CN1528930A - Micro fine-grained titanium-nickel-niobium shape memory alloy block material preparing method - Google Patents
Micro fine-grained titanium-nickel-niobium shape memory alloy block material preparing method Download PDFInfo
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- CN1528930A CN1528930A CNA2003101079313A CN200310107931A CN1528930A CN 1528930 A CN1528930 A CN 1528930A CN A2003101079313 A CNA2003101079313 A CN A2003101079313A CN 200310107931 A CN200310107931 A CN 200310107931A CN 1528930 A CN1528930 A CN 1528930A
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Abstract
The invention is a manufacturing method for a kind of micron tiny crystal titanium nickel-niobium shape memorizing alloy block materials, 45%-50% titanium, 40%-45% nickel, 5%-10% niobium are melted and produced into titanium nickel-niobium alloy cast ingot, and cuts the titanium nickel-niobium alloy block material into blank, and carries on surface finish process, and paints with glass lubricate, uses isometric curved squeezing mould with 90-120 degrees channel angle, the mould cavity surface is painted with black lead lubricate, the blank and mould are heated and carries on temperature reservation, and takes them out to be squeezed at the same time, finally gets the product. The invention solves the problem that the bad plastic property of titanium nickel-niobium shape memorizing alloy in room temperature, enhances the alloy mechanical performance, and lowers the cost.
Description
Technical field:
The present invention relates to a kind of micro fine-grained titanium-nickel-niobium (TiNi-Nb) marmen blocks preparation method, be used to obtain to improve the titanium nickel-niobium 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.The TiNi-Nb alloy has a lot of excellent properties, as: favorable mechanical performance (specific tenacity height, heat resistance is good, fatigue strength is high), high erosion resistance and shape memory and super-elasticity, and, can reach 150 ℃ because TiNi-Nb alloy hysteresis of phase transformation after suitable distortion obviously increases.Be a kind of wide transformation hysteresis shape memory alloy, connect fastening piece energy storage at room temperature with its engineering of making, it is very convenient that engineering is used, thereby be with a wide range of applications.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-niobium shape memory alloy.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 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 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 channelangular extrusion of diffiNblt-to-work alloys Systran NbderalCorporation 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, a kind of micro fine-grained titanium-nickel-niobium marmen blocks preparation method is provided, can solve the problem of titanium nickel-niobium-based shape memory alloy 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, nickel plate and technical pure niobium that the present invention selects for use purity to be respectively the titanium sponge and 99.95% (mass percent) of 99.95% (mass percent) are raw material, carry out melting under vacuum condition, make Titanium nickel-niobium alloy ingot casting.The composition of alloy (atomic percent) scope is: titanium is 45%～50%, and nickel is 40%～45%, and niobium is 5%～10%.Titanium nickel-niobium 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-niobium alloy bulks such as intensity, plasticity.
Titanium nickel of the present invention-niobium shape memory alloy preparation method is specially: is 45%～50% with raw material by the atomic percent titanium, and nickel is 40%～45%, and niobium is 5%～10% to prepare, and carries out melting under vacuum condition, makes titanium nickel-niobium alloy ingot casting.Ingot casting 800 ℃～900 ℃ annealing, is incubated 4～5 hours, block titanium nickel-niobium alloy ingot casting 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 surface cleaning is carried out on the blank surface, preheating is 20～60 minutes under 60 ℃～100 ℃ temperature, and the method that adopts dip-coating then is at blank surface applied glass protecting lubricant, and coating is wanted evenly, and coat-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 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 850 ℃～950 ℃, ready blank is placed on the asbestos tile, put into this process 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-niobium 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 swabbing 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 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-niobium micron crystalline substance, finally obtain well behaved titanium nickel-niobium alloy bulks such as intensity, plasticity.
The present invention can solve the problem of titanium nickel-niobium shape memory alloy 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.
Embodiment:
Below by specific embodiment technical scheme of the present invention is further described.
Embodiment 1:
Is 50% with raw material by the atomic percent titanium, and nickel is 40%, and niobium is 10% to be equipped with, and adopts the melting of cold wall niobium crucible vacuum magnetic suspension inductive method under argon shield, makes titanium nickel-niobium alloy ingot casting, 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-niobium 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 850 ℃, ready blank is placed on the asbestos tile, put into this process 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-niobium alloy bulk.
Embodiment 2:
Is 47% with raw material by the atomic percent titanium, and nickel is 44%, and niobium is 9% to be equipped with, and carries out melting under vacuum condition, makes titanium nickel-niobium alloy ingot casting.Ingot casting 800 ℃ of annealing, is incubated 5 hours.It is 9.3 * 9.3mm that titanium nickel-niobium 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 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 4 extruding, can obtain a micron brilliant titanium nickel-niobium alloy bulk.
