The preparation method of radiation orientation integral permanent magnetic ring
Technical field
The invention belongs to the permanent magnetic material preparing technical field, a kind of preparation method of radiation orientation integral permanent magnetic ring particularly is provided.
Background technology
The permanent-magnetic clamp demand that is applied to motor and gyroscope etc. is increasing.At present, permanent-magnetic clamp generally adopts some each watt shape permanent magnets to be assembled into permanent-magnetic clamp.The radially oriented permanent-magnetic clamp of this prepared exists magnetic field center and geometric center does not overlap, shows magnetic shortcoming pockety, causes motor or gyroscope to rotate steadily and produces a harmonic wave, has a strong impact on motor and gyrostatic performance.The radiation orientation integral permanent magnetic ring that overlap for obtaining magnetic field center and geometric center, table magnetic is evenly distributed must adopt radially oriented pressing under magnetic field technology preparation.The Chinese patent 94113830.5 of on November 11st, 1994 application discloses a kind of manufacture method of radially oriented 2-17 type permanent-magnet rare-earth ring.There is the mould structure defective in this patent, is difficult to the pressed compact demoulding, and rate of finished products is low; Simultaneously, radially oriented magnetic field is inhomogeneous, and permanent-magnetic clamp table magnetic distribution consistency is bad.The Chinese patent 01111509.2 of the Chinese patent 01209054.9 of application on January 30th, 2002 and application on October 16th, 2002 discloses the preparation method of multiple polymerization and radiation orientation device and multi-pole magnet-ring, can prepare multipole integral permanent magnetic ring, and the manufacturing radiation orientation integral ring of being unrealized.The US4533407 of application on August 6th, 1985 and application on December 16th, 1986 US4628809 disclose heat and other static pressuring processes and have prepared radially oriented rare-earth cobalt permanent magnet ring.The characteristics of this two patent are that radially oriented and vacuum hot isostatic pressing technique are combined, and can prepare radially oriented rare-earth cobalt permanent magnet ring.Because device structure complexity, technology realize that difficulty is big, can not satisfy actual manufacturing requirement.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of radiation orientation integral permanent magnetic ring, realized simple to operate, rate of finished products is high, is fit to suitability for industrialized production.
The present invention adopts the magnetic pole principle of same-sex repulsion to produce radially oriented magnetic field, has radiation orientation integral permanent magnetism blank ring by radially oriented mould compacting, obtains radiation orientation integral permanent magnetic ring through oversintering and heat treatment then.High radially oriented degree be can prepare, the radially oriented SmCo integral permanent magnetic ring of 2: 17 types, 1: the 5 radially oriented SmCo integral permanent magnetic ring of type, radially oriented neodymium iron boron integral permanent magnetic ring and radially oriented ferrite integral permanent magnetic ring that magnetic is evenly distributed shown.
Concrete technology is:
Sintering → heat treatment → radiation orientation integral permanent magnetic ring in radiation field oriented moulding → high-purity argon gas protection or the air.
The used raw material of the present invention has 2: 17 type samarium cobalt permanent magnet powder, 1: 5 type samarium cobalt permanent magnet powder, Nd-Fe-B permanent magnetic powder and ferrite permanent-magnet powder.
A, radiation field oriented moulding: radiation field is to be produced by a pair of homopolarity electromagnet, and direct current of each electromagnet (1) or arteries and veins electric current produce the N utmost point and the S utmost point (4), because the polarity of two electromagnet is identical, produces the magnetic line of force (2) that repels each other; The upper and lower magnetic conductive board (5) of radially oriented mould, magnetic conduction core rod (9), permanent-magnet powder (3) and magnetic conduction die sleeve (7) are formed the magnetic line of force (2) loop; Upper and lower non-magnetic conductive board (6), upper and lower non-magnetic conduction pressure pipe (8) is formed non-magnetic conductive loop; Magnetic loop with the magnetic line of force (2) all by permanent-magnet powder (3) thus obtain high radially oriented degree; Obtain radiation orientation integral permanent magnetism blank ring by the two-way compacting permanent-magnet powder of upper and lower non-magnetic conduction pressure pipe (8) (3) at last.
B, radiation orientation integral permanent magnetism blank ring obtain radiation orientation integral permanent magnetic ring after oversintering and heat treatment.
C, when raw material is 2: 17 type samarium cobalt permanent magnet powder or 1: 5 type samarium cobalt permanent magnet powder or Nd-Fe-B permanent magnetic powder, adopt the after-baking of high-purity argon gas protection sintering; When raw material is the ferrite permanent-magnet powder, adopt sintering after-baking in the air.
