CN100347323C - Ti-Ni base shape memory alloy and method for preparing same - Google Patents
Ti-Ni base shape memory alloy and method for preparing same Download PDFInfo
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Abstract
The present invention relates to a Ti-Ni based shape memory alloy and a preparation method thereof, which belongs to the field of shape memory materials. Titanium and nickel are used as basic components, and rare-earth elements are added. The present invention enlarges the solid solution limit of the Ti-Ni alloy by utilizing rapid coagulation technology and hot pressed sintering technology. The preparation method comprises the specific steps that a mother alloy ingot is prepared by adopting an arc melting furnace, and then the mother alloy ingot is homogenized; the homogenized mother alloy ingot is trained and processed into a shape memory alloy fiber filament by utilizing the rapid coagulation technology; if shape memory alloy fiber needs to be prepared into a board or a block material of other shapes, the shape memory alloy fiber is prepared into powder, the prepared powder is processed by adopting vacuum hot pressed sintering technology, and then the need block material is prepared. The present invention can be widely applied to the industrial fields, such as industrial automation, energy resources, aerospace, medical sanitation, instruments, meters, mechanical manufacture, etc.
Description
Technical field
The invention belongs to the shape-memory material field, be specifically related to a kind of preparation method of Ti-Ni base marmem.
Background technology
The preparation of tradition memorial alloy normally obtains alloy pig by vacuum induction melting or from power consumption and melting, be rolled into sheet material or be drawn into a material by forging repeatedly afterwards, complex manufacturing technology and its shape and size are subjected to great restriction, can not satisfy the needs of some practical application.For refractory protection and motor car engine, requiring memorial alloy heat to move the working temperature of element will be above 100 ℃, and the Ti-Ni shape memory alloy of existing excellent property is the nearly Ti-Ni alloy that waits atomic ratio, its the highest transformation temperature generally is no more than 100 ℃, obviously can not satisfy the requirement of need of work.Develop working temperature greater than 100 ℃ Ti-Ni shape memory alloy material for making shape Ti-Ni memory alloy material be adapted to the service requirements of refractory protection, motor car engine etc., pressing for.
Summary of the invention
The objective of the invention is to propose a kind ofly can satisfy needs such as refractory protection and motor car engine, transformation temperature reaches the preparation method of the Ti-Ni base marmem more than 100 ℃.
The Ti-Ni base marmem that the present invention proposes is a base stock with titanium, nickel, wherein adds rare earth element.Its component is counted by atomic percent: Ni:45～49at%, Ti:46～50at%, rare earth element: 1～9at%.
Among the present invention, what used rare earth element can be for Ce, Nd, Sm, Dy, Yb etc. is a kind of.
The preparation method of a kind of Ti-Ni base marmem that the present invention proposes, its concrete steps are:
(1) melting, can adopt a kind of of following method:
1. titanium, nickel are added heating and melting in the magnetic control smelting furnace in proportion, temperature is controlled at 900～1000 ℃, and vacuum degree control is 2 * 10
-3--2 * 10
-2, argon shield, fusion postcooling ingot casting fully; The remelting of cooling ingot casting, temperature is controlled at 650～850 ℃, adds rare earth element, stirs, and it is melted fully, casts alloy pig;
2. titanium, nickel, rare earth element are added in the magnetic control smelting furnace in proportion and heat, stir, make it to melt fully, temperature is controlled at 650～850 ℃, and vacuum degree control is 2 * 10
-4--2 * 10
-3, argon shield;
(2) refining: with mixed material melting 1-5 time, cast promptly gets master alloy ingot;
(3) homogenizing is handled: place container to be incubated 4～8 hours master alloy ingot, temperature is controlled between 750～850 ℃, carries out homogenizing and handles;
(4) rapid solidification: with the master alloy ingot scale removal that homogenizing is handled well, join in the rapid solidification equipment, heating is not less than 1000 ℃, and master alloy ingot is melted fully, is quickly cooled to room temperature then, obtains the shape memory alloy fiber yarn; The vacuum degree control of rapid solidification equipment is 2 * 10
-3～8 * 10
-3, frequency control is at 30～80Hz, and operating voltage is controlled at 10～30V, and working current is controlled at 600～1000A, and single roller diameter is 250～300mm, rotating speed is 15～30m/s, adopts argon shield;
(5) training managing: with the shape memory alloy fiber that rapid solidification makes, training managing, aging temperature is 400～550 ℃.
