CN104107908B - A kind of Nd Fe B alloys powder process antioxidant - Google Patents
A kind of Nd Fe B alloys powder process antioxidant Download PDFInfo
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- CN104107908B CN104107908B CN201410364143.0A CN201410364143A CN104107908B CN 104107908 B CN104107908 B CN 104107908B CN 201410364143 A CN201410364143 A CN 201410364143A CN 104107908 B CN104107908 B CN 104107908B
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Abstract
The present invention relates to a kind of Nd Fe B alloys powder process antioxidant, it is characterized in that: once add the neodymium iron boron powder process antioxidant accounting for meal weight 0.01 ~ 10wt%, secondary is added into the antioxidant accounting for meal weight 0.01 ~ 10wt% subsequently; Wherein component is the thymol (C of 5% ~ 35wt%
10h
14o); Calcium stearate (the C of 1% ~ 50wt%
36h
70o
4ca); The polyethylene glycol of 5% ~ 35wt% and octane (C
8h
18) mixture; The higher boiling aviation kerosine of 5% ~ 35wt%; The Stadis450 of 5% ~ 35wt%; Beneficial effect of the present invention is: not containing mordant composition in antioxidant substance component, avoid the damage produced the rubber element in ball-grinding machine or airflow milling equipment; In forming and sintering process, component materials is easy to volatilization diffusion, additive component variation, avoid and produce a large amount of bubbles at certain single temperature spot, reduce Nd-Fe-B permanent magnetic interiors of products and occur that the mechanical strength of the product that a large amount of micro-cracks causes reduces and greatly reduces the probability of three dimension scale defect, improve yield rate.
Description
Technical field
The invention belongs to Nd Fe B alloys technical field of permanent magnetic material preparation, be related specifically to the powder antioxidant in a kind of Nd Fe B alloys pulverizing process.
Background technology
Electronic product general in the world requires high trend development towards miniaturization, lightness, slimming and environmental protection and energy saving at present, and make high-performance, the demand of the Nd-Fe-Bo permanent magnet material of small size increases greatly.The preparation technology of research and development and optimization Nd-Fe-Bo permanent magnet material can not only meet the user demand of daily electronic device, adapt with the model of social economy of following environment-friendly high-efficiency especially, so the production technology optimizing Nd-Fe-Bo permanent magnet material has great importance, and is also all one of emphasis of magnetic material research field all the time.
The core of the production technology of current Nd-Fe-Bo permanent magnet material be powder preparation and shaping after sintering process.Wherein in pulverizing process, the technique of adding antioxidant and lubricant and dispersant obtains to be applied, existing scientific research report display, above three class additives whether are added in ball milling pulverizing process, the particle diameter of ball milling and the distribution of average grain size are all had a great impact, how selecting the composition of additive and control the addition of additive, is the key issue of producing high-performance Ne-Fe-B permanent-magnet material.Additive general is at present owing to producing decomposition containing mordant composition or under the high temperature of mechanical milling process generation, not only the rubber element in ball-grinding machine or airflow milling equipment is produced and damage, dispersion neodymium iron boron powder cannot be played simultaneously due to the decomposition of additive, reach the effect reducing particle agglomeration.And the difficult adding ingredient decomposed under adopting high temperature, can solve a difficult problem for pyrolytic in mechanical milling process, but in forming and sintering process subsequently, the difficult composition decomposed is not easy to volatilization diffusion, this also directly affects the magnetic property of Nd-Fe-Bo permanent magnet material.Simultaneously, the additive component adopted is single, certain the single temperature spot in sintering process can be made to produce a large amount of bubbles, Nd-Fe-B permanent magnetic interiors of products is made to occur a large amount of micro-cracks, reduce the mechanical strength of product on the one hand, huge on the impact of product magnetic property on the other hand, there is even the phenomenon that a large amount of bubble is reunited, make product occur the defect of three dimension scale, cause product rejection.
