CN107931621A - The preparation method of high temperature resistant synchronous motor magnet steel - Google Patents

The preparation method of high temperature resistant synchronous motor magnet steel Download PDF

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CN107931621A
CN107931621A CN201711187832.9A CN201711187832A CN107931621A CN 107931621 A CN107931621 A CN 107931621A CN 201711187832 A CN201711187832 A CN 201711187832A CN 107931621 A CN107931621 A CN 107931621A
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parts
magnet steel
high temperature
powder
temperature resistant
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徐嘉诚
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Zhejiang Zhong Hang Mstar Technology Ltd
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Zhejiang Zhong Hang Mstar Technology Ltd
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Abstract

The invention discloses the preparation method of high temperature resistant synchronous motor magnet steel, prepared according to the order of neodymium iron boron principal phase → richness neodymium phase powder → antioxidant → lubricant → Nd-Fe-B magnet steel → high temperature resistant Nd-Fe-B magnet steel, wherein neodymium iron boron principal phase powder and rich neodymium phase powder are prepared separately, so as to keep high remanent magnetism and keep high-coercive force.At the same time by the addition of Cu powder, alloy temper temperature is reduced, it is cost-effective；Cu mutually forms NdCu2 with rich neodymium and is distributed along crystal boundary, optimizes magnet microstructure, improves the magnetic property of magnet.By adding a small amount of Ga elements, the component of optimization sintered Nd Fe B systems, can significantly improve its magnetic property, particularly coercivity.[0021] in this patent also in Nd-Fe-B magnet steel surface spraying refractory ceramics powder, so as to improve the heat resistance of the Nd-Fe-B magnet steel.

Description

The preparation method of high temperature resistant synchronous motor magnet steel
Technical field
The present invention relates to the preparation method of Nd-Fe-B magnet steel, particularly high temperature resistant synchronous motor magnet steel.
Background technology
Synchronous motor, is a kind of common alternating current generator, and synchronous motor is the heart of electric system, it is a kind of collection rotation With static, electromagnetic change and mechanical movement in one, electric energy and the element of mechanical energy conversion are realized, its dynamic property is very multiple It is miscellaneous, and its dynamic property has extreme influence to the dynamic property of Integrated power system.
Sintered NdFeB magnet steel has the outstanding advantages such as magnetic property is high, price is low and is applied to synchronous motor field.So And its Curie temperature is relatively low, temperature coefficient is larger, and resistance to elevated temperatures is bad.As synchronous motor field is to sintered NdFeB magnet steel It is required that continuous lifting, the requirement of higher is it is also proposed to its heat resistance, but the required magnet steel research of motor at present is still In the starting stage, therefore, urgent need wants a high temperature resistant synchronous motor magnet steel to tackle the demand in market.
The content of the invention
It is a primary object of the present invention to provide a kind of preparation method of high temperature resistant synchronous motor magnet steel.
