CN103839641B - The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device and manufacture method - Google Patents

The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device and manufacture method Download PDF

Info

Publication number
CN103839641B
CN103839641B CN201410107545.2A CN201410107545A CN103839641B CN 103839641 B CN103839641 B CN 103839641B CN 201410107545 A CN201410107545 A CN 201410107545A CN 103839641 B CN103839641 B CN 103839641B
Authority
CN
China
Prior art keywords
coating
permanent magnet
rare earth
earth permanent
pivoted frame
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201410107545.2A
Other languages
Chinese (zh)
Other versions
CN103839641A (en
Inventor
陈晓东
孙宝玉
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SHENYANG ZHONGBEI VACUUM DEVICE Co Ltd
Original Assignee
SHENYANG ZHONGBEI VACUUM DEVICE Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by SHENYANG ZHONGBEI VACUUM DEVICE Co Ltd filed Critical SHENYANG ZHONGBEI VACUUM DEVICE Co Ltd
Priority to CN201410107545.2A priority Critical patent/CN103839641B/en
Publication of CN103839641A publication Critical patent/CN103839641A/en
Application granted granted Critical
Publication of CN103839641B publication Critical patent/CN103839641B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Physical Vapour Deposition (AREA)
  • Manufacturing Cores, Coils, And Magnets (AREA)

Abstract

The invention discloses the admixture plates the film equipment and the manufacture method of a kind of neodymium iron boron rare earth permanent magnet device, filming equipment is provided with vacuum chamber, cylinder rotating cathode magnetic control target, planar cathode magnetic control target, multi sphere ion target, pivoted frame and charging basket.During work, pivoted frame revolves round the sun in vacuum chamber, and netted charging basket two ends have rotating shaft to be arranged on pivoted frame i.e. along with pivoted frame revolves round the sun and rotation.Cylinder rotary magnetron target is arranged in vacuum chamber inside pivoted frame, plane magnetic control target, multi sphere ion target, anode-layer-linear ion source and heater are arranged in vacuum chamber around pivoted frame, vacuum coating is divided into 3 layers, ground floor is magnetron sputtering coating, thickness of coating is: 0.1 5 μm, and the second layer is the mixing coating of magnetron sputtering and multi sphere, and thickness of coating is: 1 15 μm, third layer is magnetron sputtering coating, and thickness of coating is: 0.1 5 μm.Use the admixture plates the film 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

