CN109346261A - A kind of the ferro-aluminum mine magnetic material and its smelting process of high cerium content - Google Patents
A kind of the ferro-aluminum mine magnetic material and its smelting process of high cerium content Download PDFInfo
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- CN109346261A CN109346261A CN201811350025.9A CN201811350025A CN109346261A CN 109346261 A CN109346261 A CN 109346261A CN 201811350025 A CN201811350025 A CN 201811350025A CN 109346261 A CN109346261 A CN 109346261A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention belongs to magnetic material technical field of smelting, 25% ~ 30% is accounted for solve the dosage of neodymium in existing rare-earth Nd-Fe-B permanent magnetic material, but the utilization of rare earth resources is extremely uneven, cause lanthanum, cerium is largely overstock, it is unstable and the problem of decline to a great extent that magnetic property after lanthanum cerium is added, provides the ferro-aluminum mine magnetic material and its smelting process of a kind of high cerium content.Be made of the raw material of following mass percent: the proportion before hydrogen is broken: praseodymium neodymium steel ingot 13% ~ 16%, cerium steel ingot 6% ~ 40%, give up block 45% ~ 80%, wherein useless block is the product after neodymium-iron-boron magnetic material equipment is scrapped, praseodymium neodymium content is 30% or more.It can achieve the requirement stablized and meet client to magnetic property.The grain boundary structure continuous uniform in the Nd-Fe-B permanent magnet material obtained by the preparation method, enhances the Magnetic isolation effect between neighboring die, thus effective improvement can be obtained in the coercivity of Nd-Fe-B permanent magnet material, and magnetic property is more excellent.
Description
Technical field
The invention belongs to magnetic material technical field of smelting, the ferro-aluminum mine magnetic material of specifically a kind of high cerium content and its
Smelting process.
Background technique
Rare earth permanent-magnetic material is the strategic material of universally acknowledged new and high technology and national defence highly sophisticated products, rare earth permanent magnet
Material is that the first big application material is widely used in automobile communication, mobile phone, new-energy automobile, electric vehicle, wind-power electricity generation etc..
Rare-earth Nd-Fe-B (sintering) permanent-magnet material is manufactured, the dosage of neodymium accounts between 25% ~ 30%, but the utilization of rare earth resources
Extremely uneven, rare earth permanent-magnetic material (referring mainly to sintered NdFeB) mainly applies neodymium, praseodymium, dysprosium, the elements such as terbium, and rich reserves
High-purity Rare Earth Lanthanum, the elements such as cerium using less, and in Rare Earth Mine, have the association of various elements, widely apply praseodymium neodymium,
Lanthanum is caused, cerium is largely overstock.
Manufacture rare-earth Nd-Fe-B (sintering) permanent-magnet material, addition lanthanum, cerium magnetic property is caused it is unstable, and substantially under
Drop.
Summary of the invention
The present invention accounts for 25% ~ 30% to solve the dosage of neodymium in existing rare-earth Nd-Fe-B (sintering) permanent-magnet material, but dilute
The utilization of soil resource is extremely uneven, causes lanthanum, and cerium is largely overstock, and it is unstable and decline to a great extent that magnetic property after lanthanum cerium is added
Problem provides the ferro-aluminum mine magnetic material and its smelting process of a kind of high cerium content.
The present invention takes following technical scheme: a kind of ferro-aluminum mine magnetic material of high cerium content, by following mass percent
Raw material composition: the proportion before hydrogen is broken: praseodymium neodymium steel ingot 13% ~ 16%, cerium steel ingot 6% ~ 40%, give up block 45% ~ 80%, wherein useless block is neodymium
Fe-Mn magnetism material equipment scrap after product, praseodymium neodymium content is 30% or more.
The praseodymium neodymium steel ingot are as follows: praseodymium neodymium 30%, gadolinium iron 10%, ferro-boron 1.05%, aluminium 0.8%, copper 1.15%, cobalt 0.6%, iron
56.4%。
In the praseodymium neodymium steel ingot: praseodymium neodymium 45%, gadolinium iron 5%, boron 1.05%, aluminium 0.8%, copper 0.15%, cobalt 0.6%.
