CN109326404B - Neodymium-iron-boron magnetic material and preparation method thereof - Google Patents
Neodymium-iron-boron magnetic material and preparation method thereof Download PDFInfo
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- CN109326404B CN109326404B CN201811247522.6A CN201811247522A CN109326404B CN 109326404 B CN109326404 B CN 109326404B CN 201811247522 A CN201811247522 A CN 201811247522A CN 109326404 B CN109326404 B CN 109326404B
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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
- H01F1/058—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IVa elements, e.g. Gd2Fe14C
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- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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- H—ELECTRICITY
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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Abstract
The invention belongs to the field of magnetic materials, and particularly relates to a neodymium iron boron magnetic material and a preparation method thereof. A neodymium iron boron magnetic material comprises the following components in parts by weight: 29-33 parts of praseodymium-neodymium alloy, 3-6 parts of dysprosium-iron alloy, 3-7 parts of ferroboron alloy, 0.6-0.8 part of ferroniobium alloy, 5-8 parts of yttrium-iron alloy, 1.0-2.5 parts of nano silicon dioxide, 0.1-0.3 part of gallium, 0.5-1 part of aluminum oxide, 1-2 parts of antioxidant and the balance of iron. The technical effect of the neodymium iron boron magnetic material obtained by the invention is that the nanometer silicon dioxide and the niobium-iron alloy are added in the neodymium iron boron magnetic material, and meanwhile, the praseodymium-neodymium alloy is taken as the main component in the component proportion, so that the Curie temperature is obviously improved, the coercive force of the neodymium iron boron magnetic material is improved, and the application value of the neodymium iron boron magnetic material is improved.
Description
Technical Field
The invention belongs to the field of magnetic materials, and particularly relates to a neodymium iron boron magnetic material and a preparation method thereof.
Background
Currently, new material industries, which are the foundation of high-tech industries, are receiving attention. The rare earth permanent magnetic material as an important component of new material industry is widely applied to industries such as energy, transportation, machinery, medical treatment, IT, household appliances and the like, the product relates to a plurality of fields of national economy, and the yield and the dosage of the product also become one of important marks for measuring the comprehensive national strength and the national economy development level. Especially, neodymium iron boron is used as a third-generation rare earth permanent magnet material, has wide market prospect, and is mainly applied to computer disk drives, nuclear magnetic resonance imagers, various audio and video equipment, microwave communication, magnetic machines, household appliances and the like. At present, the neodymium iron boron industry also enters a critical development period, and the output of the neodymium iron boron in China already accounts for about 40% of the total world output.
Neodymium iron boron magnetic materials, which are the latest result of the development of rare earth permanent magnetic materials, are called "maga" due to their excellent magnetic properties. The neodymium-iron-boron magnetic material is an alloy of neodymium, iron oxide and the like. Also known as magnetic steel. The Nd-Fe-B has very high magnetic energy and rectifying power, and the advantage of high energy density makes the Nd-Fe-B permanent magnetic material widely used in modern industry and electronic technology, so that it is possible to miniaturize, lighten and thin instruments and meters, electroacoustic motors, magnetic separation and magnetization equipment, etc. The neodymium iron boron has the advantages of high cost performance and good mechanical property; the disadvantages are that the Curie temperature of the Nd-Fe-B permanent magnet is low, and the coercive force of the magnet is low, so that the demands of products with high requirements on magnetic properties are difficult to meet. Therefore, the chemical composition of the material must be adjusted to meet the requirements of practical application.
Disclosure of Invention
The invention aims to overcome the defect of low Curie temperature in the prior art and provides a neodymium iron boron magnetic material and a preparation method thereof.
A neodymium iron boron magnetic material comprises the following components in parts by weight: 29-33 parts of praseodymium-neodymium alloy, 3-6 parts of dysprosium-iron alloy, 3-7 parts of ferroboron alloy, 0.6-0.8 part of ferroniobium alloy, 5-8 parts of yttrium-iron alloy, 1.0-2.5 parts of nano silicon dioxide, 0.1-0.3 part of gallium, 0.5-1 part of aluminum oxide, 1-2 parts of antioxidant and the balance of iron.
