CN102191394A - Preparation method of porous CuAlMn shape memory alloy with controllable pore structure parameters - Google Patents
Preparation method of porous CuAlMn shape memory alloy with controllable pore structure parameters Download PDFInfo
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Abstract
The invention discloses a preparation method of porous CuAlMn shape memory alloy with controllable pore structure parameters. The method comprises the following steps of: smelting Cu-Al-Mn alloy, atomizing the Cu-Al-Mn alloy with high-purity N2 to prepare Cu-Al-Mn alloy powder, preparing sheet NaCl powder, blending the Cu-Al-Mn alloy powder and the NaCl powder, hot-pressing and sintering the mixture in vacuum, sintering and evaporating the mixture at a high temperature to desalt the mixture, and quenching the solid solution. The porous CuAlMn shape memory alloy provided by the invention is directionally arranged and uniformly distributed in pores, high in compression strength and high in energy absorption ability. As a high-energy absorption ability and bacterial growth-preventing material, the porous CuAlMn shape memory alloy is expected to be used in aspects, such as impact energy absorption, impact prevention, noise reduction of an air conditioner air supply system and the like. By the preparation method provided by the invention, opened-hole or closed-hole porous metal materials can be prepared. The method has the advantages of controllable pore structure parameters, complete desalting and the like.
Description
Technical field
The present invention relates to the preparation method of the controlled porous C uAlMn shape memory alloy of a kind of pore structure parameter.
Background technology
In recent years, the development of aerospace industry has proposed requirement to the vibration-damping function of traditional structural materials.Rocket, satellite failure analysis result show that about 2/3 fault is relevant with vibration and noise.Aircraft is in the process of life-time service, because yaw rudder, tail fairing germinating crackle often appears in vibration, and problems such as pitot fracture, passenger cabin noise, have a strong impact on its reliability and work-ing life.Various instrument on the aircraft are in the noise and vibration environment, often break down.Vibration in the cabin and noise be serious harm people's physical and mental health also, is that environmental engineering is badly in need of one of important topic that solves.In addition, the supply air system noise on submarine and naval vessel is big, and bacterium such as is easy to grow at problem, also is that environmental engineering is badly in need of the important topic that solves.Shape memory alloy has its unique advantages in the metallic substance of numerous high dampings.Because they except that having the high damping ability usually, also have other material the unique function that can not have simultaneously, as shape memory effect and super-elasticity.
Consideration based on the application of aspects such as bone reconstruct and energy absorption, porous marmem has caused people's extensive concern, and excite constituent element as the carrying in the composite structure, be successfully applied among wing (Boeing, 1998), rotor, submarine, plate armour and other weapons system.From 1997, (the Naval Research Laboratory of United States Navy, NRL), air force (Air Force Office of Scientific Research), space agency (NASA Langley ResearchCenter), the Boeing (Boeing) and the National Science Foundation council (National Science Foundation) etc. drop into huge fund in succession, and the preparation science and the dynamic behavior of porous marmem are studied.Other country (comprising China) has also shown very big interest to this field, has launched the research of preparation and aspect of performance in succession.Yet up to the present, the research of porous marmem is also only limited to the TiNi alloy, but the price of TiNi alloy costliness is determining to a certain degree it can not be widely used in the numerous areas of damping noise reduction.And with NiTi alloy phase ratio, copper-based shape memory alloy is cheap, adds that its processing characteristics is good, simultaneously, can effectively draw up the again breeding of bacterium, this makes the porous copper-based shape memory alloy be more suitable for becoming a kind of high damping shock absorption acoustic damping materials of novel practical.In a word, copper Quito hole shape memorial alloy is as a kind of porous metal material, also should have strong, the high noise reduction of lightweight, height ratio of porous metal material and suppress good characteristic such as bacteria breed except that having the high damping characteristic; As a kind of material of high energy-absorbing noise reduction, copper Quito hole shape memorial alloy is expected to be used to impact all many-sides such as energy-absorbing, noise reduction again.
