CN106086716A - A kind of Ti Zr Nb Cu Be system amorphous composite material and preparation method thereof - Google Patents

A kind of Ti Zr Nb Cu Be system amorphous composite material and preparation method thereof Download PDF

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CN106086716A
CN106086716A CN201610389563.3A CN201610389563A CN106086716A CN 106086716 A CN106086716 A CN 106086716A CN 201610389563 A CN201610389563 A CN 201610389563A CN 106086716 A CN106086716 A CN 106086716A
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melting
spray
cast
composite material
amorphous composite
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李金山
李力源
王军
寇宏超
胡锐
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Northwestern Polytechnical University
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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

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

A kind of Ti Zr Nb Cu Be system amorphous composite material and preparation method thereof.Described Ti Zr Nb Cu Be system amorphous composite material is made up of Ti, Zr, Nb, Cu and Be, and its atomic percent is TixZr20Nb12Cu5Be63-x, wherein, 51≤x≤55.Described Ti, Zr, Nb, Cu and Be are bulk, and the purity of Ti, Zr, Nb and Cu is all >=99.99%, purity >=99% of Be.In the present invention, Ti content is high, and density is relatively low, has high fracture strength and plasticity coupling simultaneously, and preparation technology is simple, it is possible to be widely used in the of new generation Aeronautics and Astronautics high to requirement of strength and the crucial bearing of weapon needs and shell part.