Specifically, the composition comprises the following components in parts by weight: 31 parts of praseodymium-neodymium alloy, 5 parts of dysprosium-iron alloy, 5 parts of ferroboron alloy, 0.7 part of ferroniobium alloy, 6 parts of yttrium-iron alloy, 2 parts of nano silicon dioxide, 0.2 part of gallium, 0.8 part of aluminum oxide, 1.5 parts of antioxidant and the balance of iron.
Specifically, the antioxidant is a mixture of an antioxidant 1010 and an antioxidant 1076, wherein the weight part ratio of the antioxidant 1010 to the antioxidant 1076 is 1: 1-3.
Specifically, the particle size of the silica is 45 to 80 nm.
In addition, the invention also provides a method for preparing the neodymium iron boron magnetic material, which comprises the following steps:
step one, batching: weighing raw materials according to the weight parts of the components in the neodymium iron boron magnetic material, mixing the components together, and after the material mixing is finished;
smelting an alloy in a second step: putting the raw materials prepared in the step one into an intermediate frequency vacuum smelting furnace for smelting, and vacuumizing 1 x 10-1Pa, controlling the temperature of the smelting furnace within the range of 1500-2000 ℃, simultaneously filling inert gas into the smelting furnace for protection, and cooling after smelting to form neodymium iron boron blocks;
step three, hydrogen crushing: putting the neodymium iron boron block into a hydrogen crushing furnace for hydrogen explosion, and vacuumizing for 1 x 10-1Pa, controlling the temperature at 250-plus-300 ℃, injecting hydrogen to allow the raw material to absorb hydrogen for 3h, then heating to 700-plus-800 ℃, carrying out dehydrogenation, and finally cooling and discharging from the furnace;
step four, pulverizing: crushing the product obtained in the third step into fine powder particles with the particle size of 2-3 mu m in an airflow mill;
step five, orientation forming: mixing the fine powder particles in a mixer for 5-8 hours, putting the mixture into a mould, orienting the mixture in a magnetic field with the magnetic field intensity of 1.8T, and pressing the mixture to form a blank;
step six, sintering: pre-sintering the blank piece in the step five for 2 hours at 500 ℃ under a vacuum condition, and sintering the blank piece in a vacuum furnace for 6 to 8 hours at 1200 ℃;
and seventhly, tempering: preserving heat for 5-8 hours at 800-1000 ℃, preserving heat for 5-8 hours at 500-600 ℃, after air cooling, cutting and polishing, and then carrying out surface passivation and plating treatment to obtain the finished product of the neodymium iron boron magnetic material.
Specifically, in the step two alloy smelting process, the inert gas flushed in is argon or nitrogen.
Compared with the prior art, the invention has the beneficial effects that:
1. nd and B are added into Fe to form Nd-Fe-B permanent magnetic main phase. Due to the coexistence of the nano-silicon dioxide (the grain diameter of the silicon dioxide is 45-80nm) and the ferrocolumbium, the nano-silicon dioxide component and the Nd-Fe-B permanent magnet main phase are compounded into a grain boundary phase, so that the permanent magnet performance of the alloy is greatly enhanced, the magnetic performance of a magnet is effectively improved, and the coercive force performance of the magnet is obviously improved;
2. according to the component proportion, the Curie temperature of the finally prepared magnet reaches 240 ℃, the Curie temperature is obviously improved, and the application value of the magnet is improved;
3. due to the use of the niobium-iron alloy, the production process cost of the neodymium iron boron product is greatly reduced, and the production quality and the production efficiency of the product are improved;
4. the use of the antioxidant 1010 and the antioxidant 1076 is beneficial to improving the corrosion resistance of the magnet;
5. the preparation method of the neodymium iron boron magnetic material greatly improves the coercive force of the magnet, and the Curie temperature of the prepared magnet reaches 240 ℃, so that the application range is remarkably improved.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A neodymium iron boron magnetic material comprises the following components in parts by weight: 29 parts of praseodymium-neodymium alloy, 3 parts of dysprosium-iron alloy, 3 parts of ferroboron alloy, 0.6 part of ferroniobium alloy, 5 parts of yttrium-iron alloy, 1.0 part of nano silicon dioxide, 0.1 part of gallium, 0.5 part of aluminum oxide, 1 part of antioxidant and the balance of iron. The antioxidant is a mixture of antioxidant 1010 and antioxidant 1076, wherein the weight part ratio of the antioxidant 1010 to the antioxidant 1076 is 1:1, and the particle size of the silicon dioxide is 45 nm.
