Facile method for fabricating atomic oxygen resistant polyimide films with excellent optical homogeneity containing hyperbranched polysiloxane

2020 ◽  
pp. 095400832097278
Author(s):  
Gang Lv ◽  
Songpei Xie ◽  
Danbo Mao ◽  
Ge Ren ◽  
Shibin Wu ◽  
...  
Keyword(s):  
Atomic Oxygen ◽  
Protective Layer ◽  
Solid Content ◽  
Low Earth Orbit ◽  
Polyimide Films ◽  
Optical Elements ◽  
Elongation At Break ◽  
Thickness Uniformity ◽  
Hyperbranched Polysiloxane

Mechanically robust optical homogeneous polyimide (PI) films with desirable atomic oxygen (AO) erosion duration were fabricated by initially synthesizing amine-functionalized hyperbranched polysiloxane (NH2-HBPSi), then reinforcing the pristine polyimide skeleton with it via copolycondensation reactions. NH2-HBPSi macromolecule imparts desirable AO survivability to the resulting hybrids. The mass loss per unit area of hybrid films had a downward trend with rising NH2-HBPSi content and AO dose before the complete silica protective layer was formed. It has been proven by the experiments in an underground simulated AO environment. It decreased to 1% of that of pristine polyimide when NH2-HBPSi accounted for 30% of the solid content after 24 h AO attack. The stable thickness uniformity that can meet the Rayleigh criterion was achieved in a 30 wt% HBPSi PI film, mainly due to the selection of the best process parameters. Meanwhile, 30 wt% HBPSi PI demonstrates satisfactory mechanical properties, with a tensile strength of 228.9 MPa and elongation at break of 7.3%. The characterization of scanning electron microscopy confirmed that pristine polyimide was substantially eroded after AO exposure while the surface morphology of 30 wt% HBPSi polyimide showed no evident change. The low AO erosion yield and prominent film thickness uniformity may find extensive usage in ultra-lightweight space diffractive optical elements (DOE) working in low earth orbit (LEO).

Atomic Oxygen Resistant Polysiloxane Coatings for Low Earth Orbit Space Structures

2015 ◽  
Vol 830-831 ◽  
pp. 699-702 ◽  
Author(s):  
G.N. Arjun ◽  
T.L. Lincy ◽  
T.S. Sajitha ◽  
S. Bhuvaneshwari ◽  
Thomas Deepthi ◽  
...  
Keyword(s):  
Reaction Time ◽  
Surface Morphology ◽  
Mass Loss ◽  
Atomic Oxygen ◽  
Thermo Gravimetric Analysis ◽  
Orbit Space ◽  
Solid Content ◽  
Low Earth Orbit ◽  
Gravimetric Analysis ◽  
Coating Materials

Polysiloxane resin copolymer was synthesized through acid catalyzed hydrolysis of methyl triethoxysilane (MTEOS) and diethoxytetramethyldisiloxane (DEOTMDS). The effect of reaction time on the properties of the polymer was studied and this copolymer was characterized by GPC, 29Si NMR, IR, TGA, viscosity, refractive index, specific gravity and solid content. 29Si NMR and IR showed characteristic signals of Si-O-Si linkage which confirmed the formation of the polymer. GPC and solid content analysis showed an increasing trend in molecular weight with reaction time. Thermo gravimetric analysis showed that the polymer was thermally stable upto ≈ 260°C and all the polymers gave a ceramic residue in the range of 77-80% at 900°C. Siloxane prepared inhouse and methyl phenyl silsequioxane (control) were used as coating materials and atomic oxygen (AO) resistance was evaluated on Al-Kapton, carbon polyimide composite and glass polyimide composite. The mass loss and surface morphology of the coated samples were measured at different time intervals. It is observed that mass loss of polysiloxane coated samples was very less, compared to coated control samples. The morphology of all the samples were studied using FESEM. Erosion kinetics and surface morphology investigation indicate that the polysiloxane coating possesses excellent AO resistance, and displays better cracking resistance on AO exposure.

