CN105154802B - A kind of method separating out the second phase in effective suppression Ni-Mn-Sn-Fe alloy - Google Patents
A kind of method separating out the second phase in effective suppression Ni-Mn-Sn-Fe alloy Download PDFInfo
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Abstract
A kind of method separating out the second phase in effective suppression Ni Mn Sn Fe alloy, the present invention relates to the preparation method of a kind of Ni Mn Sn Fe metallic fiber, and it is in order to solve the problem that Ni Mn Sn Fe alloy easily separates out the second phase in conventional chilling process of setting.Suppression separates out the method for the second phase: one, alloy cast ingot carries out heat treatment；Two, the alloy cast ingot after cleaning is put in aluminium oxide hollow cylinder, is then placed in electromagnetic induction heating coil, inserts ceramic cylinder below alloy cylinder ingot casting；Three, evacuation, logical argon, the certain argon pressure in last maintenance work room repeatedly；Four, make metallic roll wheel rotate, connect induction heating power；Five, after alloy pool contacts with metal running roller, the molten alloy in molten bath is spun into Ni Mn Sn Fe alloy fiber.The present invention uses melt pull technique, it is ensured that the alloying element after fusing does not separate out the second phase in process of setting.
Description
Technical field
The present invention relates to the preparation method of a kind of Ni-Mn-Sn-Fe metallic fiber.
Background technology
Conventional compression air cooling technology has power consumption height, pollutes big, and inefficient shortcoming needs development other types badly
Refrigeration Technique or non-harmful cold-producing medium.Magnetic freezes as a kind of novel green refrigeration technology, is expected to become following refrigeration
Dominating of technology.Ni-Mn-Sn-Fe alloy has at the anti-magnetothermal effect at martensitic phase transformation and austenite Curie temperature simultaneously
Positive magnetothermal effect, extensive concern and the research of material educational circles as New Magnetic Field Controlled refrigerating material, can be caused.
But along with the increase of Fe content, Ni-Mn-Sn-Fe alloy can separate out the second phase, but the second relative magnetothermal effect does not has
There is contribution, but can drop the low-alloyed intensity of magnetization, it is therefore desirable to research and develop new method and suppress the precipitation of the second phase.
Summary of the invention
The present invention is directed to Ni-Mn-Sn-Fe alloy in conventional chilling process of setting, easily separate out the problem of the second phase, and provide
A kind of method separating out the second phase in effective suppression Ni-Mn-Sn-Fe alloy.
The present invention effectively suppresses the method separating out the second phase in Ni-Mn-Sn-Fe alloy to realize according to the following steps:
One, Ni-Mn-Sn-Fe alloy cylindrical ingot is sealed in quartz glass tube, use after mechanical pump evacuation
It is incubated 24～72h at a temperature of 900～950 DEG C, cools to room temperature with the furnace, obtain the ingot casting after heat treatment, use electric spark
Ingot casting after heat treatment is cut into multistage small column shaped cast ingot by wire cutting machine, put into after surface polishing light water is carried out ultrasonic
Clean, dry the alloy cylinder ingot casting after being cleaned；
Two, the alloy cylinder ingot casting after cleaning is put in aluminium oxide hollow cylinder, is then placed in melt pull equipment operating room
In electromagnetic induction heating coil in, the axis of aluminium oxide hollow cylinder is perpendicular with horizontal plane, and adjusts aluminium oxide open circles
The end face of post and load coil upper edge are in same level, after fixing aluminium oxide hollow cylinder, hollow at aluminium oxide
Aluminium oxide ceramics cylinder is inserted below alloy cylinder ingot casting, it is ensured that the lower surface of the aluminium oxide ceramics cylinder of insertion and line in cylinder
Property motor feed bar contacts, and completes the fixing assembling of aluminium oxide hollow cylinder；
Three, melt pull equipment operating room is evacuated to 2 × 10-3～5 × 10-3Pa, is passed through high-purity argon gas, repeats to take out
Vacuum, it is passed through argon twice, is the most again evacuated to 0.5 × 10-3～1 × 10-3Pa, is finally filled with high-purity argon gas until work
Make room argon pressure reach and maintain 0.02～0.05Pa, complete the pressure regulation of operating room；
Four, open metallic roll wheel and rotate control motor, connect induction heating power, make the alloy pool temperature in alumina cylinders
Degree is stable at 1300～1550 DEG C, obtains the alloy pool of pre-pull；
Five, open linear stepping motor, use the feed speed of 20～50 μm/s to make the alloy pool of pre-pull close to rotating
Metal running roller, after alloy pool contacts with metal running roller, the molten alloy in molten bath is spun into fiber, and is brought away from molten bath,
Alloy in molten bath stops linear stepping motor after ruing out of, and induction heating power is reduced to zero, finally stops metallic roll round
Dynamic, obtain Ni-Mn-Sn-Fe metallic fiber.
