CN105551790A - Sintering method for neodymium-iron-boron magnet - Google Patents
Sintering method for neodymium-iron-boron magnet Download PDFInfo
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- CN105551790A CN105551790A CN201610090762.4A CN201610090762A CN105551790A CN 105551790 A CN105551790 A CN 105551790A CN 201610090762 A CN201610090762 A CN 201610090762A CN 105551790 A CN105551790 A CN 105551790A
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- magnetic body
- iron boron
- neodymium iron
- boron magnetic
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0266—Moulding; Pressing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
- B22F3/101—Changing atmosphere
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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
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention provides a sintering method for a neodymium-iron-boron magnet. The method comprises the following steps: firstly, carrying out continuous warming or stepped warming on a green neodymium-iron-boron magnet body to reach a sintering temperature under a vacuum or protective gas condition, and obtaining a neodymium-iron-boron magnet intermediate; and carrying out constant-temperature firing on the neodymium-iron-boron magnet intermediate obtained in the previous step under a hydrogen condition, and obtaining a neodymium-iron-boron magnet blank. In a plurality of steps for preparing the neodymium-iron-boron magnet, hydrogen is filled into a system at a specific high-temperature sintering stage in the sintering process from the sintering method, so that a neodymium-rich phase in the blank material is uniform in distribution; a rare-earth phase is prevented from being consumed; a rare-earth phase oxide is avoided; rare earth does not need to add when a formula is designed; the cost is saved; the coercivity of a product is also improved; and the sintering method has very important significance for development of a neodymium-iron-boron magnet product.
Description
Technical field
The invention belongs to magnet preparing technical field, particularly relate to a kind of sintering method of neodymium iron boron magnetic body.
Background technology
Be no matter in industrial production or in daily life, hard magnetic body and permanent magnet, can keep the magnet of its magnetic for a long time, not easily loss of excitation, is not easily magnetized, and is also one of the most frequently used muscle material.Hard magnetic body can be divided into natural magnet and artificial magnet, and artificial magnet refers to that the alloy by synthesizing different materials can reach the effect identical with natural magnet (magnet), but also can improve magnetic force.Just occurred artificial magnet as far back as 18th century, but the process manufacturing more strong magnetic material is very slow, until produce alnico magnet (AlNiCo) thirties in 20th century, just makes the large-scale application of magnet become possibility.Subsequently, produce ferrite (Ferrite) the 1950's, the sixties, the appearance of rare earth permanent magnet, then for the application of magnet opens a New Times, first generation samarium cobalt permanent magnet SmCo
5, second generation precipitation hardenable samarium cobalt permanent magnet Sm
2co
17, up to now, develop into third generation Nd-Fe-Bo permanent magnet material (NdFeB).Although ferrimagnet remains the maximum permanent magnetic material of consumption at present, the output value of neodymium iron boron magnetic body substantially exceeds ferrite permanent-magnet materials, has developed into a large industry.
Neodymium iron boron magnetic body is also referred to as neodymium magnet (Neodymiummagnet), and its chemical formula is Nd
2fe
14b is a kind of artificial permanent magnet, is also the permanent magnet so far with the strongest magnetic force, and its maximum magnetic energy product (BHmax) exceeds more than 10 times, ferrite, and under the state of naked magnetic, its magnetic force can reach 3500 Gauss.The advantage of neodymium iron boron magnetic body is that cost performance is high, the mechanical property that volume is little, lightweight, good and the feature such as magnetic is strong, the advantage of high-energy-density like this makes Nd-Fe-Bo permanent magnet material obtain a wide range of applications in modern industry and electronic technology, is described as magnetic king in magnetics circle.Thus, neodymium iron boron magnetic body preparation and expansion be the focus given more sustained attention in the industry always.
At present, industry often adopts sintering process to make Nd-Fe-Bo permanent magnet material, in " key process parameter and alloying element are on the impact of Sintered NdFeB magnetic property and mechanical property ", disclose the technological process adopting sintering process to manufacture Nd-Fe-Bo permanent magnet material as Wang Wei waits, generally comprise that batching, melting, steel ingot fragmentation, powder process, vacuum preservation superfine powder, powder orientation are compressing, vacuum-sintering, inspection divide and the step such as plating.This wherein, sintering is a vital link, and the magnetic property of Nd-Fe-B permanent magnet is very responsive to sintering process, the alloy of identical component, and due to the difference of sintering process, its magnetic property can several times, Ji Shibei, even the change of hundreds of times ground.The object of sintering be below matrix phase fusing point a certain temperature through time process, pressed compact is shunk and densification, and optimizes crystal boundary by follow-up timeliness, realization is separated the drag increasing farmland displacement, makes magnet have the microscopic structure of high permanent magnetism performance.Usually the sintering method adopted at present is liquid-phase sintering and solid-phase sintering.
But in the last few years, along with the extensive use of neodymium iron boron magnetic body, facilitate the production requiring more high stability and the more neodymium iron boron magnetic body of low cost, but sintered Nd-Fe-B permanent magnet is easily oxidized at the process middle rare earth of sintering, cause during component design and must add a little rare earth, or the magnetic property problems such as especially coercive force is undesirable after sintering, become the obstacle that it further develops gradually.
Thus, how can by the improvement in magnet preparation process, reduce the consumption of unnecessary rare earth in neodymium iron boron magnetic body production process, improve magnet performance, be the focus of neodymium iron boron magnetic body production firm extensive concern always.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is the sintering method providing a kind of neodymium iron boron magnetic body, sintering method provided by the invention, when component design without the need to increasing rare extra rare earth, effectively can also improve the magnetic property of neodymium iron boron magnetic body.
