KR20170115763A - Implant comprising Bioactive color glass and preparing method thereof - Google Patents

Abstract

The implant prepared by the manufacturing method of the present invention can improve the biocompatibility, corrosion resistance, mechanical properties, low bacterial deposition rate, etc. of zirconia by introducing bioactive glass coating, roughness formation, bioceramic coating and the like into zirconia It is effective.

Description

TECHNICAL FIELD The present invention relates to a zirconia implant including a bioactive glass and a method of manufacturing the same.

The present invention relates to a zirconia implant including a bioactive glass and a method for producing the same.

Implant refers to transplantation. In order to compensate for the deficiency of a living tissue, a material used for implanting an artificial material or a natural material into a defect site to perform reconstruction and function of the shape, Valves, artificial joints, artificial teeth, guide lenses, and the like.

An artificial tooth is also called a third tooth. The artificial tooth is a biocompatible implant to the jaw bone which is increased in volume so that it can be sufficiently wrapped through additional operations such as bone grafting, osteogenesis, It is a material used for dental treatment that restores the function of natural teeth by planting the body.

Therefore, the implant should have excellent characteristics such as osseointegration, which is a morphological, physiological, and direct combination with the jaw bone in which the normal function is maintained. Several types of implants have been developed, and many methods have been proposed to reduce the failure rate of dental implants applied to the living body and to improve the fixation strength with the bones. For example, a method of mechanically fixing the bone to the bone by designing the implant in a spiral shape is generally used. However, since it is still not at a level comparable to that of a natural tooth, much research is underway to improve the bonding.

Therefore, various methods have been proposed to improve the fixation and bonding strength between implants and bones, including physical and chemical methods.

Physical methods include, for example, grinding, spraying (sand blasting, etc.), acid etching, etc., as a method of forming roughness on the surface of an implant. Specifically, sandblasting is a method of inducing strengthening by phase change using alumina having a small particle size, and acid etching is a method mainly used with sandblasting since the surface treatment effect is not shown well.

Implants with increased surface roughness in this way can achieve better mechanical constraint and strength by providing greater contact and fixation areas between the implant and bone tissue.

The chemical method is to change the chemical characteristics of the implant surface. For example, there is a method of coating calcium phosphate, which is an inorganic component similar to bone, on the surface of an implant to stimulate regeneration of bone tissue. This treatment method can induce biosynthesis and improve the biocompatibility as well as the fixation and bonding force with the physiological bones.

In addition to the inherent characteristics of such physical, chemical and biocompatible properties of implants, aesthetic properties are also required in recent years. For example, in the case of the anterior teeth (front teeth), the characteristic of the teeth is also important, but it plays a very important role in the social aspect because it is a directly exposed tooth. In addition, the aesthetic characteristics of the implant are also very important factors because the probability of being greatly damaged by the physical impact and replaced with the implant is also very high. In this way, implant materials that are the same as the color and material of natural teeth are required, and aesthetic characteristics are also considered to be very important.

For example, Korean Patent Laid-Open Publication No. 2011-0041682 discloses a method of manufacturing a zirconia tooth in which an entire artificial tooth is molded into zirconia colored with a coloring liquid similar to natural color.

On the other hand, zirconia is excellent in strength and biocompatibility and does not cause any inflammation or allergy when used in the human body because there is no corrosion. It is also widely used as an implant material to replace metals based on its excellent mechanical properties. Recently, it has been applied not only to the core of the crown bridge but also to the implant area. High biocompatibility, excellent mechanical properties and low bacterial deposition rate are highly evaluated as dental materials.

However, unlike ordinary metals, zirconia has a difficulty in forming surface roughness by spraying or acid etching. Therefore, zirconia has a disadvantage in that the bonding strength is lowered even when the surface treatment is carried out using acid etching or spraying. Delamination of the surface coating layer from zirconia occurs basically when the thermal expansion coefficients of zirconia and the coating layer are not similar to each other or when the cooling rate is too fast.

Korean Patent No. 10-1430748 discloses a biologically active hue glass comprising silicon oxide, aluminum oxide, sodium oxide, magnesium oxide, barium oxide, calcium oxide, titanium oxide and niobium oxide, BACKGROUND ART [0002] It is known for a prosthesis for a tooth including a glass.