The Ni-Mn-Sn-Fe metallic fiber of a diameter of 30～150 microns is applied as magnetic refrigerating material by the present invention.
The present invention uses melt pull technique, prepares the Ni-Mn-Sn-Fe metallic fiber of a diameter of 30～150 microns, borrows
The feature of metal bath rapid solidification in body pull technique of fluxing, it is ensured that the alloying element after fusing will not be analysed in process of setting
Go out to form the second phase, prepared the filament of diameter tens to up to a hundred microns.The fiber obtained has the biggest specific surface area,
During as magnetic refrigeration device, heat conduction efficiency has the features such as heat conduction is fast, cycle rate is fast.Additionally, due to melt pull
In technique, metal freezing speed is big, it is thus achieved that fiber crystal grain is tiny, the complete solid solution of alloying element, and crystal grain has orientation
The feature of distribution, this is to adjust the performance of fiber by modes such as subsequent heat treatment to provide possibility.The present invention is in preparation process
In solve Ni-Mn-Sn-Fe alloy block and easily produce pore, the impact of defect such as be mingled with, and when effectively controlling fusing
Sn and Mn element evaporation causes the problem that alloying component changes.The invention discloses a kind of Ni-Mn-Sn-Fe alloy block
Heat treatment, melt pull process, be prepared for the Ni-Mn-Sn-Fe micrometer fibers of different-diameter and pattern, it is thus achieved that micro-
There is not the second phase in rice fiber.
Accompanying drawing explanation
Fig. 1 is the low power back scattering scanning electron microscope (SEM) photograph of Ni-Mn-Sn-Fe alloy block；
Fig. 2 is the high power back scattering scanning electron microscope (SEM) photograph of Ni-Mn-Sn-Fe alloy block；
Fig. 3 is the photomacrograph figure of the Ni-Mn-Sn-Fe metallic fiber that embodiment one obtains；
Fig. 4 is the cross section SEM figure of the Ni-Mn-Sn-Fe metallic fiber that embodiment one obtains；
Fig. 5 is scanning electron microscope (SEM) figure of the Ni-Mn-Sn-Fe metallic fiber outer surface that embodiment one obtains；
Fig. 6 is the cross section SEM figure of the Ni-Mn-Sn-Fe metallic fiber that embodiment two obtains；
Fig. 7 is scanning electron microscope (SEM) figure of the Ni-Mn-Sn-Fe metallic fiber outer surface that embodiment two obtains；
Fig. 8 is the scanning electron microscope secondary electron scanning figure after the Ni-Mn-Sn-Fe metallic fiber polishing that embodiment one obtains；
Fig. 9 be Fig. 8 same position polishing after scanning electron microscope backscattered electron scanning figure；
Figure 10 is Ni-Mn-Sn-Fe alloy block (bulk) and Ni-Mn-Sn-Fe metallic fiber (microwire) X penetrates
Ray diffraction diagram is composed, and wherein 1 represents Ni-Mn-Sn-Fe alloy block, and 2 represent Ni-Mn-Sn-Fe metallic fiber, represents
γ phase, represents austenite phase.