Description

A kind of Ti-Zr-Nb-Cu-Be system amorphous composite material and preparation method thereof
Technical field
The present invention relates to titanium alloy or non-crystaline amorphous metal field, one has superhigh intensity and plasticity simultaneously specifically The titanium-based amorphous composite joined.
Background technology
A new generation's Aeronautics and Astronautics and weaponry propose lightweight to material, high-performance, structure-function integration are sent out Exhibition requirement, and non-crystaline amorphous metal has the mechanical property more excellent than conventional crystal alloy and wearability, unique physics and chemistry Performance, is therefore with a wide range of applications in defence and military fields such as Aero-Space, weapons, naval vessels.But, owing to lacking position Wrong sliding, the twin deformation mechanism that waits, non-crystaline amorphous metal deformation relies only on sliding and the propagation of shear band, thus its fragility limits The development of non-crystaline amorphous metal and application.In order to solve the fragility of amorphous, toughness the second phase mutually strengthens as a kind of effective method Arouse widespread concern.By adding beta stable element or additional resilient granules, people obtain has good plasticity Amorphous composite material.Both remain the high fracture strength of amorphous and high toughness, solve again the material that amorphous brittle fracture causes Material catastrophic failure.
Titanium-based amorphous alloy owing to having high intensity and low density and good corrosion resistance, at Aeronautics and Astronautics and Military field has the most potential application prospect, but the fragility of non-crystaline amorphous metal constrains its answering as high tough structural material With.Strengthen the preparation spontaneous amorphous composite material of Ti base, the problem that its brittleness at room temperature can be solved thereby through the second phase, hold concurrently simultaneously The advantages such as tool non-crystaline amorphous metal high-strength light, thus the potential Aeronautics and Astronautics as a new generation and military field special bearing Candidate materials with the tough housing of height etc..In recent years, it has been developed that some titanium-based amorphous composite systems, such as Ti-Zr- V-Cu-Be, Ti-Zr-V-Cu-Al-Be, Ti-Cu-Ni-Sn-Nb, Ti-Zr-Ni-Be-Ta etc..This kind of non-according to developed Crystal composite material, the second phase mainly includes Ta graininess solid solution, has the branch such as the β Zr of body-centered cubic structure, β Ti and α Fe Crystalline solid-solution.Through inquiry related data, being currently known the best alloy of titanium-based amorphous composite system mechanical property is β Ti The Ti that dendrite strengthens mutually66Cu8Ni4.8Sn7.2Nb1Alloy, its fracture strength is 2020MPa, and document is shown in plastic strain 32% [J.Eckert,J.Das,et al.Deformation behavior of a Ti66Cu8Ni4.8Sn7.2Nb14nanostructured composite containing ductile dendrites, Journal of Alloys and Compounds, 2007 (434-435): 13-17.], it is difficult to meet a new generation's Aeronautics and Astronautics And weapon field is to material lightweight, high-strength, the demand of high-ductility, thus find a kind of titanio with superhigh intensity and plasticity coupling Amorphous composite material has important application value in army.
Summary of the invention
For overcoming fracture strength and plastic strain present in prior art can not meet a new generation's Aeronautics and Astronautics and weapon The deficiency of domain requirement, the present invention proposes a kind of Ti-Zr-Nb-Cu-Be system amorphous composite material and preparation method thereof.
The present invention is made up of Ti, Zr, Nb, Cu and Be, and its atomic percent is TixZr20Nb12Cu5Be63-x, wherein, 51≤ x≤55.Described Ti, Zr, Nb, Cu and Be are bulk, and the purity of Ti, Zr, Nb and Cu is all >=99.99%, the purity of Be >=99%.
The detailed process that the present invention prepares described Ti-Zr-Nb-Cu-Be system amorphous composite material is as follows:
The first step, the surface of raw material processes.
Second step, prepares alloy pig；Described alloy pig is TixZr20Nb12Cu5Be63-xAlloy pig, wherein, 51≤x≤ 55；Prepared by vacuum arc melting furnace；Specifically, use electric arc melting method, surface treated raw material is being carried out Melting for the first time；After melting terminates, vacuum arc melting furnace is cooled to room temperature；By the alloy pig upset 180 after solidification, repeat The process of described first time melting, carries out second time melting to surface treated raw material；The process of described repetition melting is Three times；Logical high-purity argon gas protection in fusion process；After melting terminates, obtain TixZr20Nb12Cu5Be63-xAlloy pig.
Described electric arc melting TixZr20Nb12Cu5Be63-xDuring alloy pig, the melting electric current of vacuum arc melting furnace is 400A, Smelting time is 5min every time.
3rd step, spray to cast；The Ti that will obtainxZr20Nb12Cu5Be63-xAfter alloy pig is broken, take the alloy of 6.5g～8.0g Sample is placed in there is the silica crucible of opening lower end；Air pressure in spray to cast furnace chamber is extracted into 6 × 10-30.5 air is recharged after Pa The high-purity argon gas of pressure is as protective atmosphere；Alloy sample in silica crucible is heated to completely by the induction coil energising of spray to cast stove Fusing；Open the snifting valve of spray to cast stove, in silica crucible, inject high-purity argon gas, the gas of high-purity argon gas in spray to cast gas tank during spray to cast Pressure is 2 × 104Pa, makes alloy sample solution tapping ejection spray to cast bottom silica crucible to the oxygen-free copper mould of water-cooled In, form amorphous composite material；The power of described spray to cast stove melting is 12KW.