The preparation technology of porous marmem mainly contains following several: self propagating high temperature synthesis method (SHS), non-tight hot isostatic pressing method (CF-HIP), spark plasma sintering method (SPS) etc.Yet these methods all can't accurately be controlled pore structure (comprising pore dimension, shape, orientation, distribution etc.) parameter.In porous material, pore structure plays important effect to the overall performance of material, for the success ratio that improves specimen preparation, can accurately control and optimize material property to pore structure parameter, and necessary exploration and develop new preparation technology.
Summary of the invention
Purpose of the present invention just provides the preparation method of the controlled porous C uAlMn shape memory alloy of a kind of pore structure parameter, has that pore structure parameter is controlled, desalination characteristics completely.
The objective of the invention is to realize by following manner:
The present invention includes following steps
(1) Cu-Al-Mn alloy melting;
(2) high-purity N
2The Cu-Al-Mn alloy melt is atomized into the Cu-Al-Mn powdered alloy;
(3) the NaCl powder sieving is become the granularity of 355-800 μ m, 800-1000 μ m, standby;
(4) add the raw spirit uniform mixing with sieving out less than the Cu-Al-Mn alloy powder of 75 μ m and the granularity NaCl powder of 355-800 μ m or 800-1000 μ m;
(5) vacuum heating-press sintering
Mixed powder in (4) step is packed in the graphite mo(u)ld of vacuum hotpressing machine, be evacuated to 10
-2-10
-3Pa is warming up to 180-220 ℃ then and removes alcohol, is warming up to 750-790 ℃ subsequently and carries out hot pressed sintering, and hot pressing pressure is 25-30Mpa, forms the compound base just of Cu-Al-Mn alloy and NaCl;
(6) high temperature sintering and evaporative desalination
In the vacuum hotpressing machine, with the pressure complete discharge, and continue to be warming up to 900-990 ℃, insulation 16-38h with the complete evaporative removal of NaCl, forms porous material hot pressing billet;
(7) under the argon gas atmosphere protective condition, porous material hot pressing billet is melted quenching admittedly, obtain porous C uAlMn shape memory alloy.
Hot pressing time is preferably 2-4h in described (5) step.
In described (2) above-mentioned Cu-Al-Mn alloy melt is superheated to 1280-1320 ℃, pours in the atomisation unit, use high-purity N greater than 3MPa
2Gas atomizes by spraying gun.
Can NaCl be prepared earlier before NaCl screening in described (3), preparation process is, analytically pure NaCl powder is dissolved in distilled water after, in drying baker, dry to constant weight, after rolling fragmentation repeatedly, screening.
The step of described (7) is: under the argon gas atmosphere protective condition hot pressing billet is heated to 750-820 ℃ and is incubated 5-15 minute, and in the entry of quenching, obtain porous C uAlMn shape memory alloy.
This alloy is controlled porosity not only, and structural parameter such as pore dimension, shape, distribution, orientation all can be realized accurate control by its preparation technology; In addition, this alloy also has characteristics such as intensity height, energy-absorbing be big.And this preparation method's advantage is effective control hot-forming and two processes of evaporative desalination, consistent by the hot-forming hole orientation of impelling, guarantee that by evaporative desalination NaCl removes fully with the form of steam, thereby eliminated the corrosive nature of remaining NaCl to matrix metal, this also is the key point that this method can prepare closed-cell materials.
In the existing technology that removes NaCl, after main employing billet is made, in mobile water, remove the processing of NaCl, this method wants thoroughly to remove NaCl, then need long time, this side causes the waste of water resources, the opposing party causes the oxidation of billet easily, reduce its mechanical property, method of the present invention has been save and has been utilized water to take off the operation of NaCl for a long time after billet is made, the oxidation of the billet that can save great lot of water resources, has caused when having avoided taking off NaCl in water simultaneously, what NaCl removed is thorough, complete.
