CN103233156B - Manufacturing process of columnar crystal Al-Ni-Co-Ti permanent magnetic alloy - Google Patents

Manufacturing process of columnar crystal Al-Ni-Co-Ti permanent magnetic alloy Download PDF

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CN103233156B
CN103233156B CN201310076526.3A CN201310076526A CN103233156B CN 103233156 B CN103233156 B CN 103233156B CN 201310076526 A CN201310076526 A CN 201310076526A CN 103233156 B CN103233156 B CN 103233156B
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CN103233156A (en
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薛涛
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SHENZHEN YINGZU TECHNOLOGY Co Ltd
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SHENZHEN YINGZU TECHNOLOGY Co Ltd
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Abstract

The invention discloses a manufacturing method of a columnar crystal Al-Ni-Co-Ti permanent magnetic alloy. The manufacturing method comprises the following steps of 1, blending 7 to 8wt% of Al, 13.5 to 15wt% of Ni, 36 to 38wt% of Co, 3 to 3.5wt% of Cu, 5.5 to 7wt% of Ti, 0.5 to 1wt% of Nb, 0.5 to 1.5wt% of Ho, 0.3 to 0.9wt% of Ta, 0.3 to 0.6wt% of Bi, 0.15 to 0.5wt% of S, 0.2 to 0.6wt% of Se and the balance Fe, 2, carrying out melting and pouring, and 3, carrying out heat treatment. The columnar crystal Al-Ni-Co-Ti permanent magnetic alloy obtained by the manufacturing method has excellent magnetic properties, small brittleness and good machining properties.

Description

A kind of manufacturing process of columnar crystal Al-Ni-Co-Ti permanent magnetic alloy
Technical field
The present invention relates to a kind of manufacturing process of permanent magnet alloy, particularly relate to a kind of manufacturing process of columnar crystal Al-Ni-Co-Ti permanent magnetic alloy.
Background technology
Permanent magnet alloy is a kind of very important functional materials, and the application in modern industry and information industry is very extensive.In all kinds of permanent magnet alloy, the stability of Al-Ni-Co series permanent magnet alloy is best.Manufacture alnico and have sintering process and casting, the magnetic property of cast aluminum-molykote composite material Ni-Co permanent magnetic alloy higher than sintering alnico alloy, and adds appropriate titanium in alloying constituent, can produce the cast aluminum-molykote composite material nickel cobalt titanium permanent magnet alloy that comparison of magnetic property is high.
China Patent No. is " manufacturing process of isometric aluminium nickel cobalt titanium permanent magnet alloy " of ZL200510061461.0, vacuum melting and non-directional clotting method is used to produce isometric aluminium nickel cobalt titanium permanent magnet alloy, magnetic property is reached: remanent magnetism (Br)=760 ~ 980 (mT), coercive force (Hcb)=124 ~ 165 (KA/m), magnetic energy product (BH) max=46.40 ~ 58.40 (KJ/m3), but this magnetic property is still undesirable, particularly its magnetic energy product and remanent magnetism not high, its application is limited to.In addition, because this technology uses vacuum melting and casting technique, facility investment is large, is difficult to large-scale promotion in permanent magnet alloy manufacturing enterprise.
Using casting to manufacture in the process of aluminium nickel cobalt titanium permanent magnet alloy, directional solidification process can also be used to manufacture columnar crystal Al-Ni-Co-Ti permanent magnetic alloy, the column crystal of high-quality is very beneficial for the magnetic property improving product.Have manufacturing enterprise to use casting to produce the columnar crystal Al-Ni-Co-Ti permanent magnetic alloy that magnetic energy product reaches 87.56KJ/m3 at present, its magnetic property is far above isometric aluminium nickel cobalt titanium permanent magnet alloy.Casting is used to manufacture the prior art of columnar crystal Al-Ni-Co-Ti permanent magnetic alloy, in order to obtain good magnetic property, titanium in this kind of alloying constituent and the content of aluminium all many, but this directional freeze that also result in column crystal is more difficult, the quality of the alloy column crystal obtained is not high, the consistence of alloy column crystal quality is also bad, and the magnetic property qualification rate that directly results in product is low, and magnetic property room for promotion is limited.In addition, the alloying constituent formula of prior art also causes product crisp greatly rigid, machining difficulty, in machining process broken with fall limit, arrisdefect phenomenon is serious, causes the appearance yield of product low.
