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Efficient synthesis of analytically-pure metal (II) 4,4',4'',4''' tetraaminophthalocyanine demonstrated in experiments. Typical Polymerization proceeds in two steps: First, reaction with 3,3',4,4'' -benzophenonetetracarboxylic dianhydride. Second step cyclodehydration. New polymers expected useful in formulation of thermally stable varnishes, adhesives, and fibers.
Useful physical and chemical properties observed in compounds obtained by thermally-induced melt polymerization of maleimido-phenoxy cyclotriphosphazenes linked through hexafluoroisopropylidene-diphthalimide groups. Polymers exhibit high strength, high thermal stability, and high char yields, and appear to be excellent candidates for fabricating composite materials.
Amine terminated bisaspartimides are prepared by a Michael type reaction of an aromatic bismaleimide and an aromatic diamine in an aprotic solvent. These bisaspartimides are thermally polymerized to yield tough, resinous polymers crosslinked through -NH- groups. Such polymers are useful in applications requiring materials with resistance to change at elevated temperatures.
A soluble aromatic poly(amic acid) film was converted to a soluble polyimide by staging at 25 deg intervals to 325 C and characterized at each interval by several analytical methods. The behavior observed was consistent with an interpretation that a reduction occurred in molecular weight of the poly(amic acid) during the initial stages of cure before the ultimate molecular weight was achieved as a polyimide. This interpretation was supported by the results of solution viscosity, gel permeation chromatography, low angle laser light scattering photometry and infrared spectroscopy analysis. The results serve to increase the fundamental understanding of how polyimides are thermally formed from poly(amic acids).
New synthesis results in improved class of tough, thermally stable polyimides containing amide linkages. Linear, aromatic, polyimide/amides synthesized from isomers of DABA with 3, 3', 4, 4'- BTDA. Mechanical properties better than those of LARC-TPI polyimide. Potentially useful as matrix resins in graphite-reinforced structures, and as fibers or coating films withstanding high temperatures.
A soluble aromatic poly(amic acid) film was converted to a soluble polyimide by staging at 25 deg intervals to 325 C and characterized at each interval by several analytical methods. The behavior observed was consistent with an interpretation that a reduction occurred in molecular weight of the poly(amic acid) during the initial stages of cure before the ultimate molecular weight was achieved as a polyimide. This interpretation was supported by the results of solution viscosity, gel permeation chromatography, low angle laser light scattering photometry and infrared spectroscopy analysis. The results serve to increase the fundamental understanding of how polyimides are thermally formed from poly(amic acids).
Fully-cured aromatic polyimides were prepared from various combinations of five dianhydrides and six diamines. When heated progressively under constant load, most of the films elongated rapidly near their glass transition temperatures. In about half of the nineteen materials, the strain was self-limiting - a possible indication of strain-induced crystallinity. The presence of crystallinity was established unambiguously for one material.
The durability of titanium (Ti) alloys bonded with high temperature adhesives such as polyimides has failed to attain the level of performance required for many applications. The problem to a large part is attributed to the instability of the surface treatment on the Ti substrate. Although Ti alloy adhesive specimens with surface treatments such as chromic acid anodization, Pasa-Jell, Turco, etc. have provided high initial mechanical properties, these properties have decreased as a function of aging at ambient temperature and faster, when aged at elevated temperatures or in a hot-wet environment. As part of the High Speed Civil Transport program where Ti honeycomb sandwich structure must perform for 60,000 hours at 177 C, work was directed to the development of environmentally safe, durable Ti alloy surface treatments.
A novel series of polymers and copolymers based on a polyimide backbone with the incorporation of carbonate moieties along the backbone. The process for preparing these polymers and copolymers is also disclosed as is a novel series of dinitrodiphenyl carbonates and diaminodiphenyl carbonates. The novel polymers and copolymers exhibit high temperature capability and because of the carbonate unit, many exhibit a high degree of order and/or crystallinity.
Incorporation of PDMS moieties into a polyimide matrix lowered the surface energy resulting in enhanced adhesive interactions. Polyimide siloxane materials were generated using amine-terminated PDMS oligomers of different lengths to study changes in surface migration behavior, phase segregation, mechanical, thermal, and optical properties. These materials were characterized using contact angle goniometry, tensile testing, and differential scanning calorimetry. The surface migration behavior of the PDMS component depended upon the siloxane molecular weight as indicated by distinct relationships between PDMS chain length and advancing water contact angles. Similar correlations were observed for percent elongation values obtained from tensile testing, while the addition of PDMS reduced the modulus. High fidelity topographical modification via laser ablation patterning further reduced the polyimide siloxane surface energy. Initial particulate adhesion testing experiments demonstrated that polyimide siloxane materials exhibited greater abhesive interactions relative to their respective homopolyimides.
An aerogel and process of making the aerogel are provided. The aerogel is a polyimide aerogel having polyamide cross-links formed using a poly(maleic anhydride) cross-linker.
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The polyimide resin, LARC-160, was prepared from diethyl-3, 3', 4,4'-benzophenone tetracarboxylate, ethyl-5-norbornene-2,3-dicarboxylate and Jeffamine AP-22. The imidization reactions of NE and BTDE were studied by HPLC, C-13-NMR and IR. NE imidizes slowly at 12 C; BTDE imidizes when the resin is heated above 100 C. Both imidization reactions proceed directly to the imide. Neither amic acid is present in significant quantities at any stage of the imidization reactions. The monomer mixture was stored at 12 C for periods up to 14 months. The effects of resin aging at this temperature on the chemical composition of the resin monomer mixture and the imidized polymer formed on curing were investigated. Aging the resin monomer mixture has the effect of partially advancing the imidization reaction. The average size of the cured polymer increases slightly with resin age.
