CN1219105C - Micron fine-grained titanium-nickel alloy block material isodiametric corner extrusion preparing method - Google Patents
Micron fine-grained titanium-nickel alloy block material isodiametric corner extrusion preparing method Download PDFInfo
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- CN1219105C CN1219105C CN 03151238 CN03151238A CN1219105C CN 1219105 C CN1219105 C CN 1219105C CN 03151238 CN03151238 CN 03151238 CN 03151238 A CN03151238 A CN 03151238A CN 1219105 C CN1219105 C CN 1219105C
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Abstract
The present invention relates to a method for preparing micron fine-grained titanium-nickel alloy blocks by an isodiametric angle-bent extrusion die. The present invention comprises: 45 at% to 52 at% of titanium and 48 at% to 55 at% nickel are smelted in vacuum and prepared into a titanium-nickel alloy cast ingot; the titanium-nickel alloy cast ingot is cut into blanks, and the surface of each blank is finished and coated with glass lubricants; an isodiametric angle-bent extrusion die of which the angle of the extrusion channel is from 90 to 120 degrees is adopted, and the surface of the die cavity of the isodiametric angle-bent extrusion die is coated with graphite lubricants; the blanks and the extrusion die are respectively heated, heat preservation is carried out for the blanks and the extrusion die, and the blanks and the extrusion die are simultaneously taken out of a heating furnace for isodiametric angle bending extrusion; the titanium-nickel alloy block is obtained, which has favorable strength, favorable plasticity, etc. The present invention can solve the problem that a titanium-nickel shape memory alloy has poor room-temperature plasticity; the present invention can raise the alloy mechanical property, reduce the alloy treatment cost and improve the success ratio.
Description
Technical field:
The present invention relates to the isometrical bent angle extruding production of a kind of micron fine-grained titanium-nickel (TiNi) alloy cube matherial, be used to obtain to improve the Ti-Ni alloy bulk of cold plasticity, intensity and the shape-memory properties of shape memory alloy, and then improve the practical engineering application value of this shape memory alloy in fields such as aerospace, health care and civilian industries.Belong to metallic substance and metallurgical class technical field.
Background technology:
Shape memory alloy 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, aerospace, nuclear industry, biomedicines.Nearly atomic ratio TiNi (50at.%) alloy that waits has a lot of excellent properties, as: favorable mechanical performance (specific tenacity height, heat resistance is good, fatigue strength is high), excellent biological compatibility, high erosion resistance and shape memory and super-elasticity, thereby obtained production application widely, 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 Ti-Ni marmem.Facts have proved: tiny equiaxial crystal grain 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: press of Northwestern Polytechnical University, 1994]: add various grain-refining agents or make dendrite fragmentation when liquid by external energy, thereby refinement cast structure 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 process (Equal Channel Angular Extrusion is called for short 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.
Isometrical bent angle extrusion process principle and method be to the existing many reports of the grain refining of magnesium with good plasticity, aluminum base alloy, but the grain refining 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 channel angular extrusion of difficult-to-work alloysSystran Federal Corporation to the isometrical bent angle extruding of industrially pure titanium (CP Ti), Ti-6Al-4V, Dayton, OH 45432, USA], under non-isothermal condition, because the rapid decline of temperature, the influence of factors such as lubricating condition is 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, a kind of micron isometrical bent angle extruding production of fine-grained titanium-nickel alloy cube matherial is provided, can solve the problem of the Ni-based shape memory alloy temperature-room type plasticity of titanium 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 nickel plate that the present invention selects for use purity to be respectively the titanium sponge and 99.95% (mass percent) of 99.95% (mass percent) is a raw material, carries out melting under vacuum condition, makes Ti-Ni alloy ingot.The composition of alloy (atomic percent) scope is: titanium is 45%～52%, and nickel is 48%～55%.The Ti-Ni 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 mould, mold cavity surface applied oildag.With blank, mould difference heat tracing, and from process furnace, take out simultaneously and carry out isometrical bent angle extruding, finally obtain well behaved titanium nickel-base alloy bulks such as intensity, plasticity.
