Abstract
We characterize the material properties of a woven, multi-layered, hyperelastic composite that is useful as an envelope material for high-altitude stratospheric airships and in the design of other large structures. The composite was fabricated by sandwiching a polyaramid Nomex® core, with good tensile strength, between polyimide Kapton® films with high dielectric constant, and cured with epoxy using a vacuum bagging technique. Uniaxial mechanical tests were used to stretch the individual materials and the composite to failure in the longitudinal and transverse directions respectively. The experimental data for Kapton® were fit to a five-parameter Yeoh form of nonlinear, hyperelastic and isotropic constitutive model. Image analysis of the Nomex® sheets, obtained using scanning electron microscopy, demonstrate two families of symmetrically oriented fibers at 69.3°± 7.4° and 129°± 5.3°. Stress-strain results for Nomex® were fit to a nonlinear and orthotropic Holzapfel-Gasser-Ogden (HGO) hyperelastic model with two fiber families. We used a linear decomposition of the strain energy function for the composite, based on the individual strain energy functions for Kapton® and Nomex®, obtained using experimental results. A rule of mixtures approach, using volume fractions of individual constituents present in the composite during specimen fabrication, was used to formulate the strain energy function for the composite. Model results for the composite were in good agreement with experimental stress-strain data. Constitutive properties for woven composite materials, combining nonlinear elastic properties within a composite materials framework, are required in the design of laminated pretensioned structures for civil engineering and in aerospace applications.
Keywords
Introduction
Woven composite materials, comprised of a laminated layer sandwiched between two functional coatings, have attractive attributes such as high strength, toughness, and are lightweight which permit wide usage in civil engineering and aerospace applications. Pretensioned membrane structures in building construction are dependent on the superior mechanical properties of composite materials in the design of long-span structures as canopy roofs. Laminated membrane materials are also employed in the hull or outer envelopes of high-altitude stratospheric airships (HAA) that help contain helium, serve as a protective coating from UV degradation, withstand challenging environments due to the varying temperatures and low pressure, and endure external aerodynamic loads during operation. The development of high strength and lightweight materials, combined with additional attributes of environmental resistance and low helium permeability, have garnered much attention in recent years in the design and fabrication of envelope materials for HAA. 1
Multi-layer flexible laminates in envelope construction are comprised of sandwich structures with tailored mechanical properties, desired gas retention ability, and environmental resistance. Woven single/multilayer synthetic fabrics are a popular choice for the hull materials due to their suitable strength to weight ratio. Polyamide (Nylon®), polyester (Dacron®/Kosa®), aramid (Kevlar®), liquid crystal (Vectran®), carbon (Thornel®), polyethylene (Spectra®), polyhydroquinone-di-imidazopyridine (M5®), and PBO (Zylon®) are some materials with superior strength, toughness, and weatherability that are suitable as envelope materials for HAA. Challenges with respect to UV resistance, difficulty in processing, low stretch, and moisture resistance continue to persist with some of these materials. 1 A combination of Nomex® as a core material, sandwiched between Kapton® HN films, is a promising recent direction in the development of HAA materials. 2 Nomex® is a polyaramid, consisting of orthotropic material symmetry, and has good flame resistance, thermal insulation and tensile strength. In contrast, Kapton® HN is an aromatic and isotropic polyimide with resistance to UV, has a high dielectric constant, and is resistant to helium leakage. These properties make Kapton® an attractive choice in the fabrication of the outer layers of the composite in HAA applications.
