KR20130042441A - Porous implant, and preparing method of the same - Google Patents

Abstract

PURPOSE: A porous implant and a method for fabricating the same are provided to enable sustained release of a physiologically active material supported inside without difficult. CONSTITUTION: A method for fabricating a porous implant comprises: a step of classifying titanium or titanium alloy powder by size(S10); a step of filling a mold with the titanium or titanium alloy powder(S20); a step of sintering(S30); a step of removing the mold(S40); a step of sintering secondarily(S50); and a step of filling the porous implant with the physiologically active material. The size of the titanium or the titanium alloy powder is 1-45 micrometer. [Reference numerals] (S10) Step of classifying titanium or titanium alloy powder by sizes; (S20) Step of filling a shaping mold with the classified titanium or titanium alloy powder by sizes; (S30) Step of primarily sintering; (S40) Step of removing the shaping mold; (S50) Step of secondarily sintering;

Description

Porous implants, and methods for making the same {POROUS IMPLANT, AND PREPARING METHOD OF THE SAME}

The present application relates to a porous implant comprising internal pores uniformly connected and comprising pores of micro unit size, and a method of manufacturing the same.

In general, the implant is a biomaterial for human hard tissue replacement used in dentistry or orthopedics, and research on dental implants has been actively conducted since the mid-1960s.

Among the implant materials, titanium and titanium alloys are excellent biocompatibility materials, and are known to show good biocompatibility to surrounding tissues, as well as high corrosion resistance and little toxicity to the living body. For this reason, in the early stages of implant research, titanium or titanium alloys were simply machined and used as implants. As research progressed, bioactive substances such as hydroxyapatite were coated on the surface of implants to accelerate the healing period. For example, the Republic of Korea Patent No. 10-1042405, "hydroxyapatite coating method for bioactivation after surface modification of the dental implant" and the like.

However, the bioactive material coated on the surface is too fast to dissolve, and it is difficult to expect the effect of the coated material due to the high temperature generated in the coating process. It has been reported that such side effects can be caused, and a study was conducted on a method of supporting the bioactive material in the pores of the implant instead of coating the bioactive material on the implant surface.

However, in order to support the bioactive material in the pores inside the implant, it is necessary to easily and economically form pores uniformly connected to the inside of the implant, and the size of the pores also becomes an important factor. In general, it is difficult to expect a high treatment effect immediately after receiving an implant procedure, and a healing period of about 6 months is required until the implant and the hard tissue of the human body have a strong combination to achieve a high treatment effect. There was a difficulty in slowly releasing the bioactive material supported inside the implant for a period of 6 months.

The inventors can classify the titanium or titanium alloy powder by size and fill the molding mold with the first sintering, and then remove the molding mold and perform the second sintering to easily and economically prepare the porous implant. , The porous implant is connected to the inside of the uniform micro pores, there is no difficulty in supporting the bioactive material, and found that the bioactive material carried in the porous implant can be released slowly, Completed.

Thus, the present application, including the inner pores, the inner pores are uniformly connected, the size of the inner pores is adjustable according to the size of the titanium or titanium alloy powder is filled in the molding mold, the inner It is intended to provide a porous implant having a pore size in micro units, and a method of making the same.

However, the problem to be solved by the present invention is not limited to the above-mentioned problem, another task that is not mentioned will be clearly understood by those skilled in the art from the following description.

The first aspect of the present invention, the step of classifying the titanium or titanium alloy powder by size; A first sintering step of filling and heating a molding mold with the titanium or titanium alloy powder classified by size; And it provides a porous implant manufacturing method comprising a second sintering step of removing and heating the molding mold.

The second aspect of the present application provides a porous implant, prepared by the method of the first aspect of the present application, comprising internal pores.

According to the present invention, a porous implant can be easily and economically prepared by classifying titanium or titanium alloy powder by size and filling the molding mold with a first sintering, followed by removing the molding mold and performing a second sintering. , The porous implant of the present application is connected to the inside of the uniform fine pores, there is no difficulty in supporting the bioactive material, it is possible to achieve a slow release of the bioactive material carried in the porous implant.

