WO2017003192A1 - Alliage médical à base de tini et son procédé de production - Google Patents

Alliage médical à base de tini et son procédé de production Download PDF

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Publication number
WO2017003192A1
WO2017003192A1 PCT/KR2016/006987 KR2016006987W WO2017003192A1 WO 2017003192 A1 WO2017003192 A1 WO 2017003192A1 KR 2016006987 W KR2016006987 W KR 2016006987W WO 2017003192 A1 WO2017003192 A1 WO 2017003192A1
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Prior art keywords
tini
alloy
based medical
medical alloy
present
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Ceased
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PCT/KR2016/006987
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English (en)
Korean (ko)
Inventor
강지훈
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KANG&PARK MEDICAL CO Ltd
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KANG&PARK MEDICAL CO Ltd
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Priority claimed from KR1020160081466A external-priority patent/KR101832705B1/ko
Publication of WO2017003192A1 publication Critical patent/WO2017003192A1/fr
Anticipated expiration legal-status Critical
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent

Definitions

  • the present invention relates to a TiNi-based medical alloy, including Ti, Ni, Mo, Fe, and Al, which can provide various properties suitable for medical use while having high physical and mechanical properties, and a method for manufacturing the same.
  • TiNi-based alloys are widely used in the clinic, which exhibit unique characteristics such as shape memory effects, superelasticity, high corrosion resistance, strength, etc., and are able to withstand large loads under constant stress without permanent plastic deformation. Its use is increasing for medical use.
  • alloys of highly reactive metals are generally produced by arc melting, for example TiNi-based alloys are produced by consumable and non-consumable arc melting, firstly, complete control over the melting process and alloy composition is difficult, and secondly However, there is a problem that an expensive multi-arc melting process is required to achieve chemical homogeneity.
  • TiNi-based medical alloys with superelastic properties are widely used for medical purposes because of their high kinematic properties, suitability, and safety for human tissues, but they are difficult to work on cutting, pressing, and punching due to their rigidity and adhesion.
  • Silver can be prepared using a vacuum induction (VIM) process.
  • VIP vacuum induction
  • TiNi-based implants with stress-strain characteristics similar to human tissues (bones, cartilage, tendons) are known to be inherently difficult to regenerate if damaged after internal implantation, but are actually difficult to regenerate Or because the rupture of the implanted product (sealing material, etc.) is an important problem to be solved in order to be used for medical purposes, it is very important to improve the properties of TiNi-based alloys including tensile strength and the like.
  • the present invention is to provide a TiNi-based medical alloy containing Ti, Ni, Mo, Fe and Al, and can provide a variety of properties suitable for medical use while having high physical and mechanical properties and a method of manufacturing the same.
  • the present invention is charged with the structural strength, elastic properties, tissue compatibility, wear resistance, through vacuum induction after charging Ti, Ni, Mo, Fe and Al in the graphite crucible in a vacuum induction method (VIM) in an argon atmosphere
  • VIM vacuum induction method
  • An object of the present invention is to provide a TiNi-based medical alloy having improved properties suitable for use in medical applications such as life cycle and strain life.
  • a TiNi-based medical alloy may be provided, which is composed of Ti 44-48 wt%, Mo 0.2-3.0 wt%, Fe 0.1-2.0 wt%, Al 0.2-1.0 wt%, and balance Ni.
  • alloy components consisting of Ti 44-48 wt%, Mo 0.2-3.0 wt%, Fe 0.1-2.0 wt%, Al 0.2-1.0 wt% and balance Ni are dissolved using high frequency vacuum induction. And hot forging and hot extruding the alloy ingot obtained through the dissolving step, repeating the cold drawing and annealing at an intermediate temperature after the hot forging and hot extrusion, and the annealing. After the step of repeating, after the solution treatment for 0.5-1.5 hours at a temperature of 973K-1173K quenched to prepare a TiNi-based medical alloy comprising the step of producing a TiNi-based medical alloy.
  • the present invention includes Ti, Ni, Mo, Fe and Al, and can provide a TiNi-based medical alloy having high physical and mechanical properties and can provide a variety of properties suitable for medical use.
