KR20090000936A - Bio ceramics and fabricating merhod thereof - Google Patents

Bio ceramics and fabricating merhod thereof

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Publication number
KR20090000936A
KR20090000936A KR1020070064889A KR20070064889A KR20090000936A KR 20090000936 A KR20090000936 A KR 20090000936A KR 1020070064889 A KR1020070064889 A KR 1020070064889A KR 20070064889 A KR20070064889 A KR 20070064889A KR 20090000936 A KR20090000936 A KR 20090000936A
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KR
South Korea
Prior art keywords
apatite
porous
sol
porous member
bio
Prior art date
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KR1020070064889A
Other languages
Korean (ko)
Inventor
성훈
Original Assignee
주식회사 새한정관
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Publication date
Application filed by 주식회사 새한정관 filed Critical 주식회사 새한정관
Priority to KR1020070064889A priority Critical patent/KR20090000936A/en
Publication of KR20090000936A publication Critical patent/KR20090000936A/en

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02—Inorganic materials
    • A61L27/04—Metals or alloys
    • A61L27/06—Titanium or titanium alloys
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02—Inorganic materials
    • A61L27/10—Ceramics or glasses
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/28—Materials for coating prostheses
    • A61L27/30—Inorganic materials
    • A61L27/32—Phosphorus-containing materials, e.g. apatite
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/56—Porous materials, e.g. foams or sponges

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Medicinal Chemistry (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Transplantation (AREA)
  • Epidemiology (AREA)
  • Veterinary Medicine (AREA)
  • Dermatology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials For Medical Uses (AREA)

Abstract

Method for producing a bio ceramics according to the present invention comprises the steps of providing a base member; Forming a porous member having a porous surface on the base member by a micro arc process; Forming sol apatite on the surface of the porous member; Drying the sol-apatite hydroxide to form a gel-apatite hydroxide layer.

Therefore, the bio-ceramic and the manufacturing method according to the present invention can obtain a coating of gel hydroxide apatite in a state in which the sol-apatite hydroxide is absorbed into the pores by using a porous member having pores on the surface thereof, thereby binding and compactness There is an effect to improve.

In addition, the bioceramic according to the present invention is stable in vivo by coating apatite hydroxide on the surface of the porous member formed of titanium dioxide, and improves the biocompatibility and bioactivity of titanium dioxide. It is effective to shorten the recovery period during the implant procedure of the patient.

Description

Bio ceramics and its manufacturing method {Bio Ceramics and fabricating merhod

1a to 1d show a process diagram of a bioceramic according to the present invention.

2 is a flow chart showing a method of forming a bio-ceramic according to the present invention.

Figure 3 schematically shows a micro arc system for the surface treatment of the base member of the bioceramic according to the present invention.

4 is a view showing an XRD graph of the porous member of the bioceramic according to the present invention.

5a to 5e is a view of the surface of the porous member of the bioceramic according to the present invention.

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to bio ceramics and a method of manufacturing the same, and to a bio ceramics and a method of manufacturing the same, which have improved strength and fracture toughness by forming a gelapatite hydroxide on a porous member having a low strength.

Titanium and titanium alloys (Ti-6Al-4V) have excellent mechanical strength and are used in many places in recent years. Moreover, titanium is formed in nature in a stable state of the oxide film (TiO 2 ) to prevent oxidation, corrosion, and the like found in other metals.

One use of titanium dioxide is in vivo implants, which are widely used in orthopedic and dental prosthetics. This is because titanium dioxide itself is very bioinertness in vivo.

 However, titanium dioxide has a problem in that it takes a long time to recover after orthopedic or dental surgery due to its lack of bioactivity in vivo.

Therefore, in recent years, efforts have been made to solve the problem of long recovery time by coating a material having high bioactivity on titanium to enhance the in vivo activity of titanium dioxide.

The present invention is a bio ceramics having a predetermined strength and corrosion resistance characteristics, coated with apatite hydroxide that can maximize the activity in vivo to a porous member that can be durable (durable) for a long time in the living body and The purpose is to provide a method of manufacturing the same.

