CN103334029A - Beta titanium alloy composition and preparation method thereof - Google Patents
Beta titanium alloy composition and preparation method thereof Download PDFInfo
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Abstract
The invention provides a beta titanium alloy composition and a preparation method thereof. The composition consists of the following components in percentage by mass: 57-59% of Ti, 36-37% of Nb, 2-2.5% of Ta and 3-3.5% of Zr. The invention also relates to a preparation method of the composition. The preparation method comprises the following steps of: (I) proportioning the components in percentage by mass, mixing and pressing into an electrode; (II) smelting the electrode in a vacuum consumable electro-arc furnace to obtain an ingot; (III) performing hot working on the ingot, and performing heat treatment to obtain a crude beta titanium alloy composition; (IV) cutting the crude beta titanium alloy composition into a blank and performing surface pretreatment; (V) preheating an equal channel angular extrusion die and the blank, and coating a graphite lubricant; and heating and preserving heat; and (VI) extruding at 500-600 DEG C twice to four times and performing water quenching. The method provided by the invention is simple and easy to implement, has low cost and can remarkably refine the crystal grains; and the beta titanium alloy composition provided by the invention is a bone tissue substitute material with a broad medical prospect.
Description
Technical field
The present invention relates to a kind of titanium alloy material and preparation method thereof, particularly, relate to a kind of beta-titanium alloy composition and method of making the same.
Background technology
As medical metal material, should possess nontoxicity, antibiosis reason corrodibility, good biocompatibility and characteristics such as mechanical compatibility and workability.Use titanium alloy quality be light because it has, characteristics such as nontoxicity, corrosion-resistant, excellent biocompatibility, be the medical material of Chinese scholars primary study always.The development of medical titanium alloy can be traced back to phase early 1940s, and people such as Bothe at first are incorporated into biomedical sector with pure titanium, finds no any untoward reaction between titanium and the mouse femur.Pure titanium has good corrosion resistance in physiological environment, but its intensity is lower, and abrasion resistance properties is relatively poor, has limited it in the application of carrying than large part, and the bone that is mainly used in Oral Repair and carrying smaller portions is at present replaced.By contrast, the Ti-6Al-4V alloy has higher intensity and better machining property, and the later stage seventies is widely used as the surgical repair material, as hip joint, and knee joint etc.Simultaneously, the Ti-3Al-2.5V alloy also is used as femur and shin bone replacement material clinically.But this class alloy contains V and two kinds of elements of Al, V is considered to the element poisonous to organism, the Al element to the harm of organism be by aluminium salt in vivo accumulate the damage that causes organ, the Al element also can cause symptoms such as osteomalacia, anaemia and nervous disorders in addition, and this class alloy corrosion resistance is relatively poor relatively.Their Young's modulus and bone photo ratio still have big gap in addition, are easy to generate " stress shielding ", thereby cause bone regeneration around implant bone resorption to occur, finally cause the loosening or fracture of planting body and cause the plantation failure.Therefore, the new bio medical titanium alloy that the research and development biocompatibility is better, Young's modulus is lower, over-all properties is more excellent, to satisfy clinical requirement to the implantation piece material, become the main direction of bio-medical material research, and β type medical titanium alloy adapts to this requirement just and developed rapidly.
Since the nineties in 20th century, people have developed a series of low modulus beta-titanium alloy by adding nontoxic element nb, Ta, Zr etc., as the Ti-13Nb-13Zr alloy, and Ti-35Nb-5Ta-7Zr alloy, Ti-29Nb-13Ta-4.6Zr alloy etc.Wherein the Ti-35Nb-5Ta-7Zr alloy has excellent biological compatibility and corrosion stability, and its Young's modulus is 55GPa, is considered to one of medical beta-titanium alloy of canonical biometric that has most application prospect.But the intensity of these alloys is not high, in order to improve the intensity of beta-titanium alloy, need some special process of exploitation to make that plasticity can too not reduce when improving beta-titanium alloy intensity, and Young's modulus still keeps low numerical value.
