CN102925779A - Method for preparing cobalt-nickel-aluminum (Co-Ni-Al) alloy based on electroplating and thermal diffusion - Google Patents
Method for preparing cobalt-nickel-aluminum (Co-Ni-Al) alloy based on electroplating and thermal diffusion Download PDFInfo
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- CN102925779A CN102925779A CN2012104093114A CN201210409311A CN102925779A CN 102925779 A CN102925779 A CN 102925779A CN 2012104093114 A CN2012104093114 A CN 2012104093114A CN 201210409311 A CN201210409311 A CN 201210409311A CN 102925779 A CN102925779 A CN 102925779A
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Abstract
The invention discloses a method for preparing a cobalt-nickel-aluminum (Co-Ni-Al) alloy based on electroplating and thermal diffusion. The method comprises the following steps of: performing composite electroplating by taking an aluminum foil as a base material to obtain a Co-Ni alloy layer; and forming a Co-Ni-Al magnetically-controlled shape memory alloy through thermal diffusion. The method is simple in process and high in performance and stability, technical bottleneck problems that the conventional Co-Ni-Al magnetically-controlled memory alloy is large in driving magnetic field and small magnetic field-induced strain and the like are well solved, and practical application of the magnetically-controlled memory alloy to fields such as large-power underwater sonars, micro shifters, vibration and noise control, linear motors, microwave devices and robots is promoted.
Description
Technical field
The present invention relates to magnetic control shape memory Metallic Functional Materials technology of preparing, be specifically related to a kind of method for preparing the Co-Ni-Al alloy based on the plating thermodiffusion.
Background technology
Magnetic shape memory alloy, (Magnetic Shape Memory Alloy, MSMA) not only has the thermo-elasticity shape memory effect that the conventional shape-memory alloy is subjected to Temperature Field Control, and has the magnetic shape memory effect that is subjected to magnetic field control.Therefore, the overall characteristic that alloy has large recovery strain concurrently, exports stress, high response frequency and can accurately control greatly, make it important application be arranged in fields such as high-power underwater sonar, micro positioner, vibrations and noise control, linear motor, microwave device, robots, a new generation that is expected to become after piezoelectric ceramics and the magnetostriction materials drives and sensing material.At present, the magnetic shape memory alloy of having found mainly comprises: Ni is associated golden Ni-Mn-Ga, Ni-Al-Mn, Ni-Co-Al, Ni-Fe-Ga-Co etc.; Co is associated golden Co-Mn, Co-Ni, Co-Ni-Ga etc.; Fe is associated golden Fe-Pd, Fe-Mn-Si, Fe-Ni-Co-Ti, Fe-Pt, etc. wherein, the Ni-Mn-Ga alloy is the MSMA that finds the earliest, its research is comparatively ripe, the existing report that is applied to the aspects such as linear actuator, linear electric motors, but the stability of alloy property and repeatability are not ideal enough.
Co base ferromagnetic shape memory alloys comprises Co-Ni-Ga and Co-Ni-Al two class alloys, has the advantages such as the large and hot workability excellence of magnetocrystalline anisotropy energy.Co-Ni-Al is unique a kind of MSMA that solidifies in the eutectic mode, and has the two-phase coexistent district of broad crystallisation scope, and shows abundant multiphase coexistence behavior in the functional component scope, and the preparation method is relatively simple, and is cheap, has larger application prospect.
Both at home and abroad the researcher adopts routine to solidify, high undercooling solidifies, Co-Ni-Al alloy under the preparation conditions such as method of directional freeze, rapid solidification and powder metallurgy, have good strain-induced shape memory effect, but still the technical bottleneck that the driving magnetic field of unresolved CoNiAl alloy is large, magneto-strain is little.
Utilization of the present invention is carried out composite plating Co-Ni alloy at aluminium foil, by adjusting heat treatment process parameter, finally prepares the Co-Ni-Al alloy of high comprehensive performance.
Summary of the invention
A kind of method for preparing the Co-Ni-Al alloy based on the plating thermodiffusion provided by the invention has the following steps:
1) electroplate the Co-Ni alloy layer at the fine aluminium substrate surface, the mass ratio of nickel is 10～90% in the above-mentioned Co-Ni alloy layer;
2) Co-Ni/Al after will electroplating puts into well heater, is 250 ℃～600 ℃ insulations 60～240 hours in temperature, diffuses to form uniform Co-Ni-Al alloy, takes out after cooling to room temperature with the furnace.
Above-mentioned steps 1) the fine aluminium base material thickness is 0.01mm～0.3mm in.
