CN106098284A - A kind of preparation method of Nd Fe B alloys ultra-fine permanent magnetism powder - Google Patents

A kind of preparation method of Nd Fe B alloys ultra-fine permanent magnetism powder Download PDF

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CN106098284A
CN106098284A CN201610656341.3A CN201610656341A CN106098284A CN 106098284 A CN106098284 A CN 106098284A CN 201610656341 A CN201610656341 A CN 201610656341A CN 106098284 A CN106098284 A CN 106098284A
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powder
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CN106098284B (en
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曹江平
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Guizhou Faraday Magnetoelectric Technology Co ltd
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JIANGSU JUXIN MAGNET CO Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/044Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by jet milling

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  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
  • Hard Magnetic Materials (AREA)

Abstract

The invention provides the preparation method of a kind of Nd Fe B alloys ultra-fine permanent magnetism powder, the preparation method of described Nd Fe B alloys ultra-fine permanent magnetism powder include successively raw material preferably, formula, vacuum melting operation, vacuum pure operation soon, vacuum crystallization and thermal treatment operation, aging process, magnetic property detection operation, airflow milling manufacturing procedure, ultrasound wave sub-sieve particle size distribution detection operation, finished product batch mixing magnetic property secondary detection operation.Beneficial effect: the magnetic powder of this preparation method is applied to anti-counterfeit field and can substantially increase electronic anti-fogery product, print the antiforge function of anti-fake product, improves added value of product.

Description

A kind of preparation method of Nd Fe B alloys ultra-fine permanent magnetism powder
Technical field
The present invention relates to magnetic composite technical field, be specifically related to the preparation of a kind of Nd Fe B alloys ultra-fine permanent magnetism powder Method.
Background technology
Along with the fast development of high-tech industry, NdFeB permanet magnetic powder be widely used in Aeronautics and Astronautics, navigation, automobile and Various precision instruments, middle-size and small-size, micro high efficiency motor, computer and IT technical equipment, business automation equipment and numerous domestic The fields such as electrical equipment, and constantly expanding.But, for height anti-fake product, the electronic information industry of commodity, identify bar code printing Industry proposes new requirement to use NdFeB permanet magnetic powder.
Summary of the invention
The present invention overcomes the deficiency of background technology to provide the preparation method of a kind of Nd Fe B alloys ultra-fine permanent magnetism powder, this The fineness of bright Nd Fe B alloys ultra-fine permanent magnetism powder refines further, has expanded product applications, can apply to RMB, expensive The printing of the minitype false proof bar codes such as weight jewelry, can store more anti-counterfeiting information in less striped, substantially increase product Electronic anti-fogery ability, improve the comfort level of antiforge bar code, improve added value of product.
The invention provides following technical proposals: the preparation method of a kind of Nd Fe B alloys ultra-fine permanent magnetism powder, described neodymium ferrum The preparation method of boron alloy ultra-fine permanent magnetism powder include successively raw material preferably, formula, vacuum melting operation, vacuum pure operation soon, Vacuum crystallization and thermal treatment operation, aging process, magnetic property detection operation, airflow milling manufacturing procedure, ultrasound wave sub-sieve particle size distribution Detection operation, finished product batch mixing magnetic property secondary detection operation;The raw material that described raw material is preferably selected include praseodymium neodymium alloy, The lanthanum cerium alloy of the electrolysis of purity 40~60, the ferrum of purity 99.9, the ferro-boron of purity 18~21, purity The zircaloy of 90, the cobalt alloy of purity 90, the weight ratio of the praseodymium neodymium of described praseodymium neodymium alloy is 20 80 or 25 75.
Described formula be weight percentage 15~28 described praseodymium neodymium alloy, percentage by weight 3~6 described Lanthanum cerium alloy, the described ferro-boron of percentage by weight 1~1.5, the described zircaloy of percentage by weight 4~5, weight Described in amount percentage ratio 4~8, cobalt alloy, surplus are described ferrum, due to this ferrum purity 99.9.Think that this ferrum is pure iron.
Further, described vacuum melting operation is: the raw material prepared by described formula loads in vaccum sensitive stove crucible Row argon shield melting, the air pressure of described argon is 0.04Pa~0.05Pa, described vacuum melting operation carry out during temperature Until described batch mixing all melts after rising to 1650 DEG C, fully boiling starts casting for 3~5 minutes, completes casting cooling 30~40 Minute formed foundry alloy.