Embodiment 3:
Is 50% with raw material by the atomic percent titanium, and nickel is 45%, and niobium is 5% to be equipped with, and carries out melting under vacuum condition, makes titanium nickel-niobium alloy ingot casting.Ingot casting 900 ℃ of annealing, is incubated 4.5 hours.It is 9.3 * 9.3mm that titanium nickel-niobium 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 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-niobium alloy bulk.
Claims (1)
1, a kind of micron fine-grained titanium-nickel-niobium marmen blocks preparation method, it is characterized in that: be 45%～50% titanium with atomic percent, 40%～45% nickel, 5%～10% niobium, melting under vacuum condition, make titanium nickel-niobium alloy ingot casting, with ingot casting 800 ℃～900 ℃ annealing, be incubated 4～5 hours, cut into blank then and carry out surface smoothness and handle, after the cleaning with blank preheating 20～60 minutes under 60 ℃～100 ℃ temperature, the even coating 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 850 ℃～950 ℃, 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, 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-niobium alloy bulk.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1328407C (en) * | 2005-11-24 | 2007-07-25 | 上海交通大学 | Method for preparing microu-crystal copper-aluminium-nickle shape memory alloy cube material |
| CN100348760C (en) * | 2004-10-22 | 2007-11-14 | 中国科学院金属研究所 | Fastening ring made of wide thermal hysteresis Ti-Ni-based shape-memory alloy, preparation method and application thereof |
| CN100545283C (en) * | 2008-03-25 | 2009-09-30 | 厦门大学 | A kind of nickel titanium niobium negative thermal expansion alloy and preparation method thereof |
| CN101805843A (en) * | 2010-04-16 | 2010-08-18 | 中国石油大学(北京) | NbTi/TiNi memory alloy composite material and preparation method thereof |
| CN106929738A (en) * | 2017-04-13 | 2017-07-07 | 水利部杭州机械设计研究所 | A kind of Ni Ti Nb carbide composite coatings of anti-cavitation Anti-erosion high bond strength and preparation method thereof |
| CN108393492A (en) * | 2018-03-07 | 2018-08-14 | 吉林大学 | A method of shaping complexity NiTi alloy components using increasing material manufacturing |
| CN109554578A (en) * | 2018-12-21 | 2019-04-02 | 中国工程物理研究院机械制造工艺研究所 | A kind of negative expansion memorial alloy and preparation method thereof |
| CN111020338A (en) * | 2019-12-16 | 2020-04-17 | 四川大学 | Ultralow temperature service nickel-titanium-niobium shape memory alloy |
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2003
- 2003-10-16 CN CN 200310107931 patent/CN1209477C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100348760C (en) * | 2004-10-22 | 2007-11-14 | 中国科学院金属研究所 | Fastening ring made of wide thermal hysteresis Ti-Ni-based shape-memory alloy, preparation method and application thereof |
| CN1328407C (en) * | 2005-11-24 | 2007-07-25 | 上海交通大学 | Method for preparing microu-crystal copper-aluminium-nickle shape memory alloy cube material |
| CN100545283C (en) * | 2008-03-25 | 2009-09-30 | 厦门大学 | A kind of nickel titanium niobium negative thermal expansion alloy and preparation method thereof |
| CN101805843A (en) * | 2010-04-16 | 2010-08-18 | 中国石油大学(北京) | NbTi/TiNi memory alloy composite material and preparation method thereof |
| CN101805843B (en) * | 2010-04-16 | 2011-11-16 | 中国石油大学(北京) | NbTi/TiNi memory alloy composite material and preparation method thereof |
| CN106929738A (en) * | 2017-04-13 | 2017-07-07 | 水利部杭州机械设计研究所 | A kind of Ni Ti Nb carbide composite coatings of anti-cavitation Anti-erosion high bond strength and preparation method thereof |
| CN106929738B (en) * | 2017-04-13 | 2018-08-31 | 水利部杭州机械设计研究所 | A kind of Ni-Ti-Nb- carbide composite coatings of anti-cavitation Anti-erosion high bond strength and preparation method thereof |
| CN108393492A (en) * | 2018-03-07 | 2018-08-14 | 吉林大学 | A method of shaping complexity NiTi alloy components using increasing material manufacturing |
| CN109554578A (en) * | 2018-12-21 | 2019-04-02 | 中国工程物理研究院机械制造工艺研究所 | A kind of negative expansion memorial alloy and preparation method thereof |
| CN111020338A (en) * | 2019-12-16 | 2020-04-17 | 四川大学 | Ultralow temperature service nickel-titanium-niobium shape memory alloy |
| CN111020338B (en) * | 2019-12-16 | 2021-07-30 | 四川大学 | Ultralow temperature service nickel-titanium-niobium shape memory alloy |
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| CN1209477C (en) | 2005-07-06 |
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