CN105154802A - Method for effectively inhibiting second phase from precipitation in Ni-Mn-Sn-Fe alloy - Google Patents
Method for effectively inhibiting second phase from precipitation in Ni-Mn-Sn-Fe alloy Download PDFInfo
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- CN105154802A CN105154802A CN201510677404.9A CN201510677404A CN105154802A CN 105154802 A CN105154802 A CN 105154802A CN 201510677404 A CN201510677404 A CN 201510677404A CN 105154802 A CN105154802 A CN 105154802A
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Abstract
The invention provides a method for effectively inhibiting a second phase from precipitation in an Ni-Mn-Sn-Fe alloy, which relates to a preparation method of Ni-Mn-Sn-Fe metal fibers and aims to solve the problem that the Ni-Mn-Sn-Fe alloy can easily precipitate the second phase in the conventional cooling solidification process. The method comprises the following steps: 1. carrying out heat treatment on an alloy cast ingot; 2. putting the cleaned alloy cast ingot into an aluminum oxide hollow cylinder, putting in an electromagnetic induction heating coil, and inserting a ceramic cylinder under the alloy cylinder cast ingot; 3. repeating the vacuumizing-argon introduction process, and finally maintaining the working chamber under certain argon pressure; 4. rotating a metal roller, and switching on an induction heating power source; 5. contacting an alloy melting bath with the metal roller so that the molten alloy in the melting bath is spun into the Ni-Mn-Sn-Fe alloy fibers. The melt extraction technique is adopted to prevent the molten alloy elements from precipitating the second phase in the solidification process.
Description
Technical field
The present invention relates to a kind of preparation method of Ni-Mn-Sn-Fe steel fiber.
Background technology
It is high that conventional compression air cooling technology has power consumption, pollutes large, inefficient shortcoming, needs the Refrigeration Technique or non-harmful refrigeration agent of developing other types badly.Magnetic refrigeration, as a kind of novel green refrigeration technology, is expected to become the leading of following Refrigeration Technique.Ni-Mn-Sn-Fe alloy has the anti-magnetothermal effect at martensitic transformation place and the positive magnetothermal effect at austenite Curie temperature place simultaneously, can be used as New Magnetic Field Controlled refrigerating material, causes extensive concern and the research of material educational circles.
But along with the increase of Fe content, Ni-Mn-Sn-Fe alloy can separate out second-phase, but second-phase is not contributed magnetothermal effect, but can fall the low-alloyed specific magnetising moment, therefore need the precipitation of researching and developing new method suppression second-phase.
Summary of the invention
The present invention is directed to the problem that second-phase easily separated out by Ni-Mn-Sn-Fe alloy in conventional chilling process of setting, and a kind of method separating out second-phase in effective suppression Ni-Mn-Sn-Fe alloy is provided.
