CN103233156A - Manufacturing method of columnar crystal Al-Ni-Co-Ti permanent magnetic alloy - Google Patents

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

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CN103233156A
CN103233156A CN2013100765263A CN201310076526A CN103233156A CN 103233156 A CN103233156 A CN 103233156A CN 2013100765263 A CN2013100765263 A CN 2013100765263A CN 201310076526 A CN201310076526 A CN 201310076526A CN 103233156 A CN103233156 A CN 103233156A
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CN103233156B (en
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薛松
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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 column crystal aluminium nickel cobalt titanium permanent magnet alloy
Technical field
The present invention relates to a kind of manufacturing process of permanent magnet alloy, relate in particular to a kind of manufacturing process of column crystal aluminium nickel cobalt titanium permanent magnet 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 alloys, Al-Ni-Co series permanent magnet alloy stable best.Making alnico has sintering process and casting, and the magnetic property of casting alnico is higher than the sintered aluminium Ni-Co permanent magnetic alloy, and adds an amount of titanium in alloying constituent, can produce magnetic property than higher casting aluminium nickel cobalt titanium permanent magnet alloy.
China Patent No. be ZL200510061461.0's " manufacturing process of isometric aluminium nickel cobalt titanium permanent magnet alloy ", use vacuum melting and non-directional clotting method to produce isometric aluminium nickel cobalt titanium permanent magnet alloy, make magnetic property reach: 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 are not high, and its application is limited to.In addition, use vacuum melting and casting technique because of this technology, facility investment is big, is difficult to large-scale promotion in permanent magnet alloy manufacturing enterprise.
Using casting to make in the process of aluminium nickel cobalt titanium permanent magnet alloy, can also use directional solidification process to make the column crystal aluminium nickel cobalt titanium permanent magnet alloy, high-quality column crystal is very beneficial for improving the magnetic property of product.Have manufacturing enterprise to use casting to produce the column crystal aluminium nickel cobalt titanium permanent magnet 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.Use casting to make the prior art of column crystal aluminium nickel cobalt titanium permanent magnet alloy, in order to obtain better magnetic properties, titanium in this class alloying constituent and the content of aluminium are all many, but this has also caused the directional freeze of column crystal relatively more difficult, the quality of the alloy column crystal that obtains is not high, the consistence of alloy column crystal quality is also bad, has directly caused the magnetic property qualification rate of product low, and the magnetic property room for promotion is limited.In addition, the alloying constituent prescription of prior art also causes product crisp rigid big, the machining difficulty, in machining process broken with fall the limit, the 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 column crystal aluminium nickel cobalt titanium permanent magnet alloy, make the column crystal aluminium nickel cobalt titanium permanent magnet alloy that makes have excellent magnetism can with good machinability.
The invention provides a kind of manufacturing process of column crystal aluminium nickel cobalt titanium permanent magnet alloy, may further comprise the steps:
1) preparation of raw material:
1. starting material are prepared: select metallic material of aluminum, nickel, cobalt, copper, titanium, niobium, holmium, tantalum, bismuth, iron for use, the interpolation non-metallic material are sulphur, selenium, remove the oxide compound of metal material surface and adhere to impurity, all material beyond the sulphur removal is put into 1 hour~2 hours dryings of drying of baker of 80 ℃~100 ℃;
2. starting material are prepared as following weight percent: aluminium A1:7%~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: with iron, nickel, cobalt, copper, holmium, niobium, the tantalum smelting furnace burner hearth of packing into.Titanium, aluminium, bismuth, sulphur, selenium wouldn't be put into burner hearth, and it is outer stand-by to keep somewhere stove;
2. casting mold is prepared: casting mold is put into 1400 ℃~1500 ℃ burning mould stove roasting, make the casting mold bulk temperature reach 1400 ℃ and continue to remain on this more than temperature;
