Development of 3d-printed ti6al4v-based implant with osseointegration and immunomodulatory properties in which naturally derived hydroxyapatite is incorporated

Abstract

Titanium-based metal implants have brought about revolutionary changes in dental and orthopedic treatments, leading to advances in therapeutic technologies. However, metal-based implants still face unresolved challenges, such as difficulties or delays in osseointegration and inflammation caused by immune responses. To address these challenges, technologies such as plasma treatment of the surface of a metal-based implant or inclusion of bioactive components in implant materials are being researched, but there are problems with fracture and separation from metal implant materials. The present invention relates to a technology for providing osseointegration implant powder for use in a selective laser melting (SLM)-type metal 3D printer. The present invention provides a technology that enables printing by sintering and pulverizing horse bone and mixing the resulting horse bone with a metal powder implant material. Through the above-described configuration, the present invention has addressed the problem in which it was not possible to normally print a 3D implant structure since osseointegration components were burned off during a 3D printing process in an SLM-type metal 3D printer, and enables the printing of 3D structures including osseointegration components in an SLM-type metal 3D printer.

Description

Development of a 3D-printed TI6AL4V-based implant with osseointegration and immunomodulatory properties, containing naturally derived hydroxyapatite.

[0001] The present invention relates to a technology for manufacturing implants for use in bone using SLM 3D printing technology. More specifically, it includes a technology for manufacturing implants for improving osseointegration and immunomodulatory capabilities.

[0002] Prior art prior to the filing of the present invention disclosed a mature 3D-printed composition and its use. This technology provides a 3D structure comprising a sufficient number of chondrocytes and a cross-linked biopolymer formulation. The 3D composition exhibits mechanical stability suitable for transplantation into a subject.

[0003] Another prior art discloses a method for providing a cartilage implant containing chondrocytes. This technology discloses a method for providing a cartilage implant by differentiating iPSCs into chondrocytes and incorporating them into a matrix / scaffold.

[0004] Titanium-based metal implants have revolutionized dental and orthopedic treatment and advanced treatment techniques. However, metal-based implants still face challenges, such as difficulty or delay in osseointegration and inflammation caused by immune responses. Research is underway to address these issues, including plasma treatment of the metal implant surface and the incorporation of bioactive components into the implant material. However, these implants often break and detach from the metal implant material.

[0005] Although the technology of incorporating biocomponents is not difficult when manufacturing implants from materials such as polymers, the technology of incorporating biocomponents into metal implant materials is still in the development stage.

[0006] The present invention seeks to provide a technique for incorporating a biocomponent into a metal implant material.

[0007] To solve the above problems, the following problem-solving methods are provided.

[0008] In a method for manufacturing an osseointegration implant powder used in a metal 3D printer using the Selective Laser Melting (SLM) method,

[0009] A blood removal step (S1) for washing horse bones in water to remove blood; and

[0010] A first drying step (S2) of drying the horse bones from which blood has been removed in the above blood removal step in the shade; and

[0011] A bleaching step (S3) in which the horse bones dried in the first drying step are immersed in hydrogen peroxide solution at a ratio of 1:3 to 1:5 (v / v) to bleach them; and

[0012] An organic matter removal step (S4) in which organic matter remaining in the horse bones that have gone through the above bleaching step is removed by chemical means by immersing them in a 1M NaOH solution for 24 hours; and

[0013] A washing step (S5) of removing organic matter from the horse bones in the organic matter removal step and then washing them using distilled water; and

[0014] A secondary drying step of drying the horse bones washed in the above washing step in the shade; and

[0015] A first sintering step of sintering the horse bones dried in the above second drying step in an electric furnace at 600°C for 2 hours; and

[0016] A crushing step of crushing the first sintered horse bone using a grinder; and

[0017] A second sintering step of sintering the horse bones crushed in the above crushing step in an electric furnace at 900°C for 4 hours; and

[0018] EB (Equine Bone) powder manufactured through a fine grinding step of finely grinding the sintered horse bone in the above second sintering step using a high-energy ball mill; and

[0019] A method for manufacturing an osseointegration implant powder for use in a metal 3D printer of the Selective Laser Melting (SLM) method is provided, characterized in that the powder is manufactured by mixing the metal Ti (Ti6Al4V, average particle size of 35 μm) powder that can be used in the metal 3D printer of the Selective Laser Melting (SLM) method and the EB powder.