The composition of used 2: 17 type samarium cobalt permanent magnets of the present invention powder is Sm24.0%~28.5% Fe13.5%~16.5%Cu2.5%~4.5% Zr1.5%~3.5% Co surplus (percentage by weight); The composition of 1: 5 type samarium cobalt permanent magnet powder is Sm31.0%~40%Co surplus (percentage by weight); The composition of Nd-Fe-B permanent magnetic powder is Nd26.0%~33.0%Pr0.0%~4.0% Dy0.0%~3.5% Co0.0%~4.5% Cu0.0%~0.5% Al0.0%~0.3% B0.95%~1.15%Fe surplus (percentage by weight); The composition of ferrite permanent-magnet powder is that permanent ferrite prefiring material adds CaCO
3, SiO
2, La
2O
3Carry out wet-milling and obtain the powder of 0.4 μ m~1.0 μ m.
The invention has the advantages that: realized simple to operate, rate of finished products is high, is fit to suitability for industrialized production.
Description of drawings
Fig. 1 is of the present invention by a pair of electromagnet acquisition radiation field schematic diagram.Wherein, electromagnet 1, the magnetic line of force 2, permanent magnetism powder 3, the N utmost point and the S utmost point 4.
Fig. 2 is a radiation field oriented moulding schematic diagram of the present invention.Wherein, the upper and lower magnetic conductive board 5 of mould, magnetic conduction die sleeve 7, upper and lower non-magnetic conduction pressure pipe 8, magnetic conduction core rod 9,
Fig. 3 is radiation orientation integral permanent magnetic ring of the present invention and inner magnet line of force distribution schematic diagram thereof.The integral permanent magnetic ring and the inner magnet line of force thereof that magnetize through oversintering, heat treatment and radiation distribute, its table magnetic distribution is a horizontal distribution curve as Fig. 4, demonstrates the characteristics that radiation orientation integral permanent magnetic ring has magnetic field center and geometric center overlaps, table magnetic is evenly distributed of the present invention's preparation.
Fig. 4 is 2: the 17 of the present invention radially oriented SmCo integral permanent magnetic ring of type table magnetic scatter charts.
Fig. 5 is 2: 17 of the present invention type samarium cobalt magnet demagnetization curve figure.
Embodiment
Embodiment 1:2: the radially oriented SmCo integral permanent magnetic ring of 17 types
The present embodiment process chart is: alloy proportion → vacuum or argon shield melting → aviation gasoline protection stirring ball-milling → radiation field oriented moulding → high-purity argon gas protection sintering → multistage heat treatment → 2: the 17 radially oriented SmCo integral permanent magnetic ring of type → magnet ring processing → Performance Detection
With alloying component is that Sm25.5%Fe14.5%Cu3.8%Zr2.5%Co surplus (percentage by weight) is carried out vacuum induction or high-purity argon gas protection melting obtains 2: 17 type samarium-cobalt alloys, carries out aviation gasoline protection stirring ball-milling then and obtains 2: 17 type samarium-cobalt alloy powder that particle mean size is 3.8 μ m.2: 17 type samarium-cobalt alloy powder are packed into and are carried out the radiation field compacting in the radially oriented mould shown in Figure 2.Radiation field because the polarity of two electromagnet is identical, produces the magnetic line of force (2) that repels each other by producing the N utmost point and the S utmost point (4) as a pair of perfectly straight stream among Fig. 1 or arteries and veins electric current electromagnet (1).Mould structure shown in Figure 2 with the radiation field magnetic line of force (2) all by permanent magnetism powder (3) thus obtain high radially oriented degree, the while of the oil cylinder up and down move toward one another of press is carried out two-way compacting by upper and lower non-magnetic conduction pressure pipe (8) to 2: 17 type samarium-cobalt alloy powder and is obtained 2: 17 type SmCo radiation orientation integral permanent magnetic ring pressed compacts, and briquetting pressure is 2.0t/cm
2The pressed compact sintering furnace of packing into is evacuated to 10
-3Pa charges into the high-purity argon gas protection, and is cold soon behind 15 ℃/min to 1200 of the programming rate ℃ sintering 2h.Carry out multistage heat treatment, 900 ℃ of heat treatment 5h, 800 ℃ of heat treatment 3h, 700 ℃ of heat treatment 4h, 600 ℃ of heat treatment 3h, 500 ℃ of heat treatment 2h after fast cold.2: 17 radially oriented SmCo integral permanent magnetic rings of type are processed, radial magnetizing and Performance Detection.Fig. 4 is the table magnetic curve of a horizontal distribution of 2: 17 radially oriented SmCo integral permanent magnetic rings of type, and Fig. 5 is the demagnetization curve of magnet.By Fig. 4 and Fig. 5 as can be seen: the radiation orientation integral permanent magnetic ring of the present invention's preparation has high-performance, and magnetic field center and geometric center overlaps, table magnetic is evenly distributed characteristics.Table 1 is the table magnetic parameter of 2: 17 radially oriented SmCo integral permanent magnetic rings of type, and table 2 is performances of magnet.