In the cerium steel ingot: cerium 29.5%, gadolinium iron 4%, ferro-boron 1.05%, aluminium 0.8%, copper 0.15%, cobalt 0.6%.
A kind of method of the ferro-aluminum mine magnetic material of any high cerium content of Claims 1-4 is smelted, feature exists
In: step are as follows: ingredient, melting, hydrogen is broken and airflow milling milling, magnetic field are formed, and sintering is risen again, the specific steps are as follows:
(1) ingredient: praseodymium neodymium steel ingot, cerium steel ingot and useless block raw material are accurately weighed in proportion, are mixed, the powder in primary mill
It is broken；
(2) melting: it is≤20Pa that melting vacuum degree is controlled in smelting furnace, and refining power is 30-50KW, refines 10min, casting temperature
Degree is 1400-1440 DEG C, is poured 3min；After casting complete, the control crystallisation by cooling time is 40-50min, pressure >=0.1MPa；
Steel ingot is come out of the stove after crystallization through detecting, internal no-sundries, steel ingot fracture is white；Column crystal fraction reaches 80% or more, and nothing
Severe oxidation skin, fold and bubble；
(3) hydrogen is broken and airflow milling is milled: hydrogen flour desorption temperature is 500-600 DEG C, and hydrogen flour particle size is 0.01-0.5mm,
C content is less than 150ppm, and O content is less than 100ppm, and N content is less than 200ppm；Be milled into airflow milling: the oxygen for grinding gas contains
Charging when amount is down to 0.00ppm, the granularity of airflow milling milling are 3-5 μm；
(4) magnetic field is formed: magnet is made in isostatic pressing: control environment temperature is<28 DEG C, humidity<50%, magnetic field>=1.4T in mold,
Pressure >=4Mpa, precompressed blank exposure duration≤10 second in air, isostatic pressure >=15MPa, high pressure cavity pressure >=150Mpa；
Green density answers >=4.5g/cm after equal static pressure3；
(5) sintering is risen again: control vacuum degree is 2 × 10-3Pa, Pressure Rise Rate≤0.5Pa/Hr, suction performance≤20min, temperature are uniform
1100 DEG C ± 3 DEG C of property, is sintered specific method are as follows: A, 50min are warming up to 250 DEG C, 250 DEG C of constant temperature 2h by room temperature, then 50min
350 DEG C, constant temperature 2h are inside warming up to, 750 DEG C is then warming up in 50min again, is warming up to 1050 in 750 DEG C of constant temperature 6h, 30min
DEG C, it is warming up to 1150 DEG C in constant temperature 90min, 30min, continues constant temperature 4h, it is air-cooled to rise again to 80 DEG C；B, control heating rate is
930 DEG C, constant temperature 4h are warming up to by 80 DEG C in 80min, it is then air-cooled to 80 DEG C；C, control heating rate is in 80min by 80 DEG C
550 DEG C, constant temperature 4h are warming up to, it is magnetic to be then cooled to the ferro-aluminum mine that 70 DEG C or less obtain high cerium content by 550 DEG C in 80min
Material.
The ferro-aluminum mine magnetic material that high cerium content is prepared using the method for the invention, passes through wanting for different magnetic properties
It asks, to match different ratios, can achieve the requirement stablized and meet client to magnetic property.It is obtained by the preparation method
The Nd-Fe-B permanent magnet material in grain boundary structure continuous uniform, effectively enhance between neighboring die Magnetic isolation effect
Fruit, thus effective improvement can be obtained in the coercivity of Nd-Fe-B permanent magnet material, magnetic property is more excellent.
Specific embodiment
Embodiment 1: a kind of ferro-aluminum mine magnetic material of high cerium content, be made of the raw material of following mass percent: hydrogen is broken
Preceding proportion: praseodymium neodymium steel ingot 13% ~ 16%, cerium steel ingot 6% ~ 40%, give up block 45% ~ 80%, wherein useless block is neodymium-iron-boron magnetic material device
Material scrap after product, praseodymium neodymium content is 30% or more.
