CN104625079B - Preparing method of rare earth iron-boron-based anisotropy magnetic powder and prepared magnetic powder - Google Patents
Preparing method of rare earth iron-boron-based anisotropy magnetic powder and prepared magnetic powder Download PDFInfo
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Abstract
The invention discloses a preparing method of rare earth iron-boron-based anisotropy magnetic powder and the prepared magnetic powder. The method comprises the steps that rare earth iron-boron alloy particles are subjected to HDDR processing, the rare earth iron-boron alloy particles obtained after HDDR processing is subjected to HDDR processing again, and accordingly the high-coercivity rare earth iron-boron-based anisotropy magnetic powder is obtained. The coercivity of the rare earth iron-boron-based anisotropy magnetic powder can be greatly improved, magnetic powder cost cannot be increased, and the residual magnetism and the maximum magnetic energy product of the magnetic powder cannot be lowered greatly.
Description
Technical field
The present invention relates to field of magnetic material, more particularly to a kind of rare-earth iron-boron system anisotropic magnet powder preparation method and
Prepared magnetic.
Background technology
At present, the method that the coercivity of rare-earth iron-boron system anisotropic magnet powder is lifted is enable mainly there are following three kinds：
The first, in notification number in the Chinese patent of CN1198291C, Aichi, Janpan Zhi Gang Co., Ltd. is utilizing
HDDR (hydrongenation-disproperation-desorption-recombination, suction hydrogen-disproportionation-dehydrogenation-again
With reference to) RFeBH of PROCESS FOR TREATMENTxA small amount of diffusion based on the hydrogen compound of dysprosium (or disprosium alloy) is added in powder process
Powder, Jing after fully mixing, carries out grain boundary decision heat treatment and subsequent dehydration processes, such that it is able to obtain high-coercive force and height
Anisotropic magnetic；In this way obtained magnetic has excellent temperature stability.But this method is at least present
Following two shortcomings：One is the increase in operation, reduces production efficiency；Two are the use of a certain amount of dysprosium element, cause making
The cost of magnetic increases.
Second, in notification number in the Chinese patent of CN102648502A, Aichi, Janpan Zhi Gang Co., Ltd. is utilizing
The RFeBH of HDDR PROCESS FOR TREATMENTsxA certain amount of Nd-Cu powder or Nd-Cu-Al powder are added in powder process, Jing is fully mixed
After even, grain boundary decision heat treatment and subsequent dehydration processes are carried out, such that it is able to obtain the high coercive without rare element Dy, Ga
Power magnetic；In this way obtained magnetic has good temperature stability and cost is relatively low.But this method is at least
There are following two shortcomings：One is the increase in operation, reduces production efficiency；Two is due to the addition of a certain amount of non magnetic unit
Plain Cu, Al, cause the important technology indexs such as the remanent magnetism of magnetic and maximum magnetic energy product to be decreased obviously.
The third, in notification number in the Chinese patent of CN103782352A, Japanese Toda Kogyo Corp. is by pre-
The Nd Fe B alloys ingot rich in Nd elements and Al elements is first prepared, then coordinates enforcement suitable with material chemical component again
HDDR techniques, so as to the high-coercive force magnetic of low cost has been obtained.But magnetic obtained in this method is due to rich in nonmagnetic
Al elements, cause the important technology index such as remanent magnetism and maximum magnetic energy product of magnetic to be remarkably decreased, and have been largely affected by magnetic
Popularization and application.
The content of the invention
For above-mentioned weak point of the prior art, the invention provides a kind of rare-earth iron-boron system anisotropic magnet powder
Preparation method and prepared magnetic, can not only greatly improve the coercivity of rare-earth iron-boron system anisotropic magnet powder, and not
Magnetic cost can be increased, the remanent magnetism and maximum magnetic energy product that will not also make magnetic declines to a great extent.
The purpose of the present invention is achieved through the following technical solutions：
The preparation method of a kind of rare-earth iron-boron system anisotropic magnet powder, including carrying out at HDDR to rare-earth iron-boron alloy particle
The step of reason, also comprise the steps：HDDR process is carried out again to the rare-earth iron-boron alloy particle after HDDR is processed,
So as to obtain the rare-earth iron-boron system anisotropic magnet powder of high-coercive force.
Preferably, it is described that a HDDR process is at least carried out again to the rare-earth iron-boron alloy particle after HDDR is processed
Comprise the steps：
Step c1, second HDDR inhale hydrogen-disproportionation stage in processing：By the rare-earth iron-boron alloy after HDDR is processed
Grain is inserted in HDDR stoves, and 760～860 DEG C are heated under vacuum or inert gas environment, is then passed through hydrogen into HDDR stoves
Gas, makes the Hydrogen Vapor Pressure in HDDR stoves maintain 20～100kPa, heat-insulation pressure keeping 15～180 minutes, so as to complete to inhale hydrogen-disproportionation
The process in stage；
Step c2, second HDDR process in slow desorption-in conjunction with the stage：Hydrogen-after the completion of the disproportionation stage is being inhaled, will
Temperature in HDDR stoves is promoted to 800～900 DEG C, and makes the Hydrogen Vapor Pressure in HDDR stoves be adjusted to 1～10kPa, heat-insulation pressure keeping
15～60 minutes, so as to complete slow desorption-in conjunction with the process in stage；
Step c3, second HDDR complete dehydrogenation stage in processing：After the completion of slow desorption-in conjunction with the stage, make
Temperature in HDDR stoves maintains 800～900 DEG C, and carries out the vacuum pumping of 15～120 minutes, then makes HDDR in-furnace temperatures
Fast cooling, so as to complete the process of dehydrogenation stage completely during second HDDR is processed, obtains high-coercive force to less than 50 DEG C
Rare-earth iron-boron system anisotropic magnet powder.