The table magnetic parameter of 2: 17 radially oriented SmCo integral permanent magnetic rings of type of table 1
Maximum (Gs) | Minimum value (Gs) | Mean value (Gs) | Deviation (%) |
1568.6 | 1444.3 | 1506.5 | 4.12 |
The performance of 2: 17 type samarium cobalt magnets of table 2
Br(T) | bHc(kA/m) | jHc(kA/m) | (BH)
max(kJ/m
3)
|
1.079 | 817.4 | 1919.0 | 229.1 |
Embodiment: 1: 5 radially oriented SmCo integral permanent magnetic ring of type
The present embodiment process chart is: alloy proportion → vacuum or argon shield melting → aviation gasoline protection stirring ball-milling → radiation field oriented moulding → high-purity argon gas protection sintering → heat treatment → 1: the 5 radially oriented SmCo integral permanent magnetic ring of type → magnet ring processing → Performance Detection
With alloying component is that Sm33.0%~Co bal (percentage by weight) carries out vacuum induction or high-purity argon gas protection melting obtains 1: 5 type samarium-cobalt alloy, carries out aviation gasoline protection stirring ball-milling then and obtains 1: 5 type samarium-cobalt alloy powder that particle mean size is 8.0 μ m.1: 5 type samarium-cobalt alloy powder is packed into and is carried out the radiation field compacting in the radially oriented mould shown in Figure 2.Radiation field because the polarity of two electromagnet is identical, produces the magnetic line of force (2) that repels each other by producing the N utmost point and the S utmost point (4) as a pair of perfectly straight stream among Fig. 1 or arteries and veins electric current electromagnet (1).Mould structure shown in Figure 2 with the radiation field magnetic line of force (2) all by permanent magnetism powder (3) thus obtain high radially oriented degree, the while of the oil cylinder up and down move toward one another of press is carried out two-way compacting by upper and lower non-magnetic conduction pressure pipe (8) to 1: 5 type samarium-cobalt alloy powder and is obtained 1: 5 type SmCo radiation orientation integral permanent magnetic ring pressed compact, and briquetting pressure is 3.0t/cm
2The pressed compact sintering furnace of packing into is evacuated to 10
-3Pa charges into the high-purity argon gas protection, and 25 ℃/min to 1120 of programming rate ℃ sintering 1.5h is cooled to 900 ℃ with 0.5 ℃/min.900 ℃ of heat treatment 10h are chilled to room temperature soon with 180 ℃/min.1: 5 radially oriented SmCo integral permanent magnetic ring of type is processed, radial magnetizing and Performance Detection.Table 3 is table magnetic parameters of 1: 5 radially oriented SmCo integral permanent magnetic ring of type, and table 4 is performances of magnet.The radiation orientation integral permanent magnetic ring of the present invention preparation has high-performance, and magnetic field center and geometric center overlaps, table magnetic is evenly distributed characteristics.