To achieve the above objectives, the technical solution adopted by the present invention is：A kind of preparation side of high temperature resistant synchronous motor magnet steel Method, comprises the following steps：
Step 1: prepare neodymium iron boron principal phase powder, according to 12-14wt%PrNd, 6-7wt%B by weight percentage, Surplus is the proportioning of Fe and inevitable metal impurities, is fitted into vaccum sensitive stove, and heating-up temperature is 1500-1650 DEG C, system Principal phase slab is obtained, obtained principal phase slab is then put into hydrogen in hydrogen crushing furnace and is crushed, finally the principal phase after hydrogen crushes is through gas Stream grind granularity is 2.8-3 μm of principal phase powder；
Step 2: rich neodymium phase powder is prepared, according to 11-13wt%PrNd, 1-5wt%Co, 1- by weight percentage 5wt%Nb, 2-3wt%Cu, 0.5-0.8wt%Ga, 1-2wt%Mo, 0.2-0.5wt%Zn, 0.5-0.8wt%Ce, 0.2- 0.3wt%Ni, 0.1-0.3wt%Ti, surplus are the proportioning of Fe and inevitable metal impurities, are fitted into vaccum sensitive stove, Heating-up temperature is 1800-1850 DEG C, prepares rich neodymium phase slab, and obtained rich neodymium phase slab then is put into hydrogen in hydrogen crushing furnace breaks Broken, finally mutually the rich neodymium phase powder that granularity is 1.0-2.0 μm is made through airflow milling in the rich neodymium after hydrogen crushes；
Step 3: antioxidant is prepared, according to 50-70 part petroleum ethers in parts by weight, 20-30 parts of polyethylene oxide alkane The proportioning of base ether, 10-15 part phosphorous acid esters and 1-5 parts of rare earth nitrades, is uniformly mixed, and supernatant is taken after standing 24h；
Step 4: lubricant is prepared, according to 30-40 part calcium stearates in parts by weight, 1-5 parts of graphenes, 1-2 parts of breasts Agent, 2-8 parts of ethylene oxide/propylene oxide copolymers, the proportionings of 50-80 parts of solvents stir evenly, and add in 80 DEG C of water-baths To obtain the final product after hot 6h；
Step 5: prepare Nd-Fe-B magnet steel, according to 80-90 parts principal phase in parts by weight, 5-20 parts of rich neodymium phases, 1-2 parts Antioxidant, 0.5-2 part lubricant, be put into batch mixer mixing 2 it is small when, be pressed into hair with mould in the environment of stationary magnetic field Base, then by blank pre-burning 2 is small under 500 DEG C of vacuum conditions when, allow the antioxidant for becoming gas, lubricant discharge, Ran Houchong Argon gas protection 1200 DEG C sintering 4 it is small when, then level-one be tempered to 800 DEG C insulation 2 it is small when after, then second annealing to 400 DEG C guarantor Temperature 2 can obtain Nd-Fe-B magnet steel when small；
Step 6: high temperature resistant Nd-Fe-B magnet steel is prepared, in Nd-Fe-B magnet steel surface spraying refractory ceramics powder, wherein institute The preparation method for stating refractory ceramics powder is by 50-60 parts aluminium oxide in parts by weight, 20-30 parts of titanium dioxide, 10-15 Part silicon nitride, 1-5 parts of aluminium dihydrogen phosphates, 2-8 parts of yittrium oxide, the proportioning of 1-3 parts of nickel oxide stir evenly, and are then placed into high temperature Heated in stove, temperature is 800-900 DEG C, and heating 2h postcoolings are pulverized.
Phosphorous acid esters in the antioxidant are triethyl phosphorite, three isodecyl phosphites, triphenyl are sub- One or more in phosphate.
Solvent in the lubricant is turpentine oil or dimethylformamide.
In this patent, in order to avoid rich neodymium mutually causes coercivity to reduce by premature oxidation, therefore by neodymium iron boron principal phase powder End and rich neodymium phase powder are prepared separately, so as to can keep high remanent magnetism and keep high-coercive force.
In neodymium iron boron powder by adding Cu powder after, Cu is mainly present in the form of NdCu2 in rich neodymium phase, heat become At a temperature of shape, Cu powder will diffuse into the rich neodymium phase of liquid, and by forming the rich Nd-Cu phases of low melting point, improve the stream of magnet Become performance, optimize the microstructure of magnet, improve magnetic property.
By adding a small amount of Ga, rich neodymium is entered by the Fe atoms that Ga substitutes and mutually forms Nd-Fe-Ga-B phases, compensate for introducing Magnetic property caused by non-magnetic atom Ga reduces；In addition GaNd is liquid phase in sintering, can play and help agglomeration, make magnet Densification, reduces the intergranular directly contact of principal phase, effectively reduces the magnetic coupling between magnetic-particle, improve magnet coercive Power.
In the antioxidant that preparation process uses, have between petroleum ether and polyethylene oxide alkyl ethers and phosphorous acid esters There is synergistic effect, while under the catalysis of rare earth nitrades, antioxidant can be promoted to play effect.
