CN1224473C - Micron fine-grained titanium-nickel-copper alloy block constant-diameter corner extrusion preparation method - Google Patents
Micron fine-grained titanium-nickel-copper alloy block constant-diameter corner extrusion preparation method Download PDFInfo
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- CN1224473C CN1224473C CN 200310107937 CN200310107937A CN1224473C CN 1224473 C CN1224473 C CN 1224473C CN 200310107937 CN200310107937 CN 200310107937 CN 200310107937 A CN200310107937 A CN 200310107937A CN 1224473 C CN1224473 C CN 1224473C
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Abstract
The present invention relates to a method for preparing micron fine-grained titanium-nickel-copper alloy block material with a constant diameter and a bending angle in an extruding mode, which comprises the following steps: titanium whose atomic percent is from 48% to 55%, nickel whose atomic percent is from 35% to 47% and copper whose atomic percent is from 5% to 10% are melted under the vacuum condition to be prepared into a titanium-nickel-copper alloy ingot; the titanium-nickel-copper alloy block material is cut into billets, the surfaces of the billets are smoothed and cleaned, and glass lubricant is coated on the surfaces; an extrusion die with a constant diameter and a bending angle is adopted, and the angle of the extrusion channel of the extrusion die is from 90 to 120 degrees; graphitic lubricant is coated on the surface of the cavity of the die; the billets and the die are respectively heated, and the temperature of the billets and the die is respectively kept; meanwhile, the billets and the die are taken out of a heating furnace to be extruded into the material with a constant diameter and a bending angle; finally, the titanium-nickel-copper alloy block material with good strength, good plasticity, etc. is obtained. The present invention can solve the problem of poor room temperature plasticity of titanium-nickel-copper type memory alloy, and the mechanical property of alloy is improved; meanwhile, the alloy processing cost is reduced, and the rate of finished products of the alloy is improved.
Description
Technical field:
The present invention relates to the isometrical bent angle extruding production of a kind of micron fine-crystal titanium-nickle-copper (TiNi-Cu) alloy cube matherial, be used to obtain to improve the titanium nickel-copper alloy bulk of cold plasticity, intensity and the shape-memory properties of marmem, and then improve the practical engineering application value of this marmem in fields such as Aero-Space, health care and civilian industries.Belong to metal material and metallurgical class technical field.
Background technology:
Marmem has been subjected to the extensive attention of material circle since coming out the beginning of the seventies, demonstrate great application prospect in fields such as civilian industry, Aero-Space, nuclear industry, biomedicines.The TiNi-Cu alloy has a lot of excellent properties, as: favorable mechanical performance (specific strength height, heat resistance is good, fatigue strength is high), excellent biological compatibility, high corrosion resistance and shape memory and super-elasticity, and the TiNi-Cu alloy is rapider to the response ratio in temperature field, can make sensitive components with it, thereby be with a wide range of applications with higher response frequency.But poor because of its intensity high and low temperature plasticity, make the acquisition of its high-performance bulk very difficult.
The plasticity that how to improve material is the primary problem that solves of titanium nickel-copper marmem.Facts have proved: the crystal grain of axle such as tiny can improve the plastic deformation ability of alloy.Alloy grain process for refining commonly used generally be divided into four kinds [Zheng Laisu. Cast Alloy ﹠ Melting (M). Xi'an: publishing house of Northwestern Polytechnical University, 1994]: add various grain refiners or make dendrite fragmentation when liquid by external energy, thereby refinement cast sturcture is as element crystal grain thinnings such as interpolation zirconiums; The semi-solid-state shaping crystal grain thinning; Casting powder metallurgy is shaped; The intense plastic strain method is turned round method, isometrical bent angle extrusion (Equal Channel Angular Extrusion is hereinafter to be referred as ECAE) etc. such as pressure, all is used to prepare grained material.First three methods is casting, and grain refining effect is not obvious.Plastic deformation method can be prepared grained material, and still, in order to obtain bigger dependent variable, pressure is turned round method and can only be prepared extremely thin flaky material, and isometrical bent angle extruding rule can be prepared bigger block grained material.
ECAE technological principle and method be to the existing many reports of the grain refinement of magnesium with good plasticity, acieral, but the grain refinement of the metal alloy of intensity height, plasticity difference is subjected to the restriction of several factors.S.L.Semiatin, D.P.DeLo etc. show [Equal channelangular extrusion of difficult-to-work alloys Systran FederalCorporation to the ECAE under the Ti-6Al-4V non-isothermal condition, Dayton, OH 45432, USA], under non-isothermal condition, because the rapid decline of temperature, the influence of factor such as strain rate, lubricating condition are inappropriate, fracture in various degree all appears in the blank after isometrical bent angle extruding, thereby can not obtain big block grained material.
