CN104505206B - A kind of preparation method and product of high-coercive force sintered NdFeB - Google Patents
A kind of preparation method and product of high-coercive force sintered NdFeB Download PDFInfo
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- CN104505206B CN104505206B CN201410736135.4A CN201410736135A CN104505206B CN 104505206 B CN104505206 B CN 104505206B CN 201410736135 A CN201410736135 A CN 201410736135A CN 104505206 B CN104505206 B CN 104505206B
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Abstract
The invention discloses a kind of preparation methods of high-coercive force sintered NdFeB, including:Prepare main-phase alloy powder and crystal-boundary phase alloy powder;Crystal-boundary phase alloy powder and main-phase alloy powder will be prepared in protecting medium, protected and be uniformly mixed with nitrogen or argon gas;The mass percent that crystal-boundary phase alloy powder is added is 0.1~10%;The alloy powder that mixing is completed is carried out to be orientated die mould and isostatic cool pressing;In vacuum sintering furnace, the magnetic patch that die mould is completed is sintered 2~4h at 1000~1100 DEG C, 2~4h and 450~650 DEG C of 2~4h of second annealing is tempered using 800~950 DEG C of level-ones, sintered NdFeB is made.The invention also discloses a kind of high-coercive force sintered NdFeBs.The present invention reduces the wetting temperature between Grain-Boundary Phase and main phase by the auxiliary alloy of low melting point, extends wetting time, improves heavy rare earth utilization rate, reduces rare earth usage amount, and simple for process, and cost is relatively low, is suitble to large-scale production.
Description
Technical field
The invention belongs to permanent-magnet material technical fields, and in particular to a kind of preparation method of high-coercive force sintered NdFeB and
Product.
Background technology
True benevolence in assistant river of nineteen eighty-three Japan et al. uses on the basis of to RE-Fe-X ternary alloy three-partalloys study extensively
Powder metallurgical technique prepares magnetic energy product and is up to 290kJ/m3Neodymium iron boron (Nd-Fe-B) sintered magnet, it is dilute to have started the third generation
Native permanent-magnet material.Sintered Nd-Fe-B is widely used in military industry equipment, electro-acoustic element, motor, generator, hard disc of computer and drives
Dynamic device (HDD), voice coil motor (VCM), human body NMR imaging instrument (MRI), short-wave communication tedhnology, controller, instrument, magnetic point
From equipment, magnetic card disk and other need to use permanent-magnetic field device and equipment in.
Sintered NdFeB magnet is with Nd2Fe14B compounds are main phase, are around coated with the structure of Nd-rich phase.It is main
Technical indicator include remanent magnetism Br, maximum magnetic energy product (BH)max, coercivity Hcj, Curie temperature Tc.It is sent out by 20 years of researches
Exhibition has devised rational alloying component and ripe preparation process, makes the remanent magnetism B of magnetrReached the 96% of theoretical value with
On, magnetic energy product can reach 474kJ/m3, approached theoretical magnetic energy product 512kJ/m393%.Although coercivity has obtained one
The promotion of given layer degree, but for its theoretical value 5600kA/m, still there is prodigious gap, the water that can reach at present
Flat is probably the 1/10~1/3 of its coercivity theoretical value.Neodymium iron boron magnetic body is thus greatly limited in high operating temperature
It is applied under environment.In order to solve this problem, scientific worker has been engaged in a large amount of research, includes mainly heavy rare earth alloy,
The coercivity of raising magnet that in this way can be easily and effectively, still, since heavy rare earth atom is coupled with the anti-ferromagnetism of iron atom,
The indexs such as the remanent magnetism of magnet and maximum magnetic energy product can substantially reduce, in addition, traditional DIRECT ALLOYING, needs more to weigh dilute
Soil, it is however generally that need to add 2~10% heavy rare earth of mass fraction, can also improve the production cost of magnet.Current domestic and international one
A little enterprises and R&D institution, the method for using magnet surface diffusion can have on the basis of improve coercitive in effect, reduce
Heavy rare earth dosage.But this method, complex technical process, be not suitable for actual production, heavy rare earth diffusion length it is limited (<5 μm),
, unsuitable actual application market too small for the magnet size of diffusion is allowed in this way.