Leveling Coatings for Reducing Atomic Oxygen Defect Density in Graphite Fiber-Epoxy Composites

1994 ◽  
Vol 37 (3) ◽  
pp. 26-31
Author(s):  
D. Jaworske ◽  
K. de Groh ◽  
G. Podojil ◽  
T. McCollum ◽  
J. Anzic
Keyword(s):  
Atomic Oxygen ◽  
Defect Density ◽  
Protective Coatings ◽  
Protective Layer ◽  
Oxide Coating ◽  
Low Earth Orbit ◽  
Earth Orbit ◽  
Protective Oxide ◽  
Low Viscosity ◽  
Defect Sites

Pinholes or other defect sites in a protective oxide coating provide pathways for atomic oxygen in low-Earth orbit to reach underlying material. Onc concept for enhancing the lifetime of materials in low-Earth orbit is to apply a leveling coating to the material prior to applying any reflective and protective coatings. Using a surface-tension-leveling coating concept, a low-viscosity epoxy was applied to the surface of several composite coupons. A protective layer of 1000 Å of SiO2 was deposited on top of the leveling coating, and the coupons were exposed to an atomic oxygen environment in a plasma asher. Pinhole populations per unit area were estimated by counting the number of undercut sites observed by scanning electron microscopy. Defect density values of 180,000 defects/cm2 were reduced to about 1000 defects/cm2 as a result of the applied leveling coating. These improvements occur at a mass penalty of about 2.5 mg/cm2.

Effects of Atomic Oxygen Irradiation on PDMS/POSS Hybrid Films in Low Earth Orbit Environment

2011 ◽  
Vol 239-242 ◽  
pp. 1368-1371 ◽  
Author(s):  
Mi Mi Song ◽  
Shu Wang Duo ◽  
Ting Zhi Liu
Keyword(s):  
Photoelectron Spectroscopy ◽  
Atomic Oxygen ◽  
Orbit Space ◽  
Low Earth Orbit ◽  
Hybrid Coating ◽  
Space Environment ◽  
Earth Orbit ◽  
Chemical Compositions ◽  
Hybrid Films ◽  
Polyimide Films

In order to improve the atomic oxygen (AO) erosion resistance of polyimide films in low earth orbit space environment, a type PDMS/POSS hybrid coating on polyimide substrate was prepared based on a silanol terminated polydimethylsiloxane (PDMS-OH) and Octakis(trimethylsiloxy)octaprismosilsesquioxane (Q8[Si(CH3)3]8) by copolymerizing process in DMAc solution. The atomic oxygen exposure tests were carried out using a ground-based atomic oxygen simulation facility. The mass loss, surface morphology and surface chemical compositions of PDMS/POSS hybrid films before and after exposure to incremental AO flux were investigated by using microbalance and field emission scanning electron microscopy (FE-SEM) and X-ray photoelectron spectroscopy (XPS), respectively. The data indicated that a silica-rich layer was formed on the surface of the hybrid coating when the coating is exposed to AO flux, which could provide a protective barrier on the surface preventing further degradation of the polymer during extended exposure to AO and obviously improved the AO resistance of polyimide films.

Atomic Oxygen Resistant Films for Multi-Layer Insulation

2000 ◽  
Vol 12 (1) ◽  
pp. 113-123 ◽  
Author(s):  
Peter Schuler ◽  
H Bob Mojazza ◽  
Ross Haghighat
Keyword(s):  
Atomic Oxygen ◽  
Vacuum Ultraviolet ◽  
Thermal Control ◽  
Radiation Stability ◽  
Low Earth Orbit ◽  
Space Environment ◽  
Advanced Materials ◽  
Validation Tests ◽  
Atomic Oxygen Erosion

A series of advanced polymer films from Triton Systems is being developed to meet the challenges of harsh space environmental effects, lighter weight requirements and superior thermal control performance demands. With support from NASA, Triton Systems Inc has developed advanced new materials for thermal control films with exceptional properties and durability in the space environment. These films known as TOR™ and TOR-LM™ are amber coloured, mechanically sound, produced in continuous rolls and have undergone substantial ground-based simulation and confirming space validation tests. These films are highly resistant to atomic oxygen erosion, and have excellent vacuum ultraviolet radiation stability in ground-based simulation tests. Two applications for these films include large inflatable structures that are either deployed in low earth orbit (LEO) or travel through a LEO orbit into higher orbits, and as outer metallized layers in multi-layer insulation (MLI) blankets. This paper discusses the processing of these advanced materials into thin films, metallization of the films and characterization of their environmental durability as well as other physical, optical, thermal and mechanical properties.

