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Article

PEBAX® 5533D Formulation for Enhancement of Mechanical and Thermal Properties of Material Used in Medical Device Manufacturing

by
Mildred Guillén-Espinoza
1,
Fabián Vásquez Sancho
2,
Ricardo Starbird-Perez
3 and
Roy Zamora-Sequeira
4,5,*
1
Master Program in Medical Devices Engineering, Instituto Tecnológico de Costa Rica, Cartago 30102, Costa Rica
2
Materials Research Science and Engineering Center (CICIMA), University of Costa Rica, San José 11501-2060, Costa Rica
3
Centro de Investigación y de Servicios Químicos y Microbiológicos (CEQIATEC), School of Chemistry, Instituto Tecnológico de Costa Rica, Cartago 30102, Costa Rica
4
School of Material Engineering, Instituto Tecnológico de Costa Rica, Cartago 30102, Costa Rica
5
Centro Nacional Especializado de la Industria Gráfica y del Plástico (CEGRYPLAST) of the National Learning Institute (INA), San José 5200, Costa Rica
*
Author to whom correspondence should be addressed.
J. Compos. Sci. 2024, 8(8), 314; https://doi.org/10.3390/jcs8080314
Submission received: 5 June 2024 / Revised: 12 July 2024 / Accepted: 16 July 2024 / Published: 9 August 2024
(This article belongs to the Section Polymer Composites)
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Abstract

:
The medical device industry is constantly innovating in the search for materials that demonstrate superior performance, better intrinsic characteristics, profitability, and a positive impact on potential patients. The thermoplastic polymer resin Pebax® 5533D is one of the most widely used commercial materials for manufacturing medical device parts due to its easy processability. However, its mechanical and thermal properties require improvements to mitigate identified manufacturing defects, such as a decrease in material flexibility, high susceptibility to moisture, and thermal degradation during processing. Therefore, this study integrated different materials, such as plasticizers and filler additives, to produce a polymer compound prototype formula as a solution technique to enhance the current material’s performance. Modifying mechanical and rheological properties allows to evaluate the impacts on the polymeric material’s flexibility and thermal behavior. This was achieved by processing mixed additives using injector-molding equipment to obtain equal-molded samples of every formula. In addition, material characterization was performed to determine the variations in the samples’ crystallization, flexural strength, and moisture content. Calcium stearate was determined to be the most significant component serving as a mechanical resistance modifier and thermal stabilizer alongside calcium chloride as a moisture content reducer combined with Pebax® 5533D.

