WO2011071304A2 - 마그네슘 합금 - Google Patents

마그네슘 합금 Download PDF

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Publication number
WO2011071304A2
WO2011071304A2 PCT/KR2010/008725 KR2010008725W WO2011071304A2 WO 2011071304 A2 WO2011071304 A2 WO 2011071304A2 KR 2010008725 W KR2010008725 W KR 2010008725W WO 2011071304 A2 WO2011071304 A2 WO 2011071304A2
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WO
WIPO (PCT)
Prior art keywords
magnesium
magnesium alloy
alloy
phase
formula
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Application number
PCT/KR2010/008725
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English (en)
French (fr)
Korean (ko)
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WO2011071304A3 (ko
Inventor
구자교
석현광
양석조
김유찬
조성윤
김종택
Original Assignee
유앤아이 주식회사
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by 유앤아이 주식회사 filed Critical 유앤아이 주식회사
Priority to EP10836199.9A priority Critical patent/EP2511390A4/de
Priority to JP2012541957A priority patent/JP5894079B2/ja
Priority to CN201080055372.4A priority patent/CN102648300B/zh
Priority to US13/511,891 priority patent/US20120269673A1/en
Priority to AU2010328809A priority patent/AU2010328809B2/en
Publication of WO2011071304A2 publication Critical patent/WO2011071304A2/ko
Publication of WO2011071304A3 publication Critical patent/WO2011071304A3/ko
Priority to US15/373,538 priority patent/US9943625B2/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
    • A61L27/047—Other specific metals or alloys not covered by A61L27/042 - A61L27/045 or A61L27/06
    • 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
    • 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
    • C22C23/00—Alloys based on magnesium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C22C23/06—Alloys based on magnesium with a rare earth metal as the next major constituent