The porous C uAlMn shape memory alloy that pore structure parameter is controlled, alloying constituent is: Al:10.0-12.0wt%, Mn:2.0-4.0wt%, surplus is Cu and unavoidable impurities; The open-cell porosity scope is 50%-85%, pore shape size and used pore-forming material (sheet NaCl) particle shape consistent size, and sheetlike pores is and aligns and be evenly distributed.Utilize this technology also can prepare closed pore porous C uAlMn shape memory alloy, porosity ranges is 0%-20%, even pore distribution.
The concrete preparation method of the porous C uAlMn shape memory alloy that pore structure parameter is controlled mainly comprises:
(1) Cu-Al-Mn alloy melting
With electrolytic copper (purity 99.99%) and Cu-Al, Cu-Mn master alloy is raw material, and 1150 ℃-1250 ℃ of temperature of fusion, melt high-purity N are melted in electrolytic copper oven dry back in medium-frequency induction furnace
2Gas shiled, in the ratio adding Cu-Al and the Cu-Mn master alloy of final alloying constituent, molten even back forms the Cu-Al-Mn alloy melt of required composition;
(2) high-purity N
2Aerosolization Cu-Al-Mn alloy powder
Above-mentioned Cu-Al-Mn alloy melt is superheated to 1280-1320 ℃, pours in the atomisation unit, use high-purity N greater than 3MPa
2Gas is atomized into the Cu-Al-Mn powdered alloy by spraying gun with the Cu-Al-Mn alloy melt.For preventing that the Cu-Al-Mn alloy should be full of high-purity N in advance in the oxidation of droplet state surface in the atomizing in atomizing cup
2Gas, will control during atomizing in the atomizing cup is pressure-fired;
(3) sheet NaCl powdered preparation
For obtaining the sheet NaCl powder of different grain size scope, with analytically pure NaCl powder (about 100 μ m, square) dissolves in the distilled water and reach capacity, in drying baker, dry subsequently to constant weight to realize recrystallize, thick recrystallize particle can cover the internal surface of cylindrical beaker, after rolling fragmentation repeatedly, 35-5800 μ m is chosen in screening and two kinds of different grain sizes of 800-1000 μ m are prepared against use;
(4) Cu-Al-Mn alloy powder and NaCl powder uniform mixing
The Cu-Al-Mn alloy powder that sieves out less than 75 Jing is mixed with the NaCl powder of 355-800 μ m or 800-1000 μ m granularity, put into " V " type mixer, add an amount of raw spirit, thorough mixing forms uniform mixed powder after 30 minutes; The adding of raw spirit can make powder form " wet-milling ", thereby granulometric facies can evenly be adsorbed on the relatively large NaCl powder surface of granularity to less Cu-Al-Mn powdered alloy in mixing process;
(5) vacuum heating-press sintering
Above-mentioned compound is packed in the graphite mo(u)ld of vacuum hotpressing machine, be evacuated to 10
-2-10
-3Pa is warming up to 200 ℃ of insulation 1h earlier, to remove raw spirit residual in the mixed powder, carry out hot pressed sintering after being warming up to 780 ℃ (the NaCl fusing point is 801 ℃) subsequently, the hot pressed sintering time is 3h, and hot pressing pressure 25-28Mpa will form base at the beginning of Cu-Al-Mn alloy and NaCl compound this moment.The Cu-Al-Mn powdered alloy is easily deformable under the high temperature, and along with mixed powder constantly shrinks densification, unfused sheet NaCl powder can constantly rotate under the effect of uniaxial pressure, and final, sheet NaCl aligns by being perpendicular to the hot pressing direction;
(6) high temperature sintering and evaporative desalination
In the vacuum hotpressing machine, behind the pressure complete discharge, and continue to be warming up to 990 ℃ (the matrix alloy fusing point is 1030 ℃), insulation 24h.NaCl just melts when being higher than 801 ℃, but melt can't flow out in close-fitting graphite mo(u)ld, and when temperature continues to raise, the saturated vapor pressure of NaCl melt is soaring rapidly, reaches 922.8pa in the time of 990 ℃, far above the vacuum tightness 10 of hot pressing furnace
-2-10
-3Pa, NaCl steam are drawn out of continuously until removing fully.Meanwhile, long-time sintering under near the temperature of fusing point, the diffusion of Cu-Al-Mn matrix fully, metal frame intensity further improves.Form porous C uAlMn shape memory alloy hot pressing billet behind the furnace cooling;
(7) solid molten the quenching
Under the argon gas atmosphere protective condition, the hot pressing billet is heated to 800 ℃ and is incubated 20 minutes, and in the entry of quenching, make the CuAlMn matrix at room temperature be the martensite attitude.
