CN109338251A - Improve the hot-working method of raw amorphous composite material mechanical property in titanium-based - Google Patents

Improve the hot-working method of raw amorphous composite material mechanical property in titanium-based Download PDF

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CN109338251A
CN109338251A CN201811313062.2A CN201811313062A CN109338251A CN 109338251 A CN109338251 A CN 109338251A CN 201811313062 A CN201811313062 A CN 201811313062A CN 109338251 A CN109338251 A CN 109338251A
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composite material
titanium
amorphous composite
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raw
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王永胜
令狐嵘凯
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Taiyuan University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C45/00—Amorphous alloys
    • C22C45/10—Amorphous alloys with molybdenum, tungsten, niobium, tantalum, titanium, or zirconium or Hf as the major constituent
    • 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
    • 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
    • C22C1/11—Making amorphous alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18—High-melting or refractory metals or alloys based thereon
    • C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

Improve the hot-working method of raw amorphous composite material mechanical property in titanium-based, raw amorphous composite material is by atomicity percentage Ti in the titanium-based40Zr24V12Cu5Be19；Strain rate range is 0.0001/s ~ 0.01/s when the amorphous composite material is heated to supercooled liquid phase temperature range, keeps the temperature 3 ~ 10 minutes, deformation and deflection is after 4% ~ 40% dependent variable, and atmospheric environment is cooled to room temperature.It is 1510MPa ~ 1960MPa that amorphous composite material of the invention, which has yield strength, and breaking strain is 24.5% ~ 3.6% performance.The present invention has the advantages that prepare high-intensitive, high-ductility composite material by amorphous composite material tissue raw in optimizing.

Description

Improve the hot-working method of raw amorphous composite material mechanical property in titanium-based
Technical field
The invention belongs to technical field of composite materials, are related to a kind of amorphous composite wood for improving raw crystal phase toughening in titanium-based Expect the secondary deformation processing method of room-temperature mechanical property.This method is equally applicable to other by interior raw crystal phase and amorphous phase group At amorphous composite material.
Background technique
Atomic structure of the titanium-based amorphous alloy because of its confusing array, the mechanical property for having crystal alloy incomparable, such as High intensity, high rigidity, elastic property are excellent etc., it is made to have huge application prospect in Aeronautics and Astronautics field.However, amorphous Alloy At Room Temperature deformation realizes that tension failure seriously constrains its structure work without any plasticity by the shear band of height local Cheng Yingyong.The interior titanium-based amorphous composite material of life is the in-situ preparation β titanium dendrite on noncrystal substrate, has crystal titanium alloy and titanium-based concurrently Big " processing hardening " stage is presented in the advantages of amorphous alloy, room temperature.Compared with conventional titanium alloy, Ti44Zr20V12Cu5Be19It is non- Not only intensity high (1640 MPa of tensile strength), plasticity high (tension failure strains 15.5 %), toughness height (are broken crystal composite material Toughness is between 43.8-61.6 MPa m1/2), also there is low (the 4.97-5.2 g/cm of density3), specific strength height (315 MPacm3/ G) the advantages that.In addition, this kind of material unlike single-phase amorphous is by the stringent restriction of glass forming ability, does not need to form full amorphous Phase, is capable of forming large-sized ingot casting, such as Zhang Haifeng cast out 150 g, diameter up to 50 mm Ti50Zr23Ni3Cu6Be18It is non- Crystal composite material.Therefore, the titanium-based amorphous composite material of interior life has weight in fields such as Aeronautics and Astronautics, automobile, building, sports goods The application prospect wanted.
Existing research shows amorphous alloy 0.7T gOccur when deformed above uniform rheology (T gFor glass transition point),T x It is above occur crystallization behavior (T xFor crystallization temperature).Newton rheology, resistance of deformation occur when amorphous alloy supercooling liquid phase region deforms Very low, superior superplastic forming ability is presented in sample entirety homogeneous deformation, and especially Nieh etc. has found lanthanum base amorphous supercooled liquid phase Area can realize 20000% stretcher strain.Therefore, the enterprises such as science and technology are preferably pacified to single-phase amorphous by U.S.'s liquid metal company, China Alloy is shaped in supercooled liquid phase humidity province, obtains all polyisocyanate row parts, this is the thermo forming of single-phase amorphous alloy And engineer application provides a good way for.But its brittleness at room temperature is still unresolved after single-phase amorphous alloy hot-working, still not It can be used as structural member engineer application on a large scale.For this purpose, studying people for internally giving birth to the titanium-based amorphous composite material of β-Ti toughening Member develops two kinds of optional approach: first is that being processed and formed at one time by supercooled liquid phase temperature range, another is to pass through copper mold Technique.However, supercooled liquid phase temperature range, which is processed and formed at one time amorphous composite material technique, requires complexity, high vacuum height is such as required Pure argon environment etc.；Casting sample is influenced by copper mold cooling rate, it is difficult to prepare larger size or anisotropic approach part, generally Sample dimensions are grade, while the material cast out is difficult to the defects of avoiding loose shrinkage cavity.It is multiple that this is unfavorable for this kind of Metal Substrate The actual processing of condensation material forms and its Structural Engineering application.
Summary of the invention
Present invention aims at by inhale the amorphous composite material of raw crystal phase toughening in the obtained titanium-based of casting process into Row secondary deformation is processed to improve the room-temperature mechanical property of the material, to obtain high-intensitive and good plasticity amorphous composite wood Material.The present invention provides a kind of method for being effectively improved interior raw amorphous composite material temperature-room type plasticity and work hardening capacity, and work Skill is simple and easy.
Technical solution of the present invention: the hot-working method of raw amorphous composite material mechanical property in improvement titanium-based, including under State content:
(1) raw material are prepared
Each constituent element metal is pressed into atomicity percentage Ti40Zr24V12Cu5Be19Match 30 g of raw material, wherein titanium, zirconium, vanadium or copper are pure Spend >=99.9 %, purity >=97.0 % of beryllium；With high vacuum non-consumable arc-melting furnace at high-purity argon gas (purity >=99.99%) Protection under melting raw material, melting 4-5 obtains master alloy ingot after；Master alloy ingot is placed in inhale in arc-melting furnace and casts diameter It is 5 mm, the titanium-based amorphous composite sample of length >=50 mm column.
(2) secondary deformation processing technology
The first step, fromThe titanium-based amorphous composite material of columnIt is upper cutting ratio of height to diameter be 1:1 to 2:1 sample, respectively with 240#, 400#, 600#, 800#, 1000# abrasive paper for metallograph polish sample both ends；
Second step, the sample that the first step is obtained are placed in the sample deposition for being equipped with the mechanics machine of high temperature service, by power It learns testing machine to be heated to supercooled liquid phase temperature range (613K-680 K), keeps the temperature 3-10 minutes；
Third step carries out pressure-loaded to the sample that second step is completed, and load strain rate is 0.0001-0.01/s, by sample pressure (corresponding compressive deformation strain is 5 %-40 % for unloading after being reduced to certain displacement；
4th step, the sample after unloading take out rapidly heating furnace, are cooled to room temperature in atmospheric environment；
5th step, the institutional framework of detection the 4th step gained sample test its room-temperature mechanical property.(1) material structure, tissue, Performance characterization
Steps are as follows for sample detection after secondary deformation is processed:
(1) structure detection: the detection sample of 1-2 mm is intercepted from cylindric sample with diamond slice machine, is ground with abrasive paper for metallograph Flat detection specimen surface (240#, 600#, 1000#, 1500#) carries out X ray to detection sample with X x ray diffractometer x and spreads out Spectral line scanning is penetrated, scanning angle range is 20o~80o, scanning speed 3o/min；
(2) structure observation: with diamond slice machine from cylindric sample intercept 1-2 mm from sample, then use metallic phase mounting Model machine by the sample intercepted inlay at diameter be 20 mm, highly be 20 mm pre-grinding sample；Then pass through standard metallography microscope Technology shows the tissue of sample；
(3) Mechanics Performance Testing:First two steps are chosen by structure detection and structure observationTissue is amorphous phase and crystal phase two-phase Amorphous composite material sample, room temperature carry out Mechanics Performance Testing, obtain optimization technique.
Beneficial effects of the present invention: the present invention internally gives birth to amorphous composite material in supercooling liquid phase region and carries out hot-working, wherein Noncrystal substrate is homogeneous deformation in supercooling liquid phase region, but crystal phase passes through dislocation motion (such as dislocation when the temperature range deforms Increase and plug product) it realizes.By reasonable constituency composite system, regulation deformation temperature and strain rate, can be effectively improved Interior raw amorphous composite material temperature-room type plasticity and work hardening capacity, so that it is compound to obtain high-intensitive and good plasticity interior raw amorphous Material.The present invention has the advantages that prepare high-intensitive, high-ductility composite material by amorphous composite material tissue raw in optimizing. The present disclosure additionally applies for other amorphous composite materials by interior raw crystal phase and amorphous phase composition, multiple to carry forward vigorously interior raw amorphous The molding of condensation material actual processing provides theory and practice foundation with Structural Engineering application.
Detailed description of the invention
Fig. 1 is that ingredient is Ti40Zr24V12Cu5Be19The X x ray diffration pattern x of 3 mm ingot casting of composite material；
Fig. 2 is that ingredient is Ti40Zr24V12Cu5Be19The micro-organization chart of 3 mm ingot casting of composite material；
Fig. 3 is that ingredient is Ti40Zr24V12Cu5Be19The room temperature compression stress strain curve figure of 3 mm ingot casting of composite material；
Fig. 4 is that ingredient is Ti40Zr24V12Cu5Be19X x ray diffration pattern x after the processing of 3 mm ingot casting secondary deformation of composite material, Deflection is 4.9 %；
Fig. 5 is that ingredient is Ti40Zr24V12Cu5Be19(deflection is 4.9 %) is aobvious after the processing of 3 mm ingot casting secondary deformation of composite material Micro-assembly robot figure；
Fig. 6 is that ingredient is Ti40Zr24V12Cu5Be19After the processing of 3 mm ingot casting secondary deformation of composite material (deflection is 4.9 %) Room temperature compression stress strain curve figure；
Fig. 7 is that ingredient is Ti40Zr24V12Cu5Be19X x ray diffration pattern x after the processing of 3 mm ingot casting secondary deformation of composite material, Deflection is 8.5%；
Fig. 8 is that ingredient is Ti40Zr24V12Cu5Be19(deflection is 8.5 %) is aobvious after the processing of 3 mm ingot casting secondary deformation of composite material Micro-assembly robot figure；
Fig. 9 is that ingredient is Ti40Zr24V12Cu5Be19After the processing of 3 mm ingot casting secondary deformation of composite material (deflection is 8.5 %) Room temperature compression stress strain curve figure.
Fig. 1 is that ingredient is Ti40Zr24V12Cu5Be19The X x ray diffration pattern x of 3 mm ingot casting of composite material.As shown in Figure 1, titanium Base amorphous composite material is made of β-titanium phase and noncrystal substrate.Fig. 2 is that ingredient is Ti40Zr24V12Cu5Be193 mm of composite material casting The micro-organization chart of ingot further proves the composite material microstructure by two phase compositions.
Fig. 3 is that ingredient is Ti40Zr24V12Cu5Be19The room temperature compression stress strain curve figure of 3 mm ingot casting of composite material.By Fig. 3 is it is found that the composite material room temperature compressive deformation stress-strain diagram, yield strength 1510MPa, breaking strain 24.5 %。
Fig. 4, Fig. 5 and Fig. 6 are Ti40Zr24V12Cu5Be19(deflection is after the processing of 3 mm ingot casting secondary deformation of composite material 4.9 %) X x ray diffration pattern x, micro-organization chart and room temperature compression stress strain curve figure.By Fig. 4, Fig. 5 and Fig. 6 it is found that through After crossing supercooling liquid phase region temperature (650 K) deformation processing, the structure of titanium-based amorphous composite material is still by β-titanium phase and amorphous base Body composition, but microstructure (β-titanium phase) becomes flattening, and room temperature compression yield strength is 1690MPa, breaking strain 5.6%.
Fig. 7, Fig. 8 and Fig. 9 are Ti40Zr24V12Cu5Be19(deflection is after the processing of 3 mm ingot casting secondary deformation of composite material 8.9 %) X x ray diffration pattern x, micro-organization chart and room temperature compression stress strain curve figure.By Fig. 7, Fig. 8 and Fig. 9 it is found that becoming The structure of composite material is still made of β-titanium phase and noncrystal substrate after shape, but microstructure (β-titanium phase) further flattening, Room temperature compression yield strength is 1960MPa, breaking strain 3.6%.In conclusion internally giving birth to amorphous in supercooling liquid phase region temperature Composite material carries out deformation processing, can be effectively improved alloy structure, to obtain high-intensitive and good plasticity interior raw amorphous Composite material.
Specific embodiment
Embodiment one: the present invention provides a kind of amorphous composite material room temperature mechanical property for improving raw crystal phase toughening in titanium-based The secondary deformation processing method of energy can be prepared by this method with high-intensitive, high-ductility amorphous composite material.Its Preparation step includes:
1) ingredient, alloy melting and casting and forming, prepare raw material
Ti, Zr, V, Cu(purity >=99.9 %) and Be(purity >=97.0 %) metal is pressed into atomicity percentage Ti40Zr24V12Cu5Be19Match 30 g of raw material；With high vacuum non-consumable arc-melting furnace at high-purity argon gas (purity >=99.99%) Protection under master alloy melting raw material；Obtained master alloy is placed in inhale in arc-melting furnace and casts 5 mm of diameter, length >=50 The column sample of mm.
2) secondary deformation processing technology improves alloy property
The first step, from ingot casting cut ratio of height to diameter be 1.5:1 sample, with abrasive paper for metallograph polish sample both ends (240#, 400#, 600#, 800#, 1000#), and must assure that sample both ends section is vertical with specimen length direction；
Sample obtained in the previous step is placed in the sample deposition for being equipped with the mechanics machine of high temperature service by second step, by it It is heated to 650 K of supercooled liquid phase temperature range, keeps the temperature 10 minutes；
Third step carries out pressure-loaded to sample, load strain rate is 0.0005/s, by sample pressure after the completion of previous step It is unloaded after being reduced to certain displacement, deforming corresponding strain is 4.9 %；
4th step, the sample after unloading take out rapidly heating device, are cooled to room temperature in atmospheric environment, are cooled within about 5 minutes Room temperature；
5th step, after the completion of previous step, the institutional framework of detection gained sample tests its room-temperature mechanical property.
3) material structure and fabric analysis, mechanical property characterize
Sample after secondary deformation processing is tested and analyzed as follows:
(1) it structure detection: with diamond slice machine from the sample for intercepting 1.5 mm after secondary deformation processing on cylindric sample, uses Abrasive paper for metallograph polishes specimen surface (240#, 600#, 1000#, 1500#), carries out X ray to sample with X x ray diffractometer x The scanning of diffraction spectral line, scanning angle range are 20o~80o, scanning speed 3o/min；
(2) structure observation: intercepting the sample of 1.5 mm with diamond slice machine from cylindric sample, then uses metallographic mounting press Diameter is inlayed into be 20 mm, be highly the pre-grinding sample of 20 mm；Then sample is shown by standard optical microscopy Tissue；
(3) Mechanics Performance Testing: being the amorphous composite material of amorphous phase and crystal phase two-phase by the tissue that first two steps obtain, will It is cut into the compression sample that ratio of height to diameter is 1.5:1, carries out Mechanics Performance Testing in room temperature, obtains optimization technique.
By above-mentioned technique, a kind of amorphous composite material room temperature mechanics for improving raw crystal phase toughening in titanium-based is finally obtained The secondary deformation processing method of performance.This method is equally applicable to other be answered by interior raw crystal phase and the amorphous of amorphous phase composition Condensation material.
Embodiment two: in the secondary deformation processing technology of the present embodiment third step deflection be 8.5 % strain, it is other with it is real It is identical to apply example one.
The present invention carries out secondary deformation processing to the amorphous composite material of crystal phase toughening raw in titanium-based, and by structure with Fabric analysis, mechanical property characterize the room-temperature mechanical property that this method can be effectively improved this kind of material.
It is the explanation in relation to present pre-ferred embodiments above.Here, it should be noted is that, the present invention does not limit to In above embodiments, this method is equally applicable to other amorphous composite materials by interior raw crystal phase and amorphous phase composition.? In the case where meeting the area requirements such as claims, detailed description of the invention and attached drawing, various changes can be carried out to the present invention More implement, and these are within the scope of the program of the present invention.
Illustrate: high vacuum non-consumable arc-melting furnace of the present invention and the patent No. are described in 201210295303.1 High vacuum non-consumable arc-melting furnace is identical.Button ingot mold of the present invention and the patent No. are in 201210295303.1 The button ingot mold is identical.

Claims (3)

1. improving the hot-working method of raw amorphous composite material mechanical property in titanium-based, raw amorphous composite material is in the titanium-based By atomicity percentage Ti40Zr24V12Cu5Be19；It is characterised by comprising:
(1) amorphous composite material raw in titanium-based is heated to supercooling liquid phase region 610K ~ 680K, keeps the temperature 3 ~ 10 minutes；
(2) hot compression deformation is carried out to the sample after the completion of heat preservation, deformation strain rate is 0.0001/s ~ 0.01/s, and deformation is answered Variable is the % of 4 % ~ 40；
(3) sample after the completion of deformation is moved to atmospheric environment to be cooled to room temperature, obtains amorphous composite material
Yield strength is 1510MPa ~ 1960MPa, and breaking strain is 24.5 % ~ 3.6%.
2. improve the hot-working method of raw amorphous composite material mechanical property in titanium-based according to claim 1, it is characterized in that The preparation of raw amorphous composite material is by each constituent element metal by atomicity percentage Ti in titanium-based40Zr24V12Cu5Be19Proportion is former Material, wherein titanium, zirconium, vanadium or copper purity >=99.9 %, purity >=97.0 % of beryllium；Existed with high vacuum non-consumable arc-melting furnace Melting under the protection of the high-purity argon gas of purity >=99.99%, melting 4-5 obtain master alloy ingot after；Master alloy ingot is placed in electric arc Inhaling in smelting furnace and casting diameter is 5 mm, the titanium-based amorphous composite material of length >=50 mm column.
3. improve the hot-working method of raw amorphous composite material mechanical property in titanium-based according to claim 1, it is characterized in that Sample detection includes following content:
(1) the detection sample for intercepting 1-2 mm on raw amorphous composite material out of titanium-based with diamond slice machine, uses abrasive paper for metallograph Detection specimen surface is polished, the scanning of X x ray diffraction spectral line, scanning angle model are carried out to detection sample with X x ray diffractometer x It encloses for 20o~80o, scanning speed 3o/min；
(2) sample from intercepting 1-2 mm on raw amorphous composite material out of titanium-based with diamond slice machine, then uses metallographic Mounting press by the observation sample intercepted inlay at diameter be 20 mm, highly be 20 mm pre-grinding sample；Then pass through standard gold Phase microtechnic shows the tissue of pre-grinding sample.
CN201811313062.2A 2018-11-06 2018-11-06 Improve the hot-working method of raw amorphous composite material mechanical property in titanium-based Pending CN109338251A (en)

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CN110923587A (en) * 2019-12-20 2020-03-27 常州世竟液态金属有限公司 Low-density titanium-based block amorphous alloy
CN111074177A (en) * 2020-01-17 2020-04-28 太原理工大学 Amorphous composite material and method for preparing flexible coupling diaphragm by using same

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110923587A (en) * 2019-12-20 2020-03-27 常州世竟液态金属有限公司 Low-density titanium-based block amorphous alloy
CN111074177A (en) * 2020-01-17 2020-04-28 太原理工大学 Amorphous composite material and method for preparing flexible coupling diaphragm by using same

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Application publication date: 20190215