Graphical Abstract

1. Introduction

Polymeric materials are widely used in medical devices across various applications, particularly in the production of medical plastic parts, such as extruded tubing or injection-molded pieces. The choice of the material used for the design and manufacturing of plastic parts mainly depends on the properties and characteristics of the raw materials required for a specific function of the final medical device component [1]. Therefore, the increasing production of various types of medical devices that incorporate plastic components is driving the growth of the polymeric raw material market, which is continually developing more advanced materials that can easily comply with the specification requirements needed by an end user for a medical device application [2]. These improved materials are usually composed of polymeric compound blends or composites containing several components comprising a material that is converted into the final product part. This type of conformed raw material is more likely to be used by medical part manufacturers, as this type of application is more reliable than using all raw materials separately, as most medical device-manufacturing companies aim to save money, reduce production times, and secure the quality of their products [2,3].
A series of defects have been found during the manufacturing of plastic parts made of polyether and polyamide resins, such as Pebax® 5533D used for medical catheters, including the materials’ fast degradability due to elevated levels of moisture absorption over time and bending problems that cause unwanted deformations in the final parts, which are related to the materials’ mechanical resistance, rheological properties, and thermal stability during and after processing [4,5]. Solutions are being sought at the level of productivity in processes dedicated solely to the manufacture of these plastic parts to reduce manufacturing costs, which are mostly attributed to adjustments in equipment or operational techniques. This may help reduce some defects but will not fully solve the problem. In most cases, the problem is caused by using a material that is functional to develop a device part during the design phase but is unprofitable in the part’s manufacture, which neglects the study of the material and how variations in its composition can determine the quality of the final product [6].
Therefore, it is of great interest to improve the material properties of Pebax® 5533D by developing a formulation using Pebax® as a base resin with a series of additive components, such as lubricants and plasticizers, e.g., calcium stearate, which can improve fluency and flexural strength at percentages between 0.5% and 1% due to its easy incorporation and strong lubricity properties at low concentration levels [7]. Calcium stearate is easily dispersible in polymers and shows good thermal stability at 200 °C, the melt processing temperature of most thermoplastic polymers [8,9]. In addition, this additive has been accepted by the FDA as a “generally recognized as safe” (GRAS) material and is approved for use as a lubricant and anti-adherent agent in several medical device formulations. Furthermore, using polyethylene glycol, a biocompatible, hydrophilic, flexible, and non-toxic type of polymer with high ductility and toughness [10], can improve the mechanical properties of Pebax®. A study determined that a maximum content of approximately 10% polyethylene glycol should be used according to the requested plasticizing grade. The study focused on determining polyethylene glycol’s ability to improve the flexibility level of Pebax® 5533D without making the compound too flexible, which would make it difficult to achieve the processability and plasticization grade of the usual resins used for medical part applications [11,12,13].
Meanwhile, polypropylene is extremely versatile as a mechanical reinforcement additive because of its toughness, flexibility, and heat and chemical resistance [14]. It was found that its content percentage should vary between 0% and 10% according to the compatibility between the polymers. Increased concentrations of polypropylene may hinder its successful incorporation and proper mixing and dispersion within the Pebax® 5533 polymer net. In addition, a study determined that the moisture content of Pebax® 5533 can be reduced during the processing and shelf life of the manufactured part using calcium chloride, which can easily adsorb moisture from the polymer surface during processing while undergoing a thermal transformation due to its hygroscopic and deliquescent behavior [15]. It was found that for each part of the moisture content, half a part of the calcium chloride filler should be added, in a 2:1 ratio [16].
This study’s primary focus was investigating the material behavior of Pebax® 5533D to determine a possible innovation in the development of a polymeric compound by tailoring the formulation of the base resin with a series of additives and filler components. We aimed to reduce manufacturing defects and increase the processing capabilities and application performance of the material used for manufacturing medical plastic parts.

2. Materials and Methods

Pebax® 5533D was integrated as the main polymer base of the polymeric compound formulation and was also used as the vehicle resin (acquired from Arkema, Birdsboro, PA, USA). Pebax® 5533D is characterized as an elastomer-type thermoplastic polymer with a molecular structure composed of two blocks of flexible polyether and polyamide-12 [17], as shown in Figure 1A. The compound was prepared by incorporating the plasticizer, lubricant, and additive fillers, using 53810 OMSUR calcium stearate (Figure 1D), Polyglykol 20000 S polyethylene glycol (Figure 1C) (donated by Sur Química, San José, Costa Rica), and ESENTTTIA 20H10NA polypropylene (Figure 1B) (donated by INA, San José, Costa Rica). Roth ≥ 98% dehydrated calcium chloride (Figure 1E) (acquired from Faro Química, San Jose, Costa Rica) was also added as a desiccant filler.
The selected mixtures were determined based on the following experimental statistical model, which was designed according to the extreme vertex method with restrictions on the minimum and maximum percentages of the components and a first-order design level (Minitab® 20.1.1, Erie, PA, USA). The mixtures’ selection was based on an optimization of the study by establishing vertices, where the mixing points of one or more components had a percentage of 0% or the maximum percentage (10% for polypropylene, 10% for polyethylene glycol, and 1% for calcium stearate). This allowed us to maintain a certain level of regression when analyzing the results during the statistical analysis of the experiment. Therefore, the number of runs was reduced according to Table 1 to prioritize the most relevant formulations with respect to the highest concentration of each component.

2.1. Sample Preparation

The samples of the compound formulations consisted of unique mixtures prepared with established proportions of each raw material component processed using a plastic injection-molding machine to form solid plastic probes, as shown in Figure 2.
The raw materials, including the Pebax resin and additives, were weighed using a balance (Crown Electronic, UWE, EM-11K model, Qingdao, China). Each material combination was stored in a sealed plastic bag and agitated for 30 s to ensure uniform blending. The mixtures’ weight was selected as two kilograms according to the requirements of the injection-molding equipment feeder capacity, the number of test pieces needed, and the purge required between runs. A series of probes were molded with plastic injection equipment (HAITAN, MA1200 model, Ningbo, China). The equipment integrated an injection screw of 214 cm3 and was set up with a nozzle temperature of 240 °C, an injection pressure of 980 bar at 40.8 rpm, and an injection cycle of 23 s. Additionally, it was equipped with a mold capable of injecting two test pieces per cycle at 180 °C according to the requirements of the tensile mechanical testing needed for this study.

