CN106024238A - Gadolinium/yttrium-ion-implanted zinc-plated neodymium-iron-boron magnet and preparation method thereof - Google Patents

Gadolinium/yttrium-ion-implanted zinc-plated neodymium-iron-boron magnet and preparation method thereof Download PDF

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CN106024238A
CN106024238A CN201610555139.1A CN201610555139A CN106024238A CN 106024238 A CN106024238 A CN 106024238A CN 201610555139 A CN201610555139 A CN 201610555139A CN 106024238 A CN106024238 A CN 106024238A
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magnet
neodymium
iron
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boron
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唐睿
沈军
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Anhui One Magnet Electronic Co Ltd
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Abstract

The invention discloses a gadolinium/yttrium-ion-implanted zinc-plated neodymium-iron-boron magnet which is composed of the following components in percentage by mass: 25-35% of Pr-Nd, 0.5-1.5% of B, 0.1-1% of Al, 0-0.2% of Cu, 1-2% of Co, 0.1-1% of Ga, 0.02-0.08% of Nb, 0.01-0.05% of Zr, 0.1-1% of mesoporous silicon dioxide, and the balance of Fe and small amounts of inevitable impurities in the material. The sintered neodymium-iron-boron magnet has uniform crystal form structure; the heavy rare earth content in the region adjacent to the magnet core is lower, thereby preventing the magnetic remanence of the magnet from being influenced basically; the heavy rare earth content in the region adjacent to the magnet surface is higher, thereby obviously enhancing the coercivity of the magnet; and the defects of the neodymium-iron-boron sintered magnet are comprehensively improved, and the advantages are greatly enhanced.