The present invention compared with existing amorphous composite material, its glass transition temperature Tg>=663K, supercooled liquid phase sector width ΔTx>=60K, noncrystal substrate has good heat stability.The alloy using the present invention to prepare is increased by amorphous phase and β Ti dendrite Constituting mutually by force, wherein the volume fraction of dendrite phase is 67% ± 5%, makes this alloy show the mechanical property coupling of superelevation, its The middle Φ 3 × 6mm coupon prepared with this alloy compresses sample data and is: yield strength σy>=1400MPa, compressed rupture strength σf >=2780MPa, plastic strain ε before fracturep>=38%.
In the present invention, Ti content is high, and density is relatively low, has high fracture strength and plasticity coupling simultaneously, and prepares work Skill is simple, can be widely applied to the of new generation Aeronautics and Astronautics high to requirement of strength and the crucial bearing of weapon needs and housing class Part.
Accompanying drawing explanation
The Ti that Fig. 1 provides for the present invention51Zr20Nb12Cu5Be12The XRD diffraction curve (XRD) of amorphous composite material: Cu K α Condition.
The Ti that Fig. 2 provides for the present invention51Zr20Nb12Cu5Be12The differential thermal analysis curve of amorphous composite material: the rate of heat addition 20K/min。
The Ti that Fig. 3 provides for the present invention51Zr20Nb12Cu5Be12The optics Electronic Speculum macrograph of amorphous composite material.
The Ti that Fig. 4 provides for the present invention51Zr20Nb12Cu5Be12The compression test load-deformation curve of amorphous composite material: Uniaxially compressing, strain rate is 1 × 10-4s-1, specimen size: Φ 3 × 6mm.
Fig. 5 is the flow chart that the present invention prepares Ti-Zr-Nb-Cu-Be system amorphous composite material.
Detailed description of the invention
Embodiment one
The present embodiment is a kind of Ti-Zr-Nb-Cu-Be system amorphous composite material.
Ti-Zr-Nb-Cu-Be system amorphous composite material described in this embodiment is by five kinds of elements of Ti, Zr, Nb, Cu, Be Composition, the atomic percent of described Ti-Zr-Nb-Cu-Be system amorphous composite material is Ti51Zr20Nb12Cu5Be12, wherein Ti, Zr, Nb, Cu, Be are by being synthesized by block Ti, Zr, Nb, Cu of purity >=99.99% and the block Be melting of purity >=99%.
The preparation process of the Ti-Zr-Nb-Cu-Be system amorphous composite material that this embodiment is proposed is as follows:
The first step, the surface of raw material processes.Go load weighted Ti, Zr, Nb, Cu and Be to degrease and superficial oxidation skin.
Second step, prepares alloy pig.Described alloy pig is Ti51Zr20Nb12Cu5Be12Alloy pig.Melted by vacuum arc Furnace, prepares Ti51Zr20Nb12Cu5Be12Alloy pig.Specifically, the melting electric current of vacuum arc melting furnace is 400A, often uses The electric arc melting method of rule, is carrying out melting for the first time to surface treated raw material, and smelting time is 5min.Melting terminates After, vacuum arc melting furnace is cooled to room temperature；By the alloy pig upset 180 after solidification, repeat the mistake of described first time melting Journey, carries out second time melting to surface treated raw material, and smelting time is 5min.The process of described repetition melting is three Secondary, uniform to ensure alloy pig composition.Logical high-purity argon gas protection in fusion process.After melting terminates, obtain Ti51Zr20Nb12Cu5Be12Alloy pig.
3rd step, spray to cast.The Ti that will obtain51Zr20Nb12Cu5Be12After alloy pig is broken, the alloy sample taking 6.5g is placed in Lower end has in the silica crucible of diameter 0.5mm mouth.By mechanical pump, the air pressure in furnace chamber is extracted into 6 × 10-3Pa, then recharges The high-purity argon gas of 0.5 atmospheric pressure is as protective atmosphere.The induction coil of spray to cast stove is energized to the alloy sample in silica crucible It is heated to being completely melt.Open the snifting valve of spray to cast stove, in silica crucible, inject high-purity argon gas, high in spray to cast gas tank during spray to cast The air pressure of pure argon is 2 × 104Pa, to ensure to have enough air-flows by alloy sample solution tapping bottom silica crucible Quickly ejection, the alloy sample solution in silica crucible under the pressure of high-purity argon gas air-flow spray to cast to the oxygen-free copper mould of water-cooled In, form the bar-shaped amorphous composite material of a length of 80mm of a diameter of 4mm.The power of described spray to cast stove melting is 12KW.
Alloy bar is cut into sample Φ 3mm × 6mm, then carries out X-ray diffraction, differential thermal analysis, crystalline phase observation and single shaft Compression test.The dendrite phase volume fraction obtained is 71%, compression yield strength σyFor 1400MPa, compressed rupture strength σfFor 3000MPa, plastic strain ε before fracturepIt is 48%, glass transition temperature TgFor 665K, crystallization temperature TxFor 730K, supercooled liquid Phase region width Delta TxFor 65K.
Embodiment two
The present embodiment is a kind of Ti-Zr-Nb-Cu-Be system amorphous composite material.
Ti-Zr-Nb-Cu-Be system amorphous composite material described in this embodiment is by five kinds of elements of Ti, Zr, Nb, Cu, Be Composition, the atomic percent of described Ti-Zr-Nb-Cu-Be system amorphous composite material is Ti53Zr20Nb12Cu5Be10, wherein Ti, Zr, Nb, Cu, Be are by being synthesized by block Ti, Zr, Nb, Cu of purity >=99.99% and the block Be melting of purity >=99%.
The preparation process of the Ti-Zr-Nb-Cu-Be system amorphous composite material that this embodiment is proposed is as follows:
The first step, the surface of raw material processes.Go load weighted Ti, Zr, Nb, Cu and Be to degrease and superficial oxidation skin.
Second step, prepares alloy pig.Described alloy pig is Ti53Zr20Nb12Cu5Be10Alloy pig.Melted by vacuum arc Furnace, prepares Ti53Zr20Nb12Cu5Be10Alloy pig.Specifically, the melting electric current of vacuum arc melting furnace is 400A, often uses The electric arc melting method of rule, is carrying out melting for the first time to surface treated raw material, and smelting time is 5min.Melting terminates After, vacuum arc melting furnace is cooled to room temperature；By the alloy pig upset 180 after solidification, repeat the mistake of described first time melting Journey, carries out second time melting to surface treated raw material, and smelting time is 5min.The process of described repetition melting is three Secondary, uniform to ensure alloy pig composition.Logical high-purity argon gas protection in fusion process.After melting terminates, obtain Ti53Zr20Nb12Cu5Be10Alloy pig.
3rd step, spray to cast.The Ti that will obtain53Zr20Nb12Cu5Be10After alloy pig is broken, the alloy sample taking 7g is placed in down End has in the silica crucible of diameter 0.5mm mouth.By mechanical pump, the air pressure in furnace chamber is extracted into 6 × 10-3Pa, then recharges The high-purity argon gas of 0.5 atmospheric pressure is as protective atmosphere.The induction coil of spray to cast stove is energized to the alloy sample in silica crucible It is heated to being completely melt.Open the snifting valve of spray to cast stove, in silica crucible, inject high-purity argon gas, high in spray to cast gas tank during spray to cast The air pressure of pure argon is 2 × 104Pa, to ensure to have enough air-flows by alloy sample solution tapping bottom silica crucible Quickly ejection, the alloy sample solution in silica crucible under the pressure of high-purity argon gas air-flow spray to cast to the oxygen-free copper mould of water-cooled In, form the bar-shaped amorphous composite material of a length of 80mm of a diameter of 4mm.The power of described spray to cast stove melting is 12KW.
Alloy bar is cut into sample Φ 3mm × 6mm, then carries out X-ray diffraction, differential thermal analysis, crystalline phase observation and single shaft Compression test.The dendrite phase volume fraction obtained is 69%, compression yield strength σyFor 1500MPa, compressed rupture strength σfFor 2780MPa, plastic strain ε before fracturepIt is 38%, glass transition temperature TgFor 663K, crystallization temperature TxFor 723K, supercooled liquid Phase region width Delta TxFor 60K.
Embodiment three
The present embodiment is a kind of Ti-Zr-Nb-Cu-Be system amorphous composite material.
Ti-Zr-Nb-Cu-Be system amorphous composite material described in this embodiment is by five kinds of elements of Ti, Zr, Nb, Cu, Be Composition, the atomic percent of described Ti-Zr-Nb-Cu-Be system amorphous composite material is Ti55Zr20Nb12Cu5Be8, wherein Ti, Zr, Nb, Cu, Be are by being synthesized by block Ti, Zr, Nb, Cu of purity >=99.99% and the block Be melting of purity >=99%.
The preparation process of the Ti-Zr-Nb-Cu-Be system amorphous composite material that this embodiment is proposed is as follows:
The first step, the surface of raw material processes.Go load weighted Ti, Zr, Nb, Cu and Be to degrease and superficial oxidation skin.
Second step, prepares Ti55Zr20Nb12Cu5Be8Alloy pig.Described alloy pig is Ti55Zr20Nb12Cu5Be8Alloy Ingot.By vacuum arc melting furnace, prepare Ti55Zr20Nb12Cu5Be8Alloy pig.Specifically, the melting electricity of vacuum arc melting furnace Stream is 400A, uses conventional electric arc melting method, and surface treated raw material is carrying out melting for the first time, smelting time For 5min.After melting terminates, vacuum arc melting furnace is cooled to room temperature；By the alloy pig upset 180 after solidification, repeat described The process of melting for the first time, carries out second time melting to surface treated raw material, and smelting time is 5min.Described repetition is melted The process of refining is three times, uniform to ensure alloy pig composition.Logical high-purity argon gas protection in fusion process.After melting terminates, obtain Ti55Zr20Nb12Cu5Be8Alloy pig.
3rd step, spray to cast.The Ti that will obtain55Zr20Nb12Cu5Be8After alloy pig is broken, the alloy sample taking 8g is placed in down End has in the silica crucible of diameter 0.5mm mouth.By mechanical pump, the air pressure in furnace chamber is extracted into 6 × 10-3Pa, then recharges The high-purity argon gas of 0.5 atmospheric pressure is as protective atmosphere.The induction coil of spray to cast stove is energized to the alloy sample in silica crucible It is heated to being completely melt.Open the snifting valve of spray to cast stove, in silica crucible, inject high-purity argon gas, high in spray to cast gas tank during spray to cast The air pressure of pure argon is 2 × 104Pa, to ensure to have enough air-flows by alloy sample solution tapping bottom silica crucible Quickly ejection, the alloy sample solution in silica crucible under the pressure of high-purity argon gas air-flow spray to cast to the oxygen-free copper mould of water-cooled In, form the bar-shaped amorphous composite material of a length of 80mm of a diameter of 4mm.The power of described spray to cast stove melting is 12KW.
Alloy bar is cut into sample Φ 3mm × 6mm, then carries out X-ray diffraction, differential thermal analysis, crystalline phase observation and single shaft Compression test.The dendrite phase volume fraction obtained is 70%, compression yield strength σyFor 1450MPa, compressed rupture strength σfFor 2850MPa, plastic strain ε before fracturepIt is 42%, glass transition temperature TgFor 663K, crystallization temperature TxFor 723K, supercooled liquid Phase region width Delta TxFor 60K.