Studies show that in a large number refined crystalline strengthening can be improved the material plastic deformation ability, realize improving the optimization of intensity and plasticity.Violent plastic deformation method (being called for short SPD) is crystal grain thinning significantly, makes the material microtexture be refined to micron order even nano level, reaches the purpose that improves the material comprehensive mechanical property.In recent years, violent plastic deformation method was developed fast, mainly comprised high pressure torsion method (being called for short HPT), the folded hypodesmus of accumulation (being called for short ARB) and Equal Channel Angular Pressing method (being called for short ECAP) at present.Wherein the Equal Channel Angular Pressing method be the eighties in 20th century The former Russian scholar Segal be the method for a kind of large plastometric set of obtaining the pure shear distortion and developing.Compare with additive method, do not change the shape of material before and after the advantage of Equal Channel Angular Pressing method is to be out of shape, and preparation is simple, cost is low, and grain refining effect is obvious, the block grained material that suitable preparation is bigger.At present, Chinese scholars utilizes HPT method and ARB method to improve the existing report of Ti-Nb-Ta-Zr alloy strength, utilize the high pressure torsion method to handle Ti – 29Nb – 13Ta – 4.6Zr alloy as H. Yilmazer etc., but this method only is suitable for preparing less lamellar material, and is difficult to obtain equi-axed crystal behind the high pressure torsion.The folded hypodesmus of utilizations such as Damon Kent accumulation is bundled into sheet material with Ti – 25Nb – 3Zr – 3Mo – 2Sn alloy, though the strength of materials is greatly improved, plasticity but sharply descends.Plasticity can too not reduce and Young's modulus still keeps low numerical value when in sum, people also found a kind of effective means make to improve beta-titanium alloy intensity.
Summary of the invention
At defective of the prior art, the purpose of this invention is to provide a kind of beta-titanium alloy composition and method of making the same.
The present invention is achieved by the following technical solutions,
First aspect the present invention relates to a kind of beta-titanium alloy composition, and described composition is made up of following components by mass percentage: Ti 57～59%,
Nb 36～37%，
Ta 2～2.5%，
Zr 3～3.5%。
Second aspect the present invention relates to aforementioned beta-titanium alloy preparation of compositions method, and described method comprises the steps:
Step 1 is prepared burden each component of described beta-titanium alloy composition by following mass percent Ti57～59%, Nb36～37%, Ta2～2.5%, Zr3～3.5%, after fully mixing, be pressed into electrode;
Step 2, described electrode are carried out melting in vacuum consumable electrode arc furnace, get ingot casting;
Step 3 is carried out hot-work with ingot casting, and thermal treatment gets rough beta-titanium alloy composition;
Step 4 cuts into blank with described rough beta-titanium alloy composition, carries out surface preparation;
Step 5 is with isometrical bent angle extrusion mould and described blank preheating, at described blank and described mold cavity internal surface coated graphite lubricant; Described blank is put into described isometrical bent angle extrusion mould, heat tracing;
Step 6, under 500～600 ℃ of conditions, extruding, shrend, in the Bc mode to blank extruding 2～4 times, get final product final product beta-titanium alloy composition.
Preferably, in the step 2, described melting number of times is 3～5 times.
Preferably, in the step 3, described hot-work is specially: forge 960～980 ℃ of coggings, be of a size of Φ 40 * 160mm after the forging
3～Φ 40 * 170mm
3Described thermal treatment is specially: at 790～800 ℃ of solution treatment air cooling after 30～40 minutes.
Preferably, in the step 4, described billet size is 10 * 10 * 140mm
3～10 * 10 * 150mm
3Described blank surface roughness Ra is 2.5～3.0 μ m.
Preferably, in the step 5, described preheating temperature is 100～150 ℃, and the time is 10～20 minutes, and the thickness of described oildag is 0.3～0.4mm.
Preferably, in the step 5, described isometrical bent angle extrusion mould interior angle is 90～100 degree, and the exterior angle is 20～30 degree.
Preferably, in the step 5, described Heating temperature is 500～600 ℃, and soaking time is 30～45 minutes.
Preferably, in the step 6, described extrusion temperature is 500～600 ℃.
Preferably, in the step 6, described Bc mode is specially: blank turn 90 degrees extruding a time down around longitudinal axis dextrorotation between twice extruding passage.
Compared with prior art, the present invention has following beneficial effect:
(1) the present invention adopts isometrical bent angle pressing method to prepare the beta-titanium alloy composition, its smooth surface, zero defect;
(2) the inventive method makes beta-titanium alloy composition intensity improve greatly, and material size constancy before and after extruding, can realize the processing of relatively large material.
(3) to have a die apparatus simple in the present invention, tooling cost is low, grain refining effect is remarkable, be applicable to the advantage of the large-scale zero defect bulk of preparation, it is 90～100 ° that the present invention simultaneously adopts interior angle, the exterior angle is 20～30 ° isometrical bent angle mould, makes in the suffered plastic deformation amount in single pass extruding back greatly, realizes less passage extruding and obtains the medical beta-titanium alloy bulk of high strength.