Above-mentioned steps 1) the electroplating technique flow process is in: at room temperature the fine aluminium substrate surface is cleaned oil removing with distilled water flushing, it is that 20% nitric acid, volume ratio are that at room temperature etching time is 40 hours in the pickling solution that forms of 1% hydrofluoric acid and surplus deionized water that cleaning is placed on after the oil removing by volume ratio; Then use the deionized water washing; Under the room temperature, sample put into to mix the pH value that forms by 15 g/L single nickel salts and 112 g/L Trisodium Citrates be that 13 solution activates, place afterwards electroplate liquid to electroplate; Stopping to electroplate sample dries up.
Above-mentioned plating is take fine aluminium as anode, and the prescription of described electroplate liquid is: single nickel salt 100～250 g/L, sodium-chlor 10～20 g/L, boric acid 20～40 g/L, rose vitriol 10～120 g/L, asccharin 1g/L; Continuous current in the electroplating process, electric current 0.15A, bath pH value are 4.6.Adjust the Co-Ni alloy layer that electroplate liquid composition and electroplating parameter can obtain at the fine aluminium base material heterogeneity.
Above-mentioned steps 2) well heater is retort furnace or vacuum oven in; Retort furnace takes to pass into nitrogen, argon gas or hydrogen shield gas for avoiding the coating oxidation, or Co-Ni/Al is put into the carbon reducing agent material heat.
Above-mentioned steps 2) soaking time determines according to fine aluminium base material and thickness of coating in, is heated to diffusion and obtains homogeneous chemical composition Co-Ni-Al alloy.
Beneficial effect of the present invention:
1. adopt composite electric plating method at aluminium base preparation Co-Ni alloy, control thermal treatment process, the composition of coating and the parameters such as thickness of matrix are prepared high comprehensive performance Co-Ni-Al alloy.
2. equipment cost and the technical requirements of preparation Co-Ni-Al alloy are low, only need simple power supply and well heater can prepare the Co-Ni-Al alloy.
3. preparation method's technique of the present invention is simple, and stability is good, solves preferably the Pinch technology difficult points such as the driving magnetic field that current C o-Ni-Al magnetic control memorial alloy remains is large, magneto-strain is little.
Embodiment
Below in conjunction with specific embodiment in detail the present invention is described in detail.
Embodiment 1
1) at the fine aluminium substrate surface of 0.05mm thickness, under the room temperature fine aluminium substrate surface is cleaned oil removing with distilled water flushing, it is that 20% nitric acid, volume ratio are that at room temperature etching time is 40 hours in the pickling solution that forms of 1% hydrofluoric acid and surplus deionized water that cleaning is placed on after the oil removing by volume ratio; Then use the deionized water washing; Under the room temperature, sample put into to mix the pH value that forms by 15 g/L single nickel salts and 112 g/L Trisodium Citrates be that 13 solution activates, place afterwards electroplate liquid to electroplate; Stopping to electroplate sample dries up.
The compositing formula of above-mentioned electroplate liquid is: single nickel salt 250g/L, sodium-chlor 10 g/L, boric acid 40 g/L, rose vitriol 55 g/L, asccharin 1g/L; Electroplating parameter is: continuous current in the plating process, electric current 0.15A, bath pH value are 4.6.Stop to electroplate sample and dry up, obtain the Co-54.2%Ni alloy layer, wherein the mass ratio of nickel is 54.2% in the above-mentioned Co-Ni alloy layer;
2) Co-54.2%Ni after will electroplating/Al sample is put into retort furnace, temperature be under 550 ℃, argon gas atmosphere insulation to obtain composition after 60 hours be the Co-45.0%Ni-17%Al alloy.
3) take out after cooling to room temperature with the furnace.
Embodiment 2
1) at the fine aluminium substrate surface of 0.1mm thickness, under the room temperature fine aluminium substrate surface is cleaned oil removing with distilled water flushing, it is that 20% nitric acid, volume ratio are that at room temperature etching time is 40 hours in the pickling solution that forms of 1% hydrofluoric acid and surplus deionized water that cleaning is placed on after the oil removing by volume ratio; Then use the deionized water washing; Under the room temperature, sample put into to mix the pH value that forms by 15 g/L single nickel salts and 112 g/L Trisodium Citrates be that 13 solution activates, place afterwards electroplate liquid to electroplate; Stopping to electroplate sample dries up.
The compositing formula of above-mentioned electroplate liquid is: single nickel salt 100g/L, sodium-chlor 20 g/L, boric acid 40 g/L, rose vitriol 120 g/L, asccharin 1g/L; Electroplating parameter is: continuous current in the plating process, electric current 0.15A, bath pH value are 4.6.Stop to electroplate sample and dry up, obtain the Co-9.9%Ni alloy layer, wherein the mass ratio of nickel is 9.9% in the above-mentioned Co-Ni alloy layer;
2) Co-9.9%Ni after will electroplating/Al sample is put into Vacuum Heat and is come out of the stove, and is that to obtain composition after 200 hours be the Co-6.0%Ni-40.0%Al alloy in 300 ℃ of lower insulations in temperature.
