KR101742724B1 - Method for manufacturing porous Titanium scaffolds by utilizing freeze casting - Google Patents
Method for manufacturing porous Titanium scaffolds by utilizing freeze casting Download PDFInfo
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- KR101742724B1 KR101742724B1 KR1020150140171A KR20150140171A KR101742724B1 KR 101742724 B1 KR101742724 B1 KR 101742724B1 KR 1020150140171 A KR1020150140171 A KR 1020150140171A KR 20150140171 A KR20150140171 A KR 20150140171A KR 101742724 B1 KR101742724 B1 KR 101742724B1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
- B22F3/222—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by freeze-casting or in a supercritical fluid
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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
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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
- A61L27/50—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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
Abstract
A method for manufacturing a porous Ti metal support using freeze-molding is provided.
The present invention provides a process for producing a slurry, comprising: preparing a slurry by mixing a Ti metal powder, a freezing medium and a dispersant; Cooling the slurry while rotating to form a frozen formed body; Removing the freezing medium from the frozen formed body to form a porous body; And a step of heat-treating the porous body, wherein the freezing medium is formed by mixing one kind of additive selected from Menthol, Thymol and Polystyrene in a camphene To a method of manufacturing a porous Ti metal support.
Description
The present invention relates to a method for producing a porous metal support using freeze-molding, and more particularly, to a method for producing porous metal scaffolds by freeze- To a method for manufacturing a porous Ti metal support using freeze-thawing.
(Hereinafter referred to as " implants for living body implantation "), which are made of titanium, stainless steel alloy, cobalt-chromium alloy, bio-inert ceramic materials such as alumina and zirconia, and hydroxyapatite, Have been widely used.
Among the materials of these implantable implants, titanium has high biocompatibility, high physical properties and high fatigue resistance. Especially, when compared with cobalt-chromium alloy or stainless steel alloy, titanium has a low elastic modulus And is widely used as a material of a living implant implant.
However, although titanium has a low modulus of elasticity, due to the difference in elastic modulus with the bone, when titanium is used as the implant for implantation, a stress shielding phenomenon may occur which does not transmit stress to the bone. Researches have been actively conducted to develop a titanium alloy having a lower elastic modulus.
In addition, a material used as a living implant is required to have sufficient strength and to withstand loads over a long period of time, and to have good affinity with surrounding tissues. Therefore, recent studies have been actively carried out to develop a porous support for hard tissue application.
Development and commercialization of porous supports or porous bodies as implantable implants for living organs have been intensively competitive in developed countries such as the United States and Europe, and commercialization has been rapidly increasing in Korea as well as development studies. The following is a description of the manufacturing technology that is currently being utilized in the domestic and foreign development.
First, sponge replication is the most common method, in which a ceramic slurry is coated on the surface of a polyurethane sponge, followed by burning a polymer sponge by heat treatment, and compacting the ceramic to produce a porous article. This manufacturing technique is very useful for obtaining a very high porosity (about 80% or more) and a large pore connected three-dimensionally, but it is easy to generate cracks during heat treatment, has weaker strength than the other methods, and can not control an artificial pore structure There is a problem.
Co-extrusion is a technique for producing ceramic green fibers by coextrusion, laminating them, and preparing a porous article by heat treatment. Although it is easy to control porosity, pore size and pore arrangement, There is a disadvantage that defects such as cracks often occur during the heat treatment time and the heat treatment.
Solid freeform fabrication is a technology for manufacturing porous bodies using a computer 3-axis molding machine, which can be a complex type of pore structure. However, it requires disadvantages such as high equipment cost, limited production, and excessive heat treatment time .
The freeze casting process is a technique for producing a ceramic porous body by freezing a ceramic slurry and then removing the ice and heat-treating the ceramic slurry, which is a typical ceramic wet-process and is an environmentally friendly and very economical method. However, when the porous article is formed using the freeze-molding method, there is a problem that it is somewhat difficult to be practically used due to the relatively small pore size.
