CN104889390A - 3D printing process of rare earth permanent magnetic material - Google Patents
3D printing process of rare earth permanent magnetic material Download PDFInfo
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- CN104889390A CN104889390A CN201410078399.5A CN201410078399A CN104889390A CN 104889390 A CN104889390 A CN 104889390A CN 201410078399 A CN201410078399 A CN 201410078399A CN 104889390 A CN104889390 A CN 104889390A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Hard Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a 3D printing process of a rare earth permanent magnetic material; a metal powder direct sintering type 3D printer is selected as processing equipment; such heating devices as laser are used as heat sources; and plane slice maps obtained through computer modeling are input into the 3D printer. The rare earth permanent magnetic material is manufactured to prealloyed powder by a powder metallurgy and powder manufacturing process and put into a powder cylinder of the printer. After the powder is spread, a computer controls a laser head to control a two-dimensional scanning trace of a laser beam according to a prototype slice model, and the laser beam is used for scanning and sintering line by line and layer by layer according to a filling contour line until a three-dimensional permanent magnet is finally formed through overlapping; and then the magnet is cooled and discharged from the cylinder. The working environment of a molding chamber is a preheated and vacuum environment filled with protective hydrogen and argon gas. The magnetization can be performed before and after the sintering. The process is suitable for all rare earth permanent magnetic materials; and large and medium permanent magnets can be manufactured through selecting large and medium printers. The process is free of mold development and manufacturing costs, shortens the manufacturing period, and can obtain the better molding quality compared with a traditional sintering process; and the molding quality even reaches the forging quality.
Description
Technical field
The 3D that the present invention relates to a kind of rare earth permanent-magnetic material prints technique
Background technology
Current, the fashionable whole world of 3D printing technique.Futurist predicts that it may lead manufacturing industry new trend, starts the third time industrial revolution.Because this technology is original in western developed country, the intellectual property of current relevant technological mostly is foreign corporation and holds, and Chinese Enterprises will deeply enter this field in the future, needs to pay high patent fee, or produces many patent disputes.Therefore, in the face of 3D prints upsurge, China is badly in need of trying hard to catch up, and opens up Invention conception as early as possible, research and development implementing process, forms the own 3D of China as early as possible and prints intellectual property system.
At present, 3D prints and fails to carry out on a large scale, and be due to most widely used manufacturing industry, most industry part needs to make with metal material, and because the preparation of metal dust printed material is with to print technique complicated more than plastics, resin, form the bottleneck that 3D prints development.In other words, 3D be allowed to print the huge manufacturing industry of real arms, the preparation of metal dust printed material must be solved as early as possible and print technique with relevant.
In metal dust, especially with rare earth permanent-magnetic material for leading new material.Permanent-magnet material does not require the expenditure of energy and can keep the magnetic functional material in its magnetic field, and rare earth permanent-magnetic material is the main product of permanent-magnet material, is widely used in modern crafts and science and technology.Because rare earth resources nearly 80% is in China, China will become base and the center of rare earth permanent-magnetic material production and exploitation 21 century.And the Application and Development of new material, be the high and new technology field that national industrial policies are encouraged energetically.
In rare earth permanent-magnetic material family, neodymium iron boron is due to magnetic property high (being called as " magnetic king "), and relative price is lower, is thus used widely.What consumption was maximum is electronic information industry, and separate unit consumption is maximum, is the magnetic resonance imager of Medical Devices industry, and main magnet can have more than ten ton of weight.
On June 26th, 2013, Chinese invention patent CN103170628A (calling in the following text " this invention ") discloses a kind of neodymium iron boron preparation method based on 3D printing technique, propose 3D printing technique to be applied to neodymium iron boron first, expand 3D and be printed on selection on metal dust printed material.This invention and difference of the present invention are:
Though 1, neodymium iron boron is most widely used in rare earth permanent-magnetic material, it is the one of Rare-Earth Magnetic material after all, belongs to rare-earth-iron system.Also has numerous series such as rare earth SmCo, praseodymium iron copper boron.As the cross membership of Rare-Earth Magnetic material family, they have identical material characteristics, should have more invention that 3D print application is expanded to whole Rare-Earth Magnetic material family.