2.2. Characterization

The formulated compound was characterized by evaluating the physical, thermal, and mechanical properties of the probe test samples. These analyses aimed to identify the optimal composition for manufacturing molded plastic parts.
This characterization included determining the moisture contents of the standard sample consisting of pure Pebax and the formulated composites using thermogravimetric analysis (TA equipment, model TGA5500, New Castle, DE, USA) and the ASTM-D3850 [18] standard testing method. The density of the samples of the different mixtures was evaluated using the ASTM-D792 method [19] in triplicate at room temperature (Ohaus: Analytical balance, model: Discovery with density Kit Ohaus). The different thermal points (i.e., the glass transition temperature, melting point, and crystallization temperature), degradation behavior, and mass loss of the components of each mixture under heat exposure were identified. The thermogravimetric analysis was performed following the ASTM-D3850 [18] and ASTM-D3418 [20] standard testing methods. DSC equipment (TA Equipment, DSC2500 model, New Castle, DE, USA), with a temperature accuracy of ± 0.025 °C, and TGA equipment (TA Equipment, TGA5500 model, New Castle, DE, USA) were used for these analyses. The crystallinity effect on the samples was studied with an X-ray diffractometer (XRD) (Empyrean, Malvern-PANalytical, Malvern, UK). The bulk material was packed on a sample holder and measured in the range of (2θ) 5°–90° with a copper (Cu) anode using a GaliPix detector with a 16.8 mm anti-scatter slit. The operating conditions, including the step size, voltage, and current, were adjusted to 0.007°, 40 kV, and 40 mA, respectively. The probe sample fracture was studied using scanning electron microscopy (SEM) (JSM-IT500, JEOL, Tokyo, Japan).
The elastic modulus, tensile strength, and elastic limit of each sample were determined and evaluated with the ASTM-D638 standard testing method [21]. The flexural strength was determined using ASTM D790—Flexural Properties of Polypropylene [22]. The Vantage NX Tensile Testing Machine (Vantage NX model, Software MAP, Thwing-Albert Instrument Co., West Berlin, NJ, USA) equipment was used, and the processed data were directly obtained from the software. The parameters used for testing the tensile strength, elastic modulus, and elastic limit were a speed of 50 mm/min and a sample length setting of 100 mm. The parameters for testing the flexural strength were a 0.5 N contact force, a 25 mm/min contact speed, and a 3.23 mm depth (the dimensions of the molded test samples were as follows: 9.9 mm wide, 4 mm thick, and 157 mm long).