Kapton® films undergo large deformations and are described using hyperelastic models. Phenomenological constitutive models, relating the micro-scale to macro-scale responses in composites, are described using a strain energy density function (SEF) based on strain invariants that account for the existing material symmetries in the materials.3,4 A constitutive theory for hyperelastic, fiber reinforced composites was first given assuming the fibers to be line elements and by applying kinematic constraints of fiber inextensibility and incompressibility. 5 Several studies have applied the differential fiber layouts to model fiber reinforced composites based on transversely isotropic symmetry. 6 Previous works by Polignone and Horgan, 7 Qui and Pence,8,9 Merodio and Pence, 10 and Merodio and Ogden11–14 modelled fiber reinforced composites with transverse isotropic symmetry using a form of strain energy function based on a sub-class of strain invariants, I1 and I4. Specifically, the strain energy function consisted of one term, corresponding to the matrix contribution and included as a neo-Hookean term with I1 dependence, and a second that accounted for fiber reinforcement, in terms of invariant I4, along a specific direction. Constitutive models, such as Holzapfel-Gasser-Ogden (HGO) for fiber reinforced tissues like arteries and the myocardium,15,16 are also widely used and have been applied to glass fiber reinforced thermoplastic composites with transversely isotropic symmetries. 17 These models have widespread application in modelling mechanical operations that warrant large deformations, such as hemispherical punch forming in glass fiber reinforced thermoplastic composites, 18 double dome forming procedures, 19 thermoforming processes using glass/polypropylene prepegs, 20 and the assembly process for non-rigid parts involving multilayered carbon fiber reinforced thermoplastics composites. 21 Kinematic constraints of fiber inextensibility and incompressibility are useful to reduce the number of constants that are required to assess the form of the functional in fiber reinforced materials that undergo large deformations. 22 Material incompressibility is applicable in rubber-like materials and tissues that demonstrate negligible volumetric changes under deformation.
We fabricated a multilayered composite using Kapton® films sandwiched between Nomex® calendared paper and tested the materials under uniaxial tensile loads. We used a five-parameter incompressible Yeoh model 23 to describe the constitutive properties of Kapton® based on the experimentally obtained data. Scanning electron microscopy images of Nomex® clearly show two symmetrically oriented fibers families with fiber angles 69.3°± 7.4° and 129°± 5.3° respectively. We used a modified form of the HGO model to describe the orthotropic material symmetry of Nomex®. Finally, we used the rule of mixtures to obtain the constitutive model for the Kapton®-Nomex®-Kapton® composite using the energy superposition principle. Unknown coefficients to the model were estimated using experimental data from uniaxial testing of the Kapton® films, Nomex® sheet, and the composite material. The methods established in this study are a first step to obtain the mechanical responses of composites undergoing large deformations and can also be extended to multifunctional materials and structures that show much potential in the areas of structural health monitoring and smart actuation of control surfaces.
Materials and methods
The materials used in this study are Kapton® HN polyimide film, Nomex® and a composite with Nomex® sandwiched as the core material between Kapton® films. Mechanical tests were conducted to characterize the stress – strain behaviors under uniaxial monotonic loading conditions.
Material symmetry characterization for Nomex®
Material characterization was performed using scanning electron microscopy (ULTRA 55, Zeiss, Germany) on a 0.5 mm thick Nomex® sheet cut using a high precision microtome. Figure 1(a) and (b) show representative micrographs, imaged under 324X and 744X magnification respectively, that clearly demonstrate two families of ∼20 µm diameter fibers with near symmetric layouts. The background matrix was excluded, the fiber images binarized, and the orientation angles were quantified using Hough transform (MATLAB R 2016 b, The Mathworks, Inc., Natik, MA). 30 binarized images of the sample at various locations were used to obtain the overall angular orientation vector, split into bins of size 5°, for Nomex®. The probability distribution of the fiber angles with orientation was plotted (Figure 1(c)) and the results fitted to a bimodal Gaussian distribution function (Figure 1(d)) for each of the two fiber families. We obtained an angular mean and standard error (SEM) to be 69.3°± 7.4° for one fiber family and 129°± 5.3° for the other family.

(a) and (b) Scanning electron micrograph of Nomex® at 324X and 744X magnifications show two families of fibers in the matrix. Scale 20 µm. c. Binarized images of the two fibers were obtained using image processing. d. The angular distributions for the two peaks in Nomex® corresponding to the two fiber families are shown. A Gaussian fit was used to obtain the average angles for the two peaks.
Fabrication of composites using Nomex® and Kapton®
Kapton® films were cut from a large sheet minimizing notches at the edges. Nomex® was cut in two orthogonal directions, as indicated by the supplier, corresponding to the longitudinal and transverse directions. Composites were fabricated by sandwiching Nomex® core between two sheets of Kapton® HN using epoxy (Araldite LY 5052: Epoxy Phenol Novolac resin mixed with a hardener HY 5052; Huntsman, Switzerland). The resin and hardener were mixed in 138:38 ratio using a glass rod in an acetone-cleaned container. Air bubbles were removed by applying vacuum for 5–10 minutes.