More specifically, the interior of the porous implant of the present invention, the pores are evenly connected to the deep portion, the size of the pores can be adjusted according to the size of the titanium or titanium alloy powder filled in the molding mold, the pores It may have a micro unit size, and the sustained release bioactive material supported on the porous implant may be released slowly over a sufficient period required for the healing process using the implant, for example, about 6 months.

As it becomes possible to slowly release the bioactive substance contained therein using the porous implant of the present application, it is possible to use it to improve the process of differentiating undifferentiated cells into osteoblasts or to improve the bone quality of specific patients. Therefore, the effect of shortening the healing period using the implant and improving the success rate of the implant procedure can be expected.

1 is a flow chart of a porous implant manufacturing method according to an embodiment of the present application.
2 is a photograph of a molding mold manufactured by assembling a fire resistant tray mold and a quartz tube according to one embodiment of the present application.
Figure 3 is a SEM photograph taken after classifying the titanium powder by size according to an embodiment of the present application.
Figure 4 is a SEM photograph showing that the resin is uniformly penetrated into the porous implant by a predetermined thickness when the resin (resin) is injected into the porous implant according to an embodiment of the present application under a constant temperature and pressure.
5 is a SEM photograph showing a state in which the pores are connected in the porous implant according to an embodiment of the present application.
6A and 6B are photographs showing an experiment for confirming the presence of pores inside the porous implant by making a porous implant into a specimen and confirming the permeability of distilled water thereto.
FIGS. 7A and 7B are photographs of experimental preparations and results for confirming the presence of porous pores in the porous implants according to an embodiment of the present invention, and confirming the supporting property of the molten paraffin wax on the porous implants. to be.
8 is formed to confirm the support using a CLSM (confocal laser microscope) in a GFP (green fluorescent protein) supporting experiment for confirming the internal pores of the porous implant and the possibility of material loading by the porous implant according to an embodiment of the present application SEM image of one fracture surface.
9A to 9G show CLSM data indicating that the fracture surface of FIG. 8 was partially observed using CLSM, and that GFP was efficiently supported in the internal pores of the porous implant specimen according to the embodiment of the present application.

Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings so that those skilled in the art can easily carry out the present invention. It should be understood, however, that the present invention may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. In the drawings, the same reference numbers are used throughout the specification to refer to the same or like parts.

Throughout this specification, when a part is referred to as being "connected" to another part, it is not limited to a case where it is "directly connected" but also includes the case where it is "electrically connected" do.

Throughout this specification, when a member is located "on" another member, this includes not only when one member is in contact with another member but also when another member exists between the two members.

Throughout this specification, when an element is referred to as "including " an element, it is understood that the element may include other elements as well, without departing from the other elements unless specifically stated otherwise. The terms "about "," substantially ", etc. used to the extent that they are used throughout the specification are intended to be taken to mean the approximation of the manufacturing and material tolerances inherent in the stated sense, Accurate or absolute numbers are used to help prevent unauthorized exploitation by unauthorized intruders of the referenced disclosure. The word " step (or step) "or" step "used to the extent that it is used throughout the specification does not mean" step for.

Throughout this specification, the term "combination of these" included in the expression of the makushi form means one or more mixtures or combinations selected from the group consisting of constituents described in the expression of the makushi form, wherein the constituents It means to include one or more selected from the group consisting of.

Hereinafter, embodiments and examples of the present disclosure will be described in detail with reference to the accompanying drawings, but the present disclosure is not limited thereto.

The first aspect of the present invention, the step of classifying the titanium or titanium alloy powder by size; A first sintering step of filling and heating a molding mold with the titanium or titanium alloy powder classified by size; And it provides a porous implant manufacturing method comprising a second sintering step of removing and heating the molding mold.

In connection with the first aspect of the present application, Figure 1 shows a flow chart of a method for manufacturing a porous implant according to an embodiment of the present application. In the flow chart of Figure 1, the step of classifying the titanium or titanium alloy powder by size S10, the step of filling the titanium or titanium alloy powder classified by size into the molding mold S20, the first sintering step S30, removing the molding mold In step S40, the second sintering step is represented by S50.