The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device and manufacture method
Technical field
The invention belongs to permanent magnet devices field, particularly relate to the admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device And manufacture method.
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 medical treatment NMR (Nuclear Magnetic Resonance)-imaging, computer hard disc driver, sound equipment, mobile phone etc.;Along with energy-conservation and low-carbon economy requirement, neodymium iron boron is dilute Soil permanent magnet material starts again at auto parts and components, household electrical appliance, energy-conservation and control motor, hybrid vehicle, wind-power electricity generation etc. Field is applied.
The process of surface treatment of the rare earth permanent magnet device of prior art mainly has electroplated Ni-Cu-Ni, plating Zn, electrophoresis, spray The technology such as painting, also have and use vacuum aluminum-coated method, such as Chinese patent ZL96192129.3, disclose Vacuum Deposition Ti's and AlN Method;Another Chinese patent ZL01111757.5 discloses employing and is evaporated in vacuo zinc-plated, the method for aluminum, stannum, magnesium.
Prior art, can be around as it is shown in figure 1, have two support members 7 to be arranged side by side in the upper district within vacuum chamber 1 Rotating shaft 6 on one horizontal axis of rotation rotates.Six cylinders 5 formed by stainless steel cloth load magnetic part 14, rotating shaft 8 exist In the outer circumference direction of the rotating shaft 6 of support member 7 and be supported for an annular, rotate for around the shaft 6.As for evaporation Multiple heating boats 2 of the evaporator section of material aluminium wire 9 are arranged on one in adding that the support platform 3 processed in the district of 1 time, chamber is raised Hot boat supports on pedestal 4.Aluminium wire 9 is fixing and is wrapped on a feed roller 10 under support platform 3.The front end of aluminium wire 9 Being guided by the thermal resistance protection pipe 11 of an inner surface towards heating boat 2 and reach to heat on boat 2, a recess 12 is arranged on guarantor In a part for pillar 11, and feed gear wheel 13 is installed corresponding to recess 12, and directly contacts with aluminium wire 9, so passes through feeding Aluminium wire can be fed in heating boat 2 by aluminium wire 9 consistently, and heating evaporation deposits to complete on the magnetic part 14 in the barrel 5 rotated Aluminize in its surface.
Prior art uses evaporation coating, and film layer is poor with the adhesion of matrix, improves the anticorrosive energy of rare earth permanent magnet device Power Shortcomings;Also the prior art having have employed magnetron sputtering plating, owing to the efficiency of magnetron sputtering is low, is not suitable for low cost Producing in enormous quantities, the solution that do not has also having is installed technology, is difficult to be installed, and produces trouble;Also the prior art that has use multi sphere from , there is bulky grain during due to multi-arc ion plating film in sub-plated film, it is impossible to reaches the corrosion resistance requirement of rare earth permanent magnet device;For understanding The certainly shortcoming of multi-arc ion coating, also someone contemplates employing multi-arc ion coating and magnetron sputtering the admixture plates the film to prior art, but The most do not solve high efficiency, low-costly and in high volume production technology, device structure Shortcomings;The particularly rare earth of prior art The electroplating chemical of permanent magnet devices processes technique, and energy consumption height has pollution, it is desirable to expensive water treatment facilities, deals with improperly ecological ring Border has a strong impact on, and because the production process of the present invention is carried out in a vacuum, does not use environmental pollution material, will not give raw State environment, the most also eliminates the impact on the reduction of magnetic property of " battery " effect in electroplating process.For This, the present invention provides the vacuum the admixture plates the film equipment of a kind of novel rare-earth permanent magnet devices to compensate for the deficiencies in the prior art;Additionally The neodymium iron boron rare earth permanent magnet device using the equipment of the present invention to produce not only increases the resistance to corrosion of rare earth permanent magnet device, also Improve the magnetic property of rare earth permanent magnet device, hence it is evident that improve the magnetic energy product of rare earth permanent magnet device and coercivity, save rare dilute Soil resource, has especially saved more rare heavy rare earth consumption.
Summary of the invention
The present invention is to provide a kind of neodymium iron boron rare earth permanent magnet device the admixture plates the film equipment and manufacture method, passes through techniques below The magnetic property of scheme realization raising rare earth permanent magnet device and the resistance to corrosion of raising:
A kind of neodymium iron boron rare earth permanent magnet device the admixture plates the film equipment, described the admixture plates the film equipment include vacuum film coating chamber, Cylinder negative electrode magnetic control target, planar cathode magnetic control target, cathodic multi arc ion plating target, pivoted frame and charging basket;Described vacuum film coating chamber is by crouching Formula vaccum case, Qianmen and bonnet composition, Qianmen and vaccum case by rubber seal rings for seal, bonnet or be welded on vacuum Connecting on housing or by connector, the design of big pivoted frame is indoor in vacuum coating, and by rotating shaft support on framework, framework is pacified It is contained on vaccum case;The axis of big pivoted frame is parallel with the axis of vaccum case, and big pivoted frame is provided with 3 little pivoted frames, little turn The axis of frame is parallel with the axis of big pivoted frame, and multiple netted charging basket two ends have rotating shaft to be arranged on little pivoted frame, the axis of rotating shaft with The axis of little pivoted frame is parallel, and big pivoted frame revolves round the sun around the axis of vaccum case, and little pivoted frame i.e. revolves round the sun again around the axis of big pivoted frame Rotation, netted charging basket i.e. revolves round the sun with big pivoted frame and revolves round the sun and rotation also with little pivoted frame;Described cylinder negative electrode magnetic control target peace Being contained on the bonnet that vacuum coating is indoor, cylinder negative electrode magnetic control target is positioned at the inside of pivoted frame, and axis is parallel with pivoted frame axis, described Cylinder negative electrode magnetic control target more than one is set;Described planar cathode magnetic control target is arranged on vaccum case, is distributed in pivoted frame Periphery.
Cylinder negative electrode magnetic control target is arranged on the bonnet that vacuum coating is indoor, and power supply, cooling water and actuating device are by outside Introducing, cylinder negative electrode magnetic control target is positioned at the inside of big pivoted frame, and axis is parallel with pivoted frame axis.
Described cylinder negative electrode magnetic control target is set to one.
Described cylinder negative electrode magnetic control target, built with the magnet ring of multiple axial chargings, has magnetic guiding loop between magnet ring, magnet ring is relative Move in cylinder negative electrode magnetic control target axial reciprocating.
In described cylinder negative electrode magnetic control target or equipped with the magnetic stripe of a plurality of radial magnetizing, magnetic stripe is at cylinder negative electrode magnetic control target The most circumferentially being distributed, have interval between magnetic stripe, the quantity of magnetic stripe is 3 or more than 3, and magnetic stripe is relative to cylinder negative electrode magnetic control Target rotates coaxially.
Described magnet ring or magnetic stripe are manufactured by Nd-Fe-B rare-earth permanent magnet.
Planar cathode magnetic control target is arranged on vaccum case, is distributed in the periphery of big pivoted frame, described planar cathode magnetic control Being provided with run-track shaped ring-type magnetic stripe in target, magnetic stripe is manufactured by Nd-Fe-B rare-earth permanent magnet, and by cooling water cooling, quantity is one Or more than one.
Cathodic multi arc ion plating target is arranged on vaccum case, is distributed in the periphery of big pivoted frame, described cathodic multi arc ion plating Target is rectangle or circle, is internally provided with Magnet, and Magnet is manufactured by Nd-Fe-B rare-earth permanent magnet, and by cooling water cooling, quantity is one More than individual.
Anode-layer-linear ion source is arranged on vaccum case, is distributed in the periphery of pivoted frame.
Described vacuum coating indoor are provided with heater, and heating temperature range is at 100-600 DEG C.
Described plated film target is Al, Dy-Al, Tb-Al, Dy-Fe, Tb-Fe, Ni-Cr, Ti, Mo, Si, Al2O3、ZrO2、 More than one in AZO.
Described neodymium iron boron rare earth permanent magnet device plating membrane system is the one in Al, Dy-Al, Tb-Al, Dy-Fe, Tb-Fe Above.
Described neodymium iron boron rare earth permanent magnet device plating membrane system is Al, Ni-Cr, Ti, Mo, Si, Al2O3、ZrO2, in AZO More than one.
Described neodymium iron boron rare earth permanent magnet device plating membrane system 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, nitrogen, oxygen, hydrogen.
The gas that described gas charging system is filled with is argon.
Described vacuum pump is oil-sealed rotary pump, Roots vaccum pump, oil diffusion vacuum pump, molecular pump in one with On.
Described magnetron sputtering plating condition is, temperature 30 ~ 600 DEG C, and deposition pressure is 0.1 ~ 1Pa under the conditions of argon, merit Rate density is 1 ~ 20w/cm2;Discharge voltage 100 ~ the 3000V of linear ion source, ion energy 100 ~ 2000eV, under the conditions of argon Operating air pressure 0.01 ~ 1Pa.Described filming process uses magnetron sputtering plating and multi-arc ion plating film, magnetron sputtering plating With multi-arc ion plating film individually, be either alternatively or simultaneously operated.
The manufacture method of a kind of neodymium iron boron rare earth permanent magnet device, first carries out alloy melting, in the molten state by alloy It is cast in the rotary copper roller of band water cooling be cooled into alloy sheet, then alloy sheet is carried out hydrogen is broken, batch mixing and airflow milling, Under nitrogen protection with delivering to nitrogen protection magnetic field orientating press-molding after batch mixer batch mixing after airflow milling, at guard box after shaping Carry out isostatic pressed after interior encapsulation, send into agglomerating plant sintering afterwards and timeliness makes Nd-Fe-B rare-earth permanent magnet magnet, carry out afterwards Machining makes neodymium iron boron rare earth permanent magnet device, afterwards neodymium iron boron rare earth permanent magnet device is carried out plated film, and plated film is divided into 3 layers, Ground floor is magnetron sputtering coating, and thickness of coating is: 0.02-5 μm, and the second layer is the mixing plating of magnetron sputtering and multi-arc ion coating Layer, thickness of coating is: 1-10 μm, and third layer is magnetron sputtering coating, and thickness of coating is: 0.1-5 μm.