2, these invention related products are the small and special electric machine (see this abstract of invention) of " small-sized, ultra-thin ", and the present invention with large-scale, polynary, the high level product of the main magnet of medical magnetic resonance instrument for target, have larger accommodation.
3, the conventional preparation techniques of Rare-Earth Magnetic material is divided into sintering, bonding and thermal deformation three kinds, and wherein the magnetic property of sintered magnet is higher, and bonding magnetic material comparison of magnetic property is stablized.Sintering process need with surpassing thousand degree of high temperature sinterings, and this invention is with 20 ~ 900 degrees Centigrade workbench, as sintered, need carry out beyond invention category, what also confirm in description that this invented technology makes is " Agglutinate neodymium-iron-boron ", should belong to one and to heat bonding new technology.The present invention is then that conventional sintering technique prints the new technology of docking with 3D, and technological process and this invention have very large difference, is therefore two kinds of dissimilar techniques with this invention.
4 just because of this invention is binding type technique, so the neodymium iron boron granulation of its raw material is mechanical mixture powder, and need to add binding agent, and present invention process is alloy smelting powder, and does not need to add binding agent.
In sum, this invention belongs to neodymium iron boron 3D printing non-sintered technique;
The invention belongs to rare earth permanent-magnetic material 3D and print sintering process.
Summary of the invention
Object of the present invention, being to provide one can overall Rare-Earth Magnetic material family be raw material, be specially adapted to the manufacture of medical magnetic resonance instrument one class main equipment parts, the 3D that can dock traditional rare earth magnetic material sintering process prints Rare-Earth Magnetic material technique, and is provided for the method for preparing raw material of this technique.
Present invention process can exempt from mould development cost of manufacture, shortens fabrication cycle, can obtain the Forming Quality being better than conventional sintering technique, even reach forging quality.
The technology of the present invention official documents and correspondence is:
One, slug type 3D printer is selected to make printing device, with electro-heat equipments such as laser for thermal source.
3D printer is known technology, and " 3D printing " is the concept of a broad sense, is actually the trivial name of rapid prototyping & manufacturing technology.Though its principle is substantially identical with normal printer operation principle, the technology and the equipment that realize printing are multifarious.If most suitable known technology can not be selected to coordinate with equipment, just cannot printing be carried out, let alone research and development advanced technologies.So the selection of 3D technology and equipment, becomes starting point of the present invention.
The 3D printing technique that will propose to make sintered magnet for purposes of the present invention, so the present invention selects metal dust Direct Laser sintering technology and relevant device as enforcement instrument of the present invention.
Two, microcomputer modelling section:
The three-dimensional modeling that 3D prints is known technology, intends processing parts three-dimensional entity model, by delamination software, this model decomposition is become two dimensional planar slices by CAD software creation, then with track while scan generation software, slicing profile convert information is become laser scanning trace information.
The preparatory process that 3D prints is paving powder, and paving opaque amount is very large to printing quality influence.Paving opaque amount not only depends on operation during paving powder, but just must early excise quality control at modeling dicing phase.Powder is layering lay, the thickness that the lay thickness of every layer of powder is namely cut into slices.Cut into slices blocked up, effect that sintered body there will be " step " (forming station scalariform), profiled member form error is large, and surface quality is poor.Cut into slices thin, the making precision of profiled member is high, but paving powder difficulty increases, and the time of sintering is also spun out.Therefore, need to grasp balance between the two at sintering precision and Production Time.The present invention proposes " section differentiation strategy ": the place that namely change in shape is large or required precision is high is cut thinner, and little in change in shape or that required precision is low place is cut thicker:
Slab thicknesses: 70 ~ 100 microns
Middle thickness: 40 ~ 70 microns
Sheet thickness: 10 ~ 40 microns
Three, raw material preparation:
Present invention process needs the raw material of preparation to be rare earth permanent magnet metal dust.In view of metal dust 3D printing is the bottleneck that 3D prints at present, and magnetic prints and also to need as in conventional sintering technique orientation in magnetic field, the link magnetized is added than non-magnetic material metal, and to profiled member be magnetic can requirement, so 3D prints magnetic material the requirement stricter than common magnetic material, each performance and each procedure all will consider the impact on shaped magnet magnetic property.Present invention process requires to include following 5 aspects to material performance:
1, granularity (or claim particle diameter, refer to the mean size of powder particle):
Magnetic powder comes from the grinding of permanent-magnet alloy ingot, the HCJ of particle (characterizes permanent-magnet material and resists outside opposing magnetic field or other demagnetization effects, to keep the leading indicator of its original magnetized state ability) increase with granularity refinement, reach optimum value when a certain granularity.As overgrinding, granularity is refinement again, and HCJ can be made to decline.At present, for 3D print non-magnetic material metal dust particle diameter generally between 10 microns to 100 microns, in the majority with 30-70 micron.Experiment proves, when permanent-magnet powder granularity is 4 ~ 6 microns, coercivity and magnet density all reach maximum, realize good cooperation.Visible, the granularity requirements of magnetic material is much thinner than non-magnetic material.