However, it is known that when the bioactive active glass is coated on zirconia, the surface roughness is slightly formed and the fixing force and bonding force with bone tissue are improved. However, the biocompatibility is still unsatisfactory.

Despite the many advantages of zirconia, there are still many limitations to the processing process for improving the bonding strength and fixing force. In order to form the required surface roughness, a strong physical and chemical shock may be applied to the zirconia in the process. Such impact may cause problems between zirconia and the coating layer, such as low bonding force between zirconia and the coating layer, defects at the interface between zirconia and the coating layer and mismatch of the thermal expansion coefficient of the zirconia-coating layer, and mechanical properties of zirconia itself such as warpage of zirconia Can be greatly reduced. In some cases, biocompatibility may be lowered.

Therefore, the above problems can be minimized even if the roughness is formed in the zirconia. Various studies for development of the implant that can be compared with the corresponding biotissue should be further intensified.

Korean Patent No. 10-1430748 Korea Patent Publication No. 2011-0041682

It is an object of the present invention to provide an implant using zirconia which can improve excellent characteristics such as biocompatibility, corrosion resistance, excellent mechanical properties and low bacterial deposition rate of zirconia itself and a method for producing the same.

The present invention provides a method for manufacturing an implant comprising: a) a bioactive glass coating on a surface of a material comprising zirconia; and b) forming a roughness on the bioactive glass coated in step a).

In one embodiment of the present invention, the method of forming the roughness in the step b) is not limited within the scope of achieving the object of the present invention, but any one or more methods selected from the acid etching method and the sand blasting method .

In one embodiment of the present invention, the method may further include coating a bio-ceramic on the rough-formed bioactive glass after the step b).

The present invention also provides an implant including a material containing zirconia, a bioactive glass coating layer coated on the surface of the material, and a bio-ceramic coating layer coated on the bioactive glass coating layer.

In one embodiment of the present invention, the bioactive glass is not limited within the scope of achieving the object of the present invention, but may be selected from silicon oxide, aluminum oxide, sodium oxide, magnesium oxide, barium oxide, calcium oxide, Niobium oxide, and the like.

In one embodiment of the invention, the bio-ceramic is, but not limited within the scope that can achieve the object of the present invention, hydroxide apatite in _{(HA, Ca 10 (PO 4} ) 6 (OH) 2), phosphorus pentoxide (P ₂ O _5), the third phosphate _{(TCP, Ca 3 (PO 4} ) 2), octa-calcium phosphate _{(OCP, Ca 8 H 2 (} PO 4) 6 · 5H2O) and octa-calcium phosphate (4CP, Ca ₄ O ( PO ₄ ) ₂ ), and the like.

The implant of the present invention is made of zirconia and can prevent the adverse effect that the cytotoxicity is increased by the bioactive glass coating treatment, and thus the biocompatibility, corrosion resistance, excellent mechanical properties, low bacterial deposition rate There is an effect that the characteristics of the semiconductor device can be improved.

Therefore, it has excellent biocompatibility, can realize the same hue as the corresponding biotissue, has an effect of enhancing the bonding force between zirconia and the coating layer and maximizing the durability, and is applicable to various medical fields and has a wide range of applications .

Figs. 1 to 4 show the results of observing the degree of cell adhesion according to Comparative Example 1, Comparative Example 2, Example 1 and Example 2 using a scanning electron microscope (after 24 hours, 100 magnifications )
Figs. 5 to 7 show the results of the fracture resistance measurement in the case of Comparative Example 1, Comparative Example 2 and Example 1, respectively.
Fig. 8 shows the results of measuring the thermal expansion coefficient of the bioactive glass according to Example 1. Fig.

Hereinafter, a zirconia implant including a bioactive glass of the present invention and a method of manufacturing the same will be described in detail with reference to the accompanying drawings.

The drawings described in the present invention are provided by way of example so that a person skilled in the art can sufficiently convey the idea of the present invention. Therefore, the present invention is not limited to the illustrated drawings, but may be embodied in other forms, and the drawings may be exaggerated in order to clarify the spirit of the present invention.