Examples of techniques for solving the problems include the invention disclosed in Korean Patent No. 10-0951789 and Japanese Patent Laid-Open No. 10-2010-0039466. However, the above-mentioned prior arts do not use a metal itself as a precursor for preparing a slurry used for freeze-molding, but a ceramic powder or a polymer material (Patent No. 10-0951789), a titanium Only ceramics such as hydride (TiH2) (Laid-Open Patent No. 10-2010-0039466) have been used.
This is because, when the metal itself is used as a precursor, the slurry is prepared by adding a dispersant different from ceramics due to the electrical properties of the metal, but the freezing medium and the metal slurry are separated from each other during the freezing process, I did not. As a result, the above-described technology of the present inventors has a problem in that there is a limit to the metal porous body that can be produced, and when the heat treatment is performed, the purity of the metal can be lowered.
Therefore, a technique (Patent Registration No. 10-1229213) capable of producing various kinds of metal porous articles using a metal other than ceramics has been developed, but it has a limitation on the size and distribution of pores imparted to the produced porous body And there is a growing demand for technology development that can complement them.
SUMMARY OF THE INVENTION Accordingly, the present invention has been made keeping in mind the above problems occurring in the prior art, and it is an object of the present invention to provide a method and apparatus for freezing and sterilizing a pest using a freezing medium prepared by mixing camphene with one selected from the group consisting of menthol, thymol and polystyrene. The present invention has been made in view of the above problems, and it is an object of the present invention to provide a Ti metal support having a porous structure capable of producing a titanium porous body having a desired size.
Further, the technical problems to be solved by the present invention are not limited to the technical problems mentioned above, and other technical problems which are not mentioned can be understood from the following description in order to clearly understand those skilled in the art to which the present invention belongs .
According to an aspect of the present invention,
A Ti metal powder, a freezing medium and a dispersing agent to prepare a slurry;
Cooling the slurry while rotating to form a frozen formed body;
Removing the freezing medium from the frozen formed body to form a porous body; And
And heat treating the porous body,
Wherein the freezing medium comprises a mixture of one kind of additive selected from the group consisting of Menthol, Thymol and Polystyrene in a camphene.
In the present invention, the slurry preparation process may be performed at a temperature higher than the freezing temperature of the freezing medium.
In the present invention, the content of the additive is preferably in the range of 0 to 10% with respect to the weight of the cam pin.
The content of the Ti metal powder may be in the range of 10 to 40 vol.% Relative to the freezing medium.
The content of the dispersant is preferably 0.1 to 10% by weight relative to the content of the Ti metal powder.
The step of forming the frozen formed body is preferably performed at a temperature below the freezing temperature of the freezing medium.
In the step of forming the frozen formed article, it is preferable that the slurry is injected into a mold having a predetermined shape and is rotated and cooled.
In the step of forming the porous article, it is preferable that the freezing medium is removed from the freeze-molded body by using at least one of lyophilization, sublimation and dissolution.
Wherein the freeze-molded body is maintained at a predetermined temperature range near the freezing temperature of the freezing medium while the freeze-molded body is formed between the step of forming the freeze-molded body and the step of forming the porous body, And a growth process.
It is preferable that the predetermined temperature range is a freezing temperature of the freezing medium to a freezing temperature of -20 ° C.
The heat treatment temperature is preferably in the range of 1200 to 1350 ° C.
The heat treatment may be performed in a vacuum state.
The present invention having the above-described constitution has a beneficial effect of producing a porous metal support having a very low impurity content and a high purity because the porous metal support is produced using the Ti metal powder itself.
Further, in the present invention, the pore size, the porosity and the elastic modulus of a Ti metal support prepared by adding a freezing medium used for freezing molding to a camphene, Menthol, Thymol and polystyrene as additives And mechanical properties such as compressive strength can be more effectively controlled. Thus, it becomes possible to provide a porous metal support suitable for use as a living implant implant.
