CN103839671A - Manufacturing method for neodymium iron boron rare-earth permanent magnet components - Google Patents
Manufacturing method for neodymium iron boron rare-earth permanent magnet components Download PDFInfo
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- CN103839671A CN103839671A CN201410107557.5A CN201410107557A CN103839671A CN 103839671 A CN103839671 A CN 103839671A CN 201410107557 A CN201410107557 A CN 201410107557A CN 103839671 A CN103839671 A CN 103839671A
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Abstract
The invention discloses a manufacturing method for neodymium iron boron rare-earth permanent magnet components. Firstly, neodymium iron boron rare-earth permanent magnet blanks are manufactured, then neodymium iron boron rare-earth permanent magnets are manufactured through machining, next, the neodymium iron boron rare-earth permanent magnet components are manufactured through a film coating process, and the film coating is performed in a three-layer mode. The first layer is a magnetron sputtering coating layer, the thickness of the coating layer is 0.02 micrometer-2 micrometers, the second layer is a mixed coating layer that one or more kinds of target materials are coated through magnetron sputtering, the thickness of the mixed coating layer is 1 micrometer-20 micrometers, the third layer is a magnetron sputtering coating layer, and the thickness of the coating layer is 0.1 micrometer-5 micrometers. Magnetron sputtering film coating is adopted as the surface treatment process of the rare-earth permanent magnet components, so that the anti-corrosion capacity of the rare-earth permanent magnet components is improved, and meanwhile the magnetic performance of the rare-earth permanent magnet components is improved.
Description
Technical field
The invention belongs to permanent magnet devices field, particularly relate to a kind of manufacture method of Nd-Fe-B rare-earth permanent magnet device.
Background technology
Nd-Fe-B rare earth permanent magnetic material, is more and more applied with its good magnetic property, is widely used in medical Magnetic resonance imaging, computer hard disc driver, sound equipment, mobile phone etc.; Along with energy-conservation and requirement 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, field of wind power generation application.
The process of surface treatment of the rare earth permanent magnet device of prior art mainly contains electroplated Ni-Cu-Ni, electroplates the technology such as Zn, electrophoresis, spraying, also has and adopts vacuum aluminum-coated method, as Chinese patent ZL96192129.3, has disclosed the method for Vacuum Deposition Ti and AlN; Another Chinese patent ZL01111757.5 has disclosed and has adopted that vacuum evaporation is zinc-plated, the method for aluminium, tin, magnesium.
Prior art as shown in Figure 1, has two strutting pieces 7 to be arranged side by side in the inner Shang of vacuum chamber 1 district, can the rotating shaft 6 on a horizontal axis of rotation rotate.Six cylinders 5 that formed by stainless steel cloth pack magnetic part 14 into, by rotating shaft 8 in the outer circumference direction of the rotating shaft 6 of strutting piece 7 and be supported for an annular, for 6 rotations around the shaft.Be arranged on a heating boat supporting base 4 rising as multiple heating boats 2 of the evaporation section of the material aluminium wire 9 for evaporating in the support platform 3 of process chamber 1 inferior segment.Aluminium wire 9 is fixed and is wrapped on a feed roller 10 under support platform 3.The front end of aluminium wire 9 is reached on heating boat 2 by thermal resistance protection tube 11 guiding of an inner surface towards heating boat 2; 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 consistently aluminium wire be fed in heating boat 2 by feeding aluminium wire 9 like this, heating evaporation deposits to and on the magnetic part 14 in the barrel 5 of rotation, completes its surface and aluminize.