  • the present invention is charged with the structural strength, elastic properties, tissue compatibility, wear resistance, through vacuum induction after charging Ti, Ni, Mo, Fe and Al in the graphite crucible in a vacuum induction method (VIM) in an argon atmosphere It is possible to provide a TiNi-based medical alloy having improved properties suitable for use in medical applications, such as life cycle, strain life.
  • VIM vacuum induction method
  • 1A to 1E are diagrams for explaining the distribution of grain sizes in an Al-added TiNi-based alloy according to an embodiment of the present invention.
  • FIG. 2 is a diagram showing a stress strain of a conventional TiNi-based alloy containing no Al,
  • FIG. 3 is a view showing the maximum tensile strength and total elongation of the TiNi-based medical alloy according to an embodiment of the present invention
  • FIG. 4 is a view showing the temperature dependence of the martensite transformation of the TiNi-based medical alloy according to an embodiment of the present invention.
  • the TiNi-based medical alloy according to the embodiment of the present invention may be composed of Ti 44-48 wt%, Mo 0.2-3.0 wt%, Fe 0.1-2.0 wt%, Al 0.2-1.0 wt% and the balance Ni.
  • Ti is less than 44 wt% or more than 48 wt%, the restoring force and the damping effect below the transition temperature are remarkably inferior, and therefore, Ti is preferably added at a ratio of 44-48 wt%.
  • Mo may increase the strength and hardenability when added to the alloy, but the amount of addition may vary depending on the use of the alloy because the weldability is deteriorated, and when it is less than 0.2% by weight, the strength and the hardenability are increased. Since it is impossible to obtain and weldability falls when it exceeds 3.0 weight%, it is preferable to add in the ratio of 0.2-3.0 weight%.
  • Fe plays a role of stabilizing the ⁇ phase when added to the alloy, if the addition amount is less than 0.1% by weight there is a problem that can not sufficiently stabilize the ⁇ phase at room temperature, when the strength exceeds 2.0% by weight Since creep strength decreases while increasing, it is preferably added at a ratio of 0.1-2.0% by weight.
  • the ⁇ phase is strengthened, and as its content is increased, the strength may be increased by solid solution to titanium (Ti) base, and the specific density of the alloy may be reduced by decreasing the density of the alloy. strength), but if the amount is less than 0.2% by weight, there is a problem in that the density reduction effect is not large and the strength is lowered.
  • Ti 3 Al is formed so that the ductility of titanium Since it is sharply lowered, it is preferable to add it in the ratio of 0.2-1.0 weight%.
  • the manufacturing method of the TiNi-based medical alloy according to the present invention alloy components consisting of Ti 44-48% by weight, Mo 0.2-3.0% by weight, Fe 0.1-2.0% by weight, Al 0.2-1.0% by weight and the balance Ni
  • the step of melting using high frequency vacuum induction hot forging and hot extrusion of the alloy ingot obtained through the step of melting, and the step of hot forging and hot extrusion, cold drawing and annealing at an intermediate temperature are performed.
  • the step of repeating, and repeating the annealing comprising the step of quenching after solution treatment for 0.5-1.5 hours at a temperature of 973K-1173K, to prepare a TiNi-based medical alloy according to an embodiment of the present invention can do.
  • each of the alloying components can be loaded into granules having a size of 1-3 mm, the resulting TiNi-based medical alloy, the maximum tensile strength can have a range of 1420-1620 Mpa, superelastic section It may have a temperature range of 10-80 °C.
  • granular Ti sponge, Ni sheet and mixed alloy additives including Mo, Fe and Al
  • Ti sponge, Ni sheet and mixed alloy additives including Mo, Fe and Al
  • VIM vacuum induction melting
  • the alloy additives (including Mo, Fe and Al) to be mixed can be dissolved, and the TiNi-based medical alloy is maintained by maintaining the temperature of about 1350-1450 ° C. and a time of about 2-5 minutes while stirring the induction-melted alloy molten metal. It can be prepared.
  • the vacuum induction (VIM) process has a good mixing effect that provides chemical homogeneity of the liquid melt
  • the TiNi-based alloy can be melted in a low frequency vacuum induction furnace (VIM) furnace, and this low frequency vacuum induction ( The VIM) technique has been described as being used to melt a TiNi-based alloy because it can produce an excellent TiNi-based alloy at low cost, but other dissolution techniques performed in an inert atmosphere can of course be used.
  • the TiNi-based medical alloy dissolved through the vacuum induction melting (VIM) process as described above is injected into a preheating mold to solidify, and the alloy may be manufactured to have a fine casting surface through a casting process using the preheating mold. It is possible to optimize casting boundaries in thin sections and to minimize porosity in casting sections.
  • VIM vacuum induction melting