The invention provides a kind of sintering method of neodymium iron boron magnetic body, comprise the following steps:
A) under the condition of vacuum or protective gas, by neodymium iron boron magnetic body green compact after continuous warming or ladder-elevating temperature, arrive sintering temperature, obtain neodymium iron boron magnetic body intermediate;
B) under the condition of hydrogen, neodymium iron boron magnetic body intermediate above-mentioned steps obtained carries out after constant temperature fires, obtaining neodymium iron boron magnetic body blank.
Preferably, described sintering temperature is 1000 ~ 1100 DEG C.
Preferably, the heating rate of described continuous warming is 0.5 ~ 3 DEG C/min; The time of described continuous warming is 15 ~ 120min.
Preferably, the concrete steps of described ladder-elevating temperature are:
A1) under the condition of vacuum or protective gas, neodymium iron boron magnetic body green compact are carried out after first time, constant temperature fired, obtain the first intermediate;
A2) the first intermediate then above-mentioned steps obtained carries out after second time constant temperature fires, obtaining the second intermediate;
A3) the second intermediate above-mentioned steps obtained again carries out after third time, constant temperature fired, obtaining neodymium iron boron magnetic body intermediate.
Preferably, the temperature fired of constant temperature is 200 ~ 250 DEG C described first time; Constant temperature time of firing described first time is 90 ~ 150min;
The temperature that described second time constant temperature is fired is 450 ~ 550 DEG C; The time that described second time constant temperature is fired is 60 ~ 120min;
Described third time, the temperature fired of constant temperature was 750 ~ 850 DEG C; The time that described second time constant temperature is fired is 90 ~ 120min.
Preferably, to be describedly specially under the condition of hydrogen:
Be filled with hydrogen directly in equipment, or first the protective gas in agglomerating plant be evacuated to vacuum, then be filled with hydrogen in agglomerating plant.
Preferably, the pressure of described vacuum is for being less than or equal to 10Pa; The pressure of described hydrogen is 0.030 ~ 0.098MPa.
Preferably, described step B) also comprise,
Neodymium iron boron magnetic body intermediate after being fired by constant temperature, cools under the condition of hydrogen, obtains neodymium iron boron magnetic body blank.
Preferably, the speed of described cooling is 6.0 ~ 8.5 DEG C/min.
The invention provides a kind of neodymium iron boron magnetic body, described neodymium iron boron magnetic body is by neodymium iron boron magnetic body green compact under the condition of hydrogen, obtains after liquid-phase sintering or solid-phase sintering.
The invention provides a kind of sintering method of neodymium iron boron magnetic body, comprise the following steps, first under the condition of vacuum or protective gas, by neodymium iron boron magnetic body green compact after continuous warming or ladder-elevating temperature, arrive sintering temperature, obtain neodymium iron boron magnetic body intermediate; Then, under the condition of hydrogen, neodymium iron boron magnetic body intermediate above-mentioned steps obtained carries out after constant temperature fires, obtaining neodymium iron boron magnetic body blank.Compared with prior art, in numerous steps that the present invention is prepared at neodymium iron boron magnetic body, start with from sintering method, by the specific high temperature sintering stage in sintering process, hydrogen is filled with in system, make the rich neodymium Entropy density deviation of blank material even, stop rare-earth phase to be consumed, avoid and produce rare-earth phase oxide, not only without the need to adding a little rare earth when component design, save cost, but also improve the magnetic property of product, the development tool of sintered NdFeB product has been had very important significance.Experimental result shows; adopt the sintering method of neodymium iron boron magnetic body provided by the invention, when composition of raw materials calculates, compare in original actual production the rare earth needing extra interpolation 0.5% ~ 2%; the present invention is oxidized the method for phase by hydrogenation protecting and logical hydrogen reduction, saves the rare earth of 0.5% ~ 3%.And neodymium iron boron magnetic body prepared by the present invention compares existing technique, in normal temperature (20 DEG C) magnet performance, neodymium iron boron magnetic body remanent magnetism (Br) improves about 1.63%, HCJ (Hcj) improves about 9.17%, and squareness (HK/Hcj) improves about 1.04%; In high temperature (150 DEG C) magnet performance, neodymium iron boron magnetic body remanent magnetism (Br) improves about 10.5%, HCJ (Hcj) improves about 21%, squareness (HK/Hcj) improves about 1.04%, and the high-temperature temperature coefficient (α) of neodymium iron boron magnetic body Hcj that in addition prepared by the present invention can reach-0.420 ~-0.527%/DEG C.
Accompanying drawing explanation
Fig. 1 is neodymium iron boron magnetic body green sintering technological temperature curve synoptic diagram in the present invention;
Fig. 2 is the metallurgical microstructrue figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 1;
Fig. 3 is the metallurgical microstructrue figure of neodymium iron boron magnetic body prepared by common process;
Fig. 4 is the normal temperature magnetic performance data figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 1;
Fig. 5 is the metallurgical microstructrue figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 2;
Fig. 6 is the normal temperature magnetic performance data figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 2;
Fig. 7 is the metallurgical microstructrue figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 3;
Fig. 8 is the normal temperature magnetic performance data figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 3.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just in order to further illustrate the features and advantages of the present invention, instead of the restriction to invention claim.
The all raw materials of the present invention, be not particularly limited its source, commercially buy or prepare according to conventional method well known to those skilled in the art.
The all raw materials of the present invention, are not particularly limited its purity, and the present invention preferably adopts analysis pure.