For example, in the present application, titanium or titanium alloy powder was used to prepare a porous implant, but the titanium or titanium alloy is a biocompatible material and shows good biocompatibility to surrounding tissues, as well as resistance to corrosion. This is because the material is large and has little toxicity to the living body, and any material having these advantages can be used as an alternative material without limitation.

According to one embodiment of the present application, the method of manufacturing the porous implant may further include a step of filling a bioactive material into the porous implant formed after the second sintering step, but is not limited thereto. Here, the term "filling" means filling a material in the pores inside the porous implant, but may be a term having the same meaning as "support", but is not limited thereto. For example, BMP, PEP7, etc. may be applied as the bioactive material, but is not limited thereto. BMP described as an example of the bioactive substance is an abbreviation of Bone Morphogenetic Protein, and may include BMP-2 and BMP-6, which is evaluated as the most active substance among the bioactive substances. It is one of the substances. In addition, PEP7 described as an example of the physiologically active substance corresponds to the trade name of a synthetic peptide used as a strong bone-generating substance. The physiologically active substances may play a role in promoting bone production by, for example, differentiating undifferentiated stem cells into osteoblasts, but are not limited thereto.

In the porous implant of the present application, the pores are uniformly connected to the deep portion, and micro-sized pores are adjustable in size according to the size of the titanium or titanium alloy powder filled in the molding mold, and thus sustained-release physiology It may be advantageous to slowly release the bioactive material over a period of about 6 months after supporting the active material, but is not limited thereto. Here, the period in which the bioactive substance is slowly released is described as about 6 months, for example, in the healing process using an implant, a healing period of about 6 months is sometimes necessary, and after about 6 months Because healing is common, the need for slow release over a period exceeding about six months is small. However, the period during which the bioactive substance is slowly released is not limited to about 6 months, for example, about 1 month, about 2 months, about 3 months, about 4 months, about 5 months, or about 6 months. The physiologically active substance may be slowly released over, but is not limited thereto. As it is possible to slowly release the bioactive material contained therein using the porous implant of the present application, it is possible to improve the process of differentiating undifferentiated cells into osteoblasts or to improve the bone quality of specific patients using the porous implant. As a result, the effect of shortening the healing period using the implant and improving the success rate of the implant procedure can be expected, but is not limited thereto.

In this regard, Figure 4 is a SEM photograph showing that when the resin is injected into the porous implant according to an embodiment of the present application under a constant temperature and pressure, the resin has uniformly penetrated the inside of the porous implant by a certain thickness. The resin is injected in place of the bioactive material in order to determine whether the bioactive material can enter the porous implant, specifically, the SEM is taken after infiltrating the resin for hot mounting in the liquid phase into the liquid phase. At this time, the resin was shown to penetrate uniformly by a certain thickness according to the pressure applied from the outside, it is assumed that the similar pattern is shown even when injecting a bioactive material instead of the resin, but is not limited thereto. In addition, Figures 7a and 7b shows the results of the experiment confirmed that the paraffin wax is well supported in place of the bioactive material in the porous implant according to an embodiment of the present application, a more detailed description thereof will be described later in the Examples section of the present application It was.

According to one embodiment of the present disclosure, the step of classifying the titanium or titanium alloy powder by size may include, but is not limited to, performing through a sieve method. The term " sieving method "may refer to a method of classifying powder using a sieve having a predetermined size, but is not limited thereto.

According to one embodiment of the present disclosure, the step of classifying the titanium or titanium alloy powder by size may include classifying the titanium or titanium alloy powder in a size range of about 1 μm to about 45 μm, but is not limited thereto. It is not. For example, the step of classifying the titanium or titanium alloy powder by size may include about 2, about 3, about 4, about 4, about 4 μm of the titanium or titanium alloy powder having a size of about 1 μm to about 45 μm. It may include but is not limited to five, or about six kinds.

According to one embodiment of the present disclosure, the step of classifying the titanium or titanium alloy powder by size may include the titanium or titanium alloy powder having a size of about 1 μm or more and less than about 25 μm, and about 25 μm or more and less than about 32 μm. To be classified as being at least about 32 μm and less than about 38 μm, and at least about 38 μm and less than or equal to about 45 μm. Such a classification may correspond to the case where the titanium or titanium alloy powder is classified into about four kinds according to size, but is not limited thereto. In this regard, Figure 3 shows a SEM picture taken after classifying the titanium powder by size according to an embodiment of the present application.

