CN106825551A - Silicon steel soft magnet core high based on laser sintered 3D printing and preparation method thereof - Google Patents

Silicon steel soft magnet core high based on laser sintered 3D printing and preparation method thereof Download PDF

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Publication number
CN106825551A
CN106825551A CN201611214888.4A CN201611214888A CN106825551A CN 106825551 A CN106825551 A CN 106825551A CN 201611214888 A CN201611214888 A CN 201611214888A CN 106825551 A CN106825551 A CN 106825551A
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China
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silicon
printing
silicon steel
soft magnet
magnet core
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CN201611214888.4A
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Inventor
吴朝阳
李光强
樊希安
李�杰
王万林
夏云进
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Wuhan University of Science and Engineering WUSE
Wuhan University of Science and Technology WHUST
Anhui University of Technology AHUT
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Wuhan University of Science and Engineering WUSE
Anhui University of Technology AHUT
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Priority to CN201611214888.4A priority Critical patent/CN106825551A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/145—Chemical treatment, e.g. passivation or decarburisation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/16—Metallic particles coated with a non-metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/50—Treatment of workpieces or articles during build-up, e.g. treatments applied to fused layers during build-up
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F27/00—Details of transformers or inductances, in general
    • H01F27/24—Magnetic cores
    • H01F27/255—Magnetic cores made from particles
    • 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
    • H01F41/0206—Manufacturing of magnetic cores by mechanical means
    • H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30—Process control
    • B22F10/34—Process control of powder characteristics, e.g. density, oxidation or flowability
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30—Process control
    • B22F10/36—Process control of energy beam parameters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/60—Treatment of workpieces or articles after build-up
    • B22F10/68—Cleaning or washing
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Abstract

The invention discloses a kind of silicon steel soft magnet core high based on laser sintered 3D printing and preparation method thereof, belong to silicon steel soft magnet core technical field high.The preparation technology of silicon steel soft magnet core high of the invention is comprised the following steps：Powder preparation, laser sintered 3D printing and vacuum annealing step.The present invention not only compensate for blank of the 3D printing technique in soft magnetic materials preparation, also avoid the bottleneck that existing silicon steel high is difficult to roll, and 3D printing technique is combined with vacuum annealing in addition such that it is able to improve the magnetic property of the silicon steel soft magnet core high after printing；During prepared by silicon steel soft magnet core material powder high, using the cladding last layer SiO of the high silicon iron silicon alloy powder surface even compact after siliconising low-level oxidation2Insulating barrier, it is to avoid the use of coatings, while reduce iron loss.

Description

Silicon steel soft magnet core high based on laser sintered 3D printing and preparation method thereof
Technical field
The invention belongs to silicon steel soft magnet core technical field high, beaten based on laser sintered 3D more specifically to one kind Silicon steel soft magnet core high of print and preparation method thereof.
Background technology
Silicon steel is the important soft magnetic materials of a class, and electric power and electronics industry are in manufacture motor, transformer, transformer, reactance It is all be unable to do without when device and other electrical instrumentations.Research shows, with the increase of silicone content in silicon steel, its resistivity is improved, whirlpool Stream loss is reduced, and relative permeability and magnetic induction intensity are improved, and show excellent soft magnetic characteristic, can meet electromagnetic conversion Equip the application demand of high frequency.
Generally, the eddy-current loss of silicon steel core and silicon plate thickness square are directly proportional, so to reduce silicon steel as far as possible Gauge of sheet, the mesh of eddy-current loss is reduced to reach typically by the method for rolling by its thickness control in below 1mm 's.But, when silicone content is more than 4.5wt% in silicon steel, easily cause B2 and DO3Deng the appearance of ordered phase, its plasticity and toughness is caused Drastically decline, elongation percentage is almost equal to zero, roll, be punched and be molded and be abnormal difficult, it is difficult to by pair rolling method by its thickness Within 1mm, this brings many difficulties to the exploitation and production in enormous quantities of silicon steel product high, significantly limit silicon high for control Steel large-scale promotion application industrially.