Preferably, it is described the step of HDDR is processed is carried out to rare-earth iron-boron alloy particle to include：
Step b1, suction hydrogen-disproportionation stage：Rare-earth iron-boron alloy particle is inserted in HDDR stoves, and in vacuum or indifferent gas
760～860 DEG C are heated under body environment, then hydrogen is passed through into HDDR stoves, make the Hydrogen Vapor Pressure in HDDR stoves maintain 20
～100kPa, heat-insulation pressure keeping 0.5～4 minute, so as to the process for completing to inhale hydrogen-disproportionation stage；
Step b2, slow desorption-in conjunction with the stage：Hydrogen-after the completion of the disproportionation stage is being inhaled, the temperature in HDDR stoves is being lifted
To 800～900 DEG C, and the Hydrogen Vapor Pressure in HDDR stoves is set to be adjusted to 1～10kPa, heat-insulation pressure keeping 15～180 minutes, so as to complete
Into slow desorption-in conjunction with the process in stage.
Preferably, it is described the step of HDDR is processed is carried out to rare-earth iron-boron alloy particle also to include：
Step b3, complete dehydrogenation stage：After the completion of slow desorption-in conjunction with the stage, maintain the temperature in HDDR stoves
At 800～900 DEG C, and the vacuum pumping of 15～120 minutes is carried out, so as to complete the process of complete dehydrogenation stage.
Preferably, described rare-earth iron-boron alloy particle is obtained as follows：
Step a1, dispensing is carried out according to the chemical general formula RxT1-x-y-zByMz of rare-earth iron-boron system magnetic, and make rare earth
Ferroboron ingot casting or rare-earth iron-boron alloy rapid-hardening flake；
In chemical general formula, R is at least one in Nd, Pr, La, Ce, Dy or Tb this several element；T be Fe, Co or Ni this
At least one in several elements；M is at least one in Ga, Nb, Zr, Cu, Al, V, Ti, Mo, Si or Mn this several element；
X, y, z represents that respectively R, B, M account for overall percetage by weight, and meets following condition：27.0wt.%≤x≤
31.5wt.%, 0.9wt.%≤y≤1.1wt.%, 0.1wt.%≤z≤3.0wt.%；1-x-y-z are represented in addition to R, B, M,
Surplus is T；
Step a2, the heat treatment that homogenizes is carried out to rare-earth iron-boron alloy ingot casting or rare-earth iron-boron alloy rapid-hardening flake；
Step a3, to homogenize heat treatment after rare-earth iron-boron alloy ingot casting or rare-earth iron-boron alloy rapid-hardening flake carry out hydrogen break
Broken process, obtains rare-earth iron-boron alloy particle.
Preferably, described x, y, z meets following condition：27.5wt.%≤x≤30.0wt.%, 0.95wt.%≤y≤
1.05wt.%, 0.3wt.%≤z≤1.5wt.%.
Preferably, it is described that the heat treatment bag that homogenizes is carried out to rare-earth iron-boron alloy ingot casting or rare-earth iron-boron alloy rapid-hardening flake
Include：During rare-earth iron-boron alloy ingot casting or rare-earth iron-boron alloy rapid-hardening flake are placed in into vacuum or inert gas, and 1050～
5～40 hours are incubated at 1160 DEG C, so as to complete the heat treatment that homogenizes.
Preferably, described rare-earth iron-boron alloy ingot casting or rare-earth iron-boron alloy rapid-hardening flake to after the heat treatment that homogenizes enters
Row hydrogen break process includes：Initial temperature is set as 200～300 DEG C, and inhaling hydrogen process carries out 0.5～3 hour.
Preferably, also comprise the steps：Finely divided place is carried out to the rare-earth iron-boron system anisotropic magnet powder of high-coercive force
Reason, makes the granularity of rare-earth iron-boron system anisotropic magnet powder less than 180 μm, so as to obtain the rare-earth iron-boron of easy magnetization, high-coercive force
It is anisotropic magnet powder.
A kind of rare-earth iron-boron system anisotropic magnet powder, using the rare-earth iron-boron system anisotropy described in above-mentioned technical proposal
The preparation method of magnetic is prepared from.
As seen from the above technical solution provided by the invention, the rare-earth iron-boron magnetic that the embodiment of the present invention is provided
Preparation method employs the coercivity that HDDR process twice improves obtained magnetic, i.e., after the process of HDDR first, carry out again
Second HDDR process；For other lifting coercitive methods of magnetic, the embodiment of the present invention provided this
Preparation method can not only greatly improve the coercivity of rare-earth iron-boron system anisotropic magnet powder, and simple effective, with low cost,
With good application value.During the HDDR first of the present invention is processed, " inhaling hydrogen-disproportionation " is anti-with " dehydrogenation-be combined again "
Answer speed slow, it is hereby achieved that high magnetocrystalline anisotropy magnetic；During second HDDR of the present invention is processed, by magnetic
Established in particle, numerous crystal boundary quickly completes in a short period of time second as the diffusion admittance of hydrogen
" inhale hydrogen-disproportionation " reaction, " slow desorption-be combined again " for then carrying out lower temperature successively again process and " complete dehydrogenation "
Process, it is hereby achieved that crystal grain is more tiny, uniformity high-coercive force, high magnetocrystalline anisotropy magnetic.Additionally, this
Bright HDDR first is processed can continuously be implemented also to be interrupted enforcement with second HDDR process, continuous to implement significantly to save the time
Cost, thus be optimal selection.