Invention content
The present invention provides a kind of reduction heavy rare earth dosages, improve the coercitive method of Sintered NdFeB magnet.
The present invention also provides a kind of Sintered NdFeB magnet being prepared by the above method, coercivity is higher.
A kind of preparation method of high-coercive force sintered NdFeB, including:
(1) ingot casting or rapid casting is made using casting technique or rapid hardening belt-rejecting technology in main phase Nd Fe B alloys, then passes through
Main phase ingot casting or rapid casting are crushed by the quick-fried method with airflow milling of hydrogen is made the master alloying that average particle diameter is 2-10 μm
Grain powder, for the master alloying with atomic percentage, ingredient is (NdaPr1-a)bFe100-b-c-dBcMd;
Wherein:Nd is neodymium element, and Pr is praseodymium element, and Fe is ferro element, and B is boron element, and M is Dy (dysprosium), Tb (terbium), Ce
(cerium), Co (cobalt), Ni (nickel), V (vanadium), Ti (thallium), Mo (molybdenum), Mn (manganese), Ga (gallium), Al (aluminium), Cu (copper), Zr (zirconium), Ta
One or more of (tantalum), Ag (silver), Si (silicon), Nb (niobium) element;A, b, c, d meet following relationship:0.7≤a≤1,10
≤ b≤20,5.5≤c≤6.5,0≤d≤2.
Wherein, M is more preferably the combination of Dy, Al and Nb or the combination of Al, Co, Cu, Zr and Ga.Main phase neodymium iron boron
Alloy is still more preferably:(Pr,Nd)13.62FebalM1.58B5.98, wherein M=Al, Co, Cu, Zr, Ga;Or (Pr,
Nd)13.05Dy0.12FebalAl0.25Nb0.07B5.7;
Wherein, preferably, a, b, c, d meet following relationship:A=0.8,13.05≤b≤13.62,5.7≤c≤
5.98,0.44≤d≤1.58;
The average particle diameter of the master alloying particle powder is more preferably 2-5 μm, is still more preferably 3-4 μ
m;
(2) Grain-Boundary Phase richness heavy rare earth alloy end uses melting, rapid hardening to get rid of band, and Mechanical Crushing protects medium ball milling or straight
It is 0.1~2 μm of crystal-boundary phase alloy powder to connect atomization and be prepared into average particle diameter, and the crystal-boundary phase alloy is with atomic percent
Meter, ingredient are (RxR’1-x)yM’100-y;
Wherein:R is La (lanthanum), one or more of Ce, Pr, Nd, and R ' is one or more of Tb, Dy, Ho (holmium),
M ' is Fe, Cr (chromium), Co, Ni, V, Ti, Mo, Mn, Ga, Al, Cu, Zr, Ta, Ag, Si, Ca, B, Mg, Zn, In (indium), Sn elements
One or more of;Wherein x, y meet following relationship:0≦x<1,0<y<100;
The wherein described R is preferably Pr;The R ' is preferably Dy;The M ' is preferably one or more in Fe, Cu, Co;
Described x, y further meet following relationship:0≦x<0.6,20<y<70;The crystal-boundary phase alloy is preferably Pr37Dy30Cu33、
Dy32.5Fe62Cu5.5、Dy6Co13Cu5;
In step (1) and step (2), further preferred main phase Nd Fe B alloys, crystal-boundary phase alloy are combined as:
(Pr0.2Nd0.8)13.62Fe78.82M1.58B5.98With Pr37Dy30Cu33Combination;
Or (Pr0.2Nd0.8)13.05Dy0.12Fe80.81Al0.25Nb0.07B5.7With Dy32.5Fe62Cu5.5Combination;
Or (Pr0.2Nd0.8)13.62FebalM1.58B5.98With Dy6Co13Cu5Combination.
