Influence of Silica (SiO2) Loading on the Thermal and Swelling Properties of Hydrogenated-Nitrile-Butadiene-Rubber/Silica (HNBR/Silica) Composites
-
Muhammad Amin
und
Muhammad Ali
Abstract
Hydrogenated-Nitrile-Butadiene-Rubber (HNBR) is known for its good physical strength. It is a widely used rubber in electrical insulation and other high performance applications. Performance of HNBR is affected in high temperature and an aggressive fluid environment. Adding silica to HNBR may overcome this problem. In order to investigate the effect of fluids and temperature on HNBR/silica composites we prepared multiple composites of HNBR with 8.3, 16.7, 33.4, 50 and 66.7 phr of silica (SiO2) by two roll compounding method. Swelling index and thermo gravimetric analyses were performed. Calculations of swelling indexes were performed at different time periods with ethanol, toluene and water. For thermo gravimetric analysis (TGA), thermo grams of samples were obtained and % char yields at 550 °C were analyzed for all samples. Improvements with the addition of silica were recorded up to a great extent in both analyses. Swelling index decreased with the addition of silica as compared to neat HNBR and reached an optimum position with 50 phr silica loading in ethanol, 8.3 phr in water and 66.7 phr in toluene. Moreover, the HNBR composite with 66.7 phr of silica was found to be the highest thermally stable sample and lost less than 60% of weight at 550 °C in comparison to neat HNBR in which 80% of weight loss occurred at 550 °C.
1 Introduction
Hydrogenated-Nitrile-Butadiene-Rubber (HNBR) is a prominent and widely used elastomer [1]. It is obtained by hydrogenation of Nitrile Butadiene Rubber (NBR) [2, 3]. HNBR is known for sustainability of its physical strength and other properties in exposure to heat, oil and other chemicals [4]. This tough nature of HNBR is provided by its saturated structure and existence of many polar groups. Due to this exceptional nature, it finds usage in many industries e.g. automotive, aerospace and electrical and thermal insulations etc. [5, 6]. Although HNBR is advantageous over NBR in fuel and oil resistance and has also better oxidation and heat resistance than Ethylene-Propylene-Diene-Monomer (EPDM), it decays in high temperature environments and also swells when exposed to solvents [7,8]. Thus, the resistance of HNBR needs to be enhanced for applications in high temperature and aggressive solvent environments.
Enhancement in the properties of materials has been an area of research for a long time. Addition of fillers, to the neat materials is an efficient method to enhance their properties [9, 10, 11, 12]. Different types of fillers are used to enhance properties of polymers. In order to get optimum results from fillers, some parameters are of great concern during the preparation of composites e.g. mixing time, mixing temperature and modifier content etc. [12, 13]. Fillers are broadly categorized in two classes, extended fillers and reinforcing fillers [14, 15]. Extended fillers are generally used for the extension of formulation e.g. ATH, ZnO and ground quartz. Whereas, reinforcing fillers are used for improvement of properties e.g. physical, mechanical and thermal properties. Examples of reinforcing fillers are silica and carbon black etc. Thus, the addition of fillers may result in increased thermal and swelling resistance of overall HNBR composite. Several types of fillers were used previously to improve properties of HNBR [16] e.g. CNT [17, 18] ATH [19] and CB [20] etc. However, very limited work has been carried out on the investigation of thermal and swelling properties of HNBR composites [21, 22, 23] and almost no literature is available on these properties for HNBR/silica composites.
Silica is a reinforcing filler which has good resistivity and thermal stability thus it can bring superior enhancements in the properties of the HNBR. Interaction of silanol group of silica and hydrogen bond in polar HNBR is the reason of improvement in the properties in HNBR/SiO2 composites [24]. However, further studies are required to find the effect of loading of silica to achieve the utmost thermal properties and swelling behavior of HNBR [25].
