A SELF-COMPOSITE

Abstract

The invention relates primarily to a composite (self-composite) obtained by combining two physical forms of the same substance that have different physical structures but the same chemical structure, and more specifically, to a nano-micro hydroxyapatite self-composite obtained by combining the micro- and nano-structure properties of hydroxyapatite.

Description

1 TARIFF A SELF-COMPOSITE Technical Area The invention is based on the creation of identical substances that have different physical structures but the same chemical composition. a composite obtained by combining two physical forms of matter It relates to (self-composite), and more specifically to the microstructure of hydroxyapatite. nano-micro obtained by combining the properties of nanostructure It is related to the hydroxyapatite composite. 10 Previous Technique Hydroxyapatite is biocompatible, has no cytotoxic effects, and can be used in various morphological forms. 15, which stands out with its structure and its openness to ion and composite exchange properties. Its nature as a material makes its application areas quite broad. Hydroxyapatite It has the most stable structure compared to calcium-phosphate (Ca / P) compounds, in terms of Ca / P ratio. close to the Ca / P ratio in hard (teeth and bone) and soft (skin and muscle) tissues. This means that the structure forms a chemical bond within the body, becoming a complete unit with the existing tissue. By forming a bioactive material, it helps to remove diseased and 20 cells from the body. from the 1900s to the present day for the improvement and repair of damaged structures It has become an indispensable biomaterial for bone and tissue engineering. The porous structure of hydroxyapatite contains both anionic and cationic compounds. the presence of regions and its openness to ionic exchanges, crystallinity, temperature Its stability during increases and the fact that it does not have cytotoxic effects, making it environmentally friendly and 25 These features, along with the absence of toxic effects, make it suitable for the catalytic field. It is frequently used. Hydroxyapatite has a large surface area and an ionic structure. its susceptibility to change and composite formation, and its low water solubility. Due to its high thermal stability, it is frequently used as an adsorbent. It is used. 30 2 As can be understood from this brief information, hydroxyapatite has industrial uses. Its use in these fields is very high. Hydroxyapatite is used in these micro-fields. hydroxyapatite, nano-hydroxyapatite, or other types of these two varieties that differ from hydroxyapatite. They are used in the form of composites with other materials. Not only on their own... When used, their own physical and chemical properties are 5 This determines the efficiency of use. Hydroxyapatite has two types: nano and micro. Besides its individual use, it can be composited with many different materials. They also have uses in this way. Composites of this type... Their use combines the properties of two different materials, usually. To highlight the characteristic of one of the components that make up the composite, the other 10 The support of a material is provided by the composite created. As a result; composite The materials we have at hand have insufficient properties in the relevant field. It is used because of its durability; until now, different materials have always been used for composites. A solution was sought by using them together, which resulted in time and economic losses. This has caused it. 15 However, by combining two different forms of a material, high physical and a composite that will reveal chemical properties with current technology This has not been observed. Therefore, the inherent properties of an effective substance or material... With the use of composites, 20 advancements were made in science and materials science in a very short time. This will enable major breakthroughs in the synthesis of many new materials and the production of many materials that will make it possible to carry out the production A structure is needed that will also help reduce costs. The art is described in the Chinese patent document number CN115054733, which is listed as 25 in the known state of the art. a silk fibroin / hydroxyapatite composite micro-nanoparticle material The preparation method is described. The method involves silk fibroin nanoparticles. the powder is sequentially added to a solution containing calcium ions and phosphate ions By immersion, an auxiliary mineralization reaction is carried out, and the auxiliary 30 silk fibroin nanoparticles in the mineralization reaction process Nucleation sites are formed on their surfaces; silk fibroin nanoparticles 3 Hydroxyapatite growth can be promoted on it, and meanwhile, the next The mineralization process is also facilitated; subsequently, it undergoes auxiliary mineralization. captured silk fibroin nanoparticle powder into simulated body fluid The mineralization reaction is carried out by immersion, thus silk Self-assembly on fibroin nanoparticle powder 5 Hydroxyapatite crystals can be formed through this process and finally by freeze-drying. silk fibroin / hydroxyapatite composite micro-nanoparticles after processing The material is prepared. Silk prepared according to the invention. fibroin / hydroxyapatite composite micro-nanoparticle material directly applied to humans It can be applied to the body and has good biocompatibility, good stability and bone repair. 10 It possesses inducing ability characteristics. Brief Description of the Invention The aim of this invention is to create 15 identical organisms with different physical structures but the same chemical composition. a composite obtained by combining two physical forms of matter (self-composite) is the goal. Another objective of this invention is to compare the microstructure and nanostructure of hydroxyapatite. Nano-micro hydroxyapatite composite obtained by combining its properties 20 to accomplish. Detailed Description of the Invention To achieve the purpose of this invention, the "A Self-Composite" attached document, numbered 25, was created. as shown in the figures; Figure 1 shows the XRD pattern of nano-HA. Figure 2 shows the XRD pattern of micro-HA. Figure 3 shows the XRD pattern of Nano / Micro-HA (2:1). 30 Figure 4. SEM images of nano-HA. 4 Figure 5. TEM images of nano-HA. Figure 6. SEM images of micro-HA. Figure 7. TEM images of micro-HA. Figure 8. SEM images of Nano / Micro-HA (2:1). Figure 9. TEM images of Nano / Micro-HA (2:1). 5 Figure 10. a) Nano-Fe-HA, b) micro-Fe-HA and c) nano / micro-Fe-HA These are the PXRD patterns of the materials. Figure 11. EDS mapping images of nano-Fe-HA. Figure 12. EDS mapping images of micro-Fe-HA. Figure 13. EDS mapping images of Nano / Micro-Fe-HA (1:1). 10 Figure 14. Zoomed-in TEM of synthesized materials from 0.1 μm to 50 nm. images. (a; Nano-HA, b; Micro-HA, c; Nano / Micro-HA (2:1), d; Nano-Fe- HA, e; Micro-Fe-HA, f; Nano / Micro-Fe-HA (1:1) are the images.) Figure 15. Photocatalytic effect of different catalyst types on methylene blue. It is shown. 15 The subject of the invention is a composite, or autocomposite, consisting of materials with different physical structures but by combining two physical forms of the same substance that have the same chemical structure 20 obtained and combined before or combined with another substance Depending on their state, they reveal far more effective and superior qualities. The subject of the invention is a nano- / micro-hydroxyapatite composite, nano-hydroxyapatite and It is obtained by combining micro-hydroxyapatite structures, nano- The catalytic effects of hydroxyapatite and micro-hydroxyapatite structures are far greater than 25 It reveals a good performance. The subject of the invention is to synthesize nano- / micro-hydroxyapatite composite material. nano-hydroxyapatite (HA) and micro-hydroxyapatite (HA) are synthesized, then Nano-micro-HA 30 was synthesized using nano-HA and micro-HA. It is being synthesized. For nano-HA synthesis; Ca(NO3)2∙4H2O (CNTH, Calcium Nitrate Tetrahydrate) 7-12 Using g, DDW (Deionized Decarbonized Water) at ambient temperature (25±2°C) A 0.2M solution is prepared. (NH4)2HPO4 (DAHP, Diammonium Hydrogen) Using 2-4 g of phosphate (Cphosphate) with DDW at ambient temperature (25±2°C), the Ca / P ratio was 1.67 5. A 0.2M solution is prepared such that these two solutions are added to the flask with N2(g). in the environment, at room temperature (25±2°C) by drip method with additional columns After addition, the pH is adjusted to 11 with 25% NH3(aq). The process... then the mixing speed is kept constant and the aging process is carried out for 72 hours. is left. At the end of the aging period, 10 of the resulting solution are left in the desired amount. After being collected, washed (DDW), and filtered, they are kept in a vacuum at 80°C for 24-48 hours. It is left to undergo a drying process and Nano-HA is obtained. For micro-HA synthesis; Ca(NO3)2∙4H2O (CNTH, Calcium Nitrate Tetrahydrate) 2- 2.5 g of DDW was used to prepare a 0.1M solution at room temperature (25±2°C) for 15 minutes. It is prepared with (NH4)2HPO4 (DAHP, Diammonium Hydrogen Phosphate) 0.5-1 g. Using DDW, the Ca / P ratio will be 1.67 at ambient temperature (25±2°C). A 0.06M solution is prepared. 