For example, by classifying the titanium or titanium alloy powder by size and using the same for the preparation of the porous implant, it may be possible to control the size of the pores included in the porous implant as the size of a uniform micro unit. It is not limited.

According to one embodiment of the present application, the titanium or titanium alloy powder may include a spherical one, but is not limited thereto. When the spherical one is used as the titanium or titanium alloy powder, internal pores included in the porous implant may have the same spherical shape as the powder, but is not limited thereto.

According to the exemplary embodiment of the present application, the molding mold may include one manufactured using a quartz tube and a tray mold, but is not limited thereto. In this regard, Figure 2 shows a picture of a molding mold prepared by assembling a refractory tray mold and a quartz tube according to an embodiment of the present application.

According to one embodiment of the present application, the first sintering step may be to include heating under a high vacuum or inert atmosphere, but is not limited thereto. For example, a furnace of a high vacuum atmosphere may be used to perform the first sintering step in a high vacuum atmosphere, but is not limited thereto.

According to one embodiment of the present application, the first sintering step may include, but is not limited to, heating up slowly at an elevated temperature rate of about 10 ° C./min or less. For example, the first sintering step includes heating up slowly at a temperature increase rate of about 10 ° C./min or less, about 7 ° C./min or less, about 5 ° C./min or less, or about 3 ° C./min or less. It may be, but is not limited thereto. In this way, the temperature is slowly increased, but may not be applied to the electric furnace used at the time of temperature increase, but is not limited thereto.

According to an embodiment of the present disclosure, the first sintering step may include, but is not limited to, heating after heating at about 800 ° C. to about 1000 ° C. for about 1 hour to about 3 hours. For example, the first sintering step may be performed at a temperature of about 800 ° C. to about 900 ° C., about 800 ° C. to about 1000 ° C., or about 900 ° C. to about 1000 ° C., for about 1 hour to about 2 hours, about 1 hour to It may include, but is not limited to, heating after about 3 hours, or about 2 hours to about 3 hours. For example, the first sintering step may include, but is not limited to, cooling after heating at about 850 ° C. to about 900 ° C. for about 2 hours.

According to one embodiment of the present application, the second sintering step may be to include heating under a high vacuum or inert atmosphere, but is not limited thereto. For example, a furnace of a high vacuum atmosphere may be used to perform the second sintering step in a high vacuum atmosphere, but is not limited thereto.

According to one embodiment of the present application, the second sintering step may include, but is not limited to, heating up slowly at an elevated temperature rate of about 10 ° C./min or less. For example, the second sintering step may include heating up slowly at a heating rate of about 10 ° C./min or less, about 7 ° C./min or less, about 5 ° C./min or less, or about 3 ° C./min or less. It may be, but is not limited thereto. In this way, the temperature is slowly increased, but may not be applied to the electric furnace used at the time of temperature increase, but is not limited thereto.

According to one embodiment of the present application, the second sintering step may include, but is not limited to, cooling after heating at about 1200 ° C. to about 1400 ° C. for about 1 hour to about 3 hours. For example, the second sintering step may be performed at a temperature of about 1200 ° C. to about 1300 ° C., about 1200 ° C. to about 1400 ° C., or about 1300 ° C. to about 1400 ° C., from about 1 hour to about 2 hours, about 1 hour to It may include, but is not limited to, heating after about 3 hours, or about 2 hours to about 3 hours. For example, the second sintering step may include, but is not limited to, cooling after heating at about 1200 ° C. to about 1300 ° C. for about 2 hours. For example, the second sintering step may be performed under a higher temperature than the first sintering step, but is not limited thereto.

The second aspect of the present application provides a porous implant, prepared by the method of the first aspect of the present application, comprising internal pores.

The second aspect of the present disclosure relates to a porous implant manufactured according to the method of the first aspect of the present disclosure, and detailed descriptions of portions overlapping with the first aspect of the present disclosure are omitted, but the descriptions of the first aspect of the present disclosure Are equally applicable even if omitted from the description in the second aspect of the present application.