[0020] In addition, a method for manufacturing an osseointegration implant powder used in a metal 3D printer using a Selective Laser Melting (SLM) method is provided, characterized in that the mixing ratio of the metal Ti and the EB powder is 100:0.05 to 100:5 v / v.

[0021] In addition, a method for manufacturing an osseointegration implant powder for use in a metal 3D printer using a Selective Laser Melting (SLM) method is provided, characterized in that the average powder size of the EB powder is 1 μm or less.

[0022] In addition, a method for manufacturing an osseointegration implant powder used in a metal 3D printer using a Selective Laser Melting (SLM) method is provided, characterized in that the first sintering is performed at 600°C for 2 hours, the heating rate is 5°C / min, and 600°C is maintained for 2 hours.

[0023] In addition, a method for manufacturing an osseointegration implant powder used in a metal 3D printer using a Selective Laser Melting (SLM) method is provided, characterized in that the secondary sintering is performed at 900°C for 4 hours, the heating rate is 5°C / min, and 900°C is maintained for 4 hours.

[0024] The present invention solves the problem that in a metal 3D printer using the Selective Laser Melting (SLM) method, the osseointegration component burns out during the 3D printing process, making it impossible to print a 3D structured implant normally, and is an invention that has the effect of enabling a metal 3D printer using the Selective Laser Melting (SLM) method to print a 3D structure containing an osseointegration component.

[0025] Additionally, it is an effective technology that enables robust printing with no issues with the strength of the 3D printed result because it contains a small amount of osseointegration components.

[0026] Figure 1 is a photograph of three types of titanium and titanium and EB mixture powders to be used in SLM 3D printing of the present invention.

[0027] Figure 2 shows a surface microscope photograph and hardness measurement results of the 3D printing results of the Ti / EB mixture of the present invention and the Ti / HA used previously.

[0028] Figure 3 shows the results of measuring the hydrophilicity of the printed surface with the Ti, Ti / EB 0.05, and Ti / EB 0.5 experimental groups.

[0029] Figure 4 shows the results of confirming the chemical composition of the support using X-ray photoelectron spectroscopy (XPS) analysis of the Ti, Ti / EB 0.05, and Ti / EB 0.5 experimental groups.

[0030] Figure 5 shows the results of morphological analysis and structural characteristic analysis using a scanning electron microscope for the Ti, Ti / EB 0.05, and Ti / EB 0.5 experimental groups.

[0031] Figure 6 shows the evaluation of osteoblast adhesion / proliferation ability of the Ti, Ti / EB 0.05, and Ti / EB 0.5 experimental groups.

[0032] Figure 7 shows the results of observation of osteoblast attachment using a scanning electron microscope in the Ti, Ti / EB 0.05, and Ti / EB 0.5 experimental groups.

[0033] Figure 8 shows the results of evaluating the osteogenic differentiation ability of osteoblasts in the Ti, Ti / EB 0.05, and Ti / EB 0.5 experimental groups on a titanium / horse bone scaffold.

[0034] Figure 9 shows the results of an inflammatory response experiment of cultured RAW264.7 cells in the Ti, Ti / EB 0.05, and Ti / EB 0.5 experimental groups.

[0035] The operational effects of the invention according to the above-described configuration of the present invention are explained using drawings as follows.

[0036] The 3D printer that the present invention will be used for is a technology that creates a three-dimensional object by stacking successive layers of materials, and is widely applied in the industrial field for producing prototypes using product drawings. A 3D printer creates a three-dimensional object by stacking various materials such as plastic, metal, and ink layer by layer. The method of making an object using a 3D printer is to first scan the object to be made using a scanner.

[0037] After a three-dimensional scan, it is saved as image data on a computer, and the shape data of the saved structure is sliced ​​horizontally at a certain thickness and stacked as if integrated to print the object.