(4) the present invention applies oildag between the two the sassafras resistance that rubs can reduce extruding greatly the time at blank and die surface, makes the product smooth surface flawless of preparing; In addition, can increase substantially the intensity of product after the extruding of 4 passages, Young's modulus still keeps low numerical value, when pushing 2 or 3 times, method of the present invention can be implemented equally, and the effect in itself and 4 roads is difference slightly to some extent, and the present invention has wide bio-medical prospect.
Description of drawings
By reading the detailed description of non-limiting example being done with reference to the following drawings, it is more obvious that other features, objects and advantages of the present invention will become:
Fig. 1 is the metallographic structure shape appearance figure of the present invention's beta-titanium alloy composition after solution treatment;
Fig. 2 is the TEM image of beta-titanium alloy composition of the present invention 500 ℃ of extruding 4 passages in embodiment 1;
Fig. 3 is the TEM image of beta-titanium alloy composition of the present invention 600 ℃ of extruding 2 passages in embodiment 2;
Fig. 4 is the TEM image of beta-titanium alloy composition of the present invention 600 ℃ of extruding 4 passages in embodiment 3.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment.Following examples will help those skilled in the art further to understand the present invention, but not limit the present invention in any form.Should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make some distortion and improvement.These all belong to protection scope of the present invention.
Embodiment 1
Present embodiment relates to a kind of beta-titanium alloy composition, and its each component and percentage composition are shown in Table 1:
Present embodiment also relates to a kind of beta-titanium alloy preparation of compositions method, and described method comprises the steps:
Step 1; each component and percentage composition thereof batching in getting shown in the table 1; Ti adds with the form of titanium sponge (purity 99.5wt%); Zr adds with the form of zirconium sponge (purity 99.8wt%); Nb adds with the form of niobium plate (purity 99.6wt%); Ta adds with the form of tantalum bar (purity 99.6wt%) after fully mixing, is pressed into electrode;
Step 2, described electrode are carried out melting 3 times in vacuum consumable electrode arc furnace, get ingot casting;
Step 3 is carried out cogging at 980 ℃ to ingot casting with ingot casting and is forged, and is of a size of Φ 40 * 160mm after the forging
3, then 800 ℃ of solution treatment after 30 minutes behind the air cooling, see shown in Figure 1ly, get rough beta-titanium alloy composition;
Step 4, it is 10 * 10 * 140mm that ingot casting is cut into billet size
3Grinding process is carried out on the surface, and blank surface roughness Ra is about 2.5 μ m;
Step 5 with isometrical bent angle extrusion mould (interior angle is 90 °, and the exterior angle is 20 °) and 150 ℃ of following preheatings of described blank 20 minutes, is the oildag of 0.4mm at described blank and described mold cavity internal surface applied thickness; Described blank is put into described isometrical bent angle extrusion mould, and Heating temperature is 500 ℃, and soaking time is 40 minutes;
Step 6 under 500 ℃ of conditions, is finished isometrical bent angle extruding fast on hydropress, extruding rate is 8mm/s, and the blank after will pushing immediately after having pushed carries out shrend, in the Bc mode blank is pushed 4 times, get final product final product beta-titanium alloy composition, see shown in the accompanying drawing 2.
Table 1
Implementation result: the crystal grain that present embodiment makes is equiax crystal, and mean sizes is 0.3 μ m.
Testing method: in order to study the variation of extruding front and back material mechanical performance, be cut into tension specimen with line, the tension specimen gauge length is 10mm, and thickness is 1.6mm.Rate of extension is 1 * 10
-3s
-1, table 2 is for recording the beta-titanium alloy composition room temperature tensile performance after embodiment 1 pushes.