In addition, unless otherwise defined, technical terms and scientific terms used in the present invention have the same meanings as those of ordinary skill in the art to which the present invention belongs. In the following description and the accompanying drawings, Description of known functions and configurations that may unnecessarily obscure the subject matter will be omitted.

Also, units of% used unclearly in the present invention means weight percent.

The term " implant " as used in the present invention means an artificial material implanted into a human body and refers to a wide range of implants as artificial materials including artificial valves, artificial joints, artificial teeth, guide lenses and the like .

The present invention provides a method for manufacturing an implant comprising: a) a bioactive glass coating on a surface of a material comprising zirconia; and b) forming a roughness on the bioactive glass coated in step a).

The present invention also provides an implant including a material containing zirconia, a bioactive glass coating layer coated on the surface of the material, and a bio-ceramic coating layer coated on the bioactive glass coating layer.

In one example of the present invention, the material may mean a material containing zirconia (zirconium oxide). As a specific example, the material may refer to a zirconia substrate. The specific characteristics such as the thickness, weight, and shape of the material can be appropriately selected by those skilled in the art, as various known literatures can be referred to.

In one embodiment of the present invention, the bioactive glass include, but are not limited within the scope that can achieve the object of the present invention, a silicon oxide (SiO _2), aluminum oxide (Al ₂ O _3), sodium oxide (Na ₂ O). And may include any one or two or more selected from magnesium oxide (MgO), barium oxide (BaO), calcium oxide (CaO), titanium oxide (TiO ₂ ), and niobium oxide (Nb ₂ O ₅ ).

In one embodiment of the invention, the bio-ceramic is, but not limited within the scope that can achieve the object of the present invention, hydroxide apatite in _{(HA, Ca 10 (PO 4} ) 6 (OH) 2), phosphorus pentoxide (P ₂ O _5), the third phosphate _{(TCP, Ca 3 (PO 4} ) 2), octa-calcium phosphate _{(OCP, Ca 8 H 2 (} PO 4) 6 · 5H2O) and octa-calcium phosphate (4CP, Ca ₄ O ( PO ₄ ) ₂ ), and the like.

In one embodiment of the present invention, the bioactive glass in step a) is not limited within the scope of achieving the object of the present invention, but it may be prepared by pulverizing each component into powder form, ≪ / RTI > At this time, it is possible to mechanically crush the granules while rotating them at a constant speed by using a ball milling machine to have granules of uniform size. The ball used for ball milling may be a ball made of ceramics such as zirconia or aluminum oxide, and the balls may be the same size or different. The bioactive glass may be wet-mixed and pulverized together with a solvent such as water or an alcohol. The pulverized powder slurry can be dried, for example, at 60 to 120 DEG C for 0.5 to 12 hours. Thereafter, the heat treatment can be performed at a temperature of 1200 캜 or higher. The melt obtained through the heat treatment process may be fritted and poured into distilled water so as to be gales, so that quenching may be performed.

In one example of the present invention, the method may further include a first sintering step of sintering the material including zirconia before the step a), although the present invention is not limited within the scope of achieving the object of the present invention. When the pre-sintering is further performed before coating the bioactive glass with a material including zirconia, the first sintering step is performed such that a) the strength of the implant of the present invention, which is produced by sequentially performing steps b) and c) The durability can be further improved. In detail, the durability between the material and the bio-active glass coating layer and between the bio-active glass coating layer and the bio-ceramic coating layer can be improved to have a better bonding force between the interface and ultimately to produce an implant having excellent durability It is effective. For example, the first sintering temperature is not limited within a range that can achieve the object of the present invention, but is preferably 800 to 1,700 ° C, and preferably 1,000 to 1,700 ° C in terms of maximizing the effect Do.

In one embodiment of the present invention, the step a) is a step of coating a bioactive glass on a zirconia material. For example, the bioactive glass may be mixed with a solvent such as water and coated on the surface of zirconia, and the mixing ratio thereof may be 1 to 500 parts by weight based on 1 part by weight of the bioactive glass. However, it is needless to say that various coating methods can be performed.