3. Results and Discussion

Crystallization in a molten polymer sporadically results from nucleation events and the growth of nuclei into crystalline entities, which spread across the entire volume at the end of the transformation [23]. The structure, crystal size, and crystallinity degree depend on the type and structure of the polymer and the additives incorporated during processing, which may promote or decrease the growth of the crystalline network. Therefore, the crystallinity and, consequently, the physical and mechanical properties of thermoplastic polymers are affected by the processing conditions while compounding the plastics, such as the process temperature profile, cooling rate, etc. [23]. It has been demonstrated that the mechanical properties of polymeric blends without additives may lack strength in terms of their flexibility properties. Blending polymer materials with additives and fillers generates better mechanical properties than those of pure polymers. Moreover, the blends’ thermal properties and crystallinity degree may increase or decrease [24].
The thermal analysis results using differential scanning calorimetry (DSC) presented in Table 2 demonstrate the impact of each component’s proportion on the crystallinity of the formulated blends compared with the standard Pebax® 5533D, representing the polymer resin at its highest purity level [25].
The crystallinity temperature ranged from approximately 76.67 °C (lowest) to 96.06 °C (highest), without reaching the temperature of pure Pebax® 5533D (ca. 100 °C for the standard sample) (see Figure S1). The tendency found for the blends’ crystallinity showed that incorporating other polymeric materials into the Pebax® 5533D resin via thermal and mechanical plastic processing can lead to the rearrangement of the crystals in the main polymeric net [26]. As presented in Figure 3, the P4 sample represented the formula with the highest crystallinity temperature and proportion of polypropylene and polyethylene glycol. Both polymeric components increased the structural order in the polymeric chains while making the plastic probes, as the crystalline structure of Pebax® 5533D fractured and formed a new net with more ordered regions [25,26]. Furthermore, both the polypropylene and polyethylene glycol components exhibited affinity with the Pebax® 5533D resin based on the mixing capabilities of the different polymer blends, which also increased the polymeric blend’s crystallinity [27].
The melting temperature (Tm) ranged from 154.16 °C (lowest) to 158.01 °C (highest). The formulated blends with lower polymeric component proportions, such as the P3 formulation, presented the lowest melting temperatures compared with the standard Pebax® 5533D sample, as shown in Figure 3. Including non-polymeric components in the main polymeric network caused more pronounced variations in the heating and melting points of the blended materials. In contrast, blends containing only polymeric components exhibited similar melting points [28,29].
The mechanical test results for tensile strength and flexibility presented lower elastic modulus values for the compound materials than the standard Pebax® 5533D sample, showing the compound materials’ increased flexibility (see Figures S2 and S3). Moreover, the tensile strength values varied both above and below the standard Pebax® 5533D value depending on the polypropylene concentration, as shown in Table 3. Peng and Snyder (2019) determined a figure of merit for the flexibility of materials that defines it according to the yield strength (or elastic limit) divided by the elastic modulus [30,31]. Thus, while materials with a higher yield strength are more flexible, those with a higher elastic modulus exhibit decreased flexibility [31]. Based on this principle and the formulated compounds, each formula containing additives obtaining a higher flexibility resistance should have had a low elastic modulus [32]. The tensile test results agreed with the expected mechanical behavior (see Figure 3). The elastic moduli decreased in formulations incorporating more of the lubricants and plasticizers due to the variations in the components such as polypropylene, polyethylene glycol, and calcium stearate [31,32].
The variable mechanical behavior of the compound mixes resulted in the formulations with higher polypropylene concentrations tending to show improved tensile resistance (with a higher yield strength); conversely, those with more calcium stearate and polyethylene glycol showed the weakest tensile resistance strength but intrinsically had the highest flexibility [27,28,32]. Thus, calcium stearate and polyethylene glycol may have acted as plasticizers in the formulations [33,34]. Specifically, calcium stearate decreased the crystallization temperature in all its formulations [35]. This tendency was confirmed by the statistical models analyzing the design of the experiments performed in this investigation. For this analysis, a custom mixture design of experiments was established based on the material constraints described in Table 3, where a total value of 0.9979 was used to account for the use of an invariable amount of calcium chloride (Minitab® 20.1.1, Erie, PA, USA). The UTS (ultimate tensile strength), elastic modulus, and elastic limit (yield strength) values were analyzed with the Mixture Design function (Minitab® 20.1.1, Erie, PA, USA), including all regression terms and a confidence level of 95% for the statistical analyses [36].
As described in Table 3, there was no statistical evidence to conclude that changes in the mixtures’ compositions affected either the elastic modulus or the elastic limit of the reference material (Pebax); conversely, there was statistical evidence to conclude that the ultimate tensile strength of the material was influenced by compositional changes [36].
Although our model was reduced due to the raw material constraints in this investigation, some conclusions can be drawn from the results, especially based on the coefficients obtained for each of the mixture components [36,37]. First, the results show that polypropylene significantly influenced the material’s elastic modulus, making the material stiffer and less flexible. The mixture with 10% polypropylene showed the highest elastic modulus [37]. Meanwhile, calcium stearate, unlike polypropylene, negatively affected the material’s elastic modulus and raised its elastic limit [37]. This positively contributed to both factors of the flexibility figure of merit described by Peng and Snyder (2019) in the mixtures with maximized calcium stearate contents, exhibiting higher elastic limits [31,37]. Finally, using polyethylene glycol reduced the ultimate tensile strength along with the other two response variables. As the regression model fits the UTS response, our data show that polyethylene glycol reduced the strength of the material [14,37], which was heightened by this component having the second-highest coefficient of the model. This impact was minimal compared with the other components when analyzing the elastic modulus regression. Regarding the elastic limit, the negative contribution to this variable was minimized by the positive contribution of both polypropylene and calcium stearate [9,12,37]. Therefore, we conclude that polyethylene glycol negatively impacted the material’s overall strength, and it is not recommended for use when aiming to improve elastomers’ yield or strength properties [37].
A good regression model was not found for the elastic moduli or elastic limits of the mixtures used due to the limited experimental design model. A graphical representation of the results is shown in Figure 4, which may further the understanding of the data obtained regarding flexibility. Each of the mixtures shown in Figure 4 is labeled per the reference runs in Table 2. This graphical representation shows that mixture P5 was the most flexible, as it shows the best location in terms of a high elastic limit and low elastic modulus [32,37]. This mixture contained only calcium stearate as an additive, with no polypropylene or polyethylene glycol, confirming the assumptions made based on the design of the experiments and analysis. P2, containing 10% polypropylene, had the highest elastic modulus, which is a negative outcome when aiming to improve the flexibility of this type of plastic [33,37]. Compared with mixtures such as P5 or P6, P3, even with a low elastic modulus, is not ideal in the search for a flexible material due to its low elastic limit. As defined by Peng and Snyder (2019), although this material is not stiff or rigid, it is weaker than the other materials, which reduces its flexibility even with a low elastic modulus (see Figure 4) [31,37].
Meanwhile, the density of the probes did not significantly vary between the formulations. However, the density showed an increasing trend with the incorporation of the additives, as presented in Table 2. The formulas with higher polypropylene contents presented density values over the standard value of the pure Pebax® 5533D sample [38]. Regarding the moisture results shown in Table 2, adding the same quantity of the calcium chloride desiccant additive to each compound decreased the water content of each mixture without using dryer equipment [16,38]. Although the complete elimination of moisture was not achieved due to the exposure of the samples to open areas during processing, the desiccant effectively reduced most of the resin’s moisture content.
The thermal stability of PEBAX and the P5 sample was evaluated using thermogravimetric analysis under nitrogen and synthetic air atmospheres (see Figure 5). The PEBAX/P5 sample curves undergo only one stage of decomposition at approximately 400 °C, corresponding to the major decomposition process of PEBAX [39,40]. A similar trend is observed in the P5 thermogram, confirming that the formulation maintained PEBAX’s thermal behavior.
Additionally, the XRD analysis (Figure 6a) showed the diffraction patterns for the PEBAX and P5 samples. Since PEBAX is a semi-crystalline polymer, its XRD pattern shows a weak diffraction peak at approximately 11° and a strong diffraction peak at 23° related to the amorphous and crystalline segments of the polymer matrix, respectively [39,40]. In general, incorporating additives into a polymer matrix affects the morphology and crystallinity of the resultant matrix, and the polymer crystallinity affects the function of the intrinsic intermolecular bonding forces and their structural characteristics [40,41]. The additives’ effects are undetectable in the X-ray diffraction patterns shown in Figure 6a. However, all the samples showed a decrease in the crystallinity temperature, as reported in Table 3. The formulation’s effect on the mechanical properties was confirmed by the fracture-dominant phenomena after tensile mechanical treatment, whereby the PEBAX formulation without additives exhibited more ductile behavior compared with the fracture of the formulated sample (see Figure 6b,c) [41].