In order to be difficult to ensure that it has relatively low eddy-current loss when overcoming the shortcomings of and preparing silicon steel high using traditional rolling technique, Domestic and international researcher expands numerous studies in terms of silicon steel technology of preparing high, and thus produces various silicon steel preparation technologies high. The preparation method of current silicon steel core high mainly has：Chemical vapour deposition technique, the hot rolling-warm-rolling with rolling technique as representative- Cold-rolling process, the Near net Shaping Technology of band and double-roller rolling as representative is got rid of with single roller, the injection shaping based on powder metallurgy- Milling method and powder rolling technology etc..But these techniques or because relatively costly or because by environmental constraints or because of technical maturity Not enough or because of the problems such as stock utilization is relatively low have some limitations, therefore be not all widely used.
Such as, Chinese Patent Application No. is that 201010297551.0 application case discloses a kind of silicon steel thin belt high and its preparation Method, this application case reduces field trash and pernicious gas content in silicon steel high by vacuum metling, it is ensured that the degree of purity of molten steel, Then casting is carried out to it, 1470 DEG C~1510 DEG C of cast temperature, Cast Strip 1.5~2.0mm of thickness is carried out after going out casting roll to Cast Strip Water-spraying control, insulation, warm-rolling eventually passes recrystallization annealing and obtains product.This application case be using traditional rolling technique come Silicon steel thin belt high is prepared, but the thickness control by silicon steel product high is difficult within 1mm, so as to cause its whirlpool using the method Stream loss is still larger, it is impossible to meet the application demand that existing electromagnetic conversion equips high frequency well.
Therefore, while existing process technology is improved, the preparation technology for developing new silicon steel high is very necessary.
The content of the invention
1. the invention technical problem to be solved
It is an object of the invention to overcome due to being influenceed by silicon steel thickness of slab high limitation, its high frequency eddy current losses is of a relatively high Deficiency, there is provided a kind of silicon steel soft magnet core high based on laser sintered 3D printing and preparation method thereof.Using of the invention Method can effectively reduce the eddy-current loss of silicon steel soft magnet core high, make its on the basis of with higher magnetic permcability still have compared with Low iron loss such that it is able to meet the application demand that electromagnetic conversion equips high frequency.
2. technical scheme
To reach above-mentioned purpose, the technical scheme that the present invention is provided is：
The preparation method of a kind of silicon steel soft magnet core high based on laser sintered 3D printing of the invention, first by high silicon iron silicon Alloy powder carries out siliconising treatment, then oxidized to form fine and close SiO on high silicon iron silicon alloy powder surface2Film, by magnetic separation Obtain high silicon iron silicon alloy composite powder；Laser sintered 3D is carried out as raw material using magnetic separation gained high silicon iron silicon alloy composite powder Printing, then carries out vacuum annealing treatment and obtains final product silicon steel soft magnet core high of the invention.
Further, the specific preparation process of the high silicon iron silicon alloy composite powder is as follows：By high silicon iron silicon alloy Powder, silica flour, ammonium chloride powder and SiO 2 powder are well mixed, and are heat-treated under inert gas shielding, are heat-treated Temperature is 800~1200 DEG C, and soaking time is 0.5~5h；0.5~5h of oxidation processes at being subsequently placed in 300~700 DEG C, through magnetic Choosing treatment obtains final product high silicon iron silicon alloy composite powder.
Further, the high silicon iron silicon alloy powder, silica flour, ammonium chloride powder and SiO 2 powder account for mixed powder The degree of last gross mass is respectively 85~95wt%, 1~2wt%, 0.1~1wt% and 2~13.6wt%.
Further, the particle diameter of the high silicon iron silicon alloy powder be less than 50 μm, its Si content be 4.5~ 10.5wt%.
Further, the particle diameter of the silica flour is less than 2 μm, and the particle diameter of ammonium chloride powder is less than 1 μm, SiO 2 powder Particle diameter be less than 5 μm.
Further, described inert gas is argon gas or is nitrogen, and the oxidation processes are in air or oxygen gas Carried out under atmosphere.
Further, in the laser sintered 3D printing step, ring blank is prepared into by laser sintered 3D printing, The scan mode of 3D printing uses orthogonal scanning, and laser sintered machined parameters are：Preheating temperature is 50~80 DEG C, laser power 180~280W, sweep speed is 500~1500mm/s, and the circular material blank that laser printing is molded then is carried out into ultrasonic wave cleaning 5 ~10min, and dry base substrate in 80~150 DEG C.