As described above, by coating the bioactive glass on the surface of zirconia, the surface roughness can be improved, and the fixing force and the binding force with the bone tissues can be improved. In addition, biocompatibility such as reduction in cytotoxicity can be significantly improved by performing steps b) and c) to be carried out subsequently.

In one embodiment of the present invention, the thickness of the bioactive glass coating layer of zirconia produced in the step a) is not limited within a range that can achieve the object of the present invention, but may be 5 to 120 탆.

In one embodiment of the present invention, the zirconia coated on the surface of the bioactive glass after the step a) and before the step b) is not limited within a range that can achieve the object of the present invention, The method comprising the steps of: When the second sintering is further performed, the durability such as strength can be further improved in the implant of the present invention in which a) step b) and step c) are sequentially performed. In detail, the durability between the material and the bioactive glass coating layer and between the bioactive glass coating layer and the bio-ceramic coating layer is improved, so that it is possible to have a better bonding force between the interface and ultimately to manufacture an implant having excellent durability . As a specific example, the second sintering temperature is not limited within a range that can achieve the object of the present invention, but it is preferable that the second sintering temperature is 700 to 1,700 ° C in terms of maximizing the effect.

In one embodiment of the present invention, the step b) is not limited to the extent that the object of the present invention can be achieved, but includes the step of forming a roughness by any one or more methods selected from acid etching, sandblasting, .

In one embodiment of the present invention, the acid etch is not limited to the extent that the object of the present invention can be achieved, but the material may be immersed in an acid or acid aqueous solution containing hydrofluoric acid (HF) To form a roughness. By performing this acid etching, a fine irregular structure due to corrosion can be formed on the surface of zirconia. As a specific example, when a hydrofluoric acid aqueous solution is used, it may be an aqueous solution containing 10 to 20% of hydrofluoric acid. As a specific example, the immersion time is not limited until the required roughness can be formed, but it can be 10 to 60 minutes. As a specific example, the immersion temperature is not limited as long as the required roughness can be formed, but it may be 30 to 90 캜.

In one embodiment of the present invention, the sand blasting method is well known in the art to form roughness on the surface of a material by spraying particles such as sand or alumina onto the material, so that these methods may be used without limitation. Specifically, when sand having a small particle diameter is used, strengthening by phase change can be induced. However, when sand having a large particle diameter is used, scratches are increased and the strength may be excessively lowered. Thus, as a specific example, the particle size of the particles is not limited within a range that can achieve the object of the present invention, but it may be 75 to 250 탆. As a specific example, the injection pressure is not limited to the extent that the object of the present invention can be achieved, but it may be 1 to 6 MPa. As a specific example, the injection time is not limited within a range that can achieve the object of the present invention, but it may be 15 to 45 seconds.

The surface roughness of the implant of the present invention is not limited within a range that can achieve the object of the present invention, but may be 0.5 to 5.0 탆, preferably 1.0 to 2.0 탆. Specifically, the implant may include zirconia containing a bioactive glass coating layer having roughness formed in step b), or zirconia having a bioceramics layer formed in step c). There is no problem that the strength is excessively lowered even though the surface roughness in the above range is formed. In addition, after the roughness is formed, sintering, bioceramic coating treatment, and the like are combined, the surface roughness within the above range can be maintained, and the bioadhesiveness of the finally prepared implant is not deteriorated.

In one embodiment of the present invention, the method may further include the step of coating the bio-ceramic on the bioactive glass of the zirconia having the roughness formed in step c) a) after the step b). By combining the bio-ceramic coating of step c) with steps a) and b), mechanical properties such as fracture resistance and the like can be improved, although the properties such as biocompatibility and low bacterial deposition rate are improved. Specifically, even if the mechanical and chemical forces applied to the zirconia act strongly in the step b), the mechanical properties such as the structural stability and strength of the zirconia may be deteriorated. However, the step c) It can be silent. In addition, biocompatibility deterioration due to cytotoxicity, which is increased by the bioactive glass coating in step a), can be prevented.

In addition, even though the bio-ceramic coating layer is formed on the surface layer formed with the minute structural irregularities introduced in the step b), the fine structural irregularities (shapes such as points, dislocations, cracks, folds and wrinkles) It has the effect of being maintained without development. Therefore, the biocompatibility properties are improved and the fixation force with the bone tissue and the binding force property are also improved.