According to one embodiment of the present application, the size of the internal pores included in the porous implant may be determined according to the size of the titanium or titanium powder, but is not limited thereto. In addition, the shape of the pores included in the porous implant may be determined to be spherical according to the form of the titanium or titanium powder, but is not limited thereto.

According to one embodiment of the present application, the pore may be one having a uniform necking structure, but is not limited thereto. In this regard, Figure 5 is a SEM photograph showing a state in which the pores are connected inside the porous work plant according to an embodiment of the present application.

According to one embodiment of the present application, the size of the titanium or titanium powder may be about 1 μm to about 45 μm, but is not limited thereto. For example, the titanium or titanium powder has a size of at least about 1 μm and less than about 25 μm, at least about 25 μm and less than about 32 μm, at least about 32 μm and less than about 38 μm, and at least about 38 μm. It may be classified as having a size of about 45 μm or less, but may be used for preparing a porous implant, but is not limited thereto. In this regard, Figure 3 shows a SEM picture taken after classifying the titanium powder by size according to an embodiment of the present application.

For example, by classifying the titanium or titanium alloy powder by size and using the same for the preparation of the porous implant, it may be possible to control the size of the pores included in the porous implant as the size of a uniform micro unit. It is not limited.

For example, by adjusting the size of the titanium or titanium alloy powder to adjust the size of the pores, ultimately it is possible to achieve the effect of controlling the surface area inside the porous implant, but is not limited thereto. For example, the theoretical value of the surface area inside the porous implant according to the size of the titanium or titanium alloy powder can be expressed as shown in Table 1 below, but the actual internal surface area value is not limited thereto.

Diameter of powder (μm) Surface area inside the porous implant (cm ² / g) 50 266.4 40 333.0 30 444.0 25 532.8

According to one embodiment of the present application, the appearance of the porous implant may be determined according to the shape of the molding mold, but is not limited thereto. For example, when using a cylindrical molding mold, such as the molding mold of Figure 2 of the present application, the appearance of the porous implant prepared using the same may have a cylindrical shape, but is not limited thereto.

According to one embodiment of the present application, the porous implant may have a Young's modulus value of about 10 GPa to about 30 GPa, but is not limited thereto. For example, the porous implant may have a Young's modulus value of about 10 GPa to about 20 GPa, about 10 GPa to about 30 GPa, or about 20 GPa to about 30 GPa, but is not limited thereto. . For example, the porous implant may have a Young's modulus value similar to that of about 12 GPa to about 18 GPa, which is a Young's modulus of the human cortical bone, but is not limited thereto. For example, since the porous implant has a Young's modulus value similar to that of human cortical bone, biocompatibility may be higher when used as an implant applied to human cortical bone, but is not limited thereto.

According to one embodiment of the present application, the porous implant may be to include slowly releasing a bioactive material filled therein, but is not limited thereto. As the physiologically active substance, for example, BMP, PEP7 may be filled, but is not limited thereto.

In the porous implant of the present application, the pores are uniformly connected to the deep portion, and micro-sized pores are adjustable in size according to the size of the titanium or titanium alloy powder filled in the molding mold, and thus sustained-release physiology It may be advantageous to slowly release the bioactive material over a period of, for example, about 1 month, about 2 months, about 3 months, about 4 months, about 5 months, or about 6 months after loading the active material. However, the present invention is not limited thereto. With the porous implant of the present application, it becomes possible to slowly release the bioactive substance contained therein, thereby using it to improve the process of differentiating undifferentiated cells into osteoblasts or improving the bone quality of specific patients. As such, the effect of shortening the healing period using the implant and improving the success rate of the implant procedure can be expected, but is not limited thereto.

In this regard, Figure 4 is a SEM photograph showing that when the resin is injected into the porous implant according to an embodiment of the present application under a constant temperature and pressure, the resin has uniformly penetrated the inside of the porous implant by a certain thickness. The resin is injected in place of the bioactive material in order to determine whether the bioactive material can enter the porous implant, specifically, the SEM is taken after infiltrating the resin for hot mounting in the liquid phase into the liquid phase. At this time, the resin was infiltrated uniformly by a certain thickness according to the pressure applied from the outside, and it can be assumed that the similar pattern will be shown even when the bioactive substance is injected instead of the resin. As the bioactive material, for example, BMP, PEP7 and the like may be applied, but is not limited thereto.

