CN104889390B - The 3D printing technique of rare earth permanent-magnetic material - Google Patents

The 3D printing technique of rare earth permanent-magnetic material Download PDF

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CN104889390B
CN104889390B CN201410078399.5A CN201410078399A CN104889390B CN 104889390 B CN104889390 B CN 104889390B CN 201410078399 A CN201410078399 A CN 201410078399A CN 104889390 B CN104889390 B CN 104889390B
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powder
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sintering
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microns
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张瑞龙
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus 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
    • H01F41/02Apparatus 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
    • H01F41/0253Apparatus 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets 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
    • H01F1/04Magnets 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571Alloys 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
    • H01F1/0575Alloys 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
    • H01F1/0577Alloys 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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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Hard Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a kind of 3D printing technique of rare earth permanent-magnetic material, selection metal dust direct sintering type 3D printer is as process equipment, using electro-heat equipments such as laser as thermal source, the planar slice figure input 3D printer that microcomputer modelling is obtained.The pre-alloyed powder that rare earth permanent-magnetic material is made of powder metallurgy and flouring technology is fitted into printer powder cylinder.After powdering, computer operating laser head controls the two-dimensional scan track of laser beam according to prototype hierarchical model, and laser beam is by filling contour line successively scanning sintering line by line, and it is body formed to be finally superimposed to three-dimensional permanent magnet, cools down out cylinder.Forming room's working environment is preheating and vacuum, is filled with protectiveness hydrogen argon gas.It can be magnetized before and after sintering.Present invention process is applied to all rare earth permanent-magnetic materials, by selecting the printer of big-and-middle specification to make the permanent magnet of big-and-middle size.Exempt from mould development cost of manufacture, shorten fabrication cycle, the Forming Quality better than conventional sintering technique, even up to forging quality can be obtained.

Description

The 3D printing technique of rare earth permanent-magnetic material
Technical field
The present invention relates to a kind of 3D printing technique of rare earth permanent-magnetic material
Background technology
Currently, the 3D printing technique fashionable whole world.Futurist predicts that it may lead manufacturing industry new trend, starts the 3rd The secondary industrial revolution.Because the technology is original in western developed country, the intellectual property about technique is generally that foreign corporation holds at present Have, future, Chinese Enterprises deeply will enter this field, it is necessary to pay high patent fee, or produce many patent disputes.Cause This, in face of 3D printing upsurge, China is badly in need of trying hard to catch up, and relevant invention conception is opened up as early as possible, implementing process is researched and developed, is formed as early as possible The own 3D printing intellectual property system of China.
At present, 3D printing fails to carry out on a large scale, is due to most widely used manufacturing industry, and most of industrial parts are needed It is made of metal material, and the preparation due to metal dust print material and printing technology are complicated more than plastics, resin, form 3D and beat Print and distribute the bottleneck of exhibition.In other words, to allow 3D printing really to equip with arms huge manufacturing industry, metal dust print must be solved as early as possible Material is prepared and relevant printing technology.
In metal dust, especially using rare earth permanent-magnetic material to lead new material.Permanent-magnet material be do not need consumed energy and The magnetic functional material in its magnetic field can be kept, rare earth permanent-magnetic material is the main product of permanent-magnet material, is widely used in modern crafts With in science and technology.Because rare earth resources nearly 80% are in China, China will turn into rare earth permanent-magnetic material production and develop 21 century Base and center.And the development and application of new material, it is the high and new technology field that national industrial policies are encouraged energetically.
In rare earth permanent-magnetic material family, neodymium iron boron is high (being referred to as " magnetic king ") due to magnetic property, and relative price is relatively low, thus It is used widely.Consumption it is maximum be electronic information industry, separate unit consumption maximum be then Medical Devices industry magnetic resonance into As instrument, main magnet can have more than ten tons of weight.
On June 26th, 2013, Chinese invention patent CN103170628A (calling in the following text " invention ") discloses a kind of based on 3D The neodymium iron boron preparation method of printing technique, proposes 3D printing technique to be applied to neodymium iron boron, expands 3D printing in metal first Selection on powder print material.The invention and the difference of the present invention are:
Though the 1, neodymium iron boron is most widely used in rare earth permanent-magnetic material, it is one kind of Rare-Earth Magnetic material, category after all In rare-earth-iron system.Also numerous series such as rare earth SmCo, praseodymium iron copper boron.As the cross membership of Rare-Earth Magnetic material family, it Suffer from identical material characteristics, should have more inventions that 3D printing application is expanded to whole Rare-Earth Magnetic material family.
