CN101068945A - Method for manufacturing titanium alloy wire with enhanced properties - Google Patents

Method for manufacturing titanium alloy wire with enhanced properties Download PDF

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Publication number
CN101068945A
CN101068945A CNA2005800243125A CN200580024312A CN101068945A CN 101068945 A CN101068945 A CN 101068945A CN A2005800243125 A CNA2005800243125 A CN A2005800243125A CN 200580024312 A CN200580024312 A CN 200580024312A CN 101068945 A CN101068945 A CN 101068945A
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Prior art keywords
titanium alloy
crystal grain
tib
size
strongthener
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CNA2005800243125A
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CN101068945B (en
Inventor
威廉·M·哈努斯科
杰瑞·L·菲尔德斯
维森特·哈罗德·哈曼德
罗伯特·刘易斯·格拉博
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FMW Composite Systems Inc
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FMW Composite Systems Inc
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
    • 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
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C22C1/1042—Alloys containing non-metals starting from a melt by atomising
    • 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
    • B21C1/00—Manufacture of metal sheets, metal wire, metal rods, metal tubes by drawing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/12—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of wires
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Metal Extraction Processes (AREA)
  • Forging (AREA)

Abstract

A method for producing reinforced titanium alloy wire, comprising forming a billet of titanium alloy with grains of a precipitated discontinuous reinforcement material such as TiB and/or TiC. The billet may be formed by the hot consolidation of a titanium alloy powder formed by gas atomization. The billet is then hot formed to reduce it to rod or coil form. The rod or coil is then subjected to successive cold drawing operations to form a reinforced titanium alloy wire of reduced diameter. The cold drawing includes periodic annealing operations under low oxygen conditions to relieve work hardening and to recrystallize the reinforcement material grains to reduce the size thereof.