The praseodymium neodymium steel ingot are as follows: praseodymium neodymium 30%, gadolinium iron 10%, ferro-boron 1.05%, aluminium 0.8%, copper 1.15%, cobalt 0.6%, iron
56.4%.In the cerium steel ingot: cerium 29.5%, gadolinium iron 4%, ferro-boron 1.05%, aluminium 0.8%, copper 0.15%, cobalt 0.6%.
Smelt a kind of method of the ferro-aluminum mine magnetic material of high cerium content, it is characterised in that: step are as follows: ingredient,
Melting, hydrogen is broken and airflow milling milling, magnetic field are formed, and sintering is risen again, the specific steps are as follows:
(1) ingredient: praseodymium neodymium steel ingot, cerium steel ingot and useless block raw material are accurately weighed in proportion, are mixed, the powder in primary mill
It is broken；
(2) melting: it is≤20Pa that melting vacuum degree is controlled in smelting furnace, and refining power is 30-50KW, refines 10min, casting temperature
Degree is 1400-1440 DEG C, is poured 3min；After casting complete, the control crystallisation by cooling time is 40-50min, pressure >=0.1MPa；
Steel ingot is come out of the stove after crystallization through detecting, internal no-sundries, steel ingot fracture is white；Column crystal fraction reaches 80% or more, and nothing
Severe oxidation skin, fold and bubble；
(3) hydrogen is broken and airflow milling is milled: hydrogen flour desorption temperature is 500-600 DEG C, and hydrogen flour particle size is 0.01-0.5mm,
C content is less than 150ppm, and O content is less than 100ppm, and N content is less than 200ppm；Be milled into airflow milling: the oxygen for grinding gas contains
Charging when amount is down to 0.00ppm, the granularity of airflow milling milling are 3-5 μm；
(4) magnetic field is formed: magnet is made in isostatic pressing: control environment temperature is<28 DEG C, humidity<50%, magnetic field>=1.4T in mold,
Pressure >=4Mpa, precompressed blank exposure duration≤10 second in air, isostatic pressure >=15MPa, high pressure cavity pressure >=150Mpa；
Green density answers >=4.5g/cm after equal static pressure3；
(5) sintering is risen again: control vacuum degree is 2 × 10-3Pa, Pressure Rise Rate≤0.5Pa/Hr, suction performance≤20min, temperature are uniform
1100 DEG C ± 3 DEG C of property, is sintered specific method are as follows: A, 50min are warming up to 250 DEG C, 250 DEG C of constant temperature 2h by room temperature, then 50min
350 DEG C, constant temperature 2h are inside warming up to, 750 DEG C is then warming up in 50min again, is warming up to 1050 in 750 DEG C of constant temperature 6h, 30min
DEG C, it is warming up to 1150 DEG C in constant temperature 90min, 30min, continues constant temperature 4h, it is air-cooled to rise again to 80 DEG C；B, control heating rate is
930 DEG C, constant temperature 4h are warming up to by 80 DEG C in 80min, it is then air-cooled to 80 DEG C；C, control heating rate is in 80min by 80 DEG C
550 DEG C, constant temperature 4h are warming up to, it is magnetic to be then cooled to the ferro-aluminum mine that 70 DEG C or less obtain high cerium content by 550 DEG C in 80min
Material.
Embodiment 2: a kind of ferro-aluminum mine magnetic material of high cerium content, be made of the raw material of following mass percent: hydrogen is broken
Preceding proportion: praseodymium neodymium steel ingot 13% ~ 16%, cerium steel ingot 6% ~ 40%, give up block 45% ~ 80%, wherein useless block is neodymium-iron-boron magnetic material device
Material scrap after product, praseodymium neodymium content is 30% or more.In the praseodymium neodymium steel ingot: praseodymium neodymium 45%, gadolinium iron 5%, boron 1.05%, aluminium
0.8%, copper 0.15%, cobalt 0.6%.The method that the preparation method is the same as that of Example 1.
