CN107090554A - It is a kind of to have low elastic modulus and the β type Zr Ti Nb Ta Sn systems alloy of high intensity and preparation method thereof concurrently - Google Patents
It is a kind of to have low elastic modulus and the β type Zr Ti Nb Ta Sn systems alloy of high intensity and preparation method thereof concurrently Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C16/00—Alloys based on zirconium
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Abstract
Low elastic modulus and the β type Zr Ti Nb Ta Sn systems alloy of high intensity and preparation method thereof are had concurrently the invention provides a kind of, it is prepared from using the raw material of following species and percentage by weight by alloy melting, titanium 20.5%~27.0%, niobium 3.5%~13.5%, tin 2.5%~6.5%, tantalum 0.5%~2.5%, remaining is zirconium, and the percentage by weight ＞ 50% of zirconium, β types Zr Ti Nb Ta Sn systems alloy has a crystal phase structure of single β phases, and tensile modulus of elasticity is that 38~45GPa, tensile strength are 580~620MPa.It is no cytotoxicity element that the present invention, which prepares alloy raw materials used,；The problem of elements such as Mo and V have cytotoxicity is avoided, its tensile modulus of elasticity is approximate with the modulus of elasticity of people's bone, can effectively alleviate the modulus of elasticity between implant and people's bone and mismatch the implantation failure induced；There is higher tensile strength simultaneously, the fields such as biological and medicinal implant material are can be widely applied for.
Description
Technical field
The present invention relates to biology medical material technical field, specifically a kind of low elastic modulus and high intensity of having concurrently
Bio-medical β type Zr-Ti-Nb-Ta-Sn systems alloy and preparation method thereof.
Background technology
Bio-medical material (or abbreviation biomaterial), refers to for the purpose of medical treatment, for diagnosing, treating, repair or replace
Change human tissue organ or promote the material of its function.The difference constituted according to biomaterial, can be classified as bio-medical without
Machine nonmetallic materials, bio-medical organic material, biomedical metallic material and bio-medical composition etc..Wherein, it is raw
The characteristics such as thing medical metal material with easy processing due to being molded, higher intensity, good toughness, clinically should have become
Material, such as knochenbruch combination clamping plate, orthopedic implants, various dental materials are implanted into most commonly used load.
In biomedical metallic material, titanium or titanium alloy (especially beta titanium alloy) relies on its excellent bio-compatible
Property, corrosion resistance, comprehensive mechanical property and processing performance turned into joint prosthesis (hip, knee, shoulder, ankle, elbow, wrist, articulations digitorum manus etc.),
The preferred material of the medical embedded product such as bone wound product (intramedullary nail, steel plate, screw etc.) and backbone correcting internal fixation system.So
And, the titanium material by representative of beta titanium alloy still has clearly disadvantageous when applied to biological implantation field.Wherein, most
It is important that the modulus of elasticity of titanium alloy is substantially higher compared with the modulus of elasticity of people's bone.Elasticity between this implantation material and people's bone
The mismatch of modulus, easily causes " stress shielding " phenomenon, causes implantation material to loosen, ultimately causes graft failure.Therefore, grind
The biomedical metallic material for sending out new has become one of study hotspot of current bio-medical material.
Similar with titanium alloy, zircaloy equally has excellent mechanical performance, decay resistance, histocompatbility and nontoxic
Characteristic.At present, zircaloy is mainly used in reactor core structural material (such as fuel can) and corrosion resistant container and pipeline (as pressed
Solenoid, support and duct pipe) etc., and the zircaloy of currently acquired application is α types (crystal structure is close-packed hexagonal structure) zirconium
Alloy.At present, zirconium is as the alloying element in titanium alloy, in beta titanium alloy in the main application of biomedical materials field
In play solution strengthening and stablize β phases (crystal structure is body-centered cubic structure), β type zircaloys are in bio-medical material side
The research in face is also quite rare.