Further, the temperature of the vacuum annealing treatment is 500~850 DEG C, and soaking time is 0.5~3h.
A kind of silicon steel soft magnet core high based on laser sintered 3D printing of the invention, the iron core is using side of the invention What method was prepared, and the coated with uniform of high silicon iron silicon alloy powder has one layer of SiO in the iron core2Insulating barrier.
Further, the silicon steel soft magnet core ground high relative permeability is 80~110, and saturation induction density is 147~168emu/g.
3. beneficial effect
The technical scheme provided using the present invention, compared with prior art, with following remarkable result：
(1) preparation method of a kind of silicon steel soft magnet core high based on laser sintered 3D printing of the invention, using siliconising- Low-level oxidation technique prepares high silicon iron silicon alloy composite powder, can make the cladding of high silicon iron silicon alloy powder surface even compact Last layer SiO2Insulating barrier, it is achieved thereby that insulation good between the high silicon iron silicon alloy particle of silicon steel soft magnet core high inside, can Vortex during so that silicon steel soft magnet core high being run is limited in SiO2In high silicon iron silicon alloy particle in insulating wrapped area, quite In the operating radius for reducing vortex, and then can effectively reduce the iron loss of silicon steel soft magnet core high.
(2) preparation method of a kind of silicon steel soft magnet core high based on laser sintered 3D printing of the invention, using the party Method prepares the dispersiveness of gained silicon steel soft magnet core inside high silicon iron silicon alloy particle high preferably, by SiO between alloying pellet2Absolutely Edge layer is effectively isolated, intergranular insulating properties preferably, therefore it is possible to prevente effectively from silicon steel high coatings use, while SiO2The cladding of insulating barrier can also significantly improve the heat endurance of silicon steel soft magnet core high, be conducive to extending its service life.
(3) a kind of preparation method of silicon steel soft magnet core high based on laser sintered 3D printing of the invention, the method base In laser sintered 3D printing technique, it is applied to the preparation of soft magnetic materials such that it is able to effectively avoid existing silicon steel high and be difficult to The bottleneck of rolling, without rolling, silicon steel soft magnet core high can be obtained by 3D printing technique to selective laser sintering；In addition will 3D printing technique is combined with vacuum annealing such that it is able to further improve the magnetic property of the silicon steel soft magnet core high after printing.
(4) preparation method of a kind of silicon steel soft magnet core high based on laser sintered 3D printing of the invention, it prepares work Skill is simple, and cost is relatively low, and production efficiency is high, and environmentally safe, is suitable to popularization and application.
(5) a kind of silicon steel soft magnet core high based on laser sintered 3D printing of the invention, be by siliconising-oxidation-swash Light sintering 3D printing-vacuum annealing process is prepared, and thereby may be ensured that it has while with higher magnetic permcability Relatively low iron loss and excellent thermal stability, and its mechanical strength and consistency are also preferable, service life is more long.
Specific embodiment
To further appreciate that present disclosure, in conjunction with and embodiment the present invention is described in detail.
To avoid repeating, the raw material Unify legislation for being first related to this specific embodiment is as follows, is repeated no more in embodiment：
The high silicon iron silicon alloy powder particle diameter is less than 50 μm, and the particle diameter of silica flour is less than 2 μm, and the particle diameter of ammonium chloride powder is small In 1 μm, the particle diameter of ammonium chloride powder is less than 5 μm.
Embodiment 1
First by the high silicon iron silicon alloy powder of 85wt%, the silica flour of 1wt%, the ammonium chloride powder of 0.4wt% and The SiO 2 powder of 13.6wt% is well mixed, and is then heat-treated under argon gas protection, so as to high silicon iron silicon alloy Powder carries out siliconising treatment, and its siliconising heat treatment temperature is 800 DEG C, and soaking time is 0.5h；Again at 300 DEG C, air conditionses Under, oxidation processes 5h, magnetic separation obtains high silicon iron silicon alloy composite powder, using it as laser sintered 3D printing raw material.By swashing Light sintering 3D printing is prepared into ring blank, and the scan mode of 3D printing uses orthogonal scanning, and laser sintered machined parameters are：In advance Hot temperature is 50 DEG C, and laser power 180W, sweep speed is 500mm/s, and the circular material blank ultrasonic wave that laser printing is molded is clear 10min is washed, base substrate is dried at 80 DEG C.Then the base substrate after drying is carried out into vacuum annealing treatment, annealing heat-treats temperature is 500 DEG C, soaking time is 0.5h.After testing, the silicon steel soft magnet core high based on laser sintered 3D printing in the present embodiment, with respect to magnetic Conductance is 80, and saturation induction density is 147emu/g.
