CN103537684A - Production method for samarium cobalt alloy powder - Google Patents
Production method for samarium cobalt alloy powder Download PDFInfo
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Abstract
The invention discloses a production method for samarium cobalt alloy powder. The production method for the samarium cobalt alloy powder comprises weighing samarium, cobalt, iron, copper, zirconium and heavy rare earth element metal salt in proportion, preparing a salt solution and a salt-mixture solution, adding a little acid or alkali to control a PH (Potential of Hydrogen) value to be between 4 and 9, simultaneously adding surface active agent and dispersing agent which account 1 to 5 % of the mass of the metal salt in the metal salt solution, performing spray drying at the temperature between 300 and 350 DEG C to produce composite powder precursor, performing low temperature calcine at the temperature between 200 and 300 DEG C, performing two-step restoring on the precursor under hydrogen atmosphere with the temperature between 400 to 800 DEG C, ball-milling the restored powder to obtain the samarium cobalt alloy powder. The samarium cobalt alloy powder produced through the production method has the advantages of being reasonable in powder size, uniform in crystal grain and component distribution, high in purity and low in oxygen content. The production method has the advantages of being simple in operation, low in energy consumption, high in production efficiency and suitable for continuous production.
Description
Technical field
The present invention relates to rare earth permanent-magnetic material preparation method, be specifically related to a kind of preparation method of samarium-cobalt alloy powder.
Background technology
Samarium cobalt permanent magnet alloy is a kind of high temperature permanent magnetic material of excellent performance, because of its Curie temperature high (higher than 820 ℃), temperature stability is good, corrosion resistance is strong and the advantage such as good in oxidation resistance has the effect of not replacing in permanent-magnet material.This material is widely used in fields such as microwave communication technology, audio-visual technology, electrical engineering, instrumental technique, computing technique, automatic technology, communications and transportation, petrochemical industry, magnetization technology, magnetic separation technique, bioengineering and magnetic medical treatment and health and fitness facilitieses.
The method that tradition is prepared samarium-cobalt alloy powder is the pure element metal that adopts samarium, cobalt, iron, copper, zirconium and rare earth, in vacuum induction melting furnace, carries out high melt, then high temperature solution is carried out to chilling and obtains alloy cast ingot.Conventional method relates in a lot of patents, and as 200910080120.6,201110457035.4, samarium-cobalt alloy powder prepared by this method has following shortcoming: need to consume a large amount of electric energy, in order to prevent the oxidation of fusion process Raw, need pumping high vacuum; For reducing the volatilization loss of alloying element in high melt process; want applying argon gas protection; and alloy cast ingot could take out after cooling; cause that alloy cast ingot prepares that energy consumption is high, complicated operation, cycle are long, have potential safety hazard; because smelting temperature is high; it is inhomogeneous that ingot casting easily produces component segregation, coarse grains, Grain size distribution in condensation process, cause the decline of samarium-cobalt alloy performance, and the crystal grain of alloy powder and homogeneity of ingredients is the key of preparation high-performance samarium-cobalt permanent-magnetic material.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art, and a kind of preparation method of samarium-cobalt alloy powder is provided.
In order to reach above-mentioned technical purpose, technical scheme provided by the invention is:
A preparation method for samarium-cobalt alloy powder, described samarium-cobalt alloy powder is comprised of the element of following mass percentage content: samarium 24.5%~26%, cobalt 52%~56%, iron 7.5%~12%, copper 6.5%~8%, zirconium 2%~4%, heavy rare earth element 0.5%~1%; Described method comprises the steps:
(1) by above-mentioned each element, in the mass percentage content of samarium-cobalt alloy powder, take the slaine of above-mentioned each element; By the slaine of above-mentioned each element, to be mixed with respectively slaine mass percentage content be 20%~30% metal salt solution and mix, or after the slaine of above-mentioned each element is mixed, to be mixed with slaine mass percentage content be 20%~30% metal salt solution;
(2) add and account for the surfactant of slaine quality 1%~5% in metal salt solution and account for slaine quality 1%~5% dispersant; Regulating pH value is 4~9;
(3) metal salt solution of processing through step (2) is sprayed and is dried, prepare samarium-cobalt alloy powder presoma;
(4) samarium-cobalt alloy powder presoma is calcined in air under 200 ℃~300 ℃ conditions, decomposed the crystal salt in samarium-cobalt alloy powder presoma, remove unnecessary adsorbed water and the crystallization water, obtain samarium-cobalt alloy powder;
(5) the samarium-cobalt alloy powder after step (4) calcining is carried out to twice reduction in 400 ℃~800 ℃ under hydrogen atmosphere, every step recovery time is 30min~120min;
(6) the samarium-cobalt alloy powder after step (5) reduction is milled to the samarium-cobalt alloy powder of 3 μ m~5 μ m.
