High performance wear and mechanical properties of particle reinforced polyether ether ketone (PEEK) matrix composite material and its preparation method

Abstract

The invention relates to a particle-reinforced Poly Ether Ether Ketone (PEEK) matrix composite material which exhibits superior wear resistance and mechanical qualities, and its method of preparation. This composite material offers superior mechanical and tribological qualities, as well as an extended service life, in comparison to PEEK-based composites utilized in the contemporary medical and aviation industries.

Description

[0001] HIGH PERFORMANCE WEAR AND MECHANICAL PROPERTIES OF PARTICLE REINFORCED POLYETHER ETHER KETONE (PEEK) MATRIX COMPOSITE MATERIAL AND ITS PREPARATION METHOD

[0002] TECHNICAL FIELD

[0003] The invention relates to a particle-reinforced Poly Ether Ether Ketone (PEEK) matrix composite material which exhibits superior wear resistance and mechanical qualities, and its method of preparation. This composite material offers superior mechanical and tribological qualities, as well as an extended service life, in comparison to PEEK-based composites utilized in the contemporary medical and aviation industries.

[0004] PRIOR ART

[0005] In recent years, the manufacturing of materials has escalated due to the application of powder metallurgy. Advancements in powder technology facilitate the manufacturing of components with varied geometries through diverse pressing methods, achieving high production velocity, superior quality, minimal dimensional tolerance, and cost-effectiveness. To enhance the performance of components fabricated using powder metallurgy, novel materials with diverse architectures and enhanced properties can be achieved by incorporating alloying elements or varied particles into the metal matrix. Consequently, it is feasible to acquire novel goods for utilization in many application domains.

[0006] Composite materials are being explored to create materials that have become essential in established techniques. Composite materials are advanced materials created by amalgamating two or more substances or phases, while retaining their inherent qualities. New combinations of materials are required that exhibit great mechanical strength, tribological performance, and hardness, minimal weight, resilience to elevated temperatures, good thermophysical qualities, and exceptional corrosion resistance. Consequently, high-resistance polymers offer both manufacturing and economic benefits.

[0007] Poly-ether-ether-ketone (PEEK) is a high-performance polymer characterized by its exceptional temperature tolerance and increasing application across several fields. Owing to its superior mechanical and thermal characteristics, PEEK is commonly employed as a substitute for metal in numerous high-performance applications, including automotive, aerospace, and industrial pumps. PEEK polymer possesses remarkable physical qualities and can maintain these characteristics even in harsh situations. This polymer is renowned for its excellent flame and temperature resistance. PEEK is a rigid, durable polymer that exhibits exceptional resistance to abrasion and friction. Consequently, it can also withstand sterilization and radiation. Moreover, its biocompatibility and radiolucency have facilitated its use as a biomaterial in dentistry, trauma, spinal, and orthopedic applications. This extensive applicability is attributed to its biocompatibility, exceptional chemical and physical stability, and indirectly, its properties as an anti-aging substance. In comparison to other polymer materials, PEEK exhibits favorable tribological characteristics, particularly a low wear rate and the capacity to function at elevated temperatures (~260°C) for extended durations. Notwithstanding these enhanced mechanical and tribological characteristics, the tribological and mechanical capabilities of PEEK in dry sliding contacts require further enhancement.

[0008] Graphite is a soft carbon mineral that possesses an oily texture and may be easily flexed into thin sheets. It is one of the three principal allotropic forms of carbon, alongside diamond and amorphous carbon. In other terms, it is a mineral consisting of carbon components. Graphite's exceptional characteristics enable its extensive applications. Its softness renders it suitable for pencil production and the lubrication of moving metal components, while its fire and acid resistance makes it valuable in the casting and refractory sectors, as well as in the fabrication of crucibles and laboratory apparatus. Black flame retardant coatings are typically composed of graphite. Owing to its excellent electrical conductivity, it is utilized in the production of electrodes, motor brushes, battery bars, and electronic gadgets. Graphite is utilized as an additive in tires, automotive brake pads, matches, and engine lubricants.