Further, described vacuum pure operation soon is: by described foundry alloy through crusher in crushing formed 12mm particle diameter Grain, loads the charging basket of quick quenching furnace, described quick quenching furnace charging basket is evacuated to 10 after removing the fine powder of below 100 mesh-3Argon is added after Pa Gas shielded, argon pressure is 0.03Pa~0.04 Pa, and the aluminium alloy that described foundry alloy is formed through electric arc melting is from described quick quenching furnace Interior crucible cast gate edge flows into the edge of atwirl molybdenum wheel, the rotary action that described aluminium alloy is taken turns at described molybdenum after overflowing Lower solidification is cooled into alloy strip, the linear velocity 21~23m/s that described molybdenum wheel rotates, the solidification cooling of described aluminium alloy It is 106k/s。
Further, described vacuum crystallization and thermal treatment operation is: through forcing press, described alloy strip is pressed into 60 mesh powder body It is evacuated to 10 after loading the charging basket of vacuum crystallization furnace-2Pa, pours argon to 0.03Pa~0.04Pa, described vacuum crystallization furnace The rotational frequency of boiler tube be 22~28Hz, carry out vacuum crystallization and thermal treatment after described rotation boiler tube is heated to design temperature, Described design temperature is 690 DEG C~710 DEG C, and the time of described vacuum crystallization and thermal treatment is 10~12min, generates alloy after coming out of the stove Magnetic powder head product.
Further, described magnetic property detection operation is: described alloy magnetic powder head product is carried out magnetic property inspection when coming out of the stove Surveying, every stove must be examined;Stored classifiedly by the described alloy magnetic powder head product of same batch similar performance after testing, plain code identifies, respectively Proceed to next procedure, the detection of described magnetic property be powder is fabricated to standard sample post after utilize magnetic property automatic measuring instrument Progressive symmetric erythrokeratodermia Can detect, the detection of described magnetic property is to detect with standard sample post, and standard specimen specification is ¢ 10 × 10mm, and weight is 5.0g, described The quantity of sample column production is three pieces, and wherein two pieces are used for detecting, and other one piece keeps sample.
Further, described aging process is: the alloy magnetic of detection that will detect through described magnetic property detection operation Powder head product carries out high humidity high temperature oxidation process in batches on aging line, has detected conjunction by first high humidity, rear high temperature by described In the powder of gold magnetic powder head product, the crystalline solid of residual thoroughly eliminates, and described high humidity is to powder spray steam, and described high temperature is right Powder carries out flash baking, dries and is set as 120 DEG C~150 DEG C in temperature, drying time set 20~25min, through described always Chemical industry sequence prepares aging alloy magnetic powder head product.
Further, described airflow milling manufacturing procedure is: described airflow milling manufacturing procedure is by aging alloy described in 60 purposes Magnetic powder head product is processed as the powder of 5um~30um different-grain diameter, and the head-on collision fluid bed of application operation with closed ring carries out airflow milling.
Further, described ultrasound wave sub-sieve particle size distribution detection operation is: described ultrasound wave sub-sieve is by described neodymium iron boron Alloy ultra-fine permanent magnetism powder carries out secondary sub-sieve, and described secondary sub-sieve is to carry out ultrasonic on the mesh screen of particle diameter at the same level by corresponding powder Wavelength-division is sieved, effective solve may because of described airflow milling manufacturing procedure operational factor is wrong or equipment fault and the granule that produces not Uniform problem.
Further, described finished product batch mixing magnetic property secondary detection operation is: described finished product batch mixing is under argon shield Carrying out, described finished product mixing time is 20~25min.Described magnetic property secondary detection is magnetic powder to be made standard specimen, in magnetic Carrying out magnetic property secondary detection on dry powder detector, described magnetic property secondary detection includes remanent magnetism Br, intrinsic Hcb, intrinsic coercive The Indexs measure such as power Hcj, magnetic energy product BH, the most quantitatively pack, barrelling, enter warehouse for finished product plain code mark.
Beneficial effects of the present invention: the fineness of the Nd Fe B alloys ultra-fine permanent magnetism powder of the present invention refines further, expands Product applications, the present invention passes through first high humidity, rear high temperature by residual in the described powder having detected alloy magnetic powder head product Crystalline solid applies the head-on collision fluid bed of operation with closed ring to carry out airflow milling after thoroughly eliminating, head-on collision fluid bed is that one can by rare earth forever Magnetic alloy NdFeB is crushed to the equipment of micron-sized special gas-tight design.This finest material powder that the present invention generates The energy magnetic bar code that air brushing is tiny on commodity as the printer that dusts, can apply to RMB, valuable jewelry etc. miniature anti- The printing of pseudo bar code, can store more anti-counterfeiting information in less striped, substantially increase product electronic anti-fogery ability, Improve the comfort level of antiforge bar code, improve added value of product.
Accompanying drawing explanation
Fig. 1,2,3 are the magnetic property of the embodiment of the present invention 1, powder size distribution tests figure.Wherein Fig. 1 correspondence embodiment 1 Described in magnetic property detection operation magnetic property detection chart;Fig. 2 is powder size distribution tests figure in embodiment 1;Fig. 3 correspondence is real Execute the secondary detection operation of finished product batch mixing magnetic property described in example 1 detection chart.
Fig. 4,5,6 are the magnetic property of the embodiment of the present invention 2, powder size distribution tests figure.Wherein Fig. 4 correspondence embodiment 2 Described in magnetic property detection operation magnetic property detection chart;Fig. 5 is powder size distribution tests figure in embodiment 2;Fig. 6 correspondence is real Execute described finished product batch mixing magnetic property secondary detection operation detection chart described in example 2.