Description

A kind of galvanized neodymium-iron-boron magnet of gadolinium yttrium ion implantation and preparation method thereof
Technical field
The present invention relates to rare-earth permanent-magnet material technical field, particularly relate to the zinc-plated neodymium ferrum of a kind of gadolinium yttrium ion implantation Boron magnet and preparation method thereof.
Background technology
Nd-Fe-B permanent magnet material, as the latest result of rare earth permanent-magnetic material development, due to the magnetic property of its excellence And it is referred to as magnetic king, and it is the permanent magnet at present with the strongest magnetic force, its maximum magnetic energy product exceeds ferrite 10 More than Bei, there is small in volume, high magnetic energy product and coercivity, energy density advantages of higher so that Nd-Fe-B permanent magnet material is applied widely in modern industry and electronic technology.
Recently as neodymium iron boron magnetic body at multi-field high speed development, Sintered NdFeB magnet is with superior performance It is widely used in each side, so that computer hardware, instrument and meter, electroacoustic motor, sensor, magnetic separation The miniaturization of equipment, lightweight, the slimmings such as magnetization are possibly realized.Due to micron order neodymium iron boron magnetic body raw material powder The interaction of Van der Waals force, London forces and magnetic force between end makes powder easily be agglomerated into secondary powder particle, Define little granule group, cause the poor fluidity of powder, orientation difficulty, cause in final magnet crystal boundary rich dilute Soil phase disappearance or discontinuous, carry out affecting when grain boundary decision processes the heavy rare earth elements such as Dy/Tb along crystal boundary to Diffusion effect within magnet.
Chinese invention patent CN105702405A is pioneering uses nanoscale mesoporous material to add neodymium iron boron magnetic body to Material improves its micro structure and fault of construction, thus improves its coercivity and operating temperature, have an advantage in that Processing technique is simple, crystalline structure is homogeneous, magnet material coercivity is strong, temperature tolerance good, but it does not improve The shortcoming of the easy oxidized corrosion of neodymium iron boron magnetic body.
Have the requirement of high energy product and high-coercive force for meeting neodymium iron boron magnetic body, direct mode is a large amount of simultaneously Add the heavy rare earth elements such as Dy/Tb, but in magnet, add too much Dy can be formed instead because of Dy Yu Fe Ferromagnetic coupling, causes the remanent magnetism of magnet can decline along with the increase of Dy, and heavy rare earth element scarcity of resources, Expensive, produce high coercivity magnetic with existing technique and know from experience raising cost and aggravation resource consumption.Sintering neodymium ferrum Boron grain boundary diffusion process is to start from surface internally to permeate under the neodymium iron boron green state of sinter molding, Avoid the problem that in principal phase, heavy rare earth content is too much, it is possible to while damaging remanent magnetism hardly, magnetic is greatly improved Body coercivity, the content of heavy rare earth element significantly reduces simultaneously；But heavy rare earth can only be at the blank sintered Diffusion into the surface result in that heavy rare earth is limited in the diffusion depth within magnet, heavy rare earth concentration is from outward appearance to inner essence in decay Formula Gradient distribution.
Chinese invention patent CN105742048A uses the mode of energetic ion that rare earth and alloy are injected neodymium ferrum Boron presintered compact, solve existing grain boundary decision technology middle rare earth and alloy more remain in neodymium-iron-boron body surface Face, the problem that rare earth practical efficiency is the highest, but it simply improves the diffuser efficiency of rare earth alloy, weight The random proportioning of rare earth metal and common metal not only makes rich-Nd phase in magnet grain boundary structure complexity, crystal boundary lack Lose and discontinuous, finally affect the heavy rare earth elements such as Dy/Tb along crystal boundary to the effect of magnet diffusion inside, real The coercivity of neodymium iron boron magnetic body is not increased substantially on border.
Start with, by micron order material powder for this present invention neodymium iron boron magnetic body material powder after airflow milling grinds First carry out plating zinc on surface, particle surface one layer of nanoscale zinc layers of cladding, then mix with mesoporous silicon oxide and take Heavy rare earth alloy, more sintered densification crystal boundary occurs is injected with energetic ion form after pressed compact, presintered compact Diffusion, improves magnet border structure, thus improves the coercivity of Sintered NdFeB magnet.
Summary of the invention
The present invention is to make up the deficiencies in the prior art, it is provided that the zinc-plated neodymium-iron-boron of a kind of gadolinium yttrium ion implantation Body and preparation method thereof.