Among the present invention, shape memory alloy can be made the block materials of plate or other shape, be about to place ball mill to make powder through the shape memory alloy fiber yarn that rapid solidification obtains, its control condition is: rotating speed is 300～800 commentaries on classics/s, ratio of grinding media to material is 2: 1～5: 1, and the ball milling time is 5～10 hours; The powder that makes from ball mill enters the vacuum hotpressing device and carries out hot pressed sintering, and temperature is controlled at 800～1000 ℃, and pressure-controlling is at 10-40MPa, and soaking time is 0.5～1 hour; After training managing, aging temperature is 400～550 ℃, promptly can be made into the shape memory alloy block materials.
Because the present invention adds a large amount of rare earth elements, smelting technology with routine is difficult to make rare earth and the complete solid solution of alloy, so adopted flash set technology and mechanical alloying method to increase the solid solubility limit of rare earth element in the present invention, the result shows that effect is fine, makes that a large amount of rare earth element of interpolation is succeedd in the Ti-Ni alloy.
Along with industrial expansion, more and more harsher to the service requirements of material, under the working condition harsh conditions, the performance of material is just had higher requirement.This just requires material to have more high strength, more tough and tensile, more heat-resisting and better erosion resistance, and rapid solidification has higher speed of cooling (10
6K/S), it mainly acts on usually is motion and the diffusion that suppresses atom in the fast cold material, under many occasions, is that atom can not occupy the balance lattice point, and then makes melt obtain bigger condensate depression (a few Baidu) before forming a large amount of solid phase particles.
Flash set technology can change the weave construction of material---and its structural changes comprises that (a) enlarges solid solubility limit; (b) form novel non-equilibrium crystal or quasicrystal; (c) generate metallic glass.The variation of microtexture comprises microtexture topographical transition and size refinement.This variation is that the direction more even towards organizing, tiny, that solute segregation reduces is significantly carried out.In addition, all these variations all make the chemical ingredients of material more become even.Compare with conventional ingot casting material, the segregation degree of rapidly solidified material reduces significantly.Such as, under conventional curing condition, W reaches 99% degree of uniformity during 1600K in Ni needs 16 hours, and the segregation spacing is 100 microns; And in rapidly solidified alloy, the segregation spacing only is 1 micron, and corresponding homogenization time only is 6 seconds.
Flash set technology obtains high speed development by changing a kind of Technology of alloy microstructure and then raising alloy property in nearly ten years as a kind of, especially the preparation technology of conduct preparation amorphous alloy material.Non-crystalline material has remarkable physics, chemistry and mechanical property, it is the critical material of high-technology fields such as electronics, electric power, computer, communication, the huge market demand, industrialization prospect is boundless, so its development must drive the cooperative development of flash set technology.
The sintering process that the present invention adopts is a vacuum heating-press sintering, compares with normal sintering technology to have very big advantage.Conventional powder metallurgical technique generally is that powder is packed in the rigidity pressing mold, imposes the fixed compacting base with definite shape that is compressed to of certain pressure." compacting " is meant the powder consolidation process of no heat effect, rather than hot pressing fixed (impose certain pressure and temperature simultaneously in the powder pressing process, promptly suppress simultaneously and sintering).
Hot pressing had both had the big degree strained characteristic of die mould process, had simultaneously the sintering characteristic that makes the goods densified sintering product again, i.e. die mould under the high temperature, the sintering under the pressure.Therefore, hot pressing has following advantage: required pressure is little during (1) hot pressing, can produce massive article; (2) in very short time, just can make the goods densification; (3) can obtain the product of the extremely low even complete densification of porosity; (4) goods that can production shape more complicated; (5) can produce accurate in size goods.
The densification process of powder under the effect of pressure and temperature can be divided into three phases.Fs, body of powder almost is to be compacted in instantaneous plastic history and to cause temperature to raise, and after subsiding, impressed pressure reaches balance with the internal stress that body of powder produces, and hole closure is not taking place.The densification degree in this stage obviously depends on impressed pressure, and the highest density of pressed compact that makes of the impressed pressure that is applied reaches 95%.The subordinate phase of densification process is controlled by different creep mechanism.Heavily stressed down based on dislocation creep mechanism, but along with the continuous increase of closing of pores quantity, diffusion becomes the principal element of control sintered blank densification.
The new Ti that the present invention makes-higher transformation temperature of Ni-rare earth element shape memory alloy tool, this has just guaranteed that the present invention is at refractory protection and need be than the application in the field of the shape memory alloy of elevated operating temperature at motor car engine and other.Can be used for industrial circles such as industrial automation, the energy, space flight and aviation, health care, instrument and machinofacture.As: two-position controller, driving element, electromagnetic control apparatus, tube stub, hot machine, fire prevention gate, automobile actuator, orthodontic wire, insert type artificial blood vessel or the like.Preparation technology of the present invention has simply, and cost is low, is easy to realize industrialized characteristics, can be used for developing the amorphous nano peritectic alloy, thereby has wide research and market application foreground.