The present invention effectively suppresses the method separating out 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, at the temperature of 900 ~ 950 DEG C, 24 ~ 72h is incubated after adopting mechanical pump to vacuumize, cool to room temperature with the furnace, obtain the ingot casting after thermal treatment, adopt WEDM that the ingot casting after thermal treatment is cut into multistage small cylindrical ingot casting, put into water after surface finish light and carry out ultrasonic cleaning, dry and obtain the alloy cylinder ingot casting after cleaning;
Two, alloy cylinder ingot casting after cleaning is put into aluminum oxide hollow cylinder, then the electromagnetic induction heating coil of melt pull equipment work room is put into, axis and the horizontal plane of aluminum oxide hollow cylinder are perpendicular, and adjust the end face of aluminum oxide hollow cylinder and load coil upper edge in same level, after fixing aluminum oxide hollow cylinder, alumina-ceramic cylinder is inserted below alloy cylinder ingot casting in aluminum oxide hollow cylinder, ensure that the lower surface of the alumina-ceramic cylinder inserted contacts with linear stepping motor feed shaft, complete the fixing assembling of aluminum oxide hollow cylinder,
Three, melt pull equipment work room is evacuated to 2 × 10
-3~ 5 × 10
-3pa, passes into high-purity argon gas, repeats to vacuumize, pass into argon gas twice, and then is evacuated to 0.5 × 10
-3~ 1 × 10
-3pa, is finally filled with high-purity argon gas until working spaces's argon pressure reaches and maintains 0.02 ~ 0.05Pa, and the pressure of room of finishing the work regulates;
Four, open metal running roller to rotate and control motor, connect induction heating power, make alloy pool temperature-stable in alumina cylinders at 1300 ~ 1550 DEG C, obtain the alloy pool of pre-pull;
Five, linear stepping motor is opened, the speed of feed of 20 ~ 50 μm/s is adopted to make the alloy pool of pre-pull close to the metal running roller rotated, after alloy pool contacts with metal running roller, molten alloy in molten bath is spun into fiber, and being taken away molten bath, the alloy in molten bath runs out of rear stopping linear stepping motor, and induction heating power is reduced to zero, finally stop metal running roller to rotate, obtain Ni-Mn-Sn-Fe steel fiber.
Diameter is that the Ni-Mn-Sn-Fe steel fiber application of 30 ~ 150 microns is as magnetic refrigerating material by the present invention.
The present invention adopts melt pull technique, prepare the Ni-Mn-Sn-Fe steel fiber that diameter is 30 ~ 150 microns, by the feature of metal melt rapid solidification in melt pull technique, ensure that the alloying element after fusing can not separate out formation second-phase in process of setting, prepared the filament of diameter tens to up to a hundred microns.The fiber obtained has very large specific surface area, during as magnetic refrigeration device, heat conduction efficiency has the features such as heat conduction is fast, cycle rate is fast.In addition because metal freezing speed in melt pull technique is large, the fiber crystal grain of acquisition is tiny, the complete solid solution of alloying element, and crystal grain has the feature of orientation distribution, and this is that the performance adjusting fiber by modes such as subsequent heat treatment provides possibility.The present invention solves Ni-Mn-Sn-Fe alloy block and easily produces pore, the impact of defect such as to be mingled with in preparation process, and the problem that when effectively controlling fusing, Sn and Mn element evaporation cause alloying constituent to change.The invention discloses the thermal treatment of a kind of Ni-Mn-Sn-Fe alloy block, melt pull processing method, prepared the Ni-Mn-Sn-Fe micrometer fibers of different diameter and pattern, in the micrometer fibers of acquisition, there is not second-phase.
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 steel fiber that embodiment one obtains;
Fig. 4 is that the cross section SEM of the Ni-Mn-Sn-Fe steel fiber that embodiment one obtains schemes;
Fig. 5 is scanning electron microscope (SEM) figure of the Ni-Mn-Sn-Fe steel fiber outside surface that embodiment one obtains;
Fig. 6 is that the cross section SEM of the Ni-Mn-Sn-Fe steel fiber that embodiment two obtains schemes;
Fig. 7 is scanning electron microscope (SEM) figure of the Ni-Mn-Sn-Fe steel fiber outside surface that embodiment two obtains;
Fig. 8 is the scanning electron microscope secondary electron scintigram after the Ni-Mn-Sn-Fe steel fiber polishing that obtains of embodiment one;
Fig. 9 is scanning electron microscope backscattered electron scintigram after the polishing of Fig. 8 same position;
Figure 10 is Ni-Mn-Sn-Fe alloy block (bulk) and Ni-Mn-Sn-Fe steel fiber (microwire) X ray diffracting spectrum, wherein 1 represent Ni-Mn-Sn-Fe alloy block, 2 represent Ni-Mn-Sn-Fe steel fiber, and ★ represents γ phase, and ▼ represents austenite phase.
