CN105018888A - Manufacturing method for Ni50Mn34In12Co4 alloy film of high smoothness - Google Patents

Manufacturing method for Ni50Mn34In12Co4 alloy film of high smoothness Download PDF

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CN105018888A
CN105018888A CN201510446285.6A CN201510446285A CN105018888A CN 105018888 A CN105018888 A CN 105018888A CN 201510446285 A CN201510446285 A CN 201510446285A CN 105018888 A CN105018888 A CN 105018888A
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preparation
alloy firm
substrate
flatness
film
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CN105018888B (en
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董桂馥
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Dalian University
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Dalian University
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Abstract

The invention relates to a manufacturing method for a Ni50Mn34In12Co4 alloy film of high smoothness. The method includes the following steps that metal elements of Ni, Mn, In and Co are prepared according to the mol fractional ratio of 50:34:12:4 and placed in a vacuum nonconsumable electrode electric-arc furnace to be smelted; the electric-arc furnace is vacuumized to be of 5*10-3 Pa, and is filled with shielding gas to obtain a round target; a processed substrate and the target are placed in a vacuum system, the vacuum system is vacuumized to be of 1.0*10-4 Pa, and the distance between the substrate and the target is 3-5 cm; a laser device emits laser, the control frequency is 3-4 Hz, sputtering is conducted for 1-3 h, and a film of the required thickness is obtained; and the film is subjected to annealing for 0.5-3 h at the temperature of 800-900 DEG C, and then Ni50Mn34In12Co4 ferromagnetism shape memory alloy film of the high smoothness is obtained. The Ni50Mn34In12Co4 alloy film prepared according to the method has more accurate ingredients, lower roughness and good anisotropism. The alloy film is good in toughness, high in strength and easy to prepare and produce industrially, and is of great practical value on micro intelligence and high integration.