The invention provides a kind of sintering method of neodymium iron boron magnetic body, comprise the following steps:
A) under the condition of vacuum or protective gas, by neodymium iron boron magnetic body green compact after continuous warming or ladder-elevating temperature, arrive sintering temperature, obtain neodymium iron boron magnetic body intermediate;
B) under the condition of hydrogen, neodymium iron boron magnetic body intermediate above-mentioned steps obtained carries out after constant temperature fires, obtaining neodymium iron boron magnetic body blank.
The present invention, first under the condition of vacuum or protective gas, by neodymium iron boron magnetic body green compact after continuous warming or ladder-elevating temperature, arrives sintering temperature, obtains neodymium iron boron magnetic body intermediate.
The present invention is not particularly limited described sintering, and with the sintering method of neodymium iron boron magnetic body well known to those skilled in the art, the present invention is preferably liquid-phase sintering or solid-phase sintering, is more preferably liquid-phase sintering.The present invention is not particularly limited described protective gas, with the protective gas for Sintered NdFeB magnet well known to those skilled in the art, protective gas of the present invention is preferably inert gas and/or nitrogen, is more preferably argon gas and/or nitrogen, most preferably is argon gas or nitrogen; The pressure of the present invention to described vacuum is not particularly limited, with the vacuum pressure of Sintered NdFeB magnet well known to those skilled in the art, vacuum pressure of the present invention is preferably less than or equal to 10Pa, be more preferably and be less than or equal to 1Pa, be more preferably and be less than or equal to 0.3Pa, most preferably be 0.01 ~ 0.3Pa.
The present invention is not particularly limited described sintering temperature, with the temperature of Sintered NdFeB magnet well known to those skilled in the art, the present invention is preferably 1000 ~ 1100 DEG C, is more preferably 1010 ~ 1090 DEG C, be more preferably 1030 ~ 1070 DEG C, most preferably be 1040 ~ 1060 DEG C.The equipment of the present invention to described sintering is not particularly limited, and with the equipment of Sintered NdFeB magnet well known to those skilled in the art, the present invention is preferably vacuum sintering furnace.The early stage preparation process of the present invention to described neodymium iron boron magnetic body green compact is not particularly limited, with conventional production practices well known to those skilled in the art, also can regulate according to practical condition or quality requirement, the present invention preferably includes that batching, melting, hydrogen are quick-fried, the main process such as powder process and orientation compacting, obtains neodymium iron boron magnetic body green compact.
The present invention is the magnetic property firing effect and neodymium iron boron magnetic body improving neodymium iron boron magnetic body green compact, preferred above-mentioned steps is specially continuous warming, the speed of the present invention to described intensification is not particularly limited, with the heating rate in neodymium iron boron magnetic body sintering process well known to those skilled in the art, those skilled in the art can carry out selective control according to the concrete size of batch, product and properties of product, the speed of continuous warming of the present invention is preferably 0.5 ~ 3 DEG C/min, be more preferably 1 ~ 2.5 DEG C/min, most preferably be 1.5 ~ 2 DEG C/min; The time of described continuous warming is preferably 15 ~ 120min, is more preferably 30 ~ 100min, most preferably is 50 ~ 70min.
The present invention is the magnetic property firing effect and neodymium iron boron magnetic body improving neodymium iron boron magnetic body green compact, preferred above-mentioned steps is also preferably ladder-elevating temperature, specifically be more preferably first under the condition of vacuum or protective gas, neodymium iron boron magnetic body green compact carried out after first time, constant temperature fired, obtain the first intermediate; Then the first intermediate above-mentioned steps obtained carries out after second time constant temperature fires, obtaining the second intermediate; The second intermediate above-mentioned steps obtained again carries out after third time, constant temperature fired, obtaining neodymium iron boron magnetic body intermediate.
The present invention to described neodymium iron boron magnetic body green compact carry out first time the actual temp fired of constant temperature and the time be not particularly limited, with neodymium iron boron magnetic body green sintering process well known to those skilled in the art, those skilled in the art can carry out selective control according to the concrete size of batch and product, the present invention is that effect and properties of product are fired in raising, described first time, the temperature fired of constant temperature was preferably 200 ~ 250 DEG C, be more preferably 210 ~ 240 DEG C, most preferably be 220 ~ 230 DEG C; Constant temperature time of firing described first time is preferably 90 ~ 150min, is more preferably 100 ~ 140min, most preferably is 110 ~ 130min.The present invention is not particularly limited other conditions that described first time constant temperature is fired, with the condition of Sintered NdFeB magnet well known to those skilled in the art.Described neodymium iron boron magnetic body green compact to have been carried out first time constant temperature and have fired by the present invention under said temperature and time conditions, and in thermostatic process, discharged the steam that neodymium iron boron magnetic body green compact produce in sintering procedure.
The present invention carries out the second time actual temp fired of constant temperature to described neodymium iron boron magnetic body green compact and the time is not particularly limited, with neodymium iron boron magnetic body green sintering process well known to those skilled in the art, those skilled in the art can carry out selective control according to the concrete size of batch and product, the present invention is that effect and properties of product are fired in raising, the temperature that described second time constant temperature is fired is preferably 450 ~ 550 DEG C, be more preferably 460 ~ 540 DEG C, most preferably be 480 ~ 510 DEG C; The time that described second time constant temperature is fired is preferably 60 ~ 120min, is more preferably 70 ~ 110min, most preferably is 80 ~ 100min.The present invention is not particularly limited other conditions that described second time constant temperature is fired, with the condition of Sintered NdFeB magnet well known to those skilled in the art.Described neodymium iron boron magnetic body green compact have been carried out second time constant temperature and have fired by the present invention under said temperature and time conditions, have effectively discharged organic substance contained in neodymium iron boron magnetic body green compact.