Detailed description of the invention
Detailed description of the invention one: present embodiment effectively suppresses Ni-Mn-Sn-Fe alloy to separate out the method for the second phase by following step
Rapid enforcement:
One, Ni-Mn-Sn-Fe alloy cylindrical ingot is sealed in quartz glass tube, use after mechanical pump evacuation
It is incubated 24～72h at a temperature of 900～950 DEG C, cools to room temperature with the furnace, obtain the ingot casting after heat treatment, use electric spark
Ingot casting after heat treatment is cut into multistage small column shaped cast ingot by wire cutting machine, put into after surface polishing light water is carried out ultrasonic
Clean, dry the alloy cylinder ingot casting after being cleaned；
Two, the alloy cylinder ingot casting after cleaning is put in aluminium oxide hollow cylinder, is then placed in melt pull equipment operating room
In electromagnetic induction heating coil in, the axis of aluminium oxide hollow cylinder is perpendicular with horizontal plane, and adjusts aluminium oxide open circles
The end face of post and load coil upper edge are in same level, after fixing aluminium oxide hollow cylinder, hollow at aluminium oxide
Aluminium oxide ceramics cylinder is inserted below alloy cylinder ingot casting, it is ensured that the lower surface of the aluminium oxide ceramics cylinder of insertion and line in cylinder
Property motor feed bar contacts, and completes the fixing assembling of aluminium oxide hollow cylinder；
Three, melt pull equipment operating room is evacuated to 2 × 10-3～5 × 10-3Pa, is passed through high-purity argon gas, repeats to take out
Vacuum, it is passed through argon twice, is the most again evacuated to 0.5 × 10-3～1 × 10-3Pa, is finally filled with high-purity argon gas until work
Make room argon pressure reach and maintain 0.02～0.05Pa, complete the pressure regulation of operating room；
Four, open metallic roll wheel and rotate control motor, connect induction heating power, make the alloy pool temperature in alumina cylinders
Degree is stable at 1300～1550 DEG C, obtains the alloy pool of pre-pull；
Five, open linear stepping motor, use the feed speed of 20～50 μm/s to make the alloy pool of pre-pull close to rotating
Metal running roller, after alloy pool contacts with metal running roller, the molten alloy in molten bath is spun into fiber, and is brought away from molten bath,
Alloy in molten bath stops linear stepping motor after ruing out of, and induction heating power is reduced to zero, finally stops metallic roll round
Dynamic, obtain Ni-Mn-Sn-Fe metallic fiber.
Molten alloy is spaced with feed bar by present embodiment step 2 by aluminium oxide ceramics cylinder.And step 3 is taken out repeatedly
It is that the air concentration in studio environment is reduced by the method for argon-dilution that vacuum leads to the effect of argon, and then reaches complete
Remove air, avoid the metal in molten bath and the fiber of preparation at high temperature to aoxidize, 0.02～0.05Pa be finally passed through
Argon can maintain certain atmosphere pressures in equipment operating room, reduces element (Mn and Sn element) after metal molten
Volatilization.
Present embodiment uses melt pull method to prepare micrometer fibers, it is thus achieved that do not contain the fiber of the second phase.In preparation process
In solve Ni-Mn-Sn-Fe alloy block and easily produce pore, the impact of defect such as be mingled with, and when effectively controlling fusing
Sn and Mn element evaporation causes the problem that alloying component changes.Propose at first to alloy block in a vacuum uniform heat-transformation
Reason reduces defect and is mingled with, and uses melt pull method to prepare the Ni-Mn-Sn-Fe of different size and pattern in argon gas atmosphere
Micrometer fibers.
Detailed description of the invention two: present embodiment step one unlike detailed description of the invention one uses mechanical pump to be evacuated to
Air pressure is 10-2～10-3Pa.Other step and parameter are identical with detailed description of the invention one.
Detailed description of the invention three: the medium and small cylindrical ingot of present embodiment step one unlike detailed description of the invention one or two
Height be 30～40mm, a diameter of 10～15mm.Other step and parameter are identical with detailed description of the invention one or two.
