CN108998684A - A kind of preparation method of copper titanium-based biomaterial - Google Patents
A kind of preparation method of copper titanium-based biomaterial Download PDFInfo
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- CN108998684A CN108998684A CN201810790917.4A CN201810790917A CN108998684A CN 108998684 A CN108998684 A CN 108998684A CN 201810790917 A CN201810790917 A CN 201810790917A CN 108998684 A CN108998684 A CN 108998684A
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- 239000012620 biological material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- IUYOGGFTLHZHEG-UHFFFAOYSA-N copper titanium Chemical compound [Ti].[Cu] IUYOGGFTLHZHEG-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 239000010949 copper Substances 0.000 claims abstract description 55
- 239000010936 titanium Substances 0.000 claims abstract description 52
- 238000002844 melting Methods 0.000 claims abstract description 44
- 229910052751 metal Inorganic materials 0.000 claims abstract description 42
- 239000002184 metal Substances 0.000 claims abstract description 42
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 39
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 37
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 37
- 229910052802 copper Inorganic materials 0.000 claims abstract description 35
- 230000008018 melting Effects 0.000 claims abstract description 28
- 150000002739 metals Chemical class 0.000 claims abstract description 21
- 238000001816 cooling Methods 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 52
- 239000010955 niobium Substances 0.000 claims description 35
- 239000007789 gas Substances 0.000 claims description 30
- 229910052786 argon Inorganic materials 0.000 claims description 26
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 19
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 12
- 238000010891 electric arc Methods 0.000 claims description 12
- 230000004927 fusion Effects 0.000 claims description 12
- 229910045601 alloy Inorganic materials 0.000 claims description 11
- 239000000956 alloy Substances 0.000 claims description 11
- 238000005266 casting Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000003723 Smelting Methods 0.000 claims description 6
- 229910020018 Nb Zr Inorganic materials 0.000 claims description 4
- 239000004615 ingredient Substances 0.000 claims description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 239000000284 extract Substances 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 229910001069 Ti alloy Inorganic materials 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 11
- 230000006835 compression Effects 0.000 abstract description 7
- 238000007906 compression Methods 0.000 abstract description 7
- 210000000988 bone and bone Anatomy 0.000 abstract description 6
- 239000007943 implant Substances 0.000 abstract description 5
- 210000001519 tissue Anatomy 0.000 abstract description 4
- 208000015181 infectious disease Diseases 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000000844 anti-bacterial effect Effects 0.000 abstract 1
- 239000003519 biomedical and dental material Substances 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 230000001954 sterilising effect Effects 0.000 abstract 1
- 238000004659 sterilization and disinfection Methods 0.000 abstract 1
- 238000006467 substitution reaction Methods 0.000 abstract 1
- 238000002054 transplantation Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 14
- 230000003115 biocidal effect Effects 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 229910052737 gold Inorganic materials 0.000 description 7
- 239000010931 gold Substances 0.000 description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 6
- 238000003760 magnetic stirring Methods 0.000 description 4
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 3
- 229910001431 copper ion Inorganic materials 0.000 description 3
- 238000002513 implantation Methods 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 229910004353 Ti-Cu Inorganic materials 0.000 description 2
- ORNYFRDWFROROD-UHFFFAOYSA-N [Nb].[Zr].[Ti].[Cu] Chemical compound [Nb].[Zr].[Ti].[Cu] ORNYFRDWFROROD-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000002763 biomedical alloy Substances 0.000 description 2
- 239000005548 dental material Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000005468 ion implantation Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 238000013019 agitation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007499 fusion processing Methods 0.000 description 1
- 230000035876 healing Effects 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 230000002980 postoperative effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000001356 surgical procedure Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
Classifications
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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
-
- 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
- A61L27/02—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
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/54—Biologically active materials, e.g. therapeutic substances
-
- 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
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
-
- 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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
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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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Veterinary Medicine (AREA)
- Epidemiology (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Animal Behavior & Ethology (AREA)
- Dermatology (AREA)
- Public Health (AREA)
- Transplantation (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a kind of preparation methods of copper titanium-based biomaterial, belong to bio-medical material preparation field.The method of the invention are as follows: press Ti:41~80%, Nb:15% ~ 34%, Zr:8% ~ 15%, the mass percent of Cu:2% ~ 10% weighs the ingot of Ti, Nb, Zr and Cu respectively；First by higher melting-point Ti, Nb, Zr ingot melting, the then melting together with the ingot of Cu, furnace cooling is to obtain Ti-Nb-Zr-Cu cast metals.The compression strength that antibacterial titanium alloy biomaterial is prepared in the present invention is 970~1400MPa, and elasticity modulus is 35~58GPa, close to people's bone elasticity modulus (10 ~ 30GPa)；Containing sterilization element Cu in implant, the infection during transplant operation transplantation can be prevented, can be used for human body hard tissue substitution and is repaired；It is this preparation process cleaning, simple process, low in cost, it is easy to accomplish industrialized production.