Like other fillers, concentration of silica is also an important parameter for the stability of polymer [26, 27, 28]. Although HNBR has been studied for silica fillers, thermal and swelling properties of HNBR/SiO2 composites for different concentration of silica has not been reported yet. This is necessary to achieve high performance HNBR/SiO2 composites.
Keeping in view the importance of thermal stability and swelling behavior for HNBR/SiO2, we fabricated neat HNBR and its five HNBR/SiO2 composites with 8.3, 16.7, 33.4,50 and 66.7 phr of micro silica by two roll compounding as per recommendation of standard ASTM D-3182-07. Later on, all samples were tested for swelling behavior in ethanol, toluene and water. For investigation of thermal properties thermo gravimetric analysis (TGA) was used.
In this work, we have mainly focused on finding the effect of silica loading to achieve enhanced swelling and thermal properties of HNBR /SiO2 composites.
2 Materials
2.1 Ingredients
HNBR was procured from Lanxess Chemicals (Germany) and micro-silica (5 μm) was obtained from Wuhan Newreach Chemicals (China). Other constituents such as zinc oxide (ZnO), stearic acid (SA), mercaptobenzothiazole (MBT), sulfur (S), Tetramethyl Thiuram Tetrasulfide (TMTD) and dioctyl phthalate (DOP), Pyrolytic Boron Nitride (PBN) were industrial grade products.
2.2 Preparation of Composites
Neat HNBR and its composites were fabricated with different loadings of silica. Two roll compounding method according to ASTM D-3182-07 was used for the preparation of samples [29]. At the start HNBR was masticated and then sulphur, ZnO, stearic acid were added one after other in a sequence as given in Figure 1. The vulcanizates were made in a bolt press machine by curing them at 165 °C temperature and 10 MPa pressure for 40 minutes. All constituents were mixed in parts per hundreds ratio (phr) as given in Table 1.
Sequence of constituents’ addition in preparation HNBR Composites
HNBR Composites formulation recipes
| S.No. | Constituent | A/U | HNBR-0 | HNBR-1 | HNBR-2 | HNBR-3 | HNBR-4 | HNBR-5 |
|---|---|---|---|---|---|---|---|---|
| Blank (neat) HNBR | HNBR with 8.3 phr silica | HNBR with 16.7 phr silica | HNBR with 33.4 phr silica | HNBR with 50 phr silica | HNBR with 66.7 phr silica | |||
| 1 | HNBR | 100 | 100 | 100 | 100 | 100 | 100 | |
| 2 | S | 1.5 | 1.5 | 1.5 | 1.5 | 1.5 | 1.5 | |
| 3 | ZnO | phr | 5 | 5 | 5 | 5 | 5 | 5 |
| 4 | SA | 1 | 1 | 1 | 1 | 1 | 1 | |
| 5 | Silica | 0 | 8.3 | 16.7 | 33.3 | 50 | 66.7 | |
| 6 | PBN | 1 | 0 | 0 | 0 | 0 | 0 | |
| 7 | MBTS | 1 | 1 | 1 | 1 | 1 | 1 | |
| 8 | TMTD | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | |
| 9 | DOP | 2.5 | 2.5 | 2.5 | 2.5 | 2.5 | 2.5 |
3 Measurements, Instruments and Conditions
3.1 Swelling Properties
All six samples in approximately 1 cm × 1 cm of area and 2 mm thickness were used for the measurement of swelling properties [30, 31, 32, 33, 34]. Three solvents (water, ethanol and toluene) were used in the experiment. The dry samples’ weight (Wd) was initially recorded by an electronic digital sample having accuracy of 0.001 mg. The samples were then dipped in solvent. After a specific amount of time the weight of the swelled samples (Ws) was recorded. The measurements were also taken for multiple durations to find the effect of dipping time on the swelling of HNBR. The percentage swelling ratios for neat HNBR and its silica based composites for each solvent were then determined by the following formula [30, 31, 32, 33, 34].
