KR101256175B1 - Method for producing high hydrophilic implant - Google Patents

Abstract

Embodiments include a surface treatment step of adjusting the roughness of the implant surface; And it provides a method for producing a high hydrophilic implant comprising the step of hydrothermal treatment of the surface-treated implant.

Description

High hydrophilic implant manufacturing method {METHOD FOR PRODUCING HIGH HYDROPHILIC IMPLANT}

The example relates to a method of making a high hydrophilic implant. More particularly, the present invention relates to a method of providing an implant having improved hydrophilicity by hydrothermally treating an implant surface of which the roughness of the implant surface is controlled.

An implant is a biomedical medical instrument that is embedded in a living body and exerts its desired function. Therefore, implants should be manufactured using biocompatible materials that are very stable against biological tissues so that they do not have side effects and do not cause chemical and biochemical reactions. They are filled with complete bones without any soft tissues between bones and implants after being implanted in vivo. As the bone bonding force to be combined with the bone should be high. In addition, the implant should not be deformed or destroyed even under repeated loads and instantaneous pressures, and therefore the implant should be made of a material with very high mechanical strength.

In order to satisfy such conditions, various metals and alloys have been developed as suitable materials for implants. However, when a metal implant is implanted in a living body and placed in the body for a long time, the metal ion of the metal implant is eluted by the tissue fluid or body fluid in the body, and the metal ion of the metal implant is eluted by contacting or rubbing the metal implant in vivo. Due to the elution of these metal ions, the implant is corroded and macrophage of the living body reacts to induce inflammatory cells or giant cells.

For these reasons, the problem that the metal implant can not meet the biocompatibility (bio compatibility), chemical compatibility (mechanical compatibility) and mechanical compatibility (mechanical compatibility), etc., which is a condition to be provided as a biomaterial. In order to solve the above problems, various kinds of bio-ceramic and the like have been developed, but most of the ceramics are weak in impact and difficult to be processed, and thus, there is a problem in that they cannot be used alone to manufacture implants.

The most widely used implant materials at present are biocompatible titanium and titanium alloys. Titanium is not only easy to process, but also relatively lighter than other metals, and can be made of alloys of other metals or processed properly to improve strength, and is very dense and highly reformable in air or water. It forms an oxide film and has a very large corrosion resistance, and when it is embedded in bone, it has the great advantage of having a close bond of bone and osteointegration and is currently widely used as an implant material.

On the other hand, early dental implants used implants made of pure titanium with a smooth surface, but these implants had a problem that it took a long time or failed in the process of initial osteointegration because the average surface roughness value was not constant. .
Regarding the implant manufacturing method, Korean Patent No. 10-0750973 and the like are disclosed.

Example was devised to solve the above problems, the method of manufacturing a high hydrophilic implant according to the embodiment is to reduce the bone fusion time by producing an implant surface with improved hydrophilicity.

In order to achieve the above object, a method of manufacturing a high hydrophilic implant according to the embodiment includes a surface treatment step of adjusting the roughness of the implant surface; And hydrothermal treatment of the surface treated implant.

The method of manufacturing a high hydrophilic implant according to the embodiment can adjust the surface of the implant to the optimum roughness, thereby inducing faster initial fusion of the implant surface and the alveolar bone. In addition, the embodiment can provide an implant surface in which high hydrophilicity is simultaneously realized by hydrothermal treatment of the surface treated implant surface.

1 and 2 are flowcharts showing a method of manufacturing a high hydrophilic implant according to the embodiment.
3 is a photograph illustrating the hydrophilicity (wettability) of the implant surface according to the Examples and Comparative Examples.
4 is a photograph observing the contact angle between the implant surface and distilled water according to the Examples and Comparative Examples.

In the description of the embodiments, where each substrate, layer, film, or electrode is described as being formed "on" or "under" of each substrate, layer, film, or electrode, etc. , "On" and "under" include both "directly" or "indirectly" formed through other components. In addition, the upper or lower reference of each component is described with reference to the drawings. The size of each component in the drawings may be exaggerated for the sake of explanation and does not mean the size actually applied.

