CN109161707A - A kind of manufacturing method of biological medical titanium alloy TC4ELI stick/wire rod - Google Patents
A kind of manufacturing method of biological medical titanium alloy TC4ELI stick/wire rod Download PDFInfo
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- CN109161707A CN109161707A CN201810132357.3A CN201810132357A CN109161707A CN 109161707 A CN109161707 A CN 109161707A CN 201810132357 A CN201810132357 A CN 201810132357A CN 109161707 A CN109161707 A CN 109161707A
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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
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
- B21C37/04—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire
- B21C37/045—Manufacture of wire or bars with particular section or properties
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- 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
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Abstract
The invention belongs to medical metal material technical fields, more particularly to a kind of manufacturing method of biological medical titanium alloy TC4ELI stick/wire rod, specifically it is, vacuum melting is carried out using the vanadium-aluminium intermediate alloy and benefit aluminium of aluminothermic process production, micro intensified element tin and zirconium are added in Vacuum Melting, and micro refinement crystal grain element rare earth, new component intermediate alloy is made, new component intermediate alloy and titanium sponge ingredient, TC4ELI titan alloy casting ingot is formed, TC4ELI titanium alloy bar/wire rod is eventually fabricated.Present invention process is stablized, and avoids regional segregation caused by melting ingot casting supplement simple substance aluminium element, guarantees the uniformity of microelement.
Description
Technical field
The invention belongs to medical metal material technical fields, and in particular to a kind of biological medical titanium alloy TC4ELI stick/line
The manufacturing method of material.
Background technique
In biomedical metallic material, titanium and its alloy rely on excellent comprehensive performance, become joint prosthesis (hip, knee,
Shoulder, ankle, elbow, wrist, articulations digitorum manus etc.), bone wound product (intramedullary nail, steel plate, screw etc.), backbone correcting internal fixation system, tooth kind
The preferred material of the medical implants product such as implant, denture fixing device, tooth orthopedic wire, heart valve prosthesis, Interventional angiocarpy bracket.Tool
There is the high damage of high-fracture toughness, low crack growth rate, low gap element type Ti-6A1-4VELI (domestic trade mark TC4ELI) to hold
Titanium alloy is limited, is used widely, 80% or more titanium alloy implant product is accounted at present and uses this alloy, TC4ELI stick (line)
Processing material is the most frequently used material product.
TC4ELI titanium alloy bar (line) country has many companies to produce the product, but import is not achieved always in similar product
Product Level, especially mechanical property, grain size are generally lower than developed country's product.The medical product manufactured using domestic material
Occur various problems in process of clinical application.Especially for loads components such as bone stock head, knee joint, screws, folding occurred
Disconnected, crackle, fall off the accidents such as infection.Analysis most of reason be due to used TC4ELI titanium alloy material mechanical property not
Stablize, organizes inconsistent；Fracture toughness is low, and stress is concentrated, caused by fatigue rupture.
TC4ELI titanium alloy is typical (alpha+beta) duplex alloy, and material mechanical property is processed to it and organizes decisive work
It is chemical component and heat processing technique.It is in particular in:
1. the uniformity consistency of the distribution of principal component.TC4ELI titanium alloy national and foreign standards are all that chemical composition ranges compare
Greatly, composition tolerances are of less demanding, but the tissue of its alloy and performance depend on the aluminium of stable alpha phase in alloy and stablize β phase
The relative scale and α of vanadium, the form of β two-phase, it must be determined that influence of the principal component proportional difference to structure property.
2. the uniformity consistency of impurity content distribution.Although TC4ELI titanium alloy standard itself has required low interstitial element
Content, but impurity element influences the fracture toughness of the alloy, crack growth rate very big, O, N, H, C, Fe be not in principle
Only content wants low, it is often more important that production stick/line raw material titan alloy casting ingot in will ingot casting upper, middle and lower and ingot casting inside and outside
Uniformity.