Described the admixture plates the film operation, plated film is divided into 3 layers, and ground floor is magnetron sputtering coating, coating is Al, Dy-Al, One in Tb-Al, Dy-Fe, Tb-Fe, the second layer is the mixing coating of magnetron sputtering and multi-arc ion coating, and coating is Al, Ni- Cr、Ti、Mo、Si、Al2O3、ZrO2, more than one in AZO, third layer is magnetron sputtering coating, coating is Al, Ni-Cr, Ti, Mo、Si、Al2O3、ZrO2, more than one in AZO.
Described the admixture plates the film operation, plated film is divided into 3 layers, and ground floor is magnetron sputtering coating, and coating is Dy-Al, Tb- One in Al, Dy-Fe, Tb-Fe, the second layer is the mixing coating of magnetron sputtering and multi-arc ion coating, coating is Al, Ni-Cr, Al2O3、ZrO2, more than one in AZO, third layer is magnetron sputtering coating, and coating is Al, Ni-Cr, Al2O3、ZrO2, in AZO More than one.
Described the admixture plates the film operation, plated film is divided into 3 layers, and ground floor is magnetron sputtering coating, and coating is in Al, Ni-Cr More than one, the second layer is the mixing coating of magnetron sputtering and multi-arc ion coating, and coating is more than one in Al, Ni-Cr, Third layer is magnetron sputtering coating, and coating is more than one in Al, Ni-Cr.
Rare earth permanent magnet device sandblasting to be carried out operation before filming process, the material that sandblasting uses is quartz, glass microballoon, oxygen Change aluminum, cerium oxide, lanthana, cerium oxide and the mixture of lanthana, zirconic more than one.
Before filming process or have spraying process, sprayed on material is aluminum or containing the one in the compound of aluminum, electrophoretic paint.
In filming process or have control coating process device heating process, temperature range is at 100-600 DEG C.
After filming process or have heat treatment step.
The heat treatment temperature of described heat treatment step is at 110-890 DEG C.
The heat treatment of described heat treatment step is carried out under vacuum or protective atmosphere.
Neodymium iron boron rare earth permanent magnet device the admixture plates the film equipment or be arranged in clean room, the cleanliness factor of Factory Building 10, More than 000 grade.
Metallographic Analysis shows, described a kind of neodymium iron boron rare earth permanent magnet device in the range of device surface extends internally 1mm, In main phase grain, the content of heavy rare earth is higher than the content of device main phase grain heavy rare earth, and the heavy rare earth that content is high is distributed in principal phase R2T14The periphery of B, forms RH2T14B surrounds R2T14The new principal phase structure of B, RH2T14B phase and R2T14B is alternate without Grain-Boundary Phase;Wherein, R represents the rare earth in principal phase in Fe-B rare-earth permanent magnet structure, and T representative element Fe and Co, RH represent weight in principal phase The content of rare earth is higher than the rare earth of meansigma methods.
Beneficial effects of the present invention: have found the vacuum coating equipment that a kind of neodymium iron boron rare earth permanent magnet device is produced in enormous quantities And manufacture method, hence it is evident that improve the decay resistance of neodymium iron boron rare earth permanent magnet device, make neodymium iron boron rare earth permanent magnet device to be used for The field that the high corrosion-resistant such as offshore wind farm, hybrid vehicle requires, expands the purposes of Nd-Fe-B rare-earth permanent magnet;Ordinary circumstance Under, the face coat of Nd-Fe-B rare-earth permanent magnet all can reduce magnetic property, present invention discover that and uses the equipment of the present invention and technique raw The magnetic property of the neodymium iron boron rare earth permanent magnet device produced, especially magnetic energy product and coercivity is improved significantly, for improving neodymium iron boron The magnetic property of rare earth permanent magnet have found new method, to reducing rare-earth usage, protects 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 be the present invention vacuum coating schematic diagram
In figure: 1, vacuum chamber;2, heating boat;3, support platform;4, heating boat supports pedestal;5, charging cylinder;6、 Around the shaft;7, support member;8, rotating shaft;9, aluminium wire;10, roller;11, thermal resistance protection pipe;12, recess;13, feed gear wheel;14, magnetic Part;15, vaccum case;16, anode-layer-linear ion source;17, multi sphere ion source;18, vacuum pump;19, plane magnetic control target;20、 Heater;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, big Pivoted frame;26, charging basket;27, permanent magnet devices;28, cylinder magnetic control target;29, III grade of driving gear;30, III grade of driven gear;31, take out Vacuum line;32, little pivoted frame;33, rotating shaft I;34, rotating shaft II.