2, size distribution (in powder the granule content in different-grain diameter interval, i.e. even particle distribution degree):
Because magnetic powder particle is excessive and too small all unfavorable to magnetic property, so require that size distribution wants narrower, 4 ~ 6 micron particles account for more than 80% of total particle, are greater than the < 5% of 10 microns, are less than 1 micron of i.e. nano level < 15%;
3, ensure that magnetic powder particle crystal structure is monocrystal, monocrystal rate > 98%.Only have monocrystal could obtain high-orientation when magnetic field orientating, improve profiled member magnetic property;
4, magnetic powder particle is spherical or approximate sphericity, and when being beneficial to print sintering, " the sintering neck " that solidify rear generation by liquid phase between molten solid phase particles is formed and effectively connect.Sphere is answered smooth and crystal defect is the least possible, effectively reduces sintering temperature.Spheroidizing of powder rate answers > 98%, ensures the powder uniformity;
5, the impurity of magnetic adsorption and gas should be the least possible, and especially oxygen content answers < 0.7%, and it is hard and crisp that rare earth material makes moral character, and decay resistance is poor, is very easily oxidized.Powder oxygen content and granularity are also relevant, and when granularity is less than 4 microns, the thinner oxygen content of powder is higher, so granularity is unsuitable too small.
Four, powder is spread:
Magnetic is in loose state when loading in the powder cylinder of printer forming room, and the magnetic of pine dress there will be obvious contraction when laser sintered, has impact, so successively should retain suitable space contraction surplus on sintered part form accuracy.
Five, (printing) is sintered:
Sintering is the process procedure that 3D prints most critical, carries out scanning sintering with laser head to every layer of magnetic laid.The quality of sintering depends on laser energy density, and energy density is all relevant with laser power, focal beam spot diameter, sweep speed and sweep span.
(1) basic technology strategy and parameter:
1, laser energy density: 5x100W/cm
2above;
2, laser power and focal beam spot diameter: power 100W ~ 200W, focal beam spot diameter 70 ~ 100 microns.Power is too low or hot spot is too small, and the amount of liquid phase of generation is less than normal, and melt viscosity is too high, causes sintering to worsen; Power is too high or hot spot is excessive, and liquid phase is excessive, causes " nodularization ", and sintering bath superheat is serious, produces larger thermal stress, causes distortion and cracking.
3, sweep speed: 80 microns/S ~ 160 micron/S.Speed is too high, and cause moment laser energy density minimizing, powder smelting degree declines, and molten road is not easily straight, and hole cavity is many, and " nodularization " effect is obvious.It is too much that speed too low then unit are powder absorbs energy, and melt converges, and density declines, and extends sintering time, and working (machining) efficiency is low.
4, sweep span: 0.06mm ~ 0.08mm.Just pros and cons are close for the pros and cons of sweep span size and sweep speed.Spacing is excessive as high in same rate, energy density all can be caused low, sinter uneven.The too small then energy density of spacing is high, and molten road is too crowded.
The combination of above parameter, the present invention is referred to as synthesizing evolutionary.