The present invention is achieved by the following technical solutions:
The galvanized neodymium-iron-boron magnet of a kind of gadolinium yttrium ion implantation, is made up of by mass percentage following component:
Pr-Nd:25-35%, B:0.5-1.5%, Al:0.1-1%, Cu:0-0.2%, Co:1-2%, Ga:0.1-1%, Nb:0.02-0.08%, Zr:0.01-0.05%, mesoporous silicon oxide 0.1-1%, remaining Amount is inevitably impurity a small amount of in Fe and material；
In described Pr-Nd alloy, Nd content is 20-40wt%；
The particle diameter of described mesoporous silicon oxide is 100-200nm, aperture is 10-20nm.
The galvanized neodymium-iron-boron magnet of described a kind of gadolinium yttrium ion implantation, by following component group by mass percentage Become:
Pr-Nd:28-32%, B:0.8-1.2%, Al:0.4-0.6%, Cu:0.05-0.15%, Co: 1.4-1.6%, Ga:0.3-0.7%, Nb:0.04-0.06%, Zr:0.02-0.04%, mesoporous silicon oxide 0.2-0.5%, surplus is a small amount of inevitably impurity in Fe and material；
In described Pr-Nd alloy, Nd content is 20-40wt%；
The particle diameter of described mesoporous silicon oxide is 100-200nm, aperture is 10-20nm.
The galvanized neodymium-iron-boron magnet preparation method of a kind of described gadolinium yttrium ion implantation, comprises the following steps:
(1) weigh in proportion prepare the raw material Pr-Nd of neodymium iron boron magnetic body, B, Al, Cu, Co, Ga, Nb, Zr, Fe, send in vaccum sensitive stove after oil-free, amphidromic and rustless process, vacuum 10.2-10.6Pa, Be smelted into aluminium alloy under the conditions of temperature 1300-1400 DEG C, aluminium alloy vacuum rapid hardening furnace 1300-1400 DEG C, Under argon shield, the alloy sheet that band becomes average thickness to be 0.2-0.4mm is got rid of in rapid hardening；
(2) above-mentioned alloy sheet is sent into hydrogen crushing furnace, under the hydrogen pressure of 0.6-1.2Mpa, inhales hydrogen 2-4 hour, At a temperature of 500-650 DEG C, dehydrogenation is broken into the coarse powder that particle mean size is 100-200 μm for 6-8 hour again, Coarse powder jet mill is milled under the pressure of 0.12-0.18Mpa the fine powder that particle mean size is 3-4 μm；
(3) by above-mentioned neodymium iron boron raw material fine powder with containing concentration be 20-30g/L zinc sulfate, 25-35g/L time The sweet nitrilo acetic acid of sodium phosphate, 0.002-0.005g/L, 20-30g/L sodium lactate, the plating of 25-35g/L sodium citrate Zinc solution soaks and carries out plating zinc on surface, under the conditions of temperature 70-90 DEG C, pH4.5-5.5 zinc-plated 20-30 minute Stop when being 40-60nm to surface zinc coating thickness；
(4) the above-mentioned neodymium iron boron raw material fine powder deionized water having plated zinc layers is cleaned, filters 4-6 time, mistake The fine powder filtered is freeze-day with constant temperature 4-5 hour at 90-110 DEG C, is cooled to room temperature, under nitrogen protection fine powder With lubricant batch mixing 3-4 hour in three-dimensional material mixer of mesoporous silicon oxide and gross weight 0.1-0.3wt%, Formed and mix magnetic powder uniformly；
(5) being weighed by above-mentioned mixing magnetic powder full-automatic molding press automatic ration, oriented moulding is pressed into base, Send into after Vacuum Package, isostatic cool pressing, stripping oil in vacuum sintering furnace, at 300-400 DEG C, be incubated 0.5-1 Hour, at 800-900 DEG C, it is incubated 2-3 hour, obtains porosity 10-20% presintered compact, send into ion note Enter in device, with energetic ion form, heavy rare earth alloy Gd100-aYa is injected presintered compact surface, Implantation Energy 100-300keV, injection metering 2-8 × 1017cm-2, it is re-fed in vacuum sintering furnace sintering densification further；
(6) sinter 3-5 hour under conditions of temperature 1000-1100 DEG C, vacuum 0.004-0.006Pa, Sintered magnet is obtained after cooling, then through secondary vacuum temper, under the conditions of vacuum is 0.003-0.005Pa One-level temperature 850-950 DEG C, insulation 2-3 hour, second annealing temperature 450-550 DEG C, insulation 3-4 Hour, finally give Sintered NdFeB magnet.
A kind of galvanized neodymium-iron-boron magnet preparation method of described gadolinium yttrium ion implantation, neodymium in described step (3) Ferrum boron raw material fine powder quality and galvanizing solution volume ratio are 35-45g:1L.
A kind of galvanized neodymium-iron-boron magnet preparation method of described gadolinium yttrium ion implantation, a in described step (5) For Y atomic fraction in heavy rare earth alloy Gd100-aYa, 30at%≤a≤50at%.
Compared with prior art, the invention have the advantage that
Present invention neodymium iron boron magnetic body material powder after airflow milling grinds is started with, by direct for micron order material powder It is coated with zinc-plated, powder particle surface one layer of nanoscale zinc layers of cladding, improve the antioxidation of neodymium iron boron material powder Property, and stoping agglomerates in subsequent process to be polymerized to granule group, the beneficially oriented moulding of powder, follow-up Grain boundary decision ensure that when processing that in magnet crystal boundary, Nd-rich phase is enough and continuous, increases substantially heavy rare earth element Along crystal boundary to the diffuser efficiency within magnet, obtain overcoming while product size is required by grain boundary decision The neodymium iron boron magnetic body of higher performance；The addition of mesoporous silicon oxide makes nano-component and magnet principal phase be combined into crystal boundary Phase, both can play heterogeneous nucleating effect, it is also possible to improve neodymium-iron-boron bulk microstructure, was ensureing that remanent magnetism is basic The coercivity of magnet is improve while constant；Use ion implantation technology by heavy rare earth element Gd, Y with high energy Ionic species injects presintered compact surface, then carries out grain boundary decision process, improves border structure, improves coercivity, Reduce the usage amount of heavy rare earth element by controlling Implantation Energy and metering, improve its practical efficiency, it is to avoid Unnecessary rare-earth enrichment, in magnet surface, increases the ion implanting degree of depth and shortens the evolving path, improves diffuser efficiency； The Sintered NdFeB magnet crystalline structure produced is uniform, on the low side near the region heavy rare earth content of magnet core, protects The remanent magnetism having demonstrate,proved magnet is substantially unaffected, higher near the region heavy rare earth content of magnet surface, significantly improves The coercivity of magnet, the shortcoming of sintered NdFeB magnet is improved comprehensively, advantage is largely increased.
Detailed description of the invention
The galvanized neodymium-iron-boron magnet of a kind of gadolinium yttrium ion implantation, is made up of by mass percentage following component:
Pr-Nd:28%, B:0.8%, Al:0.4%, Cu:0.05%, Co:1.4%, Ga:0.3%, Nb: 0.04%, Zr:0.02%, mesoporous silicon oxide 0.2%, surplus is a small amount of inevitable in Fe and material Impurity；
In described Pr-Nd alloy, Nd content is 20wt%；
The particle diameter of described mesoporous silicon oxide is 100nm, aperture is 10nm.
The galvanized neodymium-iron-boron magnet preparation method of a kind of described gadolinium yttrium ion implantation, comprises the following steps:
(1) weigh in proportion prepare the raw material Pr-Nd of neodymium iron boron magnetic body, B, Al, Cu, Co, Ga, Nb, Zr, Fe, send in vaccum sensitive stove, in vacuum 10.2Pa, temperature after oil-free, amphidromic and rustless process Being smelted into aluminium alloy under the conditions of spending 1300 DEG C, aluminium alloy vacuum rapid hardening furnace is 1300 DEG C, speed under argon shield Coagulate and get rid of the alloy sheet that band becomes average thickness to be 0.2mm；
(2) above-mentioned alloy sheet is sent into hydrogen crushing furnace, under the hydrogen pressure of 0.6Mpa, inhale hydrogen 2 hours, then At a temperature of 500 DEG C, dehydrogenation is broken into the coarse powder that particle mean size is 100 μm for 6 hours, by coarse powder comminution by gas stream Machine is milled to the fine powder that particle mean size is 3 μm under the pressure of 0.12Mpa；
(3) by above-mentioned neodymium iron boron raw material fine powder with containing 20g/L zinc sulfate, 25g/L sodium hypophosphite, 0.002g/L Sweet nitrilo acetic acid, 20g/L sodium lactate, the galvanizing solution of 25g/L sodium citrate soak and carry out plating zinc on surface, in temperature Spend 70 DEG C, under the conditions of pH5 zinc-plated 20 minutes to stop when being 40nm to surface zinc coating thickness；
(4) the above-mentioned neodymium iron boron raw material fine powder deionized water having plated zinc layers is cleaned, filters 4 times, filter Good fine powder freeze-day with constant temperature 4 hours at 90 DEG C, are cooled to room temperature, under nitrogen protection fine powder and mesoporous two The lubricant of silicon oxide and gross weight 0.1wt% is batch mixing 3 hours in three-dimensional material mixer, formed uniform mixed Close magnetic powder；
(5) being weighed by above-mentioned mixing magnetic powder full-automatic molding press automatic ration, oriented moulding is pressed into base, Send into after Vacuum Package, isostatic cool pressing, stripping oil in vacuum sintering furnace, at 300 DEG C, be incubated 0.5 hour, At 800 DEG C, it is incubated 2 hours, obtains porosity 10% presintered compact, send in ion implantation apparatus, with high energy Ionic species is by heavy rare earth alloy Gd100-aYaInject presintered compact surface, Implantation Energy 100keV, injection metering 2×1017cm-2, it is re-fed in vacuum sintering furnace sintering densification further；
(6) sinter 3 hours under conditions of temperature 1000 DEG C, vacuum 0.004Pa, burnt after cooling Knot magnet, then through secondary vacuum temper, vacuum be one-level temperature 850 DEG C under the conditions of 0.003Pa, It is incubated 2 hours, second annealing temperature 450 DEG C, insulation 3 hours, finally give Sintered NdFeB magnet.
A kind of galvanized neodymium-iron-boron magnet preparation method of described gadolinium yttrium ion implantation, neodymium in described step (3) Ferrum boron raw material fine powder quality and galvanizing solution volume ratio are 40g:1L.
A kind of galvanized neodymium-iron-boron magnet preparation method of described gadolinium yttrium ion implantation, a in described step (5) For Y at heavy rare earth alloy Gd100-aYaIn atomic fraction, 30at%≤a≤50at%.

Claims (5)

1. the galvanized neodymium-iron-boron magnet of a gadolinium yttrium ion implantation, it is characterised in that pressed percent mass by following component Than composition:
Pr-Nd:25-35%, B:0.5-1.5%, Al:0.1-1%, Cu:0-0.2%, Co:1-2%, Ga: 0.1-1%, Nb:0.02-0.08%, Zr:0.01-0.05%, mesoporous silicon oxide 0.1-1%, surplus is Fe A small amount of inevitably impurity with in material；
In described Pr-Nd alloy, Nd content is 20-40wt%；
The particle diameter of described mesoporous silicon oxide is 100-200nm, aperture is 10-20nm.
The galvanized neodymium-iron-boron magnet of a kind of gadolinium yttrium ion implantation the most according to claim 1, it is characterised in that It is made up of by mass percentage following component:
Pr-Nd:28-32%, B:0.8-1.2%, Al:0.4-0.6%, Cu:0.05-0.15%, Co:1.4-1.6%, Ga:0.3-0.7%, Nb:0.04-0.06%, Zr:0.02-0.04%, mesoporous silicon oxide 0.2-0.5%, Surplus is a small amount of inevitably impurity in Fe and material；
In described Pr-Nd alloy, Nd content is 20-40wt%；
The particle diameter of described mesoporous silicon oxide is 100-200nm, aperture is 10-20nm.
3. a galvanized neodymium-iron-boron magnet preparation method for gadolinium yttrium ion implantation as claimed in claim 1, it is special Levy and be to comprise the following steps:
(1) weigh in proportion prepare the raw material Pr-Nd of neodymium iron boron magnetic body, B, Al, Cu, Co, Ga, Nb, Zr, Fe, send in vaccum sensitive stove after oil-free, amphidromic and rustless process, vacuum 10.2-10.6Pa, Be smelted into aluminium alloy under the conditions of temperature 1300-1400 DEG C, aluminium alloy vacuum rapid hardening furnace 1300-1400 DEG C, Under argon shield, the alloy sheet that band becomes average thickness to be 0.2-0.4mm is got rid of in rapid hardening；
(2) above-mentioned alloy sheet is sent into hydrogen crushing furnace, under the hydrogen pressure of 0.6-1.2Mpa, inhales hydrogen 2-4 hour, At a temperature of 500-650 DEG C, dehydrogenation is broken into the coarse powder that particle mean size is 100-200 μm for 6-8 hour again, Coarse powder jet mill is milled under the pressure of 0.12-0.18Mpa the fine powder that particle mean size is 3-4 μm；
(3) by above-mentioned neodymium iron boron raw material fine powder with being 20-30g/L zinc sulfate, 25-35g/L phosphorus containing concentration Acid sodium, the sweet nitrilo acetic acid of 0.002-0.005g/L, 20-30g/L sodium lactate, 25-35g/L sodium citrate zinc-plated Solution soaking carries out plating zinc on surface, and under the conditions of temperature 70-90 DEG C, pH4.5-5.5, zinc-plated 20-30 minute extremely Stop when surface zinc coating thickness is 40-60nm；
(4) the above-mentioned neodymium iron boron raw material fine powder deionized water having plated zinc layers is cleaned, filters 4-6 time, filter Good fine powder freeze-day with constant temperature 4-5 hour at 90-110 DEG C, is cooled to room temperature, under nitrogen protection fine powder with The lubricant of mesoporous silicon oxide and gross weight 0.1-0.3wt% batch mixing 3-4 hour in three-dimensional material mixer, Formed and mix magnetic powder uniformly；
(5) being weighed by above-mentioned mixing magnetic powder full-automatic molding press automatic ration, oriented moulding is pressed into base, Send into after Vacuum Package, isostatic cool pressing, stripping oil in vacuum sintering furnace, at 300-400 DEG C, be incubated 0.5-1 Hour, at 800-900 DEG C, it is incubated 2-3 hour, obtains porosity 10-20% presintered compact, send into ion implanting In device, with energetic ion form by heavy rare earth alloy Gd100-aYaInject presintered compact surface, Implantation Energy 100-300keV, injection metering 2-8 × 1017cm-2, it is re-fed in vacuum sintering furnace sintering densification further；
(6) sinter 3-5 hour under conditions of temperature 1000-1100 DEG C, vacuum 0.004-0.006Pa, Sintered magnet is obtained after cooling, then through secondary vacuum temper, under the conditions of vacuum is 0.003-0.005Pa One-level temperature 850-950 DEG C, insulation 2-3 hour, second annealing temperature 450-550 DEG C, insulation 3-4 Hour, finally give Sintered NdFeB magnet.
4. a galvanized neodymium-iron-boron magnet preparation method for gadolinium yttrium ion implantation as claimed in claim 3, it is special Levy and be in described step (3) that neodymium iron boron raw material fine powder quality and galvanizing solution volume ratio are 35-45g:1L.
5. a galvanized neodymium-iron-boron magnet preparation method for gadolinium yttrium ion implantation as claimed in claim 3, it is special Levy and be in described step (5) that a is that Y is at heavy rare earth alloy Gd100-aYaIn atomic fraction, 30at%≤a ≤ 50at%.
CN201610555139.1A 2016-07-14 2016-07-14 Gadolinium/yttrium-ion-implanted zinc-plated neodymium-iron-boron magnet and preparation method thereof Pending CN106024238A (en)