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, is difficult for being installed, and produces trouble; Prior art also has employing multi-arc ion plating film, has bulky grain during due to 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 has expected employing multi-arc ion coating and magnetron sputtering composite film coating to prior art, but does not all solve high efficiency, production technology low-costly and in high volume, 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 biological environment is had a strong impact on.Carry out in a vacuum because of production process of the present invention, do not use environmental pollution material, can not pollute to biological environment, also eliminate " battery " in electroplating technology process simultaneously and act on the impact of the reduction on magnetic property.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 have made up the deficiencies in the prior art; Adopt in addition the Nd-Fe-B rare-earth permanent magnet device of device fabrication of the present invention not only to improve the resistance to corrosion of rare earth permanent magnet device, also improve the magnetic property of rare earth permanent magnet device, obviously improve magnetic energy product and the coercive force of rare earth permanent magnet device, save rare rare earth resources, especially saved 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 Nd-Fe-B rare-earth permanent magnet device, is achieved through the following technical solutions and improves the magnetic property of rare earth permanent magnet device and improve resistance to corrosion:
A magnetic control film coating equipment for Nd-Fe-B 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 it is indoor that the motor transmission shaft outside vacuum chamber is sent to vacuum coating 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; The axis of pivoted frame is parallel with the axis of horizontal vacuum housing, and netted charging basket two ends have rotating shaft to be arranged on pivoted frame, and the axis of rotating shaft is parallel with the axis of pivoted frame, and pivoted frame is around the axis revolution of vaccum case, and netted charging basket revolves round the sun and rotation with pivoted frame.
Described cylinder magnetic control target is arranged on the indoor bonnet of vacuum coating, and power supply, cooling water and transmission device are introduced by outside, axis and turret shaft line parallel.
More than one cylinder magnetic control target is installed vacuum coating is indoor, described cylinder magnetic control target is arranged on respectively the inside and outside of pivoted frame.
The quantity that is arranged on the cylinder magnetic control target of pivoted frame inside is more than one, is arranged on the quantity of cylinder magnetic control target of pivoted frame outside more than two.
Be arranged on the quantity n of the cylinder magnetic control target of pivoted frame inside, be arranged on quantity 2n of cylinder magnetic control target of pivoted frame outside, n is greater than 3 integer.
The quantity that is arranged on the cylinder magnetic control target of pivoted frame inside is 3, and the quantity that is arranged on the cylinder magnetic control target of pivoted frame outside is 6.
The magnet ring that multiple axial chargings are housed in described cylinder magnetic control target, has magnetic guiding loop between magnet ring, magnet ring moves with respect 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 along circle distribution, has interval in cylinder magnetic control target between magnetic stripe, and the quantity of magnetic stripe is more than 3 or 3, and magnetic stripe is with respect 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 indoor bonnet of vacuum coating, is distributed in pivoted frame or the periphery of pivoted frame.
A kind of manufacture method of Nd-Fe-B rare-earth permanent magnet device, first carry out alloy melting, under molten condition by alloy casting to being with cooling formation alloy sheet on water-cooled rotation copper roller, then carry out hydrogen fragmentation, after hydrogen fragmentation, carry out batch mixing, 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, after shaping, in guard box, encapsulate, then take out and wait static pressure, send into afterwards agglomerating plant sintering and timeliness and make Nd-Fe-B rare-earth permanent magnet blank, carry out afterwards machining and make Fe-B rare-earth permanent magnet, carry out afterwards filming process and make Nd-Fe-B 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 μ m, the second layer is the mixing coating of more than one targets of magnetron sputtering, thickness of coating is: 1-20 μ m, the 3rd layer is magnetron sputtering coating, thickness of coating is: 0.1-5 μ m.
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, and Al and Ni-Cr be stack alternately, and the 3rd 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, the 3rd layer is magnetron sputtering coating, plated film target is Al, Ni-Cr, Ti, Mo, Si, Al
2o
3, ZrO
2, more than one in AZO.
Before described filming process, also have sandblast operation, the material that sandblast adopts be quartz or glass microballoon, aluminium oxide, cerium oxide, lanthana, cerium oxide and lanthana mixture, zirconic more than one.Before filming process or to also have spraying process, sprayed on material be aluminium or containing the one in compound, the electrophoretic paint of aluminium.
In described coating process, also have Nd-Fe-B rare-earth permanent magnet device heats operation, heating-up temperature scope is at 30-600 ℃.