In domestic traditional TC4ELI titanic alloy machining material manufacturing process, ingot casting melting aluminium, vanadium is with intermediate alloy
What method was added.The intermediate alloy that melting ingredient uses is vanadium-aluminium intermediate alloy of aluminothermic process production.In this method manufacture
Between alloy, produced under atmospheric environment, the impurity contents such as O, C, N are difficult to control, and the content of V is even more that each furnace intermediate alloy is uniform
Property all can not be consistent.Intermediate alloy quality is the important factor in order of titan alloy casting ingot quality, and then affects stick, wire rod matter
Amount.
Summary of the invention
Invention broadly provides a kind of manufacturing method of biological medical titanium alloy TC4ELI stick/wire rod, which is avoided
Regional segregation caused by melting ingot casting supplement simple substance aluminium element, guarantees the uniformity of microelement.
The present invention is to reach ultralow impurity element, and Al, V ratio are rationally uniform, while being added and strengthening the refinement of titanium alloy element
The microelement of crystal grain, design prepare new intermediate alloy and production process route.
A kind of manufacturing method of biological medical titanium alloy TC4ELI stick/wire rod, comprising the following steps:
(1) preparation of new component intermediate alloy
Domestic traditional TC4ELI titan alloy casting ingot production distribution is: vanadium-aluminium intermediate alloy of aluminothermic process production adds
Fine aluminium mends aluminium ingredient.Since the method for mending aluminium is to add aluminum shot in vanadium-aluminium intermediate alloy packet, it be easy to cause the region microsegregation of aluminium.
The present invention carries out a vacuum melting using the vanadium-aluminium intermediate alloy and benefit aluminium of aluminothermic process production, avoids melting ingot casting supplement
Regional segregation caused by simple substance aluminium element.Meanwhile it is theoretical according to microalloying complex intensifying, it is added in Vacuum Melting micro
Intensified element tin and zirconium and micro refinement crystal grain element rare earth, manufactured new component intermediate alloy ingredient are as follows: O <
0.06%, N < 0.01%, C < 0.01%, Fe < 0.15%, 0 < Sn < 0.1%, 0 < Zr < 0.1%, 0 < RE < 0.1%,
Surplus is V and Al, and V:Al=4:6；
(2) preparation of TC4ELI titan alloy casting ingot
By new component intermediate alloy, titanium sponge ingredient, secondary vacuum melting, TC4ELI are carried out using vacuum consumable electrode arc furnace
The ingredient of titan alloy casting ingot are as follows: O < 0.10%, H < 0.005%, N < 0.01%, C < 0.03%, Fe < 0.15%, 6.10%
≤ Al≤6.20%, 4.10%≤V≤4.20%, 0 < Sn < 0.09%, 0 < Zr < 0.09%, 0 < RE < 0.03%, surplus
For Ti.Because vacuum consumable water jacketed copper crucible cooling velocity is limited, in the certain situation of speed of melting, fusion process heat
Accumulation, ingot solidification speed are also variation.Therefore in order to guarantee that ingot casting principal component and microelement, impurity do not produce segregation,
Uniform quality, the position that speed of melting will be reached according to circumstances with melting ingot casting are adjusted.Principle is speed of melting than pure titanium
It is low, it is convenient for diffusion of alloy elements and homogenization.
(3) TC4ELI titanium alloy bar/wire rod preparation
For TC4ELI stick/wire rod of diameter > 30mm, preparation process are as follows: ingot formation, hot rolling, is gone at blank finishing
Oxide skin, straightening, polishing, defect detecting test；
For diameter≤30mm TC4ELI stick/wire rod, preparation process are as follows: ingot formation, blank finishing, hot rolling, drawing
It pulls out, anneal, descale, straightening, polishing, defect detecting test.
Preferably, in the preparation process of step (3) TC4ELI titanium alloy bar/wire rod, for diameter≤30mm TC4ELI
Its Hubbing method of bar is that hot pull temperature has decisive influence to stick, line tissue and mechanical performance, to guarantee that TC4ELI titanium closes
Golden performance is stablized, and hot pull must carry out at a temperature of (alpha+beta) two-phase.Due to the difference of every batch of ingot chemistry, phase transformation
Point is different, first measures TC4ELI titanium alloy from alpha+beta mutually to the phase transition temperature of β phase, hot pull temperature is lower than phase transition temperature 100-
160 DEG C, and hot pull total deformation rate > 80%.
Preferably, the diameter of the TC4ELI titan alloy casting ingot is 380-480mm.