Description

Manufacturing has the method for the titanium alloy wire that strengthens characteristic
Technical field
The present invention relates to a kind of method of making titanium alloy wire, more particularly, relate to a kind of like this method, in the method, the precipitated discontinuous particulate of strongthener such as TiB and/or TiC (precipitateddiscontinuous particulates) is added in the alloy, and this alloy is by a kind of novelty, the processing of improved method, thereby the feasible alloy strength that is caused by particulate becomes big.
Background technology
About making common alloy of titanium by adding TiB and/or TiC particulate, promptly Ti-6Al-4V is reinforced with the enhanced method early report in the document.The Ti-6Al-4V alloy is widely used in aviation field and is one of the most cheap alloy.Aviation design bound pair is the sort of not to need to spend enhancing (enhancement) characteristic that advantageous application scope that great amount of cost just can make this kind alloy enlarged great interest.In above-mentioned reported method, TiB and/or TiC additive were added in the melts before casting, formed the Ti-6Al-4V foundry goods then.These additives in described melts, dissolve and in process of cooling recrystallize, strengthen body (discontinuous reinforcement) thereby form discontinuity with various different sizes.(hotisostatic pressing, HIP) and the article of the extrusion molding tensile strength and the tensile modulus of having showed this improvement, they depend on the concentration of TiB and/or TiC additive by hot isostatic pressing.
The above results shows: the quantity of the raising of performance and the discontinuous enhancing body of generation and the enhancing body crystalline size of generation are relevant.That is to say, the volume content that people expect to strengthen body up to 40% and the size that strengthens body in ultra-fine size range.But, in known method, content exceeds the enhancing body of a little percentage point mainly in maximum sized section, and the dimensional change that strengthens body is in extensive range, and along with the level of the volume content that strengthens body towards optimal 20%-40% increases, strengthening body has increased to the transformation of large-size.This is the result that big crystal grain is removed less crystal grain in casting or manufacturing processed, and this result obviously is an inherent in these processes.This limitation has seriously suppressed the potential performance of discontinuous enhancement type titanium.
The novel method of improvement of the present invention does not have above-mentioned shortcoming, and have with or the currently known methods advantage that can not have.
Summary of the invention
The inventive method relates generally to make and is fit to the titanium alloy wire that cable/Optical Fiber Composite material is used, and it mainly comprises: the step that forms required alloy by casting ingot or gas atomization; Heat forged is so that produce the step of uniform chemical property and microstructure; Form the step that diameter for example is about 0.2 inch web or coiled material; Cold drawn precedent such as diameter are about the step of 0.005 inch wire rod.
More clearly, a kind of preferred method comprises: form the titanium alloy powder by gas atomization from the melts that is rich in boron; At about 5000-45000psi for example under the pressure of 15000psi, under the temperature of about 1650-1750 , use hot isostatic pressing that described powder metal is solidified into the bar shape, up to completely solidified, change under the required condition but remain on β, to avoid grain growing and boundary segregation; When temperature is approximately 1500-2100 , 1750  for example, hot rolling to be reducing into described bar web shape or coiled material shape, and finishes the initial decomposition of big TiB crystal grain; With the approximately cold drawn and annealing of economy of every time 10%-20%, to avoid cracking.The method according to this invention, the frequency that is increased in annealing steps under the utmost point hypoxia condition are to be used for alleviating work hardening, also are used for recrystallize TiB crystal grain to accurate dimension, and TiB crystal grain and alignment.This method novel, improvement can be made meticulous titanium alloy wire, can realize that TiB strengthens the raising of body burden and strengthens reducing of body grain-size simultaneously.Other strongtheners such as TiC can use separately, or unite use with TiB.
Embodiment
