TITANIUM CARBIDE-DOPED NICKEL OXIDE HYBRID NANOCOMPOSITES AND PREPARATION METHOD

Abstract

The invention relates to titanium carbide (TiC)-reinforced nickel oxide (NiO) hybrid nanocomposites and their preparation method. The nanocomposite, made with TiC nanoparticles on NiO nanoparticles, exhibits significantly superior electrical, dielectric, and mechanical properties compared to pure NiO nanoparticles, which are widely used as semiconductor materials.

Description

1 TARIFF TITANIUM CARBIDE-DOPED NICKEL OXIDE HYBRID NANOCOMPOSITES AND PREPARATION METHOD TECHNICAL AREA 5 The invention involves titanium carbide (TiC) reinforced nickel oxide (NiO) hybrid nanocomposites and It is related to the preparation method. PREVIOUS TECHNIQUE The 10th century, which is the fundamental technology of the industrial era of today and the centuries to come. Nanotechnology is the science of controlling matter at the atomic and molecular level. It is known that nanotechnology, based on scientific determination and experience, is the simplest form of technology. In essence, it contributes to the environment, energy, material durability, and efficient consumption. The contribution will significantly contribute to preserving the habitability of the world. It provides. Today, defense industry, pharmaceutical, automotive and electronics applications 15 For highly competitive industries like these, high value-added technology is crucial. In recent years, nanotechnology discoveries have been particularly prominent in materials science and have entered our lives. Significant progress has been made in many new products or processes. Particular attention is paid to nanotechnology. When focusing on scale, the elements represent a very promising class of materials, physical and chemical. Because they completely changed their electrical, optical and mechanical properties, they are relevant in all fields. Further developments are expected. Nanomaterials have excellent electronic, optical, magnetic, chemical and thermal properties. Due to its features, it has attracted great interest in recent years. Recently, many The researcher named the crystal because of its higher surface area and superior properties. It focuses on the synthesis of metal oxides at the nanoscale. Furthermore, these nano-metal oxides are 25... Reducing synthesis and overall production costs is of great importance. Oxide nanoparticles are extraordinary and can be used in many applications. It exhibits unique properties. Among these, nickel oxide (NiO) has Ni2+ vacancies. due to its cubic face-centered cubic (FCC) structure, it is an extraordinary p-type semiconductor. It is one of the conductive materials. In addition, it has a large bandwidth of 30 (3.6-4.3 eV). It also exhibits an exciton binding energy. NiO nanoparticles (NPs) excellent chemical stability, durability, low toxicity, cheaper and higher quality. It exhibits extraordinary physical properties with its ionization energy. In known technology, The Ni (3d) states form the lowest energy levels of the conduction band in NiO, O 2 (2p) states form the highest energy levels of the valence band. It is known that Ni (3d) and O (2p) hybridization in the NiO6 octahedron of NiO It is also known to result in electronic structures. Furthermore, NiO has a high pH of 10¹³ (ohms / cm). It is an antiferromagnetic material with electrical resistivity and a Néel temperature of 523K. Due to their unique physical properties and chemical stability, NiO nanoparticles, 5 optoelectronic devices, photodetectors, solar cells, gas sensors, solid oxide fuels It can be used in various applications such as cell making. In addition to these applications, NiO, It can also be used in electrochemical supercapacitors, smart windows, and catalysts. Therefore, NiO is an important transition metal oxide. The electrical conductivity of NiO nanoparticles. It is linked to the hope of holes associated with Ni2+ vacancies. The stoichiometric 10 of NiO The composition exhibits strong electrical resistance, but the resistance is greatly reduced with Ni2+ vacancies. However, the conductivity of NiO decreases due to Ni vacancies (VNi) and oxygen interstitials (Vo). by increasing the synthesis process or by controlling the synthesis process or by properly adjusting the metals. It can be increased by doping. The formation energy for nickel voids is due to all defects / locations. It is the lowest for substitutions, which leads to the p-type conductivity of NiO. However, 15 The presence of p-type conductivity in NiO is associated with interstitial oxygen. Titanium carbide (TiC) is a titanium alloy located in the fourth group of the periodic table. It is one of the important carbides formed as a result of the reaction of the element with carbon. Refractory Titanium carbide, which is among