In one embodiment of the present invention, the thickness of the bio-ceramic coating layer of zirconia produced in the step c) is not limited within a range that can achieve the object of the present invention, but may be 0.05 to 120 탆. If it is satisfied, the surface roughness is reduced due to the formation of a thick coating layer on the surface of the bioactive glass having roughness formed on the surface in the step b), and the thickness of the coating layer is too thin to exhibit the characteristics of the coating layer, Can be minimized. However, this is a preferable example, but the present invention is not limited thereto.

In one embodiment of the present invention, the step c) is not limited to the extent that the object of the present invention can be achieved, but it is possible to use a dip coating, an aerosol deposition (AD), a spin coating the surface of the zirconia is removed by coating, doctor blade, dry dipping, hydrothermal reaction, sol-gel method, plasma spraying or ion beam deposition or the like. And a bio-ceramic coating layer may be formed. Preferably, dip coating (immersion method) is preferable. However, the present invention is not limited thereto, and a coating layer can be formed by various known coating methods. Further, after the bio-ceramic coating layer is formed, a third sintering step may be further performed at 500 to 1,200 ° C, and if it is satisfied, the structural stability and the mechanical strength can be further improved.

In one example of the present invention, by controlling the composition and composition ratio of the components contained in the bioactive glass, it is possible to control the mechanical properties, bioactivity, glass transition temperature, and thermal expansion coefficient for coating, .

As described above, the bioactive glass is composed of silicon oxide (SiO ₂ ), aluminum oxide (Al ₂ O ₃ ), sodium oxide (Na ₂ O). Or one or more selected from magnesium oxide (MgO), barium oxide (BaO), calcium oxide (CaO), titanium oxide (TiO ₂ ) and niobium oxide (Nb ₂ O ₅ ) (SiO ₂ ), aluminum oxide (Al ₂ O ₃ ), and sodium oxide (Na ₂ O). When an implant is prepared through steps a), b) and c) using a bioactive glass containing silicon oxide (SiO ₂ ), aluminum oxide (Al ₂ O ₃ ) and sodium oxide (Na ₂ O) , Aesthetic properties, and chemical resistance properties as well as mechanical properties such as fracture resistance, strength, and abrasion resistance can be further improved. More preferably, sintering, acid etching, sand blasting, bioceramic coating, etc., are performed when 50 to 80% by weight of silicon oxide, 5 to 40% by weight of aluminum oxide and 2 to 30% The durability such as transparency and gloss, the aesthetic properties such as gloss, the hardness, the chemical durability, the stability and the bonding force can be further improved. Further, the density of the glass is further reduced, the characteristics such as the glass transition temperature, the softening temperature and the viscosity are improved, so that the bioactive glass coating layer can be formed more firmly on the zirconia surface and the coefficient of thermal expansion can do.

In detail, the bioactive glass is not limited within the scope of achieving the object of the present invention, but it is preferable that 60 to 75% by weight of silicon oxide, 8 to 18% by weight of aluminum oxide, 4 to 10% by weight of sodium oxide, , Magnesium oxide 0.1 to 5 wt%, barium oxide 0.1 to 5 wt%, calcium oxide 0.1 to 5 wt%, titanium oxide 0.1 to 5 wt%, and niobium oxide 0.1 to 5 wt%. Although the implant is performed by sintering, acid etching, sandblasting, bioceramic coating, and the like, if the weight range is satisfied, the finally prepared implant can exhibit a color very similar to the corresponding biotissue, And the bonding strength between the coating layer and the coating layer is also maximized, so that the durability can be improved. Further, the mechanical properties, water resistance and crystallization of the glass can be further improved, and the phase change of zirconia can be suppressed during the manufacturing process. Further, the thermal expansion coefficient for bioactivity, glass transition temperature, coating and the like is close to that of zirconia.

In one example of the present invention, the bioactive glass is not limited within the scope of achieving the object of the present invention, but any one or more selected from iron oxide, phosphorus pentoxide, boron oxide, potassium oxide and strontium oxide, As shown in FIG. If it is satisfied, the permeability can be further improved, the glass crystallization can be improved, the mechanical strength can be further improved, and the thermal expansion coefficient of zirconia can be made closer to that. In addition, the solubility of the bioactive glass is increased in the manufacturing process, the softening temperature is decreased, and the melting property is improved, so that the biocompatibility can be further improved. In addition, since the bioactive glass can have an appropriate brightness in the manufacturing process, it is possible to prevent the fracture of the glass and to finally manufacture a stable implant. In addition, the color of the implant can be freely controlled as shown in FIG. 8 by controlling the addition of components such as iron oxide and the ratio of the added components.

In one embodiment of the present invention, when the biologically active glass further comprises any one or two or more components selected from iron oxide, phosphorus pentoxide, boron oxide, potassium oxide, strontium oxide, etc., The amount of the above-mentioned components to be added to 100 parts by weight of the basic bioactive glass may be 0.1 to 5 parts by weight, respectively. When this is satisfied, the effect expressed by binding of these components can be further improved.

In one example of the present invention, the coefficient of thermal expansion of the bioactive glass is not limited within a range that can achieve the object of the present invention, but a coefficient of 6.5 to 12.5 × 10 ^-6 is more resistant to refractive-induced damage And it is desirable in view of being able to provide a strong adhesion to the zirconia. However, this is a preferable example, but the present invention is not limited thereto.

As described above, the bioceramics of the present invention are not limited within the scope of achieving the object of the present invention, but may be selected from the group consisting of apatite hydroxide (HA, Ca ₁₀ (PO ₄ ) ₆ (OH) ₂ ) P ₂ O ₅₎ 3 phosphate _{(TCP, Ca 3 (PO 4} ) 2), octa-calcium phosphate _{(OCP, Ca 8 H 2 (} PO 4) 6 · 5H2O) and octa-calcium phosphate (4CP, Ca ₄ O ( PO ₄ ) ₂ ), and the like.

EXAMPLES Hereinafter, the present invention will be described in detail with reference to Examples. However, the present invention is described in more detail with reference to the following Examples. However, the scope of the present invention is not limited by the following Examples.

[Comparative Example 1]

Zirconia (ZrO ₂ ) base material was sintered at 1,040 ° C in a sintering furnace. The average surface roughness of sintered zirconia was 0.025 ㎛, the hardness was 12.34 GPa, and the flexural strength was 425 MPa. The cytotoxic test results are also shown in Table 1 below.

[Comparative Example 2]

The surface of the sintered zirconia prepared in Comparative Example 1 was coated with a bioactive glass by the following method.

Specifically, 70% by weight of SiO ₂ powder, 20% by weight of Al ₂ O ₃ powder and 15% by weight of Na ₂ O powder were ball milled at 500 rpm for 50 minutes, mixed and crushed, and then melted at 1,450 ° C. . After the melting, water was quenched into cooling water and subjected to glass crystallization (frit). The crystallized glass was thoroughly dried and ball milled to form particles having an average particle diameter of about 1.5 탆 at 500 rpm for 50 minutes to prepare a SiO ₂ -Al ₂ O ₃ -Na ₂ O bioactive glass.

Next, the sintered zirconia prepared in Example 1 was immersed in a mixed solution obtained by mixing 100 parts by weight of distilled water with 1 part by weight of the bioactive glass and the bioactive glass, and then sintered at 1,450 ° C in a sintering furnace to form a bioactive glass coating layer Zirconia was formed.

The average surface roughness of the zirconia was 0.55 탆, the hardness was 6.23 GPa, and the flexural strength was 850 MPa. The cytotoxic test results are also shown in Table 1 below.

Surface roughness was formed on the bioactive glass coating layer formed on the surface of zirconia prepared in Comparative Example 2 by sandblasting.

Specifically, by spraying for 30 seconds, the alumina particles with a mean particle size of 90 ㎛ the pressure of 3.5 MPa to form a roughness on the zirconia (ZrO ₂₎ substrate produced in Comparative Example 2.

The average surface roughness of the bioactive glass coating layer was 1.25 탆, the hardness was 10.60 GPa, and the flexural strength was 650 MPa. The cytotoxic test results are also shown in Table 1 below.

Surface roughness was formed on the bioactive glass coating layer formed on the surface of zirconia prepared in Comparative Example 2 by acid etching.

Specifically, zirconia having a bioactive glass coating layer formed on the surface prepared in Comparative Example 2 was immersed in a 15% by weight hydrofluoric acid (HF) aqueous solution at 55 캜 for 30 minutes to etch the surface.

The average surface roughness of the bioactive glass coating layer formed on the zirconia surface was 1.35 탆, the hardness was 12.00 GPa, and the flexural strength was 600 MPa. The cytotoxic test results are also shown in Table 1 below.

(HA) coating layer was formed on the surface of the bioactive glass coating layer formed on the surface of the zirconia by the sand blasting method prepared in Example 1 using a dipping method / RTI >

Specifically, the zirconia was immersed in a mixture of hydroxyapatite (HA) powder and 100 parts by weight of distilled water per 1 part by weight of the powder to form a coating layer on the surface of the bioactive glass coating layer formed on the zirconia surface, Lt; / RTI >

Example 3 was carried out in the same manner as in Example 3, except that zirconia finally prepared by the acid etching method in Example 2 was used instead of zirconia finally prepared by the sandblasting method in Example 1.

[Comparative Example 3]

Example 3 was carried out in the same manner as in Example 3, except that zirconia finally prepared by the acid etching method in Example 2 was used instead of zirconia finally prepared by the sandblasting method in Example 1.

As in Comparative Example 2 and Examples 1 to 4, when the zirconia is further subjected to treatment such as bioactive glass coating or surface roughness formation, it is confirmed that the bending strength is increased and the fracture resistance is improved.

On the other hand, in the cytotoxicity test, the effect of Comparative Example 2 in which the bioactive glass coating was applied was decreased rather than that of Comparative Example 1 in which no treatment was performed. However, in the case of Example 3 and Example 4 in which bioceramics such as HA were further coated, the biocompatibility was remarkably improved again.

FIGS. 5 to 7 are photographs respectively taken after forming indentation on the surface in order to measure the fracture toughness in the case of Comparative Example 1, Comparative Example 2, Example 1 and Example 2 in order. In the case of Comparative Example 1 in which zirconia was used as it is, cracks were generated on the surface, but in Examples 1 and 2 in which sandblasting was further performed, no cracks were found on the surface.

In particular, in the case of Examples 3 and 4 in which a hydroxyapatite (HA) coating layer was further formed, it was confirmed that the two-component coating layer was further formed to maintain the high fracture resistance as well as the structural stability even though it had a complicated structure.

As a result of cell attachment test, the cell adhesion of Comparative Example 2 in which bioactive glass coating was performed showed lower cell adhesion than that of Comparative Example 1 in which no treatment was performed. In contrast, in Examples 3 and 4, in which surface roughness forming processes such as sandblasting or acid etching treatment and bioceramics coating process were sequentially combined, remarkably high cell attachment results were obtained.

This tendency is also shown in the cytotoxicity test of Table 1 below. In the cytotoxicity test, the case of Comparative Example 2 in which bioactive glass coating was performed was worse than that of Comparative Example 1 in which no treatment was performed. In contrast, in Examples 3 and 4, in which the surface roughness forming process such as sandblasting or acid etching process and the bioceramics coating process were sequentially combined, it was found to be remarkably high.

1 day 3 days Comparative Example 1 0.42 0.72 Comparative Example 2 0.38 0.64 Comparative Example 3 0.48 0.78 Example 1 0.44 0.79 Example 2 0.45 0.81 Example 3 0.52 0.92 Example 4 0.54 0.94

These results show no significant difference in biocompatibility between the zirconia implant and the bioactive glass coating alone, and the biocompatibility of the zirconia implant was not significantly improved even when only hydroxyapatite (HA) coating was applied .

On the other hand, when the roughness formation treatment such as sand blasting and acid etching and the bioceramic coating treatment proceed sequentially, it can be seen that the biocompatibility is remarkably improved by the cell adhesion test and the cytotoxicity test, and the zirconia implant It can be seen that the production is possible.

5 to 7 showing the result of the fracture resistance test for evaluating the structural stability of the surface after indentation on the surface, the mechanical strength is remarkably improved. That is, although these structures are maintained, adhesion and bond strength between the zirconia base material and the coating layer or between the coating layer and the coating layer are maintained, and thus the composite structure coated with the multilayer structure has an excellent structure stability.

In addition, fine surface irregularities such as points, dislocations, grain boundaries, cracks, folds, wrinkles and the like are introduced by the formation of the surface roughness, and even though the bioceramic coating layer is applied thereto, the fine structural irregularities are maintained without being clogged by the coating layer . That is, even though the structural unevenness is covered with the bioceramics coating layer, the surface roughness is maintained on the bioceramics coating layer, and the fixing force and the binding force for the bone tissue are finally improved.

As can be seen from FIG. 8, the thermal expansion coefficient is about 10.12 × 10 ^-6 / ° C., and the thermal expansion coefficient of zirconia is very close to 10.65 × 10 ^-6 / ° C.

Claims (10)

A method of coating a bioactive glass comprising at least one selected from the group consisting of silicon oxide, aluminum oxide, sodium oxide, magnesium oxide, barium oxide, calcium oxide, titanium oxide and niobium oxide on a surface of a material containing zirconia Step and
b) forming a roughness on the bioactive glass coated in step a). The method according to claim 1,
(HA, Ca ₁₀ (PO ₄ ) ₆ (OH) ₂ ), phosphorus pentoxide (P ₂ O ₅ ), and calcium tertiary phosphate (TCP) are formed on the roughly formed bioactive glass after the step b) _{, Ca 3 (PO 4) 2} ), octa-calcium phosphate _{(OCP, Ca 8 H 2 (} PO 4) 6 · 5H2O) and octa-calcium phosphate _{(4CP, Ca 4 O (PO} 4) 2) any one selected from or The method of claim 1, further comprising coating a bioceramic material including at least two of the bioceramics. 3. The method of claim 2,
Prior to step a), a first sintering of the material,
Further comprising the step of second sintering the bioactive glass coated zirconia after the step a) and before the step b). The method of claim 3,
Wherein the first sintering is performed at 1,000 to 1,700 ° C, and the second sintering is performed at 700 to 1,700 ° C. 5. The method of claim 4,
Wherein the method for forming the roughness in the step b) is at least one selected from an acid etching method and a sand blasting method. 6. The method of claim 5,
A surface treatment method for an implant having a surface roughness of 0.5 to 5.0 mu m. 7. The compound according to any one of claims 1 to 6,
Wherein the bioactive glass comprises silicon oxide, aluminum oxide and sodium oxide. 8. The method of claim 7,
Wherein the bioactive glass comprises 50 to 80% by weight of silicon oxide, 5 to 40% by weight of aluminum oxide, and 2 to 30% by weight of sodium oxide. 7. The compound according to any one of claims 1 to 6,
Wherein the bioactive glass comprises 60 to 75% by weight of silicon oxide, 8 to 18% by weight of aluminum oxide, 4 to 10% by weight of sodium oxide, 0.1 to 5% by weight of magnesium oxide, 0.1 to 5% by weight of barium oxide, 0.1 to 5% by weight of titanium oxide, and 0.1 to 5% by weight of niobium oxide. Materials including zirconia,
A bioactive glass coating layer coated on the material surface and
And a bio-ceramic coating layer coated on the bioactive glass coating layer,
Wherein the bioactive glass coating layer comprises silicon oxide, aluminum oxide and sodium oxide,
The body ceramic coating layer hydroxide apatite _{(HA, Ca 10 (PO 4} ) 6 (OH) 2), phosphorous pentoxide (P ₂ O _5), the third phosphate _{(TCP, Ca 3 (PO 4} ) 2), octanoic acid (PO), Ca ₈ H ₂ (PO ₄ ) ₆揃 5H ₂ O) and calcium octapphosphate ( ₄ CP, Ca ₄ O (PO ₄ ) ₂ ) and has a surface roughness of 0.5 to 5.0 ㎛.

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