Embodiment
Embodiment one: the method that present embodiment effectively suppresses Ni-Mn-Sn-Fe alloy to separate out second-phase is implemented according to the following steps:
One, Ni-Mn-Sn-Fe alloy cylindrical ingot is sealed in quartz glass tube, at the temperature of 900 ~ 950 DEG C, 24 ~ 72h is incubated after adopting mechanical pump to vacuumize, cool to room temperature with the furnace, obtain the ingot casting after thermal treatment, adopt WEDM that the ingot casting after thermal treatment is cut into multistage small cylindrical ingot casting, put into water after surface finish light and carry out ultrasonic cleaning, dry and obtain the alloy cylinder ingot casting after cleaning;
Two, alloy cylinder ingot casting after cleaning is put into aluminum oxide hollow cylinder, then the electromagnetic induction heating coil of melt pull equipment work room is put into, axis and the horizontal plane of aluminum oxide hollow cylinder are perpendicular, and adjust the end face of aluminum oxide hollow cylinder and load coil upper edge in same level, after fixing aluminum oxide hollow cylinder, alumina-ceramic cylinder is inserted below alloy cylinder ingot casting in aluminum oxide hollow cylinder, ensure that the lower surface of the alumina-ceramic cylinder inserted contacts with linear stepping motor feed shaft, complete the fixing assembling of aluminum oxide hollow cylinder,
Three, melt pull equipment work room is evacuated to 2 × 10
-3~ 5 × 10
-3pa, passes into high-purity argon gas, repeats to vacuumize, pass into argon gas twice, and then is evacuated to 0.5 × 10
-3~ 1 × 10
-3pa, is finally filled with high-purity argon gas until working spaces's argon pressure reaches and maintains 0.02 ~ 0.05Pa, and the pressure of room of finishing the work regulates;
Four, open metal running roller to rotate and control motor, connect induction heating power, make alloy pool temperature-stable in alumina cylinders at 1300 ~ 1550 DEG C, obtain the alloy pool of pre-pull;
Five, linear stepping motor is opened, the speed of feed of 20 ~ 50 μm/s is adopted to make the alloy pool of pre-pull close to the metal running roller rotated, after alloy pool contacts with metal running roller, molten alloy in molten bath is spun into fiber, and being taken away molten bath, the alloy in molten bath runs out of rear stopping linear stepping motor, and induction heating power is reduced to zero, finally stop metal running roller to rotate, obtain Ni-Mn-Sn-Fe steel fiber.
Molten alloy and feed shaft are separated by alumina-ceramic cylinder by present embodiment step 2.And the effect that step 3 vacuumizes logical argon gas is repeatedly that the method for the air concentration in studio environment by argon-dilution is reduced, and then reach and remove air completely, avoid the fiber of the metal in molten bath and preparation to be at high temperature oxidized, 0.02 ~ 0.05Pa the argon gas finally passed into can at the certain atmosphere pressures of the indoor maintenance of equipment work, reduces the volatilization of element (Mn and Sn element) after melting of metal.
Present embodiment adopts melt pull method to prepare micrometer fibers, obtains the fiber not containing second-phase.In preparation process, solve Ni-Mn-Sn-Fe alloy block easily produce pore, the impact of defect such as to be mingled with, and the problem that when effectively controlling fusing, Sn and Mn element evaporation cause alloying constituent to change.Propose first alloy block in a vacuum homogenizing thermal treatment reduce defect and being mingled with, adopt melt pull method in argon gas atmosphere, prepare the Ni-Mn-Sn-Fe micrometer fibers of different size and pattern.
