CN107845467B - Sintered neodymium-iron-boron magnetic steel and preparation method thereof - Google Patents
Sintered neodymium-iron-boron magnetic steel and preparation method thereof Download PDFInfo
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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
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01F41/0266—Moulding; Pressing
Abstract
The invention discloses sintered neodymium-iron-boron magnetic steel which comprises the following components: rare earth element R: 27.5-30.5 wt%, Al: 0.5-1.0 wt%, Pr: 0.03-0.06 wt%; c: 0.03 to 0.06 wt%, Cu: 0.35 to 0.5 wt%, Nd: 0.08 to 0.12 wt%, Ga: 0.2-0.4 wt%, Pm: 0.2-0.5 wt%, Co: 0.6-1.2 wt%, B: 0.75-1.35 wt%, the balance being Fe; the rare earth element R is a mixture of Ce, Ho, Sm, Dy and Tm, and the mass ratio of the mixture of Ce, Ho, Sm, Dy and Tm is 5: 4: 1: 0.3: 2. Simultaneously discloses a preparation method of the compound, and the preparation method is easy to operate; ho and rare earth elements such as Ce, Sm, Dy and Tm are added to replace part of expensive Nd and Pr, so that the cost is reduced, and the corrosion resistance of the sintered neodymium-iron-boron magnetic steel can be effectively improved and the weight loss is reduced due to the addition of Ho; the eutectic temperature of Ce replacing Nd is reduced, so that the sintering tempering temperature is reduced, the cost is saved, and the better performance is kept.
Description
Technical Field
The invention relates to sintered neodymium iron boron magnetic steel, in particular to sintered neodymium iron boron magnetic steel and a preparation method thereof.
Background
Because of its excellent magnetic properties, sintered nd-fe-b has been applied to new energy fields such as wind power generation and new energy automobiles in recent years, and has become one of the key materials for promoting the rapid development of new energy industries. The mass of the rare earth elements in the sintered neodymium-iron-boron permanent magnet accounts for about 30%, and at present, with the continuous expansion of the rare earth permanent magnet industry in China, the reserves of precious resources of rare earth in China are less and less, so that the prices of main rare earth metals such as praseodymium, neodymium, dysprosium and the like for manufacturing the sintered neodymium-iron-boron are higher and higher, the production cost of the sintered neodymium-iron-boron magnetic steel is greatly increased, and the development of the industry is greatly restricted. Therefore, the performance of the sintered neodymium-iron-boron magnetic steel is maintained, and meanwhile, the rare earth with low price is selected for partial substitution, so that the method has very important economic significance and social benefit.
Disclosure of Invention
The invention mainly aims to provide sintered neodymium iron boron magnetic steel which is low in cost, good in product performance and simple and convenient in preparation process and a preparation method thereof.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows: the composition consists of the following components: rare earth element R: 27.5-30.5 wt%, Al: 0.5-1.0 wt%, Pr: 0.03 to 0.06 wt%, C: 0.03 to 0.06 wt%, Cu: 0.35 to 0.5 wt%, Nd: 0.08 to 0.12 wt%, Ga: 0.2-0.4 wt%, Pm: 0.2-0.5 wt%, Co: 0.6-1.2 wt%, B: 0.75-1.35 wt%, the balance being Fe; the rare earth element R is a mixture of Ce, Ho, Sm, Dy and Tm, and the mass ratio of the mixture of Ce, Ho, Sm, Dy and Tm is 5: 4: 1: 0.3: 2.