In the lubricant that preparation process uses, calcium stearate and graphene are as inorganic lubricant, ethylene oxide/oxidation third Alkene copolymer can promote mutually as organic lubricant, it is only necessary to low dose of lubricant, with regard to lubricating action can be reached.
Refractory ceramics powder used in this patent, aluminium oxide, aluminium dihydrogen phosphate and silicon nitride, nickel oxide can be with The heat-resisting quantity of neodymium iron boron is improved, titanium dioxide can promote to bond, and yittrium oxide plays effect for catalysis oxidation aluminium.
A kind of preparation method for high temperature resistant synchronous motor magnet steel that the present invention obtains, it has the technical effect that adding by Cu powder Add, reduce alloy temper temperature, it is cost-effective；Cu mutually forms NdCu2 with rich neodymium and is distributed along crystal boundary, optimizes the microcosmic knot of magnet Structure, improves the magnetic property of magnet.By adding a small amount of Ga elements, the component of optimization sintered Nd-Fe-B system, can significantly improve Its magnetic property, particularly coercivity.
In addition in order to avoid rich neodymium mutually causes coercivity to reduce by premature oxidation in present patent application, therefore by neodymium iron boron master Phase powder and rich neodymium phase powder are prepared separately, so as to can keep high remanent magnetism and keep high-coercive force.
In this patent also in Nd-Fe-B magnet steel surface spraying refractory ceramics powder, so as to improve the Nd-Fe-B magnet steel Heat resistance.
Embodiment
It is described below for disclosing the present invention so that those skilled in the art can realize the present invention.It is excellent in being described below Embodiment is selected to be only used as illustrating, it may occur to persons skilled in the art that other obvious modifications.
Embodiment 1：
A kind of preparation method of high temperature resistant synchronous motor magnet steel provided in this embodiment, comprises the following steps：
Step 1: neodymium iron boron principal phase powder is prepared, according to 12wt%PrNd, 6wt%B by weight percentage, surplus For the proportioning of Fe and inevitable metal impurities, it is fitted into vaccum sensitive stove, heating-up temperature is 1500-1650 DEG C, and master is made Phase slab, is then put into hydrogen in hydrogen crushing furnace by obtained principal phase slab and crushes, finally the principal phase after hydrogen crushes is through airflow milling The principal phase powder that granularity is 2.8-3 μm is made；
Step 2: prepare rich neodymium phase powder, according to 11wt%PrNd, 1wt%Co by weight percentage, 1wt%Nb, 2wt%Cu, 0.5wt%Ga, 1wt%Mo, 0.2wtZn, 0.5wtCe, 0.2wt%Ni, 0.1wt%Ti, surplus are Fe and can not The proportioning of the metal impurities avoided, is fitted into vaccum sensitive stove, and heating-up temperature is 1800-1850 DEG C, prepares rich neodymium phase slab, so Obtained rich neodymium phase slab is put into hydrogen in hydrogen crushing furnace afterwards to crush, finally mutually grain is made through airflow milling in the rich neodymium after hydrogen crushes Spend the rich neodymium phase powder for 1.0-2.0 μm；
Step 3: prepare antioxidant, according to 50 parts of petroleum ethers in parts by weight, 20 parts of polyethylene oxide alkyl ethers, The proportioning of 10 parts of phosphorous acid esters and 1 part of rare earth nitrades, is uniformly mixed, and supernatant is taken after standing 24h；
Step 4: lubricant is prepared, according to 30 parts of calcium stearates in parts by weight, 1 part of graphene, 1 part of emulsifying agent, 2 Part ethylene oxide/propylene oxide copolymer, the proportioning of 50 parts of solvents stir evenly, and heat in 80 DEG C of water-baths after 6h to obtain the final product；
Step 5: prepare Nd-Fe-B magnet steel, according to 80 parts of principal phases in parts by weight, 5 parts of rich neodymium phases, 1 part of antioxidant, 0.5 part of lubricant, be put into batch mixer mixing 2 it is small when, be pressed into blank with mould in the environment of stationary magnetic field, then blank is existed When pre-burning 2 is small under 500 DEG C of vacuum conditions, the antioxidant for becoming gas, lubricant is allowed to discharge, then argon filling gas shielded is 1200 DEG C sintering 4 it is small when, then level-one be tempered to 800 DEG C insulation 2 it is small when after, then second annealing to 400 DEG C insulation 2 it is small when can obtain Nd-Fe-B magnet steel；
Step 6: high temperature resistant Nd-Fe-B magnet steel is prepared, in Nd-Fe-B magnet steel surface spraying refractory ceramics powder, wherein institute The preparation method for stating refractory ceramics powder be by 50 parts of aluminium oxide in parts by weight, 20 parts of titanium dioxide, 10 parts of silicon nitrides, 1 part of aluminium dihydrogen phosphate, 2 parts of yittrium oxide, the proportioning of 1 part of nickel oxide stir evenly, and are then placed into being heated in high temperature furnace, temperature Spend for 800-900 DEG C, heating 2h postcoolings are pulverized.
Phosphorous acid esters in the antioxidant are triethyl phosphorite, three isodecyl phosphites, triphenyl are sub- One or more in phosphate.
Solvent in the lubricant is turpentine oil or dimethylformamide.
Embodiment 2：
A kind of preparation method of high temperature resistant synchronous motor magnet steel provided in this embodiment is substantially same as Example 1, it is not It is the neodymium iron boron principal phase powder with point, according to 14wt%PrNd, 7wt%B by weight percentage, surplus is for Fe and not The proportioning of evitable metal impurities.
Embodiment 3：
A kind of preparation method of high temperature resistant synchronous motor magnet steel provided in this embodiment is substantially same as Example 1, it is not It is the rich neodymium phase powder with point, according to 13wt%PrNd, 5wt%Co, 5wt%Nb, 3wt% by weight percentage Cu, 0.8wt%Ga, 2wt%Mo, 0.5wt%Zn, 0.8wt%Ce, 0.3wt%Ni, 0.3wt%Ti, surplus is Fe and can not keep away The proportioning for the metal impurities exempted from.
Embodiment 4：
A kind of preparation method of high temperature resistant synchronous motor magnet steel provided in this embodiment is substantially same as Example 1, it is not It is the antioxidant with putting, according to 70 parts of petroleum ethers in parts by weight, 30 parts of polyethylene oxide alkyl ethers, 15 parts of phosphorous The proportioning of esters of gallic acid and 5 parts of rare earth nitrades.
Embodiment 5：
A kind of preparation method of high temperature resistant synchronous motor magnet steel provided in this embodiment is substantially same as Example 1, it is not It is the lubricant with point, according to 40 parts of calcium stearates in parts by weight, 5 parts of graphenes, 2 parts of emulsifying agents, 8 parts of oxidation second The proportioning of alkene/propylene oxide copolymer, 80 parts of solvents.
Embodiment 6：
A kind of preparation method of high temperature resistant synchronous motor magnet steel provided in this embodiment is substantially same as Example 1, it is not It is the refractory ceramics powder with point, according to 60 parts of aluminium oxide in parts by weight, 30 parts of titanium dioxide, 15 parts of nitridations Silicon, 5 parts of aluminium dihydrogen phosphates, 8 parts of yittrium oxide, the proportioning of 3 parts of nickel oxide.
Basic principle, main feature and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and what is described in the above embodiment and the description is only the present invention Principle, various changes and modifications of the present invention are possible without departing from the spirit and scope of the present invention, these change and Improvement is both fallen within the range of claimed invention.The protection domain of application claims by appended claims and its Equivalent defines.