Fig. 7,8,9 are the magnetic property of the embodiment of the present invention 3, powder size distribution tests figure.Wherein Fig. 7 correspondence embodiment 3 Described in magnetic property detection operation magnetic property detection chart;Fig. 8 is powder size distribution tests figure in embodiment 3;Fig. 9 correspondence is real Execute described finished product batch mixing magnetic property secondary detection operation detection chart described in example 3.
Detailed description of the invention
Below in conjunction with accompanying drawing, the invention will be further described with specific embodiment.
Embodiment 1, the preparation method of a kind of Nd Fe B alloys ultra-fine permanent magnetism powder, described Nd Fe B alloys ultra-fine permanent magnetism powder Preparation method include successively raw material preferably, formula, vacuum melting operation, vacuum pure operation soon, vacuum crystallization and thermal treatment operation, Aging process, magnetic property detection operation, airflow milling manufacturing procedure, ultrasound wave sub-sieve particle size distribution detection operation, finished product batch mixing Magnetic property secondary detection operation.
The raw material that described raw material is preferably selected includes the lanthanum cerium alloy of the electrolysis of praseodymium neodymium alloy, purity 40, pure The ferrum of degree 99.9, the ferro-boron of purity 21, the zircaloy of purity 90, the cobalt alloy of purity 90, described praseodymium neodymium closes The praseodymium neodymium weight ratio of gold is 20 80.
Described formula be weight percentage 28 described praseodymium neodymium alloy, the described lanthanum cerium alloy of percentage by weight 3, weight Amount the described ferro-boron of percentage ratio 1, the described zircaloy of percentage by weight 4, percentage by weight 4 described in cobalt alloy, Surplus is described ferrum.
Described vacuum melting operation is: carry out argon guarantor in the raw material loading vaccum sensitive stove crucible prepared by described formula Protecting melting, the air pressure of described argon is 0.04Pa, described vacuum melting operation carry out during temperature rise to 1650 DEG C after until Described raw material all melts, and fully boiling starts casting for 3 minutes, completes casting cooling and forms foundry alloy in 30 minutes.
Described vacuum pure operation soon is: described foundry alloy is formed through crusher in crushing the granule of 12mm particle diameter, removes Load the charging basket of quick quenching furnace after fine powder below 100 mesh, described quick quenching furnace charging basket is evacuated to 10-3Argon shield is added after Pa, Argon pressure is 0.03Pa, the aluminium alloy that described foundry alloy is formed through electric arc melting crucible cast gate edge in described quick quenching furnace Flowing into the edge of atwirl molybdenum wheel after spilling, described aluminium alloy solidifies under the rotary action that described molybdenum is taken turns and is cooled into closing Gold bar band, linear velocity 21m/s that described molybdenum wheel rotates, the solidification cooling of described aluminium alloy is 106k/s。
Described vacuum crystallization and thermal treatment operation is: through forcing press, described alloy strip is pressed into 60 mesh powder body and loads vacuum It is evacuated to 10 after the charging basket of crystallization furnace­-2Pa, pours argon to 0.03PaPa, the rotation frequency of the boiler tube of described vacuum crystallization furnace Rate is 28Hz, carries out vacuum crystallization and thermal treatment after described rotation boiler tube is heated to design temperature, and described design temperature is 690 DEG C DEG C, the time of described vacuum crystallization and thermal treatment is 10min, generates alloy magnetic powder head product after coming out of the stove.
Described magnetic property detection operation is: described alloy magnetic powder head product is carried out magnetic property detection, every stove when coming out of the stove Must examine;Stored classifiedly by the described alloy magnetic powder head product of same batch similar performance after testing, plain code identifies, and proceeds to lower road respectively Operation, described magnetic property detection be powder is fabricated to standard sample post after utilize magnetic property automatic measuring instrument to carry out performance detection, The detection of described magnetic property is to detect with standard sample post, and standard specimen specification is ¢ 10 × 10mm, and weight is 5.0g, and this specification is diameter 10mm, highly 10mm.The quantity of described sample column production is three pieces, and wherein two pieces are used for detecting, and other one piece keeps sample.