The preparation method of the sintered neodymium iron boron magnetic steel comprises the following steps:
the first step is as follows: mixing rare earth elements, namely removing surface rusts and impurities from raw material blocks of Ce, Ho, Sm, Dy and Tm, crushing the raw material blocks into small blocks with the maximum length, width and thickness of less than 40mm, grinding the small blocks into powder, and uniformly mixing the small blocks in a mass ratio of Ce to Ho to Sm to Dy to Tm of 5: 4: 1: 0.2: 2 for later use;
the second step is that: proportioning, namely removing surface rusts and impurities from raw material blocks of all components except the rare earth element R, crushing the raw material blocks into small blocks with the maximum length, the width and the thickness of less than 40mm, and weighing the small blocks according to a specified proportion for later use;
the third step: smelting, namely putting the small blocks of the raw materials obtained in the second step into a vacuum smelting furnace, heating and smelting after the vacuum degree is lower than 5pa, firstly heating to 550-650 ℃ for smelting for 8-15min, stopping heating, filling inert gas until the internal pressure in the smelting furnace is 0.05-0.08MPa, and heating to 1400-1500 ℃ for smelting for 10-15 min;
the fourth step: casting ingots, pouring the smelting liquid obtained in the third step into a cold ingot mold with the depth of 0.2-0.5mm, and cooling and forming to obtain neodymium iron boron alloy sheets;
the fifth step: preparing powder, namely putting the neodymium iron boron alloy sheet obtained in the step four into a hydrogen breaking furnace, absorbing hydrogen under 0.1Mpa for saturation, and dehydrogenating at 500-600 ℃ to obtain coarse powder; adding a lubricant into the coarse powder, and grinding the mixture into powder with the average particle size of 2.6-3.4um in a jet mill;
and a sixth step: molding, under the protection of inert gas, powder is molded in a mold with the magnetic field intensity of a press machine more than 1.5-1.7 Tesla to obtain a neodymium iron boron magnetic steel blank with the molding density of 3.5-4.0g/cm3;
The seventh step: and (3) improving the density: placing the vacuum-packaged neodymium iron boron magnetic steel blank under the pressure of 190-210MPa, and further improving the density of the neodymium iron boron magnetic steel blank by using isostatic pressing;
eighth step: sintering and tempering, namely placing the neodymium iron boron magnetic steel blank obtained in the seventh step in an inert gas protection box, introducing inert gas for 20min, then moving the blank into a vacuum sintering furnace for degassing, raising the temperature to 1000-1020 ℃, and preserving the heat for 3-4 hours for carrying out densification sintering; and (3) filling inert gas after sintering, cooling to 100 ℃, then raising the temperature to 850-class 900 ℃, preserving the heat for 1.5-2.5 hours for primary tempering, cooling the inert gas to 80-90 ℃ after heat preservation, raising the temperature to 470-class 500 ℃, preserving the heat for 4.5-5.5 hours for secondary tempering, filling the inert gas after heat preservation, cooling to below 100 ℃, and discharging to obtain the sintered neodymium-iron-boron magnetic steel.
The inert gas is argon or nitrogen; the lubricant is a special lubricant for sintering neodymium iron boron.
Wherein Ho is a rare earth metal with lower price compared with expensive rare earths such as Pr, Nd, Dy and the like. Ho replaces partial metal Pr-Nd, so that the intrinsic coercive force of the sintered Nd-Fe-B permanent magnet can be effectively improved, and Nd can be effectively promoted2Fe14The directional growth of the B main phase crystal grains ensures that the densification degree of the sintered Nd-Fe-B permanent magnet is higher, thereby improving the performance. Ce is a rare earth element with the largest content on the earth and is also the element with the lowest price, and the high-performance Nd-Ce-Fe-B sintered permanent magnet prepared by partially replacing Nd by utilizing Ce and optimizing the preparation process has very important significance. The corrosion resistance of the neodymium iron boron is improved to a certain extent by adding the Er; the addition of Sm improves the magnetism of the neodymium iron boron. The optimal proportion summarized after multiple tests is the mass ratio of the rare earth elements Ce to Ho to Sm to Dy to Tm to 5 to 4 to 1 to 0.3 to 2, so that the performance of the neodymium-iron-boron magnetic steel is improved, and the production cost is effectively reduced.
The sintered neodymium-iron-boron magnetic steel has the technical effects that Ho and rare earth elements such as Ce, Sm, Dy and Tm are added to replace part of expensive Nd and Pr, so that the cost is reduced, the corrosion resistance of the sintered neodymium-iron-boron magnetic steel can be effectively improved by adding Ho, and the weight loss is reduced; the eutectic temperature of Ce replacing Nd is reduced, so that the sintering tempering temperature is reduced, the cost is saved, and the better performance is kept.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
Example 1: the sintered neodymium iron boron magnetic steel provided by the embodiment is composed of the following components: rare earth element R: 30 wt%, Al: 0.8 wt%, Pr: 0.04 wt%, C: 0.05 wt%, Cu: 0.5 wt%, Nd: 0.1 wt%, Ga: 0.3 wt%, Pm: 0.4 wt%, Co: 0.9 wt%, B: 0.95 wt% and the balance Fe; the rare earth element R is a mixture of Ce, Ho, Sm, Dy and Tm, and the mass ratio of the mixture of Ce, Ho, Sm, Dy and Tm is 5: 4: 1: 0.3: 2.
