KR20110054556A - A surface treating method of use rf-sputtering process for dental implant fixture - Google Patents

Abstract

PURPOSE: A surface processing method of a dental implant fixture using an RF-sputtering process is provided to selectively perform an etching process and a blasting process for controlling the increasing rate of the surface area. CONSTITUTION: A surface processing method of a dental implant fixture comprises the following steps: washing contaminants from the outer surface of the dental implant fixture(S100); increasing the surface area of the dental implant fixture by surface processing(S200); preparing powder for forming a HAp target, and heating and compressing the power for obtaining the HAp target(S300); and a evaporating the HAp target on the surface of the dental implant fixture using an RF-sputtering process(S400).

Description

Surface treatment method of dental implant fixture using RF-sputtering process

1 is a real picture showing the appearance of the surface treated fixture according to the surface treatment method of the dental implant fixture according to the present invention.

2 is a process flow chart sequentially showing the surface treatment method of a dental implant fixture according to the present invention.

Figure 3 is a table showing the properties of titanium dioxide powder and HAp powder used in the blasting process in the surface treatment method of the dental implant fixture according to the present invention.

Figure 4 is a real picture showing the appearance of the HAp target used in the HAp coating step in the surface treatment method of the dental implant fixture according to the present invention.

Figure 5 is an XRD results of the HAp target used in the HAp coating step in the surface treatment method of the dental implant fixture according to the present invention.

Figure 6 is a table showing the hardness of the HAp target used in the HAp coating step in the surface treatment method of the dental implant fixture according to the present invention.

Figure 7 is a table showing the EDX results of the HAp target used in the HAp coating step in the surface treatment method of the dental implant fixture according to the present invention.

Figure 8 is a schematic diagram showing the configuration of the RF sputtering apparatus used in the HAp coating step in the surface treatment method of the dental implant fixture according to the present invention.

Figure 9 is a table showing the conditions of the HAp coating step in the surface treatment method of the dental implant fixture according to the present invention.

10 is an enlarged photograph showing an outer surface of a fixture in which a blasting process of one step is completed in the method for treating a surface of a dental implant fixture according to the present invention;

11 is an enlarged photograph showing an outer surface of a fixture in which an etching process is completed as a step in the surface treatment method of a dental implant fixture according to the present invention;

12 is an enlarged photograph showing an outer surface of an embodiment in which a HAp coating step is performed without performing an etching process as a step in the surface treatment method of a dental implant fixture according to the present invention.

13 is a component analysis table of FIG.

Figure 14 is an enlarged photograph showing the appearance of an embodiment of the present invention.

15 is a component analysis table of FIG. 14.

16 is experimental data showing the surface area change when the blasting process and the etching process are selectively performed in the surface treatment method of the dental implant fixture according to the present invention.

Explanation of symbols on the main parts of the drawings

100. RF sputtering device 120. Vacuum chamber

140. Gas injection means 160. Power supply means

 D. Deposition Object S100. Washing steps

S120. First washing process S140. 2nd washing process

S220. Blasting process S240. Etching Process

S400. HAp coating step S320. Powder manufacturing process

S340. Target formation process S400. HAp coating step

 T. HAp target

The present invention relates to a surface treatment method of a dental implant fixture using an RF-sputtering process to selectively perform a surface treatment step to increase the surface area and then to deposit HAp to improve bone fusion.

Implant means a substitute that recovers when human tissue is lost, but in the dentist, it means an artificial root that allows implantation of artificial teeth.

That is, the implant is made of titanium, etc., which has no rejection reaction to the human body to replace the tooth root of the missing tooth, the fixture (lower fixation) is fixed to the bone from which it is removed, and the upper zone part is fastened on the fixture. An artificial crown (crown) is fixed above the upper zone so that the function of the tooth can be restored.

Therefore, in the case of a general prosthesis or denture, the surrounding teeth and bones will be damaged over time, but the implant will not damage the surrounding dental tissue, and compared with natural teeth, the function or shape will be almost the same, and dental caries will not occur. Many researches and developments are underway.

The fixture is fixed by being screwed into the alveolar bone and fused with the bone during the construction of the implant. The fixture is applied to various surface treatment techniques to be fused with the bone within a short period of time after being treated on the alveolar bone.