The table magnetic parameter of 1: 5 radially oriented SmCo integral permanent magnetic ring of type of table 3
Maximum (Gs) | Minimum value (Gs) | Mean value (Gs) | Deviation (%) |
1355.8 | 1240.1 | 1296.5 | 4.35 |
The performance of 1: 5 type samarium cobalt magnet of table 4
Br(T) | bHc(kA/m) | jHc(kA/m) | (BH)
max(kJ/m
3)
|
0.97 | 676.8 | 1592.0 | 163.5 |
Embodiment 3: radially oriented neodymium iron boron integral permanent magnetic ring
The present embodiment process chart is: alloy proportion → vacuum or argon shield melting → thick middle fragmentation → airflow milling → radiation field oriented moulding → high-purity argon gas protection sintering → multistage heat treatment → radially oriented neodymium iron boron integral permanent magnetic ring → magnet ring processing → Performance Detection
With alloying component is that Nd28.5%Pr3.0%Dy1.0%Co1.5%Cu0.3%Al0.15%B1.08%Fe surplus (percentage by weight) is carried out vacuum induction or high-purity argon gas protection melting obtains Nd Fe B alloys, and airflow milling obtains the Nd Fe B alloys powder that particle mean size is 3.8 μ m after the fragmentation in thick.Carry out the radiation field compacting in the radially oriented mould shown in the Nd Fe B alloys powder load map 2.Radiation field because the polarity of two electromagnet is identical, produces the magnetic line of force (2) that repels each other by producing the N utmost point and the S utmost point (4) as a pair of perfectly straight stream among Fig. 1 or arteries and veins electric current electromagnet (1).Mould structure shown in Figure 2 with the radiation field magnetic line of force (2) all by permanent magnetism powder (3) thus obtain high radially oriented degree, the while of the oil cylinder up and down move toward one another of press is carried out two-way compacting by upper and lower non-magnetic conduction pressure pipe (8) to the Nd Fe B alloys powder and is obtained neodymium iron boron radiation orientation integral permanent magnetic ring pressed compact, and briquetting pressure is 2.5t/cm
2The pressed compact sintering furnace of packing into is evacuated to 10
-3Pa charges into the high-purity argon gas protection, and is cold soon behind 12 ℃/min to 1050 of the programming rate ℃ sintering 1.5h.Carry out multistage heat treatment, 900 ℃ of heat treatment 2h, 600 ℃ of heat treatment 2h after fast cold.Radially oriented neodymium iron boron integral permanent magnetic ring is processed, radial magnetizing and Performance Detection.Table 5 is table magnetic parameters of radially oriented neodymium iron boron integral permanent magnetic ring, and table 6 is performances of magnet.The radiation orientation integral permanent magnetic ring of the present invention preparation has high-performance, and magnetic field center and geometric center overlaps, table magnetic is evenly distributed characteristics.
The table magnetic parameter of the radially oriented neodymium iron boron integral permanent magnetic ring of table 5
Maximum (Gs) | Minimum value (Gs) | Mean value (Gs) | Deviation (%) |
1876.7 | 1722.5 | 1800.1 | 4.10 |
The performance of table 6 neodymium iron boron magnetic body
Br(T) | bHc(kA/m) | jHc(kA/m) | (BH)
max(kJ/m
3)
|
1.31 | 986.5 | 1671.6 | 324.5 |
Embodiment 4: radially oriented ferrite integral permanent magnetic ring
The present embodiment process chart is: mole proportioning → oxidation pre-burning → fine grinding powder process → radiation field oriented moulding → double sintering → radially oriented ferrite integral permanent magnetic ring → magnet ring processing → Performance Detection
Ferrite prefiring material is added CaCO by certain mole proportioning
3, SiO
2, La
2O
3Obtain 0.5 μ m permanent-magnet ferrite powder Deng carrying out wet-milling.Powder is packed into and is carried out the radiation field compacting in the radially oriented mould shown in Figure 2.Radiation field because the polarity of two electromagnet is identical, produces the magnetic line of force (2) that repels each other by producing the N utmost point and the S utmost point (4) as a pair of perfectly straight stream among Fig. 1 or arteries and veins electric current electromagnet (1).Mould structure shown in Figure 2 with the radiation field magnetic line of force (2) all by permanent magnetism powder (3) thus obtain high radially oriented degree, the oil cylinder up and down of press simultaneously move toward one another by about non-magnetic conduction pressure pipe (4) the permanent-magnet ferrite powder carried out two-way compacting obtain radiation orientation integral ferrite permanent-magnet ring pressed compact, briquetting pressure is 3.0t/cm
2Pressed compact pack into carry out 1250 ℃ of sintering 2h in two push pedal electrical kilns after, 950 ℃ of heat treatment 4h.Radially oriented ferrite integral permanent magnetic ring is processed, radial magnetizing and Performance Detection.Table 7 is table magnetic parameters of radially oriented ferrite integral permanent magnetic ring, and table 8 is performances of magnet.The radiation orientation integral permanent magnetic ring of the present invention preparation has high-performance, and magnetic field center and geometric center overlaps, table magnetic is evenly distributed characteristics.
The table magnetic parameter of the radially oriented ferrite integral permanent magnetic ring of table 7
Maximum (Gs) | Minimum value (Gs) | Mean value (Gs) | Deviation (%) |
581.5 | 532.7 | 557.6 | 4.10 |
The performance of table 2 permanent-magnet ferrite
Br(T) | bHc(kA/m) | jHc(kA/m) | (BH)
max(kJ/m
3)
|
0.40 | 272.3 | 364.3 | 30.5 |