40 mL of CO(NH2)2 (Urea) is used at a concentration of 2.1-2.5 g. A solution is prepared using DDW at room temperature (25±2°C). This prepared solution... Solutions are placed in flasks in N2(g) medium, at room temperature (25±2°C) with additional columns 20 After being added by drip method, pH is adjusted to 4 with 10% HNO3(aq). It is adjusted, then left to mix for 2-4 hours. At the end of the process, 70 mL of the solution is taken, autoclaved at 180°C for 5 hours. Hydrothermal synthesis is performed. Post-synthesis washing (DDW) and filtration processes are carried out. then it is left to dry in a 40°C vacuum for 24-48 hours and Mikro-HA is obtained. 25 is being done. For the synthesis of Nano / Micro-HA composites; prepared Nano-HA and Micro-HA 70 mL of the solutions are taken at ratios of 2:1 and 6:1 (v / v) and autoclaved. Then it is synthesized hydrothermally at 180°C for 5 hours. Synthesis end washing 30 (DDW), drying at 40°C vacuum for 24-48 hours after filtration processes. 6 left and Nano / Micro-HA (2:1) and Nano / Micro-HA (6:1) self-composites is obtained. Another application of the invention is nano / micro-Fe-HA self-composite. It is being synthesized, and for this purpose, nano-Fe-HA and micro-Fe-HA are synthesized, 5 Using these synthesized materials, nano / micro-Fe-HA composite is obtained. is being done. For nano-Fe-HA synthesis; Ca(NO3)2∙4H2O (CNTH, Calcium Nitrate Tetrahydrate) Using 7-10 g of DDW (Deionized Decarbonized Water), heat at room temperature for 10 minutes. A 0.2M solution is prepared at (25±2°C). Fe(NO3)3∙9H2O (INNH, Iron(III) Using 1.4-2 g of nitrate nonahydrate, at a Ca / Fe ratio of 9:1, DDW A 0.2M solution of (Deionized Decarbonized Water) at room temperature (25±2°C). It is prepared with (NH4)2HPO4 (DAHP, Diammonium Hydrogen Phosphate) 2-4 g. Using DDW at ambient temperature (25±2°C), the (Ca+Fe) / P ratio will be 1.67. A 0.2M solution is prepared as shown. These solutions are placed in a flask in N2(g) medium. after addition with additional columns by drip method at room temperature (25±2°C) The pH is adjusted to 11 with 25% NH3(aq), and the mixing speed is adjusted after the process. It is fixed in place and left to age for 72 hours. Aging period Finally, a sample of the resulting solution is taken, and then subjected to washing (DDW) and filtration. 20 As a result of these processes, they are left to dry in a vacuum at 80°C for 24-48 hours. Nano-Fe-HA is obtained. For micro-Fe-HA synthesis; Ca(NO3)2∙4H2O (CNTH, Calcium Nitrate Tetrahydrate) A 0.09M solution was prepared by DDW at room temperature (25±2°C) using 2-2.5 g. It is being prepared. Fe(NO3)3∙9H2O (INNH, Iron(III) Nitrate Nonahydrate) 0.4-0.8 g DDW (Deionized Decarbonized Water) is used with a Ca / Fe ratio of 9:1. A 0.01M solution is prepared at ambient temperature (25±2°C) with (NH4)2HPO4. (DAHP, Diammonium Hydrogen Phosphate) 0.5-1 g used with DDW medium A 0.06M solution is prepared at a temperature of 25±2°C such that the (Ca+Fe) / P ratio is 1.67. The solution is prepared by DDW in 40 mL using 2.1-2.5 g of CO(NH2)2 (Urea). 7 The solutions are prepared at ambient temperature (25±2°C). These prepared solutions are then poured into a flask. In N2(g) medium, at room temperature (25±2°C) by drip method with additional columns It is adjusted to pH 4 with 10% HNO3(aq) added, then left to steep for 2-4 hours. The mixture is left to mix. At the end of the process, 70 mL of the solution is taken and... It is synthesized hydrothermally at 180°C for 5 hours by autoclaving. Synthesis end 5 Washing (DDW), followed by filtration processes, then 24-48 hours in a 40°C vacuum. It is left to dry and micro-Fe-HA is obtained. For the synthesis of Nano / Micro-Fe-HA (1:1) self-composite; prepared Nano-Fe-HA and 70 mL of micro-Fe-HA solution is taken at a 1:1 (v / v) ratio, autoclaved, and then... It is synthesized hydrothermally at 180°C for 5 hours. End-of-synthesis washing (DDW), After the filtration process, they are left to dry at 40°C vacuum for 24-48 hours. Nano / Micro-Fe-HA (1:1) self-composite is obtained. After the syntheses were completed, 15 samples were taken to examine the catalytic effect of the material. Photocatalytic experiments have been conducted. For use in photocatalytic experiments. Iron-doped nano-, micro-, and nano / micro-Fe-HA materials It was synthesized by preparing 10 ppm, 100 mL solutions of methylene blue (MB). Photocatalytic experiments under UV light in a reflux condenser system. This was carried out. The characterization of the obtained products was performed using TGA (Thermal 20 Gravimetric Analysis), FTIR (Fourier Transform Infrared Spectroscopy), PXRD (Powder X-ray Diffraction Spectroscopy), SEM (Scanning Electron Electron Spectroscopy) Microscope), TEM (Transmission Electron Microscope), BET surface analysis With these techniques, the analysis of photocatalytic experiments is also done using UV-Vis Spectroscopy. This was achieved using various techniques. 