CN106158207A - A kind of preparation method of the neodymium iron boron magnetic body without heavy rare earth - Google Patents

A kind of preparation method of the neodymium iron boron magnetic body without heavy rare earth Download PDF

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CN106158207A
CN106158207A CN201610757794.5A CN201610757794A CN106158207A CN 106158207 A CN106158207 A CN 106158207A CN 201610757794 A CN201610757794 A CN 201610757794A CN 106158207 A CN106158207 A CN 106158207A
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iron boron
neodymium iron
present
temperature
preparation
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余远
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Jingci Material Technology Co Ltd
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Jingci Material Technology Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • 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
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/105—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing inorganic lubricating or binding agents, e.g. metal salts
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps

Abstract

The invention provides the preparation method of a kind of neodymium iron boron magnetic body without heavy rare earth, the present invention is directed to neodymium iron boron magnetic body when without heavy rare earth or low content heavy rare earth, the problem that the magnetic property existed reduces, on the basis of regulation is without heavy rare earth formula, uses cost relatively low, control relatively simple crystal fining method, preparation overall process is adjusted by refinement, put forth effort to control the content of C and O of magnet, optimize the temperature and time of sintering further, reduce the crystallite dimension of magnet principal crystalline phase.Thus in the case of without any heavy rare earth, it is ensured that the remanent magnetism of Nd-Fe-B magnetic material does not reduces, and can also significantly improve the coercivity of magnet alloy.

Description

A kind of preparation method of the neodymium iron boron magnetic body without heavy rare earth
Technical field
The invention belongs to magnet preparing technical field, particularly relate to the preparation side of a kind of neodymium iron boron magnetic body without heavy rare earth Method.
Background technology
Hard magnetic body i.e. permanent magnet, it is possible to the long-term magnet keeping its magnetic, is difficult to loss of excitation, is not easy to be magnetized.Thus, nothing Opinion is in commercial production or in daily life, one of muscle material that hard magnetic body is the most frequently used.Hard magnetic body can be divided into natural Magnet and artificial magnet, artificial magnet refers to can be reached and natural magnet (magnet) phase by the alloy of synthesis different materials Same effect, but also magnetic force can be improved.The sixties in 20th century, the appearance of rare earth permanent magnet, then the application for magnet opens One New Times, first generation samarium cobalt permanent magnet SmCo5, second filial generation precipitation hardenable samarium cobalt permanent magnet Sm2Co17, up to now, develop into Third generation Nd-Fe-B permanent magnet material (NdFeB).Although at present ferrimagnet remains the permanent magnet material that consumption is maximum, but neodymium ferrum The output value of boron magnet has substantially exceeded ferrite permanent-magnet materials, has evolved into a big industry.
Neodymium iron boron magnetic body is also referred to as neodymium magnet (Neodymium magnet), and its chemical formula is Nd2Fe14B, is a kind of artificial Permanent magnet, be also the permanent magnet so far with the strongest magnetic force, its maximum magnetic energy product (BH) max exceeds ferrite 10 More than Bei, when naked magnetic, its magnetic force can reach 3500 Gauss.The advantage of neodymium iron boron magnetic body is that cost performance is high, body Long-pending little, lightweight, good mechanical property and the feature such as magnetic is strong, the advantage of such high-energy-density makes Nd-Fe-B permanent magnet material Modern industry and electronic technology obtain a wide range of applications, is described as magnetic king in magnetics circle.Thus, the system of neodymium iron boron magnetic body The focus that standby and extension always gives more sustained attention in the industry.
Along with the development of the association area such as air-conditioning, electric automobile, more and more higher to the demand of neodymium iron boron magnetic body, to its performance Requirement significantly improves.Adding rare earth element in magnet is a kind of Main Means improving magnetic property, in recent years, is developing high property While energy magnet, client is stricter to the control of cost, but the price of heavy rare earth rises steadily, and various heavy rare earth Resource is all the scarce resource that some are non-renewable, and therefore, the heavy rare earth consumption reducing sintered NdFeB is particularly important.Exist at present In the case of not reducing material property, grain boundary decision is a kind of method reducing heavy rare earth content, but grain boundary decision method one Equipment and the input of manpower that aspect needs are relatively big, and will also result in the wave of heavy rare earth resource during various grain boundary decision Taking, additionally grain boundary decision has significantly restriction to the size and dimension of magnet, can not be applicable to all of magnet.
Therefore, how in the case of adding without heavy rare earth, the magnetic property of neodymium iron boron magnetic body is effectively stablized, it has also become industry Interior forward-looking neodymium iron boron magnetic body production firm and a line research worker problem demanding prompt solution.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide the system of a kind of neodymium iron boron magnetic body without heavy rare earth Preparation Method, uses the preparation method that the present invention provides, in the case of without any heavy rare earth, it is possible to stablize magnet material There is not situation about reducing in magnetic property, particularly remanent magnetism, and can also significantly improve the coercivity of neodymium iron boron magnetic body.
The invention provides the preparation method of a kind of neodymium iron boron magnetic body without heavy rare earth, comprise the following steps:
1) carry out neodymium iron boron magnetic body raw material after rapid hardening gets rid of band, obtaining neodymium iron boron and getting rid of strap；
2) neodymium iron boron that above-mentioned steps obtains is got rid of strap through the quick-fried process of hydrogen, obtain the quick-fried rear coarse powder of hydrogen；
3) the quick-fried rear coarse powder of hydrogen above-mentioned steps obtained, through Mechanical Crushing, adds after additive mixes, obtains Mixed coarse powder；
4) mixed coarse powder above-mentioned steps obtained is after anaerobic air-flow mill grinds, and obtains neodymium iron boron fine powder；
5), after neodymium iron boron fine powder addition lubricant above-mentioned steps obtained mixes again, mixed fine powder is obtained；
6) mixed fine powder above-mentioned steps obtained is after transpassivation, then after orientation compacting and isostatic pressed process, obtains Neodymium iron boron pressed compact；
7) neodymium iron boron pressed compact above-mentioned steps obtained is after low temperature sinters for a long time, then after being tempered, obtains neodymium Iron boron magnet；
The sintering temperature that described low temperature sinters for a long time is 1010～1030 DEG C；The time that described low temperature sinters for a long time is 10～15h.
Preferably, described neodymium iron boron magnetic body raw material, composition includes by mass percentage: Pr-Nd:31.5%～33.5%； B:0.85%～0.9%；Al:0.6%～0.7%；Cu:0.2%～0.6%；Co:1.0%～1.5%；Ga:0.4%～ 0.6%；Zr:0.15%～0.3%；Surplus is Fe.
Preferably, described neodymium iron boron gets rid of the average thickness of strap less than or equal to 0.3mm；Described neodymium iron boron gets rid of the column of strap Crystalline substance a size of 3.8～4.2 μm.
Preferably, in the quick-fried process of described hydrogen, the pressure of described suction hydrogen is 0.08～0.15Mpa；
The temperature of described dehydrogenation is 490～510 DEG C.
Preferably, one or more during described additive includes zinc stearate, calcium stearate and Polyethylene Glycol octane；Institute The addition stating additive is 0.03%～0.05%；
The incorporation time of described mixing is 90～150min；
Described lubricant includes methyl ester class and/or alcohols；The addition of described lubricant accounts for the ratio of neodymium iron boron fine powder quality Value is 0.1%～0.3%；
The described incorporation time again mixed is 150～210min.
Preferably, described anaerobic airflow milling is to carry out airflow milling under conditions of protective gas；
The grinding gas pressure of described airflow milling is 0.4～0.5MPa；
The grading wheel rotating speed of described airflow milling is 4800～4950rpm；
The particle mean size of described neodymium iron boron fine powder is 2.5～2.7 μm.