1 is a flow chart showing a method of manufacturing a high hydrophilic implant according to the embodiment. 1, the method of manufacturing a high hydrophilic implant according to the embodiment includes a surface treatment step (S1) for controlling the roughness of the implant surface; And hydrothermally treating the surface-treated implant (S3).

First, the surface treatment step (S1) for controlling the roughness of the implant surface is performed. Accordingly, the implant can adsorb more initial tissue fluid upon placement in the alveolar bone, and consequently, increase the migration and arrangement of osteogenic cells, thereby improving bone adhesion and biocompatibility.

The surface treatment step (S1) is not particularly limited as long as it is a method commonly used in the art to improve the roughness of the implant surface. For example, the surface treatment step may include a resorbable blast media (RBM) process, a sand blast process, a titanium plasma sprayed process, an acid-etched implant, an endophore process ( Endopore implant) and a combination thereof may be performed by a process selected from the group consisting of, but not limited thereto. More preferably, the surface treatment step may be carried out by a removable blast media process.

The removable blast median process refers to a process of increasing the surface roughness by spraying a media consisting of calcium and phosphorus onto the surface of the implant. By the above process, calcium and phosphorus remain on the surface of the implant, and the surface-treated implant can be fused without rejection when placed in the alveolar bone. In addition, since calcium and phosphorus are the main components to form the alveolar bone, it is possible to smooth the fusion of the implanted implant and alveolar bone.

For example, the removable blast media process uses calcium phosphate particles of about 180 μm to about 425 μm size to maintain the blast gun spray pressure at about 0.45 kgf / cm ² to about 0.65 kgf / cm ² . 10 seconds to about 25 seconds, but is not limited thereto. The surface roughness of the implant surface treated by the blastable median process may be about 1 μm to about 2 μm, and more specifically, the surface roughness may be about 1.2 μm to 1.8 μm, but is not limited thereto.

Alternatively, the surface treatment step may be performed by a titanium plasma sprayed process. The titanium plasma spray process is a method of dissolving another titanium at high temperature and spraying it with a spray to attach it to the implant surface. For example, the plasma spraying process may be performed by dissolving titanium-containing particles in whole or in part with a torch and spraying the same on the implant surface.

Meanwhile, the method for surface treatment of the implant using only one process has been disclosed so far, but the present disclosure is not limited thereto. That is, the embodiment may be performed together two or more of the above-mentioned processes. For example, the surface treatment step may be performed by a sandblast process first, and then by a sandblasted large grit (acid-etched; SLA). The sand blast process is to spray the fine particles on the implant surface made of titanium or titanium alloy, the fine particles may be used aluminum oxide (Al ₂ O ₃ ) of about 250 ㎛ to about 500 ㎛, but is not limited thereto. no. After the sandblasting process, the surface is post-treated with a strong acid (H ₂ SO ₄ / HCL) to solve the remaining blasting particles.

By the surface treatment step S1 mentioned above, the roughness of the implant surface is controlled. Roughness of the surface-treated implant surface may be improved to about 0.5 ㎛ to 10 ㎛. In more detail, the roughness of the surface-treated implant surface may be about 1 μm to 3 μm, but is not limited thereto. For example, the surface roughness of the implant surface treated by the blastable median process may be about 1 μm to about 2 μm, and more specifically, the surface roughness may be about 1.2 μm to 1.8 μm, but is not limited thereto. It doesn't happen. For example, the roughness of the surface of the implant surface-treated by the SLA process may be about 2 ㎛ to about 3 ㎛, more specifically, the surface roughness may be about 2.5 ㎛ to about 3 ㎛, but is not limited thereto. no.

Subsequently, the surface-treated implant surface is subjected to hydrothermal treatment (S3). In the hot water treatment, as the temperature rises, the water is changed to steam, and the inside of the chamber has a high pressure, and a metal oxide is formed due to the combination of the cation metal base material and oxygen of the anion generated during the hot water treatment process. It uses the principle of having surface characteristics.