Wherein, described heavy rare earth element is one or more in gadolinium, dysprosium, holmium, praseodymium, er element.
The slaine of described samarium is samaric nitrate, samarium trichloride or acetic acid samarium; The slaine of described cobalt, iron, copper, zirconium is chlorate, sulfate, nitrate or the oxalates of cobalt, iron, copper, zirconium; The slaine of described heavy rare earth element is nitrate, chlorate or the acetate of heavy rare earth element.
The described surfactant of step (2) is stearic acid, polyethylene glycol, urea, N, N-dimethyl formamide or dodecyl sodium sulfate; Described dispersant is triethyl group hexyl phosphoric acid, lauryl sodium sulfate, methyl anyl alcohol, cellulose derivative, polyacrylamide, guar gum or fatty acid polyethylene glycol ester.
In step (2), by adding acid or alkali to regulate metal salt solution pH value, be 4~9, described acid is HCl, HNO
3or oxalic acid, described alkali is NaOH, KOH or ammoniacal liquor.
The described spraying drying condition of step (3) is: 300 ℃~350 ℃ of temperature, 20000~30000 revs/min of rate of dryings.
Described twice reduction of step (5) is that the composite powder after calcining is reduced for the first time in 400 ℃~550 ℃ under hydrogen atmosphere, recovery time 30min~120min; Then the powder after reduction is for the first time carried out to secondary reduction, recovery time 30min~120min at 650 ℃~800 ℃.
The inventive method has overcome heritage and has answered method of smelting to prepare the shortcoming of samarium-cobalt alloy powder, adopts be dried-calcining-hydrogen heat reduction-ball milling of solution-spraying to prepare samarium-cobalt alloy powder.
Compared with prior art, beneficial effect of the present invention is:
(1) heritage answers samarium-cobalt alloy powder prepared by method of smelting to adopt the broken preparation of the quick cooling ingot casting of copper condensation mould, it is inhomogeneous that ingot casting easily produces component segregation, coarse grains, Grain size distribution in condensation process, easily cause the decline of samarium-cobalt alloy performance, and samarium-cobalt alloy powder prepared by the present invention adopts Liquid preparation methods, alloying element reaches atom level level to be mixed, component distributing is more even, and grain size is tiny and granularity concentrated.
(2) powder adopts solwution method preparation, elder generation's low temperature calcination in air, crystal salt is decomposed, and remove unnecessary adsorbed water and the crystallization water, then two step high temperature reductions under nitrogen atmosphere, have effectively removed the impurity oxygen in powder, the alloy powder purity of preparation is high, and after hydrogen reduction, in powder, retained part hydrogen, be conducive to prevent the oxidation in the follow-up use procedure of powder.
(3) heritage is answered method of smelting to prepare samarium-cobalt alloy ingot casting and need to be consumed a large amount of electric energy, in order to prevent the oxidation of fusion process Raw, needs pumping high vacuum; For reducing the volatilization loss of alloying element in high melt process, applying argon gas protection, and alloy cast ingot could take out after cooling, cause that alloy cast ingot prepares that energy consumption is high, complicated operation, cycle grow, exist potential safety hazard.Samarium-cobalt alloy powder preparation method of the present invention adopts solwution method preparation at normal temperatures, simple to operate, energy consumption is low, the cycle is short, production efficiency is high, safe and reliable, be applicable to serialization produces.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, but is not limited in following examples.Percentage composition related in embodiment 1 to 7 is mass percentage content.
Embodiment 1
Take that to produce the alloy powder that composition is samarium 25.5%, cobalt 52%, iron 10.5%, copper 8%, zirconium 4% be example.