4. Conclusions

This experimental analysis validated the dependency of the properties of the Pebax® 5533D vehicle resin on the proportions of additives. Adding different components to the Pebax® 5533D resin resulted in variations in the thermal, mechanical, and physical properties of the polymeric compounds analyzed. The analysis of the mechanical properties of the composite material revealed that using a high concentration of calcium stearate improved its elastic modulus, indicating increased flexibility. Moreover, it demonstrated higher performance processability during injection molding, leading to more homogeneous and flexible samples. The tests showed high tensile strength values in mixtures with high polypropylene concentrations due to the significant influence on the material’s elastic modulus, resulting in a more rigid and, therefore, less flexible compound mix than those with less polypropylene. Nevertheless, the Pebax resin and polypropylene showed good compatibility. Although their blend does not improve flexibility, it can be used for other applications in medical plastic components where material stiffness is required. Meanwhile, polyethylene glycol had a minimal influence on the mechanical properties compared with the other additives analyzed; therefore, its contribution to the mechanical improvements of the Pebax resin was considered negligible. In addition, adding calcium chloride as a desiccant additive reduced the moisture content in the compound samples. Incorporating calcium chloride can effectively maintain lower moisture absorption in manufactured plastic parts and reduce resin drying times before injection molding, a common industry practice to minimize moisture before processing. The impact of each tested component in the formulated compounds supports this study’s aim to investigate the additives’ effects on commercial PEBAX to improve its application in medical device material manufacturing. This study’s findings confirm that the P5 formulation is a suitable option to enhance the performance, profitability, and manufacturability of the Pebax® 5533D resin for producers of plastic medical device components.