Embodiment
Further describe the present invention below by embodiment.
Embodiment 1
51.4g nickel, 41.8g titanium are added 900 ℃ of arc-melting furnace fusings, and vacuum degree control is 2 * 10
-3, complete fusion postcooling ingot casting is treated in argon shield; The remelting of cooling ingot casting is controlled at 800 ℃ with temperature, adds the 7.5g Rare-Earth Ce, stirs, and makes it to melt fully.Melt back pours into master alloy ingot 3 times.
The master alloy ingot that cast is good 850 ℃ of insulations 4 hours in retort furnace are carried out homogenization of composition and are handled.After alloy pig after homogenization of composition is handled removes descaling, join in the rapid solidification equipment, be heated to more than 1000 ℃, alloy pig is melted fully, be quickly cooled to room temperature then, concrete processing parameter is: vacuum tightness is 2 * 10
-3, frequency is 80Hz, and operating voltage is 30V, and working current is 1000A, and single roller diameter is 250mm, rotating speed is 15m/s, adopts argon shield.Carry out training managing again, aging temperature is 400 ℃, makes the shape memory alloy fiber.
Will further make block materials, will adopt the powder process of planetary ball mill ball milling through the shape memory alloy fiber yarn that rapid solidification makes, milling parameters is: rotating speed is 800 commentaries on classics/s, and ratio of grinding media to material is 2: 1, and the ball milling time is 5 hours; The powder that then ball milling is made adopts the vacuum hotpressing device to carry out hot pressed sintering, and 800 ℃ of vacuum hotpressings, pressure is 40MPa, and soaking time is 1 hour, promptly gets block materials.With the block materials of hot pressed sintering, to 2mm, be cold-rolled to 0.5mm thickness plate through forging repeatedly again through 750 ℃ of constant temperature superplastic deformations.Afterwards with the long 2mm of wire cutting machine, the sample of wide 1mm is as test sample, with the test model that obtains after 800 ℃ of solution treatment, respectively 400 ℃, 450 ℃, 500 ℃, 550 ℃ half an hour timeliness, heat treatment process is 10 in vacuum tightness all
-4Vacuum oven in carry out.Adopt differential scanning calorimeter (DSC) method to analyze its transformation temperature, and the transformation temperature of Ti-Ni-Ce alloy after 400 ℃ of timeliness of different content of rare earth listed in table 1 with the transformation temperature control case that does not contain the binary shape memorial alloy of rare earth.
Embodiment 2
48.07g nickel, 37.58g titanium are added 950 ℃ of arc-melting furnace fusings, and vacuum degree control is 2 * 10
-2, complete fusion postcooling ingot casting is treated in argon shield; The remelting of cooling ingot casting until completely melted, is controlled at 700 ℃ with temperature, adds the 14.34g Rare-Earth Ce, and stirs, and makes it to melt fully.Melt back pours into master alloy ingot 4 times.
The master alloy ingot that cast is good 800 ℃ of insulations 6 hours in retort furnace are carried out homogenization of composition and are handled.After alloy pig after homogenization of composition is handled removes descaling, join in the rapid solidification equipment, be heated to more than 1000 ℃, alloy pig is melted fully, be quickly cooled to room temperature then, concrete processing parameter is: vacuum tightness is 5 * 10
-3, frequency is 50Hz, and operating voltage is 20V, and working current is 800A, and single roller diameter is 270mm, rotating speed is 25m/s, adopts argon shield.Carry out training managing again, aging temperature is 450 ℃.Make the shape memory alloy fiber yarn.
Will further make block materials, will adopt the powder process of planetary ball mill ball milling through the shape memory alloy fiber yarn that rapid solidification makes, milling parameters is: rotating speed is 500 commentaries on classics/s, and ratio of grinding media to material is 4: 1, and the ball milling time is 8 hours.The powder that then ball milling is made adopts the vacuum hotpressing device to carry out hot pressed sintering, and 900 ℃ of vacuum hotpressings, pressure is 20MPa, and soaking time is 1 hour.Obtain block materials, with the block materials of hot pressed sintering, through 750 ℃ of constant temperature superplastic deformations to 2mm, again through forge repeatedly be cold-rolled to 0.5mm after thin plate.Afterwards with the long 2mm of wire cutting machine, the sample of wide 1mm is as test sample, with test sample after 750 ℃ of solution treatment, respectively 400 ℃, 450 ℃, 500 ℃, 550 ℃ half an hour timeliness, heat treatment process is 10 in vacuum tightness all
-4Vacuum oven in carry out.Analyze its transformation temperature with differential scanning calorimeter (DSC) method, and the transformation temperature of Ti-Ni-Ce alloy after 450 ℃ of timeliness of different content of rare earth listed in table 1 with the transformation temperature control case that does not contain the binary shape memorial alloy of rare earth.