4 Thermal Properties
For measurement of thermal properties Thermo Gravimetric Analysis (TGA) was performed using TGA Q50 (TA instruments, USA) following ASTM E1131 and ISO 11358 standards [35, 36]. To investigate weight loss by increasing temperature, the temperature was varied from room temperature up to 550 °C and thermo grams were obtained for the samples. For comparative analysis, temperatures for 10 % weight loss and 50 % weight loss of all samples were recorded. Moreover, the % char yield was also analyzed for samples at 550 °C.
5 Results and Discussions
5.1 Analysis of Swelling Behavior
Measurements for swelling index recorded for each solvent (ethanol, toluene and water) were different. The reason for the different swelling behavior is the exertion of different magnitudes of force from each solvent which depends upon the static fluid pressure of the solvent. Swelling properties of HNBR for ethanol, water and toluene are discussed below.
In ethanol, swelling ratio of HNBR varied with the variation in silica loading.
An increase in swelling ratio with the increase of immersing time in ethanol is clear from Figure 2(a). This increase of swelling ratio is up to a certain value and then decreases. The decrease in swelling ratio is due to the dissolving of rubber compound in the ethanol [37, 38]. From Figure 2(b) it is clear that the increase in silica loading results in decrease of swelling ratio. The decrease in swelling ratio of HNBR is due to the force involved between silica particles rubber network. In ethanol HNBR-4 which has 50 phr silica shows better swelling behavior as compared to the other samples up to 140 hrs.
Swelling behavior of HNBR in ethanol (a) swelling ratio vs. swelling time (b) swelling ratio vs. silica concentration
Figure 3 shows trend of variation of swelling ratio in toluene vs. immersing time and silica concentration.
Swelling behavior of HNBR in toluene (a) swelling ratio vs. swelling time (b) Swelling ratio vs. silica concentration
In toluene, decrease in swelling ratio was also recorded with the increase of silica loading. Thus, increase of silica resulted in overall compression of the HNBR/silica composite. It also emerged that the swelling ratio of HNBR in toluene was much higher in comparison to ethanol, which reflects higher affinity of HNBR to toluene than ethanol. However, in toluene HNBR-5 with 66.7 phr silica loading showed the best swelling behavior for all time durations, while for ethanol the swelling index reached an optimum point at 50 phr silica loading.
Unexpectedly, the swelling resistance of HNBR was higher in the case of water in comparison to ethanol and toluene.
From Figure 4(a) it is clear that the swelling ratio increases with the increase of immersing time in water. Moreover, it can also be observed that 8.3 phr loading of silica gives a minimum value of the swelling ratio for HNBR/SiO2 composite. After 8.3 phr loading the swelling ratio continuously increased. This is due to the fact that silica absorbs water, because of the presence of silanol group (Si-OH) in silica which forms a hydrogen bond with water and hence the higher the silica content the higher the swelling of HNBR/SiO2 composite [39, 40]. However, as shown in Figure 4(b) at 50 phr loading of silica the graph almost becomes a horizontal straight line which means that further loading of silica does not affect the swelling behavior of HNBR. In other words the HNBR reaches its maximum swelling limit.
Swelling behavior of HNBR in water (a) swelling ratio vs. swelling time (b) Swelling ratio vs. silica concentration
5.2 Thermo Gravimetric Analysis (TGA)
In order to analyze thermal stability of each formulation its individual thermo gram was obtained which are given in Figure 5(a-e). The loss of weight was faster in the case of HNBR-0 while it was observed that the length of the slope of weight loss curve increased as function of silica loading. At the end of experiment at 550 °C the HNBR-0 lost almost 80% of its weight while HNBR-5 with 66.7 phr silica lost almost less than 60 % which is evident of improved of thermal stability through addition of silica.