Preferably, the technique of ingot formation is in step (3), fire time deformation rate > 38%, use electric furnace heating temperature for
950-1050 DEG C, keep the temperature 1-2 hours.
Preferably, it in the preparation process of step (2) TC4ELI titan alloy casting ingot, is carried out using vacuum consumable electrode arc furnace secondary
The specific method of melting is, by new component intermediate alloy, titanium sponge ingredient, mixed raw material to be squeezed on a hydraulic press,
Consutrode block is made, plasma vacuum welds unit and welds consutrode, the melting of first time consumable electrode vacuum furnace is carried out, after melted
Carry out a vacuum consumable ingot casting reconditioning；Secondary smelting welds consutrode using vacuum welding unit, carries out second of vacuum certainly
Furnace melting is consumed, carries out the ingot casting reconditioning of secondary vacuum consumable after melted.
Using the above scheme, the invention has the following advantages that
(1) present invention is using among vanadium-aluminium and benefit aluminium is together again by the way of vacuum melting, aluminium directly by being designed to
Divide disposably to supply and carry out being smelted into new ingredient vanadium-aluminium intermediate alloy in aluminothermic process vanadium-aluminium intermediate alloy, avoids melting
Ingot casting supplements regional segregation caused by simple substance aluminium element.Meanwhile, vacuum melting new component theoretical according to microalloying complex intensifying
Add people micro titanium alloy neutrality intensified element tin and zirconium, micro refinement crystal grain element rare earth during intermediate alloy.It can
Enough comply fully within the scope of national and foreign standards that (TC4ELI titanium alloy other elements content single-element < 0.1%, other elements are total
With the regulation of < 0.3), it can also guarantee the uniformity of these microelements；
(2) in order to guarantee that ingot casting principal component and microelement, impurity do not generate segregation, uniform quality, TC4ELIT titanium alloy
Using vacuum consumable electrode arc furnace melting, diffusion of alloy elements and homogenization are convenient in secondary vacuum melting；
(3) for TC4ELI stick/wire rod of diameter < 30mm, using drawing working process, the control of drawing temperature for lower than
It 100-160 DEG C of transformation temperature, ensure that hot pull carries out at a temperature of (alpha+beta) two-phase, stablize TC4ELI titanium alloy performance.
Specific embodiment
Experimental method in following embodiment is conventional method unless otherwise required, related experiment reagent and material
Material is conventional biochemical reagent and material unless otherwise required.
Invention realizes in a kind of completely new critical field at home and abroad TC4ELI titanium alloy principal component design theory and miscellaneous
Quality control method: the intermediate alloy manufacturing method of principal component region microsegregation is prevented；Microalloy is multielement enhanced；Ultralow N, H, C are miscellaneous
Matter content and microelement refine crystal grain.
One, prepared by new component intermediate alloy
In domestic traditional TC4ELI titanic alloy machining material manufacturing process, ingot casting melting aluminium, vanadium is with intermediate alloy
What method was added.The intermediate alloy that melting ingredient uses is vanadium-aluminium intermediate alloy of aluminothermic process production.In this method manufacture
Between alloy, produced under atmospheric environment, the impurity contents such as O, C, N are difficult to control, and the content of V is even more that each furnace intermediate alloy is uniform
Property all can not be consistent.Intermediate alloy quality is the important factor in order of titan alloy casting ingot quality, and then affects stick, wire rod matter
Amount.
The present invention is to avoid these problems, and to reach ultralow impurity element, Al, V ratio are rationally uniform, while reinforcing is added
The purpose that titanium alloy element refines the microelement of crystal grain designs and produces process route using entirely different intermediate alloy.