[0009] Graphene can be synthesized by various industrial techniques. The most notable methods include micromechanical separation of graphite layers (exfoliation), chemical vapor deposition, reduction of graphene oxide, and epitaxial growth. Electrons in graphene exhibit behavior akin to massless relativistic particles at ambient temperature, imparting unique characteristics to graphene, including the quantum gap effect. The primary superior qualities of graphene are its extensive surface area (2630 m2 / g), elevated electron mobility (200,000 cm2 / (V s)), exceptional thermal conductivity (5000 W / m K), and substantial Young's modulus (~1100 GPa). This material has numerous applications owing to its exceptional characteristics. These encompass conductive electrodes, field-effect transistors, sensors, clean energy devices, nanocomposites, and organic photovoltaic devices.

[0010] Boron (B) exhibits minimal solubility in metals at ambient temperature, although it substantially enhances the properties of metals due to its pronounced influence on hardenability and transformation characteristics. Boron and its compounds provide numerous advantages to metal materials, including elevated heat resistance, enhanced strength, superior elasticity, robust surface protection, significant wear and corrosion resistance, and improved adhesion and retention.

[0011] Boron compounds can be categorized into two classes based on their applications and manufacturing technologies:

[0012] 1. Boron minerals and commercially produced borates are generated in substantial quantities and utilized extensively.

[0013] 2. Specialized boron products with designated consumption sectors and restricted manufacturing.

[0014] Commercial boron minerals and borates can be synthesized by traditional chemical engineering unit activities. The predominant applications include glass, agriculture, cleaning and bleaching, flame retardants, and metallurgy. The synthesis of boron, boron fibers, boron carbide, boron nitrides, boron hydrides, and analogous specialized boron compounds necessitates particular circumstances and is predominantly employed in sophisticated technological domains. Sodium boron hydride, a notable hydrogen storage medium that has gained prominence in recent years, is a distinctive boron chemical with significant potential for extensive application Hydroxyapatite (HAp) is a compound of calcium phosphate. It constitutes a component of the raw material known as phosphoric rock. Hydroxyapatite is the primary inorganic constituent of bones and dental enamel. Hydroxyapatite predominantly exists in two forms: nano hydroxyapatite powder and micron hydroxyapatite powder. The distinction between the two powders lies in their granule size. Hydroxyapatite nanoparticles measure less than 200 nm, whereas micron hydroxyapatite ranges from 45 to 90 microns. The surface area of hydroxyapatite nanoparticles is around 9.4 m2 / g, whereas hydroxyapatite micron powder exhibits a surface area of 120 m2 / g.

[0015] Hydroxyapatite nanoparticles has numerous applications as outlined below: 1 . It is utilized to replace voids in bone tissue during surgical procedures in trauma, maxillofacial, orthopedic, and dentistry fields.

[0016] 2. The application of hydroxyapatite nanopowders is beneficial for the restoration of dental enamel and their integration into toothpaste and mouth rinses.

[0017] 3. It functions as a coating for orthopedic and dental implants.

[0018] 4. It is an agent that reduces sensitivity following tooth whitening.

[0019] 5. It is utilized as a remineralizing agent in toothpaste and for the early diagnosis of cavities.

[0020] 6. Due to its dimensions, crystallographic structure, and compositional resemblance to dense human tissue, it is advantageous for application in prostheses.

[0021] 7. Nano-hydroxyapatite is bioactive, biocompatible, and natural.

[0022] 8. It is neither poisonous nor inflammatory.

[0023] 9. Titanium and stainless steel implants are frequently coated with hydroxyapatite nanoparticles to diminish degradation rates.

[0024] 10. It substitutes xenogeneic and allogeneic bone grafts.

[0025] 11. The inclusion of hydroxyapatite nanopowders accelerates healing time.

[0026] Zirconium is a shiny, silvery-gray, ductile, and malleable metal that remains solid at ambient temperature, however can exhibit hardness and brittleness when impure. Zirconium is a highly combustible element in powdered form, although exhibits reduced flammability in solid form. Zirconium exhibits exceptional resistance to acids, saline solutions, and alkalis, making it commonly utilized in dental veneers. Zirconium possesses a melting point of 1855°C and a boiling temperature of 4371 °C. The electronegativity is 1.33 according to the Pauling scale. It ranks as the sixth lowest in electronegativity, following hafnium, yttrium, lanthanum, and actinium.