  • TiNi-based (including Mo, Fe, and Al) medical alloys have improved properties over conventional nitinol alloys (alloys of nickel and titanium).
  • nitinol alloys alloys of nickel and titanium.
  • the physical and mechanical properties of ingots, semi-finished or finished products It can be changed very finely and its casting cost can be reduced as a whole because process steps such as forging, milling and drawing are eliminated or greatly reduced.
  • the TiNi-based medical alloy sample according to the embodiment of the present invention to prepare and look at the characteristics, the electrolyte Ni plate (99.93% pure), the shape of the sponge Ti (99.74% pure), the alloy components in the form of additives layered
  • the furnace is placed inside a graphite crucible (99.9% pure), the crucible is placed inside an VIM furnace with an argon atmosphere, the VIM furnace is operated at an induction input of approximately 3000 cycles, and the alloying components charged into the crucible are thoroughly mixed.
  • the TiNi-based medical alloy shows good superelasticity, maximum tensile strength is approximately 1420MPa, yield point is approximately 510MPa, total elongation is approximately 64%, superelastic section is 5% elongation, 300MPa It appears in strength, and after 6% deformation, permanent deformation exhibits an improved characteristic of approximately 0.2, indicating that the stress-strain behavior is almost the same as human body tissue, making it suitable for medical use.
  • TiNi-based medical alloy having a superelastic properties in Ti% 44-46, Fe 1.5 or less by weight to increase the tensile strength , Mo 2 or less and residual Ni, and may further be prepared through a casting process, including Al 0.2-1.0.
  • Such TiNi-based medical alloys are suitable for use in the medical temperature range and strength characteristics of the alloy depending on Fe and Mo, tensile strength is mainly determined by iron (Fe), the alloy is granule (granule, granule) It can be prepared via a vacuum induction (VIM) process using a mixture of raw materials in the form (average granule size 1-3 mm).
  • VIM vacuum induction
  • the granule size mainly affects the contact surface of alloying elements such as nickel (Ni) and titanium (Ti), and during induction heating the granules interact with other components (interpenetration) and provide additional heat.
  • Process liquid structure which requires additional heat if the granule (granular) size exceeds approximately 3 mm, and the VIM process is not effective because of the increased technical complexity for dissolution of the alloying components.
  • VIM vacuum induction
  • the strength of the alloy is determined by the grain structure and the microstructure including the defects, it is known that the strength characteristics of the grains themselves, not the distribution of grain size is very important.
  • the maximum strength characteristic is represented by a fine grain size distribution.
  • the external load is evenly distributed, and when the grain size distribution is wide, the applied load is unevenly distributed, and as a result, the position where the crack nucleus (path) becomes. It can be localized.
  • one of the main prerequisites for strengthening the alloy is to obtain the most uniform (homogenous) microstructure, which can be achieved by adding Al to the TiNi-based medical alloy, such as the process described later, due to the high reactivity of Al
  • VIM vacuum induction
  • Al and Ni generate a self-combustion property (SHS), which may promote liquation phase separation, that is, movement of liquid components.
  • the newly formed grains of the polycrystalline structure were found to have a smaller average size compared to the alloy containing no Al, and the distribution of the grain size in the Al-added alloy was more uniform. I can see that.
  • FIGS. 1A to 1C are optical microstructure images of an Al-added TiNi-based alloy
  • FIGS. 1D and 1E are SEM images of an Al-added TiNi-based alloy, where 1 is a matrix phase.
  • 2 represents fine dispersed precipitates
  • 3 represents grain boundary dendritic precipitates, and it can be seen that the grain size is uniformly distributed in the Al-added alloy.
  • UTS User Tensile Strength: maximum tensile strength
  • the Al addition is 0.2-% by weight. Must be in the range 1.0.
  • Figure 2 is a diagram showing the stress strain of the conventional TiNi alloy containing no Al, the TiNi-based alloy conventionally does not contain Al 46 wt% Ti, 1.5 wt% Fe, 2 wt% Mo and the balance It can be made of Ni, which is the slope between A and B points in the typical stress-strain curves (strength-elongation curves, Y-axis: strength (MPa), X-axis: strain (%)) of this TiNi-based alloy.
  • the part corresponds to the region where the hyperelasticity appears, and its pressure-strain behavior is due to the reversible martensitic transformation, and further deformation can increase beyond the martensitic transformation range with pressure, corresponding to the C point. It can be seen that the maximum tensile strength (UTS) does not exceed 1400 MPa.