In addition, another object is to provide a bio-ceramic and a method of manufacturing the same that can minimize the recovery period after the implant procedure.

Method for producing a bio ceramics according to the present invention as a means for achieving the above technical problem comprises the steps of providing a base member; Forming a porous member having a porous surface on the base member by a micro arc process; Forming sol apatite on the surface of the porous member; Drying the sol-apatite hydroxide to form a gel-apatite hydroxide layer.

The base member is formed of a titanium metal layer and a titanium oxide layer.

The porous member is formed of a titanium metal layer and a porous titanium oxide layer.

The hydroxyapatite in the sol state is characterized in that the composition ratio of calcium and phosphorus is formed to 1.67: 1.

The sol apatite hydroxide is dried at room temperature to form the gel apatite hydroxide.

The micro arc system includes an anode formed of the base member; A cathode formed of stainless steel; It characterized in that it has an electrolyte in which the positive electrode and the negative electrode is contained.

The electrolyte is characterized in that using dibasic sodium phosphate (Na 2 HPO 4 ).

The micro arc system is characterized by providing a voltage of 300 ~ 350V during oxidation.

The micro arc system is characterized by providing a current of 30 ~ 35A during oxidation.

Bioceramic according to the present invention for achieving the above technical problem is a porous member having a titanium metal layer and a porous titanium oxide layer; It includes a gelated apatite hydroxide formed on the surface of the porous member.

Advantages and features of the present invention and methods for achieving them will be apparent with reference to the embodiments described below in detail with the accompanying drawings.

However, the present invention is not limited to the embodiments disclosed below, but may be implemented in various different forms, only the present embodiments to make the disclosure of the present invention complete, and common knowledge in the art to which the present invention pertains. It is provided to fully inform the person having the scope of the invention, which is defined only by the scope of the claims. Like reference numerals refer to like elements throughout.

In addition, in the drawings, the size and thickness of layers and films or regions are exaggerated for clarity of description, and when any film or layer is described as being "formed" on another film or layer, the film or layer is It may be directly on top of the other film or layer, and a third other film or layer may be interposed therebetween.

1A to 1D are views illustrating a process diagram of a bioceramic according to the present invention, and FIG. 2 is a flowchart illustrating a method of forming the bioceramic according to the present invention.

1A to 1D and FIG. 2 will be described with matching with each other.

Referring to steps S210 of FIGS. 1A and 2, a base member 100 having a predetermined strength is prepared.

The base member 100 may use a metal having a predetermined strength, and in the present invention, titanium metal may be used as an embodiment. The surface of the titanium metal may be oxidized to form a titanium oxide layer 120.

Therefore, the base member 100 is formed of a titanium metal layer 110 and a titanium oxide layer 120.

In steps S220 of FIGS. 1B and 2, a plurality of pores are formed on the titanium oxide layer 120 to form a porous titanium oxide layer 150 having a porous surface.

The porous titanium oxide layer 150 may be formed through a micro arc system. Through the micro arc system, the titanium oxide layer 150 may be thickened and densified by oxidation.

In addition, the porous titanium dioxide layer 150 may also be formed through the micro arc system.

The method by oxidation using the microarc system can be used to obtain an oxide layer of metal because a thick oxide layer (tens of micrometers) can be obtained in a short time (water).

Dipping the micro-arc system titanium into an electrolyte and applying a voltage and a current of several hundred volts and tens of amperes to obtain a very dense and thick titanium dioxide on the titanium surface. Furthermore, on the surface of titanium dioxide, a porous film can be formed from an arc (plasma flame) generated by high power.

Here, the micro-arc system will be described with reference to FIG. 3 for easy description of the present invention.

3 is a view schematically showing a micro arc system for the surface treatment of the base member of the bioceramic according to the present invention.

The micro arc system 30 may use a titanium metal plate, that is, the base member 100 as an anode, and may use the stainless steel as a cathode 310 to form the micro arc system. The electrolyte 330 may use dibasic sodium phosphate (Na 2 HPO 4 ).

After the base member 100 is immersed in the electrolyte 330, the base member 100 is applied as a positive electrode and stainless steel is used as the negative electrode 310 to apply a strong voltage and a strong current.