Description
Technical field
The present invention relates to a kind of preparation methods of copper titanium-based biomaterial, belong to technical field of biological medical material preparation.
Background technique
With the booming and important breakthrough of biotechnology, titanium or titanium alloy is because have preferable mechanical property excellent
Gesture: density is low, light, corrosion resistance, nonmagnetic, good toughness, and is widely used in bio-medical field, and biomedical titanium closes
The demand therefore rapid growth of gold, however, many pure titanium or titanium alloy find to still have many in actual medical procedure
Problem leads to disease since V and Al is there are toxic and pathogenic in the medical titanium alloys such as the pure Ti being widely used and TC4
People generates poisoning and infection phenomenons, document (M Kikuchi, M Takahashi, O Okuno.Elastic moduli after surgery
Of cast Ti-Au, Ti-Ag, and Ti-Cu alloys. " Dental Materials ", 2006,22, (7): 641-
646) antibiotic property elemental copper is added in high-purity titanium by the method for vacuum arc melting, obtained biomaterial has good
Antibiotic property, but with the increase of copper content, the elasticity modulus of alloy is also increasing, and the elasticity modulus of pure titanium is about
110GPa, when copper content increases to 10%, the elasticity modulus of alloy is about 120GPa, is unfavorable for as medical implant
Stress transfer between bone and bone is easy to produce " stress shielding " phenomenon, on the other hand, the intensity of pure titanium, plasticity_resistant deformation energy
Power, resistance fracture energy are lower, to limit the use as its implant at larger carrying position.
A large amount of research has been expanded for the antibiotic property and mechanical property that improve biomaterial at present.Document
(Masatoshi TAKAHASHI, Masafumi KIKUCHI, Yukyo TAKADA, samu OKUNO. Mechanical
Properties and Microstructures of Dental Cast Ti-Ag and Ti-Cu Alloys. Dental
Materials Journal 21 (3): 270-280,20) it joined antibiotic property elemental copper and silver in pure titanium, had
There is the titanium alloy biomaterial of whole antibiotic property and excellent mechanical performances, but this biomaterial still remains elasticity modulus
The high and bad problem of people's bone biocompatibility, patent CN201610239281.5 using plasma immersion ion injection/plating
Membrane technology forms copper ion implantation layer in medical titanium base material surface injection copper ion, so that medical titanium base material be made to be provided with
Antibiotic property can be widely used in various titanium alloy devices used in the clinical treatments fields such as orthopaedics implantation, replacement and joint prosthesis
Tool solves the problems, such as to bring pain to patient because titanium alloy implant causes infection in clinical treatment.Foregoing invention
Although the material being related to joined Cu ion to improve the antibiotic property of material, but between the extension and bone tissue of time
Friction, be formed by copper ion implantation layer can generate fall off, wear phenomenon, to reduce the antibiotic property and use of implant
Service life, and the elasticity modulus of biomaterial obtained by foregoing invention is higher, is easy to produce " stress shielding " phenomenon.
Summary of the invention
The object of the invention is that providing a kind of preparation method of copper titanium-based biomaterial, artificial implantation is further increased
Organization mechanics performance and antibiotic property solve between implantation material and bone tissue because binding force is poor, biocompatibility is low and postoperative sense
Dye causes bone tissue to be difficult to grow, healing problems, specifically includes the following steps:
(1) press Ti:41~80%, Nb:15% ~ 34%, Zr:8% ~ 15%, the mass percent of Cu:2% ~ 10%, weigh respectively Ti, Nb,
The ingot of Zr and Cu, vacuum drying are spare.
(2) gained Ti, Nb, Zr ingot in step (1) is put into a molten bath of arc-melting furnace, by Cu ingot
It is put into another molten bath of arc-melting furnace, the chamber of shield arc smelting furnace is simultaneously evacuated to 1 × 10-3~1×10-4Pa,
High-purity argon gas is then charged with to 0.06 ~ 0.04MPa；The striking under high-purity argon gas atmosphere, adjusting fusion current are 250A ~ 350A,
Magnetic stir current be 10 ~ 15A, first melting Ti, Nb, Zr ingot, overturn molten metal ingot casting, melt back 4 ~ 6 times, to gold
Category is completely melt and closes electric arc after being sufficiently mixed uniformly, and furnace cooling obtains the uniform Ti-Nb-Zr alloy of ingredient.