the carbides, has been the subject of research for over a century. It is and is expected to be included in research in the coming years. Chemical 20 TiC, which is quite stable, has a face-centered cubic (FCC) crystal structure. TiC; high melting point, low density, hardness and toughness, good heat and electrical conductivity Due to the perfect combination of physical characteristics such as these, it has been the subject of much discussion in recent years. TiC has become a material that is studied. Due to its attractive properties, it is used as a polymer and metal. and can be used as nanostructural reinforcement for ceramic matrix composites; catalysis, 25 It has widespread applications in microelectronics and industry. TiC Investigation of the structure and morphology of nanoparticles and their different compositions There are studies on combining TiC nanoparticles. However, Studies are needed to determine the dielectric properties of NiO and... Studies conducted using TiC material separately are given below. 30 In the current technique, NiO nanoparticles are produced using basic nickel carbonate as a raw material. (BNC) and by calcining malate gel using malic acid and H2O as solvent. He prepared the mixture. He investigated the reaction using TG-DTA, XRD, and FT-IR. NiO The particle size and morphology of the nanoparticles were characterized by TEM. Nickel 3 malate can be formed by the reaction of BNC and malic acid; the gel is nickel malate and residue It was determined that it consisted of malic acid; the precursor completely decomposed into NiO nanoparticles in air at 400 °C. it can transform and the average diameter of the prepared sample according to the Scherrer formula It shows that it has a cubic crystal structure of approximately 14 nm at 400 °C. NiO calcined for 1 hour exhibits a narrow particle size distribution, weak agglomeration, and 5 It had a small particle size. The particle size of NiO increased with increasing temperature. has increased. In another study, the average size was approximately 2 μm and the average thickness was... NiO nanoflakes, approximately 20 nm in size, were successfully produced using a simple two-step method. It has been synthesized. NiO, which is used as the anode electrode of lithium-ion batteries, has been synthesized. The electrochemical properties of nanoflakes were determined using conventional charge / discharge tests. It was examined and found to have 1213 mAh g⁻¹ and 902 mAh g⁻¹ at a current density of 100 mA g⁻¹. Initial discharge and charge capacities were demonstrated. After 50 cycles, NiO nanoflakes The discharge and charge capacities of the electrodes were 1015 and 990 mAh g -1, respectively. The initial discharge and charge capacities of the NiO electrode are 749 at a current density of 800 mA g -1. and while it was 541 mAh g -1, after 50 cycles it became 578 and 567 mAh g -1 respectively. 15 Nanoneedle-coupled hierarchical and nanosheet-coupled hierarchical NiO Nanoflowers are produced using a simple hydrothermal method followed by calcination. We successfully synthesized them through this method and we studied their growth mechanisms and gas detection. The effects on the properties of NiO nanocrystals on gas sensing have been determined. their properties can be significantly improved by adapting nanoscale building blocks. 20 In addition, nanoneedle-coupled hierarchical NiO structures have been shown to be nanolayer- The difference is that it exhibits faster gas response and recovery than combined ones. Nanolayer-coupled hierarchical NiO nanoflowers have been developed that are more resistant to ethanol. It showed a high gas response. In a different study with NiO nanocrystals; any 25 controlled by ion exchange membrane without added solvent or template by calcination of Ni(OH)2 precursor synthesized via easy ion diffusion It has been prepared. X-ray diffraction (XRD), scanning electron microscopy (SEM), Brunauer- Emmett-Teller (BET) isotherm, X-ray photoelectron spectroscopy (XPS), and ultraviolet- Visible (UV-vis) analysis examines crystallinity, morphology, surface and porosity properties, It has been used to study its chemical composition and optical properties in more detail. 30 Pseudocapacitive behavior of NiO samples, cyclic voltamograms in 2 M KOH. (CV) and galvanostatic charge-discharge tests were used to investigate. The results analysis showed that both specific that both capacitance and surface area decrease with increasing calcination temperatures This is demonstrated by NiO samples, including NiO-400 calcined at 400 °C. 4 Nanoflakes exhibit a peak specific capacitance of 381 F g−1 at a current density of 2Ag−1. It has, but is much lower than that of the Ni(OH)2 sample. In addition, UV-vis analysis shows three For the NiO sample, the absorption peak shifted to red with increasing temperature, and NiO- This shows that 400 has a wide bandwidth of 3.3 eV, which makes the material... This makes it interesting for application in photocatalysis. 