The implant surface treated by the step S1 may be more hydrophilic by the hot water treatment process (step S3). The hydrothermal treatment process includes placing the surface treated implant in a pressure chamber filled with an inert gas; Heating the surface treated implant in vapor phase; Dipping the surface treated implant in acetone; And it may include the step of drying the surface-treated implant. Meanwhile, after the heating step and before the acetone immersion step, the surface-treated implant may be further removed to remove calcium hydroxide, but is not limited thereto.

The heating step may be performed at a temperature of about 150 ° C. to about 350 ° C., under a pressure of about 10 kgf / cm ² to about 65 kgf / cm ² , for about 1 minute to about 30 minutes. After the heating step, a cooling process may be further performed for about 1 minute to about 150 minutes at a cooling temperature of about 0 ℃ to about 100 ℃.

Subsequently, the teaching process is a process for removing calcium hydroxide, which is performed in an agitator having a rotational speed of about 200 rpm to about 400 rpm, more specifically, about 300 rpm using ultrapure distilled water for about 120 minutes to about 180 minutes. do. Thereafter, the acetone dipping and drying steps are for removing moisture on the surface of the implant, and are performed for about 1 minute and about 1 minute to about 60 minutes, respectively.

On the other hand, the high hydrophilic implant manufacturing method according to the embodiment so far described for the process of hydrothermal treatment after the surface treatment step, but is not limited thereto. Referring to Figure 2, the method of manufacturing a high hydrophilic implant according to the embodiment may further comprise the step (S2) after the surface treatment step (S1), coating the hydroxide apatite particles on the surface-treated implant surface. . By the coating step, the high hydrophilic implant according to the embodiment may further improve the crystallinity and bonding strength.

The coating step (S2) may be carried out by high-speed collision of the apatite hydroxide particles in a vacuum state on the surface of the implant treated under room temperature conditions. The room temperature coating step may be made with reference to the method disclosed in Korean Patent No. 10-913009, but is not limited thereto. For example, the surface of the surface-treated implant in a vacuum chamber that is decompressed to less than about 10 ^-1 torr by loading the apatite hydroxide particles in one or two or more of nitrogen, argon, helium, hydrogen carrier gas of less than about 100 ℃ The coating is fastened to a thickness of about 30 μm or less. If the coating thickness of the hydroxide apatite particles exceeds about 30 ㎛ may cause a problem that the coating layer is easily peeled off after the procedure. In addition, the high-speed collision speed of the hydroxide apatite particles in the vacuum chamber may be about 100 m / s or more, and when less than about 100 m / s, the coating may be abnormally produced, resulting in a weakening of the strength of the coating layer.

Hereinafter, one or more exemplary embodiments will be described in more detail with reference to non-limiting and exemplary embodiments, but the present disclosure is not limited thereto.

[ Example  1 and Example  2]

Surface treatment step

The implant surface was subjected to a revolve blast media process to improve surface roughness. In more detail, as the media, media including calcium phosphate particles having a size of about 180 μm to about 425 μm was used. In addition, the spray pressure of the blast gun was maintained at about 0.45 kgf / cm ² to about 0.65 kgf / cm ² . Under such conditions, the implant was surface treated for about 10 seconds to about 25 seconds.

Hydrothermal Treatment Step

The hydrothermal treatment was performed through two conditions, as shown in Table 1 below, thereby obtaining two samples.

[ Comparative example  One]

In Comparative Example 1, only the surface treatment (removable blast media) processes of Examples 1 and 2 were performed on the implant in the same manner.