Preferably, the time of described passivation is 20～30h；
The oxygen content of described orientation compacting is less than or equal to 0.5%；Described orientation compacting magnetic field intensity be 1.2～ 1.8T；
The pressure that described isostatic pressed processes is 150～250Mpa；
Described green density is 3.6～3.8g/cm3。
Preferably, what described low temperature sintered for a long time concretely comprises the following steps:
A) under conditions of vacuum or protective gas, neodymium iron boron pressed compact is sequentially passed through defat and fires, deaerate for the first time Fire and second time deaerates after firing, obtain just section sintering intermediate；
B) first section sintering intermediate above-mentioned steps obtained, carries out after first stage intensification constant temperature fires, obtaining one section Sintering intermediate；
C) one-stage sintering intermediate above-mentioned steps obtained, carries out after second stage intensification constant temperature fires, obtaining two-stage nitration Sintering intermediate；
D) bis sintering intermediate above-mentioned steps obtained, after carrying out phase III cooling, obtains in the middle of three-stage sintering Body；
E) three-stage sintering intermediate above-mentioned steps obtained, carries out fourth stage intensification constant temperature and fires.
Preferably, described tempering includes one-level tempering and second annealing；
The temperature of described one-level tempering is 850～950 DEG C；The time of described one-level tempering is 4～5h；
The temperature of described second annealing is 480～520 DEG C；The time of described second annealing is 3～4h.
Preferably, middle tempering is also included before described second annealing；
In the middle of described, the temperature of tempering is (temperature of second annealing+15 DEG C)；
In the middle of described, the time of tempering is 1.5～2.5h.
The invention provides the preparation method of a kind of neodymium iron boron magnetic body without heavy rare earth, comprise the following steps, first will Neodymium iron boron magnetic body raw material carries out after rapid hardening gets rid of band, obtaining neodymium iron boron and getting rid of strap；Then the neodymium iron boron that above-mentioned steps obtains is got rid of band Sheet, through the quick-fried process of hydrogen, obtains the quick-fried rear coarse powder of hydrogen；The quick-fried rear coarse powder of hydrogen above-mentioned steps obtained again, through Mechanical Crushing, adds After additive mixes, obtain mixed coarse powder；Mixed coarse powder above-mentioned steps obtained subsequently, after anaerobic air-flow mill grinds, obtains To neodymium iron boron fine powder；After neodymium iron boron fine powder addition lubricant above-mentioned steps obtained again mixes again, obtain mixed fine powder； Mixed fine powder above-mentioned steps obtained afterwards is after transpassivation, then after orientation compacting and isostatic pressed process, obtains neodymium iron boron Pressed compact；The neodymium iron boron pressed compact finally above-mentioned steps obtained is after low temperature sinters for a long time, then after being tempered, obtains neodymium ferrum Boron magnet；The sintering temperature that described low temperature sinters for a long time is 1010～1030 DEG C；The time that described low temperature sinters for a long time is 10～15h.Compared with prior art, the present invention is directed to neodymium iron boron magnetic body when without heavy rare earth or low content heavy rare earth, exist Magnetic property reduce problem, and grain boundary decision method exist defect etc., the present invention is in the situation without heavy rare earth formula Under, use cost relatively low, control relatively simple crystal fining method, refined by the optimization of preparation overall process, put forth effort to control The content of C and O of magnet, optimizes the temperature and time of sintering further, reduces the crystallite dimension of magnet principal crystalline phase.Thus In the case of any heavy rare earth, it is ensured that in the case of material remanent magnetism does not reduces, significantly improve the coercivity of alloy.Real Testing result to show, the crystallite dimension of the neodymium iron boron magnetic body that the present invention provides is less, average grain size 4.5～5.5 μm, neodymium iron boron The remanent magnetism of magnet reaches more than 13kGs, and coercivity reaches more than 21kOe.
Accompanying drawing explanation
Fig. 1 is the metallurgical microstructrue figure of the neodymium iron boron magnetic body of the embodiment of the present invention 1 preparation；
Fig. 2 is the magnetic property curve chart of the neodymium iron boron magnetic body of the embodiment of the present invention 1 preparation.
Detailed description of the invention
In order to be further appreciated by the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but Should be appreciated that these descriptions are intended merely to further illustrate the features and advantages of the present invention rather than to invention claim Limit.
The all raw materials of the present invention, are not particularly limited its source, that commercially buy or according to people in the art Prepared by the conventional method known to Yuan.
The all raw materials of the present invention, are not particularly limited its purity, present invention preferably employs analytical pure or sintered NdFeB The conventional purity that field of magnets uses.
The invention provides the preparation method of a kind of neodymium iron boron magnetic body without heavy rare earth, comprise the following steps:
1) carry out neodymium iron boron magnetic body raw material after rapid hardening gets rid of band, obtaining neodymium iron boron and getting rid of strap；
2) neodymium iron boron that above-mentioned steps obtains is got rid of strap through the quick-fried process of hydrogen, obtain the quick-fried rear coarse powder of hydrogen；
3) the quick-fried rear coarse powder of hydrogen above-mentioned steps obtained, through Mechanical Crushing, adds after additive mixes, obtains Mixed coarse powder；
4) mixed coarse powder above-mentioned steps obtained is after anaerobic air-flow mill grinds, and obtains neodymium iron boron fine powder；
5), after neodymium iron boron fine powder addition lubricant above-mentioned steps obtained mixes again, mixed fine powder is obtained；
6) mixed fine powder above-mentioned steps obtained is after transpassivation, then after orientation compacting and isostatic pressed process, obtains Neodymium iron boron pressed compact；
7) neodymium iron boron pressed compact above-mentioned steps obtained is after low temperature sinters for a long time, then after being tempered, obtains neodymium Iron boron magnet；
The sintering temperature that described low temperature sinters for a long time is 1010～1030 DEG C；The time that described low temperature sinters for a long time is 10～15h.
First neodymium iron boron magnetic body raw material is carried out after rapid hardening gets rid of band, obtaining neodymium iron boron and getting rid of strap by the present invention.
The particular make-up of described neodymium iron boron magnetic body raw material is not particularly limited by the present invention, knows with those skilled in the art The neodymium iron boron magnetic body raw material not containing heavy rare earth form, those skilled in the art can be according to practical condition, product The factors such as product requirement and quality control select and adjust, and the present invention is further crystal grain thinning, improves the magnetic of product Can, the percentage by weight of described content of rare earth is preferably controlled between 31.5%～33.5%, B content preferably 0.85%～ Between 0.9%, Al content is preferably between 0.6%～0.7%, and Cu content is preferably between 0.2%～0.6%, and Co content is excellent Be selected between 1%～1.5%, Ga content preferably between 0.4%～0.6%, Zr content preferably 0.15%～0.3% it Between, remaining is Fe；The mass percentage content of i.e. Pr-Nd be preferably 31.5%～33.5%, more preferably 31.75%～ 33.25%, more preferably 32%～33%, most preferably 32.25%～32.75%；The mass percentage content of B is preferably 0.85%～0.9%, more preferably 0.86%～0.89%, most preferably 0.87%～0.88%；The mass percent of Al contains Amount preferably 0.6%～0.7%, more preferably 0.62%～0.68%, most preferably 0.64%～0.66%；The matter of described Cu Amount degree is preferably 0.2%～0.6%, more preferably 0.3%～0.5%, most preferably 0.35%～0.45%；Institute State the mass percentage content of Co and be preferably 1%～1.5%, more preferably 1.1%～1.4%, most preferably 1.2%～ 1.3%；The mass percentage content of described Ga is preferably 0.4%～0.6%, more preferably 0.45%～0.55%, most preferably It is 0.47%～0.53%；The mass percentage content of described Zr be preferably 0.15%～0.3%, more preferably 0.18%～ 0.27%, most preferably 0.21%～0.24%.