[0038] There is a method of melting and stacking polymers or plastics for lamination, and to create a 3D printed structure with metal, there is a method of supplying metal powder in the amount of layer stacking thickness, irradiating the metal powder with a laser to melt the metal powder and combine it with the existing laminate while stacking it in the vertical direction. This is called the SLM method. The SLM method is a method in which a laser is irradiated to the metal powder, and only the metal powder in the area where the laser was irradiated is melted and stacked.

[0039] This method is used to print and use implants for use in biological bone tissue. Biocompatibility is crucial for implants used in such bone tissue. However, implants using only metals such as titanium have had the problem of very low biocompatibility. To solve this problem, a method of plasma-coating the surface of the 3D-printed implant with hydroxyapatite (HA) is being studied. This technology offers convenience in terms of process, as it only requires a plasma coating process after 3D printing, but it has a major drawback in that the plasma-coated HA surface peels off too easily.

[0040] In order to solve this problem, the present invention developed a technology for mixing components extracted from horse bones into 3D printing metal powder using the SLM method.

[0041] As mentioned above, the SLM method prints 3D-shaped implants by melting and layering metal powder using a laser. Therefore, materials that are not burned or structurally deformed by the laser must be used in the SLM printer.

[0042] In order to solve the above problems, the present invention developed a method of using nanoparticles obtained by sintering horse bones with excellent biocompatibility by mixing them with metal powder.

[0043] For this purpose, horse bones were sintered using the following method.

[0044] 1) Wash the horse bones with tap water three times over four hours to remove blood.

[0045] 2) Dry the horse bones with the blood removed in the shade for 72 hours.

[0046] 3) Soak the dried horse bones in hydrogen peroxide solution at a ratio of 1:3 to 1:5 (v / v) and bleach at room temperature for 48 hours.

[0047] 4) After removing organic matter from the bleached horse bones by physical means, the organic matter was removed by chemical means in a 1M NaOH solution for 24 hours.

[0048] 5) After removing organic matter, wash at least 5 times using distilled water.

[0049] 6) Dry the horse bones from which organic matter has been removed in the shade at room temperature for 72 hours.

[0050] 7) Sinter the dried horse bones in an electric furnace at 600℃ for 2 hours.

[0051] (Heating rate: 5℃ / min, holding time: 2 hours)

[0052] 8) Grind the horse bones sintered in an electric furnace using a grinder.

[0053] 9) Sinter the crushed horse bones in an electric furnace at 900℃ for 4 hours.

[0054] (Heating rate: 5℃ / min, holding time: 4 hours)

[0055] 10) Finely pulverize the sintered horse bones using a high-energy ball mill.

[0056] (450 RPM, 10 minutes grinding, 50 minutes cooling, 10 times)

[0057] 11) Metal Ti powder uses a metal named Ti6Al4V, and the average particle size of the metal Ti powder (TC-450, Toho Technical Service Co.) is approximately 35 μm.

[0058] 12) The average powder size of the HB powder (Jeju, Korea) manufactured through the above steps 1) to 10) is ~1 μm, and the metal Ti and HB powder were mixed by ball milling using a planetary mill at a rotation speed of 200 rpm for 12 hours.

[0059] 13) Ti6Al4V powder with a size of 35 μm or less and HB powder with a size of 1 μm or less were mixed at 0%, 0.05%, and 0.5% (v / v) and used in the experiment.

[0060] Figure 1 is a photograph of three types of titanium and titanium and EB mixture powder to be used in the SLM 3D printing of the present invention. Ti6Al4V powder with a size of 35 μm or less and EB (a result of washing, sintering, and crushing horse bones) with a size of 1 μm or less were mixed at 0%, 0.05%, and 0.5% (v / v), respectively, and then uniformly mixed using a planetary mill (200 RPM, 12 hours). Using the mixed powder, a 3D scaffold was printed using the Selective Laser Melting method. The 3D scaffolds thus printed were named Ti (EB 0%), Ti / EB 0.05 (EB 0.05%), and Ti / EB 0.5 (EB 0.5%), respectively, and used in the experiment.