The method for manufacturing wire of the precipitation by will strengthening body and a kind of new improvement combines, thereby is strengthening body burden when very high even the inventive method is developed into, and the enhancing body of fine grain shape still can be in the great majority.Typically be applicable to what cable/Optical Fiber Composite thing was used, as United States Patent (USP) the 5th, 763, No. 079 described thin wire working method comprises four kinds of main operations, promptly, form required alloy by casting ingot, produce uniform chemical property and microstructure by heat forged, form diameter by heat forming technology and be about 0.2 inch bar (or coiled material), and cold drawn one-tenth diameter is about 0.005 inch wire rod.During cold drawn, need to carry out the process annealing operation,, thereby carry out more stretched operation so that eliminate unrelieved stress and recover ductility.This basic wire rod forms technology and is used for minimum operation sequence, the minimum contraction that influences the successional fracture of length and realize section by thermoforming, hot extrusion and final cold drawing operation.
Can find according to the present invention: the wire stretching course of processing can be designed or revise, thereby not only can realize the basic purpose that section shrinks, but also the evolution of may command microstructure.Wire stretching method of the present invention can realize the microstructure of improvement in high melting point alloy (difficult alloys), and this all can not realize with other any methods, and, this method is developed into is used to produce discontinuous enhancement type Ti-6Al-4V alloy, realizes that simultaneously TiB content increases and strengthen the purpose that the body grain-size diminishes.
Wire rod formation method of the present invention with the Ti-6Al-4V alloy-steel casting that obtains from the melts that is rich in boron to start with.Described TiB will precipitate when cooling, but rate of cooling (cooling rate) will cause undesirable big TiB grain growing.For from best microstructure, preferably use the powder metal that forms by gas atomization (gas atomization) by the melts that is rich in boron, and do not use foundry goods.Described powder forms technology and uses than casting technique cooling process faster, and its possibility that produces big TiB crystal grain is littler.In this method, use powder metallurgy technology to prepare the uniform blank of component (compositionally uniform billet), the inherent grain growing separates (chemical segregation) in the casting technique with the potential chemofacies to avoid.The above-mentioned metal alloy powders that forms of making from the Ti-6Al-4V alloy that is rich in boron at first is thermoformed into its size and has the bar that industrial wireform forming apparatus is complementary now.Described bar is hot rolled into web or the coiled material that diameter is about 0.2 inch, and this web or coiled material are transferred in the cold drawing operation then.
This fact is found: promptly selects rational cold drawn processing conditions can cause forming ductile small diameter fine wire, and can cause the successful formation of required wire microstructure, that is, and higher concentration and thinner crystal grain.The execution of this modification method need be considered the crucial processing conditions in each operation.Cold drawn section shrinks (area reduction) must be abundant, thereby in each passage centre (core) is arrived in the web cold working of minor diameter, and then keep the consistence of microstructure in whole cross section.But section shrinks can not be excessive, to avoid when the diameter of web or coiled material reduces, forms fracture (fracture), tiny crack (microcracking) or cavity (void) in web or coiled material.In the cold drawn starting stage, owing to have bigger TiB crystal grain, so material easily forms tiny crack and cavity in the zone with big TiB crystal grain.When the TiB of maximum crystal grain exists, in the starting stage of reduction operation, it is more difficult shrinking with avoiding keeping balance between tiny crack and the empty formation at section, and when the TiB grain-size was reduced, process window (processingwindow) had enlarged.