2nd, the invention related products are the small and special electric machine (see the abstract of invention) of " small-sized, ultra-thin ", and the present invention is to cure It is target with large-scale, polynary, the high level product of magnetic resonance device main magnet, there is bigger accommodation.
3rd, the conventional preparation techniques of Rare-Earth Magnetic material are divided into sintering, bonded and three kinds of thermal deformation, the wherein magnetic of sintered magnet Can be higher, and bonding magnetic material comparison of magnetic property is stable.Sintering process need to surpassing thousand degree of high temperature sinterings, and the invention be with 20~ 900 degrees Centigrade workbench, need to carry out beyond invention category if it need to sinter, the invented technology system is also confirmed in specification What is made is " Agglutinate neodymium-iron-boron ", should belong to a kind of heating and bond new technology.And the present invention is then conventional sintering technique and 3D printing pair The new technology connect, technological process has very big difference with the invention, therefore is two distinct types of technique with the invention.
4th, just because of the invention is binding type technique, so the neodymium iron boron granulation of its raw material is mechanical mixture powder, and And need to add binding agent, and present invention process is alloy smelting powder, and binding agent need not be added.
In summary, the invention belongs to neodymium iron boron 3D printing non-sintered technique;
The invention belongs to rare earth permanent-magnetic material 3D printing sintering process.
The content of the invention
The purpose of the present invention, be to provide one kind can overall Rare-Earth Magnetic material family be raw material, be particularly suitable for use in medical magnetic and be total to The class large scale equipment parts of Vibration Meter one are manufactured, and can dock the 3D printing Rare-Earth Magnetic material technique of traditional rare earth magnetic material sintering process, and Method for preparing raw material for the technique is provided.
Present invention process can exempt from mould development cost of manufacture, shorten fabrication cycle, can obtain better than conventional sintering technique Forming Quality, even up to forging quality.
The technology of the present invention official documents and correspondence is:
First, selection slug type 3D printer makees printing device, using electro-heat equipments such as laser as thermal source.
3D printer is known technology, and " 3D printing " is the concept of a broad sense, actually rapid prototyping & manufacturing technology Trivial name.Though its principle and normal printer operation principle are essentially identical, the technology and equipment five for realizing printing are spent Eight.If most suitable known technology can not be selected to coordinate with equipment, printing can not be just carried out, let alone research and development are first Enter technique.So, the selection of 3D technology and equipment, the starting point as the present invention.
It is the 3D printing technique that propose to make sintered magnet for purposes of the present invention, so, present invention selection metal Powder Direct Laser sintering technology and relevant device are used as the instrument for implementing the present invention.
2nd, microcomputer modelling is cut into slices:
The three-dimensional modeling of 3D printing is known technology, is created with CAD software and intends processing part three-dimensional entity model, with layering Slicing profile information is changed into laser and swept by the model decomposition by software into two dimensional planar slices, then with scanning Track Pick-up software Retouch trace information.
The preparatory process of 3D printing is powdering, and powdering quality influences very big to print quality.Powdering quality is not only depended on Operation during powdering, but just must early excise quality control in modeling dicing phase.Powder is that layering is laid, every layer of powder The thickness that the lay thickness at end is namely cut into slices.Section is blocked up, and " step " effect (being formed step-like), shaping occurs in sintered body Part form error is big, and surface quality is poor.Section is excessively thin, and the making precision of molding part is high, but the increase of powdering difficulty, the time of sintering Also spin out.Accordingly, it would be desirable to grasp balance between the two in sintering precision and Production Time.The present invention proposes " section difference plan Slightly ":The place that i.e. change in shape is big or required precision is high is cut thinner, is cut in the place that change in shape is small or required precision is low It is thick:
Slab thicknesses:70~100 microns
Middle thickness:40~70 microns
Sheet thickness:10~40 microns
3rd, prepared by raw material:
Present invention process needs the raw material prepared to be rare earth permanent magnet metal dust.In view of metal dust 3D printing is currently 3D The bottleneck of printing, and magnetic printing also needs to be orientated in magnetic field as in conventional sintering technique, increases than non-magnetic material metal Add the link magnetized, and the requirement for the energy that is magnetic to molding part, so 3D printing magnetic material has more tightened up than common magnetic material Requirement, each single item performance and each procedure will consider the influence to shaped magnet magnetic property.Present invention process is to raw material Performance require to include it is following 5 aspect:
1st, granularity (or particle diameter, refer to the mean size of powder particle):
Magnetic powder comes from the grinding of permanent-magnet alloy ingot, and the HCJ of particle (characterizes permanent-magnet material resistance outside reversely Magnetic field or other demagnetization effects, to keep the leading indicator of its original magnetization state capabilities) increase with granularity refinement, a certain Optimum value is reached during granularity.Such as overgrinding, granularity is refined again, can decline HCJ.It is presently used for the non-of 3D printing Magnetic material metal dust particle diameter is universal between 10 microns to 100 microns, in the majority with 30-70 microns.It is demonstrated experimentally that permanent-magnet powder grain Spend for 4~6 microns when, coercivity and magnet density all reach maximum, realize good cooperation.It can be seen that, the granularity of magnetic material will Ask much thinner than non-magnetic material.