From Figure 6 it is clear that sample HNBR-5 is more stable in comparison with other samples and hence gave highest value 383.84 °C for 10 % loss in weight. The same trend was followed when the temperature was increased and HNBR-5 was stable in comparison to other samples by having 50% loss in weight at the highest temperature of 459.23 °C. From Figure 6 it is also clear that by increasing the concentration of silica the thermal stability of rubber increases which is due to the internal strong Si-O bonding in SiO2 as well as firm interaction of silanol group of silica with polymer network.
Temperature at 10 % and 50% wt. loss with respect silica concentration
Neat sample (HNBR-0) gave the smallest char yield which was approximately 10 % of initial weight of the sample, whereas HNBR-5 gave the highest char yield which is 42.12 % of the initial weight of the sample as shown in Figure 7. From Figure 7 it is also clear the char yield increased with the increase of silica loading.
Char Yield at 550 °C versus silica concentration
6 Conclusions
Multiple HNBR/SiO2 composites were prepared with different loadings of silica and tested for swelling behavior and thermal properties. Silica improved the swelling and thermal properties of HNBR but deteriorated in water. Composite with 8.3 phr silica was found with the best swelling behavior in water and for ethanol and toluene the optimum loadings of silica were 50 phr and 66.7 phr respectively. From TGA it emerged that composite with 66.7 phr of silica was more thermally stable and showed loss of weight less than 60 % at 550 °C, which was less in comparison with other samples. Thermo grams obtained from TGA also showed that by increasing silica loading the weight loss in HNBR/SiO2 was decreased.
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- Regular Article
- Real-scale comparison between simple and composite raw sewage sampling
- 10.1515/eng-2018-0017
- The risks associated with falling parts of glazed facades in case of fire
- Implementation of high speed machining in thin-walled aircraft integral elements
- Evaluating structural crashworthiness and progressive failure of double hull tanker under accidental grounding: bottom raking case
- Influence of Silica (SiO2) Loading on the Thermal and Swelling Properties of Hydrogenated-Nitrile-Butadiene-Rubber/Silica (HNBR/Silica) Composites
- Statistical Variations and New Correlation Models to Predict the Mechanical Behavior and Ultimate Shear Strength of Gypsum Rock
- Analytic approximate solutions to the chemically reactive solute transfer problem with partial slip in the flow of a viscous fluid over an exponentially stretching sheet with suction/blowing
- Thermo-mechanical behavior simulation coupled with the hydrostatic-pressure-dependent grain-scale fission gas swelling calculation for a monolithic UMo fuel plate under heterogeneous neutron irradiation
- Optimal Auxiliary Functions Method for viscous flow due to a stretching surface with partial slip
- Vibrations Analysis of Rectangular Plates with Clamped Corners
- Evaluating Lean Performance of Indian Small and Medium Sized Enterprises in Automotive Sector
- FPGA–implementation of PID-controller by differential evolution optimization
- Thermal properties and morphology of polypropylene based on exfoliated graphite nanoplatelets/nanomagnesium oxide
- A computer-based renewable resource management system for a construction company
- Hygrothermal Aging of Amine Epoxy: Reversible Static and Fatigue Properties
- The selected roof covering technologies in the aspect of their life cycle costs
- Influence of insulated glass units thickness and weight reduction on their functional properties
- Structural analysis of conditions determining the selection of construction technology for structures in the centres of urban agglomerations
- Selection of the optimal solution of acoustic screens in a graphical interpretation of biplot and radar charts method
- Subsidy Risk Related to Construction Projects: Seeking Causes
- Multidimensional sensitivity study of the fuzzy risk assessment module in the life cycle of building objects
- Planning repetitive construction projects considering technological constraints
- Identification of risk investment using the risk matrix on railway facilities
- Comparison of energy parameters of a centrifugal pump with a multi-piped impeller in cooperation either with an annular channel and a spiral channel