In sum, method of the present invention can accurately be controlled pore structure (comprising pore dimension, shape, orientation, distribution etc.) parameter, alloy obtained by the method for the present invention has the intensity height, energy-absorbing is big, the porosity height, and save the operation of utilizing water to take off NaCl for a long time after billet is made, and the oxidation of the billet that saved water resources so on the one hand, has caused when having avoided in water, taking off NaCl, what make simultaneously that NaCl removes waits advantage thoroughly, fully.
Description of drawings
Fig. 1: process flow diagram of the present invention
Fig. 2: alloy hot pressing ingot outward appearance of the present invention, wherein (a): perforate CuAlMn hot pressing ingot, (b): closed pore CuAlMn hot pressing ingot
Fig. 3: the stereoscopic metallographic of alloy of the present invention, wherein (a): perforate CuAlMn square section, (b): perforate CuAlMn vertical section
Fig. 4: alloy metallograph of the present invention, wherein (a): perforate CuAlMn square section, (b): perforate CuAlMn vertical section, (c): closed pore CuAlMn square section, (d): closed pore CuAlMn vertical section
Embodiment
Embodiment 1: alloying constituent is Cu-11.9Al-2.5Mn (wt%), get the NaCl of 800-1000 μ m granularity, CuAlMn and NaCl are 2: 1 thorough mixing by mass ratio, make the hot pressing billet of Φ 70 by the method described in " summary of the invention ", measurement hot pressing front and back sample quality is determined that desalination is complete as is denied that line cuts into required test sample.The exterior appearance of present embodiment hot pressing billet is seen Fig. 2 (a), and its stereoscopic metallographic is seen Fig. 3 (a) and (b), and metallograph is seen Fig. 4 (a) and (b).As seen present embodiment alloy hole aligns in the form of sheets, is evenly distributed, and the pore shape size is consistent with used NaCl geomery, and present embodiment porous C uAlMn shape memory alloy pore structure and performance data are as shown in table 1.
Table 1 present embodiment porous C uAlMn shape memory alloy pore structure and performance data
| Porosity | Pore dimension | Horizontal ultimate compression strength (compression direction is perpendicular to the vertical section) | The horizontal compression Young's modulus | The horizontal compression energy-absorbing |
| 60％ | 800-1000μm | ?57.54Mpa | 2.01Gpa | 19.5MJ/m 3 |
| Perforate/closed pore | Pore shape | Vertical ultimate compression strength (compression direction is perpendicular to the square section) | Vertical compressive modulus of elasticity | Vertically compress energy-absorbing |
| Perforate | Sheet | ?30.40Mpa | 0.74Gpa | 16.9MJ/m 3 |
Embodiment 2: alloying constituent is Cu-11.9Al-2.5Mn (wt%), get the NaCl of 355-800 μ m granularity, CuAlMn and NaCl are 2: 1 thorough mixing by mass ratio, make the hot pressing billet of Φ 70 by the method described in " summary of the invention ", sample quality determines that desalination is complete before and after measuring hot pressing, and doubling cuts into required test sample.Present embodiment alloy hole aligns in the form of sheets, is evenly distributed, and the pore shape size is consistent with used NaCl geomery, and present embodiment porous C uAlMn shape memory alloy pore structure and performance data are as shown in table 2.