  • FIG. 3 is a view showing the maximum tensile strength and total elongation of the TiNi-based medical alloy according to an embodiment of the present invention
  • Al-added TiNi-based alloy was dissolved using high frequency vacuum induction, the dissolved ingot (ingot) After hot forging and hot extrusion, cold drawing and intermediate annealing were repeated to make a wire rod with a diameter of 1 mm, and a sample cut to the required length (for example, 40 mm, 100 mm, etc.) was approximately 973K-1173K. Samples were prepared by quenching and then quenching for 1 h at.
  • the maximum tensile strength (UTS) and concentration dependence (left axis: maximum tensile strength (UTS, MPa), right axis: total elongation (TEL,%), X axis: In addition, the maximum tensile strength (UTS) increases with increasing Al content within 30% -27% and shows a range of approximately 1420-16200 MPa. It can be seen that.
  • FIG. 4 is a diagram showing the temperature dependence of the martensite transformation of the TiNi-based medical alloy according to an embodiment of the present invention, the maximum tensile strength (UTS) after performing a strain-stress test for each temperature for the TiNi-based medical alloy samples The maximum tensile strength (UTS) over temperature was plotted.
  • the temperature dependence of the martensitic shear stress of the TiNi-based medical alloy according to the embodiment of the present invention (Y-axis: strength (MPa), X-axis: temperature (°C)), A (approximately) It can be seen that co-existing phases (maternal and martensitic) coexist with each other resulting in a hyperelastic effect, such as the similar dependence mentioned in the former located between points 10 ° C.) and B (approx. 80 ° C.).
  • the addition amount of Al within 1% by weight corresponds to the temperature range when the superelasticity appears near the human body temperature, and the TiNi-based medical alloy of the present invention to which Al is added within 1% by weight of the human body temperature range It can be seen that superelasticity appears at.
  • a superelastic section is a section in which a high temperature phase (austenite) and a low temperature phase (martensite) exist together, and the austenite completion temperature (A r ) and the martensite deformation temperature (M d or M s ) Within the zone (ie A r to M d ), which may undergo a reaction-organic transformation from the austenite phase to the martensite phase, so that when stress is applied to the alloy, the austenite in response to the applied stress From the transformation from martensite to the undeformed state once the strain is removed.
  • the TiNi-based alloy is not added to the conventional Al
  • the TiNi-based medical alloy according to the embodiment of the present invention has a specific temperature range (for example, due to Al addition) , 10-80 °C) shows a tendency to increase the tensile strength, so that when used for medical use can not only prevent damage more effectively, but also for medical use within the body (bio) temperature range (about 37 °C)
  • suitable superelastic properties are shown below.
  • the TiNi-based medical alloy according to the embodiment of the present invention comprises Ti 44-48 wt%, Mo 0.2-3.0 wt%, Fe 0.1-2.0 wt%, Al 0.2-1.0 wt%, and the balance Ni.
  • the maximum tensile strength may have a range of 1420-1620 Mpa
  • the hyperelastic section may have a temperature range of 10-80 °C.
  • the present invention can provide a TiNi-based medical alloy containing Ti, Ni, Mo, Fe and Al, and can provide a variety of properties suitable for medical use while having high physical and mechanical properties.
  • the present invention after charging Ti, Ni, Mo, Fe and Al into the graphite crucible inside the VIM in an argon atmosphere, and vacuum casting induction, alloy casting property, its elasticity and ancillary body dynamic compatibility, strength, corrosion resistance It is possible to provide a TiNi-based medical alloy having improved properties suitable for use in medical applications, such as weakened deformation life, increased durability.
  • the TiNi-based medical alloy of the present invention is free from foreign body reactions with biological tissues, and may be present in the human body for a longer period of time. Physical and chemical properties can provide alloys suitable for medical use.
  • the TiNi-based medical alloy of the present invention has almost no change in physical properties and thus has high transformation temperature stability, and has a low product cost of less than 5% and a relatively low production cost, compared to the existing product defect of 20-30%. Low profitability improves and is very useful not only for medical use but also for industrial use.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Materials For Medical Uses (AREA)