5 Reduction of TiO2 by graphite or metallic titanium, in continuous vacuum. It was monitored in an X-ray furnace with graphite resistance underneath. This was done in four stages. In a reaction mechanism, various reactions are likely to occur between 293 and 2300 K. This has led to the formation of oxides, oxycarbides, and titanium carbides. The study results show that when it comes to the Ti2O3 phase, 10 phases are independent of each other. a non-quenched reduced form and an oxidized form emerge. It has been observed. On the other hand, for the observed Magnéli suboxides Ti n O 2 n -1, n is the number of n. By using the linear variation of molar volumes measured in relation to their structures, It has originally confirmed the evolution of 'crystallographic shift'. TiC ceramic nanoparticles were subjected to high-energy shot milling followed by thermal processing. It was successfully synthesized in a SiO2 matrix by applying the process. The grinding procedure is as follows: A mixture of TiO2, Si, and graphite powders is heated at ambient temperature in an inert gas (Ar). This involves grinding in the atmosphere. Structural evaluation of dust particles. The tests were performed using XRD, TEM, SEM, EDX, and DSC. XRD results were obtained for TiC-SiO2. 10 hours of mechanical activation of the non-composite followed by 7 20 at 1473 K (1200 °C) It shows that it was produced after a few minutes of heat treatment. According to the results, TiC-SiO2 The nanocomposite was obtained by heat treatment at 1473 K (1200 °C) for 7 minutes. Synthesized after hourly mechanical activation. Pressure test, ceramic matrix. TiC-SiO2 composite powder, ceramic material in single-phase form TiC It has a higher toughness (i.e., less fragility) than when it is used 25 TEM results have shown that TiC and SiO2 crystallites are nanosized. Mechanical activation of the powder mixture has been demonstrated to affect the titanium carbide lattice. This caused the parameter to deviate from the standard value. This resulted in stress. from the increase in its quantity and the non-stoichiometric ratio of titanium carbide It originates from synthesis. 30 Pure and (% 10, 20 and 30 by weight) titanium carbide (TiC) reinforced zinc oxide (ZnO) nanoparticles were produced by sol-gel synthesis method. Sol-gel nanoparticles The synthesis involves dissolving the solvents in a magnetic stirrer at 90 °C for 4 hours. This has been accomplished. Filtration, drying, mortar and pestle processing of the synthesized nanoparticles have been carried out. Annealing processes were carried out on the synthesized ZnO and TiC-doped nanoparticles. structural and morphological features, field emission scanning electron microscopy (FE- SEM), X-ray diffraction (XRD), energy dispersive spectrum (EDX), and Fourier transform. The produced nanoparticles were examined using infrared spectroscopy (FT-IR) analyses. Their dielectric properties were also investigated. As a result of the analysis, TiC and ZnO 5 were found to have dielectric properties in XRD analysis. Characteristic peaks of nanoparticles were observed. In the XRD analysis results, TiC Increases and shifts in the characteristic peaks of TiC with increasing additive content. This occurred. As a result of FE-SEM analysis, the TiC doping of TiC nanoparticles was observed. It has been observed that with increasing TiC addition, growth in the ZnO structure occurs. The dielectric properties and AC conductivity values ​​of nanoparticles were positively affected by 10 It has been observed that it has an effect. In another study, nickel oxide (NiO) nanoparticles were also used. It was synthesized by the sol-gel method. The solution was prepared at pH 11 and calcination temperature at 450 °C. It has been checked. The structure, morphology, and particle size of NiO have been investigated. Structural Analysis confirmed that the cubic structure of NiO is formed without impurities. Morphological Elemental analyses revealed the ratio of NiO, Ni, and O. Morphological analysis showed approximately 15 It demonstrated NiO nanoparticles with an average diameter of 32.9 nm. Aluminum alloy (A 6063) reinforced titanium carbide (TiC) particles It is produced using the stir casting method. Aluminum alloy by weight. Titanium carbide was added in percentages of 2%, 4%, 6%, 8%, and 10%. Density, hardness, and tensile strength were improved. The strength of the composites is increased by the ratio of titanium carbide particles, respectively, to 20. It has been observed to rise to maximums of 7.8%, 20%, and 19.55%. Mechanical and The results of impact tests showed that pure composite plates were reinforced with 3% by weight of TiC. 15% improvement in modulus of elasticity and impact resistance compared to composite plate. It has been observed that 6% more energy is absorbed in the resistance. Another 25 In the study, a multiphase mixture consisting of e-glass fiber reinforced epoxy resin and TiC particles was used. The processing of a composite and the solid particle erosion behavior of the composite were investigated. Increasing the percentage of TiC particles (0-10-15-20 wt.) increases the hardness value from 29 to 53. There has also been a significant improvement in HV and erosion wear behavior. It has been observed that impact velocity significantly affects the TiC ratio and collision angle. 