Take the samaric nitrate Sm (NO of 57.05g
3)
3, 256.82g cobalt nitrate Co (NO
3)
26H
2o, 75.96g ferric nitrate Fe (NO
3)
39H
2o, 30.41g copper nitrate Cu (NO
3)
23H
2o, 18.82g zirconium nitrate Zr (NO
3)
45H
2o.
(1) add distilled water in described each slaine, to be mixed with respectively the metal salt solution of metalline 30%;
(2) each metal salt solution rapid mixing is stirred, add a small amount of HNO
3stir, controlling pH value is 4~6, obtains transparent mixed solution;
(3) add surfactant stearic acid and the 5g dispersant lauryl sodium sulfate of 10g, be fully uniformly mixed, to prevent appearance precipitation in solution, make powder good dispersion;
(4) then dry 300 ℃~350 ℃ sprayings, spraying rate of drying is 20000~30000 revs/min, prepares samarium-cobalt alloy powder presoma;
(5) by presoma in air 200 ℃~300 ℃ calcinings, decompose the crystal salt in samarium-cobalt alloy powder presoma, remove unnecessary adsorbed water and the crystallization water, obtain samarium-cobalt alloy powder;
(6) the samarium-cobalt alloy powder after calcining is once reduced in 400 ℃~550 ℃ under hydrogen atmosphere, recovery time 30min~120min;
(7) the samarium-cobalt alloy powder after reduction is for the first time carried out to secondary reduction, recovery time 30min~120min at 650 ℃~800 ℃;
(8) last, the samarium-cobalt alloy powder after thermal reduction is carried out to ball milling, obtain granularity at the samarium-cobalt alloy powder of 3 μ m~5 μ m.
Embodiment 2
Take that to produce the alloy powder that composition is samarium 24.5%, cobalt 54.5%, iron 12%, copper 6.5%, zirconium 2.5% be example.
Take the samaric nitrate Sm (NO of 54.81g
3)
3, 269.17g cobalt nitrate Co (NO
3)
26H
2o, 86.81g ferric nitrate Fe (NO
3)
39H
2o, 24.71g copper nitrate Cu (NO
3)
23H
2o, 11.76g zirconium nitrate Zr (NO
3)
45H
2o.
(1) add distilled water in described each slaine, to be mixed with respectively the metal salt solution of metalline 20%;
(2) each metal salt solution rapid mixing is stirred, add a small amount of HNO
3stir, controlling pH value is 4~6, obtains transparent mixed solution;
(3) add surfactant stearic acid and the 8g dispersant lauryl sodium sulfate of 15g, to prevent occurring that precipitation makes powder good dispersion in solution;
(4) then dry 300 ℃~350 ℃ sprayings, spraying rate of drying is 20000~30000 revs/min, prepares samarium-cobalt alloy powder presoma;
(5) by presoma in air 200 ℃~300 ℃ calcinings, decompose the crystal salt in samarium-cobalt alloy powder presoma, remove unnecessary adsorbed water and the crystallization water, obtain samarium-cobalt alloy powder;
(6) the samarium-cobalt alloy powder after calcining is once reduced in 400 ℃~550 ℃ under hydrogen atmosphere, recovery time 30min~120min;
(7) the samarium-cobalt alloy powder after reduction is for the first time carried out to secondary reduction, recovery time 30min~120min at 650 ℃~800 ℃;
(8) last, the samarium-cobalt alloy powder after thermal reduction is carried out to ball milling, obtain granularity at the samarium-cobalt alloy powder of 3 μ m~5 μ m.
Embodiment 3
Take that to produce the alloy powder that composition is samarium 25.5%, cobalt 53%, iron 12%, copper 6.5%, zirconium 2.5%, praseodymium 0.5% be example.
Take the samaric nitrate Sm (NO of 57.05g
3)
3, 261.76g cobalt nitrate Co (NO
3)
26H
2o, 86.81g ferric nitrate Fe (NO
3)
39H
2o, 24.71g copper nitrate Cu (NO
3)
23H
2o, 11.76g zirconium nitrate Zr (NO
3)
45H
2o, 1.54g praseodymium nitrate Pr (NO
3)
36H
2o.