Abstract

La présente invention concerne un alliage médical à base de TiNi et son procédé de production. L'alliage médical à base de TiNi contient de 44 à 48 % en poids de Ti, de 0,2 à 3,0 % en poids de Mo, de 0,1 à 2,0 % en poids de Fe et de 0,2 à 1,0 % en poids d'Al, le reste étant du Ni. Ledit alliage présente des propriétés physiques et mécaniques de haut niveau ainsi que diverses caractéristiques appropriées pour une utilisation médicale.
PCT/KR2016/006987 2015-06-30 2016-06-29 Alliage médical à base de tini et son procédé de production Ceased WO2017003192A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
KR20150093252 2015-06-30
KR10-2015-0093252 2015-06-30
KR10-2016-0081466 2016-06-29
KR1020160081466A KR101832705B1 (ko) 2015-06-30 2016-06-29 TiNi계 의료용 합금 및 그 제조 방법

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WO2017003192A1 true WO2017003192A1 (fr) 2017-01-05

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08299428A (ja) * 1994-10-14 1996-11-19 Osteonics Corp 生体適合性を有するチタン系合金類からなる医療器具
JPH09302450A (ja) * 1996-02-07 1997-11-25 General Electric Co <Ge> ニッケル基超合金における結晶粒度の制御
US6187045B1 (en) * 1999-02-10 2001-02-13 Thomas K. Fehring Enhanced biocompatible implants and alloys
KR20020071451A (ko) * 2001-03-05 2002-09-12 주식회사 바이오스마트 생체재료용 다공체 조성물
JP2012514524A (ja) * 2009-01-08 2012-06-28 バイオ ディージー インコーポレイテッド 生体分解性合金を含む植込み型医療装置

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08299428A (ja) * 1994-10-14 1996-11-19 Osteonics Corp 生体適合性を有するチタン系合金類からなる医療器具
JPH09302450A (ja) * 1996-02-07 1997-11-25 General Electric Co <Ge> ニッケル基超合金における結晶粒度の制御
US6187045B1 (en) * 1999-02-10 2001-02-13 Thomas K. Fehring Enhanced biocompatible implants and alloys
KR20020071451A (ko) * 2001-03-05 2002-09-12 주식회사 바이오스마트 생체재료용 다공체 조성물
JP2012514524A (ja) * 2009-01-08 2012-06-28 バイオ ディージー インコーポレイテッド 生体分解性合金を含む植込み型医療装置

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