The preparation method of the sintered neodymium iron boron magnetic steel comprises the following steps:
the first step is as follows: mixing rare earth elements, namely removing surface rusts and impurities from raw material blocks of Ce, Ho, Sm, Dy and Tm, crushing the raw material blocks into small blocks with the maximum length, width and thickness of less than 40mm, grinding the small blocks into powder, and uniformly mixing the small blocks in a mass ratio of Ce to Ho to Sm to Dy to Tm of 5: 4: 1: 0.2: 2 for later use;
the second step is that: proportioning, namely removing surface rusts and impurities from raw material blocks of all components except the rare earth element R, crushing the raw material blocks into small blocks with the maximum length, the width and the thickness of less than 40mm, and weighing the small blocks according to a specified proportion for later use;
the third step: smelting, namely putting the small blocks of the raw materials obtained in the second step into a vacuum smelting furnace, heating and smelting after the vacuum degree is lower than 5pa, firstly heating to 600 ℃ for smelting for 10min, stopping heating, filling inert gas until the internal pressure in the smelting furnace is 0.06MPa, and heating to 1450 ℃ for smelting for 15 min;
the fourth step: casting ingots, pouring the smelting liquid obtained in the third step into a cold ingot mold with the depth of 0.4mm, and cooling and forming to obtain neodymium iron boron alloy sheets;
the fifth step: preparing powder, namely putting the neodymium iron boron alloy sheet obtained in the step four into a hydrogen breaking furnace, absorbing hydrogen under 0.1Mpa for saturation, and dehydrogenating at 550 ℃ to obtain coarse powder; adding a lubricant into the coarse powder, and grinding the mixture into powder with the average particle size of 3.0um in a jet mill;
and a sixth step: molding, under the protection of inert gas, molding the powder in a mold with the magnetic field intensity of a press machine more than 1.5 Tesla to obtain a neodymium iron boron magnetic steel blank with the molding density of 3.6g/cm3;
The seventh step: and (3) improving the density: placing the vacuum-packaged neodymium iron boron magnetic steel blank under the pressure of 200MPa, and further improving the density of the neodymium iron boron magnetic steel blank by using isostatic pressing;
eighth step: sintering and tempering, namely placing the neodymium iron boron magnetic steel blank obtained in the seventh step in an inert gas protection box, introducing inert gas for 20min, moving the blank into a vacuum sintering furnace for degassing, raising the temperature to 1000 ℃, and preserving the heat for 3 hours for densification sintering; and (3) filling inert gas after sintering, cooling to 100 ℃, then heating to 850 ℃, preserving heat for 2 hours for primary tempering, cooling to 85 ℃ after heat preservation, heating to 480 ℃, preserving heat for 4.5 hours for secondary tempering, filling inert gas after heat preservation, cooling to below 100 ℃, discharging, and thus obtaining the sintered neodymium-iron-boron magnetic steel. The inert gas is argon or nitrogen; the lubricant is a special lubricant for sintering neodymium iron boron.
The product obtained is 20mm multiplied by 15mm multiplied by 1.5mm, and the magnetic performance is tested by adopting a NIM2000 magnetic tester of China measurement institute, and the result is shown in Table 1.
Example 2:
the preparation method of the sintered ndfeb magnetic steel provided by the embodiment is completely the same as that of embodiment 1, and the main difference lies in that the raw material components are different in mass percentage, and the ndfeb magnetic steel in the embodiment is composed of the following components: rare earth element R: 28.5 wt%, Al: 0.8 wt%, Pr: 0.04 wt%, C: 0.05 wt%, Cu: 0.5 wt%, Nd: 0.08 wt%, Ga: 0.3 wt%, Pm: 0.4 wt%, Co: 0.9 wt%, B: 0.95 wt% and the balance Fe; the rare earth element R is a mixture of Ce, Ho, Sm, Dy and Tm, and the mass ratio of the mixture of Ce, Ho, Sm, Dy and Tm is 5: 4: 1: 0.3: 2.
The product obtained is 20mm multiplied by 15mm multiplied by 1.5mm, and the magnetic performance is tested by adopting a NIM2000 magnetic tester of China measurement institute, and the result is shown in Table 1.
Example 3:
the preparation method of the sintered ndfeb magnetic steel provided by the embodiment is completely the same as that of embodiment 1, and the main difference lies in that the raw material components are different in mass percentage, and the ndfeb magnetic steel in the embodiment is composed of the following components: rare earth element R: 29.5 wt%, Al: 0.8 wt%, Pr: 0.04 wt%, C: 0.05 wt%, Cu: 0.5 wt%, Nd: 0.1 wt%, Ga: 0.3 wt%, Pm: 0.4 wt%, Co: 0.9 wt%, B: 0.95 wt% and the balance Fe; the rare earth element R is a mixture of Ce, Ho, Sm, Dy and Tm, and the mass ratio of the mixture of Ce, Ho, Sm, Dy and Tm is 5: 4: 1: 0.3: 2.
Taking the product with the diameter of 20mm multiplied by 15mm multiplied by 1.5mm, and adopting a NIM2000 magnetic tester of China measurement institute to carry out magnetic performance test; meanwhile, a piece of common neodymium iron boron magnetic steel on the market with the thickness of 20mm multiplied by 15mm multiplied by 1.5mm is taken, and the result is shown in table 1.