The content of the invention
In order to which the modulus of elasticity for solving titanium alloy is substantially higher compared with the modulus of elasticity of people's bone, modulus of elasticity is not between people's bone
Matching, the problem of causing implantation material loosening, the graft failure caused.The invention provides a kind of bio-medical β type zircaloys,
By adding titanium, niobium, four kinds of elements of tantalum and tin into zirconium base body, the wherein percentage by weight ＞ 50% of zirconium, prepare without V and
The bio-toxicity element such as Mo, have low elastic modulus concurrently and the new bio medical beta type zircaloy of high intensity, expand bio-medical
The class of material, to make up deficiency of the conventional titanium alloy in bio-medical field performance.
It is a kind of to have low elastic modulus and the β type Zr-Ti-Nb-Ta-Sn systems alloy of high intensity concurrently, it is characterised in that use with
The raw material of lower species and percentage by weight is prepared from by alloy melting,
Titanium 20.5%~27.0%, niobium 3.5%~13.5%, tin 2.5%~6.5%, tantalum 0.5%~2.5%, remaining is
Zirconium, and the percentage by weight ＞ 50% of zirconium,
β types Zr-Ti-Nb-Ta-Sn systems alloy has a crystal phase structure of single β phases, and tensile modulus of elasticity is 38~
45GPa, tensile strength are 580~620MPa.
The preparation method for having low elastic modulus and the β type Zr-Ti-Nb-Ta-Sn systems alloy of high intensity concurrently, its feature
It is, comprises the following steps：
(1) raw material is weighed：Weigh the raw material of following percentage by weight：Titanium 20.5%~27.0%, niobium 3.5%~
13.5%, tin 2.5%~6.5%, tantalum 0.5%~2.5%, remaining is zirconium, and the percentage by weight ＞ 50% of zirconium；
(2) raw material is mixed：Weighted zirconium, titanium, niobium, tantalum are well mixed using the method for stirring mixing, tin is individually put
Put, be not involved in batch mixing；
(3) alloy melting：Tin raw material is placed in crucible bottom, mixed zirconium, titanium, niobium, tantalum are then placed on tin
Above, by vacuumize process in stove before melting, be passed through argon gas protection carry out melting, after melting terminates, 10~40 seconds by alloy by
Settable liquid continues to cool down crucible, obtains being organized as β type Zr-Ti-Nb-Sn systems alloy to solid-state after alloy graining, whole
Individual 500~1000 seconds cooling procedure duration.
Preferably, fusion process uses water jacketed copper crucible, and non-consumable arc furnace carries out melting to alloy, and melting terminates
Afterwards, cooled down under the protection of inert gas argon gas by the way of crucible bottom leads to recirculated cooling water.
Preferably, it is 7 × 10 by degree of being evacuated in stove before alloy melting-3~8 × 10-4Pa state, is passed through argon gas guarantor
The control of gas air pressure is protected in a standard atmospheric pressure.
Preferably, melting voltage is 220V during melting, and melting electric current is 200~220A.
Preferably, the number of times of melting is 3~5 times.
Preferably, the raw material be respectively sponge zirconium of the industrial purity more than 99.0%, titanium sponge, niobium block, tantalum block and
Block tin.
The selection principle of the alloying element of β types Zr-Ti-Nb-Ta-Sn systems of the present invention alloy is as follows：
Zirconium：It is final to obtain β type Zr alloys by the addition of other alloying elements from for matrix element.
Titanium：Titanium and zirconium belong to congeners, and the two has identical crystal structure, can dissolve each other completely.The crystalline substance of titanium and zirconium
There is obvious difference between lattice parameter, the addition of titanium elements can make alloy produce obvious distortion of lattice, alloy is played
The effect of solution strengthening.
Niobium：Niobium element can stablize the high temperature β phases of zircaloy to room temperature, play β phase stabilizing elements.In addition,
The addition of niobium element can also play a part of solution strengthening and improve alloy ductility.
Tantalum：Tantalum element can stablize the high temperature β phases of zircaloy to room temperature, play β phase stabilizing elements.In addition,
The addition of tantalum element can also play a part of reduction modulus of elasticity and improve intensity.
Tin：During the high temperature β phases of zircaloy are cooled to room temperature, often along with the precipitation of micro ω phases.ω
The precipitation of phase can cause the notable rise of zircaloy modulus of elasticity, and drop low-alloyed plasticity.The addition of tin element can effectively press down
The precipitation of ω phases in alloyage, therefore have remarkable result in terms of the modulus of elasticity and raising toughness of reduction zircaloy.
Advantages of the present invention：
1. adding tin in the β type Zr-Ti-Nb-Ta-Sn systems alloy of the present invention, the addition of tin element effectively inhibits zirconium
Alloy from high temperature β phases be cooled to room temperature during ω phases precipitation, therefore reduction zircaloy modulus of elasticity and improve it is tough
Property aspect have remarkable result.The tensile modulus of elasticity that the β type Zr-Ti-Nb-Ta-Sn systems of the present invention close is 38~45GPa, hence it is evident that
It is approximate with the modulus of elasticity (~40GPa) of people's bone suitable less than the tensile modulus of elasticity (55~110GPa) of titanium alloy, Ke Yiyou
Effect alleviates the modulus of elasticity between implant and people's bone and mismatches the implantation failure induced.
2. five kinds of alloying element zirconiums, titanium, niobium, tantalum and tin selected by the β type Zr-Ti-Nb-Ta-Sn systems alloy of the present invention
It is no cytotoxicity element, efficiently avoid the problem of element such as Mo and V has cytotoxicity in some medical alloys.
3. the β type Zr-Ti-Nb-Ta-Sn systems alloy of the present invention belongs to the medical zircaloy (weight percent zirconia of new bio
＞ 50%), the medical zirconium of new bio with traditional bio-medical beta titanium alloy (titanium percentage by weight ＞ 50%) and containing Mo
There is significant difference in alloy, the kind of bio-medical material has been expanded in the research and development of β type Zr-Ti-Nb-Ta-Sn systems alloy of the invention
Class, a kind of new material is provided for the bio-medical implantation piece such as orthopedic implants.It can be widely applied for bio-medical implantation material
The fields, such as artificial limb, joint prosthesis and bone wound product such as material.
4. sponge zirconium of the raw material that preparation method of the present invention is used for purity more than 99.0%, titanium sponge,
Niobium block, tantalum block and block tin, the equal no cytotoxicity of raw material of these purity, and without import, the country can volume procurement.
Brief description of the drawings
Fig. 1 is the tensile stress-strain curve of β type Zr-Ti-Nb-Ta-Sn alloys prepared by embodiment 1.
Fig. 2 is the X ray diffracting spectrum of β type Zr-Ti-Nb-Ta-Sn alloys prepared by embodiment 1.
Fig. 3 is the tensile stress-strain curve of β type Zr-Ti-Nb-Ta-Sn alloys prepared by embodiment 2.
Fig. 4 is the X ray diffracting spectrum of β type Zr-Ti-Nb-Ta-Sn alloys prepared by embodiment 2.
Fig. 5 is the tensile stress-strain curve of β type Zr-Ti-Nb-Ta-Sn alloys prepared by embodiment 3.
Fig. 6 is the X ray diffracting spectrum of β type Zr-Ti-Nb-Ta-Sn alloys prepared by embodiment 3.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical scheme be clearly and completely described.
Embodiment 1：
1. the industrial materials for being more than 99% from purity are raw material, β type Zr-Ti-Nb-Ta-Sn systems of the invention close
The raw material components proportioning of gold：Zirconium is 73.0wt.%, and titanium is 20.5wt.%, and niobium is 3.5wt.%, and tantalum is 0.5wt.%, and tin is
2.5wt.%.
2. preparation method：
(1) raw material weighing：The industrial materials for being more than 99.0% from purity are raw material, according to following percentage by weight
Carry out weighing and burden：Zirconium is 73.0%, and titanium is 20.5%, and niobium is 3.5%, and tantalum is 0.5%, and tin is 2.5%.
(2) raw material is mixed, and weighted zirconium, titanium, niobium, tantalum is well mixed using the method for stirring mixing, tin is individually put
Put, be not involved in batch mixing.
(3) raw material melting, melting is carried out using water jacketed copper crucible non-consumable arc furnace to alloy, will during pill heat
The tin element of low melting point is placed on crucible bottom, then mixed zirconium, titanium, niobium, tantalum is placed on above tin, raw material is put into
Vacuumize process is carried out after crucible, during melting by degree of being evacuated in stove be 8 × 10-4After Pa state, argon gas protection, argon are passed through
Gas air pressure is controlled in a standard atmospheric pressure；Melting voltage is 220V during melting, and melting electric current is 200A；After melting terminates,
Cooled down under the protection of inert gas argon gas by the way of crucible bottom leads to recirculated cooling water, alloy is by settable liquid to admittedly
The cool time of state is 10~40 seconds, continues to cool down crucible bottom water flowing after alloy graining, obtains alloy cast ingot, whole cooling
Process duration about 500 seconds.In order to ensure that composition is uniform, the uniform β types Zr- of composition is finally made in alloy melt back 4 times
Ti-Nb-Ta-Sn alloys.
3. alloy is detected：
β type Zr-Ti-Nb-Ta-Sn biomedical alloys after melting is enterprising in Instron-8801 type universal testing machines
Row stretching mechanical property testing, tensile modulus of elasticity 38GPa, yield strength and the tensile strength for measuring the alloy sample be respectively
574Mpa and 598MPa.Fig. 1 is the tensile stress-strain curve of β types Zr-Ti-Nb-Ta-Sn alloys manufactured in the present embodiment.Institute
The phase composition of the β type Zr-Ti-Nb-Ta-Sn alloys of preparation is analyzed using X-ray diffractometer, and analysis result shows alloy phase
Constitute as single β phases, corresponding X ray diffracting spectrum is shown in Fig. 2.
Embodiment 2：
1. composition proportion：The industrial materials for being more than 99% from purity are raw material, β type Zr-Ti-Nb-Ta-Sn alloys
Each component percentage by weight be respectively：Zirconium is 62%, and titanium is 24%, and niobium is 8%, and tantalum is 2%, and tin is 4%.
2. preparation method：
(1) raw material weighing, the percentage by weight according to each component raw material carries out weighing and burden；
(2) raw material is mixed, and weighted zirconium, titanium, niobium, tantalum is well mixed using the method for stirring mixing, tin is individually put
Put, be not involved in batch mixing；
(3) raw material melting, melting is carried out using water jacketed copper crucible non-consumable arc furnace to alloy, will during pill heat
The tin element of low melting point is placed on crucible bottom, then mixed zirconium, titanium, niobium, tantalum is placed on above tin, raw material is put into
Vacuumize process is carried out after crucible, during melting by degree of being evacuated in stove be 9 × 10-4After Pa state, argon gas protection, argon are passed through
Gas air pressure is controlled in a standard atmospheric pressure；Melting voltage is 220V during melting, and melting electric current is 210A；After melting terminates,
Cooled down under the protection of inert gas argon gas by the way of crucible bottom leads to recirculated cooling water, alloy is by settable liquid to admittedly
The cool time of state is 10~40 seconds, continues to cool down crucible bottom water flowing after alloy graining, obtains alloy cast ingot, whole cooling
Process duration about 800 seconds.In order to ensure that composition is uniform, the uniform β types Zr- of composition is finally made in alloy melt back 4 times
Ti-Nb-Ta-Sn alloys.
3. alloy is detected：
β type Zr-Ti-Nb-Ta-Sn biomedical alloys after melting is enterprising in Instron-8801 type universal testing machines
Row stretching mechanical property testing, tensile modulus of elasticity 41GPa, yield strength and the tensile strength for measuring the alloy sample be respectively
584Mpa and 603MPa.Fig. 3 is the tensile stress-strain curve of embodiment β type Zr-Ti-Nb-Ta-Sn alloys.β after melting
The phase composition of type Zr-Ti-Nb-Sn alloys is analyzed using X-ray diffractometer, and analysis result shows that alloy phase composition is single
β phases, corresponding X ray diffracting spectrum is shown in Fig. 4.
Embodiment 3：
1. composition proportion：The industrial materials for being more than 99% from purity are raw material, each component weight percent of alloy
Than being respectively：Zirconium is 50.5%, and titanium is 27.0%, and niobium is 13.5%, and tantalum is 2.5%, and tin is 6.5%.
2. preparation method：
(1) raw material weighing, the percentage by weight according to each component raw material carries out weighing and burden；
(2) raw material is mixed, and weighted zirconium, titanium, niobium, tantalum is well mixed using the method for stirring mixing, tin is individually put
Put, be not involved in batch mixing；
(3) raw material melting, melting is carried out using water jacketed copper crucible non-consumable arc furnace to alloy, will during pill heat
The tin element of low melting point is placed on crucible bottom, then mixed zirconium, titanium, niobium, tantalum is placed on above tin, raw material is put into
Vacuumize process is carried out after crucible, during melting by degree of being evacuated in stove be 8 × 10-4After Pa state, argon gas protection, argon are passed through
Gas air pressure is controlled in a standard atmospheric pressure；Melting voltage is 220V during melting, and melting electric current is 220A；After melting terminates,
Cooled down under the protection of inert gas argon gas by the way of crucible bottom leads to recirculated cooling water, alloy is by settable liquid to admittedly
The cool time of state is 10~40 seconds, continues to cool down crucible bottom water flowing after alloy graining, obtains alloy cast ingot, whole cooling
Process duration about 1000 seconds.In order to ensure that composition is uniform, the uniform β types of composition are finally made in alloy melt back 4 times
Zr-Ti-Nb-Ta-Sn alloys.
3. alloy is detected：
β type Zr-Ti-Nb-Ta-Sn biomedical alloys after melting is enterprising in Instron-8801 type universal testing machines
Row stretching mechanical property testing, tensile modulus of elasticity 40GPa, yield strength and the tensile strength for measuring the alloy sample be respectively
591Mpa and 615MPa.Fig. 5 is the tensile stress-strain curve of embodiment β type Zr-Ti-Nb-Ta-Sn alloys.β after melting
The phase composition of type Zr-Ti-Nb-Ta-Sn alloys is analyzed using X-ray diffractometer, and analysis result shows that alloy phase composition is
Single β phases, corresponding X ray diffracting spectrum is shown in Fig. 6.
Described embodiment is a part of embodiment of the invention, rather than whole embodiments.In one kind of the present invention
Element and feature described in embodiment can be with the elements and feature phase that are shown in one or more other embodiments
With reference to.Although the present invention and its advantage have been described in detail above it should be appreciated that wanted without departing from by appended right
Various changes can be carried out in the case of seeking limited the spirit and scope of the present invention, substitutes and converts.Moreover, the present invention
Scope is not limited only to process described by specification, equipment, means, the specific embodiment of method and steps.In the art is general
Logical technical staff will readily appreciate that from the disclosure, according to the present invention can use execution to it is described herein corresponding
The essentially identical function of embodiment obtains result, the existing and in the future to be developed process essentially identical with it, set
Standby, means, method or step.Therefore, appended claim includes such process in the range of being directed at them, set
Standby, means, method or step.
Claims (7)
1. a kind of have low elastic modulus and the β type Zr-Ti-Nb-Ta-Sn systems alloy of high intensity concurrently, it is characterised in that using following
The raw material of species and percentage by weight is prepared from by alloy melting,
Titanium 20.5%~27.0%, niobium 3.5%~13.5%, tin 2.5%~6.5%, tantalum 0.5%~2.5%, remaining is zirconium,
And the percentage by weight ＞ 50% of zirconium,
β types Zr-Ti-Nb-Ta-Sn systems alloy has a crystal phase structure of single β phases, tensile modulus of elasticity be 38~45GPa,
Tensile strength is 580~620MPa.
2. have the preparation method of low elastic modulus and the β type Zr-Ti-Nb-Ta-Sn systems alloy of high intensity described in claim 1 concurrently,
It is characterised in that it includes following steps：
(1) raw material is weighed：Weigh the raw material of following percentage by weight：Titanium 20.5%~27.0%, niobium 3.5%~13.5%, tin
2.5%~6.5%, tantalum 0.5%~2.5%, remaining is zirconium, and the percentage by weight ＞ 50% of zirconium；
(2) raw material is mixed：Weighted zirconium, titanium, niobium, tantalum are well mixed using the method for stirring mixing, tin is individually placed, no
Participate in batch mixing；
(3) alloy melting：Tin raw material is placed in crucible bottom, then mixed zirconium, titanium, niobium, tantalum are placed on above tin,
By vacuumize process in stove before melting, it is passed through argon gas protection and carries out melting, after melting terminates, coagulate alloy by liquid within 10~40 seconds
Gu to solid-state, continuing to cool down crucible after alloy graining, obtain being organized as β type Zr-Ti-Nb-Sn systems alloy, whole cooling
Process duration 500~1000 seconds.
3. preparation method according to claim 2, it is characterised in that fusion process uses water jacketed copper crucible, non-consumable is true
Empty electric arc furnaces carries out melting to alloy, after melting terminates, cold using the logical circulation of crucible bottom under the protection of inert gas argon gas
But the mode of water is cooled down.
4. preparation method according to claim 3, it is characterised in that before alloy melting by degree of being evacuated in stove be 7 ×
10-3~8 × 10-4Pa state, is passed through argon gas protection gas air pressure control in a standard atmospheric pressure.
5. preparation method according to claim 2, it is characterised in that melting voltage is 220V during melting, melting electric current is
200~220A.
6. preparation method according to claim 2, it is characterised in that the number of times of melting is 3~5 times.
7. preparation method according to claim 2, it is characterised in that the raw material is respectively that industrial purity exceedes
99.0% sponge zirconium, titanium sponge, niobium block, tantalum block and block tin.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107893176A (en) * | 2017-11-08 | 2018-04-10 | 大连理工大学 | A kind of Zr Nb based alloys and its application with good increasing material manufacturing forming property |
| CN108149071A (en) * | 2017-12-25 | 2018-06-12 | 中国矿业大学 | A kind of low magnetic susceptibility β type Zr-Nb-Ta systems alloy and preparation method thereof |
| TWI755263B (en) * | 2021-01-27 | 2022-02-11 | 國立清華大學 | High strength and low modulus alloy and use thereof |
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| CN103184369A (en) * | 2013-04-10 | 2013-07-03 | 广西大学 | Beta type Zr-Nb-Ti biomedical alloy and preparation method thereof |
| CN105274393A (en) * | 2015-11-13 | 2016-01-27 | 江苏大学 | Beta type Zr-Ti-Nb-Sn system alloy and preparation method thereof |
| CN105349839A (en) * | 2015-11-12 | 2016-02-24 | 福建工程学院 | Low-elasticity modulus beta-Zr type biomedical alloy and manufacturing method thereof |
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| CN101374479A (en) * | 2005-12-15 | 2009-02-25 | 史密夫和内修有限公司 | Diffusion-hardened medical implant |
| CN103184369A (en) * | 2013-04-10 | 2013-07-03 | 广西大学 | Beta type Zr-Nb-Ti biomedical alloy and preparation method thereof |
| CN105349839A (en) * | 2015-11-12 | 2016-02-24 | 福建工程学院 | Low-elasticity modulus beta-Zr type biomedical alloy and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107893176A (en) * | 2017-11-08 | 2018-04-10 | 大连理工大学 | A kind of Zr Nb based alloys and its application with good increasing material manufacturing forming property |
| CN108149071A (en) * | 2017-12-25 | 2018-06-12 | 中国矿业大学 | A kind of low magnetic susceptibility β type Zr-Nb-Ta systems alloy and preparation method thereof |
| TWI755263B (en) * | 2021-01-27 | 2022-02-11 | 國立清華大學 | High strength and low modulus alloy and use thereof |
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Application publication date: 20170825 |