Description

A kind of Ni of high-flatness 50mn 34in 12co 4the preparation method of alloy firm
Technical field
The invention belongs to field of metal alloy technology, relate to a kind of Ni of high-flatness 50mn 34in 12co 4the preparation method of alloy firm.
Background technology
Martensite reverse transformation can be there is in Ni-Co-Mn-In monocrystalline under the action of a magnetic field, the precompression of 3% can be made to strain recover completely, theory in this process exports stress can reach 108MPa, high two orders of magnitude of output stress than Ni-Mn-Ga, this research makes magnetically driven shape memory alloy stride forward a huge step to practical.But monocrystal material complicated process of preparation, cost height limits their widespread use to a certain extent.And the grain orientation of Ni-Mn-Co-In polycrystalline is different, there is strain coordination between neighboring die, so the maximum reversible strain property in shape memory effect is lower, thus limit its widespread use, be difficult to the requirement meeting engineer applied and the development of MEMS micro element.Existing many technology carry out obtained alloy firm at present, mainly comprise magnetron sputtering (Magnetron sputtering) technology, pulsed laser deposition (Pulsed Laser Deposition) technology and molecular beam epitaxy (Molecular Beam Epitaxy) technology.Research shows, owing to being subject to the impact of sputter deposition rate when adopting magnetron sputtering technique to prepare film, the chemical composition of film is made to depart from its stoichiometric ratio, especially some volatile elements depart from even more serious, therefore magnetron sputtering technique is not suitable for preparing volatile ferromagnetic shape memory alloy film, and molecular beam epitaxy technique is high due to its apparatus expensive, maintenance cost, development is caused to be restricted.Pulsed laser deposition (PLD) method belongs to non-equilibrium film-forming method, and this depositing temperature required by technology growth film is low, and is realized the same component deposition of film by non-thermal film deposition techniques.In the process of deposition, being separated can not appear in laser and target, thus can copy on film by the chemistry of target and crystallographic characteristics, realize the same component deposition of film.In addition, in the process of doping masking, many targets alternating sputtering deposition method can being used, by controlling the umber of pulse of each target, preparing the function film of arbitrary proportion Uniform Doped.
Summary of the invention
The present invention is too large in order to solve existing ferromagnetic shape memory Film roughness, and composition departs from target, and provides a kind of Ni of high-flatness 50mn 34in 12co 4the preparation method of alloy firm.
For achieving the above object, the present invention is achieved in that a kind of Ni of high-flatness 50mn 34in 12co 4the preparation method of alloy firm, comprises the following steps: get Ni, Mn, In, Co metal simple-substance according to molfraction respectively than 50:34:12:4 and be positioned over melting in vacuum non-consumable electrode electric arc furnace; 5 × 10 are evacuated to by electric arc furnace -3pa, is filled with protection gas, obtains circular target; Substrate after process and target are placed in vacuum system, are evacuated to 1.0 × 10 -4pa, substrate temperature is 500 ~ 750 DEG C, and substrate and target distance are 3 ~ 5cm.Use laser apparatus Emission Lasers again, controlled frequency is 3 ~ 4Hz, sputters 1 ~ 3 hour, preferably 2 hours, the film of obtained required thickness; Eventually pass 800 ~ 900 DEG C of annealing 3h, prepare the Ni of high-flatness 50mn 34in 12co 4ferromagnetic shape memory alloy film.This annealing time is crystallization time, annealing temperature preferably 850 DEG C.Further, described substrate temperature is 550 ~ 700 DEG C.
Further, the purity of described Ni metal simple-substance is 99.99at.%.
Further, the purity of described Mn metal simple-substance is 99.95at.%.
Further, the purity of described In metal simple-substance is 99.99at.%.
Further, the purity of described Co metal simple-substance is 99.95at.%.
Further, described noble gas is argon gas.
For ensureing the homogeneity of alloy composition in fusion process, before each melting, by sample upset at least four times and in addition magnetic stirs.Mechanical manipulator can be adopted to realize sample upset, after melting, obtain the ingot of diameter 50mm.Ingot is put into circular target WEDM being cut into and being of a size of diameter 3mm × 2mm after polishing by emery wheel.
Further, described substrate is quartz glass substrate, and the specification of this substrate is 30mm × 30mm × 3mm; The treatment process of described substrate is: glass substrate, first through deionization washing, then in acetone ultrasonic 10 ~ 15 minutes, then use washes of absolute alcohol, is dried.
The Ni of the high-flatness that the present invention also asks protection aforesaid method to be prepared 50mn 34in 12co 4alloy firm.
Different from existing magnetic shape memory alloy Ni-Mn-In-Co film, Ni of the present invention 50mn 34in 12co 4ferromagnetic shape memory alloy film has the following advantages:
1, the Ni for preparing of the present invention 50mn 34in 12co 4the composition of alloy firm is more accurate, achieves the multi-element compounds film consistent with target material composition;