The present invention to described neodymium iron boron magnetic body green compact carry out third time the actual temp fired of constant temperature and the time be not particularly limited, with neodymium iron boron magnetic body green sintering process well known to those skilled in the art, those skilled in the art can carry out selective control according to the concrete size of batch and product, the present invention is that effect and properties of product are fired in raising, described third time, the temperature fired of constant temperature was preferably 750 ~ 850 DEG C, be more preferably 760 ~ 840 DEG C, most preferably be 780 ~ 810 DEG C; The time that described second time constant temperature is fired is preferably 90 ~ 120min, is more preferably 80 ~ 110min, most preferably is 60 ~ 90min.The present invention is not particularly limited other conditions that described third time constant temperature is fired, with the condition of Sintered NdFeB magnet well known to those skilled in the art.Described neodymium iron boron magnetic body green compact to have been carried out third time constant temperature and have fired by the present invention under said temperature and time conditions, and in thermostatic process, discharged the hydrogen that neodymium iron boron magnetic body green compact produce in sintering procedure.The present invention does not have other to limit especially, with the process of Sintered NdFeB magnet well known to those skilled in the art to the described process fired.
The present invention, after above-mentioned continuous firing or three ladder-elevating temperature constant temperature are fired, obtains neodymium iron boron magnetic body intermediate, and then under the condition of hydrogen, neodymium iron boron magnetic body intermediate above-mentioned steps obtained carries out after constant temperature fires, obtaining neodymium iron boron magnetic body blank.
The present invention is not particularly limited the concrete operations under the condition of hydrogen, with Conventional procedures well known to those skilled in the art, the present invention preferably depends on that abovementioned steps is under vacuo or under the condition of protective gas, if abovementioned steps is under vacuo, be then preferably filled with hydrogen directly in equipment; If abovementioned steps is under the condition of protective gas, then preferably first the protective gas in agglomerating plant is evacuated to vacuum, then be filled with hydrogen in agglomerating plant.The present invention is not particularly limited the described pressure being evacuated to vacuum, with the vacuum pressure of Sintered NdFeB magnet well known to those skilled in the art, the pressure being evacuated to vacuum of the present invention is preferably less than or equal to 10Pa, be more preferably and be less than or equal to 1Pa, be more preferably and be less than or equal to 0.3Pa, most preferably be 0.01 ~ 0.3Pa.
The pressure of the present invention to described hydrogen is not particularly limited, those skilled in the art can carry out selective control according to the concrete size of batch, product and properties of product, the present invention is preferably 0.030 ~ 0.098MPa, be more preferably 0.040 ~ 0.090MPa, be more preferably 0.050 ~ 0.080MPa, most preferably be 0.060 ~ 0.070MPa.The temperature that constant temperature of the present invention is fired is preferably 1000 ~ 1100 DEG C, is more preferably 1010 ~ 1090 DEG C, is more preferably 1030 ~ 1070 DEG C, most preferably is 1040 ~ 1060 DEG C and is preferably 1020 ~ 1050 DEG C; Be more preferably 1030 ~ 1040 DEG C, most preferably be 1035 DEG C.The present invention was not particularly limited the time that described constant temperature is fired, those skilled in the art can carry out selective control according to the concrete size of batch, product and properties of product, the present invention is preferably 180 ~ 600min, be more preferably 250 ~ 550min, be more preferably 300 ~ 500min, most preferably be 350 ~ 450min.
The present invention fires rear technique to described constant temperature and is not particularly limited, and with conventional steps well known to those skilled in the art, the present invention is preferably cooling step; The concrete technology of the present invention to described cooling step is not particularly limited, those skilled in the art can carry out selective control according to the concrete size of actual production process, batch, product and properties of product, the present invention is the magnetic property firing effect and neodymium iron boron magnetic body improving neodymium iron boron magnetic body green compact, and the present invention preferably cools under the condition of hydrogen; The speed of the present invention to described cooling is preferably 6.0 ~ 8.5 DEG C/min, is more preferably 6.3 ~ 8.2 DEG C/min, is more preferably 6.5 ~ 8.0 DEG C/min, most preferably is 7.0 ~ 7.5 DEG C/min.The present invention is not particularly limited above-mentioned cooled temperature, and with the chilling temperature of correlation step in neodymium iron boron magnetic body sintering process well known to those skilled in the art, the present invention is preferably less than 100 DEG C, is more preferably less than 90 DEG C, most preferably is 20 ~ 80 DEG C; The present invention is not particularly limited the time to above-mentioned cooling, and those skilled in the art can regulate accordingly according to the batch of sintering furnace and product size.
The present invention is by the specific high temperature sintering stage in sintering process, hydrogen is filled with in system, play the effect of deoxygenation and reduced oxide, filling hydrogen after firing further carries out air-cooled, makes the rich neodymium Entropy density deviation of blank material even, stops rare-earth phase to be consumed, avoid and produce rare-earth phase oxide, not only without the need to adding a little rare earth when component design, saving cost, but also having improve the coercive force of product.