In other words, conventionally known surface treatment techniques include a method of manufacturing an implant by blasting the implant surface using calcium phosphate particles, bone tissue particles, or HAp particles using a resorbable blast media (RBM) technique, and sandblast large grit acid (SLA). etch) The surface of the implant is blasted and then etched with etching solution such as HF, HCl, H ₂ SO ₄ to use the implant, and the method of anodizing the surface of titanium to give roughness. Various methods to help the growth of the pubic bone, or calcium phosphate particles, there is a method of coating the HAp particles.

However, in the case of a commercial product manufactured in this way, the increase rate of the surface area indicating the bonding area with the pubic bone is confirmed and known to be around 200-300%. In particular, the implant made of SLA has a low value even in wettability. Long bone integration is known to require a long time.

An object of the present invention is to solve the conventional problems as described above, by using a surface treatment step to selectively increase the surface area and then deposit the HAp component by using the RF-sputtering process to improve the bone fusion An object of the present invention is to provide a surface treatment method for an implant fixture.

Another object of the present invention is to provide a surface treatment method of a dental implant fixture using an RF-sputtering process to control the surface area increase rate by selectively performing a blasting process and an etching process in the surface treatment step.

The surface treatment method of a dental implant fixture using the RF (RF) -sputtering process according to the present invention, a washing step for removing contaminants attached to the outer surface of the dental implant fixture machined, and dental implant fixture It characterized in that the HAp coating step of depositing a HAp (Hydroxy Apatite) target on the outer surface by RF-sputtering method.

The washing step may include a first washing process in which the machined dental implant fixture is immersed in an organic solvent to remove organic contaminants, and a second ultrasonic immersing process of the dental implant fixture in which the organic contaminants are removed in a water soluble cleaner. Characterized in that the washing process.

Between the washing step and the HAp coating step, a surface treatment step of increasing the surface area of the dental implant fixture is carried out.

In the surface treatment step, a blasting process of increasing the surface area by blasting titanium dioxide (TiO ₂ ) or HAp powder on the outer surface of the dental implant fixture, and the surface area by etching the dental implant fixture with an increased surface area At least one of an increasing etching process is carried out.

In the blasting process, the titanium dioxide has a particle size of 50 to 200㎛, the HAp powder is characterized in that it has a particle size of 50 to 400㎛.

The etching process is characterized in that the dental implant fixture is a process of increasing the surface area by immersing in an etching solution containing one or more of sulfuric acid, hydrochloric acid, hydrofluoric acid.

Between the HAp coating step and the surface treatment step, there is provided a target forming step including a powder manufacturing process for producing a powder to form a HAp target, and a target forming process for forming a HAp target by heating and pressing the powder It features.

In the powder manufacturing process, the upper solution is maintained at pH 5.5 to 5.6 in the form of a precipitate by adding phosphoric acid to the powder containing at least one of calcium carbonate (CaCO ₃ ) and calcium oxide (CaO ₃ ) and stirring and reacting. Phosphoric acid is added so as to be heated to 60 to 90 ° C. to evaporate moisture, thereby producing a powder.

The target forming process is characterized in that the process of forming a HAp target by pressing the powder produced in the powder manufacturing process to form a predetermined shape, then heat treatment in a vacuum argon atmosphere.

The HAp coating step is a process of preheating the RF sputtering apparatus, washing the HAp target with plasma in an argon atmosphere in a vacuum state, and then sputtering.

According to the present invention as described above, there is an advantage that the surface area is increased, HAp is deposited on the outer surface to improve bone fusion.

Hereinafter, a fixture manufactured according to the method for treating a surface of a dental implant fixture according to the present invention will be described.

Figure 1 is a real picture showing the appearance of the surface treated fixture according to the surface treatment method of the dental implant fixture according to the present invention.

First, the fixture is largely inserted into and fixed to the alveolar bone consisting of sponge bone and sponge (Cortical Bone), and the upper part is located above the gum and coupled with the upper zone supporting the phosphorescent crown.

Therefore, the surface of the fixture should have a wide surface area and have similar components to the alveolar bone so that bone fusion with the alveolar bone can be improved.