The patent document show needle announced at present to the research of this problem and innovation few.Patent (the application number: 201310498178.9): mention in a kind of method of Nd Fe B alloys powder process that the antioxidant of employing is: zinc stearate (C announced
36h
70o
4zn) fusing point: 118-125 DEG C, diethylene glycol monobutyl ether C
8h
18o
3boiling point 231 DEG C, myristic acid C
14h
28o
2boiling point 199 DEG C, solvent naphtha boiling point are 60 ~ 300 DEG C; Lubricant is: isopropyl alcohol C
3h
8o boiling point is 82.5 DEG C, zinc stearate (C
36h
70o
4zn) fusing point: 118-125 DEG C, boric acid acid zinc fat, solvent naphtha.Adopt above component as powder antioxidant, because its boiling point of added material is too low, produce evaporation under high temperature (more than the 100 DEG C) effect produced in powder ball milling or airflow milling powder process, the isolation effect between this neodymium iron boron powder is weakened; Simultaneously because its boiling point is all at about 200 DEG C, a large amount of dense gas can be produced in this temperature province in the neodymium iron boron powder forming and sintering stage to distribute, make the interiors of products after sintering occur three dimension scale defect, directly cause product rejection, thus reduce yield rate.
Summary of the invention
The technical barrier that patent of the present invention solves is: provide a kind of technique relatively simple, energy-efficient and be beneficial to the antioxidant of industrialized mass production Nd Fe B alloys powder, after adopting this antioxidant, the isolation effect between neodymium iron boron powder is obvious; Additive boiling point simultaneously owing to adopting is uniformly dispersed, in the neodymium iron boron powder forming and sintering stage, the gas that evaporation produces distributes in different temperature provinces, avoids the interiors of products after sintering and occurs the product rejection that three dimension scale defect causes, thus greatly improve yield rate.
For achieving the above object, the technical solution adopted in the present invention is:
A kind of Nd Fe B alloys powder process antioxidant, it is characterized in that: adopt neodymium iron boron slab to carry out the broken process of hydrogen, the meal of gained loads in three-dimensional ball grinder, and once add the neodymium iron boron powder process antioxidant accounting for meal weight 0.01 ~ 10wt%, mixing and ball milling is after 5 hours; Secondary is added into the antioxidant accounting for meal weight 0.01 ~ 10wt% subsequently, through airflow milling 2 hours obtained fine powders;
Neodymium iron boron antioxidant constituent as above is: dispersant employing boiling point is the thymol (C of 233 ~ 235 DEG C
10h
14o) be the calcium stearate (C of 359.4 DEG C with boiling point
36h
70o
4ca) mixed; Binding agent employing boiling point is the polyethylene glycol of 197.3 DEG C; Solvent employing boiling point is the octane (C of 125.8 DEG C
8h
18); Lubricant adopts higher boiling aviation kerosine; Antisatic additive employing boiling point is the Stadis450 of 90 DEG C.
The ratio that each constituent of neodymium iron boron antioxidant as above accounts for antioxidant gross mass is respectively: the thymol (C of 5% ~ 35wt%
10h
14o); Calcium stearate (the C of 1% ~ 50wt%
36h
70o
4ca); The polyethylene glycol of 5% ~ 35wt% and octane (C
8h
18) mixture; The higher boiling aviation kerosine of 5% ~ 35wt%; The Stadis450 of 5% ~ 35wt%.
The discharging speed of Nd Fe B alloys powder meal as above is 150 ~ 200 kgs/hr, and fine powder discharging speed is 350 ~ 500 kgs/hr.
The granularity of Nd Fe B alloys powder meal as above is 1.5 ~ 2.0 μm, and the granularity of fine powder is 0.6 ~ 0.86 μm.
The beneficial effect of patent of the present invention is: not containing mordant composition in antioxidant substance component, not easily decomposes, avoid the damage produced the rubber element in ball-grinding machine or airflow milling equipment under the high temperature that mechanical milling process produces; Serve dispersion neodymium iron boron powder, reach the effect reducing particle agglomeration.Without the composition decomposed difficult under high temperature in this antioxidant ingredients, in forming and sintering process subsequently, component materials is easy to volatilization diffusion; The additive component variation adopted, certain the single temperature spot avoided in sintering process produces a large amount of bubbles, reduce Nd-Fe-B permanent magnetic interiors of products and occur that the mechanical strength of the product that a large amount of micro-cracks causes reduces and occurs the phenomenon that a large amount of bubble is reunited, product is occurred, and the probability of three dimension scale defect reduces greatly, improves yield rate.