- Influence of the contractor’s payment method on the economic effectiveness of the construction project from the contractor’s point of view
- Special Issue Automation in Finland
- Diagnostics and Identification of Injection Duration of Common Rail Diesel Injectors
- An advanced teaching scheme for integrating problem-based learning in control education
- A survey of telerobotic surface finishing
- Wireless Light-Weight IEC 61850 Based Loss of Mains Protection for Smart Grid
- Smart Adaptive Big Data Analysis with Advanced Deep Learning
- Topical Issue Desktop Grids for High Performance Computing
- A Bitslice Implementation of Anderson’s Attack on A5/1
- Efficient Redundancy Techniques in Cloud and Desktop Grid Systems using MAP/G/c-type Queues
- Templet Web: the use of volunteer computing approach in PaaS-style cloud
- Using virtualization to protect the proprietary material science applications in volunteer computing
- Parallel Processing of Images in Mobile Devices using BOINC
- “XANSONS for COD”: a new small BOINC project in crystallography
- Special Issue on Sustainable Energy, Engineering, Materials and Environment
- An experimental study on premixed CNG/H2/CO2 mixture flames
- Tidal current energy potential of Nalón river estuary assessment using a high precision flow model
- Special Spring Issue 2017
- Context Analysis of Customer Requests using a Hybrid Adaptive Neuro Fuzzy Inference System and Hidden Markov Models in the Natural Language Call Routing Problem
- Special Issue on Non-ferrous metals and minerals
- Study of strength properties of semi-finished products from economically alloyed high-strength aluminium-scandium alloys for application in automobile transport and shipbuilding
- Use of Humic Sorbent from Sapropel for Extraction of Palladium Ions from Chloride Solutions
- Topical Issue on Mathematical Modelling in Applied Sciences, II
- Numerical simulation of two-phase filtration in the near well bore zone
- Calculation of 3D Coordinates of a Point on the Basis of a Stereoscopic System
- The model of encryption algorithm based on non-positional polynomial notations and constructed on an SP-network
- A computational algorithm and the method of determining the temperature field along the length of the rod of variable cross section
- ICEUBI2017 - International Congress on Engineering-A Vision for the Future
- Use of condensed water from air conditioning systems
- Development of a 4 stroke spark ignition opposed piston engine
- Development of a Coreless Permanent Magnet Synchronous Motor for a Battery Electric Shell Eco Marathon Prototype Vehicle
- Removal of Cr, Cu and Zn from liquid effluents using the fine component of granitic residual soils
- A fuzzy reasoning approach to assess innovation risk in ecosystems
- Special Issue SEALCONF 2018
- Brush seal with thermo-regulating bimetal elements
- The CFD simulation of the flow structure in the sewage pump
- The investigation of the cavitation processes in the radial labyrinth pump
- Testing of the gaskets at liquid nitrogen and ambient temperature
- Probabilistic Approach to Determination of Dynamic Characteristics of Automatic Balancing Device
- The design method of rubber-metallic expansion joint
- The Specific Features of High-Velocity Magnetic Fluid Sealing Complexes
- Effect of contact pressure and sliding speed on the friction of polyurethane elastomer (EPUR) during sliding on steel under water wetting conditions
- Special Issue on Advance Material
- Effect of thermo-mechanical parameters on the mechanical properties of Eurofer97 steel for nuclear applications
- Failure prediction of axi-symmetric cup in deep drawing and expansion processes
- Characterization of cement composites based on recycled cellulosic waste paper fibres
- Innovative Soft Magnetic Composite Materials: Evaluation of magnetic and mechanical properties
- Statistical modelling of recrystallization and grain growth phenomena in stainless steels: effect of initial grain size distribution
- Annealing effect on microstructure and mechanical properties of Cu-Al alloy subjected to Cryo-ECAP
- Influence of heat treatment on corrosion resistance of Mg-Al-Zn alloy processed by severe plastic deformation
- The mechanical properties of OFHC copper and CuCrZr alloys after asymmetric rolling at ambient and cryogenic temperatures