A preparation method of a neodymium iron boron magnetic material comprises the following steps:
step one, batching: weighing raw materials according to the weight parts of the components in the neodymium iron boron magnetic material, mixing the components together, and after the material mixing is finished;
smelting an alloy in a second step: putting the raw materials prepared in the step one into an intermediate frequency vacuum smelting furnace for smelting, and vacuumizing 1 x 10-1Pa, controlling the temperature of the smelting furnace within 1500 ℃, simultaneously filling argon into the smelting furnace for protection, and cooling after smelting to form neodymium iron boron blocks;
step three, hydrogen crushing: putting the neodymium iron boron block into a hydrogen crushing furnace for hydrogen explosion, and vacuumizing for 1 x 10-1Pa, controlling the temperature to be 250 ℃, injecting hydrogen to allow the raw material to absorb hydrogen for 3 hours, then heating to 700 ℃, carrying out dehydrogenation, and finally cooling and discharging;
step four, pulverizing: crushing the product obtained in the third step into fine powder particles with the particle size of 2 microns in an airflow mill;
step five, orientation forming: mixing the fine powder particles in a mixer for 5 hours, putting the mixture into a mould, orienting the mixture in a magnetic field with the magnetic field intensity of 1.8T, and pressing the mixture to form a blank;
step six, sintering: pre-sintering the blank piece in the step five for 2 hours at 500 ℃ under a vacuum condition, and then sintering the blank piece in a vacuum furnace for 6 hours at 1200 ℃;
and seventhly, tempering: and (3) preserving heat for 5 hours at 800 ℃, preserving heat for 5 hours at 500 ℃, cooling in air, cutting, polishing, and performing surface passivation and plating treatment to obtain a finished product 1 of the neodymium iron boron magnetic material. The plating layer on the surface of the product generally comprises one or more of zinc plating, nickel plating, environment-friendly zinc plating, environment-friendly nickel plating, nickel-copper-nickel plating and environment-friendly nickel-copper-nickel plating.
The properties of the ndfeb magnetic material obtained in this example 1 are shown in table 1.
Example 2
A neodymium iron boron magnetic material comprises the following components in parts by weight: 31 parts of praseodymium-neodymium alloy, 5 parts of dysprosium-iron alloy, 5 parts of ferroboron alloy, 0.7 part of ferroniobium alloy, 6 parts of yttrium-iron alloy, 2 parts of nano silicon dioxide, 0.2 part of gallium, 0.8 part of aluminum oxide, 1.5 parts of antioxidant and the balance of iron. The antioxidant is a mixture of antioxidant 1010 and antioxidant 1076, wherein the weight part ratio of the antioxidant 1010 to the antioxidant 1076 is 1:2, and the particle size of the silicon dioxide is 60 nm.
A preparation method of a neodymium iron boron magnetic material comprises the following steps:
step one, batching: weighing raw materials according to the weight parts of the components in the neodymium iron boron magnetic material, mixing the components together, and after the material mixing is finished;
smelting an alloy in a second step: putting the raw materials prepared in the step one into an intermediate frequency vacuum smelting furnace for smelting, and vacuumizing 1 x 10-1Pa, controlling the temperature of the smelting furnace within 1800 ℃, simultaneously filling nitrogen into the smelting furnace for protection, and cooling after smelting to form neodymium iron boron blocks;
step three, hydrogen crushing: putting the neodymium iron boron block into a hydrogen crushing furnace for hydrogen explosion, and vacuumizing for 1 x 10-1Pa, controlling the temperature at 280 ℃, injecting hydrogen to allow the raw material to absorb hydrogen for 3 hours, then heating to 750 ℃, carrying out dehydrogenation, and finally cooling and discharging;
step four, pulverizing: crushing the product obtained in the third step into fine powder particles with the particle size of 2.3 mu m in an airflow mill;
step five, orientation forming: mixing the fine powder particles in a mixer for 7 hours, putting the mixture into a mould, orienting the mixture in a magnetic field with the magnetic field intensity of 1.8T, and pressing the mixture to form a blank;
step six, sintering: pre-sintering the blank piece in the step five for 2 hours at 500 ℃ under a vacuum condition, and sintering the blank piece in a vacuum furnace for 7 hours at 1200 ℃;
and seventhly, tempering: and (3) preserving heat for 6 hours at 900 ℃, preserving heat for 6 hours at 550 ℃, cooling in air, cutting and polishing, and performing surface passivation and plating treatment to obtain a finished product 2 of the neodymium iron boron magnetic material. The plating layer on the surface of the product generally comprises one or more of zinc plating, nickel plating, environment-friendly zinc plating, environment-friendly nickel plating, nickel-copper-nickel plating and environment-friendly nickel-copper-nickel plating.