A smooth Teflon® surface, sprayed with mold release, was used to fabricate composites in this study. The Kapton® film was placed on the surface over which the epoxy solution was uniformly spread using a hand roller. The Nomex® film was gently placed using a hand lay-up technique and the same procedure repeated with a second Kapton® film. The setup was vacuum bagged to remove trapped air bubbles and the composite was cured by placing a 5 kg block for over 12 hours. The cured sandwich composite was cut along the longitudinal and transverse directions in Nomex® as described earlier. The volume fractions of Kapton®,
Aluminum end tabs were attached and used to grip samples to the stretcher (Figure 2). Sample dimensions and other relevant details are given in Table 1.

Uniaxial tensile specimens of Kapton® film (1), Nomex® sheet (2), and the composite structure (3). Scalebar: 10 mm.
Sample test conditions used to test Kapton®, Nomex®, and composite specimens in the study.
Mechanical testing
The Nomex® and composite specimens were cut to specified dimensions in the longitudinal and transverse directions, as indicated by the supplier, for uniaxial tensile tests. Kapton® was tested using a planar biaxial testing machine (Bangalore Integrated System Solutions (P) Ltd, India) with custom made clamps and a 25 lbf load cell (Model: WMC-25, Interface Inc., Arizona, USA, 11340 gm). Nomex® and the composite were also tested on a uniaxial testing machine (Makron 25; Bangalore Integrated System Solutions (P) Ltd, India with 25 kN Model Bi-06-105 load cell). The test sample was clamped using a hydraulic grip system to apply a uniform pressure of 180–200 kPa and tested to failure (n = 3 for all groups) under displacement control using strain rates listed in Table 1.
The components of the first Piola-Kirchhoff stresses,
Marker beads in the central gage region in the specimens were tracked and the Green-Lagrange strains were quantified using custom code based on iso-parametric mapping in MATLAB R2016b.24,25 Poisson’s ratio was computed using the linear range (up to 4%) of the stress-strain curve for all the Nomex®, Kapton® and composite materials.
Constitutive model descriptions for finite elastic and incompressible materials in the study
The strain energy density function (SEF),
Various forms of
The constants, ci, i = 1:5, were determined by fitting experimental results to the model.
We used an orthotropic material symmetry to describe the strain energy function for the Nomex® sheet based on the presence of two symmetrically placed fiber families along directions
We use an additive decomposition of the SEF based on an isotropic contribution from the matrix and an anisotropic component due to the presence of fibers.
Such a form of SEF is commonly used to describe arterial tissues, the myocardium, and other materials that have defined fibers in different orientations.15,28
We used a modified HGO model to describe Nomex® given by
We enforce polyconvexity of the SEF by imposing constraints on the unknown material constants in equations (4) and (7) by
A right-handed Cartesian coordinate system was introduced along the principal material axes corresponding to the longitudinal and transverse directions. The unit vectors along two fiber directions in Nomex® are given by
Let
The constitutive equation for the composite, fabricated using a Nomex® core sandwiched between sheets of Kapton®, was given using the rule of mixtures. The SEF for the composite is given by
Cauchy stresses for the composite material under uniaxial stretch are calculated as
Experimentally obtained stresses were fit to the computed stresses for Kapton® (equation (10a)), Nomex® (equation (10b)), and the composite (equation (12)) using a nonlinear Levenberg-Marquardt optimization algorithm implemented using the ‘fmincon’ function in MATLAB. The differences between experimentally obtained Cauchy stresses in (
At least five different initial values were used in the nonlinear optimization to ensure that the converged solution corresponded to the global minimum. The optimization was terminated when either a tolerance value of 1E-08 on the objective function was reached or a value of 1E-06 applied on the estimated parameter values. The solution with a maximum
Results and discussion
Uniaxial test results
Figure 3 shows uniaxial stress-stretch plots in the longitudinal and transverse directions for Kapton® (isotropic), Nomex®, and the composite specimens (n = 3 for each group). Results for Kapton® films show nonlinear rubber-like large deformations in both the tested directions. These results confirm that Kapton may be modeled as an isotropic material. In contrast, there are clear differences in the mechanical responses of Nomex® in the longitudinal and transverse directions with the longitudinal direction stiffer than the transverse. The mechanical properties of composite are hence dominated by Nomex® in both directions. The composite has an intermediate response to that of Kapton® and Nomex® in the longitudinal direction. There are however no differences between the composite and the Nomex® in the transverse direction.