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN113223798A (en) * 2021-04-28 2021-08-06 慈溪市兴发磁业科技有限公司 Neodymium iron boron magnetic material and preparation method thereof
CN117438207A (en) * 2023-12-20 2024-01-23 江西金力永磁科技股份有限公司 Method for improving binding force of surface coating of high-grade sintered NdFeB magnet

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CN105551707A (en) * 2016-02-25 2016-05-04 廊坊京磁精密材料有限公司 Neodymium iron boron magnet raw material powder and treatment process therefor
CN105702405A (en) * 2016-04-29 2016-06-22 湖北工程学院 Nano composite NdFeB (neodymium iron boron) permanent magnetic material and preparation method
CN105742048A (en) * 2016-04-28 2016-07-06 北京科技大学 Method for improving performance of sintered neodymium-iron-boron magnet through ion implantation of rare earth and alloys

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CN105551707A (en) * 2016-02-25 2016-05-04 廊坊京磁精密材料有限公司 Neodymium iron boron magnet raw material powder and treatment process therefor
CN105742048A (en) * 2016-04-28 2016-07-06 北京科技大学 Method for improving performance of sintered neodymium-iron-boron magnet through ion implantation of rare earth and alloys
CN105702405A (en) * 2016-04-29 2016-06-22 湖北工程学院 Nano composite NdFeB (neodymium iron boron) permanent magnetic material and preparation method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113223798A (en) * 2021-04-28 2021-08-06 慈溪市兴发磁业科技有限公司 Neodymium iron boron magnetic material and preparation method thereof
CN117438207A (en) * 2023-12-20 2024-01-23 江西金力永磁科技股份有限公司 Method for improving binding force of surface coating of high-grade sintered NdFeB magnet
CN117438207B (en) * 2023-12-20 2024-04-12 江西金力永磁科技股份有限公司 Method for improving binding force of surface coating of high-grade sintered NdFeB magnet

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