2nd, size distribution (the interval granule content of different-grain diameter, i.e. even particle distribution degree in powder):
Due to magnetic powder particle it is excessive with it is too small unfavorable to magnetic property, it requires that size distribution wants narrower, 4~6 is micro- Rice grain accounts for more than the 80% of total particle, the < 5% more than 10 microns, is nano level < 15% less than 1 micron;
3rd, it is monocrystal, monocrystal rate > 98% to ensure magnetic powder particle crystal structure.Only monocrystal is in magnetic field orientating High-orientation could be obtained, molding part magnetic property is improved;
4th, magnetic powder particle is in spherical or approximate sphericity, during in favor of printing sintering, solidifying by liquid phase between molten solid phase particles Gu after the effective connection of " sintering neck " formation that generates.Sphere is answered smooth and crystal defect is as few as possible, effectively reduces sintering temperature. Spheroidizing of powder rate answers > 98%, it is ensured that the powder uniformity;
5th, the impurity and gas of magnetic adsorption should lack as far as possible, and especially oxygen content answers < 0.7%, rare earth material system Hard and crisp into moral character, decay resistance is poor, easily aoxidizes.Powder oxygen content is also relevant with granularity, and granularity is less than 4 microns When, powder is thinner, and oxygen content is higher, so granularity is unsuitable too small.
4th, powdering:
Loose state is in when magnetic is loaded in the powder cylinder of printer forming room, the magnetic of pine dress is when laser sintered Obvious contraction occurs, can have an impact to sintered part form accuracy, so should successively retain appropriate space contraction surplus.
5th, (printing) is sintered:
Sintering is the process procedure of 3D printing most critical, and sintering is scanned to the magnetic that every layer lays with laser head. The quality of sintering depends on laser energy density, and energy density and laser power, focal beam spot diameter, sweep speed and scanning Spacing is all relevant.
(1) basic technology strategy and parameter:
1st, laser energy density:5x100W/cm2More than;
2nd, laser power and focal beam spot diameter:Power 100W~200W, 70~100 microns of focal beam spot diameter.Power 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 deteriorate;Power is too high or hot spot is excessive, Liquid phase is excessive, causes " nodularization ", and sintering bath superheat is serious, produces larger thermal stress, causes to deform and ftracture.
3rd, sweep speed:80 microns/S~160 micron/S.Speed is too high, causes moment laser energy density to reduce, powder Fusing degree decline, molten road be difficult it is straight, hole cavity it is many, " nodularization " effect is obvious.The too low then unit area powder of speed is inhaled Receive energy excessive, melt convergence, consistency declines, and extends sintering time, and processing efficiency is low.
4th, sweep span:0.06mm~0.08mm.The pros and cons of sweep span size are approached with sweep speed height pros and cons.Between It is high away from excessive such as same rate, it can all cause energy density low, sinter uneven.The too small then energy density of spacing is high, and molten road is excessively It is crowded.
The combination of above parameter, the present invention is referred to as synthesizing evolutionary.
(2) special process strategy and parameter:Sintering between adjacent two layers is the difficult point of 3D printing technique, is this present invention Propose following two strategies:
1st, adjacent layer penetrates sintering strategy:To reach good bond state after the completion of being sintered between guarantee adjacent two layers, swash Light beam is when sintering new sinter layer, it is necessary to penetrates new sinter layer and reaches in sinter layer, carries out double sintering to sinter layer, makes Up and down the refuse of aspect bound fraction and be bonded to one.This strategy such as uses popular language, can be referred to as " mutton skewered plan Slightly ".
2nd, adjacent layer concave inlaid sintering strategy:Can all occur the bumps of Ge Rong roads molten bath formation during due to every layer of sintering not Flat, the injustice between adjacent layer then becomes apparent.It can be carried out for this when adjacent layer is scanned using concave inlaid mode.This plan Popular language is slightly such as used, be can be described as " egg concavity bubble wrap strategy ".
Brief description of the drawings
Accompanying drawing is rare earth permanent-magnetic material 3D printing process chart.
Embodiment
Embodiment 1:3D printing Nd-Fe-B permanent magnetic preparation
First, equipment is selected:
Direct sintering type 3D printer is selected as process equipment, using electro-heat equipments such as laser as thermal source.According to permanent magnet Product design requires the 3D printer of selection appropriate size (length, width and height size).
2nd, design setting model
3D printing is known technology, is created with CAD software and intends processing part three-dimensional entity model, with delamination software by the mould Type resolves into two dimensional planar slices, then slicing profile information is changed into laser scanning track with scanning Track Pick-up software believed Breath.
3rd, get the raw materials ready:
Get the neodymium iron boron powder manufactured with various powder metallurgy and flouring technology ready, feed quality requirements are:
1st, granularity:4~6 microns;
2nd, size distribution:4~6 microns of particle accounts for more than the 80% of total particle, the < 5% more than 10 microns, micro- less than 1 Rice is nano level < 15%;
3rd, magnetic powder particle crystal structure is monocrystal, monocrystal rate > 98%;
4th, magnetic Oxygen potential > 98%;
5th, magnetic oxygen content < 0.7%.
4th, operating process:
1st, feed:Ready alloy powder is fitted into the powder cylinder of forming room (pine dress).
2nd, magnetize:Pre-magnetizing (magnetic field orientating) is carried out to the powder in powder cylinder with magnet charger or special magnetizing coil;
3rd, vacuumize:Start shaping chamber sealing device to vacuumize with vavuum pump;
4th, preheat:Workbench in forming room is preheated, 350 degree to 380 degree Celsius of preheating temperature;
5th, it is filled with protective gas:The hydrogen-argon-mixed body containing 10% hydrogen is filled with to forming room, makes sintering process in guarantor Protect in atmosphere and carry out.Stop vacuumizing to reduce power consumption after inflation.
6th, the first floor (bottom) powdering:
Start dust feeder, manipulate powder cylinder piston (powder feeding piston) and rise, by powdering brush or powder-laying roller by powder horizontal sliding Uniformly first layer (first floor) is spread, and be compacted on to moulding cylinder working piston or substrate (self-powered platform).Powdering thickness 10~100 microns, determined by the planar slice in computer.
7th, first floor sintering (printing):
Sintering is the process procedure of 3D printing most critical, and the optical path unit in forming room is performed.Generating laser (laser Head) to start working, computer controls the two-dimensional scan track of laser beam according to the hierarchical model of prototype, and laser beam is filled out as the first floor Fill contour line and selectively progressively scan powder on workbench, carrying out next line at a certain distance after the completion of the first row scanning sweeps Retouch, completed until flood is powder sintered, powder forms the shape layer of certain thickness.The technological parameter of scanning is:
Laser energy density:5x100W/cm2More than
Laser power:100W~200W
Focal beam spot diameter:70 microns~100 microns
Sweep speed:80mm/s~160mm/s
Sweep span:0.06mm~0.08mm
It is molded thickness:0.03mm~0.04mm
8th, succeeding layer is sintered:
After the completion of the first floor is powder sintered, workbench declines a thickness, and powder cylinder then rises certain thickness distance, powdering Device spreads new powder in the manufactured first floor again, and computer calls in the data of second layer profile, and control laser beam scans burning again Tie the second layer.Adjacent layer described in the content of the invention should be used to penetrate sintering when sintering new sinter layer to sinter with adjacent layer concave inlaid Strategy.
After the completion of the second layer, continue the process of powdering-sintering, so move in circles, be layering, until three-dimensional permanent magnet body Shaping.
9th, cylinder and Powder Recovery are cooled down out:
Forming room sealing state is released after terminating, starts cooling fan, the fast quickly cooling of molding part is allowed] but.From shaping Cylinder takes out molding part, and unsintered Powder Recovery into powder cylinder.
10th, working process:
Required according to product design, Surface Machining processing is carried out to molding part, such as polished, polish, electroplate.
11st, magnetize:
Saturation is carried out according to design requirement to molding part to magnetize and magnetic testing.