Description of the drawings
In order to be illustrated more clearly that the technical scheme of the embodiment of the present invention, below will be to use needed for embodiment description
Accompanying drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this
For the those of ordinary skill in field, on the premise of creative work row is not paid, can be obtaining it according to these accompanying drawings
His accompanying drawing.
The parameter curve conversion schematic diagram of the rare-earth iron-boron magnetic preparation method that Fig. 1 is provided by the embodiment of the present invention.
Specific embodiment
With reference to the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Ground description, it is clear that described embodiment is only a part of embodiment of the invention, rather than the embodiment of whole.Based on this
Inventive embodiment, the every other enforcement that those of ordinary skill in the art are obtained under the premise of creative work is not made
Example, belongs to protection scope of the present invention.
Firstly the need of explanation, " wt.% " described in present specification represents percetage by weight, and present specification
Described in " HDDR stoves " can adopt the furnace equipment of HDDR process is carried out in prior art.Below to provided by the present invention
The preparation method and prepared magnetic of rare-earth iron-boron system anisotropic magnet powder is described in detail.
(1) preparation method of a kind of rare-earth iron-boron system anisotropic magnet powder
A kind of preparation method of rare-earth iron-boron system anisotropic magnet powder, comprises the steps：
Step a：The step of preparing rare-earth iron-boron alloy particle.
Specifically：The step of this prepares rare-earth iron-boron alloy particle can include：
(1) step a1, according to the chemical general formula R of rare-earth iron-boron system magneticxT1-x-y-zByMzDispensing is carried out, and makes rare earth
Ferroboron ingot casting or rare-earth iron-boron alloy rapid-hardening flake.
In chemical general formula, R is at least one in neodymium (Nd), praseodymium (Pr), lanthanum (La), cerium (Ce), dysprosium (Dy) or terbium (Tb)；
T is at least one in iron (Fe), cobalt (Co) or nickel (Ni)；M is gallium (Ga), niobium (Nb), zirconium (Zr), copper (Cu), aluminium (Al), vanadium
(V), at least one in titanium (Ti), molybdenum (Mo), silicon (Si) or manganese (Mn)；B is boron element.X, y, z represents that respectively R, B, M are accounted for always
The percetage by weight of body, and meet following condition：27.0wt.%≤x≤31.5wt.%, 0.9wt.%≤y≤
1.1wt.%, 0.1wt.%≤z≤3.0wt.%；In actual applications, x, y, z preferably meets following condition：27.5wt.%
≤ x≤30.0wt.%, 0.95wt.%≤y≤1.05wt.%, 0.3wt.%≤z≤1.5wt.%.1-x-y-z represent except
Outside R, B, M, surplus is T.
It should be noted that the preparation method of rare-earth iron-boron system anisotropic magnet powder that the embodiment of the present invention is provided is to changing
Formula is RxT1-x-y-zByMzRare-earth iron-boron system magnetic there is universal adaptability, but consider from production cost, rare-earth iron-boron
It is preferably also should not to add too much without the rare heavy rare earth elements such as Dy, Tb, and Co, Ga in magnetic.The raw material for preparing
Can be that rare-earth iron-boron alloy ingot casting (thickness is usually 5～15mm) or rare-earth iron-boron are smelted into using method of the prior art
Alloy rapid-hardening flake (thickness is usually 0.3 ± 0.05mm), but from the homogeneity of ingredients and the follow-up heat that homogenizes of microstructure
Manage to consider, the raw material for preparing is preferably made rare-earth iron-boron alloy rapid-hardening flake.
(2) step a2, the heat treatment that homogenizes is carried out to rare-earth iron-boron alloy ingot casting or rare-earth iron-boron alloy rapid-hardening flake.
Specifically, the purpose of heat treatment of homogenizing is to eliminate the soft magnetism phase α-Fe in alloy, and makes average crystalline substance
Particle size increases to desired value, to improve the magnetic property of powder prepared by HDDR techniques.Homogenizing in the embodiment of the present invention
Heat treatment can include：During rare-earth iron-boron alloy ingot casting or rare-earth iron-boron alloy rapid-hardening flake are placed in into vacuum or inert gas,
And 5～40 hours are incubated at 1050～1160 DEG C, so as to complete the heat treatment that homogenizes.Heat treatment homogenize preferably in vacuum or
Carry out in inert gas, this can effectively prevent rare-earth iron-boron alloy ingot casting or rare-earth iron-boron alloy rapid-hardening flake to be oxidized；Inertia
The pressure of gas is under malleation or negative pressure, if negative pressure, then reduced pressure should be with the chemical element of composition alloying component not
Out it is limited from alloy pig surface evaporation, in order to avoid cause alloy pig local part to change；If malleation, for cost and setting
Consideration in terms of the standby life-span, is advisable with 0.1～0.3MPa.The heat treatment that homogenizes preferably is carried out at 1050～1160 DEG C, if low
In 1050 DEG C, then the soft magnetism phase α-Fe in alloy can not be effectively eliminated；If being higher than 1160 DEG C, the crystal grain in alloy can be sent out
Raw abnormal growth phenomenon, or even fusing occurs, so as to influence whether finally to be obtained the magnetic property of magnetic.