The present embodiment first prepares high silicon iron silicon alloy composite powder using siliconising-low-level oxidation technique, then with high silicon iron Silicon alloy composite powder carries out laser sintered 3D printing for raw material, and silicon steel soft magnet high is prepared by vacuum annealing treatment Core, because the Surface coating of high silicon iron silicon alloy powder has one layer of SiO of densification2Insulating barrier, and can be ensured using the method SiO2The uniformity of insulating barrier cladding, SiO is passed through between the high silicon iron silicon alloy particle of silicon steel soft magnet core inside high2Insulating barrier enters Row is effectively isolated, and preferably, vortex during such that it is able to silicon steel soft magnet core high being run is limited in SiO to insulating properties2Insulating wrapped In high silicon iron silicon alloy particle in area, equivalent to the operating radius for reducing vortex, and then it is soft effectively to reduce silicon steel high The iron loss of magnetic core.Specifically, by first carrying out siliconising treatment to high silicon iron silicon alloy powder, then the iron silicon after siliconising is closed Bronze end carries out oxidation processes, such that it is able in one layer of SiO of densification of high silicon iron silicon alloy powder coated with uniform2Insulation Layer, and then improve the resistivity of high silicon iron silicon alloy powder in cladding region.Wherein, by adding appropriate SiO2Powder can Effectively to prevent silica flour from sintering, the siliconising of high silicon iron silicon alloy powder can be effectively improved by the addition of ammonium chloride powder Speed, helps lend some impetus to the progress of siliconising treatment, improve production efficiency, and the addition of itself also will not be to gained ferro-silicium The performance of powder is impacted, and is easily separated by subsequent treatment.Iron silicon can also be prevented effectively from using the method for the present invention Agglomeration in alloy powder, it is ensured that SiO there is2The uniformity and compactness of insulating barrier.
Because the dispersiveness that the present embodiment prepares gained silicon steel soft magnet core inside high silicon iron silicon alloy particle high is preferable, close By SiO between gold grain2Insulating barrier is effectively isolated, and intergranular insulating properties is preferable, therefore it is possible to prevente effectively from silicon steel high absolutely The use of edge coating, while SiO2The cladding of insulating barrier can also significantly improve the heat endurance of silicon steel soft magnet core high, favorably In its service life of extension.Therefore, gained silicon steel soft magnet core high is prepared using the method for the present embodiment while having higher Magnetic conductivity, relatively low iron loss and excellent heat endurance, disclosure satisfy that electromagnetic conversion equips the application demand of high frequency.
The present embodiment is controlled such that it is able to SiO by the numerical value to siliconising and oxidation technology parameter2Insulating barrier Thickness control effectively, therefore the selection of siliconising and oxidizing thermal treatment temperature and soaking time directly affects what is ultimately formed SiO2The thickness of insulating barrier, thus it selects the whether suitable performance for gained silicon steel soft magnet core high just most important.Hair A person of good sense optimizes design by many experiments to the numerical value of each parameter in aluminising and oxidation technology, makes SiO2The thickness of insulating barrier Optimum range is reached, such that it is able to the performance of final gained silicon steel soft magnet core high is effectively ensured.
The present embodiment is based on laser sintered 3D printing technique, is creatively applied to the preparation of soft magnetic materials, and take Preferable achievement was obtained such that it is able to effectively avoid the bottleneck that existing silicon steel high is difficult to roll, without rolling, by 3D printing skill Art can obtain silicon steel soft magnet core high to selective laser sintering.The present embodiment also mutually ties 3D printing technique with vacuum annealing Close such that it is able to further improve the magnetic property of the silicon steel soft magnet core high after printing.