Hereinafter, the porous implant of the present application will be described in more detail using examples, but the present application is not limited thereto.

[ Example ]

1. Preparation of Porous Implants

In this embodiment, a porous implant was prepared according to one embodiment of the present application, and a general order thereof was performed according to the flowchart of FIG. 1.

In the present embodiment, in order to manufacture a porous implant, Gr2, which is pure titanium powder, not titanium alloy powder, was used, which was used by TLS Technik GmbH & Co. Ltd. It was a product. At this time, the pure titanium powder was spherical in shape.

First, the titanium powder of various sizes having a diameter of about 45 μm or less was prepared, and then the powders were classified by size using a sieve method. Specifically, those having a size of about 1 μm or more and less than about 25 μm, those having a size of about 25 μm or more and less than about 32 μm, those having a size of about 32 μm or more and less than about 38 μm, and about 38 μm or more and about 45 μm It has the following size, it was used to classify according to the size to a total of four kinds. As described above, the SEM photographs were taken after classifying the titanium powders according to sizes, as shown in FIG. 3.

Thereafter, a molding mold for preparing a porous implant was prepared. In this embodiment, the molded mold was manufactured by assembling a fire resistant tray mold and a quartz tube, and a photograph thereof is shown in FIG. 2. In the photo of FIG. 2, a black block on the bottom corresponds to the fire resistant tray mold, and a plurality of transparent tubes inserted into the black block correspond to the quartz tube.

Thereafter, the molding powder was filled with the titanium powder classified by size, and a first sintering step was performed. In the first sintering, a high vacuum furnace was used to create a high vacuum atmosphere. Once heated to a temperature of about 850 ° C. at a slow rate of about 5 ° C./min, and then maintained at about 850 ° C. for about 2 hours, the first sintering step was completed by cooling to room temperature.

Thereafter, the molding mold was removed and a second sintering step was performed. The second sintering also used a high vacuum furnace to create a high vacuum atmosphere. Heated to about 1200 ° C., maintained at about 1200 ° C. for about 2 hours, and finishing the second sintering step by cooling to room temperature.

As a result, the porous implant of the present embodiment was completed, and the appearance of the porous implant was cylindrical according to the shape of the molding mold used, and spherical micro-sized pores were uniformly distributed in the porous implant according to the shape and size of the used titanium powder. there was. The pores were also necked to each other up to the deeper portion of the porous implant. SEM image showing that the pores are connected as shown in FIG.

Finally, the resin was loaded into the completed porous implant through the steps, Figure 4 of the present application, when the resin is injected into the porous implant under a constant temperature and pressure, the resin is fixed inside the porous implant It is a SEM photograph showing the penetration as uniformly as the thickness. The resin was injected in place of the bioactive material in order to determine whether the bioactive material can enter the porous implant, specifically, the SEM was taken after infiltrating the resin for hot mounting in the liquid phase into the liquid phase. At this time, the resin was infiltrated uniformly by a certain thickness according to the pressure applied from the outside, and it was estimated that the similar pattern was obtained even when the bioactive materials such as BMP and PEP7 were injected instead of the resin. In addition, referring to the thickness of the resin infiltrated, the material supported inside the porous implant over a period of about six months It was expected to be released slowly. Additional material loading experiments for the porous implants were described in more detail in Section 3 of this example.

2. Testing Physical Properties of Porous Implants

In order to confirm whether the porous implant prepared according to the present embodiment possesses suitable physical properties to be applied as an actual implant, an experiment of confirming four mechanical properties was performed, and the results were as described in Table 2 below. :

Powder size (μm) Tensile Strength (Mpa) Young's modulus (Gpa) density (%) About 1-about 25 About 368 Approximately 21 About 95 About 25-about 32 Approximately 263 About 28 About 80 About 32-About 38 Approximately 168 About 19 Approximately 73 About 38-about 45 About 160 About 22 Approximately 73

Referring to Table 2, the Young's modulus value of the porous implant prepared according to the present embodiment showed a range particularly similar to that of the human cortical bone, and thus used as an implant in the human bone. In particular, it is estimated that the biocompatibility and therapeutic effect can be maximized.