Claims (3)

  1. A kind of 1. preparation method of high temperature resistant synchronous motor magnet steel, it is characterised in that：Comprise the following steps：
    Step 1: neodymium iron boron principal phase powder is prepared, according to 12-14wt%PrNd, 6-7wt%B by weight percentage, surplus For the proportioning of Fe and inevitable metal impurities, it is fitted into vaccum sensitive stove, heating-up temperature is 1500-1650 DEG C, and master is made Phase slab, is then put into hydrogen in hydrogen crushing furnace by obtained principal phase slab and crushes, finally the principal phase after hydrogen crushes is through airflow milling The principal phase powder that granularity is 2.8-3 μm is made；
    Step 2: rich neodymium phase powder is prepared, according to 11-13wt%PrNd, 1-5wt%Co, 1-5wt% by weight percentage Nb, 2-3wt%Cu, 0.5-0.8wt%Ga, 1-2wt%Mo, 0.2-0.5wt%Zn, 0.5-0.8wt%Ce, 0.2-0.3wt% Ni, 0.1-0.3wt%Ti, surplus are the proportioning of Fe and inevitable metal impurities, are fitted into vaccum sensitive stove, heating-up temperature For 1800-1850 DEG C, rich neodymium phase slab is prepared, obtained rich neodymium phase slab then is put into hydrogen in hydrogen crushing furnace crushes, and most passes through afterwards Mutually the rich neodymium phase powder that granularity is 1.0-2.0 μm is made through airflow milling in the rich neodymium crossed after hydrogen crushes；
    Step 3: antioxidant is prepared, according to 50-70 part petroleum ethers in parts by weight, 20-30 parts of polyethylene oxide alkyl The proportioning of ether, 10-15 part phosphorous acid esters and 1-5 parts of rare earth nitrades, is uniformly mixed, and supernatant is taken after standing 24h；
    Step 4: lubricant is prepared, according to 30-40 part calcium stearates in parts by weight, 1-5 parts of graphenes, 1-2 parts of emulsifications Agent, 2-8 parts of ethylene oxide/propylene oxide copolymers, the proportioning of 50-80 parts of solvents are stirred evenly, and heated in 80 DEG C of water-baths To obtain the final product after 6h；
    Step 5: Nd-Fe-B magnet steel is prepared, according to 80-90 parts principal phase in parts by weight, 5-20 parts of rich neodymium phases, 1-2 parts of antioxygens Agent, 0.5-2 part lubricant, be put into batch mixer mixing 2 it is small when, be pressed into blank with mould in the environment of stationary magnetic field, then When pre-burning 2 is small under 500 DEG C of vacuum conditions by blank, the antioxidant for becoming gas, lubricant is allowed to discharge, then applying argon gas are protected Shield 1200 DEG C sintering 4 it is small when, then level-one be tempered to 800 DEG C insulation 2 it is small when after, then second annealing to 400 DEG C insulation 2 it is small when It can obtain Nd-Fe-B magnet steel；
    Step 6: high temperature resistant Nd-Fe-B magnet steel is prepared, in Nd-Fe-B magnet steel surface spraying refractory ceramics powder, wherein described resistance to The preparation method of refractory ceramics powder is by 50-60 parts aluminium oxide, 20-30 parts of titanium dioxide, 10-15 parts of nitrogen in parts by weight SiClx, 1-5 part aluminium dihydrogen phosphate, 2-8 parts of yittrium oxide, the proportioning of 1-3 parts of nickel oxide stir evenly, and are then placed into high temperature furnace Heated, temperature is 800-900 DEG C, and heating 2h postcoolings are pulverized.
  2. 2. the preparation method of high temperature resistant synchronous motor magnet steel according to claim 1, it is characterised in that：The antioxidant In phosphorous acid esters be triethyl phosphorite, three isodecyl phosphites, the one or more in triphenyl phosphite.
  3. 3. the preparation method of high temperature resistant synchronous motor magnet steel according to claim 1, it is characterised in that：In the lubricant Solvent be turpentine oil or dimethylformamide.
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