The actual conditions of band is got rid of in described rapid hardening by the present invention and parameter is not particularly limited, and knows with those skilled in the art Rapid hardening get rid of actual conditions and the parameter of band, those skilled in the art can according to practical condition, product requirement with And the factor such as quality control selects and adjusts, with crystal grain thinning as preferred version.The neodymium after band is got rid of in rapid hardening of the present invention Ferrum boron gets rid of the requirement of strap and is not particularly limited, and gets rid of the parameter of strap, ability with rapid hardening well known to those skilled in the art Field technique personnel can select according to factors such as practical condition, product requirement and quality controls and adjust, this Bright for further crystal grain thinning, improve the magnetic property of product, described neodymium iron boron gets rid of the thickness of strap and is preferably less than equal to 0.3mm, more preferably 0.1～0.3mm, more preferably 0.12～0.25mm, most preferably 0.15～0.2mm；Of the present invention Neodymium iron boron gets rid of the column crystal of strap and is preferably dimensioned to be 3.8～4.2 μm, more preferably 3.9～4.1 μm, most preferably 4.0 μm.This Described rapid hardening is got rid of the equipment of band and is not particularly limited by invention, gets rid of the equipment of band i.e. with rapid hardening well known to those skilled in the art Can, those skilled in the art can select according to factors such as practical condition, product requirement and quality controls and adjust Whole, rapid hardening of the present invention is got rid of the equipment of band and is preferably vacuum rapid hardening spun furnace.
Then the neodymium iron boron that above-mentioned steps obtains is got rid of strap through the quick-fried process of hydrogen by the present invention, obtains the quick-fried rear coarse powder of hydrogen.
Actual conditions and the parameter of present invention process quick-fried to described hydrogen are not particularly limited, and know with those skilled in the art The broken actual conditions of hydrogen explosion and parameter, those skilled in the art can according to practical condition, product requirement with And the factor such as quality control selects and adjusts, the present invention is further crystal grain thinning, improves the magnetic property of product, described hydrogen In quick-fried processing procedure, the pressure of described suction hydrogen is preferably 0.08～0.15MPa, more preferably 0.09～0.14MPa, most preferably 0.10～0.13MPa；After saturated suction hydrogen, the desorption temperature of the quick-fried process of described hydrogen is preferably 490～510 DEG C, more preferably 495～ 505 DEG C, most preferably 497～503 DEG C, it is specifically as follows 500 DEG C.
The quick-fried rear coarse powder of hydrogen that above-mentioned steps is obtained by the present invention again, through Mechanical Crushing, adds additive and mixes After, obtain mixed coarse powder.
The condition of described Mechanical Crushing is not particularly limited by the present invention, with Mechanical Crushing well known to those skilled in the art Condition, those skilled in the art can select according to factors such as practical condition, product requirement and quality controls Select and adjust, with crystal grain thinning as preferred version.Described additive and addition thereof are not particularly limited by the present invention, with ability Magnet mixing additive known to field technique personnel and addition thereof, those skilled in the art can be according to actual production The factors such as situation, product requirement and quality control select and adjust, and the present invention is further crystal grain thinning, improve product Magnetic property, described additive preferably includes one or more in zinc stearate, calcium stearate and Polyethylene Glycol octane, more excellent Elect zinc stearate, calcium stearate or Polyethylene Glycol octane, most preferably zinc stearate as；The addition of described additive is preferably 0.03%～0.05%, more preferably 0.035%～0.045%, most preferably 0.037%～0.043%.
The condition of described mixing is not particularly limited by the present invention, with mixing condition well known to those skilled in the art i.e. Can, those skilled in the art can select according to factors such as practical condition, product requirement and quality controls and adjust Whole, the present invention is further crystal grain thinning, improves the magnetic property of product, and the time of described mixing is preferably 90～150min, more Preferably 100～140min, most preferably 110～130min, it is specifically as follows 120min.The present invention equipment to described mixing Being not particularly limited, with magnet mixing apparatus well known to those skilled in the art, those skilled in the art can be according to reality The factors such as the border condition of production, product requirement and quality control select and adjust, and the equipment of mixing of the present invention is preferred Powder machine is mixed for three-dimensional.
The mixed coarse powder that above-mentioned steps is obtained by the present invention subsequently, after anaerobic air-flow mill grinds, obtains neodymium iron boron fine powder.
Detailed process and condition that described anaerobic air-flow mill is ground by the present invention are not particularly limited, with people in the art Airflow milling process known to Yuan, in the case of oxygen-adding amount is 0, is carried out, this area skill under conditions of protective gas Art personnel can select according to factors such as practical condition, product requirement and quality controls and adjust, and the present invention is Further crystal grain thinning, improves the magnetic property of product, the grinding gas pressure of described anaerobic airflow milling be preferably 0.4～ 0.5MPa, more preferably 0.42～0.48MPa, most preferably 0.44～0.46MPa；The grading wheel rotating speed of described airflow milling is preferred It is 4800～4950rpm, more preferably 4825～4925rpm, most preferably 4850～4900rpm；Protectiveness of the present invention Gas is preferably nitrogen or noble gas, more preferably nitrogen or argon, most preferably argon.
The granularity of described neodymium iron boron fine powder is not particularly limited by the present invention, with neodymium iron boron well known to those skilled in the art The granularity of magnet raw material fine powder, those skilled in the art can be according to practical condition, product requirement and quality control The factors such as system select and adjust, and the present invention is further crystal grain thinning, improve the magnetic property of product, described neodymium iron boron fine powder Granularity be preferably 2.5～2.7 μm, more preferably 2.55～2.65 μm, most preferably 2.57～2.63 μm.
After the neodymium iron boron fine powder addition lubricant that above-mentioned steps is obtained by the present invention again mixes again, obtain mixed thin Powder.
Described lubricant and addition thereof are not particularly limited by the present invention, mix with magnet well known to those skilled in the art Share lubricant and addition thereof, those skilled in the art can be according to practical condition, product requirement and quality The factors such as control select and adjust, and the present invention is further crystal grain thinning, improve the magnetic property of product, and described lubricant is excellent Choosing includes methyl ester class and/or alcohols, more preferably methyl ester class or alcohols, most preferably methyl ester class；The addition of described lubricant Account for the ratio of neodymium iron boron fine powder quality and be preferably 0.1%～0.3%, more preferably 0.15%～0.25%, most preferably 0.18%～0.22%.
The described condition again mixed is not particularly limited by the present invention, with mixing condition well known to those skilled in the art , those skilled in the art can carry out selecting according to factors such as practical condition, product requirement and quality controls and Adjust, the present invention is further crystal grain thinning, improve product magnetic property, the described time again mixed be preferably 150～ 210min, more preferably 160～200min, most preferably 170～190min, it is specifically as follows 180min.The present invention is to described The equipment again mixed is not particularly limited, with magnet mixing apparatus well known to those skilled in the art, art technology Personnel can select according to factors such as practical condition, product requirement and quality controls and adjust, of the present invention The equipment of mixing is preferably V-type and mixes powder machine.
Mixed fine powder above-mentioned steps obtained after the present invention is after transpassivation, then processes through orientation compacting and isostatic pressed After, obtain neodymium iron boron pressed compact.
The condition of described passivation is not particularly limited by the present invention, and those skilled in the art can be according to actual production feelings The factors such as condition, product requirement and quality control select and adjust, and the present invention is further crystal grain thinning, improve product Magnetic property, the time of described passivation is preferably 20～30h, more preferably 22～28h, and most preferably 24～26h are specifically as follows 24h。
The condition of described orientation compacting is not particularly limited by the present invention, with orientation compacting well known to those skilled in the art Condition, those skilled in the art can select according to factors such as practical condition, product requirement and quality controls Selecting and adjust, the present invention is further crystal grain thinning, improves the magnetic property of product, and the magnetic field intensity of described orientation compacting is preferably 1.2～1.8T, more preferably 1.3～1.6T, most preferably 1.4～1.5T；The oxygen content of described orientation compacting is preferably less than Equal to 0.5%, more preferably 0.1%～0.4%, most preferably 0.2%～0.3%.
The present invention is to improve the effect of compacting, also includes that isostatic pressed processes step after the compacting of described orientation；The present invention is to institute The condition stating isostatic pressed process is not particularly limited, and processes with the isostatic pressed of neodymium iron boron magnetic body well known to those skilled in the art Condition, those skilled in the art can select according to factors such as practical condition, product requirement and quality controls Selecting and adjust, the present invention is further crystal grain thinning, improves the magnetic property of product, and the pressure that described isostatic pressed processes is preferably 150～250MPa, more preferably 170～230MPa, most preferably 190～210MPa.
The density of described neodymium iron boron pressed compact is not particularly limited by the present invention, with neodymium iron boron well known to those skilled in the art The density of pressed compact, those skilled in the art can be according to factors such as practical condition, product requirement and quality controls Selecting and adjust, the present invention is further crystal grain thinning, improves the magnetic property of product, and the density of described neodymium iron boron pressed compact is excellent Elect 3.6～3.8g/cm as3, more preferably 3.65～3.75g/cm3, most preferably 3.67～3.72g/cm3。
The neodymium iron boron pressed compact that above-mentioned steps is finally obtained by the present invention is after low temperature sinters for a long time, then is tempered After, obtain neodymium iron boron magnetic body.
The sintering temperature that low temperature of the present invention sinters for a long time is preferably 1010～1030 DEG C, more preferably 1015～ 1025 DEG C, most preferably 1018～1023 DEG C；The time that described low temperature sinters for a long time is preferably 10～15h, more preferably 11 ～14h, most preferably 12～13h.
The concrete steps that described low temperature is sintered by the present invention for a long time are not particularly limited, and know with those skilled in the art Magnet sintering concrete steps, those skilled in the art can be according to practical condition, product requirement and quality The factors such as control select and adjust, and the present invention is further crystal grain thinning, improve the magnetic property of product, when described low temperature is long Between sintering be preferably multi-steps sintering, concrete steps more preferably:
A) under conditions of vacuum or protective gas, neodymium iron boron pressed compact is sequentially passed through defat and fires, deaerate for the first time Fire and second time deaerates after firing, obtain just section sintering intermediate；
B) first section sintering intermediate above-mentioned steps obtained, carries out after first stage intensification constant temperature fires, obtaining one section Sintering intermediate；
C) one-stage sintering intermediate above-mentioned steps obtained, carries out after second stage intensification constant temperature fires, obtaining two-stage nitration Sintering intermediate；
D) bis sintering intermediate above-mentioned steps obtained, after carrying out phase III cooling, obtains in the middle of three-stage sintering Body；
E) three-stage sintering intermediate above-mentioned steps obtained, carries out fourth stage intensification constant temperature and fires.
When low temperature of the present invention sinter for a long time specifically carry out by above-mentioned steps time, described low temperature sinter for a long time time Between preferably add up according to the time of each step.
The present invention is first under conditions of vacuum or protective gas, by neodymium iron boron pressed compact through primary stage ladder-elevating temperature After firing, obtain just section sintering intermediate.
The sintering of described neodymium iron boron pressed compact is not particularly limited by the present invention, with neodymium iron boron well known to those skilled in the art The sintering concept of magnet, the present invention is preferably liquid-phase sintering or solid-phase sintering, more preferably liquid-phase sintering, more preferably will Loose being placed in material boat of neodymium iron boron pressed compact is fired in agglomerating plant.
The equipment of described sintering is not particularly limited by the present invention, with sintered NdFeB magnetic well known to those skilled in the art The equipment of body, the present invention is preferably vacuum sintering furnace.Temperature homogeneity in the equipment of described sintering is not had by the present invention Limit especially, with temperature well known to those skilled in the art all with property, the furnace temperature of vacuum sintering furnace of the present invention is uniform Property be preferably ± 5 DEG C, more preferably ± 4 DEG C, most preferably ± 3 DEG C；The Pressure Rise Rate of vacuum sintering furnace of the present invention is the least In equal to 0.6Pa/h, more preferably less than or equal to 0.5Pa/h, more preferably less than equal to 0.4Pa/h.
The condition of described vacuum or protective gas is not particularly limited by the present invention, with well known to those skilled in the art Conventional production practices, those skilled in the art can be carried out according to practical condition, prescription and properties of product Selecting and adjust, the present invention is more preferably vacuum；The pressure of described vacuum is not particularly limited by the present invention, with art technology The vacuum pressure of the Sintered NdFeB magnet known to personnel, the pressure of vacuum of the present invention is preferably less than equal to 0.5Pa, more preferably 0.01～0.45Pa, more preferably 0.1～0.4Pa, most preferably 0.25～0.35Pa.Of the present invention Protective gas is preferably noble gas and/or nitrogen, more preferably argon and/or nitrogen, most preferably argon or nitrogen.
Curve of firing during described multi-steps sintering is not particularly limited by the present invention, and those skilled in the art can root Selecting according to practical condition, prescription and properties of product and adjust, multi-steps sintering process of the present invention is preferred Including primary stage sintering (or referred to as presintering i.e. includes that defat is fired, degassing for the first time is fired and second time degassing is fired), First paragraph sintering, second segment sintering, three-stage sintering and the 4th section of sintering, based on general knowledge known in this field, the primary stage sinters The stage of sintering process can be can be regarded as, then multi-steps sintering process of the present invention is five sections of sintering, it is also possible to be not considered sintering The stage of process, then multi-steps sintering process of the present invention is then four sections of sintering.
The present invention include successively defat fire (defat platform, this stage can by pressed compact with most of fat of physical absorption Class is got rid of in gaseous form), for the first time degassing fire that (the first degassing platform, the most fully gets rid of the gas of physical absorption, separately Outer rich neodymium starts liquefaction mutually) and second time degassing is fired, and (the second degassing platform, sufficiently gets rid of the gas of chemisorbed, makes richness Neodymium the most fully liquefies, and blank drastically shrinks).
The actual conditions of described defat sintering procedure is not particularly limited by the present invention, with well known to those skilled in the art The actual conditions of skimming processes in magnet sintering process, those skilled in the art can be according to practical condition, quality Requiring and properties of product select and adjust, the present invention is further crystal grain thinning, improves the magnetic property of product, described de- The thermostat temperature that fat platform temperature, i.e. defat are fired is preferably 200～300 DEG C, more preferably 220～280 DEG C, most preferably 240～260 DEG C；The heating rate that described defat is fired is preferably 5～6 DEG C/min, more preferably 5.2～5.8 DEG C/min, optimum Elect 5.4～5.6 DEG C/min as；The constant temperature time that described defat is fired is preferably 1～2h, more preferably 1.2～1.8h, most preferably It is 1.4～1.6h.
The actual conditions that the degassing of described first time is fired by the present invention is not particularly limited, and knows with those skilled in the art Magnet sintering process in the actual conditions of degasification process, those skilled in the art can be according to practical condition, matter Amount requires and properties of product select and adjust, and the present invention is further crystal grain thinning, improves the magnetic property of product, described First degassing platform temperature, the temperature fired that deaerates i.e. for the first time is preferably 500～700 DEG C, more preferably 550～650 DEG C, It is preferably 575～625 DEG C；The heating rate fired of degassing of described first time is preferably 5～6 DEG C/min, more preferably 5.2～ 5.8 DEG C/min, most preferably 5.4～5.6 DEG C/min；The constant temperature time fired of degassing of described first time is preferably 2～3h, more excellent Elect 2.2～2.8h as, most preferably 2.4～2.6h.
The actual conditions that the degassing of described second time is fired by the present invention is not particularly limited, and knows with those skilled in the art Magnet sintering process in the actual conditions of degasification process, those skilled in the art can be according to practical condition, matter Amount requires and properties of product select and adjust, and the present invention is further crystal grain thinning, improves the magnetic property of product, described Second degassing platform temperature, the temperature fired that deaerates i.e. for the second time is preferably 800～900 DEG C, more preferably 820～880 DEG C, It is preferably 840～860 DEG C；The described second time heating rate fired of degassing is preferably 4～5 DEG C/min, more preferably 4.2～ 4.8 DEG C/min, most preferably 4.4～4.6 DEG C/min；The described second time constant temperature time fired of degassing is preferably 3～5h, more excellent Elect 3.5～4.5h as, most preferably 3.8～4.2h.
First section that then above-mentioned steps is obtained by present invention sintering intermediate, carries out after first stage intensification constant temperature fires, Obtain one-stage sintering intermediate.
The parameter that described first stage intensification constant temperature is fired by the present invention is not particularly limited, and those skilled in the art are permissible Selecting according to practical condition, useful load, oxygen content and green compact size etc. or adjust, the present invention is for refining crystalline substance further Grain, improves the magnetic property of product, and the heating rate that described first stage intensification constant temperature is fired is preferably 2～3 DEG C/min, more preferably It is 2.2～2.8 DEG C/min, most preferably 2.4～2.6 DEG C/min.The perseverance that described first stage intensification constant temperature is fired by the present invention Temperature temperature is not particularly limited, and those skilled in the art can be according to practical condition, useful load, oxygen content and green compact size Etc. selecting or adjust, the present invention is further crystal grain thinning, improves the magnetic property of product, described first stage intensification constant temperature The thermostat temperature fired is preferably (sintering temperature-20 DEG C), i.e. less than sintering temperature 20 DEG C, and i.e. 980～1080 DEG C, more preferably 985～1085 DEG C, most preferably 990～1090 DEG C.The constant temperature time that described first stage intensification constant temperature is fired by the present invention does not has Having restriction especially, those skilled in the art can select according to practical condition, useful load, oxygen content and green compact size etc. Selecting or adjust, the present invention is further crystal grain thinning, improves the magnetic property of product, the perseverance that described first stage intensification constant temperature is fired The temperature time is preferably 0～1h, more preferably≤1h, most preferably 0.1～0.8h.
The present invention arranges first presintering platform before entering sintering temperature platform, the hair of all positions in can promoting stove Base, to the concordance of temperature, makes all of blank sintering more uniform.
The one-stage sintering intermediate that above-mentioned steps is obtained by the present invention again, carries out after second stage intensification constant temperature fires, To bis sintering intermediate.
The parameter that described second stage intensification constant temperature is fired by the present invention is not particularly limited, and those skilled in the art are permissible Selecting according to practical condition, useful load, oxygen content and green compact size etc. or adjust, the present invention is for refining crystalline substance further Grain, improves the magnetic property of product, and the heating rate that described second stage intensification constant temperature is fired is preferably 2～3 DEG C/min, more preferably It is 2.2～2.8 DEG C/min, most preferably 2.4～2.6 DEG C/min.The perseverance that described second stage intensification constant temperature is fired by the present invention Temperature temperature is not particularly limited, and those skilled in the art can be according to practical condition, useful load, oxygen content and green compact size Etc. selecting or adjust, the present invention is further crystal grain thinning, improves the magnetic property of product, described second stage intensification constant temperature The thermostat temperature fired is preferably sintering temperature, i.e. 1000～1100 DEG C, more preferably 1020～1080 DEG C, and most preferably 1040 ～1060 DEG C.The constant temperature time that described second stage intensification constant temperature is fired by the present invention is not particularly limited, people in the art Member can select according to practical condition, useful load, oxygen content and green compact size etc. or adjust, and the present invention is further Crystal grain thinning, improves the magnetic property of product, and the constant temperature time that described second stage intensification constant temperature is fired is preferably 3～6h, more excellent Elect 3.5～5.5h as, most preferably 4～5h.
The present invention is incubated under sintering temperature (T1), and blank is carried out further presintering, blank under this insulation platform Diffusion densification stage is basically completed, and blank shrinks and is basically completed, but organizational structure is also not up to ideal state.
The bis sintering intermediate that above-mentioned steps is obtained by the present invention subsequently, after carrying out phase III cooling, obtains three sections Sintering intermediate.
The parameter that the described phase III is lowered the temperature by the present invention is not particularly limited, and those skilled in the art can be according to reality The condition of production, useful load, oxygen content and green compact size etc. select or adjust, the cooling of phase III of the present invention cooling Mode is preferably natural cooling, more preferably with stove natural cooling.Temperature after the cooling that the described phase III is lowered the temperature by the present invention Degree is not particularly limited, and those skilled in the art can enter according to practical condition, useful load, oxygen content and green compact size etc. Row selects or adjusts, and the present invention is further crystal grain thinning, improves the magnetic property of product, after the cooling of cooling of described phase III Temperature be preferably 700～800 DEG C, more preferably 720～780 DEG C, most preferably 740～760 DEG C.
The three-stage sintering intermediate that above-mentioned steps is finally obtained by the present invention, carries out fourth stage intensification constant temperature and fires.
The parameter that described fourth stage intensification constant temperature is fired by the present invention is not particularly limited, and those skilled in the art are permissible Selecting according to practical condition, useful load, oxygen content and green compact size etc. or adjust, the present invention is for refining crystalline substance further Grain, improves the magnetic property of product, and the heating rate that described fourth stage intensification constant temperature is fired is preferably 5～7 DEG C/min, more preferably It is 5.5～6.5 DEG C/min, most preferably 5.7～6.3 DEG C/min.The perseverance that described fourth stage intensification constant temperature is fired by the present invention Temperature temperature is not particularly limited, and those skilled in the art can be according to practical condition, useful load, oxygen content and green compact size Etc. selecting or adjust, the present invention is further crystal grain thinning, improves the magnetic property of product, described fourth stage intensification constant temperature The thermostat temperature fired is preferably sintering temperature～(sintering temperature+20 DEG C), i.e. 1010～1050 DEG C, more preferably 1015～ 1045 DEG C, more preferably 1020～1040 DEG C, most preferably 1025～1035 DEG C.The present invention is to described fourth stage intensification constant temperature The constant temperature time fired is not particularly limited, those skilled in the art can according to practical condition, useful load, oxygen content and Green compact size etc. selects or adjusts, and the present invention is further crystal grain thinning, improves the magnetic property of product, described phase III The constant temperature time that intensification constant temperature is fired is preferably 5～8h, more preferably 5.5～7.5h, most preferably 6～7h.
The present invention, after second stage intensification constant temperature is fired, is the most directly warmed up to T1 DEG C without insulation after being lowered the temperature by blank ～(T1+20) DEG C carries out fourth stage intensification constant temperature and fire, on the one hand it is to avoid long-time insulation at a sintering temperature to go out Existing abnormal grain! growth or average grain size are excessive, on the other hand again can promote blank at T1 DEG C～(T1+20) DEG C insulation Spreading densification further, make blank fully shrink, organizational structure reaches perfect condition, prevents sintering temperature or sintering time not The blank underburnt caused enough, thus after avoiding burning, blank squareness is on the low side.The above-mentioned whole step of the present invention is the most preferably in vacuum Carrying out under state, to ensure that blank is not oxidized, the mechanical pump of evacuation unit to be kept and lobe pump are in running status.
After described fourth stage intensification constant temperature is fired by the present invention, i.e. technique after sintering is not particularly limited, with ability Conventional steps known to field technique personnel, the present invention is preferably cooling step；The present invention is concrete to described cooling step Technique is not particularly limited, those skilled in the art can according to actual production process, batch, the concrete size of product and Properties of product carry out selective control, and the present invention is to improve the magnetic firing effect and neodymium iron boron magnetic body of neodymium iron boron magnetic body pressed compact Can, the present invention preferably cools down under conditions of nitrogen or noble gas, more preferably in nitrogen or the condition of noble gas Under air-cooled, more specifically the most air-cooled to less than 100 DEG C under conditions of argon；The speed of described cooling is limited by the present invention the most especially System, with the cooldown rate of correlation step, this area skill in neodymium iron boron magnetic body sintering process well known to those skilled in the art Art personnel can regulate accordingly according to the actual production process of sintering furnace, batch and product size, of the present invention The speed of cooling is 0.1～0.5 DEG C/min, more preferably 0.2～0.4 DEG C/min, most preferably 0.25～0.35 DEG C/min.