Described aging process is: the alloy magnetic powder head product of detection that will detect through described magnetic property detection operation On aging line, carry out high humidity high temperature oxidation process in batches, detected described at the beginning of alloy magnetic powder by first high humidity, rear high temperature In the powder of product, the crystalline solid of residual thoroughly eliminates, and described high humidity is to powder spray steam, and vapor volume does not drop down water and is with powder Basis, described high temperature is that powder is carried out flash baking, dries and is set as 120 DEG C in temperature, and the drying time of feeding sets With humidity detector, 25min, identifies whether product dries, prepares aging alloy magnetic powder head product through described aging process;
Described airflow milling manufacturing procedure is: described aging alloy magnetic powder head product is proceeded to airflow milling, closes in order to process neodymium iron boron The ultra-fine permanent magnetism powder of gold.Described airflow milling manufacturing procedure is that alloy magnetic powder head product aging described in 60 purposes is processed as 5 to 30 not With the powder of particle diameter, the head-on collision fluid bed of application operation with closed ring carries out airflow milling, and head-on collision fluid bed is that one can be by rare earth permanent magnet Alloy NdFeB is crushed to the equipment of micron-sized special gas-tight design.Product granularity is uniform, does not generates heat, does not aoxidizes, and mill body is without mill Damaging, free from admixture is mixed into, environmentally safe.This equipment is dispensed valve control system, mill body, feeding by gas compressor, gas circuit Weighing system, hierarchy system, piece-rate system, filtration system, emergency protection system of catching fire, electric control system etc. partly forms. The powder of processing different-grain diameter need to debug the relevant parameter of feeding Weighing system, hierarchy system, piece-rate system, filtration system, its In, runner rotating speed is respectively set as between 3800 turns points.Setting of corresponding powder diameter is drawn by the test of powder size calibrating instrument Received shipment line parameter, the final Nd Fe B alloys ultra-fine permanent magnetism powder obtaining required grain size specification.
Described ultrasound wave sub-sieve particle size distribution detection operation is: ultrasound wave sizing equipment is with a kind of ultrasonic instrument dress Joining and be attached in powder vibrosieve, described ultrasound wave sub-sieve is that ultra-fine for described Nd Fe B alloys permanent magnetism powder is carried out secondary sub-sieve, Described secondary sub-sieve is that on the mesh screen of particle diameter at the same level, corresponding powder is carried out ultrasound wave sub-sieve, and effective solution may be because of described Airflow milling manufacturing procedure operational factor is wrong or equipment fault and the uneven problem of the granule that produces;Described particle size distribution detects Being that powder carries out on particle size analyzer precise determination, be analyzed D50 and D90 two item data, D50 numerical value is wanted definitely Greatly, D90 numerical value is comparatively small, otherwise wants further adjustment airflow milling and ultrasound wave sizing equipment.D50 is construed to 5 percent The particle diameter of the powder of ten;So D90 is construed to the powder diameter of 90 percent.Accompanying drawing 2 after testing, particle size distribution is: D50: 27.297um, D90:57.560um, product cut size meets preset requirement.
Described finished product batch mixing magnetic property secondary detection operation is: described finished product compounding process is by same particle size, phase The semi-finished product of nearly magnetic property are unified on batch mixer and carry out batch mixing.By particle diameter and magnetic property factory calibration, semi-finished product data are carried out Accurate calculation, quantitatively loads batch mixer batch mixing by several times, and described finished product batch mixing is carried out under argon shield, described finished product batch mixing Time is at 25min.Described magnetic property secondary detection is that magnetic powder is made standard specimen, carries out magnetic property two on magnetic dry powder detector Secondary detection, described magnetic property secondary detection includes the Indexs measure such as remanent magnetism Br, intrinsic Hcb, HCJ Hcj, magnetic energy product BH, The most quantitatively pack, barrelling, enters warehouse for finished product plain code mark.
Magnetic property detection operation magnetic property detection chart, finished product batch mixing magnetic property secondary detection operation described in the present embodiment Chart is respectively such as Fig. 1, Br:6.6615 KGs, Hcb:5.4834kOe, Hcj:9.4868 kOe, BH:9.1763MGO;Such as Fig. 3, Br:6.6615KGs, Hcb:5.4834kOe, Hcj:9.4864 kOe, BH:9.1772 MGO.The standard specimen specification of test is ¢ 10 × 10mm, coil turn 110 circle, area coil 1.252cm2, sample temperature 22 DEG C.Through test, this product magnetic property is excellent.
The preparation method of 2 one kinds of Nd Fe B alloys ultra-fine permanent magnetism powder of embodiment, described Nd Fe B alloys ultra-fine permanent magnetism powder Preparation method include successively raw material preferably, formula, vacuum melting operation, vacuum pure operation soon, vacuum crystallization and thermal treatment operation, Aging process, magnetic property detection operation, airflow milling manufacturing procedure, ultrasound wave sub-sieve particle size distribution detection operation, finished product batch mixing Magnetic property secondary detection operation.
The raw material that described raw material is preferably selected includes the lanthanum cerium alloy of the electrolysis of praseodymium neodymium alloy, purity 60, pure The ferrum of degree 99.9, the ferro-boron of purity 18, the zircaloy of purity 90, the cobalt alloy of purity 90, described praseodymium neodymium closes The praseodymium neodymium weight ratio of gold is 25 75.
Described formula be weight percentage 15 described praseodymium neodymium alloy, the described lanthanum cerium alloy of percentage by weight 6, weight hundred Cobalt alloy described in the described ferro-boron of proportion by subtraction 1.5, the described zircaloy of percentage by weight 5, percentage by weight 8, remaining Amount is described ferrum.
Described vacuum melting operation is: carry out argon guarantor in the raw material loading vaccum sensitive stove crucible prepared by described formula Protecting melting, the air pressure of described argon is 0.05Pa, described vacuum melting operation carry out during temperature rise to 1650 DEG C after until Described raw material all melts, and fully boiling starts casting for 3 minutes, completes casting cooling and forms foundry alloy in 30 minutes.