30 It has been observed. In the known technique, with TiC particles in different proportions (0-5-10-15-20-25 wt.). Mechanical and tribological behavior of reinforced epoxy matrix composite. It was examined. Hardness and tensile strength were 15%, wear resistance was 10%, and impact resistance was 10%. 6 It has been determined that the best results are obtained in terms of strength at 20% mesh ratio. Hot In another study produced using the pressing technique, the mechanical properties of Cu-TiC composites were investigated. Predicting physical characteristics using artificial neural networks (ANN) models Studies have been conducted on density, hardness, electrical conductivity, and transverse fracture strength. All characteristics of the TiC effect on friction coefficient and wear rate values ​​are very 5 It has yielded superior results. With increasing TiC content, aluminum metal matrix composites both both microhardness and ultimate tensile strength, when compared to the base alloy It has been observed that titanium carbide reinforced metal matrix composites have increased significantly. In studies on the evaluation of fatigue and impact behavior, TiC 10 Significant improvement in the fatigue and impact behavior of composites with reinforcement. It has been observed that it occurred. A BRIEF DESCRIPTION OF THE INVENTION The invention involves using Titanium 15 as a reinforcement element for Nickel Oxide (NiO) nanoparticles. Synthesis and preparation of hybrid nanocomposites with carbide (TiC) nanoparticles. It is related to the method. TiC nanoparticles on NiO nanoparticles nanoparticles NiO, a composite material widely used as a semiconductor material. electrical and dielectric properties far superior to those of pure nanoparticles, It provides mechanical properties. 20 Our invention has high bending, tensile and compressive strengths, high stiffness and wear-resistant, low density, high thermal conductivity, high Its high resistance to high temperatures and ease of processing make it suitable for use in the defense industry, medicine, It will easily meet the needs in the automotive, textile, and electrical sectors. In this way, the shortcomings of the materials currently used in these areas are addressed and 25 It is competing with equivalent materials. Our invention is used in the defense industry. A nanocomposite is formed by combining metal material with powder metallurgy when it is to be used. It is a material that offers higher mechanical strengths and tribological properties compared to its counterparts. Features include resistance to high temperatures, lubricating properties for better friction, and It provides wear resistance. With its high electrical conductivity and high thermal conductivity, it is 30. Suitable for use in electronic components and battery and solar panel applications. It is located. 7 LIST OF FIGURES Figure 1. Appearance of the NiO-TiC Nanomaterial Production Scheme. Figure 2. Appearance of XRD Analysis Results of Nanoparticles A) NiO-TiC B) NiO, C) TiC Figure 3. Appearance of Raman spectra of nanoparticles A) NiO-TiC B) 5 NiO, C) TiC Figure 4. Appearance of FT-IR spectra of NiO / TiC nanoparticles. Figure 5. FE-SEM View of Nanoparticles - 1) A) NiO, B) TiC Figure 6. FE-SEM View of Nanoparticles – 2 A) NiO-1TiC, B) NiO-5TiC, C) NiO-10TiC 10 Figure 7. Appearance of EDX spectra of nanoparticles A) NiO, B) NiO-1TiC, C) NiO-5TiC, D) NiO-10TiC, E) TiC Figure 8. Appearance of EDX mapping of TiC nanoparticles (10 µm) (magnification) A) NiO-1TiC, B) NiO-5TiC, C) NiO-10TiC Figure 9. A) Dielectric constant (ε′), B) Dielectric loss for nanocomposites. (ε″) and C) Frequency dependence of conductivity (σac) Figure 10. NiO composites containing TiC (1% to 10% by weight) nanoparticles. A) Appearance of the IV curves, B) Appearance of the current-TiC composition. Figure 11. Appearance of the DC conductivity (σdc) of NiO-TiC nanocomposite. A) NiO- 5TiC, B) NiO-10TiC 20 The Correspondences of the Numbers Shown in the Figures 1) 1. Each 2) 2. Each 3) 3. Each 25 4) 4. Each 5) 5. Each DETAILED DESCRIPTION OF THE INVENTION With this invention, 30 nanoparticles of pure NiO and TiC-doped NiO can be synthesized using a sol-gel method. To produce it, 1. Add 0.5 M Nickel (II) acetate tetrahydrate to 25 ml methanol in a beaker (1). The process was started by forming Mixture-1 (Methanol+C4H14NiO8) by adding (C4H14NiO8) and It was stirred on a magnetic stirrer until dissolved. 