Embodiment 3
44.15g nickel, 35.23g titanium, 20.62g Rare-Earth Ce are joined 800 ℃ of arc-melting furnaces, and vacuum degree control is 2 * 10
-4, stir, make it to melt fully, melt back pours into master alloy ingot 5 times.
The master alloy ingot that cast is good 750 ℃ of insulations 8 hours in retort furnace are carried out homogenization of composition and are handled.After alloy pig after homogenization of composition is handled removes descaling, join in the rapid solidification equipment, be heated to more than 1000 ℃, alloy pig is melted fully, be quickly cooled to room temperature then, concrete processing parameter is: vacuum tightness is 8 * 10
-3, frequency is 30Hz, and operating voltage is 20V, and working current is 800A, and single roller diameter is 270mm, rotating speed is 25m/s, adopts argon shield.Carry out training managing again, aging temperature is 550 ℃, makes the shape memory alloy fiber yarn.
Will further make block materials, the shape memory alloy fiber yarn that will make through rapid solidification adopts the powder process of planetary ball mill ball milling, and milling parameters is: rotating speed is 300 commentaries on classics/s, and ratio of grinding media to material is 5: 1, and the ball milling time is 10 hours.The powder that then ball milling is made adopts the vacuum hotpressing device to carry out hot pressed sintering, and 1000 ℃ of vacuum hotpressings, pressure is 40MPa, and soaking time is 0.5 hour.Make block materials, with the block materials of hot pressed sintering through 750 ℃ of constant temperature superplastic deformations to 2mm, again through forge repeatedly be cold-rolled to 0.5mm after thin plate.Afterwards with the long 2mm of wire cutting machine, the sample of wide 1mm is as test sample, with test sample after 700 ℃ of solution treatment, respectively 400 ℃, 450 ℃, 500 ℃, 550 ℃ half an hour timeliness, heat treatment process is 10 in vacuum tightness all
-4Vacuum oven in carry out.Analyze its transformation temperature with differential scanning calorimeter (DSC) method, and the transformation temperature of Ti-Ni-Ce alloy after 450 ℃ of timeliness of different content of rare earth listed in table 1 with the transformation temperature control case that does not contain the binary shape memorial alloy of rare earth.
Embodiment 4
40.08g nickel, 33.58g titanium are added 950 ℃ of arc-melting furnace fusings, and vacuum degree control is 2 * 10
-2, complete fusion postcooling ingot casting is treated in argon shield; The remelting of cooling ingot casting until completely melted, is controlled at 700 ℃ with temperature, adds the 14.34g rare-earth Sm, and stirs, and makes it to melt fully.4 cast of melt back alloy pig.
The alloy pig that cast is good 800 ℃ of insulations 6 hours in retort furnace are carried out homogenization of composition and are handled.After alloy pig after homogenization of composition is handled removes descaling, join in the rapid solidification equipment, be heated to more than 1000 ℃, alloy pig is melted fully, be quickly cooled to room temperature then, concrete processing parameter is: vacuum tightness is 5 * 10
-3, frequency is 50Hz, and operating voltage is 20V, and working current is 800A, and single roller diameter is 270mm, rotating speed is 25m/s, adopts argon shield.Carry out training managing again, aging temperature is 450 ℃, makes the shape memory alloy fiber yarn.
Will further make block materials, the shape memory alloy fiber yarn that will make through rapid solidification adopts the powder process of planetary ball mill ball milling, and milling parameters is: rotating speed is 500 commentaries on classics/s, and ratio of grinding media to material is 4: 1, and the ball milling time is 8 hours.The powder that then ball milling is made adopts the vacuum hotpressing device to carry out hot pressed sintering, and 900 ℃ of vacuum hotpressings, pressure is 20MPa, and soaking time is 1 hour.Obtain block materials, with the block materials of hot pressed sintering, through 750 ℃ of constant temperature superplastic deformations to 2mm, again through forge repeatedly be cold-rolled to 0.5mm after thin plate.Afterwards with the long 2mm of wire cutting machine, the sample of wide 1mm is as test sample, with style after 750 ℃ of solution treatment respectively 400 ℃, 450 ℃, 500 ℃, 550 ℃ half an hour timeliness, heat treatment process is 10 in vacuum tightness all
-4Vacuum oven in carry out.Analyze its transformation temperature with differential scanning calorimeter (DSC) method, and the transformation temperature of Ti-Ni-Sm alloy after 450 ℃ of timeliness of different content of rare earth listed in table 1 with the transformation temperature control case that does not contain the binary shape memorial alloy of rare earth.