The present invention is after above-mentioned steps is by neodymium iron boron magnetic body green sintering, obtain neodymium iron boron magnetic body blank, although the present invention have employed the method that substep describes in describing above, but those skilled in the art can correct understanding, above-mentioned steps of the present invention is the process of a whole set of continuous firing, has continuous print sintering curre.Continuous print sintering curre of the present invention is neodymium iron boron magnetic body green sintering technological temperature curve synoptic diagram in the present invention see Fig. 1, Fig. 1.As shown in Figure 1, the temperature curve (b) that continuous warming curve when deflation curve (a) and sintering or staged heat up, wherein T
1for the temperature that first time constant temperature is fired, T
2for the temperature that second time constant temperature is fired, T
3for the temperature that third time constant temperature is fired, T
burnfor sintering temperature, the stage of filling hydrogen is carry out at a sintering temperature in process that constant temperature fires and in cooling procedure.
The present invention obtains neodymium iron boron magnetic body blank through above-mentioned steps, then after Post isothermal treatment and reprocessing processing, obtains finished product neodymium iron boron magnetic body.The selection that the present invention processes above-mentioned Post isothermal treatment and reprocessing, concrete steps and technique etc. are not particularly limited, with the post-processing steps in neodymium iron boron magnetic body well known to those skilled in the art, those skilled in the art can be in optimized selection according to practical condition and quality requirement.
The invention provides a kind of neodymium iron boron magnetic body, described neodymium iron boron magnetic body is by neodymium iron boron magnetic body green compact under the condition of hydrogen, obtains after liquid-phase sintering or solid-phase sintering.
The present invention is not particularly limited described neodymium iron boron magnetic body, and with neodymium iron boron magnetic body well known to those skilled in the art, the present invention is preferably Sintered NdFeB magnet; The concrete composition of the present invention to described neodymium iron boron magnetic body is not particularly limited, and forms with conventional neodymium iron boron magnetic body well known to those skilled in the art.The present invention's other processing steps to described sintering are not particularly limited, with the processing step in the sintering process of neodymium iron boron magnetic body well known to those skilled in the art.
Performance Detection is carried out to the neodymium iron boron magnetic body that above-mentioned steps of the present invention obtains; experimental result shows; adopt the sintering method of neodymium iron boron magnetic body provided by the invention; when composition of raw materials calculates; compare in original actual production the rare earth needing extra interpolation 0.5% ~ 2%; the present invention is oxidized the method for phase by hydrogenation protecting and logical hydrogen reduction, saves the rare earth of 0.5% ~ 3%.
The neodymium iron boron magnetic body prepared the present invention is respectively under the condition of 20 DEG C (normal temperature) and 150 DEG C (high temperature), carry out magnet performance detection, see table 1, the neodymium iron boron magnetic body that table 1 is prepared for the present invention and the magnetic property correction data of neodymium iron boron magnetic body under normal temperature and hot conditions prepared by common process.
Neodymium iron boron magnetic body prepared by table 1 the present invention and neodymium iron boron magnetic body prepared by the common process magnetic property correction data under normal temperature and hot conditions
As shown in Table 1, neodymium iron boron magnetic body prepared by the present invention compares existing technique, in normal temperature (20 DEG C) magnet performance, neodymium iron boron magnetic body remanent magnetism (Br) improves about 1.63%, HCJ (Hcj) improves about 9.17%, and squareness (HK/Hcj) improves about 1.04%; In high temperature (150 DEG C) magnet performance, neodymium iron boron magnetic body remanent magnetism (Br) improves about 10.5%, and HCJ (Hcj) improves about 21%, and squareness (HK/Hcj) improves about 1.04%.
Learn as calculated, the high-temperature temperature coefficient (α) of neodymium iron boron magnetic body Hcj prepared by the present invention brings up to-0.420 ~-0.527%/DEG C, and the Hcj high-temperature temperature coefficient of common process be only-0.55 ~-0.78%/DEG C, this shows that sintering method of the present invention significantly can improve the temperature stability of material.
Other Performance Detection are carried out to neodymium iron boron magnetic body prepared by the present invention, see table 2, the demagnetize situation of the neodymium iron boron magnetic body that table 2 is prepared for the present invention and neodymium iron boron magnetic body prepared by common process.
Demagnetize condition: 120 DEG C × 2h, equipment: high temperature drying case.
The demagnetize situation of neodymium iron boron magnetic body prepared by table 2 the present invention and neodymium iron boron magnetic body prepared by common process
| Demagnetize | |
| Strong magnetic sintering process | 0.5％～2.8％ |
| Normal process | 5％～10％ |
As shown in Table 2, neodymium iron boron magnetic body prepared by the present invention compares existing technique, and the demagnetize situation of magnet is better.
See table 3, the aging conditions of the neodymium iron boron magnetic body that table 3 is prepared for the present invention and neodymium iron boron magnetic body prepared by common process.
Below-G conditions: temperature 130 DEG C, humidity 100%, time 240h, pressure 2.7Bar;
Equipment: HAST ageing oven
The aging conditions of neodymium iron boron magnetic body prepared by table 3 the present invention and neodymium iron boron magnetic body prepared by common process
| Weightlessness/mg/cm 2 | |
| Fill hydrogen sintering process | 0.8～1.5 |
| Normal process | 2.0～8.0 |
In order to further illustrate the present invention, be described in detail below in conjunction with the sintering method of embodiment to neodymium iron boron magnetic body provided by the invention, protection scope of the present invention is not limited by the following examples.
Embodiment 1
Preparation 38SH sintered NdFeB
First, Pr and Nd:25.1wt% is taken, Dy:2wt%, Ho:4wt% according to mass percent composition, Al:0.44wt%, B:0.94wt%, Cu:0.15wt%, Co:1.5wt%, Zr:0.15wt%, the Fe of Ga:0.2wt% and surplus, through ingot casting, fragmentation, abrasive dust, magnetic field orientating, compressing, obtains neodymium iron boron green compact.