[0061] Fig. 2 shows the surface micrographs and hardness measurement results of the 3D printing results of the Ti / EB mixture used in the existing Ti, HA and the Ti / EB mixture of the present invention. As a result of photographing the 3D printing result with an electron microscope, it was observed that the heterogeneous bone powder was embedded between the titanium structures (Ti / EB 0.5, bottom left, enlarged right). This form shows a clear difference from the recently popular hydroxyapatite (HA) plasma coating method, in which the limitation of the plasma coating method that it is prone to peeling has been recently reported. However, in the present invention, since the EB powder is embedded inside the titanium, it does not peel off and is maintained firmly even against external impact. In addition, since the EB powder can act as an attachment site when cells adhere to the outer wall, it can be confirmed in the following content that it has a positive effect not only on cell attachment but also on cell viability.

[0062] The hardness analysis results shown on the right side of Fig. 2 show that Ti / EB 0.5 has a measurement value of 650 hv, which is a high measurement value compared to the hardness of titanium or HA coating supports.

[0063] Figure 3 shows the results of measuring the hydrophilicity of the printed surfaces of the Ti, Ti / EB 0.05, and Ti / EB 0.5 experimental groups. 10 μl of distilled water was dropped onto the surface of the sample, and the contact angle, which is the angle between the sample surface and the water droplet, was measured. The specimens were placed on a Water Contact Angle Analyzer (Kruss, Easydrop), and 3-distilled water was dropped for measurement. The contact angles were measured for a total of 8 samples per experimental group. The significance of the experimental results was verified using one-way ANOVA, and a post-hoc test was performed using Duncan's Multiple Range Test. The contact angles of the Ti, Ti / EB 0.05, and Ti / EB 0.5 experimental groups were measured to be 79.7° (±1.3°), 66.8° (±2.3°), and 64.7° (±3.5°), respectively. The experimental results confirmed that the support containing EB powder exhibited higher hydrophilicity.

[0064] Figure 4 shows the chemical composition of the scaffolds using X-ray photoelectron spectroscopy (XPS) analysis of the Ti, Ti / EB 0.05, and Ti / EB 0.5 experimental groups. As the amount of EB powder added increased, the content of horse bone-derived calcium phosphate powder increased, and thus the Ca2p binding ratio tended to increase. The measurement of these components was determined to be due to the formation of covalent bonds between the titanium powder and horse bone-derived calcium phosphate powder during the process of manufacturing the 3D scaffold using a Selective Laser Melting 3D printer, thereby forming a chemical bond of the components.

[0065] Figure 5 shows the results of morphological and structural characterization analyses of the Ti, Ti / EB 0.05, and Ti / EB 0.5 experimental groups using a scanning electron microscope (SEM). The microstructure of the surface of the experimental groups was confirmed using a scanning electron microscope (FE-SEM, Carl Zeiss, SUPRA 55VP, Germany). In addition, the chemical composition of the experimental groups was confirmed using Energy Dispersive Spectrometry (EDS).

[0066] Scanning electron microscopy was performed under the conditions of acceleration voltage = 2 kV, WD = 3.5 mm, and aperture size = 30 μm, and EDS was measured under the conditions of acceleration voltage = 6 kV, WD = 5 mm, and aperture size = 60 μm. In the Ti / EB 0.05 and Ti / EB 0.5 experimental groups, it was confirmed that calcium phosphate powder derived from horse bone was protruding on the surface. In particular, as the content of EB powder increased, the surface waviness became more severe and the uniformity of the processed surface decreased.

[0067] EDS measurement results showed that as the content of EB powder increased, the content of calcium phosphate powder derived from horse bone increased, and the ratio of Ca and P increased.

[0068] Figure 6 shows the osteoblast adhesion / proliferation evaluation of the Ti, Ti / EB 0.05, and Ti / EB 0.5 experimental groups. A crucial aspect of biocompatibility testing is the attachment and proliferation of osteoblasts to implants implanted in bone. The results of this experiment were used to confirm this.

