A low power consuming, high production rate, beam builder automatically fabricates the geodetic beams in space using rods preprocessed on Earth. Three areas of the development are focused upon; (1) geodetic beam designs for local attachment of equipment or beam to beam joining in a parallel or crossing configurations, (2) evaluation of long life pultruded rods capable of service temperatures higher than possible with the HMS/P1700 rod material, and (3) evalaution of high temperature joint encapsulant materials.

Source record↗

Polyimides Made From 4,4'-Isophthaloyldiphthalic Anhydride

High-performance, thermoplastic, amorphous, and semicrystalline materials obtained. In experiments, twelve high-temperature, high-performance polyimide compositions based on 4,4'-isophthaloyldiphthalic anhydride (IDPA) prepared and characterized. Tough, film-forming, polyimides insoluble in organic solvents obtained in most cases. Three materials semicrystalline. Materials offer potential for development of semicrystalline polyimides having enhanced resistances to solvents and caustic chemicals, higher tensile strengths and moduli, enhanced thermo-oxidative stabilities below their melting temperatures, and enhanced melt processability, especially when heated to melting temperatures. Several exhibited excellent long-term thermo-oxidative stability when subjected to isothermal thermogravimetric analysis (ITGA) at temperatures of 300 degrees C and 350 degrees C in air. One area of application, manufacturing of lighter and stronger aircraft and spacecraft structures.

Pratt, J. Richard↗

Hybrid Titanium Composite Laminates: A New Aerospace Material

In the realm of aerospace design and performance, there are few boundaries in the never-ending drive for increased performance. This thirst for ever-increased performance of aerospace equipment has driven the aerospace and defense industries into developing exotic, extremely high-performance composites that are pushing the envelope in terms of strength-to-weight ratios, durability, and several other key measurements. To meet this challenge of ever-increasing improvement, engineers and scientists at NASA-Langley Research Center (NASA-LaRC) have developed a high-temperature metal laminate based upon titanium, carbon fibers, and a thermoplastic resin. This composite, known as the Hybrid Titanium Composite Laminate, or HTCL, is the latest chapter in a significant, but relatively short, history of metal laminates.

Johnson, W. S.↗

Thermal Conductivity Estimation from Transient Test Data with Embedded Thermocouples using Genetic Algorithm Optimization

Inverse heat transfer methodology previously developed to estimate thermal properties of high temperature fibrous insulation from embedded thermocouples was applied to the thermoplastic polymer, polyether-ether-ketone (PEEK). A small experimental setup was utilized to test the PEEK sample between temperatures of 300 K and 525 K at atmospheric pressure. Cylindrical plugs of PEEK with three thermocouples embedded at various depths were incorporated in the test sample. The experimental PEEK thermocouple data were used as the boundary and initial conditions of a one-dimensional numerical thermal model to predict the internal temperatures of the material. The thermal conductivity of PEEK was estimated with the Continuous Genetic Algorithm optimization technique by searching for the coefficients of a functional form of thermal conductivity that minimized the difference between the experimentally measured and model predicted internal temperature values. The thermal testing, one-dimensional numerical thermal model, optimization algorithm, analysis, and results are presented.

Thermal Properties↗

Toughened High-Temperature Thermoset Composites

Laminated composites of carbon fibers and either PMR-15 or LARC(TM)RP-46 polyimides toughened selectively by incorporating thin layers of Matrimid(TM) 5218 thermoplastic polyimide at interfaces between plies to form gradient semi-interpenetrating microstuctures. Toughening of composites accompanied by acceptably small decreases in strength and stiffness. Thick laminates of toughened composites fabricated easily at 500 psi. Materials useful in components of aircraft engines, where exposed to high temperatures for short times.

Johnston, Norman J.↗

High performance thermoplastics - A review of neat resin and composite properties

A review was made of the principal thermoplastics used to fabricate high performance composites. Neat resin tensile and fracture toughness properties, glass transition temperatures (Tg), crystalline melt temperatures (Tm) and approximate processing conditions are presented. Mechanical properties of carbon fiber composites made from many of these thermoplastics are given, including flexural, longitudinal tensile, transverse tensile and in-plane shear properties as well as short beam shear and compressive strengths and interlaminar fracture toughness.

Johnston, Norman J.↗