2. Beaker (2), 25 ml methanol Mixture-2 (Methanol+NaOH) is formed by adding 2.5 M Sodium Hydroxide (NaOH) to it. 8 magnetic is applied until the solution dissolves, and the pH balance of the solution is maintained. Mixed in a mixer. These two solutions were combined in a beaker (3) and 10 ml was added to the mixture. Mixture-3 (NiO) was formed by adding more methanol. The solution is magnetic. It was dissolved in a mixer at 90°C for four hours. After the mixing process... The solution was then allowed to reach room temperature. The nanoparticles were then 5 It was filtered through filter paper and washed with alcohol. After the filtering and washing process... Nanoparticles were dried in an oven at 70°C. The dried nanoparticles were then heated at 500°C. crushed in a mortar and pestle without being tempered in the oven for an hour, and then tempered. This was achieved. Thus, pure NiO nanoparticles were produced as a sample and TiC was added. The same process steps were repeated to produce NiO nanoparticles. TiC-reinforced 10 in nanoparticles, nano-TiC particles in 20 ml of methanol (1%, 5%, 10%) by weight percentage added and then processed using an ultrasonic homogenizer for 30 minutes. 4. Mixed in the beaker (4) and Mixture-4 (Methanol+ TiC) was formed. Mixture-3 and Mixture-4, 5. Mixture-5 (NiO + TiC) was formed by adding to Beaker (5) and pure NiO was obtained. By repeating all the procedures performed to obtain TiC-doped NiO nanocomposites, 15 The nanoparticles produced are named according to their additive amounts in Table 1. It has been given. Sample Contents TiC 100% TiC NiO 100% NiO NiO-1TiC 1% TiC, 99% NiO NiO-5TiC 5% TiC, 95% NiO NiO-10TiC 5% TiC, 90% NiO Table 1. Names of synthesized nanoparticles and their additive amounts. The functional groups of the synthesized pure and NiO-doped TiC nanoparticles are FT- Characterized using IR measurements. Analysis was performed within a scanning range of 4000-500 cm-1. This was performed and produced using an FT-IR spectrometer. XRD PEEKs of nanoparticles at CuKa (=1.5406A) radiation at 40 kV / 40 mA = 2 Obtained within a scanning range of 80°. Generating non-resonant and RRS results 25 a Raman spectrometer with excitation wavelengths of 532 and 325 nm respectively. The system was used. FE-SEM and EDX analyses determined the form and chemical composition of the nanoparticles. 9 to analyze the content as well as the particle sizes and degree of doping It has been used. TiC-doped NiO nanoparticles on 13 mm diameter discs at room temperature. Conductivity (Gp), loss factor (DF), and capacitance (Cp) measurements were performed on it. Using an impedance analyzer with a frequency range of 1 kHz to 2000 kHz, the dielectric 5 Its characteristics have been examined. Structural information and crystal size of TiC-reinforced and pure NiO nanoparticles. This was investigated using XRD analysis. When the 2θ orders of NiO nanoparticles were examined, COD data for NiO 96-101-0096 are associated with 37.202°, ​​43.221°, 62.795°, 75.220° and It shows five diffraction peaks at 2θ with an angle of 79.305°. These peak values ​​are for NiO 10 These are the characteristic peaks of nanoparticles. According to this data, the Miller indices of NiO are... (111), (200), (220), (311) and (222) correspond to the obtained results. NiO (03-065-6920) and the standard monoclinic structure of the JCPDS of the C2 / m space group are good. They are paired in a certain way. Diffraction planes of NiO nanoparticles with TiC reinforcement. This is shown in Table 2. In pure TiC nanoparticles, the angles are 35.918°, 41.674°, 60.412°, 15°. Intense peaks corresponding to 72.342° and 76.118° 2θ degrees are associated with TiC nanoparticles. It has been observed that it retains its characteristic peaks when combined with NiO nanoparticles. With increasing TiC reinforcement, the characteristic peaks of NiO and TiC nanoparticles were observed. Increases and shifts have occurred in the diffraction of nanoparticles with TiC reinforcement. The planes are shown in Table 3. 20 Sample / Diffusion plane NiO NiO-1TiC NiO-5TiC NiO-10TiC (111) 37.202 37.233 37.295 37.341 (200) 43.221 43.268 43.329 43.360 (220) 62.795 62.811 62.934 62.950 (311) 75.220 75.282 75.360 75.390 (222) 79.305 79.352 79.414 79.475 Table 2. 2θ values ​​of the diffraction planes of the synthesized NiO nanoparticles. Sample / Diffusion plane TiC NiO-1TiC NiO-5TiC NiO-10TiC (111) 35.918 35.949 36.010 36.026 (200) 41.674 41.689 41.798 41.828 (220) 60.412 60.443 60.551 60.567 (311) 72.342 72.373 72.420 72.435 (222) 76.118 76.164 76.242 76.303 Table 3. 2θ values ​​of the diffraction planes of the synthesized TiC nanoparticles. The average crystalline size of NiO nanoparticles can be determined as follows: The given Debye-Scherrer formula was used. Preferred orientation along the plane (200) is observed. 5 D = (1) Here, D is the average crystallite size of the nanoparticle, k is a value of ~0.9. The constant, λ, is the wavelength of 8.04 keV Cu-kα radiation used in XRD measurements. its length, β the full width (FWHM) density of the peaks at half maximum, and θ Bragg It shows the angle. Bragg's lattice constant calculation for NiO nanocrystals. The law of X-ray diffraction and the interplanetary space for the cubic system given below. The formula was used. nλ = 2dsinθ (2) And = (3) 20 The lattice parameter of the synthesized nanoparticles was obtained as 4.17 Å, and This value is in good agreement with previous results. Information about texture and orientation. To obtain this, the texture coefficients for the (hkl) plane were calculated using the formula (TC(hkl)). 11 TC() = ( ) ( ) ∑ ( ) ( ) (4) Here, I(hkl) is the relative density of (hkl) under consideration, Io(hkl) 47-1049 Standard density obtained from JCPDS card number and plane N considered. It represents the number. The values ​​obtained are in the range of 0.94 to 1.04. TC(hkl)~1 5 Therefore, we conclude that the crystallites are randomly oriented. using dislocation density (Ꟙ), which gives an idea about the irregularity of the structure It has been calculated. = (5) 10 Here, D is the crystallite size. δ was found to be 2.26 x 10¹⁵ lines / m². Table shows the lattice parameters of the synthesized TiC-doped NiO nanoparticles. As shown in section 4. As TiC content increases, the full width half-maximum (FWHM) of the peaks changes and becomes 15 Due to the change in the ionic radius of Ni2+ (0.69 Å) for the peak (200) compared to NiO. An angular shift has been observed. Therefore, from the expansion of the NiO lattice... The resulting surface and strain forces can be expected, which affects the optical properties of NiO nanostructures. and contributes to the development of conductivity aspects. The crystallinity of NiO nanostructures, defects in NiO nanocrystals 20 It shows that it was improved by dual contribution attributed to the reduction. Previous When several studies were examined, it was found that NiO is produced by doping NiO with a transition metal. It has been shown to lead to an improvement in its crystallinity. Synthesized When the nanoparticles were examined, it was observed that the lattice structure increased with increasing TiC reinforcement. There were reductions in the parameters, unit cell and crystallite size values. 25 It has arrived. 12 Sample 2 theta(200) β= FWHM(°) a=b=c(Å) D(nm) V(Å3) NiO 43.221 0.67812 4.464 22.666 28.890 NiO-1TiC 43.268 0.64041 4.459 16.876 28.800 NiO-5TiC 43.329 0.60303 4.453 16.843 28.685 NiO-10TiC 43.360 0.56077 4.450 16.834 28.626 Table 4. Calculated a, D and V values ​​of synthesized nanoparticles. Raman spectra of NiO at room temperature show a combined spectrum at (∼570 cm-1). Phonon (1 P) 1TO and 1LO mode, two phonons (2P) 2TO mode at ~730 cm-1, (2P) TO' It has shown that LO mode is at ~906 cm-1, 2LO mode is at ~1090 cm-1 and 5 at ~1490 cm-1. The strongest two-magnon (2M) scattering band was observed in NiO nanoparticles. Raman spectra show two overlapping spectra at 390 cm-1 and 534 cm-1, corresponding to 1TO. It showed a broad peak between 300-600 cm-1, attributed to the peak, and This corresponds to the 1LO optical mode of NiO, approximately 724 cm-1 and 1069 cm-9 respectively. The weak bands around cm-1 correspond to the 2TO and 2LO stretching modes of NiO, respectively. income. The disappearance of the 2M band is caused by smaller crystallites and defects. Antiferromagnetic binding in pure NiO nanoparticles due to disorder This indicates that its strength is decreasing. A fully stoichiometric cubic or rhombus. NiO does not exhibit first-order Raman scattering (1TO and 1LO modes). This Therefore, the presence of first-order Raman scattering peaks indicates nickel or interstitial 15 disorder caused by oxygen vacancies, surface effects and synthesized This can be attributed to the imperfection of the nanoparticles. Raman spectroscopy, carbonaceous It is considered one of the most sensitive tools for examining the structural properties of materials. Therefore, in order to confirm the presence of graphite structure in nanocomposites, Raman spectroscopy provides information about the crystal perfection of graphite-based materials. It provides information. In the Raman spectra of TiC nanoparticles synthesized with NiO, It includes three additional peaks