Described vacuum pure operation soon is: described foundry alloy is formed through crusher in crushing the granule of 12mm particle diameter, removes Load the charging basket of quick quenching furnace after fine powder below 100 mesh, described quick quenching furnace charging basket is evacuated to 10­-3Argon shield is added after Pa, Argon pressure is 0.04 Pa, the aluminium alloy that described foundry alloy is formed through electric arc melting crucible cast gate limit in described quick quenching furnace Edge flows into the edge of atwirl molybdenum wheel after overflowing, described aluminium alloy solidifies under the rotary action that described molybdenum is taken turns and is cooled into Alloy strip, linear velocity 23m/s that described molybdenum wheel rotates, the solidification cooling of described aluminium alloy is 106k/s。
Described vacuum crystallization and thermal treatment operation is: through forcing press, described alloy strip is pressed into 60 mesh powder body and loads vacuum It is evacuated to 10 after the charging basket of crystallization furnace-2Pa, pours argon to 0.04Pa, the rotational frequency of the boiler tube of described vacuum crystallization furnace For 22Hz, carrying out vacuum crystallization and thermal treatment after described rotation boiler tube is heated to design temperature, described design temperature is 690 DEG C, The time of described vacuum crystallization and thermal treatment is 10min, generates alloy magnetic powder head product after coming out of the stove.
Described magnetic property detection operation is: described alloy magnetic powder head product is carried out magnetic property detection, every stove when coming out of the stove Must examine;Stored classifiedly by the described alloy magnetic powder head product of same batch similar performance after testing, plain code identifies, and proceeds to lower road respectively Operation, described magnetic property detection be powder is fabricated to standard sample post after utilize magnetic property automatic measuring instrument to carry out performance detection, The detection of described magnetic property is to detect with standard sample post, and standard specimen specification is ¢ 10 × 10mm, and weight is 5.0g, described sample column production Quantity be three pieces, wherein two pieces are used for detecting, and other one piece keeps sample.
Described aging process is: the alloy magnetic powder head product of detection that will detect through described magnetic property detection operation On aging line, carry out high humidity high temperature oxidation process in batches, detected described at the beginning of alloy magnetic powder by first high humidity, rear high temperature In the powder of product, the crystalline solid of residual thoroughly eliminates, and described high humidity is to powder spray steam, and described high temperature is to carry out powder Flash baking, dries and is set as 150 DEG C in temperature, and the drying time of feeding sets 20min, identifies that product is with humidity detector No drying, prepares aging alloy magnetic powder head product through described aging process;
Described airflow milling manufacturing procedure is: described aging alloy magnetic powder head product is proceeded to airflow milling, closes in order to process neodymium iron boron The ultra-fine permanent magnetism powder of gold.Described airflow milling manufacturing procedure is that alloy magnetic powder head product aging described in 60 purposes is processed as 5 to 30um The powder of different-grain diameter, the head-on collision fluid bed of application operation with closed ring carries out airflow milling.
Described ultrasound wave sub-sieve particle size distribution detection operation is: ultrasound wave sizing equipment is with a kind of ultrasonic instrument dress Joining and be attached in powder vibrosieve, described ultrasound wave sub-sieve is that ultra-fine for described Nd Fe B alloys permanent magnetism powder is carried out secondary sub-sieve, Described secondary sub-sieve is that on the mesh screen of particle diameter at the same level, corresponding powder is carried out ultrasound wave sub-sieve, and effective solution may be because of described Airflow milling manufacturing procedure operational factor is wrong or equipment fault and the uneven problem of the granule that produces;Described particle size distribution detects Being that powder carries out on particle size analyzer precise determination, be analyzed D50 and D90 two item data, D50 numerical value is wanted definitely Greatly, D90 numerical value is comparatively small, otherwise wants further adjustment airflow milling and ultrasound wave sizing equipment.Accompanying drawing 5 after testing, granularity Being distributed as: D50:20.058um, D90:46.330um, product cut size meets preset requirement.
Described finished product batch mixing magnetic property secondary detection operation is: described finished product compounding process is by same particle size, phase The semi-finished product of nearly magnetic property are unified on batch mixer and carry out batch mixing.By particle diameter and magnetic property factory calibration, semi-finished product data are carried out Accurate calculation, quantitatively loads batch mixer batch mixing by several times, and described finished product batch mixing is carried out under argon shield, described finished product batch mixing Time is at 20min.Described magnetic property secondary detection is that magnetic powder is made standard specimen, carries out magnetic property two on magnetic dry powder detector Secondary detection, described magnetic property secondary detection includes the Indexs measure such as remanent magnetism Br, intrinsic Hcb, HCJ Hcj, magnetic energy product BH, The most quantitatively pack, barrelling, enters warehouse for finished product plain code mark.