Definitions

  • the present invention relates to a magnesium alloy.
  • Magnesium alloys are easy to mold, but have disadvantages of poor corrosion resistance and strength.
  • research for appropriately changing the composition of magnesium alloys is continued.
  • the study found that the mechanical strength is improved as the amount of added element increases.
  • the amount of added element increases, several phases are created, and the larger the electrical potential difference between them, the more the galvanic circuit that increases the corrosion rate is changed to a condition that is easy to form.
  • the present invention includes magnesium (Mg) and hetero elements other than the magnesium (Mg), includes a magnesium phase, and a phase consisting of magnesium and hetero elements, the magnesium phase, the magnesium and hetero atoms
  • a magnesium alloy with controlled corrosion characteristics characterized in that the difference in electrical potential between the phases of the element is between 0 seconds and 0.2V or less.
  • the present invention is characterized in that the electrical potential difference between the magnesium phase and the phase composed of magnesium and hetero elements is reduced to 0 seconds or less by adding a third element to the magnesium alloy composed of magnesium and hetero elements. It provides a method for producing a magnesium alloy controlled corrosion properties.
  • Magnesium alloy of the present invention can control the corrosion characteristics by using the electrical potential difference between magnesium and hetero elements.
  • the magnesium alloy of the present invention can also control the corrosion resistance and strength characteristics through a post-treatment process.
  • magnesium alloys can be utilized throughout the industrial and medical fields.
  • Example 2 is a graph measuring the strength of the magnesium alloy of Example 1, Example 2 and Comparative Example 1.
  • Example 3 is a graph measuring the strength of the magnesium alloy of Example 3, Example 4 and Comparative Example 2.
  • FIG. 4 is a photograph showing before and after the surface treatment of Example 2.
  • FIG. 5 is a graph showing the open circuit potential over time of magnesium of Examples 5 to 9 and Comparative Example 1;
  • 6 is a graph showing the amount of hydrogen generated according to the amount of zinc.
  • the magnesium alloy of the present invention is a magnesium alloy with controlled corrosion characteristics, and includes magnesium (Mg) and hetero elements other than the magnesium (Mg), and has a magnesium phase and a phase composed of magnesium and hetero elements. Include.
  • the difference in electrical potential between the magnesium phase and the phase composed of magnesium and hetero elements is greater than 0 and 0.2V or less, and the closer to zero, the more preferable. If the above-mentioned range is satisfied, the decomposition rate of the magnesium alloy is very low, and thus it is easy to utilize in the industrial and medical fields. And the corrosion resistance and strength of a magnesium alloy become excellent.
  • the hetero element is not particularly limited as long as it satisfies the above-described range of difference in electrical potential between the magnesium phase and the phase composed of magnesium and the hetero element.
  • the heterogeneous elements include calcium (Ca), iron (Fe), manganese (Mn), cobalt (Co), nickel (Ni), chromium (Cr), copper (Cu), cadmium (Cd), and zirconium (Zr).
  • the magnesium alloy satisfies the difference in electrical potential between the magnesium phase and the phase consisting of magnesium and hetero elements, it is preferably represented by the following formula (1).
  • Ti titanium
  • strontium Sr
  • Cr chromium
  • Mn manganese
  • Zn zinc
  • silicon Si
  • P nickel
  • Fe iron
  • the magnesium alloy of the present invention can determine the amount of Ca and X within the above-described range in consideration of the required strength and the rate of extinction of the filling metal.
  • X contains nickel (Ni). Nickel reduces the toxicity of magnesium alloys and facilitates corrosion rate control. At this time, the content of nickel is preferably 100ppm or less, more preferably 50ppm or less.
  • the iron content is preferably 1,000 ppm or less, and more preferably 500 ppm or less. At this time, if the iron content is included in the above range, the iron is not fixed to the magnesium is present as an independent factor to increase the corrosion rate of the magnesium alloy.
  • the magnesium alloy satisfies the difference in electrical potential between the magnesium phase and the phase composed of magnesium and heteroatoms, it is preferably represented by the following formula (2).
  • the magnesium alloy represented by the formula (2) the total weight, calcium (Ca) is greater than 0 to 23% by weight or less; Y is greater than 0 and less than or equal to 10 weight percent; And magnesium (Mg).
  • Y is Mn or Zn.
  • magnesium alloy represented by Chemical Formula 2 satisfies the above-described range, it is possible to provide a magnesium alloy in which mechanical properties and corrosion resistance are improved at the same time, and brittle fracture does not occur.
  • the magnesium alloy represented by the formula (2) is based on the total weight, the calcium (Ca) is preferably more than 0 to 23% by weight, Y is 0.1 to 5% by weight and magnesium (Mg) preferably comprises a residual amount.
  • the calcium (Ca) is more preferably 0 to 23% by weight or less, Y is 0.1 to 3% by weight and Mg more preferably contains the remaining amount. The reason for this is that in view of the possible side effects of impurities, if the same corrosion rate is achieved, it is advantageous that the content of impurities is small.
  • the magnesium alloy satisfies the difference in electrical potential between the magnesium phase and the phase composed of magnesium and heteroatoms, it is preferably represented by the following formula (3).
  • Z is more than 0 and 40% by weight or less based on the total weight;
  • Magnesium (Mg) contains the balance.
  • Z is manganese (Mn), cobalt (Co), nickel (Ni), chromium (Cr), copper (Cu), cadmium (Cd), zirconium (Zr), silver (Ag), gold (Au) ), Palladium (Pd), platinum (Pt), lithium (Re), iron (Fe), zinc (Zn), molybdenum (Mo), niobium (Nb), tantalum (Ta), titanium (Ti), strontium (Sr) ), Silicon (Si), phosphorus (P) and selenium (Se).
  • the magnesium alloy is subjected to a surface treatment.
  • the surface treatment is preferably shot peening.
  • the magnesium alloy included in the implant of the present invention can perform a surface coating.
  • corrosion products may be generated on the surface of the magnesium alloy, thereby delaying the decomposition rate.
  • the surface coating may be performed with a ceramic and / or a polymer.
  • the surface coating with ceramic will be described.
  • the surface of the magnesium alloy may be coated with a corrosion product.
  • the corrosion product is a ceramic
  • the ceramic may be magnesium oxide, calcium phosphate.
  • it may be further coated with a polymer.
  • the type of the polymer is the same as that of the polymer described later.
  • the polymer used to coat the surface of the magnesium alloy with a polymer is not particularly limited as long as it is used in the art.
  • the polymer is poly (L-lactide), poly (glycolide), poly (DL-lactide), poly (dioxanone), poly (DL-lactide-co L-lactide), poly (DL-lactide-co-glycolide ), poly (glycolide-co-trimethylene carbonate), poly (L-lactide-co-glycolide), poly (e-caprolactone) or polymers thereof.
  • the magnesium alloy according to the present invention may be variously changed depending on the use. For example, it may be utilized by coating on surfaces of ceramics, metals, polymers, and the like. In addition, the magnesium alloy according to the present invention can be utilized in combination with magnesium and dissimilar metals, ceramics or polymers.
  • the present invention is characterized in that the electrical potential difference between the magnesium phase and the phase composed of magnesium and hetero elements is reduced to 0 seconds or less by adding a third element to the magnesium alloy composed of magnesium and hetero elements. It provides a method for producing a magnesium alloy controlled corrosion properties.