For achieving the above object, the present invention determines thing phase composition and pattern by X-ray diffractometer (XRD) and SEM (SEM), measures permanent magnetism characteristic parameter with B-H magnetic property measuring instrument.
Accompanying drawing explanation
Fig. 1 be in embodiment 1 N45 grade neodymium-iron-boron cylinder finished product XRD diffracting spectrum;
Fig. 2 be in embodiment 1 N45 grade neodymium-iron-boron cylinder finished product SEM shape appearance figure;
Fig. 3 is the magnetic property figure of N45 grade neodymium-iron-boron cylinder finished product in embodiment 1;
Fig. 4 is the magnetic property figure of 48M grade neodymium-iron-boron cylinder finished product in embodiment 2;
Fig. 5 is the magnetic property figure of 40SH grade neodymium-iron-boron cylinder finished product in embodiment 3;
Fig. 6 is the magnetic property figure of 35SH grade neodymium-iron-boron cylinder finished product in embodiment 4.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in limiting the scope of the invention for illustration of the present invention.The present invention can implement by the either type described in summary of the invention.
Embodiment 1
A kind of neodymium-ferrum-boron ball mill powder process antioxidant, it is characterized in that: adopt neodymium iron boron N45 slab to carry out the broken process of hydrogen, the meal of gained loads in three-dimensional ball grinder, and once add the neodymium iron boron powder process antioxidant accounting for meal weight 0.5wt%, mixing and ball milling is after 5 hours; Secondary is added into the antioxidant accounting for meal weight 0.8wt% subsequently, through airflow milling 2 hours obtained fine powders.Neodymium iron boron antioxidant constituent as above is: dispersant employing boiling point is the thymol (C of 233 ~ 235 DEG C
10h
14o) be the calcium stearate (C of 359.4 DEG C with boiling point
36h
70o
4ca) mixed; Binding agent employing boiling point is the polyethylene glycol of 197.3 DEG C; Solvent employing boiling point is the octane (C of 125.8 DEG C
8h
18); Lubricant adopts higher boiling aviation kerosine; Antisatic additive employing boiling point is the Stadis450 of 90 DEG C.The ratio that each constituent of neodymium iron boron antioxidant as above accounts for antioxidant gross mass is respectively: the thymol (C of 19%
10h
14o); Calcium stearate (the C of 12wt%
36h
70o
4ca); The polyethylene glycol of 22wt% and octane (C
8h
18) mixture; The higher boiling aviation kerosine of 27wt%; The Stadis450 of 20wt%.
The discharging speed of Nd Fe B alloys powder meal as above is 150 kgs/hr, and fine powder discharging speed is 500 kgs/hr; The granularity of Nd Fe B alloys powder meal is 2.0 μm, and the granularity of fine powder is 0.86 μm.
The beneficial effect of patent of the present invention is: not containing mordant composition in antioxidant substance component, not easily decomposes, avoid the damage produced the rubber element in ball-grinding machine or airflow milling equipment under the high temperature that mechanical milling process produces; Serve dispersion neodymium iron boron powder, reach the effect reducing particle agglomeration.Without the composition decomposed difficult under high temperature in this antioxidant ingredients, in forming and sintering process subsequently, component materials is easy to volatilization diffusion; The additive component variation adopted, certain the single temperature spot avoided in sintering process produces a large amount of bubbles, reduce Nd-Fe-B permanent magnetic interiors of products and occur that the mechanical strength of the product that a large amount of micro-cracks causes reduces and occurs the phenomenon that a large amount of bubble is reunited, product is occurred, and the probability of three dimension scale defect reduces greatly, improves yield rate.
Adopt neodymium iron boron cylindrical product prepared by the present embodiment neodymium iron boron alloy powder after testing: remanent magnetization Br is 13.274kGs; Magnetic induction coercivity H
cbfor 12.719kOe; HCJ H
cjfor 13.314kOe; Maximum magnetic energy product (BH)
maxfor 42.695MGO.