Here, the voltage may provide 300V to 350V. And the current can provide 30A to 35A.

Meanwhile, the porosity formed in the base member was observed by setting the time for immersing the negative electrode and the positive electrode metal plate in the electrolyte 330 as 5 minutes, 10 minutes, 20 minutes, 30 minutes, and 40 minutes, respectively. The porosity will be described later with reference to FIGS. 5A to 5E.

As such, the strong currents and voltages provided by the micro arc system 30 may cause micro arcs on the titanium metal surface and cause thermal decomposition of oxygen anions (O 2- ) rapidly attracted by the anode of the titanium metal.

That is, on the titanium metal surface, oxygen pyrolyzed by a micro arc may react with the titanium surface to generate a thick titanium dioxide layer 150.

By the way, the feature of the titanium dioxide layer is that it is porous. This may be due to the high energy of the micro arc.

As described above, the porous member 10 having a porous surface may be formed through the micro arc system 30.

Referring to steps S230 of FIGS. 1C and 2, a process of coating apatite hydroxide on the surface of the porous member 10 is performed.

The apatite hydroxide is a material having a composition very similar to that of bone, which is not only very stable in vivo but also has high activity and is easy to use in the application of implants.

The step of filling the surface of the porous member 10 is immersed in the hydroxyapatite solution 210 in the sol (sol) state on the surface of the porous member 10 subjected to the micro-arc process.

Here, the process of making a sol of apatite hydroxide is configured as follows. In order to make calcium (Ca 2+ ) ions of hydroxide apatite colloidal in solution, calcium ethoxide (Ca (C 2 H 5 O) 2 ), diethoxide) was dispersed in ethanol and then ethanediol (HOCH 2 CH) 2 OH, ethanediol).

Next, triethyl phosphate diluted in ethanol may be used for colloidal dispersion of phosphorus (P 5+ ) ions. The two dispersion solutions may be sterilized to form a final apatite hydroxide sol 210.

The composition ratio of calcium and phosphorus is preferably 1.67: 1. Dipping the porous member into the colloid of the sol-state apatite may absorb the sol-state apatite 210 through the pores of the porous titanium dioxide layer 150.

Referring to steps S240 of FIGS. 1D and 2, a process of drying the sol apatite hydroxide 210 is performed.

As such, when the sol-shaped apatite hydroxide 210 is dried at room temperature, the gel-apatite hydroxide 20 may be formed. That is, the dense apatite membrane can be formed through the drying process.

In other words, the sol-state apatite 210 in the sol state filled in the porous member 10 forms a gel-apatite hydroxide 20 in the dry state to obtain a uniform coating on a complex surface than the conventional sol-gel method. There are advantages to it.

In addition, the coating with sol-gel may cause other phases of instability in the body even with a slight change in the composition of the hydroxyapatite, which has the advantage of effectively adjusting the composition of calcium and phosphorus in the sol state.

The apatite hydroxide structure coated on the porous member through the process as described above may allow the implant to be durable for a long time with great strength and corrosion resistance in vivo. In addition, hydroxyapatite in vivo can maximize the activity in vivo to minimize the recovery period after implantation.

 Figure 4 is a view showing an XRD graph of the porous member of the bioceramic according to the present invention.

Referring to FIG. 4, phase characteristics of the zirconia-hydroxyapatite mixed powder were investigated using XRD (X-ray diffraction: Rigaku Ulitma 2000). The target of the XRD was a copper target.

Here, the graph is a graph measured for each time the base member is immersed in the micro arc system. From the bottom of the graph the XRD data of the base member are shown for 5, 10, 20, 30 and 40 minutes for the soaking time, respectively.

As shown in FIG. 4, the anatase and lutheryl phases of the two crystalline phases of titanium were measured, and it can be determined that the phase characteristics of the base member are maintained even through the micro-arc process.

5A to 5E are images of the surface of the bioceramic according to the present invention.

5A to 5E, SEM images of the surface of the porous member are taken.

The angle was measured according to the time the porous member is placed in the electrolyte, it can be seen that as the time increases the number and size of the pores on the surface of the porous conflict.