scholarly journals Preparation and Properties of Intrinsically Atomic-Oxygen Resistant Polyimide Films Containing Polyhedral Oligomeric Silsesquioxane (POSS) in the Side Chains

Polymers ◽  
2020 ◽  
Vol 12 (12) ◽  
pp. 2865 ◽  
Author(s):  
Hao Wu ◽  
Yan Zhang ◽  
Yi-Dan Guo ◽  
Hao-Ran Qi ◽  
Yuan-Cheng An ◽  
...  
Keyword(s):  
Atomic Oxygen ◽  
Linear Thermal Expansion ◽  
Polyhedral Oligomeric Silsesquioxane ◽  
Tensile Modulus ◽  
Low Earth Orbit ◽  
Molecular Structures ◽  
Polyimide Films ◽  
Passivation Layers ◽  
Pyromellitic Anhydride ◽  
Oligomeric Silsesquioxane

The relatively poor atomic-oxygen (AO) resistance of the standard polyimide (PI) films greatly limits the wide applications in low earth orbit (LEO) environments. The introduction of polyhedral oligomeric silsesquioxane (POSS) units into the molecular structures of the PI films has been proven to be an effective procedure for enhancing the AO resistance of the PI films. In the current work, a series of POSS-substituted poly (pyromellitic anhydride-4,4′-oxydianiline) (PMDA-ODA) films (POSS-PI) with different POSS contents were synthesized via a POSS-containing diamine, N-[(heptaisobutyl-POSS)propyl]-3,5-diaminobenzamide (DABA-POSS). Subsequently, the effects of the molecular structures on the thermal, tensile, optical, and especially the AO-erosion behaviors of the POSS-PI films were investigated. The incorporation of the latent POSS substituents decreased the thermal stability and the high-temperature dimensional stability of the pristine PI-0 (PMDA-ODA) film. For instance, the PI-30 film with the DABA-POSS content of 30 wt% in the film exhibited a 5% weight loss temperature (T5%) of 512 °C and a coefficient of linear thermal expansion (CTE) of 54.6 × 10−6/K in the temperature range of 50–250 °C, respectively, which were all inferior to those of the PI-0 film (T5% = 574 °C; CTE = 28.9 × 10−6/K). In addition, the tensile properties of the POSS-containing PI films were also deteriorated, to some extent, due to the incorporation of the DABA-POSS components. The tensile strength (TS) of the POSS-PI films decreased with the order of PI-0 > PI-10 > PI-15 > PI-20 > PI-25 > PI-30, and so did the tensile modulus (TM) and the elongations at break (Eb). PI-30 showed the TS, TM, and Eb values of 75.0 MPa, 1.55 GPa, and 16.1%, respectively, which were all lower than those of the PI-0 film (TS = 131.0 MPa, TM = 1.88 GPa, Eb = 73.2%). Nevertheless, the incorporation of POSS components obviously increased the AO resistance of the PI films. All of the POSS-PI films survived from the AO exposure with the total fluence of 2.16 × 1021 atoms/cm2, while PI-0 was totally eroded under the same circumstance. The PI-30 film showed an AO erosion yield (Es) of 1.1 × 10−25 cm3/atom, which was approximately 3.67% of the PI-0 film (Es = 3.0 × 10−24 cm3/atom). Inert silica or silicate passivation layers were detected on the surface of the POSS-PI films after AO exposure, which efficiently prevented the further erosion of the under-layer materials.

Characterization of Rh/Si multilayer structure by HREM and HAADF

1992 ◽  
Vol 50 (1) ◽  
pp. 122-123
Author(s):  
Y. Cheng ◽  
J. Liu ◽  
M.B. Stearns ◽  
D.G. Steams
Keyword(s):  
Normal Incidence ◽  
High Resolution Electron Microscopy ◽  
X Rays ◽  
Beam Direction ◽  
Cross Sectional ◽  
Optical Elements ◽  
Resolution Electron ◽  
Point To Point ◽  
Better Than