(3) the resulting Ti-Nb-Zr alloy cast ingot of step (2) is put into the molten bath for placing Cu ingot, is then vacuumized
To 1 × 10-3~1×10-4Pa extracts exhaust gas caused by melting Ti, Nb, Zr ingot out, be filled with high-purity argon gas to 0.06 ~
0.04MPa；The striking under high-purity argon gas atmosphere adjusts fusion current in 180A ~ 250A, and magnetic stir current is 10 ~ 15A, repeatedly
Melting closes electric arc after metal is completely melt and is sufficiently mixed uniformly, and resulting cast metals are cold with furnace under an inert atmosphere
But to taking out after room temperature, Ti-Nb-Zr-Cu cast metals are obtained.
Preferably, the purity of titanium block of the present invention is 99.995%, the purity of niobium metal ingot is 99.95%, zirconium ingot
Purity be 99.5%, the purity of copper metal ingot is 99.995%.
Preferably, the purity of argon being filled in step (2) of the present invention and step (3) is 99.999%.
The invention has the benefit that
(1) the method for the invention preparation process carried out under high vacuum environment and melted ingot casting under vacuum conditions with
Furnace is cooled to room temperature, so that raw material be prevented to contact with air and generate oxidation, ensure that experimental result accuracy and can
By property.
(2) the method for the invention is in fusion process, first higher melting-point Ti, Nb, Zr ingot of melting, then with Cu
Ingot melting together, using high current fusing and electromagnetic agitation and repeatedly overturning ingot casting carry out melting, advantageous fusing point compared with
The homogenization of high niobium element and zr element.
(3) cupric titanium-base alloy biomaterial is prepared with ingredient and even tissue, compression strength using the method for the present invention
The features such as higher (970 ~ 1400MPa), elasticity modulus low (35 ~ 58GPa), this both facilitates the biofacies for improving medical titanium
Capacitive.
(4) Cu that cupric titanium-base alloy biomaterial is added to 2 ~ 10% is prepared using the method for the present invention, this measure is greatly
While improving the antibiotic property of biological medical titanium alloy, the springform for being added to the titanium alloy biomaterial of 10% Cu is also allowed
Amount maintains 58GPa.
The method of the present invention simple process, operation are convenient, low in cost, it is easy to accomplish industrialized production.
Detailed description of the invention
The XRD diffracting spectrum of Ti-30Nb-15Zr-15Cu biomaterial in Fig. 1 embodiment of the present invention 4；
Ti-30Nb-15Zr-15Cu biomaterial metallurgical microscopic in Fig. 2 embodiment of the present invention 4；
Ti-30Nb-15Zr-15Cu biomaterial SEM pattern in Fig. 3 embodiment of the present invention 4.
Specific embodiment
Invention is further described in detail in the following with reference to the drawings and specific embodiments, but protection scope of the present invention is simultaneously
It is not limited to the content.
Embodiment 1
(1) press Ti:75%, Nb:15%, Zr:8%, the mass percent of Cu:2%, weigh respectively purity be 99.995%, 99.95%,
The ingot of 99.5% and 99.995% Ti, Nb, Zr, Cu are respectively put into vacuum oven, spare.
(2) it is put into a water jacketed copper crucible of arc-melting furnace by Ti, Nb, Zr ingot obtained by step (1), by Cu gold
Belong to ingot to be put into another water jacketed copper crucible of arc-melting furnace, the chamber of shield arc smelting furnace is simultaneously evacuated to 1 × 10- 3Pa is then charged with high-purity argon gas to 0.05MPa；The striking under high-purity argon gas atmosphere adjusts fusion current in 250A, magnetic stirring
Electric current is 10A, first melting Ti, Nb, Zr ingot, overturning molten metal ingot casting, melt back 4 times, it is ensured that melting is uniform；To
Metal is completely melt and closes electric arc after being sufficiently mixed uniformly.
(3) step (2) resulting cast metals are ploughed under to the water for placing Cu ingot by the mechanical arm of arc-melting furnace
In cold copper crucible, it is then evacuated to 1 × 10-3Exhaust gas caused by melting Ti, Nb, Zr ingot is extracted out, is filled with high-purity by Pa
Argon gas is to 0.05MPa；The striking under high-purity argon gas atmosphere adjusts fusion current in 180A, and magnetic stir current is 10A, and overturning is molten
The cast metals of change, melt back 5 times, it is ensured that melting is uniform；Electric arc is closed after metal is completely melt and is sufficiently mixed uniformly.