  • the magnesium alloy is preferably an alloy containing magnesium and calcium. It is preferable that a said 3rd element is zinc.
  • Method for producing a magnesium alloy for controlling the corrosion characteristics according to the present invention may include a) providing the magnesium alloy, b) molding the magnesium alloy.
  • the step a) is a step of melting and providing the magnesium.
  • step a) may be a step of melting and providing the magnesium in an inert gas atmosphere or in a vacuum atmosphere such as argon (Ar) that does not react with magnesium.
  • the magnesium may be melted using various methods such as resistance heating, which generates heat by applying electricity to the resistor, induction heating by flowing a current through an induction coil, or by laser or focused light. It may be a step of providing.
  • the resistance heating method of the above-described melting method is the most economical. It is preferable to stir the molten alloy (hereinafter, molten metal) so that impurities can be mixed well when melting magnesium.
  • Step b) included in the method for producing a magnesium alloy of the present invention may be a step of molding the molten magnesium alloy into at least one selected from the group consisting of a cooling method, an extrusion method, and a metal processing method.
  • the said cooling method can be used for the purpose of improving the mechanical strength of a magnesium alloy.
  • a method of immersing the crucible containing molten magnesium in water may be used.
  • a cooling method of spraying the molten magnesium using an inert gas such as argon may be used.
  • the spraying cooling method can be cooled at a much higher rate to show very fine texture.
  • the extrusion method is used for the purpose of making the structure of magnesium uniform and improving mechanical performance. Due to the extrusion method it is possible to control the strength characteristics and corrosion resistance of the magnesium alloy of the present invention.
  • the extrusion method is preferably made at 300 to 450 °C.
  • the extrusion of the magnesium may be carried out within 10: 1 to 30: 1 reduction ratio (extrusion ratio) before and after extrusion.
  • the extrusion ratio increases, the microstructure of the extrusion material becomes uniform, and there is an advantage in that defects formed during casting are easily removed. In this case, it is preferable to increase the extrusion device capacity.
  • the metal processing method is not particularly limited as long as it is a metal processing method known in the art.
  • the molten magnesium is poured directly into a mold processed in a form close to the final product, manufactured by an intermediate material such as a rod or plate, and then milled or milled, and a large amount of magnesium alloy is used. And a method of producing the final product shape by pressing forging with a force.
  • the components were mixed in the composition shown in Table 1, and charged in a crucible having an internal diameter of 50 mm made of stainless steel (SUS 410). Subsequently, argon (Ar) gas was flowed around the crucible so that magnesium in the crucible did not come into contact with air, and the crucible temperature was raised from about 700 ° C. to 750 ° C. using a resistance furnace to melt magnesium. The crucible was shaken and stirred so that the molten magnesium and impurities could be mixed well. The molten magnesium was cooled to produce magnesium in the solid state. In addition, when cooling, the crucible was immersed in water (20 ° C.) for the purpose of improving the mechanical strength of magnesium, so that the molten magnesium was cooled rapidly to prepare a magnesium alloy.
  • argon (Ar) gas was flowed around the crucible so that magnesium in the crucible did not come into contact with air, and the crucible temperature was raised from about 700 ° C. to 750 °
  • Example 1 The magnesium alloys of Example 1, Example 2 and Comparative Example 1 were extruded. At this time, the extrusion temperature was carried out in the range of 370 ⁇ 375 °C, the cross-sectional area reduction ratio (extrusion ratio) before and after extrusion was fixed to 15: 1.
  • the extruded magnesium alloys of Example 1 and Ex. 2 were extruded from the magnesium alloys of Example 3 and Example 2.
  • the extruded magnesium alloys of Example 4 and Comparative Example 1 were referred to as Comparative Example 2.
  • the corrosion rate of the magnesium alloy is measured by the amount of hydrogen generated when the magnesium alloy is immersed in the solution of Table 2 below. This is because hydrogen is generated when magnesium is biodegraded, because the solution of Table 2 is the same conditions as the living body, that is, the biosimulation solution.
  • the corrosion characteristics of the magnesium alloy were significantly different due to the added element and the extrusion. Through this, it can be seen that the magnesium alloy can control various decomposition rates according to the added element and the post-treatment method.
  • the magnesium alloys of Examples 1 to 4, Comparative Example 1 and Comparative Example 2 were subjected to electric discharge machining to form a diameter of 3 mm and a length of 6 mm.
  • the lower and upper surfaces of the discharged specimens were polished with 1000 times emery paper to level the surfaces.
  • the machined test specimen was placed horizontally on a jig made of cemented carbide (tungsten carbide), and then a force was applied from the direction of the specimen using a head of a compression tester with a maximum load of 20 tons. At this time, the vertical descending speed of the head was set to 10-4 / s.
  • the deformation amount and the compressive stress change amount were recorded in real time using an extensometer and a stress cell mounted on the compression tester. At this time, the size of the specimen was small, so that the strain gauge was mounted on the jig of the tester which pressed the specimen rather than the specimen, and was measured larger than the actual deformation of the specimen.
  • Example 2 is a graph measuring the strength of the magnesium alloy of Example 1, Example 2 and Comparative Example 1.
  • 3 is a graph measuring the strength of the magnesium alloy of Example 3, Example 4 and Comparative Example 2.
  • Table 3 is a table showing the strength of the magnesium alloy of Examples 1 to 6.
  • Y.S represents yield strength
  • UCS represents ultimate compression strength.
  • Example 1 Example 2
  • Example 3 Example 4 Comparative Example 1 Comparative Example 2 Strength (MPa) YS 87 100 155 165 47 48 UCS 180 230 365 400 146 208
  • the magnesium alloys of Examples 1 to 4 according to the present invention have a short corrosion resistance property of 2 to 3 days through composition control and post-treatment process (extrusion) control. It is understood that the intensity can be controlled from 87 MPa to 400 MPa for over a year. It can be inferred that this property can be used to produce magnesium alloys that can maintain their strength in the required period.
  • the magnesium alloy of Example 2 was glossy before the surface treatment, but after the surface treatment, the magnesium alloy disappeared.
  • the magnesium alloys of Examples 5 to 9 were prepared by using the preparation method of Example 1 as components in the composition of Table 4 below.
  • Example 5 Example 6
  • Example 7 Example 8
  • Mg 2 Ca (% by weight) 93.65 95.78 97.89 99.58 100 Zn (% by weight) 6.35 4.22 2.11 0.42 0
  • FIG. 5 is a graph showing the open circuit potential over time of magnesium of Examples 5 to 9 and Comparative Example 1;
  • Comparative Example 1 and Example 5 have the smallest difference in the open circuit potential, and thus have the best corrosion resistance. However, Comparative Example 1 and Example 9 show the fastest corrosion rate because of the large difference in the open circuit potential. .
  • Test Example 5 Evaluation of biodegradation rate due to electrical potential difference
  • the corrosion rate of the magnesium alloy is measured by the amount of hydrogen generated when the magnesium alloy is immersed in the solution of Table 2.
  • the x-axis represents Zn (at%) contained in Mg 2 Ca.
  • the zinc content (x-axis) represents Zn (at%) contained in Mg 2 Ca.
  • the decomposition rate increases rapidly when the open circuit potential difference exceeds 0.2V.
  • the decomposition rate is represented by the amount of hydrogen generated.