[0069] In the present invention, the osteoblast proliferation ability of Ti, Ti / EB 0.05, and Ti / EB 0.5 3D scaffolds was evaluated using the WST-1 cytotoxicity Kit. The osteoblasts used were MC3T3-E1 (ATCC, CRL-2593) cell lines derived from Mus musculus mouse. The osteoblasts were cultured using Dulbecco's Modified Eagle's Medium (DMEM, Welgene) containing 10% fetal bovine serum (FBS, Welgene) and 1% antibiotics (Antibiotics, Welgene), and the osteoblasts were treated at a concentration of 1 × 105 cells / well on the titanium / horse bone scaffolds. The osteoblasts were cultured in a CO2 incubator at (37 ± 1) ℃ and (5 ± 1)% CO2 concentration. The proliferation capacity of osteoblasts was quantified by measuring the absorbance (OD450) at a wavelength of 450 nm after treating the WST-1 cytotoxicity kit (Daeillab, EZ-3000) reagent for 1 hour on days 1, 3, and 7. The test results were verified for significance using one-way ANOVA, and a post-hoc test was performed using Duncan's Multiple Range Test. There was no significant difference between the experimental groups in the test results on day 1 and day 3 after cell culture, and in the test results on day 7 after cell culture, it was confirmed that the Ti / EB 0.05 experimental group showed the highest proliferation capacity significantly.

[0070] The results of this experiment confirmed that when 0.05% of equine bone powder was included, it contributed to improving the proliferation ability of osteoblasts.

[0071] Figure 7 shows the results of observing the osteoblast attachment in the Ti, Ti / EB 0.05, and Ti / EB 0.5 experimental groups using a scanning electron microscope. The attachment of osteoblasts to the surface of the experimental groups was confirmed using a scanning electron microscope (FE-SEM, Carl Zeiss, SUPRA 55VP, Germany) under the conditions of acceleration voltage = 2 kV, WD = 3.5 mm, and aperture size = 30 μm. The osteoblasts used were MC3T3-E1 (ATCC, CRL-2593) cell lines derived from Mus musculus mouse, and the osteoblasts were cultured using Dulbecco's Modified Eagle's Medium (DMEM, Welgene) containing 10% fetal bovine serum (Fetal Bovine Serum, Welgene) and 1% antibiotics (Antibiotics, Welgene).

[0072] Osteoblasts were cultured on Ti, Ti / EB 0.05, and Ti / EB 0.5 supports at a concentration of 1×105 cells / well for 24 hours, fixed with 4% paraformaldehyde, and treated with 2% Osmium Tetroxide solution for 30 minutes (Vapor Fixation).

[0073] The samples were coated with platinum (approximately 25 nm), a conductive material, for scanning electron microscopy (SEM) observation and then pretreated. An increase in the cell surface area of ​​osteoblasts was observed in the experimental group containing horse bone-derived calcium phosphate powder (EB). The filopodia at the cell tips tended to extend toward the horse bone powder (EB). This can be interpreted as demonstrating the biocompatibility of osteoblasts and EB powder particles.

[0074] Figure 8 shows the results of evaluating the osteogenic differentiation ability of osteoblasts in the Ti, Ti / EB 0.05, and Ti / EB 0.5 experimental groups on titanium / horse bone scaffolds. In the present invention, the initial osteogenic differentiation ability was evaluated by measuring ALP activity. This experiment was performed to quantitatively evaluate the amount of alkaline phosphatase (ALP), an early marker, secreted into the cell matrix when osteoblasts were differentiated on each of the Ti, Ti / EB 0.05, and Ti / EB 0.5 scaffolds. The osteoblasts used were MC3T3-E1 (ATCC, CRL-2593) cell lines derived from Mus musculus, mouse, and the osteoblasts were cultured using Dulbecco's Modified Eagle's Medium (DMEM, Welgene) containing 10% fetal bovine serum (Fetal Bovine Serum, Welgene) and 1% antibiotics (Antibiotics, Welgene). Osteoblasts were cultured on titanium / horse bone scaffolds at a density of 1*?*105 cells / well for 1 week and then replaced with osteogenic differentiation medium. Osteogenic differentiation medium was prepared by adding 0.1 μM dexamethasone, 100 μM ascorbic acid, and 10 mM β-glycerophospate to Dulbecco's Modified Eagle's Medium (DMEM, Welgene) containing 10% fetal bovine serum (Fetal Bovine Serum, Welgene) and 1% antibiotics (Antibiotics, Welgene). Osteoblasts were cultured in a CO2 incubator at (37 ± 1) ℃ and (5 ± 1)% CO2 concentration. Samples were prepared by adding 1X Assay buffer with Triton X-100 to the cells on days 1, 3, and 7 after the initiation of osteogenic differentiation, incubating them at 4 ℃ for 15 minutes, and collecting the supernatant to prepare cell extracts.To detect the activity of ALP, an equal amount of pNPP colorimetric alkaline phosphatase substrate was mixed with the cell extract, incubated for 60 minutes, and the absorbance at 405 nm was measured using a microplate reader.

[0075] After osteoblasts were differentiated for 1, 3, and 7 days on each of the Ti, Ti / EB 0.05, and Ti / EB 0.5 supports, the ALP concentration in the cell matrix was measured. As a result, it was confirmed that the concentration of ALP increased as the osteogenic differentiation period increased in all experimental groups, and in particular, it was confirmed that the ALP concentration of the Ti / EB 0.05 experimental group was the highest on the 7th day.

[0076] Figure 9 shows the results of an inflammatory response experiment of Ti / EB using the Western blot technique for the Ti, Ti / EB 0.05, and Ti / EB 0.5 experimental groups. To investigate the inflammatory response of each scaffold of Ti, Ti / EB 0.05, and Ti / EB 0.5, the expression of inflammatory proteins (pro-inflammatory proteins: IL-6 and TNF-α; anti-inflammatory proteins: IL-4 and TGF-β) was tested using the Western blot method. This experiment was conducted to observe the response of macrophages when the 3D printed implant was implanted in the body. The scaffold was placed on the bottom of a well plate, and a transwell insert was then placed on the scaffold. Raw264.7 cells were seeded on the transwell insert, which did not make direct contact with the scaffold, and the difference in the expression of inflammatory proteins (IL-6 and TNF-α) was observed between the experimental groups. Although there were no significant differences between the experimental groups, Raw 264.7 cells cultured on the Ti / EB 0.05 scaffold showed the lowest expression of anti-inflammatory proteins (IL-4 and TGF-β). This result confirms that the scaffold containing EB powder exhibits a lower inflammatory response and better biocompatibility.

[0077] As described above, biocompatibility tests were conducted on the Ti, Ti / EB 0.05, and Ti / EB 0.5 experimental groups. The results showed that using Ti together with EB powder resulted in higher biocompatibility than using Ti alone.

[0078] The composition of the invention that exhibits the above-mentioned effects is as follows.

[0079] In a method for manufacturing an osseointegration implant powder used in a metal 3D printer using the Selective Laser Melting (SLM) method,

[0080] A blood removal step (S1) for washing horse bones in water to remove blood; and

[0081] A first drying step (S2) of drying the horse bones from which blood has been removed in the above blood removal step in the shade; and

[0082] A bleaching step (S3) in which the horse bones dried in the first drying step are immersed in hydrogen peroxide solution at a ratio of 1:3 to 1:5 (v / v) to bleach them; and

[0083] An organic matter removal step (S4) in which organic matter remaining in the horse bones that have gone through the above bleaching step is removed by chemical means by immersing them in a 1M NaOH solution for 24 hours; and

[0084] A washing step (S5) of removing organic matter from the horse bones in the organic matter removal step and then washing them using distilled water; and

[0085] A secondary drying step of drying the horse bones washed in the above washing step in the shade; and

[0086] A first sintering step of sintering the horse bones dried in the above second drying step in an electric furnace at 600°C for 2 hours; and