Table 2
Embodiment 2
Present embodiment relates to a kind of beta-titanium alloy composition, and its each component and percentage composition are shown in Table 3:
Present embodiment also relates to a kind of beta-titanium alloy preparation of compositions method, and described method comprises the steps:
Step 1; each component and percentage composition thereof batching in getting shown in the table 3; Ti adds with the form of titanium sponge (purity 99.5wt%); Zr adds with the form of zirconium sponge (purity 99.8wt%); Nb adds with the form of niobium plate (purity 99.6wt%); Ta adds with the form of tantalum bar (purity 99.6wt%) after fully mixing, is pressed into electrode;
Step 2, described electrode are carried out melting 3 times in vacuum consumable electrode arc furnace, get ingot casting;
Step 3 is carried out cogging at 960 ℃ to ingot casting with ingot casting and is forged, and is of a size of Φ 40 * 170mm after the forging
3, then 800 ℃ of solution treatment after 40 minutes behind the air cooling, see shown in Figure 1ly, get rough beta-titanium alloy composition;
Step 4, it is 10 * 10 * 145mm that ingot casting is cut into billet size
3Grinding process is carried out on the surface, and blank surface roughness Ra is about 2.8 μ m;
Step 5 with isometrical bent angle extrusion mould (interior angle is 95 °, and the exterior angle is 25 °) and 100 ℃ of following preheatings of described blank 10 minutes, is the oildag of 0.3mm at described blank and described mold cavity internal surface applied thickness; Described blank is put into described isometrical bent angle extrusion mould, and Heating temperature is 550 ℃, and soaking time is 45 minutes;
Step 6 under 600 ℃ of conditions, is finished isometrical bent angle extruding fast on hydropress, extruding rate is 8mm/s, and the blank after will pushing immediately after having pushed carries out shrend, in the Bc mode blank is pushed 2 times, get final product final product beta-titanium alloy composition, see shown in the accompanying drawing 3.
Table 3
| Component | Nb | Ta | Zr | Ti |
| Mass percent | 37 | 2.5 | 3.5 | 59 |
| （wt%) |
Implementation result: the crystal grain that present embodiment makes is equiax crystal, and mean sizes is 0.6 μ m.
Testing method: in order to study the variation of extruding front and back material mechanical performance, be cut into tension specimen with line, the tension specimen gauge length is 10mm, and thickness is 1.6mm.Rate of extension is 1 * 10
-3s
-1, table 4 is for recording the beta-titanium alloy composition room temperature tensile performance after embodiment 2 pushes.
Table 4
Embodiment 3
Present embodiment relates to a kind of beta-titanium alloy composition, and its each component and percentage composition are shown in Table 5:
Present embodiment also relates to a kind of beta-titanium alloy preparation of compositions method, and described method comprises the steps:
Step 1; each component and percentage composition thereof batching in getting shown in the table 5; Ti adds with the form of titanium sponge (purity 99.5wt%); Zr adds with the form of zirconium sponge (purity 99.8wt%); Nb adds with the form of niobium plate (purity 99.6wt%); Ta adds with the form of tantalum bar (purity 99.6wt%) after fully mixing, is pressed into electrode;
Step 2, described electrode are carried out melting 3 times in vacuum consumable electrode arc furnace, get ingot casting;
Step 3 is carried out cogging at 980 ℃ to ingot casting with ingot casting and is forged, and is of a size of Φ 40 * 160mm after the forging
3, then 800 ℃ of solution treatment after 30 minutes behind the air cooling, see shown in Figure 1ly, get rough beta-titanium alloy composition;
Step 4, it is 10 * 10 * 150mm that ingot casting is cut into billet size
3Grinding process is carried out on the surface, and blank surface roughness Ra is about 3.0 μ m;
Step 5 with isometrical bent angle extrusion mould (interior angle is 100 °, and the exterior angle is 30 °) and 110 ℃ of following preheatings of described blank 15 minutes, is the oildag of 0.35mm at described blank and described mold cavity internal surface applied thickness; Described blank is put into described isometrical bent angle extrusion mould, and Heating temperature is 600 ℃, and soaking time is 30 minutes;
Step 6 under 600 ℃ of conditions, is finished isometrical bent angle extruding fast on hydropress, extruding rate is 8mm/s, and the blank after will pushing immediately after having pushed carries out shrend, in the Bc mode blank is pushed 4 times, get final product final product beta-titanium alloy composition, see shown in the accompanying drawing 4.
Table 5
| Component | Nb | Ta | Zr | Ti |
| Mass percent | 36.5 | 2 | 3.5 | 58 |
| （wt%) |
Implementation result: the crystal grain that present embodiment makes is equiax crystal, and mean sizes is about 0.5 μ m.
Testing method: in order to study the variation of extruding front and back material mechanical performance, be cut into tension specimen with line, the tension specimen gauge length is 10mm, and thickness is 1.6mm.Rate of extension is 1 * 10
-3s
-1, table 6 is for recording the beta-titanium alloy composition room temperature tensile performance after embodiment 3 pushes.
Table 6
More than specific embodiments of the invention are described.It will be appreciated that the present invention is not limited to above-mentioned specific implementations, those skilled in the art can make various distortion or modification within the scope of the claims, and this does not influence flesh and blood of the present invention.