Especially with (Pr0.2Nd0.8)13.62FebalM1.58B5.98With Dy6Co13Cu5Combination when, obtained sintering neodymium iron
The coercivity of boron magnet is up to 1629.0kA/m;
The average particle diameter of the crystal-boundary phase alloy is preferably 0.1~1.5 μm, is still more preferably 0.8~1.5 μ
m;
(3) will prepare crystal-boundary phase alloy powder and main phase Nd Fe B alloys powder with mass fraction be 0.1~10%,
The batch mixer that gasoline, petroleum ether are either protected in other organic protection media with nitrogen or argon gas is sufficiently mixed uniformly;
In the step, the mass percent of crystal-boundary phase alloy powder addition is preferably 1~5%, further preferably 2~
3%;
(4) alloy powder that mixing is completed is subjected to orientation die mould under the magnetic field of 1.2~3.0T;The magnetic that die mould is completed
Block carries out the isostatic cool pressing of 100~220MPa, its die mould is made to become green compact;
The whereabouts die mould preferably carries out under the conditions of 1.8T;The isostatic cool pressing is carried out at 200MPa;
(5) in vacuum sintering furnace, the magnetic patch that die mould is completed is sintered 2~4h at 1000~1100 DEG C, using 800~
950 DEG C of level-ones are tempered 2~4h and 450~650 DEG C of 2~4h of second annealing, and final magnet is made;
Further preferred sintering condition is in the step:1050~1090 DEG C of 3~4h of sintering, using 890~900 DEG C
Level-one is tempered 2~3h and 500~520 DEG C of 2~4h of second annealing.Further preferred sintering condition is:1050~1085 DEG C of burnings
3~4h of knot is tempered 2h and 500~520 DEG C of 3~4h of second annealing, at the sintering condition using 890~900 DEG C of level-ones
The coercivity for managing obtained Sintered NdFeB magnet is more than 1400kA/m;3h is especially sintered at 1050 DEG C, using 890 DEG C of level-ones
After 2h and 520 DEG C of second annealing 3h processing of tempering, coercivity is more than 1600kA/m.
Magnetics parameter of the coercivity as a structure sensitive, it is considered that, tiny and uniform main phase particle surface packet
It is thick to cover one layer of 2~5nm, uniform and continuous Nd-rich phase is the ideal microstructure knot of high-coercive force Sintered NdFeB magnet
Structure.The present invention adds low melting point heavy rare earth alloy in crystal boundary, advanced optimizes grain boundary structure, eliminates grain boundary defects, in sintering and
During tempering heat treatment, heavy rare earth is spread to main phase grain boundary layer, realizes boundary magnetic hardening;Low melting point is added by crystal boundary
Rich heavy rare earth crystal-boundary phase alloy reduces the wetting temperature between main phase and Grain-Boundary Phase, extends wetting time, can correspondingly reduce
Sintering and heat treatment temperature inhibit the abnormal growth of solid-phase sintering and crystal grain.To realize do not added in main-phase alloy or
Under conditions of a small amount of addition heavy rare earth, heavy rare earth dosage is reduced, prepares inexpensive high-coercive force Sintered NdFeB magnet.
The present invention also provides a kind of high-coercive force sintered NdFeB, the sintered NdFeB is by any of the above-described technical solution institute
The preparation method for the high-coercive force sintered NdFeB stated is prepared.
The present invention in the sintering and heat treatment process of magnet, passes through eutectic using low melting point richness heavy rare earth crystal-boundary phase alloy
The auxiliary alloy of point reduces the wetting temperature between Grain-Boundary Phase and main phase, extends wetting time, improves heavy rare earth utilization rate;Pass through eutectic
Point Grain-Boundary Phase, improves crystal boundary mobility, reduces sintering and heat treatment temperature, optimizes grain boundary structure, reduces grain boundary defects, inhibits anti-
Magnetize forming core;It is spread to main phase boundary layer by heavy rare earth, realizes the magnetic hardening on main phase grain boundary.Initially is being free of or is containing
In the master alloying of a small amount of heavy rare earth, only crystal boundary adds a small amount of low melting point richness heavy rare earth alloy, keeps remanent magnetism, increases substantially coercive
Power realizes that one of heavy rare earth efficiently utilizes.Method provided by the invention, simple for process, cost is relatively low, is suitble to extensive raw
Production.
Compared with prior art, the present invention having the advantage that:
1) present invention design low melting point richness heavy rare earth Grain-Boundary Phase, optimizes the wet processes of liquid sintering process, extends wetting
Time improves heavy rare earth toward the diffuser efficiency in main phase boundary layer, realizes the efficient utilization of grain boundary magnetic hardening and heavy rare earth.
2) improve grain boundary structure, eliminate grain boundary defects, reduce sintering and heat treatment temperature, inhibit the abnormal growth of crystal grain,
Improve coercivity.
3) preparation process provided by the invention is simple, and heavy rare earth dosage is relatively low, and coercivity is higher, really realize it is low at
The preparation of this high-coercive force sintered NdFeB.
Specific implementation mode
A kind of preparation method of high-coercive force low cost sintered NdFeB, described in main phase Nd Fe B alloys with atom hundred
Divide than meter, ingredient is (NdaPr1-a)bFe100-b-c-dBcMd, wherein Nd is neodymium element, and Pr is praseodymium element, and Fe is ferro element, and B is
Boron element, M Dy, one kind in Tb, Ce, Co, Ni, V, Ti, Mo, Mn, Ga, Al, Cu, Zr, Ta, Ag, Si, Nb element or several
Kind;A, b, c, d meet following relationship:0.7≤a≤1,10≤b≤20,5.5≤c≤6.5,0≤d≤2.
For crystal-boundary phase alloy with atomic percentage, ingredient is (RxR’1-x)yM’100-y, one in R La, Ce, Pr, Nd
Kind or it is several, R ' is one or more of Tb, Dy, Ho, M ' is Fe, Cr, Co, Ni, V, Ti, Mo, Mn, Ga, Al, Cu, Zr,
One or more of Ta, Ag, Si, Ca, B, Mg, Zn, In, Sn element;Wherein x, y meet following relationship:0≦x<1,0<y<
100。
A kind of preparation method of high-coercive force low cost sintered NdFeB, the crystal boundary richness heavy rare earth alloy, fusing point
Between 300~900 DEG C, after powder particle is made, size is between 0.1~1 μm.
A kind of high-coercive force low-cost sintered neodymium iron boron preparation method, the rich heavy rare earth crystal-boundary phase alloy of low melting point,
During sintering and tempering heat treatment, heavy rare earth is spread to main phase grain boundary layer, realizes boundary magnetic hardening;Utilize low melting point
Crystal-boundary phase alloy extends wetting time, improves Grain-Boundary Phase mobility, optimizes grain boundary structure, reduces grain boundary defects;Added by crystal boundary
Add low melting point richness heavy rare earth crystal-boundary phase alloy, reduce sintering and heat treatment temperature, inhibits the abnormal growth of solid-phase sintering and crystal grain.
Under conditions of not added in main-phase alloy or add heavy rare earth on a small quantity, crystal boundary addition, reduce heavy rare earth dosage, prepare it is low at
This high-coercive force Sintered NdFeB magnet.
A kind of preparation method of high-coercive force low cost sintered NdFeB, its steps are:
1) ingot casting or rapid casting is made using casting technique or rapid hardening belt-rejecting technology in main phase Nd Fe B alloys, then passes through hydrogen
Main phase ingot casting or rapid casting are crushed by the quick-fried method with airflow milling is made the particle powder that average particle diameter is 2~10 μm,
For the master alloying with atomic percentage, ingredient is (NdaPr1-a)bFe100-b-c-dBcMd;
2) Grain-Boundary Phase richness heavy rare earth alloy end uses melting, rapid hardening to get rid of band, and Mechanical Crushing protects medium ball milling or direct
It is 0.1~1 μm of powder that atomization, which is prepared into average particle diameter, and the crystal-boundary phase alloy is with atomic percentage, ingredient
(RxR’1-x)yM’100-y;
3) crystal-boundary phase alloy powder and master alloying powder will be prepared with mass fraction for 0.1~10%, in gasoline, oil
The batch mixer that ether is either protected in other organic protection media with nitrogen or argon gas is sufficiently mixed uniformly;
4) alloy powder that mixing is completed is subjected to orientation die mould under the magnetic field of 1.2~3.0T;The magnetic that die mould is completed
Block carries out the isostatic cool pressing of 100~220MPa, its die mould is made to become green compact;
5) in vacuum sintering furnace, the magnetic patch that die mould is completed is sintered 2~4h at 1000~1100 DEG C, using 800~
950 DEG C of level-ones are tempered 2~4h and 450~650 DEG C of 2~4h of second annealing, and final magnet is made.The present invention and prior art phase
Than having the advantage that:1) present invention design low melting point richness heavy rare earth Grain-Boundary Phase, optimizes the wetting of liquid sintering process
Journey extends wetting time, improves heavy rare earth toward the diffuser efficiency in main phase boundary layer, realizes grain boundary magnetic hardening and heavy rare earth
Efficiently utilize.2) improve grain boundary structure, eliminate grain boundary defects, reduce sintering and heat treatment temperature, inhibit the abnormal growth of crystal grain,
Improve coercivity.3) preparation process provided by the invention is simple, and heavy rare earth dosage is relatively low, and coercivity is really realized height
The preparation of inexpensive high-coercive force sintered NdFeB.