The properties of the neodymium iron boron magnetic material obtained in this example 2 are shown in table 1.
Example 3
A neodymium iron boron magnetic material comprises the following components in parts by weight: 33 parts of praseodymium-neodymium alloy, 6 parts of dysprosium-iron alloy, 7 parts of ferroboron alloy, 0.8 part of ferroniobium alloy, 8 parts of yttrium-iron alloy, 2.5 parts of nano silicon dioxide, 0.3 part of gallium, 1 part of aluminum oxide, 2 parts of antioxidant and the balance of iron. The antioxidant is a mixture of antioxidant 1010 and antioxidant 1076, wherein the weight part ratio of the antioxidant 1010 to the antioxidant 1076 is 1:3, and the particle size of the silicon dioxide is 80 nm.
A preparation method of a neodymium iron boron magnetic material comprises the following steps:
step one, batching: weighing raw materials according to the weight parts of the components in the neodymium iron boron magnetic material, mixing the components together, and after the material mixing is finished;
smelting an alloy in a second step: putting the raw materials prepared in the step one into an intermediate frequency vacuum smelting furnace for smelting, and vacuumizing 1 x 10-1Pa, controlling the temperature of the smelting furnace within 2000 ℃, simultaneously filling argon into the smelting furnace for protection, and cooling after smelting to form neodymium iron boron blocks;
step three, hydrogen crushing: putting the neodymium iron boron block into a hydrogen crushing furnace for hydrogen explosion, and vacuumizing for 1 x 10-1Pa, controlling the temperature to 300 ℃, injecting hydrogen to allow the raw material to absorb hydrogen for 3 hours, then heating to 800 ℃, carrying out dehydrogenation, and finally cooling and discharging;
step four, pulverizing: crushing the product obtained in the third step into fine powder particles with the particle size of 3 mu m in an airflow mill;
step five, orientation forming: mixing the fine powder particles in a mixer for 8 hours, putting the mixture into a mould, orienting the mixture in a magnetic field with the magnetic field intensity of 1.8T, and pressing the mixture to form a blank;
step six, sintering: pre-sintering the blank piece in the fifth step for 2 hours at 500 ℃ under vacuum, and sintering the blank piece in a vacuum furnace for 8 hours at 1200 ℃;
and seventhly, tempering: and (3) after the temperature is kept at 1000 ℃ for 8 hours, then the temperature is kept at 600 ℃ for 8 hours, and after air cooling, cutting and polishing are carried out, and then surface passivation and plating treatment are carried out, thus obtaining the finished product 3 of the neodymium iron boron magnetic material. The plating layer on the surface of the product generally comprises one or more of zinc plating, nickel plating, environment-friendly zinc plating, environment-friendly nickel plating, nickel-copper-nickel plating and environment-friendly nickel-copper-nickel plating.
Comparative example 1
The composition of the ndfeb magnetic material of comparative example 1 is substantially the same as that of example 1, except that: 1.0 part of nano silicon dioxide is removed from the components of the neodymium iron boron magnetic material in the embodiment 1, and other components are kept unchanged, so that the components of the neodymium iron boron magnetic material in the comparative example 1 in parts by weight are obtained.
The preparation method of the neodymium iron boron magnetic material of the comparative example 1 is the same as that of the neodymium iron boron magnetic material of the example 1, and a neodymium iron boron magnetic material finished product 4 is finally obtained.
Comparative example 2
The composition of the ndfeb magnetic material of comparative example 2 is substantially the same as that of example 1, except that: and (3) removing 0.6 part of niobium-iron alloy from the components of the neodymium-iron-boron magnetic material in the embodiment 1, and keeping other components unchanged to obtain the components of the neodymium-iron-boron magnetic material in the comparative example 2 in parts by weight.
The preparation method of the neodymium iron boron magnetic material of the comparative example 2 is the same as that of the neodymium iron boron magnetic material of the example 1, and a neodymium iron boron magnetic material finished product 5 is finally obtained.
The finished nd-fe-b magnetic materials prepared in examples 1-3 and comparative examples 1-2 were respectively tested for magnetic properties using an NIM-10000H rare earth permanent magnet non-destructive tester, and the test results are shown in table 1 below.
TABLE 1 nd-fe-b magnetic material Performance Table
As can be seen from table 1, the technical effect of the neodymium iron boron magnetic material obtained by the present invention is that the nano silicon dioxide and the niobic alloy are added in the neodymium iron boron magnetic material, and meanwhile, the praseodymium neodymium alloy is mainly used in the component ratio, such that the curie temperature is significantly increased, the coercive force of the neodymium iron boron magnetic material is increased, and the application value thereof is improved.
The above embodiments are only some examples of the present invention, and the present invention is not limited thereto in any way, and any simple modification, equivalent change and modification to the above embodiments according to the technical spirit of the present invention are within the technical scope of the present invention.
Claims (5)
1. The neodymium-iron-boron magnetic material is characterized by comprising the following components in parts by weight: 29-33 parts of praseodymium-neodymium alloy, 3-6 parts of dysprosium-iron alloy, 3-7 parts of ferroboron alloy, 0.6-0.8 part of ferroniobium alloy, 5-8 parts of yttrium-iron alloy, 1.0-2.5 parts of nano silicon dioxide, 0.1-0.3 part of gallium, 0.5-1 part of aluminum oxide, 1-2 parts of antioxidant and the balance of iron, wherein the particle size of the silicon dioxide is 45-80 nm.
2. The neodymium-iron-boron magnetic material of claim 1: the method is characterized in that: comprises the following components in parts by weight: 31 parts of praseodymium-neodymium alloy, 5 parts of dysprosium-iron alloy, 5 parts of ferroboron alloy, 0.7 part of ferroniobium alloy, 6 parts of yttrium-iron alloy, 2 parts of nano silicon dioxide, 0.2 part of gallium, 0.8 part of aluminum oxide, 1.5 parts of antioxidant and the balance of iron.
3. A neodymium-iron-boron magnetic material according to claim 1 or 2: the method is characterized in that: the antioxidant is a mixture of an antioxidant 1010 and an antioxidant 1076, wherein the weight part ratio of the antioxidant 1010 to the antioxidant 1076 is 1: 1-3.
4. A method of preparing the neodymium iron boron magnetic material according to claim 1, characterized by comprising the following steps:
step one, batching: weighing raw materials according to the weight parts of the components in the neodymium iron boron magnetic material, mixing the components together, and after the material mixing is finished;
smelting an alloy in a second step: putting the raw materials prepared in the step one into an intermediate frequency vacuum smelting furnace for smelting, and vacuumizing 1 x 10- 1Pa, controlling the temperature of the smelting furnace within the range of 1500-2000 ℃, simultaneously filling inert gas into the smelting furnace for protection, and cooling after smelting to form neodymium iron boron blocks;
step three, hydrogen crushing: putting the neodymium iron boron block into a hydrogen crushing furnace for hydrogen explosion, and vacuumizing for 1 x 10-1Pa, controlling the temperature at 250-plus-300 ℃, injecting hydrogen to allow the raw material to absorb hydrogen for 3h, then heating to 700-plus-800 ℃, carrying out dehydrogenation, and finally cooling and discharging from the furnace;
step four, pulverizing: crushing the product obtained in the third step into fine powder particles with the particle size of 2-3 mu m in an airflow mill;
step five, orientation forming: mixing the fine powder particles in a mixer for 5-8 hours, putting the mixture into a mould, orienting the mixture in a magnetic field with the magnetic field intensity of 1.8T, and pressing the mixture to form a blank;
step six, sintering: pre-sintering the blank piece in the step five for 2 hours at 500 ℃ under a vacuum condition, and sintering the blank piece in a vacuum furnace for 6 to 8 hours at 1200 ℃;
and seventhly, tempering: preserving heat for 5-8 hours at 800-1000 ℃, preserving heat for 5-8 hours at 500-600 ℃, after air cooling, cutting and polishing, and then carrying out surface passivation and plating treatment to obtain the finished product of the neodymium iron boron magnetic material.
5. The method for preparing neodymium iron boron magnetic material according to claim 4, characterized in that: in the step two alloy smelting process, the inert gas is argon or nitrogen.
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