3. melting: when the casting mold bulk temperature in burning the mould stove reaches 1400 ℃, start smelting furnace, after treating that iron, nickel, cobalt, copper, holmium, niobium, tantalum in the smelting furnace thorax melts fully, add titanium, aluminium, bismuth, sulphur, selenium continuation melting, stir molten steel then and pull slag in the molten steel out, before the cast with molten steel temperature control in 1600 ℃~1650 ℃ scopes;
4. cast: the high temperature casting mold is taken out from burn the mould stove, place on the water mold and add foundary weight, open the water coolant of crystallizer, rapidly the molten steel in the smelting furnace is watered then and pour among the high temperature casting mold;
5. cylindrulite oriented growth: behind the casting complete, remove foundary weight, and rapidly with a prior preheating heat to 1200 ℃~1300 ℃ stay-warm case with on the whole casting mold cover, leave standstill motionless foundry goods in casting mold and be cooled to room temperature fully, close the crystallizer water coolant then, finally demould takes out the cylindrulite foundry goods;
3) thermal treatment:
1. annealing: foundry goods is put into annealing furnace, slowly be warming up to 1060 ℃~1120 ℃ with stove, and be incubated 2 hours, cool to room temperature then with the furnace, the foundry goods after the annealing is roughly ground processing;
2. preheating before solid molten: will roughly grind product after the processing proper alignment in the box of packing into, and be placed on then and be heated to 900 ℃~1000 ℃ in the high temperature box furnace, and be incubated 20 minutes~30 minutes;
3. solid molten processing the: the product of pre-heat penetration is delivered in 1255 ℃~1275 ℃ the High Temperature Furnaces Heating Apparatus, be incubated 15 minutes~20 minutes;
4. magnetic field control speed cooling: the product that solid solution is finished takes out from High Temperature Furnaces Heating Apparatus, puts into the magnetic field that magnetic induction density is 1T, makes product temperature drop to 840 ℃~870 ℃ in 90 seconds~110 seconds, naturally cools to 650 ℃~700 ℃ then in magnetic field;
5. isothermal processes: will be cooled to 650 ℃~700 ℃ product through magnetic field control speed and put into 800 ℃ moderate oven preheating 10 minutes, put into 840 ℃~860 ℃ constant-temperature oven then rapidly, and apply the magnetic field that magnetic induction density is 1T immediately, product heat tracing 15 minutes~18 minutes in constant-temperature oven takes out then and naturally cools to room temperature;
6. temper: adopt three grades of tempering systems, change the product behind the isothermal over to tempering stove, at first 650 ℃~670 ℃ insulations 5 hours, cool to 600 ℃~620 ℃ insulations 8 hours with stove then, cool to 560 ℃~580 ℃ insulations 15 hours with stove again, come out of the stove below the last furnace cooling to 300 ℃.
The invention has the beneficial effects as follows:
1. by optimizing the alloying constituent prescription, both kept the titanium that improves the necessary high level of magnetic property, again by in composition, adding an amount of niobium, tantalum, bismuth, sulphur, selenium, even feasible titanium content is up to 7 percent alloy, in castingprocesses, also can use the method for directional freeze to obtain column crystal high-quality, high conformity, be very beneficial for improving the magnetic property of product.
2. by optimizing the alloying constituent prescription, particularly by in composition, adding an amount of holmium, make that the equi-axed crystal between the column crystal is mingled with minimizing, improved the quality of column crystal; Add an amount of holmium and can also in heat treatment process, impel the ferromagnetic phase particle major axis of separating out along the field direction preferred arrangement, the single shaft shape anisotropic of precipitated phase is improved.The two has and is beneficial to very much the raising magnetic property.
3. by optimizing the alloying constituent prescription, in composition, add an amount of holmium, sulphur, bismuth, selenium, reduced the crisp rigid of alloy, obviously improved machinability, significantly reduced the fragmentation that occurs in the machining process and fallen limit, arrisdefect phenomenon.
4. in heat treatment process, used magnetic induction density to reach the magnetic field of 1T, and prior art generally adopt magnetic induction density 0.3T~0.45T than low-intensity magnetic field.Stronger magnetic field energy accelerates the process of alloy spinodal decomposition, and makes the alloy spinodal decomposition carry out more fully, and magnetic property is increased.
5. by adopting the alloying constituent prescription of optimizing and the scientific and reasonable manufacturing process that adapts with it, can produce the column crystal aluminium nickel cobalt titanium permanent magnet alloy of high magnetic characteristics in batches, the magnetic property index is 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 that domestic and international each manufacturing enterprise makes in batches before this magnetic property superorder far away, the magnetic property index of aluminium nickel cobalt titanium permanent magnet alloy.
6. aspect alloy casting, adopt antivacuum casting method, facility investment is few, is conducive to apply.
Embodiment
The present invention is further described below in conjunction with embodiment.
Embodiment one:
Batching: prepare burden by following weight percent: aluminium A1:7%, 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 inevitable denier in iron and the material; In order to reduce the fusing point of metal tantalum, guaranteeing under tantalum and the niobium situation that shared weight percent is constant in batching that adopt the tantalum-niobium alloy form to add, the weight percent of tantalum is 60% in this tantalum-niobium alloy, the weight percent of niobium is 40%.
Be example with 100 kilograms of aluminium nickel cobalt titanium permanent magnet alloys of melting, each set of dispense is such as shown in the table 1-1:
Each set of dispense ratio among the table 1-1 embodiment one
Figure BSA00000863307700041
Niobium in the starting material adopts the niobium powder, and tantalum-niobium alloy adopts thickness less than 1 millimeter thin slice, and other metallic substance is the nuggets shape.
With the impurity that the metallic substance in all raw material is removed oxide on surface or adhered to, then all raw material beyond the sulphur removal S is put into 2 hours dryings of drying of baker baking of 100 ℃.
Carrying out furnace charge filling before the melting earlier prepares with casting mold: the starting material that the prepare smelting furnace burner hearth of in order iron, nickel, cobalt, copper, holmium, niobium, tantalum-niobium alloy being packed into.Titanium, aluminium, bismuth, sulphur, selenium wouldn't be put into burner hearth, and it is outer stand-by to keep somewhere stove, in order to all add after the fusing at the starting material of having put into again.For the directional freeze that makes the later stage carries out obtaining high-quality alloy column crystal smoothly, casting mold adopts high temperature material to make, and integral body is heated to more than 1400 ℃ and heat preservation for standby use in High Temperature Furnaces Heating Apparatus before melting.
Melting: when the casting mold bulk temperature in the High Temperature Furnaces Heating Apparatus reaches 1400 ℃, start smelting furnace, after treating that iron, nickel, cobalt, copper, holmium, niobium, tantalum-niobium alloy in the smelting furnace thorax melts fully, add titanium, aluminium, bismuth, sulphur, selenium and continue melting, stir molten steel then and pull slag in the molten steel out.Before the cast molten steel temperature is controlled in 1600 ℃~1650 ℃ scopes.
Cast and directional freeze: the high temperature casting mold is taken out from burn the mould stove, place on the water mold and add foundary weight, open the water coolant of crystallizer, rapidly the molten steel in the smelting furnace is watered then and pour among the high temperature casting mold.Behind the casting complete, remove foundary weight, and rapidly with a prior preheating heat to 1250 ℃ stay-warm case with on the whole casting mold cover, leave standstill motionless foundry goods in casting mold and be cooled to room temperature fully, close the crystallizer water coolant then, finally demould takes out the column crystal foundry goods.
Thermal treatment:
1. annealing: foundry goods is put into annealing furnace, slowly be warming up to 1100 ℃ with stove, and be incubated 2 hours, cool to room temperature then with the furnace.Foundry goods after the annealing is roughly ground processing.
2. solid molten preceding preheating: the product that will roughly grind after processing is put into the box proper alignment, is placed on then and is heated to 950 ℃ in the high temperature box furnace, is incubated 20 minutes.
3. solid molten processing the: the product of pre-heat penetration is delivered in 1265 ℃ the High Temperature Furnaces Heating Apparatus, be incubated 15 minutes.
4. magnetic field control speed cooling: the product that solid solution is finished takes out from High Temperature Furnaces Heating Apparatus, puts into the magnetic field that magnetic induction density is 1T, with making for 110 seconds product temperature drop to 850 ℃, naturally cools to 650 ℃ then in magnetic field.
5. isothermal processes: will be cooled to 650 ℃ product through magnetic field control speed and put into 800 ℃ moderate oven preheating 10 minutes, and put into 855 ℃ constant-temperature oven then rapidly, and apply the magnetic field that magnetic induction density is 1T immediately.Product heat tracing 15 minutes in constant-temperature oven takes out then and naturally cools to room temperature.
6. temper: adopt three grades of tempering systems.Change the product behind the isothermal over to tempering stove, at first 660 ℃ of insulations 5 hours, cool to 610 ℃ of insulations 8 hours with stove then, cool to 570 ℃ of insulations 15 hours with stove again,
Come out of the stove below the last furnace cooling to 300 ℃.
Column crystal aluminium nickel cobalt titanium permanent magnet alloy product by above technology is made detects according to GB/T3217-92 " permanent magnetism (Hard Magnetic) magnetism of material test method ", records its magnetic property shown in table 1-2:
The magnetic property of table 1-2 embodiment one
Figure BSA00000863307700051
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 inevitable denier in iron and the material; In order to reduce the fusing point of metal tantalum, guaranteeing under tantalum and the niobium situation that shared weight percent is constant in batching that adopt the tantalum-niobium alloy form to add, the weight percent of tantalum is 60% in this tantalum-niobium alloy, the weight percent of niobium is 40%.
Be example with 100 kilograms of aluminium nickel cobalt titanium permanent magnet alloys of melting, each set of dispense is such as shown in the table 2-1:
Each set of dispense ratio among the table 2-1 embodiment two
Niobium in the starting material adopts the niobium powder, and tantalum-niobium alloy adopts thickness less than 1 millimeter thin slice, and other metallic substance is the nuggets shape.
With the impurity that the metallic substance in all raw material is removed oxide on surface or adhered to, then all raw material beyond the sulphur removal S is put into 2 hours dryings of drying of baker baking of 100 ℃.
Carrying out furnace charge filling before the melting earlier prepares with casting mold: the starting material that the prepare smelting furnace burner hearth of in order iron, nickel, cobalt, copper, holmium, niobium, tantalum-niobium alloy being packed into.Titanium, aluminium, bismuth, sulphur, selenium wouldn't be put into burner hearth, and it is outer stand-by to keep somewhere stove, in order to all add after the fusing at the starting material of having put into again.For the directional freeze that makes the later stage carries out obtaining high-quality alloy column crystal smoothly, casting mold adopts high temperature material to make, and integral body is heated to more than 1400 ℃ and heat preservation for standby use in High Temperature Furnaces Heating Apparatus before melting.
Melting: when the casting mold bulk temperature in the High Temperature Furnaces Heating Apparatus reaches 1400 ℃, start smelting furnace, after treating that iron, nickel, cobalt, copper, holmium, niobium, tantalum-niobium alloy in the smelting furnace thorax melts fully, add titanium, aluminium, bismuth, sulphur, selenium and continue melting, stir molten steel then and pull slag in the molten steel out.Before the cast molten steel temperature is controlled in 1600 ℃~1650 ℃ scopes.
Cast and directional freeze: the high temperature casting mold is taken out from burn the mould stove, place on the water mold and add foundary weight, open the water coolant of crystallizer, rapidly the molten steel in the smelting furnace is watered then and pour among the high temperature casting mold.Behind the casting complete, remove foundary weight, and rapidly with a prior preheating heat to 1250 ℃ stay-warm case with on the whole casting mold cover, leave standstill motionless foundry goods in casting mold and be cooled to room temperature fully, close the crystallizer water coolant then, finally demould takes out the column crystal foundry goods.
Thermal treatment:
1. annealing: foundry goods is put into annealing furnace, slowly be warming up to 1100 ℃ with stove, and be incubated 2 hours, cool to room temperature then with the furnace.Foundry goods after the annealing is roughly ground processing.
2. solid molten preceding preheating: the product that will roughly grind after processing is put into the box proper alignment, is placed on then and is heated to 950 ℃ in the high temperature box furnace, is incubated 20 minutes.
3. solid molten processing the: the product of pre-heat penetration is delivered in 1255 ℃ the High Temperature Furnaces Heating Apparatus, be incubated 15 minutes.
4. magnetic field control speed cooling: the product that solid solution is finished takes out from High Temperature Furnaces Heating Apparatus, puts into the magnetic field that magnetic induction density is 1T, with making for 110 seconds product temperature drop to 850 ℃, naturally cools to 650 ℃ then in magnetic field.
5. isothermal processes: will be cooled to 650 ℃ product through magnetic field control speed and put into 800 ℃ moderate oven preheating 10 minutes, and put into 845 ℃ constant-temperature oven then rapidly, and apply the magnetic field that magnetic induction density is 1T immediately.Product heat tracing 15 minutes in constant-temperature oven takes out then and naturally cools to room temperature.
6. temper: adopt three grades of tempering systems.Change the product behind the isothermal over to tempering stove, at first 660 ℃ of insulations 5 hours, cool to 610 ℃ of insulations 8 hours with stove then, cool to 570 ℃ of insulations 15 hours with stove again, come out of the stove below the last furnace cooling to 300 ℃.
Column crystal aluminium nickel cobalt titanium permanent magnet alloy product by above technology is made detects according to GB/T3217-92 " permanent magnetism (Hard Magnetic) magnetism of material test method ", records its magnetic property shown in table 2-2:
The magnetic property of table 2-2 embodiment two
Figure BSA00000863307700071
Embodiment three:
Batching: prepare burden by following weight percent: aluminium A1:7.8%, 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 inevitable denier in iron and the material; In order to reduce the fusing point of metal tantalum, guaranteeing under tantalum and the niobium situation that shared weight percent is constant in batching that adopt the tantalum-niobium alloy form to add, the weight percent of tantalum is 60% in this tantalum-niobium alloy, the weight percent of niobium is 40%.
Be example with 100 kilograms of aluminium nickel cobalt titanium permanent magnet alloys of melting, each set of dispense is such as shown in the table 3-1:
Each set of dispense ratio among the table 3-1 embodiment three
Figure BSA00000863307700072
Niobium in the starting material adopts the niobium powder, and tantalum-niobium alloy adopts thickness less than 1 millimeter thin slice, and other metallic substance is the nuggets shape.
With the impurity that the metallic substance in all raw material is removed oxide on surface or adhered to, then all raw material beyond the sulphur removal S is put into 2 hours dryings of drying of baker baking of 100 ℃.
Carrying out furnace charge filling before the melting earlier prepares with casting mold: the starting material that the prepare smelting furnace burner hearth of in order iron, nickel, cobalt, copper, holmium, niobium, tantalum-niobium alloy being packed into.Titanium, aluminium, bismuth, sulphur, selenium wouldn't be put into burner hearth, and it is outer stand-by to keep somewhere stove, in order to all add after the fusing at the starting material of having put into again.For the directional freeze that makes the later stage carries out obtaining high-quality alloy column crystal smoothly, casting mold adopts high temperature material to make, and integral body is heated to more than 1400 ℃ and heat preservation for standby use in High Temperature Furnaces Heating Apparatus before melting.
Melting: when the casting mold bulk temperature in the High Temperature Furnaces Heating Apparatus reaches 1400 ℃, start smelting furnace, after treating that iron, nickel, cobalt, copper, holmium, niobium, tantalum-niobium alloy in the smelting furnace thorax melts fully, add titanium, aluminium, bismuth, sulphur, selenium and continue melting, stir molten steel then and pull slag in the molten steel out.Before the cast molten steel temperature is controlled in 1600 ℃~1650 ℃ scopes.
Cast and directional freeze: the high temperature casting mold is taken out from burn the mould stove, place on the water mold and add foundary weight, open the water coolant of crystallizer, rapidly the molten steel in the smelting furnace is watered then and pour among the high temperature casting mold.Behind the casting complete, remove foundary weight, and rapidly with a prior preheating heat to 1250 ℃ stay-warm case with on the whole casting mold cover, leave standstill motionless foundry goods in casting mold and be cooled to room temperature fully, close the crystallizer water coolant then, finally demould takes out the column crystal foundry goods.