(2) special process strategy and parameter: the sintering between adjacent two layers is the difficult point that 3D prints technique, the present invention proposes following two strategies for this reason:
1, adjacent layer penetrates sintering strategy: after having sintered between guarantee adjacent two layers, reach good bond state, laser beam is when sintering new sinter layer, must penetrate new sinter layer reaches in sinter layer, double sintering is carried out to sinter layer, makes the refuse of upper and lower aspect bound fraction and be bonded to one.This strategy, as used popular language, can be referred to as " mutton skewered strategy ".
2, adjacent layer concave inlaid sintering strategy: uneven owing to all can occur that molten bath, Ge Rong road is formed during every layer of sintering, the injustice between adjacent layer is then more obvious.Can, when adjacent layer scans, adopt concave inlaid mode to carry out for this reason.This strategy, as used popular language, can be described as " egg concavity bubble wrap strategy ".
Accompanying drawing explanation
Accompanying drawing is that rare earth permanent-magnetic material 3D prints process chart.
Detailed description of the invention
Embodiment 1:3D prints Nd-Fe-B permanent magnetic preparation
One, equipment is selected:
Select direct sintering type 3D printer as process equipment, with electro-heat equipments such as laser for thermal source.The 3D printer selecting appropriate size (length, width and height size) is required according to permanent magnet product design.
Two, design setting model
3D prints to known technology, intends processing parts three-dimensional entity model, by delamination software, this model decomposition is become two dimensional planar slices by CAD software creation, then with track while scan generation software, slicing profile convert information is become laser scanning trace information.
Three, get the raw materials ready:
Get the neodymium iron boron powder manufactured with various powder metallurgy and flouring technology ready, feed quality requirements is:
1, granularity: 4 ~ 6 microns;
2, size distribution: the particle of 4 ~ 6 microns accounts for more than 80% of total particle, is greater than the < 5% of 10 microns, is less than 1 micron of i.e. nano level < 15%;
3, magnetic powder particle crystal structure is monocrystal, monocrystal rate > 98%;
4, magnetic powder ball rate > 98%;
5, magnetic oxygen content < 0.7%.
Four, operating process:
1, feed: ready alloy powder is loaded (pine dress) in the powder cylinder of forming room.
2, magnetize: with magnet charger or special magnetizing coil, pre-magnetizing (magnetic field orientating) is carried out to the powder in powder cylinder;
3, vacuumize: start forming room's sealing device and vacuum pump evacuation;
4, preheating: preheating is carried out to the workbench in forming room, 350 degree to 380 degree Celsius of preheat temperature;
5, be filled with protective gas: be filled with the hydrogen-argon-mixed body containing 10% hydrogen to forming room, sintering process is carried out in protective atmosphere.Stop after inflation vacuumizing to reduce power consumption.
6, the first floor (bottom) spreads powder:
Start dust feeder, handle powder cylinder piston (powder feeding piston) to rise, whitewashed by paving or powder-laying roller by ground floor (first floor) in powder horizontal sliding to the upper uniform spreading of moulding cylinder working piston or substrate (self-powered platform), and in addition compacting.Paving powder thickness 10 ~ 100 microns, is determined by the planar slice in computer.
7, first floor sintering (printing):
Sintering is the process procedure that 3D prints most critical, is performed by the optical path unit in forming room.Generating laser (laser head) is started working, computer controls the two-dimensional scan track of laser beam according to the hierarchical model of prototype, the powder that laser beam is lined by line scan on workbench selectively by the filling outline line of the first floor, next line scanning is carried out at a certain distance after the first row has scanned, complete until flood is powder sintered, powder forms the shape layer of certain thickness.The technological parameter of scanning is:
Laser energy density: 5x100W/cm
2above
Laser power: 100W ~ 200W
Focal beam spot diameter: 70 microns ~ 100 microns
Sweep speed: 80mm/s ~ 160mm/s
Sweep span: 0.06mm ~ 0.08mm
Shaping thickness: 0.03mm ~ 0.04mm
8, succeeding layer sintering:
The first floor is powder sintered complete after, workbench declines a thickness, and powder cylinder then rises certain thickness distance, and power spreading device spreads new powder at the manufactured first floor again, and the data of second layer profile called in by computer, controls laser beam and scans the sintering second layer again.Adjacent layer described in summary of the invention should be used when sintering new sinter layer to penetrate sintering and to sinter strategy with adjacent layer concave inlaid.