Embodiment two: it is 10 that present embodiment and embodiment one adopt mechanical pump to be evacuated to air pressure unlike step one
-2~ 10
-3pa.Other step and parameter identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two are 30 ~ 40mm unlike the height of the medium and small cylindrical ingot of step one, and diameter is 10 ~ 15mm.Other step and parameter identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three are carried out at 150 DEG C unlike the oven dry described in step one.Other step and parameter identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four are 99.9% unlike the purity of the high-purity argon gas described in step 3.Other step and parameter identical with one of embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five are evacuated to 0.5 × 10 again unlike step 3
-3pa, is finally filled with high-purity argon gas until working spaces's argon pressure reaches and maintains 0.02Pa.Other step and parameter identical with one of embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six are 120mm unlike the diameter of the metal running roller described in step 4, and control rotating speed is 1000 ~ 1700r/min.Other step and parameter identical with one of embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven connect induction heating power unlike step 4,15 ~ 20s is heated every 2kw, regulate heating power to 13 ~ 20kw gradually, finally make alloy pool temperature-stable in alumina cylinders at 1300 ~ 1550 DEG C.Other step and parameter identical with one of embodiment one to seven.
Present embodiment stops 15 ~ 20s under different capacity, melted state and progressively regulating power whether is reached by observing alloy, prevent from causing alloy not melt because power is too low, the too high alloying element of power volatilizees serious problem, thus the volatilization loss of alloying element after reducing fusing.
Embodiment nine: the diameter of the Ni-Mn-Sn-Fe steel fiber that one of present embodiment and embodiment one to eight obtain unlike step 5 is 30 ~ 150 microns.Other step and parameter identical with one of embodiment one to eight.
Embodiment one: the present embodiment effectively suppresses the method separating out 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, adopts mechanical pump to be evacuated down to air pressure to 10
-3at the temperature of 950 DEG C, 48h is incubated after Pa, cool to room temperature with the furnace, obtain the ingot casting after thermal treatment, adopting WEDM the ingot casting after thermal treatment to be cut into multistage small cylindrical ingot casting (is highly 36mm, diameter is 10mm), put into water after surface finish light and carry out ultrasonic cleaning 3 times, dry 120 minutes at 150 DEG C, obtain the alloy cylinder ingot casting after cleaning;
Two, alloy cylinder ingot casting after cleaning is put into aluminum oxide hollow cylinder (the internal diameter 2mm larger than cylinder ingot diameters of aluminum oxide hollow cylinder, wall thickness is 3mm) in, then the electromagnetic induction heating coil of melt pull equipment work room is put into, axis and the horizontal plane of aluminum oxide hollow cylinder are perpendicular, and adjust the end face of aluminum oxide hollow cylinder and load coil upper edge in same level, after fixing aluminum oxide hollow cylinder, alumina-ceramic cylinder is inserted below alloy cylinder ingot casting in aluminum oxide hollow cylinder, ensure that the lower surface of the alumina-ceramic cylinder inserted contacts with linear stepping motor feed shaft, complete the fixing assembling of aluminum oxide hollow cylinder,
Three, melt pull equipment work room is evacuated to 2 × 10
-3pa, passes into the argon gas that purity is 99.9%, repeats to vacuumize, pass into argon gas twice, and then is evacuated to 0.5 × 10
-3pa, be finally filled with purity be the argon gas of 99.9% until working spaces's argon pressure reaches and maintains 0.02Pa, the pressure of room of finishing the work regulates;
Four, open metal (copper) running roller and rotate control motor, the diameter of copper running roller is 120mm, and rotating speed is 1700r/min, connect induction heating power, heat 15s every 2kw, finally make alloy pool temperature-stable in alumina cylinders at 1400 DEG C, obtain the alloy pool of pre-pull;
Five, linear stepping motor is opened, first the alloy cylinder ingot casting molten bath after fusing is made to reach the metal running roller 2mm place of distance rotation with the speed of 200 μm/s, the speed of feed of 30 μm/s is adopted to make the alloy pool of pre-pull close to the metal running roller rotated, after alloy pool contacts with metal running roller, molten alloy in molten bath is spun into fiber, and taken away molten bath, alloy in molten bath runs out of rear stopping linear stepping motor, induction heating power is reduced to zero, finally stop metal running roller to rotate, obtain Ni-Mn-Sn-Fe steel 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 second-phase, therefrom can find that there is obvious Second Phase Precipitation, and crystals has a small amount of distribution, and all the other are mainly distributed in grain boundaries.
