KR101042405B1 - HA coating methods after two-step surface modification of dental implant for bioactivity - Google Patents

Abstract

The present invention comprises the steps of forming a micropore on the surface of the implant; Forming nanotubes on the surface of the implant in which the micropores are formed; Preparing a target to be coated on the surface of the nanotube using tooth powder; To provide a hydroxyapatite coating method for bioactivation after surface modification of the dental implant comprising the step of coating the implant surface by the EB-PVD method using the prepared tooth powder or artificially manufactured HA, As such, the present invention increases the biocompatibility through the surface modification for dental implants by forming micropores and nanotubes in two steps on the implant surface and coating them with EB-PVD method using extracted teeth or artificially manufactured HA. It is a very useful invention that can shorten the procedure period and extend the period of use as much as possible.

Implants, Surface Modification, Anodization, Bioactivity, Hydroxyapatite, Coating

Description

HA coating methods after two-step surface modification of dental implant for bioactivity

The present invention relates to a hydroxyapatite coating method for bioactivation after surface modification of a dental implant, and more specifically, to prepare a sputtering target using the extracted tooth micropore and nanotube in two steps on the implant surface The present invention relates to the development of a dental implant surface capable of shortening the dental procedure by permanently increasing the biocompatibility and bone fusion by coating tooth powder or artificial HA and shortening the dental procedure.

Recently, the economic level has been improved, the number of patients who want to implant implants for dental prosthetics is increasing significantly, and the demand for dental implants is greatly increased accordingly.

However, due to the problem of surface modification of dental implants, hydroxyapatite (HA) coating has been used on the surface of expensive implants to improve clinical biocompatibility. However, the problem that the life of the HA is greatly reduced due to the peeling phenomenon of HA in the clinically used implant surface.

In addition, although the conventional thermal spray method, Solgel method, anodization method, etc. have been studied, these problems had a problem of peeling when used clinically.

Major surface treatment technologies used to date include physical vapor deposition (PVD), chemical vapor deposition (CVD), ion beam enhanced deposition (IBED), and ion implantation methods to improve wear, corrosion and oxidation resistance of various dental materials. It is widely used to improve biocompatibility.

In particular, the thermal spray method is currently widely used when coating bio-ceramic implants commercially. However, there are disadvantages such as microcrack, low bonding strength of coating layer and implant surface, phase change by exposure at high temperature, uneven coating density and irregular microstructure control, which result in graft failure. have.

Recently, surface modification of commercially available implants is treated with alumina powder or HA powder on the surface to give macro roughness and micro roughness by anodization to facilitate the reaction with bone. The most prominent problem is the need for shortening the bonding time with the bone and the strength of adhesion at the interface.

To this end, in the prior art, HA is sprayed on the surface by thermal spraying to perform coating treatment, but it is a cause of implant failure due to peeling phenomenon at the interface.

In recent years, studies on surface treatment by anodization have been conducted. In particular, research has been carried out to the step of coating HA on the surface of nanotubes by electrochemical method. HA coating method using this electrochemical electrodeposition method is carried out by many researchers, and because of the low running temperature it is possible to avoid unwanted phase change of the material. However, although the complex shape and thickness can be easily adjusted and the manufacturing cost is lower than other processes, these studies are an electrochemical method of coating artificial HA, which leaves harmful residues in the nanotubes. Has

Therefore, in order to improve this, according to the type of cells on the surface of the micro-sized micropore and nano-sized nanotubes by the surface treatment using anodizing method, and then coated with the bioactive material HA by EB-PVD method It is an object of the present invention to provide a coating method that can minimize the phenomenon of peeling off the surface.

As such, the present invention increases the biocompatibility through the surface modification for dental implants by forming micropores and nanotubes in two steps on the implant surface and coating them with EB-PVD method using extracted teeth or artificially manufactured HA. It has a very useful effect of shortening the procedure period and extending the use period as much as possible.

Hereinafter, the present invention will be described in detail.

The hydroxyapatite coating method for bioactivation after surface modification of the dental implant according to the present invention comprises the steps of: forming micropores on the surface of the implant; Forming nanotubes on the surface of the implant in which the micropores are formed; Preparing a target to be coated on the surface of the nanotube using tooth powder; Coating the surface of the implant by the EB-PVD method using the prepared tooth powder or artificially manufactured HA.

Hereinafter, described in more detail through an embodiment of the present invention.

EXAMPLE

(1) Alloy production

Four kinds of alloys are manufactured by using a vacuum arc-melting furnace, but in the present invention, the weight ratio of Ta, Zr, and Nb is different with respect to Ti (balance).

(a) 67wt% Ti-30wt% Ta-3wt% Zr

(b) 65wt% Ti-30wt% Ta-15wt% Zr

(c) 67wt% Ti-30wt% Nb-3wt% Zr

(d) 65wt% Ti-30wt% Nb-15wt% Zr

(2) two-step anodization

① Step 1: Micropore Formation

Electrolyte: 1M H ₃ PO ₄

DC voltage, current: 180 V, 30 mA (constant current)

Time: 20min, 150min

Electrode: Anode (Sample), Cathode (Platinum)

② Step 2: Nanotube Formation

Electrolyte: 1M H ₃ PO ₄ + 0.8% NaF

DC voltage: 5 to 10 V 10 mA (constant current) Rise to 20 V ⇒ 20 V (hold constant voltage)

Time: 120min

Electrode: working electrode (sample), auxiliary electrode (platinum), reference electrode (saturated calomel)

(3) HA powder tooth powder target production

Firing: 1350 ℃ / 3hr

Properties: Porosity 24.5% (196.6 1500 ℃)

Specific gravity: 2.35 (2.45 ℃)

Plastic shrinkage: -5%

Circumference: hand machined (2hr) 50mm

Processing is diamond paste

Washing: ultrasonic 30min

Dry 26hrs at 110 ℃

(4) Conditions for Implant Surface Coating of HA by EB-PVD Method

1 is a surface photograph of the development alloy, (a) 67 wt% Ti-30 wt% Ta-3 wt% Zr, (b) 65 wt% Ti-30 wt% Ta-15 wt% Zr, (c) 67 wt% Ti-30 wt The surface photograph of% Nb-3wt% Zr, (d) 65wt% Ti-30wt% Nb-15wt% Zr alloy. When Zr content is increased, it changes to need-like needle structure.

2 is a microporous photo on the surface of the development alloy, (a) 67 wt% Ti-30 wt% Ta-3 wt% Zr, (b) 65 wt% Ti-30 wt% Ta-15 wt% Zr, (c) 67 wt% Surface photograph of% Ti-30wt% Nb-3wt% Zr, (d) 65wt% Ti-30wt% Nb-15wt% Zr alloy, and micropores are well formed on the surface due to high voltage applied to titanium oxide film formed on the surface It became.

3 is a photo of nanotubes formed on the surface of the development alloy, (a) 67 wt% Ti-30 wt% Ta-3 wt% Zr, (b) 65 wt% Ti-30 wt% Ta-15 wt% Zr, (c) 67 wt% Surface image of% Ti-30wt% Nb-3wt% Zr, (d) 65wt% Ti-30wt% Nb-15wt% Zr alloy, in which the formation of nanotubes was formed with a size of 100 nm in diameter, (a) Nanotubes appearing in Ti alloys are formed along the phases α and β. The thickness is formed to about 500nm.

Figure 4 is a micropore and nanotube formation photograph formed in two steps on the surface of the development alloy, 65wt% Ti-30wt% Ta-15wt% Zr alloy (a) is 500 times, (b) is 1,000 times, (c) was observed at 30,000 times and (d) 50,000 times, and micropores were formed well at the low magnification of (a), and inside the nanotubes as shown in (d), the surface needed for excellent bioactivation was formed. Can be provided.

FIG. 5 is a tooth powder target manufacturing photograph, which is a target prepared by using a tooth powder to be coated on a nanotube surface, and used as a target for EB-PVD without a defect and having a very good target.

6 is a tooth powder coating surface of a two-step surface, (a) 67 wt% Ti-30 wt% Ta-3 wt% Zr, (b) 65 wt% Ti-30 wt% Ta-15 wt% Zr, (c) 67 wt% Surface image of Ti-30wt% Nb-3wt% Zr, (d) 65wt% Ti-30wt% Nb-15wt% Zr alloy, micropoa-nanotube as a result of coating by EB-PVD method using tooth powder target HA (hydroxyapatite) is well coated on the surface to facilitate fusion with bone.

As described above, the present invention has been described by means of a limited embodiment, but the present invention is not limited thereto and is intended by those skilled in the art to which the present invention pertains to the technical spirit of the present invention and claims to be described below. Various modifications and variations are possible within the scope of equivalents.

Figure 1-Surface photograph of development alloy

Figure 2-Photo micropore formation on the surface of the development alloy

Figure 3-Photo nanotube formation on the surface of the development alloy

Fig. 4-Micropore and nanotube formation photograph formed in two steps on the surface of the development alloy

Figure 5-Tooth powder target production photo

Figure 6-Tooth powder coating surface of 2 step surface

Claims (2)

In the surface modification method of the dental implant to form a nanotube on the surface of the implant, the coating on the nanotube surface using a tooth powder or artificially manufactured HA,  Forming a micropore before forming the nanotubes on the implant surface, forming the nanotubes on the implant surface on which the micropores are formed, and coating the implant surface with the tooth powder or artificially manufactured HA by EB-PVD; Hydroxyapatite coating method for bioactivation after surface modification of the dental implant, characterized in that consisting of. The method of claim 1, The implant is prepared using a vacuum arc-melting furnace, 67wt% Ti-30wt% Ta-3wt% Zr, 65wt% Ti-30wt% Ta-15wt% Zr, 67wt% Ti-30wt% Nb-3wt% Zr , Hydroxyapatite coating method for bioactivation after surface modification of the dental implant, characterized in that consisting of any one of 65wt% Ti-30wt% Nb-15wt% Zr alloy.

Images