Such a porous metal scaffold can be used as a porous bone graft material that can be used as a living implant material such as living tissue and dentin to replace the bones of a human body damaged by disease or accident, and has high added value in the field of biotechnology (BT) Can be created.
FIG. 1 is a schematic view illustrating a method of manufacturing a porous Ti metal support using freezing according to an embodiment of the present invention. Referring to FIG.
FIG. 2 is a scanning electron micrograph of a porous Ti metal support prepared by the process according to the present invention, showing the type of additives (menthol, thymol and polystyrene) and texture changes with time of molding.
FIG. 3 is a graph showing the comparison of the growth rate of pore size according to the kind of the additives used and the time for forming the porous Ti metal supports prepared by the production method according to the present invention.
FIG. 4 is a graph showing the pore distribution by analyzing the porous Ti metal supports prepared by the manufacturing method according to the present invention using microcity according to the kinds of the additives used and the molding time.
FIG. 5 is a view showing a pore formation state of a porous metal support manufactured according to an embodiment of the present invention in a three-dimensional structure according to the type of additive used.
Hereinafter, the present invention will be described.
First, a method for producing a porous Ti metal support of the present invention comprises: preparing a slurry by mixing a Ti metal powder, a freezing medium and a dispersing agent; Cooling the slurry while rotating to form a frozen formed body; Removing the freezing medium from the frozen formed body to form a porous body; And a step of heat-treating the porous body. In the present invention, the freezing medium is prepared by mixing one kind of additives selected from camphene, Menthol, Thymol and polystyrene.
FIG. 1 is a schematic view illustrating a method of manufacturing a porous Ti metal support using freezing according to an embodiment of the present invention. Referring to FIG.
As shown in FIG. 1, in the present invention, a Ti metal powder, a freezing medium and a dispersant are mixed to prepare a slurry.
That is, it is preferable that the slurry is prepared in a state of good fluidity by mixing the metal powder, the freezing medium and the dispersant, and the present process is preferably performed at a temperature higher than the freezing temperature of the freezing medium.
In the present invention, titanium metal powder is used as the metal powder, and titanium powder is more preferably used because titanium has excellent properties as a material of a living implant. Such a metal powder is formed as a porous metal support which is the final product.
In the present invention, a camphene is used as the freezing medium because the freezing point of the campphin can be easily evaporated at a room temperature of 35 to 45 ° C, Can be improved.
At this time, in the present invention, it is preferable that one kind of additive selected from the group consisting of menthol, thymol and polystyrene in addition to the camphin is mixed with the cam pin as the freezing medium. The pore size of the Ti porous body produced by mixing the above-mentioned additives into the cam pin is increased and the distribution thereof is also variable, and thus it is suitable to be used as a living implant.
In the present invention, the content of the additive is desirably in the range of 0 to 10% with respect to the weight of the cam pin
In the present invention, the kind of the dispersant is not particularly limited as long as the titanium powder and the freezing medium can be uniformly dispersed and can be easily dried and evaporated. For example, an oligomeric polyester may be used as a dispersant.
These dispersants serve to disperse the metal powder in the frozen media. If a dispersant is not used, the metal powder can be rapidly layered with the freezing medium.
On the other hand, the content of the Ti metal powder is preferably 10 to 40% Vol. If the content of the metal powder is less than 10 vol.%, It is difficult to form the porous support structure due to the insufficient amount of metal in the process of removing the freezing medium after freezing. If the content of the metal powder exceeds 40 vol.%, The connected pores may not grow sufficiently.
In the present invention, a dispersant is used to help disperse the Ti metal powder in the freezing medium in the above process.