Claims (10)
1. a beta-titanium alloy composition is characterized in that, described composition is made up of following components by mass percentage: Ti 57～59%,
Nb 36～37%，
Ta 2～2.5%，
Zr 3～3.5%。
2. a beta-titanium alloy preparation of compositions method as claimed in claim 1 is characterized in that described method comprises the steps:
Step 1 is prepared burden each component of described beta-titanium alloy composition by following mass percent Ti57～59%, Nb36～37%, Ta2～2.5%, Zr3～3.5%, after fully mixing, be pressed into electrode;
Step 2, described electrode are carried out melting in vacuum consumable electrode arc furnace, get ingot casting;
Step 3 is carried out hot-work with ingot casting, and thermal treatment gets rough beta-titanium alloy composition;
Step 4 cuts into blank with described rough beta-titanium alloy composition, carries out surface preparation;
Step 5 is with isometrical bent angle extrusion mould and described blank preheating, at described blank and described mold cavity internal surface coated graphite lubricant; Described blank is put into described isometrical bent angle extrusion mould, heat tracing;
Step 6, under 500～600 ℃ of conditions, the extruding, shrend is pushed 2～4 times blank in the Bc mode again, get final product final product beta-titanium alloy composition.
3. beta-titanium alloy preparation of compositions method as claimed in claim 2 is characterized in that, in the step 2, described melting number of times is 3～5 times.
4. beta-titanium alloy preparation of compositions method as claimed in claim 2 is characterized in that, in the step 3, described hot-work is specially: forge 960～980 ℃ of coggings, be of a size of Φ 40 * 160mm after the forging
3～Φ 40 * 170mm
3Described thermal treatment is specially: at 790～800 ℃ of solution treatment air cooling after 30～40 minutes.
5. beta-titanium alloy preparation of compositions method as claimed in claim 2 is characterized in that, in the step 4, described billet size is 10 * 10 * 140mm
3～10 * 10 * 150mm
3Described blank surface roughness Ra is 2.5～3.0 μ m.
6. beta-titanium alloy preparation of compositions method as claimed in claim 2 is characterized in that, in the step 5, described preheating temperature is 100～150 ℃, and the time is 10～20 minutes, and the thickness of described oildag is 0.3～0.4mm.
7. beta-titanium alloy preparation of compositions method as claimed in claim 2 is characterized in that, in the step 5, described isometrical bent angle extrusion mould interior angle is 90～100 degree, and the exterior angle is 20～30 degree.
8. beta-titanium alloy preparation of compositions method as claimed in claim 2 is characterized in that, in the step 5, described Heating temperature is 500～600 ℃, and soaking time is 30～45 minutes.
9. beta-titanium alloy preparation of compositions method as claimed in claim 2 is characterized in that, in the step 6, described extrusion temperature is 500～600 ℃.
10. beta-titanium alloy preparation of compositions method as claimed in claim 2 is characterized in that, in the step 6, described Bc mode is specially: blank turn 90 degrees extruding a time down around longitudinal axis dextrorotation between twice extruding passage.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104762578A (en) * | 2015-04-30 | 2015-07-08 | 西北有色金属研究院 | Preparation method for TLM titanium alloy foil with nanocrystalline structure |
| CN106756239A (en) * | 2017-01-11 | 2017-05-31 | 东南大学 | A kind of medical embedded porous titanium alloy and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1528941A (en) * | 2003-09-26 | 2004-09-15 | 上海交通大学 | Micro grain titanium-nickel-palladium-base high-temperature shape memory alloy preparing method |
| CN102146534A (en) * | 2011-03-09 | 2011-08-10 | 东南大学 | Low-elasticity high-strength near beta-type Ti-Nb-Ta-Zr alloy and preparation method of near beta-type Ti-Nb-Ta-Zr alloy |
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2013
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1528941A (en) * | 2003-09-26 | 2004-09-15 | 上海交通大学 | Micro grain titanium-nickel-palladium-base high-temperature shape memory alloy preparing method |
| CN102146534A (en) * | 2011-03-09 | 2011-08-10 | 东南大学 | Low-elasticity high-strength near beta-type Ti-Nb-Ta-Zr alloy and preparation method of near beta-type Ti-Nb-Ta-Zr alloy |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104762578A (en) * | 2015-04-30 | 2015-07-08 | 西北有色金属研究院 | Preparation method for TLM titanium alloy foil with nanocrystalline structure |
| CN106756239A (en) * | 2017-01-11 | 2017-05-31 | 东南大学 | A kind of medical embedded porous titanium alloy and preparation method |
| CN106756239B (en) * | 2017-01-11 | 2019-03-19 | 东南大学 | A kind of medical embedded porous titanium alloy and preparation method |
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