Thermal treatment:
1. annealing: foundry goods is put into annealing furnace, slowly be warming up to 1100 ℃ with stove, and be incubated 2 hours, cool to room temperature then with the furnace.Foundry goods after the annealing is roughly ground processing.
2. solid molten preceding preheating: will roughly grind the product proper alignment after processing, and be placed on and be heated to 950 ℃ in the high temperature box furnace, and be incubated 20 minutes.
3. solid molten processing the: the product of pre-heat penetration is delivered in 1270 ℃ the High Temperature Furnaces Heating Apparatus, be incubated 20 minutes.
4. magnetic field control speed cooling: the product that solid solution is finished takes out from High Temperature Furnaces Heating Apparatus, puts into the magnetic field that magnetic induction density is 1T, with making for 90 seconds product temperature drop to 850 ℃, naturally cools to 650 ℃ then in magnetic field.
5. isothermal processes: will be cooled to 650 ℃ product through magnetic field control speed and put into 800 ℃ moderate oven preheating 10 minutes, and put into 860 ℃ constant-temperature oven then rapidly, and apply the magnetic field that magnetic induction density is 1T immediately.Product heat tracing 18 minutes in constant-temperature oven takes out then and naturally cools to room temperature.
6. temper: adopt three grades of tempering systems.Change the product behind the isothermal over to tempering stove, at first 660 ℃ of insulations 5 hours, cool to 610 ℃ of insulations 8 hours with stove then, cool to 570 ℃ of insulations 15 hours with stove again, come out of the stove below the last furnace cooling to 300 ℃.
Column crystal aluminium nickel cobalt titanium permanent magnet alloy product by above technology is made detects according to GB/T3217-92 " permanent magnetism (Hard Magnetic) magnetism of material test method ", records its magnetic property shown in table 3-2:
The magnetic property of table 3-2 embodiment three
Figure BSA00000863307700081
Above content be in conjunction with concrete preferred implementation to further describing that the present invention does, can not assert that concrete enforcement of the present invention is confined to these explanations.For the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, can also make some simple deduction or replace, all should be considered as belonging to protection scope of the present invention.

Claims (1)

1. the manufacturing process of a column crystal aluminium nickel cobalt titanium permanent magnet alloy is characterized in that, may further comprise the steps:
1) starting material preparation:
1. starting material are prepared: select metallic material of aluminum Al, nickel, cobalt Co, copper Cu, titanium Ti, niobium Nb, holmium Ho, tantalum Ta, bismuth Bi, iron Fe for use, adding non-metallic material is sulphur S, selenium Se, remove the oxide compound of metal material surface and adhere to impurity, all material beyond the sulphur removal S is put into 1 hour~2 hours dryings of drying of baker of 80 ℃~100 ℃;
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: with iron, nickel, cobalt, copper, holmium, niobium, the tantalum smelting furnace burner hearth of packing into, titanium, aluminium, bismuth, sulphur, selenium wouldn't be put into burner hearth, and it is outer stand-by to keep somewhere stove;
2. casting mold is prepared: casting mold is put into 1400 ℃~1500 ℃ burning mould stove roasting, make the casting mold bulk temperature reach 1400 ℃ and continue to remain on this more than temperature;
3. melting: when the casting mold bulk temperature in burning the mould stove reaches 1400 ℃, start smelting furnace, after treating that iron, nickel, cobalt, copper, holmium, niobium, tantalum in the smelting furnace thorax melts fully, add titanium, aluminium, bismuth, sulphur, selenium continuation melting, stir molten steel then and pull slag in the molten steel out, before the cast with molten steel temperature control in 1600 ℃~1650 ℃ scopes;
4. cast: the high temperature casting mold is taken out from burn the mould stove, place on the water mold and add foundary weight, open the water coolant of crystallizer, rapidly the molten steel in the smelting furnace is watered then and pour among the high temperature casting mold;