Variations in the Cauchy stress with stretch obtained from uniaxial stretching of Kapton®, Nomex®, and composite samples are shown corresponding to (a) longitudinal and (b) transverse directions. n = 3 for each group tested in the study. Samples were cut based on markings provided by the manufacturer.
The composite and Nomex® samples have near linear initial response of∼4% stretch and are followed by non-linear response until failure. We used these results to compute the elastic moduli, Poisson’s ratio, and the maximum stretch to failure in the two directions for all the samples in the study (Figure 4). The elastic moduli, reported as Mean ± Std., were significantly different in the longitudinal (2.86 ± 0.36 GPa; p < 0.05) direction as compared to the transverse (1.70 ± 0.10 GPa) direction for Nomex® samples (Figure 4(a)). Modulus in the longitudinal direction was 1.68 times higher as compared to the transverse direction. The elastic modulus of Kapton® was 2.00 ± 0.08 GPa. Similar differences were seen in the moduli of the composite in the longitudinal (2.80 ± 0.08 GPa) and transverse (1.76 ± 0.04 GPa) directions as compared to the corresponding directions in the Nomex® samples. A higher contribution from Nomex® samples is expected because of a higher volume fraction used during the composite fabrication.

Comparisons in the measured mechanical properties (Mean ± Std.) of Kapton®, Nomex® and composite in the longitudinal and transverse directions obtained using uniaxial mechanical experiments (n = 3). (a) Elastic moduli, (b) Poisson’s ratio and (c) percentage elongation.
Poisson’s ratios for Nomex® samples were higher in the longitudinal (0.46 ± 0.01) as compared to the transverse (0.40 ± 0.02) direction (p < 0.05) (Figure 4(b)). There were no significant differences in the Poisson’s ratio values for composite samples in the longitudinal direction (0.43 ± 0.02) as compared to the transverse direction (0.40 ± 0.02). Finally, Kapton® specimens had values of 0.37 ± 0.01 which is significantly lower than that for rubber-like materials. Figure 4(c) shows the percentage elongation at rupture for all the materials. There was higher variability in the values reported for the composites that demonstrate the importance of the fabrication process in the overall mechanical behavior of the composite.
Uniaxial tensile tests are useful in quantifying properties, such as elastic modulus, Poisson’s ratio, elongation at break, etc., of the Nomex® and sandwich composites in our study. We show that the stress-strain results obtained from uniaxial tests on samples, oriented in the longitudinal and transverse directions respectively, may be used to estimate the role of fiber orientations in the overall material behaviors of composites. Kapton® is primarily important as a gas barrier in the fabrication of composites for HAA applications as compared to Nomex® that is useful in the structural properties. Combining both these materials in the sandwich construction hence offers several advantages that are not seen in the individual materials for the construction of HAA. Such materials, with high specific modulus and gas diffusion properties, make them suitable for HAA applications.
Verification of constitutive models with experimental data for materials in the study
A five-parameter isotropic and incompressible Yeoh model was used for Kapton® samples (equation (4)). In contrast, an incompressible HGO form of constitutive model (equation (7)) was used to fit the Nomex® data in either the longitudinal or the transverse directions based on the inclusion of two symmetrically orientated fiber families at

Experimental stress-stretch data for a representative Kapton® sample were fit to an incompressible five parameter Yeoh model (equation (4); r2=0.999).
Unknown constants to material model for Kapton® were obtained by fitting a five parameter Yeoh model (equation (4)) to the experimentally obtained uniaxial data.
Modified HGO model fits for a representative Nomex® sample are shown in Figure 6 and the constants from tested specimens in the longitudinal and transverse directions (n = 3) are listed in Table 3. In addition to the unknown material constants, values of fiber orientations (±

Results from a representative sample of Nomex®, tested in the longitudinal (r2=0.996) and transverse (r2=0.993) directions, were fit to an incompressible modified HGO model (equation (7)).