(3) step a3, to homogenize heat treatment after rare-earth iron-boron alloy ingot casting or rare-earth iron-boron alloy rapid-hardening flake carry out
Hydrogen break process, obtains rare-earth iron-boron alloy particle.
Specifically, hydrogen break process can be carried out according to hydrogen break process of the prior art, it should be noted that just
Beginning temperature (should be preferably set for 200～300 DEG C) below 600 DEG C, and inhaling hydrogen process preferably carries out 0.5～3 hour, and this can be with
Rare-earth iron-boron alloy ingot casting or rare-earth iron-boron alloy rapid-hardening flake is set fully to inhale hydrogen.The hydrogen environment that hydrogen break process is used can be
The environment that pure hydrogen environment, or hydrogen mix with inert gas；And hydrogen break process is usual to the hydrogen dividing potential drop of hydrogen environment
It is not particularly limited, but preferably in the range of 0.05～0.3MPa, preferably in 0.1～0.2MPa；If the hydrogen of hydrogen environment point
Force down in 0.05MPa, then absorption hydrogen is very slow, low production efficiency；If the hydrogen dividing potential drop of hydrogen environment is higher than 0.3MPa, it is difficult to ensure
Production security, considers also not calculate from financial cost.In actual applications, during hydrogen break process, it is desirable that
Alloy material carries out continuous overturning stirring, so as to make its further refinement, and steadily entering for follow-up gas solid state reaction
Capable and final fine crushing creates condition advantageously.
Step b：The step of HDDR being carried out to rare-earth iron-boron alloy particle and processes.
Specifically, there is HDDR process twice in the present invention, step b is carried out at HDDR to rare-earth iron-boron alloy particle
Reason is HDDR process first, and HDDR process first can be carried out according to HDDR techniques of the prior art, but preferably according to following
The step of carry out：
(1) step b1, suction hydrogen-disproportionation stage：Rare-earth iron-boron alloy particle is inserted in HDDR stoves, and in vacuum or inertia
760～860 DEG C are heated under gaseous environment, then hydrogen is passed through into HDDR stoves, the Hydrogen Vapor Pressure in HDDR stoves is maintained
20～100kPa, heat-insulation pressure keeping 0.5～4 hour, so as to the process for completing to inhale hydrogen-disproportionation stage.
Specifically, in the process of HDDR first, " inhaling hydrogen-disproportionation stage " is the key that magnetocrystalline anisotropy is generated；It is logical
Cross and the hydrogen dividing potential drop and temperature in HDDR stoves is controlled, " inhaling hydrogen-disproportionation " reacting balance can be made, lentamente carried out, so as to
Anisotropic magnet powder finally high magnetocrystalline to be obtained has established microstructure basis.
(2) step b2, slow desorption-in conjunction with the stage：Hydrogen-after the completion of the disproportionation stage is being inhaled, by the temperature in HDDR stoves
It is promoted to 800～900 DEG C, and makes the Hydrogen Vapor Pressure in HDDR stoves be adjusted to 1～10kPa, heat-insulation pressure keeping 15～180 minutes, from
And complete slow desorption-in conjunction with the process in stage.
Specifically, in the process of HDDR first, " slow desorption-in conjunction with the stage " it is to obtain high magnetocrystalline anisotropy
Necessary condition；By being controlled to the hydrogen dividing potential drop and temperature in HDDR stoves, can make " slow desorption-in conjunction with " react flat
Surely, lentamente carry out, be conducive to obtaining the anisotropic powder of high magnetocrystalline；And by the temperature and temperature retention time in HDDR stoves
It is controlled, the R to be formed can be madexT1-x-y-zByMzCrystal grain is moderately grown up, so as to processing and carry for second follow-up HDDR
The anisotropy and high-coercive force of high obtained magnetic creates precondition.
(3) step b3, complete dehydrogenation stage：After the completion of slow desorption-in conjunction with the stage, tie up the temperature in HDDR stoves
Hold at 800～900 DEG C, and carry out the vacuum pumping of 15～120 minutes, complete the process of complete dehydrogenation stage.
Specifically, in the process of HDDR first, " complete dehydrogenation stage " is not essential, and whether it performs needs regards
Depending on the actual conditions of target product；If first HDDR has " complete dehydrogenation stage " in processing, advantageously in raising most
The coercivity of magnetic is obtained eventually, but the remanent magnetism that magnetic is finally obtained can be made to be declined slightly with maximum magnetic energy product, while also can increase
Time cost；If first HDDR does not have " complete dehydrogenation stage " in processing, be conducive to finally being obtained the remanent magnetism of magnetic with most
The raising of big magnetic energy product, at the same can improve production efficiency, but be declined slightly can the coercivity of final magnetic.In practical application
In, first HDDR is processed and can continuously implemented with second HDDR process, it is also possible to which interruption is implemented, but to save process time,
Preferably continuously implement.