at approximately 250 cm⁻¹, 400 cm⁻¹ and 600 cm⁻¹; this indicates that TiC This further confirms its formation. FT-IR spectrum, transmittance graph (%) and waveform of NiO nanoparticles. According to the peak values ​​corresponding to the number (cm-1), the wide 25 corresponding to 2366 cm-1. The peak can be attributed to O–H stretching vibration. In addition, the peak at 980 cm⁻¹ is ultra-fine. C–O suggests that NiO clusters lead to strong physical absorption of CO2 and H2O. This is attributed to the stretching of the Ni-O bond. The strong, dense peak found at 521 cm⁻¹ is due to the stretching of the Ni-O bond. 13 It is connectable (Table 5). FT-IR spectra were altered with TiC, TiC particles at 501 cm- It has a peak at 1 that is attributed to Ti-C vibration. Band position Result 2366 cm−1 O–H stretching vibrations 980 cm−1 C–O stretching vibrations 521 cm−1 Ni–O bond stress 1105 cm−1, 1031 cm−1 Carbonyl group 1380 NO Germe, Nitro group 871 cm−1 NO Vibration, Nitro group 501 cm−1 Ti-C stretching vibrations Table 5. FT-IR band position and band assignment of NiO-TiC nanoparticles. Table 6 shows the weight percentages of the elements contributing to the EDX analysis results. It has been shown. According to SEM images, the particles are nano-sized and made of TiC. nanoparticles are evenly distributed on NiO nanorods and plates It has been observed. SEM images show that NiO-TiC particles are synthesized at the nanoscale. 10 This has been revealed. The elements Ni, O, Ti, and C were detected in the EDX spectra. The particle size distributions of spherical NiO nanoparticles are clearly defined. The dimensions are well defined and match the XRD results. In SEM images, nanospheres are observed as the percentage of additive increases. It showed a slight change towards nanorods. NiO and TiC: NiO 15 From SEM images of nanodust, highly porous nanoparticles are observed. that it is molded, which in turn helps in the development of active sites on NiO. and it has been determined that it highlights the sensing ability of the synthesized samples. FE-SEM The images show nanoparticles arranged in a regular, layered pattern, layers within layers. It has transitioned from a rough and discontinuous morphology to an asymmetrical structure of varying sizes. 20 This reveals that this morphology is related to ultrasound application. Ultrasound waves its passage through dispersed material in the liquid medium, and the particles that precipitate when their volumes increase. bubbles that release large amounts of energy capable of breaking down the material structure This leads to its formation. When the distribution of TiC nanoparticles on the NiO structure was examined, TiC 25 Nanoparticles retain their original layered structure; however, some particles differ from others. 14 In addition to having a much larger and more heterogeneous size and shape distribution, As the irregular edges of the layers and clumps also indicate, the oxidation process They have defective lamellae caused by the EDX analysis result. The doping ratio is... With the increase, increases in Ti and C amounts were observed. In the EDX analysis results, Ni, O, The presence of Ti and C elements was observed in the samples. 5 Sample Content (by weight %) Ni O Ti C TiC - - 77.10 22.90 NiO 88.07 11.93 - - NiO-1TiC 79.26 5.08 3.40 1.78 NiO-5TiC 71.13 6.07 5.48 3.25 NiO-10TiC 64.70 7.25 6.41 5.59 Table 6. EDX analysis results of nanocomposites. Dielectric constants and dielectric loss factors at room temperature from 20 Hz to 3 MHz. Measurements were taken in the frequency range. The dielectric constant and dielectric loss values ​​increased by 10 and the frequency decreased and nanocomposite samples were more than the pure form of the compounds It has been found to exhibit good electrical properties. For the pure form of the compound, at 1 kHz... The dielectric constant was found to be 362. For the resulting composite, it was found to be 133. As can be seen, the dielectric constant of the composite is lower than that of the compound. It was observed. From the AC electrical properties results, multiple 15 in the composite samples It has been confirmed that the interfaces improve the dielectric properties compared to composites. Furthermore, according to another study, the synthesized NiO-Fe2O3 composite (maximum dc conductivity 0.0039 S cm-1) higher dc conductivity compared to the compound It was found that it showed. In other similar studies, lanthanum, cerium, copper and chromium, etc. The contribution of metals to the dielectric and electrical properties was investigated. As a result of the contribution, 20 Significant improvements in electrical properties were found. In this study, increasing frequencies The obtained and calculated ε′, ε″ and σac values ​​of NiO-TiC nanoparticles are shown in