Summary of the invention
In order to solve the problems of the prior art, the invention provides a kind of manufacturing process of columnar crystal Al-Ni-Co-Ti permanent magnetic alloy, making the columnar crystal Al-Ni-Co-Ti permanent magnetic alloy obtained have excellent magnetic property and good machinability.
The invention provides a kind of manufacturing process of columnar crystal Al-Ni-Co-Ti permanent magnetic alloy, comprise the following steps:
1) preparation of raw material:
1. starting material prepare: select metallic material of aluminum, nickel, cobalt, copper, titanium, niobium, holmium, tantalum, bismuth, iron, interpolation non-metallic material are sulphur, selenium, remove the oxide compound of metal material surface and attachment impurity, all material beyond sulphur removal is put into the baker drying of drying in 1 hour ~ 2 hours of 80 DEG C ~ 100 DEG C;
2. starting material are prepared as following weight percent: aluminium Al:7% ~ 8%, nickel: 13.5% ~ 15%, cobalt Co:36% ~ 38%, copper Cu:3% ~ 3.5%, titanium Ti:5.5% ~ 7%, niobium Nb:0.5% ~ 1%, holmium Ho:0.5% ~ 1.5%, tantalum Ta:0.3% ~ 0.9%, bismuth Bi:0.3% ~ 0.6%, sulphur S:0.15% ~ 0.5%, selenium Se:0.2% ~ 0.6%, iron Fe: surplus;
2) melting and cast:
1. furnace charge filling: iron, nickel, cobalt, copper, holmium, niobium, tantalum are loaded smelting furnace burner hearth.Titanium, aluminium, bismuth, sulphur, selenium wouldn't put into burner hearth, and indwelling stove is outer stand-by;
2. casting mold prepares: the burning mould stove roasting of casting mold being put into 1400 DEG C ~ 1500 DEG C, makes casting mold bulk temperature reach 1400 DEG C and continue to remain on more than this temperature;
3. melting: when burning the casting mold bulk temperature in mould stove and reaching 1400 DEG C, start smelting furnace, after the iron in smelting furnace thorax, nickel, cobalt, copper, holmium, niobium, tantalum melt completely, add titanium, aluminium, bismuth, sulphur, selenium continuation melting, then stir molten steel and the slag pulled out in molten steel, before cast, molten steel temperature is controlled within the scope of 1600 DEG C ~ 1650 DEG C;
4. pour into a mould: taken out from burning mould stove by high temperature casting mold, being placed on water mold and adding foundary weight, open the water coolant of crystallizer, then rapid being watered by molten steel in smelting furnace is poured among high temperature casting mold;
5. cylindrulite oriented growth: after casting complete, remove foundary weight, and heat on whole casting mold cover to the stay-warm case of 1200 DEG C ~ 1300 DEG C with a prior preheating rapidly, leave standstill motionless until the foundry goods in casting mold is cooled to room temperature completely, then close crystallizer water coolant, finally demould takes out cylindrulite foundry goods;
3) thermal treatment:
1. anneal: foundry goods is put into annealing furnace, is slowly warming up to 1060 DEG C ~ 1120 DEG C, and is incubated 2 hours, then cool to room temperature with the furnace with stove, the foundry goods after annealing carries out corase grind processing;
2. solid molten front preheating: the product after corase grind processing is loaded proper alignment in box, is then placed in high temperature box furnace and is heated to 900 DEG C ~ 1000 DEG C, be incubated 20 minutes ~ 30 minutes;
3. solution treated: delivered to by the product of pre-heat penetration in the High Temperature Furnaces Heating Apparatus of 1255 DEG C ~ 1275 DEG C, is incubated 15 minutes ~ 20 minutes;
4. magnetic field control speed cooling: admittedly molten complete product is taken out from High Temperature Furnaces Heating Apparatus, puts into the magnetic field that magnetic induction density is 1T, made product temperature drop to 840 DEG C ~ 870 DEG C in 90 seconds ~ 110 seconds, then naturally cool to 650 DEG C ~ 700 DEG C in magnetic field;