Cold drawn complete processing of the present invention is used for decomposing big TiB crystal grain and does not form deleterious tiny crack or cavity.We find: for the frequent annealing steps that alleviates work hardening (work hardening) and increase also will recrystallize TiB crystal grain to an accurate dimensions, and TiB crystal grain and alignment.Annealing steps has been applied in the known wire stretching operation, but the low and lasting time weak point of the usage frequency of its annealing steps.According to the present invention, the increase of annealing steps usage frequency, improved annealed demand under the utmost point hypoxia condition,, thereby may hinder TiB to strengthen body processing with the surfacing excessive loss of avoiding causing by oxygen gas pollution and the gap oxygen (oxygen interstitial) that obtained by wire rod metallurgy.Therefore, the inventive method can realize the manufacturing of meticulous titanium alloy wire, can obtain higher enhancing body of content and the less enhancing body crystal grain of size simultaneously.
According to a preferred embodiment of the inventive method, a kind of acceptable powdered alloy be comprise Ti-6Al-4V-1.7B component, size range for-35 orders (mesh) to+270 purpose gas atomization spherical powders.A kind of acceptable gap component (interstitial content) is the oxygen of content less than 1500ppm.The powder of this character has been used to make synthetic panel, and has been found and can produces uniform chemical property and microstructure.Powder metal is solidified into bar-shaped being based on to carry out synthetic panel effective means.For example, determine: uncontaminated curing mold (non-contaminating consolidation tooling) is essential, as vacuum outgas soft steel (vacuum degassed mild steel) or conventional titanium alloy.Be solidified into bar and be by at about 5000-45000psi for example under the temperature condition of the pressure of 15000psi and about 1650-1750 , use the hot isostatic pressing realization.These conditions are solidified completely in order to realization, and maintain safely under the required condition of β transformation, to prevent grain growing and boundary segregation.In about 1500-2100  temperature range, for example hot rolling (hot reduction) during 1750  temperature with so that described bar reduces into web shape or coiled material shape, and is finished the initial decomposition of big TiB crystal grain.Determine: it is effective that about 50: 1 cross section hot rolling rate (hotreduction in section area) is decomposed initial big TiB crystal grain.Follow-up cold-drawing process must carry out enough cold working on the whole thickness direction of web or coiled material, and the growth of annealing and must alleviate work hardening and not having crystal grain.Determine: each passage must have about 10% economy, guaranteeing cold worked abundant consistence, and avoid from the tiny crack and the cavity that form during specific diameter (nominal diameter) is the initial cold drawn step that begins of 0.2 inch condition.Relative reduction in area can increase to each passage and be about 15% mid point up to cross section reduction operation, and 20% the relative reduction in area of may having an appointment when reducing the operation end to the cross section.With the temperature of about 1200-2000 , for example, the temperature of 1750  with about 1 hour of rare gas element cooling (the forced inert gas cooling) annealing of pressurization, just can fully be eliminated work hardening in rare gas element, recrystallize TiB with avoid grain growing.Annealing is interrupted to be carried out, and the corresponding accumulation of each annealed time point sectional shrinkage is approximately 50%.
Aforesaid method of the present invention is produced has the Ti-6Al-4V alloy that volumetric concentration is the fine-grain shape TiB enhancing body of 1%-50%, and described enhancing body aligns with the axle center of wire rod.This method is effective to multiple titanium alloy, for example Ti-6Al-2Sn-4Zr-2Mo alloy, Ti-6Al-4Sn-4Zr-1Nb-1Mo-0.2Si alloy, Ti-3Al-2.5V alloy, Ti-10V-2Fe-3Al alloy, Ti-5Al-2.5Sn alloy and Ti-8Al-1Mo-1V alloy.And this method strengthens body such as TiC to other precipitated discontinuous equally, or the mixture of TiB and TiC is effective.This method can be used the blank that casting forms from the melts that is rich in boron, but will be caused the increase of the inherent risk that forms tiny crack and cavity by the big TiB grain growing degree that slow refrigerative casting process (slow cooled casting) is caused.After the contraction and annealing conditions of the high relative reduction in area of inherent in conjunction with suitable control provided by the invention, can produce the Ti alloy with high performance wire rod that other any known metallurgical methods all can not be produced in the wire rod formation technology.
Above invention has been described in conjunction with most preferred embodiment, but the present invention is not limited to the embodiment of above announcement, and should contain various modification, equivalent combinations of carrying out according to essence of the present invention.