[0027] Zirconium is a naturally occurring element with five isotopes, of which zirconium- 90, zirconium-91 , and zirconium-92 are stable. The predominant isotope is 90Zr, constituting 51 % of zirconium. The rarest isotope is 96Zr. Zirconium is present in the Earth's crust at a quantity of 130 mg / kg and in saltwater at 0.026 pg / L.

[0028] In the currently developed method, carbon nanotubes (CNTs) were employed to enhance the performance of PEEK by the incorporation of suitable additives. The impact on the mechanical properties of carbon fiber (CF) / PEEK composite material and the interlayer shear strength was found to be 35.8%, 25.4%, and 23.7% respectively. Another study examined short fiber and hybrid carbon fiber PEEK composite materials under tensile and compressive circumstances, including quasistatic and high strain rate, to assess strain rate dependence. Various temperatures, including room temperature, +85°C, and -50°C, were employed to examine the temperature dependence of the materials. The hybrid laminate comprised a bonded short fiber core reinforced with external unidirectional plies oriented at 0° to optimize reinforcement while reducing the quantity of costly unidirectional composite utilized. The advantageous impact of the hybridization method was evident under compression throughout all high strain rate test conditions, with the hybrid laminate surpassing the performance of individual components for strength and strain rate sensitivity. The external unidirectional (UD) layers facilitated the containment of the short fiber core, enhancing structural integrity. The response to tension was mostly influenced by the UD layers, exhibiting a 288% enhancement in strength at room temperature compared to the short fiber material. Nevertheless, in high-temperature quasi-static conditions, the strength diminished by 64% as a result of the detachment of the UD reinforcement. This study illustrates the appropriateness of hybrid composites for impact applications and supplies material characteristics for the future design of composite structures exposed to impact events.

[0029] The developed method involved comparing the influence of nano and micro particles on the tribological properties of PEEK with those of pristine PEEK (PEEK- SOO). The coefficient of friction was noted to decline from 0.5 for pure PEEK to 0.24 for silica (SiO2) loaded PEEK. The integration of nanoparticles into the polymer matrix results in a substantial reduction in the coefficient of friction. In certain instances, it has been observed that the reduction in friction results from the development of a transfer film, contingent upon the roughness levels of the counter plate. The visual inspection of the steel counter plates demonstrated the development of a polymer transfer coating on the steel.

[0030] The friction and wear characteristics of PEEK and multi-scale particle-filled PEEK were evaluated utilizing a rate-increasing methodology during a sliding wear test, without altering the polymer sample or the counter body. The findings indicated that including different fillers markedly enhanced the tribological performance of PEEK, particularly under elevated load circumstances, namely at a pv condition of 4 MPa and 0.5-4 m / s, resulting in a reduction of the average specific wear rate from 19 mm. Following the incorporation of hard fillers, the minimum friction coefficient of around 0.1 was recorded for the PEEK composite, ranging from 3 N -1 m -1 to 0.42 mm 3 N -1 m -1. Comparable friction coefficients and wear rates for PEEK and PEEK composites were observed in speed increase testing relative to those assessed in constant speed tests. This indicates that the speed enhancement technique was effectively utilized in the examination of the tribological performance of polymer materials.

[0031] Hybrid composites comprising PEEK reinforced with short carbon fibers and nano silica were synthesized by a melt mixing technique at 400 °C. The initial length of the fibers was 6 mm, and the dimensions of the nano-SiO2 particles were 13 nm, presented as polymer granules. Microhardness tests indicated a substantial enhancement in the hardness of the composites attributable to the incorporation of SCFs and nano-SiO2 particles. The influence of nano-SiO2 concentration on the tribological characteristics of PEEK / SCF / nano-SiO2 composites was examined. Tribological experiments were conducted at standard pressures of 2, 3.75, 6.25, and 10 MPa utilizing a pin-on-disc configuration. All experiments were conducted at room temperature, under dry sliding conditions, and at a sliding speed of 0.25 m / sec. Scanning electron microscopy (SEM) was used to evaluate the worn surfaces and investigate the wear mechanisms that occur under various tribological circumstances. The inclusion of nano-SiO2 particles dramatically lowered friction coefficients at all pressures. Furthermore, increasing the nanoparticle content reduced the friction coefficients in almost all circumstances.