As in figure 2 it is shown, the admixture plates the film equipment that the present invention is magnetron sputtering plating and multi-arc ion plating film work in combination.? One connection has the centrage of the horizontal vacuum housing 15 of vacuum pump 18 to be provided with a column type magnetic control target 28, at big pivoted frame 25 Circumference on be disposed with multiple (in figure being 3) little pivoted frame 32, the circumference of each little pivoted frame 32 being disposed with multiple (is 6 in figure Individual) stainless (steel) wire finish mix basket 26, charging basket 26 is built with permanent magnet devices 27.Driving motor (not shown) outside vacuum chamber is passed through Movable sealing power transmission shaft connects I grade of driving gear 21, drives the I grade of driven gear 22 being fixed on big pivoted frame 25 to complete big pivoted frame 25 Revolve round the sun around cylinder magnetic control target 28.The II grade of driving gear 23 being fixed on big pivoted frame 25 drives fixing by the revolution of big pivoted frame 25 II grade of driven gear 24 I 33 rotation around the shaft on little pivoted frame 32;The III grade of driving gear 29 being fixed on little pivoted frame 32 carries Dynamic III grade of driven gear 30 II 34 rotates around the shaft, and the two ends of charging basket 26 are provided with rotating shaft and rotating shaft II 34 and III grade of driven gear 30 Couple, therefore charging basket 26 can reach sun and planet gear revolution add rotation purpose, make permanent magnet devices 27 stir-fry in charging basket 26 By target material on uniform deposition.Outside circular vacuum housing 15, be provided with anode-layer-linear ion source 16, more than 1 multi sphere from Component 17, more than one plane magnetic control target 19, connect vacuum-pumping pipeline 31 and the heater 20 of vacuum pump 18.
Room, filming process initial vacuum evacuation reaches E-4Pa magnitude, backfilled with argon, operating air pressure 0.01 ~ 1Pa, charging basket 26 Revolution adds rotation, starting cathode layer linear ion source, discharge voltage 100 ~ 3000V, and ion bom bardment permanent magnet devices 27, through 5 ~ 10 Minute stop bombardment.Charging basket 26 is insulation, it is also possible to meet negative pressure-50 ~-200V.The purpose of icon bombardment cleaning in advance, is clear Wash the oxide on permanent magnet devices 27 surface, containing hydrocarbons so that it is surface coarsening increases surface and can make with ion assisted deposition etc. With.Heater 20 is heated to 120 ~ 600 DEG C to permanent magnet devices 27 in charging basket 26 and charging basket 26, plays removing steam, improves film Layer adhesive force effect.Filming process is when being heated to 200 DEG C, and charging basket 26 revolution adds rotation and after high-pressure ion cleans, very Empty room 15 evacuation again reaches E-4Pa magnitude, backfilled with argon, operating air pressure 0.1 ~ 1Pa, separately or concurrently starts plane magnetic control Target 19, column type magnetic controlled sputtering target 28 and multi sphere ion source 17 so that it is individually work or alternation or simultaneously work, will Target material deposits to be formed on permanent magnet devices 27 simple substance film and the coating of deielectric-coating.
Detailed description of the invention
The remarkable result of the present invention is further illustrated below by the contrast of embodiment.
Embodiment 1
By following technique manufacture:
1, choose alloy 600Kg melting by table one A1, A2, A3, A4 composition respectively, in the molten state alloy casting is arrived With being cooled into alloy sheet in the rotary copper roller of water cooling, then carry out hydrogen and crush, carry out batch mixing after hydrogen is broken, carry out after batch mixing Airflow milling, the most under nitrogen protection with delivering to nitrogen protection magnetic field orientating press-molding after batch mixer batch mixing, in guard box Oxygen content 150ppm, alignment magnetic field 1.8T, mould cavity temperature 2 DEG C, magnetic piece size 62 × 52 × 42mm, differently-oriented directivity is 42 Dimensional directions, encapsulates in guard box after shaping, then takes out and carry out isostatic pressed, and hydrostatic pressure 200MPa sends into burning afterwards Knot equipment sintering and timeliness.
2, carry out machining after timeliness, be processed into square piece 30 × 20 × 10 mm size, workpiece selectivity is carried out down Angle, sandblasting, aluminium-plated, electrophoresis, spraying, carrying out vacuum coating afterwards, ground floor uses magnetron sputtering plating, and the second layer is that magnetic control spatters Penetrating the mixing coating with multi-arc ion coating, third layer is magnetron sputtering coating, and thickness of coating is respectively as follows: 0.02-5 μm, 0.1-15 μ M, 1-5 μm;Some experiments have also carried out plating the 4th layer, and the 4th layer is magnetron sputtering coating, thickness 0.1-5 μm, does not marks for the 4th layer The note symbol of element be only triple-layer coating, and the measurement result of material, magnetic property and the decay resistance of the selection of each layer lists table in Two.
The composition of the RE permanent magnetic alloy of table one, embodiment and comparative example
Numbering Composition
A1 Nd30Dy1Fe67.9B0.9Al0.2
A2 Nd30Dy1Fe67.5Co1.2Cu0.1B0.9Al0.1
A3 (Pr0.2Nd0.8)25Dy5Fe67.4Co1.2Cu0.3B0.9Al0.2
A4 (Pr0.2Nd0.8)25Dy5Tb1Fe65Co2.4Cu0.3B0.9Al0.2Ga0.1Zr0.1
Table two, the coating material of the present invention, magnetic property and the measurement result of decay resistance