Titanium of the present invention is Ni-based shape memory alloy preparation method be specially: raw material is pressed atomic percent titanium 45%～52%, and nickel 48%～55% prepares, and carries out melting under vacuum condition, makes titanium nickel-base alloy ingot casting.Ingot casting 800 ℃～900 ℃ annealing, is incubated 4～5 hours, block Ti-Ni alloy line is cut into blank, with the wire electric discharge patterning method 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 surface cleaning is carried out on the blank surface, blank is placed on the clean stainless steel pallet, preheating is 20～60 minutes under 60 ℃～100 ℃ temperature, the method that adopts dip-coating then is at blank surface applied glass protecting lubricant, coating is wanted evenly, and coat-thickness is 0.2～0.4mm, and 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 mould, 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 coat-thickness is wanted evenly.
The mould that coats oildag is placed in 300 ℃～600 ℃ the process furnace and heats, be incubated 1～1.5 hour after reaching temperature; The another one process furnace is heated to 900 ℃～980 ℃, ready blank is placed on the asbestos tile, put into this process furnace, treat that temperature is raised to 900 ℃～980 ℃ 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 applies glass lubricant, mold cavity coated graphite lubricant, push totally 2～8 times again, can obtain the brilliant titanium nickel-base alloy bulk of micron, 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.Extruding is preceding to mold cavity and blank branch to be extruded. do not carry out different swabbing, 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 swabbing processing method is simple, and cost is low, and after actually operating, blank and mould come off voluntarily, do not bond together good manufacturability mutually.Determining of blank end radian and blank surface smooth finish helps blank and reduces friction in extrusion process, improves the homogeneity of the plastic flow of blank.The determining and the blank that heats and mould taken out from process furnace simultaneously of blank, mold heated time and soaking time carries out isometrical bent angle extruding, can prevent grain growth, help forming tiny titanium nickel micron crystalline substance, finally obtain well behaved titanium nickel-base alloy bulks such as intensity, plasticity.
The present invention can solve the problem of the Ni-based shape memory alloy temperature-room type plasticity of titanium difference, improves its mechanical property, reduces the cost that high-temperature shape memory alloy is handled simultaneously, improves its lumber recovery.
Embodiment:
Below by specific embodiment technical scheme of the present invention is further described.
Embodiment 1:
With atomic percent is 50% titanium, and 50% nickel is equipped with, and adopts the melting of cold wall copper crucible vacuum magnetic suspension inductive method under argon shield, makes Ti-Ni alloy 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 Ti-Ni 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, reaches the surface accuracy more than 4 grades, and blank surface processing roughness is not less than R
a=1.25～2.5 μ m.With acetone surface cleaning is carried out on the blank surface, blank is placed on the clean stainless steel pallet, preheating is 30 minutes under 80 ℃ temperature, the method that adopts dip-coating then is at blank surface applied glass protecting lubricant, coating is wanted evenly, and coat-thickness is about 0.2mm, 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 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 oildag is placed in 300 ℃ the process furnace and heats, reached after the temperature insulation 1 hour; The another one process furnace is heated to 900 ℃, ready blank is placed on the asbestos tile, put into this process 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 2 extruding, can obtain the brilliant Ti-Ni alloy bulk of micron.
Embodiment 2:
With atomic percent is 45% titanium, and 55% nickel is equipped with, and carries out melting under vacuum condition, makes Ti-Ni alloy ingot.Ingot casting 800 ℃ of annealing, is incubated 5 hours.It is 9.3 * 9.3mm that Ti-Ni 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, reaches the surface accuracy more than 4 grades, and blank surface processing roughness is not less than R
a=1.25～2.5 μ m.With acetone surface cleaning is carried out on the blank surface, blank is placed on the clean stainless steel pallet, preheating is 50 minutes under 65 ℃ temperature, the method that adopts dip-coating then is at blank surface applied glass protecting lubricant, coating is wanted evenly, and coat-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 oildag is placed in 400 ℃ the process furnace and heats, reached after the temperature insulation 1 hour; The another one process furnace is heated to 950 ℃, ready blank is placed on the asbestos tile, put into this process furnace, 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 the brilliant Ti-Ni alloy bulk of micron.