Supplementary Materials

The following supporting information can be downloaded at https://www.mdpi.com/article/10.3390/jcs8080314/s1, Figure S1: DSC thermograms of (a) PEBAX and P5 sample (b) under N2; Figure S2: Stress–strain curves of PEBAX (yellow line) and P5 sample (blue line) (separation rate: 500 mm/min); Figure S3: Stress–strain curves of PEBAX (yellow line) and P5 sample (blue line) (separation rate: 5 mm/min).

Author Contributions

Conceptualization, M.G.-E. and R.Z.-S.; methodology, M.G.-E., R.Z.-S., R.S.-P. and F.V.S.; validation, R.Z.-S. and R.S.-P.; formal analysis, R.S.-P.; investigation, M.G.-E.; resources, M.G.-E. and R.Z.-S.; data curation, R.S.-P.; writing—original draft preparation, M.G.-E.; writing—review and editing, M.G.-E.; visualization, R.Z.-S. and R.S.-P.; supervision, R.Z.-S. and R.S.-P.; project administration, M.G.-E. and R.Z.-S. All authors have read and agreed to the published version of the manuscript.

Funding

This research was partially funded by the Master Program in Medical Device Engineering at the Instituto Tecnológico de Costa Rica.

Data Availability Statement

Data are contained within the article and the Supplementary Materials.

Acknowledgments

The authors thank the Medical Devices Master Program and the Postgraduate Office at the TEC for their support during this project, with the valuable contributions of Pedro Araya Castillo and Cristhian Alvarez Cabrera as part of the TEC students’ team for this investigation project. In addition, we want to recognize and thank Giovanni Sáenz-Arce from the Physics Department (Universidad Nacional, Costa Rica) for his involvement in the experimental design. The authors acknowledge the support of the Institutional Microscopy Laboratory of the Costa Rican Institute of Technology in the SEM image acquisition.

Conflicts of Interest

The authors declare no conflicts of interest.