[ Comparative example  2]

Comparative Example 2 was subjected to the same surface treatment (removable blast media) process in the same manner as in Example 1 and Example 2 to the implant. Subsequently, a coating step was performed as follows. First, the prepared HA powder was put into a hopper and a booster pump and a rotary pump were operated to reduce the vacuum chamber until it reached a range of about 10 ⁻² torr to 10 ⁻³ torr. Carrier gas of about 10 L / min to 100 L / min was introduced into the hopper while maintaining the pressure in the chamber constant. At this time, the hopper is already connected to the vacuum chamber, and shows a very low pressure. Turbulence occurs in the hopper due to the carrier gas introduced at 1 atm, and thus, fine HA powder is introduced into the vacuum chamber together with the carrier gas. The HA powder thus injected was sprayed through a spray nozzle having a fine hole. At this time, the HA powder was further accelerated due to the pressure difference before and after the nozzle and collided with the titanium implant surface, that is, the surface of the specimen. An HA coating layer about 5 μm thick was formed.

[Implant Surface Characterization]

Experiments were carried out on the hydrophilicity, contact angle, and cell adhesion for the Examples and Comparative Examples.

3 and Table 3 are photographs of hydrophilicity (or wettability) test results and measured values thereof. 3 is a photograph of 30 μl of ultrapure distilled water at room temperature dropping to the center of the disk and after 10 seconds. In addition, Table 3 is the value which measured the width | variety of the said water droplet using CAD.

3 and Table 3, in Example 1 and Example 2 compared to Comparative Example 1 and Comparative Example 2, the area of the water droplets increased by about three times or more. From this, it can be seen that the embodiments are significantly improved hydrophilicity compared to the comparative examples. That is, it can be seen that the hydrophilicity of the implant is further improved by the hydrothermal treatment performed after the RBM treatment.

Figure 4 is a photograph observing the contact angle test results using a contact angle measuring instrument (OCA 15 plus, Dataphysics Germany). When the samples prepared by Comparative Example 1, Comparative Example 2 and Example 2 were placed on the stage of the contact angle measuring instrument, about 8 μl of distilled water was formed at the end of the syringe, and the stage was raised so that the distilled water reached the surface of the sample. The contact angle between the sample and distilled water was measured. Referring to Table 4 below, Comparative Example 1 has a contact angle of about 86.5 °, Comparative Example 2 is about 102.2 ° to about 104.3 °, while the contact angle of Example 1 is significantly reduced to about 47.6 ° to 49.2 ° Could know. That is, it can be seen that the hydrophilicity of the implant is improved by performing the hydrothermal treatment (Example 1 and Example 2) after the RBM treatment, rather than simply performing the RBM treatment only on the implant.

Table 5 below is a graph showing the results of Cell adhesion assay of the Examples and Comparative Examples. As a sample, four disks having a diameter of 10 mm × 1.6 mm were used, and osteoblasts (MC3T3-E1 cells) were attached to each disk at 1 × 10 ⁴ cells / 100 μl. After 4 hours, the extent to which the osteoblasts adhered to the sample was measured at 595 nm by Elisa Reader through crystal violet staining. Referring to Table 5 below, it was found that the most increased cell adhesion in Example 1.

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.

Claims (5)

Surface treatment step of adjusting the roughness of the implant surface; And
Hydrothermal treatment of the surface-treated implant,
The hydrothermal treatment step,
Placing the surface treated implant in a pressure chamber filled with an inert gas;
Heating the surface treated implant in vapor phase;
Dipping the surface treated implant in acetone; And
Method for producing a high hydrophilic implant comprising the step of drying the surface-treated implant.
The method of claim 1,
The surface treatment step is selected from the group consisting of a resorbable blast media (RBM) process, a sandblast process, a titanium plasma sprayed process, an acid-etched implant, and a combination thereof. High hydrophilic implant manufacturing method carried out by the process.
3. The method of claim 2,
The removable blast media process,
180 to 425 ㎛ size calcium phosphate particles to the implant for a high hydrophilic implant manufacturing method for 10 seconds to 25 seconds under a pressure condition of 0.45 kgf / cm ² to 0.65 kgf / cm ² .
delete The method of claim 1,
In the heating step,
Method for producing a high hydrophilic implant is carried out for 1 to 30 minutes at a temperature of 150 ℃ to 350 ℃, 10 kgf / cm ² to 65 kgf / cm ² .

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