Magnetic property detection operation magnetic property detection chart, finished product batch mixing magnetic property secondary detection operation described in the present embodiment Chart is respectively such as Fig. 4, Br:6.7683KGs, Hcb:5.5262kOe, Hcj:9.0376kOe, BH:9.4131MGO;Such as Fig. 6, Br: 6.6995KGs, Hcb:5.5020kOe, Hcj:9.4086kOe, BH:9.2730MGO.The standard specimen specification of test be ¢ 10 × 10mm, coil turn 110 circle, area coil 1.252cm2, sample temperature 22 DEG C.Through test, this product magnetic property is excellent.
Embodiment 3, the preparation method of a kind of Nd Fe B alloys ultra-fine permanent magnetism powder, described Nd Fe B alloys ultra-fine permanent magnetism powder Preparation method include successively raw material preferably, formula, vacuum melting operation, vacuum pure operation soon, vacuum crystallization and thermal treatment operation, Aging process, magnetic property detection operation, airflow milling manufacturing procedure, ultrasound wave sub-sieve particle size distribution detection operation, finished product batch mixing Magnetic property secondary detection operation;The raw material that described raw material is preferably selected includes the electrolysis of praseodymium neodymium alloy, purity 50 Lanthanum cerium alloy, the ferrum of purity 99.9, the ferro-boron of purity 20, the zircaloy of purity 90, the cobalt alloy of purity 90, The praseodymium neodymium weight ratio of described praseodymium neodymium alloy is 20 80.The purity of described ferro-boron refers to the purity of boron.
Described formula be weight percentage 18 described praseodymium neodymium alloy, the described lanthanum cerium alloy of percentage by weight 5, weight Cobalt described in the amount described ferro-boron of percentage ratio 1.3, the described zircaloy of percentage by weight 4.5, percentage by weight 6 closes Gold, surplus are described iron powder.
Described vacuum melting operation is: carry out argon guarantor in the batch mixing loading vaccum sensitive stove crucible prepared by described formula Protecting melting, the air pressure of described argon is 0.045Pa, described vacuum melting operation carry out during temperature rise to 1650 DEG C after until Described batch mixing all melts, and fully boiling starts casting for 4 minutes, completes casting cooling and forms foundry alloy in 35 minutes.
Described vacuum pure operation soon is: described foundry alloy is formed through crusher in crushing the granule of 12mm particle diameter, removes Load the charging basket of quick quenching furnace after fine powder below 100 mesh, described quick quenching furnace charging basket is evacuated to 10-3Argon shield is added after Pa, Argon pressure is 0.035 Pa, the aluminium alloy that described foundry alloy is formed through electric arc melting crucible cast gate limit in described quick quenching furnace Edge flows into the edge of atwirl molybdenum wheel after overflowing, described aluminium alloy solidifies under the rotary action that described molybdenum is taken turns and is cooled into Alloy strip, linear velocity 22m/s that described molybdenum wheel rotates, the solidification cooling of described aluminium alloy is 106k/s。
Described vacuum crystallization and thermal treatment operation is: through forcing press, described alloy strip is pressed into 60 mesh powder body and loads vacuum It is evacuated to 10 after the charging basket of crystallization furnace-2Pa, pours argon to 0.035Pa, the rotational frequency of the boiler tube of described vacuum crystallization furnace For 26Hz, carrying out vacuum crystallization and thermal treatment after described rotation boiler tube is heated to design temperature, described design temperature is 700 DEG C, The time of described vacuum crystallization and thermal treatment is 11min, generates alloy magnetic powder head product after coming out of the stove.
Described magnetic property detection operation is: described alloy magnetic powder head product is carried out magnetic property detection, every stove when coming out of the stove Must examine;Stored classifiedly by the described alloy magnetic powder head product of same batch similar performance after testing, plain code identifies, and proceeds to lower road respectively Operation, described magnetic property detection be powder is fabricated to standard sample post after utilize magnetic property automatic measuring instrument to carry out performance detection, The detection of described magnetic property is to detect with standard sample post, and standard specimen specification is ¢ 10 × 10mm, and weight is 5.0g, described sample column production Quantity be three pieces, wherein two pieces are used for detecting, and other one piece keeps sample.