Embodiment 2
First by the high silicon iron silicon alloy powder of 87wt%, the silica flour of 1.4wt%, the ammonium chloride powder of 0.6wt% and The SiO 2 powder of 11wt% is well mixed, and is then heat-treated under argon gas protection, and heat treatment temperature is 900 DEG C, is protected The warm time is 2.5h；Again at 400 DEG C, under Oxygen Condition, oxidation processes 3.5h, magnetic separation obtains high silicon iron silicon alloy composite powder End, using it as laser sintered 3D printing raw material.Ring blank, the scanning side of 3D printing are prepared into by laser sintered 3D printing Formula uses orthogonal scanning, and laser sintered machined parameters are：Preheating temperature is 55 DEG C, laser power 220W, and sweep speed is 700mm/s, the circular material blank ultrasonic wave that laser printing is molded cleans 8min, and base substrate is dried at 90 DEG C.In vacuum annealing step, Annealing heat-treats temperature is 600 DEG C, and soaking time is 1.5h, the silicon steel soft magnetism high based on laser sintered 3D printing in the present embodiment The relative permeability of iron core is 87, and saturation induction density is 154emu/g.
Embodiment 3
First by the high silicon iron silicon alloy powder of 89wt%, the silica flour of 1.4wt%, the ammonium chloride powder of 0.4wt% and The SiO 2 powder of 9.2wt% is well mixed, and is then heat-treated under nitrogen protection, and heat treatment temperature is 1100 DEG C, Soaking time is 2.5h；Again at 600 DEG C, under Oxygen Condition, oxidation processes 3.5h, magnetic separation obtains high silicon iron silicon alloy and is combined Powder, using it as laser sintered 3D printing raw material.Ring blank, the scanning of 3D printing are prepared into by laser sintered 3D printing Mode uses orthogonal scanning, and laser sintered machined parameters are：Preheating temperature is 65 DEG C, laser power 220W, and sweep speed is 900mm/s, the circular material blank ultrasonic wave that laser printing is molded cleans 7min, and base substrate is dried at 110 DEG C.Vacuum annealing step In, annealing heat-treats temperature is 700 DEG C, and soaking time is 2h, and the silicon steel high based on laser sintered 3D printing is soft in the present embodiment The relative permeability of magnetic core is 97, and saturation induction density is 160emu/g.
Embodiment 4
First by the high silicon iron silicon alloy powder of 93wt%, the silica flour of 1.6wt%, the ammonium chloride powder of 0.9wt% and The SiO 2 powder of 4.5wt% is well mixed, and is then heat-treated under nitrogen protection, and heat treatment temperature is 1200 DEG C, Soaking time is 3.5h；Again at 700 DEG C, under air conditionses, oxidation processes 2.5h, magnetic separation obtains high silicon iron silicon alloy and is combined Powder, using it as laser sintered 3D printing raw material.Ring blank, the scanning of 3D printing are prepared into by laser sintered 3D printing Mode uses orthogonal scanning, and laser sintered machined parameters are：Preheating temperature is 70 DEG C, laser power 260W, and sweep speed is 1100mm/s, the circular material blank ultrasonic wave that laser printing is molded cleans 6min, and base substrate is dried at 120 DEG C.Vacuum annealing step In, annealing heat-treats temperature is 850 DEG C, and soaking time is 2h, and the silicon steel high based on laser sintered 3D printing is soft in the present embodiment Magnetic core, relative permeability is 94, and saturation induction density is 159emu/g.
Embodiment 5
First by the high silicon iron silicon alloy powder of 95wt%, the silica flour of 2.0wt%, the ammonium chloride powder of 1wt% and 2wt% SiO 2 powder is well mixed, and is then heat-treated under argon gas protection, and heat treatment temperature is 840 DEG C, and soaking time is 5h；Again at 560 DEG C, under air conditionses, oxidation processes 0.5h, magnetic separation obtains high silicon iron silicon alloy composite powder, using its as Laser sintered 3D printing raw material.Ring blank is prepared into by laser sintered 3D printing, the scan mode of 3D printing is using orthogonal Scan, laser sintered machined parameters are：Preheating temperature is 75 DEG C, and laser power 280W, sweep speed is 1500mm/s, by laser The circular material blank ultrasonic wave cleaning 5min of printing shaping, base substrate is dried at 120 DEG C.In vacuum annealing step, annealing heat-treats temperature It is 55 DEG C to spend, and soaking time is 3h, the silicon steel soft magnet core high based on laser sintered 3D printing, relative permeability in the present embodiment It is 103, saturation induction density is 161emu/g.