[0032] The effects of nanoparticles and short carbon fiber reinforced PEEK hybrid composites with low loading, i.e. 1 vol.% nano-SiO2 particles, on the tribological behavior of short carbon fibers (SCFs) / polytetrafluoroethylene (PTFE)Zgraphite filled polyetheretherketone (PEEK) were studied. In this work, the impacts of nanoparticle concentration ranging from 1 to 4 vol.% on the composite's structure and tribological performance were examined. Scanning electron microscopes were used to investigate polished composite sections. The included nanoparticles greatly lowered the friction coefficients of the composite. Nanoparticle agglomerates appear to exert an abrasive impact on the SCF at low pressure shear rates (pv), resulting in high wear rates. Under these conditions, increasing the nanoparticle content lowers wear resistance. With high pv factors, nanoparticles significantly boosted the wear resistance of the composite, but nanoparticle quantity had no meaningful effect on wear resistance. To determine the graphene-enhanced tribological performance of PEEK / SCF / PTFE hybrid composites, polyetheretherketone (PEEK)Zshort carbon fiber (SCF) / polytetrafluoroethylene (PTFE)Zgraphene (GE) composites (PSPGE) with varying weight percentages of GE were successfully constructed. The influence of GE on the tribological behavior of PEEK composites was studied at various applied pressures, sliding speeds, and temperatures. The characterization results demonstrated that the tribological performance improved as the GE loading increased, and the PEEKZSCFZPTFE composites with 2.0 wt% GE filling had the lowest coefficient of friction and wear rate. PSPGE demonstrated high lubrication and wear resistance efficiency, particularly under severe environments. Furthermore, PSPGE composites' better thermal conductivity allowed for the transmission of friction heat, which increased wear resistance. As a result, the newly created PSP2.0GE composite can be used in a variety of new applications as an enhanced friction material.

[0033] The micromechanical characteristics of PEEK-based hybrid composites reinforced with short carbon fibers (SCF) and nano-SiO2 particles were studied utilizing nanoindentation and nanoscratching techniques. The composites were created using a melt mixing technique at 400 °C. Pure polymer is granular, nanoparticles are 13 nm in size, and short carbon fibers have an original length of 6 mm. Each sample underwent more than 30 nanoindentation and three nanoscratching tests. The surface topography of indented and scraped regions was measured using AFM. The impact of reinforcing particles on typical nanoindentation load-displacement curves in composites were studied. Furthermore, the overall reinforcing effects of carbon fibers and nanoparticles were studied. Nanoscratch tests were successfully used to analyze friction qualities in the matrix, fiber, and interphase areas, as well as to determine interphase thickness. There were significant changes between the nanoindentation responses and microfriction characteristics of composites in matrix and fiber phases. The results showed that the presence of reinforcements increased hardness and elastic modulus significantly.

[0034] A hybrid wear method was proposed by combining different types of polymers to investigate the effect of filler type on the friction and wear performance of PEEK and PTFE composites under hybrid wear conditions. The role of various fillers (i.e. nanosized, micron-sized particles, and short-cut carbon fibers) in the PEEK-PTFE-steel hybrid wear system was investigated. Experiments resembling the operating conditions of a simple bearing were carried out under dry conditions on a newly constructed dual-pin-on-disc tribometer, with composite pins filled with different fillers, unfilled PEEK, and PTFE sliding across steel rings in the same wear track. The results showed that the two polymer components have a synergistic impact, which improves the tribological performance of the hybrid system.

[0035] In order to develop and optimize high performance PEEK / CF / Nanosilica hybrid composites, the tribological properties of PEEK / CF / nanosilica composites containing varying amounts of silica nanoparticles against steel were investigated using a ring- on-block tribometer, followed by characterization of the respective transfer films and polymer worn surfaces. The findings indicate that the presence of silica nanoparticles has a considerable impact on the friction and wear parameters of PEEK / CF / nanosilica composites. Under low load conditions, the coefficient of friction and specific wear rate were inversely proportional to the nanosilica content. The coefficient of friction reduced as the nanofiller content rose, however the specific wear rate increased with the nanosilica loading. When the load conditions were increased, the difference in tribological characteristics became minor, showing a reduced reliance on nanosilica loading.