(4) it is taken out after cooling to step (3) resulting cast metals with the furnace room temperature under an inert atmosphere, obtains button-type
Cast metals；
The Ti-15Nb-8Zr-2Cu mechanics of biomaterials performance that the present embodiment is prepared obtains after tested: elasticity modulus 58GPa,
The intensity of compression strength 970MPa, material are higher, and elasticity modulus is lower, meet the mechanical compatibility requirement of transplant.
Embodiment 2
(1) press Ti:55%, Nb:34%, Zr:6%, the mass percent of Cu:5%, weigh respectively purity be 99.995%, 99.95%,
The ingot of 99.5% and 99.995% Ti, Nb, Zr, Cu are respectively put into vacuum oven, spare.
(2) it is put into a water jacketed copper crucible of arc-melting furnace by Ti, Nb, Zr ingot obtained by step (1), by Cu gold
Belong to ingot to be put into another water jacketed copper crucible of arc-melting furnace, the chamber of shield arc smelting furnace is simultaneously evacuated to 1 × 10- 3Pa is then charged with high-purity argon gas to 0.04MPa；The striking under high-purity argon gas atmosphere adjusts fusion current in 300A, magnetic stirring
Electric current is 12A, first melting Ti, Nb, Zr ingot, overturning molten metal ingot casting, melt back 5 times, it is ensured that melting is uniform；To
Metal is completely melt and closes electric arc after being sufficiently mixed uniformly.
(3) step (2) resulting cast metals are ploughed under to the water for placing Cu ingot by the mechanical arm of arc-melting furnace
In cold copper crucible, it is then evacuated to 1 × 10-3Exhaust gas caused by melting Ti, Nb, Zr ingot is extracted out, is filled with high-purity by Pa
Argon gas is to 0.04MPa；The striking under high-purity argon gas atmosphere adjusts fusion current in 220A, and magnetic stir current is 12A, and overturning is molten
The cast metals of change, melt back 5 times, it is ensured that melting is uniform；Electric arc is closed after metal is completely melt and is sufficiently mixed uniformly.
(4) it is taken out after cooling to step (3) resulting cast metals with the furnace room temperature under an inert atmosphere, obtains button-type
Cast metals.
The Ti-34Nb-6Zr-5Cu mechanics of biomaterials performance that the present embodiment is prepared obtains after tested: elasticity modulus
The intensity of 35GPa, compression strength 1080MPa, material are higher, and elasticity modulus is lower, and the mechanical compatibility for meeting transplant is wanted
It asks.
Embodiment 3
(1) press Ti:53%, Nb:25%, Zr:15%, the mass percent of Cu:7%, weigh respectively purity be 99.995%, 99.95%,
The ingot of 99.5% and 99.995% Ti, Nb, Zr, Cu are respectively put into vacuum oven, spare.
(2) it is put into a water jacketed copper crucible of arc-melting furnace by Ti, Nb, Zr ingot obtained by step (1), by Cu gold
Belong to ingot to be put into another water jacketed copper crucible of arc-melting furnace, the chamber of shield arc smelting furnace is simultaneously evacuated to 1 × 10- 4Pa is then charged with high-purity argon gas to 0.05MPa；The striking under high-purity argon gas atmosphere adjusts fusion current in 320A, magnetic stirring
Electric current is 12A, first melting Ti, Nb, Zr ingot, overturning molten metal ingot casting, melt back 5 times, it is ensured that melting is uniform；To
Metal is completely melt and closes electric arc after being sufficiently mixed uniformly.
(3) step (2) resulting cast metals are ploughed under to the water for placing Cu ingot by the mechanical arm of arc-melting furnace
In cold copper crucible, it is then evacuated to 1 × 10-4Exhaust gas caused by melting Ti, Nb, Zr ingot is extracted out, is filled with high-purity by Pa
Argon gas is to 0.05MPa；The striking under high-purity argon gas atmosphere adjusts fusion current in 250A, and magnetic stir current is 12A, and overturning is molten
The cast metals of change, melt back 5 times, it is ensured that melting is uniform；Electric arc is closed after metal is completely melt and is sufficiently mixed uniformly.
(4) it is taken out after cooling to step (3) resulting cast metals with the furnace room temperature under an inert atmosphere, obtains button-type
Cast metals.