Comparative example 1
Choose alloy 600Kg melting by A1, A2, A3, A4 composition of table one respectively, in the molten state alloy casting is arrived It is cooled into alloy sheet with on the chill roll of the rotation of water cooling, then uses vacuum hydrogen crushing furnace that alloy sheet is carried out coarse crushing, Hydrogen crushes laggard row airflow milling, under nitrogen protection with delivering to nitrogen protection magnetic field orientating press-molding after batch mixer batch mixing, takes To magnetic field intensity 1.8T, magnetic piece size 62 × 52 × 42mm, differently-oriented directivity is 42 dimensional directions, seals after shaping in guard box Dress, then takes out and carries out isostatic pressed, hydrostatic pressure 200MPa, sends into vacuum sintering furnace sintering and timeliness afterwards, then carries out machine Tool process, be processed into square piece 30 × 20 × 10 mm size, workpiece selectivity carried out chamfering or sandblasting, carry out afterwards electroplated Ni- The measurement result of Cu-Ni, magnetic property and decay resistance lists table three in.
Table three, the magnetic property of comparative example and the measurement result of decay resistance
Embodiment 2
Choosing the composition in embodiment 1 and make neodymium iron boron rare earth permanent magnet device, coating selects ground floor plating Dy-Al alloy, The second layer plates Al+ Al, and temperature experiment made by the coating of third layer plating Al, and result lists table four in, does not heats also when sequence number 1 is for plated film Do not carry out the comparative example of heat treatment, by table four it can be seen that the heat treatment temperature after coating temperature and plated film is to material Magnetic property has an impact, hence it is evident that improve the coercivity of magnet, namely improves the use temperature of magnet, is using temperature on an equal basis Under, it is possible to reduce the consumption of heavy rare earth, save scarce resource.
Table four, coating temperature and heat treatment temperature are on magnetic property and the impact of decay resistance
Note: 1, corrosion resistance (PCT test)
Experiment condition: sample 10X10X10mm, 2 normal atmospheres, 120 DEG C, 100% humidity, 48 hours, weightless < 5mg/ cm2
2, salt spray test:
Experiment condition: 5%NaCl solution, tests for 25 DEG C >=48 hours, and surface is not changed in.
In embodiment, sandblasting operation to be had before vacuum coating operation: because rare earth permanent magnet device is in the course of processing, at it All can there is a certain amount of oils and fats and dirty in surface, and these dirts are to technique for vacuum coating stability and the corrosion resistant of coated product Erosion performance has a great impact, and therefore configures rational cleaning equipment and technique is rare earth permanent magnet component vacuum coating quality performance Basic guarantee, only reasonably cleaning guarantee coating has good adhesive force.The material that sandblasting operation uses Be quartz, glass microballoon, aluminium oxide, cerium oxide, lanthana, cerium oxide and lanthana mixture, zirconic more than one. Before vacuum coating operation or also spraying process, sprayed on material is aluminum or containing the one in the compound of aluminum, electrophoretic paint.
In embodiment, in filming process mesohigh Ion Cleaning operation: vacuum chamber is higher than the E-4Pa order of magnitude, fills Argon, operating air pressure 0.01 ~ 1Pa, charging basket revolves round the sun and adds rotation, starting cathode layer linear ion source, discharge voltage 100 ~ 3000V, Ion bom bardment rare earth permanent magnet device 5 ~ 10 minutes.Charging basket is insulation, it is also possible to meet negative pressure-50 ~-200V.
In embodiment, coating process configures: reasonably Process configuration includes that the configuration of single, double magnetron cathode (includes plane, circle Post rotary magnetron cathode arrangement), multi sphere cathode arrangement, anode-layer-linear ion source, heater and vacuum pump etc..Different plated films Process configuration causes throughput rate, ion energy etc. to change, and has a major impact coated product performance.Vacuum chamber is higher than The E-4Pa order of magnitude, backfilled with argon, operating air pressure 3E-1Pa, charging basket revolution adds rotation, magnetron sputtering deposition and arc evaporation deposition Individually work or individually alternation or simultaneously work;Magnetron sputtering deposition and arc evaporation deposition respectively with ion bom bardment Work independently or individually alternation.
In embodiment, coating process feeds: the structure of charging basket has considerable influence to coated product outward appearance and coating quality, should Avoid the occurrence of surface tear and other physical damnifications.Charging basket is the cylinder type made of stainless (steel) wire or polygonal column structure, in Between have dividing plate to form multiple insulating space, one or a few permanent magnet devices is placed in each space.
In embodiment, after vacuum coating operation or have heat treatment step, heat treatment temperature 100-900 DEG C.
By relatively further illustrating of embodiment and comparative example, the technology of the present invention is used to significantly improve the magnetic of magnet Energy and decay resistance, be technique and the equipment and technology having very much development.