The transformation temperature of table 1 Ti-Ni-rare earth element alloy
| M s(℃) | M f(℃) | A s(℃) | A f(℃) | |
| Embodiment 1 | 44.93 | 74.14 | 111.27 | 140.01 |
| Embodiment 2 | 53.01 | 68.87 | 112.15 | 136.55 |
| Embodiment 3 | 49.50 | 72.55 | 115.26 | 139.72 |
| Embodiment 4 | 48.30 | 71.38 | 114.03 | 138.16 |
| Comparative Examples 1 | 25.30 | 38.07 | 35.79 | 40.51 |
By the data of table 1 as can be seen, the transformation temperature of the Ti-Ni-rare earth element shape memory alloy of embodiment 1-4 is all than the height of Comparative Examples 1, especially martensite reverses alternating temperature degree (As) all above 100 ℃, this shows to add the transformation temperature that rare earth element can improve alloy in the Ti-Ni alloy.
Claims (2)
1, a kind of preparation method of Ti-Ni base marmem is a basal component with titanium, nickel, wherein adds rare earth element, and its component is counted by atomic percent: Ni:45～49at%, Ti:46～50at%, rare earth element: 1～9at%; Here rare earth element is a kind of of Ce, Nd, Sm, Dy, Yb; It is characterized in that concrete steps are:
(1) melting, adopt a kind of of following method:
1. titanium, nickel are added heating and melting in the magnetic control smelting furnace in proportion, temperature is 900～1000 ℃, and vacuum tightness is 2 * 10
-3--2 * 10
-2, argon shield, fusion postcooling ingot casting fully; The remelting of cooling ingot casting, temperature is 650～850 ℃, adds rare earth element, stirs, and it is melted fully, casts alloy pig;
2. titanium, nickel, rare earth element are added in the magnetic control smelting furnace in proportion and heat, stir, make it to melt fully, temperature is 650～850 ℃, and vacuum tightness is 2 * 10
-4--2 * 10
-3, argon shield;
(2) refining: with mixed material melting 1-5 time, cast promptly gets master alloy ingot;
(3) homogenizing is handled: place container to be incubated 4～8 hours master alloy ingot, temperature is 750～850 ℃, carries out homogenizing and handles;
(4) rapid solidification: with the master alloy ingot scale removal that homogenizing is handled well, join in the rapid solidification equipment, heating is not less than 1000 ℃, and master alloy ingot is melted fully, is quickly cooled to room temperature then, obtains the shape memory alloy fiber yarn; The vacuum tightness of rapid solidification equipment is 2 * 10
-3～8 * 10
-3, frequency is 30～80Hz, and operating voltage is 10～30V, and working current is 600～1000A, and single roller diameter is 250～300mm, rotating speed is 15～30m/s, adopts argon shield;
(5) training managing: with the shape memory alloy fiber yarn that rapid solidification makes, training managing, temperature is 400～550 ℃.
2, the preparation method of Ti-Ni base marmem according to claim 1, it is characterized in that shape memory alloy is made block materials, concrete steps are: will place ball mill to make powder through the shape memory alloy fiber yarn that rapid solidification obtains, its control condition is: rotating speed is 300～800 commentaries on classics/s, ratio of grinding media to material is 2: 1～5: 1, and the ball milling time is 5～10 hours; The powder that makes from ball mill enters the vacuum hotpressing device and carries out hot pressed sintering, and temperature is 800-1000 ℃, and pressure is 10-40MPa, and soaking time is 0.5-1 hour; After training managing, temperature is 400～550 ℃, promptly makes desired shape memorial alloy block materials.
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| CN104388754A (en) * | 2014-12-15 | 2015-03-04 | 苏州宽温电子科技有限公司 | Shape memory alloy |
| CN114562435A (en) * | 2016-09-14 | 2022-05-31 | 智能合金有限公司 | Shape memory alloy actuator with strain gauge sensor and position estimation and method of making the same |
| CN108707780A (en) * | 2018-04-30 | 2018-10-26 | 苏州诺弘添恒材料科技有限公司 | A method of it prepares with coating titanium copper gallium memorial alloy |
| CN113174512B (en) * | 2021-03-29 | 2022-05-20 | 西安交通大学 | Non-cold-deformation high-elastic thermal effect Ti-Ni bulk material and preparation method thereof |
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