Understand after testing, after HDDR process first (the single HDDR process for adopting in prior art), can be obtained
The excellent magnetic of comprehensive magnetic energy, its Exemplary magnetic can be as follows：Br=13.0～14.0kGs, iHc=12.0～16.0kOe,
(BH) max=35.0～40.0MGOe；Although first HDDR processes obtained magnetic, its remanent magnetism Br, maximum magnetic energy product (BH)
Max is preferable, but its HCJ iHc relative deficiencies, causes its maximum operation (service) temperature less than 80 DEG C, therefore in prior art
Its application is greatly limit merely through the obtained magnetic of single HDDR process.
Step c：Second HDDR process is carried out to the rare-earth iron-boron alloy particle after HDDR is processed, so as to obtain height
Coercitive rare-earth iron-boron system anisotropic magnet powder.
Specifically, step c to the rare-earth iron-boron alloy particle after HDDR is processed carries out second HDDR process
It is second HDDR process, second HDDR is processed and preferably carried out according to the following steps：
(1) step c1, second HDDR inhale hydrogen-disproportionation stage in processing：Rare-earth iron-boron after HDDR is processed is closed
Gold grain is inserted in HDDR stoves, and 760～860 DEG C are heated under vacuum or inert gas environment, is then led to into HDDR stoves
Enter hydrogen, make the Hydrogen Vapor Pressure in HDDR stoves maintain 20～100kPa, heat-insulation pressure keeping 15～180 minutes, so as to complete to inhale hydrogen-
The process in disproportionation stage.
Specifically, in second HDDR is processed, " inhaling hydrogen-disproportionation stage " can be within the very short time (about 15 minutes)
Reaction is finished, and its reason is：After the process of HDDR first, the internal shape of original big crystal grain (tens microns to microns up to a hundred)
Into about 0.3 μm of little crystal grain of large number of average grain diameter, a large amount of crystal boundaries are there are between these little crystal grains, be that protium expands
Dissipate and enter powder particle inside there is provided convenient condition, thus " inhaling hydrogen-disproportionation " reaction can be rapidly completed.
(2) slow desorption during step c2, second HDDR are processed-in conjunction with the stage：Inhaling hydrogen-after the completion of the disproportionation stage,
Temperature in HDDR stoves is promoted to into 800～900 DEG C, and makes the Hydrogen Vapor Pressure in HDDR stoves be adjusted to 1～10kPa, insulation is protected
Pressure 15～60 minutes, so as to complete slow desorption-in conjunction with the process in stage.
Specifically, in second HDDR is processed, " slow desorption-in conjunction with the stage " chemical reaction can be enable to put down
Surely, lentamente carry out, so that the new R for being formedxT1-x-y-zByMzThe direction of easy axis of crystal grain cluster is consistent.
(3) complete dehydrogenation stage in step c3, second HDDR process：After the completion of slow desorption-in conjunction with the stage, make
Temperature in HDDR stoves maintains 800～900 DEG C, and carries out the vacuum pumping of 15～120 minutes, then makes HDDR in-furnace temperatures
Fast cooling, so as to complete the process of dehydrogenation stage completely during second HDDR is processed, obtains high-coercive force to less than 50 DEG C
Rare-earth iron-boron system anisotropic magnet powder.
Specifically, in second HDDR is processed, " complete dehydrogenation stage " is essential, its objective is to make alloy powder
In remaining protium it is completely out；If not carrying out " complete dehydrogenation stage ", the coercivity of final obtained magnetic can be made
Step-down, is also easy to cause magnet hydrogen-induced cracking.
Understand after testing, after second HDDR is processed, the Exemplary magnetic of obtained magnetic can be as follows：Br=12.5～
13.8kGs, iHc=16.0～20.0kOe, (BH) max=30.0～38.0MGOe；With obtained magnetic after first time HDDR process
Powder is compared, and second HDDR processes the magnetic for preparing, and its remanent magnetism Br and maximum magnetic energy product (BH) max has to a certain degree underground
Drop, but its HCJ iHc is remarkably reinforced, and its maximum operation (service) temperature can be improved to 100 DEG C～120 DEG C, therefore using this
Magnetic obtained in bright provided rare-earth iron-boron magnetic preparation method, its application is significantly widened.
In addition to above-mentioned technical proposal, the preparation side of the rare-earth iron-boron system anisotropic magnet powder that the embodiment of the present invention is provided
Method can also comprise the steps：
Step d：Finely divided process is carried out to the rare-earth iron-boron system anisotropic magnet powder of high-coercive force, makes rare-earth iron-boron system each
The granularity of anisotropy magnetic is less than 180 μm, so as to obtain the rare-earth iron-boron system anisotropic magnet powder of easy magnetization, high-coercive force.
Specifically, through the magnetic obtained by above-mentioned steps a, step b and step c, its powder particle is big and size distribution
, there are the different some particle adhesions of direction of easy axis together in wide ranges, the magnetic property of magnetic fails to give full play to.
The granularity of magnetic can be adjusted by the process of this step d, its granularity is preferably less than 180 μm, preferably 45～150
Between μm, if the granularity of magnetic is less than 45 μm, then due to the increase of specific surface area, magnetic is easy to oxidation, while crystal grain lacks
Fall into and increase, so as to magnetic property can be caused to be decreased obviously；If the granularity of magnetic is more than 150 μm, then direction of easy axis is different
Some particle adhesions problem together increases, so as to remanent magnetism can be caused to be decreased obviously.Finely divided process can adopt existing skill
The powder-making techniques such as band sieve ball milling, air-flow crushing in art are processed, but for the purpose for preventing magnetic from aoxidizing, finely divided process
During preferably carry out under vacuum or inert gas shielding.