Table 1:
remanence/KGs | Magnetic energy product/MGOe | Intrinsic coercivity/KOe | |
Example 1 | 13.23 | 42.05 | 12.94 |
Example 2 | 12.91 | 40.47 | 12.87 |
Example 3 | 13.15 | 41.22 | 12.90 |
Ordinary Nd-Fe-B magnetic steel in market | 12.77 | 38.66 | 11.65 |
The test results show that the coercive force and the magnetic energy product of the sintered neodymium iron boron magnetic steel are obviously higher than those of the sintered neodymium iron boron magnetic steel in the prior art, and the performance of the product is improved while the sintering cost is reduced.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (3)
1. The utility model provides a sintering neodymium iron boron magnetic steel which characterized in that: the composition consists of the following components: rare earth element R: 27.5-30.5 wt%, Al: 0.5-1.0 wt%, Pr: 0.03-0.06 wt%; c: 0.03 to 0.06 wt%, Cu: 0.35 to 0.5 wt%, Nd: 0.08 to 0.12 wt%, Ga: 0.2-0.4 wt%, Pm: 0.2-0.5 wt%, Co: 0.6-1.2 wt%, B: 0.75-1.35 wt%, the balance being Fe; the rare earth element R is a mixture of Ce, Ho, Sm, Dy and Tm, and the mass ratio of the mixture of Ce, Ho, Sm, Dy and Tm is 5: 4: 1: 0.3: 2.
2. The method for preparing sintered NdFeB magnetic steel according to claim 1, comprising the following steps:
the first step is as follows: mixing rare earth elements, namely removing surface rusts and impurities from raw material blocks of Ce, Ho, Sm, Dy and Tm, crushing the raw material blocks into small blocks with the maximum length, width and thickness of less than 40mm, grinding the small blocks into powder, and uniformly mixing the small blocks in a mass ratio of Ce to Ho to Sm to Dy to Tm of 5: 4: 1: 0.3: 2 for later use;
the second step is that: proportioning, namely removing surface rusts and impurities from raw material blocks of all components except the rare earth element R, crushing the raw material blocks into small blocks with the maximum length, the width and the thickness of less than 40mm, and weighing the small blocks according to a specified proportion for later use;
the third step: smelting, namely putting the raw material mixture obtained in the two steps into a vacuum smelting furnace, heating and smelting after the vacuum degree is lower than 5pa, firstly heating to 550-650 ℃ for smelting for 8-15min, stopping heating, filling inert gas until the internal pressure in the smelting furnace is 0.05-0.08MPa, and heating to 1400-1500 ℃ for smelting for 10-15 min;
the fourth step: casting ingots, pouring the smelting liquid obtained in the third step into a cold ingot mold with the depth of 0.2-0.5mm, and cooling and forming to obtain neodymium iron boron alloy sheets;
the fifth step: preparing powder, namely putting the neodymium iron boron alloy sheet obtained in the step four into a hydrogen breaking furnace, absorbing hydrogen under 0.1Mpa for saturation, and dehydrogenating at 500-600 ℃ to obtain coarse powder; adding a lubricant into the coarse powder, and grinding the mixture into powder with the average particle size of 2.6-3.4um in a jet mill;
and a sixth step: molding, under the protection of inert gas, the powder is molded in a mold with the magnetic field intensity of 1.5-1.7 Tesla of a press to obtain a neodymium iron boron magnetic steel blank with the molding density of 3.5-4.0g/cm3;
The seventh step: and (3) improving the density: placing the vacuum-packaged neodymium iron boron magnetic steel blank under the pressure of 190-210MPa, and further improving the density of the neodymium iron boron magnetic steel blank by using isostatic pressing;
eighth step: sintering and tempering, namely placing the neodymium iron boron magnetic steel blank obtained in the seventh step in an inert gas protection box, introducing inert gas for 20min, then moving the blank into a vacuum sintering furnace for degassing, raising the temperature to 1000-1020 ℃, and preserving the heat for 3-4 hours for carrying out densification sintering; and (3) filling inert gas after sintering, cooling to 100 ℃, then raising the temperature to 850-class 900 ℃, preserving the heat for 1.5-2.5 hours for primary tempering, cooling the inert gas to 80-90 ℃ after heat preservation, raising the temperature to 470-class 500 ℃, preserving the heat for 3.5-4 hours for secondary tempering, filling the inert gas after heat preservation, cooling to below 100 ℃, and discharging to obtain the sintered neodymium-iron-boron magnetic steel.
3. A method for preparing sintered ndfeb magnetic steel according to claim 2, characterized in that: the inert gas is argon or nitrogen; the lubricant is a special lubricant for sintering neodymium iron boron.
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