3. Experimental Support of Materials in Porous Implants

In addition to the experiments associated with FIG. 4 of the present application, additional experiments were conducted to confirm that the material can be effectively loaded in the porous implant prepared according to the present embodiment, and related experimental data are shown in FIGS. 6A to 9G. .

First, the porous implant prepared according to the present embodiment was fabricated into a specimen having a diameter of about 3 mm and a length of about 10 mm, and fitted to the end of the syringe tightly, and then distilled water was put in and pushed out. Before and after the bet was photographed, respectively, are shown in Figures 6a and 6b. In FIG. 6B, it was confirmed that distilled water continuously dropped drops, and through this, it was confirmed that pores were formed in the porous implant of the present application.

Next, a porous implant prepared according to the present example was prepared as a specimen, inserted into the end of the silicon tube, and the experiment was performed to suck the melted paraffin wax with a syringe. Preparations for the experiment are as shown in Figure 7a. At this time, if the molten paraffin wax is sucked in spite of the end of the silicon tube clogged with the specimen, it means that the specimen is capable of supporting the material inside as a porous structure, on the contrary, the molten paraffin wax to the specimen If it could not be sucked by the clogged silicon tube, this would mean that the specimen was pore-free and unable to carry material therein. As a result, it was confirmed that the paraffin wax penetrated the inside of the specimen as shown in FIG. 7B, and in particular, the paraffin wax was found in the center of the specimen, reconfirming that the specimen was effective in supporting the porous material as a porous structure. Could. Specifically, it can be seen from the photograph of FIG. 7b that the open pore structure is connected to the inside of the specimen. However, since the strength of the paraffin wax itself is weak, a slight portion of titanium was found in the surface polishing process.

Next, an experiment using a fluorescent material, Green Fluorescence Protein (GFP), was performed to more clearly confirm that the material can be supported in the porous implant prepared according to the present embodiment. First, the GFP solution was diluted to about 500 μg / ml, and one end of the silicone hose was fitted with the specimen and the other end with a syringe. The end of the specimen was inserted into the GFP solution. Attempt to pull the solution by pulling. Thereafter, the specimen was separated from one end of the silicone hose and immersed in a GFP solution to maintain a vacuum for 30 minutes, and then dried at room temperature for 24 hours. Then, the degree of GFP loading was confirmed by using a CLSM (Confocal Laser Scanning Microscope, confocal laser microscope). Here, GFP is a protein that is generally used to determine mobility by using fluorescence in vivo, and corresponds to a protein having a molecular weight similar to that of the bioactive substance, but not a bioactive substance. The porous implant specimen prepared according to the present invention was used to indirectly check whether the bioactive material can be efficiently supported.

On the other hand, in order to observe the GFP using the CLSM, the surface of the specimen should be formed in a plane, but in the experiment of this embodiment, it is necessary to cut the specimen to confirm that the GFP penetrated into the specimen. Since the micropores on the surface of the specimen could be swept or filled due to friction with the cutting tool in the process, they could not be observed in a planar manner and replaced by observing the fracture surface after fracture. At this time, the SEM image of the fracture surface after the fracture is shown in FIG. In the case of such a fracture surface, since there is a height difference unlike a general cut surface, it may act as a obstacle for observing GFP using CLSM, but it has succeeded in capturing and observing a partially focused area. As a result of the observation, it was confirmed that GFP was uniformly supported up to the inside of the specimen, and through this, the porous implant inside had a structure connected by uniform micropores, thereby confirming that the bioactive material could be easily loaded effectively. Could. Experimental data confirming GFP loading using CLSM are shown in FIGS. 9A to 9G.