Embodiment 3:
With atomic percent is 52% titanium, and 48% nickel is equipped with, and carries out melting under vacuum condition, makes Ti-Ni alloy ingot.Ingot casting 900 ℃ of annealing, is incubated 4.5 hours.It is 9.3 * 9.3mm that Ti-Ni 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, reaches the surface accuracy more than 4 grades, and blank surface processing roughness should be not less than R
a=1.25～2.5 μ m.With acetone surface cleaning is carried out on the blank surface, blank is placed on the clean stainless steel pallet, preheating is 20 minutes under 100 ℃ temperature, the method that adopts dip-coating then is at blank surface applied glass protecting lubricant, coating is wanted evenly, and coat-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 oildag is placed in 550 ℃ the process furnace and heats, reached after the temperature insulation 1 hour; Ready blank is placed on the asbestos tile, puts into the process furnace that another one is heated to 970 ℃, treat that temperature is raised to 970 ℃ 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 the brilliant Ti-Ni alloy bulk of micron.
Claims (1)
1, a kind of micron isometrical bent angle extruding production of fine-grained titanium-nickel alloy cube matherial, it is characterized in that: selecting the purity mass percent for use is that 99.95% titanium sponge and 99.95% nickel plate are raw material, it with atomic percent 45%～52% titanium, 48%～55% nickel, melting under vacuum condition, make titanium nickel-base alloy ingot casting, with ingot casting 800 ℃～900 ℃ annealing, be incubated 4～5 hours, adopt the Wire EDM method that ingot casting is cut into blank then and carry out surface smoothness and handle, reach the surface accuracy more than 4 grades, blank surface processing roughness R
a=1.25～2.5 μ m, after cleaning with acetone with blank preheating 20～60 minutes under 60 ℃～100 ℃ temperature, evenly apply glass protecting lubricant on the blank surface then, coat-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 mould, 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 process furnace heating and is incubated 1～1.5 hour, the another one process furnace is heated to 900 ℃～980 ℃, ready blank is put into this process 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, 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, obtain the brilliant titanium nickel-base alloy bulk of micron.
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| CN 03151238 CN1219105C (en) | 2003-09-26 | 2003-09-26 | Micron fine-grained titanium-nickel alloy block material isodiametric corner extrusion preparing method |
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| CN 03151238 CN1219105C (en) | 2003-09-26 | 2003-09-26 | Micron fine-grained titanium-nickel alloy block material isodiametric corner extrusion preparing method |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN1298875C (en) * | 2005-07-07 | 2007-02-07 | 上海交通大学 | Preparation method of high wear resistance titanium nickel alloy material |
| CN100366380C (en) * | 2005-07-20 | 2008-02-06 | 哈尔滨工业大学 | Method of comtinuously preparing alloy semi solid rod and its device |
| CN101381820B (en) * | 2007-09-05 | 2010-05-19 | 中国科学院金属研究所 | Method for preparing low nickel content ternary TiNiHf shape memory alloy sheet material |
| CN101649430B (en) * | 2009-06-30 | 2011-01-19 | 镇江忆诺唯记忆合金有限公司 | NiTiCrRE shape memory alloy hot rolled board preparation method |
| CN103624509A (en) * | 2013-11-27 | 2014-03-12 | 山东建筑大学 | Large plastic deformation method for achieving titanium alloy low-temperature superplasticity |
| CN103820744B (en) * | 2014-02-24 | 2016-01-13 | 上海交通大学 | The preparation method of the ultra-fine grain titanium matrix composite being matrix with two-phase region titanium alloy |
| CN103878273A (en) * | 2014-02-28 | 2014-06-25 | 深圳市欧蒂姆光学有限公司 | Manufacturing facility of titanium-nickel shape memory-alloy spectacle frame part |
| CN107520297A (en) * | 2017-08-31 | 2017-12-29 | 温州圣蓝工贸有限公司 | The manufacturing process and equipment of beam parts in a kind of Ti-Ni shape memory alloy glasses frame |
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