Detailed description of the invention four: the drying described in present embodiment step one unlike one of detailed description of the invention one to three
Carry out at 150 DEG C.Other step and parameter are identical with one of detailed description of the invention one to three.
Detailed description of the invention five: high-purity described in present embodiment step 3 unlike one of detailed description of the invention one to four
The purity of argon is 99.9%.Other step and parameter are identical with one of detailed description of the invention one to four.
Detailed description of the invention six: present embodiment is step 3 evacuation again unlike one of detailed description of the invention one to five
To 0.5 × 10-3Pa, is finally filled with high-purity argon gas until operating room's argon pressure reaches and maintains 0.02Pa.Other step and
Parameter is identical with one of detailed description of the invention one to five.
Detailed description of the invention seven: the metal described in present embodiment step 4 unlike one of detailed description of the invention one to six
A diameter of 120mm of running roller, controlling rotating speed is 1000～1700r/min.Other step and parameter and detailed description of the invention one
Identical to one of six.
Detailed description of the invention eight: present embodiment step 4 unlike one of detailed description of the invention one to seven is connected sensing and added
Thermoelectric generator, heats 15～20s every 2kw, and gradually regulation heating power is to 13～20kw, finally makes in alumina cylinders
Alloy pool temperature stabilization at 1300～1550 DEG C.Other step and parameter are identical with one of detailed description of the invention one to seven.
Present embodiment stops 15～20s under different capacity, progressively regulates by observing alloy whether to reach molten state
Power, prevents from causing alloy not melt because power is too low, the problem that the volatilization of power too high alloying element is serious, thus reduces
The volatilization loss of alloying element after fusing.
Detailed description of the invention nine: present embodiment step 5 unlike one of detailed description of the invention one to eight obtains
A diameter of 30～150 microns of Ni-Mn-Sn-Fe metallic fiber.Other step and parameter and detailed description of the invention one to eight it
One is identical.
Embodiment one: the present embodiment effectively suppresses the method separating out the second phase in Ni-Mn-Sn-Fe alloy real according to the following steps
Existing:
One, Ni-Mn-Sn-Fe alloy cylindrical ingot is sealed in quartz glass tube, uses mechanical pump to be evacuated down to air pressure
To 10-3At a temperature of 950 DEG C, it is incubated 48h after Pa, cools to room temperature with the furnace, obtain the ingot casting after heat treatment, use electricity
Ingot casting after heat treatment is cut into multistage small column shaped cast ingot (height is 36mm, a diameter of 10mm) by spark line cutting machine,
Put into after surface polishing light and water carries out ultrasonic cleaning 3 times, dry 120 minutes at 150 DEG C, the conjunction after being cleaned
Gold cylinder ingot casting；
Two, aluminium oxide hollow cylinder put into by the alloy cylinder ingot casting after cleaning, and (internal diameter of aluminium oxide hollow cylinder is cast than cylinder
The big 2mm of ingot diameter, wall thickness are 3mm) in, it is then placed in the electromagnetic induction heating line in melt pull equipment operating room
In circle, the axis of aluminium oxide hollow cylinder is perpendicular with horizontal plane, and adjusts end face and the sensing heating of aluminium oxide hollow cylinder
Coil upper edge is in same level, after fixing aluminium oxide hollow cylinder, and alloy cylinder ingot casting in aluminium oxide hollow cylinder
Insert aluminium oxide ceramics cylinder below, it is ensured that the lower surface of the aluminium oxide ceramics cylinder of insertion and linear stepping motor feed bar phase
Contact, completes the fixing assembling of aluminium oxide hollow cylinder；
Three, melt pull equipment operating room is evacuated to 2 × 10-3Pa, is passed through the argon that purity is 99.9%, repeats
Evacuation, it is passed through argon twice, is the most again evacuated to 0.5 × 10-3Pa, is finally filled with the argon that purity is 99.9% straight
Reach to operating room's argon pressure and maintain 0.02Pa, completing the pressure regulation of operating room；
Four, opening metal (copper) running roller and rotate control motor, a diameter of 120mm of copper running roller, rotating speed is 1700r/min,
Connect induction heating power, heat 15s every 2kw, finally make the alloy pool temperature stabilization in alumina cylinders exist
1400 DEG C, obtain the alloy pool of pre-pull；
Five, opening linear stepping motor, the alloy cylinder ingot casting molten bath after first making fusing with the speed of 200 μm/s reaches
At the metal running roller 2mm that distance rotates, the feed speed of 30 μm/s is used to make the alloy pool of pre-pull close to rotation
Metal running roller, after alloy pool contacts with metal running roller, the molten alloy in molten bath is spun into fiber, and is brought away from molten bath,
Alloy in molten bath stops linear stepping motor after ruing out of, and induction heating power is reduced to zero, finally stops metallic roll round
Dynamic, obtain Ni-Mn-Sn-Fe metallic fiber.
