CN103839671B - A kind of manufacture method of neodymium iron boron rare earth permanent magnet device - Google Patents
A kind of manufacture method of neodymium iron boron rare earth permanent magnet device Download PDFInfo
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- CN103839671B CN103839671B CN201410107557.5A CN201410107557A CN103839671B CN 103839671 B CN103839671 B CN 103839671B CN 201410107557 A CN201410107557 A CN 201410107557A CN 103839671 B CN103839671 B CN 103839671B
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Abstract
The invention discloses a kind of manufacture method of neodymium iron boron rare earth permanent magnet device, first Nd-Fe-B rare-earth permanent magnet blank is become, carry out machining afterwards and make Fe-B rare-earth permanent magnet, carry out filming process afterwards and make neodymium iron boron rare earth permanent magnet device, plated film is divided into 3 layers, ground floor is magnetron sputtering coating, thickness of coating is: 0.02-2 μm, the second layer is the mixing coating of more than one targets of magnetron sputtering, thickness of coating is: 1-20 μm, third layer is magnetron sputtering coating, and thickness of coating is: 0.1-5 μm; Adopt magnetron sputtering plating of the present invention to make the surface treatment procedure of rare earth permanent magnet device, not only increase the resistance to corrosion of rare earth permanent magnet device, also improve the magnetic property of rare earth permanent magnet device simultaneously.
Description
Technical field
The invention belongs to permanent magnet devices field, particularly relate to a kind of manufacture method of neodymium iron boron rare earth permanent magnet device.
Background technology
Nd-Fe-B rare earth permanent magnetic material, is more and more applied with the magnetic property that it is excellent, is widely used in the Magnetic resonance imaging of medical treatment, computer hard disc driver, sound equipment, mobile phone etc.; Along with energy-conservation and requirement that is low-carbon economy, Nd-Fe-B rare earth permanent magnetic material starts again at auto parts and components, household electrical appliance, energy-conservation and control motor, hybrid vehicle, and field of wind power generation is applied.
The process of surface treatment of the rare earth permanent magnet device of prior art mainly contains the technology such as electroplated Ni-Cu-Ni, plating Zn, electrophoresis, spraying, also has the vacuum aluminum-coated method that adopts, as Chinese patent ZL96192129.3, discloses the method for Vacuum Deposition Ti and AlN; Another Chinese patent ZL01111757.5 discloses the method adopting vacuum evaporation zinc-plated, aluminium, tin, magnesium.
Prior art as shown in Figure 1, has two strutting pieces 7 to be arranged side by side in the upper district of vacuum chamber 1 inside, can the rotating shaft 6 on a horizontal axis of rotation rotate.Six cylinders 5 formed by stainless steel cloth load magnetic part 14, are supported for an annular by rotating shaft 8 in the outer circumference direction of the rotating shaft 6 of strutting piece 7, for 6 rotating around the shaft.Multiple heating boats 2 as the evaporation section of the material aluminium wire 9 for evaporating are arranged on the heating boat supporting base 4 that a support platform 3 in process chamber 1 inferior segment rises.Aluminium wire 9 is fixed and is wrapped on a feed roller 10 under support platform 3.Led by the thermal resistance protection tube 11 of an inner surface towards heating boat 2 and reach on heating boat 2 in the front end of aluminium wire 9; a recess 12 is arranged in a part for protection tube 11; and feed gear wheel 13 is installed corresponding to recess 12; and directly contact with aluminium wire 9; can be fed in heating boat 2 by aluminium wire consistently by feeding aluminium wire 9 like this, heating evaporation deposits to and the magnetic part 14 in the barrel 5 of rotation completes its surface aluminizes.
Prior art adopts evaporation coating, and the adhesion of rete and matrix is poor, improves the resistance to corrosion Shortcomings of rare earth permanent magnet device; Prior art also has employing magnetron sputtering plating, because the efficiency of magnetron sputtering is low, is not suitable for low cost and produces in enormous quantities, owing to not solving the technology that is installed of rare earth permanent magnet device, be not easily installed, produce trouble; Prior art also has employing multi-arc ion plating film, there is bulky grain due to during multi-arc ion plating film, can not reach the corrosion resistance requirement of rare earth permanent magnet device; In order to solve the shortcoming of multi-arc ion coating, also someone contemplates employing multi-arc ion coating and magnetron sputtering composite film coating to prior art, but does not all solve high efficiency, low-costly and in high volume production technology, device structure Shortcomings; The particularly electroplating chemical treatment process of prior art rare earth permanent magnet device, energy consumption is high pollution, requires expensive water treatment facilities, deals with improperly and have a strong impact on biological environment.Because production process of the present invention is carried out in a vacuum, do not use environmental pollution material, can not pollute to biological environment, also eliminate the impact of " battery " effect on the reduction of magnetic property in electroplating process simultaneously.For this reason, the vacuum magnetic control film coating equipment and the manufacture method that the invention provides a kind of novel rare-earth permanent magnet devices compensate for the deficiencies in the prior art; The neodymium iron boron rare earth permanent magnet device of device fabrication of the present invention is adopted to not only increase the resistance to corrosion of rare earth permanent magnet device in addition, also improve the magnetic property of rare earth permanent magnet device, significantly improve magnetic energy product and the coercive force of rare earth permanent magnet device, save rare rare earth resources, especially save more rare heavy rare earth consumption.
Summary of the invention
The present invention is to provide a kind of vacuum coating equipment and manufacture method of neodymium iron boron rare earth permanent magnet device, is achieved through the following technical solutions the magnetic property and raising resistance to corrosion that improve rare earth permanent magnet device:
A magnetic control film coating equipment for neodymium iron boron rare earth permanent magnet device, comprises vacuum film coating chamber, cylinder negative electrode magnetic control target, anode-layer-linear ion source, heater, pivoted frame and netted charging basket; Described vacuum film coating chamber is made up of horizontal vacuum housing, Qianmen and bonnet, Qianmen and vaccum case pass through rubber seal rings for seal, bonnet or be welded on horizontal vacuum housing or by connector connects, the transmission device of pivoted frame is arranged on bonnet, and the motor transmission shaft outside vacuum chamber is sent to vacuum coating indoor by dynamic sealing device; Pivoted frame design is indoor in vacuum coating, and by rotating shaft support on framework, framework is fixed on vaccum case; Not only the axis of pivoted frame and the axis being parallel of horizontal vacuum housing, netted charging basket two ends have rotating shaft to be arranged on pivoted frame, the axis of rotating shaft and the axis being parallel of pivoted frame, and pivoted frame revolves round the sun around the axis of vaccum case, and netted charging basket revolves round the sun but also rotation with pivoted frame.
Described cylinder magnetic control target is arranged on the bonnet of vacuum coating indoor, and power supply, cooling water and transmission device are introduced by outside, axis and turret shaft line parallel.
Be provided with more than one cylinder magnetic control target in vacuum coating indoor, described cylinder magnetic control target is arranged on the inside and outside of pivoted frame respectively.
The quantity being arranged on the cylinder magnetic control target of pivoted frame inside is more than one, is arranged on the quantity more than two of the cylinder magnetic control target of pivoted frame outside.
Be arranged on the quantity n of the cylinder magnetic control target of pivoted frame inside, be arranged on quantity 2n of the cylinder magnetic control target of pivoted frame outside, n be greater than 3 integer.
The quantity being arranged on the cylinder magnetic control target of pivoted frame inside is 3, and the quantity being arranged on the cylinder magnetic control target of pivoted frame outside is 6.
Described cylinder magnetic control target, built with the magnet ring of multiple axial charging, has magnetic guiding loop between magnet ring, and magnet ring moves relative to cylinder magnetic control target axial reciprocating.
In described cylinder magnetic control target or the magnetic stripe of many radial magnetizings is housed, magnetic stripe circumferentially distributes in cylinder magnetic control target, has interval between magnetic stripe, and the quantity of magnetic stripe is more than 3 or 3, and magnetic stripe is relative to cylinder magnetic control target coaxial rotation.
Described magnet ring or magnetic stripe are manufactured by Nd-Fe-B rare-earth permanent magnet.
Described anode-layer-linear ion source is arranged on the bonnet of vacuum coating indoor, is distributed in pivoted frame or the periphery of pivoted frame.
A kind of manufacture method of neodymium iron boron rare earth permanent magnet device, first alloy melting is carried out, in the molten state cooling on alloy casting to the water-cooled rotary copper roller of band is formed alloy sheet, then hydrogen fragmentation is carried out, batch mixing is carried out after hydrogen fragmentation, the laggard row airflow milling of batch mixing, afterwards under nitrogen protection with delivering to nitrogen protection magnetic field orientating press-molding after batch mixer batch mixing, encapsulate in guard box after shaping, then take out and carry out isostatic pressed, feeding agglomerating plant sintering and timeliness make Nd-Fe-B rare-earth permanent magnet blank afterwards, carry out machining afterwards and make Fe-B rare-earth permanent magnet, carry out filming process afterwards and make neodymium iron boron rare earth permanent magnet device, plated film is divided into 3 layers, ground floor is magnetron sputtering coating, thickness of coating is: 0.02-2 μm, the second layer is the mixing coating of more than one targets of magnetron sputtering, thickness of coating is: 1-20 μm, third layer is magnetron sputtering coating, thickness of coating is: 0.1-5 μm.
Described plated film is divided into 3 layers, and ground floor is magnetron sputtering Dy-Al layer, and the second layer is magnetron sputtering Al and Ni-Cr mixing coating, Al and Ni-Cr be superposition alternately, and third layer is magnetron sputtering Al layer.
Described plated film is divided into 3 layers, and ground floor is magnetron sputtering coating, and plated film target is more than one in Al, Dy-Al, Tb-Al, Dy-Fe, Tb-Fe, and the second layer is magnetron sputtering coating, and plated film target is Al, Ni-Cr, Ti, Mo, Si, Al
2o
3, ZrO
2, more than one in AZO, third layer is magnetron sputtering coating, and plated film target is Al, Ni-Cr, Ti, Mo, Si, Al
2o
3, ZrO
2, more than one in AZO.
Also have sandblasting operation before described filming process, the material that sandblasting adopts be quartz or glass microballoon, aluminium oxide, cerium oxide, lanthana, cerium oxide and lanthana mixture, zirconic more than one.Before filming process or also have spraying process, sprayed on material is aluminium or containing the one in the compound of aluminium, electrophoretic paint.
Also have neodymium iron boron rare earth permanent magnet device heating process in described coating process, heating temperature range is at 30-600 DEG C.
Heat treatment step is also had, heat treatment temperature 60-900 DEG C after described filming process.
Described plated film target is Al, Dy-Al, Tb-Al, Dy-Fe, Tb-Fe, Ni-Cr, Ti, Mo, Si, Al
2o
3, ZrO
2, more than one in AZO.
Described neodymium iron boron rare earth permanent magnet device plated film film is Al, Ni-Cr, Al
2o
3in more than one.
Described neodymium iron boron rare earth permanent magnet device plated film film is more than one in Al, Ni-Cr, AZO.
Described neodymium iron boron rare earth permanent magnet device plated film film is more than one in Dy-Al, Al, Ni-Cr.
Described neodymium iron boron rare earth permanent magnet device plated film film is more than one in Al, Ti, Ni-Cr.
Described neodymium iron boron rare earth permanent magnet device plated film film is Al.
Described gas charging system or be filled with a kind of gas or be filled with more than one gas.
The gas that described gas charging system is filled with is more than one in argon gas, nitrogen, oxygen, hydrogen.
The gas that described gas charging system is filled with is argon gas.
Also be filled with oxygen in described coating process, the volume content of oxygen is the 0.1-5% of argon gas.
Described vacuum pump is more than one in oil-sealed rotary pump, Roots vacuum pump, oily diffusion vacuum pump, molecular pump.
Described magnetron sputtering plating condition is, temperature 30 ~ 600 DEG C, and deposition pressure is 0.1 ~ 1Pa under argon gas condition, and power density is 1 ~ 20w/cm2.Discharge voltage 100 ~ the 3000V of linear ion source, ion energy 100 ~ 2000eV, operating air pressure 0.01 ~ 1Pa under argon gas condition.
In described filming process multiple cylinder magnetic control target can adopt work independently, some work, alternation or the mode of operation that simultaneously works.
Rare earth permanent magnet device carries out filming process after machining operation, plated film is divided into 3 layers, ground floor is magnetron sputtering Dy-Al layer, thickness of coating is: 0.02-5 μm, the second layer is magnetron sputtering Al and Ni-Cr mixing coating, Al and Ni-Cr be superposition alternately, and thickness of coating is: 1-10 μm, third layer is magnetron sputtering Al layer, and thickness of coating is: 0.1-5 μm.
Or rare earth permanent magnet device carries out filming process after machining operation, vacuum coating is divided into 3 layers, ground floor is magnetron sputtering Al layer, thickness of coating is: 0.02-5 μm, the second layer is magnetron sputtering Al and Ni-Cr mixing coating, Al and Ni-Cr be superposition alternately, and thickness of coating is: 1-10 μm, third layer is magnetron sputtering Al layer, and thickness of coating is: 0.1-5 μm.
Before filming process, rare earth permanent magnet device will carry out sandblasting operation, sandblasting adopt material be quartz, glass microballoon, aluminium oxide, cerium oxide, lanthana, cerium oxide and lanthana mixture, zirconic more than one.
Before filming process or have spraying process, sprayed on material is aluminium or containing the one in the compound of aluminium, electrophoretic paint.
In filming process or have and control the device heats operation of coating process, temperature range is at 30-600 DEG C.
After filming process or have heat treatment step, heat treatment temperature 60-900 DEG C.
Described heat treatment step carries out under vacuum or protective atmosphere.
Vacuum coating equipment or be arranged in clean room, the cleanliness factor of factory building 10, more than 000 grade.
Metallographic Analysis shows, and described a kind of neodymium iron boron rare earth permanent magnet device to extend internally within the scope of 1mm the content of heavy rare earth main phase grain higher than the average content of heavy rare earth in device main phase grain from device surface, and the heavy rare earth that content is high is distributed in principal phase R
2t
14the periphery of B, forms RH
2t
14b surrounds R
2t
14the new principal phase structure of B, RH
2t
14b phase and R
2t
14b is alternate with Grain-Boundary Phase; Wherein, the rare earth of R representative in Fe-B rare-earth permanent magnet structure in principal phase, T representative element Fe and Co, RH represent the rare earth of content higher than mean value of heavy rare earth in principal phase.
The present invention have found the magnetic control film coating equipment of a kind of neodymium iron boron rare earth permanent magnet device production in enormous quantities and a kind of manufacture method of neodymium iron boron rare earth permanent magnet device, significantly improve the decay resistance of neodymium iron boron rare earth permanent magnet device, make neodymium iron boron rare earth permanent magnet device can be used for the field of the high corrosion-resistant such as offshore wind farm, hybrid vehicle requirement, expand the purposes of Nd-Fe-B rare-earth permanent magnet; Generally; the face coat of Nd-Fe-B rare-earth permanent magnet all can reduce magnetic property; the present invention finds the magnetic property of the neodymium iron boron rare earth permanent magnet device adopting equipment and process of the present invention to produce; especially magnetic energy product and coercive force are improved significantly; for the magnetic property improving Nd-Fe-B rare-earth permanent magnet have found new method; to minimizing rare-earth usage, protect rare natural resources significant.
Accompanying drawing explanation
The present invention is further illustrated below by accompanying drawing:
Fig. 1 be prior art vacuum coating schematic diagram
Fig. 2 is vacuum coating schematic diagram of the present invention
In figure: 1, vacuum chamber; 2, boat is heated; 3, support platform; 4, boat supporting base is heated; 5, charging cylinder; 6, around the shaft; 7, strutting piece; 8, rotating shaft; 9, aluminium wire; 10, roller; 11, thermal resistance protection tube; 12, recess; 13, feed gear wheel; 14, magnetic part; 15, vaccum case; 16, linear anode ion source; 17, inner cylinder magnetic control target; 18, vacuum pump; 19, exterior cylindrical magnetic control target; 20, sputtering sedimentation district; 21, I grade from moving gear; 22, I grade of driven gear; 23, II grade of driving gear; 24, II grade of driven gear; 25, pivoted frame; 26, charging basket; 27, permanent magnet devices; 28, dividing plate; 29, rotating shaft I; 30, rotating shaft II; 31, vacuum-pumping pipeline; 32, heater.
As shown in Figure 2, the present invention is vacuum magnetron sputtering coating film equipment.A horizontal vacuum housing 15, a pivoted frame 25 is supported on framework with rotating shaft I 29, framework is fixed in vaccum case 15, and pivoted frame 25 is circumferentially furnished with multiple (in figure being 8) stainless (steel) wire finish mix basket 26 centered by rotating shaft I 29, and charging basket 26 is built with permanent magnet devices 27.Drive motors (not marking) outside vacuum chamber connects I grade of driving gear 21 by movable sealing power transmission shaft, drives the I grade of driven gear 22 be fixed on pivoted frame 25 to complete the central axis of pivoted frame 25 I 29(vaccum case 15 around the shaft) do sun revolution.Within charging basket 26 revolves round the sun footprint, what be the center of circle with rotating shaft I 29 is circumferentially provided with three 3 cover inner cylinder magnetic control target sources 17 be fixed on vaccum case 15 bonnet.Pivoted frame 25 peripheral circumferential is provided with 1 cover anode linear ion source 16 and 6 in vaccum case 15 and overlaps exterior cylindrical magnetic control target source 19, enclose in pivoted frame 25 and be circumferentially provided with 1 cover anode linear ion source 16, anode ion source and magnetic control target source are arranged on the bonnet of vacuum coating indoor; Vaccum case 15 outer wall has the vacuum-pumping pipeline 31 connecting vacuum pump 18, in vaccum case 15, is provided with dividing plate 28 and heater 32; 1 cover inner cylinder magnetic control target source and 2 cover exterior cylindrical magnetic control target sources are combined into 3 atmosphere independently vacuum magnetic control film coating sputtering sedimentation region 20 by its median septum 28.The II grade of driving gear 23 be fixed on vaccum case 15 drives II 30 rotations around the shaft of II grade of driven gear 24 by the revolution of pivoted frame 25, the two ends of charging basket 26 are provided with rotating shaft and connect with rotating shaft II 30, therefore charging basket 26 can reach revolution and adds rotation object, and permanent magnet devices 27 is stir-fried by target material on uniform deposition in charging basket 26.
Room, filming process initial vacuum vacuumizes and reaches E-4Pa magnitude, backfilled with argon, operating air pressure 0.01 ~ 1Pa, and charging basket 26 revolution adds rotation, starts linear anode ion source, discharge voltage 100 ~ 3000V, Ions Bombardment permanent magnet devices 27, stops bombardment through 5 ~ 10 minutes.Charging basket 26 is insulation, also can meet negative pressure-50 ~-200V.The object of icon bombardment cleaning is in advance the oxide on cleaning permanent magnet devices 27 surface, containing hydrocarbons, make its surface coarsening increase the effect such as surface energy and ion assisted deposition.In heater 32 pairs of charging baskets 26 and charging basket 26, permanent magnet devices 27 is heated to 120 ~ 600 DEG C, plays removing steam, improves film adhesion effect.Filming process is when being heated to 200 DEG C, charging basket 26 revolution add rotation and through high-pressure ion cleaning after, vacuum chamber 15 again vacuumizes and reaches E-4Pa magnitude, backfilled with argon, operating air pressure 0.1 ~ 1Pa, respectively or simultaneously inner circular column type magnetic control target source 17 and sputtering sedimentation district, 28,3, outer cylindrical magnetic control target source works independently respectively or alternation or simultaneously work, target material sputtering sedimentation to permanent magnet devices 27 will be formed the coating of simple substance film and deielectric-coating.
Embodiment
Contrast below by embodiment further illustrates remarkable result of the present invention.
Embodiment
By following manufacture technics:
1, press table one A1 respectively, A2, A3, A4 composition chooses alloy 600Kg melting, in the molten state cooling on alloy casting to the water-cooled rotary copper roller of band is formed alloy sheet, then hydrogen fragmentation is carried out, batch mixing is carried out after hydrogen fragmentation, the laggard row airflow milling of batch mixing, afterwards under nitrogen protection with delivering to nitrogen protection magnetic field orientating press-molding after batch mixer batch mixing, alignment magnetic field 2.0T, magnetic patch size 62 × 52 × 42mm, direction of orientation is 42 dimensional directions, encapsulate in guard box after shaping, then take out and carry out isostatic pressed, hydrostatic pressure 200MPa, send into agglomerating plant sintering and timeliness afterwards.
2, machining is carried out after timeliness, be processed into square piece 40 × 20 × 5mm size, workpiece selectivity carried out chamfering, sandblasting, aluminium-plated, electrophoresis, spraying, carry out vacuum coating afterwards, ground floor is magnetron sputtering coating, and thickness of coating is: 0.02-5 μm, and the second layer is magnetron sputtering coating, thickness of coating is: 1-10 μm, third layer is magnetron sputtering coating, and thickness of coating is: 0.1-5 μm, and the measurement result of material, magnetic property and decay resistance that each layer is selected lists table two in.