2, the Ni for preparing of the present invention 50mn 34in 12co 4the roughness of alloy firm is lower, and its average roughness is at about 45nm;
3, the Ni for preparing of the present invention 50mn 34in 12co 4the magnetic domain of alloy firm tends to a direction arrangement, and anisotropy is strong;
4, low in raw material price required for the present invention, rich reserves, alloy firm good toughness, the intensity of preparation are large, and preparation technology is simple, is easy to suitability for industrialized production, provide new thinking for solving Ni-Mn-In-Co bulk defect, for micro-intellectuality and highly integratedly have important practical value.
Accompanying drawing explanation
Fig. 1 is Ni prepared by the present invention 50mn 34in 12co 4the AFM shape appearance figure of alloy firm, wherein (a) is the AFM shape appearance figure of substrate temperature 700 DEG C of obtained alloy firms; B () is the AFM shape appearance figure of substrate temperature 650 DEG C of obtained alloy firms; C () is the AFM shape appearance figure of substrate temperature 600 DEG C of obtained alloy firms; D () is the AFM shape appearance figure of substrate temperature 550 DEG C of obtained alloy firms;
Fig. 2 is Ni prepared by the present invention 50mn 34in 12co 4the magnetic domain shape appearance figure of alloy firm, wherein (a) is the magnetic domain shape appearance figure of substrate temperature 700 DEG C of obtained alloy firms; B () is the magnetic domain shape appearance figure of substrate temperature 650 DEG C of obtained alloy firms; C () is the magnetic domain shape appearance figure of substrate temperature 600 DEG C of obtained alloy firms; D () is the magnetic domain shape appearance figure of substrate temperature 550 DEG C of obtained alloy firms.
Embodiment
Content of the present invention is described in detail below by embodiment; but be not used in and limit the scope of the invention; if no special instructions; all commercially, vacuum non-consumable electrode electric arc furnace used in the present invention is purchased from Shenyang tech equipment responsibility company limited for experimental drug involved in the present invention and raw material.TOL-25B excimer laser is purchased from peace low-light machine institute, and PLD-450 vacuum system is purchased from Shenyang tech equipment responsibility company limited.CSPM5500 type Scanning Probe Microscopy is purchased from basis nanometer Instrument Ltd..
Embodiment 1
Tested alloys target selects purity to be 99.99at.%-Ni, 99.95at.%-Mn, 99.99at.%-In, 99.95at.%-Co tetra-kinds of metal simple-substances, according to molfraction than getting the Ni of 50 parts, the Mn of 34 parts, In and the 4 part Co of 12 parts puts into vacuum non-consumable electrode electric arc furnace, first vacuumized by furnace chamber before melting, vacuum tightness reaches 5 × 10 -3after Pa, be filled with Ar and protect gas.In order to make material composition even, with mechanical manipulator material overturning before each melting, at least melting overturns 4 times, and adds magnetic agitation in fusion process.The ingot of diameter 50mm is obtained after melting.Ingot casting is put into circular target WEDM being cut into and being of a size of diameter 3mm × 2mm after polishing by emery wheel.Selection specification is the substrate of silica glass as film of 30mm × 30mm × 3mm.Pre-treatment is carried out to quartz glass substrate: washed through deionization by quartz glass substrate, then in acetone ultrasonic 10 ~ 15 minutes, last washes of absolute alcohol, dry.Then circular target and quartz glass substrate are put into PLD-450 vacuum system, be evacuated to 1.0 × 10 -4pa, quartz glass substrate plate temperature is 700 DEG C, and quartz glass substrate and target spacing are 4cm.With TOL-25B excimer laser as laser source Emission Lasers, controlled frequency is 4Hz, sputters 2 hours.Beat at Ni by controlling laser 50mn 34in 12co 4time on ferromagnetic shape memory alloy target controls the thickness of film.Eventually pass 850 DEG C of annealing 3h, prepare Ni 50mn 34in 12co 4ferromagnetic shape memory alloy film.
Embodiment 2
Tested alloys target selects purity to be 99.99at.%-Ni, 99.95at.%-Mn, 99.99at.%-In, 99.95at.%-Co tetra-kinds of metal simple-substances, according to molfraction than getting the Ni of 50 parts, the Mn of 34 parts, In and the 4 part Co of 12 parts puts into vacuum non-consumable electrode electric arc furnace, first vacuumized by furnace chamber before melting, vacuum tightness reaches 5 × 10 -3after Pa, be filled with Ar and protect gas.In order to make material composition even, with mechanical manipulator material overturning before each melting, at least melting overturns 4 times, and adds magnetic agitation in fusion process.The ingot of diameter 50mm is obtained after melting.Ingot casting is put into circular target WEDM being cut into and being of a size of diameter 3mm × 2mm after polishing by emery wheel.Selection specification is the substrate of silica glass as film of 30mm × 30mm × 3mm.Pre-treatment is carried out to quartz glass substrate: washed through deionization by quartz glass substrate, then in acetone ultrasonic 10 ~ 15 minutes, last washes of absolute alcohol, dry.Then circular target and quartz glass substrate are put into PLD-450 vacuum system, be evacuated to 1.0 × 10 -4pa, quartz glass substrate plate temperature is 650 DEG C, and quartz glass substrate and target spacing are 4cm.With TOL-25B excimer laser as laser source Emission Lasers, controlled frequency is 4Hz, sputters 2 hours.Beat at Ni by controlling laser 50mn 34in 12co 4time on ferromagnetic shape memory alloy target controls the thickness of film.Eventually pass 850 DEG C of annealing 3h, prepare Ni 50mn 34in 12co 4ferromagnetic shape memory alloy film.
Embodiment 3
Tested alloys target selects purity to be 99.99at.%-Ni, 99.95at.%-Mn, 99.99at.%-In, 99.95at.%-Co tetra-kinds of metal simple-substances, according to molfraction than getting the Ni of 50 parts, the Mn of 34 parts, In and the 4 part Co of 12 parts puts into vacuum non-consumable electrode electric arc furnace, first vacuumized by furnace chamber before melting, vacuum tightness reaches 5 × 10 -3after Pa, be filled with Ar and protect gas.In order to make material composition even, with mechanical manipulator material overturning before each melting, at least melting overturns 4 times, and adds magnetic agitation in fusion process.The ingot of diameter 50mm is obtained after melting.Ingot casting is put into circular target WEDM being cut into and being of a size of diameter 3mm × 2mm after polishing by emery wheel.Selection specification is the substrate of silica glass as film of 30mm × 30mm × 3mm.Pre-treatment is carried out to quartz glass substrate: washed through deionization by quartz glass substrate, then in acetone ultrasonic 10 ~ 15 minutes, last washes of absolute alcohol, dry.Then circular target and quartz glass substrate are put into PLD-450 vacuum system, be evacuated to 1.0 × 10 -4pa, quartz glass substrate plate temperature is 600 DEG C, and quartz glass substrate and target spacing are 4cm.With TOL-25B excimer laser as laser source Emission Lasers, controlled frequency is 4Hz, sputters 2 hours.Beat at Ni by controlling laser 50mn 34in 12co 4time on ferromagnetic shape memory alloy target controls the thickness of film.Eventually pass 850 DEG C of annealing 3h, prepare Ni 50mn 34in 12co 4ferromagnetic shape memory alloy film.
Embodiment 4
Tested alloys target selects purity to be 99.99at.%-Ni, 99.95at.%-Mn, 99.99at.%-In, 99.95at.%-Co tetra-kinds of metal simple-substances, according to molfraction than getting the Ni of 50 parts, the Mn of 34 parts, In and the 4 part Co of 12 parts puts into vacuum non-consumable electrode electric arc furnace, first vacuumized by furnace chamber before melting, vacuum tightness reaches 5 × 10 -3after Pa, be filled with Ar and protect gas.In order to make material composition even, with mechanical manipulator material overturning before each melting, at least melting overturns 4 times, and adds magnetic agitation in fusion process.The ingot of diameter 50mm is obtained after melting.Ingot casting is put into circular target WEDM being cut into and being of a size of diameter 3mm × 2mm after polishing by emery wheel.Selection specification is the substrate of silica glass as film of 30mm × 30mm × 3mm.Pre-treatment is carried out to quartz glass substrate: washed through deionization by quartz glass substrate, then in acetone ultrasonic 10 ~ 15 minutes, last washes of absolute alcohol, dry.Then circular target and quartz glass substrate are put into PLD-450 vacuum system, be evacuated to 1.0 × 10 -4pa, quartz glass substrate plate temperature is 550 DEG C, and quartz glass substrate and target spacing are 4cm.With TOL-25B excimer laser as laser source Emission Lasers, controlled frequency is 4Hz, sputters 2 hours.Beat at Ni by controlling laser 50mn 34in 12co 4time on ferromagnetic shape memory alloy target controls the thickness of film.Eventually pass 850 DEG C of annealing 3h, prepare Ni 50mn 34in 12co 4ferromagnetic shape memory alloy film.
By Ni prepared by embodiment 1 ~ 4 50mn 34in 12co 4alloy firm adopts CSPM5500 type Scanning Probe Microscopy to analyze its surface topography, degree of roughness and magnetic domain.Result is as shown in Fig. 1,2 and table 1.As seen from Figure 1, along with the reduction of base reservoir temperature, the crystal grain distribution of film surface is tending towards evenly, size is less gradually, and when base reservoir temperature is 600 DEG C, film surface grain-size is minimum, and median size is about 142.1nm.As can be seen from Figure 2, along with the minimizing of substrate temperature, there is huge change in line direction, farmland gradually.When base reservoir temperature is 700 DEG C, a farmland ancient piece of jade, round, flat and with a hole in its centre presents parallel distribution, and farmland line is based on a directional spreding, and colour-change is obvious, and anisotropy is strong.When base reservoir temperature is 650 DEG C, the quantity of farmland line reduces, and color also becomes dull, and farmland, local line presents both direction distribution.And when base reservoir temperature is 600 DEG C, magnetic domain becomes tiny, and based on both direction, present bending labyrinth shape.And when base reservoir temperature is 550 DEG C, magnetic domain becomes larger magnetic line distribution, and a farmland ancient piece of jade, round, flat and with a hole in its centre is all arranged in parallel.Table 1 is Ni prepared by embodiment 1 ~ 4 50mn 34in 12co 4the roughness grain-size data of alloy firm.As can be seen from Table 1, along with the reduction of base reservoir temperature, Ni 50mn 34in 12co 4the roughness of alloy firm crystal grain reduces.
Table 1 Ni 50mn 34in 12co 4the roughness of ferromagnetic shape memory alloy film and grain-size
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.

Claims (10)

1. the Ni of a high-flatness 50mn 34in 12co 4the preparation method of alloy firm, is characterized in that, comprises the following steps: get Ni, Mn, In, Co metal simple-substance according to molfraction respectively than 50:34:12:4 and be positioned over melting in vacuum non-consumable electrode electric arc furnace; 5 × 10 are evacuated to by electric arc furnace -3pa, is filled with noble gas, obtains circular target; Substrate after process and target are placed in vacuum system, are evacuated to 1.0 × 10 -4pa, substrate temperature is 500 ~ 750 DEG C, and substrate and target distance are 3 ~ 5cm; Use laser apparatus Emission Lasers again, controlled frequency is 3 ~ 4Hz, sputters 1 ~ 3 hour, the film of obtained required thickness; Eventually pass 800 ~ 900 DEG C of annealing 0.5 ~ 3h, prepare the Ni of high-flatness 50mn 34in 12co 4ferromagnetic shape memory alloy film.
2. the Ni of a kind of high-flatness according to claim 1 50mn 34in 12co 4the preparation method of alloy firm, is characterized in that, described substrate temperature is 550 ~ 700 DEG C.
3. the Ni of a kind of high-flatness according to claim 1 50mn 34in 12co 4the preparation method of alloy firm, is characterized in that, the purity of described Ni metal simple-substance is 99.99at.%.
4. the Ni of a kind of high-flatness according to claim 1 50mn 34in 12co 4the preparation method of alloy firm, is characterized in that, the purity of described Mn metal simple-substance is 99.95at.%.
5. the Ni of a kind of high-flatness according to claim 1 50mn 34in 12co 4the preparation method of alloy firm, is characterized in that, the purity of described In metal simple-substance is 99.99at.%.
6. the Ni of a kind of high-flatness according to claim 1 50mn 34in 12co 4the preparation method of alloy firm, is characterized in that, the purity of described Co metal simple-substance is 99.95at.%.
7. the Ni of a kind of high-flatness according to claim 1 50mn 34in 12co 4the preparation method of alloy firm, is characterized in that, described noble gas is argon gas.
8. the Ni of a kind of high-flatness according to claim 1 50mn 34in 12co 4the preparation method of alloy firm, is characterized in that, for ensureing the homogeneity of alloy composition in fusion process, before each melting, by sample upset at least four times and in addition magnetic stirs.
9. the Ni of a kind of high-flatness according to claim 1 50mn 34in 12co 4the preparation method of alloy firm, is characterized in that, described substrate is quartz glass substrate; The treatment process of described substrate is: silica glass glass substrate, first through deionization washing, then in acetone ultrasonic 10 ~ 15 minutes, then use washes of absolute alcohol, is dried.
10. the Ni of the high-flatness prepared by any one method described in claim 1 ~ 9 50mn 34in 12co 4alloy firm.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106544630A (en) * 2016-10-25 2017-03-29 中国计量大学 A kind of preparation method of high saturation and magnetic intensity manganese bismuth permanent magnets films

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
A. SOKOLOV，ET AL.: "Evidence of Martensitic Phase Transitions in Magnetic Ni-Mn-In Thin Films", 《APPLIED PHYSICS LETTERS》 *
CHAO JING,ET AL.: "Epitaxial growth of single-crystalline Ni46Co4Mn37In13 thin film and investigation of its magnetoresistance", 《PROGRESS IN NATURAL SCIENCE MATERIALS INTERNATIONAL》 *
Y.FENG,ET AL.: "Microstructure,phase transitions and mechnical properties of Ni50Mn34In16-yCoy alloys", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106544630A (en) * 2016-10-25 2017-03-29 中国计量大学 A kind of preparation method of high saturation and magnetic intensity manganese bismuth permanent magnets films
CN106544630B (en) * 2016-10-25 2019-04-09 中国计量大学 A kind of preparation method of high saturation and magnetic intensity manganese bismuth permanent magnets films

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