1. purifying method new component intermediate alloy designs
Domestic traditional TC4ELI titan alloy casting ingot production distribution is: vanadium-aluminium intermediate alloy of aluminothermic process production adds
Fine aluminium mends aluminium ingredient.Since the method for mending aluminium is to add aluminum shot in vanadium-aluminium intermediate alloy packet, it be easy to cause the region microsegregation of aluminium.
So the present invention is among the vanadium-aluminium and benefit aluminium is together again by the way of vacuum melting, aluminium is directly pressed design
Ingredient is disposably supplied to carry out being smelted into new ingredient vanadium-aluminium intermediate alloy in conventional aluminothermic process vanadium-aluminium intermediate alloy, keeps away
Regional segregation caused by melting ingot casting supplement simple substance aluminium element is exempted from.Meanwhile it is theoretical according to microalloying complex intensifying, vacuum is molten
Refine new component intermediate alloy adds people micro titanium alloy neutrality intensified element tin and zirconium, micro refinement crystal grain element dilute in the process
Soil.Can either comply fully within the scope of national and foreign standards (TC4ELI titanium alloy other elements content single-element < 0.1%,
The regulation of his element summation < 0.3%), it can also guarantee the uniformity of these microelements.
Raw material: vanadium-aluminium intermediate alloy (V > 55%) of conventional aluminothermic process production, fine aluminium grain (Al > 99.8%), pure tin
Grain (Sn > 99.8%), sponge zirconium, rare earth (RE > 99%)
2. new component intermediate alloy produces
It is added in vacuum electron beam furnace, sufficiently examines above-mentioned raw materials by design ingredient using vacuum electron beam furnace melting
Consider scaling loss factor, refine under high vacuum state, effectively remove impurity element, it is new that melting is made that ingredient is uniform, impurity content is low
Ingredient intermediate alloy ingot casting, it is spare that Mechanical Crushing is processed into master alloy particle.
New component intermediate alloy ingredient are as follows:
O < 0.06%, N < 0.01%, C < 0.01%, Fe < 0.15%, 0 < Sn < 0.1%, 0 < Zr < 0.1%, 0
< RE < 0.1%, surplus are V and Al, and V:Al=4:6.
Two, prepared by TC4ELI. titan alloy casting ingot
1. raw material: 1. 2. 0 grade of titanium sponge of little particle passes through 2. titan alloy casting ingot of the new component intermediate alloy life of vacuum melting
The deciding factor that control is titanic alloy machining material amount height is produced, TC4ELIT titanium alloy uses vacuum consumable electrode arc furnace melting,
Secondary vacuum melting, ingot diameters control within the scope of 380mm-480mm.This is because the cooling speed of vacuum consumable water jacketed copper crucible
Degree is limited, and in the certain situation of speed of melting, the accumulation of fusion process heat, ingot solidification speed is also variation.Therefore
In order to guarantee ingot casting principal component and microelement, impurity does not generate segregation, uniform quality, and speed of melting will according to circumstances and melting
The position that ingot casting reaches is adjusted.Principle is that speed of melting is lower than pure titanium, is convenient for diffusion of alloy elements and homogenization.
The TC4ELI titan alloy casting ingot technological process of production:
--- hydraulic press is crushed to consutrode block --- plasma vacuum welding that intermediate alloy+titanium sponge ingredient is blended
Unit welds a consutrode --- consumable electrode vacuum furnace melting --- a vacuum consumable ingot casting reconditioning --- group weldering secondary vacuum
--- secondary vacuum consumable smelting --- secondary vacuum consumable ingot casting --- removes ingot casting riser, machining is gone to consumable smelting electrode
--- detecting a flaw, sampling analysis ingredient --- except ingot casting surface layer (strips off the skin), ingot casting storage is spare.
3. ingot chemistry control range (on ingot casting, in, under):
O < 0.10%, H < 0.005%, N < 0.01%, C < 0.03%, Fe < 0.15%, 6.10%≤Al≤
6.20%, 4.10%≤V≤4.20%, 0 < Sn < 0.09%, 0 < Zr < 0.09%, 0 < RE < 0.03%, surplus Ti.