Then green compact are loaded vacuum sintering furnace, be evacuated to vacuum degree to 0.3Pa, neodymium iron boron magnetic body green compact are carried out after first time, constant temperature fired 90min, obtaining the first intermediate at 200 DEG C; Then the first intermediate above-mentioned steps obtained carries out after second time constant temperature fires 60min, obtaining the second intermediate at 500 DEG C; The second intermediate above-mentioned steps obtained again carries out after third time, constant temperature fired 90min, obtaining neodymium iron boron magnetic body intermediate at 750 DEG C.
After neodymium iron boron magnetic body intermediate above-mentioned steps obtained again carries out constant temperature liquid-phase sintering 30min at 1020 DEG C, hydrogen 0.052MPa is filled to above-mentioned neodymium iron boron magnetic body intermediate, above-mentioned fill hydrogen effect under, close hydrogen charging valve, liquid-phase sintering intermediate after logical hydrogen constant temperature liquid-phase sintering 30min;
Then sintering 60min is continued at this temperature, stop heating, enter cooling stage, in sintering furnace, fill hydrogen to 0.085-0.098MPa, machine air blast of blowing in is cooled to 60 DEG C and comes out of the stove, and obtaining specification is 51.2*51*29mm (direction of orientation is 29 sizes) neodymium iron boron magnetic body blank.
Finally, with surface grinding machine, oriented surface one side 60% is shown in light, is glued on iron staff with 502,9.59*6.69*0.88 (M) black-film is cut into inside diameter slicer, with the solution oil removing adding cleaning agent except glue, fall the radian of 0.2mm with automatic chamfering machine, remove burrs on edges, pass through ultrasonic oil removal, pickling, passivation, automatic zincincation, obtaining zinc coating thickness is 8 μm, is of a size of the neodymium iron boron magnetic body finished product of 9.95*6.69*0.88 (M).
Use XJ-63 type metallomicroscope to observe to the neodymium iron boron magnetic body that above-mentioned steps obtains, as shown in Figure 2, Fig. 2 is the metallurgical microstructrue figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 1 to result; See the metallurgical microstructrue figure that Fig. 3, Fig. 3 are neodymium iron boron magnetic body prepared by common process.As can be seen from the contrast of Fig. 2 and Fig. 3, compare the sintering process not filling hydrogen, the remarkable densification of neodymium iron boron magnetic body crystal grain that the present embodiment prepares, through survey calculation, the crystal grain mean value of neodymium iron boron magnetic body prepared by the embodiment of the present invention 1 is 4.62 μm, and the crystal grain mean value of neodymium iron boron magnetic body prepared by common process is 6.78 μm, the present invention compares the crystallite dimension refinement of common process 31.8%.
Detect the magnetic property of the neodymium iron boron magnetic body product that above-mentioned steps obtains and magnet density, experimental result is the normal temperature magnetic performance data figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 1 see Fig. 4, Fig. 4.See table 4, table 4 is neodymium iron boron magnetic body magnetic property data at ambient and elevated temperatures prepared by embodiment 1.
Neodymium iron boron magnetic body magnetic property data at ambient and elevated temperatures prepared by table 4 embodiment 1
Carry out other Performance Detection to neodymium iron boron magnetic body prepared by the present embodiment, see table 5, table 5 is the magnet composition situation of neodymium iron boron magnetic body prepared by the embodiment of the present invention 1.
Equipment: ICP.
The composition situation of neodymium iron boron magnetic body prepared by table 5 embodiment of the present invention 1
| Total amount of rare earth | |
| Formula | 31.1 |
| Fill hydrogen sintering process | 31.0 |
| Normal sintering process | 29.2 |
As shown in Table 5, neodymium iron boron magnetic body prepared by the embodiment of the present invention 1 compares existing technique, and the rare earth Expenditure Levels of magnet is few especially.
See table 6, table 6 is the aging conditions of neodymium iron boron magnetic body prepared by the embodiment of the present invention 1.
Below-G conditions: temperature 130 DEG C, humidity 100%, time 240h, pressure 2.7Bar;
Equipment: HAST ageing oven
The aging conditions of neodymium iron boron magnetic body prepared by table 6 embodiment of the present invention 1
| Weightlessness/mg/cm 2 | |
| Fill hydrogen sintering process | 1.5 |
Obviously can be found out by above-mentioned testing result, neodymium iron boron magnetic body sintering method provided by the invention, significantly can improve the magnet performance such as remanent magnetism, coercive force, maximum magnetic energy product, squareness of magnet, and there is good high-temperature stability.
Embodiment 2
Preparation 42SH sintered NdFeB
First, by 42SH formula batching, through ingot casting, fragmentation, abrasive dust, magnetic field orientating, compressing, obtain neodymium iron boron green compact.
Then green compact are loaded vacuum sintering furnace, be evacuated to vacuum degree and be less than 0.3Pa, neodymium iron boron magnetic body green compact are carried out after first time, constant temperature fired 70min, obtaining the first intermediate at 230 DEG C; Then the first intermediate above-mentioned steps obtained carries out after second time constant temperature fires 80min, obtaining the second intermediate at 520 DEG C; The second intermediate above-mentioned steps obtained again carries out after third time, constant temperature fired 120min, obtaining neodymium iron boron magnetic body intermediate at 780 DEG C.
After neodymium iron boron magnetic body intermediate above-mentioned steps obtained again carries out constant temperature liquid-phase sintering 30min at 1040 DEG C, to above-mentioned neodymium iron boron magnetic body intermediate 0.065MPa, under the effect of above-mentioned hydrogen, after filling hydrogen constant temperature liquid-phase sintering 40min, close charge valve, liquid-phase sintering intermediate;
Then sintering 60min is continued at this temperature, stop heating, enter cooling stage, in sintering furnace, fill hydrogen to 0.085-0.098Mpa, machine air blast of blowing in is cooled to 60 DEG C and comes out of the stove, and obtaining specification is 51*44*31mm (direction of orientation is 29 sizes) neodymium iron boron magnetic body blank.
Finally, with surface grinding machine, oriented surface one side 60% is shown in light, is glued on iron staff with 502,17*8*1.4 (M) black-film is cut into inside diameter slicer, with the solution oil removing adding cleaning agent except glue, fall the radian of 0.2mm with automatic chamfering machine, remove burrs on edges, pass through ultrasonic oil removal, pickling, passivation, automatic zincincation, obtaining zinc coating thickness is 10 μm, is of a size of the neodymium iron boron magnetic body finished product of 17*8*1.4 (M).
Use XJ-63 type metallomicroscope to observe to the neodymium iron boron magnetic body that above-mentioned steps obtains, as shown in Figure 5, Fig. 5 is the metallurgical microstructrue figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 2 to result; As can be seen from Figure 5, the remarkable densification of neodymium iron boron magnetic body crystal grain that the present embodiment prepares, through survey calculation, the crystal grain mean value of neodymium iron boron magnetic body prepared by the embodiment of the present invention 2 is 4.83 μm.
Detect the magnetic property of the neodymium iron boron magnetic body product that above-mentioned steps obtains and magnet density, experimental result is the normal temperature magnetic performance data figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 2 see Fig. 6, Fig. 6.See table 7, table 7 is neodymium iron boron magnetic body magnetic property data at ambient and elevated temperatures prepared by embodiment 2.
Neodymium iron boron magnetic body magnetic property data at ambient and elevated temperatures prepared by table 7 embodiment 2
Carry out other Performance Detection to neodymium iron boron magnetic body prepared by the present embodiment, see table 8, table 8 is the composition situation of neodymium iron boron magnetic body prepared by the embodiment of the present invention 2.
Equipment: ICP.
The demagnetize situation of neodymium iron boron magnetic body prepared by table 8 embodiment of the present invention 2
| Total amount of rare earth | |
| Formula | 31.6 |
| Fill hydrogen sintering process | 31.3 |
| Normal sintering process | 29.4 |
As shown in Table 8, neodymium iron boron magnetic body prepared by the embodiment of the present invention 2 compares existing technique, and the rare earth consumption of magnet is few especially.
See table 9, table 9 is the aging conditions of neodymium iron boron magnetic body prepared by the embodiment of the present invention 2.
Below-G conditions: temperature 130 DEG C, humidity 100%, time 240h, pressure 2.7Bar;
Equipment: HAST ageing oven
The aging conditions of neodymium iron boron magnetic body prepared by table 9 embodiment of the present invention 2
| Weightlessness/mg/cm 2 | |
| Fill hydrogen sintering process | 0.8 |
Obviously can be found out by above-mentioned testing result, neodymium iron boron magnetic body sintering method provided by the invention, significantly can improve the magnet performance such as remanent magnetism, coercive force, maximum magnetic energy product, squareness of magnet, and there is good high-temperature stability.
Embodiment 3
Preparation 52M sintered NdFeB
First, by 52M formula batching, through ingot casting, fragmentation, abrasive dust, magnetic field orientating, compressing, obtain neodymium iron boron green compact.
Then green compact are loaded vacuum sintering furnace, be evacuated to vacuum degree and be less than 0.2Pa, neodymium iron boron magnetic body green compact are carried out after first time, constant temperature fired 80min, obtaining the first intermediate at 180 DEG C; Then the first intermediate above-mentioned steps obtained carries out after second time constant temperature fires 70min, obtaining the second intermediate at 480 DEG C; The second intermediate above-mentioned steps obtained again carries out after third time, constant temperature fired 150min, obtaining neodymium iron boron magnetic body intermediate at 790 DEG C.
After neodymium iron boron magnetic body intermediate above-mentioned steps obtained again carries out constant temperature liquid-phase sintering 30min at 1038 DEG C, hydrogen 0.08MPa is filled to above-mentioned neodymium iron boron magnetic body intermediate, above-mentioned fill the effect of hydrogen under, close charge valve, liquid-phase sintering intermediate after logical hydrogen constant temperature liquid-phase sintering 35min;
Then sintering 60min is continued at this temperature, stop heating, enter cooling stage, in sintering furnace, fill hydrogen to 0.085-0.98Mpa, machine air blast of blowing in is cooled to 60 DEG C and comes out of the stove, and obtaining specification is 53*37*32mm (direction of orientation is 32 sizes) neodymium iron boron magnetic body blank.
Finally, with surface grinding machine, oriented surface one side 60% is shown in light, is glued on iron staff with 502,14*6*3.2 (M) black-film is cut into inside diameter slicer, with the solution oil removing adding cleaning agent except glue, fall the radian of 0.2mm with automatic chamfering machine, remove burrs on edges, pass through ultrasonic oil removal, pickling, passivation, automatic zincincation, obtaining zinc coating thickness is 10 μm, is of a size of the neodymium iron boron magnetic body finished product of 14*6*3.2 (M).