Embodiment 6
First by the high silicon iron silicon alloy powder of 88wt%, the silica flour of 1.7wt%, the ammonium chloride powder of 0.3wt% and The SiO 2 powder of 10wt% is well mixed, and is then heat-treated under nitrogen protection, and heat treatment temperature is 1050 DEG C, is protected The warm time is 1h；Again at 480 DEG C, under Oxygen Condition, oxidation processes 2h, magnetic separation obtains high silicon iron silicon alloy composite powder, with It is used as laser sintered 3D printing raw material.Ring blank is prepared into by laser sintered 3D printing, the scan mode of 3D printing is adopted With orthogonal scanning, laser sintered machined parameters are：Preheating temperature is 80 DEG C, and laser power 210W, sweep speed is 800mm/s, The circular material blank ultrasonic wave that laser printing is molded cleans 8.5min, and base substrate is dried at 130 DEG C.In vacuum annealing step, annealing Heat treatment temperature is 810 DEG C, and soaking time is 0.7h, the silicon steel soft magnet high based on laser sintered 3D printing in the present embodiment Core, relative permeability is 82, and saturation induction density is 148emu/g.
Embodiment 7
First by the high silicon iron silicon alloy powder of 93wt%, the silica flour of 1.6wt%, the ammonium chloride powder of 0.1wt% and The SiO 2 powder of 5.3wt% is well mixed, and is then heat-treated under nitrogen protection, and heat treatment temperature is 1080 DEG C, Soaking time is 4h；Again at 320 DEG C, under air conditionses, oxidation processes 0.5h, magnetic separation obtains high silicon iron silicon alloy composite powder End, using it as laser sintered 3D printing raw material.Ring blank, the scanning side of 3D printing are prepared into by laser sintered 3D printing Formula uses orthogonal scanning, and laser sintered machined parameters are：Preheating temperature is 54 DEG C, laser power 270W, and sweep speed is 1200mm/s, the circular material blank ultrasonic wave that laser printing is molded cleans 9.5min, and base substrate is dried at 150 DEG C.Vacuum annealing is walked In rapid, annealing heat-treats temperature is 670 DEG C, and soaking time is 1.3h, the silicon high based on laser sintered 3D printing in the present embodiment Steel soft magnet core, relative permeability is 100, and saturation induction density is 162emu/g.
Embodiment 8
First by the high silicon iron silicon alloy powder of 92wt%, the silica flour of 1.5wt%, 0.5wt% ammonium chloride powder and 6wt% SiO 2 powder be well mixed, then argon gas protection under be heat-treated, heat treatment temperature be 960 DEG C, soaking time It is 3h；Again at 610 DEG C, under Oxygen Condition, oxidation processes 3h, magnetic separation obtains high silicon iron silicon alloy composite powder, using its as Laser sintered 3D printing raw material.Ring blank is prepared into by laser sintered 3D printing, the scan mode of 3D printing is using orthogonal Scan, laser sintered machined parameters are：Preheating temperature is 76 DEG C, and laser power 245W, sweep speed is 1400mm/s, by laser The circular material blank ultrasonic wave cleaning 6.5min of printing shaping, base substrate is dried at 125 DEG C.In vacuum annealing step, annealing heat-treats Temperature is 83 DEG C, and soaking time is 2.5h, the silicon steel soft magnet core high based on laser sintered 3D printing in the present embodiment, with respect to magnetic Conductance is 110, and saturation induction density is 168emu/g.
In sum, using technical scheme, there can be higher magnetic permcability silicon steel soft magnet core high is ensured On the basis of, its iron loss is significantly reduced, while being also avoided that the use of coatings in existing silicon steel high, improve silicon steel high soft The heat endurance of magnetic core, and extend its service life.The present invention is also innovatively by laser sintered 3D printing technique application In in the production of silicon steel soft magnet core high, not only compensate for blank of the 3D printing technique in soft magnetic materials preparation, also avoid Existing silicon steel high is difficult to the bottleneck for rolling, and without rolling, silicon steel high can be obtained to selective laser sintering by 3D printing technique Soft magnet core, its preparation process is simple, efficiency high, and it is environmentally safe.