Table 2 present embodiment porous C uAlMn shape memory alloy pore structure and performance data
| Porosity | Pore dimension | Horizontal ultimate compression strength (compression direction is perpendicular to the vertical section) | The horizontal compression Young's modulus | The horizontal compression energy-absorbing |
| 60％ | 355-800μm | ?100.41Mpa | 3.36Gpa | 35.8MJ/m 3 |
| Perforate/closed pore | Pore shape | Vertical ultimate compression strength (compression direction is perpendicular to the square section) | Vertical compressive modulus of elasticity | Vertically compress energy-absorbing |
| Perforate | Sheet | ?51.50Mpa | 1.02Gpa | 25.7MJ/m 3 |
Embodiment 3: alloying constituent is Cu-11.9Al-2.5Mn (wt%), get the NaCl of 355-800 μ m granularity, CuAlMn and NaCl are 3: 1 thorough mixing by mass ratio, make the hot pressing billet of Φ 70 by the method described in " summary of the invention ", sample quality determines that desalination is complete before and after measuring hot pressing, and doubling cuts into required test sample.The compression curve of present embodiment sample is seen Fig. 5 (a).Present embodiment alloy hole aligns in the form of sheets, is evenly distributed, and the pore shape size is consistent with used NaCl geomery, and present embodiment porous C uAlMn shape memory alloy pore structure and performance data are as shown in table 3.
Table 3 present embodiment porous C uAlMn shape memory alloy pore structure and performance data
| Porosity | Pore dimension | Horizontal ultimate compression strength (compression direction is perpendicular to the vertical section) | The horizontal compression Young's modulus | The horizontal compression energy-absorbing |
| 51％ | 355-800μm | ?123.46Mpa | 4.23Gpa | 31.7MJ/m 3 |
| Perforate/closed pore | Pore shape | Vertical ultimate compression strength (compression direction is perpendicular to the square section) | Vertical compressive modulus of elasticity | Vertically compress energy-absorbing |
| Perforate | Sheet | ?63.54Mpa | 1.54Gpa | 17.8MJ/m 3 |
Embodiment 4: alloying constituent is Cu-11.9Al-2.5Mn (wt%), get the NaCl of 355-800 μ m granularity, CuAlMn and NaCl are 4: 1 thorough mixing by mass ratio, make the hot pressing billet of Φ 70 by the method described in " summary of the invention ", sample quality determines that desalination is complete before and after measuring hot pressing, and doubling cuts into required test sample.The exterior appearance of present embodiment hot pressing billet is seen Fig. 2 (b), and its metallograph is seen Fig. 4 (c), (d), and compression curve is seen Fig. 5 (b).Present embodiment alloy hole is a closed pore, is spherical, is evenly distributed.With respect to used NaCl powder, formed hole has obvious shrinkage phenomenon, this be since when CuAlMn powder volume mark in CuAlMn and the NaCl mixed powder greater than 50% the time, the CuAlMn powder just wraps up the NaCl particle wherein fully, behind the NaCl evaporative removal, form independently blind hole crack, during high temperature sintering, the CuAlMn matrix is because the continuous densification of diffusion, impel the flaky storage pore of script constantly to shrink nodularization, present embodiment porous C uAlMn shape memory alloy pore structure and performance data are as shown in table 4.