Use XJ-63 type metallomicroscope to observe to the neodymium iron boron magnetic body that above-mentioned steps obtains, as shown in Figure 7, Fig. 7 is the metallurgical microstructrue figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 3 to result; As can be seen from Figure 7, the remarkable densification of neodymium iron boron magnetic body crystal grain that the present embodiment prepares, through survey calculation, the crystal grain mean value of neodymium iron boron magnetic body prepared by the embodiment of the present invention 3 is 4.63 μm.
Detect the magnetic property of the neodymium iron boron magnetic body product that above-mentioned steps obtains and magnet density, experimental result is the normal temperature magnetic performance data figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 3 see Fig. 8, Fig. 8.See table 10, table 10 is neodymium iron boron magnetic body magnetic property data at ambient and elevated temperatures prepared by embodiment 3.
Neodymium iron boron magnetic body magnetic property data at ambient and elevated temperatures prepared by table 10 embodiment 3
Carry out other Performance Detection to neodymium iron boron magnetic body prepared by the present embodiment, see table 11, table 11 is the composition situation of neodymium iron boron magnetic body prepared by the embodiment of the present invention 3.
Equipment: ICP.
The composition situation of neodymium iron boron magnetic body prepared by table 11 embodiment of the present invention 3
| Total amount of rare earth | |
| Formula | 30 |
| Fill hydrogen sintering process | 29.8 |
| Normal sintering process | 28.6 |
As shown in Table 11, neodymium iron boron magnetic body prepared by the embodiment of the present invention 3 compares existing technique, and the rare earth consumption of magnet is few especially.
See table 12, table 12 is the aging conditions of neodymium iron boron magnetic body prepared by the embodiment of the present invention 3.
Below-G conditions: temperature 130 DEG C, humidity 100%, time 240h, pressure 2.7Bar;
Equipment: HAST ageing oven
The aging conditions of neodymium iron boron magnetic body prepared by table 12 embodiment of the present invention 3
| Weightlessness/mg/cm 2 | |
| Fill hydrogen sintering process | 0.6 |
Obviously can be found out by above-mentioned testing result, neodymium iron boron magnetic body sintering method provided by the invention, significantly can improve the magnet performance such as remanent magnetism, coercive force, maximum magnetic energy product, squareness of magnet, and there is good high-temperature stability.
Above the sintering method of a kind of neodymium iron boron magnetic body provided by the present invention is described in detail.Apply a concrete example herein to set forth principle of the present invention and execution mode, the explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection range of the claims in the present invention.
Claims (10)
1. a sintering method for neodymium iron boron magnetic body, comprises the following steps:
A) under the condition of vacuum or protective gas, by neodymium iron boron magnetic body green compact after continuous warming or ladder-elevating temperature, arrive sintering temperature, obtain neodymium iron boron magnetic body intermediate;
B) under the condition of hydrogen, neodymium iron boron magnetic body intermediate above-mentioned steps obtained carries out after constant temperature fires, obtaining neodymium iron boron magnetic body blank.
2. sintering method according to claim 1, is characterized in that, described sintering temperature is 1000 ~ 1100 DEG C.
3. sintering method according to claim 1, is characterized in that, the heating rate of described continuous warming is 0.5 ~ 3 DEG C/min; The time of described continuous warming is 15 ~ 120min.
4. sintering method according to claim 1, is characterized in that, the concrete steps of described ladder-elevating temperature are:
A1) under the condition of vacuum or protective gas, neodymium iron boron magnetic body green compact are carried out after first time, constant temperature fired, obtain the first intermediate;
A2) the first intermediate then above-mentioned steps obtained carries out after second time constant temperature fires, obtaining the second intermediate;
A3) the second intermediate above-mentioned steps obtained again carries out after third time, constant temperature fired, obtaining neodymium iron boron magnetic body intermediate.
5. sintering method according to claim 4, is characterized in that, described first time the temperature fired of constant temperature be 200 ~ 250 DEG C; Constant temperature time of firing described first time is 90 ~ 150min;
The temperature that described second time constant temperature is fired is 450 ~ 550 DEG C; The time that described second time constant temperature is fired is 60 ~ 120min;
Described third time, the temperature fired of constant temperature was 750 ~ 850 DEG C; The time that described second time constant temperature is fired is 90 ~ 120min.
6. sintering method according to claim 1, is characterized in that, is describedly specially under the condition of hydrogen:
Be filled with hydrogen directly in equipment, or first the protective gas in agglomerating plant be evacuated to vacuum, then be filled with hydrogen in agglomerating plant.
7. sintering method according to claim 6, is characterized in that, the pressure of described vacuum is for being less than or equal to 10Pa; The pressure of described hydrogen is 0.030 ~ 0.098MPa.
8. sintering method according to claim 1, is characterized in that, described step B) also comprise,
Neodymium iron boron magnetic body intermediate after being fired by constant temperature, cools under the condition of hydrogen, obtains neodymium iron boron magnetic body blank.
9. sintering method according to claim 8, is characterized in that, the speed of described cooling is 6.0 ~ 8.5 DEG C/min.
10. a neodymium iron boron magnetic body, is characterized in that, described neodymium iron boron magnetic body is by neodymium iron boron magnetic body green compact under the condition of hydrogen, obtains after liquid-phase sintering or solid-phase sintering.
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| WO2021219063A1 (en) * | 2020-04-30 | 2021-11-04 | 烟台正海磁性材料股份有限公司 | Fine-grain high-coercivity sintered neodymium iron boron magnet and preparation method therefor |
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