[0087] A crushing step of crushing the first sintered horse bone using a grinder; and

[0088] A second sintering step of sintering the horse bones crushed in the above crushing step in an electric furnace at 900°C for 4 hours; and

[0089] EB (Equine Bone) powder manufactured through a fine grinding step of finely grinding the sintered horse bone in the above second sintering step using a high-energy ball mill; and

[0090] A method for manufacturing an osseointegration implant powder for use in a metal 3D printer of the Selective Laser Melting (SLM) method is provided, characterized in that the powder is manufactured by mixing the metal Ti (Ti6Al4V, average particle size of 35 μm) powder that can be used in the metal 3D printer of the Selective Laser Melting (SLM) method and the EB powder.

[0091] In addition, a method for manufacturing an osseointegration implant powder used in a metal 3D printer using a Selective Laser Melting (SLM) method is provided, characterized in that the mixing ratio of the metal Ti and the EB powder is 100:0.05 to 100:5 v / v.

[0092] In addition, a method for manufacturing an osseointegration implant powder for use in a metal 3D printer using a Selective Laser Melting (SLM) method is provided, characterized in that the average powder size of the EB powder is 1 μm or less.

[0093] In addition, a method for manufacturing an osseointegration implant powder used in a metal 3D printer using a Selective Laser Melting (SLM) method is provided, characterized in that the first sintering is performed at 600°C for 2 hours, the heating rate is 5°C / min, and 600°C is maintained for 2 hours.

[0094] In addition, a method for manufacturing an osseointegration implant powder used in a metal 3D printer using a Selective Laser Melting (SLM) method is provided, characterized in that the secondary sintering is performed at 900°C for 4 hours, the heating rate is 5°C / min, and 900°C is maintained for 4 hours.

Claims

1. A method for manufacturing osseointegration implant powder used in a metal 3D printer using the Selective Laser Melting (SLM) method, A blood removal step (S1) for washing horse bones in water to remove blood; and A first drying step (S2) of drying the horse bones from which blood has been removed in the above blood removal step in the shade; and A bleaching step (S3) in which the horse bones dried in the first drying step are immersed in hydrogen peroxide solution at a ratio of 1:3 to 1:5 (v / v) to bleach them; and An organic matter removal step (S4) in which organic matter remaining in the horse bones that have gone through the above bleaching step is removed by chemical means by immersing them in a 1M NaOH solution for 24 hours; and A washing step (S5) of removing organic matter from the horse bones in the organic matter removal step and then washing them using distilled water; and A secondary drying step of drying the horse bones washed in the above washing step in the shade; and A first sintering step of sintering the horse bones dried in the above second drying step in an electric furnace at 600°C for 2 hours; and A crushing step of crushing the first sintered horse bone using a grinder; and A second sintering step of sintering the horse bones crushed in the above crushing step in an electric furnace at 900°C for 4 hours; and EB (Equine Bone) powder manufactured through a fine grinding step of finely grinding the sintered horse bone in the above second sintering step using a high-energy ball mill; and A method for manufacturing an osseointegration implant powder for use in a metal 3D printer using the Selective Laser Melting (SLM) method, characterized in that the powder is manufactured by mixing the metal Ti (Ti6Al4V, average particle size of 35 μm) powder that can be used in the metal 3D printer using the Selective Laser Melting (SLM) method and the EB powder.

2. In paragraph 1, A method for manufacturing an osseointegration implant powder used in a metal 3D printer using a Selective Laser Melting (SLM) method, characterized in that the mixing ratio of the metal Ti and the EB powder is 100:0.05 to 100:5 v / v.

3. In paragraph 2, A method for manufacturing an osseointegration implant powder for use in a metal 3D printer using a Selective Laser Melting (SLM) method, characterized in that the average powder size of the above EB powder is 1 μm or less.

4. In paragraph 3, A method for manufacturing an osseointegration implant powder for use in a metal 3D printer using a Selective Laser Melting (SLM) method, characterized in that the first sintering is performed at 600°C for 2 hours, the heating rate is 5°C / min, and the 600°C is maintained for 2 hours.

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