Summary of the invention:
The objective of the invention is at the deficiencies in the prior art, provide a kind of micron fine-crystal titanium-nickle-copper alloy bulk isometrical bent angle extruding production, can solve the problem of titanium nickel-copper marmem temperature-room type plasticity difference, improve its mechanical property, reduce the cost that high-temperature shape memory alloy is handled simultaneously, improve its lumber recovery.
For realizing such purpose, the present invention selects for use purity to be respectively the nickel plate of titanium sponge and 99.95% (mass percent) of 99.95% (mass percent) and 99.9% copper is raw material, carries out melting under vacuum condition, makes the titanium nickel copper alloy ingot casting.The composition of alloy (atomic percentage) scope is: titanium is 48%～55%, and nickel is 35%～47%, and copper is 5%～10%.Titanium nickel-copper alloy bulk is cut into blank, carry out surface smoothness and handle, and the coating glass lubricant.Mould employing squeezing passage angle is 90～120 ° an isometrical bent angle extrusion die, mold cavity surface applied graphitic lubricant.With blank, mould difference heat tracing, and from heating furnace, take out simultaneously and carry out isometrical bent angle extruding, finally obtain well behaved titanium nickel-copper alloy bulks such as intensity, plasticity.
Titanium nickel of the present invention-copper marmem preparation method is specially: is 48%～55% with raw material by the atomic percent titanium, and nickel is 35%～47%, and copper is 5%～10% to prepare, and carries out melting under vacuum condition, makes titanium nickel-copper alloy casting ingot.Ingot casting 800 ℃～900 ℃ annealing, is incubated 4～5 hours, block titanium nickel-copper alloy casting ingot line is cut into blank, blank is carried out surface treatment, reach the surface accuracy more than 4 grades, blank surface processing roughness is not less than R
a=1.25～2.5 μ m.With acetone blank surface is carried out surface clean, preheating is 20～60 minutes under 60 ℃～100 ℃ temperature, adopts the method for dip-coating to apply glass protecting lubricant in blank surface then, and coating is wanted evenly, and coating layer thickness is 0.2～0.4mm.Coating back blank was dried 20～60 minutes under 60 ℃～100 ℃ temperature, if occur falling to being coated with, cut, defective such as peel off, should carry out coating or flush away recoat.
The present invention adopts isometrical bent angle extrusion die, and the squeezing passage angle of mould is 90～120 °.With acetone mould is carried out surface and die cavity and clean, preheating is 1～1.5 hour under 60 ℃～100 ℃ temperature, coated graphite lubricant then, and coating layer thickness is wanted evenly.
The mould that coats graphitic lubricant is placed in 300 ℃～600 ℃ the heating furnace and heats, be incubated 1～1.5 hour after reaching temperature; The another one heating furnace is heated to 850 ℃～950 ℃, ready blank is placed on the asbestos shingle, put into this heating furnace, treat that temperature is raised to 850 ℃～950 ℃ after, be incubated 15～30 minutes.The blank and the mould that heat are taken out simultaneously, rapidly blank is put into mould then, on universal hydraulic testing machine, blank is pushed, extruding beginning temperature 〉=750 ℃, extruding finishing temperature 〉=600 ℃.Repeat the blank that squeezes out is carried out surface treatment and coating glass lubricant, mold cavity coated graphite lubricant, pushes totally 2～8 times, can obtain micron brilliant titanium nickel-copper alloy bulk, its microcosmic average grain size is 0.2～0.6 μ m.
The present invention adopts isometrical bent angle extrusion process, is characterized in making sample size constancy before and after distortion, handle simply, and the rate of becoming a useful person height, and can realize big workpiece processing.Before the extruding mold cavity and blank to be extruded are carried out different lubricated respectively, the rapid temperature drop that both can effectively stop the high temperature blank, can reduce simultaneously the sliding-frictional resistance between blank and mold work surface significantly, thereby improve the flow uniformity of alloy material effectively, guarantee carrying out smoothly of extrusion process; The lubricated process is simple, and cost is low, and after practical operation, blank and mould come off voluntarily, do not bond together good manufacturability mutually.Determining of blank end radian and blank surface fineness helps blank and reduces friction in extrusion process, improves the mobile uniformity of plasticity of blank.The determining and the blank that heats and mould taken out from heating furnace simultaneously of blank, mold heated time and temperature retention time carries out isometrical bent angle extruding, can prevent grain growth, help forming tiny titanium nickel-copper micron crystalline substance, finally obtain well behaved titanium nickel-copper alloy bulks such as intensity, plasticity.