The surface treatment method for making the surface state of such fixture is described with reference to FIG. 2.

2 is a process flowchart showing the surface treatment method of the dental implant fixture according to the present invention in order.

As shown in the figure, the surface treatment method of the fixture using the RF-sputtering process, washing step (S100) for removing contaminants attached to the outer surface of the dental implant fixture largely machined, and the outer surface of the dental implant fixture HAp (Hydroxy Apatite) target (T) is made of a HAp coating step (S400) of depositing by RF-sputtering method.

The washing step (S100) is a process for removing organic contaminants, metal contaminants, etc. attached to the outer surface of the finished fixture, such contaminants are removed by a number of processes.

That is, the washing step (S100) is a first washing process (S120) to remove the organic contaminants by immersing the machined dental implant fixture in an organic solvent, and ultrasonically immersed in a water-soluble detergent to remove the organic contaminants It consists of a second washing process (S140) for washing.

In the first washing process (S120), the fixture is immersed in an ultrasonic cleaning tank containing an organic solvent of 40 to 80 ℃, and then dissolved by removing the organic cutting oil and organic contaminants attached to the outer surface of the fixture using ultrasonic waves for 3 to 5 minutes. Done.

After the first washing process (S120), a process of applying hot air to the fixture and drying may be performed.

After the first washing process S120, a second washing process S140 is performed. The second washing process (S140) is a process of immersing the fixture in an ultrasonic washing tank containing a water-soluble cleaner at 20 to 60 ° C. and then cleaning the ultrasonically for 5 to 10 minutes, by removing inorganic / metal contaminants from the outside of the fixture. Will be removed.

After the cleaning step (S100), the surface treatment step (S200) may be selectively carried out.

That is, a surface treatment step S200 may be performed between the cleaning step S100 and the HAp coating step S400 to increase the surface area of the fixture outer surface.

The surface treatment step (S200) is a blasting process (S220) to increase the surface area by using a blasting (blusting) process on the outer surface of the dental implant fixture washed, and the surface area by etching the dental implant fixture with an increased surface area One or more of the etching process (S240) to increase the can be carried out.

When the blasting process (S220) is performed after the washing step (S100), the blasting process (S220) is a surface area by blasting the titanium dioxide (TiO ₂ ) or HAp powder on the outer surface of the fixture (roughing) to rough the surface In order to increase this, in the embodiment of the present invention, as shown in the photo of Figure 3 titanium dioxide (TiO ₂ ) having a particle size of 50 to 200㎛ and HAp powder having a particle size of 50 to 400㎛ Used.

After the blasting process (S220), an etching process (S240) is performed. The etching process (S240) is a process of increasing the surface area by dipping the fixture in an etching solution containing one or more of sulfuric acid, hydrochloric acid, hydrofluoric acid.

That is, although the inorganic / metal contaminants remaining on the surface of the fixture are removed in the etching process (S240), the biggest purpose of the etching process (S240) is the surface of the fixture whose surface is roughened through the blasting process (S220). Etching was performed by etching to allow a larger surface area.

In addition, the etching process S240 may be performed immediately after the cleaning step S100 without performing the blasting process S220.

After the etching process (S240), the HAp coating step (S400) is performed. The HAp coating step (S400) is a process of sputtering and depositing HAp (Hydroxy Apatite) powder, which is similar to bone tissue of the body, on the surface of the etched fixture.

That is, in the exemplary embodiment of the present invention, the HAp target T as shown in FIG. 4 is manufactured, charged into an RF-sputtering apparatus (see 100 in FIG. 8), and then deposited on the outer surface of the deposition target (such as a fixture). .

Meanwhile, a target forming step S300 is performed before the HAp coating step S400. The target forming step (S300) is a process for manufacturing a HAp target (T) which is a raw material to be deposited on the outer surface of the fixture in the HAp coating step (S400).

That is, the target forming step (S300) is a powder manufacturing process (S320) for producing a powder to form a HAp target (T), and heating and pressurizing the powder to produce a HAp target (T) as shown in FIG. Target formation process (S340) is made.