The Rh/Si multilayer (ML) thin films are promising optical elements for soft x-rays since they have a calculated normal incidence reflectivity of ∼60% at a x-ray wavelength of ∼13 nm. However, a reflectivity of only 28% has been attained to date for ML fabricated by dc magnetron sputtering. In order to determine the cause of this degraded reflectivity the microstructure of this ML was examined on cross-sectional specimens with two high-resolution electron microscopy (HREM and HAADF) techniques.Cross-sectional specimens were made from an as-prepared ML sample and from the same ML annealed at 298 °C for 1 and 100 hours. The specimens were imaged using a JEM-4000EX TEM operating at 400 kV with a point-to-point resolution of better than 0.17 nm. The specimens were viewed along Si [110] projection of the substrate, with the (001) Si surface plane parallel to the beam direction.

Preparation and Characterization of β-glucosidase Films for Stabilization and Handling in Dry Configurations

2020 ◽  
Vol 21 (8) ◽  
pp. 741-747
Author(s):  
Liguang Zhang ◽  
Yanan Shen ◽  
Wenjing Lu ◽  
Lengqiu Guo ◽  
Min Xiang ◽  
...  
Keyword(s):  
Tensile Strength ◽  
Protein Function ◽  
Protein Stabilization ◽  
Functional Protein ◽  
Elongation At Break ◽  
Gelatin Films ◽  
The Stability ◽  
And Function ◽  
General Method

Background: Although the stability of proteins is of significance to maintain protein function for therapeutical applications, this remains a challenge. Herein, a general method of preserving protein stability and function was developed using gelatin films. Method: Enzymes immobilized onto films composed of gelatin and Ethylene Glycol (EG) were developed to study their ability to stabilize proteins. As a model functional protein, β-glucosidase was selected. The tensile properties, microstructure, and crystallization behavior of the gelatin films were assessed. Result: Our results indicated that film configurations can preserve the activity of β-glucosidase under rigorous conditions (75% relative humidity and 37°C for 47 days). In both control films and films containing 1.8 % β-glucosidase, tensile strength increased with increased EG content, whilst the elongation at break increased initially, then decreased over time. The presence of β-glucosidase had a negligible influence on tensile strength and elongation at break. Scanning electron-microscopy (SEM) revealed that with increasing EG content or decreasing enzyme concentrations, a denser microstructure was observed. Conclusion: In conclusion, the dry film is a promising candidate to maintain protein stabilization and handling. The configuration is convenient and cheap, and thus applicable to protein storage and transportation processes in the future.

scholarly journals The Effect of Low Earth Orbit Atomic Oxygen Exposure on Phenylphosphine Oxide-Containing Polymers

2000 ◽  
Vol 12 (1) ◽  
pp. 43-52 ◽  
Author(s):  
John W Connell
Keyword(s):  
Thin Film ◽  
Atomic Oxygen ◽  
Low Earth Orbit ◽  
Space Environment ◽  
Earth Orbit ◽  
Cooperative Effort ◽  
Flight Experiment ◽  
Oxygen Exposure ◽  
Atomic Oxygen Exposure ◽  
Phenylphosphine Oxide

Thin films of phenylphosphine oxide-containing polymers were exposed to low Earth orbit aboard a space shuttle flight (STS-85) as part of flight experiment designated Evaluation of Space Environment and Effects on Materials (ESEM). This flight experiment was a cooperative effort between the NASA Langley Research Center (LaRC) and the National Space Development Agency of Japan (NASDA). The thin-film samples described herein were part of an atomic oxygen exposure (AOE) experiment and were exposed to primarily atomic oxygen (∼1×1019 atoms cm−2). The thin-film samples consisted of three phosphine oxide-containing polymers (arylene ether, benzimidazole and imide). Based on post-flight analyses using atomic force microscopy, x-ray photo-electron spectroscopy and weight loss data, it was found that the exposure of these materials to atomic oxygen (AO) produces a phosphorus oxide layer on the surface of the samples. Earlier work has shown that this layer provides a barrier towards further attack by AO. Consequently, these materials do not exhibit linear erosion rates which is in contrast with most organic polymers. Qualitatively, the results obtained from these analyses compare favourably with those obtained from samples exposed to AO and/or an oxygen plasma in ground-based exposure experiments. The results of the low Earth orbit AO exposure on these materials will be compared with those of ground-based exposure to AO.

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