The Ti-25Nb-15Zr-7Cu mechanics of biomaterials performance that the present embodiment is prepared obtains after tested: elasticity modulus
The intensity of 54GPa, compression strength 1280MPa, material are higher, and elasticity modulus is lower, and the mechanical compatibility for meeting transplant is wanted
It asks.
Embodiment 4
(1) press Ti:45%, Nb:30%, Zr:15%, the mass percent of Cu:10%, weigh respectively purity be 99.995%,
99.95%, the ingot of 99.5% and 99.995% Ti, Nb, Zr, Cu is respectively put into vacuum oven, spare.
(2) it is put into a water jacketed copper crucible of arc-melting furnace by Ti, Nb, Zr ingot obtained by step (1), by Cu gold
Belong to ingot to be put into another water jacketed copper crucible of arc-melting furnace, the chamber of shield arc smelting furnace is simultaneously evacuated to 1 × 10- 4Pa is then charged with high-purity argon gas to 0.06MPa；The striking under high-purity argon gas atmosphere adjusts fusion current in 350A, magnetic stirring
Electric current is 15A, first melting Ti, Nb, Zr ingot, overturning molten metal ingot casting, melt back 6 times, it is ensured that melting is uniform；To
Metal is completely melt and closes electric arc after being sufficiently mixed uniformly.
(3) step (2) resulting cast metals are ploughed under to the water for placing Cu ingot by the mechanical arm of arc-melting furnace
In cold copper crucible, it is then evacuated to 1 × 10-4Exhaust gas caused by melting Ti, Nb, Zr ingot is extracted out, is filled with high-purity by Pa
Argon gas is to 0.06MPa；The striking under high-purity argon gas atmosphere adjusts fusion current in 250A, and magnetic stir current is 15A, and overturning is molten
The cast metals of change, melt back 6 times, it is ensured that melting is uniform；Electric arc is closed after metal is completely melt and is sufficiently mixed uniformly.
(4) it is taken out after cooling to step (3) resulting cast metals with the furnace room temperature under an inert atmosphere, obtains button-type
Cast metals.
The XRD diffracting spectrum of the Ti-30Nb-15Zr-10Cu biomaterial that the present embodiment is prepared as shown in Figure 1, by
Figure is it can be seen that be mainly α-Ti matrix, β-Ti matrix, CuZr, CuTi3 and Nb phase in tissue；,.
The Ti-30Nb-15Zr-10Cu biomaterial metallurgical microscopic that the present embodiment is prepared is as shown in Fig. 2, can by figure
To find out occurring apparent precipitated phase in Ti-30Nb-15Zr-10Cu biomedical alloy material, precipitated phase is in reticular structure；
Ti-30Nb-15Zr-10Cu biomaterial SEM shape appearance figure that the present embodiment is prepared is as shown in figure 3, Ti- as seen from the figure
The reticular structure of 30Nb-15Zr-10Cu biomedical alloy material interlinks together, enhances the toughness of material and strong
Degree, wherein white precipitated phase may be β-Ti, conversion of the α-Ti to β-Ti can substantially reduce Ti-30Nb-15Zr-10Cu biology
The elasticity modulus of material.
The Ti-30Nb-15Zr-10Cu mechanics of biomaterials performance that the present embodiment is prepared obtains after tested: elasticity modulus
The intensity of 46GPa, compression strength 1400MPa, material are higher, and elasticity modulus is lower, and the mechanical compatibility for meeting transplant is wanted
It asks.
According to embodiment interpretation of result, titanium alloy biomaterial is provided with excellent antibiotic property after copper is added, this
It lifts while the antibiotic property for significantly improving biological medical titanium alloy, also allows the titanium alloy for being added to 2 ~ 10% Cu biological
The elasticity modulus of material maintains 35 ~ 58GPa；Meanwhile with the increase of niobium and zirconium content, the resistance to compression of titanium niobium zirconium copper biomaterial
Intensity can be raised to 1400MPa；The obtained titanium niobium zirconium copper biomaterial of the invention patent has ingredient and even tissue, mechanics
It has excellent performance the advantages that excellent with antibiotic property.