In FIG. 9D, which includes half cuts (left) and half fractures (right), the left side cut by the diamond cutter shows a solid surface profile, with GFP stained with scratches. Confirmed. Also on the right side of FIG. 9D, GFP was found in some focused portions. In addition, FIG. 9E is a portion corresponding to the center portion of the specimen, and the GFP loading was surely confirmed. 9F and 9G, two specimens were inserted side by side at one end of the silicone hose, and then GFP was observed in the inner specimen, and even in this case, GFP was observed to a lesser extent. From this, it can be seen that the porous implant according to the present application is connected with uniform micropores, thereby effectively and easily supporting a bioactive substance similar to GFP.

It will be understood by those of ordinary skill in the art that the foregoing description of the embodiments is for illustrative purposes and that those skilled in the art can easily modify the invention without departing from the spirit or essential characteristics thereof. It is therefore to be understood that the above-described embodiments are illustrative in all aspects and not restrictive. For example, each component described as a single entity may be distributed and implemented, and components described as being distributed may also be implemented in a combined form.

The scope of the present invention is defined by the appended claims rather than the detailed description, and all changes or modifications derived from the meaning and scope of the claims and their equivalents should be interpreted as being included in the scope of the present invention .

Claims (21)

Classifying the titanium or titanium alloy powder by size;
A first sintering step of filling and heating a molding mold with the titanium or titanium alloy powder classified by size; And
A second sintering step of removing and heating the molding mold
/ RTI >
Method of making porous implants.
The method of claim 1,
Comprising the step of filling the bioactive material in the porous implant formed after the second sintering step, porous implant manufacturing method.
The method of claim 1,
The step of classifying the titanium or titanium alloy powder by size comprises performing by a sieve method (sieving method), porous implant manufacturing method.
The method of claim 1,
The classifying the titanium or titanium alloy powder by size includes classifying the titanium or titanium alloy powder in a size range of 1 μm to 45 μm, wherein the porous implant is manufactured.
The method of claim 1,
The step of classifying the titanium or titanium alloy powder by size, the size of the titanium or titanium alloy powder 1 μm or more and less than 25 μm, 25 μm or more and less than 32 μm size, 32 μm or more and less than 38 μm size And, and comprising a sorting of 38 μm or more and 45 μm or less in size, porous implant manufacturing method.
The method of claim 1,
The titanium or titanium alloy powder comprises a spherical one, a porous implant manufacturing method.
The method of claim 1,
The molding mold will be prepared using a quartz tube and a tray mold, porous implant manufacturing method.
The method of claim 1,
The first sintering step comprises heating under a high vacuum or inert atmosphere, porous implant manufacturing method.
The method of claim 1,
Wherein the first sintering step comprises heating to a temperature increase rate of 10 ℃ / min or less, the porous implant manufacturing method.
The method of claim 1,
The first sintering step comprises heating after cooling for 1 hour to 3 hours at 800 ℃ to 1000 ℃, porous implant manufacturing method.
The method of claim 1,
The second sintering step comprises heating under a high vacuum or inert atmosphere, porous implant manufacturing method.
The method of claim 1,
The second sintering step comprises heating to a heating rate of 10 ° C / min or less, the porous implant manufacturing method.
The method of claim 1,
The second sintering step comprises heating after heating for 1 to 3 hours at 1200 ℃ to 1400 ℃, a porous implant manufacturing method.
14. Prepared by the method according to claim 1 and comprising internal pores,
Porous Implants.
15. The method of claim 14,
The size of the inner pores is determined by the size of the titanium or titanium powder, porous implant.
15. The method of claim 14,
The internal pore is to have a uniform necking structure, porous implant.
The method of claim 15,
The size of the titanium or titanium powder is 1 μm to 45 μm, porous implant.
The method of claim 15,
The titanium or titanium powder is classified as having a size of 1 μm or more and less than 25 μm, a size of 25 μm or more and less than 32 μm, a size of 32 μm or more and less than 38 μm, and a size of 38 μm or more and 45 μm or less. Porous implant, which is used for the manufacture.
15. The method of claim 14,
The appearance of the porous implant is determined according to the shape of the molding mold, porous implant.
15. The method of claim 14,
The porous implant has a Young's modulus value of 10 GPa to 30 GPa, porous implant.
15. The method of claim 14,
The porous implant is to release the bioactive material filled therein, a porous implant.

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