(1) add distilled water in described each slaine, to be mixed with respectively the metal salt solution of metalline 25%;
(2) each metal salt solution rapid mixing is stirred, add a small amount of HNO
3stir, controlling pH value is 4~6, obtains transparent mixed solution;
(3) add surfactant stearic acid and the 8g dispersant lauryl sodium sulfate of 15g, to prevent appearance precipitation in solution, make powder good dispersion;
(4) then dry 300 ℃~350 ℃ sprayings, spraying rate of drying is 20000~30000 revs/min, prepares samarium-cobalt alloy powder presoma;
(5) by presoma in air 200 ℃~300 ℃ calcinings, decompose the crystal salt in samarium-cobalt alloy powder presoma, remove unnecessary adsorbed water and the crystallization water, obtain samarium-cobalt alloy powder;
(6) the samarium-cobalt alloy powder after calcining is once reduced in 400 ℃~550 ℃ under hydrogen atmosphere, recovery time 30min~120min;
(7) the samarium-cobalt alloy powder after reduction is for the first time carried out to secondary reduction, recovery time 30min~120min at 650 ℃~800 ℃;
(8) last, the samarium-cobalt alloy powder after thermal reduction is carried out to ball milling, obtain granularity at the samarium-cobalt alloy powder of 3 μ m~5 μ m.
Embodiment 4
Take that to produce the alloy powder that composition is samarium 25.5%, cobalt 53%, iron 12%, copper 6.5%, zirconium 2.5%, gadolinium 0.5% be example.
Take the samaric nitrate Sm (NO of 57.05g
3)
3, 261.76g cobalt nitrate Co (NO
3)
26H
2o, 86.81g ferric nitrate Fe (NO
3)
39H
2o, 24.71g copper nitrate Cu (NO
3)
23H
2o, 11.76g zirconium nitrate Zr (NO
3)
45H
2o, 1.44g gadolinium nitrate Gd (NO
3)
36H
2o.
(1) add distilled water in described each slaine, to be mixed with respectively the metal salt solution of metalline 25%;
(2) each metal salt solution rapid mixing is stirred, add a small amount of HNO
3stir, controlling pH value is 4~6, obtains transparent mixed solution;
(3) add surfactant stearic acid and the 8g dispersant lauryl sodium sulfate of 15g, to prevent appearance precipitation in solution, make powder good dispersion;
(4) then dry 300 ℃~350 ℃ sprayings, spraying rate of drying is 20000~30000 revs/min, prepares samarium-cobalt alloy powder presoma;
(5) by presoma in air 200 ℃~300 ℃ calcinings, decompose the crystal salt in samarium-cobalt alloy powder presoma, remove unnecessary adsorbed water and the crystallization water, obtain samarium-cobalt alloy powder;
(6) the samarium-cobalt alloy powder after calcining is once reduced in 400 ℃~550 ℃ under hydrogen atmosphere, recovery time 30min~120min;
(7) the samarium-cobalt alloy powder after reduction is for the first time carried out to secondary reduction, recovery time 30min~120min at 650 ℃~800 ℃;
(8) last, the samarium-cobalt alloy powder after thermal reduction is carried out to ball milling, obtain granularity at the samarium-cobalt alloy powder of 3 μ m~5 μ m.
Embodiment 5
Take that to produce the alloy powder that composition is samarium 25.5%, cobalt 53%, iron 12%, copper 6.2%, zirconium 2.5%, dysprosium 0.8% be example.
Take the samaric nitrate Sm (NO of 57.05g
3)
3, 261.76g cobalt nitrate Co (NO
3)
26H
2o, 86.81g ferric nitrate Fe (NO
3)
39H
2o, 23.57g copper nitrate Cu (NO
3)
23H
2o, 11.76g zirconium nitrate Zr (NO
3)
45H
2o, 2.16g dysprosium nitrate D
y(NO
3)
35H
2o.