Claims (13)

1. the admixture plates the film equipment of a neodymium iron boron rare earth permanent magnet device, it is characterised in that: described the admixture plates the film equipment includes Vacuum film coating chamber, cylinder negative electrode magnetic control target, planar cathode magnetic control target, cathodic multi arc ion plating 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, and Qianmen and vaccum case are close by rubber Seal seals, bonnet or be welded on vaccum case or connect by connector, the design of big pivoted frame in vacuum coating indoor, By rotating shaft support on framework, framework is arranged on vaccum case;The axis of big pivoted frame is parallel with the axis of vaccum case, greatly Being provided with 3 little pivoted frames on pivoted frame, the axis of little pivoted frame is parallel with the axis of big pivoted frame, and multiple netted charging basket two ends have rotating shaft to pacify Being contained on little pivoted frame, the axis of rotating shaft is parallel with the axis of little pivoted frame, and big pivoted frame revolves round the sun around the axis of vaccum case, little pivoted frame The i.e. axis around big pivoted frame revolves round the sun and rotation, and netted charging basket i.e. revolves round the sun also with the revolution of little pivoted frame again certainly with big pivoted frame Turn;Described cylinder negative electrode magnetic control target is arranged on the bonnet that vacuum coating is indoor, and cylinder negative electrode magnetic control target is positioned at pivoted frame Portion, axis is parallel with pivoted frame axis, and described cylinder negative electrode magnetic control target arranges more than one;Described planar cathode magnetic control target It is arranged on vaccum case, is distributed in the periphery of pivoted frame;Described cylinder negative electrode magnetic control target and the target of planar cathode magnetic control target It is respectively the one in Dy-Al, Tb-Al, Dy-Fe, Tb-Fe, Al, Ni-Cr, Ti, Mo, Si, Al2O3, ZrO2, AZO, and cylinder In the target of negative electrode magnetic control target or planar cathode magnetic control target, at least a kind of target is selected from Dy-Al, Tb-Al, Dy-Fe, Tb-Fe; Described vacuum coating indoor are provided with heater, and heating temperature range is at 100-600 DEG C.
The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device the most according to claim 1, it is characterised in that: described Cylinder negative electrode magnetic control target built with the magnet ring of multiple axial chargings, have magnetic guiding loop between magnet ring, magnet ring is relative to cylinder negative electrode magnetic Control target axial reciprocating moves, and described magnet ring is manufactured by Nd-Fe-B rare-earth permanent magnet.
The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device the most according to claim 1, it is characterised in that: described Cylinder negative electrode magnetic control target built with the magnetic stripe of a plurality of radial magnetizing, magnetic stripe is circumferentially distributed in cylinder negative electrode magnetic control target, Having interval between magnetic stripe, the quantity of magnetic stripe is 3 or more than 3, and magnetic stripe coaxially turns relative to cylinder negative electrode magnetic control target sleeve pipe Dynamic, described magnetic stripe is manufactured by Nd-Fe-B rare-earth permanent magnet.
The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device the most according to claim 1, it is characterised in that: described Planar cathode magnetic control target in be provided with run-track shaped annular magnetic stripe, magnetic stripe is manufactured by Nd-Fe-B rare-earth permanent magnet, with cooling water Cooling, quantity is more than one.
The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device the most according to claim 1, it is characterised in that: described Cathodic multi arc ion plating target be arranged on vaccum case, be distributed in the periphery of pivoted frame, described cathodic multi arc ion plating target is rectangle Or circular, it is internally provided with Magnet, Magnet is manufactured by Nd-Fe-B rare-earth permanent magnet, and by cooling water cooling, quantity is more than one.
The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device the most according to claim 1, it is characterised in that: described Anode-layer-linear ion source be arranged on vaccum case, be distributed in the periphery of pivoted frame.
7. the manufacture of the neodymium iron boron rare earth permanent magnet device of the admixture plates the film equipment used as described in any one of claim 1-6 Method, it is characterised in that: first carry out alloy melting, in the molten state by alloy casting to the rotary copper roller of band water cooling It is cooled into alloy sheet, then alloy sheet is carried out hydrogen is broken, batch mixing and airflow milling, after airflow milling, use batch mixing under nitrogen protection Deliver to nitrogen protection magnetic field orientating press-molding after machine batch mixing, in guard box, carry out isostatic pressed after encapsulation after shaping, send afterwards Enter agglomerating plant sintering and timeliness makes Nd-Fe-B rare-earth permanent magnet magnet, carry out machining afterwards and make Nd-Fe-B rare-earth permanent magnet Device, afterwards in the indoor mixing that neodymium iron boron rare earth permanent magnet device carries out magnetron sputtering plating and multi-arc ion coating of vacuum coating Plated film, plated film is divided into 3 layers, and ground floor is magnetron sputtering coating, and coating is the one in Dy-Al, Tb-Al, Dy-Fe, Tb-Fe, Thickness of coating is: 0.02-5 μm, and the second layer is the mixing coating of magnetron sputtering and multi-arc ion coating, and thickness of coating is: 1-10 μm, Third layer is magnetron sputtering coating, and thickness of coating is: 0.1-5 μm;Heat treatment step is also had after described the admixture plates the film operation, Heat treatment temperature 60-900 DEG C.
The manufacture method of a kind of neodymium iron boron rare earth permanent magnet device the most according to claim 7, it is characterised in that: described is mixed Closing plated film and belong to physical vapour deposition (PVD), magnetic control film coating material is Al, Dy-Al, Tb-Al, Dy-Fe, Tb-Fe, Ti, Mo, Si, stainless Steel, Al2O3, one in ZrO, AZO, the mixing coating of described magnetron sputtering and arc evaporation, Coating Materials is Al, Ti, Mo, Si, rustless steel, Al2O3, more than one in ZrO, ITO, AZO.
The manufacture method of a kind of neodymium iron boron rare earth permanent magnet device the most according to claim 7, it is characterised in that: described is true Being provided with anode-layer-linear ion source in empty coating chamber, described magnetron sputtering plating condition is, temperature 30 ~ 600 DEG C, deposition pressure Strong is 0.1 ~ 1Pa under the conditions of argon, and power density is 1 ~ 20w/cm2, the discharge voltage 100 ~ 3000V of linear ion source, ion Energy 100 ~ 2000eV, operating air pressure 0.01 ~ 1Pa under the conditions of argon, in described filming process use magnetron sputtering plating and Multi-arc ion plating film is individually, be either alternatively or simultaneously operated.
The manufacture method of a kind of neodymium iron boron rare earth permanent magnet device the most according to claim 7, it is characterised in that: described Also having sandblasting operation before filming process, the material that sandblasting uses is quartz, glass microballoon, aluminium oxide, cerium oxide, lanthana, oxygen Change cerium and the mixture of lanthana, zirconic more than one, before filming process or also spraying process, sprayed on material is aluminum Or containing the one in the compound of aluminum, electrophoretic paint.
The manufacture method of 11. a kind of neodymium iron boron rare earth permanent magnet device according to claim 7, it is characterised in that: described Also having the device heating process controlling coating process in filming process, temperature range is at 100-600 DEG C.
The manufacture method of 12. a kind of neodymium iron boron rare earth permanent magnet device according to claim 7, it is characterised in that: described The admixture plates the film operation, plated film is divided into 3 layers, and ground floor is magnetron sputtering coating, and coating is Al, Dy-Al, Tb-Al, Dy-Fe, Tb- One in Fe, the second layer is the mixing coating of magnetron sputtering and multi-arc ion coating, coating is Al, Ni-Cr, Ti, Mo, Si, Al2O3、ZrO2, more than one in AZO, third layer is magnetron sputtering coating, and coating is Al, Ni-Cr, Ti, Mo, Si, Al2O3、 ZrO2, more than one in AZO.
The manufacture method of 13. a kind of neodymium iron boron rare earth permanent magnet device according to claim 7, it is characterised in that: described A kind of neodymium iron boron rare earth permanent magnet device in the range of device surface extends internally 1mm main phase grain the content of heavy rare earth higher than crystalline substance The content of heavy rare earth in grain principal phase, the heavy rare earth that content is high is distributed in principal phase R2T14The periphery of B, forms RH2T14B surrounds R2T14B New principal phase structure, RH2T14B phase and R2T14B is alternate without Grain-Boundary Phase;Wherein, R represents at Fe-B rare-earth permanent magnet structure Rare earth in middle principal phase, T representative element Fe and Co, RH represent that in principal phase, the content of heavy rare earth is higher than the rare earth of meansigma methods.
CN201410107545.2A 2014-03-22 2014-03-22 The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device and manufacture method Active CN103839641B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410107545.2A CN103839641B (en) 2014-03-22 2014-03-22 The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device and manufacture method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410107545.2A CN103839641B (en) 2014-03-22 2014-03-22 The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device and manufacture method