5. cylindrulite oriented growth: behind the casting complete, remove foundary weight, and rapidly with a prior preheating heat to 1200 ℃~1300 ℃ stay-warm case with on the whole casting mold cover, leave standstill motionless foundry goods in casting mold and be cooled to room temperature fully, close the crystallizer water coolant then, finally demould takes out the cylindrulite foundry goods;
3) thermal treatment:
1. annealing: foundry goods is put into annealing furnace, slowly be warming up to 1060 ℃~1120 ℃ with stove, and be incubated 2 hours, cool to room temperature then with the furnace, the foundry goods after the annealing is roughly ground processing;
2. preheating before solid molten: will roughly grind product after the processing proper alignment in the box of packing into, and be placed on then and be heated to 900 ℃~1000 ℃ in the high temperature box furnace, and be incubated 20 minutes~30 minutes;
3. solid molten processing the: the product of pre-heat penetration is delivered in 1255 ℃~1275 ℃ the High Temperature Furnaces Heating Apparatus, be incubated 15 minutes~20 minutes;
4. magnetic field control speed cooling: the product that solid solution is finished takes out from High Temperature Furnaces Heating Apparatus, puts into the magnetic field that magnetic induction density is 1T, makes product temperature drop to 840 ℃~870 ℃ in 90 seconds~110 seconds, naturally cools to 650 ℃~700 ℃ then in magnetic field;
5. isothermal processes: will be cooled to 650 ℃~700 ℃ product through magnetic field control speed and put into 800 ℃ moderate oven preheating 10 minutes, put into 840 ℃~860 ℃ constant-temperature oven then rapidly, and apply the magnetic field that magnetic induction density is 1T immediately, product heat tracing 15 minutes~18 minutes in constant-temperature oven takes out then and naturally cools to room temperature;
6. temper: adopt three grades of tempering systems, change the product behind the isothermal over to tempering stove, at first 650 ℃~670 ℃ insulations 5 hours, cool to 600 ℃~620 ℃ insulations 8 hours with stove then, cool to 560 ℃~580 ℃ insulations 15 hours with stove again, come out of the stove below the last furnace cooling to 300 ℃.
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CN105603227A (en) * 2016-01-07 2016-05-25 燕山大学 Preparation method of Al-Co-Ni quasicrystal
CN106816247A (en) * 2015-12-01 2017-06-09 中国科学院宁波材料技术与工程研究所 High stability cobalt-based permanent magnet, its preparation method and regulation and control method
CN108149148A (en) * 2016-12-06 2018-06-12 深圳市英族科技有限公司 Manufacturing process of columnar crystal permanent magnet alloy
CN109082603A (en) * 2018-08-17 2018-12-25 杭州红山磁性材料有限公司 A kind of alnico and preparation method thereof
CN109518065A (en) * 2018-12-26 2019-03-26 杭州科德磁业有限公司 The preparation method of big specification abnormity alnico magnet on brushless exciter
CN112981211A (en) * 2021-02-19 2021-06-18 杭州红山磁性材料有限公司 Alnico large circular magnetic steel
CN113102686A (en) * 2021-04-01 2021-07-13 杭州红山磁性材料有限公司 Alnico integral magnetic steel orientation casting method

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CN104975314A (en) * 2015-06-19 2015-10-14 武汉吉和昌化工科技股份有限公司 Nickel-cobalt-titanium ternary alloy electroplating polishing process
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
CN106816247A (en) * 2015-12-01 2017-06-09 中国科学院宁波材料技术与工程研究所 High stability cobalt-based permanent magnet, its preparation method and regulation and control method
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
CN105603227A (en) * 2016-01-07 2016-05-25 燕山大学 Preparation method of Al-Co-Ni quasicrystal
CN108149148A (en) * 2016-12-06 2018-06-12 深圳市英族科技有限公司 Manufacturing process of columnar crystal permanent magnet alloy
CN109082603A (en) * 2018-08-17 2018-12-25 杭州红山磁性材料有限公司 A kind of alnico and preparation method thereof
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
CN109518065A (en) * 2018-12-26 2019-03-26 杭州科德磁业有限公司 The preparation method of big specification abnormity alnico magnet on brushless exciter
CN112981211A (en) * 2021-02-19 2021-06-18 杭州红山磁性材料有限公司 Alnico large circular magnetic steel
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
CN113102686A (en) * 2021-04-01 2021-07-13 杭州红山磁性材料有限公司 Alnico integral magnetic steel orientation casting method

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