Table 4 present embodiment porous C uAlMn shape memory alloy pore structure and performance data
| Porosity | Pore dimension | Horizontal ultimate compression strength (compression direction is perpendicular to the vertical section) | The horizontal compression Young's modulus | The horizontal compression energy-absorbing |
| 17％ | 50-500μm | ?736.75Mpa | 8.62Gpa | 120.1MJ/m 3 |
| Perforate/closed pore | Pore shape | Vertical ultimate compression strength (compression direction is perpendicular to the square section) | Vertical compressive modulus of elasticity | Vertically compress energy-absorbing |
| Closed pore | Spherical | ?736.35Mpa | 8.62Gpa | 120.1MJ/m 3 |
Claims (5)
1. the preparation method of the controlled porous C uAlMn shape memory alloy of a pore structure parameter is characterized in that, may further comprise the steps
(1) Cu-Al-Mn alloy melting;
(2) high-purity N 2 is atomized into the Cu-Al-Mn powdered alloy with the Cu-Al-Mn alloy melt;
(3) the NaCl powder sieving is become the granularity of 355-800 μ m, 800-1000 μ m, standby;
(4) add the raw spirit uniform mixing with sieving out less than the Cu-Al-Mn alloy powder of 75 μ m and the granularity NaCl powder of 355-800 μ m or 800-1000 μ m;
(5) vacuum heating-press sintering
Mixed powder in (4) step is packed in the graphite mo(u)ld of vacuum hotpressing machine, be evacuated to 10-2-10-3Pa, be warming up to 180-220 ℃ then and remove alcohol, be warming up to 750-790 subsequently? carry out hot pressed sintering, hot pressing pressure is 25-30Mpa, forms base at the beginning of Cu-Al-Mn powdered alloy and NaCl compound in hot pressing time 2-6 hour;
(6) high temperature sintering and evaporative desalination
In the vacuum hotpressing machine, with the pressure complete discharge, and continue to be warming up to 900-990 ℃, insulation 16-38h with the complete evaporative removal of NaCl, forms the hot pressing billet of porous material;
(7) under the argon gas atmosphere protective condition with the solid solution of porous material hot pressing billet, quenching, obtain porous C uAlMn shape memory alloy.
2. method according to claim 1 is characterized in that, hot pressing time is 2-4h in described (5) step.
3. method according to claim 1 is characterized in that, in described (2) above-mentioned Cu-Al-Mn alloy melt is superheated to 1280-1320 ℃, pours in the atomisation unit, uses greater than 3MPa high-purity N 2 gas to atomize by spraying gun.
4. method according to claim 1 is characterized in that, before the NaCl screening NaCl is prepared earlier in described (3), preparation process is, analytically pure NaCl powder is dissolved in distilled water after, in drying baker, dry to constant weight, after rolling fragmentation repeatedly, screening.
5. method according to claim 1 is characterized in that, the step of described (7) is: under the argon gas atmosphere protective condition hot pressing billet is heated to 750-820 ℃ and is incubated 5-15 minute, and in the entry of quenching, obtain porous C uAlMn shape memory alloy.
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| CN103421981A (en) * | 2013-08-08 | 2013-12-04 | 常熟市东方特种金属材料厂 | High-damping shape memory alloy |
| CN107043867A (en) * | 2017-01-09 | 2017-08-15 | 河北工业大学 | A kind of preparation method of porous copper-based shape memory alloy |
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| CN107043867B (en) * | 2017-01-09 | 2019-02-22 | 河北工业大学 | A kind of preparation method of porous copper-based shape memory alloy |
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| CN108817403A (en) * | 2018-06-28 | 2018-11-16 | 西北工业大学 | A kind of preparation method of nuclear battery transom porous platinum ventail |
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| CN109277571A (en) * | 2018-09-25 | 2019-01-29 | 中南大学 | A kind of therlo/polymer/carbon nano-tube damping material and preparation method |
| CN111216876A (en) * | 2018-11-26 | 2020-06-02 | 埃姆普里萨有限公司 | Thermally configurable structural element, in particular for an aircraft component |
| CN110788340A (en) * | 2019-11-13 | 2020-02-14 | 中南大学 | Preparation method of 4D printing copper-based shape memory alloy and 4D printing copper-based shape memory alloy |
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Application publication date: 20110921 |