Described aging process is: the alloy magnetic powder head product of detection that will detect through described magnetic property detection operation On aging line, carry out high humidity high temperature oxidation process in batches, detected described at the beginning of alloy magnetic powder by first high humidity, rear high temperature In the powder of product, the crystalline solid of residual thoroughly eliminates, and described high humidity is to powder spray steam, and vapor volume does not drop down water and is with powder Basis, described high temperature is that powder is carried out flash baking, dries and is set as 130 DEG C in temperature, and the drying time of feeding sets With humidity detector, 23min, identifies whether product dries, prepares aging alloy magnetic powder head product through described aging process;
Described airflow milling manufacturing procedure is: described aging alloy magnetic powder head product is proceeded to airflow milling, closes in order to process neodymium iron boron The ultra-fine permanent magnetism powder of gold.Described airflow milling manufacturing procedure be alloy magnetic powder head product aging described in 60 purposes is processed as 5um~ The powder of 30um different-grain diameter, the head-on collision fluid bed of application operation with closed ring carries out airflow milling, and head-on collision fluid bed is that a kind of energy is by dilute Soil permanent-magnet alloy NdFeB is crushed to the equipment of micron-sized special gas-tight design.Product granularity is uniform, does not generates heat, does not aoxidizes, mill Body is without abrasion, and free from admixture is mixed into, environmentally safe.This equipment is dispensed valve control system by gas compressor, gas circuit, mill Body, feeding Weighing system, hierarchy system, piece-rate system, filtration system, catch fire the portions such as emergency protection system, electric control system It is grouped into.The powder of processing different-grain diameter need to debug feeding Weighing system, hierarchy system, piece-rate system, filtration system relevant Parameter, wherein, runner rotating speed is respectively set as between 3500 turns points.Corresponding powder is drawn by the test of powder size calibrating instrument The equipment operational factor of particle diameter, the final Nd Fe B alloys ultra-fine permanent magnetism powder obtaining required grain size specification.
Described ultrasound wave sub-sieve particle size distribution detection operation is: ultrasound wave sizing equipment is with a kind of ultrasonic instrument dress Joining and be attached in powder vibrosieve, described ultrasound wave sub-sieve is that ultra-fine for described Nd Fe B alloys permanent magnetism powder is carried out secondary sub-sieve, Described secondary sub-sieve is that on the mesh screen of particle diameter at the same level, corresponding powder is carried out ultrasound wave sub-sieve, and effective solution may be because of described Airflow milling manufacturing procedure operational factor is wrong or equipment fault and the uneven problem of the granule that produces;Described particle size distribution detects Being that powder carries out on particle size analyzer precise determination, be analyzed D50 and D90 two item data, D50 numerical value is wanted definitely Greatly, D90 numerical value is comparatively small, otherwise wants further adjustment airflow milling and ultrasound wave sizing equipment.Each due to the present embodiment The value of individual parameter is between embodiment 1 and embodiment 2, should comply with requirement by particle size distribution for reason, and passes through Detection particle size distribution meets the requirements really.As shown in Figure 8, D10:4.382um, D50:10.689um, D90:21.655um.
Described finished product batch mixing magnetic property secondary detection operation is: described finished product compounding process is by same particle size, phase The semi-finished product of nearly magnetic property are unified on batch mixer and carry out batch mixing.By particle diameter and magnetic property factory calibration, semi-finished product data are carried out Accurate calculation, quantitatively loads batch mixer batch mixing by several times, and described finished product batch mixing is carried out under argon shield, described finished product batch mixing Time is at 23min.Described magnetic property secondary detection is that magnetic powder is made standard specimen, carries out magnetic property two on magnetic dry powder detector Secondary detection, described magnetic property secondary detection includes the Indexs measure such as remanent magnetism Br, intrinsic Hcb, HCJ Hcj, magnetic energy product BH, The most quantitatively pack, barrelling, enters warehouse for finished product plain code mark.
Magnetic property detection operation magnetic property detection chart, finished product batch mixing magnetic property secondary detection operation described in the present embodiment Chart is respectively such as Fig. 7, Br:6.6651KGs, Hcb:5.5383kOe, Hcj:9.6276kOe, BH:9.2885MGO;Such as Fig. 9, Br: 6.6680KGs, Hcb:5.4580kOe, Hcj:9.5743kOe, BH:9.1507MGO.The standard specimen specification of test be ¢ 10 × 10mm, coil turn 110 circle, area coil 1.252cm2, sample temperature 22 DEG C.Through test, this product magnetic property is excellent.
Above example is in order to illustrate technical scheme and unrestricted, and those of ordinary skill in the art are to the present invention Technical scheme made other amendment equivalents, without departing from the scope of technical solution of the present invention, all should contain this In the protection domain of invention.

Claims (6)

1. the preparation method of a Nd Fe B alloys ultra-fine permanent magnetism powder, it is characterised in that described Nd Fe B alloys ultra-fine permanent magnetism powder Preparation method include successively raw material preferably, formula, vacuum melting operation, vacuum quick quenching operation, vacuum crystallization and thermal treatment work Sequence, aging process, magnetic property detection operation, airflow milling manufacturing procedure, ultrasound wave sub-sieve particle size distribution detection operation, finished product mix Material magnetic property secondary detection operation.
The preparation method of Nd Fe B alloys the most according to claim 1 ultra-fine permanent magnetism powder, it is characterised in that described raw material Preferably selected raw material includes praseodymium neodymium alloy, the lanthanum cerium alloy of electrolysis of purity 40~60, purity 99.9 Ferrum, the ferro-boron of purity 18~21, the zircaloy of purity 90, the cobalt alloy of purity 90, described praseodymium neodymium alloy Praseodymium is 20 80 or 25 75 with the weight ratio of neodymium.