The present invention can solve the problem of titanium nickel-copper marmem temperature-room type plasticity difference, improves its mechanical property, reduces the cost that high-temperature shape memory alloy is handled simultaneously, improves its lumber recovery.
The specific embodiment:
Below by specific embodiment technical scheme of the present invention is further described.
Embodiment 1:
Is 55% with raw material by the atomic percent titanium, and nickel is 35%, and copper is 10% to be equipped with, and adopts the melting of cold wall copper crucible vacuum magnetic suspension actinobolia under argon shield, makes titanium nickel-copper alloy casting ingot, about 90 grams of the quality of each ingot.Ingot casting 850 ℃ of annealing, is incubated 4 hours.It is 9.3 * 9.3mm that titanium nickel-copper alloy bulk line is cut into cross section, and length is the blank of 87mm, with the wire electric discharge patterning method blank is carried out surface treatment, and blank surface processing roughness is not less than R
a=1.25～2.5 μ m.With acetone blank surface is carried out surface clean, preheating is 30 minutes under 80 ℃ temperature, adopt the method for dip-coating to apply glass protecting lubricant then in blank surface, coating is wanted evenly, coating layer thickness is about 0.2mm, coating back blank dry 20 minutes under 90 ℃ temperature, as if occurring falling to being coated with, cut, defective such as peeling off, should carry out coating or flush away recoat.Is that 120 degree moulds carry out surface and die cavity and clean with acetone to the extruding angle, and preheating is 1 hour under 80 ℃ temperature, coated graphite lubricant then, and coating is even.
The mould that coats graphitic lubricant is placed in 300 ℃ the heating furnace and heats, reached after the temperature insulation 1 hour; The another one heating furnace is heated to 850 ℃, ready blank is placed on the asbestos shingle, put into this heating furnace, treat that temperature is raised to 850 ℃ after, be incubated 20 minutes.The blank and the mould that heat are taken out simultaneously, rapidly blank is put into mould then, push immediately on universal hydraulic testing machine, the blank that extruding is come out carries out surface treatment etc. again and carries out 2 extruding, can obtain a micron brilliant titanium nickel-copper alloy bulk.
Embodiment 2:
Is 50% with raw material by the atomic percent titanium, and nickel is 43%, and copper is 7% to be equipped with, and carries out melting under vacuum condition, makes titanium nickel-copper alloy casting ingot.Ingot casting 800 ℃ of annealing, is incubated 5 hours.It is 9.3 * 9.3mm that titanium nickel-copper alloy bulk line is cut into cross section, and length is the blank of 87mm, with the wire electric discharge patterning method blank is carried out surface treatment, and blank surface processing roughness is not less than R
a=1.25～2.5 μ m.With acetone blank surface is carried out surface clean, blank is placed on the clean stainless steel pallet, preheating is 50 minutes under 65 ℃ temperature, adopt the method for dip-coating to apply glass protecting lubricant then in blank surface, coating is wanted evenly, and coating layer thickness is about 0.3mm, and coating back blank was dried 20 minutes under 90 ℃ temperature, if occur falling to being coated with, cut, defective such as peel off, should carry out coating or flush away recoat.Is that 90 degree moulds carry out surface and die cavity and clean with acetone to the extruding angle, and preheating is 1.5 hours under 60 ℃ temperature, coated graphite lubricant then, and coating is even.
The mould that coats graphitic lubricant is placed in 400 ℃ the heating furnace and heats, reached after the temperature insulation 1 hour; The another one heating furnace is heated to 900 ℃, ready blank is placed on the asbestos shingle, put into this heating furnace, treat that temperature is raised to 900 ℃ after, be incubated 20 minutes.The blank and the mould that heat are taken out simultaneously, rapidly blank is put into mould then, push immediately on universal hydraulic testing machine, the blank that extruding is come out carries out surface treatment etc. again and carries out 4 extruding, can obtain a micron brilliant titanium nickel-copper alloy bulk.