The composition of the RE permanent magnetic alloy of table one, prior art
| Numbering | Composition |
| A1 | Ｎd 30Dy 1Fe 67.9Ｂ 0.9A l0.2 |
| A2 | Ｎd 30Dy 1Fe 67.5Co 1.2Cu 0.1Ｂ 0.9Al 0.1 |
| A3 | (Ｐr 0.2Ｎd 0.8) 25Dy 5Fe 67.4Co 1.2Cu 0.3Ｂ 0.9Al 0.2 |
| A4 | (Ｐr 0.2Ｎd 0.8) 25Dy 5Tb 1Fe 65Co 2.4Cu 0.3Ｂ 0.9Al 0.2Ga 0.1Zr 0.1 |
The measurement result of table two, coating material of the present invention, magnetic property and decay resistance
Comparative example
Press table one A1 respectively, A2, A3, A4 composition chooses alloy 600Kg melting, in the molten state cooling on alloy casting to the chill roll of the water-cooled rotation of band is formed alloy sheet, then the involutory gold plaque of vacuum hydrogen crushing furnace is used to carry out coarse crushing, the broken laggard row airflow milling of hydrogen, under nitrogen protection with delivering to nitrogen protection magnetic field orientating press-molding after batch mixer batch mixing, alignment magnetic field 2.0T, magnetic patch size 62 × 52 × 42mm, direction of orientation is 42 dimensional directions, encapsulate in guard box after shaping, then take out and carry out isostatic pressed, hydrostatic pressure 200MPa, send into vacuum sintering furnace sintering and timeliness afterwards, carry out machining again, be processed into square piece 40 × 20 × 5mm size, workpiece selectivity is carried out chamfering or sandblasting, carry out electroplated Ni-Cu-Ni afterwards, the measurement result of magnetic property and decay resistance lists table three in.
The measurement result of table three, magnetic property and decay resistance
Note: 1, corrosion resistance (PCT test)
Experiment condition: sample 10X10X10mm, 2 standard atmospheric pressures, 120 DEG C, 100% humidity, 48 hours, weightless <5mg/cm
2.
2, salt mist test:
Experiment condition: 5%NaCl solution, tests for 25 DEG C >=48 hours, and surface is change not.
In embodiment, sandblasting operation to be had: because rare earth permanent magnet device is in the course of processing before vacuum coating operation, a certain amount of grease and dirty all can be there is on its surface, and the decay resistance of these dirts to technique for vacuum coating stability and coated product has a great impact, therefore configure the basic guarantee that rational cleaning equipment and technique are rare earth permanent magnet component vacuum coating quality performances, only have rational cleaning guarantee coating to have good adhesive force.Sandblasting operation adopt material be quartz, glass microballoon, aluminium oxide, cerium oxide, lanthana, cerium oxide and lanthana mixture, zirconic more than one.Before vacuum coating operation or also have spraying process, sprayed on material is aluminium or containing the one in the compound of aluminium, electrophoretic paint.
In embodiment, in filming process mesohigh Ion Cleaning operation: vacuum chamber higher than the E-4Pa order of magnitude, applying argon gas, operating air pressure 0.01 ~ 1Pa, charging basket revolution adds rotation, starting cathode linear ion source, discharge voltage 100 ~ 3000V, Ions Bombardment rare earth permanent magnet device 5 ~ 10 minutes.Charging basket is insulation, also can meet negative pressure-50 ~-200V.
In embodiment, different coating process configuration causes the change such as throughput rate, ion energy, has material impact to coated product performance.Coating process is in vacuum chamber under 200 DEG C of ambient temperatures, vacuum chamber higher than the E-4Pa order of magnitude, backfilled with argon, operating air pressure 3E-1Pa, charging basket revolution adds rotation, and magnetron sputtering individually works or alternation or simultaneously work; Magnetron sputtering and Ions Bombardment individually work or alternation.
In embodiment, coating process is feeded: the structure of charging basket has considerable influence to coated product outward appearance and coating quality, should avoid occurring surface tear and other physical damnifications.Charging basket is the cylinder type made of stainless (steel) wire or polygonal column structure, and centre has dividing plate to form multiple insulating space, and one or a few permanent magnet devices is placed in each space.
In embodiment, heat treatment step will be had after vacuum coating operation, temperature 60-900 DEG C.
By relatively further illustrating of embodiment and comparative example, adopting technology of the present invention to significantly improve decay resistance and the magnetic property of magnet, is the technology and equipment technology having very much development.