After the present invention terminates, the most also include tempering step；The detailed process of described tempering step is not had by the present invention Having restriction especially, the detailed process being tempered with magnet well known to those skilled in the art, those skilled in the art can root Selecting according to factors such as practical condition, product requirement and quality controls and adjust, the present invention is for refining crystalline substance further Grain, improves the magnetic property of product, and described tempering preferably includes one-level tempering and second annealing；The temperature of described one-level tempering is preferred It is 850～950 DEG C, more preferably 870～930 DEG C, most preferably 890～910 DEG C；The time of described one-level tempering is preferably 4 ～5h, more preferably 4.2～4.8h, most preferably 4.4～4.6h.The temperature of described second annealing is preferably 480～520 DEG C, More preferably 490～510 DEG C, most preferably 495～505 DEG C；The time of described second annealing is preferably 3～4h, more preferably 3.2～3.8h, most preferably 3.4～3.6h.The present invention is further crystal grain thinning, the magnetic property of raising product, described two grades Middle tempering is also included before tempering；Described in the middle of tempering temperature be preferably (temperature of second annealing+15 DEG C), i.e. 495～ 535 DEG C, more preferably 500～530 DEG C, most preferably 510～520 DEG C；Described in the middle of tempering time be preferably 1.5～ 2.5h, more preferably 1.7～2.3h, most preferably 1.9～2.1h.
Other conditions in above-mentioned drawing process are not particularly limited by the present invention, with magnetic well known to those skilled in the art The condition of body drawing process, those skilled in the art can be according to practical condition, product requirement and quality control Selecting etc. factor and adjust, the present invention is further crystal grain thinning, improves the magnetic property of product, and described drawing process is preferred Carrying out under vacuum, the heating rate of described drawing process is preferably 5～7 DEG C/min, more preferably 5.5～6.5 DEG C/ Min, most preferably 5.7～6.3 DEG C/min；The type of cooling in described drawing process is preferably applying argon gas cooling.
The present invention has prepared the neodymium iron boron magnetic body without heavy rare earth through above-mentioned steps, present invention employs specific Formula without heavy rare earth, by the column crystal size that controls the strictest during getting rid of band, then raising point during airflow milling powder Level wheel speed, controls alloy powder granularity, simultaneously strict in whole preparation technology controls contacting of powder and oxygen, minimizing powder The usage amount of lubricant, thus control the C of magnet, O content, burns finally by using low-temperature sintering or segmentation in sintering process Combine specific tempering process, strictly control crystallite dimension, prepare crystallite dimension little, C, low high performance sintered of O content Neodymium iron boron.On the premise of the cardinal principle of this method is not use heavy rare earth, on the one hand reduce carbon and the content of oxygen of magnet Thus reduce the consumption to rare earth element, and the principle on the other hand refined by neodymium iron boron crystal grain, reduce magnet crystallite dimension, by Effective demagnetizing factor N in neodymium iron boroneffIncrease with the increase of crystallite dimension, therefore, the reduction of the coercivity crystal grain of magnet And increase.Test result indicate that, the crystallite dimension of the neodymium iron boron magnetic body that the present invention provides is less, average grain size 4.5～5.5 μm, the remanent magnetism of neodymium iron boron magnetic body reaches more than 13kGs, and coercivity reaches more than 21kOe.
In order to further illustrate the present invention, a kind of neodymium ferrum without the heavy rare earth present invention provided below in conjunction with embodiment The preparation method of boron magnet is described in detail, but it is to be understood that these embodiments are to be front with technical solution of the present invention Put and implement, give detailed embodiment and concrete operating process, be simply the spy further illustrating the present invention Advantage of seeking peace rather than limiting to the claimed invention, protection scope of the present invention is also not necessarily limited to following embodiment.
Embodiment 1
Being 32.5% according to the percentage by weight of PrNd content, B content is 0.88%, and Al content is 0.66, and Cu content is 0.15%, Co content is 1.2%, and Ga content is 0.5%, and Zr content is 0.2%, and remaining is Fe formula dispensing, uses rapid hardening to get rid of Band technique, makes average thickness ＜ 0.3mm by dispensing, gets rid of strap between column crystal size 3.8～4.2 μm.
Use HD process rejection tablet is crushed, hydrogen quick-fried suction hydrogen pressure is 0.098Mpa, until inhale hydrogen reach saturated after carry out Dehydrogenation, degassing temperature is 500 DEG C.
Then hydrogen coarse powder after quick-fried is carried out further Mechanical Crushing, add after 0.035% kollag by three-dimensional Mixed powder machine mixes powder 120min.The coarse powder mixed carries out airflow milling powder, and air flow mill grading wheel is transferred to 4900rpm, adding of airflow milling Oxygen amount is 0ppm, grinds gas pressure 0.45Mpa, and the particle mean size of powder is 2.66 μm.Add to the fine powder prepared through airflow milling Mix powder machine with V-arrangement after the fluid lubricant adding 0.15% and mix powder 180min.
Above-mentioned powder is pressed into square pressed compact, pressing process with all-sealed mo(u)ldenpress after the deactivation period of 24h Middle control press oxygen content is less than 0.5%, and press orientation electric current is 1.5T, and green density is about 3.6g/cm3.After suppressing Blank encapsulation after carry out isostatic pressed process, hydrostatic pressure is 200Mpa.
Being placed in vacuum sintering furnace by pressed compact and carry out heat treatment, in vacuum sintering furnace, vacuum reaches to start during 0.3Pa Heat up, heating rate 5～7 DEG C/min, through 250 DEG C, 650 DEG C, after 850 DEG C of insulation platforms after 1030 DEG C of sintered heat insulating 12h Cooling, after burning, blank is tempered through 900 DEG C of * 4.5h one-levels, is incubated 3h and carries out second annealing process at 480 DEG C.In omnidistance mistake Strictly to control magnet oxygen content in journey, final magnet Control for Oxygen Content is between 600～800ppm.
The magnet preparing the embodiment of the present invention 1 neodymium iron boron magnetic body without heavy rare earth carries out metallographic observation, and result sees Fig. 1, Fig. 1 are the metallurgical microstructrue figure of the neodymium iron boron magnetic body of the embodiment of the present invention 1 preparation, and embodiment 1 is made as can be seen from Figure 1 The standby neodymium iron boron magnetic body crystallite dimension obtained is less, and average grain size is 5.21 μm.
The magnet preparing the embodiment of the present invention 1 neodymium iron boron magnetic body without heavy rare earth carries out magnetic property and C, and O content is examined Survey, see table 1, the neodymium iron boron magnetic body without heavy rare earth that table 1 is prepared for the embodiment of the present invention and the conventional magnetic containing heavy rare earth The magnetic property of body and C, O content synopsis.
Embodiment 2
Being 32.5% according to the percentage by weight of PrNd content, B content is 0.88%, and Al content is 0.66, and Cu content is 0.15%, Co content is 1.2%, and Ga content is 0.5%, and Zr content is 0.2%, and remaining is Fe formula dispensing, uses rapid hardening to get rid of Band technique, makes average thickness ＜ 0.3mm by dispensing, gets rid of strap between column crystal size 3.8～4.2 μm.
Use HD process rejection tablet is crushed, hydrogen quick-fried suction hydrogen pressure is 0.098Mpa, until inhale hydrogen reach saturated after carry out Dehydrogenation, degassing temperature is 500 DEG C.
Then hydrogen coarse powder after quick-fried is carried out further Mechanical Crushing, add after 0.035% kollag by three-dimensional Mixed powder machine mixes powder 120min.The coarse powder mixed carries out airflow milling powder, and air flow mill grading wheel is transferred to 4900rpm, adding of airflow milling Oxygen amount is 0ppm, grinds gas pressure 0.45Mpa, and the particle mean size of powder is 2.66 μm.Add to the fine powder prepared through airflow milling Mix powder machine with V-arrangement after the fluid lubricant adding 0.15% and mix powder 180min.
Above-mentioned powder is pressed into square pressed compact, pressing process with all-sealed mo(u)ldenpress after the deactivation period of 24h Middle control press oxygen content is less than 0.5%, and press orientation electric current is 1.5T, and green density is about 3.6g/cm3.After suppressing Blank encapsulation after carry out isostatic pressed process, hydrostatic pressure is 200Mpa.
Being placed in sintering furnace by neodymium iron boron pressed compact, begin to warm up intensification to below 0.3Pa after evacuation, intensification 40min arrives It is incubated 150min after 250 DEG C, is then passed through 70min and is warmed up to 650 DEG C, be incubated 80min at 650 DEG C, be then passed through 40min and heat up To 850 DEG C, 850 DEG C be incubated 250min, then entered 60min be warmed up to 1010 DEG C insulation 30min, be then passed through 10min heat up To 1030 DEG C, at 1030 DEG C, it is incubated 5h.Then cool to 700 DEG C through 90min, then be warmed up to 1030 DEG C through 90min, It is incubated 7h at 1030 DEG C and naturally cools to room temperature, the neodymium iron boron magnetic body blank after being sintered.
Blank after oversintering is warmed up to 900 DEG C of insulation 5h and carries out one-level tempering, and then cooling is warmed up to 480 DEG C of guarantors Temperature 3h carries out second annealing, obtains neodymium iron boron magnetic body.
Strictly to control magnet oxygen content during whole process, final magnet Control for Oxygen Content is between 600～800ppm.
The magnet preparing the embodiment of the present invention 2 neodymium iron boron magnetic body without heavy rare earth carries out metallographic observation, and result sees Fig. 2, Fig. 2 are the metallurgical microstructrue figure of the neodymium iron boron magnetic body of the embodiment of the present invention 2 preparation, and embodiment 2 is made as can be seen from Figure 2 The standby neodymium iron boron magnetic body crystallite dimension obtained is less, and average grain size is 5.26 μm.
The magnet preparing the embodiment of the present invention 2 neodymium iron boron magnetic body without heavy rare earth carries out magnetic property and C, and O content is examined Survey, see table 1, the neodymium iron boron magnetic body without heavy rare earth that table 1 is prepared for the embodiment of the present invention and the conventional magnetic containing heavy rare earth The magnetic property of body and C, O content synopsis.
Comparative example 1
Being 33.3% according to the percentage by weight of PrNd content, B content is 1.04%, and Al content is 1%, and Cu content is 0.1%, Co content is 1%, and Nb content is 0.2%, and Zr content is 0.02%, and remaining is Fe formula dispensing, uses rapid hardening to get rid of band Technique is made and is got rid of band.
Using HD process rejection tablet to be crushed, hydrogen quick-fried suction hydrogen pressure is 0.098Mpa, only to inhale hydrogen reach saturated after carry out Dehydrogenation, degassing temperature is 580 DEG C.
Then hydrogen coarse powder after quick-fried is carried out further Mechanical Crushing, mixed by three-dimensional after adding 500ppm kollag Powder machine mixes powder 120min.The coarse powder mixed carries out airflow milling powder, and air flow mill grading wheel is transferred to 4000rpm, the oxygenation of airflow milling Amount is about 300ppm, grinds gas pressure 0.45Mpa, and the particle mean size of powder is 3.2 μm.To the fine powder prepared through airflow milling Mix powder machine with V-arrangement after adding the fluid lubricant of 0.15% and mix powder 90min.
Above-mentioned powder is pressed into square pressed compact, pressing process with all-sealed mo(u)ldenpress after the deactivation period of 24h Middle control press oxygen content is less than 0.5%, and press orientation electric current is 1.5T, and green density is about 3.6g/cm3.After suppressing Blank encapsulation after carry out isostatic pressed process, hydrostatic pressure is 200Mpa.
Then pressed compact is placed in vacuum sintering furnace and carries out heat treatment, when vacuum reaches 0.3Pa in vacuum sintering furnace Start to warm up, heating rate 5～7 DEG C/min, through 250 DEG C, 650 DEG C, at 1035 DEG C of sintered heat insulating 8h after 850 DEG C of insulation platforms Rear cooling, after burning, blank is tempered through 900 DEG C of * 4.5h one-levels, is incubated 3h and carries out second annealing process at 570 DEG C.Magnet Magnetic property and C, O content is shown in Table 1.
Comparative example 2
Being 29.6% according to the percentage by weight of PrNd content, Dy content is 2%, and B content is 0.93%, and Al content is 0.4%, Cu content is 0.45%, and Co content is 1.2%, and Ga content is 0.2%, and Zr content is 0.4%, and remaining is joined for Fe formula Material, uses rapid hardening belt-rejecting technology to make and gets rid of band.
Using HD process rejection tablet to be crushed, hydrogen quick-fried suction hydrogen pressure is 0.098Mpa, only to inhale hydrogen reach saturated after carry out Dehydrogenation, degassing temperature is 580 DEG C.Then hydrogen coarse powder after quick-fried is carried out further Mechanical Crushing, add 350ppm solid profit Powder 120min is mixed with three-dimensional mixed powder machine after lubrication prescription.The coarse powder mixed carries out airflow milling powder, and air flow mill grading wheel is transferred to 4400rpm, the oxygen-adding amount of airflow milling is about 0ppm, grinds gas pressure 0.45Mpa, and the particle mean size of powder is 2.9 μm.To The fine powder prepared through airflow milling mixes powder machine with V-arrangement after adding the fluid lubricant of 0.15% and mixes powder 300min.
Above-mentioned powder is pressed into square pressed compact, pressing process with all-sealed mo(u)ldenpress after the deactivation period of 24h Middle control press oxygen content is less than 0.5%, and press orientation electric current is 1.5T, and green density is about 3.6g/cm3。
Carrying out isostatic pressed process after the blank encapsulation after compacting, hydrostatic pressure is 200Mpa.Then pressed compact is placed in Carrying out heat treatment in vacuum sintering furnace, in vacuum sintering furnace, vacuum reaches to start to warm up during 0.3Pa, heating rate 5～7 DEG C/min, and through 250 DEG C, 650 DEG C, cooling down after 1042 DEG C of sintered heat insulating 8h after 850 DEG C of insulation platforms, after burning, blank passes through 900 DEG C of * 4.5h one-level tempering, are incubated 3h at 530 DEG C and carry out second annealing process.The magnetic property of magnet and C, O content is shown in Table 1。
The magnetic of the neodymium iron boron magnetic body without heavy rare earth prepared by table 1 embodiment of the present invention and the routine magnet containing heavy rare earth Performance and C, O content synopsis
Upper table be embodiment and comparative example performance data, comparative example and comparative example 1 it can be seen that, although comparative example 1 Content of rare earth higher than embodiment, but owing in embodiment, we strictly control magnet oxygen content, reduce the oxygen consumption to rare earth, And in embodiment after airflow milling powder average powder particle size than comparative example little 0.6 μm, under in sintering, we use lower temperature burn Knot and multi-steps sintering, refined crystallite dimension so that coercivity is greatly improved.
Comparative example and comparative example 2 it can be seen that, although embodiment Rare-Earth Content is higher, but remanent magnetism does not the most drop Low, embodiment uses entirely without heavy rare earth formula, and uses the formula of 2%Dy in comparative example 2, the coercivity phase of embodiment magnet More taller than comparative example 2, and both C, O content is more or less the same, and both differ primarily in that the average of powder after airflow milling powder Granularity, and the difference of sintering process, owing to using lower powder size and sintering at a lower temperature, magnet in embodiment Crystallite dimension less, owing to effective demagnetizing factor Neff of neodymium iron boron increases with the increase of crystallite dimension, therefore, magnet The reduction of coercivity crystal grain and increase, we successfully use to prepare without heavy rare earth formula and (use than comparative example 2 to utilize this principle The Dy formula of 2%) performance higher 42SH magnet.
Above the preparation method of a kind of neodymium iron boron magnetic body without heavy rare earth that the present invention provides is carried out detailed Jie Continuing, principle and the embodiment of the present invention are set forth by specific case used herein, and the explanation of above example is only It is the method and core concept thereof being adapted to assist in and understanding the present invention, including best mode, and also makes any skill of this area Art personnel can put into practice the present invention, including manufacturing and using any device or system, and the method implementing any combination.Should Point out, for those skilled in the art, under the premise without departing from the principles of the invention, it is also possible to this Bright carrying out some improvement and modification, these improve and modify in the protection domain also falling into the claims in the present invention.The present invention is special Profit protection scope be defined by the claims, and those skilled in the art can be included it is conceivable that other embodiments.As Really these other embodiments have the structural element being not different from claim character express, if or they include with power The character express that profit requires is without the equivalent structural elements of essence difference, then these other embodiments also should be included in claim In the range of.

Claims (10)

1. the preparation method of the neodymium iron boron magnetic body without heavy rare earth, it is characterised in that comprise the following steps:
1) carry out neodymium iron boron magnetic body raw material after rapid hardening gets rid of band, obtaining neodymium iron boron and getting rid of strap；
2) neodymium iron boron that above-mentioned steps obtains is got rid of strap through the quick-fried process of hydrogen, obtain the quick-fried rear coarse powder of hydrogen；
3) the quick-fried rear coarse powder of hydrogen above-mentioned steps obtained, through Mechanical Crushing, adds after additive mixes, obtains mixed thick Powder；
4) mixed coarse powder above-mentioned steps obtained is after anaerobic air-flow mill grinds, and obtains neodymium iron boron fine powder；
5), after neodymium iron boron fine powder addition lubricant above-mentioned steps obtained mixes again, mixed fine powder is obtained；
6) mixed fine powder above-mentioned steps obtained is after transpassivation, then after orientation compacting and isostatic pressed process, obtains neodymium ferrum Boron pressed compact；
7) neodymium iron boron pressed compact above-mentioned steps obtained is after low temperature sinters for a long time, then after being tempered, obtains neodymium iron boron Magnet；
The sintering temperature that described low temperature sinters for a long time is 1010～1030 DEG C；The time that described low temperature sinters for a long time be 10～ 15h。
Preparation method the most according to claim 1, it is characterised in that described neodymium iron boron magnetic body raw material, by mass percentage Composition includes: Pr-Nd:31.5%～33.5%；B:0.85%～0.9%；Al:0.6%～0.7%；Cu:0.2%～ 0.6%；Co:1.0%～1.5%；Ga:0.4%～0.6%；Zr:0.15%～0.3%；Surplus is Fe.
Preparation method the most according to claim 1, it is characterised in that described neodymium iron boron gets rid of the average thickness of strap and is less than In 0.3mm；Described neodymium iron boron gets rid of column crystal a size of 3.8～4.2 μm of strap.
Preparation method the most according to claim 1, it is characterised in that in the quick-fried process of described hydrogen, the pressure of described suction hydrogen is 0.08～0.15Mpa；
The temperature of described dehydrogenation is 490～510 DEG C.
Preparation method the most according to claim 1, it is characterised in that described additive includes zinc stearate, calcium stearate With one or more in Polyethylene Glycol octane；The addition of described additive is 0.03%～0.05%；
The incorporation time of described mixing is 90～150min；
Described lubricant includes methyl ester class and/or alcohols；The addition of described lubricant accounts for the ratio of neodymium iron boron fine powder quality 0.1%～0.3%；
The described incorporation time again mixed is 150～210min.
Preparation method the most according to claim 1, it is characterised in that described anaerobic airflow milling is the bar at protective gas Under part, carry out airflow milling；
The grinding gas pressure of described airflow milling is 0.4～0.5MPa；
The grading wheel rotating speed of described airflow milling is 4800～4950rpm；
The particle mean size of described neodymium iron boron fine powder is 2.5～2.7 μm.
Preparation method the most according to claim 1, it is characterised in that the time of described passivation is 20～30h；
The oxygen content of described orientation compacting is less than or equal to 0.5%；The magnetic field intensity of described orientation compacting is 1.2～1.8T；
The pressure that described isostatic pressed processes is 150～250Mpa；
Described green density is 3.6～3.8g/cm3。
Preparation method the most according to claim 1, it is characterised in that what described low temperature sintered for a long time concretely comprises the following steps:
A) under conditions of vacuum or protective gas, neodymium iron boron pressed compact is sequentially passed through defat and fires, deaerate for the first time and fire After firing with second time degassing, obtain just section sintering intermediate；
B) first section sintering intermediate above-mentioned steps obtained, carries out after first stage intensification constant temperature fires, obtaining one-stage sintering Intermediate；
C) one-stage sintering intermediate above-mentioned steps obtained, carries out after second stage intensification constant temperature fires, obtaining bis sintering Intermediate；
D) bis sintering intermediate above-mentioned steps obtained, after carrying out phase III cooling, obtains three-stage sintering intermediate；
E) three-stage sintering intermediate above-mentioned steps obtained, carries out fourth stage intensification constant temperature and fires.
Preparation method the most according to claim 1, it is characterised in that described tempering includes one-level tempering and second annealing；
The temperature of described one-level tempering is 850～950 DEG C；The time of described one-level tempering is 4～5h；
The temperature of described second annealing is 480～520 DEG C；The time of described second annealing is 3～4h.
Preparation method the most according to claim 1, it is characterised in that also include middle tempering before described second annealing；
In the middle of described, the temperature of tempering is (temperature of second annealing+15 DEG C)；
In the middle of described, the time of tempering is 1.5～2.5h.
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CN108417375A (en) * 2018-02-05 2018-08-17 宁波松科磁材有限公司 A kind of preparation method without heavy rare earth sintered Nd-Fe-B permanent magnet
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
CN108806912A (en) * 2018-05-02 2018-11-13 宁波科田磁业有限公司 A kind of no heavy rare earth Sintered NdFeB magnet and preparation method thereof
CN109102976A (en) * 2018-08-10 2018-12-28 浙江东阳东磁稀土有限公司 A method of improving rare-earth Nd-Fe-B magnetic property
CN109243746A (en) * 2018-09-08 2019-01-18 江西理工大学 Ultra-fine Grained sintered permanent magnet made of a kind of delay sintering of low temperature and preparation method thereof
CN110739113A (en) * 2019-10-09 2020-01-31 宁波科田磁业有限公司 high-performance sintered Nd-Fe-B material and preparation method thereof
CN112466643A (en) * 2020-10-28 2021-03-09 杭州永磁集团有限公司 Preparation method of sintered neodymium-iron-boron material
CN112670047A (en) * 2020-12-11 2021-04-16 东莞市嘉达磁电制品有限公司 High-temperature-resistant neodymium-iron-boron magnet and preparation method thereof
WO2021244316A1 (en) * 2020-06-03 2021-12-09 厦门钨业股份有限公司 R-t-b-based permanent magnetic material, raw material composition, preparation method therefor and use thereof

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WO2021244316A1 (en) * 2020-06-03 2021-12-09 厦门钨业股份有限公司 R-t-b-based permanent magnetic material, raw material composition, preparation method therefor and use thereof
CN112466643A (en) * 2020-10-28 2021-03-09 杭州永磁集团有限公司 Preparation method of sintered neodymium-iron-boron material
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CN112670047A (en) * 2020-12-11 2021-04-16 东莞市嘉达磁电制品有限公司 High-temperature-resistant neodymium-iron-boron magnet and preparation method thereof

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