Claims (4)

1. a Ti-Zr-Nb-Cu-Be system amorphous composite material, it is characterised in that described Ti-Zr-Nb-Cu-Be system amorphous Composite is made up of Ti, Zr, Nb, Cu and Be, and its atomic percent is TixZr20Nb12Cu5Be63-x, wherein, 51≤x≤55.
2. Ti-Zr-Nb-Cu-Be system as claimed in claim 1 amorphous composite material, it is characterised in that described Ti, Zr, Nb and Cu Purity all >=99.99%, purity >=99% of Be.
3. prepare the method for Ti-Zr-Nb-Cu-Be system amorphous composite material described in claim 1 for one kind, it is characterised in that concrete Process is as follows:
The first step, the surface of raw material processes；
Second step, prepares alloy pig；Described alloy pig is TixZr20Nb12Cu5Be63-xAlloy pig, wherein, 51≤x≤55；Logical Cross vacuum arc melting furnace to prepare；Specifically, use electric arc melting method, surface treated raw material is being carried out for the first time Melting；After melting terminates, vacuum arc melting furnace is cooled to room temperature；By the alloy pig upset 180 after solidification, repeat described the The process of melting once, carries out second time melting to surface treated raw material；The process of described repetition melting is three times；Molten Logical high-purity argon gas protection during refining；After melting terminates, obtain TixZr20Nb12Cu5Be63-xAlloy pig；
3rd step, spray to cast；The Ti that will obtainxZr20Nb12Cu5Be63-xAfter alloy pig is broken, take the alloy sample of 6.5g～8.0g It is placed in there is the silica crucible of opening lower end；Air pressure in spray to cast furnace chamber is extracted into 6 × 10-30.5 atmospheric pressure is recharged after Pa High-purity argon gas is as protective atmosphere；Alloy sample in silica crucible is heated to melting completely by the induction coil energising of spray to cast stove Change；Open the snifting valve of spray to cast stove, in silica crucible, inject high-purity argon gas, the air pressure of high-purity argon gas in spray to cast gas tank during spray to cast It is 2 × 104Pa, make alloy sample solution tapping ejection spray to cast bottom silica crucible to the oxygen-free copper mould of water-cooled, Form amorphous composite material；The power of described spray to cast stove melting is 12KW.
4. the method preparing Ti-Zr-Nb-Cu-Be system amorphous composite material as claimed in claim 3, it is characterised in that electric arc melts Refining TixZr20Nb12Cu5Be63-xDuring alloy pig, the melting electric current of vacuum arc melting furnace is 400A, and each smelting time is 5min。
CN201610389563.3A 2016-06-03 2016-06-03 A kind of Ti Zr Nb Cu Be system amorphous composite material and preparation method thereof Pending CN106086716A (en)

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Cited By (1)

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CN114672745A (en) * 2022-03-24 2022-06-28 松山湖材料实验室 Titanium-based amorphous composite material and preparation method and application thereof

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CN102925822A (en) * 2012-10-19 2013-02-13 南京理工大学 Metal glass composite material with high-oxygen content and preparation method thereof
CN103834822A (en) * 2014-02-28 2014-06-04 西北工业大学 Smelting and casting method and casting device of titanium-based amorphous composite material
CN105112819A (en) * 2015-09-14 2015-12-02 西北工业大学 Method for regulating micro structure of Ti-Zr-Nb-Cu-Be-system amorphous composite material

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Publication number Priority date Publication date Assignee Title
JP2000160308A (en) * 1998-09-25 2000-06-13 Japan Science & Technology Corp High specific strength titanium base amorphous alloy
CN102181809A (en) * 2011-04-21 2011-09-14 南京理工大学 Large-size metallic glass composite material with tensile ductility and preparation method thereof
CN102925822A (en) * 2012-10-19 2013-02-13 南京理工大学 Metal glass composite material with high-oxygen content and preparation method thereof
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114672745A (en) * 2022-03-24 2022-06-28 松山湖材料实验室 Titanium-based amorphous composite material and preparation method and application thereof
CN114672745B (en) * 2022-03-24 2023-03-10 松山湖材料实验室 Titanium-based amorphous composite material and preparation method and application thereof

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