Claims (11)
1. the manufacture method of a neodymium iron boron rare earth permanent magnet device, it is characterized in that: first carry out alloy melting, in the molten state cooling on alloy casting to the water-cooled rotary copper roller of band is formed alloy sheet, then hydrogen fragmentation is carried out, batch mixing is carried out after hydrogen fragmentation, the laggard row airflow milling of batch mixing, afterwards under nitrogen protection with delivering to nitrogen protection magnetic field orientating press-molding after batch mixer batch mixing, encapsulate in guard box after shaping, then take out and carry out isostatic pressed, feeding agglomerating plant sintering and timeliness make Nd-Fe-B rare-earth permanent magnet blank afterwards, carry out machining afterwards and make Fe-B rare-earth permanent magnet, carry out magnetron sputtering membrane process in vacuum coating indoor afterwards and make neodymium iron boron rare earth permanent magnet device, plated film is divided into 3 layers, ground floor is magnetron sputtering coating, thickness of coating is: 0.02-2 μm, the second layer is the mixing coating of more than one targets of magnetron sputtering, thickness of coating is: 1-20 μm, third layer is magnetron sputtering coating, thickness of coating is: 0.1-5 μm,
Described plated film ground floor is magnetron sputtering Dy-Al layer, and the second layer is magnetron sputtering Al and Ni-Cr mixing coating, Al and Ni-Cr be superposition alternately, and third layer is magnetron sputtering Al layer;
Heat treatment step is also had, heat treatment temperature 60-900 DEG C after described filming process.
2. the manufacture method of a kind of neodymium iron boron rare earth permanent magnet device according to claim 1, it is characterized in that: before described filming process, also have sandblasting operation, sandblasting adopt material be quartz or glass microballoon, aluminium oxide, cerium oxide, lanthana, cerium oxide and lanthana mixture, zirconic more than one, also have spraying process before filming process, sprayed on material is aluminium or containing the one in the compound of aluminium or electrophoretic paint.
3. the manufacture method of a kind of neodymium iron boron rare earth permanent magnet device according to claim 1, is characterized in that: also have neodymium iron boron rare earth permanent magnet device heating process in described coating process, heating temperature range is at 30-600 DEG C.
4. the manufacture method of a kind of neodymium iron boron rare earth permanent magnet device according to claim 1, it is characterized in that: described vacuum coating indoor are also provided with anode-layer-linear ion source, described magnetron sputtering plating condition is, temperature 30 ~ 600 DEG C, deposition pressure is 0.1 ~ 1Pa under argon gas condition, power density is 1 ~ 20w/cm2, discharge voltage 100 ~ the 3000V of anode-layer-linear ion source, ion energy 100 ~ 2000eV, operating air pressure 0.01 ~ 1Pa under argon gas condition, the independent plated film of different target more than one cylinder negative electrode magnetic control target is adopted in described filming process, alternate plating or simultaneously plated film.
5. the manufacture method of a kind of neodymium iron boron rare earth permanent magnet device according to claim 1, is characterized in that: be also filled with oxygen in described magnetron sputtering membrane process, and the volume content of oxygen is the 0.1-5% of argon gas.
6. the manufacture method of a kind of neodymium iron boron rare earth permanent magnet device according to claim 1, it is characterized in that: described a kind of neodymium iron boron rare earth permanent magnet device to extend internally within the scope of 1mm the content of heavy rare earth main phase grain higher than the average content of heavy rare earth in device main phase grain from device surface, and the heavy rare earth that content is high is distributed in principal phase R
2t
14the periphery of B, forms RH
2t
14b surrounds R
2t
14the new principal phase structure of B, RH
2t
14b phase and R
2t
14b is alternate with Grain-Boundary Phase;
Wherein, the rare earth of R representative in Fe-B rare-earth permanent magnet structure in principal phase, T representative element Fe and Co, RH represent the rare earth of content higher than mean value of heavy rare earth in principal phase.
7. the magnetic control film coating equipment of a neodymium iron boron rare earth permanent magnet device, use in the manufacture method of neodymium iron boron rare earth permanent magnet device as claimed in claim 1, it is characterized in that: this filming equipment comprises vacuum film coating chamber, cylinder negative electrode magnetic control target, anode-layer-linear ion source, pivoted frame and charging basket; Described vacuum film coating chamber is made up of horizontal vacuum housing, Qianmen and bonnet, Qianmen and vaccum case pass through rubber seal rings for seal, bonnet or be welded on vaccum case or be connected on vaccum case by connector, the transmission device of pivoted frame is arranged on bonnet, and the motor transmission shaft outside vacuum chamber is sent to vacuum coating indoor by dynamic sealing device; Pivoted frame design is indoor in vacuum coating, and be supported on framework, frame installation is on vaccum case; The axis of pivoted frame and the axis being parallel of vaccum case, not only charging basket two ends have rotating shaft to be arranged on pivoted frame, the axis of rotating shaft and the axis being parallel of pivoted frame, and pivoted frame revolves round the sun around the axis of vaccum case, and charging basket revolves round the sun but also rotation with pivoted frame; Described cylinder magnetic control target is arranged on the bonnet of vacuum coating indoor, its axis and turret shaft line parallel.