The preparation method of Nd Fe B alloys the most according to claim 1 ultra-fine permanent magnetism powder, it is characterised in that described formula is The described praseodymium neodymium alloy of percentage by weight 15~28, the described lanthanum cerium alloy of percentage by weight 3~6, weight percent Described ferro-boron than 1~1.5, the described zircaloy of percentage by weight 4~5, percentage by weight 4~8 Described cobalt alloy, surplus are described ferrum.
The preparation method of Nd Fe B alloys the most according to claim 3 ultra-fine permanent magnetism powder, it is characterised in that:
One, described vacuum melting operation is: carry out argon guarantor in the raw material loading vaccum sensitive stove crucible prepared by described formula Protecting melting, the air pressure of described argon is 0.04Pa~0.05Pa, and during described vacuum melting operation is carried out, temperature rises to 1650 Until described raw material all melts after DEG C, fully boiling starts casting for 3~5 minutes, completes casting cooling and is formed for 30~40 minutes Foundry alloy;
Two, described vacuum quick quenching operation is: described foundry alloy is formed through crusher in crushing the granule of 12mm particle diameter, removes Load the charging basket of quick quenching furnace after fine powder below 100 mesh, described quick quenching furnace charging basket is evacuated to 10-3Add argon after Pa to protect Protecting, argon pressure is 0.03Pa~0.04 Pa, and the aluminium alloy that described foundry alloy is formed through electric arc melting is in described quick quenching furnace Crucible cast gate edge flows into the edge of atwirl molybdenum wheel after overflowing, described aluminium alloy is solidifying under the rotary action that described molybdenum is taken turns Admittedly be cooled into alloy strip, the linear velocity 21~23m/s that described molybdenum wheel rotates, the solidification cooling of described aluminium alloy is 106k/s;
Three, described vacuum crystallization and thermal treatment operation is: through forcing press, described alloy strip is pressed into 60 mesh powder body and loads vacuum It is evacuated to 10 after the charging basket of crystallization furnace-2Pa, pours argon to 0.03Pa~0.04Pa, the boiler tube of described vacuum crystallization furnace Rotational frequency is 22~28Hz, carries out described vacuum crystallization and thermal treatment operation after described rotation boiler tube is heated to design temperature, Described design temperature is 690 DEG C~710 DEG C, and the time that described vacuum crystallization and thermal treatment operation is carried out is 10~12min, comes out of the stove Rear generation alloy magnetic powder head product;
Four, described magnetic property detection operation is: described alloy magnetic powder head product is carried out magnetic property detection when coming out of the stove, and every stove must Inspection;Stored classifiedly by the described alloy magnetic powder head product of same batch similar performance after testing, plain code identifies, and proceeds to lower road work respectively Sequence, described magnetic property detection be powder is fabricated to standard sample post after utilize magnetic property automatic measuring instrument to carry out performance detection, institute Stating magnetic property detection is to detect with standard sample post, and standard specimen specification is ¢ 10 × 10mm, and weight is 5.0g, described sample column production Quantity is three pieces, and wherein two pieces are used for detecting, and other one piece keeps sample;
Five, described aging process is: the alloy magnetic powder head product of detection that will detect through described magnetic property detection operation On aging line, carry out high humidity high temperature oxidation process in batches, detected described at the beginning of alloy magnetic powder by first high humidity, rear high temperature In the powder of product, the crystalline solid of residual thoroughly eliminates, and described high humidity is to powder spray steam, and described high temperature is to carry out powder Flash baking, dries and is set as 120 DEG C~150 DEG C in temperature, and drying time sets 20~25min, through described aging process system Obtain aging alloy magnetic powder head product;
Six, described airflow milling manufacturing procedure is: described airflow milling manufacturing procedure is by alloy magnetic powder primiparity aging described in 60 purposes Product are processed as the powder of 5um~30um different-grain diameter, and the head-on collision fluid bed of application operation with closed ring carries out airflow milling and obtains neodymium iron boron Alloy ultra-fine permanent magnetism powder;
Seven, described ultrasound wave sub-sieve particle size distribution detection operation is: described ultrasound wave sub-sieve is by ultra-fine for described Nd Fe B alloys Permanent magnetism powder carries out secondary sub-sieve, and described secondary sub-sieve is that on the mesh screen of particle diameter at the same level, corresponding powder is carried out ultrasound wave sub-sieve;
Eight, described finished product batch mixing magnetic property secondary detection operation is: described finished product compounding process is by same particle size, close The semi-finished product of magnetic property are unified on batch mixer and carry out batch mixing.
5. by particle diameter and magnetic property factory calibration, semi-finished product data are carried out accurate calculation, quantitatively load batch mixer batch mixing by several times, Described finished product batch mixing is carried out under argon shield, and described finished product mixing time is 20~25min.
6. magnetic property secondary detection described in is that magnetic powder is made standard specimen, carries out magnetic property secondary inspection on magnetic dry powder detector Surveying, described magnetic property secondary detection includes the Indexs measure such as remanent magnetism Br, intrinsic Hcb, HCJ Hcj, magnetic energy product BH, then The most quantitatively pack, barrelling, enters warehouse for finished product plain code mark.
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