Embodiment 2
A kind of neodymium-ferrum-boron ball mill powder process antioxidant, it is characterized in that: adopt neodymium iron boron 48M slab to carry out the broken process of hydrogen, the meal of gained loads in three-dimensional ball grinder, and once add the neodymium iron boron powder process antioxidant accounting for meal weight 0.9wt%, mixing and ball milling is after 5 hours; Secondary is added into the antioxidant accounting for meal weight 0.6wt% subsequently, through airflow milling 2 hours obtained fine powders.Neodymium iron boron antioxidant constituent as above is: dispersant employing boiling point is the thymol (C of 233 ~ 235 DEG C
10h
14o) be the calcium stearate (C of 359.4 DEG C with boiling point
36h
70o
4ca) mixed; Binding agent employing boiling point is the polyethylene glycol of 197.3 DEG C; Solvent employing boiling point is the octane (C of 125.8 DEG C
8h
18); Lubricant adopts higher boiling aviation kerosine; Antisatic additive employing boiling point is the Stadis450 of 90 DEG C.The ratio that each constituent of neodymium iron boron antioxidant as above accounts for antioxidant gross mass is respectively: the thymol (C of 17%
10h
14o); Calcium stearate (the C of 11wt%
36h
70o
4ca); The polyethylene glycol of 25wt% and octane (C
8h
18) mixture; The higher boiling aviation kerosine of 17wt%; The Stadis450 of 30wt%.
The discharging speed of Nd Fe B alloys powder meal as above is 200 kgs/hr, and fine powder discharging speed is 450 kgs/hr; The granularity of Nd Fe B alloys powder meal is 1.8 μm, and the granularity of fine powder is 0.8 μm.
The beneficial effect of patent of the present invention is: not containing mordant composition in antioxidant substance component, not easily decomposes, avoid the damage produced the rubber element in ball-grinding machine or airflow milling equipment under the high temperature that mechanical milling process produces; Serve dispersion neodymium iron boron powder, reach the effect reducing particle agglomeration.Without the composition decomposed difficult under high temperature in this antioxidant ingredients, in forming and sintering process subsequently, component materials is easy to volatilization diffusion; The additive component variation adopted, certain the single temperature spot avoided in sintering process produces a large amount of bubbles, reduce Nd-Fe-B permanent magnetic interiors of products and occur that the mechanical strength of the product that a large amount of micro-cracks causes reduces and occurs the phenomenon that a large amount of bubble is reunited, product is occurred, and the probability of three dimension scale defect reduces greatly, improves yield rate.
Adopt neodymium iron boron cylindrical product prepared by the present embodiment neodymium iron boron alloy powder after testing: remanent magnetization Br is 13.708kGs; Magnetic induction coercivity H
cbfor 13.115kOe; HCJ H
cjfor 15.333kOe; Maximum magnetic energy product (BH)
maxfor 46.065MGO.
Embodiment 3
A kind of neodymium-ferrum-boron ball mill powder process antioxidant, it is characterized in that: adopt neodymium iron boron 40SH slab to carry out the broken process of hydrogen, the meal of gained loads in three-dimensional ball grinder, and once add the neodymium iron boron powder process antioxidant accounting for meal weight 10wt%, mixing and ball milling is after 5 hours; Secondary is added into the antioxidant accounting for meal weight 1.6wt% subsequently, through airflow milling 2 hours obtained fine powders.Neodymium iron boron antioxidant constituent as above is: dispersant employing boiling point is the thymol (C of 233 ~ 235 DEG C
10h
14o) be the calcium stearate (C of 359.4 DEG C with boiling point
36h
70o
4ca) mixed; Binding agent employing boiling point is the polyethylene glycol of 197.3 DEG C; Solvent employing boiling point is the octane (C of 125.8 DEG C
8h
18); Lubricant adopts higher boiling aviation kerosine; Antisatic additive employing boiling point is the Stadis450 of 90 DEG C.The ratio that each constituent of neodymium iron boron antioxidant as above accounts for antioxidant gross mass is respectively: the thymol (C of 15%
10h
14o); Calcium stearate (the C of 18wt%
36h
70o
4ca); The polyethylene glycol of 27wt% and octane (C
8h
18) mixture; The higher boiling aviation kerosine of 23wt%; The Stadis450 of 17wt%.