25 of the synthesized materials... The most important analyses in its characterization are PXRD, SEM, and TEM analyses. PXRD analyses of the obtained Nano-, Micro-, and Nano / Micro-Hydroxyapatite samples. Upon examination, it was found that a Nano / Micro-Hydroxyapatite composite was synthesized. It can be seen. 8 The XRD pattern of the synthesized microhydroxyapatite is shown in Figure 2. 10% The peaks with the highest diffraction intensity are shown from left to right according to the JCPDS 9-432 reference chart. to the right respectively 8.17 (1 0 0), 3.44 (0 0 2), 3.17 (1 0 2), 3.08 (2 1 0), 2.814 (2 1 1), 2.778 (1 1 2), 2.720 (3 0 0), 2.631 (2 0 2), 2.262 (3 1 0), 1.943 (2 2 2), 1.890 (3 1 2), 1.841 (2 1 3), 1.780 (4 1 0), 1.754 (4 0 2, 3 0 3), 1.722 (0 0 4, 4 1 1) 5 It is in the form of. For nano hydroxyapatite, the peak of 100 (2 1 1) is the reflection peak, while for micro For hydroxyapatite, the peak of 100 (3 0 0) is the reflection peak. However, nano The intensity of the (0 0 2) reflection peak, which is 40 in hydroxyapatite, is higher in microhydroxyapatite. lower and (3 1 0) reflected peak intensity is higher It is seen. 10 The XRD pattern of synthesized Nano / Micro-Hydroxyapatite (2:1) is shown in Figure 3. It is observed that hydroxyapatite with more than 10% diffraction intensity peaks are seen in JCPDS 9-432. According to reference card number, from left to right respectively 8.17 (1 0 0), 3.44 (0 0 2), 3.17 (1 0 2), 3.08 (2 1 0), 2.814 (2 1 1), 2.778 (1 1 2), 2.720 (3 0 0), 2.631 (2 0 2), 15 2.262 (3 1 0), 1.943 (2 2 2), 1.890 (3 1 2), 1.841 (2 1 3), 1.780 (4 1 0), 1.754 (4 0 2, 3 0 3), 1.722 (0 0 4, 4 1 1). Nano / Micro-HA (2:1) in Figure 3 XRD patterns correspond to characteristic peaks of JCPDS 9-432. This demonstrates nano / micro-self-composite with nano-HA and micro-HA PXRD. When the patterns are compared, the self-composite nano and micro hydroxyapatite 20 It is seen that their structures contain... The SEM image of Nano-HA shown in Figure 4 and the TEM image shown in Figure 5. From the images, it can be seen that Nano-HA has a rod-type morphology at the nanoscale. It is understood that SEM and TEM images of micro-HA are shown in Figures 6 and 7. This is seen in Figure 6, which shows SEM images of Mikro-HA. When its morphological structure is examined, it has a plate / sheet-like structure. This is understood from the TEM images of Mikro-HA in Figure 7. The formation of a microstructure is observed in hydroxyapatite. Nano / micro hydroxyapatite SEM and TEM images of the self-composite are shown in Figures 8 and 9. Figure 30 When the SEM images of Nano / Micro-HA (2:1) in 8 are examined, morphological 9 The structure contains nano and micro-sized hydroxyapatite particles and is rod-type. It is seen that it is in structure. In Figure 9, Nano / Micro-HA (2:1) TEM The images are shown. When the images are examined, it is seen that the microstructure has shrunk. It appears that it interacts with the nanostructure and a composite structure is formed. Nano / micro-HA self-composite, nano-HA and micro-hydroxyapatite structures to compare their catalytic effects from wastewater containing methylene blue (MM) Removing methylene blue from wastewater by breaking it down using a photocatalytic method. Studies have been conducted on breaking down methylene blue and improving its photocatalytic performance. to increase and improve its mechanical properties with nano-hydroxyapatite 10 A new material, nano / micro-Fe-, is created by attaching iron to micro-hydroxyapatite. Catalyst synthesis was achieved by synthesizing HA. The synthesized Nano-Fe-HA, PXRD patterns of micro-Fe-HA and nano / micro-Fe-HA materials are shown in Figure 10. It is observed that peaks with diffraction intensity above 10% are compared with the JCPDS reference number 9-432. According to the card, from left to right respectively 8.17 (1 0 0), 3.44 (0 0 2), 3.17 (1 0 2), 3.08 (2 1 15 0), 2.814 (2 1 1), 2.778 (1 1 2), 2.720 (3 0 0), 2.631 (2 0 2), 2.262 (3 1 0), 1.943 (2 2 2), 1.890 (3 1 2), 1.841 (2 1 3), 1.780 (4 1 0), 1.754 (4 0 2, 3 0 3), 1.722 (0 0 4, The PXRD patterns of the materials shown in Figure 10 are as follows: 4 1 1). It is consistent with the characteristic peaks of hydroxyapatite with card number 9-432. The added Fe entered the structure without disrupting the hydroxyapatite structure. Materials from SEM-EDS mapping images of synthesized products the constituent elements show a homogeneous distribution in the material This is seen in Figures 11, 12 and 13. The synthesized Nano-Fe-HA, micro-Fe-HA and TEM images of nano / micro-Fe-HA self-composite structures are shown in Figure 14. 