The HAp target (T) was prepared in a disc shape having a diameter of 76.2 mm and a thickness of 10 mm in the embodiment of the present invention. In the powder manufacturing process (S320), calcium carbonate (CaCO ₃ ) and calcium oxide (CaO _3). Phosphoric acid is added to the powder containing at least one of), stirred and reacted to add a phosphoric acid so that the upper solution maintains a pH of 5.5 to 5.6 while the precipitate is formed, and is heated to 60 to 90 ° C. to evaporate the water. Made.

As described above, it can be seen that the powder for preparing the HAp target (T) includes 69.1 wt% of calcium (Ca) and 30.9 wt% of phosphorus (P) as shown in FIG. 7.

The HAp target manufacturing powder having the composition as described above is made into a disk form as shown in FIG. 4 through the target forming process (S340).

The target forming process (S340) is a process of forming a predetermined shape by pressing the powder produced in the powder manufacturing process (S320), heat treatment in an argon atmosphere in a vacuum state to form a HAp target (T).

HAp target (T) made through the target formation process (S340) can be seen that the XRD analysis of Figure 5 includes a large amount of Ca ₅ (PO ₄ ) ₃ OH.

In addition, the HAp target T manufactured through the target forming process S340 has a hardness of Hv 470 or higher as shown in FIG. 6.

The HAp target T manufactured through the target forming process S340 is deposited on the deposition target (D. fixture) through the RF sputtering apparatus 100 having the configuration as shown in FIG. 8.

Referring to the configuration of the RF sputtering apparatus 100 schematically, the RF sputtering apparatus 100 is a vacuum chamber 120, the HAp target (T) and the deposition target (D) is charged, and the gas injection into the vacuum chamber It comprises a gas injection means 140 for guiding the power supply means 160 for applying RF power to the vacuum chamber and the HAp target (T).

 The power supply means is connected to the HAp target (T) and the negative (-) pole and a positive (+) pole is connected to the inner wall of the vacuum chamber 120 so that sputtering can be generated.

In addition, an argon (Ar) gas is injected into the vacuum chamber 120 to allow deposition in an argon atmosphere, and a separate heater may be provided to heat the inside of the vacuum chamber 120 to a predetermined temperature range. It may be.

The HAp coating step S400 is performed using the RF sputtering apparatus 100 configured as described above.

The HAp coating step (S400) is a process of preheating the RF sputtering apparatus 100, plasma cleaning the HAp target T in a vacuum argon atmosphere, and then sputtering.

At this time, the condition of the HAp coating step (S400) is as shown in FIG.

Hereinafter, with reference to FIGS. 10 to 16, which surface states and characteristics of the fixtures manufactured through the above steps have respective stages will be described.

10 is an enlarged photograph showing an outer surface of a fixture in which a blasting process is completed as a step in the surface treatment method of a dental implant fixture according to the present invention, and the surface of the fixture in which the blasting process (S220) is completed is roughened You can see that.

In addition, when the etching process (S240) is performed after the blasting process (S220) as shown in Figure 11 it can be seen that the surface area of the fixture is much wider than the case of performing only the blasting process (S220).

That is, the embodiment (second from the left of FIG. 16) which sequentially performed the blasting process (S220) and the etching process (S240) as shown in Figure 16 showed an increase in surface area of more than 900%, but only the blasting process (S220) In this case, the surface area increase, such as when only the HAp powder was blasted, was relatively low.

However, compared to the surface area increase rate according to the prior art, it showed a significantly increased surface area increase rate of 400%.

The fixture having the increased surface area through the blasting process (S220) and the etching process (S240) has a surface state as shown in FIG. 14 by depositing the HAp target (T) on the outer surface of the fixture through the HAp coating step (S400). And component analysis of the sample surface of FIG. 14 resulted in the same results as FIG. 15.

That is, FIG. 15 is a component analysis table of FIG. 14, and the content of Ti, which is the raw material of the fixture, was the highest, and 12.73 wt% of calcium (Ca) and 7.04 wt% of phosphorus (P) were included.

Therefore, it can be seen that the HAp component is deposited on the outer surface of the fixture through the HAp coating step (S400).

In addition, when the etching process (S240) is not performed before the HAp coating step (S400), less HAp components are detected as shown in FIGS. 12 and 13.