5. isothermal processes: be cooled to the product of 650 DEG C ~ 700 DEG C to put into the moderate oven preheating 10 minutes of 800 DEG C by through magnetic field control speed, then the constant-temperature oven of 840 DEG C ~ 860 DEG C is put into rapidly, and applying magnetic induction density is the magnetic field of 1T immediately, product heating and thermal insulation 15 minutes ~ 18 minutes in constant-temperature oven, then takes out and naturally cools to room temperature;
6. temper: adopt three grades of tempering systems, product after isothermal is proceeded to tempering stove, first 650 DEG C ~ 670 DEG C insulations 5 hours, then 600 DEG C ~ 620 DEG C insulations 8 hours are cooled to stove, cool to 560 DEG C ~ 580 DEG C insulations 15 hours with stove again, last furnace cooling is come out of the stove to less than 300 DEG C.
The invention has the beneficial effects as follows:
1. by optimized alloy component prescription, both the titanium improving the necessary high level of magnetic property had been remained, again by adding appropriate niobium, tantalum, bismuth, sulphur, selenium in composition, even make titanium content up to 7 percent alloy, in castingprocesses, the method for directional freeze also can be used to obtain high-quality, column crystal that consistence is good, be very beneficial for the magnetic property improving product.
2., by optimized alloy component prescription, particularly by adding appropriate holmium in composition, making the equi-axed crystal between column crystal be mingled with minimizing, improve the quality of column crystal; Add the ferromagnetic phase particle long axis field direction preferred arrangement that appropriate holmium can also impel precipitation in heat treatment process, the single shaft shape anisotropic of precipitated phase is improved.Both has and is beneficial to very much raising magnetic property.
3. by optimized alloy component prescription, in composition, add appropriate holmium, sulphur, bismuth, selenium, reduce the crisp rigid of alloy, significantly improve machinability, significantly decrease the fragmentation that occurs in machining process and fall limit, arrisdefect phenomenon.
4. in heat treatment process, employ the magnetic field that magnetic induction density reaches 1T, and prior art generally adopts the comparatively low-intensity magnetic field of magnetic induction density 0.3T ~ 0.45T.Stronger magnetic field energy accelerates the process of alloy spinodal decomposition, and makes alloy spinodal decomposition carry out more abundant, and magnetic property is increased.
5. by adopting the alloying constituent formula optimized and the scientific and reasonable manufacturing process adapted with it, the columnar crystal Al-Ni-Co-Ti permanent magnetic alloy of high magnetic characteristics can be gone out by batch micro operations, magnetic property index be reached: remanent magnetism (Br)=1.15 ~ 1.22 (T), coercive force (Hcb)=126.6 ~ 135.1 (KA/m), HCJ (Hcj)=128.8 ~ 137.4 (KA/m), magnetic energy product (BH) max=100.2 ~ 104.3 (KJ/m3).The various aluminium nickel cobalts of domestic and international each manufacturing enterprise batch micro operations, the magnetic property index of aluminium nickel cobalt titanium permanent magnet alloy before this magnetic property superorder far away.
6. in alloy casting, adopt antivacuum casting method, facility investment is few, is conducive to applying.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
Embodiment one:
Batching: prepare burden by following weight percent: aluminium Al:7%, nickel: 15%, cobalt Co:38%, copper Cu:3%, titanium Ti:5.5%, niobium Nb:0.6%, holmium Ho:0.5%, tantalum Ta:0.3%, bismuth Bi:0.3%, sulphur S:0.2%, selenium Se:0.2%, surplus is the impurity of inevitably denier in iron and material; In order to reduce the fusing point of metal tantalum, when ensureing tantalum and niobium shared weight percent being constant in batching, employing tantalum-niobium alloy form adds, and in this tantalum-niobium alloy, the weight percent of tantalum is 60%, and the weight percent of niobium is 40%.