Claims (26)

1. method of making the enhancement type titanium alloy wire comprises:
Formation contains the precipitated discontinuous reinforcement material billet of titanium alloy with grains;
The described blank of thermoforming is to reduce into it web shape or coiled material shape; And
The wire rod that in subsequent operations, described web or the cold drawn one-tenth diameter of coiled material is diminished, described cold drawing operation is included under the hypoxia condition described wire rod is carried out periodicity annealing, to alleviate work hardening and described strongthener crystal grain is carried out recrystallize, so that reduce its size.
2. the method for claim 1 is characterized in that, described blank before thermoforming by heat forged, to produce uniform chemical property and microstructure.
3. the method for claim 1 is characterized in that, described strongthener is TiB.
4. method as claimed in claim 3 is characterized in that, described blank is to cast to form from the melts that is rich in boron.
5. method as claimed in claim 3 is characterized in that, described blank forms by solidifying titanium alloy powder, and described titanium alloy powder is formed by gas atomization from the melts that is rich in boron.
6. method as claimed in claim 5 is characterized in that, described powder be contain Ti-6Al-4V-1.7B synthetics, size range for-35 orders to+270 orders, interstitial oxygen content gas atomization powder less than 1500ppm.
7. the method for claim 1 is characterized in that, described strongthener is TiC.
8. the method for claim 1 is characterized in that, described strongthener is TiB and TiC.
9. method as claimed in claim 5 is characterized in that, described curing is to be that 15000psi, temperature are that the hot isostatic pressing of 1650-1750  carries out by pressure.
10. the method for claim 1 is characterized in that, described titanium alloy is Ti-6Al-4V.
11. the method for claim 1 is characterized in that, described titanium alloy is Ti-6Al-2Sn-4Zr-2Mo.
12. the method for claim 1 is characterized in that, described thermoforming is to carry out in the temperature of 1750 .
13. method as claimed in claim 12 is characterized in that, described thermoforming causes 50: 1 cross section hot rolling rate, so that decompose the size of strongthener crystal grain and reduction strongthener crystal grain.
14. the method for claim 1, it is characterized in that, described cold drawing operation is periodically to carry out so that reduce the size of described wire rod, and this cold drawing operation preceding half stage of required diameter reduction during with each stretched operation economy be that 10% speed is carried out.
15. method as claimed in claim 14 is characterized in that, described economy increases to 15% when the mid point of diameter reduction, and increases to 20% near the diameter reduction terminal point time.
16. the method for claim 1 is characterized in that, described annealing is meant in rare gas element cooled off 1 hour with pressurized inert gas, and described annealing is interrupted to be carried out, and the gauge or diameter of wire accumulation sectional shrinkage of each annealed time point correspondence is 50%.
17. a method of making the enhancement type titanium alloy wire comprises:
From the melts that is rich in boron, form titanium alloy powder by gas atomization;
Under certain heat and pressure, described titanium alloy powder is solidified into and contains the blank that precipitated discontinuous TiB strengthens body crystal grain;
The described blank of thermoforming, it being reduced into web shape or coiled material shape, and the size of decomposing TiB crystal grain and reduction TiB crystal grain;
The wire rod that in subsequent operations described web or the cold drawn one-tenth diameter of coiled material is diminished, described cold drawing operation are included under the hypoxia condition described wire rod are carried out periodicity annealing, to alleviate work hardening and described TiB crystal grain is carried out recrystallize, so that reduce its size.
18. method as claimed in claim 17 is characterized in that, described powder be contain Ti-6Al-4V-1.7B synthetics, size range for-35 orders to+270 orders, interstitial oxygen content gas atomization powder less than 1500ppm.
19. method as claimed in claim 17 is characterized in that, described titanium alloy is Ti-6Al-4V.
20. method as claimed in claim 17 is characterized in that, described titanium alloy is Ti-6Al-2Sn-4Zr-2Mo.
21. method as claimed in claim 17 is characterized in that, described curing is to be that 15000psi, temperature are that the hot isostatic pressing of 1650-1750  carries out by pressure.
22. method as claimed in claim 17 is characterized in that, described thermoforming is to carry out in the temperature of 1750 .
23. method as claimed in claim 22 is characterized in that, described thermoforming causes 50: 1 the size of hot rolling rate in cross section to decompose strongthener crystal grain and to reduce strongthener crystal grain.
24. method as claimed in claim 17, it is characterized in that, described cold drawing operation is periodically to carry out so that reduce the size of described wire rod, and this cold drawing operation preceding half stage of required diameter reduction during with each stretched operation economy be that 10% speed is carried out.
25. method as claimed in claim 24 is characterized in that, described economy increases to 15% when the mid point of diameter reduction, and increases to 20% near the diameter reduction terminal point time.
26. method as claimed in claim 17 is characterized in that, described annealing is meant in rare gas element cooled off 1 hour with pressurized inert gas, and described annealing is interrupted to be carried out, and the gauge or diameter of wire accumulation sectional shrinkage of each annealed time point correspondence is 50%.
CN2005800243125A 2004-07-22 2005-05-25 Method for manufacturing titanium alloy wire with enhanced properties Expired - Fee Related CN101068945B (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US10/895,885 2004-07-22
US10/895,885 US20060016521A1 (en) 2004-07-22 2004-07-22 Method for manufacturing titanium alloy wire with enhanced properties
PCT/US2005/018492 WO2006022951A2 (en) 2004-07-22 2005-05-25 Method for manufacturing titanium alloy wire with enhanced properties

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CN101068945A true CN101068945A (en) 2007-11-07
CN101068945B CN101068945B (en) 2010-07-14

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US (1) US20060016521A1 (en)
EP (1) EP1784269B1 (en)
JP (1) JP5037340B2 (en)
KR (1) KR101184464B1 (en)
CN (1) CN101068945B (en)
ES (1) ES2385086T3 (en)
WO (1) WO2006022951A2 (en)

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CN102851541A (en) * 2012-09-27 2013-01-02 苏州东海玻璃模具有限公司 TiC particle-reinforced titanium-aluminum-molybdenum-silicon alloy material synthesized in situ and preparation method thereof
CN102851537A (en) * 2012-09-27 2013-01-02 苏州东海玻璃模具有限公司 In-situ synthesis TiC particle enhanced titanium-aluminum-molybdenum-palladium alloy material and method for preparing same

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