Fig. 1 and Fig. 2 is the back scattering scanning electron microscope (SEM) photograph of Ni-Mn-Sn-Fe alloy block, and in figure, darker regions is the second phase,
Therefrom it appeared that there is obvious Second Phase Precipitation, crystals has a small amount of distribution, and remaining is mainly distributed on grain boundaries.
Fig. 3 is the photomacrograph of the Ni-Mn-Sn-Fe metallic fiber that the present embodiment one obtains, it appeared that fiber system from figure
Standby amount is big, and seriality is good, and length is up to 15 cm.Fig. 4 and Fig. 5 is that the metallic fiber of Ni-Mn-Sn-Fe is transversal
Scanning electron microscope (SEM) pattern of face and outer surface.The horizontal stroke of fiber from Fig. 4 it is found that during feed speed 30 μm/s
Cross section is not the circle of rule, but is made up of the circular arc portion of the planar section in left side with right side.Planar section is by copper roller
During wheel pull liquation, liquation contacts with copper wheel, partially solidified formed, and circular arc portion be by pull after fiber
Formed freely solidifying.Showing in Fig. 5 that the free coagulation surface of fiber is made up of cellular crystal, cellular crystal crystal grain diameter is several
Hundred nanometers, illustrate to experienced by process of setting rapid solidification.
Fig. 8 and Fig. 9 be the Ni-Mn-Sn-Fe fiber of As-deposited state after the sanding and polishing of surface, at scanning electron microscope secondary electron and
Scanned photograph under back scattering state, illustrates that melt pull method inhibits the precipitation of Ni-Mn-Sn-Fe the second phase well.Figure
10 is X ray diffracting spectrum, demonstrates that Ni-Mn-Sn-Fe alloy block occurs obvious second phase diffraction maximum before getting rid of silk,
And fiber prepared by melt pull method does not has the diffraction maximum of the second phase, the most single austenite phase.Fig. 8 and Fig. 9 illustrates melt
Pull method inhibits the precipitation of the second phase in alloy.
Embodiment two: the present embodiment step 5 unlike embodiment one uses the feed speed of 50 μm/s to make pre-pull
Alloy pool is close to the metal running roller rotated.
Ni-Mn-Sn-Fe metal fibers cross section and scanning electron microscope (SEM) pattern of outer surface that the present embodiment obtains such as are schemed
Shown in 6 and Fig. 7, when feed speed is 50 μm/s, the cross section of fiber is Near Banded, and Fig. 7 shows that fiber freely solidifies
Surface is made up of cellular crystal equally, and crystallite dimension is more bigger than Fig. 5.