For melting 100 kilograms of aluminium nickel cobalt titanium permanent magnet alloys, each component proportion is as shown in table 1-1:
Each component proportion in table 1-1 embodiment one
Niobium in starting material adopts niobium powder, the thin slice that tantalum-niobium alloy adopts thickness to be less than 1 millimeter, and other metallic substance is nuggets shape.
Metallic substance in all raw material is removed the impurity of oxide on surface or attachment, then all raw material beyond sulphur removal S is put into the baker baking drying of drying in 2 hours of 100 DEG C.
First carry out furnace charge filling before melting to prepare with casting mold: iron, nickel, cobalt, copper, holmium, niobium, tantalum-niobium alloy are loaded smelting furnace burner hearth by starting material in order that prepare.Titanium, aluminium, bismuth, sulphur, selenium wouldn't put into burner hearth, and indwelling stove is outer stand-by, to add after the starting material put into all melt again.Carry out smoothly to make the directional freeze in later stage obtaining high-quality alloy column crystal, casting mold adopts high temperature material to make, and before melting, in High Temperature Furnaces Heating Apparatus, entirety is heated to more than 1400 DEG C and heat preservation for standby use.
Melting: when the casting mold bulk temperature in High Temperature Furnaces Heating Apparatus reaches 1400 DEG C, start smelting furnace, after the iron in smelting furnace thorax, nickel, cobalt, copper, holmium, niobium, tantalum-niobium alloy melt completely, add titanium, aluminium, bismuth, sulphur, selenium continuation melting, then stir molten steel and the slag pulled out in molten steel.Before cast, molten steel temperature is controlled within the scope of 1600 DEG C ~ 1650 DEG C.
Cast and directional freeze: taken out from burning mould stove by high temperature casting mold, being placed on water mold and adding foundary weight, open the water coolant of crystallizer, then rapid being watered by molten steel in smelting furnace is poured among high temperature casting mold.After casting complete, remove foundary weight, and rapidly heat to the stay-warm case of 1250 DEG C by whole casting mold cover with a prior preheating, standing motionless until the foundry goods in casting mold is cooled to room temperature completely, then close crystallizer water coolant, finally demould takes out column crystal foundry goods.
Thermal treatment:
1. anneal: foundry goods is put into annealing furnace, is slowly warming up to 1100 DEG C with stove, and be incubated 2 hours, then cool to room temperature with the furnace.Foundry goods after annealing is carried out corase grind processing.
2. solid molten front preheating: the product after corase grind processing is put into box proper alignment, is then placed in high temperature box furnace and is heated to 950 DEG C, be incubated 20 minutes.
3. solution treated: delivered to by the product of pre-heat penetration in the High Temperature Furnaces Heating Apparatus of 1265 DEG C, is incubated 15 minutes.
4. magnetic field control speed cooling: admittedly molten complete product is taken out from High Temperature Furnaces Heating Apparatus, putting into the magnetic field that magnetic induction density is 1T, with making for 110 seconds product temperature drop to 850 DEG C, then naturally cooling to 650 DEG C in magnetic field.
5. isothermal processes: be cooled to the product of 650 DEG C to put into the moderate oven preheating 10 minutes of 800 DEG C by through magnetic field control speed, then put into rapidly the constant-temperature oven of 855 DEG C, and to apply magnetic induction density be immediately the magnetic field of 1T.Product heating and thermal insulation 15 minutes in constant-temperature oven, then takes out and naturally cools to room temperature.
6. temper: adopt three grades of tempering systems.Product after isothermal is proceeded to tempering stove, and first 660 DEG C of insulations 5 hours, then cool to 610 DEG C of insulations 8 hours with stove, then cool to 570 DEG C of insulations 15 hours with stove, last furnace cooling is come out of the stove to less than 300 DEG C.
The columnar crystal Al-Ni-Co-Ti permanent magnetic alloy product made by above technique, detects according to GB/T 3217-92 " permanent magnetism (Hard Magnetic) magnetism of material test method ", records its magnetic property as shown in table 1-2:
The magnetic property of table 1-2 embodiment one
Embodiment two:
Batching: prepare burden by following weight percent: aluminium Al:7.5%, nickel: 14.5%, cobalt Co:36%, copper Cu:3.2%, titanium Ti:6%, niobium Nb:1%, holmium Ho:0.8%, tantalum Ta:0.6%, bismuth Bi:0.3%, sulphur S:0.4%, selenium Se:0.4%, surplus is the impurity of inevitably denier in iron and material; In order to reduce the fusing point of metal tantalum, when ensureing tantalum and niobium shared weight percent being constant in batching, employing tantalum-niobium alloy form adds, and in this tantalum-niobium alloy, the weight percent of tantalum is 60%, and the weight percent of niobium is 40%.
For melting 100 kilograms of aluminium nickel cobalt titanium permanent magnet alloys, each component proportion is as shown in table 2-1:
Each component proportion in table 2-1 embodiment two
Niobium in starting material adopts niobium powder, the thin slice that tantalum-niobium alloy adopts thickness to be less than 1 millimeter, and other metallic substance is nuggets shape.
Metallic substance in all raw material is removed the impurity of oxide on surface or attachment, then all raw material beyond sulphur removal S is put into the baker baking drying of drying in 2 hours of 100 DEG C.
First carry out furnace charge filling before melting to prepare with casting mold: iron, nickel, cobalt, copper, holmium, niobium, tantalum-niobium alloy are loaded smelting furnace burner hearth by starting material in order that prepare.Titanium, aluminium, bismuth, sulphur, selenium wouldn't put into burner hearth, and indwelling stove is outer stand-by, to add after the starting material put into all melt again.Carry out smoothly to make the directional freeze in later stage obtaining high-quality alloy column crystal, casting mold adopts high temperature material to make, and before melting, in High Temperature Furnaces Heating Apparatus, entirety is heated to more than 1400 DEG C and heat preservation for standby use.
Melting: when the casting mold bulk temperature in High Temperature Furnaces Heating Apparatus reaches 1400 DEG C, start smelting furnace, after the iron in smelting furnace thorax, nickel, cobalt, copper, holmium, niobium, tantalum-niobium alloy melt completely, add titanium, aluminium, bismuth, sulphur, selenium continuation melting, then stir molten steel and the slag pulled out in molten steel.Before cast, molten steel temperature is controlled within the scope of 1600 DEG C ~ 1650 DEG C.
Cast and directional freeze: taken out from burning mould stove by high temperature casting mold, being placed on water mold and adding foundary weight, open the water coolant of crystallizer, then rapid being watered by molten steel in smelting furnace is poured among high temperature casting mold.After casting complete, remove foundary weight, and rapidly heat to the stay-warm case of 1250 DEG C by whole casting mold cover with a prior preheating, standing motionless until the foundry goods in casting mold is cooled to room temperature completely, then close crystallizer water coolant, finally demould takes out column crystal foundry goods.
Thermal treatment:
1. anneal: foundry goods is put into annealing furnace, is slowly warming up to 1100 DEG C with stove, and be incubated 2 hours, then cool to room temperature with the furnace.Foundry goods after annealing is carried out corase grind processing.
2. solid molten front preheating: the product after corase grind processing is put into box proper alignment, is then placed in high temperature box furnace and is heated to 950 DEG C, be incubated 20 minutes.
3. solution treated: delivered to by the product of pre-heat penetration in the High Temperature Furnaces Heating Apparatus of 1255 DEG C, is incubated 15 minutes.
4. magnetic field control speed cooling: admittedly molten complete product is taken out from High Temperature Furnaces Heating Apparatus, putting into the magnetic field that magnetic induction density is 1T, with making for 110 seconds product temperature drop to 850 DEG C, then naturally cooling to 650 DEG C in magnetic field.
5. isothermal processes: be cooled to the product of 650 DEG C to put into the moderate oven preheating 10 minutes of 800 DEG C by through magnetic field control speed, then put into rapidly the constant-temperature oven of 845 DEG C, and to apply magnetic induction density be immediately the magnetic field of 1T.Product heating and thermal insulation 15 minutes in constant-temperature oven, then takes out and naturally cools to room temperature.
6. temper: adopt three grades of tempering systems.Product after isothermal is proceeded to tempering stove, and first 660 DEG C of insulations 5 hours, then cool to 610 DEG C of insulations 8 hours with stove, then cool to 570 DEG C of insulations 15 hours with stove, last furnace cooling is come out of the stove to less than 300 DEG C.
The columnar crystal Al-Ni-Co-Ti permanent magnetic alloy product made by above technique, detects according to GB/T 3217-92 " permanent magnetism (Hard Magnetic) magnetism of material test method ", records its magnetic property as shown in table 2-2:
The magnetic property of table 2-2 embodiment two
Embodiment three:
Batching: prepare burden by following weight percent: aluminium Al:7.8%, nickel: 14.5%, cobalt Co:37.5%, copper Cu:3.3%, titanium Ti:6.5%, niobium Nb:1%, holmium Ho:1.3%, tantalum Ta:0.9%, bismuth Bi:0.5%, sulphur S:0.5%, selenium Se:0.4%, surplus is the impurity of inevitably denier in iron and material; In order to reduce the fusing point of metal tantalum, when ensureing tantalum and niobium shared weight percent being constant in batching, employing tantalum-niobium alloy form adds, and in this tantalum-niobium alloy, the weight percent of tantalum is 60%, and the weight percent of niobium is 40%.
For melting 100 kilograms of aluminium nickel cobalt titanium permanent magnet alloys, each component proportion is as shown in table 3-1:
Each component proportion in table 3-1 embodiment three
Niobium in starting material adopts niobium powder, the thin slice that tantalum-niobium alloy adopts thickness to be less than 1 millimeter, and other metallic substance is nuggets shape.
Metallic substance in all raw material is removed the impurity of oxide on surface or attachment, then all raw material beyond sulphur removal S is put into the baker baking drying of drying in 2 hours of 100 DEG C.
First carry out furnace charge filling before melting to prepare with casting mold: iron, nickel, cobalt, copper, holmium, niobium, tantalum-niobium alloy are loaded smelting furnace burner hearth by starting material in order that prepare.Titanium, aluminium, bismuth, sulphur, selenium wouldn't put into burner hearth, and indwelling stove is outer stand-by, to add after the starting material put into all melt again.Carry out smoothly to make the directional freeze in later stage obtaining high-quality alloy column crystal, casting mold adopts high temperature material to make, and before melting, in High Temperature Furnaces Heating Apparatus, entirety is heated to more than 1400 DEG C and heat preservation for standby use.
Melting: when the casting mold bulk temperature in High Temperature Furnaces Heating Apparatus reaches 1400 DEG C, start smelting furnace, after the iron in smelting furnace thorax, nickel, cobalt, copper, holmium, niobium, tantalum-niobium alloy melt completely, add titanium, aluminium, bismuth, sulphur, selenium continuation melting, then stir molten steel and the slag pulled out in molten steel.Before cast, molten steel temperature is controlled within the scope of 1600 DEG C ~ 1650 DEG C.
Cast and directional freeze: taken out from burning mould stove by high temperature casting mold, being placed on water mold and adding foundary weight, open the water coolant of crystallizer, then rapid being watered by molten steel in smelting furnace is poured among high temperature casting mold.After casting complete, remove foundary weight, and rapidly heat to the stay-warm case of 1250 DEG C by whole casting mold cover with a prior preheating, standing motionless until the foundry goods in casting mold is cooled to room temperature completely, then close crystallizer water coolant, finally demould takes out column crystal foundry goods.