8. the magnetic control film coating equipment of a kind of neodymium iron boron rare earth permanent magnet device according to claim 7, it is characterized in that: this filming equipment also comprises anode-layer-linear ion source, described anode-layer-linear ion source is arranged on the bonnet of vacuum coating indoor, its axis and turret shaft line parallel.
9. the magnetic control film coating equipment of a kind of neodymium iron boron rare earth permanent magnet device according to claim 7, it is characterized in that: in described vacuum coating indoor, more than one cylinder negative electrode magnetic control target is installed, described cylinder negative electrode magnetic control target is arranged on the inside and outside of pivoted frame respectively, the quantity being arranged on the cylinder negative electrode magnetic control target of described pivoted frame inside is more than one, is arranged on the quantity more than two of the cylinder negative electrode magnetic control target of pivoted frame outside; Magnetic control target or be single target structure or for twin target structure, is arranged on the bonnet of vacuum coating indoor.
10. the magnetic control film coating equipment of a kind of neodymium iron boron rare earth permanent magnet device according to claim 7, it is characterized in that: described cylinder negative electrode magnetic control target is built with the magnet ring of multiple axial charging, magnetic guiding loop is had between magnet ring, magnet ring moves relative to cylinder negative electrode magnetic control target axial reciprocating, and described magnet ring is manufactured by Nd-Fe-B rare-earth permanent magnet.
The magnetic control film coating equipment of 11. a kind of neodymium iron boron rare earth permanent magnet device according to claim 7, it is characterized in that: described cylinder negative electrode magnetic control target is built with the magnetic stripe of many radial magnetizings, magnetic stripe circumferentially distributes in cylinder negative electrode magnetic control target, interval is had between magnetic stripe, the quantity of magnetic stripe is more than 3, magnetic stripe is relative to cylinder negative electrode magnetic control target sleeve pipe coaxial rotation, and described magnetic stripe is manufactured by Nd-Fe-B rare-earth permanent magnet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410107557.5A CN103839671B (en) | 2014-03-22 | 2014-03-22 | A kind of manufacture method of neodymium iron boron rare earth permanent magnet device |
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| CN106876072A (en) * | 2015-12-11 | 2017-06-20 | 中国科学院宁波材料技术与工程研究所 | The method for improving neodymium-iron-boron magnetic material magnetic property |
| CN105755441B (en) * | 2016-04-20 | 2019-01-11 | 中国科学院宁波材料技术与工程研究所 | A kind of method that magnetron sputtering method expands infiltration heavy rare earth raising coercivity of sintered ndfeb |
| CN106710767B (en) * | 2016-12-09 | 2018-08-17 | 宁波大榭开发区银鑫磁业有限公司 | The corrosion-resistant more coating neodymium iron borons of one kind and preparation process |
| CN111292951B (en) * | 2020-02-28 | 2022-03-22 | 安徽大地熊新材料股份有限公司 | Method for improving coercive force of sintered neodymium-iron-boron magnet |
| CN111986913B (en) * | 2020-09-23 | 2022-03-11 | 赣州富尔特电子股份有限公司 | Method for improving performance of sintered neodymium-iron-boron magnet |
| CN112281129B (en) * | 2020-10-19 | 2023-03-10 | 南昌航空大学 | Preparation process of Ni-Cr corrosion-resistant alloy coating on surface of sintered NdFeB magnet |
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| US5314756A (en) * | 1991-11-27 | 1994-05-24 | Hitachi Metals, Ltd. | Permanent magnet of rare-earth-element/transition-metal system having improved corrosion resistance and manufacturing method thereof |
| JPH11238620A (en) * | 1998-02-23 | 1999-08-31 | Seiko Epson Corp | Permanent magnet and its manufacture |
| CN101373650B (en) * | 2007-08-23 | 2011-11-09 | 北京中科三环高技术股份有限公司 | Surface pretreating method of dry method spray sand type neodymium iron boron permanent magnetic material |
| JP4983619B2 (en) * | 2008-01-23 | 2012-07-25 | Ｔｄｋ株式会社 | permanent magnet |
| CN102041506A (en) * | 2009-10-13 | 2011-05-04 | 北京中科三环高技术股份有限公司 | Surface treatment method of permanent magnet material |
| CN103290382B (en) * | 2013-05-15 | 2015-09-09 | 宁波韵升股份有限公司 | The planetary work rest of a kind of vacuum plating unit |
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