Fig. 3 is the photomacrograph of the Ni-Mn-Sn-Fe steel fiber that the present embodiment one obtains, and can find that from figure fiber preparation amount is large, continuity is good, and length can reach 15 cm.Fig. 4 and Fig. 5 is the metal fibers cross section of Ni-Mn-Sn-Fe and scanning electron microscope (SEM) pattern of outside surface.Can find from Fig. 4, during speed of feed 30 μm/s, the cross section of fiber is not the circle of rule, but is made up of the planar section in left side and the circular arc portion on right side.Planar section is that liquation contacts with copper wheel, partial coagulation is formed by copper running roller pull liquation process, and circular arc portion be by pull after fiber freely solidify formed.Show the free coagulation surface of fiber in Fig. 5 to be made up of cellular crystal, cellular crystal crystal grain diameter is hundreds of nanometer, illustrates in process of setting and experienced by rapid solidification.
Fig. 8 and Fig. 9 be the Ni-Mn-Sn-Fe fiber of As-deposited state after surface finish polishing, the scanned photograph under scanning electron microscope secondary electron and back scattering state, illustrates that melt pull method inhibits the precipitation of Ni-Mn-Sn-Fe second-phase well.Figure 10 is X ray diffracting spectrum, demonstrates Ni-Mn-Sn-Fe alloy block before getting rid of silk, occurs obvious second-phase diffraction peak, and the standby fiber of melt pull legal system does not have the diffraction peak of second-phase, only has single austenite phase.Fig. 8 and Fig. 9 illustrates that melt pull method inhibits the precipitation of second-phase in alloy.
Embodiment two: the present embodiment and embodiment one adopt the speed of feed of 50 μm/s to make the alloy pool of pre-pull close to the metal running roller rotated unlike step 5.
Scanning electron microscope (SEM) pattern of the Ni-Mn-Sn-Fe metal fibers cross section that the present embodiment obtains and outside surface as shown in Figure 6 and Figure 7, when speed of feed is 50 μm/s, the cross section of fiber is Near Banded, Fig. 7 shows the free coagulation surface of fiber and is made up of cellular crystal equally, and grain-size is more bigger than Fig. 5.
Claims (9)
1. effectively suppress the method separating out second-phase in Ni-Mn-Sn-Fe alloy, it is characterized in that following these steps to realize:
One, Ni-Mn-Sn-Fe alloy cylindrical ingot is sealed in quartz glass tube, at the temperature of 900 ~ 950 DEG C, 24 ~ 72h is incubated after adopting mechanical pump to vacuumize, cool to room temperature with the furnace, obtain the ingot casting after thermal treatment, adopt WEDM that the ingot casting after thermal treatment is cut into multistage small cylindrical ingot casting, put into water after surface finish light and carry out ultrasonic cleaning, dry and obtain the alloy cylinder ingot casting after cleaning;
Two, alloy cylinder ingot casting after cleaning is put into aluminum oxide hollow cylinder, then the electromagnetic induction heating coil of melt pull equipment work room is put into, axis and the horizontal plane of aluminum oxide hollow cylinder are perpendicular, and adjust the end face of aluminum oxide hollow cylinder and load coil upper edge in same level, after fixing aluminum oxide hollow cylinder, alumina-ceramic cylinder is inserted below alloy cylinder ingot casting in aluminum oxide hollow cylinder, ensure that the lower surface of the alumina-ceramic cylinder inserted contacts with linear stepping motor feed shaft, complete the fixing assembling of aluminum oxide hollow cylinder,
Three, melt pull equipment work room is evacuated to 2 × 10
-3~ 5 × 10
-3pa, passes into high-purity argon gas, repeats to vacuumize, pass into argon gas twice, and then is evacuated to 0.5 × 10
-3~ 1 × 10
-3pa, is finally filled with high-purity argon gas until working spaces's argon pressure reaches and maintains 0.02 ~ 0.05Pa, and the pressure of room of finishing the work regulates;
Four, open metal running roller to rotate and control motor, connect induction heating power, make alloy pool temperature-stable in alumina cylinders at 1300 ~ 1550 DEG C, obtain the alloy pool of pre-pull;
Five, linear stepping motor is opened, the speed of feed of 20 ~ 50 μm/s is adopted to make the alloy pool of pre-pull close to the metal running roller rotated, after alloy pool contacts with metal running roller, molten alloy in molten bath is spun into fiber, and being taken away molten bath, the alloy in molten bath runs out of rear stopping linear stepping motor, and induction heating power is reduced to zero, finally stop metal running roller to rotate, obtain Ni-Mn-Sn-Fe steel fiber.