Thermal treatment:
1. anneal: foundry goods is put into annealing furnace, is slowly warming up to 1100 DEG C with stove, and be incubated 2 hours, then cool to room temperature with the furnace.Foundry goods after annealing is carried out corase grind processing.
2. solid molten front preheating: the product proper alignment after processing will be roughly ground, be placed in high temperature box furnace and be heated to 950 DEG C, be incubated 20 minutes.
3. solution treated: delivered to by the product of pre-heat penetration in the High Temperature Furnaces Heating Apparatus of 1270 DEG C, is incubated 20 minutes.
4. magnetic field control speed cooling: admittedly molten complete product is taken out from High Temperature Furnaces Heating Apparatus, putting into the magnetic field that magnetic induction density is 1T, with making for 90 seconds product temperature drop to 850 DEG C, then naturally cooling to 650 DEG C in magnetic field.
5. isothermal processes: be cooled to the product of 650 DEG C to put into the moderate oven preheating 10 minutes of 800 DEG C by through magnetic field control speed, then put into rapidly the constant-temperature oven of 860 DEG C, and to apply magnetic induction density be immediately the magnetic field of 1T.Product heating and thermal insulation 18 minutes in constant-temperature oven, then takes out and naturally cools to room temperature.
6. temper: adopt three grades of tempering systems.Product after isothermal is proceeded to tempering stove, and first 660 DEG C of insulations 5 hours, then cool to 610 DEG C of insulations 8 hours with stove, then cool to 570 DEG C of insulations 15 hours with stove, last furnace cooling is come out of the stove to less than 300 DEG C.
The columnar crystal Al-Ni-Co-Ti permanent magnetic alloy product made by above technique, detects according to GB/T 3217-92 " permanent magnetism (Hard Magnetic) magnetism of material test method ", records its magnetic property as shown in table 3-2:
The magnetic property of table 3-2 embodiment three
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.

Claims (1)

1. a manufacturing process for columnar crystal Al-Ni-Co-Ti permanent magnetic alloy, is characterized in that, comprises the following steps:
1) starting material preparation:
1. starting material prepare: select metallic material of aluminum A1, nickel, cobalt Co, copper Cu, titanium Ti, niobium Nb, holmium Ho, tantalum Ta, bismuth Bi, iron Fe, adding non-metallic material is sulphur S, selenium Se, remove the oxide compound of metal material surface and attachment impurity, all material beyond sulphur removal S is put into the baker drying of drying in 1 hour ~ 2 hours of 80 DEG C ~ 100 DEG C;
2. starting material are prepared as following weight percent: aluminium Al:7% ~ 8%, nickel: 13.5% ~ 15%, cobalt Co:36% ~ 38%, copper Cu:3% ~ 3.5%, titanium Ti:5.5% ~ 7%, niobium Nb:0.5% ~ 1%, holmium Ho:0.5% ~ 1.5%, tantalum Ta:0.3% ~ 0.9%, bismuth Bi:0.3% ~ 0.6%, sulphur S:0.15% ~ 0.5%, selenium Se:0.2% ~ 0.6%, iron Fe: surplus;
2) melting and cast:
1. furnace charge filling: iron, nickel, cobalt, copper, holmium, niobium, tantalum are loaded smelting furnace burner hearth, and titanium, aluminium, bismuth, sulphur, selenium wouldn't put into burner hearth, indwelling stove is outer stand-by;
2. casting mold prepares: the burning mould stove roasting of casting mold being put into 1400 DEG C ~ 1500 DEG C, makes casting mold bulk temperature reach 1400 DEG C and continue to remain on more than this temperature;
3. melting: when burning the casting mold bulk temperature in mould stove and reaching 1400 DEG C, start smelting furnace, after the iron in smelting furnace thorax, nickel, cobalt, copper, holmium, niobium, tantalum melt completely, add titanium, aluminium, bismuth, sulphur, selenium continuation melting, then stir molten steel and the slag pulled out in molten steel, before cast, molten steel temperature is controlled within the scope of 1600 DEG C ~ 1650 DEG C;