Publications (2)

Publication Number Publication Date
CN103839641A CN103839641A (en) 2014-06-04
CN103839641B true CN103839641B (en) 2016-10-05

Family

ID=50803050

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410107545.2A Active CN103839641B (en) 2014-03-22 2014-03-22 The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device and manufacture method

Country Status (1)

Country Link
CN (1) CN103839641B (en)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104480440A (en) 2014-11-05 2015-04-01 烟台首钢磁性材料股份有限公司 Small size neodymium-iron-boron magnet surface vacuum film plating method and special film plating equipment
CN106198366A (en) * 2016-06-23 2016-12-07 宁波国际材料基因工程研究院有限公司 A kind of screening technique of high flux soft magnetic materials surface anticorrosion layer
US10704139B2 (en) * 2017-04-07 2020-07-07 Applied Materials, Inc. Plasma chamber target for reducing defects in workpiece during dielectric sputtering
CN108950503B (en) * 2018-07-30 2020-03-31 山西金山磁材有限公司 Sintered neodymium iron boron coating film and vacuum coating process thereof
CN112746260B (en) * 2020-12-30 2023-02-28 湖南柯盛新材料有限公司 Process for manufacturing rotary target material by cold spraying and production equipment thereof
CN113838660A (en) * 2021-11-25 2021-12-24 天津三环乐喜新材料有限公司 Vacuum coating equipment and method for surface protection of neodymium iron boron rare earth permanent magnet device

Citations (7)

* Cited by examiner, † Cited by third party
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
CN2254448Y (en) * 1996-02-07 1997-05-21 郑德恩 Multiarc-magnetic control sputter vacuum ion goldplating equipment
JP2000012366A (en) * 1998-06-23 2000-01-14 Matsushita Electric Ind Co Ltd Manufacture of soft magnetic film
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
CN101619443A (en) * 2009-07-27 2010-01-06 浙江工业大学 High-efficiency film coating machine for solar thermal-collecting tubes
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

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103820766B (en) * 2014-03-22 2016-04-06 沈阳中北真空设备有限公司 A kind of magnetic control film coating equipment of neodymium iron boron rare earth permanent magnet device and manufacture method
CN103820765A (en) * 2014-03-22 2014-05-28 沈阳中北真空设备有限公司 Composite coating equipment and manufacturing method for neodymium iron boron rare-earth permanent magnetic device
CN103854819B (en) * 2014-03-22 2016-10-05 沈阳中北通磁科技股份有限公司 A kind of the admixture plates the film method of neodymium iron boron rare earth permanent magnet device

Patent Citations (7)

* Cited by examiner, † Cited by third party
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
CN2254448Y (en) * 1996-02-07 1997-05-21 郑德恩 Multiarc-magnetic control sputter vacuum ion goldplating equipment
JP2000012366A (en) * 1998-06-23 2000-01-14 Matsushita Electric Ind Co Ltd Manufacture of soft magnetic film
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
CN101619443A (en) * 2009-07-27 2010-01-06 浙江工业大学 High-efficiency film coating machine for solar thermal-collecting tubes
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

Also Published As

Publication number Publication date
CN103839641A (en) 2014-06-04

Similar Documents

Publication Publication Date Title
CN103854819B (en) A kind of the admixture plates the film method of neodymium iron boron rare earth permanent magnet device
CN103824693B (en) A kind of manufacture method of the neodymium iron boron rare earth permanent magnet device with composite film coating
CN103839641B (en) The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device and manufacture method
CN103820765A (en) Composite coating equipment and manufacturing method for neodymium iron boron rare-earth permanent magnetic device
CN103839671B (en) A kind of manufacture method of neodymium iron boron rare earth permanent magnet device
CN103820766B (en) A kind of magnetic control film coating equipment of neodymium iron boron rare earth permanent magnet device and manufacture method
CN100392147C (en) Pair target twin magnetic controlled sputtering ion plating deposition device
CN103668095B (en) A kind of high power pulse plasma enhancing combined magnetic-controlled sputter deposition apparatus and using method thereof
CN107058947A (en) For preparing fuel battery metal double polar plate amorphous carbon-film magnetron sputtering continuous lines
CN102776474B (en) Nano composite coating layer for surface treatment of substrate, and preparation method and device of nano composite coating layer
CN110592544B (en) Vertical magnetron sputtering coating device for long outer cladding tube
CN107604328A (en) A kind of fuel battery metal double polar plate highly effective ring vacuum coater
CN108018497A (en) A kind of method that neodymium iron boron magnetic body and neodymium iron boron magnetic body surface prepares aluminum alloy coating
CN102443796A (en) Porous Fe-Al intermetallic compound coating and its preparation method
CN201670871U (en) Novel high-efficient coater
CN202658221U (en) Magnetron sputtering target of magnetron sputtering coating machine
CN101949000A (en) Vacuum magnetron sputtering multi-arc ion composite coating machine
CN201144276Y (en) Plasma evaporation coater
CN103866241A (en) Composite magnetron sputtering coating device for ion-assisted thermal evaporation
CN110993231A (en) Surface-alloyed high-corrosion-resistance sintered NdFeB magnet and preparation method thereof
CN114134456B (en) Magnetron sputtering preparation method of Cr coating of zirconium alloy cladding
CN202658220U (en) Magnetic control sputtering target of magnetic control sputtering film plating machine
CN100469946C (en) Preparation method of TiC ceramic coating
CN204779787U (en) Magnetron sputtering target rifle
CN207958490U (en) The vacuum magnetic control coating equipment of Nd-Fe-B permanent magnetic is made for heavy rare earth diffusion method

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant