International Journal of Mechanical Engineering and Technology (IJMET) Volume 10, Issue 01, January 2019, pp. 2075-2084, Article ID: IJMET_10_01_203 Available online at http://www.iaeme.com/ijmet/issues.asp?JType=IJMET&VType=10&IType=1 ISSN Print: 0976-6340 and ISSN Online: 0976-6359 © IAEME Publication Scopus Indexed FABRICATION OF BIO-POLYMER MATRIX COMPOSITE (PMCS) USED FOR BIOMEDICAL APPLICATION Mohamed Khazal Hussien Middle Technical University, IRAQ Raid K Salim Al-furat Al-awsat Technical University, IRAQ ABSTRACT In this researcha biomaterial additives were added to a polymeric materials to impr0ve the mechanical properties of the resultant composite,which can be used in bi0medical applications:as examplereplace or supplement functions of living tissues of human body. The present work is c0ncerned with study the mechanical properties (Compressive strength, Tensile strength, Impact strength, Wear resistance and hardness) for the resultant composite material. Epoxy was reinforced with < 75 µm of caw bone particulates. Three percentage of particles were used (5, 10 and 15) %, and the most effective addition was (10-15 wt. %). X-ray results showed that 71 % caw bone is calcium phosphate hydroxide (apatite). Also results showed that compressive and tensile strength of the resultant composite was increased by 18% and 24% respectively, as compared to as received epoxy. Hardness and impact strength of the fabricated composite also increased by 15% and 41% compared to the unreinforced epoxy. Wear resistance of the composite was improved pronouncedly through the resultant composite additions of bone particles, where wear rate decreased by 82%. Finally, the impact strength of the epoxy reinforced caw bone was increased by 41% compared to that unreinforced epoxy Keywords: Biomaterials, Polymer Matrix Composite, Mechanical Properties, Caw Bone, Epoxy Cite this Article: Mohamed Khazal Hussien and Raid K Salim, Fabrication of BioPolymer Matrix Composite (Pmcs) used for Biomedical Application, International Journal of Mechanical Engineering and Technology, 10(1), 2019, pp. 2075-2084. http://www.iaeme.com/IJMET/issues.asp?JType=IJMET&VType=10&IType=1 http://www.iaeme.com/IJMET/index.asp 2075 editor@iaeme.com Fabrication of Bio-Polymer Matrix Composite (Pmcs) used for Biomedical Application 1. INTRODUCTION Biomaterials are materials of manmade origin or natural source that are used to direct replace or supplement the functions of living tissues of the human body[1]. A deterioration of all tissues with age progressis the major contributor to the need for spare parts for the human body. As example, Bone is susceptible to fracture as a result of resorption, pathology and trauma [2].The density of bone decreases due to the growing cells become gradually less creative in making new bone and repairing a fracture. The strength ofbones with lower density, greatly deteriorates and an unfortunate result is that many old people spinal pr0blems or have collapsed vertebrae and fracture their hips [3].In early days, many type of natural materials such as wood, rubber glue, and tissues from living forms, and fabricated materials such as glass, gold, zinc and iron were used as biomaterials established on trial and error [4]. Titanium, stainless steel and its alloys have been used for the fracture fixation treatments [5].Nevertheless, these are implants and metallic devices are not "biodegradable" and needa second surgery to remove it from the human body. This is cause to increase chances of complications and infection with elevate the health care cost and hospitalization time[6].Thedeficiencies of various metallic materialscontains; very high stiffness compared to tissues, corrosion, high density andlow biocompatibility. While, thedisadvantages of other materials such as ceramic, comprise: brittleness, difficult to fabricate, low mechanical reliability, low fracture strength withhigh density and lack of resilience. All thementioned complexities provide way for the next generation bone implants that have better biocompatibility. The use of natural material (from animal sourcei.e. Cow bone)as reinforcement in polymer matrix compositewas good example of the substitute material based that are gaining attention [7]. Composites generally aim to combine the properties of different materials for medical applications, as example "biocompatible" polymeric materials have been typically applied as matrix for composite materials associated with ceramic fillers in tissue engineering. Where, polymers are known to be flexible and exhibit l0w mechanical stiffness and strength, while ceramics are generally stiff and brittle materials [8].The interest of fundamental research and industrial applications in natural fiber reinforced polymer composite materials is rapidly growing. Their properties such as;biodegradable, renewable, cheap, completely or partially recyclable and acceptable mechanical properties make them an cute ecological alternative to carbon, glass as well as manmade fiber used for the fabrication of composites [9].Nowadays, biomaterials are used in many medical systems and devices:screws, plates, wires and pins for bone treatments; dental and maxillofacial applications; skull reconstruction; artificial hearts; synthetic blood vessels and t0tal artificial joint implants. [10]. Many of researchers studied the ability of fabrication biocomposites which are composed of synthetic or natural resins reinforced with natural fibers, some of them are selected in the following: Oladele IO and Isola BA 2016[11] investigated the mechanical properties of epoxy composite reinforced by goat bone particles. The results showed that the improving in the mechanical properties were obtained at higher wt. % reinforced composites (16-20 wt. %), where at 16 wt. %, composites possessed the best tensile and bending properties as well as good hardness properties.OladeleIOet al. 2016 [12] explained the effects of cow bone particles additions on the tribological behavior and mechanical properties of polyethylene composite reinforced by cow bone so as to study the ability of using this new material for engineering applications. The results exposed that the hardness values and tensile strength of the resultant composite increase as the wt. % of the bone particles increased, while the rigidity and impact strength decreased. IsiakaOluwole2013 [13]studied the reinforcement efficiency of bone particles and b0ne ash on the mechanical properties of polyester matrix so as to investigate the suitability of the resultant composite as biomaterial. The tensile test result http://www.iaeme.com/IJMET/index.asp 2076 editor@iaeme.com Mohamed Khazal Hussien and Raid K Salim showed that, 8 wt. % bone particle reinforced polyester composites has higher tensile properties, whilein bending test, bone ash reinforced composites exhibited the best bending properties. Jyoti Prakash Dhal1 and S. C. Mishra 2012 [14] prepared a low cost polymer composite using brown grass flower broom as reinforcement. Results revealed that the prepared composite has a light weight and high strength depending on the mechanical and physical characterization such as: density measurement, porosity (void fraction) measurement, hardness and bending strength measurement. Many other researchers have initiated to focus attention on the biocomposites which are composed of synthetic or natural resins reinforced with natural reinforcements. They explained the effect of bone particle size dispersed on the mechanical properties of matrix composites so as to studyits suitability as biomaterials. The researchers also conclude that these materials are structurally compatible[15]. This research aims to improve the mechanical properties of polymeric materials (epoxy) using biomaterial (cow bone particles) as a reinforcement particles. 2. EXPERIMENTAL WORK 2.1. Materials The main materials used in this work are: epoxy resin and cow bones. Boneswere procure from the marketand scraped to remove meat remnants, washed thoroughly to remove any oil.They sun dried for 4 weeks, then calcined in the furnace at 300 ºC for 5 hours to eliminate any protein present and then cooled in air, after which it was crushed with jaw-crusher and finally milled using laboratory ball mill. Particleswere sieved to obtain the required grain size of < 75 μm. Figure (1) shows steps of bone particles preparation. a b c d Figure 1 the steps of bone particles preparation: a- Cleaning and cutting. b- Drying. c- Crushing process. d- Milling process The composite was manufactured using the open mould technique. A mixing ratio of 2:1 (epoxy: hardener) was selected based on the epoxy-hardener manufacturer’s instruction. Bone particulate was varied in a predetermined percentage of 5, 10 and 15 wt. %. The additives mixed with epoxy using electric stirrer for 20 minute for each case to guarantee high level of homogeneity. The manufacture process contains consecutive steps; Epoxy resin (polymer) fabrication, powder mixing, particulate filled polymer matrix composites fabrication (mixing http://www.iaeme.com/IJMET/index.asp 2077 editor@iaeme.com Fabrication of Bio-Polymer Matrix Composite (Pmcs) used for Biomedical Application the product of step (1 and 2), pouring the mixture of composite into a mold, curing at constant temperature and time, and ejecting the final composite material from the mold, then the composite were cut to the standard dimensionsto produce tensile, flexural and impacttest specimens. The mold with the dimension (4 x 80 x 200) mm was shown in figure (2) a and b. a b Figure 2 a- mold used. b- Tensile test specimens A special mold has been used for the preparation of compression test specimens. The mold was hollow cylinder with 12.5mm diameter and 25mm length. It was manufactured according to (ASTM-D695) standardsas shown in Fig (3) a. Othermold has been used for the preparation of wear test specimens. The mold was hollow cylinder with 10 mm diameter and 20 mm length. It was manufactured according to (ASTM-G99) standardsthe length to diameter ratio was nearly (2:1), fig (3) b.All the specimen were left to cure in the mould for 8 hours thenit rem0ved and dried in air for 14 days before testing. a b Figure 3 a- Compression test specimens. b- Wear test specimens. 2.2. Mechanical Testing 2.2.1. Tensile test This test was fabricated according to ASTM D3039 standardization, the specimens were cut to (4 x 13 x 200) mm, with a gauge length of (150) mm and the test was perf0rmed using (united test) tensile tester in the Specialized Institute for Engineering Industries at Baghdad. 2.2.2. Compression test The compression test was carried out using a universal testing instrument (united test) according to ASTM D695 M-89at the Institute of Technology –Mechanical department. 2.2.3. Wear test Wear test specimens were performed according to ASTM G 99 – 04 standardization, where their dimensions were (10× 20) mm. Experiments were carried out under, varying loads of (5, http://www.iaeme.com/IJMET/index.asp 2078 editor@iaeme.com Mohamed Khazal Hussien and Raid K Salim 7.5, 10, 12.5 and 15) N, Constant speed of (250 rpm) and a duration of 15 minutes for each test.Wear rate can be determine according the standardization: Wr = (ΔW / S) (1) Where: Wr= Wear rate (gm/cm) ΔW = Weight difference of sample before and after each test (ΔW=W1-W2) gm, and S = Total sliding distance (cm) A sliding distance is calculated by the following formula: S= V × t × 100 (2) Where: V = Linear velocity (m/min) t = Time of running (min) A linear velocity of (m/min) is calculated by using the formula: V =2π × 𝑟× n (3) Where: 𝑟 = Distance from the center of pin to the center of disc, m, and n = Disc rotational speed (rpm) 2.2.4. Hardness Test This test was performed on samples which had dimensions of (20x20x5) mm according to ASTM D2240 using the Durometer tester. 2.2.5 Impact test The impact test were carried on (impact tester machine) at the university of technology / the applied science department to measure impact strength .Specimen were cut into dimensions of (4 x 10 x 55 ) mm according to ( ISO 179-1982 E ). 2.2.6. X-ray diffraction (XRD) X-ray diffraction was also carried out on the bone particles to determine the elemental chemical composition of the cow bone particulate. The Instrument was used with X-Ray diffraction spectrometer at the ministry of science and technology. 3. RESULTS AND DISCUSSIONS 3.1. XRD Test The X-Ray Diffraction analysis showed that the main elements present in cow bone is calcium phosphate hydroxide (Apatite) with 71% as shown in figure(4). http://www.iaeme.com/IJMET/index.asp 2079 editor@iaeme.com Fabrication of Bio-Polymer Matrix Composite (Pmcs) used for Biomedical Application Figure 4 The X-Ray Diffraction analysis. 3.2. Tensile Strength Tensile strength was influenced by the change of weight fraction of the reinforcement.At 5 % wt. the tensile strength was decreasedas compared to the received sample. This decrease may be due to either poor adhesion or direct c0ntact of particles and void formation. Increasing percentage of filler caused improvement in the strength of the resultant composite as compared with as received one, the stresses reaches to maximum value of (90 MPa) with 10% wt. of reinforcement materials as shown in Figure (5).The stress increases proportionally with increasing weight fraction of fillers due to the bond created between the surface of fillers and matrix,which increases slippage of the particles as well as increasing wettability leading to increase in the strength. stress - strain curve 100 90 stress, MPa 80 70 60 50 40 pure epoxy 30 20 5 % bone particulate 10 0 0 2 4 6 8 strain Figure 5 stress-strain curveof the resultant composite as compared with received material. 3.3. Compression Strength Compression stress-strain curves of the resultant composite as c0mpared with as received are shown in Figure (6). It is clear that the increasing compression stress is a function of reinforcement materials content, therefore; the compression strength is directly proportional to the reinforcement content. Increasingthe weight percent of filler causes drops in strain of the resultant composite and increases in stress reaching maximum at10 % wt. of fillers up to (127.55 MPa). Increases in weight percent of fillers leads to decrease in the movement of http://www.iaeme.com/IJMET/index.asp 2080 editor@iaeme.com Mohamed Khazal Hussien and Raid K Salim particles which cause increasing in the transmitting stresses from matrix to fillers particles.After which, the stress was drops at15%due to the particles become segregated in matrix materials. stress strain curve 140 120 stress, MPa 100 80 60 pure epoxy 5 % bone particulate 10 % bone particulate 15 % bone particulate 40 20 0 0 5 10 15 20 25 strain % 30 35 40 Figure 6 stress-strain curveof the resultant composite as compared with received material 3.4. Wear Resistance Epoxy reinforced with b0ne particles (reinforcement) clearly affected the wear rate of the composite material.Figure(7)showswear test results, it can be noticed, that in all tested materials, the intensity of wear rate rises as the applied load increase. The characteristic of that increase is not the same for all specimens depending on the percent of the bone particles. The weight loss of each specimen after wear testing was taken in 0rder to calculate the wear rate (gm/cm) of the samples.This figure shows that the greater the percent of the reinf0rcement particles (bone) the higher wear resistance (i.e. decrease in wear rate). Thus the fabricated composite showed improvement in average wear resistance as the bone percentage increased, compared to pure epoxy. This improvement in wear resistance is due to high surface contact that’s lead to strong bond formed between matrix and filler, as well as the nature of these granules which have high abrasion resistance. wear resistance, gm/cm 0.000002 0.0000018 pure epoxy 0.0000016 0.0000014 5 % bone particulate 0.0000012 0.000001 0.0000008 0.0000006 0.0000004 0.0000002 0 4 5 6 7 8 9 10 11 force, N 12 13 14 15 16 Figure 7 Comparison between wear rates of the fabricated composite (5%, 10% and 15%) and received material. http://www.iaeme.com/IJMET/index.asp 2081 editor@iaeme.com Fabrication of Bio-Polymer Matrix Composite (Pmcs) used for Biomedical Application 3.5. Hardness Test Hardness property is a measure of the resistance of the materials to surface indentation, similar response mode to other mechanical properties was observed with a slight difference. Hardness test results are shown in Figure (8). It is n0ted that all composite materials have higher hardness than that of as received material.The increase in this property is due to the high hardness pr0perty of the reinforcement particles in addition to the strengthening resulting from carrying of the load by these particles.It was noticed that hardness property increase as the reinforcement increased. Best result was obtained at 15 wt. % bone reinforced sample with a value of 55.1 HD compared to the unreinforced epoxy matrix with a value of 48 HD. 56 hardness 54 pure 5 % bone particulate 10 % bone particulate 15 % bone particulate 52 55.1 53.3 50.8 50 48.2 48 46 44 Figure 8 hardness test results 3.6. Impact test In this test, un-n0tched specimens were used. The lack of a notch makes this test method especially useful for reinforced materiel where a notch may mask the effect of orientation. Results of this test were illustrated in figure (9).It can see that the resultant c0mposite with 15% wt. of reinforcement give the best toughness properties because of the unique properties of bone particles which have high impact resistance. Figure 9 impact test results http://www.iaeme.com/IJMET/index.asp 2082 editor@iaeme.com Mohamed Khazal Hussien and Raid K Salim 4. CONCLUSIONS From the research, it was observed that the cow b0ne can be used as reinforcement in polymeric material to develop composites materials for biomedical applications having met the necessary structural conditions. The c0nclusions derived from this experimental work can be summarized as follows: 1. The presence of 71% calcium phosphate hydroxide (apatite) in the reinforcement as a natural material approve its usability as a suitable reinforcement material in a polymeric matrix for the devel0pment of composite material used in biomedical applications. 2. Reinforcement of epoxy with 10 % wt. bone particulate provide the best mechanical properties.Where, Compressive and tensile strength of the resultant composite increased by 18% and 24% respectively (at 10 % of bone particulate reinforcement), as compared with received epoxy. 3. Wear resistance was highly enhanced within 10% wt. of bone particulate reinforcement, where wear rate decreased about 82% as compared with as received epoxy. 4. The hardness and impact strength of composite reinf0rced with natural particles increased about 15% and 41% respectively, as compared with received epoxy. 5. Composite specimen with best combination of mechanical and wear properties was 10 wt. % of caw bone particles reinforced epoxy matrix. This feat positioned the specimenas the most appropriate material in"biomedical application" having met the structural conditions necessary. 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