With reference to specific example, the present invention will be further described, but the present invention is not limited solely to following instance.
Embodiment 1:
1) it uses rapid hardening slab, hydrogen quick-fried main-phase alloy and three kinds of alloying technologys of airflow milling prepares master alloying powder, powder
Last particle diameter is substantially at 3.5 μm or so, and for the master alloying in terms of atomic percentage, ingredient is (Pr0.2Nd0.8)13.62Fe78.82M1.58B5.98, wherein Pr:Nd=1:4, M Al=0.72, Co=0.49, Cu=0.14, Zr=0.14, Ga=
0.09;
2) crystal-boundary phase alloy is by electric arc melting, and Mechanical Crushing, it is about 0.85 μ that protection medium, which is milled to average grain size,
M, auxiliary alloy is in terms of atomic percentage, ingredient Pr37Dy30Cu33;
3) crystal-boundary phase alloy powder and master alloying powder will be prepared in gasoline, petroleum ether or other organic protection media
In, the batch mixer protected with nitrogen or argon gas is sufficiently mixed uniformly, wherein mass fraction shared by auxiliary alloy powder is 2.0%;
4) alloy powder that mixing is completed is subjected to orientation die mould under the magnetic field of 1.8T;The magnetic patch that die mould is completed carries out
The isostatic cool pressing of 200MPa makes its die mould become green compact;
5) in vacuum sintering furnace, the magnetic patch that die mould is completed is sintered 4h at 1085 DEG C, 2h is tempered using 900 DEG C of level-ones
With 500 DEG C of second annealing 4h, final magnet is made.
The Sintered NdFeB magnet prepared is put into VSM and measures its magnetic property, it is as a result as follows:Br=1.35T, Hcj=
1450.2kA/m,(BH)max=351.75kJ/m3。
Embodiment 2:
1) it uses rapid hardening slab, hydrogen quick-fried main-phase alloy and three kinds of alloying technologys of airflow milling prepares master alloying powder, powder
Last particle diameter is substantially at 3.5 μm or so, and for the master alloying in terms of atomic percentage, ingredient is (Pr0.2Nd0.8)13.05Dy0.12Fe80.81Al0.25Nb0.07B5.7
2) crystal-boundary phase alloy is by electric arc melting, and Mechanical Crushing, it is about 1.5 μ that protection medium, which is milled to average grain size,
M, auxiliary alloy are calculated in mass percent, ingredient Dy32.5Fe62Cu5.5。
3) crystal-boundary phase alloy powder and master alloying powder will be prepared in gasoline, petroleum ether or other organic protection media
In, the batch mixer protected with nitrogen or argon gas is sufficiently mixed uniformly, wherein mass fraction shared by auxiliary alloy powder is 3.0%:
4) alloy powder that mixing is completed is subjected to orientation die mould under the magnetic field of 1.8T;The magnetic patch that die mould is completed carries out
The isostatic cool pressing of 200MPa makes its die mould become green compact;
5) in vacuum sintering furnace, the magnetic patch that die mould is completed is sintered 4h at 1090 DEG C, 2h is tempered using 890 DEG C of level-ones
With 520 DEG C of second annealing 3.5h, final magnet is made.