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  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
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  • Mechanical Engineering (AREA)
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PCT/KR2010/008725 2009-12-07 2010-12-07 마그네슘 합금 WO2011071304A2 (ko)

Priority Applications (6)

Application Number Priority Date Filing Date Title
EP10836199.9A EP2511390A4 (de) 2009-12-07 2010-12-07 Magnesiumlegierung
JP2012541957A JP5894079B2 (ja) 2009-12-07 2010-12-07 マグネシウム合金
CN201080055372.4A CN102648300B (zh) 2009-12-07 2010-12-07 镁合金
US13/511,891 US20120269673A1 (en) 2009-12-07 2010-12-07 Magnesium alloy
AU2010328809A AU2010328809B2 (en) 2009-12-07 2010-12-07 Magnesium alloy
US15/373,538 US9943625B2 (en) 2009-12-07 2016-12-09 Magnesium alloy

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR10-2009-0120356 2009-12-07
KR20090120356 2009-12-07

Related Child Applications (2)

Application Number Title Priority Date Filing Date
US13/511,891 A-371-Of-International US20120269673A1 (en) 2009-12-07 2010-12-07 Magnesium alloy
US15/373,538 Division US9943625B2 (en) 2009-12-07 2016-12-09 Magnesium alloy

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WO2011071304A2 true WO2011071304A2 (ko) 2011-06-16
WO2011071304A3 WO2011071304A3 (ko) 2011-10-27

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US (2) US20120269673A1 (de)
EP (1) EP2511390A4 (de)
JP (1) JP5894079B2 (de)
KR (1) KR101470052B1 (de)
CN (1) CN102648300B (de)
AU (1) AU2010328809B2 (de)
WO (1) WO2011071304A2 (de)

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WO2011071304A3 (ko) 2011-10-27
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JP2013512346A (ja) 2013-04-11
US20120269673A1 (en) 2012-10-25
AU2010328809A1 (en) 2012-07-05
EP2511390A2 (de) 2012-10-17
US20170119922A1 (en) 2017-05-04
CN102648300A (zh) 2012-08-22
KR101470052B1 (ko) 2014-12-11
US9943625B2 (en) 2018-04-17
CN102648300B (zh) 2015-06-17
JP5894079B2 (ja) 2016-03-23

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