(1) add distilled water in described each slaine, to be mixed with respectively the metal salt solution of metalline 25%;
(2) each metal salt solution rapid mixing is stirred, add a small amount of HNO
3stir, controlling pH value is 4~6, obtains transparent mixed solution;
(3) add surfactant stearic acid and the 8g dispersant lauryl sodium sulfate of 15g, to prevent appearance precipitation in solution, make powder good dispersion;
(4) then dry 300 ℃~350 ℃ sprayings, spraying rate of drying is 20000~30000 revs/min, prepares samarium-cobalt alloy powder presoma;
(5) by presoma in air 200 ℃~300 ℃ calcinings, decompose the crystal salt in samarium-cobalt alloy powder presoma, remove unnecessary adsorbed water and the crystallization water, obtain samarium-cobalt alloy powder;
(6) the samarium-cobalt alloy powder after calcining is once reduced in 400 ℃~550 ℃ under hydrogen atmosphere, recovery time 30min~120min;
(7) the samarium-cobalt alloy powder after reduction is for the first time carried out to secondary reduction, recovery time 30min~120min at 650 ℃~800 ℃;
(8) last, the samarium-cobalt alloy powder after thermal reduction is carried out to ball milling, obtain granularity at the samarium-cobalt alloy powder of 3 μ m~5 μ m.
Embodiment 6
Take that to produce the alloy powder that composition is samarium 25.5%, cobalt 53%, iron 12%, copper 6.2%, zirconium 2.5%, holmium 0.8% be example.
Take the samaric nitrate Sm (NO of 57.05g
3)
3, 261.76g cobalt nitrate Co (NO
3)
26H
2o, 86.81g ferric nitrate Fe (NO
3)
39H
2o, 23.57g copper nitrate Cu (NO
3)
23H
2o, 11.76g zirconium nitrate Zr (NO
3)
45H
2o, 1.54g holmium nitrate HoNO
35H
2o.
(1) each slaine taking is mixed, add distilled water in the slaine of described mixing, be mixed with the metal salt solution of metalline 25%;
(2) in metal salt solution, add a small amount of HNO
3stir, controlling pH value is 4~6, obtains transparent mixed solution;
(3) add surfactant stearic acid and the 8g dispersant lauryl sodium sulfate of 15g, to prevent appearance precipitation in solution, make powder good dispersion;
(4) then dry 300 ℃~350 ℃ sprayings, spraying rate of drying is 20000~30000 revs/min, prepares samarium-cobalt alloy powder presoma;
(5) by presoma in air 200 ℃~300 ℃ calcinings, decompose the crystal salt in samarium-cobalt alloy powder presoma, remove unnecessary adsorbed water and the crystallization water, obtain samarium-cobalt alloy powder;
(6) the samarium-cobalt alloy powder after calcining is once reduced in 400 ℃~550 ℃ under hydrogen atmosphere, recovery time 30min~120min;
(7) the samarium-cobalt alloy powder after reduction is for the first time carried out to secondary reduction, recovery time 30min~120min at 650 ℃~800 ℃;
(8) last, the samarium-cobalt alloy powder after thermal reduction is carried out to ball milling, obtain granularity at the samarium-cobalt alloy powder of 3 μ m~5 μ m.
Embodiment 7
Take that to produce the alloy powder that composition is samarium 25.5%, cobalt 53%, iron 12%, copper 6%, zirconium 2.5%, erbium 1% be example.
Take the samaric nitrate Sm (NO of 57.05g
3)
3, 261.76g cobalt nitrate Co (NO
3)
26H
2o, 86.81g ferric nitrate Fe (NO
3)
39H
2o, 22.81g copper nitrate Cu (NO
3)
23H
2o, 11.76g zirconium nitrate Zr (NO
3)
45H
2o, 1.91g erbium nitrate ErNO
35H
2o.
(1) each slaine taking is mixed, add distilled water in the slaine of described mixing, be mixed with the metal salt solution of metalline 25%;
(2) in metal salt solution, add a small amount of HNO
3stir, controlling pH value is 4~6, obtains transparent mixed solution;
(3) add surfactant stearic acid and the 8g dispersant lauryl sodium sulfate of 15g, to prevent occurring that precipitation makes powder good dispersion in solution;
(4) then dry 300 ℃~350 ℃ sprayings, spraying rate of drying is 20000~30000 revs/min, prepares samarium-cobalt alloy powder presoma;
(5) by presoma in air 200 ℃~300 ℃ calcinings, decompose the crystal salt in samarium-cobalt alloy powder presoma, remove unnecessary adsorbed water and the crystallization water, obtain samarium-cobalt alloy powder;
(6) the samarium-cobalt alloy powder after calcining is once reduced in 400 ℃~550 ℃ under hydrogen atmosphere, recovery time 30min~120min;
(7) the samarium-cobalt alloy powder after reduction is for the first time carried out to secondary reduction, recovery time 30min~120min at 650 ℃~800 ℃;
(8) last, the samarium-cobalt alloy powder after thermal reduction is carried out to ball milling, obtain granularity at the samarium-cobalt alloy powder of 3 μ m~5 μ m.