[0036] LIST OF FIGURES

[0037] Figure 1. View of XRD Analysis Results of the produced Hybrid Composites

[0038] Figure 2. View of FT-IR Spectra of the produced Hybrid Composites

[0039] Figure 3. View of Hardness Values of the produced Hybrid Composites

[0040] Figure 4. View of Friction Coefficient Results of Samples 1 ) Reference, 2) A, 3) B, 4) C, 5) E

[0041] Figure 5. View of Weight Loss Changes in Samples During Wear Tests 1 ) Reference, 2) A, 3) B 4) C, 5) E

[0042] Figure 6. View of Stress-Strain and Force-Displacement Results 1 ) Reference 2) A, 3) B, 4) C, 5) E

[0043] Figure 7. View of Maximum Stress Changes

[0044] DETAILED DESCRIPTION OF THE INVENTION

[0045] The invention pertains to a Poly Ether Ether Ketone (PEEK) matrix composite material having at least one of the reinforcing elements graphite (Gr), boron (B), hydroxyapatite (HAp), and zirconium (Zr) with excellent service life-wear and mechanical qualities, as well as its fabrication technique. In our invention, the PEEK matrix material has a particle size of at least 50 pm, and reinforcing elements (Gr, B, HAp, and Zr) are smaller than the matrix material, with a maximum particle size of 35 pm and a purity of at least 90% (optimal 99.9%). Table 1 indicates the sample amounts used by weight in the created powders, as well as the composite names. The matrix material was changed to PEEK and combined with the reinforcing components, whose percentages by weight are listed in Table 1. The obtained powders were combined in a magnetic mill with ethyl alcohol and stearic acid at a speed of at least 300 rpm (optimum 400-650 rpm) for at least 2 hours (ideally 3-6 hours). The resultant solution was then dried in an oven at at least 80 °C (optimal 100- 120 °C) for at least 12 hours (optimal 14-16 hours) without being exposed to air. After drying, the resultant slurry was placed into a zinc stearate-lubricated mold (Zn(C18H35O2)2), and test samples were prepared in a hydraulic press with a pressing pressure of at least 10 MPa.

[0046] Peek Graphite Boron HAp Zirconium

[0047] Group A %90 %10

[0048] Group B %80 %10 %10

[0049] Group C %80 %10 - %10

[0050] Group D %80 %10 - - %10

[0051] Table 1. Composition ratios values (wt%)

[0052] The samples obtained after hydraulic pressing were held at two different temperatures (250 °C and 300 °C) for at least 200 minutes (ideally 240-300 minutes) until the sintering process was complete. The final samples' microstructures were examined using XRD, FT-IR, SEM, and EDS investigations. The tribological properties of the hybrid composites created for the test conditions were assessed using wear and hardness tests, while mechanical properties were assessed using compression testing.

[0053] XRD analysis was first done on the samples that had been prepared for microstructure examination. XRD analyses were performed on metallographically produced and sintered samples without Bakelite. XRD research revealed that the Peek matrix structure had distinctive peaks of Gr, B, HAp, and Zr reinforcing components. XRD analysis revealed matrix-specific peaks at 20 degrees, consistent with previous research.

[0054] When the FT-IR peaks of the created bulk hybrid composites are investigated, a pair of peaks around 1500 cm-1 and 1600 cm-1 most likely indicate the existence of aromatic rings in the structure, specifically benzene rings in the polymer. The absorption at wave numbers 900 cm-1 and 670 cm-1 corresponds to C-H out-of-plane bending vibrations. Furthermore, many sharp peaks between 1225 cm-1 and 950 cm- 1 are most likely caused by C-H in-plane bending vibrations. The less intense tiny peaks around 1250 cm-1 and 1730 cm-1 are owing to the presence of ether and ketone functional groups, respectively. Two less intense peaks in the region of 2800 cm-1 to 3000 cm-1 are due to aliphatic C-H stretching vibrations.