Claims (8)
1. the method separating out the second phase in an effective suppression Ni-Mn-Sn-Fe alloy, it is characterised in that be to follow these steps to reality
Existing:
One, Ni-Mn-Sn-Fe alloy cylindrical ingot is sealed in quartz glass tube, use after mechanical pump evacuation
It is incubated 24～72h at a temperature of 900～950 DEG C, cools to room temperature with the furnace, obtain the ingot casting after heat treatment, use electric spark
Ingot casting after heat treatment is cut into multistage small column shaped cast ingot by wire cutting machine, put into after surface polishing light water is carried out ultrasonic
Clean, dry the alloy cylinder ingot casting after being cleaned；
Two, the alloy cylinder ingot casting after cleaning is put in aluminium oxide hollow cylinder, is then placed in melt pull equipment operating room
In electromagnetic induction heating coil in, the axis of aluminium oxide hollow cylinder is perpendicular with horizontal plane, and adjusts aluminium oxide open circles
The end face of post and load coil upper edge are in same level, after fixing aluminium oxide hollow cylinder, hollow at aluminium oxide
Aluminium oxide ceramics cylinder is inserted below alloy cylinder ingot casting, it is ensured that the lower surface of the aluminium oxide ceramics cylinder of insertion and line in cylinder
Property motor feed bar contacts, and completes the fixing assembling of aluminium oxide hollow cylinder；
Three, melt pull equipment operating room is evacuated to 2 × 10-3～5 × 10-3Pa, is passed through high-purity argon gas, repeats to take out very
Empty, be passed through argon twice, be the most again evacuated to 0.5 × 10-3～1 × 10-3Pa, is finally filled with high-purity argon gas until operating room
Ar pressure reaches and maintains 0.02～0.05Pa, completes the pressure regulation of operating room；
Four, open metallic roll wheel and rotate control motor, connect induction heating power, make the alloy pool temperature in alumina cylinders
Degree is stable at 1300～1550 DEG C, obtains the alloy pool of pre-pull；
Five, open linear stepping motor, use the feed speed of 20～50 μm/s to make the alloy pool of pre-pull close to rotating
Metal running roller, after alloy pool contacts with metal running roller, the molten alloy in molten bath is spun into fiber, and is brought away from molten bath,
Alloy in molten bath stops linear stepping motor after ruing out of, and induction heating power is reduced to zero, finally stops metallic roll round
Dynamic, obtain Ni-Mn-Sn-Fe metallic fiber；
Wherein a diameter of 120mm of the metal running roller described in step 4, controlling rotating speed is 1000～1700r/min.
The method separating out the second phase in a kind of effective suppression Ni-Mn-Sn-Fe alloy the most according to claim 1, it is special
Levy that to be that step one uses mechanical pump to be evacuated to air pressure pressure be 10-2～10-3Pa。
The method separating out the second phase in a kind of effective suppression Ni-Mn-Sn-Fe alloy the most according to claim 1, it is special
Levy and be that the height of the medium and small cylindrical ingot of step one is 30～40mm, a diameter of 10～15mm.
The method separating out the second phase in a kind of effective suppression Ni-Mn-Sn-Fe alloy the most according to claim 1, it is special
Levy and be that the drying described in step one is carried out at 150 DEG C.
The method separating out the second phase in a kind of effective suppression Ni-Mn-Sn-Fe alloy the most according to claim 1, it is special
Levy and be that the purity of the high-purity argon gas described in step 3 is 99.9%.
The method separating out the second phase in a kind of effective suppression Ni-Mn-Sn-Fe alloy the most according to claim 1, it is special
Levy and be that step 3 is evacuated to 0.5 × 10 again-3Pa, is finally filled with high-purity argon gas until operating room's ar pressure reaches and ties up
Hold at 0.02Pa.
The method separating out the second phase in a kind of effective suppression Ni-Mn-Sn-Fe alloy the most according to claim 1, it is special
Levying and be that step 4 connects induction heating power, heat 15～20s every 2kW, gradually regulation heating power is to 13～20kW,
Finally make the alloy pool temperature stabilization in alumina cylinders at 1300～1550 DEG C.
The method separating out the second phase in a kind of effective suppression Ni-Mn-Sn-Fe alloy the most according to claim 1, it is special
Levy the Ni-Mn-Sn-Fe metallic fiber being that step 5 obtains a diameter of 30～150 microns.
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