Claims (3)
1. a kind of preparation method of copper titanium-based biomaterial, which is characterized in that specifically includes the following steps:
(1) press Ti:41~80%, Nb:15% ~ 34%, Zr:8% ~ 15%, the mass percent of Cu:2% ~ 10%, weigh respectively Ti, Nb,
The ingot of Zr and Cu, vacuum drying are spare；
(2) gained Ti, Nb, Zr ingot in step (1) is put into a molten bath of arc-melting furnace, Cu ingot is put into
In another molten bath of arc-melting furnace, the chamber of shield arc smelting furnace is simultaneously evacuated to 1 × 10-3~1×10-4Pa, then
High-purity argon gas is filled with to 0.06 ~ 0.04MPa；The striking under high-purity argon gas atmosphere, adjusting fusion current are 250A ~ 350A, and magnetic stirs
Mixing electric current is 10 ~ 15A, and first melting Ti, Nb, Zr ingot overturns molten metal ingot casting, melt back 4 ~ 6 times, complete to metal
Running down is simultaneously sufficiently mixed uniformly rear closing electric arc, the furnace cooling acquisition uniform Ti-Nb-Zr alloy of ingredient；
(3) the resulting Ti-Nb-Zr alloy cast ingot of step (2) is put into the molten bath for placing Cu ingot, is then evacuated to 1
×10-3~1×10-4Pa extracts exhaust gas caused by melting Ti, Nb, Zr ingot out, be filled with high-purity argon gas to 0.06 ~
0.04MPa；The striking under high-purity argon gas atmosphere adjusts fusion current in 180A ~ 250A, and magnetic stir current is 10 ~ 15A, repeatedly
Melting closes electric arc after metal is completely melt and is sufficiently mixed uniformly, and resulting cast metals are cold with furnace under an inert atmosphere
But to taking out after room temperature, Ti-Nb-Zr-Cu cast metals are obtained.
2. according to the preparation method of right copper titanium-based biomaterial, it is characterised in that: the purity of titanium block is 99.995%, niobium metal
The purity of ingot is 99.95%, the purity of zirconium ingot is 99.5%, the purity of copper metal ingot is 99.995%.
3. the preparation method of cupric titanium-base alloy biomaterial according to claim 1, it is characterised in that: step (2) and step
Suddenly the purity of argon being filled in (3) is 99.999%.
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| CN109602957A (en) * | 2018-12-19 | 2019-04-12 | 云南大学 | A kind of bio-medical porous titanium niobium copper orthopedic implanting material and its preparation method and application |
| CN111020342A (en) * | 2019-12-27 | 2020-04-17 | 昆明理工大学 | Method for preparing antibacterial titanium alloy through deformation strengthening |
| CN112846172A (en) * | 2021-01-08 | 2021-05-28 | 江西理工大学 | Biomedical titanium-copper microsphere integrated microsphere powder, biomedical titanium-copper alloy and preparation process |
| CN113755718A (en) * | 2021-06-02 | 2021-12-07 | 北京航空航天大学 | TiZrNbCuAg antibacterial alloy and preparation method thereof |
| CN114470317A (en) * | 2022-01-21 | 2022-05-13 | 江苏科技大学 | Titanium alloy material for repairing skull and preparation method thereof |
| CN114875293A (en) * | 2022-04-14 | 2022-08-09 | 湖南大学 | Ti-Zr-Nb-Ta-Cu high-entropy alloy, preparation method thereof and application thereof in medical antibacterial material |
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| CN109602957A (en) * | 2018-12-19 | 2019-04-12 | 云南大学 | A kind of bio-medical porous titanium niobium copper orthopedic implanting material and its preparation method and application |
| CN111020342A (en) * | 2019-12-27 | 2020-04-17 | 昆明理工大学 | Method for preparing antibacterial titanium alloy through deformation strengthening |
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| CN112846172B (en) * | 2021-01-08 | 2022-10-25 | 江西理工大学 | Biomedical titanium-copper microsphere integrated microsphere powder, biomedical titanium-copper alloy and preparation process |
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| CN114470317A (en) * | 2022-01-21 | 2022-05-13 | 江苏科技大学 | Titanium alloy material for repairing skull and preparation method thereof |
| CN114875293A (en) * | 2022-04-14 | 2022-08-09 | 湖南大学 | Ti-Zr-Nb-Ta-Cu high-entropy alloy, preparation method thereof and application thereof in medical antibacterial material |
| CN116144981A (en) * | 2023-02-21 | 2023-05-23 | 昆明理工大学 | Stable beta-phase-containing titanium alloy cast ingot and preparation method thereof |
| CN116144981B (en) * | 2023-02-21 | 2024-02-27 | 昆明理工大学 | Stable beta-phase-containing titanium alloy cast ingot and preparation method thereof |
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Application publication date: 20181214 |