Modified HGO model constants (equation (7)) were estimated by fitting the uniaxial experimental results for Nomex® in the longitudinal (L) and transverse (T) directions.
L: longitudinal T: transverse.
aWith reference to longitudinal direction.

A rule of mixtures model was used to obtain the properties of the composite laminate (equation (12)) using the individual properties of Nomex® and Kapton®. Experimental data from the (a) longitudinal (n = 3) and (b) transverse (n = 3) directions obtained for the composite materials (n = 3) with model fits are shown below (r2=0.91for both). (Mean ± Std.) used in the plots below.
Constitutive models for fiber reinforced composites are essential to predict the mechanical behavior under different loading conditions. Macro-scale models represent the composite material with average properties. In contrast, micromechanical models are based on the microstructure and constitutive properties of the elemental constituents like the matrix and fibers. Such approaches use homogenization techniques to estimate the effective mechanical properties of the composite us the using the individual contributions of the constituents and fiber-matrix interactions. Micromechanical models based on theories, such as the Hashin-Roshen model, Mori-Tanaka model, or the self-consistent models, are also useful in this context to estimate of the composite properties more accurately.29–31
Constitutive models for fiber reinforced composites in the literature were obtained by superposing the stress-strain responses of the constituent fiber and matrix.32–34 Aboshio and colleagues 32 calculated the strain energy density by integrating the stress-strain curves and estimated the material parameters using the strain energy density versus invariant plots. Homogenization techniques to estimate the material properties of multi-layered, thick laminate composites undergoing small strains are based on force-deformation equivalence with strain equality at the interfaces.35–37 Other micromechanical approaches include material heterogeneities at smaller scales and volume average the constitutive behavior of each phase to obtain the effective stress and strain potentials for the composite.38,39 We used a linear superposition of the strain energy function for each individual material within a macroscopic rule of mixtures model and have neglected the interfacial stress discontinuities to quantify the overall mechanical properties of the composite. The strain energy of the composite is lower than the sum of the strain energies of the individual components associated with Kapton® and Nomex®. Because the strain energy function is continuous throughout the deformation regime, we show that the rule of mixtures provides an upper bound to the mechanical properties of composite, not only in the linear regime but also in the non-linear part. Earlier studies by Aboshio and co-workers 32 have used a similar approach based on the volume fractions of individual constituents in obtaining the mechanical properties of composite in the entire deformation regime. Such models are useful to obtain the envelope material in HAA which withstands the pressure differences between the interior and the exterior of the ship and maintains the desired aerodynamic configuration during lift. The constitutive model for the honey-comb structure of Nomex® is also useful in analyzing helicopter blades under different loading conditions. Methods used in the current study may be extended to equibiaxial and non-equibiaxial tensile tests to gain additional insights into the constitutive properties of sandwich composites that leverage direction dependent responses for specific applications. Determination of shear strength and tear resistance are other important criteria which will be required for such applications.
Conclusions
We fabricated a multi-layered composite using a Nomex® sheet sandwiched between Kapton® HN films with epoxy and vacuum bagging technique. The constitutive properties of the composite were obtained using a continuum mechanical framework and experimental results from uniaxial experiments. A five-parameter incompressible Yeoh model fit the stress - strain responses of Kapton® films. SEM images show two distinct families of symmetrically oriented fibers in the matrix of Nomex®. An incompressible, two fiber family, modified HGO model was used to quantify the material responses of Nomex®. The fiber orientation angles, estimated using the model for Nomex®, are in good agreement with data obtained from the analysis of SEM images. The material properties of Nomex® sheet dominate the stress-strain responses of the composite laminate. A constitutive model for the composite was obtained using a rule of mixtures model and a linear decomposition of the strain energy function based on individual components in the laminate structure. The theoretically obtained stress-strain results agree with experimental data. These results are useful in the design of composite laminates in engineering applications that undergo large deformation.
Footnotes
Acknowledgements
We thank Nimesh R. Chahare for help with mechanical tests. We also thank the MNCF lab staff members, CeNSE department, IISc for help with scanning electron microscopy.
Declaration of Conflicting Interests
The author(s) declared no potential conflicts of interest with respect to the research, authorship, and/or publication of this article.
Funding
The author(s) received no financial support for the research, authorship, and/or publication of this article.