It should be noted that the process through above-mentioned steps a, step b, step c and step d can be obtained high-coercive force, height
(invention people this magnetic processing method provided by the present invention is called t-HDDR to the rare-earth iron-boron system anisotropic magnet powder of magnetic property
Technique), its technological process is with reference to shown in Fig. 1；Two horizontal dotted lines in Fig. 1 represent respectively HDDR first and " take off completely in processing
The temperature and hydrogen dividing potential drop of hydroformylation stage ".
As fully visible, the embodiment of the present invention has carried out second HDDR process, relative to it again after the process of HDDR first
It is lifted for the coercitive method of magnetic, and this preparation method that the embodiment of the present invention is provided can not only greatly improve dilute
The coercivity of unmanufactured iron boron system anisotropic magnet powder, and it is simple effective, with low cost, with good application value.
In order to more clearly from show technical scheme provided by the present invention and produced technique effect, below with several
The preparation method of rare-earth iron-boron system anisotropic magnet powder that group comparative example is provided the embodiment of the present invention and prepared
Magnetic is described in detail.
Embodiment 1～12
Respectively dispensing is carried out according to the magnetic composition proportion scheme in table 1 below, and according in above-mentioned technical proposal of the present invention
Described rare-earth iron-boron system anisotropic magnetic powder, preparation method thereof completes 12 specific embodiment of the invention, rectifys so as to be obtained 12 kinds high
The rare-earth iron-boron system anisotropic magnet powder of stupid power, then using vibrating specimen magnetometer of the prior art (VSM) to every kind of rare earth
HCJ iHc, the remanent magnetism Br of iron boron system anisotropic magnet powder and maximum magnetic energy product (BH) max these performance indications are carried out
Measurement, its measurement result can be with as shown in table 3 below.Wherein, embodiments of the invention 2 are carrying out being performed when first HDDR is processed
The step for " complete dehydrogenation stage ", and remaining embodiment of the present invention is carrying out being not carried out " completely when first HDDR is processed
The step for dehydrogenation stage "；The specific embodiment of this 12 present invention is carrying out being performed both by " second when second HDDR is processed
Secondary HDDR process in dehydrogenation stage completely " the step for (in second HDDR is processed dehydrogenation stage completely, the temperature in HDDR stoves
Spend for 825 DEG C, hydrogen dividing potential drop<1.0Pa, pumpdown time are 1h).Machined parameters selected by each specific embodiment of the invention can
With as shown in table 2 below.
Comparative example 1～5
Carry out dispensing according to the magnetic composition proportion scheme in table 1 below respectively, and according to being only performed once in prior art
The magnetic preparation method of HDDR process completes the comparative example of 5 prior arts, so as to 5 kinds of rare-earth iron-boron systems are obtained respectively to different
Property magnetic, then using vibrating specimen magnetometer of the prior art (VSM) in every kind of rare-earth iron-boron system anisotropic magnet powder
Report coercivity iHc, remanent magnetism Br and maximum magnetic energy product (BH) max these performance indications to measure, its measurement result can be as
Shown in table 3 below.Wherein, the machined parameters selected by each comparative example can be with as shown in table 2 below.
Table 1：
Table 2：
Table 3：
Being contrasted embodiment 1～12 with comparative example 1～5 with reference to table 1～3 at least can draw to draw a conclusion：
(1) knowable to embodiments of the invention 1～12 and comparative example of the prior art 1～5 being contrasted：With existing skill
The magnetic preparation method only with single HDDR process in art is compared, rare-earth iron-boron system provided by the present invention anisotropic magnetic
Magnetic obtained by powder, preparation method thereof, its coercivity iHc is obtained for significant raising, and the lifting amplitude of coercivity iHc is up to
2kOe～4kOe.
(2) knowable to embodiments of the invention 1 and embodiments of the invention 2 being contrasted：Both are in preparation method
Differing only in embodiment 2 is carrying out the step for performing " complete dehydrogenation stage " when first HDDR is processed, and embodiment 1 is simultaneously
The step for being not carried out, but from the performance of obtained magnetic, the magnetic obtained by embodiment 1 has relatively higher remanent magnetism
Br and maximum magnetic energy product (BH) max, and the magnetic obtained by embodiment 2 has relatively higher coercivity iHc.This shows：
In the rare-earth iron-boron system anisotropic magnetic powder, preparation method thereof that the present invention is provided, if carrying out arranging " complete when HDDR first is processed
The step for full dehydrogenation stage ", then be conducive to improving the coercivity of final magnetic.
(3) knowable to embodiments of the invention 3, embodiment 4 and embodiment 5 being contrasted：Before other conditions are constant
Put, incrementally increase the temperature and time of " slow desorption-be combined the stage again " during first HDDR is processed, obtained magnetic can be made
Remanent magnetism Br and maximum magnetic energy product (BH) max step up, and the coercivity iHc of obtained magnetic is then on a declining curve.This table
It is bright：In the rare-earth iron-boron system anisotropic magnetic powder, preparation method thereof that the present invention is provided, if in the " slow de- of the process of HDDR first
The step for hydrogen-be combined the stage again ", is using relatively low temperature and relatively short time, then be conducive to improving final magnetic
The coercivity of powder.