[0055] The SEM images of the hybrid composites show that the reinforcing elements are evenly dispersed inside the Peek matrix structure. The Peek matrix has a grain size of 44pm in SEM pictures, making it easier to install reinforcement elements in vacant areas. Choose reinforcement components with smaller grain sizes than the matrix structure. The SEM images show that selecting a lower grain size greatly reduces agglomeration and clumping of the reinforcing pieces. Furthermore, when the sintering temperature increased, the pores contracted and took on a circular shape. In other words, the granules' porosity decreased, becoming more isolated and spherical. The EDX analysis results show that the peaks of the reinforcement elements utilized in the study (Gr, B, HAp, and Zr) originated within the Peek matrix structure.

[0056] A material's tribological qualities are inextricably linked to its hardness, which is always interpreted as the scratch resistance, wear resistance, and cutting resistance of the material surface. All reinforced composites performed better in terms of hardness than the pure Peek sample. The pure Peek sample crushed at 10 MPa pressure and sintered at 250 °C yielded the lowest hardness results. The hardness levels of the pure Peek sample in terms of Vickers are identical to the findings of literature investigations. The D30-300 sample, pressed under 30 MPa pressure and sintered at 300 °C, produced the highest hardness result. The addition of B reinforcement strengthens cross-network structures and allows for the rearranging of amorphous polymer chains in composites. This results in increased hardness values versus the imposed normal load.

[0057] The friction coefficient findings of hybrid composites that have passed the wear tests at a sliding distance of 1000 meters show that the Gr, B, HAp, and Zr additives reduce the friction coefficient value while increasing the resistance to friction. The Gr and B additives operate as a bridge, connecting securely to the Peek matrix and forming chemical bonds rather than mechanical ones; as a result, more energy is required to break the interface layer during wear. Gr and B have extremely high strength, which can protect the Peek matrix and composites from breakage to some extent.

[0058] The drop in COF and wear weight loss values of Peek composites caused by B and Gr additions is attributed to an increase in heat conductivity under dry sliding conditions. In our invention, thermal conductivity appears to be a wear resistance parameter because it decreases slightly with the concentration of Gr and B and the water lubricant lessens the temperature increase in the bearing region. It is obvious that the friction coefficient of PEEK and reinforced hybrid composites steadily increases before fluctuating within a consistent range.

[0059] As pressing pressure and sintering temperature increase, the change in average friction coefficient steadily reduces, and friction coefficient values drop as Gr, B, HAp, and Zr content increases. The average friction coefficient of all hybrid composites is less than that of pure PEEK. The average friction coefficient of PEEK is approximately 0.38, indicating that Peek has low friction reduction capabilities.

[0060] The grooves on the worn surface in the pure PEEK sample are mostly caused by the opposing side of the steel pin's significantly higher hardness than the PEEK. During the friction and wear process, the steel pin's harsh protrusions pierce the PEEK, removing the softer PEEK under the contact load and friction shear.

[0061] PEEK is transmitted to the opposite surface by a combination of plastic deformation, delamination, and friction shear, forming a lubricating film. The wear attributes of PEEK / Gr-B samples show that adding Gr and B with large specific surface area and wrinkling improves the composites' hardness and compressive strength, resulting in much less flow stress. Less plastic deformation occurred at the sliding contact surface, resulting in decreased composite toughness. Gr and B will progressively be released on the worn surface, absorbing the majority of the applied load and encouraging the production of protective and in situ tribolayers at the interface between the composites and the steel pin. These morphological characteristics imply that the addition of Gr and B altered the composites' primary wear mechanism from adhesive wear and abrasive wear to fatigue wear. The composites' tight interfacial connection makes it difficult to detach Gr and B from the PEEK matrix, hence increasing wear resistance. In addition to the exfoliation caused by fatigue wear, other reinforcing elements and pure PEEK samples were badly damaged by the wear debris produced by fatigue wear. Wear debris on the composites' surfaces created abrasive wear, resulting in deep grooves. With B reinforcement in hybrid composites, the B- layered structure generated by weak Van der Waals contacts between each layer improves tribological performance, allowing for the production of a continuous and complete lubricant layer between the interfaces. At the same time, softer lubricant coatings efficiently cover the worn surface, filling in wear marks and wear debris, thereby boosting wear resistance.