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Figure 1. Molecular structures of (A) Pebax® 5533D polymer resin and (B) polypropylene, (C) polyethylene glycol, (D) calcium stearate, and (E) calcium chloride additives.
Figure 1. Molecular structures of (A) Pebax® 5533D polymer resin and (B) polypropylene, (C) polyethylene glycol, (D) calcium stearate, and (E) calcium chloride additives.
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Figure 2. Diagram of compound samples preparation process.
Figure 2. Diagram of compound samples preparation process.
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Figure 3. Comparison of thermal and mechanical properties including (a) elastic modulus, (b) elastic limit, (c) melting point, and (d) crystallinity temperature for tested polymer compound formulations.
Figure 3. Comparison of thermal and mechanical properties including (a) elastic modulus, (b) elastic limit, (c) melting point, and (d) crystallinity temperature for tested polymer compound formulations.
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Figure 4. Comparative data on the elastic moduli and elastic limits of tested polymer compounds.
Figure 4. Comparative data on the elastic moduli and elastic limits of tested polymer compounds.
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Figure 5. Thermograms of pristine (a) PEBAX under N2 (red solid line) and air (black solid line) atmospheres and (b) sample P5 under N2 (green solid line) and air (black dashed line) atmospheres.
Figure 5. Thermograms of pristine (a) PEBAX under N2 (red solid line) and air (black solid line) atmospheres and (b) sample P5 under N2 (green solid line) and air (black dashed line) atmospheres.
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Figure 6. (a) Comparative XRD diffractograms of PEBAX (red) and P5 formulation (green). SEM images of the tensile fracture of (b) PEBAX and (c) P5 formulation samples.
Figure 6. (a) Comparative XRD diffractograms of PEBAX (red) and P5 formulation (green). SEM images of the tensile fracture of (b) PEBAX and (c) P5 formulation samples.
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Table 1. Table presenting reduced design for mixture DOE comprising components A (Pebax® 5533D), B (polypropylene), C (Polyglykol 20000 S polyethylene glycol), D (53810 OMSUR calcium stearate), E (Roth ≥ 98% dehydrated calcium chloride), and Std (standard Pebax® 5533D resin) for polymer compound testing.
Table 1. Table presenting reduced design for mixture DOE comprising components A (Pebax® 5533D), B (polypropylene), C (Polyglykol 20000 S polyethylene glycol), D (53810 OMSUR calcium stearate), E (Roth ≥ 98% dehydrated calcium chloride), and Std (standard Pebax® 5533D resin) for polymer compound testing.
Ref. RunFormulaA (%)B (%)C (%)D (%)E (%)
P1489.177.502.500.630.21
P2589.2910.000.000.500.21
P31188.790.0010.001.000.21
P41679.7910.0010.000.000.21
P51599.290.000.000.500.21
P6398.790.000.001.000.21
P7793.922.502.500.880.21
Std18100.000.000.000.000.00
Table 2. Thermal and mechanical characterization results of the DSC test, tensile test, density by weight, and TGA test to obtain moisture contents of the Pebax® 5533D compound mixtures.
Table 2. Thermal and mechanical characterization results of the DSC test, tensile test, density by weight, and TGA test to obtain moisture contents of the Pebax® 5533D compound mixtures.
Ref.
Run 		Crystallinity
Temperature (°C)
± 0.025 Accuracy 		Tm (°C)
± 0.025
Accuracy 		Ultimate
Tensile
Strength
(MPa) 		Elastic
Modulus
(MPa) 		Elastic
Limit
(MPa) 		Flexural
Strength
(MPa) 		Density
@ 23 °C
(g/cm3) 		Moisture
Content
(%)
P191.010155.15023.20141.7111.928.14 ± 0.401.01530.186
P292.670155.52026.10173.1611.1110.67 ± 0.071.00570.339
P376.670154.16012.90131.724.6910.74 ± 0.221.00170.279
P496.060157.28019.80145.3811.369.69 ± 0.241.02230.262
P594.740158.01024.20133.1613.157.56 ± 0.181.01470.276
P690.510154.79023.60139.2612.717.32 ± 0.061.01570.272
P793.720154.73021.70145.0213.477.83 ± 0.161.01200.147
Std (Pebax)100.82157.1322.00149.125.559.14 ± 0.291.00570.351
Table 3. Predicted statistical models of response variables for mixture design of experiments of Pebax® 5533D compound prototypes.
Table 3. Predicted statistical models of response variables for mixture design of experiments of Pebax® 5533D compound prototypes.
Response VariableR-SquaredPebax CoefficientPP CoefficientPEG CoefficientEC CoefficientANOVA p-Value
UTS93.19%23.274863.5181−62.8362−40.1190.009
Elastic modulus64.44%143.407343.892−2.399−79.1090.207
Elastic limit39.00%8.47448.27−28.652311.8090.534
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MDPI and ACS Style

Guillén-Espinoza, M.; Sancho, F.V.; Starbird-Perez, R.; Zamora-Sequeira, R. PEBAX® 5533D Formulation for Enhancement of Mechanical and Thermal Properties of Material Used in Medical Device Manufacturing. J. Compos. Sci. 2024, 8, 314. https://doi.org/10.3390/jcs8080314

AMA Style

Guillén-Espinoza M, Sancho FV, Starbird-Perez R, Zamora-Sequeira R. PEBAX® 5533D Formulation for Enhancement of Mechanical and Thermal Properties of Material Used in Medical Device Manufacturing. Journal of Composites Science. 2024; 8(8):314. https://doi.org/10.3390/jcs8080314

Chicago/Turabian Style

Guillén-Espinoza, Mildred, Fabián Vásquez Sancho, Ricardo Starbird-Perez, and Roy Zamora-Sequeira. 2024. "PEBAX® 5533D Formulation for Enhancement of Mechanical and Thermal Properties of Material Used in Medical Device Manufacturing" Journal of Composites Science 8, no. 8: 314. https://doi.org/10.3390/jcs8080314

APA Style

Guillén-Espinoza, M., Sancho, F. V., Starbird-Perez, R., & Zamora-Sequeira, R. (2024). PEBAX® 5533D Formulation for Enhancement of Mechanical and Thermal Properties of Material Used in Medical Device Manufacturing. Journal of Composites Science, 8(8), 314. https://doi.org/10.3390/jcs8080314

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