At this time, the content of the dispersant is preferably in the range of 1 to 10% by weight with respect to the content of the Ti metal powder. If the dispersing agent is less than 1 wt%, the metal powder can not be dispersed in the freezing medium. If the dispersing agent is more than 10 wt%, it may not evaporate sufficiently in a subsequent step. Further, in the subsequent heat treatment step, It is because.
In the present invention, ball-miling or stirring may be performed to more uniformly mix the Ti metal powder, the freezing medium and the dispersing agent.
Next, in the present invention, it is preferable that the slurry is cooled while being rotated to form a frozen formed body, and this step is preferably performed at a temperature below the freezing temperature of the freezing medium.
In the above-described process, the mixed slurry is injected into a mold having a predetermined shape, rotated together with the mold in the mold, and cooled to form a freezing molding agent. At this time, it is needless to say that the mold into which the slurry is injected may be manufactured in various shapes depending on the field in which the porous metal support is used. The mold may be made of various materials.
In this process, metal powder can be prevented from being precipitated in the slurry by rotating the slurry at a constant speed range in the mold, and by freezing the slurry in this state, the frozen formed body can be formed. That is, the present invention uses a principle that the metal powder to be precipitated in the freezing medium is uniformly distributed in the freezing medium by applying a constant driving force from the outside.
Meanwhile, the porosity and the pore size of the porous metal support produced through the control of the freezing temperature can be controlled in this step. That is, by varying the freezing temperature during the rotation of the slurry, the porosity and the pore size can be controlled by controlling the interval of the coagulation phase of the freezing medium.
Further, in the present invention, it is possible to grow the frozen granules of the frozen media by using the local remelting phenomenon while maintaining the frozen formed body formed in the above process at a certain temperature range near the freezing temperature of the frozen media.
The reason for carrying out this step is that the freezing medium needs to sufficiently grow into granules in order to secure the pore characteristics of the porous metal support such as the porosity, the pore size, and the three-dimensional space connectivity of the gas space.
For this purpose, in the present invention, it is desirable to grow the frozen formed body by keeping the frozen body at a freezing temperature and a freezing temperature of -20 캜 for a certain period of time. If the freezing temperature is exceeded, the freezing medium is melted as a whole and the freeze-molded body is disintegrated. At a temperature too lower than the freezing temperature, the granule growth does not occur or occurs very slowly.
Next, in the present invention, the freezing medium is removed from the frozen formed body to form a porous body. That is, the porous article can be formed by removing the freezing medium from the frozen formed article formed by the above-described process.
At this time, in the present invention, the freezing medium may be removed from the frozen formed body by using one or more of lyophilization, sublimation and dissolution. In other words, by freezing the frozen compacted body in a frozen state and rapidly drying it, the freezing medium is sublimated or the frozen medium in the frozen state is melted, whereby the frozen medium in the frozen body is finally poured into pores in the porous body .
Subsequently, in the present invention, the formed porous article is subjected to heat treatment.
In this step, heat treatment is performed in order to impart strength to the porous body formed in the above-described step, and mechanical properties such as elasticity and rigidity similar to those of a living bone tissue can be imparted to the porous body having pores formed by such heat treatment.
At this time, in the present invention, it is preferable to limit the heat treatment temperature to 1200 to 1350 ° C. If the heat treatment temperature is less than 1200 ° C, grains constituting the porous body may not be formed properly, On the other hand, if the temperature is higher than 1350 ° C, there is a problem that a part of the sintered porous body melts and flows down.
It is preferable that the heat treatment is performed in a vacuum state because the porous body is oxidized by the non-reactant such as oxygen and the unnecessary impurities are mixed in the porous body.
Hereinafter, the present invention will be described in more detail by way of examples.
(Example)
5.89 g of a Ti metal powder (Alfa Aesar, Ward Hill, Mass., USA), 10 g of a freezing medium consisting of a mixture of camphin (C10H16) and additives (one selected from the group consisting of menthol, thymol and polystyrene) and an oligomer polyester -4, UniQema, Everburg, Belgium) were prepared. In the present embodiment, experiments were conducted by dividing the case where the additives are monosilane, thymol, and polystyrene.