25 It is seen that the TEM images also show that the structure has been damaged due to the entry of iron into the structure. No degradation was observed. When the BET analyses of the samples shown in Table 1 are examined, it is seen that the self-composites that surface areas have an intermediate value between micro and nano scales, and this is 30 This shows that pore diameters vary depending on the environment. Table 1. BET surface area results of the materials. When SEM-TEM images were examined, it was observed that the self-composite hydroxyapatites were of different types (5). It was observed that it contains nanorods of average dimensions according to the Debye-Scherrer method. Crystal sizes varied in the self-composite structures; the self-composite Their dimensions are between nano and micro structures. The average crystalline size of the materials. Their magnitudes are given in Table 2. Table 2. Average crystal sizes of the materials. 11 After the synthesis of nano-micro composites, their catalytic effect is most pronounced in wastewater. methylene blue, one of the pollutants found, is removed from water for photocatalysis. Studies have been conducted on its removal through degradation. Photocatalytic experiment In their studies, they found that a basic environment increased the catalytic active site of the catalyst and It was observed that its effect on degradation was positive. At pH 11, 5 from the catalyst Independent, direct decomposition occurred. The pH that works best. The contribution of this point to the active site of hydroxyapatite is observed at pH 9. This has been observed. Accordingly, the parameters determined were used in the process. In the experiments, the material that worked best was Nano / Micro-Fe-HA (1:1) and It was observed that the degradation was completed at 86%. The reusability of the catalyst is 10 Measured across 4 different sets, the average was taken, resulting in success in 3 cycles. It has yielded results. Effect of Catalyst Type on Degradation: To determine the photocatalytic catalytic effects, different types of catalysts were used with methylene blue. optimum conditions to study the degradation effects on blue This has been determined. Figure 15 shows different catalysts applied with the selected parameters. The photocatalytic effect of these types on methylene blue is observed. Nano / Micro-Fe-HA The degradation of (1:1) reached 54.4% in the first 30 minutes. In the 2nd hour, this reached 20%. This situation approaches 72% for Nano / Micro-Fe-HA (1:1) while for other catalysts... This situation reaches a maximum level of 40% (Nano-Fe-HA). At the end of the 4th hour, however... Nano / Micro-Fe-HA (1:1) catalyst had the highest degradation amount at 86.03%. It has yielded results and appears to be the type of catalyst that operates with the highest efficiency. This invention represents the first time novel self-composite materials of hydroxyapatite have been developed. Iron-fixed Nano / Micro-Fe-HA that can be used in photocatalytic treatment. The self-composite has been synthesized. 12 Industrial Application of the Invention The significance of this discovery lies in the fact that, for the first time, a substance can be synthesized using its nano and micro structures. The synthesis of the composite is the process of analyzing the resulting structure of the material. It is called a "self-composite". This study shows how a substance can be formed from 5 different types. composite prepared from crystal structures, that is, self-composite, far superior properties compared to the single crystal form / structure of the substance It has been proven that this is possible. In fact, self-composites of different materials can be formed. This also paves the way for the synthesis of composites, bringing new superior achievements to the scientific world. It has been shown that materials with similar properties can be synthesized. 10 Around these fundamental concepts, a wide variety of inventions can be developed for the subject of the invention, "A Self-Composite". It is possible to develop applications, and the invention is illustrated with the examples described here. It cannot be restricted, it is essentially as stated in the claims.