The powder of preparation in embodiment 1 to 7 is carried out to grain size analysis, BET specific surface, morphology analysis and chemical composition analysis:
Results of grain size analysis shows, powder agglomerates particle mean size 4.3 μ m;
BET surface analysis granularity shows, BET powder size 3.6 μ m;
ESEM morphology analysis result shows powder in the form of sheets, and individual particle granularity is less than 5 μ m;
Chemical composition analysis shows that powder oxygen content is 0.1%, each element powders distributed components.
Claims (7)
1. the preparation method of a samarium-cobalt alloy powder, it is characterized in that, described samarium-cobalt alloy powder is comprised of the element of following mass percentage content: samarium 24.5%~26%, cobalt 52%~56%, iron 7.5%~12%, copper 6.5%~8%, zirconium 2%~4%, heavy rare earth element 0.5%~1%; Described method comprises the steps:
(1) by above-mentioned each element, in the mass percentage content of samarium-cobalt alloy powder, take the slaine of above-mentioned each element; By the slaine of above-mentioned each element, to be mixed with respectively slaine mass percentage content be 20%~30% metal salt solution and mix, or after the slaine of above-mentioned each element is mixed, to be mixed with slaine mass percentage content be 20%~30% metal salt solution; (2) add and account for the surfactant of slaine quality 1%~5% in metal salt solution and account for slaine quality 1%~5% dispersant; Regulating pH value is 4~9;
(3) metal salt solution of processing through step (2) is sprayed and is dried, prepare samarium-cobalt alloy powder presoma;
(4) samarium-cobalt alloy powder presoma is calcined in air under 200 ℃~300 ℃ conditions, decomposed the crystal salt in samarium-cobalt alloy powder presoma, remove unnecessary adsorbed water and the crystallization water, obtain samarium-cobalt alloy powder;
(5) the samarium-cobalt alloy powder after step (4) calcining is carried out to twice reduction in 400 ℃~800 ℃ under hydrogen atmosphere, every step recovery time is 30min~120min;
(6) the samarium-cobalt alloy powder after step (5) reduction is milled to the samarium-cobalt alloy powder of 3 μ m~5 μ m.
2. the method for claim 1, is characterized in that, described heavy rare earth element is one or more in gadolinium, dysprosium, holmium, praseodymium, er element.
3. the method for claim 1, is characterized in that, the slaine of described samarium is samaric nitrate, samarium trichloride or acetic acid samarium; The slaine of described cobalt, iron, copper, zirconium is chlorate, sulfate, nitrate or the oxalates of cobalt, iron, copper, zirconium; The slaine of described heavy rare earth element is nitrate, chlorate or the acetate of heavy rare earth element.
4. the method for claim 1, is characterized in that, the described surfactant of step (2) is stearic acid, polyethylene glycol, urea, N, N-dimethyl formamide or dodecyl sodium sulfate; Described dispersant is triethyl group hexyl phosphoric acid, lauryl sodium sulfate, methyl anyl alcohol, cellulose derivative, polyacrylamide, guar gum or fatty acid polyethylene glycol ester.
5. the method for claim 1, is characterized in that, in step (2), by adding acid or alkali to regulate metal salt solution pH value, is 4~9, and described acid is HCl, HNO
3or oxalic acid, described alkali is NaOH, KOH or ammoniacal liquor.
6. the method for claim 1, is characterized in that, the described spraying drying condition of step (3) is: 300 ℃~350 ℃ of temperature, 20000~30000 revs/min of rate of dryings.
7. the method for claim 1, is characterized in that, described twice reduction of step (5) is that the composite powder after calcining is reduced for the first time in 400 ℃~550 ℃ under hydrogen atmosphere, recovery time 30min~120min; Then the powder after reduction is for the first time carried out to secondary reduction, recovery time 30min~120min at 650 ℃~800 ℃.
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