10 g of the prepared titanium, 10 g of freezing medium containing the individual additives of camphin and 0.1 g of oligomer polyester were mixed and ball milled for 24 hours at a temperature of about 60 캜 to prepare a slurry.
Then, the slurry was poured into a mold made of aluminum, the mold was rotated at a rotating speed of 20 rpm, and held at about 42 캜 for 2 to 6 days to form a freeze-molded body. The frozen formed body was separated from the mold, and the frozen medium was removed by maintaining the temperature of about -60 ° C under vacuum to remove the freezing medium from the frozen formed body to form a porous body.
Subsequently, the porous body was subjected to heat treatment at about 1300 캜 for about 2 hours to prepare porous Ti metal supports according to the present invention, respectively.
FIG. 2 is a scanning electron microscope (SEM) image of a porous Ti metal support prepared by the above-mentioned production method, showing the type of additives (menthol, thymol and polystyrene) and the texture change with time. FIG. 3 is a graph showing the comparison of the growth rate of pore size according to the type of additives used and the time for forming porous Ti metal supports prepared by the method of the present invention. And FIG. 4 is a graph showing the pore distribution by analyzing the porous Ti metal supports prepared by the above-described production method using microcity according to the kinds of the additives used and the molding time.
As shown in FIG. 2-4, it can be seen that the pore size increases with increasing molding time for all additives.
In addition, it can be seen that the additive Menthol, which is an additive added to the freezing medium, contributes to the formation of a tissue having a uniform pore distribution. In the case of thymol and polystyrene as additives, .
This can also be confirmed by referring to FIG. 5. Specifically, it can be seen that the case of the additive Mansol has uniformly formed pore channels, and the pore size is smaller than that of other additives. In addition, the additives, thymol and polystyrene, have elliptical pore channels and large pore sizes. It was found that the growth rate of porosity was faster with time when thymol and polystyrene were added as an additive.
While the present invention has been particularly shown and described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, Of course, this is possible. Therefore, the scope of the present invention should not be limited to the described embodiments, but should be defined by the equivalents as well as the claims that follow.
Claims (11)
Cooling the slurry while rotating to form a frozen formed body;
Removing the freezing medium from the frozen formed body to form a porous body; And
And heat treating the porous body,
Wherein the freezing medium is prepared by mixing one kind of additive selected from Menthol, Thymol and Polystyrene in a camphene in the range of 0 to 10% based on the weight of the cam pin. A method for manufacturing a porous Ti metal support.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20210109928A (en) | 2020-02-28 | 2021-09-07 | 한국에너지기술연구원 | Porous sintered titanium sheet and method of manufacturing thereof |
| KR20230116285A (en) | 2022-01-28 | 2023-08-04 | 한국에너지기술연구원 | Sintered metal powder based porous transport layer for improving gas-liquid transport in polymer electrolyte membrane water electrolysis cells, method for manufacturing the sintered metal powder based porous transport layer, and water electrolysis device including the sintered metal powder based porous transport layer |
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| KR101930474B1 (en) * | 2017-05-31 | 2018-12-18 | 한국생산기술연구원 | Method of manufacturing porous metal scaffolds coated with porous oxidation film and porous metal scaffolds manufactured thereby |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20210109928A (en) | 2020-02-28 | 2021-09-07 | 한국에너지기술연구원 | Porous sintered titanium sheet and method of manufacturing thereof |
| KR20230116285A (en) | 2022-01-28 | 2023-08-04 | 한국에너지기술연구원 | Sintered metal powder based porous transport layer for improving gas-liquid transport in polymer electrolyte membrane water electrolysis cells, method for manufacturing the sintered metal powder based porous transport layer, and water electrolysis device including the sintered metal powder based porous transport layer |
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