Figure. This is shown in Figure 8. These figures show that the values ​​of ε′ and ε″ decrease as the frequency increases, and further It shows that when high frequencies are reached, constant numbers are reached. Low The composite with the highest dielectric constant at the frequencies is TiC 25, which has the highest dielectric constant by weight. It was found that the nanoparticles have a doping effect. The detected ε′ values, with several previous reports and also with the results obtained regarding the pure form of NiO It was observed that it was higher when compared. The increase in ε′ values, quantum size state occurring in synthesized NiO nanoparticles This can be attributed to the ε″ value, which also tends to decrease with frequency and is highest at high frequencies. is low. These values ​​can be explained by defects in the prepared nanostructures, therefore 5 A higher value indicates larger defects in the samples. Table 7 shows the dielectric constant and dielectric loss factor observed at a frequency of 1 kHz. and includes AC conductivity values. When the values ​​at 1 kHz frequencies are analyzed, TiC An improvement in electrical properties is observed as the content increases. Sample Dielectric Constant (ε') Dielectric Loss (ε') σac conductivity (S / cm) AC conductivity (log σac) (S / cm) NiO 22.928 30.639 1.808x10-8 -7.742 1wt% TiC, 99% NiO 25,548 34,140 2,015x10-8 -7,695 5wt% TiC, 95% NiO 47,013 58,009 3,529x10-8 -7,452 10wt% TiC, 90% NiO 49,596 256,242 1,250x10-7 -6,902 TiC 54.835 9905.399 4.681x10-6 -5.329 Table 7. Electrical analysis results at 1 kHz. As the TiC doping ratio by weight increases, both at constant voltage and at increasing speeds A significant increase in current value was observed at different voltages. Table 8 shows the current values ​​at different voltages. Numerical indicators of the change in current values ​​of NiO and NiO nanoparticles It shows. 15 16 Sample 0.1V 2V 5V 10V NiO 2.00x10-7 8.04x10-7 2.23x10-6 5.53x10-6 1wt% TiC, 99% NiO 2.02x10-7 9.40x10-7 3.31x10-6 1.13x10-5 5wt% TiC, 95% NiO 5.01x10-7 1.04x10-7 3.23x10-6 9.55x10-5 10wt% TiC, 90% NiO 4.05x10-6 1.02x10-7 2.62x10-4 5.61x10-4 Table 8. Current values ​​of NiO nanocomposites in different voltage ranges. DC conductivity of NiO composites doped with 5% and 10% by weight of TiC The temperature change has been studied from room temperature to 350 K. Semiconductor materials. As a characteristic feature, the σdc value of TiC-doped NiO composites is 5. It increases with temperature. Composites are linear compared to the change in lnσ-1000 / T. It has undergone a change. This relationship is explained by the Arrhenius formula. Here, σo pre- The exponential factor is Ea, the activation energy is kB, the Boltzmann constant is T, and T is the temperature. Activation their energies are 0.038 eV for 5% TiC-reinforced composite and for 10% TiC-reinforced composite. It was found to be 0.023 eV. 10 σ = σ exp (6) 20

Claims

17 REQUESTS 1) 0.5 M Nickel (II) acetate tetrahydrate into 25 ml methanol in Beaker 1 (1) Mixture-1 (Methanol + C4H14NiO8) is formed by adding (C4H14NiO8) and Stirring on a magnetic stirrer until dissolved, 2. Beaker (2), 25 ml 5 Mixture-2 is formed by adding 2.5 M Sodium Hydroxide (NaOH) to methanol. (Methanol + NaOH) is formed and the pH balance of the solution is maintained until the solute is dissolved. Mixing these two solutions in a magnetic stirrer until 3. Beaker (3) by combining them and adding another 10 ml of methanol to the mixture, Mixture-3 (NiO) the solution was prepared by stirring it in a magnetic stirrer at 90°C for four hours. dissolving, mixing, and then cooling the solution to room temperature. allowing it to reach, filtering the nanoparticles through filter paper and with alcohol. washing, filtering and after washing the nanoparticles in an oven Drying at 70°C, then placing the dried nanoparticles in an oven at 500°C for one hour. crushing in a mortar without annealing and then the annealing process 15 Obtaining pure NiO nanoparticles and TiC-added NiO by carrying out the process. Repeating the same process steps to produce TiC-reinforced nanoparticles in nanoparticles, nano-TiC particles in 20 ml of methanol (1%, 5%, 10%) by weight Addition in the specified percentages, followed by 30 minutes in an ultrasonic homogenizer. Mixing in Beaker (4) and Mixture-4 (Methanol+TiC) 20 The formation of Mixture-3 and Mixture-4 by adding Mixture-5 to the 5th Beaker (5) (NiO+TiC) formation and all procedures performed to obtain pure NiO It is a hybrid nanocomposite material obtained by repetition, and its characteristic is that it maximizes 10% by weight Titanium Carbide (TiC) and at least 90% by weight Nickel Oxide (NiO) It is characterized by containing nanoparticles. 25

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