Phenylethynyl-containing reactive additive (PERA) compounds and mixtures have been found to be useful for improving the processability of oligomers, polymers, co-oligomers, and copolymers that contain phenylethynyl groups. The additives can be incorporated in different forms: A solution of an amide acid or an imide of a PERA can be added to a solution of phenylethynyl-containing oligomer, polymer, co-oligomer, or copolymer; or An imide powder of a PERA can be mixed with a dry powder of a phenylethynyl-containing oligomer, polymer, co-oligomer, or copolymer. The effect of a given PERA on the processability and other properties of the resin system depends on whether the PERA is used in the amide acid or an imide form. With proper formulation, the PERA reduces the melt viscosity of the resin and thereby reduces the processing pressures needed to form the adhesive bonds, consolidate filled or unfilled moldings, or fabricate fiber-reinforced composite laminates. During thermal cure, a PERA reacts with itself as well as with the phenylethynyl-containing host resin and thereby becomes chemically incorporated into the resin system. The effects of the PERA on mechanical properties, relative to those of the host resin, depend on the amount of PERA used. Typically, the incorporation of the PERA results in (1) increases in the glass-transition temperature (Tg), modulus of elasticity, and parameters that characterize behavior under compression, and (2) greater retention of the aforementioned mechanical properties at elevated temperatures without (3) significant reduction of toughness or damage tolerance. Of the formulations tested thus far, the ones found to yield the best overall results were those for which the host resin was the amide acid form of a phenylethynyl-terminated imide (PETI) co-oligomer having a molecular weight of 5,000 g/mole [hence, designated PETI-5] and a PERA denoted as PERA-1. PETI-5 was made from 3,3',4'4'-biphenyltetracarboxylic dianhydride, 3,4'-oxydianiline (3,4'-ODA), 1,3-bis(3-aminophenoxy) benzene (1,3-APB), and 4-phenylethynylphthalic anhydride (PEPA). PERA-1 was made from 3,5-diamino- 4.-phenylethynylbenzophenon and equimolar amounts of phthalic anhydride and PEPA. To make PERA-1 in the imide form, the aforementioned ingredients were processed by refluxing in glacial acetic acid. To make the amide form of PERA-1, the ingredients were reacted in N-methyl-2-pyrrolidinone (NMP) under nitrogen at a temperature of 23 C (see figure). On the basis of the processability and other properties, a blend comprising 20 weight percent of PERA-1 and 80 weight percent PETI-5 was selected for further evaluation. Relative to neat PETI-5, the blend exhibited an increase in Tg; improved processability; and comparable values of shear strength in adhesion to titanium panels, open-hole compressive properties, compression properties after impact, and resistance to microcracking.
The thermal imidization of a number of polyimide precursors in the form of powders, films, and prepregs was examined by an in situ diffuse reflectance-FTIR technique where infrared spectra were determined while the material was being heated. An analysis of these spectra revealed that, with the exception of one water soluble adhesive, each precursor developed an anhydride band around 1850 cm/cu during imidization. This band diminished in intensity during final stages of cure. Efforts were made to quantify the amount of anhydride in several samples. Evidence obtained could be interpreted to mean that poly(amic acid) resins undergo an initial reduction in molecular weight during imidization before recombining to achieve their ultimate molecular weights as polyimides. Several reports in the literature are cited to support this interpretation. This report serves both to document anhydride formation during imidization and to increase our fundamental understanding of how polyimides cure.
Organically modified montmorrrillonite clay, containing a long chain aliphatic quarternary ammonium cation, was used to prepare polyimide/organoclay hybrids. Several approaches were examined in an attempt to achieve fully exfoliated nanocomposites. These included simple mixing of the clay in a pre-made high molecular weight poly(amide acid) solution; simple mixing followed by sonication of the organoclay/poly(amide acid) solutions; and the preparation of high molecular weight poly(amide acid)s in the presence of the organoclay dispersed in N-methyl-2-pyrrolidinone (NMP). The best results were obtained using the in-situ polymerization approach. The resulting nanocomposite films (both amide acid and imide), containing 3-8% by weight of organoclay, were characterized by differential scanning calorimetry (DSC), dynamic thermogravimetric analysis (TGA), transmission electron microscopy (TEM), X-ray diffraction (XRD), and thin film tensile properties. A significant degree of dispersion was observed in the nanocomposite films of the amide acid and the imide. After thermal treatment of amide acid films to effect imidization, in both air and nitrogen, the films were visually darker than control films without clay and the level of clay dispersion appeared to have decreased. In the latter case, the separation between the layers of the clay decreased to a spacing less than that present in the original organoclay. These observations suggest that thermal degradation of the aliphatic quarternary ammonium cation occurred likely during thermal treatment to effect imidization and solvent removal. These thermal degradation effects were less pronounced when thermal treatment was performed under nitrogen. The polyimide/organoclay hybrid films exhibited higher room temperature tensile moduli and lower strength and elongation to break than the control films.