The Sintered NdFeB magnet prepared is put into VSM and measures its magnetic property, it is as a result as follows:Br=1.35T, Hcj=
1329.0kA/m,(BH)max=369.71kJ/m3。
Embodiment 3:
1) it uses rapid hardening slab, hydrogen quick-fried main-phase alloy and three kinds of alloying technologys of airflow milling prepares master alloying powder, powder
Last particle diameter is substantially at 3.5 μm or so, and for the master alloying in terms of atomic percentage, ingredient is (Pr0.2Nd0.8)13.62FebalM1.58B5.98, wherein M is Al=0.72, Co=0.49, Cu=0.14, Zr=0.14, Ga=0.09;
2) crystal-boundary phase alloy is by electric arc melting, and Mechanical Crushing, it is about 1.3 μ that protection medium, which is milled to average grain size,
M. the auxiliary alloy is in terms of atomic percentage, ingredient Dy6Co13Cu5。
3) crystal-boundary phase alloy powder and master alloying powder will be prepared in gasoline, petroleum ether or other organic protection media
In, the batch mixer protected with nitrogen or argon gas is sufficiently mixed uniformly, wherein mass fraction shared by auxiliary alloy powder is 3.0%:
4) alloy powder that mixing is completed is subjected to orientation die mould under the magnetic field of 1.8T;The magnetic patch that die mould is completed carries out
The isostatic cool pressing of 200MPa makes its die mould become green compact;
5) in vacuum sintering furnace, the magnetic patch that die mould is completed is sintered 3h at 1050 DEG C, 2h is tempered using 890 DEG C of level-ones
With 520 DEG C of second annealing 3h, final magnet is made.
The Sintered NdFeB magnet prepared is put into VSM and measures its magnetic property, it is as a result as follows:Br=1.38T, Hcj=
1629.0kA/m,(BH)max=398.63kJ/m3。
Claims (1)
1. a kind of preparation method of high-coercive force sintered NdFeB, which is characterized in that including:
(1)The main-phase alloy powder that average particle diameter is 2-5 μm is prepared using main-phase alloy, the main-phase alloy is with atom hundred
Divide than meter, ingredient is (Pr0.2Nd0.8)13.62Fe78.82M1.58B5.98;
Wherein:The M is the combination of Al, Co, Cu, Zr and Ga;
(2)It is 0.1 ~ 1.5 μm of crystal-boundary phase alloy powder, the crystal-boundary phase alloy to prepare average particle diameter using crystal-boundary phase alloy
With atomic percentage, ingredient Pr37Dy30Cu33;
(3)Crystal-boundary phase alloy powder and main-phase alloy powder will be prepared in gasoline or petroleum ether, protected with nitrogen or argon gas
Shield is uniformly mixed;The mass percent that crystal-boundary phase alloy powder is added is 1 ~ 5%;
(4)The alloy powder that mixing is completed is subjected to orientation die mould under the magnetic field of 1.8T;The magnetic patch that die mould is completed carries out
The isostatic cool pressing of 200MPa makes its die mould become green compact;
(5)In vacuum sintering furnace, the magnetic patch that die mould is completed is sintered 3 ~ 4h at 1050 ~ 1090 °C, using 890 ~ 900 °C one
Grade 2 ~ 3h and 500 ~ 520 °C of 2 ~ 4h of second annealing of tempering, is made final Sintered NdFeB magnet.
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CN113674945B (en) * | 2021-06-11 | 2023-06-27 | 烟台正海磁性材料股份有限公司 | Low-cost high-coercivity LaCe-rich neodymium-iron-boron permanent magnet and preparation method and application thereof |
CN113517125B (en) * | 2021-07-12 | 2023-05-05 | 安徽大地熊新材料股份有限公司 | High-stability sintered NdFeB magnet and preparation method thereof |
CN113643870A (en) * | 2021-07-30 | 2021-11-12 | 宁波中杭磁材有限公司 | High-performance cerium-iron-boron magnet and preparation method thereof |
CN114005633B (en) * | 2021-10-21 | 2022-11-15 | 钢铁研究总院 | Rare earth soft magnetic material with multi-shell structure and preparation method thereof |
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WO2012102497A2 (en) * | 2011-01-25 | 2012-08-02 | Industry-University Cooperation Foundation, Hanyang University | R-fe-b sintered magnet with enhanced mechanical properties and method for producing the same |
CN103426578B (en) * | 2012-05-22 | 2016-04-27 | 比亚迪股份有限公司 | A kind of rare earth permanent-magnetic material and preparation method thereof |
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