Claims (5)
1. a kind of ferro-aluminum mine magnetic material of high cerium content, it is characterised in that: be made of the raw material of following mass percent: hydrogen is broken
Preceding proportion: praseodymium neodymium steel ingot 13% ~ 16%, cerium steel ingot 6% ~ 40%, give up block 45% ~ 80%, wherein useless block is neodymium-iron-boron magnetic material device
Material scrap after product, praseodymium neodymium content is 30% or more.
2. a kind of ferro-aluminum mine magnetic material of high cerium content according to claim 1, it is characterised in that: the praseodymium neodymium steel ingot
Are as follows: praseodymium neodymium 30%, gadolinium iron 10%, ferro-boron 1.05%, aluminium 0.8%, copper 1.15%, cobalt 0.6%, iron 56.4%.
3. a kind of ferro-aluminum mine magnetic material of high cerium content according to claim 1, it is characterised in that: the praseodymium neodymium steel ingot
In: praseodymium neodymium 45%, gadolinium iron 5%, boron 1.05%, aluminium 0.8%, copper 0.15%, cobalt 0.6%.
4. a kind of ferro-aluminum mine magnetic material of high cerium content according to claim 1, it is characterised in that: the cerium steel ingot
In: cerium 29.5%, gadolinium iron 4%, ferro-boron 1.05%, aluminium 0.8%, copper 0.15%, cobalt 0.6%.
5. smelting a kind of method of the ferro-aluminum mine magnetic material of any high cerium content of Claims 1-4, feature exists
In: step are as follows: ingredient, melting, hydrogen is broken and airflow milling milling, magnetic field are formed, and sintering is risen again, the specific steps are as follows:
(1) ingredient: praseodymium neodymium steel ingot, cerium steel ingot and useless block raw material are accurately weighed in proportion, are mixed, the powder in primary mill
It is broken；
(2) melting: it is≤20Pa that melting vacuum degree is controlled in smelting furnace, and refining power is 30-50KW, refines 10min, casting temperature
Degree is 1400-1440 DEG C, is poured 3min；After casting complete, the control crystallisation by cooling time is 40-50min, pressure >=0.1MPa；
Steel ingot is come out of the stove after crystallization through detecting, internal no-sundries, steel ingot fracture is white；Column crystal fraction reaches 80% or more, and nothing
Severe oxidation skin, fold and bubble；
(3) hydrogen is broken and airflow milling is milled: hydrogen flour desorption temperature is 500-600 DEG C, and hydrogen flour particle size is 0.01-0.5mm,
C content is less than 150ppm, and O content is less than 100ppm, and N content is less than 200ppm；Be milled into airflow milling: the oxygen for grinding gas contains
Charging when amount is down to 0.00ppm, the granularity of airflow milling milling are 3-5 μm；
(4) magnetic field is formed: magnet is made in isostatic pressing: control environment temperature is<28 DEG C, humidity<50%, magnetic field>=1.4T in mold,
Pressure >=4Mpa, precompressed blank exposure duration≤10 second in air, isostatic pressure >=15MPa, high pressure cavity pressure >=150Mpa；
Green density answers >=4.5g/cm after equal static pressure3；
(5) sintering is risen again: control vacuum degree is 2 × 10-3Pa, Pressure Rise Rate≤0.5Pa/Hr, suction performance≤20min, temperature are uniform
1100 DEG C ± 3 DEG C of property, is sintered specific method are as follows: A, 50min are warming up to 250 DEG C, 250 DEG C of constant temperature 2h by room temperature, then 50min
350 DEG C, constant temperature 2h are inside warming up to, 750 DEG C is then warming up in 50min again, is warming up to 1050 in 750 DEG C of constant temperature 6h, 30min
DEG C, it is warming up to 1150 DEG C in constant temperature 90min, 30min, continues constant temperature 4h, it is air-cooled to rise again to 80 DEG C；B, control heating rate is
930 DEG C, constant temperature 4h are warming up to by 80 DEG C in 80min, it is then air-cooled to 80 DEG C；C, control heating rate is in 80min by 80 DEG C
550 DEG C, constant temperature 4h are warming up to, it is magnetic to be then cooled to the ferro-aluminum mine that 70 DEG C or less obtain high cerium content by 550 DEG C in 80min
Material.
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