After the second layer completes, continue the process of paving powder-sintering, so move in circles, be layering, until three-dimensional permanent magnet is body formed.
9, cylinder and Powder Recovery is cooled out:
Namely remove forming room's sealing state after terminating, start cooling fan, make profiled member cold fast] but.Profiled member is taken out from moulding cylinder, and unsintered Powder Recovery in powder cylinder.
10, processing process:
According to product design requirement, Surface Machining process is carried out to profiled member, as polishing, polishing, plating etc.
11, magnetize:
According to designing requirement, saturation magnetization and magnetic testing are carried out to profiled member.
According to embodiment 1 neodymium iron boron magnetic body that the inventive method manufactures, through measurement performance parameter be:
Magnet density d=6.32g/cm
3, magnetic energy product BHmax=76KJ/m
3
(conventional process parameters density=6.25g/cm
3, magnetic energy product=70KJ/m
3)
Embodiment 2:3D prints samarium cobalt permanent magnet preparation
Samarium cobalt permanent magnet preparation is substantially identical with neodymium iron boron, but due to the fusing point (1495 degree Celsius of cobalt, 1935 degree Celsius of cobalt oxide) higher than the fusing point (1535 degree Celsius) of iron, the fusing point of fusing point difference also much larger than iron and neodymium of cobalt and samarium is poor, and therefore it prints sintering process method and some parameter and neodymium iron boron following difference:
1, NdFeB magnetic powder particle requirement is monocrystal, and SmCo powder is polycrystal;
2, high requirement is had to vacuum and temperature stability during SmCo powder sintering.Need in sintering process to continue to start vavuum pump, to keep the vacuum of shaping indoor.In traditional handicraft, sintering temperature is the key parameter determining magnet magnetic property.3D prints in technique, then determined by laser energy density.Density is higher, causes magnet to burn out, and on the low side, magnetic property does not reach requirement.Require during operation that laser power keeps high homogeneity, implement the aging technique standardization of height.Its parameter is:
Laser energy density: 5x120W/cm
2
Laser power: 120W ~ 220W
Focal beam spot diameter: 90 ~ 120 microns
According to embodiment 2 samarium-cobalt magnet that the present invention manufactures, through measurement performance parameter be:
Remanent magnetism Br=10.8 ~ 10.9KGs, magnetic energy product BHmax=180 ~ 200KJ/m
2)
(traditional handicraft remanent magnetism=10.5 ~ 10.8KGs, magnetic energy product=160 ~ 180kj/m
3)
Claims (1)
1. the 3D of rare earth permanent-magnetic material prints technique, it is characterized in that, comprises the following steps:
(1) select metal dust direct sintering type 3D printer as process equipment, with electro-heat equipments such as laser for thermal source;
(2) design setting model: the direct sintering type 3D printer selected by the input of part three-dimensional entity model created by CAD and delamination software;
(3) get the raw materials ready: the rare earth permanent magnet alloy powder end manufactured with various powder metallurgy and flouring technology;
(4) feed: in the powder cylinder of the direct sintering type 3D printer selected by alloy powder is loaded;
(5) preheating: to workbench preheating in forming room;
(6) powder is spread: handle powder cylinder powder feeding piston and rise, by also compacting in powder horizontal sliding to moulding cylinder working piston;
(7) (printing) is sintered: laser head work, computer controls the two-dimensional scan track of laser beam according to prototype hierarchical model, the powder that laser beam is lined by line scan on workbench selectively by filling outline line, until the powder sintered one-tenth shape layer of flood; Successively spread powder sintering again, be layering body formed to three-dimensional permanent magnet.
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| CN116833428A (en) * | 2023-08-31 | 2023-10-03 | 北京清研智束科技有限公司 | Scanning method and printing method for contour area and filling area in 3D printing |
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