The neodymium iron boron magnetic body of embodiment 1 manufactured according to the inventive method, be through measurement performance parameter:
Magnet density d=6.32g/cm3, magnetic energy product BHmax=76KJ/m3
(conventional process parameters density=6.25g/cm3, magnetic energy product=70KJ/m3)
Embodiment 2:3D printing samarium cobalt permanent magnet preparation
Samarium cobalt permanent magnet preparation is substantially the same with neodymium iron boron, but (1495 degree Celsius, cobalt oxide is taken the photograph due to the fusing point of cobalt 1935 degree of family name) it is (1535 degree Celsius) higher than the fusing point of iron, the fusing point difference of cobalt and samarium is poor also much larger than the fusing point of iron and neodymium, therefore its Printing sintering process method and some parameters have following difference with neodymium iron boron:
1st, NdFeB magnetic powder particle requirement is monocrystal, and SmCo powder is polycrystal;
2nd, there is high requirement to vacuum and temperature stability during SmCo powder sintering.Lasting startup vacuum is needed in sintering process Pump, to keep the vacuum that shaping is indoor.In traditional handicraft, sintering temperature is the key parameter for determining magnet magnetic property.3D is beaten Print in technique, then determined by laser energy density.Density is higher, causes magnet to burn out, relatively low, and magnetic property does not reach requirement. Require that laser power keeps high homogeneity during operation, implement the aging technique standardization of height.Its parameter is:
Laser energy density:5x120W/cm2
Laser power:120W~220W
Focal beam spot diameter:90~120 microns
According to the samarium-cobalt magnet of embodiment 2 produced by the present invention, it is through measurement performance parameter:
Remanent magnetism Br=10.8~10.9KGs, magnetic energy product BHmax=180~200KJ/m2)
(traditional handicraft remanent magnetism=10.5~10.8KGs, magnetic energy product=160~180kj/m3)

Claims (1)

1. the 3D printing technique of rare earth permanent-magnetic material, it is characterised in that comprise the following steps:
(1) selection metal dust direct sintering type 3D printer is as process equipment, using laser electro-heat equipment as thermal source;
(2) design setting model:The direct sintering type 3D selected by the input of part three-dimensional entity model created with CAD and delamination software is beaten Print machine;
(3) get the raw materials ready:The SmCo powder manufactured with various powder metallurgy and flouring technology, feed quality requirements are:
1st, granularity:4~6 microns;
2nd, size distribution:4~6 microns of particle accounts for more than the 80% of total particle, the < 5% more than 10 microns, less than 1 micron i.e. Nano level < 15%;
3rd, magnetic powder particle crystal structure is polycrystal;
4th, magnetic Oxygen potential > 98%;
5th, magnetic amount of oxidation < 0.7%;
(4) feed:In the powder cylinder for alloy powder being fitted into selected direct sintering type 3D printer;
(5) magnetize:Pre-magnetizing is carried out to the powder in powder cylinder with magnet charger or special magnetizing coil;
(6) vacuumize:Start shaping chamber sealing device to vacuumize with vavuum pump, and persistently start vacuum in whole sintering process Pump;
(7) preheat:Workbench in forming room is preheated, 350 DEG C to 380 DEG C of preheating temperature;
(8) powdering:Manipulate powder cylinder powder feeding piston to rise, in powder horizontal sliding to moulding cylinder working piston and will be compacted, powdering is thick 10~100 microns of degree, is determined by the planar slice in computer;
(9) (printing) is sintered:Laser head works, and computer controls the two-dimensional scan track of laser beam according to prototype hierarchical model, Laser beam is selectively progressively scanned the powder on workbench by filling contour line, is entered at a certain distance after the completion of the first row scanning Row next line is scanned, until flood is powder sintered into shape layer, then successively powdering is sintered, be layering to three-dimensional permanent magnet body into Type, the technological parameter of scanning is:
Laser energy density:5×120W/cm2
Laser power:120W~220W
Focal beam spot diameter:90~120 microns;
(10) cylinder and Powder Recovery are cooled down out:I.e. contact moudling room sealing state after terminating, starts cooling fan, allows shaping Part is quickly cooled down;Molding part is taken out from moulding cylinder, and unsintered milling is recovered in powder cylinder;
(11) working process:Required according to product design, Surface Machining processing is carried out to molding part, wherein, the Surface Machining Processing includes polishing, polishing, plating;
(12) magnetize:According to design requirement, saturation is carried out to molding part and magnetized and magnetic testing.
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