(4) knowable to embodiments of the invention 6～10 are contrasted：On the premise of other conditions are constant, progressively shorten
The process time of " second HDDR complete dehydrogenation stages in processing ", the coercivity iHc that can make obtained magnetic is stepped up,
And make remanent magnetism Br and maximum magnetic energy product (BH) max on a declining curve.This shows：The rare-earth iron-boron system provided in the present invention is respectively to different
Property magnetic preparation method in, if adopting relatively short process time at " second HDDR process in completely dehydrogenation stage ",
So be conducive to improving the coercivity of final magnetic.
(5) knowable to embodiments of the invention 11 and comparative example of the prior art 4 being contrasted：Comparative example 4 is due to receiving
To the impact containing 2.0wt.% heavy rare earth elements Dy and higher this double factor of rare earth element total content, therefore the existing skills of Jing
After single HDDR in art is processed, the magnetic that coercivity iHc is up to 17.5kOe is obtained.Embodiment 11 is the base in comparative example 4
Second HDDR process for implementing the present invention is added on plinth, as a result the coercivity iHc of obtained magnetic is by original 17.5kOe
19.5kOe is further promoted to, this absolutely proves the rare-earth iron-boron system anisotropic magnetic powder, preparation method thereof pair provided in the present invention
In improve magnetic coercivity be fruitful.
(6) knowable to embodiments of the invention 12 and comparative example of the prior art 5 being contrasted：Comparative example 5 is due to receiving
To containing a certain amount of Al, Cu element and rare earth element nd, the impact of more this double factor of Ga contents, therefore the existing skills of Jing
After single HDDR in art is processed, coercivity iHc is obtained up to the magnetic of 16.4kOe.Embodiment 12 is on the basis of comparative example 5
Upper to add second HDDR process for implementing the present invention, as a result the coercivity iHc of obtained magnetic is big by original 16.4kOe
Width is improved to 20.4kOe.
Present inventor had found by the analysis to embodiment 12, and after second HDDR is processed, magnetic is rectified
Why stupid power is significantly lifted, and is primarily due to following two factors：First factor is that second HDDR processes further
Magnetic crystal grain has been refined, therefore coercivity is enhanced；Second factor is, during second HDDR process is implemented,
With there occurs grain boundary decision heat treatment, i.e., element al, Cu, Ga and Nd more than needed enter grain boundary by thermal diffusion, make
Crystal grain is isolated from one another, reduces intercrystalline magneto-coupling effect, so that the coercivity of magnetic is further improved.
It should be strongly noted that in actual batch production process, the rare-earth iron-boron system that the present invention is provided is respectively to different
Property magnetic preparation method has further the advantage that：
(1) adopted with Aichi, Janpan Zhi Gang Co., Ltd. in prior art " single HDDR processs+grain boundary decision it is hot at
Reason " method is compared, and the magnetic obtained by the embodiment of the present invention is suitable therewith in terms of magnetic property, but the Rare-earth Iron that the present invention is provided
Boron system anisotropic magnetic powder, preparation method thereof can save many intermediate links, for example：Single HDDR process after cooling, discharging,
Batch mixing, charging, the link such as intensification, therefore rare-earth iron-boron system anisotropic magnetic powder, preparation method thereof provided by the present invention again have
Process time is short, it is simple to operate the features such as, be very suitable for expeditiously being produced in batches.
(2) " more Nd, Al element of raw alloy addition adopted with Japanese Toda Kogyo Corp. in prior art
+ prolonged single HDDR process " method is compared, prepared by the rare-earth iron-boron system anisotropic magnet powder that the embodiment of the present invention is provided
On time cost therewith quite, the magnetic obtained by the embodiment of the present invention is slightly below Japanese family field to method in coercivity index
The magnetic that Industrial Co., Ltd is produced, but the magnetic obtained by the embodiment of the present invention has on remanent magnetism and maximum magnetic energy product index
Have a clear superiority.
As fully visible, the embodiment of the present invention can simply, efficiently at low cost mass-produce the Rare-earth Iron of high-coercive force
Boron system anisotropic magnet powder, not only greatly improved the coercivity of rare-earth iron-boron system anisotropic magnet powder, and will not significantly increase
Plus magnetic cost, the remanent magnetism and maximum magnetic energy product that will not also make magnetic declines to a great extent, with good popularization in industrial production
Using value.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art the invention discloses technical scope in, the change or replacement that can be readily occurred in,
All should be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be defined.
Claims (8)
1. a kind of preparation method of rare-earth iron-boron system anisotropic magnet powder, including to rare-earth iron-boron alloy particle HDDR process is carried out
The step of, it is characterised in that also comprise the steps：Rare-earth iron-boron alloy particle after HDDR is processed at least is carried out again
HDDR process, so as to obtain the rare-earth iron-boron system anisotropic magnet powder of high-coercive force；
Wherein, it is described the step of HDDR is processed is carried out to rare-earth iron-boron alloy particle to include：
Step b1, suction hydrogen-disproportionation stage：Rare-earth iron-boron alloy particle is inserted in HDDR stoves, and in vacuum or inert gas ring
760～860 DEG C are heated under border, then hydrogen is passed through into HDDR stoves, make the Hydrogen Vapor Pressure in HDDR stoves maintain 20～
100kPa, heat-insulation pressure keeping 0.5～4 hour, so as to the process for completing to inhale hydrogen-disproportionation stage；
Step b2, slow desorption-in conjunction with the stage：Inhaling hydrogen-after the completion of the disproportionation stage, the temperature in HDDR stoves is promoted to
800～900 DEG C, and make the Hydrogen Vapor Pressure in HDDR stoves be adjusted to 1～10kPa, heat-insulation pressure keeping 15～180 minutes, so as to complete
Slow desorption-in conjunction with the process in stage；
Wherein, it is described the rare-earth iron-boron alloy particle after HDDR is processed at least is carried out again a HDDR process include as
Lower step：
Step c1, second HDDR inhale hydrogen-disproportionation stage in processing：Rare-earth iron-boron alloy particle after HDDR is processed is put
In entering HDDR stoves, and 760～860 DEG C are heated under vacuum or inert gas environment, are then passed through hydrogen into HDDR stoves, made
Hydrogen Vapor Pressure in HDDR stoves maintains 20～100kPa, heat-insulation pressure keeping 15 minutes, so as to complete to inhale the place in hydrogen-disproportionation stage
Reason；
Step c2, second HDDR process in slow desorption-in conjunction with the stage：Hydrogen-after the completion of the disproportionation stage is being inhaled, by HDDR stoves
Interior temperature is promoted to 800～900 DEG C, and makes the Hydrogen Vapor Pressure in HDDR stoves be adjusted to 1～10kPa, heat-insulation pressure keeping 15～60
Minute, so as to complete slow desorption-in conjunction with the process in stage；
Step c3, second HDDR complete dehydrogenation stage in processing：After the completion of slow desorption-in conjunction with the stage, HDDR stoves are made
Interior temperature maintains 800～900 DEG C, and carries out the vacuum pumping of 15～120 minutes, then makes the fast prompt drop of HDDR in-furnace temperatures
Temperature, so as to complete the process of dehydrogenation stage completely during second HDDR is processed, obtains the Rare-earth Iron of high-coercive force to less than 50 DEG C
Boron system anisotropic magnet powder.
2. preparation method according to claim 1, it is characterised in that described carries out HDDR to rare-earth iron-boron alloy particle
The step of process, also includes：
Step b3, complete dehydrogenation stage：After the completion of slow desorption-in conjunction with the stage, the temperature in HDDR stoves is set to maintain 800
～900 DEG C, and the vacuum pumping of 15～120 minutes is carried out, so as to complete the process of complete dehydrogenation stage.
3. preparation method according to claim 1, it is characterised in that described rare-earth iron-boron alloy particle is by following step
It is rapid to be obtained：
Step a1, according to the chemical general formula R of rare-earth iron-boron system magneticxT1-x-y-zByMzDispensing is carried out, and makes rare-earth iron-boron alloy
Ingot casting or rare-earth iron-boron alloy rapid-hardening flake；
In chemical general formula, R is at least one in Nd, Pr, La, Ce, Dy or Tb this several element；This is several for Fe, Co or Ni for T
At least one in element；M is at least one in Ga, Nb, Zr, Cu, Al, V, Ti, Mo, Si or Mn this several element；x、y、z
Represent that R, B, M account for overall percetage by weight respectively, and meet following condition：27.0wt.%≤x≤31.5wt.%,
0.9wt.%≤y≤1.1wt.%, 0.1wt.%≤z≤3.0wt.%；1-x-y-z represent that in addition to R, B, M, surplus is T；
Step a2, the heat treatment that homogenizes is carried out to rare-earth iron-boron alloy ingot casting or rare-earth iron-boron alloy rapid-hardening flake；
Step a3, the broken place of hydrogen is carried out to the rare-earth iron-boron alloy ingot casting or rare-earth iron-boron alloy rapid-hardening flake after the heat treatment that homogenizes
Reason, obtains rare-earth iron-boron alloy particle.
4. preparation method according to claim 3, it is characterised in that described x, y, z meets following condition：
27.5wt.%≤x≤30.0wt.%, 0.95wt.%≤y≤1.05wt.%, 0.3wt.%≤z≤1.5wt.%.
5. preparation method according to claim 3, it is characterised in that described to rare-earth iron-boron alloy ingot casting or rare-earth iron-boron
The heat treatment that carries out homogenizing of alloy rapid-hardening flake includes：Rare-earth iron-boron alloy ingot casting or rare-earth iron-boron alloy rapid-hardening flake are placed in very
In empty or inert gas, and 5～40 hours are incubated at 1050～1160 DEG C, so as to complete the heat treatment that homogenizes.
6. preparation method according to claim 3, it is characterised in that described to the rare-earth iron-boron after the heat treatment that homogenizes
Alloy cast ingot or rare-earth iron-boron alloy rapid-hardening flake carry out hydrogen break process to be included：Initial temperature is set as 200～300 DEG C, inhales hydrogen
Process carries out 0.5～3 hour.
7. preparation method according to any one of claim 1 to 6, it is characterised in that also comprise the steps：
Finely divided process is carried out to the rare-earth iron-boron system anisotropic magnet powder of high-coercive force, rare-earth iron-boron system anisotropic magnet powder is made
Granularity be less than 180 μm, so as to obtain the rare-earth iron-boron system anisotropic magnet powder of easy magnetization, high-coercive force.
8. a kind of rare-earth iron-boron system anisotropic magnet powder, it is characterised in that using any one of the claims 1 to 7
The preparation method of rare-earth iron-boron system anisotropic magnet powder be prepared from.
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