After described filming process, also have heat treatment step, heat treatment temperature 60-900 ℃.
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 Nd-Fe-B rare-earth permanent magnet device plated film film is Al, Ni-Cr, Al
2o
3in more than one.
Described Nd-Fe-B rare-earth permanent magnet device plated film film is more than one in Al, Ni-Cr, AZO.
Described Nd-Fe-B rare-earth permanent magnet device plated film film is more than one in Dy-Al, Al, Ni-Cr.
Described Nd-Fe-B rare-earth permanent magnet device plated film film is more than one in Al, Ti, Ni-Cr.
Described Nd-Fe-B 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.
In described coating process, be also filled with oxygen, the 0.1-5% that the volume content of oxygen is 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, 30 ~ 600 ℃ of temperature, and deposition pressure is 0.1 ~ 1Pa under argon gas condition, 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 targets can adopt work independently, some work, alternation or the mode of operation of simultaneously working.
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 μ m, the second layer is magnetron sputtering Al and Ni-Cr mixing coating, and Al and Ni-Cr be stack alternately, and thickness of coating is: 1-10 μ m, the 3rd layer is magnetron sputtering Al layer, and thickness of coating is: 0.1-5 μ m.
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 μ m, the second layer is magnetron sputtering Al and Ni-Cr mixing coating, and Al and Ni-Cr be stack alternately, and thickness of coating is: 1-10 μ m, the 3rd layer is magnetron sputtering Al layer, and thickness of coating is: 0.1-5 μ m.
Rare earth permanent magnet device will carry out sandblast operation before filming process, the material that sandblast adopts be quartz, glass microballoon, aluminium oxide, cerium oxide, lanthana, cerium oxide and lanthana mixture, zirconic more than one.
Before filming process or to have spraying process, sprayed on material be aluminium or containing the one in compound, the electrophoretic paint of aluminium.
In filming process or have the device heats operation of coating process of control, temperature range is at 30-600 ℃.
After filming process or have a heat treatment step, heat treatment temperature 60-900 ℃.
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 is more than 10,000 grades.
Metallographic Analysis shows, described a kind of Nd-Fe-B rare-earth permanent magnet device extends internally from device surface, and main phase grain, the content of heavy rare earth is higher than the average content of heavy rare earth in device main phase grain within the scope of 1mm, 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, R representative rare earth in principal phase in Fe-B rare-earth permanent magnet structure, T representative element Fe and Co, RH represents that the content of heavy rare earth in principal phase is higher than the rare earth of mean value.
The present invention has found a kind of magnetic control film coating equipment of Nd-Fe-B rare-earth permanent magnet device production in enormous quantities and a kind of manufacture method of Nd-Fe-B rare-earth permanent magnet device, obviously improve the decay resistance of Nd-Fe-B rare-earth permanent magnet device, make Nd-Fe-B rare-earth permanent magnet device can be used for the field of the high corrosion-resistant such as offshore wind farm, hybrid vehicle requirement, expanded 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 Nd-Fe-B rare-earth permanent magnet device that adopts equipment and process production of the present invention; especially magnetic energy product and coercive force are improved significantly; for the magnetic property that improves Nd-Fe-B rare-earth permanent magnet has found new method; to reducing rare earth consumption, protect rare natural resources significant.
Accompanying drawing explanation
Further illustrate the present invention 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, heating boat; 3, support platform; 4, heating boat supporting base; 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 level is from moving gear; 22, I level driven gear; 23, II level driving gear; 24, II level 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, is furnished with multiple (being 8 in figure) stainless (steel) wire finish mix basket 26 on the circumference of pivoted frame 25 centered by rotating shaft I 29, and permanent magnet devices 27 is housed in charging basket 26.Drive motors (not marking) outside vacuum chamber connects I level driving gear 21 by movable sealing power transmission shaft, drives the I level driven gear 22 being fixed on pivoted frame 25 to complete pivoted frame 25 central axis of I 29(vaccum case 15 around the shaft) do sun revolution.Within charging basket 26 revolves round the sun track scope, the circumference take rotating shaft I 29 as the center of circle is provided with three and is fixed on the cover of 3 on vaccum case 15 bonnets inner cylinder magnetic control target source 17.In interior pivoted frame 25 peripheral circumferential of vaccum case 15, be provided with 1 cover anode linear ion source 16 and 6 cover exterior cylindrical magnetic control target sources 19, in pivoted frame 25, enclose on circumference and be provided with 1 cover anode linear ion source 16, anode ion source and magnetic control target source are arranged on the indoor bonnet of vacuum coating; On vaccum case 15 outer walls, there is the vacuum-pumping pipeline 31 that connects vacuum pump 18, in vaccum case 15, be 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 independently vacuum magnetic control film coating sputtering sedimentation region 20 of 3 atmosphere by its median septum 28.The II level driving gear 23 being fixed on vaccum case 15 drives 24 II 30 rotations around the shaft of II level driven gear 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 add rotation object, make permanent magnet devices 27 in charging basket 26, stir-fry by uniform deposition on target material.
Chamber, filming process initial vacuum vacuumizes and reaches E-4Pa magnitude, recharges argon gas, operating air pressure 0.01 ~ 1Pa, and charging basket 26 revolution add rotation, start linear anode ion source, discharge voltage 100 ~ 3000V, Ions Bombardment permanent magnet devices 27, stopped bombarding through 5 ~ 10 minutes.Charging basket 26 insulate, and also can meet negative pressure-50 ~-200V.The object of icon bombardment cleaning in advance, be clean the oxide on permanent magnet devices 27 surfaces, containing hydrocarbons, make its surface coarsening increase surface can and the effect such as ion assisted deposition.Heater 32 is heated to 120 ~ 600 ℃ to charging basket 26 and the interior permanent magnet devices 27 of charging basket 26, plays and removes steam, improves film adhesion effect.Filming process is in the time being heated to 200 ℃, charging basket 26 revolution adds rotation and after high-pressure ion cleans, vacuum chamber 15 again vacuumizes and reaches E-4Pa magnitude, recharge argon gas, 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 circle column type magnetic control target source works independently respectively or alternation or simultaneously work, by target material sputtering sedimentation to the coating that forms simple substance film and deielectric-coating on permanent magnet devices 27.
Embodiment
Further illustrate remarkable result of the present invention below by the contrast of embodiment.
Embodiment
Press following technique manufacture:
1, press respectively table one A1, A2, A3, A4 composition is chosen alloy 600Kg melting, under molten condition by alloy casting to being with cooling formation alloy sheet on water-cooled rotation copper roller, then carry out hydrogen fragmentation, after hydrogen fragmentation, carry out batch mixing, 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, after shaping, in guard box, encapsulate, then take out and wait static pressure, hydrostatic pressure 200MPa, send into afterwards agglomerating plant sintering and timeliness.
2, after timeliness, carry out machining, be processed into square piece 40 × 20 × 5 mm sizes, workpiece selectivity is carried out to chamfering, sandblast, aluminium-plated, electrophoresis, spraying, carried out vacuum coating afterwards, ground floor is magnetron sputtering coating, and thickness of coating is: 0.02-5 μ m, and the second layer is magnetron sputtering coating, thickness of coating is: 1-10 μ m, the 3rd layer is magnetron sputtering coating, and thickness of coating is: 0.1-5 μ m, the measurement result of each layer of material of selecting, magnetic property and decay resistance is listed 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 respectively table one A1, A2, A3, A4 composition is chosen alloy 600Kg melting, under molten condition by alloy casting to cooling formation alloy sheet on the chill roll with water-cooled rotation, then use the involutory gold plaque of vacuum hydrogen crushing furnace 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, after shaping, in guard box, encapsulate, then take out and wait static pressure, hydrostatic pressure 200MPa, send into afterwards vacuum sintering furnace sintering and timeliness, carry out again machining, be processed into square piece 40 × 20 × 5 mm sizes, workpiece selectivity is carried out to chamfering or sandblast, carry out afterwards electroplated Ni-Cu-Ni, the measurement result of magnetic property and decay resistance is listed 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 ℃, 100% humidity, 48 hours, weightless <5mg/cm
2.
2, salt mist test:
Experiment condition: 5%NaCl solution, within 25 ℃ >=48 hours, to test, surface does not change.
In embodiment, before vacuum coating operation, to there is sandblast operation: because rare earth permanent magnet device is in the course of processing, all can there is a certain amount of grease and dirty on its surface, and these dirts have a great impact the decay resistance of technique for vacuum coating stability and coated product, therefore configuring rational cleaning equipment and technique is the basic guarantee of rare earth permanent magnet component vacuum coating quality performance, only has rational cleaning guarantee coating to have good adhesive force.Sandblast 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 to also have spraying process, sprayed on material be aluminium or containing the one in compound, the electrophoretic paint of aluminium.
In embodiment, in filming process mesohigh Ion Cleaning operation: vacuum chamber vacuumizes the order of magnitude higher than E-4Pa, 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 insulate, and also can meet negative pressure-50 ~-200V.
In embodiment, different coating process configurations cause the variation such as throughput rate, ion energy, and coated product performance is had to material impact.Coating process is in vacuum chamber under 200 ℃ of ambient temperatures, and vacuum chamber vacuumizes the order of magnitude higher than E-4Pa, recharges argon gas, operating air pressure 3E-1Pa, and charging basket revolution adds rotation, and magnetron sputtering works independently respectively or alternation or simultaneously work; Magnetron sputtering and Ions Bombardment work independently respectively or alternation.
In embodiment, coating process charging: 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 cylinder type or the polygon column structure that stainless (steel) wire is made, and centre has dividing plate to form multiple insulating spaces, and one or a few permanent magnet devices is placed in each space.
In embodiment, after vacuum coating operation, to there be heat treatment step, temperature 60-900 ℃.
By relatively further illustrating of embodiment and comparative example, adopt technology of the present invention obviously to improve decay resistance and the magnetic property of magnet, be the technology and equipment technology that has very much development.
Claims (14)
1. the manufacture method of a Nd-Fe-B rare-earth permanent magnet device, it is characterized in that: first carry out alloy melting, under molten condition by alloy casting to being with cooling formation alloy sheet on water-cooled rotation copper roller, then carry out hydrogen fragmentation, after hydrogen fragmentation, carry out batch mixing, 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, after shaping, in guard box, encapsulate, then take out and wait static pressure, send into afterwards agglomerating plant sintering and timeliness and make Nd-Fe-B rare-earth permanent magnet blank, carry out afterwards machining and make Fe-B rare-earth permanent magnet, make Nd-Fe-B rare-earth permanent magnet device at the indoor magnetron sputtering membrane process that carries out of vacuum coating afterwards, plated film is divided into 3 layers, ground floor is magnetron sputtering coating, thickness of coating is: 0.02-2 μ m, the second layer is the mixing coating of more than one targets of magnetron sputtering, thickness of coating is: 1-20 μ m, the 3rd layer is magnetron sputtering coating, thickness of coating is: 0.1-5 μ m.
2. the manufacture method of a kind of Nd-Fe-B rare-earth permanent magnet device according to claim 1, it is characterized in that: described plated film is divided into 3 layers, ground floor is magnetron sputtering Dy-Al layer, the second layer is magnetron sputtering Al and Ni-Cr mixing coating, Al and Ni-Cr be stack alternately, and the 3rd layer is magnetron sputtering Al layer.
3. the manufacture method of a kind of Nd-Fe-B rare-earth permanent magnet device according to claim 1, it is characterized in that: described plated film is divided into 3 layers, ground floor is magnetron sputtering coating, plated film target is more than one in Al, Dy-Al, Tb-Al, Dy-Fe, Tb-Fe, 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, the 3rd layer is magnetron sputtering coating, plated film target is Al, Ni-Cr, Ti, Mo, Si, Al
2o
3, ZrO
2, more than one in AZO.
4. the manufacture method of a kind of Nd-Fe-B rare-earth permanent magnet device according to claim 1, it is characterized in that: before described filming process, also have sandblast operation, sandblast adopt material be quartz or glass microballoon, aluminium oxide, cerium oxide, lanthana, cerium oxide and lanthana mixture, zirconic more than one, before filming process or to also have spraying process, sprayed on material be aluminium or containing the one in compound, the electrophoretic paint of aluminium.
5. the manufacture method of a kind of Nd-Fe-B rare-earth permanent magnet device according to claim 1, is characterized in that: in described coating process, also have Nd-Fe-B rare-earth permanent magnet device heats operation, heating-up temperature scope is at 30-600 ℃.
6. the manufacture method of a kind of Nd-Fe-B rare-earth permanent magnet device according to claim 1, is characterized in that: after described filming process, also have heat treatment step, heat treatment temperature 60-900 ℃.
7. the manufacture method of a kind of Nd-Fe-B rare-earth permanent magnet device according to claim 1, it is characterized in that: the indoor anode-layer-linear ion source that is also provided with of described vacuum coating, described magnetron sputtering plating condition is, 30 ~ 600 ℃ of temperature, 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, in described filming process, adopt the independent plated film of the more than one cylinder negative electrode of different targets magnetic control target, alternate plating or simultaneously plated film.
8. the manufacture method of a kind of Nd-Fe-B rare-earth permanent magnet device according to claim 1, is characterized in that: in described magnetron sputtering membrane process, be also filled with oxygen, the 0.1-5% that the volume content of oxygen is argon gas.
9. the manufacture method of a kind of Nd-Fe-B rare-earth permanent magnet device according to claim 1, it is characterized in that: described a kind of Nd-Fe-B rare-earth permanent magnet device extends internally from device surface, and main phase grain, the content of heavy rare earth is higher than the average content of heavy rare earth in device main phase grain within the scope of 1mm, 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.
10. a magnetic control film coating equipment for Nd-Fe-B rare-earth permanent magnet device as claimed in claim 1, 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 by connector connects, the transmission device of pivoted frame is arranged on bonnet, and it is indoor that the motor transmission shaft outside vacuum chamber is sent to vacuum coating by dynamic sealing device; Pivoted frame design is indoor in vacuum coating, is supported on framework, and frame installation is on vaccum case; The axis of pivoted frame is parallel with the axis of vaccum case, and charging basket two ends have rotating shaft to be arranged on pivoted frame, and the axis of rotating shaft is parallel with the axis of pivoted frame, and pivoted frame is around the axis revolution of vaccum case, and charging basket revolves round the sun and rotation with pivoted frame; Described cylinder magnetic control target is arranged on the indoor bonnet of vacuum coating, its axis and turret shaft line parallel.
The magnetic control film coating equipment of 11. a kind of Nd-Fe-B rare-earth permanent magnet devices according to claim 10, 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 indoor bonnet of vacuum coating, its axis and turret shaft line parallel.
The magnetic control film coating equipment of 12. a kind of Nd-Fe-B rare-earth permanent magnet devices according to claim 10, it is characterized in that: more than one cylinder negative electrode magnetic control target is installed described vacuum coating is indoor, described cylinder negative electrode magnetic control target is arranged on respectively the inside and outside of pivoted frame, the quantity that is arranged on the cylinder negative electrode magnetic control target of described pivoted frame inside is more than one, is arranged on the quantity of cylinder negative electrode magnetic control target of pivoted frame outside more than two; Magnetic control target or be single target structure or for twin target structure, is arranged on the indoor bonnet of vacuum coating.
The magnetic control film coating equipment of 13. a kind of Nd-Fe-B rare-earth permanent magnet devices according to claim 10, it is characterized in that: the magnet ring that multiple axial chargings are housed in described cylinder negative electrode magnetic control target, between magnet ring, there is magnetic guiding loop, magnet ring moves with respect 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 14. a kind of Nd-Fe-B rare-earth permanent magnet devices according to claim 10, it is characterized in that: in described cylinder negative electrode magnetic control target or the magnetic stripe of many radial magnetizings is housed, magnetic stripe in cylinder negative electrode magnetic control target along circle distribution, between magnetic stripe, there is interval, the quantity of magnetic stripe is more than 3, magnetic stripe is with respect 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.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105755441A (en) * | 2016-04-20 | 2016-07-13 | 中国科学院宁波材料技术与工程研究所 | Method for diffusing permeation of heavy rare earth through magnetron sputtering method to improve coercivity of sintered neodymium iron boron |
| CN106710767A (en) * | 2016-12-09 | 2017-05-24 | 宁波大榭开发区银鑫磁业有限公司 | Corrosion-resistant multi-coating neodymium iron boron and preparation process |
| 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 |
| CN111292951A (en) * | 2020-02-28 | 2020-06-16 | 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 |
| CN111986913A (en) * | 2020-09-23 | 2020-11-24 | 赣州富尔特电子股份有限公司 | Method for improving performance of sintered neodymium-iron-boron magnet |
| CN112281129A (en) * | 2020-10-19 | 2021-01-29 | 南昌航空大学 | Preparation process of Ni-Cr corrosion-resistant alloy coating on surface of sintered NdFeB magnet |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1073036A (en) * | 1991-11-27 | 1993-06-09 | 日立金属株式会社 | Corrosion proof rare earth element/transition metal series permanent magnet and manufacture method thereof have been improved |
| JPH11238620A (en) * | 1998-02-23 | 1999-08-31 | Seiko Epson Corp | Permanent magnet and its manufacture |
| CN101373650A (en) * | 2007-08-23 | 2009-02-25 | 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 |
| JP2009176880A (en) * | 2008-01-23 | 2009-08-06 | Tdk Corp | 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 |
| CN103290382A (en) * | 2013-05-15 | 2013-09-11 | 宁波韵升股份有限公司 | Planetary workpiece frame of vacuum coating machine |
-
2014
- 2014-03-22 CN CN201410107557.5A patent/CN103839671B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1073036A (en) * | 1991-11-27 | 1993-06-09 | 日立金属株式会社 | Corrosion proof rare earth element/transition metal series permanent magnet and manufacture method thereof have been improved |
| JPH11238620A (en) * | 1998-02-23 | 1999-08-31 | Seiko Epson Corp | Permanent magnet and its manufacture |
| CN101373650A (en) * | 2007-08-23 | 2009-02-25 | 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 |
| JP2009176880A (en) * | 2008-01-23 | 2009-08-06 | Tdk Corp | 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 |
| CN103290382A (en) * | 2013-05-15 | 2013-09-11 | 宁波韵升股份有限公司 | Planetary workpiece frame of vacuum coating machine |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105755441A (en) * | 2016-04-20 | 2016-07-13 | 中国科学院宁波材料技术与工程研究所 | Method for diffusing permeation of heavy rare earth through magnetron sputtering method to improve coercivity of sintered neodymium iron boron |
| 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 |
| CN106710767A (en) * | 2016-12-09 | 2017-05-24 | 宁波大榭开发区银鑫磁业有限公司 | Corrosion-resistant multi-coating neodymium iron boron and preparation process |
| 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 |
| CN111292951A (en) * | 2020-02-28 | 2020-06-16 | 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 |
| CN111986913A (en) * | 2020-09-23 | 2020-11-24 | 赣州富尔特电子股份有限公司 | Method for improving performance 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 |
| CN112281129A (en) * | 2020-10-19 | 2021-01-29 | 南昌航空大学 | Preparation process of Ni-Cr corrosion-resistant alloy coating on surface of sintered NdFeB 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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