2. separate out the method for second-phase in a kind of effective suppression Ni-Mn-Sn-Fe alloy according to claim 1, it is characterized in that step one adopts mechanical pump to be evacuated to air pressure is 10
-2~ 10
-3pa.
3. separate out the method for second-phase in a kind of effective suppression Ni-Mn-Sn-Fe alloy according to claim 1, it is characterized in that the height of the medium and small cylindrical ingot of step one is 30 ~ 40mm, diameter is 10 ~ 15mm.
4. separate out the method for second-phase in a kind of effective suppression Ni-Mn-Sn-Fe alloy according to claim 1, it is characterized in that the oven dry described in step one is carried out at 150 DEG C.
5. separate out the method for second-phase in a kind of effective suppression Ni-Mn-Sn-Fe alloy according to claim 1, it is characterized in that the purity of the high-purity argon gas described in step 3 is 99.9%.
6. separate out the method for second-phase in a kind of effective suppression Ni-Mn-Sn-Fe alloy according to claim 1, it is characterized in that step 3 is evacuated to 0.5 × 10 again
-3pa, is finally filled with high-purity argon gas until working spaces's argon pressure reaches and maintains 0.02Pa.
7. separate out the method for second-phase in a kind of effective suppression Ni-Mn-Sn-Fe alloy according to claim 1, it is characterized in that the diameter of the metal running roller described in step 4 is 120mm, control rotating speed is 1000 ~ 1700r/min.
8. in a kind of effective suppression Ni-Mn-Sn-Fe alloy according to claim 1, separate out the method for second-phase, it is characterized in that step 4 connects induction heating power, 15 ~ 20s is heated every 2kw, regulate heating power to 13 ~ 20kw gradually, finally make alloy pool temperature-stable in alumina cylinders at 1300 ~ 1550 DEG C.
9. separate out the method for second-phase in a kind of effective suppression Ni-Mn-Sn-Fe alloy according to claim 1, it is characterized in that the diameter of the Ni-Mn-Sn-Fe steel fiber that step 5 obtains is 30 ~ 150 microns.
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| CN102808113A (en) * | 2012-08-24 | 2012-12-05 | 叶绿均 | Process for preparing nickel-base superalloy |
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2015
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Patent Citations (5)
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|---|---|---|---|---|
| US5725687A (en) * | 1994-11-16 | 1998-03-10 | The Foundation: The Research Institute Of Electric And Magnetic Alloys | Wear-resistant high permability alloy and method of manufacturing the same and magnetic recording and reproducing head |
| JP2006257541A (en) * | 2005-02-16 | 2006-09-28 | Mitsubishi Materials Corp | Co-base alloy having excellent erosion resistance to molten lead-free solder and lead-free soldering equipment member composed of the co-base alloy |
| JP2010013679A (en) * | 2008-07-01 | 2010-01-21 | Toyota Central R&D Labs Inc | Ferromagnetic shape memory alloy sintered compact and method for manufacturing the same |
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