3) take out after cooling to room temperature with the furnace.
Embodiment 3
1) at the fine aluminium substrate surface of 0.2mm thickness, under the room temperature fine aluminium substrate surface is cleaned oil removing with distilled water flushing, it is that 20% nitric acid, volume ratio are that at room temperature etching time is 40 hours in the pickling solution that forms of 1% hydrofluoric acid and surplus deionized water that cleaning is placed on after the oil removing by volume ratio; Then use the deionized water washing; Under the room temperature, sample put into to mix the pH value that forms by 15 g/L single nickel salts and 112 g/L Trisodium Citrates be that 13 solution activates, place afterwards electroplate liquid to electroplate; Stopping to electroplate sample dries up.
The compositing formula of above-mentioned electroplate liquid is: single nickel salt 175g/L, sodium-chlor 20 g/L, boric acid 20 g/L, rose vitriol 10 g/L, asccharin 1g/L; Electroplating parameter is: continuous current in the plating process, electric current 0.15A, bath pH value are 4.6.Stop to electroplate sample and dry up, obtain the Co-41.5%Ni alloy layer, wherein the mass ratio of nickel is 41.5% in the above-mentioned Co-Ni alloy layer;
2) Co-41.5%Ni after will electroplating/Al sample is put into retort furnace, is that to obtain composition after 180 hours be the Co-35.0%Ni-14.5%Al alloy for 400 ℃, nitrogen atmosphere insulation in temperature.
3) take out after cooling to room temperature with the furnace.
Embodiment 4
1) at the fine aluminium substrate surface of 0.15mm thickness, under the room temperature fine aluminium substrate surface is cleaned oil removing with distilled water flushing, it is that 20% nitric acid, volume ratio are that at room temperature etching time is 40 hours in the pickling solution that forms of 1% hydrofluoric acid and surplus deionized water that cleaning is placed on after the oil removing by volume ratio; Then use the deionized water washing; Under the room temperature, sample put into to mix the pH value that forms by 15 g/L single nickel salts and 112 g/L Trisodium Citrates be that 13 solution activates, place afterwards electroplate liquid to electroplate; Stopping to electroplate sample dries up.
The compositing formula of above-mentioned electroplate liquid is: single nickel salt 250g/L, sodium-chlor 20 g/L, boric acid 30 g/L, rose vitriol 10 g/L, asccharin 1g/L; Electroplating parameter is: continuous current in the plating process, electric current 0.15A, bath pH value are 4.6.Stop to electroplate sample and dry up, obtain the Co-88.3%Ni alloy layer, wherein the mass ratio of nickel is 88.3% in the above-mentioned Co-Ni alloy layer;
2) Co-88.3%Ni after will electroplating/Al sample is put into retort furnace, temperature be under 600 ℃, carbon dust coat insulation to obtain composition after 80 hours be the Co-80%Ni-9.4%Al alloy.
3) take out after cooling to room temperature with the furnace.
Embodiment 5
1) at the fine aluminium substrate surface of 0.3mm thickness, under the room temperature fine aluminium substrate surface is cleaned oil removing with distilled water flushing, it is that 20% nitric acid, volume ratio are that at room temperature etching time is 40 hours in the pickling solution that forms of 1% hydrofluoric acid and surplus deionized water that cleaning is placed on after the oil removing by volume ratio; Then use the deionized water washing; Under the room temperature, sample put into to mix the pH value that forms by 15 g/L single nickel salts and 112 g/L Trisodium Citrates be that 13 solution activates, place afterwards electroplate liquid to electroplate; Stopping to electroplate sample dries up.
The compositing formula of above-mentioned electroplate liquid is: single nickel salt 220g/L, sodium-chlor 15 g/L, boric acid 40 g/L, rose vitriol 50 g/L, asccharin 1g/L; Electroplating parameter is: continuous current in the plating process, electric current 0.15A, bath pH value are 4.6.Stop to electroplate sample and dry up, obtain the Co-49.9%Ni alloy layer, wherein the mass ratio of nickel is 49.9% in the above-mentioned Co-Ni alloy layer;
2) Co-49.9%Ni after will electroplating/Al sample is put into retort furnace, is 450 ℃ in temperature, comes out of the stove at Vacuum Heat that to obtain composition after 240 hours be the Co-14.9%Ni-70.2%Al alloy in interior insulation.
3) take out after cooling to room temperature with the furnace.