Ingot chemistry control range be much higher than national standard and international standard, ensure that stick, line products material it is highly reliable
Property.
Three, TC4ELI titanium alloy bar (line) material production technology
1. titanium alloy bar (line) material production technology specifically includes that titan alloy casting ingot cogging, blank finishing, hot rolling (heat rotation
Forging), drawing, annealing, descale, straightening, polishing, a series of production processes of defect detecting test.TC4ELI titanium alloy bar (line) material
Steady production key be production process above method control.
Above-mentioned process are as follows:
Titan alloy casting ingot founding --- ingot casting hammer cogging --- polishing finishing blank --- hot rolling (hot-swage) --- heat
Drawing --- stripping oxide skin processing --- alignment --- polishing --- finishing polish --- flaw detection --- Mechanics Performance Testing --- at
Product storage.
2. ingot formation:
1500 tons or more hydraulic rapid forging press coggings, fire time deformation rate > 38%.Electric furnace heating, heating temperature: 950-1050
DEG C, keep the temperature 1-2 hours.
1. for the TC4ELI bar of diameter > 30mm, blank that the ingot casting by vacuum melting three times is forged into
Heating, is directly shaped with hot-rolling mill (hot-swage).
Electric furnace heating, 850-960 DEG C of temperature, soaking time 30-60 minutes.
The bar of hot rolling (hot-swage) manufacture is machined descale, polishing, defect detecting test, mechanical property by alignment
It can test, warehousing finished products.
2. being the most frequently used specification of biological medical titanium alloy for diameter < 30mm TC4ELI stick, wire rod, to pass through drawing
Working process.
3. one of core of the invention technology is exactly stick to these specifications, wire drawing technology.According to finished product stick,
The specification of wire rod, hot rolling (hot-swage) product carry out further drawing processing as blank.TC4ELI be two-phase titanium alloy (α+
β), resistance of deformation is larger, and ordinary room temperature drawing can not carry out at all.It has to reach the Alloy during Superplastic temperature hot pull and be only
Most viable method, therefore the present invention is specially to develop tubular type continuous furnace hot-drawn drawing machine, drawing speed is adjustable.Lubricant
To develop five yuan of compounds of powdery certainly.
Hot pull temperature has decisive influence to stick, line tissue and mechanical performance, to guarantee that TC4ELI titanium alloy performance is steady
Fixed, hot pull must carry out at a temperature of (alpha+beta) two-phase.Due to the difference of every batch of ingot chemistry, transformation temperature is different, first
First to measure (alpha+beta) of the batch titanium alloy -- β phase transition temperature formulates hot pull temperature according to transformation temperature.Temperature controls model
It encloses are as follows: hot pull temperature is lower than 100-160 DEG C of transformation temperature.Secondly, according to stick to be processed, the whole hot pull linear velocity of line gauge style and
Pass reduction, total deformation rate > 80%.
The stretched peeling processing of hot-drawn spike pulling, line is straightened, and is polished, finishing polish, flaw detection processing, mechanical property is surveyed
Finished product stick, wire rod are completed in examination, manufacture.
4.TC4ELI titanium alloy bar (line) material mechanical performance index
Tensile strength σ b:950-1080MPa
Yield strength σ 0.2:850-990MPa
Elongation percentage δ: > 18%
Contraction percentage of area Ψ: > 30%
Kie > 53MPa ∫m﹋
Metallographic structure reaches GB/T13810-2016A1-A3 rank.
It will be apparent to those skilled in the art that can make various other according to the above description of the technical scheme and ideas
Corresponding change and deformation, and all these changes and deformation all should belong to the protection scope of the claims in the present invention
Within.