4. pour into a mould: taken out from burning mould stove by high temperature casting mold, being placed on water mold and adding foundary weight, open the water coolant of crystallizer, then rapid being watered by molten steel in smelting furnace is poured among high temperature casting mold;
5. cylindrulite oriented growth: after casting complete, remove foundary weight, and heat on whole casting mold cover to the stay-warm case of 1200 DEG C ~ 1300 DEG C with a prior preheating rapidly, leave standstill motionless until the foundry goods in casting mold is cooled to room temperature completely, then close crystallizer water coolant, finally demould takes out cylindrulite foundry goods;
3) thermal treatment:
1. anneal: foundry goods is put into annealing furnace, is slowly warming up to 1060 DEG C ~ 1120 DEG C, and is incubated 2 hours, then cool to room temperature with the furnace with stove, the foundry goods after annealing carries out corase grind processing;
2. solid molten front preheating: the product after corase grind processing is loaded proper alignment in box, is then placed in high temperature box furnace and is heated to 900 DEG C ~ 1000 DEG C, be incubated 20 minutes ~ 30 minutes;
3. solution treated: delivered to by the product of pre-heat penetration in the High Temperature Furnaces Heating Apparatus of 1255 DEG C ~ 1275 DEG C, is incubated 15 minutes ~ 20 minutes;
4. magnetic field control speed cooling: admittedly molten complete product is taken out from High Temperature Furnaces Heating Apparatus, puts into the magnetic field that magnetic induction density is 1T, made product temperature drop to 840 DEG C ~ 870 DEG C in 90 seconds ~ 110 seconds, then naturally cool to 650 DEG C ~ 700 DEG C in magnetic field;
5. isothermal processes: be cooled to the product of 650 DEG C ~ 700 DEG C to put into the moderate oven preheating 10 minutes of 800 DEG C by through magnetic field control speed, then the constant-temperature oven of 840 DEG C ~ 860 DEG C is put into rapidly, and applying magnetic induction density is the magnetic field of 1T immediately, product heating and thermal insulation 15 minutes ~ 18 minutes in constant-temperature oven, then takes out and naturally cools to room temperature;
6. temper: adopt three grades of tempering systems, product after isothermal is proceeded to tempering stove, first 650 DEG C ~ 670 DEG C insulations 5 hours, then 600 DEG C ~ 620 DEG C insulations 8 hours are cooled to stove, cool to 560 DEG C ~ 580 DEG C insulations 15 hours with stove again, last furnace cooling is come out of the stove to less than 300 DEG C.
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CN104975314B (en) * 2015-06-19 2018-08-07 武汉吉和昌化工科技股份有限公司 A kind of nickel-cobalt-titanium ternary alloys plating bright technique
CN106816247B (en) * 2015-12-01 2019-07-09 中国科学院宁波材料技术与工程研究所 High stability cobalt-based permanent magnet, preparation method and regulation method
CN105603227B (en) * 2016-01-07 2017-08-04 燕山大学 A kind of preparation method of Al Co Ni quasi-crystalline substances
CN108149148A (en) * 2016-12-06 2018-06-12 深圳市英族科技有限公司 A kind of manufacturing process of column crystal permanent-magnet alloy
CN109082603B (en) * 2018-08-17 2020-02-11 杭州红山磁性材料有限公司 Alnico permanent magnetic alloy and preparation method thereof
CN109518065B (en) * 2018-12-26 2021-01-05 杭州科德磁业有限公司 Preparation method of large-size special-shaped aluminum-nickel-cobalt magnet for brushless exciter
CN112981211B (en) * 2021-02-19 2022-04-12 杭州红山磁性材料有限公司 Alnico large circular magnetic steel
CN113102686B (en) * 2021-04-01 2022-11-29 杭州红山磁性材料有限公司 Alnico integral magnetic steel orientation casting method

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