As such, as the number and size of the pores increases on the surface of the porous member, the amount of sol-hydrated apatite penetrating the surface of the porous member increases.

Accordingly, the sol-apatite hydroxide is used on the surface of the porous member, and the sol-state apatite can be dried to form a gel-apatite hydroxide layer.

In other words, the gel-apatite hydroxide can be expected to coat a large amount on the surface of the porous member.

Bio-ceramics and a method for manufacturing the same according to the present invention can obtain a coating of gel-apatite hydroxide in a state in which sol-apatite hydroxide is absorbed into the pores by using a porous member having pores on the surface thereof, thereby improving bonding strength and compactness. It can be effected.

Bio-ceramics and a method for manufacturing the same according to the present invention can obtain a coating of gel-apatite hydroxide in a state in which sol-apatite hydroxide is absorbed into the pores by using a porous member having pores on the surface thereof, thereby improving bonding strength and compactness. It can be effected.

The bio-ceramic according to the present invention has the effect of coating the surface of the porous member formed of titanium dioxide with apatite hydroxide to improve the stability and activity in vivo and shorten the recovery period during the implant procedure of the patient.

Claims (10)

Providing a base member; Forming a porous member having a porous surface on the base member by a micro arc process; Forming sol apatite on the surface of the porous member; And drying the sol-apatite hydroxide to form a gel-apatite hydroxide layer. The method of claim 1, And said base member is formed of a titanium metal layer and a titanium oxide layer. The method of claim 1, Wherein said porous member is formed of a titanium metal layer and a porous titanium oxide layer. The method of claim 1, The sol hydroxide apatite is a bio-ceramic forming method, characterized in that the composition ratio of calcium and phosphorus is formed 1.67: 1. The method of claim 1, Wherein the sol-apatite hydroxide is dried at room temperature to form the gel-apatite hydroxide. The method of claim 1, The micro arc system An anode formed of the base member; A cathode formed of stainless steel; And a cathode in which the positive electrode and the negative electrode are contained. The method of claim 6, The electrolyte is a method of forming a bio-ceramic, characterized in that using dibasic sodium phosphate (Na 2 HPO 4 ). The method of claim 6, The micro-arc system is bio-ceramic forming method, characterized in that to provide a voltage 300 ~ 350V during oxidation. The method of claim 6, The micro-arc system is bio-ceramic forming method, characterized in that to provide a current 30 ~ 35A during oxidation. A porous member having a titanium metal layer and a porous titanium oxide layer; Bio ceramics comprising a gelated apatite hydroxide formed on the surface of the porous member.
KR1020070064889A 2007-06-29 2007-06-29 Bio ceramics and fabricating merhod thereof KR20090000936A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103046101A (en) * 2013-01-29 2013-04-17 哈尔滨工业大学 Preparation method of two-stage hole micro-arc oxidization biological coating with bacteriostatic effect
KR20190085679A (en) * 2018-01-11 2019-07-19 강릉원주대학교산학협력단 Method for coating bioceramic on a titanium implant surface and titanium implant prepared by the method
CN110560695A (en) * 2019-09-03 2019-12-13 西安建筑科技大学 Titanium-based functional gradient material with porous surface and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103046101A (en) * 2013-01-29 2013-04-17 哈尔滨工业大学 Preparation method of two-stage hole micro-arc oxidization biological coating with bacteriostatic effect
CN103046101B (en) * 2013-01-29 2015-02-11 哈尔滨工业大学 Preparation method of two-stage hole micro-arc oxidization biological coating with bacteriostatic effect
KR20190085679A (en) * 2018-01-11 2019-07-19 강릉원주대학교산학협력단 Method for coating bioceramic on a titanium implant surface and titanium implant prepared by the method
CN110560695A (en) * 2019-09-03 2019-12-13 西安建筑科技大学 Titanium-based functional gradient material with porous surface and preparation method thereof
CN110560695B (en) * 2019-09-03 2021-10-22 西安建筑科技大学 Titanium-based functional gradient material with porous surface and preparation method thereof

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