Claims (10)

1. a kind of preparation method of the silicon steel soft magnet core high based on laser sintered 3D printing, it is characterised in that：First by high silicon iron Silicon alloy powder carries out siliconising treatment, then oxidized to form fine and close SiO on high silicon iron silicon alloy powder surface2Film, by magnetic Choosing obtains high silicon iron silicon alloy composite powder；Carried out as raw material using magnetic separation gained high silicon iron silicon alloy composite powder laser sintered 3D printing, then carries out vacuum annealing treatment and obtains final product silicon steel soft magnet core high of the invention.
2. the preparation method of a kind of silicon steel soft magnet core high based on laser sintered 3D printing according to claim 1, its It is characterised by, the specific preparation process of the high silicon iron silicon alloy composite powder is as follows：By high silicon iron silicon alloy powder, silica flour, Ammonium chloride powder and SiO 2 powder are well mixed, are heat-treated under inert gas shielding, and heat treatment temperature is 800~ 1200 DEG C, soaking time is 0.5~5h；0.5~5h of oxidation processes at being subsequently placed in 300~700 DEG C, height is obtained final product through magnetic separation treatment Ferrosilicon silicon alloy composite powder.
3. the preparation method of a kind of silicon steel soft magnet core high based on laser sintered 3D printing according to claim 2, its It is characterised by：The high silicon iron silicon alloy powder, silica flour, ammonium chloride powder and SiO 2 powder account for mixed-powder gross mass Degree is respectively 85~95wt%, 1~2wt%, 0.1~1wt% and 2~13.6wt%.
4. the preparation method of a kind of silicon steel soft magnet core high based on laser sintered 3D printing according to Claims 2 or 3, It is characterized in that：The particle diameter of the high silicon iron silicon alloy powder is less than 50 μm, and its Si content is 4.5~10.5wt%.
5. the preparation method of a kind of silicon steel soft magnet core high based on laser sintered 3D printing according to Claims 2 or 3, It is characterized in that：The particle diameter of the silica flour is less than 2 μm, and the particle diameter of ammonium chloride powder is less than 1 μm, and the particle diameter of SiO 2 powder is small In 5 μm.
6. the preparation method of a kind of silicon steel soft magnet core high based on laser sintered 3D printing according to Claims 2 or 3, It is characterized in that：Described inert gas is argon gas or is nitrogen, and the oxidation processes are carried out under air or oxygen atmosphere 's.
7. the system of a kind of silicon steel soft magnet core high based on laser sintered 3D printing according to any one of claim 1-3 Preparation Method, it is characterised in that：In the laser sintered 3D printing step, ring blank is prepared into by laser sintered 3D printing, The scan mode of 3D printing uses orthogonal scanning, and laser sintered machined parameters are：Preheating temperature is 50~80 DEG C, laser power 180~280W, sweep speed is 500~1500mm/s, and the circular material blank that laser printing is molded then is carried out into ultrasonic wave cleaning 5 ~10min, and dry base substrate in 80~150 DEG C.
8. the preparation method of a kind of silicon steel soft magnet core high based on laser sintered 3D printing according to claim 7, its It is characterised by：The temperature of the vacuum annealing treatment is 500~850 DEG C, and soaking time is 0.5~3h.
9. a kind of silicon steel soft magnet core high based on laser sintered 3D printing, it is characterised in that：The iron core is to use claim What the method any one of 1-8 was prepared, and there be the coated with uniform of high silicon iron silicon alloy powder in the iron core One layer of SiO2Insulating barrier.
10. a kind of silicon steel soft magnet core high based on laser sintered 3D printing according to claim 9, it is characterised in that： The silicon steel soft magnet core ground high relative permeability is 80~110, and saturation induction density is 147~168emu/g.
CN201611214888.4A 2016-12-26 2016-12-26 Silicon steel soft magnet core high based on laser sintered 3D printing and preparation method thereof Pending CN106825551A (en)

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Application publication date: 20170613