Embodiment 3:
Is 48% with raw material by the atomic percent titanium, and nickel is 47%, and copper is 5% to be equipped with, and carries out melting under vacuum condition, makes titanium nickel-copper alloy casting ingot.Ingot casting 900 ℃ of annealing, is incubated 4.5 hours.It is 9.3 * 9.3mm that titanium nickel-copper alloy bulk line is cut into cross section, and length is the blank of 87mm, with the wire electric discharge patterning method blank is carried out surface treatment, and blank surface processing roughness should be not less than R
a=1.25～2.5 μ m.With acetone blank surface is carried out surface clean, blank is placed on the clean stainless steel pallet, preheating is 20 minutes under 100 ℃ temperature, adopt the method for dip-coating to apply glass protecting lubricant then in blank surface, coating is wanted evenly, and coating layer thickness is about 0.4mm, and coating back blank was dried 30 minutes under 90 ℃ temperature, if occur falling to being coated with, cut, defective such as peel off, should carry out coating or flush away recoat.Is that 90 degree moulds carry out surface and die cavity and clean with acetone to the extruding angle, and preheating is 1 hour under 90 ℃ temperature, coated graphite lubricant then, and coating is even.
The mould that coats graphitic lubricant is placed in 550 ℃ the heating furnace and heats, reached after the temperature insulation 1 hour; Ready blank is placed on the asbestos shingle, puts into the heating furnace that another one is heated to 950 ℃, treat that temperature is raised to 950 ℃ after, be incubated 20 minutes.The blank and the mould that heat are taken out simultaneously, rapidly blank is put into mould then, push immediately on universal hydraulic testing machine, the blank that extruding is come out carries out surface treatment etc. again and carries out 4 extruding, can obtain a micron brilliant titanium nickel-copper alloy bulk.
Claims (1)
1, a kind of micron isometrical bent angle extruding production of fine-crystal titanium-nickle-copper alloy bulk, it is characterized in that: be 48%～55% titanium with atomic percent, 35%～47% nickel, 5%～10% copper, melting under vacuum condition, make titanium nickel-copper alloy casting ingot, with ingot casting 800 ℃～900 ℃ annealing, be incubated 4～5 hours, cut into blank then and carry out the surface smoothness processing, again blank surface is carried out surface clean, after the cleaning with blank preheating 20～60 minutes under 60 ℃～100 ℃ temperature, evenly apply glass protecting lubricant in blank surface then, coating layer thickness is 0.2～0.4mm, and coating back blank was dried 20～60 minutes under 60 ℃～100 ℃ temperature; Employing squeezing passage angle is 90～120 ° an isometrical bent angle extrusion die, with acetone mould is carried out surface and die cavity cleaning, preheating even coated graphite lubricant after 1～1.5 hour under 60 ℃～100 ℃ temperature, then mould is placed in 300 ℃～600 ℃ the heating furnace heating and is incubated 1～1.5 hour, the another one heating furnace is heated to 850 ℃～950 ℃, ready blank is put into this heating furnace heating and is incubated 15～30 minutes, then blank and the mould that heats taken out simultaneously, and rapidly blank is put into mould, on universal hydraulic testing machine, blank is pushed, repeat the blank that squeezes out is carried out surface treatment and coating glass lubricant, mold cavity coated graphite lubricant, push again totally 2～8 times, obtain micron brilliant titanium nickel-copper alloy bulk.
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| CN 200310107937 CN1224473C (en) | 2003-10-16 | 2003-10-16 | Micron fine-grained titanium-nickel-copper alloy block constant-diameter corner extrusion preparation method |
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| CN1330783C (en) * | 2005-06-30 | 2007-08-08 | 上海交通大学 | Preparation method of fine crystal wear resistant material titanium nickel copper alloy |
| CN100398682C (en) * | 2005-12-22 | 2008-07-02 | 上海交通大学 | Method for preparing micro-grain manganese bronze alloy |
| CN1330782C (en) * | 2005-12-22 | 2007-08-08 | 上海交通大学 | Method for preparing micro-grain aluminium bronze alloy |
| CN100348754C (en) * | 2005-12-22 | 2007-11-14 | 上海交通大学 | Method for preparing micro-grain silicon bronze alloy |
| JP4518205B2 (en) * | 2008-12-01 | 2010-08-04 | 住友金属工業株式会社 | Manufacturing method of upper glass forming material for hot drilling and billet for hot extrusion pipe making |
| CN104928524A (en) * | 2015-03-24 | 2015-09-23 | 河南机电高等专科学校 | Cu-Al-Ti-Fe-Ni system copper alloy |
| CN117340173B (en) * | 2023-12-06 | 2024-03-08 | 成都先进金属材料产业技术研究院股份有限公司 | Method for inhibiting cracking in nickel-copper alloy forging process |
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