Claims

13 REQUESTS 1. Two substances of the same substance that have different physical structures but the same chemical structure. obtained by combining its physical form and without combining Much more effective than their previous forms or when combined with other substances. 5 and a composite characterized by revealing superior properties In other words, self-composite.

2. By combining nano-hydroxyapatite and micro-hydroxyapatite structures 10 of the obtained nano-hydroxyapatite and micro-hydroxyapatite structures by revealing a performance far superior to its catalytic effects Characterized nano- / micro-hydroxyapatite self-composite.

3. Synthesis of nano-hydroxyapatite (HA) and micro-hydroxyapatite (HA), nano-HA and micro-HA synthesized subsequently were used to produce nano-micro-HA 15 a nano- / micro- like the one in Claim 2 characterized by its synthesis Hydroxyapatite self-composite.

4. Using Ca(NO3)2∙4H2O (CNTH, Calcium Nitrate Tetrahydrate) 7-12 g DDW (Deionized Decarbonized Water) at ambient temperature (25±2°C) 20 Preparation of a 0.2M solution: (NH4)2HPO4 (DAHP, Diammonium Hydrogen) Ca / P ratio determined by DDW at ambient temperature (25±2°C) using 2-4 g of phosphate. A 0.2M solution is prepared such that the concentration is 1.67, and these two solutions are placed in a flask. Dropping with additional columns in N2(g) medium, at room temperature (25±2°C) After addition via the method, pH is adjusted to 11 with 25% NH3(aq), 25 Following the process, the mixing speed is kept constant and the aging process is carried out for 72 hours. the solution formed in the desired amount at the end of the aging period is left to... After being collected, washed (DDW), and filtered, the product is stored in a vacuum at 80°C for 24 hours. By leaving it to dry for 48 hours and obtaining Nano-HA. A nano- / micro-hydroxyapatite 30 as characterized in Claim 2 or 3 self-composite. 14 5. For micro-HA synthesis; Ca(NO3)2∙4H2O (CNTH, Calcium Nitrate Using 2-2.5 g of (tetrahydrate) by DDW at room temperature (25±2°C) Preparation of a 0.1M solution: (NH4)2HPO4 (DAHP, Diammonium Hydrogen) Ca / P 5 phosphate (0.5-1 g) was analyzed by DDW at ambient temperature (25±2°C). Preparation of a 0.06M solution of CO(NH2)2 (Urea) such that the ratio is 1.