[0062] The pure PEEK sample exhibits a high level of adhesive material and plastic deformation, as well as visible grooves and wear debris.

[0063] The higher the Gr and B concentration, the greater the wear resistance. The wear results show very smooth, shallow, narrow grooves parallel to the sliding direction, minor amounts of micro cracks, a water wave-like scrape, a spill pit, and plastic deformation in the A and B samples. The Zr and HAp reinforcements produced better results than the pure PEEK sample.

[0064] PEEK'S low hardness, ease of plastic deformation, and poor friction heat dissipation contribute to the high response time and average friction coefficient, which are primarily due to the strong adhesion and ploughing effect on the friction surface; however, the friction heat loss in composites improves and the adhesion effect decreases. Gr and B's self-lubricating properties help to reduce the friction coefficient of composites. PEEK / Gr-B has a higher friction reduction than PEEK / Gr due to B's superior self-lubricating properties.

[0065] In summary, the lubricant coatings produce a low-strength bond at the contact, resulting in a lower coefficient of friction and wear rate than PEEK. Thus, Gr and B can effectively prevent direct contact between the friction pair surfaces. Thus, wear of these composites is further reduced.

[0066] Compression tests were performed on hybrid composite samples created within the scope of the invention. Compression tests were conducted at room temperature utilizing the Universal Testing Machine in accordance with the ASTM D3410 / D3410M- 03 test standard. The crosshead speed of the machine was set to 0.5 mm / min for all analyses. Total duration 3600 sn

[0067] Temperature 22+2 °C

[0068] According to the compression test results, while PEEK'S maximum compression strength is around 35 MPa, the compression strength of Group A composite was determined to be 35 MPa, 35 MPa, 36 MPa, and 55 MPa, respectively. The maximum compression strength was 96 MPa in sample B4. It was discovered that the mechanical properties of the composite having 80% Peek, 10% graphite, and 10% boron in the weight contribution ratio were superior to those of the Peek composite. This is owing to the fact that graphite and boron, which are utilized as additives, have a higher strength than Peek and are dispersed uniformly throughout the microstructure. When the reference samples and other finished composites are tested, it is discovered that the B4 sample has the maximum toughness. It has been determined that adding graphite and boron to the Peek matrix increases the compressive strength and toughness of the composites. It has also been determined that raising the applied compressive force and sintering temperature are effective parameters for enhancing the toughness of composite materials.

[0069] The addition of the reinforcement pieces employed in our invention greatly improved the PEEK material's characteristics. Compared to pure PEEK samples, the results were 240% higher hardness, 500% compressive pressure, and 52% reduced friction coefficient.

Claims

CLAIMS1. It is a particle-reinforced composite material exhibiting extended service life, wear resistance, and superior mechanical capabilities, characterized by; a Poly Ether Ether Ketone (PEEK) matrix and incorporating at least one reinforcement element: Graphite, Boron, Hydroxyapatite (HAp), or Zirconium.

2. It is a method of preparation a particle-reinforced composite material with enhanced durability, wear resistance, and mechanical qualities, characterized by;- preparation of powders comprising a matrix material with a particle size of no less than 50 pm, constituting at least 80% by weight, and reinforcement elements having a maximum size of 35 pm, wherein at least one reinforcement element comprises a minimum of 10% by weight and possesses at least 90% purity,- mixing the prepared powders in a magnetic stirrer with ethyl alcohol and stearic acid at a speed of at least 300 rpm for at least 2 hours,- evaporating the resultant solution in an oven for a minimum of 12 hours at a temperature of no less than 80 °C, ensuring no exposure to air,- putting the slurry into a mold coated with zinc stearate (Zn(Ci8H3sO2)2) during the drying process,- preparation of test samples using a hydraulic press at a minimum pressure of 10 MPa,- finalizing of the sintering process, which include waiting period of at least 200 minutes at temperatures of 250 °C and 300 °C following hydraulic pressing.

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