The discharging speed of Nd Fe B alloys powder meal as above is 200 kgs/hr, and fine powder discharging speed is 480 kgs/hr; The granularity of Nd Fe B alloys powder meal is 1.6 μm, and the granularity of fine powder is 0.7 μm.
The beneficial effect of patent of the present invention is: not containing mordant composition in antioxidant substance component, not easily decomposes, avoid the damage produced the rubber element in ball-grinding machine or airflow milling equipment under the high temperature that mechanical milling process produces; Serve dispersion neodymium iron boron powder, reach the effect reducing particle agglomeration.Without the composition decomposed difficult under high temperature in this antioxidant ingredients, in forming and sintering process subsequently, component materials is easy to volatilization diffusion; The additive component variation adopted, certain the single temperature spot avoided in sintering process produces a large amount of bubbles, reduce Nd-Fe-B permanent magnetic interiors of products and occur that the mechanical strength of the product that a large amount of micro-cracks causes reduces and occurs the phenomenon that a large amount of bubble is reunited, product is occurred, and the probability of three dimension scale defect reduces greatly, improves yield rate.
Adopt neodymium iron boron cylindrical product prepared by the present embodiment neodymium iron boron alloy powder after testing: remanent magnetization Br is 12.607kGs; Magnetic induction coercivity H
cbfor 12.715kOe; HCJ H
cjfor 19.402kOe; Maximum magnetic energy product (BH)
maxfor 40.163MGO.
Embodiment 4
A kind of neodymium-ferrum-boron ball mill powder process antioxidant, it is characterized in that: adopt neodymium iron boron 35SH slab to carry out the broken process of hydrogen, the meal of gained loads in three-dimensional ball grinder, and once add the neodymium iron boron powder process antioxidant accounting for meal weight 1.6wt%, mixing and ball milling is after 5 hours; Secondary is added into the antioxidant accounting for meal weight 1.8wt% subsequently, through airflow milling 2 hours obtained fine powders.Neodymium iron boron antioxidant constituent as above is: dispersant employing boiling point is the thymol (C of 233 ~ 235 DEG C
10h
14o) be the calcium stearate (C of 359.4 DEG C with boiling point
36h
70o
4ca) mixed; Binding agent employing boiling point is the polyethylene glycol of 197.3 DEG C; Solvent employing boiling point is the octane (C of 125.8 DEG C
8h
18); Lubricant adopts higher boiling aviation kerosine; Antisatic additive employing boiling point is the Stadis450 of 90 DEG C.The ratio that each constituent of neodymium iron boron antioxidant as above accounts for antioxidant gross mass is respectively: the thymol (C of 21%
10h
14o); Calcium stearate (the C of 19wt%
36h
70o
4ca); The polyethylene glycol of 20wt% and octane (C
8h
18) mixture; The higher boiling aviation kerosine of 27wt%; The Stadis450 of 23wt%.
The discharging speed of Nd Fe B alloys powder meal as above is 260 kgs/hr, and fine powder discharging speed is 460 kgs/hr; The granularity of Nd Fe B alloys powder meal is 1.8 μm, and the granularity of fine powder is 0.8 μm.
The beneficial effect of patent of the present invention is: not containing mordant composition in antioxidant substance component, not easily decomposes, avoid the damage produced the rubber element in ball-grinding machine or airflow milling equipment under the high temperature that mechanical milling process produces; Serve dispersion neodymium iron boron powder, reach the effect reducing particle agglomeration.Without the composition decomposed difficult under high temperature in this antioxidant ingredients, in forming and sintering process subsequently, component materials is easy to volatilization diffusion; The additive component variation adopted, certain the single temperature spot avoided in sintering process produces a large amount of bubbles, reduce Nd-Fe-B permanent magnetic interiors of products and occur that the mechanical strength of the product that a large amount of micro-cracks causes reduces and occurs the phenomenon that a large amount of bubble is reunited, product is occurred, and the probability of three dimension scale defect reduces greatly, improves yield rate.