67. Solution prepared with 40 mL DDW at room temperature (25±2°C) using 2.1-2.5 g. preparation, these prepared solutions are placed in a flask in N2(g) environment, room after being added by drip method with additional columns at temperature (25±2°C Adjusting the pH to 4 with 10% HNO3(aq), then immersing for 10 minutes between 2-4 hours. left to mix, and at the end of the process, 70 mL of the solution is taken Hydrothermal synthesis at 180°C for 5 hours by autoclaving, end of synthesis. Washing (DDW), followed by filtration processes, then 24-48 hours in a 40°C vacuum. characterized by being left to dry and obtaining Micro-HA A nano- / micro-hydroxyapatite self-composite as in claim 2 or 3. 15 6. 2:1 and 6:1 (v / v) mixtures of prepared Nano-HA and Micro-HA solutions. 70 mL of the mixture was taken and autoclaved, then kept at 180°C for 5 hours. hydrothermal synthesis, post-synthesis washing (DDW), and filtration processes. then left to dry in a 40°C vacuum for 24-48 hours and Nano / Micro-20 By obtaining HA (2:1) and Nano / Micro-HA (6:1) self-composites a nano- / micro- as in any of Claims 2 to 5 characterized Hydroxyapatite self-composite.

7. Nano-Fe-HA and micro-Fe-HA were synthesized, and these synthesized substances were 25 a nano / micro-Fe-HA characterized by its production through its use self-composite.

8. Using Ca(NO3)2∙4H2O (CNTH, Calcium Nitrate Tetrahydrate) 7-10 g DDW (Deionized Decarbonized Water) at ambient temperature (25±2°C) for 30 minutes Preparation of a 0.2M solution: Fe(NO3)3∙9H2O (INNH, Iron(III) Nitrate Using 1.4-2 g of (nonahydrate) calcium (Ca / Fe) in a 9:1 ratio, DDW 0.2M of (Deionized Decarbonized Water) at ambient temperature (25±2°C) Solution preparation: (NH4)2HPO4 (DAHP, Diammonium Hydrogen Phosphate) (Ca+Fe) / P ratio determined by DDW at ambient temperature (25±2°C) using 2-4 g. A 0.2M solution is prepared to obtain a concentration of 1.67, and these solutions are poured into the flask in 5 increments. Dropping with additional columns in N2(g) medium, at room temperature (25±2°C) After addition via this method, adjust the pH to 11 with 25% NH3(aq), Following the process, the mixing speed is kept constant and the aging process is carried out for 72 hours. the solution formed in the desired amount at the end of the aging period is left to... After being collected, washed (DDW), and filtered, the products are stored in a vacuum at 80°C for 24-10 days. By leaving it to dry for 48 hours and obtaining Nano-Fe-HA. A nano / micro-Fe-HA self-composite as characterized in Claim 7.

9. Using Ca(NO3)2∙4H2O (CNTH, Calcium Nitrate Tetrahydrate) 2-2.5 g Preparation of a 0.09M solution by DDW at ambient temperature (25±2°C), 15 Fe(NO3)3∙9H2O (INNH, Iron(III) Nitrate Nonahydrate) 0.4-0.8 g using DDW (Deionized Whey) at a Ca / Fe ratio of 9:

1. A 0.01M solution of decarbonized water at room temperature (25±2°C) Preparation: (NH4)2HPO4 (DAHP, Diammonium Hydrogen Phosphate) 0.5-1 g Using DDW at ambient temperature (25±2°C), the (Ca+Fe) / P ratio was 1.

67. A 0.06M solution is prepared such that CO(NH2)2 (Urea) contains 2.1-2.5 g. 40 mL of solution was prepared using DDW at room temperature (25±2°C) preparation, these prepared solutions are placed in a flask in N2(g) environment, room added by drip method with additional columns at temperature (25±2°C) Adjusting the pH to 4 with 10% HNO3(aq), then simmering for 2-4 hours. left to mix, and at the end of the process, 70 mL of the solution is taken Hydrothermal synthesis at 180°C for 5 hours by autoclaving, end of synthesis. Washing (DDW), followed by filtration processes, then 24-48 hours in a 40°C vacuum. characterized by being left to dry and obtaining Micro-Fe-HA A nano / micro-Fe-HA self-composite as in Claim 7. 30 16 10. 1:1 (v / v) mixture of prepared Nano-Fe-HA and Micro-Fe-HA solutions 70 mL is taken, autoclaved, and hydrothermated at 180°C for 5 hours. synthesis, post-synthesis washing (DDW), and filtration processes followed Drying at 40°C vacuum for 24-48 hours and Nano / Micro-Fe-HA (1:1) self-composite is obtained by any 5 of 7-9 A nano / micro-Fe-HA self-composite, like the one in the first one. 15 25

Images