That is, when the HAp coating step (S400) is performed without performing the etching process (S240), it can be seen that the surface area is reduced as shown in FIG. 12. As for the deposition amount, as shown in FIG. 13, 9.67 wt% of calcium (Ca) and phosphorus ( P) 5.73% by weight can be shown that the etching process (S240) is selectively carried out can increase the surface area.

As a result, according to the embodiment of the present invention, the blasting process S220 and the etching process S240 may be selectively performed to control the increase rate of the surface area of the fixture.

The scope of the present invention is not limited to the above-exemplified embodiments, and many other modifications based on the present invention will be possible to those skilled in the art within the above technical scope.

In the method for surface treatment of dental implant fixtures using the RF-sputtering process according to the present invention, the blasting process and the etching process are selectively performed to increase the surface area of the fixture, and then the human body using the RF sputtering device. HAp similar to the bone tissue was deposited.

Therefore, there is an advantage that the rejection reaction is minimized and bone fusion is improved by maximizing the surface area.

In addition, as the surface area increases, bone fusion is possible within a short time, and after bone fusion is completed, there is an advantage in that the bonding performance with the alveolar bone is more improved.

In addition, the present invention can control the surface area increase rate of the fixture by selectively performing the blasting process and the etching process, there is an advantage that the surface area required for the fixture can be implemented.

Claims (10)

A cleaning step of removing contaminants attached to the outer surface of the machined dental implant fixture, A surface treatment method of a dental implant fixture using an RF-sputtering process comprising a HAp coating step of depositing a HAp (Hydroxy Apatite) target on the outer surface of a dental implant fixture by RF-sputtering. The method of claim 1, wherein the washing step, A first washing process of dipping the machined dental implant fixture in an organic solvent to remove organic contaminants; A method of treating a surface of a dental implant fixture using an RF-sputtering process, comprising a second washing process in which an organic contaminant-removed dental implant fixture is immersed in an aqueous detergent and ultrasonically cleaned. According to claim 1, Between the washing step and the HAp coating step, Surface treatment step of increasing the surface area of the dental implant fixture, characterized in that the surface treatment method of the dental implant fixture using the RF sputtering process. The method of claim 3, wherein in the surface treatment step, A blasting process of increasing the surface area by blasting titanium dioxide (TiO ₂ ) or HAp powder on the outer surface of the dental implant fixture, A surface treatment method of a dental implant fixture using an RF-sputtering process, characterized in that at least one of the etching processes for etching the dental implant fixture with an increased surface area is performed to increase the surface area. The method of claim 4, wherein in the blasting process, The titanium dioxide has a particle size of 50 to 200㎛, The HAp powder has a particle size of 50 to 400 ㎛ surface treatment method of the dental implant fixture using the RF sputtering process. The method of claim 4, wherein the etching process, The surface treatment method of the dental implant fixture using an RF sputtering process characterized in that the process of increasing the surface area by immersing the dental implant fixture in an etching solution containing one or more of sulfuric acid, hydrochloric acid, hydrofluoric acid. According to claim 3, Between the HAp coating step and the surface treatment step, A powder manufacturing process for preparing a powder to form an HAp target, And a target forming step including a target forming step of heating and pressurizing the powder to form a HAp target. The method of claim 7, wherein the powder manufacturing process, Phosphoric acid is added to the powder containing at least one of calcium carbonate (CaCO ₃ ) and calcium oxide (CaO ₃ ), and the mixture is stirred and reacted to add phosphoric acid so that the upper solution maintains a pH of 5.5 to 5.6 in the form of a precipitate. Method of treating the surface of the dental implant fixture using an RF sputtering process characterized in that the process of heating to 60 to 90 ℃ evaporates the water to make a powder. The method of claim 7, wherein the target forming process, Pressing the powder produced in the powder manufacturing process to form a predetermined shape, and then heat-treated in a vacuum argon atmosphere to form a HAp target surface of the dental implant fixture using an RF-sputtering process Treatment method. The method of claim 3, wherein the HAp coating step, And preheating the RF sputtering device, washing the HAp target with a plasma in an argon atmosphere in a vacuum state, and then sputtering the sputtering process.

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