Adopt neodymium iron boron cylindrical product prepared by the present embodiment neodymium iron boron alloy powder after testing: remanent magnetization Br is 12.163kGs; Magnetic induction coercivity H
cbfor 11.891kOe; HCJ H
cjfor 20.544kOe; Maximum magnetic energy product (BH)
maxfor 36.094MGO.
Claims (4)
1. a Nd Fe B alloys powder process antioxidant, it is characterized in that: adopt neodymium iron boron slab to carry out the broken process of hydrogen, the meal of gained loads in three-dimensional ball grinder, once add the Nd Fe B alloys powder process antioxidant accounting for meal weight 0.01 ~ 10wt%, mixing and ball milling is after 5 hours; Secondary is added into the antioxidant accounting for meal weight 0.01 ~ 10wt% subsequently, through airflow milling 2 hours obtained fine powders; Described antioxidant is made up of dispersant, binding agent, solvent, lubricant and antisatic additive, and wherein dispersant employing boiling point is the thymol (C of 233 ~ 235 DEG C
10h
14o) be the calcium stearate (C of 359.4 DEG C with boiling point
36h
70o
4ca) mixed, binding agent employing boiling point is the polyethylene glycol of 197.3 DEG C, and solvent employing boiling point is the octane (C of 125.8 DEG C
8h
18), lubricant adopts higher boiling aviation kerosine, and antisatic additive employing boiling point is the Stadis450 of 90 DEG C.
2. a kind of Nd Fe B alloys powder process antioxidant according to claim 1, is characterized in that: the ratio that each constituent accounts for antioxidant gross mass is respectively: the thymol (C of 5% ~ 35wt%
10h
14o); Calcium stearate (the C of 1% ~ 50wt%
36h
70o
4ca); The polyethylene glycol of 5% ~ 35wt% and octane (C
8h
18) mixture; The higher boiling aviation kerosine of 5% ~ 35wt%; The Stadis450 of 5% ~ 35wt%.
3. a kind of Nd Fe B alloys powder process antioxidant according to claim 1, is characterized in that: the discharging speed of Nd Fe B alloys powder meal is 150 ~ 200 kgs/hr, and fine powder discharging speed is 350 ~ 500 kgs/hr.
4. a kind of Nd Fe B alloys powder process antioxidant according to claim 1, it is characterized in that: the granularity of Nd Fe B alloys powder meal is 1.5 ~ 2.0 μm, the granularity of fine powder is 0.6 ~ 0.86 μm.
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| CN104985173A (en) * | 2015-07-29 | 2015-10-21 | 安徽万磁电子有限公司 | Anti-oxidant for improving orientation degree of sintered NdFeB powder |
| CN107256748A (en) * | 2017-06-20 | 2017-10-17 | 乳源瑶族自治县力强磁铁制品有限公司 | A kind of preparation method of high performance sintered neodymium-iron-boron rare earth permanent-magnetic material |
| CN108133818A (en) * | 2017-12-07 | 2018-06-08 | 北京京磁电工科技有限公司 | Sintered NdFeB anti-oxidation processing method |
| CN108417376A (en) * | 2018-02-05 | 2018-08-17 | 宁波松科磁材有限公司 | A kind of Sintered NdFeB magnet preparation method without heavy rare earth |
| CN109434092B (en) * | 2018-08-31 | 2021-07-13 | 江西理工大学 | Environment-friendly dispersion solution and method for preparing neodymium iron boron magnet material by using same |
| CN110444359B (en) * | 2019-07-09 | 2021-09-14 | 浙江东阳东磁稀土有限公司 | Method for reducing oxygen content of sintered neodymium-iron-boron material and additive |
| CN111724962B (en) * | 2020-07-01 | 2021-01-01 | 宁波美固力磁电有限公司 | Oxidation-resistant treatment process for neodymium iron boron magnet |
| CN112509776B (en) * | 2020-11-24 | 2023-08-22 | 福建省长汀卓尔科技股份有限公司 | Internal additive for samarium cobalt alloy powder and preparation method of samarium cobalt sintered permanent magnet |
| CN113897613B (en) * | 2021-09-29 | 2024-02-27 | 烟台佳隆纳米产业有限公司 | High-temperature antioxidant for hot rolling of phosphorus-free steel pipe and preparation method thereof |
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