Claims (6)
1. one kind based on the method for electroplating thermodiffusion and prepare the Co-Ni-Al alloy, it is characterized in that the method has the following steps:
1) electroplate the Co-Ni alloy layer at the fine aluminium substrate surface, the mass ratio of nickel is 10～90% in the above-mentioned Co-Ni alloy layer;
2) Co-Ni/Al after will electroplating puts into well heater, is 250 ℃～600 ℃ insulations 60～240 hours in temperature, diffuses to form uniform Co-Ni-Al alloy, takes out after cooling to room temperature with the furnace.
2. method according to claim 1 is characterized in that: the fine aluminium base material thickness is 0.01mm～0.3mm above-mentioned steps 1).
3. method according to claim 1, it is characterized in that: the electroplating technique flow process is above-mentioned steps 1): at room temperature the fine aluminium substrate surface is cleaned oil removing with distilled water flushing, it is that 20% nitric acid, volume ratio are that at room temperature etching time is 40 hours in the pickling solution that forms of 1% hydrofluoric acid and surplus deionized water that cleaning is placed on after the oil removing by volume ratio; Then use the deionized water washing; Under the room temperature, sample put into to mix the pH value that forms by 15 g/L single nickel salts and 112 g/L Trisodium Citrates be that 13 solution activates, place afterwards electroplate liquid to electroplate; Stopping to electroplate sample dries up.
4. method according to claim 3, it is characterized in that: above-mentioned plating is take fine aluminium as anode; The prescription of described electroplate liquid is: single nickel salt 100～250 g/L, sodium-chlor 10～20 g/L, boric acid 20～40 g/L, rose vitriol 10～120 g/L, asccharin 1g/L; Continuous current in the electroplating process, electric current 0.15A, bath pH value are 4.6.
5. method according to claim 1 is characterized in that: well heater is retort furnace or vacuum oven above-mentioned steps 2); Retort furnace takes to pass into nitrogen, argon gas or hydrogen shield gas for avoiding the coating oxidation, or Co-Ni/Al is put into the carbon reducing agent material heat.
6. method according to claim 1 is characterized in that: soaking time determines according to fine aluminium base material and thickness of coating above-mentioned steps 2), is heated to diffusion and obtains homogeneous chemical composition Co-Ni-Al alloy.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107584134A (en) * | 2017-09-20 | 2018-01-16 | 安徽大学 | A kind of microwave spark system for the spherical semi-hard magnet Co Ni non-crystaline amorphous metals of grade method |
| CN113667860A (en) * | 2021-08-17 | 2021-11-19 | 宁波微泰真空技术有限公司 | Ultra-pure copper-aluminum ingot and preparation method and application thereof |
| CN113684389A (en) * | 2021-08-16 | 2021-11-23 | 大连大学 | Method for improving superelasticity of Co-Ni-Al magnetic memory alloy by controlling gamma phase distribution |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1219092C (en) * | 2003-04-08 | 2005-09-14 | 中国科学院金属研究所 | High-damping shape memory alloy |
| JP2006328436A (en) * | 2005-05-23 | 2006-12-07 | Nec Tokin Corp | Ti-Ni-Nb ALLOY ELEMENT |
| JP3872323B2 (en) * | 2001-09-21 | 2007-01-24 | 独立行政法人科学技術振興機構 | Co-Ni-Ga based Heusler type magnetic shape memory alloy and method for producing the same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP3872323B2 (en) * | 2001-09-21 | 2007-01-24 | 独立行政法人科学技術振興機構 | Co-Ni-Ga based Heusler type magnetic shape memory alloy and method for producing the same |
| CN1219092C (en) * | 2003-04-08 | 2005-09-14 | 中国科学院金属研究所 | High-damping shape memory alloy |
| JP2006328436A (en) * | 2005-05-23 | 2006-12-07 | Nec Tokin Corp | Ti-Ni-Nb ALLOY ELEMENT |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107584134A (en) * | 2017-09-20 | 2018-01-16 | 安徽大学 | A kind of microwave spark system for the spherical semi-hard magnet Co Ni non-crystaline amorphous metals of grade method |
| CN107584134B (en) * | 2017-09-20 | 2019-06-21 | 安徽大学 | A kind of microwave spark system for the spherical semi-hard magnet Co-Ni amorphous alloy of grade method |
| CN113684389A (en) * | 2021-08-16 | 2021-11-23 | 大连大学 | Method for improving superelasticity of Co-Ni-Al magnetic memory alloy by controlling gamma phase distribution |
| CN113684389B (en) * | 2021-08-16 | 2022-07-29 | 大连大学 | Method for improving superelasticity of Co-Ni-Al magnetic memory alloy by controlling gamma phase distribution |
| CN113667860A (en) * | 2021-08-17 | 2021-11-19 | 宁波微泰真空技术有限公司 | Ultra-pure copper-aluminum ingot and preparation method and application thereof |
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