Claims (5)
1. a kind of manufacturing method of biological medical titanium alloy TC4ELI stick/wire rod, it is characterised in that: the following steps are included:
(1) preparation of new component intermediate alloy
Vacuum melting is carried out using the vanadium-aluminium intermediate alloy and benefit aluminium of aluminothermic process production, is added in Vacuum Melting micro-
Measure intensified element tin and zirconium and micro refinement crystal grain element rare earth, manufactured new component intermediate alloy ingredient are as follows: O <
0.06%, N < 0.01%, C < 0.01%, Fe < 0.15%, 0 < Sn < 0.1%, 0 < Zr < 0.1%, 0 < RE < 0.1%,
Surplus is V and Al, and V:Al=4:6；
(2) preparation of TC4ELI titan alloy casting ingot
By new component intermediate alloy, titanium sponge ingredient, secondary vacuum melting is carried out using vacuum consumable electrode arc furnace, TC4ELI titanium closes
The ingredient of golden ingot casting are as follows: O < 0.10%, H < 0.005%, N < 0.01%, C < 0.03%, Fe < 0.15%, 6.10%≤Al
≤ 6.20%, 4.10%≤V≤4.20%, 0 < Sn < 0.09%, 0 < Zr < 0.09%, 0 < RE < 0.03%, surplus are
Ti；
(3) TC4ELI titanium alloy bar/wire rod preparation
For TC4ELI stick/wire rod of diameter > 30mm, preparation process are as follows: ingot formation, blank finishing, hot rolling, deoxidation
Skin, straightening, polishing, defect detecting test；
For diameter≤30mm TC4ELI stick/wire rod, preparation process are as follows: ingot formation, hot rolling, drawing, moves back at blank finishing
Fire, descale, straightening, polishing, defect detecting test.
2. the manufacturing method of biological medical titanium alloy TC4ELI stick/wire rod according to claim 1, it is characterised in that: step
Suddenly in (3) TC4ELI titanium alloy bar/wire rod preparation process, for diameter≤30mm TC4ELI bar, its Hubbing method is,
First measurement TC4ELI titanium alloy from alpha+beta mutually to the phase transition temperature of β phase, hot pull temperature be lower than 100-160 DEG C of phase transition temperature, and
Hot pull total deformation rate > 80%.
3. the manufacturing method of biological medical titanium alloy TC4ELI stick/wire rod according to claim 1, it is characterised in that: institute
The diameter for stating TC4ELI titan alloy casting ingot is 380-480mm.
4. the manufacturing method of biological medical titanium alloy TC4ELI stick/wire rod according to claim 1, it is characterised in that: step
Suddenly the technique of ingot formation is in (3), and fire time deformation rate > 38% uses electric furnace heating temperature for 950-1050 DEG C, keeps the temperature 1-2
Hour.
5. the manufacturing method of biological medical titanium alloy TC4ELI stick/wire rod according to claim 1, it is characterised in that: step
Suddenly in the preparation process of (2) TC4ELI titan alloy casting ingot, use vacuum consumable electrode arc furnace carry out secondary smelting specific method for,
By new component intermediate alloy, titanium sponge ingredient, mixed raw material is squeezed on a hydraulic press, consutrode block is made, etc.
Ion vacuum welds unit and welds consutrode, carries out the melting of first time consumable electrode vacuum furnace, carries out a vacuum consumable after melted
Ingot casting reconditioning；Secondary smelting welds consutrode using vacuum welding unit, second of consumable electrode vacuum furnace melting is carried out, after melted
Carry out the ingot casting reconditioning of secondary vacuum consumable.
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| CN112296120A (en) * | 2020-10-30 | 2021-02-02 | 西安圣泰金属材料有限公司 | Method for processing high-strength TC4 titanium alloy ultrafine grain wire for medical treatment |
| CN112877566A (en) * | 2021-01-11 | 2021-06-01 | 复旦大学附属中山医院 | Low-clearance medical titanium alloy TC4ELI and preparation method thereof |
| CN113528893A (en) * | 2021-07-21 | 2021-10-22 | 西安圣泰金属材料有限公司 | TC4ELI titanium alloy for ultrasonic scalpel and production method of titanium alloy bar |
| CN113684384A (en) * | 2021-07-09 | 2021-11-23 | 宝鸡安钛泽科技金属有限公司 | Manufacturing method of low-clearance high-vanadium titanium alloy for sports equipment |
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